 
data_99src141 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C46 H37 O6 Sb' 
_chemical_formula_weight          807.51 
 
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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Sb'  'Sb'  -0.5866   1.5461 
 '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)/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                    10.082(2) 
_cell_length_b                    20.406(4) 
_cell_length_c                    18.756(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  103.87(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      3746.2(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     51055 
_cell_measurement_theta_min       2.00
_cell_measurement_theta_max       26.37 
 
_exptl_crystal_description        'chunky needle' 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.35
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.432 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1648 
_exptl_absorpt_coefficient_mu     0.787 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD' 
_diffrn_measurement_method        'Φ & ω scans' 
_diffrn_detector_area_resol_mean  9.091 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             51055 
_diffrn_reflns_av_R_equivalents   0.0986 
_diffrn_reflns_av_sigmaI/netI     0.0501 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          2.00 
_diffrn_reflns_theta_max          26.37 
_reflns_number_total              7657 
_reflns_number_gt                 6257 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor & COLLECT (Hooft, 1998)'
_computing_data_reduction         
'DENZO (Otwinowski & Minor & COLLECT (Hooft, 1998)' 
_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 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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_number_reflns          7657 
_refine_ls_number_parameters      478 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0474 
_refine_ls_R_factor_gt            0.0348 
_refine_ls_wR_factor_ref          0.1072 
_refine_ls_wR_factor_gt           0.0959 
_refine_ls_goodness_of_fit_ref    0.796 
_refine_ls_restrained_S_all       0.796 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Sb1 Sb 0.149259(14) 0.355445(8) 0.100394(8) 0.01422(8) Uani 1 d . . . 
O1 O 0.05547(17) 0.26874(8) 0.04608(9) 0.0190(4) Uani 1 d . . . 
O2 O -0.06899(18) 0.33721(9) -0.03593(10) 0.0217(4) Uani 1 d . . . 
O3 O -0.17296(18) 0.24185(10) -0.12846(10) 0.0248(4) Uani 1 d . . . 
H3 H -0.2261 0.2722 -0.1281 0.037 Uiso 1 calc R . . 
O4 O 0.23601(17) 0.43469(8) 0.16708(9) 0.0200(4) Uani 1 d . . . 
O5 O 0.12187(18) 0.50225(9) 0.08049(10) 0.0226(4) Uani 1 d . . . 
O6 O 0.26448(17) 0.60533(8) 0.15212(10) 0.0201(4) Uani 1 d . . . 
H6 H 0.1925 0.6148 0.1230 0.030 Uiso 1 calc R . . 
C1 C 0.2393(3) 0.37390(13) 0.01235(14) 0.0195(5) Uani 1 d . . . 
C2 C 0.1793(3) 0.41332(13) -0.04695(15) 0.0243(6) Uani 1 d . . . 
H2 H 0.1015 0.4376 -0.0465 0.029 Uiso 1 calc R . . 
C3 C 0.2373(3) 0.41592(15) -0.10673(16) 0.0333(7) Uani 1 d . . . 
H3A H 0.1976 0.4417 -0.1471 0.040 Uiso 1 calc R . . 
C4 C 0.3541(4) 0.38030(19) -0.10681(18) 0.0453(9) Uani 1 d . . . 
H4 H 0.3924 0.3822 -0.1472 0.054 Uiso 1 calc R . . 
C5 C 0.4136(4) 0.34211(19) -0.0472(2) 0.0499(10) Uani 1 d . . . 
H5 H 0.4931 0.3189 -0.0470 0.060 Uiso 1 calc R . . 
C6 C 0.3559(3) 0.33824(17) 0.01211(18) 0.0356(7) Uani 1 d . . . 
H6A H 0.3952 0.3117 0.0519 0.043 Uiso 1 calc R . . 
C7 C -0.0379(2) 0.37242(12) 0.12890(14) 0.0178(5) Uani 1 d . . . 
C8 C -0.1440(3) 0.40851(14) 0.08610(15) 0.0240(6) Uani 1 d . . . 
H8 H -0.1318 0.4319 0.0456 0.029 Uiso 1 calc R . . 
C9 C -0.2684(3) 0.40905(14) 0.10488(17) 0.0311(7) Uani 1 d . . . 
H9 H -0.3409 0.4326 0.0762 0.037 Uiso 1 calc R . . 
C10 C -0.2867(3) 0.37513(16) 0.16569(19) 0.0351(7) Uani 1 d . . . 
H10 H -0.3717 0.3751 0.1769 0.042 Uiso 1 calc R . . 
C11 C -0.1792(3) 0.34136(16) 0.20966(17) 0.0330(7) Uani 1 d . . . 
H11 H -0.1907 0.3198 0.2514 0.040 Uiso 1 calc R . . 
