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Copy path[8]α-Oligothiophenes.cif
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[8]α-Oligothiophenes.cif
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data_HT5H
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common H-T5-H
_chemical_melting_point ?
_chemical_formula_moiety 'C12 H4 S5'
_chemical_formula_sum
'C12 H4 S5'
_chemical_formula_weight 308.45
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'
'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 Pnma
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
_cell_length_a 11.171(4)
_cell_length_b 25.098(9)
_cell_length_c 3.8852(13)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 1089.3(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 153(2)
_cell_measurement_reflns_used 999
_cell_measurement_theta_min 5
_cell_measurement_theta_max 60
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.881
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 624
_exptl_absorpt_coefficient_mu 1.028
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7904
_exptl_absorpt_correction_T_max 0.9504
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_special_details
;
Sample presented scattering with large rocking curves,
so 1 deg frame widths were used for data collection.
;
_diffrn_ambient_temperature 153(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 'ccd area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9472
_diffrn_reflns_av_R_equivalents 0.1112
_diffrn_reflns_av_sigmaI/netI 0.0660
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -32
_diffrn_reflns_limit_k_max 32
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_limit_l_max 5
_diffrn_reflns_theta_min 1.62
_diffrn_reflns_theta_max 27.25
_reflns_number_total 1228
_reflns_number_gt 870
_reflns_threshold_expression >2sigma(I)
_computing_data_collection BrukerSMART
_computing_cell_refinement CellNow
_computing_data_reduction BrukerSAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Diamond3.0
_computing_publication_material WinGX
_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^)+(0.0236P)^2^+37.7608P] 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 constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1228
_refine_ls_number_parameters 79
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.1344
_refine_ls_R_factor_gt 0.1033
_refine_ls_wR_factor_ref 0.2358
_refine_ls_wR_factor_gt 0.2230
_refine_ls_goodness_of_fit_ref 1.142
_refine_ls_restrained_S_all 1.139
_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 0.7331(3) 0.7500 0.1987(9) 0.0151(7) Uani 1 2 d SU . .
S2 S 1.03565(18) 0.67302(9) -0.2116(6) 0.0138(5) Uani 1 1 d . . .
S3 S 0.7378(2) 0.59376(9) 0.1873(7) 0.0189(6) Uani 1 1 d . . .
C2 C 0.8314(8) 0.7005(4) 0.067(3) 0.0149(19) Uani 1 1 d . . .
C1 C 0.9366(8) 0.7216(4) -0.073(3) 0.016(2) Uani 1 1 d . . .
C3 C 0.8311(8) 0.6443(3) 0.061(2) 0.0123(18) Uani 1 1 d . . .
C4 C 0.9361(8) 0.6238(4) -0.080(2) 0.0152(19) Uani 1 1 d . . .
C5 C 0.9401(9) 0.5675(4) -0.088(3) 0.020(2) Uani 1 1 d . . .
H5 H 1.0050 0.5472 -0.1764 0.024 Uiso 1 1 calc R . .
C6 C 0.8390(9) 0.5464(4) 0.048(3) 0.021(2) Uani 1 1 d . . .
H6 H 0.8251 0.5092 0.0655 0.026 Uiso 1 1 calc R . .
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 0.0087(14) 0.0182(15) 0.0184(17) 0.000 0.0095(13) 0.000
S2 0.0084(9) 0.0173(10) 0.0159(11) -0.0019(10) -0.0045(8) 0.0007(9)
S3 0.0141(11) 0.0190(11) 0.0236(13) 0.0014(10) 0.0050(10) -0.0008(9)
C2 0.010(4) 0.021(5) 0.014(5) 0.000(4) -0.003(4) 0.001(4)
C1 0.008(4) 0.023(5) 0.017(5) -0.003(4) 0.002(4) 0.004(4)
C3 0.011(4) 0.012(4) 0.014(4) -0.003(4) -0.002(4) -0.001(3)
C4 0.010(4) 0.025(5) 0.011(4) -0.001(4) -0.001(3) -0.001(4)
C5 0.016(5) 0.022(5) 0.023(5) -0.002(4) -0.003(4) 0.003(4)
C6 0.026(5) 0.011(5) 0.027(6) 0.003(4) -0.005(5) 0.004(4)
_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 1.736(10) 7_575 ?
