Multi-Site Reactivity: Reduction of Six Equivalents of Nitrite To Give an Fe6(NO)6 Cluster with a Dramatically Expanded Octahedral Core
T. David Harris; Theodore A. Betley; Journal of the American Chemical Society 133 (2011) 13852–13855; doi:10.1021/ja2052655

data_4106704
_publ_section_title
;
 Multi-Site Reactivity: Reduction of Six Equivalents of Nitrite To Give an
 Fe6(NO)6 Cluster with a Dramatically Expanded Octahedral Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13852
_journal_page_last               13855
_journal_paper_doi               10.1021/ja2052655
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C79 H121.5 Fe6 N20.5 O12'
_chemical_formula_weight         1885.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.322(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0992(19)
_cell_length_b                   13.669(2)
_cell_length_c                   24.162(3)
_cell_measurement_reflns_used    6470
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      2.25
_cell_volume                     4314.0(10)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector 
;
_diffrn_measurement_method       'phi and omega 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  0.1200
_diffrn_reflns_av_sigmaI/netI    0.1115
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37276
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.9895
_exptl_absorpt_correction_T_min  0.9591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             1982
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.597
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8193
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1746
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+45.1377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2239
_refine_ls_wR_factor_ref         0.2609
_reflns_number_gt                4450
_reflns_number_total             8193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2052655_si_002_2.cif
_cod_data_source_block           tdh48a
_cod_original_cell_volume        4314.0(11)
_cod_original_formula_sum        'C79 H121.50 Fe6 N20.50 O12'
_cod_database_code               4106704