Structure and properties of novel M(dmit)2 salts with the Me3N+­TEMPO cation radical (Me3N+­TEMPO = N,N,N­trimethyl(1­oxyl­2,2,6,6­tetramethylpiperidin­4­yl)ammonium)
Aonuma, Shuji; Casellas, Helene; Faulmann, Christophe; Garreau de Bonneval, Benedicte; Malfant, Isabelle; Cassoux, Patrick; Lacroix, Pascal G.; Hosokoshi, Yuko; Inoue, Katsuya; Journal of Materials Chemistry 11 (2001) 337–; doi:10.1039/b008424g

data_7204049
_publ_section_title
;
 Structure and properties of novel M(dmit)2 salts with the
 Me3N+&#x00AD;TEMPO cation radical (Me3N+&#x00AD;TEMPO =
 N,N,N&#x00AD;trimethyl(1&#x00AD;oxyl&#x00AD;2,2,6,6&#x00AD;tetramethylpiperidin&#x00AD;4&#x00AD;yl)ammonium)
;
_journal_issue                   2
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              337
_journal_paper_doi               10.1039/b008424g
_journal_volume                  11
_journal_year                    2001
_chemical_formula_moiety         'C6 Ni S10, C12 H26 N2 O'
_chemical_formula_sum            'C18 H26 N2 Ni O S10'
_chemical_formula_weight         665.72
_chemical_name_common            (Me3N-Tempo)Ni(dmit)2
_chemical_name_systematic
; 
[(N,N,N-trimethyl-(1-oxyl-2,2,6,6-tetramethylpiperidin-4-yl)ammonium] 
bis(2-thioxo-1,3-dithiole-4,5-dithiolato-S4,S5)nickelate(III) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.251(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3716(11)
_cell_length_b                   11.9980(19)
_cell_length_c                   28.592(4)
_cell_measurement_reflns_used    3253
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.22
_cell_volume                     2871.2(7)
_computing_cell_refinement       'IPDS software (Stoe, 1996)'
_computing_data_collection       'IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, X-Red 1.08, 1996)'
_computing_molecular_graphics    'CAMERON (Watkin, Prout & Pearce, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scan '
_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  0.2928
_diffrn_reflns_av_sigmaI/netI    0.3232
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27237
_diffrn_reflns_theta_full        26.15
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.27
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'narrow plate'
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.716
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         5644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.716
_refine_ls_R_factor_all          0.3304
_refine_ls_R_factor_gt           0.0715
_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^)+(0.0889P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1551
_refine_ls_wR_factor_ref         0.2509
_reflns_number_gt                985
_reflns_number_total             5644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b008424g.txt
_cod_data_source_block           (NMe3-tempo)-Ni(dmit)2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7204049