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_7204123
_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_moiety         'C9 H9 S4 1+,I3 1-,0.5(I2)'
_chemical_formula_sum            'C9 H9 I5 S4'
_chemical_formula_weight         879.90
_chemical_name_systematic
; 4-iodo-4',5,5'-trimethyltetrathiafulvalenium triiodide    
hemi(diiodine)
;
_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                 107.20(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.034(1)
_cell_length_b                   8.077(1)
_cell_length_c                   17.960(1)
_cell_measurement_reflns_used    417
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.9
_cell_measurement_theta_min      12.0
_cell_volume                     1944.8(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'SMART 1K CCD area detector'
_diffrn_measurement_method       '\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  0.1516
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13637
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.410
_exptl_absorpt_correction_T_max  0.9329
_exptl_absorpt_correction_T_min  0.1241
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'XPREP (SHELXTL,1997), R(int)=0.184 before correction'
_exptl_crystal_colour            'black             '
_exptl_crystal_density_diffrn    3.005
_exptl_crystal_description       'plate             '
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.836
_refine_diff_density_min         -2.108
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.177
_refine_ls_goodness_of_fit_obs   1.248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4308
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.308
_refine_ls_restrained_S_obs      1.247
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_obs          0.0766
_refine_ls_shift/esd_max         -0.014
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+35.2117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2244
_refine_ls_wR_factor_obs         0.1772
_reflns_number_observed          3068
_reflns_number_total             4458
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b101866n.txt
_cod_data_source_block           5.I4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+35.2117P] 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^)+(0.0430P)^2^+35.2117P] 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      'P2(1)/n  '
_cod_database_code               7204123