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_4001432
_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           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 99.276(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.211(3)
_cell_length_b                   7.7363(7)
_cell_length_c                   12.7856(18)
_cell_measurement_reflns_used    7272
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      1.8
_cell_volume                     2265.9(5)
_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      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 1 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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10847
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.989
_exptl_absorpt_correction_T_max  0.9271
_exptl_absorpt_correction_T_min  0.7253
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x 12 x  8 =   768 sampling points was used
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                1063
_reflns_number_total             2339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071652q-file001.cif
_cod_data_source_block           CoRTback
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constr.' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4001432
_exptl_absorpt_correction_t_ave  0.8766