# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Keith Izod'
_publ_contact_author_email       K.J.IZOD@NCL.AC.UK

_publ_section_title              
;
Mixed Donor-Functionalised Phosphinomethanide Complexes
of the Alkali Metals; Synthesis, Structures, and Solution Dynamics
;
loop_
_publ_author_name
'Keith Izod'
'William Clegg'
'Ross W Harrington'
'Corrine Wills'
'Jonathan Young'

# Attachment 'dalton.cif'

data_ki166_compound12
_database_code_depnum_ccdc_archive 'CCDC 720586'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H49 N Na O2 P Si2'
_chemical_formula_sum            'C28 H49 N Na O2 P Si2'
_chemical_formula_weight         541.82

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   11.7246(16)
_cell_length_b                   21.945(5)
_cell_length_c                   12.9043(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.349(8)
_cell_angle_gamma                90.00
_cell_volume                     3276.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    95525
_cell_measurement_theta_min      4.0
_cell_measurement_theta_max      22.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
High-angle data were weak for this sample, so data collection was restricted
to a maximum 2theta value of 45 degrees.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77315
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.01
_diffrn_reflns_theta_max         22.50
_reflns_number_total             4251
_reflns_number_gt                3354
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Nonius COLLECT'
_computing_cell_refinement       EvalCCD
_computing_data_reduction        EvalCCD
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_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^)+(0.0495P)^2^+3.3118P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4251
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0557
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.145
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Na Na 0.47281(12) 0.55845(7) 0.75667(11) 0.0361(4) Uani 1 1 d . . .
P P 0.23236(8) 0.58442(4) 0.75825(7) 0.0225(3) Uani 1 1 d . . .
N N 0.4716(3) 0.65701(15) 0.6656(2) 0.0408(9) Uani 1 1 d . . .
O1 O 0.4036(2) 0.46063(11) 0.71149(19) 0.0340(6) Uani 1 1 d . . .
O2 O 0.6631(2) 0.52149(12) 0.79130(19) 0.0399(7) Uani 1 1 d . . .
Si1 Si 0.24384(9) 0.67499(4) 0.93472(8) 0.0274(3) Uani 1 1 d . . .
Si2 Si 0.02267(9) 0.67332(5) 0.75744(9) 0.0400(3) Uani 1 1 d . . .
C1 C 0.1598(3) 0.64016(16) 0.8191(3) 0.0279(9) Uani 1 1 d . . .
C2 C 0.2017(3) 0.60014(15) 0.6147(3) 0.0260(9) Uani 1 1 d . . .
C3 C 0.1181(3) 0.56921(16) 0.5446(3) 0.0302(9) Uani 1 1 d . . .
H3 H 0.0777 0.5362 0.5697 0.036 Uiso 1 1 calc R . .
C4 C 0.0923(3) 0.58525(19) 0.4394(3) 0.0404(10) Uani 1 1 d . . .
H4 H 0.0350 0.5634 0.3935 0.048 Uiso 1 1 calc R . .
C5 C 0.1499(4) 0.6327(2) 0.4020(3) 0.0468(11) Uani 1 1 d . . .
H5 H 0.1313 0.6447 0.3305 0.056 Uiso 1 1 calc R . .
C6 C 0.2355(4) 0.66306(19) 0.4692(3) 0.0448(11) Uani 1 1 d . . .
H6 H 0.2760 0.6954 0.4423 0.054 Uiso 1 1 calc R . .
C7 C 0.2638(3) 0.64768(16) 0.5747(3) 0.0318(9) Uani 1 1 d . . .
C8 C 0.3550(3) 0.68509(17) 0.6438(3) 0.0369(10) Uani 1 1 d . . .
H8A H 0.3615 0.7251 0.6097 0.044 Uiso 1 1 calc R . .
H8B H 0.3283 0.6927 0.7116 0.044 Uiso 1 1 calc R . .
C9 C 0.5479(4) 0.6978(2) 0.7376(4) 0.0623(14) Uani 1 1 d . . .
H9A H 0.6255 0.6800 0.7531 0.093 Uiso 1 1 calc R . .
