A {Fe(NO)3}10 Trinitrosyliron Complex Stabilized by an N-Heterocyclic Carbene and the Cationic and Neutral {Fe(NO)2}9/10 Products of Its NO Release
Chung-Hung Hsieh; Marcetta Y. Darensbourg; Journal of the American Chemical Society 132 (2010) 14118–14125; doi:10.1021/ja104135x

data_4103197
_publ_section_title
;
 A {Fe(NO)3}10 Trinitrosyliron Complex Stabilized by an N-Heterocyclic
 Carbene and the Cationic and Neutral {Fe(NO)2}9/10 Products of Its NO
 Release
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14118
_journal_page_last               14125
_journal_paper_doi               10.1021/ja104135x
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C4.5 H9 B0.5 F2 Fe N2.5 O1.5 S'
_chemical_formula_weight         253.46
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.089(5)
_cell_length_b                   7.999(3)
_cell_length_c                   15.361(5)
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.55
_cell_volume                     1731.2(11)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19743
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  0.7829
_exptl_absorpt_correction_T_min  0.5359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark brown '
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle '
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4306
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                4022
_reflns_number_total             4306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104135x_si_002.cif
_cod_data_source_block           2feins
_cod_original_cell_volume        1731.1(10)
_cod_original_formula_sum        'C4.50 H9 B0.50 F2 Fe N2.50 O1.50 S'
_cod_database_code               4103197