data_complex1
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C10 H22 O4 S Sn2'
_chemical_formula_weight 475.72
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'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Sn' 'Sn' -0.6537 1.4246
'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 8.1880(8)
_cell_length_b 9.8539(9)
_cell_length_c 11.5691(12)
_cell_angle_alpha 98.7370(10)
_cell_angle_beta 99.6800(10)
_cell_angle_gamma 110.703(2)
_cell_volume 837.82(14)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 3277
_cell_measurement_theta_min 2.571
_cell_measurement_theta_max 28.084
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.46
_exptl_crystal_size_mid 0.39
_exptl_crystal_size_min 0.18
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.886
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 460
_exptl_absorpt_coefficient_mu 3.106
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.3292
_exptl_absorpt_correction_T_max 0.6048
_exptl_absorpt_process_details sadabs
_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 '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 4286
_diffrn_reflns_av_R_equivalents 0.0183
_diffrn_reflns_av_sigmaI/netI 0.0318
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.02
_reflns_number_total 2895
_reflns_number_gt 2452
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_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^)+(0.0447P)^2^+0.9773P] 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 2895
_refine_ls_number_parameters 160
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0366
_refine_ls_R_factor_gt 0.0300
_refine_ls_wR_factor_ref 0.0830
_refine_ls_wR_factor_gt 0.0767
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_restrained_S_all 1.053
_refine_ls_shift/su_max 0.091
_refine_ls_shift/su_mean 0.002
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
C2 C 1.0457(6) 0.7538(6) 0.3187(5) 0.0397(11) Uani 1 1 d . . .
H2A H 1.0582 0.8399 0.3781 0.048 Uiso 1 1 calc R . .
H2B H 0.9975 0.6662 0.3505 0.048 Uiso 1 1 calc R . .
Sn1 Sn 0.61472(4) 0.96456(3) 0.29290(3) 0.03353(12) Uani 1 1 d . . .
Sn2 Sn 0.18490(4) 0.39669(3) 0.23117(3) 0.03548(12) Uani 1 1 d . . .
O1 O 0.3397(4) 0.9045(3) 0.3178(3) 0.0416(8) Uani 1 1 d . . .
C5 C 0.6539(8) 1.1917(6) 0.3487(7) 0.0575(16) Uani 1 1 d . . .
H5A H 0.7158 1.2480 0.2972 0.086 Uiso 1 1 calc R . .
H5B H 0.7242 1.2306 0.4303 0.086 Uiso 1 1 calc R . .
H5C H 0.5393 1.1993 0.3437 0.086 Uiso 1 1 calc R . .
C1 C 0.2291(6) 0.7700(5) 0.2989(4) 0.0331(10) Uani 1 1 d . . .
O2 O 0.2647(5) 0.6619(4) 0.2647(4) 0.0485(9) Uani 1 1 d . . .
C7 C 0.6925(7) 0.8594(6) 0.4250(5) 0.0448(12) Uani 1 1 d . . .
H7A H 0.8213 0.8947 0.4472 0.067 Uiso 1 1 calc R . .
H7B H 0.6424 0.7535 0.3934 0.067 Uiso 1 1 calc R . .
H7C H 0.6493 0.8821 0.4947 0.067 Uiso 1 1 calc R . .
O3 O 0.9237(5) 1.0634(4) 0.2733(3) 0.0447(9) Uani 1 1 d . . .
C6 C 0.5301(8) 0.8698(7) 0.1049(5) 0.0508(13) Uani 1 1 d . . .
H6A H 0.4248 0.8861 0.0716 0.076 Uiso 1 1 calc R . .
H6B H 0.5025 0.7647 0.0910 0.076 Uiso 1 1 calc R . .
H6C H 0.6245 0.9158 0.0671 0.076 Uiso 1 1 calc R . .
C8 C 0.2112(10) 0.4228(7) 0.4192(5) 0.0636(17) Uani 1 1 d . . .
H8A H 0.2028 0.3307 0.4408 0.095 Uiso 1 1 calc R . .
H8B H 0.1170 0.4499 0.4411 0.095 Uiso 1 1 calc R . .
H8C H 0.3258 0.4996 0.4610 0.095 Uiso 1 1 calc R . .
C4 C 1.0052(7) 0.9030(5) 0.1345(5) 0.0374(11) Uani 1 1 d . . .
H4A H 1.1256 0.9082 0.1338 0.045 Uiso 1 1 calc R . .
