Thiolate S-Oxygenation Controls Nitric Oxide (NO) Photolability of a Synthetic Iron Nitrile Hydratase (Fe-NHase) Model Derived from Mixed Carboxamide/Thiolate Ligand
Michael J. Rose; Nolan M. Betterley; Pradip K. Mascharak; Journal of the American Chemical Society 131 (2009) 8340–8341; doi:10.1021/ja9004656

data_4104547
_publ_contact_author_address
;
Department of Chemistry and Biochemistry,
University of California, Santa Cruz,
1156 High Street,
Santa Cruz, CA 95064
USA
;
_publ_contact_author_email       pradip@chemsitry.ucsc.edu
_publ_contact_author_fax         '+1 831 459 2935'
_publ_contact_author_name        'Pradip Mascharak'
_publ_contact_author_phone       '+1 831 459 4251'
_publ_section_title
;
 Thiolate S-Oxygenation Controls Nitric Oxide (NO) Photolability of a
 Synthetic Iron Nitrile Hydratase (Fe-NHase) Model Derived from Mixed
 Carboxamide/Thiolate Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8340
_journal_page_last               8341
_journal_paper_doi               10.1021/ja9004656
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C27 H20 Cl2 Fe N5 O3 S2, C10 H20 N'
_chemical_formula_sum            'C35 H40 Cl2 Fe N6 O3 S2'
_chemical_formula_weight         783.60
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.72(3)
_cell_angle_beta                 82.65(3)
_cell_angle_gamma                88.48(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6049(19)
_cell_length_b                   9.6051(19)
_cell_length_c                   19.251(4)
_cell_measurement_reflns_used    4064
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.19
_cell_volume                     1747.1(6)
_computing_cell_refinement       'Bruker SAINT v7.33A'
_computing_data_collection       'Bruker APEX-II v2.1'
_computing_data_reduction        'Bruker SAINT v7.33A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       \w/2\q-scans
_diffrn_radiation_monochromator  'channel-cut Si-<111> crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.1262
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9014
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.9115
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sheldrick, 2008'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2233
_reflns_number_gt                3253
_reflns_number_total             4190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9004656_si_002_1.cif
_cod_data_source_block           dmapfeno
_cod_database_code               4104547