# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2001

data_global
_journal_coden_Cambridge          440
_publ_requested_journal         'New Journal of Chemistry'
loop_
_publ_author_name
'Marek Necas'
'Jaromir Marek'
'Josef Novosad'
'StJ. Foreman, Mark R.'
'J. Derek Woollins'

_publ_contact_author_name     	'Dr J Novosad'  
_publ_contact_author_address 
;
Dr J Novosad
Department of Inorganic Chemistry
Faculty of Science, Masaryk University
Kotlarska 2
Brno
611 37
CZECH REPUBLIC
;

_publ_contact_author_email       'NOVOSAD@CHEMI.MUNI.CZ'
_publ_section_title
;
New Mixed-Donor Asymmetrical P-N-P Ligands and their Complexes
;

data_1.cif
#data_man11 
_database_code_CSD                153013
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'Ph2P(S)-NH-P(O)(OPh)2'
_chemical_formula_sum 
'C24 H21 N O3 P2 S' 
_chemical_formula_weight          465.42 

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' 

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/n

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x+1/2, y+1/2, -z+1/2' 
'-x, -y, -z' 
'x-1/2, -y-1/2, z-1/2' 

_cell_length_a                    9.7380(10) 
_cell_length_b                    18.582(2) 
_cell_length_c                    12.5640(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.84(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2246.5(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.25 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.376 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              968 
_exptl_absorpt_coefficient_mu     0.313 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.8720 
_exptl_absorpt_correction_T_max   0.9258 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14139 
_diffrn_reflns_av_R_equivalents   0.0726 
_diffrn_reflns_av_sigmaI/netI     0.0545 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          3.68 
_diffrn_reflns_theta_max          25.55 
_reflns_number_total              3566 
_reflns_number_gt                 2452 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0316P)^2^+2.3023P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3566 
_refine_ls_number_parameters      284 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0933 
_refine_ls_R_factor_gt            0.0475 
_refine_ls_wR_factor_ref          0.1173 
_refine_ls_wR_factor_gt           0.0907 
_refine_ls_goodness_of_fit_ref    1.235 
_refine_ls_restrained_S_all       1.235 
_refine_ls_shift/su_max           0.000 
_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 
P1 P 0.17977(10) -0.00165(5) 0.63300(7) 0.0228(2) Uani 1 d . . . 
O1 O 0.2358(3) -0.05037(13) 0.73269(17) 0.0260(6) Uani 1 d . . . 
O2 O 0.3022(3) 0.05446(13) 0.64764(18) 0.0304(6) Uani 1 d . . . 
O3 O 0.1591(2) -0.03862(13) 0.52840(17) 0.0258(6) Uani 1 d . . . 
N N 0.0347(3) 0.03513(17) 0.6558(2) 0.0236(7) Uani 1 d . . . 
H0 H -0.016(4) 0.0356(18) 0.607(3) 0.017(11) Uiso 1 d . . . 
C1 C 0.1545(4) -0.10928(19) 0.7590(3) 0.0268(9) Uani 1 d . . . 
C2 C 0.1387(4) -0.1690(2) 0.6932(3) 0.0318(9) Uani 1 d . . . 
H2 H 0.1746 -0.1697 0.6270 0.038 Uiso 1 calc R . . 
C3 C 0.0688(4) -0.2283(2) 0.7259(3) 0.0371(10) Uani 1 d . . . 
H3 H 0.0570 -0.2701 0.6820 0.044 Uiso 1 calc R . . 
C4 C 0.0167(4) -0.2267(2) 0.8217(3) 0.0405(11) Uani 1 d . . . 
H4 H -0.0298 -0.2677 0.8440 0.049 Uiso 1 calc R . . 
C5 C 0.0315(5) -0.1660(2) 0.8854(3) 0.0433(11) Uani 1 d . . . 
H5 H -0.0071 -0.1649 0.9504 0.052 Uiso 1 calc R . . 
C6 C 0.1026(4) -0.1062(2) 0.8551(3) 0.0363(10) Uani 1 d . . . 
H6 H 0.1151 -0.0646 0.8993 0.044 Uiso 1 calc R . . 
C7 C 0.3366(4) 0.0940(2) 0.5597(2) 0.0253(8) Uani 1 d . . . 
C8 C 0.4727(4) 0.0895(2) 0.5421(3) 0.0301(9) Uani 1 d . . . 
H8 H 0.5376 0.0597 0.5860 0.036 Uiso 1 calc R . . 
C9 C 0.5126(5) 0.1298(2) 0.4586(3) 0.0377(10) Uani 1 d . . . 
H9 H 0.6055 0.1271 0.4443 0.045 Uiso 1 calc R . . 
C10 C 0.4181(5) 0.1734(2) 0.3967(3) 0.0394(11) Uani 1 d . . . 
H10 H 0.4465 0.2016 0.3409 0.047 Uiso 1 calc R . . 
C11 C 0.2828(5) 0.1764(2) 0.4151(3) 0.0410(11) Uani 1 d . . . 
H11 H 0.2178 0.2062 0.3713 0.049 Uiso 1 calc R . . 
C12 C 0.2404(4) 0.1360(2) 0.4979(3) 0.0343(10) Uani 1 d . . . 
H12 H 0.1469 0.1377 0.5110 0.041 Uiso 1 calc R . . 
P2 P 0.00298(10) 0.09354(5) 0.75215(7) 0.0246(2) Uani 1 d . . . 
S S 0.15217(11) 0.10010(6) 0.87258(7) 0.0367(3) Uani 1 d . . . 
C13 C -0.1606(4) 0.0642(2) 0.7865(3) 0.0260(8) Uani 1 d . . . 
C14 C -0.2301(4) 0.1101(2) 0.8484(3) 0.0378(10) Uani 1 d . . . 
H14 H -0.1906 0.1556 0.8699 0.045 Uiso 1 calc R . . 
C15 C -0.3553(5) 0.0906(3) 0.8788(3) 0.0442(11) Uani 1 d . . . 
H15 H -0.4016 0.1229 0.9200 0.053 Uiso 1 calc R . . 
C16 C -0.4130(5) 0.0246(3) 0.8496(3) 0.0445(11) Uani 1 d . . . 
H16 H -0.4991 0.0111 0.8705 0.053 Uiso 1 calc R . . 
C17 C -0.3446(5) -0.0220(2) 0.7895(3) 0.0456(12) Uani 1 d . . . 
H17 H -0.3841 -0.0677 0.7697 0.055 Uiso 1 calc R . . 
C18 C -0.2195(4) -0.0028(2) 0.7578(3) 0.0338(9) Uani 1 d . . . 
H18 H -0.1738 -0.0353 0.7165 0.041 Uiso 1 calc R . . 
C19 C -0.0356(4) 0.17747(19) 0.6813(3) 0.0244(8) Uani 1 d . . . 
C20 C 0.0690(4) 0.2284(2) 0.6819(3) 0.0335(9) Uani 1 d . . . 
H20 H 0.1581 0.2200 0.7226 0.040 Uiso 1 calc R . . 
C21 C 0.0434(5) 0.2915(2) 0.6231(3) 0.0405(10) Uani 1 d . . . 
H21 H 0.1155 0.3260 0.6234 0.049 Uiso 1 calc R . . 
C22 C -0.0853(4) 0.3047(2) 0.5644(3) 0.0344(10) Uani 1 d . . . 
H22 H -0.1023 0.3482 0.5250 0.041 Uiso 1 calc R . . 
C23 C -0.1896(4) 0.2545(2) 0.5631(3) 0.0331(9) Uani 1 d . . . 
H23 H -0.2786 0.2632 0.5224 0.040 Uiso 1 calc R . . 
C24 C -0.1645(4) 0.1912(2) 0.6209(3) 0.0326(9) Uani 1 d . . . 
H24 H -0.2367 0.1567 0.6192 0.039 Uiso 1 calc R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
P1 0.0199(5) 0.0276(5) 0.0204(4) 0.0008(4) 0.0015(4) 0.0018(4) 
O1 0.0241(14) 0.0291(14) 0.0241(12) 0.0053(10) 0.0010(11) 0.0013(12) 
O2 0.0257(15) 0.0381(16) 0.0266(12) 0.0057(11) 0.0013(11) -0.0093(13) 
O3 0.0237(14) 0.0305(14) 0.0229(12) -0.0042(10) 0.0023(10) 0.0068(12) 
N 0.0182(19) 0.0311(18) 0.0194(15) -0.0075(13) -0.0040(14) 0.0039(15) 
C1 0.020(2) 0.030(2) 0.0293(18) 0.0077(16) 0.0016(16) 0.0046(18) 
C2 0.027(2) 0.040(2) 0.0289(19) 0.0006(17) 0.0058(17) -0.0002(19) 
C3 0.037(3) 0.033(2) 0.042(2) 0.0004(18) 0.0082(19) 0.002(2) 
C4 0.040(3) 0.041(3) 0.042(2) 0.011(2) 0.012(2) 0.000(2) 
C5 0.049(3) 0.048(3) 0.037(2) 0.009(2) 0.019(2) 0.002(2) 
C6 0.043(3) 0.040(2) 0.0281(19) 0.0004(17) 0.0113(18) 0.005(2) 
C7 0.026(2) 0.028(2) 0.0216(17) -0.0020(15) 0.0026(16) -0.0033(18) 
C8 0.023(2) 0.031(2) 0.0356(19) -0.0030(17) 0.0038(17) -0.0008(19) 
C9 0.037(3) 0.039(2) 0.040(2) -0.0085(19) 0.017(2) -0.007(2) 
C10 0.052(3) 0.034(2) 0.035(2) 0.0015(18) 0.016(2) -0.006(2) 
C11 0.041(3) 0.042(3) 0.040(2) 0.0072(19) 0.005(2) 0.009(2) 
C12 0.026(2) 0.045(3) 0.033(2) 0.0038(18) 0.0092(18) 0.005(2) 
P2 0.0225(5) 0.0277(5) 0.0231(4) -0.0053(4) 0.0021(4) 0.0014(5) 
S 0.0345(6) 0.0439(6) 0.0285(5) -0.0102(4) -0.0057(4) 0.0026(5) 
C13 0.025(2) 0.031(2) 0.0215(17) -0.0025(15) 0.0026(16) 0.0044(18) 
C14 0.041(3) 0.037(2) 0.038(2) -0.0054(18) 0.016(2) -0.002(2) 
C15 0.039(3) 0.054(3) 0.044(2) 0.001(2) 0.019(2) 0.008(2) 
C16 0.035(3) 0.060(3) 0.041(2) 0.007(2) 0.014(2) -0.008(2) 
C17 0.047(3) 0.046(3) 0.045(2) -0.004(2) 0.010(2) -0.017(2) 
C18 0.037(3) 0.033(2) 0.0328(19) -0.0035(18) 0.0100(18) -0.004(2) 
C19 0.020(2) 0.027(2) 0.0262(18) -0.0074(15) 0.0052(16) -0.0024(17) 
C20 0.023(2) 0.045(3) 0.032(2) -0.0006(18) -0.0003(17) -0.005(2) 
C21 0.040(3) 0.042(3) 0.040(2) 0.0016(19) 0.006(2) -0.012(2) 
C22 0.038(3) 0.033(2) 0.034(2) 0.0022(17) 0.0092(19) -0.002(2) 
C23 0.026(2) 0.033(2) 0.039(2) 0.0049(17) 0.0027(18) 0.0042(19) 
C24 0.027(2) 0.032(2) 0.039(2) -0.0010(18) 0.0034(19) -0.0014(19) 

_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 
P1 O3 1.469(2) . ? 
P1 O2 1.573(3) . ? 
P1 O1 1.573(2) . ? 
P1 N 1.634(3) . ? 
O1 C1 1.419(4) . ? 
O2 C7 1.409(4) . ? 
N P2 1.689(3) . ? 
C1 C2 1.379(5) . ? 
C1 C6 1.379(5) . ? 
C2 C3 1.389(5) . ? 
C3 C4 1.377(5) . ? 
C4 C5 1.377(6) . ? 
C5 C6 1.392(6) . ? 
C7 C12 1.366(5) . ? 
C7 C8 1.380(5) . ? 
C8 C9 1.392(5) . ? 
C9 C10 1.374(6) . ? 
C10 C11 1.373(6) . ? 
C11 C12 1.396(5) . ? 
P2 C13 1.798(4) . ? 
P2 C19 1.806(4) . ? 
P2 S 1.9337(14) . ? 
C13 C18 1.395(5) . ? 
C13 C14 1.397(5) . ? 
C14 C15 1.380(6) . ? 
C15 C16 1.375(6) . ? 
C16 C17 1.385(6) . ? 
C17 C18 1.386(6) . ? 
C19 C24 1.387(5) . ? 
C19 C20 1.390(5) . ? 
C20 C21 1.389(5) . ? 
C21 C22 1.374(6) . ? 
C22 C23 1.377(5) . ? 
C23 C24 1.384(5) . ? 

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 
O3 P1 O2 114.32(14) . . ? 
O3 P1 O1 115.23(14) . . ? 
O2 P1 O1 97.16(13) . . ? 
O3 P1 N 110.41(16) . . ? 
O2 P1 N 111.25(16) . . ? 
O1 P1 N 107.74(15) . . ? 
C1 O1 P1 119.5(2) . . ? 
C7 O2 P1 121.4(2) . . ? 
P1 N P2 130.7(2) . . ? 
C2 C1 C6 122.4(4) . . ? 
C2 C1 O1 119.7(3) . . ? 
C6 C1 O1 117.7(3) . . ? 
C1 C2 C3 118.4(3) . . ? 
C4 C3 C2 120.3(4) . . ? 
C5 C4 C3 120.4(4) . . ? 
C4 C5 C6 120.4(4) . . ? 
C1 C6 C5 118.1(4) . . ? 
C12 C7 C8 122.3(3) . . ? 
C12 C7 O2 121.3(3) . . ? 
C8 C7 O2 116.4(3) . . ? 
C7 C8 C9 118.4(4) . . ? 
C10 C9 C8 120.2(4) . . ? 
C11 C10 C9 120.3(4) . . ? 
C10 C11 C12 120.3(4) . . ? 
C7 C12 C11 118.4(4) . . ? 
N P2 C13 104.11(16) . . ? 
N P2 C19 104.40(15) . . ? 
C13 P2 C19 104.75(16) . . ? 
N P2 S 113.79(13) . . ? 
C13 P2 S 114.73(12) . . ? 
C19 P2 S 113.92(12) . . ? 
C18 C13 C14 118.3(4) . . ? 
C18 C13 P2 123.5(3) . . ? 
C14 C13 P2 118.1(3) . . ? 
C15 C14 C13 121.2(4) . . ? 
C16 C15 C14 120.2(4) . . ? 
C15 C16 C17 119.4(4) . . ? 
C16 C17 C18 120.9(4) . . ? 
C17 C18 C13 120.0(4) . . ? 
C24 C19 C20 118.6(3) . . ? 
C24 C19 P2 122.1(3) . . ? 
C20 C19 P2 119.2(3) . . ? 
C21 C20 C19 120.1(4) . . ? 
C22 C21 C20 120.7(4) . . ? 
C21 C22 C23 119.8(4) . . ? 
C22 C23 C24 119.9(4) . . ? 
C23 C24 C19 121.0(4) . . ? 

loop_ 
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_distance_DH 
_geom_hbond_distance_HA 
_geom_hbond_distance_DA 
_geom_hbond_angle_DHA 
_geom_hbond_site_symmetry_A 
N H0 O3  0.73(3) 2.02(4) 2.752(4) 179(4) 3_556 

_diffrn_measured_fraction_theta_max    0.820 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.858 
_refine_diff_density_max    0.379 
_refine_diff_density_min   -0.419 
_refine_diff_density_rms    0.078 

data_2.cif
#data_man13 
_database_code_CSD                153014
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'Ph2P(Se)-NH-P(O)(OPh)2'
_chemical_formula_sum 
'C24 H21 N O3 P2 Se' 
_chemical_formula_weight          512.32 

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' 
'Se'  'Se'  -0.0929   2.2259 
'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)/n

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x+1/2, y+1/2, -z+1/2' 
'-x, -y, -z' 
'x-1/2, -y-1/2, z-1/2' 

_cell_length_a                    9.745(2) 
_cell_length_b                    18.799(4) 
_cell_length_c                    12.423(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.21(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2252.5(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.70 
_exptl_crystal_size_mid           0.50 
_exptl_crystal_size_min           0.50 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.511 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1040 
_exptl_absorpt_coefficient_mu     1.835 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.3598 
_exptl_absorpt_correction_T_max   0.4605 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             12723 
_diffrn_reflns_av_R_equivalents   0.1021 
_diffrn_reflns_av_sigmaI/netI     0.0716 
_diffrn_reflns_limit_h_min        -6 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -21 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          3.49 
_diffrn_reflns_theta_max          25.55 
_reflns_number_total              3566 
_reflns_number_gt                 2255 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0452P)^2^+13.9817P] 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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0053(9) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          3566 
_refine_ls_number_parameters      285 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1120 
_refine_ls_R_factor_gt            0.0571 
_refine_ls_wR_factor_ref          0.1714 
_refine_ls_wR_factor_gt           0.1239 
_refine_ls_goodness_of_fit_ref    1.111 
_refine_ls_restrained_S_all       1.111 
_refine_ls_shift/su_max           0.011 
_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 
Se Se 0.66172(8) 0.08951(4) 0.89413(6) 0.0426(3) Uani 1 d . . . 
P2 P 0.50371(18) 0.08648(10) 0.76145(15) 0.0290(5) Uani 1 d . . . 
P1 P 0.67835(18) -0.00542(9) 0.63287(15) 0.0285(5) Uani 1 d . . . 
O O 0.6555(5) -0.0384(2) 0.5242(4) 0.0329(12) Uani 1 d . . . 
O1 O 0.8028(5) 0.0497(3) 0.6492(4) 0.0358(12) Uani 1 d . . . 
C2 C 0.9747(7) 0.0880(4) 0.5467(6) 0.0322(17) Uani 1 d . . . 
H2 H 1.0387 0.0578 0.5898 0.039 Uiso 1 calc R . . 
C15 C 0.3183(8) 0.2508(4) 0.5801(6) 0.0371(18) Uani 1 d . . . 
H15 H 0.2291 0.2615 0.5422 0.044 Uiso 1 calc R . . 
N N 0.5343(6) 0.0321(3) 0.6612(5) 0.0256(13) Uani 1 d . . . 
H0 H 0.490(8) 0.025(4) 0.602(6) 0.03(2) Uiso 1 d . . . 
C6 C 0.7439(8) 0.1333(4) 0.5012(6) 0.0383(18) Uani 1 d . . . 
H6 H 0.6497 0.1340 0.5129 0.046 Uiso 1 calc R . . 
C13 C 0.4700(7) 0.1719(4) 0.6930(6) 0.0328(17) Uani 1 d . . . 
C12 C 0.5982(8) -0.1161(4) 0.8493(6) 0.0380(18) Uani 1 d . . . 
H12 H 0.6069 -0.0756 0.8956 0.046 Uiso 1 calc R . . 
C24 C 0.2695(8) 0.1015(4) 0.8592(6) 0.0406(19) Uani 1 d . . . 
H24 H 0.3105 0.1454 0.8842 0.049 Uiso 1 calc R . . 
C7 C 0.6526(7) -0.1160(4) 0.7526(6) 0.0322(17) Uani 1 d . . . 
C21 C 0.1504(8) -0.0268(4) 0.7903(7) 0.046(2) Uani 1 d . . . 
H21 H 0.1102 -0.0713 0.7673 0.055 Uiso 1 calc R . . 
C1 C 0.8384(7) 0.0906(4) 0.5633(6) 0.0282(15) Uani 1 d . . . 
C20 C 0.2773(8) -0.0074(4) 0.7613(6) 0.0389(19) Uani 1 d . . . 
H20 H 0.3233 -0.0389 0.7184 0.047 Uiso 1 calc R . . 
C8 C 0.6356(8) -0.1727(4) 0.6811(6) 0.0376(18) Uani 1 d . . . 
H8 H 0.6702 -0.1705 0.6135 0.045 Uiso 1 calc R . . 
C16 C 0.4248(8) 0.2988(4) 0.5782(6) 0.0401(19) Uani 1 d . . . 
H16 H 0.4099 0.3420 0.5384 0.048 Uiso 1 calc R . . 
C11 C 0.5308(9) -0.1764(4) 0.8771(7) 0.048(2) Uani 1 d . . . 
H11 H 0.4952 -0.1781 0.9444 0.057 Uiso 1 calc R . . 
C14 C 0.3389(7) 0.1872(4) 0.6361(6) 0.0361(18) Uani 1 d . . . 
H14 H 0.2649 0.1543 0.6359 0.043 Uiso 1 calc R . . 
C18 C 0.5779(8) 0.2194(4) 0.6931(6) 0.0404(19) Uani 1 d . . . 
H18 H 0.6670 0.2088 0.7316 0.048 Uiso 1 calc R . . 
C19 C 0.3381(7) 0.0573(4) 0.7940(6) 0.0336(17) Uani 1 d . . . 
C10 C 0.5145(8) -0.2346(4) 0.8078(7) 0.045(2) Uani 1 d . . . 
H10 H 0.4671 -0.2758 0.8275 0.053 Uiso 1 calc R . . 
C4 C 0.9230(9) 0.1741(4) 0.4045(7) 0.047(2) Uani 1 d . . . 
H4 H 0.9529 0.2035 0.3502 0.056 Uiso 1 calc R . . 
C23 C 0.1425(9) 0.0821(5) 0.8882(7) 0.048(2) Uani 1 d . . . 
H23 H 0.0966 0.1126 0.9324 0.057 Uiso 1 calc R . . 
C17 C 0.5549(8) 0.2830(4) 0.6359(7) 0.045(2) Uani 1 d . . . 
H17 H 0.6287 0.3161 0.6362 0.054 Uiso 1 calc R . . 
C5 C 0.7880(9) 0.1755(4) 0.4212(7) 0.048(2) Uani 1 d . . . 
H5 H 0.7237 0.2054 0.3778 0.057 Uiso 1 calc R . . 
C9 C 0.5669(8) -0.2329(4) 0.7104(7) 0.043(2) Uani 1 d . . . 
H9 H 0.5560 -0.2729 0.6632 0.051 Uiso 1 calc R . . 
C22 C 0.0830(8) 0.0177(5) 0.8520(7) 0.051(2) Uani 1 d . . . 
H22 H -0.0050 0.0047 0.8702 0.061 Uiso 1 calc R . . 
C3 C 1.0172(9) 0.1299(4) 0.4666(7) 0.045(2) Uani 1 d . . . 
H3 H 1.1110 0.1285 0.4538 0.054 Uiso 1 calc R . . 
O2 O 0.7335(5) -0.0567(2) 0.7292(4) 0.0306(11) Uani 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Se 0.0348(5) 0.0472(5) 0.0413(5) -0.0103(4) -0.0095(4) 0.0039(4) 
P2 0.0216(9) 0.0289(9) 0.0354(11) -0.0058(8) 0.0006(8) 0.0013(8) 
P1 0.0210(9) 0.0290(9) 0.0340(11) 0.0003(8) -0.0016(8) 0.0014(8) 
O 0.026(3) 0.036(3) 0.036(3) -0.003(2) 0.001(2) 0.007(2) 
O1 0.023(2) 0.046(3) 0.035(3) 0.004(2) -0.005(2) -0.011(2) 
C2 0.024(4) 0.025(3) 0.047(5) -0.002(3) 0.001(3) 0.000(3) 
C15 0.031(4) 0.037(4) 0.045(5) 0.001(3) 0.011(3) 0.007(3) 
N 0.021(3) 0.029(3) 0.025(3) -0.010(3) -0.002(3) 0.002(2) 
C6 0.025(4) 0.049(5) 0.041(5) -0.001(4) 0.003(3) 0.005(4) 
C13 0.025(4) 0.030(4) 0.044(4) -0.007(3) 0.007(3) -0.002(3) 
C12 0.044(5) 0.032(4) 0.040(5) 0.003(3) 0.012(4) 0.008(3) 
C24 0.048(5) 0.040(4) 0.035(4) -0.011(3) 0.010(4) -0.003(4) 
C7 0.026(4) 0.029(4) 0.040(4) 0.005(3) -0.001(3) 0.008(3) 
C21 0.034(4) 0.042(5) 0.061(6) -0.003(4) 0.006(4) -0.014(4) 
C1 0.027(4) 0.030(4) 0.028(4) -0.002(3) 0.004(3) -0.007(3) 
C20 0.042(5) 0.030(4) 0.044(5) -0.008(3) 0.005(4) -0.002(3) 
C8 0.035(4) 0.032(4) 0.044(5) 0.001(3) 0.000(4) 0.004(3) 
C16 0.043(5) 0.033(4) 0.045(5) -0.002(3) 0.008(4) -0.004(4) 
C11 0.059(6) 0.037(5) 0.049(5) 0.008(4) 0.016(4) 0.006(4) 
C14 0.025(4) 0.031(4) 0.052(5) -0.003(3) 0.003(4) -0.002(3) 
C18 0.026(4) 0.039(4) 0.053(5) 0.000(4) -0.002(4) -0.011(3) 
C19 0.027(4) 0.030(4) 0.043(4) 0.001(3) 0.003(3) 0.004(3) 
C10 0.038(4) 0.037(4) 0.062(6) 0.008(4) 0.019(4) 0.003(4) 
C4 0.061(6) 0.039(4) 0.044(5) 0.005(4) 0.019(4) -0.004(4) 
C23 0.043(5) 0.054(5) 0.052(5) -0.004(4) 0.025(4) 0.005(4) 
C17 0.036(4) 0.044(5) 0.056(5) -0.007(4) 0.009(4) -0.016(4) 
C5 0.045(5) 0.044(5) 0.055(5) 0.014(4) 0.009(4) 0.005(4) 
C9 0.037(4) 0.035(4) 0.056(5) -0.005(4) 0.009(4) 0.000(4) 
C22 0.032(4) 0.056(5) 0.066(6) 0.007(5) 0.006(4) -0.004(4) 
C3 0.040(5) 0.044(5) 0.054(5) -0.011(4) 0.018(4) -0.011(4) 
O2 0.024(2) 0.028(2) 0.039(3) 0.007(2) 0.000(2) 0.001(2) 

_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 
Se P2 2.089(2) . ? 
P2 N 1.671(6) . ? 
P2 C19 1.804(8) . ? 
P2 C13 1.825(7) . ? 
P1 O 1.473(5) . ? 
P1 O2 1.571(5) . ? 
P1 O1 1.585(5) . ? 
P1 N 1.654(6) . ? 
O1 C1 1.399(8) . ? 
C2 C1 1.374(9) . ? 
C2 C3 1.379(11) . ? 
C15 C16 1.378(10) . ? 
C15 C14 1.383(10) . ? 
C6 C1 1.372(10) . ? 
C6 C5 1.387(11) . ? 
C13 C18 1.379(10) . ? 
C13 C14 1.398(10) . ? 
C12 C11 1.378(11) . ? 
C12 C7 1.381(10) . ? 
C24 C23 1.386(11) . ? 
C24 C19 1.395(10) . ? 
C7 C8 1.382(10) . ? 
C7 O2 1.419(8) . ? 
C21 C22 1.365(12) . ? 
C21 C20 1.385(11) . ? 
C20 C19 1.389(10) . ? 
C8 C9 1.389(11) . ? 
C16 C17 1.397(11) . ? 
C11 C10 1.388(11) . ? 
C18 C17 1.393(11) . ? 
C10 C9 1.380(11) . ? 
C4 C5 1.361(11) . ? 
C4 C3 1.387(11) . ? 
C23 C22 1.388(12) . ? 

