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_4336174
_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         'C15 H14 Cu N2 O3 S, H2 O'
_chemical_formula_sum            'C15 H16 Cu N2 O4 S'
_chemical_formula_weight         383.90
_chemical_name_common            RM-5
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'Patterson methods'
_atom_sites_solution_secondary   'difference Fourier'
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 99.315(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.032(2)
_cell_length_b                   17.395(5)
_cell_length_c                   13.098(4)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.8
_cell_volume                     1581.0(8)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_publication_material  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS DUO'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25338
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.593
_diffrn_reflns_theta_min         1.963
_exptl_absorpt_coefficient_mu    1.534
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       needle
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0159P)^2^+1.3404P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4638
_reflns_number_total             4837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401295t_si_004.cif
_cod_data_source_block           mn2126
_cod_database_code               4336174
_shelx_estimated_absorpt_t_min   0.631
_shelx_estimated_absorpt_t_max   0.825
_diffrn_reflns_sigmai/neti       0.0113
_shelxl_version_number           2012-4
_shelx_res_checksum              28306