Nucleophile and Base Differentiation of Pyridine in Reaction with Tetrahalocatechols and the Formation of Manganese(III)-Catecholate and Pyridinium-Catecholate Complexes for the in situ Generation of Hydrogen Peroxide from Dioxygen
Bakewell, Nicholas Owen; Thavarajah, Rumintha; Motevalli, Majid; Sheriff, Tippu S.; New Journal of Chemistry  (2017) –; doi:10.1039/C7NJ02725G

data_7056745
_publ_section_title
;
 Nucleophile and Base Differentiation of Pyridine in Reaction with
 Tetrahalocatechols and the Formation of Manganese(III)-Catecholate and
 Pyridinium-Catecholate Complexes for the in situ Generation of Hydrogen
 Peroxide from Dioxygen
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/C7NJ02725G
_journal_year                    2017
_chemical_formula_moiety         'C11 H7 N O2 Cl4, C3 H8 O'
_chemical_formula_sum            'C14 H15 Cl4 N O3'
_chemical_formula_weight         387.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.874(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2167(7)
_cell_length_b                   14.4067(10)
_cell_length_c                   13.1603(9)
_cell_measurement_reflns_used    3717
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.62
_cell_volume                     1747.3(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2014.11.0.1'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17047
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.3756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                2761
_reflns_number_total             4337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02725g2.cif
_cod_data_source_block           RT_CL_1NIL
_cod_database_code               7056745
_shelx_res_checksum              11312