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 
N P2 C19 104.0(3) . . ? 
N P2 C13 103.3(3) . . ? 
C19 P2 C13 105.3(3) . . ? 
N P2 Se 114.5(2) . . ? 
C19 P2 Se 114.4(3) . . ? 
C13 P2 Se 114.0(2) . . ? 
O P1 O2 115.5(3) . . ? 
O P1 O1 113.9(3) . . ? 
O2 P1 O1 97.5(3) . . ? 
O P1 N 110.6(3) . . ? 
O2 P1 N 108.0(3) . . ? 
O1 P1 N 110.6(3) . . ? 
C1 O1 P1 122.0(4) . . ? 
C1 C2 C3 119.0(7) . . ? 
C16 C15 C14 121.3(7) . . ? 
P1 N P2 131.8(4) . . ? 
C1 C6 C5 119.1(7) . . ? 
C18 C13 C14 120.6(7) . . ? 
C18 C13 P2 118.8(5) . . ? 
C14 C13 P2 120.4(5) . . ? 
C11 C12 C7 118.3(7) . . ? 
C23 C24 C19 120.9(7) . . ? 
C12 C7 C8 122.2(7) . . ? 
C12 C7 O2 118.2(6) . . ? 
C8 C7 O2 119.5(7) . . ? 
C22 C21 C20 120.3(7) . . ? 
C6 C1 C2 121.5(7) . . ? 
C6 C1 O1 122.1(6) . . ? 
C2 C1 O1 116.4(6) . . ? 
C21 C20 C19 120.9(7) . . ? 
C7 C8 C9 118.5(8) . . ? 
C15 C16 C17 118.8(7) . . ? 
C12 C11 C10 120.7(8) . . ? 
C15 C14 C13 119.2(7) . . ? 
C13 C18 C17 119.2(7) . . ? 
C20 C19 C24 118.1(7) . . ? 
C20 C19 P2 123.9(6) . . ? 
C24 C19 P2 117.9(6) . . ? 
C9 C10 C11 120.1(8) . . ? 
C5 C4 C3 120.3(8) . . ? 
C24 C23 C22 119.5(8) . . ? 
C18 C17 C16 120.8(7) . . ? 
C4 C5 C6 120.2(8) . . ? 
C10 C9 C8 120.1(8) . . ? 
C21 C22 C23 120.2(8) . . ? 
C2 C3 C4 120.0(7) . . ? 
C7 O2 P1 119.9(4) . . ? 

loop_ 
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_distance_DH 
_geom_hbond_distance_HA 
_geom_hbond_distance_DA 
_geom_hbond_angle_DHA 
_geom_hbond_site_symmetry_A 
N H0 O  0.81(7) 1.97(7) 2.743(7) 159(7) 3_656 

_diffrn_measured_fraction_theta_max    0.820 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.858 
_refine_diff_density_max    0.993 
_refine_diff_density_min   -0.864 
_refine_diff_density_rms    0.127 

data_4.cif
#data_m 
_database_code_CSD                153015
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'iPr2P(Se)-NH-P(O)(OPh)2'
_chemical_formula_sum 
'C18 H25 N O3 P2 Se' 
_chemical_formula_weight          444.29 

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' 
'Se'  'Se'  -0.0929   2.2259 
'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                    18.491(4) 
_cell_length_b                    23.200(5) 
_cell_length_c                    9.642(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.59(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4089.9(15) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.30 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.443 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1824 
_exptl_absorpt_coefficient_mu     2.009 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.5004 
_exptl_absorpt_correction_T_max   0.5840 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             29324 
_diffrn_reflns_av_R_equivalents   0.0464 
_diffrn_reflns_av_sigmaI/netI     0.0398 
_diffrn_reflns_limit_h_min        -24 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        -29 
_diffrn_reflns_limit_k_max        29 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.34 
_diffrn_reflns_theta_max          28.66 
_reflns_number_total              9677 
_reflns_number_gt                 7729 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0535P)^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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0000(2) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          9677 
_refine_ls_number_parameters      652 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0472 
_refine_ls_R_factor_gt            0.0340 
_refine_ls_wR_factor_ref          0.0895 
_refine_ls_wR_factor_gt           0.0857 
_refine_ls_goodness_of_fit_ref    1.054 
_refine_ls_restrained_S_all       1.054 
_refine_ls_shift/su_max           0.333 
_refine_ls_shift/su_mean          0.021 

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 
Se1 Se 0.367428(11) 0.633083(9) 0.33652(2) 0.01890(7) Uani 1 d . . . 
P2 P 0.41773(3) 0.67343(2) 0.18185(5) 0.01360(11) Uani 1 d . . . 
P1 P 0.53768(3) 0.76091(2) 0.19562(5) 0.01299(11) Uani 1 d . . . 
O2 O 0.61788(7) 0.75553(6) 0.27723(14) 0.0156(3) Uani 1 d . . . 
C15 C 0.28541(13) 0.69216(12) 0.0094(3) 0.0256(5) Uani 1 d . . . 
O3 O 0.53231(8) 0.75656(6) 0.04376(14) 0.0180(3) Uani 1 d . . . 
C3 C 0.57955(14) 0.95421(10) 0.1148(3) 0.0336(6) Uani 1 d . . . 
C6 C 0.60242(12) 0.88848(10) 0.3555(2) 0.0214(4) Uani 1 d . . . 
C13 C 0.35667(11) 0.72189(9) 0.0707(2) 0.0176(4) Uani 1 d . . . 
N1 N 0.48698(9) 0.71476(7) 0.26269(18) 0.0139(3) Uani 1 d . . . 
C1 C 0.55481(11) 0.87110(8) 0.2406(2) 0.0171(4) Uani 1 d . . . 
C7 C 0.65903(11) 0.70495(8) 0.2714(2) 0.0172(4) Uani 1 d . . . 
O1 O 0.51499(7) 0.82041(6) 0.25316(15) 0.0171(3) Uani 1 d . . . 
C8 C 0.66319(12) 0.66736(9) 0.3825(2) 0.0225(4) Uani 1 d . . . 
C14 C 0.33876(14) 0.77422(10) 0.1542(3) 0.0251(5) Uani 1 d . . . 
C17 C 0.51378(14) 0.58453(10) 0.1665(3) 0.0255(5) Uani 1 d . . . 
C9 C 0.70597(14) 0.61837(10) 0.3809(3) 0.0305(5) Uani 1 d . . . 
C11 C 0.73846(14) 0.64712(11) 0.1597(3) 0.0339(6) Uani 1 d . . . 
C12 C 0.69577(12) 0.69598(10) 0.1595(3) 0.0244(5) Uani 1 d . . . 
C4 C 0.62747(14) 0.97265(10) 0.2296(3) 0.0333(6) Uani 1 d . . . 
C16 C 0.46396(12) 0.62523(9) 0.0738(2) 0.0193(4) Uani 1 d . . . 
C10 C 0.74325(14) 0.60852(11) 0.2700(3) 0.0340(6) Uani 1 d . . . 
C5 C 0.63836(13) 0.94025(10) 0.3496(3) 0.0290(5) Uani 1 d . . . 
C2 C 0.54203(13) 0.90259(10) 0.1191(3) 0.0258(5) Uani 1 d . . . 
Se2 Se 0.122621(13) 0.695490(10) 0.62284(3) 0.03241(8) Uani 1 d . . . 
P3 P 0.00073(3) 0.57081(2) 0.65868(5) 0.01564(11) Uani 1 d . . . 
P4 P 0.12128(3) 0.61855(2) 0.51155(6) 0.01829(12) Uani 1 d . . . 
O6 O -0.04482(8) 0.51906(6) 0.64073(15) 0.0198(3) Uani 1 d . . . 
O4 O -0.04074(8) 0.62910(6) 0.62461(15) 0.0195(3) Uani 1 d . . . 
O5 O 0.03721(8) 0.58239(6) 0.81392(15) 0.0193(3) Uani 1 d . . . 
C19 C -0.08171(12) 0.65695(9) 0.7162(2) 0.0215(4) Uani 1 d . . . 
C33 C 0.14556(16) 0.66487(12) 0.2617(3) 0.0335(6) Uani 1 d . . . 
C31 C 0.09284(12) 0.62592(9) 0.3233(2) 0.0220(5) Uani 1 d . . . 
C30 C 0.14479(13) 0.56735(11) 0.9726(2) 0.0263(5) Uani 1 d . . . 
N2 N 0.06299(9) 0.56851(7) 0.55696(19) 0.0179(4) Uani 1 d . . . 
C34 C 0.21014(11) 0.58302(9) 0.5329(2) 0.0215(4) Uani 1 d . . . 
C26 C 0.06627(13) 0.48634(9) 0.9062(2) 0.0238(5) Uani 1 d . . . 
C29 C 0.19048(14) 0.53260(12) 1.0619(3) 0.0325(6) Uani 1 d . . . 
C27 C 0.11240(13) 0.45233(10) 0.9972(3) 0.0275(5) Uani 1 d . . . 
C21 C -0.19683(16) 0.68016(13) 0.7803(3) 0.0433(7) Uani 1 d . . . 
C36 C 0.21000(14) 0.52616(11) 0.4563(3) 0.0263(5) Uani 1 d . . . 
C28 C 0.17447(13) 0.47484(11) 1.0745(3) 0.0316(5) Uani 1 d . . . 
C24 C -0.04663(14) 0.69258(10) 0.8188(3) 0.0275(5) Uani 1 d . . . 
C25 C 0.08304(11) 0.54386(9) 0.8965(2) 0.0184(4) Uani 1 d . . . 
C35 C 0.24211(17) 0.57607(14) 0.6863(3) 0.0375(6) Uani 1 d . . . 
C32 C 0.01500(15) 0.64800(13) 0.2918(3) 0.0348(6) Uani 1 d . . . 
C22 C -0.16316(17) 0.71591(11) 0.8832(3) 0.0439(7) Uani 1 d . . . 
C23 C -0.08873(17) 0.72225(11) 0.9032(3) 0.0387(6) Uani 1 d . . . 
C18 C 0.41253(15) 0.59244(11) -0.0357(3) 0.0298(5) Uani 1 d . . . 
C20 C -0.15599(14) 0.65037(12) 0.6948(3) 0.0317(6) Uani 1 d . . . 
H16 H 0.4914(13) 0.6517(10) 0.030(3) 0.025(6) Uiso 1 d . . . 
H1N H 0.4912(12) 0.7146(9) 0.346(2) 0.011(5) Uiso 1 d . . . 
H31 H 0.0963(11) 0.5884(9) 0.287(2) 0.011(5) Uiso 1 d . . . 
H2 H 0.5064(13) 0.8915(10) 0.045(3) 0.026(6) Uiso 1 d . . . 
H26 H 0.0254(13) 0.4705(10) 0.852(2) 0.020(6) Uiso 1 d . . . 
H13 H 0.3840(11) 0.7333(9) -0.002(2) 0.009(5) Uiso 1 d . . . 
H35C H 0.2133(14) 0.5500(11) 0.726(3) 0.031(7) Uiso 1 d . . . 
H15C H 0.2587(14) 0.7165(11) -0.043(3) 0.024(6) Uiso 1 d . . . 
H8 H 0.6381(13) 0.6735(10) 0.460(3) 0.025(6) Uiso 1 d . . . 
H6 H 0.6091(13) 0.8673(10) 0.433(3) 0.027(7) Uiso 1 d . . . 
H2N H 0.0565(14) 0.5398(11) 0.506(3) 0.033(7) Uiso 1 d . . . 
H17C H 0.5424(15) 0.6065(12) 0.237(3) 0.039(8) Uiso 1 d . . . 
H28 H 0.2068(13) 0.4501(10) 1.133(3) 0.025(6) Uiso 1 d . . . 
H34 H 0.2376(15) 0.6104(12) 0.491(3) 0.040(7) Uiso 1 d . . . 
H9 H 0.7068(12) 0.5892(10) 0.461(2) 0.021(6) Uiso 1 d . . . 
H36C H 0.2575(15) 0.5103(11) 0.460(3) 0.035(7) Uiso 1 d . . . 
H33C H 0.1307(15) 0.6678(13) 0.168(3) 0.043(8) Uiso 1 d . . . 
H15B H 0.2594(14) 0.6819(11) 0.083(3) 0.029(7) Uiso 1 d . . . 
H3 H 0.5695(17) 0.9710(14) 0.032(3) 0.055(9) Uiso 1 d . . . 
H29 H 0.2332(14) 0.5472(11) 1.118(3) 0.034(7) Uiso 1 d . . . 
H32C H -0.0221(15) 0.6223(12) 0.327(3) 0.041(8) Uiso 1 d . . . 
H35B H 0.2409(15) 0.6090(13) 0.728(3) 0.038(8) Uiso 1 d . . . 
H4 H 0.6490(14) 1.0057(12) 0.228(3) 0.033(7) Uiso 1 d . . . 
H23 H -0.0644(14) 0.7464(12) 0.972(3) 0.034(7) Uiso 1 d . . . 
H18C H 0.3797(15) 0.5692(12) 0.003(3) 0.040(8) Uiso 1 d . . . 
H14C H 0.3133(13) 0.7636(11) 0.236(3) 0.032(7) Uiso 1 d . . . 
H14B H 0.3071(15) 0.7997(11) 0.093(3) 0.037(7) Uiso 1 d . . . 
H24 H 0.0013(15) 0.6948(11) 0.830(3) 0.033(7) Uiso 1 d . . . 
H11 H 0.7643(15) 0.6396(11) 0.086(3) 0.038(8) Uiso 1 d . . . 
H36B H 0.1812(14) 0.5017(11) 0.495(3) 0.033(7) Uiso 1 d . . . 
H10 H 0.7736(17) 0.5754(13) 0.263(3) 0.057(9) Uiso 1 d . . . 
H17B H 0.5415(14) 0.5633(11) 0.105(3) 0.036(7) Uiso 1 d . . . 
H20 H -0.1742(15) 0.6290(11) 0.630(3) 0.035(8) Uiso 1 d . . . 
H21 H -0.2519(17) 0.6734(13) 0.759(3) 0.053(9) Uiso 1 d . . . 
H18B H 0.3859(15) 0.6177(13) -0.112(3) 0.043(8) Uiso 1 d . . . 
H32B H 0.0130(16) 0.6830(14) 0.331(3) 0.050(9) Uiso 1 d . . . 
H12 H 0.6941(14) 0.7229(12) 0.084(3) 0.040(7) Uiso 1 d . . . 
H14A H 0.3806(17) 0.7956(12) 0.188(3) 0.048(9) Uiso 1 d . . . 
H18A H 0.4395(17) 0.5673(13) -0.080(3) 0.054(9) Uiso 1 d . . . 
H17A H 0.4875(15) 0.5571(12) 0.208(3) 0.041(8) Uiso 1 d . . . 
H5 H 0.6716(14) 0.9538(11) 0.432(3) 0.034(7) Uiso 1 d . . . 
H36A H 0.1907(14) 0.5288(11) 0.359(3) 0.036(7) Uiso 1 d . . . 
H32A H 0.0043(17) 0.6488(13) 0.200(4) 0.050(9) Uiso 1 d . . . 
H33B H 0.1925(17) 0.6490(12) 0.265(3) 0.044(8) Uiso 1 d . . . 
H15A H 0.2945(16) 0.6607(13) -0.044(3) 0.045(8) Uiso 1 d . . . 
H33A H 0.1485(15) 0.6982(13) 0.307(3) 0.039(8) Uiso 1 d . . . 
H27 H 0.1017(15) 0.4124(13) 1.004(3) 0.048(8) Uiso 1 d . . . 
H35A H 0.2912(17) 0.5654(12) 0.689(3) 0.044(8) Uiso 1 d . . . 
H30 H 0.1542(14) 0.6017(12) 0.960(3) 0.036(8) Uiso 1 d . . . 
H22 H -0.1973(18) 0.7354(14) 0.940(3) 0.065(10) Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Se1 0.02250(12) 0.01738(11) 0.01836(11) 0.00181(8) 0.00807(8) -0.00399(8) 
P2 0.0166(2) 0.0124(2) 0.0123(2) -0.00129(18) 0.00351(19) -0.00221(19) 
P1 0.0165(2) 0.0112(2) 0.0115(2) 0.00030(18) 0.00302(19) -0.00154(19) 
O2 0.0164(7) 0.0130(7) 0.0169(7) -0.0019(5) 0.0006(6) -0.0006(5) 
C15 0.0195(11) 0.0354(14) 0.0210(12) 0.0002(11) -0.0001(9) -0.0012(10) 
O3 0.0241(7) 0.0188(7) 0.0117(7) 0.0017(5) 0.0044(6) -0.0018(6) 
C3 0.0393(14) 0.0203(12) 0.0443(16) 0.0156(11) 0.0166(12) 0.0053(11) 
C6 0.0203(10) 0.0217(11) 0.0229(11) -0.0038(9) 0.0054(9) -0.0009(9) 
C13 0.0181(10) 0.0199(10) 0.0155(10) 0.0021(8) 0.0044(8) 0.0002(8) 
N1 0.0199(9) 0.0129(8) 0.0091(8) -0.0012(6) 0.0030(7) -0.0041(6) 
C1 0.0173(10) 0.0108(9) 0.0243(11) -0.0003(8) 0.0069(8) 0.0006(7) 
C7 0.0162(9) 0.0140(9) 0.0211(10) -0.0046(8) 0.0021(8) -0.0020(7) 
O1 0.0198(7) 0.0106(6) 0.0218(8) -0.0013(5) 0.0059(6) -0.0019(5) 
C8 0.0230(11) 0.0232(11) 0.0207(11) 0.0017(9) 0.0013(9) 0.0001(9) 
C14 0.0233(11) 0.0226(11) 0.0290(12) 0.0003(10) 0.0022(10) 0.0073(10) 
C17 0.0302(12) 0.0174(11) 0.0306(13) -0.0025(10) 0.0097(11) 0.0024(10) 
C9 0.0313(13) 0.0239(12) 0.0334(13) 0.0061(10) -0.0044(11) 0.0022(10) 
C11 0.0327(13) 0.0334(13) 0.0378(15) -0.0046(11) 0.0126(12) 0.0097(11) 
C12 0.0262(11) 0.0229(11) 0.0251(12) 0.0004(9) 0.0074(9) 0.0014(9) 
C4 0.0335(13) 0.0145(11) 0.0558(17) -0.0026(11) 0.0196(12) -0.0062(10) 
C16 0.0231(10) 0.0165(10) 0.0196(10) -0.0049(8) 0.0074(9) -0.0037(8) 
C10 0.0322(13) 0.0218(12) 0.0465(16) -0.0026(11) 0.0010(12) 0.0103(10) 
C5 0.0261(12) 0.0247(12) 0.0377(14) -0.0122(10) 0.0099(11) -0.0074(9) 
C2 0.0312(12) 0.0194(11) 0.0268(12) 0.0037(9) 0.0043(10) 0.0023(9) 
Se2 0.03450(14) 0.01871(13) 0.04847(17) -0.01759(10) 0.02083(12) -0.01203(10) 
P3 0.0175(3) 0.0132(2) 0.0168(3) -0.00318(19) 0.0045(2) -0.00259(19) 
P4 0.0200(3) 0.0126(2) 0.0240(3) -0.0043(2) 0.0088(2) -0.0043(2) 
O6 0.0221(7) 0.0200(7) 0.0185(7) -0.0049(6) 0.0071(6) -0.0071(6) 
O4 0.0219(7) 0.0175(7) 0.0201(8) -0.0006(6) 0.0061(6) 0.0025(6) 
O5 0.0242(8) 0.0157(7) 0.0177(7) -0.0032(6) 0.0024(6) 0.0014(6) 
C19 0.0256(11) 0.0138(10) 0.0275(11) 0.0033(9) 0.0118(9) 0.0055(8) 
C33 0.0409(16) 0.0279(14) 0.0335(15) 0.0127(12) 0.0113(13) -0.0028(12) 
C31 0.0274(11) 0.0151(10) 0.0249(11) 0.0027(9) 0.0086(9) 0.0010(9) 
C30 0.0316(13) 0.0268(13) 0.0200(11) 0.0013(9) 0.0020(9) -0.0067(10) 
N2 0.0197(9) 0.0126(8) 0.0228(9) -0.0063(7) 0.0079(7) -0.0055(7) 
C34 0.0178(10) 0.0227(11) 0.0251(11) -0.0022(9) 0.0068(9) -0.0041(9) 
C26 0.0252(11) 0.0190(11) 0.0269(12) -0.0005(9) 0.0029(9) -0.0009(9) 
C29 0.0262(12) 0.0452(15) 0.0249(12) 0.0043(11) -0.0005(10) -0.0052(11) 
C27 0.0331(13) 0.0230(12) 0.0272(12) 0.0043(9) 0.0070(10) 0.0027(10) 
C21 0.0297(14) 0.0416(16) 0.064(2) 0.0171(14) 0.0232(14) 0.0172(12) 
C36 0.0243(12) 0.0275(12) 0.0267(13) -0.0045(10) 0.0023(10) 0.0090(10) 
C28 0.0283(12) 0.0406(14) 0.0261(12) 0.0089(11) 0.0050(10) 0.0074(11) 
C24 0.0319(13) 0.0199(11) 0.0335(13) -0.0029(9) 0.0141(11) -0.0004(10) 
C25 0.0218(10) 0.0200(10) 0.0142(9) -0.0020(8) 0.0060(8) 0.0016(8) 
C35 0.0358(15) 0.0457(17) 0.0285(14) -0.0107(13) -0.0037(12) 0.0029(13) 
C32 0.0336(14) 0.0314(14) 0.0391(16) 0.0037(12) 0.0042(12) 0.0087(11) 
C22 0.0541(17) 0.0282(14) 0.0580(19) 0.0086(13) 0.0365(16) 0.0176(13) 
C23 0.0583(18) 0.0206(12) 0.0430(16) -0.0037(11) 0.0269(14) 0.0043(12) 
C18 0.0363(14) 0.0264(12) 0.0269(13) -0.0123(11) 0.0050(11) -0.0029(11) 
C20 0.0244(12) 0.0317(13) 0.0396(15) 0.0073(12) 0.0067(11) 0.0056(10) 

_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 
Se1 P2 2.0929(7) . ? 
P2 N1 1.6936(17) . ? 
P2 C13 1.824(2) . ? 
P2 C16 1.826(2) . ? 
P1 O3 1.4563(14) . ? 
P1 O1 1.5680(14) . ? 
P1 O2 1.5765(15) . ? 
P1 N1 1.6202(17) . ? 
O2 C7 1.404(2) . ? 
C15 C13 1.526(3) . ? 
C3 C4 1.378(4) . ? 
C3 C2 1.388(3) . ? 
C6 C1 1.369(3) . ? 
C6 C5 1.378(3) . ? 
C13 C14 1.520(3) . ? 
C1 C2 1.371(3) . ? 
C1 O1 1.402(2) . ? 
C7 C12 1.374(3) . ? 
C7 C8 1.375(3) . ? 
C8 C9 1.386(3) . ? 
C17 C16 1.514(3) . ? 
C9 C10 1.375(4) . ? 
C11 C12 1.381(3) . ? 
C11 C10 1.383(4) . ? 
C4 C5 1.369(4) . ? 
C16 C18 1.516(3) . ? 
Se2 P4 2.0810(7) . ? 
P3 O6 1.4620(14) . ? 
P3 O4 1.5651(15) . ? 
P3 O5 1.5704(15) . ? 
P3 N2 1.6210(18) . ? 
P4 N2 1.6858(18) . ? 
P4 C31 1.821(2) . ? 
P4 C34 1.822(2) . ? 
O4 C19 1.404(2) . ? 
O5 C25 1.396(2) . ? 
C19 C20 1.367(3) . ? 
C19 C24 1.375(3) . ? 
C33 C31 1.514(3) . ? 
C31 C32 1.515(3) . ? 
C30 C29 1.374(3) . ? 
C30 C25 1.375(3) . ? 
C34 C36 1.512(3) . ? 
C34 C35 1.517(3) . ? 
C26 C25 1.376(3) . ? 
C26 C27 1.378(3) . ? 
C29 C28 1.382(4) . ? 
C27 C28 1.375(3) . ? 
C21 C22 1.370(5) . ? 
C21 C20 1.383(4) . ? 
C24 C23 1.390(3) . ? 
C22 C23 1.369(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 
N1 P2 C13 106.30(9) . . ? 
N1 P2 C16 102.89(9) . . ? 
C13 P2 C16 110.12(10) . . ? 
N1 P2 Se1 108.13(6) . . ? 
C13 P2 Se1 113.10(7) . . ? 
C16 P2 Se1 115.37(7) . . ? 
O3 P1 O1 115.79(8) . . ? 
O3 P1 O2 114.47(8) . . ? 
O1 P1 O2 100.06(8) . . ? 
O3 P1 N1 113.51(9) . . ? 
O1 P1 N1 103.84(8) . . ? 
O2 P1 N1 107.80(8) . . ? 
C7 O2 P1 121.40(12) . . ? 
C4 C3 C2 120.6(2) . . ? 
C1 C6 C5 118.6(2) . . ? 
C14 C13 C15 108.80(19) . . ? 
C14 C13 P2 110.26(15) . . ? 
C15 C13 P2 111.83(16) . . ? 
P1 N1 P2 129.29(11) . . ? 
C6 C1 C2 122.9(2) . . ? 
C6 C1 O1 117.36(19) . . ? 
C2 C1 O1 119.68(19) . . ? 
C12 C7 C8 122.6(2) . . ? 
C12 C7 O2 119.52(19) . . ? 
C8 C7 O2 117.79(18) . . ? 
C1 O1 P1 122.41(12) . . ? 
C7 C8 C9 118.5(2) . . ? 
C10 C9 C8 119.9(2) . . ? 
C12 C11 C10 120.2(2) . . ? 
C7 C12 C11 118.2(2) . . ? 
C5 C4 C3 120.2(2) . . ? 
C17 C16 C18 111.17(19) . . ? 
C17 C16 P2 109.91(15) . . ? 
C18 C16 P2 113.99(16) . . ? 
C9 C10 C11 120.6(2) . . ? 
C4 C5 C6 120.1(2) . . ? 
C1 C2 C3 117.5(2) . . ? 
O6 P3 O4 115.42(9) . . ? 
O6 P3 O5 114.28(8) . . ? 
O4 P3 O5 100.34(8) . . ? 
O6 P3 N2 110.49(9) . . ? 
O4 P3 N2 105.75(9) . . ? 
O5 P3 N2 109.85(9) . . ? 
N2 P4 C31 102.89(10) . . ? 
N2 P4 C34 105.06(10) . . ? 
C31 P4 C34 106.04(11) . . ? 
N2 P4 Se2 114.56(7) . . ? 
C31 P4 Se2 114.39(7) . . ? 
C34 P4 Se2 112.87(8) . . ? 
C19 O4 P3 123.99(13) . . ? 
C25 O5 P3 124.88(12) . . ? 
C20 C19 C24 122.1(2) . . ? 
C20 C19 O4 118.6(2) . . ? 
C24 C19 O4 119.23(19) . . ? 
C33 C31 C32 111.6(2) . . ? 
C33 C31 P4 109.87(18) . . ? 
C32 C31 P4 110.84(18) . . ? 
C29 C30 C25 119.1(2) . . ? 
P3 N2 P4 132.37(11) . . ? 
C36 C34 C35 110.8(2) . . ? 
C36 C34 P4 113.81(16) . . ? 
C35 C34 P4 111.83(17) . . ? 
C25 C26 C27 118.3(2) . . ? 
C30 C29 C28 120.3(2) . . ? 
C28 C27 C26 121.0(2) . . ? 
C22 C21 C20 120.3(3) . . ? 
C27 C28 C29 119.5(2) . . ? 
C19 C24 C23 118.3(2) . . ? 
C30 C25 C26 121.7(2) . . ? 
C30 C25 O5 115.84(19) . . ? 
C26 C25 O5 122.39(19) . . ? 
C23 C22 C21 120.4(2) . . ? 
C22 C23 C24 120.2(3) . . ? 
C19 C20 C21 118.7(3) . . ? 

