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_4103200
_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            'C27 H32 Fe N4 O3.5 S'
_chemical_formula_weight         556.48
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.201(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.344(12)
_cell_length_b                   8.202(6)
_cell_length_c                   22.232(17)
_cell_measurement_reflns_used    6664
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.28
_cell_volume                     2976(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0588
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31187
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.9414
_exptl_absorpt_correction_T_min  0.8379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'purple '
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1709
_reflns_number_gt                4582
_reflns_number_total             6786
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104135x_si_005.cif
_cod_data_source_block           fe
_cod_original_cell_volume        2975(4)
_cod_original_formula_sum        'C27 H32 Fe N4 O3.50 S'
_cod_database_code               4103200