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_4001438
_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                82.416(17)
_cell_angle_beta                 66.981(17)
_cell_angle_gamma                80.951(18)
_cell_formula_units_Z            4
_cell_length_a                   12.333(2)
_cell_length_b                   12.6886(18)
_cell_length_c                   15.462(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      1.65
_cell_volume                     2192.6(6)
_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      210(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_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  0.1206
_diffrn_reflns_av_sigmaI/netI    0.1566
_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            25102
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    2.056
_exptl_absorpt_correction_T_max  0.9245
_exptl_absorpt_correction_T_min  0.7070
_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    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1538
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0862P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                3604
_reflns_number_total             7854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm071652q-file007.cif
_cod_data_source_block           Co210Kup
_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_cell_volume        2192.7(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4001438
_exptl_absorpt_correction_t_ave  0.8837