Diiron Carbonyl Complexes Bearing an N,C,S-Pincer Ligand: Reactivity toward Phosphines, Heterolytic Fe‒Fe Cleavage, and Electrocatalytic Proton Reduction
Hirotsu, Masakazu; Santo, Kiyokazu; Tsuboi, Chiaki; Kinoshita, Isamu; Organometallics 33 (2014) 4260–; doi:10.1021/om500558h

data_4084243
_publ_section_title
;
 Diiron Carbonyl Complexes Bearing an N,C,S-Pincer Ligand: Reactivity
 toward Phosphines, Heterolytic Fe--Fe Cleavage, and Electrocatalytic
 Proton Reduction
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4260
_journal_paper_doi               10.1021/om500558h
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C38 H22 Fe2 N2 O4 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C40 H26 Cl4 Fe2 N2 O4 S2'
_chemical_formula_weight         916.27
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.263(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1004(12)
_cell_length_b                   13.1729(9)
_cell_length_c                   18.3841(14)
_cell_measurement_reflns_used    12076
_cell_measurement_temperature    193
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      4.0192
_cell_volume                     3743.0(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -80.0000 - 100.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 35.3353
              2theta: 9.7650
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 35.3353
              2theta: 9.7650
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 35.3353
              2theta: 9.7650
scan:
    Number of images: 100
               Slice: -30.0000 - 20.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 35.3353
              2theta: 9.7650
;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w or \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34864
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         4.02
_diffrn_source_current           100.0000
_diffrn_source_power             4.0000
_diffrn_source_voltage           40.0000
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.7839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         8433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+1.0684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                6423
_reflns_number_total             8433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500558h_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084240--4084243.cif.
;
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4084243