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Copy path[1]DPh-BTBT.CIF
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[1]DPh-BTBT.CIF
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data_shelxl
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C24 H14 S2'
_chemical_formula_weight 366.47
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0181 0.0091
'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'
'S' 'S' 0.3331 0.5567
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting ?
_symmetry_space_group_name_H-M ?
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 6.334(2)
_cell_length_b 7.462(5)
_cell_length_c 19.516(2)
_cell_angle_alpha 90.00
_cell_angle_beta 93.06(3)
_cell_angle_gamma 90.00
_cell_volume 921.1(7)
_cell_formula_units_Z 2
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.321
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 380
_exptl_absorpt_coefficient_mu 2.629
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min 0.7790
_exptl_absorpt_correction_T_max 0.7790
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 296(2)
_diffrn_radiation_wavelength 1.00000
_diffrn_radiation_type ?
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 4197
_diffrn_reflns_av_R_equivalents 0.0822
_diffrn_reflns_av_sigmaI/netI 0.0676
_diffrn_reflns_limit_h_min -3
_diffrn_reflns_limit_h_max 3
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_theta_min 2.94
_diffrn_reflns_theta_max 56.44
_reflns_number_total 1860
_reflns_number_gt 1284
_reflns_threshold_expression >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1706P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1860
_refine_ls_number_parameters 152
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1064
_refine_ls_R_factor_gt 0.0843
_refine_ls_wR_factor_ref 0.2377
_refine_ls_wR_factor_gt 0.2231
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_restrained_S_all 1.011
_refine_ls_shift/su_max 0.013
_refine_ls_shift/su_mean 0.003
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 0.2095(3) 0.40762(10) 0.95623(4) 0.0345(8) Uani 1 1 d . . .
C1 C 0.4121(10) 0.4703(3) 1.01501(15) 0.0261(19) Uani 1 1 d . . .
C2 C 0.3718(10) 0.4630(4) 0.88881(15) 0.031(2) Uani 1 1 d . . .
C3 C 0.5704(10) 0.5287(3) 0.91070(15) 0.028(2) Uani 1 1 d . . .
C4 C 0.7111(14) 0.5786(5) 0.86184(17) 0.035(3) Uani 1 1 d . . .
C5 C 0.6471(11) 0.5663(4) 0.79208(16) 0.027(2) Uani 1 1 d . . .
C6 C 0.4469(10) 0.5056(4) 0.77031(15) 0.024(2) Uani 1 1 d . . .
C7 C 0.3077(12) 0.4508(4) 0.81891(16) 0.029(2) Uani 1 1 d . . .
C8 C 0.3805(9) 0.5017(4) 0.69591(14) 0.029(2) Uani 1 1 d . . .
C9 C 0.4731(11) 0.6194(4) 0.64937(16) 0.034(2) Uani 1 1 d . . .
C10 C 0.4057(11) 0.6148(4) 0.57973(17) 0.039(2) Uani 1 1 d . . .
H5 H 0.4650 0.6937 0.5493 0.047 Uiso 1 1 calc R . .
C11 C 0.2534(10) 0.4958(5) 0.55568(17) 0.039(2) Uani 1 1 d . . .
C12 C 0.1594(11) 0.3797(5) 0.60120(18) 0.042(2) Uani 1 1 d . . .
H7 H 0.0528 0.3019 0.5855 0.051 Uiso 1 1 calc R . .
C13 C 0.2269(11) 0.3814(4) 0.67064(17) 0.041(3) Uani 1 1 d . . .
H1 H 0.830(11) 0.617(5) 0.873(2) 0.012(12) Uiso 1 1 d . . .
H2 H 0.764(11) 0.608(5) 0.765(2) 0.034(13) Uiso 1 1 d . . .
H3 H 0.157(13) 0.422(6) 0.805(2) 0.029(15) Uiso 1 1 d . . .
H4 H 0.585(10) 0.704(6) 0.667(2) 0.041(13) Uiso 1 1 d . . .