_diffrn_measured_fraction_theta_max    0.899 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.971 
_refine_diff_density_max    0.511 
_refine_diff_density_min   -0.644 
_refine_diff_density_rms    0.081 

data_5.cif
#data_man58b 
_database_code_CSD                153016
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'Ph2P(Se)-NH-P(S)(OPh)2'
_chemical_formula_sum 
'C24 H21 N O2 P2 S Se' 
_chemical_formula_weight          528.38 

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' 
'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' 
'Se'  'Se'  -0.0929   2.2259 
'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' 

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/c

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x, y, -z+1/2' 
'x+1/2, y+1/2, z' 
'-x+1/2, y+1/2, -z+1/2' 
'-x, -y, -z' 
'x, -y, z-1/2' 
'-x+1/2, -y+1/2, -z' 
'x+1/2, -y+1/2, z-1/2' 

_cell_length_a                    23.236(5) 
_cell_length_b                    9.654(2) 
_cell_length_c                    22.026(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  108.97(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4672.5(16) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.40
_exptl_crystal_size_min           0.40
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.502 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2144 
_exptl_absorpt_coefficient_mu     1.855 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2880 
_diffrn_reflns_av_R_equivalents   0.0495 
_diffrn_reflns_av_sigmaI/netI     0.0336 
_diffrn_reflns_limit_h_min        -22 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          3.37 
_diffrn_reflns_theta_max          22.67 
_reflns_number_total              2789 
_reflns_number_gt                 2268 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0768P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2789 
_refine_ls_number_parameters      284 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0492 
_refine_ls_R_factor_gt            0.0342 
_refine_ls_wR_factor_ref          0.1014 
_refine_ls_wR_factor_gt           0.0939 
_refine_ls_goodness_of_fit_ref    1.015 
_refine_ls_restrained_S_all       1.015 
_refine_ls_shift/su_max           0.002 
_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 
Se Se 0.270825(16) 0.76585(4) 0.202641(17) 0.02262(19) Uani 1 d . . . 
P2 P 0.36178(4) 0.75354(8) 0.25921(4) 0.0141(3) Uani 1 d . . . 
S S 0.47369(4) 0.53359(8) 0.14809(4) 0.0182(3) Uani 1 d . . . 
P1 P 0.40396(4) 0.63102(8) 0.15410(4) 0.0132(3) Uani 1 d . . . 
O2 O 0.39504(10) 0.7858(2) 0.12871(11) 0.0152(5) Uani 1 d . . . 
O1 O 0.34087(10) 0.5680(2) 0.11226(10) 0.0163(5) Uani 1 d . . . 
N N 0.40442(14) 0.6517(3) 0.22752(15) 0.0155(7) Uani 1 d . . . 
H0 H 0.4307(16) 0.619(4) 0.2508(17) 0.004(10) Uiso 1 d . . . 
C16 C 0.40633(18) 0.5220(4) 0.44979(19) 0.0304(10) Uani 1 d . . . 
H16 H 0.4176 0.4724 0.4881 0.036 Uiso 1 calc R . . 
C22 C 0.4588(2) 1.1694(4) 0.3101(2) 0.0370(11) Uani 1 d . . . 
H22 H 0.4785 1.2540 0.3213 0.044 Uiso 1 calc R . . 
C21 C 0.49191(18) 1.0480(4) 0.32158(18) 0.0278(9) Uani 1 d . . . 
H21 H 0.5339 1.0504 0.3409 0.033 Uiso 1 calc R . . 
C1 C 0.32567(16) 0.4250(3) 0.11077(16) 0.0167(8) Uani 1 d . . . 
C13 C 0.37698(15) 0.6674(3) 0.33573(16) 0.0163(8) Uani 1 d . . . 
C17 C 0.37711(19) 0.4566(4) 0.39249(19) 0.0307(10) Uani 1 d . . . 
H17 H 0.3672 0.3632 0.3922 0.037 Uiso 1 calc R . . 
C18 C 0.36245(17) 0.5293(4) 0.33557(18) 0.0243(9) Uani 1 d . . . 
H18 H 0.3427 0.4848 0.2970 0.029 Uiso 1 calc R . . 
C19 C 0.39985(16) 0.9191(3) 0.27644(16) 0.0169(8) Uani 1 d . . . 
C23 C 0.3966(2) 1.1652(4) 0.2821(2) 0.0364(11) Uani 1 d . . . 
H23 H 0.3743 1.2471 0.2743 0.044 Uiso 1 calc R . . 
C20 C 0.46229(16) 0.9230(4) 0.30420(17) 0.0217(9) Uani 1 d . . . 
H20 H 0.4845 0.8411 0.3112 0.026 Uiso 1 calc R . . 
C6 C 0.3416(2) 0.3406(4) 0.0698(2) 0.0384(11) Uani 1 d . . . 
H6 H 0.3647 0.3742 0.0455 0.046 Uiso 1 calc R . . 
C15 C 0.41872(17) 0.6616(4) 0.44998(18) 0.0275(10) Uani 1 d . . . 
H15 H 0.4375 0.7065 0.4887 0.033 Uiso 1 calc R . . 
C5 C 0.3230(2) 0.2036(5) 0.0646(2) 0.0517(14) Uani 1 d . . . 
H5 H 0.3338 0.1440 0.0369 0.062 Uiso 1 calc R . . 
C14 C 0.40367(17) 0.7353(4) 0.39351(18) 0.0198(9) Uani 1 d . . . 
H14 H 0.4113 0.8299 0.3941 0.024 Uiso 1 calc R . . 
C3 C 0.27266(18) 0.2435(4) 0.1407(2) 0.0243(9) Uani 1 d . . . 
H3 H 0.2489 0.2109 0.1644 0.029 Uiso 1 calc R . . 
C4 C 0.2886(2) 0.1561(4) 0.1003(2) 0.0348(10) Uani 1 d . . . 
H4 H 0.2761 0.0641 0.0970 0.042 Uiso 1 calc R . . 
C24 C 0.36734(18) 1.0409(4) 0.26572(18) 0.0254(9) Uani 1 d . . . 
H24 H 0.3252 1.0387 0.2472 0.030 Uiso 1 calc R . . 
C2 C 0.29130(16) 0.3800(4) 0.14674(17) 0.0201(8) Uani 1 d . . . 
H2 H 0.2808 0.4396 0.1746 0.024 Uiso 1 calc R . . 
C12 C 0.32300(16) 0.8372(3) 0.02569(17) 0.0186(8) Uani 1 d . . . 
H12 H 0.2914 0.8212 0.0420 0.022 Uiso 1 calc R . . 
C7 C 0.38247(15) 0.8200(3) 0.06391(16) 0.0140(8) Uani 1 d . . . 
C9 C 0.41660(18) 0.8852(4) -0.02195(18) 0.0276(10) Uani 1 d . . . 
H9 H 0.4482 0.9024 -0.0382 0.033 Uiso 1 calc R . . 
C8 C 0.42982(17) 0.8419(4) 0.04050(17) 0.0240(9) Uani 1 d . . . 
H8 H 0.4699 0.8279 0.0664 0.029 Uiso 1 calc R . . 
C11 C 0.31106(18) 0.8779(3) -0.03621(17) 0.0240(9) Uani 1 d . . . 
H11 H 0.2709 0.8890 -0.0625 0.029 Uiso 1 calc R . . 
C10 C 0.35793(18) 0.9031(4) -0.06043(18) 0.0254(9) Uani 1 d . . . 
H10 H 0.3495 0.9320 -0.1027 0.030 Uiso 1 calc R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Se 0.0087(3) 0.0306(3) 0.0262(3) -0.00274(15) 0.0024(2) 0.00477(14) 
P2 0.0102(6) 0.0142(5) 0.0176(6) -0.0011(3) 0.0041(5) 0.0021(3) 
S 0.0117(5) 0.0190(5) 0.0247(6) -0.0040(4) 0.0071(4) 0.0027(3) 
P1 0.0084(5) 0.0128(5) 0.0183(5) -0.0009(3) 0.0042(4) -0.0006(3) 
O2 0.0139(14) 0.0145(12) 0.0165(14) 0.0004(10) 0.0039(11) 0.0003(10) 
O1 0.0115(13) 0.0151(12) 0.0203(13) -0.0030(9) 0.0025(11) -0.0035(10) 
N 0.0077(17) 0.0139(15) 0.0220(18) 0.0041(13) 0.0011(15) 0.0076(13) 
C16 0.032(3) 0.037(2) 0.027(2) 0.0075(18) 0.016(2) 0.0043(19) 
C22 0.054(3) 0.016(2) 0.040(3) -0.0054(17) 0.014(2) -0.0106(19) 
C21 0.023(2) 0.023(2) 0.033(2) -0.0033(17) 0.0031(19) -0.0082(17) 
C1 0.015(2) 0.0146(18) 0.0188(19) -0.0024(14) 0.0035(17) -0.0027(14) 
C13 0.0079(19) 0.0179(19) 0.025(2) 0.0004(15) 0.0084(16) 0.0060(14) 
C17 0.041(3) 0.021(2) 0.035(3) 0.0076(18) 0.019(2) -0.0015(17) 
C18 0.024(2) 0.024(2) 0.027(2) -0.0047(16) 0.0109(18) -0.0029(16) 
C19 0.019(2) 0.0148(18) 0.0174(19) -0.0018(14) 0.0064(16) 0.0004(15) 
C23 0.044(3) 0.018(2) 0.043(3) -0.0021(18) 0.009(2) 0.0081(19) 
C20 0.019(2) 0.019(2) 0.028(2) 0.0005(15) 0.0081(18) 0.0026(15) 
C6 0.052(3) 0.033(2) 0.045(3) -0.014(2) 0.036(2) -0.020(2) 
C15 0.023(2) 0.037(2) 0.025(2) -0.0039(17) 0.0117(19) -0.0034(17) 
C5 0.075(4) 0.032(2) 0.065(3) -0.027(2) 0.048(3) -0.025(3) 
C14 0.013(2) 0.0242(19) 0.024(2) -0.0010(16) 0.0086(18) -0.0044(14) 
C3 0.017(2) 0.028(2) 0.031(2) 0.0032(16) 0.013(2) -0.0065(15) 
C4 0.039(3) 0.023(2) 0.048(3) -0.0070(19) 0.022(2) -0.0151(18) 
C24 0.021(2) 0.020(2) 0.031(2) 0.0005(16) 0.0045(19) 0.0066(16) 
C2 0.012(2) 0.023(2) 0.027(2) -0.0013(15) 0.0083(17) 0.0014(15) 
C12 0.012(2) 0.0166(18) 0.026(2) -0.0011(15) 0.0050(17) -0.0018(14) 
C7 0.014(2) 0.0111(17) 0.017(2) -0.0012(14) 0.0052(16) -0.0025(14) 
C9 0.027(3) 0.033(2) 0.026(2) 0.0014(17) 0.013(2) -0.0036(17) 
C8 0.016(2) 0.032(2) 0.022(2) 0.0014(16) 0.0028(18) -0.0031(16) 
C11 0.021(2) 0.019(2) 0.023(2) -0.0008(15) -0.0048(18) -0.0003(15) 
C10 0.037(3) 0.0176(19) 0.020(2) 0.0040(15) 0.007(2) -0.0004(16) 

_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 
Se P2 2.0787(12) . ? 
P2 N 1.699(3) . ? 
P2 C19 1.806(3) . ? 
P2 C13 1.808(3) . ? 
S P1 1.9148(12) . ? 
P1 O1 1.578(2) . ? 
P1 O2 1.586(2) . ? 
P1 N 1.626(3) . ? 
O2 C7 1.400(4) . ? 
O1 C1 1.423(4) . ? 
C16 C17 1.377(6) . ? 
C16 C15 1.378(6) . ? 
C22 C23 1.375(6) . ? 
C22 C21 1.380(6) . ? 
C21 C20 1.380(5) . ? 
C1 C6 1.354(5) . ? 
C1 C2 1.366(5) . ? 
C13 C18 1.375(5) . ? 
C13 C14 1.386(5) . ? 
C17 C18 1.380(5) . ? 
C19 C24 1.376(5) . ? 
C19 C20 1.380(5) . ? 
C23 C24 1.369(5) . ? 
C6 C5 1.385(6) . ? 
C15 C14 1.376(5) . ? 
C5 C4 1.372(6) . ? 
C3 C4 1.361(5) . ? 
C3 C2 1.379(5) . ? 
C12 C11 1.358(5) . ? 
C12 C7 1.375(5) . ? 
C7 C8 1.375(5) . ? 
C9 C10 1.362(5) . ? 
C9 C8 1.373(5) . ? 
C11 C10 1.381(5) . ? 

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 
N P2 C19 106.70(15) . . ? 
N P2 C13 98.82(15) . . ? 
C19 P2 C13 106.10(16) . . ? 
N P2 Se 113.70(12) . . ? 
C19 P2 Se 114.11(12) . . ? 
C13 P2 Se 115.94(12) . . ? 
O1 P1 O2 99.65(13) . . ? 
O1 P1 N 109.42(14) . . ? 
O2 P1 N 101.14(14) . . ? 
O1 P1 S 114.61(10) . . ? 
O2 P1 S 117.08(10) . . ? 
N P1 S 113.37(12) . . ? 
C7 O2 P1 122.8(2) . . ? 
C1 O1 P1 124.4(2) . . ? 
P1 N P2 131.6(2) . . ? 
C17 C16 C15 119.5(4) . . ? 
C23 C22 C21 120.0(4) . . ? 
C22 C21 C20 119.6(4) . . ? 
C6 C1 C2 122.3(3) . . ? 
C6 C1 O1 118.6(3) . . ? 
C2 C1 O1 118.9(3) . . ? 
C18 C13 C14 119.8(3) . . ? 
C18 C13 P2 118.0(3) . . ? 
C14 C13 P2 122.1(3) . . ? 
C16 C17 C18 120.1(4) . . ? 
C13 C18 C17 120.2(4) . . ? 
C24 C19 C20 119.5(3) . . ? 
C24 C19 P2 121.1(3) . . ? 
C20 C19 P2 119.4(3) . . ? 
C24 C23 C22 120.2(4) . . ? 
C19 C20 C21 120.3(3) . . ? 
C1 C6 C5 118.9(4) . . ? 
C14 C15 C16 120.8(4) . . ? 
C4 C5 C6 119.8(4) . . ? 
C15 C14 C13 119.4(3) . . ? 
C4 C3 C2 120.8(4) . . ? 
C3 C4 C5 120.0(4) . . ? 
C23 C24 C19 120.4(4) . . ? 
C1 C2 C3 118.2(3) . . ? 
C11 C12 C7 119.1(3) . . ? 
C12 C7 C8 121.3(3) . . ? 
C12 C7 O2 119.2(3) . . ? 
C8 C7 O2 119.4(3) . . ? 
C10 C9 C8 121.0(4) . . ? 
C9 C8 C7 118.5(3) . . ? 
C12 C11 C10 120.6(4) . . ? 
C9 C10 C11 119.5(3) . . ? 

loop_ 
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_distance_DH 
_geom_hbond_distance_HA 
_geom_hbond_distance_DA 
_geom_hbond_angle_DHA 
_geom_hbond_site_symmetry_A 
N H0 S  0.73(4) 2.71(4) 3.432(4) 170(3) 2_655 

_diffrn_measured_fraction_theta_max    0.416 
_diffrn_reflns_theta_full              22.67 
_diffrn_measured_fraction_theta_full   0.416 
_refine_diff_density_max    0.686 
_refine_diff_density_min   -0.980 
_refine_diff_density_rms    0.091 


data_6.cif
#data_man52b 
_database_code_CSD                153017
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'Ph2P(S)-NH-P(S)(OPh)2'
_chemical_formula_sum 
'C24 H21 N O2 P2 S2' 
_chemical_formula_weight          481.48 

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' 

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/c

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x, y, -z+1/2' 
'x+1/2, y+1/2, z' 
'-x+1/2, y+1/2, -z+1/2' 
'-x, -y, -z' 
'x, -y, z-1/2' 
'-x+1/2, -y+1/2, -z' 
'x+1/2, -y+1/2, z-1/2' 

_cell_length_a                    23.166(5) 
_cell_length_b                    9.633(2) 
_cell_length_c                    22.060(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  109.23(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      4648.2(16) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     130(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.50
_exptl_crystal_size_min           0.30
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.376 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2000 
_exptl_absorpt_coefficient_mu     0.389 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4134 
_diffrn_reflns_av_R_equivalents   0.0131 
_diffrn_reflns_av_sigmaI/netI     0.0238 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        0 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          3.74 
_diffrn_reflns_theta_max          25.09 
_reflns_number_total              4026 
_reflns_number_gt                 3437 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0561P)^2^+5.3652P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4026 
_refine_ls_number_parameters      280 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0430 
_refine_ls_R_factor_gt            0.0332 
_refine_ls_wR_factor_ref          0.0993 
_refine_ls_wR_factor_gt           0.0936 
_refine_ls_goodness_of_fit_ref    1.066 
_refine_ls_restrained_S_all       1.066 
_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 
P1 P 0.09611(2) 0.12851(5) 0.84606(2) 0.01597(14) Uani 1 d . . . 
S1 S 0.02596(2) 0.03163(5) 0.85197(2) 0.02147(14) Uani 1 d . . . 
P2 P 0.14043(2) 0.24604(5) 0.74175(2) 0.01725(14) Uani 1 d . . . 
S2 S 0.22516(2) 0.25294(6) 0.79509(3) 0.02617(15) Uani 1 d . . . 
O2 O 0.10476(6) 0.28406(14) 0.87025(6) 0.0189(3) Uani 1 d . . . 
O1 O 0.15951(6) 0.06639(14) 0.88851(6) 0.0199(3) Uani 1 d . . . 
N1 N 0.09573(7) 0.14622(17) 0.77199(8) 0.0178(4) Uani 1 d . . . 
C18 C 0.14225(11) 0.0230(2) 0.66532(11) 0.0294(5) Uani 1 d . . . 
C1 C 0.17480(9) -0.0754(2) 0.88978(9) 0.0208(4) Uani 1 d . . . 
C8 C 0.17675(9) 0.3354(2) 0.97348(10) 0.0244(5) Uani 1 d . . . 
C6 C 0.20974(9) -0.1189(2) 0.85384(10) 0.0239(5) Uani 1 d . . . 
C9 C 0.18847(10) 0.3784(2) 1.03613(11) 0.0290(5) Uani 1 d . . . 
C24 C 0.13906(11) 0.5326(2) 0.73405(11) 0.0307(5) Uani 1 d . . . 
C21 C 0.01293(11) 0.5494(2) 0.68114(11) 0.0332(5) Uani 1 d . . . 
C13 C 0.12535(9) 0.1613(2) 0.66516(9) 0.0193(4) Uani 1 d . . . 
C12 C 0.06903(10) 0.3448(2) 0.95733(10) 0.0279(5) Uani 1 d . . . 
C4 C 0.21210(13) -0.3464(3) 0.89861(14) 0.0416(6) Uani 1 d . . . 
C20 C 0.04079(10) 0.4214(2) 0.69814(10) 0.0261(5) Uani 1 d . . . 
C16 C 0.09660(12) 0.0151(3) 0.55093(12) 0.0372(6) Uani 1 d . . . 
C11 C 0.08198(11) 0.3891(3) 1.02034(11) 0.0342(5) Uani 1 d . . . 
C5 C 0.22848(11) -0.2565(2) 0.85900(11) 0.0297(5) Uani 1 d . . . 
C17 C 0.12785(13) -0.0491(2) 0.60826(12) 0.0392(6) Uani 1 d . . . 
C7 C 0.11692(9) 0.31989(19) 0.93514(9) 0.0186(4) Uani 1 d . . . 
C19 C 0.10404(9) 0.4128(2) 0.72451(9) 0.0205(4) Uani 1 d . . . 
C3 C 0.17687(16) -0.2998(3) 0.93416(16) 0.0560(9) Uani 1 d . . . 
C23 C 0.11078(13) 0.6590(2) 0.71733(13) 0.0410(6) Uani 1 d . . . 
C15 C 0.08166(11) 0.1531(3) 0.55031(11) 0.0319(5) Uani 1 d . . . 
C22 C 0.04837(13) 0.6679(2) 0.69074(12) 0.0397(6) Uani 1 d . . . 
C2 C 0.15834(13) -0.1622(3) 0.93033(14) 0.0429(7) Uani 1 d . . . 
C10 C 0.14124(11) 0.4063(2) 1.05929(10) 0.0315(5) Uani 1 d . . . 
C14 C 0.09615(10) 0.2269(2) 0.60739(10) 0.0239(5) Uani 1 d . . . 
H6 H 0.2229 -0.0519 0.8231 0.050 Uiso 1 d . . . 
H5 H 0.2515 -0.2891 0.8260 0.050 Uiso 1 d . . . 
H9 H 0.2324 0.3902 1.0631 0.050 Uiso 1 d . . . 
H15 H 0.0563 0.2038 0.5058 0.050 Uiso 1 d . . . 
H8 H 0.2110 0.3098 0.9533 0.050 Uiso 1 d . . . 
H24 H 0.1885 0.5233 0.7577 0.050 Uiso 1 d . . . 
H11 H 0.0457 0.4084 1.0411 0.050 Uiso 1 d . . . 
H22 H 0.0266 0.7534 0.6809 0.050 Uiso 1 d . . . 
H20 H 0.0182 0.3252 0.6944 0.050 Uiso 1 d . . . 
H18 H 0.1660 -0.0245 0.7108 0.050 Uiso 1 d . . . 
H10 H 0.1530 0.4333 1.1067 0.050 Uiso 1 d . . . 
H12 H 0.0246 0.3305 0.9257 0.050 Uiso 1 d . . . 
H21 H -0.0378 0.5442 0.6633 0.050 Uiso 1 d . . . 
H16 H 0.0842 -0.0489 0.5069 0.050 Uiso 1 d . . . 
H23 H 0.1367 0.7430 0.7264 0.050 Uiso 1 d . . . 
H3 H 0.1682 -0.3699 0.9641 0.050 Uiso 1 d . . . 
H14 H 0.0861 0.3306 0.6059 0.050 Uiso 1 d . . . 
H17 H 0.1443 -0.1514 0.6089 0.050 Uiso 1 d . . . 
H2 H 0.1281 -0.1262 0.9545 0.050 Uiso 1 d . . . 
H4 H 0.2247 -0.4564 0.8974 0.050 Uiso 1 d . . . 
H0 H 0.0565 0.1018 0.7391 0.050 Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
P1 0.0158(3) 0.0143(3) 0.0167(3) 0.00140(18) 0.0038(2) 0.00074(18) 
S1 0.0197(3) 0.0219(3) 0.0230(3) 0.0038(2) 0.0072(2) -0.00258(19) 
P2 0.0169(3) 0.0163(3) 0.0178(3) 0.00062(19) 0.0045(2) -0.00263(19) 
S2 0.0171(3) 0.0312(3) 0.0268(3) 0.0029(2) 0.0026(2) -0.0049(2) 
O2 0.0224(7) 0.0158(7) 0.0164(7) 0.0004(5) 0.0035(5) 0.0004(5) 
O1 0.0182(7) 0.0173(7) 0.0206(7) 0.0008(5) 0.0017(6) 0.0036(5) 
N1 0.0171(8) 0.0177(8) 0.0180(9) 0.0006(6) 0.0050(7) -0.0030(6) 
C18 0.0420(13) 0.0210(11) 0.0272(12) 0.0002(9) 0.0141(10) -0.0003(9) 
C1 0.0209(10) 0.0187(10) 0.0202(10) 0.0024(8) 0.0033(8) 0.0054(8) 
C8 0.0228(10) 0.0179(10) 0.0282(11) 0.0003(8) 0.0025(8) -0.0005(8) 
C6 0.0217(10) 0.0247(11) 0.0253(11) -0.0011(9) 0.0076(8) -0.0003(8) 
C9 0.0293(12) 0.0219(11) 0.0272(12) -0.0016(9) -0.0021(9) -0.0023(9) 
C24 0.0384(13) 0.0205(11) 0.0293(12) 0.0016(9) 0.0061(10) -0.0080(9) 
C21 0.0397(14) 0.0272(12) 0.0317(13) 0.0024(10) 0.0102(10) 0.0094(10) 
C13 0.0172(9) 0.0202(10) 0.0217(10) -0.0008(8) 0.0080(8) -0.0045(8) 
C12 0.0243(11) 0.0331(12) 0.0240(11) -0.0023(9) 0.0049(9) 0.0021(9) 
C4 0.0510(15) 0.0258(12) 0.0540(17) 0.0095(11) 0.0255(13) 0.0165(11) 
C20 0.0286(11) 0.0202(11) 0.0297(12) 0.0007(9) 0.0096(9) 0.0015(9) 
C16 0.0504(15) 0.0382(14) 0.0290(13) -0.0099(11) 0.0214(11) -0.0081(12) 
C11 0.0370(13) 0.0380(14) 0.0284(13) -0.0029(10) 0.0119(10) 0.0042(10) 
C5 0.0271(12) 0.0288(12) 0.0345(13) -0.0047(10) 0.0118(10) 0.0048(9) 
C17 0.0623(17) 0.0234(12) 0.0375(14) -0.0054(10) 0.0238(12) -0.0013(11) 
C7 0.0236(10) 0.0128(9) 0.0169(10) 0.0008(7) 0.0034(8) 0.0006(8) 
C19 0.0284(11) 0.0164(10) 0.0167(10) -0.0002(8) 0.0077(8) -0.0018(8) 
C3 0.086(2) 0.0341(15) 0.068(2) 0.0309(14) 0.0525(18) 0.0283(15) 
C23 0.0584(17) 0.0181(11) 0.0412(15) 0.0011(10) 0.0091(12) -0.0086(11) 
C15 0.0351(12) 0.0418(14) 0.0211(11) -0.0007(10) 0.0122(9) 0.0023(11) 
C22 0.0628(17) 0.0190(11) 0.0348(13) 0.0044(10) 0.0126(12) 0.0102(11) 
C2 0.0628(17) 0.0328(13) 0.0488(16) 0.0168(12) 0.0395(14) 0.0208(12) 
C10 0.0472(14) 0.0215(11) 0.0202(11) -0.0008(9) 0.0035(10) 0.0024(10) 
C14 0.0244(11) 0.0277(11) 0.0217(11) 0.0018(9) 0.0104(8) 0.0031(8) 

_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 
P1 O1 1.5767(14) . ? 
P1 O2 1.5811(14) . ? 
P1 N1 1.6400(17) . ? 
P1 S1 1.9153(8) . ? 
P2 N1 1.7021(16) . ? 
P2 C19 1.796(2) . ? 
P2 C13 1.804(2) . ? 
P2 S2 1.9288(10) . ? 
O2 C7 1.408(2) . ? 
O1 C1 1.409(2) . ? 
C18 C17 1.379(3) . ? 
C18 C13 1.388(3) . ? 
C1 C2 1.367(3) . ? 
C1 C6 1.372(3) . ? 
C8 C7 1.373(3) . ? 
C8 C9 1.382(3) . ? 
C6 C5 1.388(3) . ? 
C9 C10 1.378(3) . ? 
C24 C23 1.375(3) . ? 
C24 C19 1.386(3) . ? 
C21 C22 1.381(4) . ? 
C21 C20 1.385(3) . ? 
C13 C14 1.383(3) . ? 
C12 C7 1.373(3) . ? 
C12 C11 1.389(3) . ? 
C4 C5 1.369(4) . ? 
C4 C3 1.380(4) . ? 
C20 C19 1.390(3) . ? 
C16 C15 1.373(4) . ? 
C16 C17 1.379(4) . ? 
C11 C10 1.369(3) . ? 
C3 C2 1.387(4) . ? 
C23 C22 1.372(4) . ? 
C15 C14 1.387(3) . ? 

