Nitrogen Oxide Atom-Transfer Redox Chemistry; Mechanism of NO(g) to Nitrite Conversion Utilizing μ-oxo Heme-Fe(III)-O-Cu(II)(L) Constructs.
Hematian, Shabnam; Kenkel, Isabell; Shubina, Tatyana E.; Dürr, Maximilian; Liu, Jeffrey J.; Siegler, Maxime A.; Ivanovic-Burmazovic, Ivana; Karlin, Kenneth D.; Journal of the American Chemical Society 137 (2015) 6602–6615; doi:10.1021/jacs.5b02174

data_4123603
_publ_section_title
;
 Nitrogen Oxide Atom-Transfer Redox Chemistry; Mechanism of NO(g) to
 Nitrite Conversion Utilizing \m-oxo Heme-Fe(III)-O-Cu(II)(L) Constructs.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6602
_journal_page_last               6615
_journal_paper_doi               10.1021/jacs.5b02174
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'2(C66 H54 Cu Fe N8 O5), 2(C24 B F20), 3(C7 H8)'
_chemical_formula_sum            'C201 H132 B2 Cu2 F40 Fe2 N16 O10'
_chemical_formula_weight         3951.63
_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                91.5300(12)
_cell_angle_beta                 97.5727(14)
_cell_angle_gamma                112.0953(15)
_cell_formula_units_Z            1
_cell_length_a                   13.4443(2)
_cell_length_b                   16.3732(2)
_cell_length_c                   25.7041(4)
_cell_measurement_reflns_used    37226
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.92
_cell_measurement_theta_min      4.17
_cell_volume                     5178.94(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3875
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            61250
_diffrn_reflns_theta_full        71.90
_diffrn_reflns_theta_max         71.90
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2010
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
;
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.00042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1544
_refine_ls_number_reflns         20331
_refine_ls_number_restraints     1057
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+1.7309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                19196
_reflns_number_total             20331
_reflns_threshold_expression     I>\s(I)
_cod_data_source_file            ja5b02174_si_003.cif
_cod_data_source_block           '[(TMPP)FeIII-O-CuII(tmpa)][B(C6F5)4'
_cod_depositor_comments
'Adding full bibliography for 4123603--4123605.cif.'
_cod_original_cell_volume        5178.93(13)
_cod_database_code               4123603