C12 C -0.0546(3) 0.33974(14) 0.19151(16) 0.0249(6) Uani 1 d . . . 
H12 H 0.0182 0.3169 0.2209 0.030 Uiso 1 calc R . . 
C13 C 0.2857(2) 0.29361(13) 0.17322(14) 0.0174(5) Uani 1 d . . . 
C14 C 0.2919(3) 0.22717(13) 0.15674(15) 0.0229(6) Uani 1 d . . . 
H14 H 0.2288 0.2092 0.1171 0.028 Uiso 1 calc R . . 
C15 C 0.3921(3) 0.18796(14) 0.19961(16) 0.0267(6) Uani 1 d . . . 
H15 H 0.3959 0.1437 0.1884 0.032 Uiso 1 calc R . . 
C16 C 0.4858(3) 0.21353(14) 0.25833(16) 0.0277(6) Uani 1 d . . . 
H16 H 0.5529 0.1869 0.2868 0.033 Uiso 1 calc R . . 
C17 C 0.4798(3) 0.27913(16) 0.27484(17) 0.0365(7) Uani 1 d . . . 
H17 H 0.5433 0.2966 0.3146 0.044 Uiso 1 calc R . . 
C18 C 0.3804(3) 0.31931(14) 0.23295(16) 0.0281(6) Uani 1 d . . . 
H18 H 0.3771 0.3634 0.2448 0.034 Uiso 1 calc R . . 
C19 C -0.0378(2) 0.28152(13) -0.01323(13) 0.0171(5) Uani 1 d . . . 
C20 C -0.1125(2) 0.22184(13) -0.05449(14) 0.0188(5) Uani 1 d . . . 
C21 C -0.0059(2) 0.16937(13) -0.05835(14) 0.0212(6) Uani 1 d . . . 
C22 C 0.0095(3) 0.11370(14) -0.01488(16) 0.0280(6) Uani 1 d . . . 
H22 H -0.0484 0.1063 0.0162 0.034 Uiso 1 calc R . . 
C23 C 0.1128(3) 0.06870(16) -0.01799(18) 0.0365(7) Uani 1 d . . . 
H23 H 0.1229 0.0312 0.0109 0.044 Uiso 1 calc R . . 
C24 C 0.1987(3) 0.07932(18) -0.06300(19) 0.0427(9) Uani 1 d . . . 
H24 H 0.2665 0.0490 -0.0651 0.051 Uiso 1 calc R . . 
C25 C 0.1848(3) 0.13519(18) -0.1053(2) 0.0433(9) Uani 1 d . . . 
H25 H 0.2441 0.1430 -0.1355 0.052 Uiso 1 calc R . . 
C26 C 0.0825(3) 0.17971(17) -0.10302(16) 0.0340(7) Uani 1 d . . . 
H26 H 0.0732 0.2172 -0.1320 0.041 Uiso 1 calc R . . 
C27 C -0.2250(2) 0.19941(13) -0.01833(14) 0.0204(5) Uani 1 d . . . 
C28 C -0.3159(3) 0.15178(13) -0.05457(17) 0.0263(6) Uani 1 d . . . 
H28 H -0.3010 0.1319 -0.0966 0.032 Uiso 1 calc R . . 
C29 C -0.4281(3) 0.13382(14) -0.02853(18) 0.0326(7) Uani 1 d . . . 
H29 H -0.4882 0.1021 -0.0531 0.039 Uiso 1 calc R . . 
C30 C -0.4506(3) 0.16309(16) 0.03399(18) 0.0331(7) Uani 1 d . . . 
H30 H -0.5274 0.1519 0.0507 0.040 Uiso 1 calc R . . 
C31 C -0.3601(3) 0.20842(16) 0.07130(17) 0.0332(7) Uani 1 d . . . 
H31 H -0.3735 0.2268 0.1144 0.040 Uiso 1 calc R . . 
C32 C -0.2488(3) 0.22684(14) 0.04497(15) 0.0274(6) Uani 1 d . . . 
H32 H -0.1887 0.2583 0.0703 0.033 Uiso 1 calc R . . 
C33 C 0.1954(2) 0.49286(12) 0.14135(14) 0.0166(5) Uani 1 d . . . 
C34 C 0.2433(2) 0.55042(12) 0.19508(13) 0.0170(5) Uani 1 d . . . 
C35 C 0.3795(2) 0.53500(12) 0.24784(14) 0.0169(5) Uani 1 d . . . 
C36 C 0.4894(3) 0.51687(14) 0.21866(15) 0.0239(6) Uani 1 d . . . 
H36 H 0.4783 0.5155 0.1680 0.029 Uiso 1 calc R . . 
