data_00src130
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C44 H45 O4 Sb'
_chemical_formula_weight          759.55
 
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                    9.5400(19)
_cell_length_b                    13.248(3)
_cell_length_c                    28.592(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  98.73(3)
_cell_angle_gamma                 90.00
_cell_volume                      3571.6(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     57917
_cell_measurement_theta_min       2.11
_cell_measurement_theta_max       27.50
 
_exptl_crystal_description        prism
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.1
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.413
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1568
_exptl_absorpt_coefficient_mu     0.816
_exptl_absorpt_correction_type    multi-scans
_exptl_absorpt_correction_T_min   0.8874
_exptl_absorpt_correction_T_max   0.9229
_exptl_absorpt_process_details    'SORTAV (Bleeing, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'Phi and Omega scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             57917
_diffrn_reflns_av_R_equivalents   0.0723
_diffrn_reflns_av_sigmaI/netI     0.0470
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -34
_diffrn_reflns_limit_l_max        36
_diffrn_reflns_theta_min          2.11
_diffrn_reflns_theta_max          27.50
_reflns_number_total              7391
_reflns_number_gt                 6026
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'COLLECT (Hooft, 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'CAMERON (Watkin, Pearce 1995)'
_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)+(0.1000P)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          7391
_refine_ls_number_parameters      443
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0778
_refine_ls_R_factor_gt            0.0577
_refine_ls_wR_factor_ref          0.1945
_refine_ls_wR_factor_gt           0.1866
_refine_ls_goodness_of_fit_ref    1.430
_refine_ls_restrained_S_all       1.430
_refine_ls_shift/su_max           0.010
_refine_ls_shift/su_mean          0.001
 
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
Sb1 Sb 0.15449(3) 0.13382(2) 0.122833(10) 0.02940(17) Uani 1 1 d . . .
O1 O 0.1704(4) 0.2560(2) 0.07512(11) 0.0341(8) Uani 1 1 d . . .
O2 O 0.4055(4) 0.2377(3) 0.05606(14) 0.0507(11) Uani 1 1 d . . .
O3 O 0.1221(4) 0.0112(2) 0.16932(11) 0.0348(8) Uani 1 1 d . . .
O4 O 0.3509(4) 0.0064(3) 0.17399(13) 0.0442(10) Uani 1 1 d . . .
C1 C 0.2379(5) 0.0372(4) 0.06693(16) 0.0310(11) Uani 1 1 d . . .
C2 C 0.3525(5) -0.0273(4) 0.06781(17) 0.0356(12) Uani 1 1 d . . .
H2 H 0.4108 -0.0322 0.0969 0.043 Uiso 1 1 calc R . .
C3 C 0.3963(6) -0.0896(4) 0.02964(18) 0.0381(12) Uani 1 1 d . . .
H3 H 0.4766 -0.1301 0.0358 0.046 Uiso 1 1 calc R . .
C4 C 0.3286(6) -0.0880(4) -0.00938(19) 0.0416(13) Uani 1 1 d . . .
H4 H 0.3496 -0.1252 -0.0350 0.050 Uiso 1 1 calc R . .
C5 C 0.2153(6) -0.0229(4) -0.01055(18) 0.0453(14) Uani 1 1 d . . .
H5 H 0.1583 -0.0177 -0.0399 0.054 Uiso 1 1 calc R . .
C6 C 0.1691(6) 0.0402(4) 0.02719(18) 0.0416(14) Uani 1 1 d . . .
H6 H 0.0894 0.0813 0.0208 0.050 Uiso 1 1 calc R . .
C7 C -0.0675(6) 0.1475(4) 0.12795(17) 0.0343(12) Uani 1 1 d . . .
C8 C -0.1559(5) 0.0652(4) 0.14423(19) 0.0408(13) Uani 1 1 d . . .
H8 H -0.1116 0.0042 0.1534 0.049 Uiso 1 1 calc R . .
C9 C -0.2993(6) 0.0736(4) 0.1466(2) 0.0465(15) Uani 1 1 d . . .
H9 H -0.3508 0.0201 0.1564 0.056 Uiso 1 1 calc R . .
C10 C -0.3598(6) 0.1621(5) 0.1341(2) 0.0496(15) Uani 1 1 d . . .
H10 H -0.4558 0.1718 0.1352 0.060 Uiso 1 1 calc R . .
C11 C -0.2769(6) 0.2419(5) 0.1190(2) 0.0504(16) Uani 1 1 d . . .
H11 H -0.3232 0.3026 0.1108 0.061 Uiso 1 1 calc R . .
C12 C -0.1267(5) 0.2371(4) 0.11541(18) 0.0396(13) Uani 1 1 d . . .
