
 
data_2ac
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'EDT-TTF(CN)(CF3)'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H4 F3 N S6'
_chemical_formula_weight          387.50
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)

 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    5.0849(5)
_cell_length_b                    10.9285(12)
_cell_length_c                    12.7619(13)
_cell_angle_alpha                 90.00
_cell_angle_beta                  97.741(12)
_cell_angle_gamma                 90.00
_cell_volume                      702.72(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     4870
_cell_measurement_theta_min       2.45
_cell_measurement_theta_max       25.75
 
_exptl_crystal_description        PLATE
_exptl_crystal_colour             'dark violet'
_exptl_crystal_size_max           0.39
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.831
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              388
_exptl_absorpt_coefficient_mu     0.991
_exptl_absorpt_correction_type  multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min   0.7860
_exptl_absorpt_correction_T_max   0.8508


 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'STOE IPDS'
_diffrn_measurement_method        'Oscillation, phi incr. 1.8 deg' 
_diffrn_detector_area_resol_mean  6.66
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             6805
_diffrn_reflns_av_R_equivalents   0.0334
_diffrn_reflns_av_sigmaI/netI     0.0438
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.46
_diffrn_reflns_theta_max          25.99
_reflns_number_total              2682
_reflns_number_gt                 1986
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'EXPOSE, Stoe-IPDS'
_computing_cell_refinement        'CELL, Stoe-IPDS'
_computing_data_reduction          'INTEGRATE, Stoe-IPDS'
_computing_structure_solution      'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0424P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     Constr.
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    -0.04(11)
_refine_ls_number_reflns          2682
_refine_ls_number_parameters      199
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0557
_refine_ls_R_factor_gt            0.0327
_refine_ls_wR_factor_ref          0.0765
_refine_ls_wR_factor_gt           0.0691
_refine_ls_goodness_of_fit_ref    0.954
_refine_ls_restrained_S_all       0.954
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1 S 0.38687(19) 0.66499(9) 0.02574(7) 0.0431(3) Uani 1 1 d . . .
S4 S 0.1364(2) 0.90104(9) -0.04349(8) 0.0443(3) Uani 1 1 d . . .
S6 S 0.1141(2) 0.66956(10) 0.23479(8) 0.0479(3) Uani 1 1 d . . .
S5 S -0.16920(19) 0.90112(9) 0.16657(8) 0.0444(3) Uani 1 1 d . . .
S2 S 0.6747(2) 0.63693(10) -0.15747(9) 0.0540(3) Uani 1 1 d . . .
S3 S 0.3822(3) 0.91765(10) -0.23831(9) 0.0594(3) Uani 1 1 d . . .
C1 C 0.1789(7) 0.7862(3) 0.0523(3) 0.0377(9) Uani 1 1 d . . .
C2 C 0.4653(7) 0.7277(3) -0.0928(3) 0.0366(9) Uani 1 1 d . . .
C3 C 0.7275(17) 0.7211(11) -0.2677(7) 0.053(3) Uani 0.60 1 d P . .
H3A H 0.8659 0.7809 -0.2473 0.063 Uiso 0.60 1 calc PR . .
H3B H 0.7893 0.6667 -0.3193 0.063 Uiso 0.60 1 calc PR . .
C4 C 0.4824(17) 0.7863(11) -0.3182(6) 0.053(2) Uani 0.60 1 d P . .
H4A H 0.3371 0.7282 -0.3292 0.064 Uiso 0.60 1 calc PR . .
H4B H 0.5132 0.8164 -0.3871 0.064 Uiso 0.60 1 calc PR . .
C'3 C 0.577(4) 0.7055(16) -0.2966(12) 0.069(4) Uani 0.40 1 d P . .
H'3A H 0.6869 0.6682 -0.3443 0.082 Uiso 0.40 1 calc PR . .
H'3B H 0.3943 0.6834 -0.3210 0.082 Uiso 0.40 1 calc PR . .
C'4 C 0.603(3) 0.8410(13) -0.3036(11) 0.060(4) Uani 0.40 1 d P . .
H'4A H 0.5760 0.8651 -0.3775 0.072 Uiso 0.40 1 calc PR . .
H'4B H 0.7817 0.8646 -0.2743 0.072 Uiso 0.40 1 calc PR . .
C5 C 0.3520(8) 0.8346(4) -0.1235(3) 0.0395(9) Uani 1 1 d . . .
C6 C 0.0577(7) 0.7869(3) 0.1407(3) 0.0376(9) Uani 1 1 d . . .
C7 C -0.2211(8) 0.8354(4) 0.2867(3) 0.0420(10) Uani 1 1 d . . .
C8 C -0.0912(8) 0.7330(4) 0.3180(3) 0.0419(9) Uani 1 1 d . . .
C9 C -0.4032(9) 0.8971(4) 0.3460(3) 0.0552(11) Uani 1 1 d . . .
C10 C -0.1037(9) 0.6727(5) 0.4222(3) 0.0578(11) Uani 1 1 d . . .
F1 F -0.3458(6) 0.6377(3) 0.4337(2) 0.0957(11) Uani 1 1 d . . .
F2 F 0.0397(7) 0.5717(4) 0.4334(2) 0.1040(12) Uani 1 1 d . . .
F3 F -0.0272(9) 0.7444(4) 0.5012(2) 0.1113(13) Uani 1 1 d . . .
N N -0.5513(9) 0.9403(4) 0.3932(4) 0.0808(13) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1 C2 1.754(3) . ?
S1 C1 1.757(4) . ?
S4 C1 1.745(4) . ?
S4 C5 1.753(3) . ?
S6 C8 1.732(4) . ?
S6 C6 1.754(4) . ?
S5 C7 1.745(4) . ?
S5 C6 1.761(4) . ?
S2 C3 1.732(9) . ?
S2 C2 1.743(3) . ?
S2 C'3 1.929(16) . ?
S3 C'4 1.705(12) . ?
S3 C5 1.748(4) . ?
S3 C4 1.871(10) . ?
C1 C6 1.356(4) . ?
C2 C5 1.337(5) . ?
C3 C4 1.503(14) . ?
C'3 C'4 1.49(2) . ?
C7 C8 1.334(5) . ?
C7 C9 1.440(5) . ?
C8 C10 1.493(5) . ?
C9 N 1.130(5) . ?
C10 F3 1.294(6) . ?
C10 F1 1.316(5) . ?
C10 F2 1.320(6) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 S1 C1 94.82(16) . . ?
C1 S4 C5 94.70(17) . . ?
C8 S6 C6 94.07(17) . . ?
C7 S5 C6 93.07(17) . . ?
C3 S2 C2 104.7(4) . . ?
C3 S2 C'3 25.2(5) . . ?
C2 S2 C'3 96.7(6) . . ?
C'4 S3 C5 107.0(5) . . ?
C'4 S3 C4 27.3(5) . . ?
C5 S3 C4 96.9(3) . . ?
C6 C1 S4 123.5(3) . . ?
C6 C1 S1 121.1(3) . . ?
S4 C1 S1 115.37(17) . . ?
C5 C2 S2 128.7(3) . . ?
C5 C2 S1 117.1(3) . . ?
S2 C2 S1 114.2(2) . . ?
C4 C3 S2 112.9(6) . . ?
C3 C4 S3 113.6(7) . . ?
C'4 C'3 S2 115.3(12) . . ?
C'3 C'4 S3 112.9(11) . . ?
C2 C5 S3 128.1(3) . . ?
C2 C5 S4 118.0(3) . . ?
S3 C5 S4 113.9(2) . . ?
C1 C6 S6 121.0(3) . . ?
C1 C6 S5 122.8(3) . . ?
S6 C6 S5 116.14(17) . . ?
C8 C7 C9 124.2(4) . . ?
C8 C7 S5 118.8(3) . . ?
C9 C7 S5 117.0(3) . . ?
C7 C8 C10 124.0(4) . . ?
C7 C8 S6 117.8(3) . . ?
C10 C8 S6 118.1(3) . . ?
N C9 C7 176.8(5) . . ?
F3 C10 F1 106.1(4) . . ?
F3 C10 F2 108.6(4) . . ?
F1 C10 F2 104.9(5) . . ?
F3 C10 C8 112.4(4) . . ?
F1 C10 C8 112.3(4) . . ?
F2 C10 C8 112.1(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.973
_diffrn_reflns_theta_full              25.99
_diffrn_measured_fraction_theta_full   0.973
_refine_diff_density_max    0.297
_refine_diff_density_min   -0.357
_refine_diff_density_rms    0.069