H4B H 0.9442 0.8916 0.0520 0.045 Uiso 1 1 calc R . .
O4 O 1.1457(5) 1.1611(4) 0.1858(3) 0.0454(9) Uani 1 1 d . . .
C10 C 0.4168(9) 0.4454(7) 0.1599(7) 0.071(2) Uani 1 1 d . . .
H10A H 0.5197 0.5162 0.2201 0.106 Uiso 1 1 calc R . .
H10B H 0.3995 0.4865 0.0909 0.106 Uiso 1 1 calc R . .
H10C H 0.4358 0.3555 0.1364 0.106 Uiso 1 1 calc R . .
C9 C -0.0657(8) 0.3580(6) 0.1173(5) 0.0532(14) Uani 1 1 d . . .
H9A H -0.0506 0.3664 0.0379 0.080 Uiso 1 1 calc R . .
H9B H -0.1103 0.4303 0.1485 0.080 Uiso 1 1 calc R . .
H9C H -0.1498 0.2597 0.1140 0.080 Uiso 1 1 calc R . .
C3 C 1.0225(6) 1.0519(5) 0.2068(4) 0.0317(10) Uani 1 1 d . . .
S1 S 0.88996(16) 0.73712(13) 0.18210(12) 0.0386(3) 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
C2 0.036(3) 0.037(3) 0.052(3) 0.018(2) 0.016(2) 0.016(2)
Sn1 0.0343(2) 0.02373(18) 0.0436(2) 0.00583(14) 0.01126(14) 0.01250(14)
Sn2 0.0347(2) 0.02493(19) 0.0468(2) 0.00739(14) 0.01378(15) 0.01022(14)
O1 0.0327(18) 0.0256(17) 0.069(2) 0.0081(16) 0.0200(16) 0.0118(14)
C5 0.051(3) 0.032(3) 0.093(5) 0.010(3) 0.031(3) 0.015(2)
C1 0.034(2) 0.030(2) 0.038(3) 0.010(2) 0.008(2) 0.014(2)
O2 0.043(2) 0.0241(18) 0.078(3) 0.0059(17) 0.0154(18) 0.0144(15)
C7 0.050(3) 0.049(3) 0.042(3) 0.013(2) 0.015(2) 0.025(3)
O3 0.0383(19) 0.0338(19) 0.061(2) 0.0028(16) 0.0202(17) 0.0121(15)
C6 0.053(3) 0.056(3) 0.046(3) 0.011(3) 0.008(2) 0.026(3)
C8 0.089(5) 0.050(4) 0.046(3) 0.007(3) 0.007(3) 0.025(3)
C4 0.043(3) 0.027(2) 0.047(3) 0.011(2) 0.014(2) 0.016(2)
O4 0.049(2) 0.0239(17) 0.067(2) 0.0116(16) 0.0271(18) 0.0119(15)
C10 0.061(4) 0.037(3) 0.123(6) 0.014(3) 0.057(4) 0.016(3)
C9 0.057(3) 0.038(3) 0.056(3) 0.006(3) 0.000(3) 0.017(3)
C3 0.031(2) 0.023(2) 0.043(3) 0.0096(19) 0.009(2) 0.0119(19)
S1 0.0338(6) 0.0221(5) 0.0567(8) 0.0091(5) 0.0078(5) 0.0084(5)
_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
C2 C1 1.514(6) 1_655 ?
C2 S1 1.802(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
Sn1 C7 2.106(5) . ?
Sn1 C6 2.122(5) . ?
Sn1 C5 2.125(5) . ?
Sn1 O1 2.198(3) . ?
Sn1 O3 2.433(3) . ?
Sn2 C9 2.115(5) . ?
Sn2 C8 2.116(6) . ?
Sn2 C10 2.126(6) . ?
Sn2 O4 2.194(3) 1_445 ?
Sn2 O2 2.410(3) . ?
O1 C1 1.273(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C1 O2 1.227(6) . ?
C1 C2 1.514(6) 1_455 ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
O3 C3 1.228(6) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C4 C3 1.521(6) . ?
C4 S1 1.796(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O4 C3 1.277(5) . ?
O4 Sn2 2.194(3) 1_665 ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
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 C2 S1 112.4(3) 1_655 . ?
C1 C2 H2A 109.1 1_655 . ?
S1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 1_655 . ?
S1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
C7 Sn1 C6 124.9(2) . . ?
