# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1193

data_dw9817 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
  "Paper 9/01222B" 
  "A Simple Route to Multifunctional Phosphide and Amide Donor Sets, 
...."
  "M.A. beswick, A. Bashall, A.D. Hopkins, S.J. Kidd, Y.G. Lawson,
  M. McPartlin, P.R. Raithby, A. Rothenberger, D. Stalke and D.S. 
Wright"
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C34 H88 As2 K2 N10 P2' 
_chemical_formula_weight          927.12 
 
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' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'As'  'As'   0.0499   2.0058 
 '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                    14.014(3) 
_cell_length_b                    12.750(3) 
_cell_length_c                    15.014(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  105.48(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2585.4(10) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       10 
_cell_measurement_theta_max       12.5 
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             'Dark orange' 
_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     1.191 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              992 
_exptl_absorpt_coefficient_mu     1.547 
_exptl_absorpt_correction_type    'Psi scans' 
_exptl_absorpt_correction_T_min   0.5765 
_exptl_absorpt_correction_T_max   0.7472 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       173(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   'Stoe four circle' 
_diffrn_measurement_method        'omega/theta scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             3473 
_diffrn_reflns_av_R_equivalents   0.0985 
_diffrn_reflns_av_sigmaI/netI     0.1376 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -1 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          4.09 
_diffrn_reflns_theta_max          22.50 
_reflns_number_total              3357 
_reflns_number_gt                 1956 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Stoe control software, DIF4' 
_computing_cell_refinement        'Stoe control software, DIF4' 
_computing_data_reduction         'Stoe software, REDU4' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL-PLUS (Sheldrick, 1991)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_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  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^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          3357 
_refine_ls_number_parameters      226 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1468 
_refine_ls_R_factor_gt            0.0733 
_refine_ls_wR_factor_ref          0.1854 
_refine_ls_wR_factor_gt           0.1536 
_refine_ls_goodness_of_fit_ref    1.014 
_refine_ls_restrained_S_all       1.014 
_refine_ls_shift/su_max           0.027 
_refine_ls_shift/su_mean          0.002 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
As1 As 0.73901(7) 0.07631(9) 0.44258(7) 0.0304(4) Uani 1 1 d . . . 
N1 N 0.5414(7) -0.3141(7) 0.2951(6) 0.043(2) Uani 1 1 d . . . 
N2 N 0.5682(6) -0.1184(7) 0.1848(5) 0.037(2) Uani 1 1 d . . . 
N3 N 0.3632(6) -0.0432(7) 0.1856(5) 0.035(2) Uani 1 1 d . . . 
N4 N 0.8314(6) 0.1088(8) 0.5542(6) 0.053(3) Uani 1 1 d . . . 
N5 N 0.7239(5) -0.0687(7) 0.4572(5) 0.032(2) Uani 1 1 d . . . 
P1 P 0.58900(18) 0.1269(2) 0.45626(18) 0.0296(7) Uani 1 1 d . . . 
C1 C 0.4572(10) -0.3823(12) 0.2989(10) 0.085(5) Uani 1 1 d . . . 
H1A H 0.4682 -0.4531 0.2782 0.127 Uiso 1 1 calc R . . 
H1B H 0.3959 -0.3536 0.2586 0.127 Uiso 1 1 calc R . . 
H1C H 0.4517 -0.3854 0.3626 0.127 Uiso 1 1 calc R . . 
C2 C 0.6266(10) -0.3581(12) 0.3545(9) 0.083(5) Uani 1 1 d . . . 
H2A H 0.6364 -0.4291 0.3335 0.125 Uiso 1 1 calc R . . 
H2B H 0.6187 -0.3613 0.4174 0.125 Uiso 1 1 calc R . . 
H2C H 0.6842 -0.3147 0.3542 0.125 Uiso 1 1 calc R . . 
C3 C 0.5477(9) -0.3111(10) 0.1982(8) 0.056(3) Uani 1 1 d . . . 
H3A H 0.4801 -0.3044 0.1566 0.068 Uiso 1 1 calc R . . 
H3B H 0.5757 -0.3782 0.1837 0.068 Uiso 1 1 calc R . . 
C4 C 0.6101(8) -0.2226(9) 0.1791(8) 0.048(3) Uani 1 1 d . . . 
H4A H 0.6762 -0.2263 0.2239 0.058 Uiso 1 1 calc R . . 
H4B H 0.6194 -0.2320 0.1165 0.058 Uiso 1 1 calc R . . 
C5 C 0.6451(8) -0.0399(9) 0.1933(8) 0.055(3) Uani 1 1 d . . . 
H5A H 0.6688 -0.0404 0.1375 0.082 Uiso 1 1 calc R . . 
