Synthesis, electrical properties and crystal structure of a new radical-ion salt based on π-extended bis(TTF) and a Keggin heteropolymolybdate
Peng, Jun; Wang, Enbo; Zhou, Yunshan; Xing, Yan; Jia, Hengqing; Lin, Yonghua; Shen, Yongjia; Journal of the Chemical Society, Dalton Transactions  (1998) 3865–; doi:10.1039/a804934c

data_7026987
_publ_section_title
;
 Synthesis, electrical properties and crystal structure of a new
 radical-ion salt based on \p-extended bis(TTF) and a Keggin
 heteropolymolybdate
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3865
_journal_paper_doi               10.1039/a804934c
_journal_year                    1998
_chemical_formula_sum            'C84 H120 Cl4 Mo12 O44 S24 Si'
_chemical_formula_weight         3924.41
_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
_cell_angle_alpha                98.54(3)
_cell_angle_beta                 116.37(3)
_cell_angle_gamma                107.25(3)
_cell_formula_units_Z            1
_cell_length_a                   15.088(3)
_cell_length_b                   16.416(3)
_cell_length_c                   16.675(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      4.79
_cell_volume                     3339(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13408
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.625
_exptl_absorpt_correction_T_max  0.96207
_exptl_absorpt_correction_T_min  0.66665
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_F_000             1946
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         5.128
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.141
_refine_ls_goodness_of_fit_obs   1.291
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         11236
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.419
_refine_ls_restrained_S_obs      1.291
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_obs          0.0942
_refine_ls_shift/esd_max         12.018
_refine_ls_shift/esd_mean        0.684
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1986P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3683
_refine_ls_wR_factor_obs         0.2811
_reflns_number_observed          7531
_reflns_number_total             11552
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            804934csup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1986P)^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^)+(0.1986P)^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_cell_volume        3338.9(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7026987