#===END

 
data_2bc
 
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
3,4-ethylendithio-3'-carbomethoxy-4'-trifluoromethyltetrathiafulvalene
 ?
;
_chemical_name_common           'EDT-TTF(CO2Me)(CF3)'


_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C11 H7 F3 O2 S6'
_chemical_formula_weight          420.53
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    5.1515(12)
_cell_length_b                    11.998(2)
_cell_length_c                    12.974(3)
_cell_angle_alpha                 103.96(3)
_cell_angle_beta                  90.02(3)
_cell_angle_gamma                 90.45(3)
_cell_volume                      778.2(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     2150
_cell_measurement_theta_min       1.7
_cell_measurement_theta_max       25.45
 
_exptl_crystal_description        needle
_exptl_crystal_colour             'dark violet'
_exptl_crystal_size_max           0.6
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.795
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              424
_exptl_absorpt_coefficient_mu     0.910
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'STOE IPDS'
_diffrn_measurement_method        'Oscillation, phi incr. 1.8 deg' 
_diffrn_detector_area_resol_mean  6.66
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             7498
_diffrn_reflns_av_R_equivalents   0.1265
_diffrn_reflns_av_sigmaI/netI     0.2045
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.75
_diffrn_reflns_theta_max          25.94
_reflns_number_total              2778
_reflns_number_gt                 989
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'EXPOSE, Stoe-IPDS'
_computing_cell_refinement        'CELL, Stoe-IPDS'
_computing_data_reduction          'INTEGRATE, Stoe-IPDS'
_computing_structure_solution      'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0167P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constrain
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2778
_refine_ls_number_parameters      199
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1597
_refine_ls_R_factor_gt            0.0442
_refine_ls_wR_factor_ref          0.0909
_refine_ls_wR_factor_gt           0.0691
_refine_ls_goodness_of_fit_ref    0.702
_refine_ls_restrained_S_all       0.702
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1 S 0.8057(4) 0.34166(13) 0.22964(15) 0.0464(5) Uani 1 1 d . . .
S3 S 0.2079(4) 0.12987(13) 0.03126(15) 0.0474(6) Uani 1 1 d . . .
S2 S 0.5859(4) 0.11211(14) 0.22628(16) 0.0505(6) Uani 1 1 d . . .
S4 S 0.4142(4) 0.36299(13) 0.04205(16) 0.0511(6) Uani 1 1 d . . .
S5 S 0.0942(4) 0.40266(15) -0.13245(18) 0.0657(7) Uani 1 1 d . . .
S6 S -0.1549(4) 0.12743(16) -0.14383(17) 0.0623(7) Uani 1 1 d . . .
C2 C 0.5795(14) 0.2347(5) 0.1736(5) 0.0391(17) Uani 1 1 d . . .
C1 C 0.4191(13) 0.2410(4) 0.0923(5) 0.0383(17) Uani 1 1 d . . .
C4 C 0.8030(13) 0.1706(5) 0.3251(5) 0.0405(19) Uani 1 1 d . . .
C3 C 0.9102(12) 0.2750(5) 0.3260(5) 0.0369(16) Uani 1 1 d . . .
C5 C 0.0796(13) 0.2044(5) -0.0571(6) 0.0451(19) Uani 1 1 d . . .
C6 C 0.1720(12) 0.3107(5) -0.0521(5) 0.0387(18) Uani 1 1 d . . .
C7 C -0.189(2) 0.2148(7) -0.2347(7) 0.113(4) Uani 1 1 d . . .
H7A H -0.1085 0.1724 -0.2998 0.135 Uiso 1 1 calc R . .
H7B H -0.3739 0.2147 -0.2497 0.135 Uiso 1 1 calc R . .
C8 C -0.115(3) 0.3177(10) -0.2236(9) 0.188(8) Uani 1 1 d . . .
H8A H -0.2750 0.3612 -0.2169 0.226 Uiso 1 1 calc R . .
H8B H -0.0442 0.3201 -0.2922 0.226 Uiso 1 1 calc R . .
C9 C 0.8545(17) 0.0973(6) 0.4020(6) 0.051(2) Uani 1 1 d . . .
C10 C 1.1062(14) 0.3461(6) 0.4006(6) 0.045(2) Uani 1 1 d . . .
C11 C 1.3685(15) 0.3671(6) 0.5517(6) 0.082(3) Uani 1 1 d . . .
H11A H 1.4107 0.3273 0.6054 0.123 Uiso 1 1 calc R . .
H11B H 1.2981 0.4410 0.5846 0.123 Uiso 1 1 calc R . .
H11C H 1.5226 0.3770 0.5132 0.123 Uiso 1 1 calc R . .
O1 O 1.1781(10) 0.3006(4) 0.4791(4) 0.0692(16) Uani 1 1 d . . .
O2 O 1.1693(10) 0.4388(4) 0.3884(4) 0.0716(16) Uani 1 1 d . . .
F1 F 1.1023(9) 0.0676(3) 0.4072(3) 0.0692(13) Uani 1 1 d . . .
F2 F 0.7833(9) 0.1477(3) 0.5019(3) 0.0783(14) Uani 1 1 d . . .
F3 F 0.7175(9) 0.0000(3) 0.3765(3) 0.0770(14) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1 C3 1.726(7) . ?
S1 C2 1.750(6) . ?
S3 C1 1.748(6) . ?
S3 C5 1.748(7) . ?
S2 C4 1.714(6) . ?
S2 C2 1.766(6) . ?
S4 C1 1.741(6) . ?
S4 C6 1.749(6) . ?
S5 C8 1.733(8) . ?
S5 C6 1.739(7) . ?
S6 C5 1.748(7) . ?
S6 C7 1.767(8) . ?
C2 C1 1.356(7) . ?
C4 C3 1.363(8) . ?
C4 C9 1.505(9) . ?
C3 C10 1.507(9) . ?
C5 C6 1.345(8) . ?
C7 C8 1.264(10) . ?
C9 F3 1.331(7) . ?
C9 F1 1.334(8) . ?
C9 F2 1.344(8) . ?
C10 O2 1.202(8) . ?
C10 O1 1.321(8) . ?
C11 O1 1.453(7) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C3 S1 C2 95.0(3) . . ?
C1 S3 C5 94.5(3) . . ?
C4 S2 C2 94.4(3) . . ?
C1 S4 C6 94.8(3) . . ?
C8 S5 C6 101.6(4) . . ?
C5 S6 C7 101.3(4) . . ?
C1 C2 S1 123.6(4) . . ?
C1 C2 S2 121.6(4) . . ?
S1 C2 S2 114.7(4) . . ?
C2 C1 S4 120.9(4) . . ?
C2 C1 S3 123.3(4) . . ?
S4 C1 S3 115.8(4) . . ?
C3 C4 C9 127.2(6) . . ?
C3 C4 S2 118.3(5) . . ?
C9 C4 S2 114.5(5) . . ?
C4 C3 C10 130.3(7) . . ?
C4 C3 S1 117.0(5) . . ?
C10 C3 S1 112.7(5) . . ?
C6 C5 S3 117.7(5) . . ?
C6 C5 S6 128.1(5) . . ?
S3 C5 S6 114.2(4) . . ?
C5 C6 S5 128.4(5) . . ?
C5 C6 S4 117.1(5) . . ?
S5 C6 S4 114.4(3) . . ?
C8 C7 S6 127.8(7) . . ?
C7 C8 S5 131.1(9) . . ?
F3 C9 F1 106.6(6) . . ?
F3 C9 F2 105.0(6) . . ?
F1 C9 F2 106.3(6) . . ?
F3 C9 C4 111.0(6) . . ?
F1 C9 C4 114.3(7) . . ?
F2 C9 C4 113.0(6) . . ?
O2 C10 O1 126.4(6) . . ?
O2 C10 C3 119.3(7) . . ?
O1 C10 C3 114.1(6) . . ?
C10 O1 C11 115.2(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.915
_diffrn_reflns_theta_full              25.94
_diffrn_measured_fraction_theta_full   0.915
_refine_diff_density_max    0.291
_refine_diff_density_min   -0.285
_refine_diff_density_rms    0.063

