Nitrate-to-Nitrite-to-Nitric Oxide Conversion Modulated by Nitrate-Containing {Fe(NO)2}9 Dinitrosyl Iron Complex (DNIC)
Fu-Te Tsai; Yu-Ching Lee; Ming-Hsi Chiang; Wen-Feng Liaw; Inorganic Chemistry 52 (2013) 464–473; doi:10.1021/ic3023437

data_4331774
_publ_section_title
;
 Nitrate-to-Nitrite-to-Nitric Oxide Conversion Modulated by
 Nitrate-Containing {Fe(NO)2}9 Dinitrosyl Iron Complex (DNIC)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              464
_journal_page_last               473
_journal_paper_doi               10.1021/ic3023437
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C36 H30 Fe0.5 N3 O6 P2'
_chemical_formula_weight         690.49
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 109.8290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.6357(4)
_cell_length_b                   20.3175(4)
_cell_length_c                   20.8288(5)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3456
_cell_measurement_theta_min      2.2770
_cell_volume                     6622.6(3)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29394
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       Lump
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0767P)^2^+3.9646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                6137
_reflns_number_total             6763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3023437_si_003_1.cif
_cod_data_source_block           100549lt_0m
_cod_original_formula_sum        'C36 H30 Fe0.50 N3 O6 P2'
_cod_database_code               4331774