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 P1 O2 99.76(8) . . ? 
O1 P1 N1 109.25(8) . . ? 
O2 P1 N1 101.32(8) . . ? 
O1 P1 S1 114.83(6) . . ? 
O2 P1 S1 117.05(6) . . ? 
N1 P1 S1 113.09(7) . . ? 
N1 P2 C19 106.53(9) . . ? 
N1 P2 C13 98.99(9) . . ? 
C19 P2 C13 105.91(9) . . ? 
N1 P2 S2 114.12(6) . . ? 
C19 P2 S2 114.25(7) . . ? 
C13 P2 S2 115.54(7) . . ? 
C7 O2 P1 122.43(12) . . ? 
C1 O1 P1 123.96(12) . . ? 
P1 N1 P2 130.16(10) . . ? 
C17 C18 C13 119.9(2) . . ? 
C2 C1 C6 122.4(2) . . ? 
C2 C1 O1 118.91(19) . . ? 
C6 C1 O1 118.49(18) . . ? 
C7 C8 C9 118.3(2) . . ? 
C1 C6 C5 118.2(2) . . ? 
C10 C9 C8 120.7(2) . . ? 
C23 C24 C19 119.6(2) . . ? 
C22 C21 C20 119.6(2) . . ? 
C14 C13 C18 119.51(19) . . ? 
C14 C13 P2 122.77(16) . . ? 
C18 C13 P2 117.68(16) . . ? 
C7 C12 C11 118.5(2) . . ? 
C5 C4 C3 119.8(2) . . ? 
C21 C20 C19 120.0(2) . . ? 
C15 C16 C17 119.8(2) . . ? 
C10 C11 C12 120.5(2) . . ? 
C4 C5 C6 120.7(2) . . ? 
C18 C17 C16 120.5(2) . . ? 
C12 C7 C8 122.11(19) . . ? 
C12 C7 O2 119.38(17) . . ? 
C8 C7 O2 118.43(18) . . ? 
C24 C19 C20 119.9(2) . . ? 
C24 C19 P2 120.13(17) . . ? 
C20 C19 P2 119.91(16) . . ? 
C4 C3 C2 120.4(2) . . ? 
C22 C23 C24 120.8(2) . . ? 
C16 C15 C14 120.1(2) . . ? 
C23 C22 C21 120.2(2) . . ? 
C1 C2 C3 118.5(2) . . ? 
C11 C10 C9 119.9(2) . . ? 
C13 C14 C15 120.1(2) . . ? 

_diffrn_measured_fraction_theta_max    0.456 
_diffrn_reflns_theta_full              25.09 
_diffrn_measured_fraction_theta_full   0.456 
_refine_diff_density_max    0.425 
_refine_diff_density_min   -0.322 
_refine_diff_density_rms    0.065 

data_7.cif
#data_man89 
_database_code_CSD                153018
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'iPr2P(S)-NH-P(S)(OPh)2'
_chemical_formula_sum 
'C18 H25 N O2 P2 S2' 
_chemical_formula_weight          413.45 

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' 
'P'  'P'   0.1023   0.0942 
'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' 
'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                    8.494(2) 
_cell_length_b                    9.173(2) 
_cell_length_c                    13.751(3) 
_cell_angle_alpha                 97.97(3) 
_cell_angle_beta                  104.38(3) 
_cell_angle_gamma                 92.35(3) 
_cell_volume                      1024.6(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.340 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              436 
_exptl_absorpt_coefficient_mu     0.428 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3764 
_diffrn_reflns_av_R_equivalents   0.0163 
_diffrn_reflns_av_sigmaI/netI     0.0332 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          3.69 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              3602 
_reflns_number_gt                 2585 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0745P)^2^+3.1152P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3602 
_refine_ls_number_parameters      333 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1081 
_refine_ls_R_factor_gt            0.0771 
_refine_ls_wR_factor_ref          0.2127 
_refine_ls_wR_factor_gt           0.1908 
_refine_ls_goodness_of_fit_ref    1.089 
_refine_ls_restrained_S_all       1.089 
_refine_ls_shift/su_max           1.306 
_refine_ls_shift/su_mean          0.019 

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 
P1 P 0.32126(16) 0.66449(17) 0.58888(11) 0.0529(4) Uani 1 d . . . 
P2 P 0.64334(17) 0.73491(18) 0.75645(10) 0.0544(5) Uani 1 d . . . 
S1 S 0.2961(2) 0.6248(2) 0.44314(13) 0.0821(6) Uani 1 d . . . 
S2 S 0.5567(2) 0.8442(2) 0.85402(13) 0.0846(7) Uani 1 d . . . 
N1 N 0.5147(6) 0.6485(6) 0.6535(4) 0.0480(12) Uani 1 d . . . 
O2 O 0.7596(5) 0.6127(5) 0.7950(3) 0.0796(15) Uani 1 d . . . 
O1 O 0.7631(4) 0.8251(5) 0.7106(3) 0.0626(12) Uani 1 d . . . 
C31 C 0.1946(7) 0.5359(8) 0.6295(5) 0.0649(17) Uani 1 d . . . 
C32 C 0.2321(15) 0.3859(9) 0.5998(10) 0.108(3) Uani 1 d . . . 
C6 C 0.9940(7) 0.9190(8) 0.8516(4) 0.0595(15) Uani 1 d . . . 
C4 C 1.1131(9) 1.1627(10) 0.8602(6) 0.084(2) Uani 1 d . . . 
C33 C 0.1914(9) 0.5732(8) 0.7384(6) 0.0664(17) Uani 1 d . . . 
C3 C 0.9947(11) 1.1813(12) 0.7770(7) 0.111(3) Uani 1 d . . . 
C1 C 0.8791(6) 0.9386(7) 0.7666(4) 0.0598(16) Uani 1 d . . . 
C23 C 0.0925(13) 0.8633(12) 0.5749(8) 0.151(5) Uani 1 d . . . 
H23A H 0.0261 0.7894 0.5928 0.227 Uiso 1 d R . . 
H23B H 0.0758 0.8497 0.5025 0.227 Uiso 1 d R . . 
H23C H 0.0629 0.9595 0.5978 0.227 Uiso 1 d R . . 
C5 C 1.1103(8) 1.0349(10) 0.8980(5) 0.074(2) Uani 1 d . . . 
C22 C 0.3843(14) 0.9633(10) 0.5957(8) 0.139(4) Uani 1 d . . . 
H22A H 0.4951 0.9562 0.6322 0.208 Uiso 1 d R . . 
H22B H 0.3532 1.0611 0.6126 0.208 Uiso 1 d R . . 
H22C H 0.3749 0.9429 0.5240 0.208 Uiso 1 d R . . 
C21 C 0.2718(10) 0.8485(8) 0.6249(6) 0.093(2) Uani 1 d . . . 
H21 H 0.2879 0.8668 0.6988 0.111 Uiso 1 d R . . 
C2 C 0.8772(10) 1.0693(11) 0.7294(6) 0.111(4) Uani 1 d . . . 
C7 C 0.700(3) 0.520(2) 0.8534(18) 0.057(6) Uani 0.534(9) d P A 1 
C8 C 0.6302(16) 0.399(3) 0.8182(14) 0.084(8) Uani 0.534(9) d P A 1 
H8 H 0.5901 0.3767 0.7480 0.100 Uiso 0.534(9) calc PR A 1 
C9 C 0.605(2) 0.287(2) 0.8792(17) 0.090(7) Uani 0.534(9) d P A 1 
H9 H 0.5243 0.2100 0.8588 0.107 Uiso 0.534(9) calc PR A 1 
C10 C 0.7286(17) 0.3141(14) 0.9791(9) 0.067(4) Uani 0.534(9) d P A 1 
H10 H 0.7207 0.2513 1.0256 0.080 Uiso 0.534(9) calc PR A 1 
C11 C 0.8544(16) 0.4253(12) 1.0085(8) 0.064(3) Uani 0.534(9) d P A 1 
H11 H 0.9313 0.4311 1.0705 0.077 Uiso 0.534(9) calc PR A 1 
C12 C 0.8644(14) 0.5267(12) 0.9452(7) 0.057(3) Uani 0.534(9) d P A 1 
H12 H 0.9552 0.5920 0.9539 0.068 Uiso 0.534(9) calc PR A 1 
C7A C 0.746(4) 0.490(4) 0.847(2) 0.065(9) Uani 0.466(9) d P A 2 
C8A C 0.713(3) 0.374(2) 0.8158(12) 0.068(4) Uani 0.466(9) d P A 2 
H8A H 0.7146 0.3472 0.7482 0.081 Uiso 0.466(9) calc PR A 2 
C9A C 0.672(2) 0.263(2) 0.8629(15) 0.069(5) Uani 0.466(9) d P A 2 
H9A H 0.7030 0.1698 0.8421 0.083 Uiso 0.466(9) calc PR A 2 
C10A C 0.5938(17) 0.2708(14) 0.9337(11) 0.049(3) Uani 0.466(9) d P A 2 
H10A H 0.5637 0.1887 0.9596 0.058 Uiso 0.466(9) calc PR A 2 
C11A C 0.5603(16) 0.4102(12) 0.9663(9) 0.056(3) Uani 0.466(9) d P A 2 
H11A H 0.5052 0.4242 1.0171 0.067 Uiso 0.466(9) calc PR A 2 
C12A C 0.6048(15) 0.5320(13) 0.9270(8) 0.051(3) Uani 0.466(9) d P A 2 
H12A H 0.5674 0.6248 0.9397 0.062 Uiso 0.466(9) calc PR A 2 
H6 H 0.991(7) 0.835(6) 0.872(4) 0.050(16) Uiso 1 d . . . 
H32A H 0.163(11) 0.308(10) 0.621(6) 0.12(3) Uiso 1 d . . . 
H5 H 1.174(8) 1.012(7) 0.950(5) 0.08(2) Uiso 1 d . . . 
H33B H 0.104(9) 0.516(8) 0.745(5) 0.08(2) Uiso 1 d . . . 
H33C H 0.158(9) 0.678(9) 0.753(5) 0.09(2) Uiso 1 d . . . 
H32B H 0.243(15) 0.360(13) 0.523(11) 0.19(5) Uiso 1 d . . . 
H32C H 0.311(4) 0.362(4) 0.648(3) 0.000(9) Uiso 1 d . . . 
H1 H 0.552(6) 0.605(6) 0.625(4) 0.029(17) Uiso 1 d . . . 
H33A H 0.303(8) 0.569(7) 0.780(5) 0.071(19) Uiso 1 d . . . 
H3 H 0.994(11) 1.283(10) 0.751(7) 0.12(3) Uiso 1 d . . . 
H4 H 1.194(9) 1.239(8) 0.892(6) 0.10(2) Uiso 1 d . . . 
H2 H 0.787(10) 1.081(9) 0.679(7) 0.11(3) Uiso 1 d . . . 
H31 H 0.090(9) 0.547(7) 0.588(5) 0.08(2) Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
P1 0.0372(7) 0.0668(9) 0.0524(8) 0.0221(7) -0.0011(6) 0.0123(6) 
P2 0.0444(8) 0.0734(10) 0.0438(8) 0.0351(7) -0.0023(6) -0.0160(7) 
S1 0.0572(10) 0.1319(17) 0.0553(9) 0.0287(10) -0.0006(7) 0.0317(10) 
S2 0.0928(13) 0.0935(13) 0.0660(10) 0.0035(9) 0.0316(9) -0.0503(11) 
N1 0.036(2) 0.063(3) 0.048(3) 0.027(2) 0.005(2) 0.002(2) 
O2 0.053(2) 0.100(3) 0.078(3) 0.060(3) -0.022(2) -0.007(2) 
O1 0.044(2) 0.098(3) 0.043(2) 0.037(2) -0.0029(16) -0.025(2) 
C31 0.032(3) 0.082(5) 0.073(4) -0.001(3) 0.008(3) -0.010(3) 
C32 0.137(9) 0.059(5) 0.132(9) 0.003(5) 0.057(8) -0.032(5) 
C6 0.053(3) 0.077(4) 0.042(3) 0.012(3) 0.000(2) -0.002(3) 
C4 0.058(4) 0.109(6) 0.081(5) 0.006(4) 0.023(4) -0.037(4) 
C33 0.063(4) 0.062(4) 0.078(5) 0.014(3) 0.024(4) 0.001(3) 
C3 0.087(5) 0.136(8) 0.102(6) 0.055(6) 0.001(5) -0.063(5) 
C1 0.039(3) 0.098(5) 0.041(3) 0.025(3) 0.003(2) -0.025(3) 
C23 0.148(9) 0.178(10) 0.145(9) 0.071(8) 0.025(7) 0.131(9) 
C5 0.050(4) 0.114(6) 0.043(3) -0.007(4) -0.004(3) 0.003(4) 
C22 0.185(11) 0.089(6) 0.136(8) 0.081(6) -0.007(7) 0.012(6) 
C21 0.111(6) 0.080(5) 0.089(5) 0.045(4) 0.004(4) 0.050(4) 
C2 0.076(5) 0.156(8) 0.090(5) 0.082(6) -0.020(4) -0.067(5) 
C7 0.100(16) 0.021(7) 0.055(9) 0.022(6) 0.018(11) 0.024(10) 
C8 0.037(7) 0.16(2) 0.096(12) 0.099(14) 0.042(8) 0.064(11) 
C9 0.063(11) 0.124(14) 0.126(15) 0.093(12) 0.057(11) 0.069(10) 
C10 0.079(9) 0.082(8) 0.053(7) 0.042(6) 0.025(6) 0.024(7) 
C11 0.089(9) 0.062(7) 0.044(6) 0.020(5) 0.012(5) 0.019(6) 
C12 0.076(7) 0.055(6) 0.041(5) 0.019(5) 0.013(5) 0.020(5) 
C7 0.093(15) 0.09(2) 0.041(9) 0.039(12) 0.045(9) 0.077(14) 
C8 0.092(16) 0.073(13) 0.048(8) 0.016(8) 0.028(9) 0.026(10) 
C9 0.056(11) 0.061(10) 0.093(12) 0.038(9) 0.008(9) 0.006(8) 
C10 0.061(9) 0.046(7) 0.047(7) 0.019(6) 0.020(7) 0.015(6) 
C11 0.087(9) 0.044(7) 0.046(6) 0.012(5) 0.030(6) 0.004(6) 
C12 0.063(7) 0.047(7) 0.048(6) 0.019(5) 0.017(5) -0.003(5) 

_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 
P1 N1 1.686(5) . ? 
P1 C21 1.789(7) . ? 
P1 C31 1.800(6) . ? 
P1 S1 1.942(2) . ? 
P2 O2 1.584(4) . ? 
P2 O1 1.585(3) . ? 
P2 N1 1.636(5) . ? 
P2 S2 1.877(3) . ? 
O2 C7 1.41(2) . ? 
O2 C7 1.43(3) . ? 
O1 C1 1.401(6) . ? 
C31 C32 1.451(11) . ? 
C31 C33 1.496(9) . ? 
C6 C1 1.362(7) . ? 
C6 C5 1.388(9) . ? 
C4 C5 1.349(11) . ? 
C4 C3 1.358(11) . ? 
C3 C2 1.373(10) . ? 
C1 C2 1.366(10) . ? 
C23 C21 1.528(11) . ? 
C22 C21 1.552(12) . ? 
C7 C8 1.21(3) . ? 
C7 C12 1.63(3) . ? 
C8 C9 1.45(2) . ? 
C9 C10 1.49(3) . ? 
C10 C11 1.389(18) . ? 
C11 C12 1.373(14) . ? 
C7 C8 1.09(4) . ? 
C7 C12 1.83(2) . ? 
C8 C9 1.36(2) . ? 
C9 C10 1.30(2) . ? 
C10 C11 1.360(17) . ? 
C11 C12 1.385(15) . ? 

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 
N1 P1 C21 107.8(3) . . ? 
N1 P1 C31 106.5(3) . . ? 
C21 P1 C31 109.4(4) . . ? 
N1 P1 S1 111.2(2) . . ? 
C21 P1 S1 110.2(3) . . ? 
C31 P1 S1 111.7(2) . . ? 
O2 P2 O1 98.8(2) . . ? 
O2 P2 N1 104.1(3) . . ? 
O1 P2 N1 101.7(2) . . ? 
O2 P2 S2 116.2(2) . . ? 
O1 P2 S2 116.0(2) . . ? 
N1 P2 S2 117.5(2) . . ? 
P2 N1 P1 136.5(4) . . ? 
C7 O2 C7 20.2(11) . . ? 
C7 O2 P2 115.2(10) . . ? 
C7 O2 P2 134.8(10) . . ? 
C1 O1 P2 124.7(3) . . ? 
C32 C31 C33 114.9(8) . . ? 
C32 C31 P1 110.0(5) . . ? 
C33 C31 P1 114.0(5) . . ? 
C1 C6 C5 118.0(7) . . ? 
C5 C4 C3 119.2(7) . . ? 
C4 C3 C2 120.5(8) . . ? 
C6 C1 C2 120.9(6) . . ? 
C6 C1 O1 122.2(6) . . ? 
C2 C1 O1 116.8(5) . . ? 
C4 C5 C6 121.8(7) . . ? 
C23 C21 C22 111.2(7) . . ? 
C23 C21 P1 109.3(7) . . ? 
C22 C21 P1 110.9(7) . . ? 
C1 C2 C3 119.6(7) . . ? 
C8 C7 O2 123.2(19) . . ? 
C8 C7 C12 116.9(15) . . ? 
O2 C7 C12 98.2(16) . . ? 
C7 C8 C9 124(2) . . ? 
C8 C9 C10 110.2(17) . . ? 
C11 C10 C9 125.2(11) . . ? 
C12 C11 C10 119.5(11) . . ? 
C11 C12 C7 112.5(13) . . ? 
C8 C7 O2 129(2) . . ? 
C8 C7 C12 104(2) . . ? 
O2 C7 C12 108.3(15) . . ? 
C7 C8 C9 128.2(19) . . ? 
C10 C9 C8 127.7(19) . . ? 
C9 C10 C11 114.1(14) . . ? 
C10 C11 C12 122.7(12) . . ? 
C11 C12 C7 112.5(14) . . ? 

_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    1.128 
_refine_diff_density_min   -0.933 
_refine_diff_density_rms    0.086 

data_9.cif
#data_man68d 
_database_code_CSD                153019
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'Ph2P(S)-NH-P(S)iPr2'
_chemical_formula_sum 
'C18 H25 N P2 S2' 
_chemical_formula_weight          381.45 

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' 
'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            Orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x+1/2, -y, z+1/2' 
'-x, y+1/2, -z+1/2' 
'x+1/2, -y+1/2, -z' 

_cell_length_a                    10.154(2) 
_cell_length_b                    17.574(4) 
_cell_length_c                    22.213(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3963.8(14) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.278 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1616 
_exptl_absorpt_coefficient_mu     0.429 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3332 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0291 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        0 
_diffrn_reflns_theta_min          2.96 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              3332 
_reflns_number_gt                 3096 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0498P)^2^+0.7138P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.29(8) 
_refine_ls_number_reflns          3332 
_refine_ls_number_parameters      431 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0324 
_refine_ls_R_factor_gt            0.0275 
_refine_ls_wR_factor_ref          0.0763 
_refine_ls_wR_factor_gt           0.0737 
_refine_ls_goodness_of_fit_ref    1.050 
_refine_ls_restrained_S_all       1.050 
_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_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
P1 P 0.47181(9) 0.02248(4) 1.09100(4) 0.0174(2) Uani 1 d . . . 
P2 P 0.57875(9) -0.12702(4) 1.03516(3) 0.0168(2) Uani 1 d . . . 
P3 P 0.55525(8) -0.06472(5) 0.78216(3) 0.0175(2) Uani 1 d . . . 
P4 P 0.67066(9) 0.06808(4) 0.85439(3) 0.01676(19) Uani 1 d . . . 
S1 S 0.46032(10) -0.01303(5) 1.17327(3) 0.0271(2) Uani 1 d . . . 
S2 S 0.60561(10) -0.15118(4) 0.94997(3) 0.0249(2) Uani 1 d . . . 
S3 S 0.57696(9) -0.00596(5) 0.70882(3) 0.0262(2) Uani 1 d . . . 
S4 S 0.69986(9) 0.08370(5) 0.94050(3) 0.0226(2) Uani 1 d . . . 
N1 N 0.5589(3) -0.03261(14) 1.04411(12) 0.0186(6) Uani 1 d . . . 
H1 H 0.593(3) -0.0114(18) 1.0142(15) 0.012(8) Uiso 1 d . . . 
N2 N 0.6052(3) -0.01863(15) 0.84372(11) 0.0177(6) Uani 1 d . . . 
H2 H 0.598(4) -0.045(2) 0.8748(18) 0.032(11) Uiso 1 d . . . 
C1 C 0.5562(4) 0.11199(17) 1.08221(13) 0.0199(7) Uani 1 d . . . 
C2 C 0.6892(4) 0.1151(2) 1.09559(16) 0.0292(9) Uani 1 d . . . 
H2A H 0.7320 0.0719 1.1098 0.035 Uiso 1 calc R . . 
C3 C 0.7583(4) 0.1818(2) 1.08796(18) 0.0375(10) Uani 1 d . . . 
H3 H 0.8477 0.1835 1.0970 0.045 Uiso 1 calc R . . 
C4 C 0.6958(5) 0.2453(2) 1.06719(17) 0.0390(10) Uani 1 d . . . 
H4 H 0.7432 0.2900 1.0612 0.047 Uiso 1 calc R . . 
C5 C 0.5628(5) 0.2436(2) 1.05511(18) 0.0386(10) Uani 1 d . . . 
H5 H 0.5200 0.2874 1.0419 0.046 Uiso 1 calc R . . 
C6 C 0.4932(4) 0.17714(19) 1.06257(16) 0.0293(9) Uani 1 d . . . 
H6 H 0.4034 0.1760 1.0544 0.035 Uiso 1 calc R . . 
C7 C 0.3124(4) 0.03620(17) 1.05627(14) 0.0191(7) Uani 1 d . . . 
C8 C 0.3038(4) 0.04367(18) 0.99404(14) 0.0227(8) Uani 1 d . . . 
H8 H 0.3799 0.0428 0.9708 0.027 Uiso 1 calc R . . 
C9 C 0.1828(3) 0.05238(18) 0.96663(15) 0.0234(8) Uani 1 d . . . 
H9 H 0.1775 0.0568 0.9250 0.028 Uiso 1 calc R . . 
C10 C 0.0695(4) 0.05453(19) 1.00118(16) 0.0277(8) Uani 1 d . . . 
H10 H -0.0122 0.0602 0.9828 0.033 Uiso 1 calc R . . 
C11 C 0.0783(4) 0.0481(2) 1.06336(16) 0.0311(9) Uani 1 d . . . 
H11 H 0.0025 0.0505 1.0868 0.037 Uiso 1 calc R . . 
C12 C 0.1986(4) 0.03825(19) 1.09028(15) 0.0254(8) Uani 1 d . . . 
H12 H 0.2036 0.0329 1.1319 0.030 Uiso 1 calc R . . 
C13 C 0.7244(4) -0.15557(19) 1.07830(15) 0.0258(8) Uani 1 d . . . 
H13 H 0.7450 -0.2079 1.0665 0.031 Uiso 1 calc R . . 
C14 C 0.8421(4) -0.1067(2) 1.05985(17) 0.0362(9) Uani 1 d . . . 
H14A H 0.8314 -0.0562 1.0756 0.054 Uiso 1 calc R . . 
H14B H 0.8474 -0.1046 1.0167 0.054 Uiso 1 calc R . . 
H14C H 0.9215 -0.1286 1.0756 0.054 Uiso 1 calc R . . 
C15 C 0.7070(4) -0.1558(2) 1.14632(15) 0.0334(9) Uani 1 d . . . 
H15A H 0.7846 -0.1763 1.1649 0.050 Uiso 1 calc R . . 
H15B H 0.6323 -0.1865 1.1568 0.050 Uiso 1 calc R . . 
H15C H 0.6933 -0.1047 1.1602 0.050 Uiso 1 calc R . . 
C16 C 0.4354(4) -0.17557(18) 1.06596(15) 0.0241(8) Uani 1 d . . . 
H16 H 0.4216 -0.1581 1.1074 0.029 Uiso 1 calc R . . 
C17 C 0.3113(4) -0.1591(2) 1.02963(19) 0.0357(9) Uani 1 d . . . 
H17A H 0.3250 -0.1738 0.9885 0.054 Uiso 1 calc R . . 
H17B H 0.2917 -0.1057 1.0315 0.054 Uiso 1 calc R . . 
H17C H 0.2389 -0.1875 1.0460 0.054 Uiso 1 calc R . . 
C18 C 0.4635(4) -0.26111(19) 1.06696(17) 0.0354(9) Uani 1 d . . . 
H18A H 0.3891 -0.2875 1.0835 0.053 Uiso 1 calc R . . 
H18B H 0.5397 -0.2708 1.0914 0.053 Uiso 1 calc R . . 
H18C H 0.4794 -0.2787 1.0267 0.053 Uiso 1 calc R . . 
C19 C 0.3862(3) -0.09188(17) 0.79597(14) 0.0181(7) Uani 1 d . . . 
C20 C 0.3275(3) -0.08731(18) 0.85200(14) 0.0215(7) Uani 1 d . . . 
H20 H 0.3747 -0.0685 0.8847 0.026 Uiso 1 calc R . . 
C21 C 0.1994(4) -0.11058(19) 0.85935(15) 0.0253(8) Uani 1 d . . . 
H21 H 0.1599 -0.1072 0.8970 0.030 Uiso 1 calc R . . 
C22 C 0.1292(4) -0.13881(18) 0.81142(15) 0.0241(8) Uani 1 d . . . 
H22 H 0.0425 -0.1545 0.8167 0.029 Uiso 1 calc R . . 
C23 C 0.1870(4) -0.14389(18) 0.75584(15) 0.0242(8) Uani 1 d . . . 
H23 H 0.1394 -0.1631 0.7235 0.029 Uiso 1 calc R . . 
C24 C 0.3154(4) -0.12064(17) 0.74771(14) 0.0216(8) Uani 1 d . . . 
H24 H 0.3544 -0.1242 0.7100 0.026 Uiso 1 calc R . . 
C25 C 0.6436(3) -0.15422(19) 0.78175(14) 0.0202(7) Uani 1 d . . . 
C26 C 0.5944(4) -0.21798(19) 0.81027(14) 0.0249(8) Uani 1 d . . . 
H26 H 0.5136 -0.2156 0.8299 0.030 Uiso 1 calc R . . 
C27 C 0.6643(4) -0.2850(2) 0.80982(15) 0.0336(9) Uani 1 d . . . 
H27 H 0.6313 -0.3274 0.8298 0.040 Uiso 1 calc R . . 
C28 C 0.7825(4) -0.2897(2) 0.78007(17) 0.0344(9) Uani 1 d . . . 
H28 H 0.8293 -0.3351 0.7798 0.041 Uiso 1 calc R . . 
C29 C 0.8316(4) -0.2269(2) 0.75060(17) 0.0348(9) Uani 1 d . . . 
H29 H 0.9114 -0.2303 0.7302 0.042 Uiso 1 calc R . . 
C30 C 0.7630(4) -0.1584(2) 0.75099(16) 0.0283(9) Uani 1 d . . . 
H30 H 0.7963 -0.1161 0.7310 0.034 Uiso 1 calc R . . 
C31 C 0.5572(4) 0.13845(18) 0.82245(16) 0.0261(8) Uani 1 d . . . 
H31 H 0.5702 0.1399 0.7787 0.031 Uiso 1 calc R . . 
C32 C 0.5850(5) 0.2177(2) 0.8478(2) 0.0451(11) Uani 1 d . . . 
H32A H 0.5296 0.2543 0.8280 0.068 Uiso 1 calc R . . 
H32B H 0.6757 0.2305 0.8410 0.068 Uiso 1 calc R . . 
H32C H 0.5672 0.2181 0.8902 0.068 Uiso 1 calc R . . 
C33 C 0.4148(4) 0.1166(2) 0.83502(17) 0.0337(9) Uani 1 d . . . 
H33A H 0.4030 0.1092 0.8775 0.051 Uiso 1 calc R . . 
H33B H 0.3941 0.0703 0.8141 0.051 Uiso 1 calc R . . 
H33C H 0.3576 0.1565 0.8214 0.051 Uiso 1 calc R . . 
C34 C 0.8230(3) 0.06829(18) 0.81072(13) 0.0203(7) Uani 1 d . . . 
H34 H 0.8009 0.0530 0.7695 0.024 Uiso 1 calc R . . 
C35 C 0.8883(4) 0.1459(2) 0.80750(19) 0.0387(10) Uani 1 d . . . 
H35A H 0.9016 0.1651 0.8475 0.058 Uiso 1 calc R . . 
H35B H 0.8329 0.1803 0.7854 0.058 Uiso 1 calc R . . 
H35C H 0.9718 0.1414 0.7875 0.058 Uiso 1 calc R . . 
C36 C 0.9166(4) 0.0088(2) 0.83614(16) 0.0322(9) Uani 1 d . . . 
H36A H 0.9941 0.0062 0.8114 0.048 Uiso 1 calc R . . 
H36B H 0.8738 -0.0399 0.8366 0.048 Uiso 1 calc R . . 
H36C H 0.9411 0.0226 0.8764 0.048 Uiso 1 calc R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
P1 0.0231(5) 0.0146(4) 0.0146(4) -0.0005(3) 0.0009(4) 0.0021(4) 
P2 0.0210(5) 0.0133(4) 0.0160(4) -0.0011(3) -0.0025(4) 0.0016(4) 
P3 0.0166(5) 0.0229(4) 0.0130(3) -0.0003(3) 0.0002(4) 0.0004(4) 
P4 0.0183(5) 0.0166(4) 0.0153(4) 0.0010(3) 0.0033(4) 0.0005(4) 
S1 0.0388(6) 0.0269(4) 0.0155(4) 0.0029(3) 0.0018(4) 0.0048(4) 
S2 0.0392(6) 0.0198(4) 0.0156(4) -0.0024(3) 0.0003(4) 0.0065(4) 
S3 0.0265(5) 0.0378(5) 0.0143(4) 0.0059(3) 0.0004(4) -0.0034(4) 
S4 0.0283(5) 0.0225(4) 0.0169(4) -0.0025(3) 0.0028(4) -0.0054(4) 
N1 0.0232(16) 0.0145(12) 0.0179(13) 0.0022(10) 0.0035(13) -0.0042(13) 
N2 0.0209(16) 0.0220(13) 0.0100(12) 0.0038(11) -0.0019(12) -0.0004(13) 
C1 0.029(2) 0.0175(15) 0.0129(14) -0.0039(12) 0.0006(16) 0.0006(16) 
C2 0.035(2) 0.0233(17) 0.0294(18) -0.0039(15) -0.0074(18) 0.0006(18) 
C3 0.039(3) 0.033(2) 0.040(2) -0.0081(17) -0.008(2) -0.011(2) 
C4 0.054(3) 0.0238(19) 0.039(2) -0.0043(16) -0.001(2) -0.016(2) 
C5 0.055(3) 0.0153(16) 0.046(2) 0.0031(16) -0.004(2) -0.001(2) 
C6 0.035(2) 0.0201(17) 0.0330(18) -0.0034(14) -0.0008(19) 0.0029(17) 
C7 0.0215(18) 0.0151(14) 0.0208(16) 0.0001(12) 0.0013(16) 0.0014(15) 
C8 0.0199(19) 0.0259(17) 0.0223(16) 0.0042(14) 0.0060(16) 0.0037(16) 
C9 0.0229(19) 0.0257(16) 0.0215(16) 0.0012(14) -0.0004(16) 0.0013(17) 
C10 0.023(2) 0.0282(17) 0.0320(18) 0.0014(15) -0.0036(17) -0.0019(18) 
C11 0.024(2) 0.038(2) 0.0315(18) -0.0009(16) 0.0085(18) -0.0007(18) 
C12 0.030(2) 0.0284(17) 0.0179(16) -0.0016(14) 0.0050(16) -0.0015(17) 
C13 0.029(2) 0.0210(16) 0.0271(18) -0.0060(14) -0.0102(17) 0.0052(17) 
C14 0.025(2) 0.045(2) 0.039(2) -0.0131(18) -0.0035(19) 0.0037(19) 
C15 0.039(2) 0.0312(18) 0.0303(18) -0.0029(16) -0.017(2) 0.0035(19) 
C16 0.031(2) 0.0204(16) 0.0207(16) -0.0017(13) -0.0023(16) -0.0041(17) 
C17 0.026(2) 0.0210(17) 0.060(3) -0.0009(18) -0.005(2) -0.0028(17) 
C18 0.047(2) 0.0210(17) 0.039(2) 0.0046(15) -0.013(2) -0.0084(19) 
C19 0.0147(17) 0.0177(15) 0.0219(15) 0.0030(12) -0.0021(14) 0.0022(15) 
C20 0.0200(19) 0.0262(16) 0.0183(15) -0.0018(13) -0.0031(15) -0.0002(17) 
C21 0.022(2) 0.0281(17) 0.0256(17) 0.0013(14) 0.0050(17) -0.0016(17) 
C22 0.0142(18) 0.0217(16) 0.0363(19) 0.0074(15) -0.0040(16) -0.0022(16) 
C23 0.027(2) 0.0205(16) 0.0249(17) 0.0020(14) -0.0109(17) -0.0032(17) 
C24 0.027(2) 0.0178(15) 0.0196(15) -0.0013(13) -0.0047(16) 0.0039(17) 
C25 0.0198(19) 0.0272(17) 0.0137(14) -0.0066(13) -0.0041(15) 0.0041(16) 
C26 0.0226(19) 0.0317(18) 0.0203(16) -0.0033(14) 0.0004(16) 0.0027(17) 
C27 0.044(3) 0.0303(19) 0.0267(19) -0.0046(15) -0.005(2) 0.007(2) 
C28 0.031(2) 0.039(2) 0.0333(19) -0.0149(17) -0.013(2) 0.015(2) 
C29 0.0151(19) 0.046(2) 0.044(2) -0.0229(19) -0.0024(18) 0.005(2) 
C30 0.022(2) 0.0336(19) 0.0295(18) -0.0122(16) -0.0039(17) -0.0022(18) 
C31 0.031(2) 0.0222(16) 0.0248(16) 0.0090(14) 0.0065(17) 0.0068(18) 
C32 0.051(3) 0.0229(18) 0.061(3) 0.0061(18) 0.012(3) 0.012(2) 
C33 0.027(2) 0.0381(19) 0.0362(19) 0.0142(17) 0.0068(18) 0.0129(19) 
C34 0.0171(18) 0.0250(16) 0.0188(16) -0.0011(13) 0.0050(15) -0.0001(16) 
C35 0.031(2) 0.035(2) 0.050(2) -0.0025(19) 0.017(2) -0.011(2) 
C36 0.020(2) 0.049(2) 0.0275(18) -0.0012(17) 0.0009(17) 0.005(2) 