S1 C2 1.736(10) . ?
S2 C1 1.732(9) . ?
S2 C4 1.739(10) . ?
S3 C3 1.714(9) . ?
S3 C6 1.727(10) . ?
C2 C1 1.399(13) . ?
C2 C3 1.409(12) . ?
C1 C1 1.427(18) 7_575 ?
C3 C4 1.392(12) . ?
C4 C5 1.415(13) . ?
C5 C6 1.354(15) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
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 C2 91.4(6) 7_575 . ?
C1 S2 C4 90.0(4) . . ?
C3 S3 C6 91.2(5) . . ?
C1 C2 C3 112.0(8) . . ?
C1 C2 S1 112.0(7) . . ?
C3 C2 S1 136.0(8) . . ?
C2 C1 C1 112.2(5) . 7_575 ?
C2 C1 S2 113.0(7) . . ?
C1 C1 S2 134.7(3) 7_575 . ?
C4 C3 C2 112.0(9) . . ?
C4 C3 S3 110.5(7) . . ?
C2 C3 S3 137.5(8) . . ?
C3 C4 C5 113.9(8) . . ?
C3 C4 S2 113.1(7) . . ?
C5 C4 S2 133.0(7) . . ?
C6 C5 C4 110.8(9) . . ?
C6 C5 H5 124.6 . . ?
C4 C5 H5 124.6 . . ?
C5 C6 S3 113.6(8) . . ?
C5 C6 H6 123.2 . . ?
S3 C6 H6 123.2 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 S1 C2 C1 0.0(10) 7_575 . . . ?
C2 S1 C2 C3 -178.6(8) 7_575 . . . ?
C3 C2 C1 C1 179.0(6) . . . 7_575 ?
S1 C2 C1 C1 0.0(7) . . . 7_575 ?
C3 C2 C1 S2 -0.3(11) . . . . ?
S1 C2 C1 S2 -179.3(5) . . . . ?
C4 S2 C1 C2 -0.1(7) . . . . ?
C4 S2 C1 C1 -179.2(5) . . . 7_575 ?
C1 C2 C3 C4 0.7(13) . . . . ?
S1 C2 C3 C4 179.4(8) . . . . ?
C1 C2 C3 S3 179.1(8) . . . . ?
S1 C2 C3 S3 -2.3(19) . . . . ?
C6 S3 C3 C4 -0.5(8) . . . . ?
C6 S3 C3 C2 -178.8(12) . . . . ?
C2 C3 C4 C5 179.4(9) . . . . ?
S3 C3 C4 C5 0.6(11) . . . . ?
C2 C3 C4 S2 -0.8(11) . . . . ?
S3 C3 C4 S2 -179.6(5) . . . . ?
C1 S2 C4 C3 0.6(7) . . . . ?
C1 S2 C4 C5 -179.7(10) . . . . ?
C3 C4 C5 C6 -0.4(13) . . . . ?
S2 C4 C5 C6 179.9(8) . . . . ?
C4 C5 C6 S3 0.0(12) . . . . ?
C3 S3 C6 C5 0.3(9) . . . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 27.25
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max 1.166
_refine_diff_density_min -1.598
_refine_diff_density_rms 0.203
#===END
data_TIPST5TIPS
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common TIPS-T5-TIPS
_chemical_melting_point ?
_chemical_formula_moiety 'C30 H44 S5 Si2'
_chemical_formula_sum
'C30 H44 S5 Si2'
_chemical_formula_weight 621.13
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'
'Si' 'Si' 0.0817 0.0704
'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 Tetragonal
_symmetry_space_group_name_H-M P-421c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
_cell_length_a 16.2367(15)
_cell_length_b 16.2367(15)
_cell_length_c 13.0410(17)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 3438.0(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 153(2)
_cell_measurement_reflns_used 999
_cell_measurement_theta_min 5
_cell_measurement_theta_max 60
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.2
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.200
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1328
_exptl_absorpt_coefficient_mu 0.425
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.903
_exptl_absorpt_correction_T_max 0.919
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 153(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 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 38409
_diffrn_reflns_av_R_equivalents 0.0767
_diffrn_reflns_av_sigmaI/netI 0.0607
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 1.77
_diffrn_reflns_theta_max 29.60
_reflns_number_total 4814
_reflns_number_gt 4241
_reflns_threshold_expression >2sigma(I)
_computing_data_collection BrukerSMART
_computing_cell_refinement BrukerSMART
_computing_data_reduction BrukerSAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Diamond
_computing_publication_material WinGX
_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^)+(0.0669P)^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 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 0.41(10)
_refine_ls_number_reflns 4814
_refine_ls_number_parameters 168
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0589
_refine_ls_R_factor_gt 0.0483
_refine_ls_wR_factor_ref 0.1190
_refine_ls_wR_factor_gt 0.1092
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_restrained_S_all 1.037
_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
C1 C 0.77221(16) 0.83700(17) 0.2782(2) 0.0182(6) Uani 1 1 d . . .