#===END

data_3bc
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
4,5-bis(trifluoromethyl)-4',5'-bis(methoxycarbonyl)tetrathiafulvalene
;
_chemical_name_common          'o-(CF3)2-TTF-o-(CO2Me)'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C12 H6 F6 O4 S4'
_chemical_formula_weight          456.41
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P21/a
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z'
 
_cell_length_a                    7.4209(8)
_cell_length_b                    17.0659(17)
_cell_length_c                    13.5707(15)
_cell_angle_alpha                 90.00
_cell_angle_beta                  97.834(13)
_cell_angle_gamma                 90.00
_cell_volume                      1702.6(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     8000
_cell_measurement_theta_min       1.85
_cell_measurement_theta_max       25.85
 
_exptl_crystal_description        'bulk'
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.36
_exptl_crystal_size_mid           0.36
_exptl_crystal_size_min           0.16
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.781
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              912
_exptl_absorpt_coefficient_mu     0.636
_exptl_absorpt_correction_type  gaussian
_exptl_absorpt_process_details
;
a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_absorpt_correction_T_min   0.7816
_exptl_absorpt_correction_T_max   0.9013
_exptl_absorpt_correction_T_ave   0.8597


 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'STOE IPDS'
_diffrn_measurement_method        'Oscillation, phi incr. 1.4 deg' 
_diffrn_detector_area_resol_mean  6.66
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             12937
_diffrn_reflns_av_R_equivalents   0.0639
_diffrn_reflns_av_sigmaI/netI     0.0535
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.93
_diffrn_reflns_theta_max          25.86
_reflns_number_total              3263
_reflns_number_gt                 2161
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'EXPOSE, Stoe-IPDS'
_computing_cell_refinement        'CELL, Stoe-IPDS'
_computing_data_reduction          'INTEGRATE, Stoe-IPDS'
_computing_structure_solution      'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0434P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          3263
_refine_ls_number_parameters      289
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0612
_refine_ls_R_factor_gt            0.0320
_refine_ls_wR_factor_ref          0.0783
_refine_ls_wR_factor_gt           0.0706
_refine_ls_goodness_of_fit_ref    0.898
_refine_ls_restrained_S_all       0.898
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1 S 0.78962(8) 0.84970(4) 0.57327(4) 0.05360(19) Uani 1 1 d . . .
S2 S 0.52343(8) 0.93762(4) 0.67401(4) 0.04925(18) Uani 1 1 d . . .
S3 S 0.22510(8) 0.92198(4) 0.47713(4) 0.05080(19) Uani 1 1 d . . .
S4 S 0.48771(8) 0.82752(4) 0.37998(4) 0.0546(2) Uani 1 1 d . . .
C1 C 0.5674(3) 0.88684(15) 0.56695(15) 0.0434(5) Uani 1 1 d . . .
C2 C 0.8376(3) 0.86146(14) 0.70161(15) 0.0416(5) Uani 1 1 d . . .
C3 C 0.7171(3) 0.90105(14) 0.74688(15) 0.0400(5) Uani 1 1 d . . .
C4 C 1.0112(4) 0.8239(2) 0.7490(2) 0.0587(7) Uani 1 1 d . . .
C5 C 0.7304(4) 0.91767(17) 0.85677(17) 0.0539(7) Uani 1 1 d . . .
C6 C 0.4423(3) 0.87963(15) 0.48567(15) 0.0428(6) Uani 1 1 d . . .
C7 C 0.1589(3) 0.89035(14) 0.35499(15) 0.0382(5) Uani 1 1 d . . .
C8 C 0.2763(3) 0.84722(13) 0.31138(15) 0.0379(5) Uani 1 1 d . . .
C9 C -0.0222(3) 0.91859(15) 0.30997(16) 0.0450(6) Uani 1 1 d . . .
C10 C -0.2335(3) 0.92750(18) 0.16457(19) 0.0625(7) Uani 1 1 d . . .
H10A H -0.2470 0.9105 0.0965 0.094 Uiso 1 1 calc R . .
H10B H -0.2373 0.9837 0.1669 0.094 Uiso 1 1 calc R . .
H10C H -0.3307 0.9064 0.1964 0.094 Uiso 1 1 calc R . .
C11 C 0.2424(3) 0.81311(15) 0.20865(16) 0.0416(5) Uani 1 1 d . . .
C12 C 0.2933(5) 0.8302(2) 0.04365(19) 0.0947(12) Uani 1 1 d . . .
H12A H 0.3520 0.8660 0.0038 0.142 Uiso 1 1 calc R . .
H12B H 0.1660 0.8274 0.0188 0.142 Uiso 1 1 calc R . .
H12C H 0.3467 0.7791 0.0407 0.142 Uiso 1 1 calc R . .
F1 F 1.1126(18) 0.8668(8) 0.8191(7) 0.078(2) Uani 0.58 1 d P . .
F2 F 0.9832(13) 0.7566(5) 0.7877(8) 0.085(2) Uani 0.58 1 d P . .
F3 F 1.1222(10) 0.8124(7) 0.6814(8) 0.084(3) Uani 0.58 1 d P . .
F4 F 0.7782(6) 0.8545(2) 0.9109(2) 0.0881(12) Uani 0.80 1 d P . .
