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_4314386
_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(bipa)(OAc)(OCH3)(PF6)'
_chemical_formula_sum            'C19 H26 F6 Mn N6 O3 P'
_chemical_formula_weight         586.37
_chemical_melting_point          484
_chemical_name_common            manganese(III)(acetate)(methanolate)monomer
_chemical_name_systematic
; 
 manganese(acetato)(methoxide)(bis(N-methylimdazol-2-yl)-picolyl)
 hexafluorophosphate 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.55(3)
_cell_angle_beta                 71.63(3)
_cell_angle_gamma                75.65(3)
_cell_formula_units_Z            2
_cell_length_a                   8.945(2)
_cell_length_b                   11.336(2)
_cell_length_c                   12.647(3)
_cell_measurement_temperature    100(2)
_cell_volume                     1177.2(5)
_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 0.862
_diffrn_measured_fraction_theta_max 0.862
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6898
_diffrn_reflns_theta_full        71.33
_diffrn_reflns_theta_max         71.33
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    5.970
_exptl_absorpt_correction_type
'Program sadabs, SAINT software package, Bruker Nonius, Karlsruhe'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                2813
_reflns_number_total             3943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0347788si20030711_042806_2.cif
_cod_data_source_block           complex2
_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        1177.2(4)
_cod_database_code               4314386