C37 C 0.6142(3) 0.50092(14) 0.26437(16) 0.0280(6) Uani 1 d . . . 
H37 H 0.6867 0.4890 0.2444 0.034 Uiso 1 calc R . . 
C38 C 0.6316(3) 0.50263(14) 0.33982(16) 0.0283(6) Uani 1 d . . . 
H38 H 0.7154 0.4913 0.3705 0.034 Uiso 1 calc R . . 
C39 C 0.5248(3) 0.52116(14) 0.36939(16) 0.0267(6) Uani 1 d . . . 
H39 H 0.5367 0.5227 0.4201 0.032 Uiso 1 calc R . . 
C40 C 0.3992(3) 0.53766(13) 0.32346(14) 0.0226(6) Uani 1 d . . . 
H40 H 0.3277 0.5506 0.3437 0.027 Uiso 1 calc R . . 
C41 C 0.1306(2) 0.56349(12) 0.23537(13) 0.0179(5) Uani 1 d . . . 
C42 C 0.0708(2) 0.51232(13) 0.26490(14) 0.0221(6) Uani 1 d . . . 
H42 H 0.0952 0.4694 0.2575 0.027 Uiso 1 calc R . . 
C43 C -0.0248(3) 0.52442(15) 0.30532(15) 0.0261(6) Uani 1 d . . . 
H43 H -0.0633 0.4897 0.3253 0.031 Uiso 1 calc R . . 
C44 C -0.0630(3) 0.58766(16) 0.31599(16) 0.0302(7) Uani 1 d . . . 
H44 H -0.1280 0.5957 0.3427 0.036 Uiso 1 calc R . . 
C45 C -0.0047(4) 0.63894(15) 0.2869(2) 0.0377(8) Uani 1 d . . . 
H45 H -0.0302 0.6818 0.2942 0.045 Uiso 1 calc R . . 
C46 C 0.0920(3) 0.62714(15) 0.24675(18) 0.0308(7) Uani 1 d . . . 
H46 H 0.1311 0.6621 0.2274 0.037 Uiso 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 
Sb1 C1 2.100(3) . ? 
Sb1 O4 2.1024(17) . ? 
Sb1 C13 2.109(2) . ? 
Sb1 C7 2.109(2) . ? 
Sb1 O1 2.1449(17) . ? 
O1 C19 1.299(3) . ? 
O2 C19 1.228(3) . ? 
O3 C20 1.434(3) . ? 
O4 C33 1.310(3) . ? 
O5 C33 1.218(3) . ? 
O6 C34 1.426(3) . ? 
C1 C6 1.384(4) . ? 
C1 C2 1.388(4) . ? 
C2 C3 1.384(4) . ? 
C3 C4 1.384(5) . ? 
C4 C5 1.377(5) . ? 
C5 C6 1.376(5) . ? 
C7 C8 1.386(4) . ? 
C7 C12 1.395(4) . ? 
C8 C9 1.382(4) . ? 
C9 C10 1.384(4) . ? 
C10 C11 1.379(5) . ? 
C11 C12 1.379(4) . ? 
C13 C18 1.389(4) . ? 
C13 C14 1.395(4) . ? 
C14 C15 1.385(4) . ? 
C15 C16 1.371(4) . ? 
C16 C17 1.379(4) . ? 
C17 C18 1.384(4) . ? 
C19 C20 1.540(4) . ? 
C20 C27 1.525(4) . ? 
C20 C21 1.531(4) . ? 
C21 C26 1.378(4) . ? 
C21 C22 1.385(4) . ? 
C22 C23 1.400(4) . ? 
C23 C24 1.364(5) . ? 
C24 C25 1.377(5) . ? 
C25 C26 1.383(5) . ? 
C27 C32 1.385(4) . ? 
C27 C28 1.396(4) . ? 
C28 C29 1.384(4) . ? 
C29 C30 1.382(4) . ? 
C30 C31 1.368(4) . ? 
C31 C32 1.382(4) . ? 
C33 C34 1.548(3) . ? 
C34 C35 1.521(3) . ? 
C34 C41 1.532(3) . ? 
C35 C40 1.385(4) . ? 
C35 C36 1.398(4) . ? 
C36 C37 1.381(4) . ? 
C37 C38 1.384(4) . ? 
C38 C39 1.377(4) . ? 
C39 C40 1.392(4) . ? 
C41 C42 1.386(4) . ? 
C41 C46 1.387(4) . ? 
C42 C43 1.384(4) . ? 
C43 C44 1.375(4) . ? 
C44 C45 1.376(4) . ? 
C45 C46 1.388(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 
C1 Sb1 O4 97.66(9) . . ? 
C1 Sb1 C13 106.19(10) . . ? 
O4 Sb1 C13 87.77(9) . . ? 