F5 F 0.8558(8) 0.9708(3) 0.8866(4) 0.0875(15) Uani 0.80 1 d P . .
F6 F 0.5794(6) 0.9446(4) 0.8815(4) 0.100(2) Uani 0.80 1 d P . .
F'1 F 0.984(2) 0.7719(10) 0.8193(13) 0.154(8) Uani 0.42 1 d P . .
F'2 F 1.095(2) 0.7873(11) 0.6872(13) 0.137(7) Uani 0.42 1 d P . .
F'3 F 1.109(3) 0.8768(13) 0.7924(12) 0.123(6) Uani 0.42 1 d P . .
F'4 F 0.887(3) 0.9333(12) 0.9039(15) 0.093(7) Uani 0.20 1 d P . .
F'5 F 0.617(4) 0.9731(16) 0.8737(18) 0.130(12) Uani 0.20 1 d P . .
F'6 F 0.666(2) 0.8596(8) 0.9070(9) 0.074(4) Uani 0.20 1 d P . .
O1 O -0.1185(3) 0.95569(16) 0.35540(14) 0.0919(8) Uani 1 1 d . . .
O2 O -0.0608(2) 0.90017(11) 0.21575(11) 0.0572(5) Uani 1 1 d . . .
O3 O 0.1603(3) 0.75389(12) 0.18902(13) 0.0723(6) Uani 1 1 d . . .
O4 O 0.3162(2) 0.85732(11) 0.14603(11) 0.0569(5) Uani 1 1 d . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1 C2 1.741(2) . ?
S1 C1 1.758(2) . ?
S2 C3 1.745(2) . ?
S2 C1 1.760(2) . ?
S3 C7 1.749(2) . ?
S3 C6 1.756(2) . ?
S4 C8 1.744(2) . ?
S4 C6 1.759(2) . ?
C1 C6 1.348(3) . ?
C2 C3 1.335(3) . ?
C2 C4 1.503(3) . ?
C3 C5 1.508(3) . ?
C4 F'3 1.25(2) . ?
C4 F'2 1.273(16) . ?
C4 F2 1.291(9) . ?
C4 F3 1.330(9) . ?
C4 F'1 1.339(18) . ?
C4 F1 1.346(13) . ?
C5 F'4 1.28(2) . ?
C5 F6 1.297(5) . ?
C5 F'5 1.31(2) . ?
C5 F5 1.323(7) . ?
C5 F4 1.326(5) . ?
C5 F'6 1.329(14) . ?
C7 C8 1.339(3) . ?
C7 C9 1.479(3) . ?
C8 C11 1.500(3) . ?
C9 O1 1.188(3) . ?
C9 O2 1.310(3) . ?
C10 O2 1.449(3) . ?
C11 O3 1.192(3) . ?
C11 O4 1.311(3) . ?
C12 O4 1.452(3) . ?
F2 F'1 0.50(3) . ?
F2 F'2 1.767(19) . ?
F4 F'6 0.833(12) . ?
F4 F'4 1.58(2) . ?
F5 F'4 0.71(2) . ?
F5 F'5 1.76(3) . ?
F6 F'5 0.58(3) . ?
F6 F'6 1.605(16) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 S1 C1 93.99(10) . . ?
C3 S2 C1 93.47(11) . . ?
C7 S3 C6 94.14(10) . . ?
C8 S4 C6 94.55(10) . . ?
C6 C1 S1 122.99(17) . . ?
C6 C1 S2 122.40(17) . . ?
S1 C1 S2 114.57(11) . . ?
C3 C2 C4 127.4(2) . . ?
C3 C2 S1 117.41(16) . . ?
C4 C2 S1 115.18(18) . . ?
C2 C3 C5 126.3(2) . . ?
C2 C3 S2 118.14(16) . . ?
C5 C3 S2 115.52(18) . . ?
F'3 C4 F'2 111.1(12) . . ?
F'3 C4 F2 124.4(9) . . ?
F'2 C4 F2 87.1(10) . . ?
F'3 C4 F3 93.1(11) . . ?
F'2 C4 F3 21.5(12) . . ?
F2 C4 F3 107.4(7) . . ?
F'3 C4 F'1 106.1(11) . . ?
F'2 C4 F'1 106.1(11) . . ?
F2 C4 F'1 21.9(11) . . ?
F3 C4 F'1 124.2(9) . . ?
F'3 C4 F1 17.2(14) . . ?
F'2 C4 F1 117.2(10) . . ?
F2 C4 F1 107.6(8) . . ?
F3 C4 F1 103.2(8) . . ?
F'1 C4 F1 88.9(10) . . ?
F'3 C4 C2 107.6(9) . . ?
F'2 C4 C2 113.1(8) . . ?
F2 C4 C2 112.2(5) . . ?
F3 C4 C2 110.1(5) . . ?
F'1 C4 C2 112.6(8) . . ?
F1 C4 C2 115.8(5) . . ?
F'4 C5 F6 123.9(11) . . ?
F'4 C5 F'5 109.0(15) . . ?
F6 C5 F'5 25.7(15) . . ?
F'4 C5 F5 31.6(9) . . ?
F6 C5 F5 105.9(4) . . ?
F'5 C5 F5 83.8(13) . . ?
F'4 C5 F4 74.7(9) . . ?
F6 C5 F4 108.7(4) . . ?
F'5 C5 F4 128.4(13) . . ?
F5 C5 F4 105.3(3) . . ?
F'4 C5 F'6 105.5(10) . . ?
F6 C5 F'6 75.3(7) . . ?
F'5 C5 F'6 99.5(14) . . ?
F5 C5 F'6 129.9(6) . . ?
F4 C5 F'6 36.6(6) . . ?
F'4 C5 C3 117.7(10) . . ?
F6 C5 C3 112.3(3) . . ?
F'5 C5 C3 110.7(11) . . ?
F5 C5 C3 112.3(3) . . ?
F4 C5 C3 111.8(3) . . ?
F'6 C5 C3 112.8(6) . . ?
C1 C6 S3 122.73(17) . . ?
C1 C6 S4 121.75(17) . . ?
S3 C6 S4 115.52(11) . . ?
C8 C7 C9 127.32(19) . . ?
C8 C7 S3 118.22(15) . . ?
C9 C7 S3 114.40(16) . . ?
C7 C8 C11 125.96(18) . . ?
C7 C8 S4 117.54(15) . . ?
C11 C8 S4 116.49(15) . . ?
O1 C9 O2 124.6(2) . . ?
O1 C9 C7 122.4(2) . . ?
O2 C9 C7 113.0(2) . . ?
O3 C11 O4 126.1(2) . . ?
O3 C11 C8 123.6(2) . . ?
O4 C11 C8 110.3(2) . . ?
F'1 F2 C4 84(3) . . ?
F'1 F2 F'2 124(3) . . ?
C4 F2 F'2 46.0(7) . . ?
F'6 F4 C5 71.9(11) . . ?
F'6 F4 F'4 115.2(15) . . ?
C5 F4 F'4 51.3(7) . . ?
F'4 F5 C5 71(2) . . ?
F'4 F5 F'5 110(3) . . ?
C5 F5 F'5 47.7(9) . . ?
F'5 F6 C5 78(3) . . ?
F'5 F6 F'6 128(3) . . ?
C5 F6 F'6 53.3(5) . . ?
F2 F'1 C4 74(3) . . ?
C4 F'2 F2 46.9(6) . . ?
F5 F'4 C5 78(2) . . ?
F5 F'4 F4 130(3) . . ?
C5 F'4 F4 54.0(8) . . ?
F6 F'5 C5 76(3) . . ?
F6 F'5 F5 118(3) . . ?
C5 F'5 F5 48.5(9) . . ?
F4 F'6 C5 71.5(11) . . ?
F4 F'6 F6 118.4(15) . . ?
C5 F'6 F6 51.4(6) . . ?
C9 O2 C10 116.86(19) . . ?
C11 O4 C12 115.6(2) . . ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              25.86
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    0.211
_refine_diff_density_min   -0.166
_refine_diff_density_rms    0.044