H12 H -0.0765 0.2911 0.1054 0.047 Uiso 1 1 calc R . .
C13 C 0.2309(5) 0.2225(3) 0.17510(16) 0.0313(12) Uani 1 1 d . . .
C14 C 0.1769(6) 0.2018(4) 0.22195(18) 0.0434(14) Uani 1 1 d . . .
H14 H 0.1133 0.1497 0.2248 0.052 Uiso 1 1 calc R . .
C15 C 0.2236(7) 0.2603(4) 0.2580(2) 0.0502(16) Uani 1 1 d . . .
H15 H 0.2005 0.2511 0.2881 0.060 Uiso 1 1 calc R . .
C16 C 0.3121(7) 0.3382(5) 0.2465(2) 0.0546(18) Uani 1 1 d . . .
H16 H 0.3427 0.3828 0.2710 0.065 Uiso 1 1 calc R . .
C17 C 0.3659(7) 0.3611(4) 0.1999(2) 0.0531(18) Uani 1 1 d . . .
H17 H 0.4279 0.4143 0.1974 0.064 Uiso 1 1 calc R . .
C18 C 0.3214(5) 0.3028(4) 0.16341(18) 0.0362(12) Uani 1 1 d . . .
H18 H 0.3457 0.3124 0.1334 0.043 Uiso 1 1 calc R . .
C19 C 0.2928(6) 0.2735(4) 0.04791(17) 0.0382(14) Uani 1 1 d . . .
C20 C 0.2888(8) 0.3407(5) 0.0059(2) 0.0595(19) Uani 1 1 d . . .
H20 H 0.3870 0.3491 0.0003 0.071 Uiso 1 1 calc R . .
C21 C 0.2178(6) 0.2893(4) -0.03249(17) 0.0397(13) Uani 1 1 d . . .
C22 C 0.0744(6) 0.2667(4) -0.0260(2) 0.0483(15) Uani 1 1 d . . .
H22 H 0.0310 0.2860 -0.0004 0.058 Uiso 1 1 calc R . .
C23 C 0.0197(7) 0.2172(4) -0.0603(2) 0.0586(19) Uani 1 1 d . . .
H23 H -0.0738 0.1962 -0.0615 0.070 Uiso 1 1 calc R . .
C24 C 0.0984(10) 0.1886(5) -0.1012(3) 0.082(3) Uani 1 1 d . . .
H24 H 0.0453 0.1521 -0.1254 0.098 Uiso 1 1 calc R . .
C25 C 0.2447(10) 0.2098(5) -0.1079(2) 0.078(3) Uani 1 1 d . . .
H25 H 0.2876 0.1900 -0.1336 0.093 Uiso 1 1 calc R . .
C26 C 0.3008(6) 0.2590(5) -0.0733(2) 0.0494(15) Uani 1 1 d . . .
H26 H 0.3951 0.2785 -0.0716 0.059 Uiso 1 1 calc R . .
C27 C 0.2381(7) 0.4428(4) 0.0190(2) 0.062(2) Uani 1 1 d . . .
H27 H 0.1415 0.4368 0.0264 0.074 Uiso 1 1 calc R . .
C28 C 0.3197(6) 0.4993(4) 0.05425(19) 0.0449(15) Uani 1 1 d . . .
H28A H 0.4194 0.4925 0.0515 0.054 Uiso 1 1 calc R . .
H28B H 0.3057 0.4746 0.0851 0.054 Uiso 1 1 calc R . .
C29 C 0.2766(6) 0.6095(4) 0.0492(2) 0.0440(14) Uani 1 1 d . . .
H29A H 0.3432 0.6532 0.0687 0.053 Uiso 1 1 calc R . .
H29B H 0.1817 0.6207 0.0565 0.053 Uiso 1 1 calc R . .
C30 C 0.2835(7) 0.6227(4) -0.0045(2) 0.0469(15) Uani 1 1 d . . .
H30A H 0.2187 0.6746 -0.0186 0.056 Uiso 1 1 calc R . .
H30B H 0.3789 0.6387 -0.0101 0.056 Uiso 1 1 calc R . .
C31 C 0.2388(7) 0.5207(4) -0.0225(2) 0.0553(17) Uani 1 1 d . . .
H31A H 0.3029 0.4972 -0.0435 0.066 Uiso 1 1 calc R . .
H31B H 0.1444 0.5247 -0.0407 0.066 Uiso 1 1 calc R . .
C32 C 0.2303(6) -0.0247(4) 0.18580(16) 0.0336(12) Uani 1 1 d . . .
