A Dinitrosyliron Complex within the Homoleptic Fe(NO)4 Anion: NO as Nitroxyl and Nitrosyl Ligands within a Single Structure
Zong-Sian Lin; Tzung-Wen Chiou; Kuan-Yu Liu; Chang-Chih Hsieh; Jen-Shiang K. Yu; Wen-Feng Liaw; Inorganic Chemistry 51 (2012) 10092–10094; doi:10.1021/ic3018437

data_4330533
_publ_section_title
;
 A Dinitrosyliron Complex within the Homoleptic Fe(NO)4 Anion: NO as
 Nitroxyl and Nitrosyl Ligands within a Single Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10092
_journal_page_last               10094
_journal_paper_doi               10.1021/ic3018437
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C36 H30 Fe N5 O4 P2'
_chemical_formula_weight         714.44
_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                72.133(2)
_cell_angle_beta                 80.266(2)
_cell_angle_gamma                87.330(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8887(4)
_cell_length_b                   11.7543(5)
_cell_length_c                   16.4900(6)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.55
_cell_volume                     1797.98(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23839
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'light red-brown'
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       columnar
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6269
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.355
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1425P)^2^+3.1510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2299
_refine_ls_wR_factor_ref         0.2569
_reflns_number_gt                4686
_reflns_number_total             6269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3018437_si_001.cif
_cod_data_source_block           2
_cod_original_cell_volume        1797.98(12)
_cod_database_code               4330533