Syntheses and electrochemical characterization of heteroleptic cyclopentadienyl‒dithiolene d2 tungsten complexes. Structures and magnetic properties of charge-transfer salts †
Jourdain, Isabelle V.; Fourmigué, Marc; Guyon, Fabrice; Amaudrut, Jacques; Journal of the Chemical Society, Dalton Transactions  (1998) 483–; doi:10.1039/a706495k

data_7028189
_publ_section_title
;
 Syntheses and electrochemical characterization of heteroleptic
 cyclopentadienyl--dithiolene d2 tungsten complexes. Structures and
 magnetic properties of charge-transfer salts&#x200A;&#x2020;
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              483
_journal_paper_doi               10.1039/a706495k
_journal_year                    1998
_chemical_formula_moiety         'C14 H14 S4 W, C12 H4 N4'
_chemical_formula_sum            'C26 H18 N4 S4 W'
_chemical_formula_weight         698.53
_chemical_name_common            '[(\h^5^-C~5~H~5~)~2~W(dddt)][tcnq]'
_chemical_name_systematic
; 
Bis
(\h^5^-cyclopentadienyl)(5,6-dihydro-1,4-dithiine-2,3-dithiolato)
tungsten (V) tetracyanoquinodimethane salt  
;
_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
_cell_angle_alpha                84.310(14)
_cell_angle_beta                 81.450(15)
_cell_angle_gamma                89.320(15)
_cell_formula_units_Z            2
_cell_length_a                   9.5090(14)
_cell_length_b                   10.5400(14)
_cell_length_c                   12.385(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      1.45
_cell_volume                     1221.4(3)
_computing_cell_refinement       'CELL (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'ORTEP (XTAL 3.4)'
_computing_structure_refinement  'SHELXTL 5.04'
_computing_structure_solution    'SHELXTL 5.04'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_measurement_method       rotation
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3624
_diffrn_reflns_theta_max         24.09
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.095
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   'numerical (FACEIT, STOE)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.957
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.970
_refine_ls_goodness_of_fit_obs   0.965
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_restrained_S_obs      0.965
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_obs          0.0246
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0552
_refine_ls_wR_factor_obs         0.0503
_reflns_number_observed          3084
_reflns_number_total             3624
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k706495sup1.cif
_cod_data_source_block           wtcnq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               7028189