Characterization of Two Distinct Adducts in the Reaction of a Nonheme Diiron(II) Complex with O2
Jonathan R. Frisch; Van V. Vu; Marlène Martinho; Eckard Münck; Lawrence Que; Inorganic Chemistry 48 (2009) 8325–8336; doi:10.1021/ic900961k

data_4303042
_publ_section_title
;
Characterization of Two Distinct Adducts in the Reaction of a Nonheme
Diiron(II) Complex with O2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8325
_journal_page_last               8336
_journal_paper_doi               10.1021/ic900961k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'C45 H55 As Fe2 N10 O3, C24 H20 B, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C72 H78 As B F3 Fe2 N11 O6 S'
_chemical_formula_weight         1479.94
_chemical_name_common            '[Fe2(N-EtHPTB)(O2AsMe2)](BPh4)(OTf)(CH3CN)'
_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                 103.4900(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1151(12)
_cell_length_b                   15.6370(12)
_cell_length_c                   28.473(2)
_cell_measurement_reflns_used    3592
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.56
_cell_volume                     6977.0(9)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            80047
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.7181
_exptl_absorpt_correction_T_min  0.5582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.51
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         15840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+4.8828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                12452
_reflns_number_total             15840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900961k_si_003_2.cif
_cod_data_source_block           arsinate
_cod_database_code               4303042