_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 
P1 N1 1.674(3) . ? 
P1 C1 1.802(3) . ? 
P1 C7 1.809(4) . ? 
P1 S1 1.9348(11) . ? 
P2 N1 1.683(3) . ? 
P2 C16 1.821(4) . ? 
P2 C13 1.832(4) . ? 
P2 S2 1.9585(11) . ? 
P3 N2 1.668(3) . ? 
P3 C19 1.808(3) . ? 
P3 C25 1.811(3) . ? 
P3 S3 1.9412(11) . ? 
P4 N2 1.679(3) . ? 
P4 C34 1.826(3) . ? 
P4 C31 1.833(3) . ? 
P4 S4 1.9550(11) . ? 
C1 C6 1.382(5) . ? 
C1 C2 1.383(5) . ? 
C2 C3 1.376(5) . ? 
C3 C4 1.365(6) . ? 
C4 C5 1.377(7) . ? 
C5 C6 1.375(5) . ? 
C7 C12 1.381(5) . ? 
C7 C8 1.391(4) . ? 
C8 C9 1.379(5) . ? 
C9 C10 1.384(5) . ? 
C10 C11 1.389(5) . ? 
C11 C12 1.371(6) . ? 
C13 C15 1.521(5) . ? 
C13 C14 1.528(5) . ? 
C16 C17 1.524(5) . ? 
C16 C18 1.531(5) . ? 
C19 C20 1.382(5) . ? 
C19 C24 1.386(5) . ? 
C20 C21 1.373(5) . ? 
C21 C22 1.374(5) . ? 
C22 C23 1.370(5) . ? 
C23 C24 1.378(5) . ? 
C25 C26 1.381(5) . ? 
C25 C30 1.394(5) . ? 
C26 C27 1.375(5) . ? 
C27 C28 1.373(6) . ? 
C28 C29 1.377(6) . ? 
C29 C30 1.390(5) . ? 
C31 C33 1.521(6) . ? 
C31 C32 1.529(5) . ? 
C34 C35 1.519(5) . ? 
C34 C36 1.522(5) . ? 

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 
N1 P1 C1 100.73(14) . . ? 
N1 P1 C7 106.51(14) . . ? 
C1 P1 C7 105.24(15) . . ? 
N1 P1 S1 115.65(10) . . ? 
C1 P1 S1 114.37(10) . . ? 
C7 P1 S1 113.07(11) . . ? 
N1 P2 C16 108.76(16) . . ? 
N1 P2 C13 107.75(15) . . ? 
C16 P2 C13 108.69(16) . . ? 
N1 P2 S2 110.16(10) . . ? 
C16 P2 S2 111.89(11) . . ? 
C13 P2 S2 109.48(12) . . ? 
N2 P3 C19 106.13(15) . . ? 
N2 P3 C25 105.97(14) . . ? 
C19 P3 C25 104.00(15) . . ? 
N2 P3 S3 113.26(10) . . ? 
C19 P3 S3 112.99(11) . . ? 
C25 P3 S3 113.68(11) . . ? 
N2 P4 C34 105.19(14) . . ? 
N2 P4 C31 107.99(16) . . ? 
C34 P4 C31 109.00(15) . . ? 
N2 P4 S4 109.00(10) . . ? 
C34 P4 S4 113.02(11) . . ? 
C31 P4 S4 112.29(12) . . ? 
P1 N1 P2 134.97(18) . . ? 
P3 N2 P4 132.58(16) . . ? 
C6 C1 C2 119.1(3) . . ? 
C6 C1 P1 122.5(3) . . ? 
C2 C1 P1 118.4(3) . . ? 
C3 C2 C1 120.3(4) . . ? 
C4 C3 C2 120.1(4) . . ? 
C3 C4 C5 120.3(4) . . ? 
C6 C5 C4 119.9(4) . . ? 
C5 C6 C1 120.2(4) . . ? 
C12 C7 C8 119.2(3) . . ? 
C12 C7 P1 121.3(2) . . ? 
C8 C7 P1 119.5(3) . . ? 
C9 C8 C7 120.4(3) . . ? 
C8 C9 C10 119.9(3) . . ? 
C9 C10 C11 119.8(4) . . ? 
C12 C11 C10 120.1(4) . . ? 
C11 C12 C7 120.7(3) . . ? 
C15 C13 C14 111.0(3) . . ? 
C15 C13 P2 115.3(3) . . ? 
C14 C13 P2 109.7(2) . . ? 
C17 C16 C18 110.4(3) . . ? 
C17 C16 P2 111.9(2) . . ? 
C18 C16 P2 108.4(3) . . ? 
C20 C19 C24 119.6(3) . . ? 
C20 C19 P3 123.1(3) . . ? 
C24 C19 P3 117.2(3) . . ? 
C21 C20 C19 119.9(3) . . ? 
C20 C21 C22 120.5(3) . . ? 
C23 C22 C21 120.0(3) . . ? 
C22 C23 C24 120.3(3) . . ? 
C23 C24 C19 119.8(3) . . ? 
C26 C25 C30 119.8(3) . . ? 
C26 C25 P3 121.6(3) . . ? 
C30 C25 P3 118.7(3) . . ? 
C27 C26 C25 120.3(3) . . ? 
C28 C27 C26 120.4(4) . . ? 
C27 C28 C29 119.9(3) . . ? 
C28 C29 C30 120.6(4) . . ? 
C29 C30 C25 119.0(4) . . ? 
C33 C31 C32 109.8(3) . . ? 
C33 C31 P4 110.8(2) . . ? 
C32 C31 P4 110.8(3) . . ? 
C35 C34 C36 111.2(3) . . ? 
C35 C34 P4 113.4(2) . . ? 
C36 C34 P4 109.3(2) . . ? 

loop_ 
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_distance_DH 
_geom_hbond_distance_HA 
_geom_hbond_distance_DA 
_geom_hbond_angle_DHA 
_geom_hbond_site_symmetry_A 
N1 H1 S4  0.84(3) 2.58(3) 3.395(3) 165(3) . 
N2 H2 S2  0.83(4) 2.51(4) 3.316(3) 164(3) . 

_diffrn_measured_fraction_theta_max    0.852 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.852 
_refine_diff_density_max    0.349 
_refine_diff_density_min   -0.239 
_refine_diff_density_rms    0.054 

data_10.cif
#data_m 
_database_code_CSD                153020
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'PhC(O)-NH-P(S)(OPh)2'
_chemical_formula_sum 
'C19 H16 N O3 P S' 
_chemical_formula_weight          369.36 

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' 

_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                    9.974(2) 
_cell_length_b                    13.675(3) 
_cell_length_c                    15.078(3) 
_cell_angle_alpha                 76.93(3) 
_cell_angle_beta                  70.93(3) 
_cell_angle_gamma                 68.82(3) 
_cell_volume                      1798.7(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.35
_exptl_crystal_size_mid           0.30
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.364 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              768 
_exptl_absorpt_coefficient_mu     0.286 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             12158 
_diffrn_reflns_av_R_equivalents   0.0219 
_diffrn_reflns_av_sigmaI/netI     0.0481 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          3.31 
_diffrn_reflns_theta_max          28.72 
_reflns_number_total              7912 
_reflns_number_gt                 5947 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0454P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7912 
_refine_ls_number_parameters      579 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0523 
_refine_ls_R_factor_gt            0.0334 
_refine_ls_wR_factor_ref          0.0817 
_refine_ls_wR_factor_gt           0.0780 
_refine_ls_goodness_of_fit_ref    0.963 
_refine_ls_restrained_S_all       0.963 
_refine_ls_shift/su_max           6.309 
_refine_ls_shift/su_mean          0.557 

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 
P2 P 0.13144(5) 0.29587(3) 0.85582(3) 0.01514(10) Uani 1 d . . . 
S2 S -0.02584(5) 0.41051(4) 0.91482(3) 0.02330(11) Uani 1 d . . . 
O6 O -0.00725(12) 0.32232(10) 0.70905(9) 0.0209(3) Uani 1 d . . . 
O4 O 0.28762(12) 0.26569(9) 0.87709(8) 0.0180(3) Uani 1 d . . . 
N2 N 0.20462(15) 0.30861(11) 0.73796(10) 0.0158(3) Uani 1 d . . . 
O5 O 0.10075(12) 0.18538(9) 0.87814(9) 0.0196(3) Uani 1 d . . . 
C20 C 0.29559(17) 0.23666(14) 0.97122(12) 0.0170(3) Uani 1 d . . . 
C32 C 0.20173(18) 0.33089(13) 0.57343(12) 0.0167(3) Uani 1 d . . . 
C38 C 0.12419(17) 0.31995(12) 0.67690(12) 0.0159(3) Uani 1 d . . . 
C27 C -0.1268(2) 0.15049(16) 0.90337(17) 0.0307(5) Uani 1 d . . . 
C26 C -0.03040(18) 0.16582(13) 0.94129(13) 0.0199(4) Uani 1 d . . . 
C25 C 0.2760(2) 0.31334(15) 1.02347(13) 0.0233(4) Uani 1 d . . . 
C23 C 0.3173(2) 0.17738(16) 1.15318(14) 0.0252(4) Uani 1 d . . . 
C31 C -0.0549(2) 0.15809(16) 1.03732(14) 0.0305(4) Uani 1 d . . . 
C24 C 0.2863(2) 0.28256(16) 1.11552(14) 0.0259(4) Uani 1 d . . . 
C33 C 0.35611(19) 0.30915(15) 0.53598(13) 0.0226(4) Uani 1 d . . . 
C37 C 0.1139(2) 0.36564(16) 0.51150(14) 0.0256(4) Uani 1 d . . . 
C36 C 0.1795(2) 0.38021(18) 0.41462(14) 0.0318(5) Uani 1 d . . . 
C34 C 0.4207(2) 0.32343(16) 0.43913(14) 0.0263(4) Uani 1 d . . . 
C22 C 0.3377(2) 0.10176(16) 1.09921(14) 0.0265(4) Uani 1 d . . . 
C35 C 0.3322(2) 0.35965(16) 0.37830(14) 0.0271(4) Uani 1 d . . . 
C21 C 0.32702(19) 0.13101(14) 1.00698(13) 0.0227(4) Uani 1 d . . . 
C29 C -0.2810(2) 0.11988(17) 1.06209(19) 0.0402(6) Uani 1 d . . . 
C28 C -0.2545(2) 0.12866(17) 0.9661(2) 0.0428(6) Uani 1 d . . . 
C30 C -0.1822(2) 0.13456(18) 1.09823(17) 0.0392(5) Uani 1 d . . . 
P1 P 0.19465(5) 0.83253(3) 0.36435(3) 0.01700(10) Uani 1 d . . . 
S1 S -0.01610(5) 0.89373(4) 0.38841(4) 0.02431(11) Uani 1 d . . . 
O3 O 0.49659(12) 0.68396(10) 0.30744(9) 0.0214(3) Uani 1 d . . . 
O2 O 0.29554(14) 0.90155(10) 0.29637(8) 0.0222(3) Uani 1 d . . . 
O1 O 0.25916(13) 0.80075(10) 0.45263(8) 0.0198(3) Uani 1 d . . . 
N1 N 0.25688(15) 0.72526(11) 0.30864(10) 0.0167(3) Uani 1 d . . . 
C19 C 0.40638(17) 0.66528(13) 0.28183(12) 0.0168(3) Uani 1 d . . . 
C17 C 0.4094(2) 0.49187(14) 0.11883(13) 0.0209(4) Uani 1 d . . . 
C1 C 0.19372(18) 0.74950(13) 0.53983(12) 0.0171(3) Uani 1 d . . . 
C6 C 0.1137(2) 0.80843(16) 0.61408(14) 0.0238(4) Uani 1 d . . . 
C14 C 0.59185(19) 0.50594(14) 0.21357(14) 0.0228(4) Uani 1 d . . . 
C13 C 0.44990(17) 0.58012(13) 0.22227(12) 0.0160(3) Uani 1 d . . . 
C15 C 0.6409(2) 0.42487(15) 0.15869(14) 0.0266(4) Uani 1 d . . . 
C8 C 0.2964(2) 1.02287(14) 0.39072(13) 0.0214(4) Uani 1 d . . . 
C11 C 0.6014(2) 0.98055(16) 0.30303(15) 0.0277(4) Uani 1 d . . . 
C9 C 0.3766(2) 1.07278(15) 0.41310(14) 0.0279(4) Uani 1 d . . . 
C18 C 0.35876(19) 0.57274(13) 0.17428(12) 0.0175(4) Uani 1 d . . . 
C7 C 0.37167(18) 0.95220(13) 0.32488(12) 0.0167(3) Uani 1 d . . . 
C2 C 0.2190(2) 0.64212(15) 0.55017(15) 0.0272(4) Uani 1 d . . . 
C3 C 0.1605(3) 0.59319(17) 0.63841(17) 0.0367(5) Uani 1 d . . . 
C12 C 0.52251(19) 0.93051(14) 0.27978(13) 0.0211(4) Uani 1 d . . . 
C16 C 0.5498(2) 0.41739(15) 0.11132(14) 0.0249(4) Uani 1 d . . . 
C5 C 0.0558(2) 0.75824(18) 0.70223(15) 0.0339(5) Uani 1 d . . . 
C4 C 0.0797(2) 0.6502(2) 0.71390(17) 0.0393(6) Uani 1 d . . . 
C10 C 0.5288(2) 1.05131(17) 0.36966(15) 0.0315(5) Uani 1 d . . . 
H16 H 0.581(2) 0.3603(19) 0.0732(17) 0.029(7) Uiso 1 d . . . 
H34 H 0.527(3) 0.3074(18) 0.4144(16) 0.028(7) Uiso 1 d . . . 
H14 H 0.652(3) 0.5088(18) 0.2472(17) 0.029(7) Uiso 1 d . . . 
H25 H 0.253(2) 0.3860(19) 0.9986(17) 0.032(7) Uiso 1 d . . . 
H12 H 0.567(3) 0.8823(19) 0.2344(17) 0.023(7) Uiso 1 d . . . 
H17 H 0.348(2) 0.4859(18) 0.0855(17) 0.026(7) Uiso 1 d . . . 
H33 H 0.417(3) 0.2838(18) 0.5743(17) 0.035(7) Uiso 1 d . . . 
H1N H 0.192(3) 0.7065(18) 0.3007(17) 0.042(7) Uiso 1 d . . . 
H18 H 0.260(3) 0.6252(18) 0.1769(16) 0.033(7) Uiso 1 d . . . 
H6 H 0.101(2) 0.879(2) 0.6034(17) 0.033(7) Uiso 1 d . . . 
H35 H 0.379(2) 0.3716(18) 0.3119(17) 0.027(7) Uiso 1 d . . . 
H22 H 0.357(3) 0.0307(19) 1.1262(17) 0.035(7) Uiso 1 d . . . 
H21 H 0.339(2) 0.0783(19) 0.9689(17) 0.036(7) Uiso 1 d . . . 
H9 H 0.335(2) 1.1215(19) 0.4554(17) 0.033(7) Uiso 1 d . . . 
H37 H 0.009(3) 0.3813(18) 0.5383(17) 0.035(7) Uiso 1 d . . . 
H8 H 0.192(3) 1.0337(18) 0.4215(17) 0.029(7) Uiso 1 d . . . 
H27 H -0.100(2) 0.1532(19) 0.8328(18) 0.046(7) Uiso 1 d . . . 
H11 H 0.705(3) 0.9669(18) 0.2733(16) 0.042(7) Uiso 1 d . . . 
H23 H 0.324(3) 0.1574(19) 1.2170(17) 0.036(7) Uiso 1 d . . . 
H2N H 0.288(3) 0.3125(19) 0.7179(17) 0.035(7) Uiso 1 d . . . 
H2 H 0.280(3) 0.6030(19) 0.4995(17) 0.044(7) Uiso 1 d . . . 
H15 H 0.742(3) 0.3738(18) 0.1522(16) 0.046(7) Uiso 1 d . . . 
H24 H 0.275(3) 0.3341(19) 1.1534(17) 0.038(7) Uiso 1 d . . . 
H31 H 0.017(2) 0.1663(18) 1.0629(16) 0.053(7) Uiso 1 d . . . 
H10 H 0.583(2) 1.0843(18) 0.3889(16) 0.043(7) Uiso 1 d . . . 
H36 H 0.122(3) 0.4047(19) 0.3699(17) 0.043(7) Uiso 1 d . . . 
H4 H 0.038(2) 0.6187(19) 0.7746(18) 0.050(7) Uiso 1 d . . . 
H30 H -0.199(3) 0.1263(18) 1.1710(18) 0.050(7) Uiso 1 d . . . 
H3 H 0.176(2) 0.5165(19) 0.6481(16) 0.057(7) Uiso 1 d . . . 
H29 H -0.369(3) 0.1034(19) 1.1054(17) 0.053(7) Uiso 1 d . . . 
H5 H 0.000(3) 0.8023(19) 0.7542(17) 0.043(7) Uiso 1 d . . . 
H28 H -0.322(3) 0.1174(18) 0.9381(17) 0.058(7) Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
P2 0.0124(2) 0.0172(2) 0.0161(2) -0.00294(17) -0.00334(17) -0.00477(17) 
S2 0.0185(2) 0.0219(2) 0.0262(3) -0.00927(19) -0.00365(19) -0.00087(17) 
O6 0.0140(6) 0.0288(7) 0.0232(7) -0.0070(5) -0.0049(5) -0.0085(5) 
O4 0.0145(6) 0.0251(6) 0.0157(6) -0.0016(5) -0.0055(5) -0.0069(5) 
N2 0.0106(7) 0.0213(7) 0.0165(8) -0.0023(6) -0.0036(6) -0.0062(6) 
O5 0.0163(6) 0.0193(6) 0.0220(7) -0.0038(5) 0.0001(5) -0.0081(5) 
C20 0.0104(8) 0.0253(9) 0.0149(9) -0.0012(7) -0.0030(6) -0.0063(7) 
C32 0.0166(8) 0.0173(8) 0.0195(9) -0.0032(7) -0.0056(7) -0.0079(7) 
C38 0.0138(8) 0.0132(8) 0.0221(9) -0.0037(7) -0.0066(7) -0.0036(6) 
C27 0.0351(11) 0.0254(10) 0.0392(13) 0.0058(9) -0.0188(10) -0.0160(9) 
C26 0.0124(8) 0.0172(8) 0.0279(10) -0.0017(7) -0.0016(7) -0.0060(7) 
C25 0.0266(10) 0.0223(10) 0.0243(10) -0.0007(8) -0.0086(8) -0.0112(8) 
C23 0.0218(9) 0.0362(11) 0.0192(10) 0.0012(8) -0.0076(8) -0.0119(8) 
C31 0.0273(10) 0.0384(12) 0.0275(11) -0.0028(9) -0.0022(8) -0.0175(9) 
C24 0.0299(10) 0.0326(11) 0.0204(10) -0.0054(8) -0.0068(8) -0.0143(9) 
C33 0.0169(9) 0.0342(10) 0.0206(10) -0.0067(8) -0.0067(8) -0.0092(8) 
C37 0.0191(9) 0.0363(11) 0.0227(10) -0.0003(8) -0.0084(8) -0.0096(8) 
C36 0.0290(11) 0.0462(13) 0.0222(11) 0.0051(9) -0.0138(9) -0.0135(9) 
C34 0.0202(10) 0.0394(11) 0.0232(10) -0.0075(9) -0.0026(8) -0.0143(8) 
C22 0.0266(10) 0.0231(10) 0.0275(11) 0.0045(8) -0.0112(8) -0.0061(8) 
C35 0.0315(11) 0.0343(11) 0.0177(10) -0.0002(8) -0.0052(8) -0.0159(9) 
C21 0.0213(9) 0.0227(9) 0.0242(10) -0.0041(8) -0.0080(8) -0.0045(7) 
C29 0.0199(10) 0.0278(11) 0.0615(17) 0.0034(11) 0.0028(10) -0.0118(9) 
C28 0.0298(11) 0.0323(12) 0.0748(19) 0.0096(12) -0.0260(12) -0.0186(10) 
C30 0.0354(12) 0.0411(13) 0.0340(13) -0.0043(10) 0.0081(10) -0.0194(10) 
P1 0.0172(2) 0.0200(2) 0.0158(2) -0.00520(18) -0.00329(18) -0.00738(17) 
S1 0.0176(2) 0.0243(2) 0.0291(3) -0.0112(2) -0.00379(19) -0.00186(18) 
O3 0.0139(6) 0.0334(7) 0.0217(7) -0.0081(6) -0.0040(5) -0.0107(5) 
O2 0.0292(7) 0.0288(7) 0.0159(6) -0.0024(5) -0.0060(5) -0.0176(6) 
O1 0.0210(6) 0.0284(7) 0.0144(6) -0.0019(5) -0.0038(5) -0.0139(5) 
N1 0.0115(7) 0.0210(7) 0.0204(8) -0.0064(6) -0.0049(6) -0.0055(6) 
C19 0.0135(8) 0.0222(9) 0.0160(9) -0.0011(7) -0.0037(7) -0.0079(7) 
C17 0.0225(9) 0.0223(9) 0.0199(9) -0.0028(7) -0.0082(8) -0.0067(7) 
C1 0.0148(8) 0.0208(9) 0.0185(9) 0.0006(7) -0.0071(7) -0.0080(7) 
C6 0.0216(9) 0.0219(10) 0.0230(10) -0.0022(8) -0.0057(8) -0.0020(7) 
C14 0.0167(9) 0.0261(10) 0.0268(10) -0.0044(8) -0.0079(8) -0.0057(7) 
C13 0.0136(8) 0.0185(8) 0.0156(9) -0.0011(7) -0.0029(7) -0.0065(6) 
C15 0.0187(9) 0.0258(10) 0.0307(11) -0.0070(8) -0.0057(8) -0.0003(8) 
C8 0.0213(9) 0.0238(9) 0.0188(10) -0.0042(7) -0.0017(8) -0.0092(8) 
C11 0.0194(9) 0.0304(11) 0.0329(12) 0.0028(9) -0.0067(8) -0.0115(8) 
C9 0.0388(11) 0.0259(10) 0.0233(11) -0.0057(8) -0.0063(9) -0.0152(9) 
C18 0.0148(8) 0.0198(9) 0.0171(9) -0.0025(7) -0.0039(7) -0.0046(7) 
C7 0.0204(8) 0.0167(8) 0.0157(9) 0.0011(7) -0.0064(7) -0.0092(7) 
C2 0.0315(10) 0.0201(9) 0.0371(12) -0.0035(9) -0.0195(9) -0.0070(8) 
C3 0.0474(13) 0.0279(11) 0.0498(15) 0.0149(10) -0.0350(12) -0.0212(10) 
C12 0.0214(9) 0.0178(9) 0.0198(10) -0.0024(7) -0.0016(7) -0.0045(7) 
C16 0.0282(10) 0.0219(9) 0.0226(10) -0.0072(8) -0.0055(8) -0.0041(8) 
C5 0.0228(10) 0.0493(13) 0.0232(11) -0.0016(10) -0.0041(8) -0.0074(9) 
C4 0.0341(12) 0.0565(15) 0.0332(13) 0.0239(11) -0.0202(10) -0.0288(11) 
C10 0.0375(12) 0.0365(11) 0.0327(12) 0.0003(9) -0.0142(9) -0.0239(10) 

_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 
P2 O4 1.5816(12) . ? 
P2 O5 1.5897(12) . ? 
P2 N2 1.6809(16) . ? 
P2 S2 1.9109(10) . ? 
O6 C38 1.2312(19) . ? 
O4 C20 1.405(2) . ? 
N2 C38 1.358(2) . ? 
O5 C26 1.419(2) . ? 
C20 C25 1.372(2) . ? 
C20 C21 1.381(2) . ? 
C32 C37 1.377(2) . ? 
C32 C33 1.398(2) . ? 
C32 C38 1.498(2) . ? 
C27 C26 1.361(3) . ? 
C27 C28 1.402(3) . ? 
C26 C31 1.373(3) . ? 
C25 C24 1.383(3) . ? 
C23 C22 1.376(3) . ? 
C23 C24 1.382(3) . ? 
C31 C30 1.400(3) . ? 
C33 C34 1.390(3) . ? 
C37 C36 1.393(3) . ? 
C36 C35 1.384(3) . ? 
C34 C35 1.369(3) . ? 
C22 C21 1.386(3) . ? 
C29 C30 1.360(3) . ? 
C29 C28 1.369(4) . ? 
P1 O1 1.5718(13) . ? 
P1 O2 1.5902(14) . ? 
P1 N1 1.6738(15) . ? 
P1 S1 1.9022(9) . ? 
O3 C19 1.2090(19) . ? 
O2 C7 1.4032(19) . ? 
O1 C1 1.414(2) . ? 
N1 C19 1.390(2) . ? 
C19 C13 1.485(2) . ? 
C17 C18 1.384(2) . ? 
C17 C16 1.389(3) . ? 
C1 C2 1.378(2) . ? 
C1 C6 1.378(3) . ? 
C6 C5 1.394(3) . ? 
C14 C15 1.382(3) . ? 
C14 C13 1.397(2) . ? 
C13 C18 1.374(2) . ? 
C15 C16 1.367(3) . ? 
C8 C9 1.377(3) . ? 
C8 C7 1.380(2) . ? 
C11 C12 1.374(3) . ? 
C11 C10 1.389(3) . ? 
C9 C10 1.390(3) . ? 
C7 C12 1.384(2) . ? 
C2 C3 1.389(3) . ? 
C3 C4 1.378(3) . ? 
C5 C4 1.388(3) . ? 

