New bi(tetrathiafulvalenyl) derivatives and their radical cations: synthetic and X-ray structural studies
John, Derek E.; Moore, Adrian J.; Bryce, Martin R.; Batsanov, Andrei S.; Leech, Michael A.; Howard, Judith A. K.; Journal of Materials Chemistry 10 (2000) 1273–; doi:10.1039/b000790k

data_7203967
_publ_section_title
;
 New bi(tetrathiafulvalenyl) derivatives and their radical cations:
 synthetic and X-ray structural studies
;
_journal_issue                   6
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1273
_journal_paper_doi               10.1039/b000790k
_journal_volume                  10
_journal_year                    2000
_chemical_formula_sum            'C18 H18 S14'
_chemical_formula_weight         683.16
_chemical_melting_point          433.6(5)
_chemical_name_systematic
; 
 4-bis[4',5,5'-tris(methylsulfanyl)tetrathiafulvalenyl] 
;
_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                 96.20(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.374(1)
_cell_length_b                   12.684(2)
_cell_length_c                   26.295(3)
_cell_measurement_reflns_used    371
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      15.7
_cell_volume                     2776.6(6)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_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      120(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21201
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0.14
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.6938
_exptl_absorpt_correction_T_min  0.4647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS (G.M.Sheldrick,1997), R(int)=0.050 before correction'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.187
_refine_ls_goodness_of_fit_obs   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         21168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_restrained_S_obs      1.203
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_obs          0.0420
_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^)+(0.0000P)^2^+10.3475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1194
_refine_ls_wR_factor_obs         0.1145
_reflns_number_observed          19392
_reflns_number_total             21201
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000790k.txt
_cod_data_source_block           9
_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.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' 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:

'_chemical_melting_point' value '160-161 deg.C' was changed to
'433.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

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^)+(0.0000P)^2^+10.3475P] 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^)+(0.0000P)^2^+10.3475P] where P=(Fo^2^+2Fc^2^)/3'.

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

The following automatic conversions were performed:

data name '_exptl_absorp_process_details' was replaced with
'_exptl_absorpt_process_details' as specified in the replacement file
'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               7203967