Order-Disorder Transition Coupled with Magnetic Bistability in the Ferricinium Salt of a Radical Nickel Dithiolene Complex
Olivier Jeannin; Rodolphe Clérac; Marc Fourmigué; Journal of the American Chemical Society 128 (2006) 14649–14656; doi:10.1021/ja064842v

data_4111060
_publ_contact_author_address
;
Sciences Chimiques de Rennes
UMR 6226 CNRS-Universit\'e Rennes1
Campus de Beaulieu Bat 10C
35042 Rennes cedex
France
;
_publ_contact_author_email       marc.fourmigue@univ-rennes1.fr
_publ_contact_author_fax         '33(0)2 23 23 52 43'
_publ_contact_author_name        'FOURMIGUE Marc'
_publ_contact_author_phone       '33(0)2 23 23 67 32'
_publ_section_title
;
 Order-Disorder Transition Coupled with Magnetic Bistability in the
 Ferricinium Salt of a Radical Nickel Dithiolene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14649
_journal_page_last               14656
_journal_paper_doi               10.1021/ja064842v
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C10 H10 Fe,C8 F6 N2 Ni S4'
_chemical_formula_sum            'C18 H10 F6 Fe N2 Ni S4'
_chemical_formula_weight         611.08
_chemical_name_common            Cp2Fe,Ni(tfadt)2
_chemical_name_systematic
;
 ?
;
_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                74.955(15)
_cell_angle_beta                 83.431(16)
_cell_angle_gamma                76.137(16)
_cell_formula_units_Z            2
_cell_length_a                   7.8764(11)
_cell_length_b                   11.5708(16)
_cell_length_c                   12.9460(16)
_cell_measurement_reflns_used    6932
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      1.65
_cell_volume                     1104.5(3)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1.8 deg'
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12861
_diffrn_reflns_theta_full        25.96
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  0.8508
_exptl_absorpt_correction_T_min  0.4986
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    Constr.
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0869P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                2131
_reflns_number_total             3992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064842vsi20060707_123814.cif
_cod_data_source_block           oj96bt
_cod_database_code               4111060
_exptl_absorpt_correction_t_ave  0.7585