Nickel Dithiolene Chelate Rings in a New Role as η5-Coordinating Ligands: Synthesis, Structural Characterization, and Redox Reactivity of an "Fe2Ni" Bis-Double-Decker
Daniel J. Harrison; Antonio G. De Crisci; Alan J. Lough; Mitchell J. Kerr; Ulrich Fekl; Inorganic Chemistry 47 (2008) 10199–10201; doi:10.1021/ic801487f

data_4306663
_publ_section_title
;
Nickel Dithiolene Chelate Rings in a New Role as \h5-Coordinating Ligands:
Synthesis, Structural Characterization, and Redox Reactivity of an
"Fe2Ni" Bis-Double-Decker
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10199
_journal_page_last               10201
_journal_paper_doi               10.1021/ic801487f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C28 H42 Fe2 Ni S4, B F4'
_chemical_formula_sum            'C28 H42 B F4 Fe2 Ni S4'
_chemical_formula_weight         764.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.1233(17)
_cell_angle_beta                 101.2840(19)
_cell_angle_gamma                104.741(2)
_cell_formula_units_Z            1
_cell_length_a                   8.2743(2)
_cell_length_b                   8.3071(3)
_cell_length_c                   12.9787(5)
_cell_measurement_reflns_used    10562
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.7
_cell_volume                     799.37(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\w scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10562
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.781
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             395
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3599
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0473P)^2^+0.6597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                2902
_reflns_number_total             3599
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic801487f_si_002.cif
_cod_data_source_block           k08209
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4306663