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_7213073
_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_moiety         'C9 H7 N O S6, 0.75(C4 H8 O)'
_chemical_formula_sum            'C12 H13 N O1.75 S6'
_chemical_formula_weight         391.59
_chemical_name_common            'EDT-TTF-CONH2, 0.75 THF'
_chemical_name_systematic
; 
3-amido-3',4'-ethylenedithiotetrathiafulvalene, THF solvate 
;
_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                 95.681(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.3477(6)
_cell_length_b                   30.765(3)
_cell_length_c                   16.438(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      1.8
_cell_volume                     3194.4(6)
_computing_cell_refinement       'SELECT (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      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       'Oscillation, phi incr. 0.7'
_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  0.2173
_diffrn_reflns_av_sigmaI/netI    0.2480
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23683
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.827
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         6153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.827
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.1899
_refine_ls_R_factor_obs          0.0689
_refine_ls_shift/esd_max         0.019
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1512
_refine_ls_wR_factor_obs         0.1173
_reflns_number_observed          2399
_reflns_number_total             6153
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            902852hsup1.cif
_cod_data_source_block           AMI
_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^)+(0.0427P)^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^)+(0.0427P)^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        3194.4(5)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7213073