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_4319574
_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         3(C10H8F8NiS8),3(C6H4S4),CH2Cl2
_chemical_formula_sum            'C49 H36 Cl2 F12 Ni3 S36'
_chemical_formula_weight         2253.97
_chemical_name_common            '[(F4Ni)3 (TTF)3,CH2Cl2]'
_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                91.10(3)
_cell_angle_beta                 110.78(3)
_cell_angle_gamma                116.01(3)
_cell_formula_units_Z            1
_cell_length_a                   12.330(3)
_cell_length_b                   12.726(3)
_cell_length_c                   15.706(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      1.85
_cell_volume                     2025.5(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      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'Oscillation, phi inc.=1.6'
_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  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1714
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19853
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    1.749
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_correction_T_min  0.7826
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Faceit, STOE-IPDS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0450
_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 
 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+3.0000*P+(0.0264P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                3076
_reflns_number_total             7360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0013835_2.cif
_cod_data_source_block           doe36bmer
_cod_depositor_comments
;
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 
;
_cod_original_cell_volume        2025.3(7)
_cod_database_code               4319574