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_4119720
_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         'C31 H49 Fe N7 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C33 H49 F6 Fe N7 O6 P2 S2'
_chemical_formula_weight         935.70
_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                81.424(8)
_cell_angle_beta                 76.624(6)
_cell_angle_gamma                81.593(7)
_cell_formula_units_Z            2
_cell_length_a                   10.502(2)
_cell_length_b                   11.823(2)
_cell_length_c                   18.286(4)
_cell_measurement_reflns_used    6618
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     2169.4(7)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0337
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17728
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       prism
_exptl_crystal_F_000             972.00
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     566
_refine_ls_number_reflns         9568
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 0.9080\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                6739
_reflns_number_total             9568
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja3122944_si_004.cif
_cod_data_source_block           '[Fe(LH2)(PMe3)2(PhN=NH)](OTf)2(4a)'
_cod_database_code               4119720