Phase Competition and Weak Hydrogen Bonding in the Giant Hysteresis of an S = 1/2 Nickel Dithiolene Complex: Combined Structural and Magnetic Studies
Jeannin, Olivier; Clérac, Rodolphe; Fourmigué, Marc; Chemistry of Materials 19 (2007) 5946–; doi:10.1021/cm071652q

data_4001434
_publ_section_title
;
 Phase Competition and Weak Hydrogen Bonding in the Giant Hysteresis of an
 S = 1/2 Nickel Dithiolene Complex: Combined Structural and Magnetic
 Studies
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5946
_journal_paper_doi               10.1021/cm071652q
_journal_volume                  19
_journal_year                    2007
_chemical_formula_moiety         'C8 F6 N2 Ni S4, C10 H10 Co'
_chemical_formula_sum            'C18 H10 Co F6 N2 Ni S4'
_chemical_formula_weight         614.16
_chemical_name_common            'Cp2Co, 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                82.475(12)
_cell_angle_beta                 67.071(12)
_cell_angle_gamma                80.971(13)
_cell_formula_units_Z            4
_cell_length_a                   12.3208(14)
_cell_length_b                   12.6666(12)
_cell_length_c                   15.3798(16)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      1.65
_cell_volume                     2176.7(4)
_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      198(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1.5 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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21117
_diffrn_reflns_theta_full        25.88
_diffrn_reflns_theta_max         25.88
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  0.6734
_exptl_absorpt_correction_T_min  0.3547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.829
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    Constr.
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                5446
_reflns_number_total             7813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071652q-file003.cif
_cod_data_source_block           Co198Kdown
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4001434