N-N Bond Cleavage of Hydrazines with a Multiproton-Responsive Pincer-Type Iron Complex
Kazuki Umehara; Shigeki Kuwata; Takao Ikariya; Journal of the American Chemical Society 135 (2013) 6754–6757; doi:10.1021/ja3122944

data_4119719
_publ_section_title
;
 N-N Bond Cleavage of Hydrazines with a Multiproton-Responsive Pincer-Type
 Iron Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6754
_journal_page_last               6757
_journal_paper_doi               10.1021/ja3122944
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C27 H46 Fe N6 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C29 H46 F6 Fe N6 O6 P2 S2'
_chemical_formula_weight         870.62
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                88.464(10)
_cell_angle_beta                 77.257(8)
_cell_angle_gamma                65.722(7)
_cell_formula_units_Z            2
_cell_length_a                   10.697(2)
_cell_length_b                   12.004(3)
_cell_length_c                   17.782(4)
_cell_measurement_reflns_used    5618
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.38
_cell_volume                     2024.9(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16558
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.627
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       prism
_exptl_crystal_F_000             904.00
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.550
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.519
_refine_ls_extinction_coef       684(40)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8878
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 0.5400\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                6491
_reflns_number_total             8878
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja3122944_si_003.cif
_cod_data_source_block           '[Fe(LH2)(CH3CN)(PMe3)2](OTf)2(2)'
_cod_database_code               4119719