Synthesis, Crystal Structure, and Physical Properties of (BEDT-TTF)[Ni(tdas)~2~] (BEDT-TTF = Bis(ethylenedithio)tetrathiafulvalene; tdas = 1,2,5-Thiadiazole-3,4-dithiolate): First Monomeric [Ni(tdas)~2~]- Monoanion
S. Curreli; P. Deplano; M. L. Mercuri; L. Pilia; A. Serpe; John A. Schlueter; Michael A. Whited; Urs Geiser; E. Coronado; C. J. Gómez-García; E. Canadell; Inorganic Chemistry 43 (2004) 2049–2056; doi:10.1021/ic035079y

data_4310720
_publ_contact_author_address
;
   Materials Science Divisions
   Argonne National Laboratory
   9700 South Cass Avenue
   Argonne, IL 60439, USA
;
_publ_contact_author_email       JASchlueter@anl.gov
_publ_contact_author_fax         '(630) 252-9151'
_publ_contact_author_name        'Schlueter, Dr. John A.'
_publ_contact_author_phone       '(630) 252-3588'
_publ_section_title
;
 Synthesis, Crystal Structure, and Physical Properties of
 (BEDT-TTF)[Ni(tdas)~2~] (BEDT-TTF =
 Bis(ethylenedithio)tetrathiafulvalene; tdas =
 1,2,5-Thiadiazole-3,4-dithiolate): First Monomeric [Ni(tdas)~2~]-
 Monoanion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2049
_journal_page_last               2056
_journal_paper_doi               10.1021/ic035079y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '(C10 H8 S8) Ni (C2 S3 N2)2'
_chemical_formula_sum            'C14 H8 N4 Ni S14'
_chemical_formula_weight         739.79
_chemical_name_systematic
;
Bis(ethylenedithio)tetrathiafulvalenium bis(1,2,5-thiadizole-3,4-dithiol)
Nickel (II)
;
_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           'manual editing of SHELXL-97 cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.974(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2324(6)
_cell_length_b                   13.2740(5)
_cell_length_c                   10.9467(4)
_cell_measurement_reflns_used    2116
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.143
_cell_measurement_theta_min      2.38
_cell_volume                     2485.45(16)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens SMART CCD area detector'
_diffrn_measurement_method       'area detector \w scans'
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33500
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 1918
_diffrn_standards_interval_time  1175
_diffrn_standards_number         216
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(Sheldrick, 2001)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         8224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0381P)^2^+1.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.1009
_reflns_number_gt                5411
_reflns_number_total             8224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035079ysi20030915_121614.cif
_cod_data_source_block           etnitdas
_cod_database_code               4310720