H5B H 0.7002 -0.0558 0.2473 0.082 Uiso 1 1 calc R . . 
H5C H 0.6182 0.0295 0.2009 0.082 Uiso 1 1 calc R . . 
C6 C 0.4856(8) -0.0969(10) 0.1042(7) 0.047(3) Uani 1 1 d . . . 
H6A H 0.4466 -0.1620 0.0863 0.057 Uiso 1 1 calc R . . 
H6B H 0.5121 -0.0761 0.0519 0.057 Uiso 1 1 calc R . . 
C7 C 0.4184(8) -0.0118(10) 0.1212(7) 0.051(3) Uani 1 1 d . . . 
H7A H 0.4586 0.0508 0.1457 0.061 Uiso 1 1 calc R . . 
H7B H 0.3714 0.0079 0.0617 0.061 Uiso 1 1 calc R . . 
C8 C 0.2900(10) -0.1188(12) 0.1472(9) 0.078(5) Uani 1 1 d . . . 
H8A H 0.2452 -0.0908 0.0905 0.117 Uiso 1 1 calc R . . 
H8B H 0.2523 -0.1352 0.1918 0.117 Uiso 1 1 calc R . . 
H8C H 0.3218 -0.1827 0.1328 0.117 Uiso 1 1 calc R . . 
C9 C 0.3187(9) 0.0492(11) 0.2140(8) 0.065(4) Uani 1 1 d . . . 
H9A H 0.2671 0.0764 0.1615 0.097 Uiso 1 1 calc R . . 
H9B H 0.3696 0.1030 0.2356 0.097 Uiso 1 1 calc R . . 
H9C H 0.2893 0.0307 0.2643 0.097 Uiso 1 1 calc R . . 
C11 C 0.8111(8) 0.1451(9) 0.6364(7) 0.049(3) Uani 1 1 d . . . 
H11A H 0.8734 0.1555 0.6841 0.073 Uiso 1 1 calc R . . 
H11B H 0.7705 0.0932 0.6578 0.073 Uiso 1 1 calc R . . 
H11C H 0.7751 0.2118 0.6242 0.073 Uiso 1 1 calc R . . 
C10 C 0.9341(7) 0.1186(10) 0.5546(8) 0.052(3) Uani 1 1 d . . . 
H10A H 0.9738 0.1354 0.6172 0.078 Uiso 1 1 calc R . . 
H10B H 0.9411 0.1747 0.5122 0.078 Uiso 1 1 calc R . . 
H10C H 0.9571 0.0522 0.5347 0.078 Uiso 1 1 calc R . . 
C13 C 0.7014(8) -0.1019(9) 0.5447(8) 0.051(3) Uani 1 1 d . . . 
H13A H 0.7621 -0.0996 0.5955 0.077 Uiso 1 1 calc R . . 
H13B H 0.6752 -0.1736 0.5378 0.077 Uiso 1 1 calc R . . 
H13C H 0.6521 -0.0544 0.5583 0.077 Uiso 1 1 calc R . . 
C12 C 0.8127(7) -0.1248(9) 0.4500(8) 0.048(3) Uani 1 1 d . . . 
H12A H 0.8712 -0.0935 0.4926 0.072 Uiso 1 1 calc R . . 
H12B H 0.8186 -0.1197 0.3866 0.072 Uiso 1 1 calc R . . 
H12C H 0.8076 -0.1987 0.4661 0.072 Uiso 1 1 calc R . . 
C17 C 0.5927(8) 0.2591(9) 0.3021(7) 0.048(3) Uani 1 1 d . . . 
H17A H 0.5903 0.3310 0.2785 0.072 Uiso 1 1 calc R . . 
H17B H 0.5375 0.2186 0.2636 0.072 Uiso 1 1 calc R . . 
H17C H 0.6554 0.2263 0.3004 0.072 Uiso 1 1 calc R . . 
C16 C 0.6629(8) 0.3336(9) 0.4585(8) 0.053(3) Uani 1 1 d . . . 
H16A H 0.6586 0.4020 0.4279 0.079 Uiso 1 1 calc R . . 
H16B H 0.7286 0.3033 0.4646 0.079 Uiso 1 1 calc R . . 
H16C H 0.6521 0.3424 0.5199 0.079 Uiso 1 1 calc R . . 
C15 C 0.4824(7) 0.3043(9) 0.4002(8) 0.049(3) Uani 1 1 d . . . 
H15A H 0.4744 0.3745 0.3726 0.073 Uiso 1 1 calc R . . 
H15B H 0.4762 0.3084 0.4636 0.073 Uiso 1 1 calc R . . 
H15C H 0.4310 0.2577 0.3637 0.073 Uiso 1 1 calc R . . 