C2 C 0.74081(18) 0.85266(18) 0.3741(2) 0.0232(6) Uani 1 1 d . . .
H2 H 0.7665 0.8356 0.4360 0.028 Uiso 1 1 calc R . .
C3 C 0.66608(18) 0.89700(18) 0.3703(2) 0.0214(6) Uani 1 1 d . . .
C4 C 0.63965(16) 0.91453(16) 0.2721(2) 0.0156(5) Uani 1 1 d . . .
C5 C 0.56420(16) 0.96000(15) 0.2720(2) 0.0143(5) Uani 1 1 d . . .
C6 C 0.53726(16) 0.97719(17) 0.3707(2) 0.0179(6) Uani 1 1 d . . .
C7 C 0.90526(19) 0.8144(2) 0.1165(2) 0.0281(7) Uani 1 1 d . . .
H7 H 0.8569 0.8080 0.0697 0.034 Uiso 1 1 calc R . .
C8 C 0.9299(2) 0.9048(2) 0.1108(3) 0.0518(11) Uani 1 1 d . . .
H8A H 0.8856 0.9389 0.1390 0.062 Uiso 1 1 calc R . .
H8B H 0.9396 0.9201 0.0391 0.062 Uiso 1 1 calc R . .
H8C H 0.9804 0.9135 0.1505 0.062 Uiso 1 1 calc R . .
C9 C 0.9737(2) 0.7603(2) 0.0715(3) 0.0394(8) Uani 1 1 d . . .
H9A H 0.9571 0.7023 0.0749 0.047 Uiso 1 1 calc R . .
H9B H 1.0245 0.7682 0.1110 0.047 Uiso 1 1 calc R . .
H9C H 0.9833 0.7758 -0.0002 0.047 Uiso 1 1 calc R . .
C10 C 0.94226(19) 0.80109(19) 0.3557(2) 0.0270(6) Uani 1 1 d . . .
H10 H 0.9164 0.7766 0.4184 0.032 Uiso 1 1 calc R . .
C11 C 0.9566(3) 0.8925(2) 0.3797(4) 0.0592(13) Uani 1 1 d . . .
H11A H 0.9034 0.9201 0.3890 0.071 Uiso 1 1 calc R . .
H11B H 0.9864 0.9183 0.3227 0.071 Uiso 1 1 calc R . .
H11C H 0.9892 0.8976 0.4426 0.071 Uiso 1 1 calc R . .
C12 C 1.02602(19) 0.7583(2) 0.3428(3) 0.0344(8) Uani 1 1 d . . .
H12A H 1.0174 0.6997 0.3286 0.041 Uiso 1 1 calc R . .
H12B H 1.0582 0.7644 0.4059 0.041 Uiso 1 1 calc R . .
H12C H 1.0559 0.7836 0.2856 0.041 Uiso 1 1 calc R . .
C13 C 0.84466(18) 0.66621(17) 0.2413(2) 0.0241(6) Uani 1 1 d . . .
H13 H 0.8971 0.6365 0.2255 0.029 Uiso 1 1 calc R . .
C14 C 0.8136(3) 0.6337(2) 0.3446(3) 0.0432(9) Uani 1 1 d . . .
H14A H 0.8533 0.6476 0.3984 0.052 Uiso 1 1 calc R . .
H14B H 0.8072 0.5738 0.3409 0.052 Uiso 1 1 calc R . .
H14C H 0.7603 0.6590 0.3606 0.052 Uiso 1 1 calc R . .