C33 C 0.1926(7) -0.1095(4) 0.22245(19) 0.0469(15) Uani 1 1 d . . .
H33 H 0.0992 -0.1346 0.2081 0.056 Uiso 1 1 calc R . .
C34 C 0.1649(5) -0.0599(4) 0.27047(17) 0.0313(11) Uani 1 1 d . . .
C35 C 0.0288(7) -0.0558(5) 0.2939(2) 0.0557(17) Uani 1 1 d . . .
H35 H -0.0474 -0.0908 0.2774 0.067 Uiso 1 1 calc R . .
C36 C -0.0028(8) -0.0074(6) 0.3371(3) 0.071(2) Uani 1 1 d . . .
H36 H -0.0899 -0.0073 0.3479 0.085 Uiso 1 1 calc R . .
C37 C 0.1133(9) 0.0354(5) 0.3575(2) 0.0611(19) Uani 1 1 d . . .
H37 H 0.1151 0.0690 0.3862 0.073 Uiso 1 1 calc R . .
C38 C 0.2431(8) 0.0299(5) 0.3346(2) 0.065(2) Uani 1 1 d . . .
H38 H 0.3209 0.0625 0.3516 0.078 Uiso 1 1 calc R . .
C39 C 0.2721(6) -0.0153(5) 0.2917(2) 0.0530(16) Uani 1 1 d . . .
H39 H 0.3592 -0.0120 0.2810 0.064 Uiso 1 1 calc R . .
C40 C 0.2908(7) -0.1939(5) 0.2161(2) 0.0571(17) Uani 1 1 d . . .
H40 H 0.3871 -0.1703 0.2279 0.068 Uiso 1 1 calc R . .
C41 C 0.2560(9) -0.2806(5) 0.2505(2) 0.066(2) Uani 1 1 d . . .
H41A H 0.2934 -0.2671 0.2834 0.079 Uiso 1 1 calc R . .
H41B H 0.1555 -0.2958 0.2471 0.079 Uiso 1 1 calc R . .
C42 C 0.3428(10) -0.3640(5) 0.2279(3) 0.075(2) Uani 1 1 d . . .
H42A H 0.4337 -0.3722 0.2479 0.090 Uiso 1 1 calc R . .
H42B H 0.2924 -0.4276 0.2281 0.090 Uiso 1 1 calc R . .
C43 C 0.3701(12) -0.3438(6) 0.1771(3) 0.092(3) Uani 1 1 d . . .
H43A H 0.4706 -0.3377 0.1754 0.110 Uiso 1 1 calc R . .
H43B H 0.3293 -0.3960 0.1554 0.110 Uiso 1 1 calc R . .
C44 C 0.2965(9) -0.2476(5) 0.1676(2) 0.067(2) Uani 1 1 d . . .
H44A H 0.2011 -0.2591 0.1513 0.080 Uiso 1 1 calc R . .
H44B H 0.3465 -0.2056 0.1478 0.080 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
Sb1 C13 1.952(4) . ?
Sb1 O1 2.137(3) . ?
Sb1 O3 2.151(3) . ?
Sb1 C7 2.152(6) . ?
Sb1 C1 2.283(5) . ?
O1 C19 1.516(7) . ?
O2 C19 1.166(6) . ?
O3 C32 1.169(6) . ?
O4 C32 1.313(7) . ?
C1 C6 1.224(6) . ?
C1 C2 1.385(7) . ?
C2 C3 1.479(8) . ?
C3 C4 1.201(7) . ?
C4 C5 1.379(8) . ?
C5 C6 1.484(8) . ?
C7 C12 1.340(7) . ?
C7 C8 1.496(8) . ?
C8 C9 1.384(8) . ?
C9 C10 1.331(9) . ?
C10 C11 1.426(9) . ?
C11 C12 1.454(8) . ?
C13 C18 1.442(7) . ?
C13 C14 1.531(8) . ?
C14 C15 1.312(7) . ?
C15 C16 1.403(9) . ?
C16 C17 1.529(10) . ?
C17 C18 1.314(7) . ?
C19 C20 1.490(8) . ?
C20 C21 1.380(7) . ?
C20 C27 1.502(9) . ?
C21 C22 1.440(9) . ?
C21 C26 1.559(9) . ?
C22 C23 1.229(8) . ?
C23 C24 1.529(12) . ?
C24 C25 1.465(12) . ?
C25 C26 1.237(9) . ?
C27 C28 1.394(7) . ?
C27 C31 1.574(9) . ?
C28 C29 1.517(7) . ?
C29 C30 1.558(9) . ?
C30 C31 1.486(8) . ?
C32 C33 1.614(8) . ?
C33 C40 1.488(9) . ?