C14 C 0.5847(7) 0.2611(8) 0.4014(7) 0.031(2) Uani 1 1 d . . . 
K1 K 0.51088(15) -0.10107(17) 0.35744(14) 0.0316(6) Uani 1 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 
As1 0.0220(6) 0.0440(7) 0.0252(6) 0.0016(6) 0.0060(4) -0.0010(6) 
N1 0.052(6) 0.043(6) 0.034(5) 0.005(5) 0.014(5) -0.002(5) 
N2 0.038(5) 0.044(6) 0.032(5) -0.005(4) 0.017(4) -0.004(5) 
N3 0.031(5) 0.047(6) 0.031(5) -0.010(4) 0.015(4) 0.004(4) 
N4 0.027(5) 0.089(9) 0.037(5) -0.023(5) 0.001(4) -0.004(5) 
N5 0.021(4) 0.049(6) 0.025(5) 0.003(4) 0.003(3) 0.009(4) 
P1 0.0230(14) 0.0351(17) 0.0323(16) 0.0038(13) 0.0100(12) 0.0013(12) 
C1 0.085(11) 0.099(12) 0.071(10) 0.005(9) 0.023(9) -0.027(9) 
C2 0.073(10) 0.108(13) 0.060(9) 0.021(9) 0.004(8) 0.019(9) 
C3 0.083(9) 0.050(8) 0.041(7) -0.005(6) 0.026(7) 0.015(7) 
C4 0.047(7) 0.051(8) 0.055(8) -0.002(6) 0.027(6) 0.005(6) 
C5 0.057(8) 0.057(9) 0.055(8) -0.004(7) 0.024(7) -0.015(7) 
C6 0.048(7) 0.074(10) 0.022(6) 0.002(6) 0.013(5) 0.001(7) 
C7 0.049(7) 0.073(9) 0.030(7) 0.015(6) 0.009(6) 0.017(7) 
C8 0.079(10) 0.104(12) 0.061(9) -0.020(9) 0.033(8) -0.023(9) 
C9 0.060(8) 0.087(11) 0.052(8) 0.011(7) 0.023(7) 0.014(8) 
C11 0.042(7) 0.062(9) 0.034(7) -0.009(6) -0.004(5) 0.006(6) 
C10 0.022(6) 0.082(10) 0.048(7) -0.006(7) 0.001(5) -0.008(6) 
C13 0.032(6) 0.068(10) 0.056(8) 0.011(7) 0.014(6) 0.010(6) 
C12 0.033(7) 0.057(8) 0.053(7) 0.004(6) 0.009(6) 0.009(6) 
C17 0.046(7) 0.067(9) 0.036(6) 0.016(6) 0.018(5) 0.003(6) 
C16 0.055(8) 0.052(9) 0.052(8) 0.017(6) 0.017(6) -0.003(6) 
C15 0.044(7) 0.054(8) 0.046(7) 0.001(6) 0.007(6) 0.011(6) 
C14 0.022(5) 0.030(6) 0.040(6) 0.003(5) 0.007(5) -0.001(5) 
K1 0.0285(12) 0.0425(16) 0.0248(12) -0.0004(11) 0.0088(10) -0.0007(11) 
 
_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 
As1 N4 1.871(8) . ? 
As1 N5 1.880(9) . ? 
As1 P1 2.260(3) . ? 
As1 K1 3.846(3) . ? 
N1 C2 1.403(14) . ? 
N1 C1 1.479(14) . ? 
N1 C3 1.481(13) . ? 
N1 K1 2.941(9) . ? 
N2 C5 1.451(13) . ? 
N2 C6 1.460(12) . ? 
N2 C4 1.464(13) . ? 
N2 K1 2.920(8) . ? 
N3 C8 1.413(14) . ? 
N3 C7 1.446(12) . ? 
N3 C9 1.451(14) . ? 
N3 K1 2.938(8) . ? 
N4 C11 1.417(13) . ? 
N4 C10 1.443(12) . ? 
N5 C12 1.463(12) . ? 
N5 C13 1.493(12) . ? 
N5 K1 2.990(7) . ? 
P1 C14 1.893(10) . ? 
P1 K1 3.314(4) . ? 
P1 K1 3.461(3) 3_656 ? 
C3 C4 1.501(15) . ? 
C6 C7 1.502(15) . ? 
C9 K1 3.531(12) . ? 
C13 K1 3.321(11) . ? 
C17 C14 1.524(13) . ? 
C16 C14 1.513(14) . ? 
C15 C14 1.533(13) . ? 
K1 P1 3.461(3) 3_656 ? 
 
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 
N4 As1 N5 100.7(4) . . ? 
N4 As1 P1 107.1(3) . . ? 
N5 As1 P1 97.7(2) . . ? 
N4 As1 K1 138.0(3) . . ? 
