 
data_2005slh0412
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C36 H48 Hg2 O8 P4 S8'
_chemical_formula_weight          1390.28
 
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'
 'P'  'P'   0.1023   0.0942
 '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'
 'Hg'  'Hg'  -2.3894   9.2266
 '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                    15.2643(4)
_cell_length_b                    14.7356(3)
_cell_length_c                    10.5323(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.9880(10)
_cell_angle_gamma                 90.00
_cell_volume                      2360.04(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     5232
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.35
_exptl_crystal_size_min           0.2
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.956
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1352
_exptl_absorpt_coefficient_mu     7.034
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details  
'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(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 95mm CCD camera on κ-goniostat' 
_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             21610
_diffrn_reflns_av_R_equivalents   0.0320
_diffrn_reflns_av_sigmaI/netI     0.0300
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        19
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.07
_diffrn_reflns_theta_max          27.49
_reflns_number_total              5390
_reflns_number_gt                 4941
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_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
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0182P)²+2.4232P] 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      SHELXL
_refine_ls_extinction_coef        0.00164(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          5390
_refine_ls_number_parameters      267
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0253
_refine_ls_R_factor_gt            0.0211
_refine_ls_wR_factor_ref          0.0472
_refine_ls_wR_factor_gt           0.0458
_refine_ls_goodness_of_fit_ref    1.042
_refine_ls_restrained_S_all       1.042
_refine_ls_shift/su_max           0.004
_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 0.68860(18) 0.34618(18) 0.4769(3) 0.0160(5) Uani 1 1 d . . .
H1A H 0.6461 0.3442 0.5427 0.019 Uiso 1 1 calc R . .
H1B H 0.6592 0.3229 0.3960 0.019 Uiso 1 1 calc R . .
C2 C 0.7197(2) 0.44209(18) 0.4596(3) 0.0216(6) Uani 1 1 d . . .
H2A H 0.7453 0.4658 0.5415 0.032 Uiso 1 1 calc R . .
H2B H 0.6699 0.4801 0.4279 0.032 Uiso 1 1 calc R . .
H2C H 0.7643 0.4427 0.3980 0.032 Uiso 1 1 calc R . .
C3 C 0.86612(17) 0.16156(17) 0.5970(2) 0.0119(5) Uani 1 1 d . . .
C4 C 0.93458(18) 0.12673(18) 0.5326(3) 0.0151(5) Uani 1 1 d . . .
H4 H 0.9235 0.1073 0.4467 0.018 Uiso 1 1 calc R . .
C5 C 1.01924(18) 0.12003(19) 0.5931(3) 0.0174(6) Uani 1 1 d . . .
H5 H 1.0657 0.0960 0.5489 0.021 Uiso 1 1 calc R . .
C6 C 1.03496(17) 0.14882(17) 0.7181(3) 0.0143(5) Uani 1 1 d . . .
C7 C 0.96617(18) 0.18209(19) 0.7840(3) 0.0182(6) Uani 1 1 d . . .
H7 H 0.9770 0.2004 0.8704 0.022 Uiso 1 1 calc R . .
C8 C 0.88275(17) 0.18828(18) 0.7236(2) 0.0158(5) Uani 1 1 d . . .
H8 H 0.8361 0.2110 0.7686 0.019 Uiso 1 1 calc R . .
C9 C 1.18764(18) 0.1109(2) 0.7256(3) 0.0236(6) Uani 1 1 d . . .
H9A H 1.1770 0.0465 0.7064 0.035 Uiso 1 1 calc R . .
H9B H 1.2415 0.1171 0.7828 0.035 Uiso 1 1 calc R . .
H9C H 1.1943 0.1440 0.6464 0.035 Uiso 1 1 calc R . .
C10 C 0.46938(19) 0.29316(19) 0.3964(3) 0.0262(7) Uani 1 1 d . . .
H10A H 0.5097 0.2832 0.3290 0.031 Uiso 1 1 calc R . .
H10B H 0.4971 0.2681 0.4774 0.031 Uiso 1 1 calc R . .
C11 C 0.4518(2) 0.39184(19) 0.4105(3) 0.0228(6) Uani 1 1 d . . .
H11A H 0.4214 0.4151 0.3314 0.034 Uiso 1 1 calc R . .
H11B H 0.5076 0.4242 0.4285 0.034 Uiso 1 1 calc R . .
H11C H 0.4148 0.4011 0.4810 0.034 Uiso 1 1 calc R . .
C12 C 0.27007(17) 0.12772(17) 0.2874(2) 0.0121(5) Uani 1 1 d . . .
C13 C 0.25633(18) 0.16804(18) 0.1674(2) 0.0148(5) Uani 1 1 d . . .
H13 H 0.3030 0.1999 0.1332 0.018 Uiso 1 1 calc R . .
C14 C 0.17585(18) 0.16213(18) 0.0981(2) 0.0160(5) Uani 1 1 d . . .
H14 H 0.1670 0.1892 0.0161 0.019 Uiso 1 1 calc R . .
C15 C 0.10699(17) 0.11571(18) 0.1498(2) 0.0142(5) Uani 1 1 d . . .
C16 C 0.12062(18) 0.07279(17) 0.2670(3) 0.0143(5) Uani 1 1 d . . .
H16 H 0.0745 0.0393 0.3000 0.017 Uiso 1 1 calc R . .
C17 C 0.20222(18) 0.07921(18) 0.3357(3) 0.0142(5) Uani 1 1 d . . .
H17 H 0.2118 0.0502 0.4162 0.017 Uiso 1 1 calc R . .
C18 C -0.04531(19) 0.0752(2) 0.1240(3) 0.0244(7) Uani 1 1 d . . .
H18A H -0.0349 0.0098 0.1338 0.037 Uiso 1 1 calc R . .
H18B H -0.0972 0.0854 0.0641 0.037 Uiso 1 1 calc R . .
H18C H -0.0552 0.1017 0.2068 0.037 Uiso 1 1 calc R . .
O1 O 0.76518(11) 0.29123(11) 0.51614(17) 0.0131(4) Uani 1 1 d . . .
O2 O 1.11465(12) 0.14740(14) 0.78611(18) 0.0199(4) Uani 1 1 d . . .
O3 O 0.38588(12) 0.24871(12) 0.36235(18) 0.0159(4) Uani 1 1 d . . .
O4 O 0.02955(12) 0.11695(14) 0.07604(18) 0.0200(4) Uani 1 1 d . . .
P1 P 0.75961(4) 0.18322(4) 0.51719(6) 0.01068(13) Uani 1 1 d . . .
P2 P 0.37510(4) 0.14187(4) 0.37469(6) 0.01088(13) Uani 1 1 d . . .
S1 S 0.74214(4) 0.12994(5) 0.34365(6) 0.01462(14) Uani 1 1 d . . .
S2 S 0.66195(4) 0.14424(5) 0.62586(6) 0.01508(14) Uani 1 1 d . . .
S3 S 0.46505(4) 0.07634(5) 0.27690(6) 0.01542(14) Uani 1 1 d . . .
S4 S 0.62116(4) -0.10986(4) 0.44098(6) 0.01445(14) Uani 1 1 d . . .
Hg1 Hg 0.590100(6) 0.064829(7) 0.438723(9) 0.01528(5) Uani 1 1 d . . .
 