#===END

data_4bc

 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Trans-4,4'-bis(trifluoromethyl)-5,5'-bis(methoxycarbonyl)tetrathiafulvalene
;
_chemical_name_common             'E-(CF3,CO2Me)2 TTF'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C12 H6 F6 O4 S4'
_chemical_formula_weight          456.41
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M     Pbam
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, z'
 'x+1/2, -y+1/2, -z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, y, -z'
 '-x-1/2, y-1/2, z'
 'x-1/2, -y-1/2, z'
 
_cell_length_a                    28.000(3)
_cell_length_b                    8.7129(9)
_cell_length_c                    7.2091(7)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1758.8(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     3389
_cell_measurement_theta_min       2.4
_cell_measurement_theta_max       23.3
 
_exptl_crystal_description        prism
_exptl_crystal_colour             'dark red'
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.05
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.724
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              912
_exptl_absorpt_coefficient_mu     0.616
_exptl_absorpt_correction_type  multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min   0.9272
_exptl_absorpt_correction_T_max   0.9372

 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Stoe-IPDS'
_diffrn_measurement_method        'Oscillation, phi incr. 0.8 deg.'
_diffrn_detector_area_resol_mean  6.66
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             10664
_diffrn_reflns_av_R_equivalents   0.0815
_diffrn_reflns_av_sigmaI/netI     0.0791
_diffrn_reflns_limit_h_min        -34
_diffrn_reflns_limit_h_max        34
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        8
_diffrn_reflns_theta_min          2.45
_diffrn_reflns_theta_max          25.98
_reflns_number_total              1861
_reflns_number_gt                 833
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'EXPOSE, Stoe-IPDS'
_computing_cell_refinement        'CELL, Stoe-IPDS'
_computing_data_reduction         'INTEGRATE, Stoe-IPDS'
_computing_structure_solution     'SHELX-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0215P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment    constrain
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          1861
_refine_ls_number_parameters      151
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1057
_refine_ls_R_factor_gt            0.0342
_refine_ls_wR_factor_ref          0.0647
_refine_ls_wR_factor_gt           0.0530
_refine_ls_goodness_of_fit_ref    0.767
_refine_ls_restrained_S_all       0.767
_refine_ls_shift/su_max           0.003
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1A S 0.06911(3) 0.11842(13) 0.0000 0.0706(4) Uani 1 2 d S . .
S2A S 0.04269(3) -0.20961(15) 0.0000 0.0789(4) Uani 1 2 d S . .
O1A O 0.19998(10) -0.0279(4) 0.0000 0.1166(14) Uani 1 2 d S . .
O2A O 0.16381(8) 0.1968(4) 0.0000 0.0935(11) Uani 1 2 d S . .
F1A F 0.11156(9) -0.4295(3) 0.0000 0.1116(11) Uani 1 2 d S . .
F2A F 0.16416(6) -0.3032(2) 0.1475(3) 0.1169(8) Uani 1 1 d . . .
C1A C 0.02333(11) -0.0189(5) 0.0000 0.0644(12) Uani 1 2 d S . .
C2A C 0.10298(12) -0.1641(5) 0.0000 0.0624(12) Uani 1 2 d S . .
C3A C 0.13621(17) -0.2984(6) 0.0000 0.0847(15) Uani 1 2 d S . .
C4A C 0.11519(12) -0.0163(5) 0.0000 0.0598(12) Uani 1 2 d S . .
C5A C 0.16492(14) 0.0468(6) 0.0000 0.0697(13) Uani 1 2 d S . .
C6A C 0.20957(13) 0.2747(6) 0.0000 0.1095(19) Uani 1 2 d S . .
H6A1 H 0.2046 0.3837 0.0000 0.164 Uiso 1 2 calc SR . .
H6A2 H 0.2272 0.2459 -0.1087 0.164 Uiso 0.50 1 calc PR . .
H6A3 H 0.2272 0.2459 0.1087 0.164 Uiso 0.50 1 calc PR . .
S1B S 0.07557(3) 0.93630(13) 0.5000 0.0728(4) Uani 1 2 d S . .
S2B S 0.02620(3) 1.23553(14) 0.5000 0.0821(4) Uani 1 2 d S . .
O1B O 0.19227(11) 1.1723(5) 0.5000 0.1460(18) Uani 1 2 d S . .
O2B O 0.17249(9) 0.9302(5) 0.5000 0.1127(14) Uani 1 2 d S . .
F1B F 0.07868(14) 1.4999(4) 0.5000 0.1743(19) Uani 1 2 d S . .
F2B F 0.13810(9) 1.4145(3) 0.3569(4) 0.1555(10) Uani 1 1 d . . .
C1B C 0.02144(11) 1.0358(4) 0.5000 0.0602(12) Uani 1 2 d S . .
C2B C 0.08806(13) 1.2361(5) 0.5000 0.0688(12) Uani 1 2 d S . .
C3B C 0.1098(2) 1.3922(7) 0.5000 0.1026(19) Uani 1 2 d S . .
C4B C 0.11067(12) 1.1014(5) 0.5000 0.0642(12) Uani 1 2 d S . .
C5B C 0.16307(15) 1.0755(8) 0.5000 0.0805(14) Uani 1 2 d S . .
C6B C 0.22254(14) 0.8842(8) 0.5000 0.139(2) Uani 1 2 d S . .
H6B1 H 0.2246 0.7742 0.5000 0.209 Uiso 1 2 calc SR . .
H6B2 H 0.2380 0.9240 0.6087 0.209 Uiso 0.50 1 calc PR . .
H6B3 H 0.2380 0.9240 0.3913 0.209 Uiso 0.50 1 calc PR . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1A C4A 1.744(4) . ?
S1A C1A 1.753(4) . ?
S2A C2A 1.734(4) . ?
S2A C1A 1.748(4) . ?
O1A C5A 1.178(4) . ?
O2A C5A 1.307(5) . ?
O2A C6A 1.450(4) . ?
F1A C3A 1.335(5) . ?
F2A C3A 1.321(3) . ?
C1A C1A 1.347(6) 5 ?
C2A C4A 1.333(5) . ?
C2A C3A 1.495(6) . ?
C3A F2A 1.321(3) 6 ?
C4A C5A 1.497(5) . ?
S1B C4B 1.742(4) . ?
S1B C1B 1.746(3) . ?
S2B C2B 1.732(4) . ?
S2B C1B 1.745(4) . ?
O1B C5B 1.175(5) . ?
O2B C5B 1.293(6) . ?
O2B C6B 1.458(5) . ?
F1B C3B 1.281(6) . ?
F2B C3B 1.314(3) . ?
C1B C1B 1.353(6) 5_576 ?
C2B C4B 1.333(5) . ?
C2B C3B 1.491(7) . ?
C3B F2B 1.314(3) 6_556 ?
C4B C5B 1.484(5) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C4A S1A C1A 94.7(2) . . ?
C2A S2A C1A 94.9(2) . . ?
C5A O2A C6A 116.5(3) . . ?
C1A C1A S2A 122.2(4) 5 . ?
C1A C1A S1A 122.8(4) 5 . ?
S2A C1A S1A 114.96(18) . . ?
C4A C2A C3A 126.6(4) . . ?
C4A C2A S2A 118.1(3) . . ?
C3A C2A S2A 115.3(3) . . ?
F2A C3A F2A 107.2(4) . 6 ?
F2A C3A F1A 106.2(3) . . ?
F2A C3A F1A 106.2(3) 6 . ?
F2A C3A C2A 113.2(3) . . ?
F2A C3A C2A 113.2(3) 6 . ?
F1A C3A C2A 110.4(4) . . ?
C2A C4A C5A 126.4(4) . . ?
C2A C4A S1A 117.4(3) . . ?
C5A C4A S1A 116.2(3) . . ?
O1A C5A O2A 124.9(4) . . ?
O1A C5A C4A 124.9(5) . . ?
O2A C5A C4A 110.2(4) . . ?
C4B S1B C1B 94.57(19) . . ?
C2B S2B C1B 94.5(2) . . ?
C5B O2B C6B 117.7(4) . . ?
C1B C1B S2B 121.8(4) 5_576 . ?
C1B C1B S1B 122.8(4) 5_576 . ?
S2B C1B S1B 115.40(18) . . ?
C4B C2B C3B 127.5(4) . . ?
C4B C2B S2B 118.2(3) . . ?
C3B C2B S2B 114.3(4) . . ?
F1B C3B F2B 107.6(4) . . ?
F1B C3B F2B 107.6(4) . 6_556 ?
F2B C3B F2B 103.4(5) . 6_556 ?
F1B C3B C2B 112.9(4) . . ?
F2B C3B C2B 112.4(4) . . ?
F2B C3B C2B 112.4(4) 6_556 . ?
C2B C4B C5B 127.1(4) . . ?
C2B C4B S1B 117.3(3) . . ?
C5B C4B S1B 115.6(4) . . ?
O1B C5B O2B 124.1(4) . . ?
O1B C5B C4B 125.3(5) . . ?
O2B C5B C4B 110.5(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              25.98
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.179
_refine_diff_density_min   -0.163
_refine_diff_density_rms    0.038

