Stabilization of Isolated Mixed-Valence Trimers in a Novel Nickel Dithiolene Complex with CF2 Substituents
Olivier J. Dautel; Marc Fourmigué; Inorganic Chemistry 40 (2001) 2083–2087; doi:10.1021/ic0013835

data_4319573
_publ_section_title
;
 Stabilization of Isolated Mixed-Valence Trimers in a Novel Nickel
 Dithiolene Complex with CF2 Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2083
_journal_page_last               2087
_journal_paper_doi               10.1021/ic0013835
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C10 H8 F4 Ni S8, C16 H36 N'
_chemical_formula_sum            'C26 H44 F4 N Ni S8'
_chemical_formula_weight         761.81
_chemical_name_common            ((F4-Ni)TBA)
_chemical_name_systematic        ((C4H9)4-N)(Ni(F2-PDT)2)
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.379(4)
_cell_length_b                   8.9702(18)
_cell_length_c                   18.527(4)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      1.9
_cell_volume                     3553.0(12)
_computing_cell_refinement       'select, 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, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, phi incr.=1.1'
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20627
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.9400
_exptl_absorpt_correction_T_min  0.7770
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   FACEIT-STOE,IPDS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.706
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6766
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.706
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0496
_reflns_number_gt                4660
_reflns_number_total             6766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0013835_1.cif
_cod_data_source_block           dop122fmer
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4319573