C15 C 0.7831(2) 0.6452(2) 0.1556(3) 0.0420(9) Uani 1 1 d . . .
H15A H 0.8039 0.6662 0.0901 0.050 Uiso 1 1 calc R . .
H15B H 0.7298 0.6707 0.1708 0.050 Uiso 1 1 calc R . .
H15C H 0.7765 0.5853 0.1513 0.050 Uiso 1 1 calc R . .
S1 S 0.70758(4) 0.87615(4) 0.18361(5) 0.01786(14) Uani 1 1 d . . .
S2 S 0.60158(5) 0.93770(5) 0.46446(6) 0.02502(17) Uani 1 1 d . . .
S3 S 0.5000 1.0000 0.17838(7) 0.01605(18) Uani 1 2 d S . .
Si1 Si 0.86954(4) 0.77947(4) 0.24641(6) 0.01660(16) Uani 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
C1 0.0139(12) 0.0166(12) 0.0242(14) 0.0011(10) -0.0037(10) 0.0066(10)
C2 0.0219(14) 0.0261(15) 0.0217(15) -0.0034(12) -0.0014(11) 0.0053(11)
C3 0.0230(14) 0.0217(14) 0.0193(14) -0.0023(11) 0.0003(11) 0.0062(11)
C4 0.0119(12) 0.0146(12) 0.0204(13) -0.0014(10) 0.0018(10) 0.0048(9)
C5 0.0113(11) 0.0118(12) 0.0196(13) 0.0016(9) -0.0014(10) 0.0037(9)
C6 0.0174(14) 0.0171(13) 0.0193(14) -0.0002(11) -0.0003(11) 0.0037(10)
C7 0.0223(15) 0.0333(17) 0.0288(16) 0.0097(14) 0.0020(13) 0.0048(13)
C8 0.046(2) 0.039(2) 0.070(3) 0.022(2) 0.025(2) 0.0044(18)
C9 0.038(2) 0.050(2) 0.0308(17) 0.0020(16) 0.0120(15) 0.0118(16)
C10 0.0216(15) 0.0297(16) 0.0298(16) -0.0050(13) -0.0037(12) 0.0051(12)
C11 0.045(2) 0.037(2) 0.095(4) -0.033(2) -0.030(2) 0.0101(18)
C12 0.0225(16) 0.0385(19) 0.042(2) -0.0029(15) -0.0103(14) 0.0097(13)
C13 0.0227(14) 0.0175(13) 0.0320(16) -0.0020(13) 0.0054(13) 0.0038(10)
C14 0.054(2) 0.0240(16) 0.052(2) 0.0047(16) 0.0181(18) 0.0002(16)
C15 0.040(2) 0.0306(18) 0.055(2) -0.0103(16) -0.0051(18) -0.0041(15)
S1 0.0142(3) 0.0194(3) 0.0200(3) 0.0003(3) 0.0009(3) 0.0061(2)
S2 0.0234(4) 0.0339(4) 0.0177(3) -0.0016(3) -0.0014(3) 0.0175(3)
S3 0.0132(4) 0.0167(4) 0.0183(4) 0.000 0.000 0.0050(3)
Si1 0.0114(3) 0.0143(3) 0.0241(4) -0.0001(3) -0.0002(3) 0.0062(3)
_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
C1 C2 1.374(4) . ?
C1 S1 1.740(3) . ?
C1 Si1 1.882(3) . ?
C2 C3 1.412(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(4) . ?
C3 S2 1.744(3) . ?
C4 C5 1.430(3) . ?
C4 S1 1.713(3) . ?
C5 C6 1.388(4) . ?
C5 S3 1.732(3) . ?
C6 C6 1.419(5) 2_675 ?
C6 S2 1.731(3) . ?
C7 C8 1.523(5) . ?
C7 C9 1.534(4) . ?
C7 Si1 1.879(3) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.535(5) . ?
C10 C12 1.536(4) . ?
C10 Si1 1.884(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.532(5) . ?
C13 C15 1.538(5) . ?
C13 Si1 1.884(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
S3 C5 1.732(3) 2_675 ?
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 C1 S1 110.7(2) . . ?
C2 C1 Si1 127.2(2) . . ?
