[Fe4] and [Fe6] Hydride Clusters Supported by Phosphines: Synthesis, Characterization, and Application in N2 Reduction.
Araake, Ryoichi; Sakadani, Kazuki; Tada, Mizuki; Sakai, Yoichi; Ohki, Yasuhiro; Journal of the American Chemical Society 139 (2017) 5596–5606; doi:10.1021/jacs.7b01965

data_4126170
_publ_section_title
;
 [Fe4] and [Fe6] Hydride Clusters Supported by Phosphines: Synthesis,
 Characterization, and Application in N2 Reduction.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5596
_journal_page_last               5606
_journal_paper_doi               10.1021/jacs.7b01965
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C42 H114 Fe6.4 N6 Si12'
_chemical_formula_sum            'C42 H114 Fe6.4 N6 Si12'
_chemical_formula_weight         1397.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                87.674(6)
_cell_angle_beta                 84.043(6)
_cell_angle_gamma                62.903(4)
_cell_formula_units_Z            2
_cell_length_a                   14.5261(14)
_cell_length_b                   14.9231(14)
_cell_length_c                   19.419(2)
_cell_measurement_reflns_used    11106
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     3727.1(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b29'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b29'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_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 Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30430
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.520
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         3.113
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1484.80
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.15
_refine_diff_density_min         -1.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     612
_refine_ls_number_reflns         16372
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                10967
_reflns_number_total             16372
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja7b01965_si_002.cif
_cod_data_source_block           NFeN-HB
_cod_database_code               4126170