Synthesis and crystal engineering of new halogenated tetrathiafulvalene (TTF) derivatives and their charge transfer complexes and radical ion salts
Batsanov, Andrei S.; Bryce, Martin R.; Chesney, Antony; Howard, Judith A. K.; John, Derek E.; Moore, Adrian J.; Wood, Clare L.; Gershtenman, Hagit; Becker, James Y.; Khodorkovsky, Vladimir Y.; Ellern, Arkady; Bernstein, Joel; Perepichka, Igor F.; Rotello, Vincent; Gray, Mark; Cuello, Alejandro O.; Journal of Materials Chemistry 11 (2001) 2181–; doi:10.1039/b101866n

data_7204116
_publ_section_title
;
 Synthesis and crystal engineering of new halogenated
 tetrathiafulvalene (TTF) derivatives and their charge transfer
 complexes and radical ion salts
;
_journal_issue                   9
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2181
_journal_paper_doi               10.1039/b101866n
_journal_volume                  11
_journal_year                    2001
_chemical_formula_sum            'C6 I4 S4'
_chemical_formula_weight         707.90
_chemical_melting_point          476.15
_chemical_name_systematic        ' 4,4',5,5'-tetraiodotetrathiafulvalene '
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                95.18(1)
_cell_angle_beta                 91.92(1)
_cell_angle_gamma                96.69(1)
_cell_formula_units_Z            2
_cell_length_a                   4.190(1)
_cell_length_b                   11.746(2)
_cell_length_c                   14.294(3)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     695.2(3)
_computing_cell_refinement       'P3, (Siemens, 1988)'
_computing_data_collection       'P3, (Siemens, 1988)'
_computing_data_reduction        'XDISK (Siemens, 1988)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P\=1'
_diffrn_measurement_method       '2\q/\w 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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3149
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    9.528
_exptl_absorpt_correction_T_max  0.252
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL (XPREP, 1997) program'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_description       needle
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.291
_refine_diff_density_min         -2.861
_refine_diff_density_rms         0.353
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.140
_refine_ls_goodness_of_fit_obs   1.165
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_restrained_S_obs      1.165
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_obs          0.0540
_refine_ls_shift/esd_max         0.027
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.09P)^2^+6.0P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1533
_refine_ls_wR_factor_obs         0.1409
_reflns_number_observed          2377
_reflns_number_total             2640
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            b101866n.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '203\% C' was changed to '476.15' -
it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.09P)^2^+6.0P] 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^)+(0.09P)^2^+6.0P] 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-1
_cod_database_code               7204116