S1 C1 Si1 122.08(16) . . ?
C1 C2 C3 112.4(3) . . ?
C1 C2 H2 123.8 . . ?
C3 C2 H2 123.8 . . ?
C4 C3 C2 113.9(3) . . ?
C4 C3 S2 112.9(2) . . ?
C2 C3 S2 133.2(2) . . ?
C3 C4 C5 111.9(2) . . ?
C3 C4 S1 110.47(19) . . ?
C5 C4 S1 137.6(2) . . ?
C6 C5 C4 111.9(2) . . ?
C6 C5 S3 112.87(18) . . ?
C4 C5 S3 135.2(2) . . ?
C5 C6 C6 111.96(14) . 2_675 ?
C5 C6 S2 112.97(18) . . ?
C6 C6 S2 135.07(9) 2_675 . ?
C8 C7 C9 110.1(3) . . ?
C8 C7 Si1 114.6(3) . . ?
C9 C7 Si1 113.3(2) . . ?
C8 C7 H7 106.1 . . ?
C9 C7 H7 106.1 . . ?
Si1 C7 H7 106.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C12 109.0(3) . . ?
C11 C10 Si1 115.4(2) . . ?
C12 C10 Si1 112.8(2) . . ?
C11 C10 H10 106.3 . . ?
C12 C10 H10 106.3 . . ?
Si1 C10 H10 106.3 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C15 110.4(3) . . ?
C14 C13 Si1 112.1(2) . . ?
C15 C13 Si1 112.4(2) . . ?
C14 C13 H13 107.2 . . ?
C15 C13 H13 107.2 . . ?
Si1 C13 H13 107.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 S1 C1 92.50(13) . . ?
C6 S2 C3 90.32(13) . . ?
C5 S3 C5 90.34(18) 2_675 . ?
C7 Si1 C1 107.95(13) . . ?
C7 Si1 C10 115.64(15) . . ?
C1 Si1 C10 105.47(13) . . ?
C7 Si1 C13 109.24(15) . . ?
C1 Si1 C13 108.19(13) . . ?
C10 Si1 C13 110.04(14) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 C1 C2 C3 -1.0(3) . . . . ?
Si1 C1 C2 C3 -179.5(2) . . . . ?
C1 C2 C3 C4 0.7(4) . . . . ?
C1 C2 C3 S2 -176.6(3) . . . . ?
C2 C3 C4 C5 -179.5(2) . . . . ?
S2 C3 C4 C5 -1.7(3) . . . . ?
C2 C3 C4 S1 -0.1(3) . . . . ?
S2 C3 C4 S1 177.78(15) . . . . ?
C3 C4 C5 C6 1.6(3) . . . . ?
S1 C4 C5 C6 -177.6(3) . . . . ?
C3 C4 C5 S3 -179.9(2) . . . . ?
S1 C4 C5 S3 0.9(5) . . . . ?
C4 C5 C6 C6 179.6(3) . . . 2_675 ?
S3 C5 C6 C6 0.7(4) . . . 2_675 ?
C4 C5 C6 S2 -0.8(3) . . . . ?
S3 C5 C6 S2 -179.71(14) . . . . ?
C3 C4 S1 C1 -0.4(2) . . . . ?
C5 C4 S1 C1 178.8(3) . . . . ?
C2 C1 S1 C4 0.8(2) . . . . ?
Si1 C1 S1 C4 179.42(18) . . . . ?
C5 C6 S2 C3 -0.1(2) . . . . ?
C6 C6 S2 C3 179.4(4) 2_675 . . . ?
C4 C3 S2 C6 1.0(2) . . . . ?
C2 C3 S2 C6 178.3(3) . . . . ?
C6 C5 S3 C5 -0.25(14) . . . 2_675 ?
C4 C5 S3 C5 -178.8(3) . . . 2_675 ?
C8 C7 Si1 C1 64.3(3) . . . . ?
C9 C7 Si1 C1 -168.2(2) . . . . ?
C8 C7 Si1 C10 -53.5(3) . . . . ?
C9 C7 Si1 C10 73.9(3) . . . . ?
C8 C7 Si1 C13 -178.3(2) . . . . ?
C9 C7 Si1 C13 -50.8(3) . . . . ?
C2 C1 Si1 C7 -156.1(3) . . . . ?
