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_7028188
_publ_contact_author             'Fabrice Guyon'
_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         'C21 H26 S5 W, C12 F4 N4, C2 H3 N'
_chemical_formula_sum            'C35 H29 F4 N5 S5 W'
_chemical_formula_weight         939.78
_chemical_name_common
'[(\h^5^C~5~H~4~CMe~3~)~2~W(C~3~S~5~)][tcnqf~4~], CH~3~CN'
_chemical_name_systematic
; 
Bis
(\h^5^-tert-butylcyclopentadienyl)(4,5-disulfanyl-1,3-dithiole-2-
thionato) tungsten (V)
tetrafluoro-7,7,8,8-tetracyanoquinodimethane salt, acetonitrile
solvate  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.390(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9560(13)
_cell_length_b                   21.020(3)
_cell_length_c                   21.722(4)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      1.45
_cell_volume                     3610.1(10)
_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      293(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  0.0815
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22608
_diffrn_reflns_theta_max         24.22
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.544
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_type   ' Multi-scan (XPREP, SHELXTL 5.04) '
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.542
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.842
_refine_ls_goodness_of_fit_obs   0.952
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_restrained_S_obs      0.952
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_obs          0.0360
_refine_ls_shift/esd_max         0.094
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0797
_refine_ls_wR_factor_obs         0.0690
_reflns_number_observed          3538
_reflns_number_total             5715
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            k706495sup1.cif
_cod_data_source_block           buwf4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^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^)+(0.0346P)^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 
;
_cod_original_sg_symbol_H-M      'P 2~1~/n'
_cod_database_code               7028188