 
data_2005slh0414
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C26 H28 Cd N2 O4 P2 S4'
_chemical_formula_weight          735.08
 
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'
 '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'
 'Cd'  'Cd'  -0.8075   1.2024
 '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                    10.3791(6)
_cell_length_b                    17.5735(8)
_cell_length_c                    8.1030(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  100.512(3)
_cell_angle_gamma                 90.00
_cell_volume                      1453.16(12)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3477
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        'cut block'
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.06
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.680
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              744
_exptl_absorpt_coefficient_mu     1.186
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8708
_exptl_absorpt_correction_T_max   0.9323
_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             31919
_diffrn_reflns_av_R_equivalents   0.0360
_diffrn_reflns_av_sigmaI/netI     0.0226
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -22
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          3.71
_diffrn_reflns_theta_max          27.49
_reflns_number_total              3339
_reflns_number_gt                 2952
_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     ?
_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)+(0.0225P)²+1.2448P] 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        0.0041(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3339
_refine_ls_number_parameters      181
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0291
_refine_ls_R_factor_gt            0.0236
_refine_ls_wR_factor_ref          0.0572
_refine_ls_wR_factor_gt           0.0543
_refine_ls_goodness_of_fit_ref    1.046
_refine_ls_restrained_S_all       1.046
_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 -0.00175(18) 0.64240(12) 0.9704(2) 0.0255(4) Uani 1 1 d . . .
H1A H 0.0112 0.5883 0.9980 0.038 Uiso 1 1 calc R . .
H1B H 0.0053 0.6720 1.0741 0.038 Uiso 1 1 calc R . .
H1C H 0.0653 0.6594 0.9078 0.038 Uiso 1 1 calc R . .
C2 C -0.32606(17) 0.64859(10) 0.6214(2) 0.0159(3) Uani 1 1 d . . .
C3 C -0.35943(17) 0.72187(10) 0.6659(2) 0.0188(4) Uani 1 1 d . . .
H3 H -0.2989 0.7510 0.7428 0.023 Uiso 1 1 calc R . .
C4 C -0.48014(17) 0.75185(10) 0.5982(2) 0.0198(4) Uani 1 1 d . . .
H4 H -0.5025 0.8016 0.6290 0.024 Uiso 1 1 calc R . .
C5 C -0.56941(17) 0.70998(10) 0.4852(2) 0.0173(4) Uani 1 1 d . . .
C6 C -0.53937(17) 0.63641(10) 0.4425(2) 0.0181(4) Uani 1 1 d . . .
H6 H -0.6010 0.6070 0.3676 0.022 Uiso 1 1 calc R . .
C7 C -0.41718(17) 0.60655(10) 0.5115(2) 0.0181(4) Uani 1 1 d . . .
H7 H -0.3957 0.5563 0.4827 0.022 Uiso 1 1 calc R . .
C8 C -0.77761(17) 0.70741(11) 0.3013(2) 0.0227(4) Uani 1 1 d . . .
H8A H -0.7360 0.6906 0.2083 0.034 Uiso 1 1 calc R . .
H8B H -0.8505 0.7417 0.2585 0.034 Uiso 1 1 calc R . .
H8C H -0.8107 0.6631 0.3538 0.034 Uiso 1 1 calc R . .
C9 C -0.22953(17) 0.55529(11) 0.1802(2) 0.0206(4) Uani 1 1 d . . .
H9 H -0.1721 0.5977 0.1873 0.025 Uiso 1 1 calc R . .
C10 C -0.34702(17) 0.55887(11) 0.0677(2) 0.0202(4) Uani 1 1 d . . .
H10 H -0.3673 0.6022 -0.0022 0.024 Uiso 1 1 calc R . .
C11 C -0.43516(17) 0.49879(10) 0.0575(2) 0.0157(4) Uani 1 1 d . . .
C12 C -0.39584(18) 0.43597(11) 0.1594(2) 0.0217(4) Uani 1 1 d . . .
H12 H -0.4517 0.3930 0.1563 0.026 Uiso 1 1 calc R . .
C13 C -0.27497(18) 0.43661(11) 0.2652(2) 0.0223(4) Uani 1 1 d . . .
H13 H -0.2494 0.3927 0.3316 0.027 Uiso 1 1 calc R . .
N1 N -0.19236(15) 0.49556(8) 0.2792(2) 0.0179(3) Uani 1 1 d . . .
O1 O -0.12995(12) 0.65339(7) 0.86919(16) 0.0199(3) Uani 1 1 d . . .
O2 O -0.68397(12) 0.74646(7) 0.42235(17) 0.0240(3) Uani 1 1 d . . .
P1 P -0.16434(4) 0.61181(3) 0.69173(6) 0.01517(11) Uani 1 1 d . . .
S1 S -0.16540(4) 0.49911(2) 0.71843(6) 0.01703(11) Uani 1 1 d . . .
S2 S -0.04333(4) 0.64747(2) 0.54092(6) 0.01855(11) Uani 1 1 d . . .
Cd1 Cd 0.0000 0.5000 0.5000 0.01638(7) Uani 1 2 d S . .
 