#===END

data_(1c)2-TCNQ 

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common          '(EDT TTF CF3)2 TCNQ'   


_chemical_melting_point           ?
_chemical_formula_moiety          'C9 H5 F3 S6, 0.5(C12 H4 N4)' 

_chemical_formula_sum
 'C15 H7 F3 N2 S6'
_chemical_formula_weight          464.59
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P21/c

 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    13.2146(15)
_cell_length_b                    11.1448(8)
_cell_length_c                    13.1662(15)
_cell_angle_alpha                 90.00
_cell_angle_beta                  106.997(13)
_cell_angle_gamma                 90.00
_cell_volume                      1854.3(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     8000
_cell_measurement_theta_min       2.4
_cell_measurement_theta_max       25.7
 
_exptl_crystal_description        'platelet'
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.5
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.664
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              936
_exptl_absorpt_coefficient_mu     0.768
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8216
_exptl_absorpt_correction_T_max   0.9119
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;

 

_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'STOE IPDS'
_diffrn_measurement_method        'oscillation, phi incr. 1.7 deg'
_diffrn_detector_area_resol_mean  6.66
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             13683
_diffrn_reflns_av_R_equivalents   0.0650
_diffrn_reflns_av_sigmaI/netI     0.0603
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          2.44
_diffrn_reflns_theta_max          25.83
_reflns_number_total              3518
_reflns_number_gt                 2190
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'EXPOSE, Stoe-IPDS'
_computing_cell_refinement        'CELL, Stoe-IPDS'
_computing_data_reduction          'INTEGRATE, Stoe-IPDS'
_computing_structure_solution     'SHELXs-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0414P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constrain
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0000(7)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3518
_refine_ls_number_parameters      236
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0692
_refine_ls_R_factor_gt            0.0339
_refine_ls_wR_factor_ref          0.0814
_refine_ls_wR_factor_gt           0.0730
_refine_ls_goodness_of_fit_ref    0.868
_refine_ls_restrained_S_all       0.868
_refine_ls_shift/su_max           4.925
_refine_ls_shift/su_mean          0.021
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
S1 S 0.94722(5) 0.22237(7) 0.16058(5) 0.0466(2) Uani 1 1 d . . .
S2 S 0.88591(5) 0.17779(7) -0.07090(5) 0.0466(2) Uani 1 1 d . . .
S3 S 1.18766(5) 0.15446(7) 0.17929(5) 0.0509(2) Uani 1 1 d . . .
S4 S 0.66283(5) 0.25729(8) -0.10515(5) 0.0529(2) Uani 1 1 d . . .
S5 S 1.13058(6) 0.11560(8) -0.05361(6) 0.0532(2) Uani 1 1 d . . .
S6 S 0.74352(6) 0.32432(9) 0.16200(6) 0.0693(3) Uani 1 1 d . . .
C6 C 0.79027(19) 0.2388(2) -0.0175(2) 0.0395(6) Uani 1 1 d . . .
F1 F 1.43171(15) 0.2121(2) 0.23372(18) 0.0932(7) Uani 1 1 d . . .
C4 C 1.3971(2) 0.1052(3) 0.1948(3) 0.0595(8) Uani 1 1 d . . .
C'1 C 1.1083(2) 0.4768(2) 0.0502(2) 0.0489(7) Uani 1 1 d . . .
C3 C 1.2608(2) 0.0955(3) 0.0198(2) 0.0520(7) Uani 1 1 d . . .
H3 H 1.3115 0.0735 -0.0130 0.062 Uiso 1 1 calc R . .
C5 C 0.98804(19) 0.1839(2) 0.04926(19) 0.0407(6) Uani 1 1 d . . .
C1 C 1.0885(2) 0.1571(2) 0.0568(2) 0.0415(6) Uani 1 1 d . . .
F2 F 1.46402(14) 0.0682(2) 0.14364(18) 0.0977(8) Uani 1 1 d . . .
F3 F 1.40765(15) 0.0329(2) 0.27556(18) 0.0996(8) Uani 1 1 d . . .
C9 C 0.8180(2) 0.2611(2) 0.0864(2) 0.0428(6) Uani 1 1 d . . .
C'5 C 1.0396(2) 0.5177(3) 0.1091(2) 0.0531(7) Uani 1 1 d . . .
H'5 H 1.0672 0.5295 0.1819 0.064 Uiso 1 1 calc R . .
C2 C 1.2869(2) 0.1118(3) 0.1233(2) 0.0461(7) Uani 1 1 d . . .
C'2 C 1.2135(3) 0.4543(3) 0.0989(2) 0.0532(7) Uani 1 1 d . . .
C'6 C 1.0633(3) 0.4607(3) -0.0625(2) 0.0531(7) Uani 1 1 d . . .
H'6 H 1.1059 0.4350 -0.1033 0.064 Uiso 1 1 calc R . .
N2 N 1.2962(3) 0.4843(3) 0.3000(2) 0.0908(10) Uani 1 1 d . . .
C7 C 0.5885(2) 0.2292(4) -0.0117(3) 0.0685(9) Uani 1 1 d . . .
H7A H 0.5136 0.2324 -0.0495 0.082 Uiso 1 1 calc R . .
H7B H 0.6042 0.1486 0.0162 0.082 Uiso 1 1 calc R . .
