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_4343558
_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         'C74.75 H121 Fe2 N6 P4'
_chemical_formula_sum            'C74.75 H121 Fe2 N6 P4'
_chemical_formula_weight         1339.41
_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                86.399(14)
_cell_angle_beta                 78.867(12)
_cell_angle_gamma                67.779(8)
_cell_formula_units_Z            2
_cell_length_a                   11.554(3)
_cell_length_b                   12.902(4)
_cell_length_c                   27.798(8)
_cell_measurement_reflns_used    9090
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.02
_cell_volume                     3763.7(19)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            30012
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1447.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.090
_refine_diff_density_min         -0.650
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     782
_refine_ls_number_reflns         16485
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0642P)^2^+4.8302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                10526
_reflns_number_total             16485
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic5b00536_si_001.cif
_cod_data_source_block           FeNpNP_mN2
_cod_depositor_comments
'Adding full bibliography for 4343557--4343561.cif.'
_cod_original_cell_volume        3763.4(18)
_cod_database_code               4343558