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_7056747
_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 Br3 N O2,Br, C2H6O'
_chemical_formula_sum            'C13 H13 Br4 N O3'
_chemical_formula_weight         550.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2017-10-22T17:55:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-10-24 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.134(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.353(5)
_cell_length_b                   14.954(8)
_cell_length_c                   13.404(7)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.77
_cell_measurement_wavelength     0.71073
_cell_volume                     1667.6(16)
_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    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17057
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.038
_diffrn_reflns_theta_min         2.045
_exptl_absorpt_coefficient_mu    9.66
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.028
_refine_ls_R_factor_gt           0.022
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+4.3780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0
_reflns_number_gt                3883
_reflns_number_total             4355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02725g2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7056747