N5 As1 K1 49.6(2) . . ? 
P1 As1 K1 59.14(8) . . ? 
C2 N1 C1 107.0(10) . . ? 
C2 N1 C3 111.8(10) . . ? 
C1 N1 C3 108.2(9) . . ? 
C2 N1 K1 109.7(8) . . ? 
C1 N1 K1 110.2(7) . . ? 
C3 N1 K1 109.9(7) . . ? 
C5 N2 C6 110.5(9) . . ? 
C5 N2 C4 109.3(8) . . ? 
C6 N2 C4 111.3(9) . . ? 
C5 N2 K1 104.1(6) . . ? 
C6 N2 K1 112.1(6) . . ? 
C4 N2 K1 109.3(6) . . ? 
C8 N3 C7 112.1(9) . . ? 
C8 N3 C9 110.6(9) . . ? 
C7 N3 C9 108.7(9) . . ? 
C8 N3 K1 116.8(8) . . ? 
C7 N3 K1 106.2(6) . . ? 
C9 N3 K1 101.7(6) . . ? 
C11 N4 C10 113.6(8) . . ? 
C11 N4 As1 127.0(7) . . ? 
C10 N4 As1 118.3(7) . . ? 
C12 N5 C13 108.0(8) . . ? 
C12 N5 As1 110.4(6) . . ? 
C13 N5 As1 116.0(7) . . ? 
C12 N5 K1 130.6(6) . . ? 
C13 N5 K1 89.1(5) . . ? 
As1 N5 K1 101.9(3) . . ? 
C14 P1 As1 98.1(3) . . ? 
C14 P1 K1 129.0(3) . . ? 
As1 P1 K1 85.02(9) . . ? 
C14 P1 K1 117.7(3) . 3_656 ? 
As1 P1 K1 129.27(11) . 3_656 ? 
K1 P1 K1 97.00(8) . 3_656 ? 
N1 C3 C4 113.5(10) . . ? 
N2 C4 C3 114.0(9) . . ? 
N2 C6 C7 112.9(9) . . ? 
N3 C7 C6 112.6(9) . . ? 
N3 C9 K1 54.6(5) . . ? 
N5 C13 K1 64.2(5) . . ? 
C16 C14 C17 109.5(8) . . ? 
C16 C14 C15 108.7(9) . . ? 
C17 C14 C15 107.9(8) . . ? 
C16 C14 P1 111.8(7) . . ? 
C17 C14 P1 114.1(7) . . ? 
C15 C14 P1 104.5(7) . . ? 
N2 K1 N3 62.3(2) . . ? 
N2 K1 N1 63.2(2) . . ? 
N3 K1 N1 94.6(2) . . ? 
N2 K1 N5 88.9(2) . . ? 
N3 K1 N5 141.3(2) . . ? 
N1 K1 N5 94.4(2) . . ? 
N2 K1 C13 113.7(2) . . ? 
N3 K1 C13 164.4(3) . . ? 
N1 K1 C13 96.6(3) . . ? 
N5 K1 C13 26.7(2) . . ? 
N2 K1 P1 109.12(19) . . ? 
N3 K1 P1 104.13(19) . . ? 
N1 K1 P1 153.4(2) . . ? 
N5 K1 P1 59.21(18) . . ? 
C13 K1 P1 61.9(2) . . ? 
N2 K1 P1 167.59(19) . 3_656 ? 
N3 K1 P1 113.06(16) . 3_656 ? 
N1 K1 P1 107.09(18) . 3_656 ? 
N5 K1 P1 99.99(15) . 3_656 ? 
C13 K1 P1 73.90(19) . 3_656 ? 
P1 K1 P1 83.00(8) . 3_656 ? 
N2 K1 C9 81.1(3) . . ? 
N3 K1 C9 23.7(2) . . ? 
N1 K1 C9 117.3(3) . . ? 
N5 K1 C9 136.7(3) . . ? 
C13 K1 C9 145.9(3) . . ? 
P1 K1 C9 84.5(2) . . ? 
P1 K1 C9 97.9(2) 3_656 . ? 
N2 K1 As1 86.47(17) . . ? 
N3 K1 As1 118.19(18) . . ? 
N1 K1 As1 118.06(19) . . ? 
N5 K1 As1 28.58(17) . . ? 
C13 K1 As1 46.5(2) . . ? 
P1 K1 As1 35.84(5) . . ? 
P1 K1 As1 105.48(7) 3_656 . ? 
C9 K1 As1 108.3(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.992 
_diffrn_reflns_theta_full              22.50 
_diffrn_measured_fraction_theta_full   0.992 
_refine_diff_density_max    0.719 
_refine_diff_density_min   -0.693 
_refine_diff_density_rms    0.110