 
data_2005slh1128
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C28 H32 Cd N2 O4 P2 S4'
_chemical_formula_weight          763.14
 
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'
 'Cd'  'Cd'  -0.8075   1.2024
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 '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'
 
_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                    8.1800(2)
_cell_length_b                    9.8839(2)
_cell_length_c                    10.4172(2)
_cell_angle_alpha                 90.7370(10)
_cell_angle_beta                  101.8980(10)
_cell_angle_gamma                 100.7850(10)
_cell_volume                      808.42(3)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     7252
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.568
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              388
_exptl_absorpt_coefficient_mu     1.069
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7399
_exptl_absorpt_correction_T_max   0.8147
_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             16301
_diffrn_reflns_av_R_equivalents   0.0422
_diffrn_reflns_av_sigmaI/netI     0.0317
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.60
_diffrn_reflns_theta_max          27.50
_reflns_number_total              3694
_reflns_number_gt                 3527
_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)+(0.0326P)²+1.1715P] 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        0.0104(17)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3694
_refine_ls_number_parameters      172
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0313
_refine_ls_R_factor_gt            0.0298
_refine_ls_wR_factor_ref          0.0759
_refine_ls_wR_factor_gt           0.0748
_refine_ls_goodness_of_fit_ref    1.042
_refine_ls_restrained_S_all       1.042
_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 1.0199(3) 0.7728(2) 0.5449(2) 0.0225(5) Uani 1 1 d . . .
H1A H 1.0244 0.6746 0.5594 0.027 Uiso 1 1 calc R . .
H1B H 0.9551 0.8047 0.6059 0.027 Uiso 1 1 calc R . .
C2 C 1.19682(15) 0.85754(19) 0.56996(12) 0.0236(5) Uani 1 1 d . . .
H2A H 1.2600 0.8253 0.5092 0.035 Uiso 1 1 calc R . .
H2B H 1.2549 0.8481 0.6606 0.035 Uiso 1 1 calc R . .
H2C H 1.1911 0.9546 0.5564 0.035 Uiso 1 1 calc R . .
C3 C 0.69814(12) 0.77633(11) 0.19725(9) 0.0219(5) Uani 1 1 d R . .
C4 C 0.79914(12) 0.89282(11) 0.16123(9) 0.0292(6) Uani 1 1 d R . .
H4 H 0.8975 0.9393 0.2219 0.035 Uiso 1 1 calc R . .
C5 C 0.75616(12) 0.94130(11) 0.03650(9) 0.0350(6) Uani 1 1 d R . .
H5 H 0.8252 1.0209 0.0119 0.042 Uiso 1 1 calc R . .
C6 C 0.61218(12) 0.87328(11) -0.05221(9) 0.0322(6) Uani 1 1 d R . .
C7 C 0.51117(12) 0.75678(11) -0.01620(9) 0.0599(12) Uani 1 1 d R . .
H7 H 0.4128 0.7103 -0.0768 0.072 Uiso 1 1 calc R . .
C8 C 0.55415(13) 0.70830(11) 0.10853(9) 0.0535(10) Uani 1 1 d R . .
H8 H 0.4851 0.6287 0.1331 0.064 Uiso 1 1 calc R . .
C9 C 0.66165(12) 1.02282(11) -0.22435(9) 0.0555(10) Uani 1 1 d R . .
H9A H 0.6660 1.1065 -0.1713 0.083 Uiso 1 1 d R . .
H9B H 0.6111 1.0348 -0.3163 0.083 Uiso 1 1 d R . .
H9C H 0.7773 1.0058 -0.2177 0.083 Uiso 1 1 d R . .
C10 C 0.1838(3) 0.5813(3) 0.2853(2) 0.0289(6) Uani 1 1 d . . .
H10 H 0.1912 0.6469 0.3548 0.035 Uiso 1 1 calc R . .
C11 C 0.0725(3) 0.5895(3) 0.1674(2) 0.0299(6) Uani 1 1 d . . .
H11 H 0.0058 0.6592 0.1576 0.036 Uiso 1 1 calc R . .
C12 C 0.0583(3) 0.4968(2) 0.06422(19) 0.0151(4) Uani 1 1 d . . .
C13 C 0.1566(5) 0.3976(3) 0.0880(3) 0.0558(11) Uani 1 1 d . . .
H13 H 0.1513 0.3299 0.0208 0.067 Uiso 1 1 calc R . .
C14 C 0.2634(5) 0.3961(3) 0.2095(3) 0.0497(10) Uani 1 1 d . . .