 
_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 1.443(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C7 1.388(2) . ?
C2 C3 1.398(2) . ?
C2 P1 1.7919(18) . ?
C3 C4 1.377(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(3) . ?
C4 H4 0.9500 . ?
C5 O2 1.365(2) . ?
C5 C6 1.389(3) . ?
C6 C7 1.392(2) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 O2 1.425(2) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N1 1.335(2) . ?
C9 C10 1.384(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(2) . ?
C11 C11 1.491(3) 3_465 ?
C12 C13 1.384(2) . ?
C12 H12 0.9500 . ?
C13 N1 1.336(2) . ?
C13 H13 0.9500 . ?
N1 Cd1 2.4267(15) . ?
O1 P1 1.5943(13) . ?
P1 S1 1.9926(6) . ?
P1 S2 2.0059(7) . ?
S1 Cd1 2.6812(5) . ?
S2 Cd1 2.6613(5) . ?
Cd1 N1 2.4267(15) 3_566 ?
Cd1 S2 2.6613(5) 3_566 ?
Cd1 S1 2.6812(5) 3_566 ?
 
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 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C7 C2 C3 118.95(16) . . ?
C7 C2 P1 120.07(13) . . ?
C3 C2 P1 120.81(13) . . ?
C4 C3 C2 119.99(17) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.60(17) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
O2 C5 C6 124.36(16) . . ?
O2 C5 C4 115.35(16) . . ?
C6 C5 C4 120.29(16) . . ?
C5 C6 C7 118.72(16) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
C2 C7 C6 121.41(17) . . ?
C2 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 123.71(17) . . ?
N1 C9 H9 118.1 . . ?
C10 C9 H9 118.1 . . ?
C9 C10 C11 119.74(17) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 116.60(16) . . ?
C10 C11 C11 121.7(2) . 3_465 ?
C12 C11 C11 121.7(2) . 3_465 ?
C13 C12 C11 119.66(17) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
N1 C13 C12 123.62(17) . . ?
N1 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
C9 N1 C13 116.61(16) . . ?
C9 N1 Cd1 121.78(12) . . ?
C13 N1 Cd1 121.09(12) . . ?
C1 O1 P1 118.86(12) . . ?
C5 O2 C8 117.97(14) . . ?
O1 P1 C2 99.44(8) . . ?
O1 P1 S1 111.25(5) . . ?
C2 P1 S1 111.69(6) . . ?
O1 P1 S2 110.14(5) . . ?
C2 P1 S2 110.37(6) . . ?
S1 P1 S2 113.15(3) . . ?
P1 S1 Cd1 84.59(2) . . ?
P1 S2 Cd1 84.87(2) . . ?
N1 Cd1 N1 180.0 . 3_566 ?
N1 Cd1 S2 90.68(4) . 3_566 ?
N1 Cd1 S2 89.32(4) 3_566 3_566 ?
N1 Cd1 S2 89.32(4) . . ?
N1 Cd1 S2 90.68(4) 3_566 . ?
S2 Cd1 S2 180.00(2) 3_566 . ?
N1 Cd1 S1 86.94(4) . . ?
N1 Cd1 S1 93.06(4) 3_566 . ?
S2 Cd1 S1 102.689(13) 3_566 . ?
S2 Cd1 S1 77.311(13) . . ?
N1 Cd1 S1 93.06(4) . 3_566 ?
N1 Cd1 S1 86.94(4) 3_566 3_566 ?
S2 Cd1 S1 77.311(13) 3_566 3_566 ?
S2 Cd1 S1 102.689(13) . 3_566 ?
S1 Cd1 S1 180.0 . 3_566 ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.538
_refine_diff_density_min   -0.450
_refine_diff_density_rms    0.068
