Self-Assembly of Dinitrosyl Iron Units into Imidazolate-Edge-Bridged Molecular Squares: Characterization Including Mössbauer Spectroscopy
Jennifer L. Hess; Chung-Hung Hsieh; Scott M. Brothers; Michael B. Hall; Marcetta Y. Darensbourg; Journal of the American Chemical Society 133 (2011) 20426–20434; doi:10.1021/ja208384d

data_4107216
_publ_section_title
;
 Self-Assembly of Dinitrosyl Iron Units into Imidazolate-Edge-Bridged
 Molecular Squares: Characterization Including M\"ossbauer Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20426
_journal_page_last               20434
_journal_paper_doi               10.1021/ja208384d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C28 H20 Fe4 N16 O8'
_chemical_formula_weight         932.00
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 103.239(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.348(14)
_cell_length_b                   7.370(4)
_cell_length_c                   20.786(11)
_cell_measurement_reflns_used    3118
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.63
_cell_measurement_theta_min      2.33
_cell_volume                     3631(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0973
_diffrn_reflns_av_sigmaI/netI    0.1116
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19482
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0411P)^2^+5.7849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                2736
_reflns_number_total             4436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja208384d_si_002.cif
_cod_data_source_block           bztetra_0m
_cod_database_code               4107216