Reaction of a Copper(II)-Nitrosyl Complex with Hydrogen Peroxide: Phenol Ring Nitration through a Putative Peroxynitrite Intermediate
Apurba Kalita; Ramesh C. Deka; Biplab Mondal; Inorganic Chemistry 52 (2013) 10897–10903; doi:10.1021/ic400890f

data_4336152
_publ_contact_author_address
;Indian Institute of Technology Guwahati
Assam-781039, India
;
_publ_contact_author_email       biplab@iitg.ernet.in
_publ_contact_author_name        'Dr. Biplab Mondal'
_publ_section_title
;
 Reaction of a Copper(II)-Nitrosyl Complex with Hydrogen Peroxide: Phenol
 Ring Nitration through a Putative Peroxynitrite Intermediate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10897
_journal_page_last               10903
_journal_paper_doi               10.1021/ic400890f
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_compound_source        Synthesised
_chemical_formula_sum            'C17 H24 Cl Cu N4 O9'
_chemical_formula_weight         527.39
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                89.6260(10)
_cell_angle_beta                 82.1540(10)
_cell_angle_gamma                76.9530(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8228(2)
_cell_length_b                   10.2640(2)
_cell_length_c                   11.3496(2)
_cell_measurement_reflns_used    9176
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     1103.96(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0969
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17450
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.166
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       cube
_exptl_crystal_F_000             542
_exptl_crystal_recrystallization_method 'Acetronitrile / DMF'
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5436
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0837P)^2^+0.6929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                4770
_reflns_number_total             5436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400890f_si_002.cif
_cod_data_source_block           complex-1
_cod_database_code               4336152