Copper Complexes Relevant to the Catalytic Cycle of Copper Nitrite Reductase: Electrochemical Detection of NO(g) Evolution and Flipping of NO2 Binding Mode upon CuII →CuI Reduction
Ram Chandra Maji; Suman Kumar Barman; Suprakash Roy; Sudip K. Chatterjee; Faye L. Bowles; Marilyn M. Olmstead; Apurba K. Patra; Inorganic Chemistry 52 (2013) 11084–11095; doi:10.1021/ic401295t

data_4336173
_publ_section_title
;
 Copper Complexes Relevant to the Catalytic Cycle of Copper Nitrite
 Reductase: Electrochemical Detection of NO(g) Evolution and Flipping of
 NO2 Binding Mode upon CuII \\rightarrow CuI Reduction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11084
_journal_page_last               11095
_journal_paper_doi               10.1021/ic401295t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C14 H15 Cl Cu N2 O6 S'
_chemical_formula_sum            'C14 H15 Cl Cu N2 O6 S'
_chemical_formula_weight         438.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.839(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6173(4)
_cell_length_b                   19.0453(11)
_cell_length_c                   11.2557(7)
_cell_measurement_reflns_used    4870
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      2.90
_cell_volume                     1617.65(16)
_computing_cell_refinement       'SAINT (Bruker, 2011)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT (Bruker, 2011)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18900
_diffrn_reflns_theta_full        31.53
_diffrn_reflns_theta_max         31.53
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2009)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.059
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5392
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0400P)^2^+1.2035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                5171
_reflns_number_total             9006
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic401295t_si_003.cif
_cod_data_source_block           mn2094tw
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4336173