N2 Activation by an Iron Complex with a Strong Electron-Donating Iminophosphorane Ligand.
Suzuki, Tatsuya; Wasada-Tsutsui, Yuko; Ogawa, Takahiko; Inomata, Tomohiko; Ozawa, Tomohiro; Sakai, Yoichi; Fryzuk, Michael D.; Masuda, Hideki; Inorganic chemistry 54 (2015) 9271–9281; doi:10.1021/acs.inorgchem.5b00536

data_4343561
_publ_section_title
;
 N2 Activation by an Iron Complex with a Strong Electron-Donating
 Iminophosphorane Ligand.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9271
_journal_page_last               9281
_journal_paper_doi               10.1021/acs.inorgchem.5b00536
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C78 H130 Fe2 N6 O2 P4'
_chemical_formula_sum            'C78 H130 Fe2 N6 O2 P4'
_chemical_formula_weight         1419.51
_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                74.6192(7)
_cell_angle_beta                 77.0841(9)
_cell_angle_gamma                71.9256(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5965(4)
_cell_length_b                   17.3450(5)
_cell_length_c                   22.1096(6)
_cell_measurement_reflns_used    27314
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.00
_cell_volume                     4027.6(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            39599
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     829
_refine_ls_number_reflns         18222
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0699P)^2^+1.5922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                13023
_reflns_number_total             18222
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b00536_si_001.cif
_cod_data_source_block           Fe_N2_Et2O
_cod_depositor_comments
'Adding full bibliography for 4343557--4343561.cif.'
_cod_original_cell_volume        4027.6(3)
_cod_database_code               4343561