C1 Sb1 C7 138.70(10) . . ? 
O4 Sb1 C7 89.58(8) . . ? 
C13 Sb1 C7 114.71(10) . . ? 
C1 Sb1 O1 89.93(9) . . ? 
O4 Sb1 O1 171.98(7) . . ? 
C13 Sb1 O1 87.64(8) . . ? 
C7 Sb1 O1 86.37(8) . . ? 
C19 O1 Sb1 112.77(15) . . ? 
C33 O4 Sb1 115.41(15) . . ? 
C6 C1 C2 120.6(3) . . ? 
C6 C1 Sb1 115.9(2) . . ? 
C2 C1 Sb1 123.15(19) . . ? 
C3 C2 C1 119.0(3) . . ? 
C4 C3 C2 120.3(3) . . ? 
C5 C4 C3 120.1(3) . . ? 
C6 C5 C4 120.2(3) . . ? 
C5 C6 C1 119.8(3) . . ? 
C8 C7 C12 120.6(2) . . ? 
C8 C7 Sb1 123.63(19) . . ? 
C12 C7 Sb1 115.51(19) . . ? 
C9 C8 C7 118.6(3) . . ? 
C8 C9 C10 121.0(3) . . ? 
C11 C10 C9 120.1(3) . . ? 
C10 C11 C12 119.8(3) . . ? 
C11 C12 C7 119.8(3) . . ? 
C18 C13 C14 119.1(2) . . ? 
C18 C13 Sb1 120.80(19) . . ? 
C14 C13 Sb1 119.65(18) . . ? 
C15 C14 C13 119.9(2) . . ? 
C16 C15 C14 120.9(3) . . ? 
C15 C16 C17 119.4(2) . . ? 
C16 C17 C18 120.8(3) . . ? 
C17 C18 C13 119.9(3) . . ? 
O2 C19 O1 123.7(2) . . ? 
O2 C19 C20 120.3(2) . . ? 
O1 C19 C20 116.0(2) . . ? 
O3 C20 C27 109.1(2) . . ? 
O3 C20 C21 107.1(2) . . ? 
C27 C20 C21 114.6(2) . . ? 
O3 C20 C19 107.7(2) . . ? 
C27 C20 C19 109.9(2) . . ? 
C21 C20 C19 108.2(2) . . ? 
C26 C21 C22 119.1(3) . . ? 
C26 C21 C20 119.0(3) . . ? 
C22 C21 C20 121.8(2) . . ? 
C21 C22 C23 119.5(3) . . ? 
C24 C23 C22 120.7(3) . . ? 
C23 C24 C25 119.7(3) . . ? 
C24 C25 C26 120.0(3) . . ? 
C21 C26 C25 121.0(3) . . ? 
C32 C27 C28 118.1(2) . . ? 
C32 C27 C20 124.1(2) . . ? 
C28 C27 C20 117.7(2) . . ? 
C29 C28 C27 120.6(3) . . ? 
C30 C29 C28 120.0(3) . . ? 
C31 C30 C29 120.1(3) . . ? 
C30 C31 C32 120.0(3) . . ? 
C31 C32 C27 121.2(3) . . ? 
O5 C33 O4 123.7(2) . . ? 
O5 C33 C34 121.1(2) . . ? 
O4 C33 C34 115.3(2) . . ? 
O6 C34 C35 107.22(18) . . ? 
O6 C34 C41 111.8(2) . . ? 
C35 C34 C41 112.1(2) . . ? 
O6 C34 C33 107.12(19) . . ? 
C35 C34 C33 111.0(2) . . ? 
C41 C34 C33 107.49(19) . . ? 
C40 C35 C36 118.6(2) . . ? 
C40 C35 C34 122.9(2) . . ? 
C36 C35 C34 118.5(2) . . ? 
C37 C36 C35 120.6(3) . . ? 
C36 C37 C38 120.2(3) . . ? 
C39 C38 C37 119.9(2) . . ? 
C38 C39 C40 120.1(3) . . ? 
C35 C40 C39 120.6(2) . . ? 
C42 C41 C46 118.6(2) . . ? 
C42 C41 C34 120.8(2) . . ? 
C46 C41 C34 120.5(2) . . ? 
C43 C42 C41 120.8(3) . . ? 
C44 C43 C42 120.2(3) . . ? 
C43 C44 C45 119.7(3) . . ? 
C44 C45 C46 120.4(3) . . ? 
C41 C46 C45 120.4(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.970 
_diffrn_reflns_theta_full              26.37 
_diffrn_measured_fraction_theta_full   0.970 
_refine_diff_density_max    0.840 
_refine_diff_density_min   -1.190 
_refine_diff_density_rms    0.092 
