Insight into the Dinuclear {Fe(NO)2}10{Fe(NO)2}10 and Mononuclear {Fe(NO)2}10 Dinitrosyliron Complexes
Shih-Wey Yeh; Chih-Wei Lin; Ya-Wen Li; I-Jui Hsu; Chien-Hong Chen; Ling-Yun Jang; Jyh-Fu Lee; Wen-Feng Liaw; Inorganic Chemistry 51 (2012) 4076–4087; doi:10.1021/ic202332d

data_4328771
_publ_section_title
;
 Insight into the Dinuclear {Fe(NO)2}10{Fe(NO)2}10 and Mononuclear
 {Fe(NO)2}10 Dinitrosyliron Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4076
_journal_page_last               4087
_journal_paper_doi               10.1021/ic202332d
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C82 H83 Fe2 N6 O4.5 P4 S2'
_chemical_formula_weight         1524.24
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 97.0980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7472(4)
_cell_length_b                   14.1277(3)
_cell_length_c                   28.1653(5)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.4747
_cell_measurement_theta_min      2.6188
_cell_volume                     8192.3(3)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68015
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       Lump
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         1.169
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         16788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1651
_refine_ls_wR_factor_ref         0.1773
_reflns_number_gt                12089
_reflns_number_total             16788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202332d_complex2.cif
_cod_data_source_block           111036lts
_cod_original_formula_sum        'C82 H83 Fe2 N6 O4.50 P4 S2'
_cod_database_code               4328771