H9B H 0.5166 0.7027 0.8030 0.093 Uiso 1 1 calc R . .
H9C H 0.5522 0.7377 0.7042 0.093 Uiso 1 1 calc R . .
C10 C 0.5205(4) 0.6514(2) 0.5688(4) 0.0582(13) Uani 1 1 d . . .
H10A H 0.4752 0.6218 0.5221 0.087 Uiso 1 1 calc R . .
H10B H 0.6007 0.6374 0.5856 0.087 Uiso 1 1 calc R . .
H10C H 0.5182 0.6911 0.5338 0.087 Uiso 1 1 calc R . .
C11 C 0.1615(3) 0.50930(15) 0.7704(2) 0.0217(8) Uani 1 1 d . . .
C12 C 0.0824(3) 0.50516(16) 0.8395(3) 0.0276(9) Uani 1 1 d . . .
H12 H 0.0564 0.5416 0.8679 0.033 Uiso 1 1 calc R . .
C13 C 0.0401(3) 0.44971(17) 0.8685(3) 0.0310(9) Uani 1 1 d . . .
H13 H -0.0137 0.4486 0.9162 0.037 Uiso 1 1 calc R . .
C14 C 0.0758(3) 0.39650(17) 0.8283(3) 0.0335(9) Uani 1 1 d . . .
H14 H 0.0473 0.3584 0.8477 0.040 Uiso 1 1 calc R . .
C15 C 0.1538(3) 0.39923(16) 0.7593(3) 0.0315(9) Uani 1 1 d . . .
H15 H 0.1780 0.3624 0.7309 0.038 Uiso 1 1 calc R . .
C16 C 0.1981(3) 0.45403(16) 0.7298(2) 0.0232(8) Uani 1 1 d . . .
C17 C 0.2868(3) 0.45286(17) 0.6572(3) 0.0310(9) Uani 1 1 d . . .
H17A H 0.2812 0.4135 0.6192 0.037 Uiso 1 1 calc R . .
H17B H 0.2691 0.4857 0.6044 0.037 Uiso 1 1 calc R . .
C18 C 0.4490(4) 0.40712(18) 0.7663(3) 0.0450(11) Uani 1 1 d . . .
H18A H 0.3982 0.3948 0.8158 0.067 Uiso 1 1 calc R . .
H18B H 0.5264 0.4157 0.8048 0.067 Uiso 1 1 calc R . .
H18C H 0.4534 0.3742 0.7158 0.067 Uiso 1 1 calc R . .
C19 C -0.0890(3) 0.6188(2) 0.6882(4) 0.0496(12) Uani 1 1 d . . .
H19A H -0.0554 0.5952 0.6361 0.074 Uiso 1 1 calc R . .
H19B H -0.1558 0.6419 0.6528 0.074 Uiso 1 1 calc R . .
H19C H -0.1140 0.5911 0.7396 0.074 Uiso 1 1 calc R . .
C20 C 0.0395(4) 0.7336(2) 0.6574(4) 0.0703(16) Uani 1 1 d . . .
H20A H 0.1050 0.7600 0.6847 0.105 Uiso 1 1 calc R . .
H20B H -0.0312 0.7581 0.6432 0.105 Uiso 1 1 calc R . .
H20C H 0.0537 0.7142 0.5923 0.105 Uiso 1 1 calc R . .
C21 C -0.0550(4) 0.7128(3) 0.8553(4) 0.090(2) Uani 1 1 d . . .
H21A H -0.0716 0.6833 0.9080 0.135 Uiso 1 1 calc R . .
H21B H -0.1277 0.7301 0.8189 0.135 Uiso 1 1 calc R . .
H21C H -0.0062 0.7455 0.8900 0.135 Uiso 1 1 calc R . .
C22 C 0.3915(3) 0.63929(17) 0.9710(3) 0.0352(10) Uani 1 1 d . . .
H22A H 0.3830 0.5954 0.9815 0.053 Uiso 1 1 calc R . .