 
_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 O1 1.452(3) . ?
C1 C2 1.507(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.392(4) . ?
C3 C8 1.392(4) . ?
C3 P1 1.793(3) . ?
C4 C5 1.393(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(4) . ?
C5 H5 0.9500 . ?
C6 O2 1.357(3) . ?
C6 C7 1.397(4) . ?
C7 C8 1.376(4) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 O2 1.435(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 O3 1.450(3) . ?
C10 C11 1.489(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C17 1.390(4) . ?
C12 C13 1.396(4) . ?
C12 P2 1.790(3) . ?
C13 C14 1.376(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.403(4) . ?
C14 H14 0.9500 . ?
C15 O4 1.357(3) . ?
C15 C16 1.387(4) . ?
C16 C17 1.388(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 O4 1.428(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O1 P1 1.5939(18) . ?
O3 P2 1.5895(18) . ?
P1 S1 1.9858(9) . ?
P1 S2 2.0392(9) . ?
P2 S4 1.9938(9) 3_656 ?
P2 S3 2.0309(9) . ?
S1 Hg1 2.7773(6) . ?
S2 Hg1 2.4659(7) . ?
S3 Hg1 2.4518(7) . ?
S4 P2 1.9938(9) 3_656 ?
S4 Hg1 2.6172(7) . ?
 
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
O1 C1 C2 107.6(2) . . ?
O1 C1 H1A 110.2 . . ?
C2 C1 H1A 110.2 . . ?
O1 C1 H1B 110.2 . . ?
C2 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.2(2) . . ?
C4 C3 P1 121.7(2) . . ?
C8 C3 P1 118.75(19) . . ?
C3 C4 C5 120.6(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 119.3(2) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
O2 C6 C5 124.8(2) . . ?
O2 C6 C7 114.9(2) . . ?
C5 C6 C7 120.3(2) . . ?
C8 C7 C6 119.9(2) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C3 120.6(2) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
O2 C9 H9A 109.5 . . ?
O2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 107.7(2) . . ?
O3 C10 H10A 110.2 . . ?
C11 C10 H10A 110.2 . . ?
O3 C10 H10B 110.2 . . ?
C11 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
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 . . ?
C17 C12 C13 119.5(2) . . ?
C17 C12 P2 122.3(2) . . ?
C13 C12 P2 118.23(19) . . ?
C14 C13 C12 120.7(2) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 119.3(2) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
O4 C15 C16 124.9(2) . . ?
O4 C15 C14 114.6(2) . . ?
C16 C15 C14 120.5(2) . . ?
C15 C16 C17 119.4(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C12 120.5(2) . . ?
C16 C17 H17 119.7 . . ?
C12 C17 H17 119.7 . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C1 O1 P1 121.11(16) . . ?
C6 O2 C9 117.8(2) . . ?
C10 O3 P2 121.48(17) . . ?
C15 O4 C18 118.4(2) . . ?
O1 P1 C3 97.71(11) . . ?
O1 P1 S1 113.04(7) . . ?
C3 P1 S1 113.88(9) . . ?
O1 P1 S2 109.10(7) . . ?
C3 P1 S2 111.36(9) . . ?
S1 P1 S2 111.04(4) . . ?
O3 P2 C12 99.66(11) . . ?
O3 P2 S4 108.63(8) . 3_656 ?
C12 P2 S4 114.91(9) . 3_656 ?
O3 P2 S3 110.49(8) . . ?
C12 P2 S3 107.40(9) . . ?
S4 P2 S3 114.71(4) 3_656 . ?
P1 S1 Hg1 81.62(3) . . ?
P1 S2 Hg1 88.92(3) . . ?
P2 S3 Hg1 101.54(3) . . ?
P2 S4 Hg1 103.38(3) 3_656 . ?
S3 Hg1 S2 142.00(2) . . ?
S3 Hg1 S4 101.76(2) . . ?
S2 Hg1 S4 113.07(2) . . ?
S3 Hg1 S1 110.48(2) . . ?
S2 Hg1 S1 78.27(2) . . ?
S4 Hg1 S1 100.76(2) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.918
_refine_diff_density_min   -1.320
_refine_diff_density_rms    0.105
