Apparent Anti-Woodward-Hoffmann Addition to a Nickel Bis(dithiolene) Complex: The Reaction Mechanism Involves Reduced, Dimetallic Intermediates
Li Dang; Mohamed F. Shibl; Xinzheng Yang; Daniel J. Harrison; Aiman Alak; Alan J. Lough; Ulrich Fekl; Edward N. Brothers; Michael B. Hall; Inorganic Chemistry 52 (2013) 3711–3723; doi:10.1021/ic302236u

data_4334287
_publ_section_title
;
 Apparent Anti-Woodward-Hoffmann Addition to a Nickel Bis(dithiolene)
 Complex: The Reaction Mechanism Involves Reduced, Dimetallic
 Intermediates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3711
_journal_page_last               3723
_journal_paper_doi               10.1021/ic302236u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C18 H4 F24 Ni2 S8), C8 F12 Ni S4'
_chemical_formula_sum            'C44 H8 F60 Ni5 S20'
_chemical_formula_weight         2611.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8830(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6053(4)
_cell_length_b                   12.3214(5)
_cell_length_c                   21.4161(7)
_cell_measurement_reflns_used    26282
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     3849.1(2)
_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    'SHELXTL V6.1'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1(Sheldrick, 2001)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f 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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26282
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.253
_exptl_crystal_description       plate
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+1.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                5107
_reflns_number_total             8756
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302236u_si_002.cif
_cod_data_source_block           k06102
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334287