H14 H 0.3282 0.3253 0.2236 0.060 Uiso 1 1 calc R . .
Cd1 Cd 0.5000 0.5000 0.5000 0.01600(9) Uani 1 2 d S . .
N1 N 0.2801(2) 0.48773(18) 0.30666(17) 0.0164(4) Uani 1 1 d . . .
O1 O 0.93680(19) 0.78788(16) 0.40960(15) 0.0178(3) Uani 1 1 d . . .
O2 O 0.5610(3) 0.9092(3) -0.17778(18) 0.0423(5) Uani 1 1 d . . .
P1 P 0.74344(7) 0.70985(6) 0.35933(5) 0.01456(13) Uani 1 1 d . . .
S1 S 0.59519(6) 0.76815(5) 0.47183(5) 0.01375(12) Uani 1 1 d . . .
S2 S 0.72568(7) 0.50568(6) 0.34536(6) 0.02099(13) 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 1.456(3) . ?
C1 C2 1.500(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C3 P1 1.8115(10) . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 O2 1.3616(19) . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 O2 1.417(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 N1 1.315(3) . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(3) . ?
C12 C12 1.484(4) 2_565 ?
C13 C14 1.384(3) . ?
C13 H13 0.9500 . ?
C14 N1 1.318(3) . ?
C14 H14 0.9500 . ?
Cd1 N1 2.3926(17) . ?
Cd1 N1 2.3926(17) 2_666 ?
Cd1 S1 2.6568(5) . ?
Cd1 S1 2.6568(5) 2_666 ?
Cd1 S2 2.6825(6) 2_666 ?
Cd1 S2 2.6825(6) . ?
O1 P1 1.6007(15) . ?
P1 S2 1.9971(8) . ?
P1 S1 2.0015(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 108.38(16) . . ?
O1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
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 120.0 . . ?
C4 C3 P1 122.4 . . ?
C8 C3 P1 117.6 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
O2 C6 C7 115.02(11) . . ?
O2 C6 C5 124.95(11) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 H8 120.0 . . ?
C3 C8 H8 120.0 . . ?
O2 C9 H9A 109.5 . . ?
O2 C9 H9B 109.4 . . ?
H9A C9 H9B 109.5 . . ?
O2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 123.7(2) . . ?
N1 C10 H10 118.2 . . ?
C11 C10 H10 118.2 . . ?
C12 C11 C10 120.0(2) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 116.0(2) . . ?
C11 C12 C12 121.7(2) . 2_565 ?
C13 C12 C12 122.3(2) . 2_565 ?
C12 C13 C14 120.1(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
N1 C14 C13 123.6(2) . . ?
N1 C14 H14 118.2 . . ?
C13 C14 H14 118.2 . . ?
N1 Cd1 N1 180.0 . 2_666 ?
N1 Cd1 S1 89.45(4) . . ?
N1 Cd1 S1 90.55(4) 2_666 . ?
N1 Cd1 S1 90.55(4) . 2_666 ?
N1 Cd1 S1 89.45(4) 2_666 2_666 ?
S1 Cd1 S1 180.0 . 2_666 ?
N1 Cd1 S2 91.31(5) . 2_666 ?
N1 Cd1 S2 88.69(5) 2_666 2_666 ?
S1 Cd1 S2 102.650(16) . 2_666 ?
S1 Cd1 S2 77.350(16) 2_666 2_666 ?
N1 Cd1 S2 88.69(5) . . ?
N1 Cd1 S2 91.31(5) 2_666 . ?
S1 Cd1 S2 77.350(16) . . ?
S1 Cd1 S2 102.650(16) 2_666 . ?
S2 Cd1 S2 180.0 2_666 . ?
C10 N1 C14 116.6(2) . . ?
C10 N1 Cd1 121.82(15) . . ?
C14 N1 Cd1 121.13(16) . . ?
C1 O1 P1 118.11(13) . . ?
C6 O2 C9 118.60(18) . . ?
O1 P1 C3 99.96(7) . . ?
O1 P1 S2 111.39(6) . . ?
C3 P1 S2 110.26(5) . . ?
O1 P1 S1 110.50(6) . . ?
C3 P1 S1 110.87(4) . . ?
S2 P1 S1 113.11(3) . . ?
P1 S1 Cd1 85.07(2) . . ?
P1 S2 Cd1 84.46(2) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.655
_refine_diff_density_min   -0.692
_refine_diff_density_rms    0.087