S1 C1 Si1 C7 25.5(2) . . . . ?
C2 C1 Si1 C10 -31.9(3) . . . . ?
S1 C1 Si1 C10 149.67(18) . . . . ?
C2 C1 Si1 C13 85.8(3) . . . . ?
S1 C1 Si1 C13 -92.6(2) . . . . ?
C11 C10 Si1 C7 65.2(3) . . . . ?
C12 C10 Si1 C7 -61.0(3) . . . . ?
C11 C10 Si1 C1 -54.0(3) . . . . ?
C12 C10 Si1 C1 179.9(2) . . . . ?
C11 C10 Si1 C13 -170.4(3) . . . . ?
C12 C10 Si1 C13 63.4(3) . . . . ?
C14 C13 Si1 C7 -179.0(2) . . . . ?
C15 C13 Si1 C7 -53.9(3) . . . . ?
C14 C13 Si1 C1 -61.7(3) . . . . ?
C15 C13 Si1 C1 63.3(3) . . . . ?
C14 C13 Si1 C10 53.0(3) . . . . ?
C15 C13 Si1 C10 178.1(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 29.60
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.701
_refine_diff_density_min -0.547
_refine_diff_density_rms 0.141
#===END
data_TIPST7TIPS
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common TIPS-T7-TIPS
_chemical_melting_point ?
_chemical_formula_moiety 'C34 H44 S7 Si2'
_chemical_formula_sum
'C34 H44 S7 Si2'
_chemical_formula_weight 733.29
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'
'S' 'S' 0.1246 0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Si' 'Si' 0.0817 0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M Pccn
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
_cell_length_a 17.9934(16)
_cell_length_b 29.790(3)
_cell_length_c 13.4276(12)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 7197.6(11)
_cell_formula_units_Z 8
_cell_measurement_temperature 153(2)
_cell_measurement_reflns_used 999
_cell_measurement_theta_min 5
_cell_measurement_theta_max 60
_exptl_crystal_description plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3104
_exptl_absorpt_coefficient_mu 0.529
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.8150
_exptl_absorpt_correction_T_max 0.9490
_exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 153(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 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 68999
_diffrn_reflns_av_R_equivalents 0.0747
_diffrn_reflns_av_sigmaI/netI 0.0491
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -38
_diffrn_reflns_limit_k_max 38
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 1.32
_diffrn_reflns_theta_max 27.56
_reflns_number_total 8281
_reflns_number_gt 6504
_reflns_threshold_expression >2sigma(I)
_computing_data_collection BrukerSMART
_computing_cell_refinement BrukerSMART
_computing_data_reduction BrukerSAINT
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics Diamond3.0
_computing_publication_material WinGX
_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^)+(0.0482P)^2^+0.0134P] 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 constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 8281
_refine_ls_number_parameters 400
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0529
_refine_ls_R_factor_gt 0.0366
_refine_ls_wR_factor_ref 0.0953
_refine_ls_wR_factor_gt 0.0823
_refine_ls_goodness_of_fit_ref 1.010
_refine_ls_restrained_S_all 1.010
_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
C1 C 0.35852(12) 0.58529(7) 0.70104(16) 0.0223(5) Uani 1 1 d . . .
C2 C 0.33707(12) 0.56840(7) 0.61019(16) 0.0229(5) Uani 1 1 d . . .
H2 H 0.3450 0.5836 0.5489 0.028 Uiso 1 1 calc R . .
C3 C 0.30194(12) 0.52597(7) 0.61749(15) 0.0204(4) Uani 1 1 d . . .
C4 C 0.29579(11) 0.51034(7) 0.71426(15) 0.0185(4) Uani 1 1 d . . .
C5 C 0.26783(11) 0.46581(7) 0.71806(15) 0.0182(4) Uani 1 1 d . . .
C6 C 0.25471(11) 0.44850(7) 0.62362(15) 0.0183(4) Uani 1 1 d . . .
C7 C 0.23433(11) 0.40275(7) 0.62697(15) 0.0175(4) Uani 1 1 d . . .
C8 C 0.23153(11) 0.38646(7) 0.72382(15) 0.0176(4) Uani 1 1 d . . .