H6 H 0.224(13) 0.495(7) 0.511(3) 0.058(15) Uiso 1 1 d . . .
H8 H 0.162(7) 0.299(5) 0.6993(17) 0.021(10) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.058(2) 0.0226(4) 0.0228(4) -0.0011(2) 0.0018(5) -0.0057(4)
C1 0.042(6) 0.0135(10) 0.0229(12) -0.0007(8) 0.0003(18) -0.0005(16)
C2 0.056(7) 0.0140(10) 0.0222(11) 0.0007(8) 0.005(2) -0.0017(17)
C3 0.047(7) 0.0130(10) 0.0226(12) 0.0002(8) 0.0011(19) 0.0028(17)
C4 0.058(9) 0.0211(13) 0.0237(13) -0.0006(10) -0.004(2) -0.003(2)
C5 0.037(7) 0.0220(13) 0.0236(12) 0.0007(10) 0.005(2) -0.0017(19)
C6 0.032(6) 0.0156(10) 0.0257(12) -0.0001(9) -0.002(2) -0.0056(17)
C7 0.042(8) 0.0192(12) 0.0240(12) -0.0007(9) 0.001(2) -0.003(2)
C8 0.046(6) 0.0178(11) 0.0218(11) -0.0006(9) 0.0006(19) 0.0041(16)
C9 0.057(7) 0.0229(13) 0.0238(13) 0.0000(10) 0.003(2) -0.0008(19)
C10 0.067(8) 0.0276(14) 0.0234(13) 0.0047(10) 0.004(2) 0.006(2)
C11 0.060(8) 0.0340(16) 0.0225(13) -0.0009(11) 0.000(2) 0.005(2)
C12 0.066(8) 0.0331(17) 0.0277(14) -0.0036(12) 0.000(2) -0.004(2)
C13 0.074(8) 0.0266(14) 0.0232(13) -0.0002(10) 0.002(2) -0.007(2)
_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 C1 1.739(5) . ?
S1 C2 1.762(4) . ?
C1 C1 1.360(10) 3_667 ?
C1 C3 1.448(4) 3_667 ?
C2 C3 1.396(8) . ?
C2 C7 1.406(5) . ?
C3 C4 1.390(7) . ?
C3 C1 1.448(4) 3_667 ?
C4 C5 1.403(5) . ?
C5 C6 1.392(8) . ?
C6 C7 1.391(7) . ?
C6 C8 1.490(5) . ?
C8 C13 1.395(7) . ?
C8 C9 1.413(5) . ?
C9 C10 1.403(5) . ?
C10 C11 1.375(8) . ?
C11 C12 1.396(6) . ?
C12 C13 1.399(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
C1 S1 C2 89.4(2) . . ?
C1 C1 C3 114.1(5) 3_667 3_667 ?
C1 C1 S1 113.3(3) 3_667 . ?
C3 C1 S1 132.5(4) 3_667 . ?
C3 C2 C7 121.9(4) . . ?
C3 C2 S1 114.0(2) . . ?
C7 C2 S1 124.0(5) . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 C1 131.9(5) . 3_667 ?
C2 C3 C1 109.1(4) . 3_667 ?
C3 C4 C5 119.1(6) . . ?
C6 C5 C4 121.9(5) . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 C8 120.1(5) . . ?
C5 C6 C8 120.6(4) . . ?
C6 C7 C2 118.8(6) . . ?
C13 C8 C9 118.6(3) . . ?
C13 C8 C6 120.8(3) . . ?
C9 C8 C6 120.6(4) . . ?
C10 C9 C8 119.5(5) . . ?
C11 C10 C9 121.2(4) . . ?
C10 C11 C12 119.9(4) . . ?
C11 C12 C13 119.5(5) . . ?
C8 C13 C12 121.3(4) . . ?
_diffrn_measured_fraction_theta_max 0.416
_diffrn_reflns_theta_full 56.44
_diffrn_measured_fraction_theta_full 0.416
_refine_diff_density_max 1.130
_refine_diff_density_min -0.426
_refine_diff_density_rms 0.129