Syntheses, Structures, and Reactivities of {Fe-NO}6 Nitrosyls Derived from Polypyridine-Carboxamide Ligands: Photoactive NO-Donors and Reagents for S-Nitrosylation of Alkyl Thiols
Raman K. Afshar; Apurba K. Patra; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 43 (2004) 5736–5743; doi:10.1021/ic040057c

data_4311473
_publ_section_title
;
 Syntheses, Structures, and Reactivities of {Fe-NO}6 Nitrosyls Derived
 from Polypyridine-Carboxamide Ligands: Photoactive NO-Donors and Reagents
 for S-Nitrosylation of Alkyl Thiols
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5736
_journal_page_last               5743
_journal_paper_doi               10.1021/ic040057c
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C24.5 H27.25 Cl2 Fe N7.75 O10'
_chemical_formula_weight         717.04
_chemical_name_common            '[Fe(PaNPy3)(NO)](ClO4)2.1.75CH3CN'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 93.221(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.665(5)
_cell_length_b                   18.429(6)
_cell_length_c                   21.460(7)
_cell_measurement_reflns_used    841
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      2.5
_cell_volume                     5791(3)
_computing_cell_refinement       'SMART 5.054 (Bruker, 2002)'
_computing_data_collection       'SMART 5.054 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28549
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  0.9549
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.500
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5938
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+81.0180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.1998
_reflns_number_gt                5002
_reflns_number_total             5938
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic040057c_2.cif
_cod_data_source_block           mn1521
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C24.50 H27.25 Cl2 Fe N7.75 O10'
_cod_database_code               4311473