C'3 C 1.2840(3) 0.4121(3) 0.0425(3) 0.0612(8) Uani 1 1 d . . .
N1 N 1.3407(3) 0.3774(3) -0.0013(3) 0.0829(9) Uani 1 1 d . . .
C'4 C 1.2597(3) 0.4712(3) 0.2107(3) 0.0641(9) Uani 1 1 d . . .
C8 C 0.6102(2) 0.3133(4) 0.0774(3) 0.0686(10) Uani 1 1 d . . .
H8A H 0.5655 0.2915 0.1213 0.082 Uiso 1 1 calc R . .
H8B H 0.5884 0.3925 0.0488 0.082 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
S1 C9 1.755(3) . ?
S1 C5 1.757(3) . ?
S2 C6 1.753(3) . ?
S2 C5 1.755(2) . ?
S3 C2 1.748(3) . ?
S3 C1 1.756(3) . ?
S4 C6 1.753(3) . ?
S4 C7 1.812(3) . ?
S5 C3 1.724(3) . ?
S5 C1 1.763(3) . ?
S6 C9 1.741(3) . ?
S6 C8 1.792(3) . ?
C6 C9 1.332(4) . ?
F1 C4 1.325(4) . ?
C4 F3 1.309(3) . ?
C4 F2 1.324(4) . ?
C4 C2 1.486(4) . ?
C'1 C'2 1.374(4) . ?
C'1 C'5 1.430(4) . ?
C'1 C'6 1.439(4) . ?
C3 C2 1.316(4) . ?
C5 C1 1.336(4) . ?
C'5 C'6 1.340(4) 3_765 ?
C'2 C'3 1.431(5) . ?
C'2 C'4 1.431(5) . ?
C'6 C'5 1.340(4) 3_765 ?
N2 C'4 1.141(4) . ?
C7 C8 1.463(4) . ?
C'3 N1 1.137(4) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C9 S1 C5 94.68(12) . . ?
C6 S2 C5 94.48(12) . . ?
C2 S3 C1 93.87(13) . . ?
C6 S4 C7 98.05(13) . . ?
C3 S5 C1 94.32(13) . . ?
C9 S6 C8 103.54(14) . . ?
C9 C6 S4 125.2(2) . . ?
C9 C6 S2 118.0(2) . . ?
S4 C6 S2 116.62(15) . . ?
F3 C4 F2 107.0(3) . . ?
F3 C4 F1 107.3(3) . . ?
F2 C4 F1 105.7(3) . . ?
F3 C4 C2 113.4(3) . . ?
F2 C4 C2 111.7(3) . . ?
F1 C4 C2 111.4(3) . . ?
C'2 C'1 C'5 121.4(3) . . ?
C'2 C'1 C'6 121.1(3) . . ?
C'5 C'1 C'6 117.6(3) . . ?
C2 C3 S5 118.6(2) . . ?
C1 C5 S2 122.9(2) . . ?
C1 C5 S1 122.26(19) . . ?
S2 C5 S1 114.76(14) . . ?
C5 C1 S3 122.0(2) . . ?
C5 C1 S5 122.95(19) . . ?
S3 C1 S5 114.99(15) . . ?
C6 C9 S6 129.1(2) . . ?
C6 C9 S1 117.2(2) . . ?
S6 C9 S1 113.69(15) . . ?
C'6 C'5 C'1 121.9(3) 3_765 . ?
C3 C2 C4 124.1(3) . . ?
C3 C2 S3 118.2(2) . . ?
C4 C2 S3 117.6(2) . . ?
C'1 C'2 C'3 122.7(3) . . ?
C'1 C'2 C'4 121.7(3) . . ?
C'3 C'2 C'4 115.5(3) . . ?
C'5 C'6 C'1 120.5(3) 3_765 . ?
C8 C7 S4 114.5(2) . . ?
N1 C'3 C'2 179.0(4) . . ?
N2 C'4 C'2 179.6(4) . . ?
C7 C8 S6 118.0(2) . . ?
 
_diffrn_measured_fraction_theta_max    0.982
_diffrn_reflns_theta_full              25.83
_diffrn_measured_fraction_theta_full   0.982
_refine_diff_density_max    0.316
_refine_diff_density_min   -0.202
_refine_diff_density_rms    0.051

#===END

data_(1c)FeCl4 
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             'EDT-TTF-CF3, FeCl4'
_chemical_melting_point           ?

_chemical_formula_moiety          'C9 H5 F3 S6, Cl4 Fe '
_chemical_formula_sum
 'C9 H5 Cl4 F3 Fe S6'
_chemical_formula_weight          560.14
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0171   0.0103
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    P212121

 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 

_cell_length_a                    5.9348(5)
_cell_length_b                    14.4165(15)
_cell_length_c                    21.785(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1863.9(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     41486
_cell_measurement_theta_min       2.3452
_cell_measurement_theta_max       26.0485
 
_exptl_crystal_description        'needle'
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.36
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.06

_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.996
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1104
_exptl_absorpt_coefficient_mu     2.072
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7334
_exptl_absorpt_correction_T_max   0.7693

_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;

 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   'horizontally mounted graphite crystal'
_diffrn_measurement_device_type   'KappaCCD'
_diffrn_measurement_method        'CCD'
_diffrn_detector_area_resol_mean  9
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             38263
_diffrn_reflns_av_R_equivalents   0.1099
_diffrn_reflns_av_sigmaI/netI     0.0626
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        26
_diffrn_reflns_theta_min          2.34
_diffrn_reflns_theta_max          26.02
_reflns_number_total              3675
_reflns_number_gt                 2932
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement        'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction         'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?



