Halogen-bonded tris(2,4-bis(trichloromethyl)-1,3,5-triazapentadienato)-M(iii) [M = Mn, Fe, Co] complexes and their catalytic activity in the peroxidative oxidation of 1-phenylethanol to acetophenone
Shixaliyev, Namiq Q.; Gurbanov, Atash V.; Maharramov, Abel M.; Mahmudov, Kamran T.; Kopylovich, Maximilian N.; Martins, Luísa M. D. R. S.; Muzalevskiy, Vasily M.; Nenajdenko, Valentine G.; Pombeiro, Armando J. L.; New J. Chem. 38 (2014) 4807–; doi:10.1039/C4NJ00797B

data_7054307
_publ_section_title
;
 Halogen-bonded
 tris(2,4-bis(trichloromethyl)-1,3,5-triazapentadienato)-M(iii) [M = Mn,
 Fe, Co] complexes and their catalytic activity in the peroxidative
 oxidation of 1-phenylethanol to acetophenone
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              4807
_journal_paper_doi               10.1039/C4NJ00797B
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         'C12 H6 Cl18 Fe N9, 2(C2 H6 O S)'
_chemical_formula_sum            'C16 H18 Cl18 Fe N9 O2 S2'
_chemical_formula_weight         1126.48
_chemical_name_systematic
; 
 ? 
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.4670(10)
_cell_angle_beta                 76.0640(10)
_cell_angle_gamma                75.1320(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0591(4)
_cell_length_b                   13.5688(5)
_cell_length_c                   16.6349(6)
_cell_measurement_reflns_used    9558
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.26
_cell_volume                     2112.09(14)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24444
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1114
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.738
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         10409
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0749
_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^)+(0.06P)^2^+7P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.1888
_reflns_number_gt                7390
_reflns_number_total             10409
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4nj00797b2.cif
_cod_data_source_block           NM15
_cod_depositor_comments
'Adding full bibliography for 7054306--7054308.cif.'
_cod_database_code               7054307