C33 C34 1.580(8) . ?
C34 C39 1.255(7) . ?
C34 C35 1.550(9) . ?
C35 C36 1.461(10) . ?
C36 C37 1.301(10) . ?
C37 C38 1.488(11) . ?
C38 C39 1.429(10) . ?
C40 C44 1.567(9) . ?
C40 C41 1.579(9) . ?
C41 C42 1.577(10) . ?
C42 C43 1.538(12) . ?
C43 C44 1.460(10) . ?
 
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
C13 Sb1 O1 88.78(16) . . ?
C13 Sb1 O3 93.06(17) . . ?
O1 Sb1 O3 175.84(12) . . ?
C13 Sb1 C7 98.9(2) . . ?
O1 Sb1 C7 98.36(16) . . ?
O3 Sb1 C7 77.67(17) . . ?
C13 Sb1 C1 138.06(19) . . ?
O1 Sb1 C1 84.94(15) . . ?
O3 Sb1 C1 96.14(15) . . ?
C7 Sb1 C1 123.08(17) . . ?
C19 O1 Sb1 125.3(3) . . ?
C32 O3 Sb1 110.8(4) . . ?
C6 C1 C2 110.4(5) . . ?
C6 C1 Sb1 115.9(4) . . ?
C2 C1 Sb1 133.7(3) . . ?
C1 C2 C3 130.0(4) . . ?
C4 C3 C2 120.2(5) . . ?
C3 C4 C5 110.0(5) . . ?
C4 C5 C6 130.8(5) . . ?
C1 C6 C5 118.7(5) . . ?
C12 C7 C8 119.6(5) . . ?
C12 C7 Sb1 115.8(4) . . ?
C8 C7 Sb1 124.5(3) . . ?
C9 C8 C7 124.4(5) . . ?
C10 C9 C8 116.7(6) . . ?
C9 C10 C11 119.8(6) . . ?
C10 C11 C12 126.0(5) . . ?
C7 C12 C11 113.6(5) . . ?
C18 C13 C14 128.9(4) . . ?
C18 C13 Sb1 115.7(4) . . ?
C14 C13 Sb1 115.2(3) . . ?
C15 C14 C13 117.5(6) . . ?
C14 C15 C16 113.3(6) . . ?
C15 C16 C17 130.1(5) . . ?
C18 C17 C16 117.6(6) . . ?
C17 C18 C13 112.5(6) . . ?
O2 C19 C20 108.3(6) . . ?
O2 C19 O1 126.5(5) . . ?
C20 C19 O1 125.2(5) . . ?
C21 C20 C19 107.2(5) . . ?
C21 C20 C27 120.3(6) . . ?
C19 C20 C27 108.0(6) . . ?
C20 C21 C22 111.2(6) . . ?
C20 C21 C26 118.7(6) . . ?
C22 C21 C26 130.0(5) . . ?
C23 C22 C21 107.7(6) . . ?
C22 C23 C24 123.0(7) . . ?
C25 C24 C23 129.8(5) . . ?
C26 C25 C24 107.5(7) . . ?
C25 C26 C21 121.9(7) . . ?
C28 C27 C20 119.8(5) . . ?
C28 C27 C31 97.4(5) . . ?
C20 C27 C31 111.4(6) . . ?
C27 C28 C29 109.5(4) . . ?
C28 C29 C30 98.6(4) . . ?
C31 C30 C29 100.8(5) . . ?
C30 C31 C27 111.6(5) . . ?
O3 C32 O4 121.6(5) . . ?
O3 C32 C33 105.9(5) . . ?
O4 C32 C33 132.5(5) . . ?
C40 C33 C34 127.5(5) . . ?
C40 C33 C32 103.7(5) . . ?
C34 C33 C32 111.0(4) . . ?
C39 C34 C35 116.6(5) . . ?
C39 C34 C33 112.7(5) . . ?
C35 C34 C33 130.7(5) . . ?
C36 C35 C34 132.4(5) . . ?
C37 C36 C35 107.4(7) . . ?
C36 C37 C38 119.3(6) . . ?
C39 C38 C37 132.9(6) . . ?
C34 C39 C38 111.3(6) . . ?
C33 C40 C44 123.8(5) . . ?
C33 C40 C41 106.0(6) . . ?
C44 C40 C41 105.0(5) . . ?
C42 C41 C40 94.7(6) . . ?
C43 C42 C41 116.1(6) . . ?
C44 C43 C42 100.4(7) . . ?
C43 C44 C40 108.3(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.901
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.901
_refine_diff_density_max    1.434
_refine_diff_density_min   -1.477
_refine_diff_density_rms    0.173