C9 C 0.20794(11) 0.34116(7) 0.72783(15) 0.0167(4) Uani 1 1 d . . .
C10 C 0.19474(11) 0.32372(7) 0.63372(15) 0.0174(4) Uani 1 1 d . . .
C11 C 0.16630(11) 0.27949(7) 0.63804(15) 0.0168(4) Uani 1 1 d . . .
C12 C 0.15667(11) 0.26456(6) 0.73534(15) 0.0163(4) Uani 1 1 d . . .
C13 C 0.12088(11) 0.22175(7) 0.73880(15) 0.0168(4) Uani 1 1 d . . .
C14 C 0.10579(12) 0.20531(7) 0.64410(15) 0.0187(4) Uani 1 1 d . . .
C15 C 0.06466(12) 0.16470(7) 0.64440(16) 0.0219(5) Uani 1 1 d . . .
H15 H 0.0511 0.1490 0.5855 0.026 Uiso 1 1 calc R . .
C16 C 0.04648(12) 0.15031(7) 0.73824(16) 0.0204(4) Uani 1 1 d . . .
C17 C 0.40499(14) 0.65848(8) 0.84865(18) 0.0330(6) Uani 1 1 d . . .
H17 H 0.4075 0.6330 0.8969 0.040 Uiso 1 1 calc R . .
C18 C 0.52116(12) 0.60971(7) 0.72183(17) 0.0259(5) Uani 1 1 d . . .
H18 H 0.5559 0.6356 0.7302 0.031 Uiso 1 1 calc R . .
C19 C 0.41244(13) 0.67127(7) 0.61100(18) 0.0280(5) Uani 1 1 d . . .
H19 H 0.4199 0.6516 0.5516 0.034 Uiso 1 1 calc R . .
C20 C 0.32767(18) 0.67832(11) 0.8596(2) 0.0594(9) Uani 1 1 d . . .
H20A H 0.3188 0.6861 0.9295 0.071 Uiso 1 1 calc R . .
H20B H 0.2906 0.6563 0.8379 0.071 Uiso 1 1 calc R . .
H20C H 0.3236 0.7054 0.8184 0.071 Uiso 1 1 calc R . .
C21 C 0.46538(18) 0.69185(10) 0.8812(2) 0.0610(10) Uani 1 1 d . . .
H21A H 0.4633 0.7186 0.8388 0.073 Uiso 1 1 calc R . .
H21B H 0.5143 0.6777 0.8749 0.073 Uiso 1 1 calc R . .
H21C H 0.4571 0.7005 0.9507 0.073 Uiso 1 1 calc R . .
C22 C 0.53618(14) 0.57748(8) 0.80831(18) 0.0336(6) Uani 1 1 d . . .
H22A H 0.5024 0.5518 0.8038 0.040 Uiso 1 1 calc R . .
H22B H 0.5281 0.5931 0.8716 0.040 Uiso 1 1 calc R . .
H22C H 0.5877 0.5669 0.8049 0.040 Uiso 1 1 calc R . .
C23 C 0.54077(14) 0.58748(8) 0.62271(18) 0.0334(6) Uani 1 1 d . . .
H23A H 0.5920 0.5764 0.6252 0.040 Uiso 1 1 calc R . .
H23B H 0.5360 0.6095 0.5688 0.040 Uiso 1 1 calc R . .
H23C H 0.5069 0.5623 0.6105 0.040 Uiso 1 1 calc R . .
C24 C 0.47326(15) 0.70744(8) 0.6044(2) 0.0421(7) Uani 1 1 d . . .
H24A H 0.4677 0.7242 0.5420 0.051 Uiso 1 1 calc R . .
H24B H 0.5223 0.6931 0.6061 0.051 Uiso 1 1 calc R . .
H24C H 0.4686 0.7281 0.6609 0.051 Uiso 1 1 calc R . .
C25 C 0.33548(14) 0.69204(8) 0.5980(2) 0.0409(7) Uani 1 1 d . . .
H25A H 0.3269 0.7142 0.6508 0.049 Uiso 1 1 calc R . .
H25B H 0.2976 0.6684 0.6020 0.049 Uiso 1 1 calc R . .
H25C H 0.3325 0.7068 0.5329 0.049 Uiso 1 1 calc R . .