C7 Sn1 C5 117.8(3) . . ?
C6 Sn1 C5 116.9(3) . . ?
C7 Sn1 O1 94.24(18) . . ?
C6 Sn1 O1 94.24(19) . . ?
C5 Sn1 O1 87.85(18) . . ?
C7 Sn1 O3 89.15(18) . . ?
C6 Sn1 O3 88.99(18) . . ?
C5 Sn1 O3 84.97(18) . . ?
O1 Sn1 O3 172.81(12) . . ?
C9 Sn2 C8 119.6(3) . . ?
C9 Sn2 C10 119.3(3) . . ?
C8 Sn2 C10 120.2(3) . . ?
C9 Sn2 O4 92.95(18) . 1_445 ?
C8 Sn2 O4 98.4(2) . 1_445 ?
C10 Sn2 O4 87.64(19) . 1_445 ?
C9 Sn2 O2 90.47(17) . . ?
C8 Sn2 O2 87.0(2) . . ?
C10 Sn2 O2 83.54(18) . . ?
O4 Sn2 O2 171.12(13) 1_445 . ?
C1 O1 Sn1 122.8(3) . . ?
Sn1 C5 H5A 109.5 . . ?
Sn1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Sn1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C1 O1 123.6(4) . . ?
O2 C1 C2 122.3(4) . 1_455 ?
O1 C1 C2 114.1(4) . 1_455 ?
C1 O2 Sn2 148.7(3) . . ?
Sn1 C7 H7A 109.5 . . ?
Sn1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Sn1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 O3 Sn1 143.5(3) . . ?
Sn1 C6 H6A 109.5 . . ?
Sn1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Sn1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Sn2 C8 H8A 109.5 . . ?
Sn2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Sn2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C4 S1 118.3(3) . . ?
C3 C4 H4A 107.7 . . ?
S1 C4 H4A 107.7 . . ?
C3 C4 H4B 107.7 . . ?
S1 C4 H4B 107.7 . . ?
H4A C4 H4B 107.1 . . ?
C3 O4 Sn2 126.6(3) . 1_665 ?
Sn2 C10 H10A 109.5 . . ?
Sn2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Sn2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Sn2 C9 H9A 109.5 . . ?
Sn2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Sn2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C3 O4 125.0(4) . . ?
O3 C3 C4 123.1(4) . . ?
O4 C3 C4 111.8(4) . . ?
C4 S1 C2 102.5(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
C7 Sn1 O1 C1 -61.7(4) . . . . ?
C6 Sn1 O1 C1 63.8(4) . . . . ?
C5 Sn1 O1 C1 -179.4(4) . . . . ?
O3 Sn1 O1 C1 -179.7(9) . . . . ?
Sn1 O1 C1 O2 -0.4(7) . . . . ?
Sn1 O1 C1 C2 -178.6(3) . . . 1_455 ?
O1 C1 O2 Sn2 167.7(4) . . . . ?
C2 C1 O2 Sn2 -14.2(9) 1_455 . . . ?
C9 Sn2 O2 C1 57.3(7) . . . . ?
C8 Sn2 O2 C1 -62.4(7) . . . . ?
C10 Sn2 O2 C1 176.8(7) . . . . ?
O4 Sn2 O2 C1 170.0(8) 1_445 . . . ?
C7 Sn1 O3 C3 107.9(5) . . . . ?
C6 Sn1 O3 C3 -17.1(5) . . . . ?
C5 Sn1 O3 C3 -134.1(6) . . . . ?
O1 Sn1 O3 C3 -133.8(10) . . . . ?
Sn1 O3 C3 O4 138.3(4) . . . . ?
Sn1 O3 C3 C4 -38.7(8) . . . . ?
Sn2 O4 C3 O3 -12.7(7) 1_665 . . . ?
Sn2 O4 C3 C4 164.6(3) 1_665 . . . ?
S1 C4 C3 O3 -20.6(6) . . . . ?
S1 C4 C3 O4 162.0(4) . . . . ?
C3 C4 S1 C2 -71.0(4) . . . . ?
C1 C2 S1 C4 -56.5(4) 1_655 . . . ?
_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full 25.02
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max 0.847
_refine_diff_density_min -1.406
_refine_diff_density_rms 0.151
data_complex2
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C56 H116 O8 S2 Sn4'
_chemical_formula_weight 1456.37
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'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Sn' 'Sn' -0.6537 1.4246
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M pbca
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'