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 
O4 P2 O5 102.68(7) . . ? 
O4 P2 N2 93.56(7) . . ? 
O5 P2 N2 103.50(8) . . ? 
O4 P2 S2 116.96(5) . . ? 
O5 P2 S2 116.44(5) . . ? 
N2 P2 S2 120.08(6) . . ? 
C20 O4 P2 118.99(10) . . ? 
C38 N2 P2 122.19(12) . . ? 
C26 O5 P2 124.70(11) . . ? 
C25 C20 C21 122.35(17) . . ? 
C25 C20 O4 119.18(16) . . ? 
C21 C20 O4 118.45(16) . . ? 
C37 C32 C33 118.20(17) . . ? 
C37 C32 C38 117.32(15) . . ? 
C33 C32 C38 124.48(15) . . ? 
O6 C38 N2 118.79(16) . . ? 
O6 C38 C32 124.01(15) . . ? 
N2 C38 C32 117.19(14) . . ? 
C26 C27 C28 117.5(2) . . ? 
C27 C26 C31 121.61(18) . . ? 
C27 C26 O5 117.62(17) . . ? 
C31 C26 O5 120.71(16) . . ? 
C20 C25 C24 118.06(18) . . ? 
C22 C23 C24 120.14(18) . . ? 
C26 C31 C30 119.6(2) . . ? 
C25 C24 C23 120.78(19) . . ? 
C34 C33 C32 121.58(17) . . ? 
C32 C37 C36 119.84(18) . . ? 
C35 C36 C37 121.53(19) . . ? 
C35 C34 C33 119.74(18) . . ? 
C23 C22 C21 119.99(19) . . ? 
C34 C35 C36 119.10(19) . . ? 
C20 C21 C22 118.67(18) . . ? 
C30 C29 C28 119.3(2) . . ? 
C29 C28 C27 122.0(2) . . ? 
C29 C30 C31 119.9(2) . . ? 
O1 P1 O2 100.57(7) . . ? 
O1 P1 N1 107.37(8) . . ? 
O2 P1 N1 101.79(7) . . ? 
O1 P1 S1 116.42(6) . . ? 
O2 P1 S1 117.64(6) . . ? 
N1 P1 S1 111.45(6) . . ? 
C7 O2 P1 125.83(11) . . ? 
C1 O1 P1 123.50(10) . . ? 
C19 N1 P1 123.75(12) . . ? 
O3 C19 N1 119.26(15) . . ? 
O3 C19 C13 122.15(15) . . ? 
N1 C19 C13 118.59(14) . . ? 
C18 C17 C16 121.41(17) . . ? 
C2 C1 C6 121.95(18) . . ? 
C2 C1 O1 119.72(17) . . ? 
C6 C1 O1 118.20(15) . . ? 
C1 C6 C5 119.17(19) . . ? 
C15 C14 C13 121.11(17) . . ? 
C18 C13 C14 119.14(16) . . ? 
C18 C13 C19 123.10(15) . . ? 
C14 C13 C19 117.74(15) . . ? 
C16 C15 C14 119.68(17) . . ? 
C9 C8 C7 117.96(17) . . ? 
C12 C11 C10 119.80(18) . . ? 
C8 C9 C10 119.92(19) . . ? 
C13 C18 C17 119.32(16) . . ? 
C8 C7 C12 123.21(16) . . ? 
C8 C7 O2 120.85(15) . . ? 
C12 C7 O2 115.87(15) . . ? 
C1 C2 C3 118.2(2) . . ? 
C4 C3 C2 121.1(2) . . ? 
C11 C12 C7 118.21(17) . . ? 
C15 C16 C17 119.34(17) . . ? 
C4 C5 C6 119.7(2) . . ? 
C3 C4 C5 119.9(2) . . ? 
C11 C10 C9 120.87(18) . . ? 

loop_ 
_geom_hbond_atom_site_label_D 
_geom_hbond_atom_site_label_H 
_geom_hbond_atom_site_label_A 
_geom_hbond_distance_DH 
_geom_hbond_distance_HA 
_geom_hbond_distance_DA 
_geom_hbond_angle_DHA 
_geom_hbond_site_symmetry_A 
N1 H1N O6  0.83(2) 2.07(2) 2.8942(18) 172(2) 2_566 
N2 H2N O3  0.80(2) 2.08(2) 2.8661(19) 169(2) 2_666 

_diffrn_measured_fraction_theta_max    0.847 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.969 
_refine_diff_density_max    0.293 
_refine_diff_density_min   -0.327 
_refine_diff_density_rms    0.048 

data_11.cif
#data_j 
_database_code_CSD                153021
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          '[Ph2P(S)-N-P(O)(OPh)2]2Pd'
_chemical_formula_sum 
'C24 H20 N O3 P2 Pd0.50 S' 
_chemical_formula_weight          517.61 

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' 
'Pd'  'Pd'  -0.9988   1.0072 
'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)/n

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'-x+1/2, y+1/2, -z+1/2' 
'-x, -y, -z' 
'x-1/2, -y-1/2, z-1/2' 

_cell_length_a                    10.678(2) 
_cell_length_b                    9.294(2) 
_cell_length_c                    23.112(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.24(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2263.9(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.519 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1056 
_exptl_absorpt_coefficient_mu     0.696 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.8184 
_exptl_absorpt_correction_T_max   0.8734 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10385 
_diffrn_reflns_av_R_equivalents   0.0236 
_diffrn_reflns_av_sigmaI/netI     0.0282 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          3.46 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3913 
_reflns_number_gt                 3322 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0358P)^2^+0.8296P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3913 
_refine_ls_number_parameters      366 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0315 
_refine_ls_R_factor_gt            0.0249 
_refine_ls_wR_factor_ref          0.0650 
_refine_ls_wR_factor_gt           0.0638 
_refine_ls_goodness_of_fit_ref    1.065 
_refine_ls_restrained_S_all       1.065 
_refine_ls_shift/su_max           0.150 
_refine_ls_shift/su_mean          0.006 

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 
Pd1 Pd 0.5000 0.0000 0.0000 0.01117(8) Uani 1 d S . . 
P2 P 0.69327(5) 0.15083(6) 0.07458(2) 0.01359(13) Uani 1 d . . . 
S1 S 0.69706(5) 0.10396(6) -0.01067(2) 0.01804(14) Uani 1 d . . . 
P1 P 0.45309(5) 0.17431(6) 0.11826(2) 0.01471(14) Uani 1 d . . . 
O2 O 0.35072(13) 0.05673(16) 0.12885(6) 0.0161(3) Uani 1 d . . . 
O1 O 0.37010(14) 0.27005(16) 0.06975(7) 0.0189(3) Uani 1 d . . . 
C7 C 0.3831(2) -0.0454(2) 0.17409(10) 0.0148(5) Uani 1 d . . . 
C19 C 0.8099(2) 0.0491(2) 0.12292(10) 0.0155(5) Uani 1 d . . . 
N1 N 0.55056(16) 0.09453(18) 0.08150(7) 0.0139(4) Uani 1 d . . . 
C13 C 0.71773(19) 0.3394(2) 0.09170(10) 0.0156(5) Uani 1 d . . . 
C10 C 0.4356(2) -0.2507(3) 0.26030(11) 0.0236(5) Uani 1 d . . . 
H10 H 0.451(2) -0.315(3) 0.2894(11) 0.026(7) Uiso 1 d . . . 
O3 O 0.51152(15) 0.24853(17) 0.17181(7) 0.0227(4) Uani 1 d . . . 
C22 C 0.9866(2) -0.1178(3) 0.19526(11) 0.0252(6) Uani 1 d . . . 
H22 H 1.046(2) -0.173(3) 0.2195(10) 0.020(6) Uiso 1 d . . . 
C14 C 0.7859(2) 0.3851(3) 0.14515(11) 0.0195(5) Uani 1 d . . . 
H14 H 0.825(2) 0.320(3) 0.1715(11) 0.025(7) Uiso 1 d . . . 
C16 C 0.7397(2) 0.6309(3) 0.11778(11) 0.0243(6) Uani 1 d . . . 
H16 H 0.748(2) 0.724(3) 0.1252(11) 0.024(7) Uiso 1 d . . . 
C1 C 0.2731(2) 0.3635(2) 0.08102(10) 0.0200(5) Uani 1 d . . . 
C11 C 0.4896(2) -0.2605(3) 0.21024(11) 0.0252(6) Uani 1 d . . . 
H11 H 0.543(2) -0.337(3) 0.2047(11) 0.032(7) Uiso 1 d . . . 
C8 C 0.3288(2) -0.0338(3) 0.22432(11) 0.0226(5) Uani 1 d . . . 
H8 H 0.277(3) 0.045(3) 0.2276(11) 0.029(7) Uiso 1 d . . . 
C3 C 0.0538(3) 0.4216(4) 0.06738(13) 0.0369(7) Uani 1 d . . . 
H3 H -0.026(3) 0.397(3) 0.0513(12) 0.040(8) Uiso 1 d . . . 
C18 C 0.6606(2) 0.4412(3) 0.05120(11) 0.0214(5) Uani 1 d . . . 
H18 H 0.618(2) 0.410(2) 0.0170(10) 0.013(6) Uiso 1 d . . . 
C17 C 0.6718(2) 0.5864(3) 0.06480(12) 0.0260(6) Uani 1 d . . . 
H17 H 0.637(2) 0.645(3) 0.0380(12) 0.031(7) Uiso 1 d . . . 
C12 C 0.4628(2) -0.1583(3) 0.16620(10) 0.0206(5) Uani 1 d . . . 
H12 H 0.493(2) -0.167(2) 0.1301(10) 0.013(6) Uiso 1 d . . . 
C20 C 0.9227(2) 0.0067(2) 0.10373(11) 0.0208(5) Uani 1 d . . . 
H20 H 0.936(2) 0.034(2) 0.0640(11) 0.015(6) Uiso 1 d . . . 
C23 C 0.8750(2) -0.0764(3) 0.21412(11) 0.0229(5) Uani 1 d . . . 
H23 H 0.859(2) -0.107(2) 0.2496(11) 0.016(6) Uiso 1 d . . . 
C2 C 0.1490(2) 0.3237(3) 0.06124(12) 0.0284(6) Uani 1 d . . . 
H2 H 0.133(2) 0.239(3) 0.0453(11) 0.024(7) Uiso 1 d . . . 
C15 C 0.7969(2) 0.5307(3) 0.15792(11) 0.0240(6) Uani 1 d . . . 
H15 H 0.845(2) 0.567(3) 0.1927(11) 0.029(7) Uiso 1 d . . . 
C24 C 0.7867(2) 0.0078(2) 0.17845(10) 0.0192(5) Uani 1 d . . . 
H24 H 0.708(2) 0.031(2) 0.1911(10) 0.015(6) Uiso 1 d . . . 
C5 C 0.2074(3) 0.5909(3) 0.11265(14) 0.0354(7) Uani 1 d . . . 
H5 H 0.230(3) 0.693(4) 0.1293(13) 0.055(9) Uiso 1 d . . . 
C21 C 1.0106(2) -0.0749(3) 0.14070(12) 0.0271(6) Uani 1 d . . . 
H21 H 1.081(2) -0.094(2) 0.1289(10) 0.013(6) Uiso 1 d . . . 
C6 C 0.3042(2) 0.4952(3) 0.10673(12) 0.0256(6) Uani 1 d . . . 
H6 H 0.390(3) 0.518(3) 0.1200(12) 0.032(8) Uiso 1 d . . . 
C9 C 0.3560(2) -0.1381(3) 0.26773(11) 0.0269(6) Uani 1 d . . . 
H9 H 0.323(2) -0.131(3) 0.3023(12) 0.029(7) Uiso 1 d . . . 
C4 C 0.0833(3) 0.5549(3) 0.09283(14) 0.0369(7) Uani 1 d . . . 
H4 H 0.015(3) 0.618(3) 0.0950(13) 0.049(9) Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Pd1 0.01091(13) 0.01142(13) 0.01088(13) -0.00152(9) 0.00083(9) -0.00028(9) 
P2 0.0136(3) 0.0136(3) 0.0131(3) -0.0004(2) 0.0006(2) -0.0010(2) 
S1 0.0160(3) 0.0231(3) 0.0153(3) -0.0013(2) 0.0034(2) -0.0048(2) 
P1 0.0162(3) 0.0138(3) 0.0143(3) -0.0012(2) 0.0029(2) -0.0006(2) 
O2 0.0137(8) 0.0159(8) 0.0182(8) 0.0016(7) 0.0006(6) 0.0006(6) 
O1 0.0206(8) 0.0175(8) 0.0196(8) 0.0025(7) 0.0058(7) 0.0054(7) 
C7 0.0133(11) 0.0152(11) 0.0147(11) 0.0015(9) -0.0016(9) -0.0028(9) 
C19 0.0154(11) 0.0106(10) 0.0191(12) -0.0027(9) -0.0017(9) -0.0011(9) 
N1 0.0151(9) 0.0128(9) 0.0131(9) -0.0016(8) 0.0001(7) -0.0014(7) 
C13 0.0118(10) 0.0167(12) 0.0188(12) 0.0015(10) 0.0040(9) 0.0004(9) 
C10 0.0237(13) 0.0232(13) 0.0217(13) 0.0085(11) -0.0028(10) -0.0045(10) 
O3 0.0248(9) 0.0244(9) 0.0194(8) -0.0072(7) 0.0052(7) -0.0047(7) 
C22 0.0251(13) 0.0156(12) 0.0306(14) -0.0013(11) -0.0088(11) 0.0026(10) 
C14 0.0159(12) 0.0203(13) 0.0223(12) -0.0001(11) 0.0029(10) -0.0006(10) 
C16 0.0270(13) 0.0143(13) 0.0334(15) -0.0034(11) 0.0106(11) -0.0041(10) 
C1 0.0208(12) 0.0190(12) 0.0225(12) 0.0068(10) 0.0106(10) 0.0047(10) 
C11 0.0228(13) 0.0208(13) 0.0312(14) 0.0049(11) 0.0014(11) 0.0049(11) 
C8 0.0204(12) 0.0235(13) 0.0247(13) -0.0005(11) 0.0062(10) 0.0026(10) 
C3 0.0183(14) 0.056(2) 0.0372(16) 0.0093(15) 0.0066(12) 0.0000(14) 
C18 0.0225(12) 0.0192(12) 0.0206(13) 0.0010(11) -0.0017(10) -0.0020(10) 
C17 0.0298(14) 0.0187(13) 0.0294(14) 0.0095(12) 0.0044(12) 0.0043(11) 
C12 0.0216(12) 0.0229(13) 0.0180(12) 0.0000(11) 0.0054(10) 0.0000(10) 
C20 0.0196(12) 0.0187(12) 0.0235(13) -0.0047(11) 0.0013(10) -0.0008(10) 
C23 0.0273(13) 0.0194(13) 0.0192(13) 0.0047(11) -0.0047(11) -0.0040(10) 
C2 0.0260(14) 0.0288(15) 0.0311(15) 0.0011(13) 0.0066(11) -0.0050(12) 
C15 0.0209(12) 0.0256(14) 0.0248(13) -0.0061(11) 0.0018(11) -0.0050(10) 
C24 0.0194(12) 0.0176(12) 0.0194(12) -0.0023(10) -0.0007(10) -0.0002(10) 
C5 0.0323(15) 0.0209(14) 0.058(2) 0.0034(14) 0.0210(14) 0.0056(12) 
C21 0.0194(13) 0.0202(13) 0.0392(16) -0.0065(12) -0.0026(12) 0.0050(11) 
C6 0.0229(13) 0.0175(13) 0.0389(16) 0.0008(12) 0.0122(12) 0.0005(11) 
C9 0.0329(14) 0.0336(15) 0.0155(12) 0.0026(11) 0.0080(11) -0.0015(12) 
C4 0.0314(16) 0.0298(15) 0.0527(19) 0.0080(15) 0.0166(14) 0.0106(13) 

_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 
Pd1 N1 2.0699(17) . ? 
Pd1 N1 2.0699(17) 3_655 ? 
Pd1 S1 2.3641(7) . ? 
Pd1 S1 2.3641(7) 3_655 ? 
Pd1 P2 2.8378(9) . ? 
Pd1 P2 2.8378(9) 3_655 ? 
P2 N1 1.6431(18) . ? 
P2 C19 1.802(2) . ? 
P2 C13 1.806(2) . ? 
P2 S1 2.0246(9) . ? 
P1 O3 1.4659(16) . ? 
P1 O1 1.5858(16) . ? 
P1 O2 1.5922(16) . ? 
P1 N1 1.6245(18) . ? 
O2 C7 1.414(3) . ? 
O1 C1 1.408(3) . ? 
C7 C12 1.381(3) . ? 
C7 C8 1.383(3) . ? 
C19 C24 1.399(3) . ? 
C19 C20 1.405(3) . ? 
C13 C14 1.396(3) . ? 
C13 C18 1.400(3) . ? 
C10 C11 1.376(4) . ? 
C10 C9 1.376(4) . ? 
C22 C21 1.385(4) . ? 
C22 C23 1.387(4) . ? 
C14 C15 1.385(3) . ? 
C16 C17 1.383(4) . ? 
C16 C15 1.386(4) . ? 
C1 C6 1.378(3) . ? 
C1 C2 1.381(3) . ? 
C11 C12 1.388(3) . ? 
C8 C9 1.392(3) . ? 
C3 C4 1.385(4) . ? 
C3 C2 1.388(4) . ? 
C18 C17 1.386(4) . ? 
C20 C21 1.388(3) . ? 
C23 C24 1.391(3) . ? 
C5 C4 1.372(4) . ? 
C5 C6 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 
N1 Pd1 N1 180.0 . 3_655 ? 
N1 Pd1 S1 79.34(6) . . ? 
N1 Pd1 S1 100.66(6) 3_655 . ? 
N1 Pd1 S1 100.66(6) . 3_655 ? 
N1 Pd1 S1 79.34(6) 3_655 3_655 ? 
S1 Pd1 S1 180.0 . 3_655 ? 
N1 Pd1 P2 34.88(5) . . ? 
N1 Pd1 P2 145.12(5) 3_655 . ? 
S1 Pd1 P2 44.67(2) . . ? 
S1 Pd1 P2 135.33(2) 3_655 . ? 
N1 Pd1 P2 145.12(5) . 3_655 ? 
N1 Pd1 P2 34.88(5) 3_655 3_655 ? 
S1 Pd1 P2 135.33(2) . 3_655 ? 
S1 Pd1 P2 44.67(2) 3_655 3_655 ? 
P2 Pd1 P2 180.0 . 3_655 ? 
N1 P2 C19 109.39(10) . . ? 
N1 P2 C13 113.04(9) . . ? 
C19 P2 C13 108.18(10) . . ? 
N1 P2 S1 100.95(7) . . ? 
C19 P2 S1 111.76(8) . . ? 
C13 P2 S1 113.40(8) . . ? 
N1 P2 Pd1 46.08(6) . . ? 
C19 P2 Pd1 118.70(7) . . ? 
C13 P2 Pd1 132.67(7) . . ? 
S1 P2 Pd1 55.17(3) . . ? 
P2 S1 Pd1 80.17(4) . . ? 
O3 P1 O1 116.53(9) . . ? 
O3 P1 O2 113.76(9) . . ? 
O1 P1 O2 100.04(8) . . ? 
O3 P1 N1 115.77(9) . . ? 
O1 P1 N1 102.63(9) . . ? 
O2 P1 N1 106.29(9) . . ? 
C7 O2 P1 118.85(13) . . ? 
C1 O1 P1 124.03(14) . . ? 
C12 C7 C8 121.4(2) . . ? 
C12 C7 O2 119.7(2) . . ? 
C8 C7 O2 118.9(2) . . ? 
C24 C19 C20 120.0(2) . . ? 
C24 C19 P2 120.38(17) . . ? 
C20 C19 P2 119.58(18) . . ? 
P1 N1 P2 125.99(11) . . ? 
P1 N1 Pd1 125.05(10) . . ? 
P2 N1 Pd1 99.04(9) . . ? 
C14 C13 C18 119.7(2) . . ? 
C14 C13 P2 121.75(17) . . ? 
C18 C13 P2 118.49(17) . . ? 
C11 C10 C9 120.4(2) . . ? 
C21 C22 C23 120.0(2) . . ? 
C15 C14 C13 120.0(2) . . ? 
C17 C16 C15 120.2(2) . . ? 
C6 C1 C2 122.2(2) . . ? 
C6 C1 O1 119.6(2) . . ? 
C2 C1 O1 118.0(2) . . ? 
C10 C11 C12 120.4(2) . . ? 
C7 C8 C9 118.9(2) . . ? 
C4 C3 C2 120.6(3) . . ? 
C17 C18 C13 119.6(2) . . ? 
C16 C17 C18 120.4(2) . . ? 
C7 C12 C11 118.8(2) . . ? 
C21 C20 C19 119.2(2) . . ? 
C22 C23 C24 120.3(2) . . ? 
C1 C2 C3 118.1(3) . . ? 
C14 C15 C16 120.1(2) . . ? 
C23 C24 C19 119.6(2) . . ? 
C4 C5 C6 120.3(3) . . ? 
C22 C21 C20 120.8(3) . . ? 
C1 C6 C5 118.7(2) . . ? 
C10 C9 C8 120.1(2) . . ? 
C5 C4 C3 120.1(3) . . ? 

