The crystal chemistry of amide‐functionalized ethylenedithiotetrathiafulvalenes: EDT‐TTF‐CONRR′ (R, R′ = H, Me)
Heuzé, Karine; Fourmigué, Marc; Batail, Patrick; Journal of Materials Chemistry 9 (1999) 2373–; doi:10.1039/a902852h

data_7213072
_publ_section_title
;
 The crystal chemistry of amide&#x2010;functionalized
 ethylenedithiotetrathiafulvalenes: EDT&#x2010;TTF&#x2010;CONRR&#x2032;
 (R, R&#x2032; = H, Me)
;
_journal_issue                   10
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2373
_journal_paper_doi               10.1039/a902852h
_journal_volume                  9
_journal_year                    1999
_chemical_formula_sum            'C9 H6 O2 S6'
_chemical_formula_weight         338.50
_chemical_name_common            EDT-TTF-CO2H
_chemical_name_systematic
; 
4-(4',5'-ethylenedithiotetrathiafulvalenyl)carboxylic acid 
;
_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                 92.29(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.3720(8)
_cell_length_b                   27.142(6)
_cell_length_c                   14.238(2)
_cell_measurement_reflns_used    2109
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.6
_cell_volume                     2460.5(7)
_computing_cell_refinement       'CELL (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Oscillation, phi incr. 0.9'
_diffrn_radiation_detector       'area detector'
_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  0.4439
_diffrn_reflns_av_sigmaI/netI    0.5141
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19288
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.712
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.716
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.2866
_refine_ls_R_factor_obs          0.0819
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1902
_refine_ls_wR_factor_obs         0.1232
_reflns_number_observed          1035
_reflns_number_total             4613
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902852hsup1.cif
_cod_data_source_block           acid
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^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^)+(0.0000P)^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      P2(1)/n
_cod_database_code               7213072