MnII and CuII complexes with arylhydrazones of active methylene compounds as effective heterogeneous catalysts for solvent- and additive-free microwave-assisted peroxidative oxidation of alcohols
Mahmudov, Kamran T.; Sutradhar, Manas; Martins, Luísa M. D. R. S.; Guedes da Silva, M. Fátima C.; Ribera, Alice; Nunes, Ana V. M.; Gahramanova, Shahnaz I.; Marchetti, Fabio; Pombeiro, Armando J. L.; RSC Advances 5 (2015) 25979–; doi:10.1039/C5RA02667A

data_7235885
_publ_section_title
;
 MnII and CuII complexes with arylhydrazones of active methylene compounds
 as effective heterogeneous catalysts for solvent- and additive-free
 microwave-assisted peroxidative oxidation of alcohols
;
_journal_issue                   33
_journal_name_full               'RSC Advances'
_journal_page_first              25979
_journal_paper_doi               10.1039/C5RA02667A
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         '2(C9 H7 N4 O4 S), H12 Mn O6, 4(H2 O)'
_chemical_formula_sum            'C18 H34 Mn N8 O18 S2'
_chemical_formula_weight         769.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-09-06 deposited with the CCDC.
2015-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                85.652(3)
_cell_angle_beta                 82.940(3)
_cell_angle_gamma                76.401(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2288(4)
_cell_length_b                   9.9748(6)
_cell_length_c                   11.5954(6)
_cell_measurement_reflns_used    7963
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.67
_cell_measurement_theta_min      2.92
_cell_volume                     805.54(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury CSD 3.3'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II Photon 100'
_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  0.0254
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.702
_diffrn_reflns_theta_min         1.772
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       prism
_exptl_crystal_F_000             399
_exptl_crystal_recrystallization_method
'Slow evaporation of a methanol solution'
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^+0.2133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4434
_reflns_number_total             4954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra02667a2.cif
_cod_data_source_block           Compound1
_cod_database_code               7235885
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.880
_shelxl_version_number           2014-3
_shelx_res_checksum              23758
_shelx_hkl_checksum              21846