_diffrn_measured_fraction_theta_max    0.919 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.919 
_refine_diff_density_max    0.649 
_refine_diff_density_min   -0.395 
_refine_diff_density_rms    0.062 

data_12.cif
#data_man70 
_database_code_CSD                153022
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          '[iPr2P(S)-N-P(O)(OPh)2]2Pd'
_chemical_formula_sum 
'C36 H48 N2 O6 P4 Pd S2' 
_chemical_formula_weight          899.16 

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' 
'Pd'  'Pd'  -0.9988   1.0072 
'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                    11.605(2) 
_cell_length_b                    12.181(2) 
_cell_length_c                    15.930(3) 
_cell_angle_alpha                 110.77(3) 
_cell_angle_beta                  91.19(3) 
_cell_angle_gamma                 106.59(3) 
_cell_volume                      1999.1(6) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     130(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.494 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              928 
_exptl_absorpt_coefficient_mu     0.775 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7026 
_diffrn_reflns_av_R_equivalents   0.0564 
_diffrn_reflns_av_sigmaI/netI     0.1221 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.64 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              6705 
_reflns_number_gt                 3988 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0633P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          6705 
_refine_ls_number_parameters      463 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1212 
_refine_ls_R_factor_gt            0.0422 
_refine_ls_wR_factor_ref          0.1220 
_refine_ls_wR_factor_gt           0.1030 
_refine_ls_goodness_of_fit_ref    0.982 
_refine_ls_restrained_S_all       0.982 
_refine_ls_shift/su_max           0.007 
_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 
Pd1 Pd 0.5000 0.5000 0.5000 0.01501(15) Uani 1 d S . . 
P2 P 0.21776(12) 0.32172(12) 0.46173(9) 0.0182(3) Uani 1 d . . . 
S1 S 0.52613(11) 0.30793(11) 0.41628(9) 0.0212(3) Uani 1 d . . . 
P1 P 0.31249(11) 0.57857(12) 0.59026(8) 0.0167(3) Uani 1 d . . . 
O1 O 0.0951(3) 0.3157(3) 0.4831(2) 0.0244(8) Uani 1 d . . . 
O2 O 0.2596(3) 0.2095(3) 0.4645(2) 0.0196(8) Uani 1 d . . . 
N1 N 0.3233(4) 0.4467(4) 0.5216(3) 0.0167(9) Uani 1 d . . . 
O3 O 0.2379(3) 0.3089(3) 0.3611(2) 0.0219(8) Uani 1 d . . . 
C7 C 0.1867(4) 0.2043(4) 0.2833(3) 0.0174(11) Uani 1 d . . . 
C2 C 0.3662(5) 0.1978(5) 0.5890(4) 0.0296(13) Uani 1 d . . . 
C17 C 0.1809(6) 0.6115(6) 0.4607(4) 0.0336(14) Uani 1 d . . . 
C1 C 0.2579(5) 0.1820(5) 0.5431(3) 0.0205(11) Uani 1 d . . . 
C13 C 0.3029(5) 0.5808(5) 0.7044(3) 0.0227(12) Uani 1 d . . . 
C11 C 0.2069(5) 0.0891(5) 0.1312(4) 0.0281(13) Uani 1 d . . . 
C12 C 0.2570(5) 0.1882(5) 0.2138(3) 0.0235(12) Uani 1 d . . . 
C8 C 0.0726(5) 0.1238(5) 0.2743(4) 0.0274(13) Uani 1 d . . . 
C16 C 0.1851(5) 0.6191(5) 0.5574(3) 0.0210(11) Uani 1 d . . . 
C14 C 0.4050(5) 0.5422(5) 0.7335(4) 0.0272(12) Uani 1 d . . . 
C5 C 0.1502(6) 0.1042(6) 0.6446(5) 0.0443(17) Uani 1 d . . . 
C3 C 0.3646(6) 0.1642(6) 0.6632(4) 0.0354(14) Uani 1 d . . . 
C10 C 0.0941(5) 0.0094(5) 0.1210(3) 0.0263(13) Uani 1 d . . . 
C18 C 0.1899(6) 0.7482(6) 0.6238(4) 0.0401(16) Uani 1 d . . . 
C9 C 0.0271(5) 0.0250(5) 0.1930(4) 0.0313(14) Uani 1 d . . . 
C6 C 0.1491(5) 0.1336(5) 0.5686(4) 0.0297(13) Uani 1 d . . . 
C4 C 0.2573(6) 0.1180(6) 0.6913(4) 0.0423(16) Uani 1 d . . . 
C15 C 0.1798(5) 0.5010(6) 0.7138(4) 0.0388(16) Uani 1 d . . . 
Pd2 Pd 0.0000 0.5000 0.0000 0.01377(14) Uani 1 d S . . 
P4 P 0.20142(11) 0.44496(12) 0.05606(8) 0.0151(3) Uani 1 d . . . 
S2 S 0.04629(11) 0.31825(11) -0.01816(9) 0.0188(3) Uani 1 d . . . 
P3 P 0.27558(11) 0.69742(12) 0.05903(9) 0.0162(3) Uani 1 d . . . 
O6 O 0.2467(3) 0.6964(3) -0.0391(2) 0.0204(8) Uani 1 d . . . 
O5 O 0.2288(3) 0.8084(3) 0.1170(2) 0.0200(8) Uani 1 d . . . 
N2 N 0.1784(3) 0.5713(4) 0.0563(3) 0.0158(9) Uani 1 d . . . 
C34 C 0.3316(4) 0.4132(5) 0.0035(3) 0.0183(11) Uani 1 d . . . 
C24 C 0.1331(5) 0.7847(5) 0.2451(4) 0.0237(12) Uani 1 d . . . 
C19 C 0.2339(5) 0.8381(5) 0.2115(3) 0.0196(11) Uani 1 d . . . 
C26 C 0.4173(5) 0.8268(5) -0.0787(4) 0.0241(12) Uani 1 d . . . 
C25 C 0.2974(5) 0.7952(4) -0.0671(3) 0.0171(11) Uani 1 d . . . 
C29 C 0.2648(5) 0.9427(6) -0.1206(4) 0.0301(13) Uani 1 d . . . 
C36 C 0.3252(5) 0.4133(6) -0.0907(4) 0.0321(14) Uani 1 d . . . 
C28 C 0.3855(5) 0.9780(5) -0.1323(4) 0.0312(13) Uani 1 d . . . 
C21 C 0.3406(6) 0.9504(6) 0.3602(4) 0.0380(15) Uani 1 d . . . 
C23 C 0.1386(5) 0.8140(5) 0.3367(4) 0.0300(13) Uani 1 d . . . 
C31 C 0.2175(5) 0.4454(5) 0.1691(3) 0.0229(12) Uani 1 d . . . 
C35 C 0.3421(6) 0.2924(6) 0.0040(4) 0.0369(15) Uani 1 d . . . 
C22 C 0.2406(6) 0.8949(5) 0.3946(4) 0.0305(13) Uani 1 d . . . 
C33 C 0.1000(5) 0.4502(5) 0.2123(4) 0.0260(12) Uani 1 d . . . 
C32 C 0.3268(5) 0.5491(6) 0.2300(4) 0.0312(14) Uani 1 d . . . 
C30 C 0.2205(5) 0.8498(5) -0.0879(4) 0.0266(12) Uani 1 d . . . 
C27 C 0.4612(5) 0.9192(5) -0.1120(4) 0.0291(13) Uani 1 d . . . 
C20 C 0.3375(5) 0.9209(5) 0.2682(4) 0.0315(14) Uani 1 d . . . 
O4 O 0.4014(3) 0.7142(3) 0.0870(2) 0.0204(8) Uani 1 d . . . 
H15B H 0.1594 0.4239 0.6847 0.050 Uiso 1 d . . . 
H35C H 0.2773 0.2376 -0.0163 0.050 Uiso 1 d . . . 
H9 H -0.0570 -0.0420 0.1857 0.050 Uiso 1 d . . . 
H35B H 0.3605 0.3053 0.0554 0.050 Uiso 1 d . . . 
H26 H 0.4678 0.7785 -0.0571 0.050 Uiso 1 d . . . 
H15A H 0.1417 0.5355 0.7154 0.050 Uiso 1 d . . . 
H17B H 0.1824 0.5335 0.4182 0.050 Uiso 1 d . . . 
H34 H 0.3918 0.4800 0.0307 0.050 Uiso 1 d . . . 
H36B H 0.2540 0.3529 -0.1254 0.050 Uiso 1 d . . . 
H36A H 0.3252 0.4759 -0.0949 0.050 Uiso 1 d . . . 
H31 H 0.1984 0.3700 0.1593 0.050 Uiso 1 d . . . 
H17A H 0.2411 0.6656 0.4619 0.050 Uiso 1 d . . . 
H24 H 0.0712 0.7403 0.2025 0.050 Uiso 1 d . . . 
H6 H 0.0936 0.1359 0.5414 0.050 Uiso 1 d . . . 
H27 H 0.5542 0.9598 -0.1154 0.050 Uiso 1 d . . . 
H35A H 0.4129 0.2680 -0.0352 0.050 Uiso 1 d . . . 
H18A H 0.2369 0.7979 0.6208 0.050 Uiso 1 d . . . 
H33C H 0.0257 0.3832 0.1755 0.050 Uiso 1 d . . . 
H33B H 0.1005 0.5411 0.2288 0.050 Uiso 1 d . . . 
H8 H 0.0255 0.1285 0.3253 0.050 Uiso 1 d . . . 
H32B H 0.3392 0.5411 0.2965 0.050 Uiso 1 d . . . 
H12 H 0.3327 0.2552 0.2324 0.050 Uiso 1 d . . . 
H28 H 0.4271 1.0405 -0.1531 0.050 Uiso 1 d . . . 
H32A H 0.3078 0.6369 0.2486 0.050 Uiso 1 d . . . 
H33A H 0.1068 0.4391 0.2733 0.050 Uiso 1 d . . . 
H3 H 0.4373 0.1873 0.7002 0.050 Uiso 1 d . . . 
H15C H 0.1832 0.4950 0.7745 0.050 Uiso 1 d . . . 
H36C H 0.3838 0.3827 -0.1244 0.050 Uiso 1 d . . . 
H22 H 0.2429 0.9045 0.4686 0.050 Uiso 1 d . . . 
H21 H 0.4206 1.0162 0.4025 0.050 Uiso 1 d . . . 
H30 H 0.1343 0.8332 -0.0811 0.050 Uiso 1 d . . . 
H4 H 0.2680 0.1133 0.7543 0.050 Uiso 1 d . . . 
H20 H 0.3816 0.9653 0.2441 0.050 Uiso 1 d . . . 
H10 H 0.0664 -0.0758 0.0531 0.050 Uiso 1 d . . . 
H23 H 0.0457 0.7625 0.3530 0.050 Uiso 1 d . . . 
H2 H 0.4362 0.2337 0.5608 0.050 Uiso 1 d . . . 
H18C H 0.1216 0.7866 0.5900 0.050 Uiso 1 d . . . 
H17C H 0.1120 0.6401 0.4438 0.050 Uiso 1 d . . . 
H29 H 0.1867 0.9585 -0.1503 0.050 Uiso 1 d . . . 
H13 H 0.3026 0.6582 0.7350 0.050 Uiso 1 d . . . 
H14C H 0.4803 0.5907 0.7317 0.050 Uiso 1 d . . . 
H14B H 0.4186 0.5615 0.7965 0.050 Uiso 1 d . . . 
H14A H 0.3983 0.4565 0.7082 0.050 Uiso 1 d . . . 
H16 H 0.1110 0.5584 0.5598 0.050 Uiso 1 d . . . 
H5 H 0.0787 0.0810 0.6706 0.050 Uiso 1 d . . . 
H32C H 0.3935 0.5632 0.1989 0.050 Uiso 1 d . . . 
H18B H 0.2429 0.7965 0.7024 0.050 Uiso 1 d . . . 
H11 H 0.2597 0.0846 0.0843 0.050 Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Pd1 0.0148(3) 0.0158(3) 0.0134(3) 0.0036(2) 0.0068(2) 0.0052(2) 
P2 0.0174(7) 0.0187(7) 0.0166(7) 0.0051(5) 0.0050(5) 0.0045(6) 
S1 0.0197(7) 0.0176(7) 0.0241(7) 0.0046(5) 0.0109(5) 0.0062(5) 
P1 0.0173(7) 0.0186(7) 0.0130(7) 0.0039(5) 0.0054(5) 0.0064(5) 
O1 0.0141(18) 0.024(2) 0.032(2) 0.0082(16) 0.0082(15) 0.0040(15) 
O2 0.0203(19) 0.0189(19) 0.0208(19) 0.0091(15) 0.0097(15) 0.0054(15) 
N1 0.018(2) 0.016(2) 0.015(2) 0.0030(17) 0.0073(17) 0.0076(18) 
O3 0.028(2) 0.021(2) 0.0145(19) 0.0047(15) 0.0067(15) 0.0049(16) 
C7 0.021(3) 0.017(3) 0.012(2) 0.0016(19) 0.000(2) 0.007(2) 
C2 0.031(3) 0.026(3) 0.031(3) 0.010(2) 0.007(2) 0.008(3) 
C17 0.042(4) 0.038(4) 0.029(3) 0.015(3) 0.000(3) 0.022(3) 
C1 0.027(3) 0.015(3) 0.021(3) 0.007(2) 0.008(2) 0.008(2) 
C13 0.024(3) 0.026(3) 0.016(3) 0.005(2) 0.006(2) 0.007(2) 
C11 0.038(3) 0.026(3) 0.020(3) 0.009(2) 0.008(2) 0.009(3) 
C12 0.027(3) 0.021(3) 0.021(3) 0.009(2) 0.003(2) 0.004(2) 
C8 0.025(3) 0.026(3) 0.027(3) 0.004(2) 0.007(2) 0.009(2) 
C16 0.018(3) 0.027(3) 0.018(3) 0.006(2) 0.002(2) 0.011(2) 
C14 0.025(3) 0.036(3) 0.025(3) 0.017(2) 0.002(2) 0.008(2) 
C5 0.049(4) 0.046(4) 0.053(4) 0.034(3) 0.030(3) 0.017(3) 
C3 0.042(4) 0.037(4) 0.031(3) 0.015(3) -0.004(3) 0.014(3) 
C10 0.039(3) 0.018(3) 0.014(3) 0.001(2) 0.001(2) 0.004(2) 
C18 0.043(4) 0.033(4) 0.042(4) -0.002(3) -0.005(3) 0.030(3) 
C9 0.023(3) 0.029(3) 0.036(4) 0.008(3) 0.002(2) 0.003(2) 
C6 0.032(3) 0.028(3) 0.037(3) 0.018(3) 0.013(3) 0.012(3) 
C4 0.052(4) 0.051(4) 0.036(4) 0.027(3) 0.013(3) 0.019(3) 
C15 0.032(3) 0.057(4) 0.025(3) 0.017(3) 0.015(3) 0.007(3) 
Pd2 0.0127(3) 0.0135(3) 0.0160(3) 0.0061(2) 0.0028(2) 0.0046(2) 
P4 0.0133(6) 0.0178(7) 0.0167(7) 0.0079(5) 0.0049(5) 0.0066(5) 
S2 0.0169(6) 0.0145(6) 0.0244(7) 0.0065(5) 0.0021(5) 0.0052(5) 
P3 0.0155(7) 0.0153(7) 0.0157(7) 0.0050(5) 0.0029(5) 0.0030(5) 
O6 0.024(2) 0.0180(19) 0.0178(19) 0.0084(15) 0.0044(15) 0.0024(15) 
O5 0.026(2) 0.0183(19) 0.0152(18) 0.0043(14) 0.0041(15) 0.0082(15) 
N2 0.014(2) 0.015(2) 0.018(2) 0.0060(17) 0.0040(17) 0.0051(17) 
C34 0.016(3) 0.021(3) 0.020(3) 0.010(2) 0.005(2) 0.007(2) 
C24 0.018(3) 0.024(3) 0.030(3) 0.012(2) 0.005(2) 0.007(2) 
C19 0.029(3) 0.015(3) 0.017(3) 0.006(2) 0.005(2) 0.010(2) 
C26 0.028(3) 0.025(3) 0.023(3) 0.009(2) 0.004(2) 0.014(2) 
C25 0.026(3) 0.012(3) 0.014(3) 0.0049(19) 0.005(2) 0.006(2) 
C29 0.032(3) 0.036(4) 0.030(3) 0.017(3) 0.008(2) 0.017(3) 
C36 0.034(3) 0.040(4) 0.026(3) 0.014(3) 0.013(3) 0.016(3) 
C28 0.042(4) 0.020(3) 0.030(3) 0.011(2) 0.007(3) 0.004(3) 
C21 0.041(4) 0.029(3) 0.029(3) 0.002(3) -0.008(3) 0.001(3) 
C23 0.035(3) 0.032(3) 0.030(3) 0.014(3) 0.014(3) 0.017(3) 
C31 0.025(3) 0.028(3) 0.017(3) 0.008(2) 0.008(2) 0.011(2) 
C35 0.041(4) 0.045(4) 0.042(4) 0.023(3) 0.019(3) 0.031(3) 
C22 0.052(4) 0.026(3) 0.022(3) 0.012(2) 0.015(3) 0.020(3) 
C33 0.028(3) 0.033(3) 0.018(3) 0.011(2) 0.008(2) 0.009(2) 
C32 0.023(3) 0.052(4) 0.019(3) 0.014(3) 0.004(2) 0.012(3) 
C30 0.031(3) 0.029(3) 0.022(3) 0.009(2) 0.011(2) 0.013(3) 
C27 0.025(3) 0.029(3) 0.028(3) 0.008(2) 0.009(2) 0.004(2) 
C20 0.035(3) 0.025(3) 0.025(3) 0.005(2) 0.006(3) -0.001(3) 
O4 0.0128(17) 0.022(2) 0.023(2) 0.0073(15) 0.0036(14) 0.0014(14) 

_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 
Pd1 N1 2.042(4) 2_666 ? 
Pd1 N1 2.042(4) . ? 
Pd1 S1 2.3565(14) 2_666 ? 
Pd1 S1 2.3565(14) . ? 
Pd1 P1 2.8393(14) 2_666 ? 
Pd1 P1 2.8393(14) . ? 
P2 O1 1.458(4) . ? 
P2 O3 1.583(3) . ? 
P2 O2 1.590(4) . ? 
P2 N1 1.608(4) . ? 
S1 P1 2.0153(19) 2_666 ? 
P1 N1 1.633(4) . ? 
P1 C16 1.809(5) . ? 
P1 C13 1.815(5) . ? 
P1 S1 2.0153(19) 2_666 ? 
O2 C1 1.406(6) . ? 
O3 C7 1.390(6) . ? 
C7 C8 1.373(7) . ? 
C7 C12 1.380(7) . ? 
C2 C1 1.369(8) . ? 
C2 C3 1.380(8) . ? 
C17 C16 1.509(8) . ? 
C1 C6 1.368(7) . ? 
C13 C14 1.513(7) . ? 
C13 C15 1.525(7) . ? 
C11 C10 1.355(8) . ? 
C11 C12 1.402(7) . ? 
C8 C9 1.381(8) . ? 
C16 C18 1.537(7) . ? 
C5 C4 1.371(10) . ? 
C5 C6 1.380(8) . ? 
C3 C4 1.367(9) . ? 
C10 C9 1.387(7) . ? 
Pd2 N2 2.047(4) 2_565 ? 
Pd2 N2 2.047(4) . ? 
Pd2 S2 2.3463(13) 2_565 ? 
Pd2 S2 2.3463(13) . ? 
Pd2 P4 2.8184(14) 2_565 ? 
Pd2 P4 2.8184(14) . ? 
P4 N2 1.633(4) . ? 
P4 C31 1.805(5) . ? 
P4 C34 1.813(5) . ? 
P4 S2 2.013(2) . ? 
P3 O4 1.453(4) . ? 
P3 O6 1.587(4) . ? 
P3 O5 1.590(3) . ? 
P3 N2 1.611(4) . ? 
O6 C25 1.408(6) . ? 
O5 C19 1.414(6) . ? 
C34 C36 1.501(8) . ? 
C34 C35 1.514(8) . ? 
C24 C23 1.369(8) . ? 
C24 C19 1.384(7) . ? 
C19 C20 1.376(8) . ? 
C26 C25 1.368(7) . ? 
C26 C27 1.384(8) . ? 
C25 C30 1.354(7) . ? 
C29 C28 1.381(8) . ? 
C29 C30 1.383(8) . ? 
C28 C27 1.379(8) . ? 
C21 C20 1.376(8) . ? 
C21 C22 1.394(8) . ? 
C23 C22 1.366(8) . ? 
C31 C32 1.520(8) . ? 
C31 C33 1.547(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 
N1 Pd1 N1 180.0 2_666 . ? 
N1 Pd1 S1 101.46(12) 2_666 2_666 ? 
N1 Pd1 S1 78.54(12) . 2_666 ? 
N1 Pd1 S1 78.54(12) 2_666 . ? 
N1 Pd1 S1 101.46(12) . . ? 
S1 Pd1 S1 180.0 2_666 . ? 
N1 Pd1 P1 34.43(11) 2_666 2_666 ? 
N1 Pd1 P1 145.57(11) . 2_666 ? 
S1 Pd1 P1 135.56(5) 2_666 2_666 ? 
S1 Pd1 P1 44.44(5) . 2_666 ? 
N1 Pd1 P1 145.57(11) 2_666 . ? 
N1 Pd1 P1 34.43(11) . . ? 
S1 Pd1 P1 44.44(5) 2_666 . ? 
S1 Pd1 P1 135.56(5) . . ? 
P1 Pd1 P1 180.0 2_666 . ? 
O1 P2 O3 115.6(2) . . ? 
O1 P2 O2 114.4(2) . . ? 
O3 P2 O2 98.92(19) . . ? 
O1 P2 N1 115.9(2) . . ? 
O3 P2 N1 103.0(2) . . ? 
O2 P2 N1 107.0(2) . . ? 
P1 S1 Pd1 80.59(6) 2_666 . ? 
N1 P1 C16 114.8(2) . . ? 
N1 P1 C13 110.9(2) . . ? 
C16 P1 C13 107.8(2) . . ? 
N1 P1 S1 99.49(16) . 2_666 ? 
C16 P1 S1 112.93(19) . 2_666 ? 
C13 P1 S1 110.70(19) . 2_666 ? 
N1 P1 Pd1 45.00(14) . . ? 
C16 P1 Pd1 134.41(17) . . ? 
C13 P1 Pd1 117.56(18) . . ? 
S1 P1 Pd1 54.96(5) 2_666 . ? 
C1 O2 P2 120.7(3) . . ? 
P2 N1 P1 129.5(3) . . ? 
P2 N1 Pd1 127.3(2) . . ? 
P1 N1 Pd1 100.6(2) . . ? 
C7 O3 P2 126.2(3) . . ? 
C8 C7 C12 121.8(5) . . ? 
C8 C7 O3 122.8(4) . . ? 
C12 C7 O3 115.4(4) . . ? 
C1 C2 C3 118.6(5) . . ? 
C6 C1 C2 121.9(5) . . ? 
C6 C1 O2 119.6(5) . . ? 
C2 C1 O2 118.4(5) . . ? 
C14 C13 C15 111.2(5) . . ? 
C14 C13 P1 109.8(4) . . ? 
C15 C13 P1 112.7(4) . . ? 
C10 C11 C12 120.9(5) . . ? 
C7 C12 C11 118.0(5) . . ? 
C7 C8 C9 118.8(5) . . ? 
C17 C16 C18 111.7(5) . . ? 
C17 C16 P1 111.6(4) . . ? 
C18 C16 P1 109.7(4) . . ? 
C4 C5 C6 120.9(6) . . ? 
C4 C3 C2 120.8(6) . . ? 
C11 C10 C9 119.9(5) . . ? 
C8 C9 C10 120.6(5) . . ? 
C1 C6 C5 118.3(6) . . ? 
C3 C4 C5 119.4(6) . . ? 
N2 Pd2 N2 180.0 2_565 . ? 
N2 Pd2 S2 79.16(12) 2_565 2_565 ? 
N2 Pd2 S2 100.84(12) . 2_565 ? 
N2 Pd2 S2 100.84(12) 2_565 . ? 
N2 Pd2 S2 79.16(12) . . ? 
S2 Pd2 S2 180.0 2_565 . ? 
N2 Pd2 P4 34.88(11) 2_565 2_565 ? 
N2 Pd2 P4 145.12(11) . 2_565 ? 
S2 Pd2 P4 44.73(5) 2_565 2_565 ? 
S2 Pd2 P4 135.27(5) . 2_565 ? 
N2 Pd2 P4 145.12(11) 2_565 . ? 
N2 Pd2 P4 34.88(11) . . ? 
S2 Pd2 P4 135.27(5) 2_565 . ? 
S2 Pd2 P4 44.73(5) . . ? 
P4 Pd2 P4 180.0 2_565 . ? 
N2 P4 C31 111.7(2) . . ? 
N2 P4 C34 114.8(2) . . ? 
C31 P4 C34 108.0(2) . . ? 
N2 P4 S2 100.25(15) . . ? 
C31 P4 S2 111.46(18) . . ? 
C34 P4 S2 110.52(17) . . ? 
N2 P4 Pd2 45.78(14) . . ? 
C31 P4 Pd2 118.29(17) . . ? 
C34 P4 Pd2 133.62(17) . . ? 
S2 P4 Pd2 55.11(5) . . ? 
P4 S2 Pd2 80.16(6) . . ? 
O4 P3 O6 115.6(2) . . ? 
O4 P3 O5 114.0(2) . . ? 
O6 P3 O5 99.32(19) . . ? 
O4 P3 N2 115.7(2) . . ? 
O6 P3 N2 103.0(2) . . ? 
O5 P3 N2 107.3(2) . . ? 
C25 O6 P3 125.1(3) . . ? 
C19 O5 P3 118.0(3) . . ? 
P3 N2 P4 129.1(2) . . ? 
P3 N2 Pd2 127.2(2) . . ? 
P4 N2 Pd2 99.35(19) . . ? 
C36 C34 C35 111.5(5) . . ? 
C36 C34 P4 111.0(4) . . ? 
C35 C34 P4 110.5(4) . . ? 
C23 C24 C19 118.6(5) . . ? 
C20 C19 C24 121.5(5) . . ? 
C20 C19 O5 119.6(5) . . ? 
C24 C19 O5 118.9(5) . . ? 
C25 C26 C27 118.3(5) . . ? 
C30 C25 C26 122.6(5) . . ? 
C30 C25 O6 116.8(5) . . ? 
C26 C25 O6 120.4(4) . . ? 
C28 C29 C30 120.2(5) . . ? 
C27 C28 C29 119.5(5) . . ? 
C20 C21 C22 120.0(5) . . ? 
C22 C23 C24 121.3(5) . . ? 
C32 C31 C33 110.8(4) . . ? 
C32 C31 P4 112.8(4) . . ? 
C33 C31 P4 110.8(4) . . ? 
C23 C22 C21 119.6(5) . . ? 
C25 C30 C29 118.9(5) . . ? 
C28 C27 C26 120.5(5) . . ? 
C21 C20 C19 119.0(5) . . ? 