C26 C -0.01764(13) 0.08391(7) 0.89320(16) 0.0268(5) Uani 1 1 d . . .
H26 H -0.0127 0.1096 0.9407 0.032 Uiso 1 1 calc R . .
C27 C -0.03422(12) 0.06960(7) 0.65699(17) 0.0250(5) Uani 1 1 d . . .
H27 H -0.0404 0.0889 0.5966 0.030 Uiso 1 1 calc R . .
C28 C -0.11906(13) 0.14399(8) 0.76660(19) 0.0331(6) Uani 1 1 d . . .
H28 H -0.1617 0.1225 0.7695 0.040 Uiso 1 1 calc R . .
C29 C 0.05271(15) 0.05615(9) 0.90461(19) 0.0388(6) Uani 1 1 d . . .
H29A H 0.0603 0.0489 0.9751 0.047 Uiso 1 1 calc R . .
H29B H 0.0953 0.0733 0.8799 0.047 Uiso 1 1 calc R . .
H29C H 0.0479 0.0283 0.8662 0.047 Uiso 1 1 calc R . .
C30 C -0.08561(15) 0.05666(9) 0.9284(2) 0.0429(7) Uani 1 1 d . . .
H30A H -0.0897 0.0291 0.8889 0.052 Uiso 1 1 calc R . .
H30B H -0.1307 0.0747 0.9199 0.052 Uiso 1 1 calc R . .
H30C H -0.0796 0.0489 0.9989 0.052 Uiso 1 1 calc R . .
C31 C 0.03693(14) 0.04286(8) 0.63967(18) 0.0317(6) Uani 1 1 d . . .
H31A H 0.0436 0.0212 0.6939 0.038 Uiso 1 1 calc R . .
H31B H 0.0795 0.0634 0.6378 0.038 Uiso 1 1 calc R . .
H31C H 0.0334 0.0268 0.5762 0.038 Uiso 1 1 calc R . .
C32 C -0.10188(14) 0.03848(8) 0.65841(19) 0.0369(6) Uani 1 1 d . . .
H32A H -0.1030 0.0207 0.5970 0.044 Uiso 1 1 calc R . .
H32B H -0.1473 0.0565 0.6632 0.044 Uiso 1 1 calc R . .
H32C H -0.0986 0.0183 0.7159 0.044 Uiso 1 1 calc R . .
C33 C -0.12422(15) 0.17431(9) 0.8584(2) 0.0515(8) Uani 1 1 d . . .
H33A H -0.0810 0.1943 0.8605 0.062 Uiso 1 1 calc R . .
H33B H -0.1253 0.1558 0.9186 0.062 Uiso 1 1 calc R . .
H33C H -0.1697 0.1923 0.8547 0.062 Uiso 1 1 calc R . .
C34 C -0.12747(17) 0.17136(11) 0.6713(2) 0.0622(10) Uani 1 1 d . . .
H34A H -0.1732 0.1892 0.6747 0.075 Uiso 1 1 calc R . .
H34B H -0.1299 0.1510 0.6139 0.075 Uiso 1 1 calc R . .
H34C H -0.0847 0.1915 0.6639 0.075 Uiso 1 1 calc R . .
S1 S 0.33266(3) 0.548586(17) 0.79662(4) 0.02196(13) Uani 1 1 d . . .
S2 S 0.27274(3) 0.486844(18) 0.52963(4) 0.02298(13) Uani 1 1 d . . .
S3 S 0.25377(3) 0.426627(17) 0.81164(4) 0.02062(12) Uani 1 1 d . . .
S4 S 0.20988(3) 0.362365(17) 0.53911(4) 0.01993(12) Uani 1 1 d . . .
S5 S 0.18642(3) 0.303678(16) 0.82281(4) 0.01744(12) Uani 1 1 d . . .
S6 S 0.13548(3) 0.241405(17) 0.55003(4) 0.02043(12) Uani 1 1 d . . .
S7 S 0.08373(3) 0.186721(17) 0.82764(4) 0.01959(12) Uani 1 1 d . . .
Si1 Si 0.42385(3) 0.633519(19) 0.72258(5) 0.02223(14) Uani 1 1 d . . .
Si2 Si -0.03052(3) 0.109576(19) 0.76615(5) 0.02120(14) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11