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_4103198
_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            'C21 H25 B F4 Fe N5 O3.5'
_chemical_formula_weight         546.12
_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                104.936(6)
_cell_angle_beta                 95.022(6)
_cell_angle_gamma                101.285(6)
_cell_formula_units_Z            2
_cell_length_a                   8.252(4)
_cell_length_b                   10.218(5)
_cell_length_c                   15.767(8)
_cell_measurement_reflns_used    2530
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      3.5
_cell_volume                     1246.3(11)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       Omega
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0734
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10520
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9361
_exptl_absorpt_correction_T_min  0.8244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'green '
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle     '
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         3996
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+3.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                3038
_reflns_number_total             3996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104135x_si_003.cif
_cod_data_source_block           m
_cod_original_formula_sum        'C21 H25 B F4 Fe N5 O3.50'
_cod_database_code               4103198