_diffrn_measured_fraction_theta_max    0.947 
_diffrn_reflns_theta_full              25.05 
_diffrn_measured_fraction_theta_full   0.947 
_refine_diff_density_max    0.751 
_refine_diff_density_min   -1.226 
_refine_diff_density_rms    0.118 

data_13.cif
#data_man67 
_database_code_CSD                153023
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          '[Ph2P(S)-N-P(S)(OPh)2]2Pd'
_chemical_formula_sum 
'C24 H20 N O2 P2 Pd0.50 S2' 
_chemical_formula_weight          533.67 

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' 
'Pd'  'Pd'  -0.9988   1.0072 
'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                    10.698(2) 
_cell_length_b                    10.890(2) 
_cell_length_c                    11.220(2) 
_cell_angle_alpha                 108.78(3) 
_cell_angle_beta                  105.07(3) 
_cell_angle_gamma                 95.40(3) 
_cell_volume                      1172.2(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     130(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.70 
_exptl_crystal_size_mid           0.60 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.512 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              544 
_exptl_absorpt_coefficient_mu     0.757 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.6193 
_exptl_absorpt_correction_T_max   0.9631 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       130(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4349 
_diffrn_reflns_av_R_equivalents   0.0291 
_diffrn_reflns_av_sigmaI/netI     0.0471 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.80 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              4110 
_reflns_number_gt                 3361 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0621P)^2^+3.6876P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4110 
_refine_ls_number_parameters      286 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0641 
_refine_ls_R_factor_gt            0.0448 
_refine_ls_wR_factor_ref          0.1255 
_refine_ls_wR_factor_gt           0.1172 
_refine_ls_goodness_of_fit_ref    1.012 
_refine_ls_restrained_S_all       1.012 
_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 
Pd1 Pd 0.0000 0.0000 0.0000 0.01851(15) Uani 1 d S . . 
S1 S -0.14514(11) -0.20372(10) -0.10290(11) 0.0244(3) Uani 1 d . . . 
S2 S 0.18116(11) -0.10531(11) 0.02573(11) 0.0247(3) Uani 1 d . . . 
P1 P -0.10049(11) -0.27891(11) -0.27151(11) 0.0224(3) Uani 1 d . . . 
P2 P 0.18096(11) -0.18099(11) -0.16285(11) 0.0210(3) Uani 1 d . . . 
O2 O -0.1706(3) -0.4314(3) -0.3363(3) 0.0261(7) Uani 1 d . . . 
O1 O -0.1743(3) -0.2262(3) -0.3817(3) 0.0263(7) Uani 1 d . . . 
C13 C 0.2962(4) -0.2910(4) -0.1644(4) 0.0232(9) Uani 1 d . . . 
C2 C -0.3983(5) -0.3439(5) -0.5025(5) 0.0303(10) Uani 1 d . . . 
C7 C -0.1084(4) -0.5281(4) -0.2996(5) 0.0270(10) Uani 1 d . . . 
C1 C -0.3114(4) -0.2284(5) -0.4158(4) 0.0271(10) Uani 1 d . . . 
N1 N 0.0452(4) -0.2650(4) -0.2719(4) 0.0261(8) Uani 1 d . . . 
C3 C -0.5312(5) -0.3416(5) -0.5444(5) 0.0326(11) Uani 1 d . . . 
C6 C -0.3530(5) -0.1122(5) -0.3699(5) 0.0321(11) Uani 1 d . . . 
C4 C -0.5752(5) -0.2258(5) -0.5016(5) 0.0372(12) Uani 1 d . . . 
C16 C 0.4652(5) -0.4677(5) -0.1599(5) 0.0343(11) Uani 1 d . . . 
C5 C -0.4884(6) -0.1123(5) -0.4151(5) 0.0409(13) Uani 1 d . . . 
C18 C 0.2641(5) -0.4025(4) -0.1337(5) 0.0287(10) Uani 1 d . . . 
C15 C 0.4964(5) -0.3589(5) -0.1915(5) 0.0330(11) Uani 1 d . . . 
C17 C 0.3492(5) -0.4906(5) -0.1324(5) 0.0337(11) Uani 1 d . . . 
C14 C 0.4123(4) -0.2705(4) -0.1940(4) 0.0254(9) Uani 1 d . . . 
C19 C 0.2399(4) -0.0502(4) -0.2121(4) 0.0251(9) Uani 1 d . . . 
C20 C 0.1805(5) -0.0516(5) -0.3384(5) 0.0295(10) Uani 1 d . . . 
C24 C 0.3452(5) 0.0518(4) -0.1257(4) 0.0265(10) Uani 1 d . . . 
C8 C -0.0413(5) -0.5982(5) -0.3803(5) 0.0316(11) Uani 1 d . . . 
C22 C 0.3291(5) 0.1490(5) -0.2918(5) 0.0336(11) Uani 1 d . . . 
C9 C 0.0189(6) -0.6948(5) -0.3444(5) 0.0405(12) Uani 1 d . . . 
C23 C 0.3900(5) 0.1513(5) -0.1651(5) 0.0348(11) Uani 1 d . . . 
C12 C -0.1201(5) -0.5513(5) -0.1900(5) 0.0341(11) Uani 1 d . . . 
C21 C 0.2263(5) 0.0499(5) -0.3761(5) 0.0359(11) Uani 1 d . . . 
C10 C 0.0096(6) -0.7200(5) -0.2350(5) 0.0419(13) Uani 1 d . . . 
C11 C -0.0594(6) -0.6504(5) -0.1571(5) 0.0427(13) Uani 1 d . . . 
H6 H -0.2812 -0.0296 -0.3113 0.050 Uiso 1 d . . . 
H18 H 0.1731 -0.4204 -0.1122 0.050 Uiso 1 d . . . 
H17 H 0.3208 -0.5741 -0.1168 0.050 Uiso 1 d . . . 
H24 H 0.3868 0.0617 -0.0295 0.050 Uiso 1 d . . . 
H22 H 0.3716 0.2180 -0.3148 0.050 Uiso 1 d . . . 
H12 H -0.1750 -0.5058 -0.1391 0.050 Uiso 1 d . . . 
H8 H -0.0367 -0.5780 -0.4695 0.050 Uiso 1 d . . . 
H3 H -0.6044 -0.4294 -0.6020 0.050 Uiso 1 d . . . 
H5 H -0.5029 -0.0199 -0.3851 0.050 Uiso 1 d . . . 
H2 H -0.3707 -0.4369 -0.5416 0.050 Uiso 1 d . . . 
H15 H 0.5863 -0.3403 -0.2052 0.050 Uiso 1 d . . . 
H23 H 0.4692 0.2289 -0.1037 0.050 Uiso 1 d . . . 
H14 H 0.4320 -0.1965 -0.2158 0.050 Uiso 1 d . . . 
H20 H 0.0981 -0.1230 -0.3930 0.050 Uiso 1 d . . . 
H21 H 0.1763 0.0426 -0.4729 0.050 Uiso 1 d . . . 
H9 H 0.0806 -0.7392 -0.3984 0.050 Uiso 1 d . . . 
H4 H -0.6796 -0.2246 -0.5257 0.050 Uiso 1 d . . . 
H16 H 0.5218 -0.5300 -0.1788 0.050 Uiso 1 d . . . 
H10 H 0.0545 -0.7949 -0.2161 0.050 Uiso 1 d . . . 
H11 H -0.0645 -0.6459 -0.0618 0.050 Uiso 1 d . . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
Pd1 0.0208(3) 0.0160(2) 0.0163(2) 0.00476(17) 0.00456(18) -0.00043(17) 
S1 0.0234(6) 0.0200(5) 0.0259(6) 0.0078(4) 0.0044(4) -0.0022(4) 
S2 0.0240(6) 0.0240(5) 0.0248(6) 0.0068(4) 0.0079(4) 0.0044(4) 
P1 0.0240(6) 0.0177(5) 0.0211(6) 0.0069(4) 0.0010(4) 0.0008(4) 
P2 0.0198(6) 0.0194(5) 0.0220(6) 0.0074(4) 0.0041(4) 0.0026(4) 
O2 0.0214(15) 0.0192(15) 0.0302(17) 0.0075(13) -0.0011(13) 0.0004(12) 
O1 0.0236(16) 0.0290(17) 0.0273(16) 0.0147(14) 0.0036(13) 0.0047(13) 
C13 0.021(2) 0.020(2) 0.028(2) 0.0078(18) 0.0060(18) 0.0073(17) 
C2 0.025(2) 0.029(2) 0.030(2) 0.010(2) -0.0006(19) 0.0035(19) 
C7 0.026(2) 0.018(2) 0.031(2) 0.0101(19) -0.0005(19) 0.0003(18) 
C1 0.025(2) 0.033(3) 0.025(2) 0.013(2) 0.0038(18) 0.011(2) 
N1 0.028(2) 0.0233(19) 0.0227(19) 0.0047(15) 0.0069(16) 0.0031(16) 
C3 0.027(2) 0.036(3) 0.034(3) 0.016(2) 0.003(2) 0.005(2) 
C6 0.039(3) 0.030(3) 0.024(2) 0.008(2) 0.006(2) 0.012(2) 
C4 0.028(3) 0.047(3) 0.040(3) 0.022(2) 0.007(2) 0.013(2) 
C16 0.033(3) 0.032(3) 0.032(3) 0.005(2) 0.004(2) 0.014(2) 
C5 0.052(3) 0.043(3) 0.041(3) 0.022(3) 0.019(3) 0.031(3) 
C18 0.029(2) 0.022(2) 0.035(3) 0.010(2) 0.010(2) 0.0057(19) 
C15 0.024(2) 0.037(3) 0.031(3) 0.006(2) 0.005(2) 0.009(2) 
C17 0.045(3) 0.020(2) 0.031(3) 0.0069(19) 0.005(2) 0.007(2) 
C14 0.022(2) 0.027(2) 0.027(2) 0.0089(19) 0.0076(18) 0.0053(18) 
C19 0.025(2) 0.023(2) 0.027(2) 0.0092(18) 0.0070(19) 0.0067(18) 
C20 0.030(2) 0.030(2) 0.027(2) 0.011(2) 0.004(2) 0.007(2) 
C24 0.030(2) 0.020(2) 0.024(2) 0.0064(18) 0.0035(19) 0.0006(18) 
C8 0.042(3) 0.024(2) 0.026(2) 0.0058(19) 0.010(2) 0.005(2) 
C22 0.051(3) 0.021(2) 0.040(3) 0.015(2) 0.023(2) 0.017(2) 
C9 0.051(3) 0.026(3) 0.040(3) 0.008(2) 0.011(2) 0.014(2) 
C23 0.042(3) 0.020(2) 0.040(3) 0.007(2) 0.014(2) 0.001(2) 
C12 0.036(3) 0.035(3) 0.031(3) 0.012(2) 0.010(2) 0.004(2) 
C21 0.040(3) 0.042(3) 0.040(3) 0.026(2) 0.018(2) 0.017(2) 
C10 0.052(3) 0.026(3) 0.042(3) 0.013(2) 0.003(3) 0.009(2) 
C11 0.062(4) 0.030(3) 0.037(3) 0.016(2) 0.011(3) 0.007(3) 

_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 
Pd1 S1 2.3315(15) . ? 
Pd1 S1 2.3315(15) 2 ? 
Pd1 S2 2.3442(13) 2 ? 
Pd1 S2 2.3442(13) . ? 
S1 P1 2.0059(17) . ? 
S2 P2 2.0077(16) . ? 
P1 N1 1.553(4) . ? 
P1 O1 1.586(3) . ? 
P1 O2 1.598(3) . ? 
P2 N1 1.596(4) . ? 
P2 C13 1.797(4) . ? 
P2 C19 1.803(4) . ? 
O2 C7 1.411(5) . ? 
O1 C1 1.412(5) . ? 
C13 C14 1.383(6) . ? 
C13 C18 1.402(6) . ? 
C2 C3 1.383(7) . ? 
C2 C1 1.384(7) . ? 
C7 C12 1.366(7) . ? 
C7 C8 1.384(7) . ? 
C1 C6 1.368(7) . ? 
C3 C4 1.371(7) . ? 
C6 C5 1.405(7) . ? 
C4 C5 1.369(8) . ? 
C16 C17 1.374(7) . ? 
C16 C15 1.378(7) . ? 
C18 C17 1.384(7) . ? 
C15 C14 1.379(7) . ? 
C19 C20 1.388(6) . ? 
C19 C24 1.395(6) . ? 
C20 C21 1.396(7) . ? 
C24 C23 1.386(6) . ? 
C8 C9 1.395(7) . ? 
C22 C21 1.359(7) . ? 
C22 C23 1.392(7) . ? 
C9 C10 1.366(8) . ? 
C12 C11 1.409(7) . ? 
C10 C11 1.378(8) . ? 

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 
S1 Pd1 S1 180.0 . 2 ? 
S1 Pd1 S2 89.13(5) . 2 ? 
S1 Pd1 S2 90.87(5) 2 2 ? 
S1 Pd1 S2 90.87(5) . . ? 
S1 Pd1 S2 89.13(5) 2 . ? 
S2 Pd1 S2 180.0 2 . ? 
P1 S1 Pd1 101.88(6) . . ? 
P2 S2 Pd1 100.31(6) . . ? 
N1 P1 O1 105.32(19) . . ? 
N1 P1 O2 109.70(19) . . ? 
O1 P1 O2 100.49(17) . . ? 
N1 P1 S1 120.92(15) . . ? 
O1 P1 S1 112.04(14) . . ? 
O2 P1 S1 106.51(14) . . ? 
N1 P2 C13 106.6(2) . . ? 
N1 P2 C19 108.3(2) . . ? 
C13 P2 C19 108.7(2) . . ? 
N1 P2 S2 117.63(15) . . ? 
C13 P2 S2 105.67(15) . . ? 
C19 P2 S2 109.58(16) . . ? 
C7 O2 P1 121.0(3) . . ? 
C1 O1 P1 122.6(3) . . ? 
C14 C13 C18 119.6(4) . . ? 
C14 C13 P2 123.4(3) . . ? 
C18 C13 P2 117.0(3) . . ? 
C3 C2 C1 118.9(4) . . ? 
C12 C7 C8 123.1(4) . . ? 
C12 C7 O2 119.3(4) . . ? 
C8 C7 O2 117.6(4) . . ? 
C6 C1 C2 122.0(4) . . ? 
C6 C1 O1 118.2(4) . . ? 
C2 C1 O1 119.6(4) . . ? 
P1 N1 P2 132.9(2) . . ? 
C4 C3 C2 120.1(5) . . ? 
C1 C6 C5 117.8(5) . . ? 
C5 C4 C3 120.4(5) . . ? 
C17 C16 C15 120.5(4) . . ? 
C4 C5 C6 120.6(5) . . ? 
C17 C18 C13 119.8(4) . . ? 
C16 C15 C14 120.3(4) . . ? 
C16 C17 C18 119.9(4) . . ? 
C15 C14 C13 119.9(4) . . ? 
C20 C19 C24 119.4(4) . . ? 
C20 C19 P2 119.6(3) . . ? 
C24 C19 P2 121.0(3) . . ? 
C19 C20 C21 119.4(4) . . ? 
C23 C24 C19 120.4(4) . . ? 
C7 C8 C9 117.3(4) . . ? 
C21 C22 C23 120.2(4) . . ? 
C10 C9 C8 121.0(5) . . ? 
C24 C23 C22 119.5(5) . . ? 
C7 C12 C11 118.2(5) . . ? 
C22 C21 C20 121.0(5) . . ? 
C9 C10 C11 120.7(5) . . ? 
C10 C11 C12 119.6(5) . . ? 

_diffrn_measured_fraction_theta_max    0.988 
_diffrn_reflns_theta_full              25.05 
_diffrn_measured_fraction_theta_full   0.988 
_refine_diff_density_max    1.777 
_refine_diff_density_min   -1.286 
_refine_diff_density_rms    0.106 

data_14.cif
#data_m 
_database_code_CSD                153024
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          '(PhO)2P(O)-NH-P(S)(OPh)2' 
_chemical_formula_sum 
'C24 H21 N O5 P2 S' 
_chemical_formula_weight          497.42 

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' 

_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    Cc

loop_ 
_symmetry_equiv_pos_as_xyz 
'x, y, z' 
'x, -y, z+1/2' 
'x+1/2, y+1/2, z' 
'x+1/2, -y+1/2, z+1/2' 

_cell_length_a                    10.829(2) 
_cell_length_b                    22.400(4) 
_cell_length_c                    10.007(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  98.22(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2402.5(8) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     130(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.375 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1032 
_exptl_absorpt_coefficient_mu     0.304 
_exptl_absorpt_correction_type    ? 
_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          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2253 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0467 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -26 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        0 
_diffrn_reflns_theta_min          3.80 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              2253 
_reflns_number_gt                 1999 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 F^2^ against ALL reflections.  The weighted R-factor wR and 
goodness of fit S are based on F^2^, conventional R-factors R are based 
on F, with F set to zero for negative F^2^. The threshold expression of 
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ 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^)+(0.0606P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.01(9) 
_refine_ls_number_reflns          2253 
_refine_ls_number_parameters      301 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0441 
_refine_ls_R_factor_gt            0.0332 
_refine_ls_wR_factor_ref          0.0890 
_refine_ls_wR_factor_gt           0.0853 
_refine_ls_goodness_of_fit_ref    1.040 
_refine_ls_restrained_S_all       1.039 
_refine_ls_shift/su_max           0.005 
_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 
C15 C 0.5652(5) 0.6896(2) 1.3894(5) 0.0406(12) Uani 1 d . . . 
H15 H 0.6031 0.7237 1.4294 0.049 Uiso 1 d R . . 
C14 C 0.4388(4) 0.68122(18) 1.3836(4) 0.0284(9) Uani 1 d . . . 
H14 H 0.3906 0.7086 1.4231 0.034 Uiso 1 d R . . 
C16 C 0.6376(4) 0.6480(2) 1.3352(5) 0.0353(10) Uani 1 d . . . 
H16 H 0.7231 0.6533 1.3389 0.042 Uiso 1 d R . . 
C13 C 0.3857(3) 0.63099(16) 1.3206(4) 0.0188(8) Uani 1 d . . . 
C17 C 0.5825(4) 0.5982(2) 1.2725(5) 0.0310(9) Uani 1 d . . . 
H17 H 0.6306 0.5703 1.2344 0.037 Uiso 1 d R . . 
O3 O 0.2588(2) 0.62112(11) 1.3275(3) 0.0191(6) Uani 1 d . . . 
C18 C 0.4548(3) 0.58891(17) 1.2657(4) 0.0207(8) Uani 1 d . . . 
H18 H 0.4175 0.5543 1.2275 0.025 Uiso 1 d R . . 
P2 P 0.15232(8) 0.61438(4) 1.20217(8) 0.0143(2) Uani 1 d . . . 
S1 S 0.17494(8) 0.65919(4) 1.04655(9) 0.0209(2) Uani 1 d . . . 
O4 O 0.0344(2) 0.62729(11) 1.2747(3) 0.0188(6) Uani 1 d . . . 
N1 N 0.1335(3) 0.54223(14) 1.1727(3) 0.0158(6) Uani 1 d . . . 
H0 H 0.142(4) 0.532(2) 1.098(5) 0.019 Uiso 1 d . . . 
C19 C 0.0219(3) 0.68015(16) 1.3467(4) 0.0197(8) Uani 1 d . . . 
P1 P 0.10235(8) 0.49053(4) 1.27896(8) 0.0125(2) Uani 1 d . . . 
C24 C -0.0380(4) 0.72822(19) 1.2781(5) 0.0297(9) Uani 1 d . . . 
H24 H -0.0648 0.7249 1.1859 0.036 Uiso 1 d R . . 
C20 C 0.0623(4) 0.6822(2) 1.4822(4) 0.0298(9) Uani 1 d . . . 
H20 H 0.1049 0.6502 1.5266 0.036 Uiso 1 d R . . 
O1 O 0.1735(2) 0.43343(11) 1.2390(2) 0.0154(5) Uani 1 d . . . 
O5 O 0.1287(2) 0.50838(11) 1.4203(3) 0.0178(5) Uani 1 d . . . 
O2 O -0.0367(2) 0.47219(11) 1.2277(2) 0.0178(5) Uani 1 d . . . 
C23 C -0.0567(4) 0.77837(19) 1.3521(6) 0.0381(11) Uani 1 d . . . 
H23 H -0.0954 0.8108 1.3055 0.046 Uiso 1 d R . . 
C21 C 0.0417(4) 0.7326(2) 1.5534(5) 0.0359(10) Uani 1 d . . . 
H21 H 0.0667 0.7352 1.6461 0.043 Uiso 1 d R . . 
C1 C 0.3057(3) 0.43527(15) 1.2501(4) 0.0142(7) Uani 1 d . . . 
C7 C -0.0946(3) 0.42618(17) 1.2926(4) 0.0207(8) Uani 1 d . . . 
C22 C -0.0176(4) 0.78074(19) 1.4876(5) 0.0370(11) Uani 1 d . . . 
H22 H -0.0346 0.8153 1.5331 0.044 Uiso 1 d R . . 
C2 C 0.3553(4) 0.43239(16) 1.1317(4) 0.0191(8) Uani 1 d . . . 
H2 H 0.3028 0.4290 1.0500 0.023 Uiso 1 d R . . 
C6 C 0.3768(3) 0.43883(16) 1.3744(4) 0.0184(8) Uani 1 d . . . 
H6 H 0.3405 0.4408 1.4531 0.022 Uiso 1 d R . . 
C8 C -0.1282(4) 0.37584(19) 1.2192(5) 0.0329(10) Uani 1 d . . . 
H8 H -0.1135 0.3708 1.1305 0.039 Uiso 1 d R . . 
C12 C -0.1206(4) 0.4333(2) 1.4216(4) 0.0296(9) Uani 1 d . . . 
H12 H -0.0971 0.4690 1.4657 0.036 Uiso 1 d R . . 
C3 C 0.4845(3) 0.43303(17) 1.1389(4) 0.0219(8) Uani 1 d . . . 
H3 H 0.5201 0.4316 1.0597 0.026 Uiso 1 d R . . 
C5 C 0.5058(3) 0.43981(17) 1.3805(4) 0.0220(8) Uani 1 d . . . 
H5 H 0.5579 0.4416 1.4627 0.026 Uiso 1 d R . . 
C9 C -0.1886(4) 0.3305(2) 1.2765(7) 0.0477(14) Uani 1 d . . . 
H9 H -0.2153 0.2952 1.2330 0.057 Uiso 1 d R . . 
C11 C -0.1801(4) 0.3869(3) 1.4791(5) 0.0431(14) Uani 1 d . . . 
H11 H -0.1944 0.3925 1.5677 0.052 Uiso 1 d R . . 
C4 C 0.5590(3) 0.43720(18) 1.2625(4) 0.0221(8) Uani 1 d . . . 
H4 H 0.6452 0.4385 1.2660 0.026 Uiso 1 d R . . 
C10 C -0.2132(4) 0.3361(3) 1.4061(7) 0.0505(16) Uani 1 d . . . 
H10 H -0.2524 0.3071 1.4515 0.061 Uiso 1 d R . . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
C15 0.042(3) 0.034(2) 0.042(3) 0.007(2) -0.007(2) -0.022(2) 
C14 0.034(2) 0.021(2) 0.028(2) 0.0007(16) -0.0030(18) -0.0023(17) 
C16 0.019(2) 0.048(3) 0.038(2) 0.008(2) 0.0023(18) -0.0142(19) 
C13 0.0179(19) 0.0220(18) 0.0162(18) 0.0059(14) 0.0007(15) -0.0026(14) 
C17 0.022(2) 0.042(2) 0.029(2) 0.0051(19) 0.0026(18) -0.0031(18) 
O3 0.0166(13) 0.0240(14) 0.0164(13) -0.0011(11) 0.0012(10) -0.0007(10) 
C18 0.021(2) 0.0232(19) 0.0182(18) 0.0038(15) 0.0031(16) -0.0030(15) 
P2 0.0149(4) 0.0155(4) 0.0127(4) 0.0005(4) 0.0027(3) 0.0026(3) 
S1 0.0239(5) 0.0208(5) 0.0185(4) 0.0067(4) 0.0048(4) 0.0010(4) 
O4 0.0187(13) 0.0181(13) 0.0207(13) -0.0020(10) 0.0069(11) 0.0023(10) 
N1 0.0187(15) 0.0212(16) 0.0077(14) -0.0009(12) 0.0030(12) 0.0004(12) 
C19 0.0130(17) 0.0212(19) 0.027(2) -0.0028(15) 0.0094(15) 0.0005(14) 
P1 0.0123(4) 0.0154(4) 0.0099(4) 0.0012(3) 0.0020(3) 0.0006(4) 
C24 0.026(2) 0.029(2) 0.034(2) 0.0003(18) 0.0020(17) 0.0071(17) 
C20 0.035(2) 0.030(2) 0.027(2) 0.0006(17) 0.0166(18) 0.0037(18) 
O1 0.0087(12) 0.0184(12) 0.0189(13) 0.0011(10) 0.0013(10) -0.0010(9) 
O5 0.0170(12) 0.0235(13) 0.0122(13) 0.0019(10) 0.0001(10) 0.0000(11) 
O2 0.0108(12) 0.0265(13) 0.0161(12) 0.0021(11) 0.0023(9) -0.0007(10) 
C23 0.034(2) 0.017(2) 0.064(3) -0.005(2) 0.012(2) 0.0080(18) 
C21 0.043(3) 0.036(2) 0.033(2) -0.013(2) 0.019(2) -0.007(2) 
C1 0.0099(16) 0.0136(17) 0.0189(19) 0.0024(13) 0.0016(14) 0.0011(13) 
C7 0.0084(15) 0.027(2) 0.026(2) 0.0086(16) 0.0029(15) 0.0029(14) 
C22 0.030(2) 0.027(2) 0.057(3) -0.019(2) 0.019(2) -0.0004(19) 
C2 0.0189(19) 0.0236(18) 0.0143(17) -0.0030(14) 0.0003(14) 0.0020(15) 
C6 0.0143(17) 0.0225(19) 0.0185(18) 0.0023(14) 0.0025(14) 0.0030(15) 
C8 0.022(2) 0.032(2) 0.048(3) 0.000(2) 0.0135(19) 0.0053(17) 
C12 0.0128(19) 0.053(3) 0.023(2) 0.0053(19) 0.0022(16) 0.0018(18) 
C3 0.0197(19) 0.027(2) 0.0195(19) -0.0011(15) 0.0059(15) 0.0019(15) 
C5 0.0156(18) 0.028(2) 0.0209(19) 0.0016(15) -0.0023(15) 0.0033(15) 
C9 0.024(2) 0.029(2) 0.091(4) 0.004(3) 0.010(3) -0.0010(19) 
C11 0.016(2) 0.081(4) 0.033(3) 0.031(3) 0.0067(18) 0.010(2) 
C4 0.0124(17) 0.028(2) 0.025(2) 0.0001(16) -0.0010(14) 0.0035(15) 
C10 0.018(2) 0.049(3) 0.086(4) 0.036(3) 0.013(3) 0.005(2) 

_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 
C15 C14 1.374(7) . ? 
C15 C16 1.379(7) . ? 
C14 C13 1.375(6) . ? 
C16 C17 1.372(7) . ? 
C13 C18 1.367(5) . ? 
C13 O3 1.403(5) . ? 
C17 C18 1.390(5) . ? 
O3 P2 1.585(3) . ? 
P2 O4 1.584(3) . ? 
P2 N1 1.650(3) . ? 
P2 S1 1.8978(12) . ? 
O4 C19 1.402(4) . ? 
N1 P1 1.640(3) . ? 
C19 C20 1.364(6) . ? 
C19 C24 1.387(6) . ? 
P1 O5 1.458(3) . ? 
P1 O1 1.574(2) . ? 
P1 O2 1.575(2) . ? 
C24 C23 1.376(6) . ? 
C20 C21 1.371(6) . ? 
O1 C1 1.420(4) . ? 
O2 C7 1.412(4) . ? 
C23 C22 1.363(8) . ? 
C21 C22 1.374(7) . ? 
C1 C6 1.369(5) . ? 
C1 C2 1.371(5) . ? 
C7 C8 1.367(6) . ? 
C7 C12 1.369(6) . ? 
C2 C3 1.391(5) . ? 
C6 C5 1.389(5) . ? 
C8 C9 1.376(7) . ? 
C12 C11 1.391(7) . ? 
C3 C4 1.380(6) . ? 
C5 C4 1.387(6) . ? 
C9 C10 1.367(9) . ? 
C11 C10 1.371(9) . ? 

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 
C14 C15 C16 120.7(4) . . ? 
C13 C14 C15 118.7(4) . . ? 
C17 C16 C15 119.6(4) . . ? 
C18 C13 C14 122.1(4) . . ? 
C18 C13 O3 120.5(3) . . ? 
C14 C13 O3 117.0(3) . . ? 
C16 C17 C18 120.6(4) . . ? 
C13 O3 P2 125.6(2) . . ? 
C13 C18 C17 118.3(4) . . ? 
O4 P2 O3 99.38(14) . . ? 
O4 P2 N1 100.01(15) . . ? 
O3 P2 N1 106.97(15) . . ? 
O4 P2 S1 119.14(11) . . ? 
O3 P2 S1 115.75(11) . . ? 
N1 P2 S1 113.48(12) . . ? 
C19 O4 P2 122.2(2) . . ? 
P1 N1 P2 127.4(2) . . ? 
C20 C19 C24 121.8(4) . . ? 
C20 C19 O4 119.8(4) . . ? 
C24 C19 O4 118.3(4) . . ? 
O5 P1 O1 115.73(14) . . ? 
O5 P1 O2 115.64(15) . . ? 
O1 P1 O2 100.69(13) . . ? 
O5 P1 N1 113.93(16) . . ? 
O1 P1 N1 104.82(15) . . ? 
O2 P1 N1 104.41(15) . . ? 
C23 C24 C19 117.5(4) . . ? 
C19 C20 C21 119.4(4) . . ? 
C1 O1 P1 118.8(2) . . ? 
C7 O2 P1 120.5(2) . . ? 
C22 C23 C24 121.2(4) . . ? 
C20 C21 C22 119.8(5) . . ? 
C6 C1 C2 123.3(3) . . ? 
C6 C1 O1 120.2(3) . . ? 
C2 C1 O1 116.5(3) . . ? 
C8 C7 C12 121.9(4) . . ? 
C8 C7 O2 117.1(4) . . ? 
C12 C7 O2 120.9(4) . . ? 
C23 C22 C21 120.2(4) . . ? 
C1 C2 C3 118.1(3) . . ? 
C1 C6 C5 118.2(3) . . ? 
C7 C8 C9 119.3(5) . . ? 
C7 C12 C11 118.2(5) . . ? 
C4 C3 C2 120.1(4) . . ? 
C4 C5 C6 120.0(3) . . ? 
C10 C9 C8 119.8(5) . . ? 
C10 C11 C12 120.1(5) . . ? 
C3 C4 C5 120.3(3) . . ? 
C9 C10 C11 120.7(5) . . ? 

_diffrn_measured_fraction_theta_max    0.499 
_diffrn_reflns_theta_full              25.05 
_diffrn_measured_fraction_theta_full   0.499 
_refine_diff_density_max    0.387 
_refine_diff_density_min   -0.403 
_refine_diff_density_rms    0.063