 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0000P)²+2.9092P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constrain
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.04(3)
_refine_ls_number_reflns          3675
_refine_ls_number_parameters      208
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0675
_refine_ls_R_factor_gt            0.0411
_refine_ls_wR_factor_ref          0.0545
_refine_ls_wR_factor_gt           0.0497
_refine_ls_goodness_of_fit_ref    1.066
_refine_ls_restrained_S_all       1.066
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Fe1 Fe 0.23546(10) 0.43796(4) 0.17998(3) 0.01772(15) Uani 1 1 d . . .
Cl2 Cl -0.13115(17) 0.44355(8) 0.17561(5) 0.0248(3) Uani 1 1 d . . .
Cl1 Cl 0.32489(18) 0.43690(8) 0.27859(5) 0.0248(3) Uani 1 1 d . . .
Cl3 Cl 0.3452(2) 0.30865(8) 0.13590(5) 0.0247(3) Uani 1 1 d . . .
Cl4 Cl 0.36448(18) 0.55687(8) 0.12756(5) 0.0260(3) Uani 1 1 d . . .
S5 S -0.4270(2) 0.51829(8) 0.42456(5) 0.0203(3) Uani 1 1 d . . .
S6 S 0.0627(2) 0.61910(9) 0.48721(5) 0.0266(3) Uani 1 1 d . . .
S1 S -0.14699(19) 0.68672(8) 0.17898(5) 0.0190(3) Uani 1 1 d . . .
S4 S -0.2416(2) 0.58468(7) 0.30731(5) 0.0183(3) Uani 1 1 d . . .
S2 S 0.2761(2) 0.76096(8) 0.22778(5) 0.0201(3) Uani 1 1 d . . .
S3 S 0.16098(19) 0.66842(8) 0.35864(5) 0.0197(3) Uani 1 1 d . . .
F1 F -0.0829(6) 0.7150(2) 0.03390(13) 0.0549(10) Uani 1 1 d . . .
F2 F -0.3117(5) 0.8077(3) 0.07582(13) 0.0557(10) Uani 1 1 d . . .
F3 F 0.0094(7) 0.8553(3) 0.04547(16) 0.0777(13) Uani 1 1 d . . .
C4 C -0.0948(8) 0.7870(3) 0.0726(2) 0.0291(13) Uani 1 1 d . . .
C3 C 0.1952(8) 0.7976(3) 0.15574(19) 0.0187(11) Uani 1 1 d . . .
H3 H 0.2827 0.8390 0.1334 0.022 Uiso 1 1 calc R . .
C2 C 0.0012(7) 0.7640(3) 0.13318(19) 0.0169(10) Uani 1 1 d . . .
C1 C 0.0405(7) 0.6922(3) 0.23952(19) 0.0151(10) Uani 1 1 d . . .
C5 C -0.0038(7) 0.6507(3) 0.29537(19) 0.0160(11) Uani 1 1 d . . .
C6 C -0.2072(7) 0.5744(3) 0.38673(17) 0.0153(10) Uani 1 1 d . . .
C7 C -0.0170(7) 0.6127(3) 0.4098(2) 0.0173(11) Uani 1 1 d . . .
C9 C -0.3342(8) 0.5237(3) 0.50420(19) 0.0218(11) Uani 1 1 d . . .
H9A H -0.4643 0.5162 0.5307 0.026 Uiso 1 1 calc R . .
H9B H -0.2331 0.4721 0.5120 0.026 Uiso 1 1 calc R . .
C8 C -0.2162(8) 0.6122(3) 0.52103(19) 0.0254(12) Uani 1 1 d . . .
H8A H -0.2034 0.6162 0.5653 0.031 Uiso 1 1 calc R . .
H8B H -0.3055 0.6645 0.5071 0.031 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Fe1 Cl2 2.1793(12) . ?
Fe1 Cl3 2.1958(13) . ?
Fe1 Cl4 2.1977(13) . ?
Fe1 Cl1 2.2129(12) . ?
S5 C6 1.742(4) . ?
S5 C9 1.822(4) . ?
S6 C7 1.755(5) . ?
S6 C8 1.815(5) . ?
S1 C1 1.727(4) . ?
S1 C2 1.735(4) . ?
S4 C5 1.723(4) . ?
S4 C6 1.749(4) . ?
S2 C3 1.724(4) . ?
S2 C1 1.733(4) . ?
S3 C5 1.709(4) . ?
S3 C7 1.732(4) . ?
F1 C4 1.338(5) . ?
F2 C4 1.323(6) . ?
F3 C4 1.304(5) . ?
C4 C2 1.476(6) . ?
C3 C2 1.342(6) . ?
C1 C5 1.381(6) . ?
C6 C7 1.354(6) . ?
C9 C8 1.501(6) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
Cl2 Fe1 Cl3 107.96(5) . . ?
Cl2 Fe1 Cl4 107.23(5) . . ?
Cl3 Fe1 Cl4 109.37(5) . . ?
Cl2 Fe1 Cl1 106.39(5) . . ?
Cl3 Fe1 Cl1 110.34(5) . . ?
Cl4 Fe1 Cl1 115.23(5) . . ?
C6 S5 C9 101.8(2) . . ?
C7 S6 C8 98.1(2) . . ?
C1 S1 C2 94.8(2) . . ?
C5 S4 C6 95.8(2) . . ?
C3 S2 C1 94.8(2) . . ?
C5 S3 C7 95.8(2) . . ?
F3 C4 F2 108.4(4) . . ?
F3 C4 F1 106.0(4) . . ?
F2 C4 F1 105.1(4) . . ?
F3 C4 C2 113.0(4) . . ?
F2 C4 C2 112.2(4) . . ?
F1 C4 C2 111.6(4) . . ?
C2 C3 S2 117.5(3) . . ?
C3 C2 C4 125.3(4) . . ?
C3 C2 S1 117.1(3) . . ?
C4 C2 S1 117.6(3) . . ?
C5 C1 S1 122.0(3) . . ?
C5 C1 S2 122.1(3) . . ?
S1 C1 S2 115.7(2) . . ?
C1 C5 S3 122.5(3) . . ?
C1 C5 S4 121.9(3) . . ?
S3 C5 S4 115.4(2) . . ?
C7 C6 S5 129.7(3) . . ?
C7 C6 S4 115.4(3) . . ?
S5 C6 S4 114.8(2) . . ?
C6 C7 S3 117.4(3) . . ?
C6 C7 S6 127.1(3) . . ?
S3 C7 S6 115.4(3) . . ?
C8 C9 S5 114.2(3) . . ?
C9 C8 S6 111.9(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.999
_diffrn_reflns_theta_full              26.02
_diffrn_measured_fraction_theta_full   0.999
_refine_diff_density_max    0.410
_refine_diff_density_min   -0.420
_refine_diff_density_rms    0.105