H22B H 0.4316 0.6578 1.0359 0.053 Uiso 1 1 calc R . .
H22C H 0.4364 0.6462 0.9143 0.053 Uiso 1 1 calc R . .
C23 C 0.2685(4) 0.75939(16) 0.9202(3) 0.0397(10) Uani 1 1 d . . .
H23A H 0.3170 0.7661 0.8661 0.060 Uiso 1 1 calc R . .
H23B H 0.3074 0.7760 0.9873 0.060 Uiso 1 1 calc R . .
H23C H 0.1940 0.7799 0.8997 0.060 Uiso 1 1 calc R . .
C24 C 0.1791(4) 0.66884(19) 1.0591(3) 0.0482(11) Uani 1 1 d . . .
H24A H 0.1014 0.6866 1.0475 0.072 Uiso 1 1 calc R . .
H24B H 0.2279 0.6908 1.1158 0.072 Uiso 1 1 calc R . .
H24C H 0.1744 0.6258 1.0785 0.072 Uiso 1 1 calc R . .
C25 C 0.6652(4) 0.5561(2) 0.9662(3) 0.0599(14) Uani 1 1 d . . .
H25A H 0.6530 0.5979 0.9397 0.090 Uiso 1 1 calc R . .
H25B H 0.7103 0.5570 1.0371 0.090 Uiso 1 1 calc R . .
H25C H 0.5902 0.5369 0.9684 0.090 Uiso 1 1 calc R . .
C26 C 0.7291(3) 0.5205(2) 0.8953(3) 0.0438(11) Uani 1 1 d . . .
H26A H 0.8062 0.5388 0.8948 0.053 Uiso 1 1 calc R . .
H26B H 0.7399 0.4780 0.9205 0.053 Uiso 1 1 calc R . .
C27 C 0.7145(3) 0.4834(2) 0.7214(3) 0.0439(11) Uani 1 1 d . . .
H27A H 0.7104 0.4402 0.7424 0.053 Uiso 1 1 calc R . .
H27B H 0.7969 0.4944 0.7244 0.053 Uiso 1 1 calc R . .
C28 C 0.6498(4) 0.4922(2) 0.6107(3) 0.0557(12) Uani 1 1 d . . .
H28A H 0.5675 0.4836 0.6092 0.084 Uiso 1 1 calc R . .
H28B H 0.6809 0.4644 0.5628 0.084 Uiso 1 1 calc R . .
H28C H 0.6591 0.5344 0.5884 0.084 Uiso 1 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
Na 0.0249(8) 0.0379(9) 0.0448(9) 0.0100(7) 0.0034(7) 0.0003(7)
P 0.0222(5) 0.0196(5) 0.0245(5) -0.0005(4) 0.0000(4) -0.0001(4)
N 0.0331(19) 0.043(2) 0.045(2) 0.0164(16) 0.0015(16) -0.0103(16)
O1 0.0338(15) 0.0294(15) 0.0396(15) 0.0030(12) 0.0086(12) 0.0050(12)
O2 0.0343(15) 0.0495(18) 0.0359(16) -0.0037(13) 0.0062(13) 0.0048(13)
Si1 0.0338(6) 0.0203(6) 0.0283(6) -0.0008(4) 0.0051(5) 0.0003(5)
Si2 0.0293(6) 0.0302(6) 0.0563(8) -0.0083(5) -0.0055(5) 0.0089(5)
C1 0.025(2) 0.022(2) 0.035(2) -0.0025(16) 0.0004(16) 0.0026(16)
C2 0.025(2) 0.023(2) 0.029(2) 0.0056(16) 0.0020(17) 0.0034(17)
C3 0.029(2) 0.029(2) 0.031(2) 0.0036(17) -0.0020(17) -0.0022(17)
C4 0.039(2) 0.046(3) 0.033(2) 0.005(2) -0.0074(19) -0.008(2)
C5 0.053(3) 0.052(3) 0.031(2) 0.015(2) -0.004(2) -0.003(2)
C6 0.050(3) 0.041(3) 0.041(3) 0.018(2) 0.001(2) -0.009(2)
C7 0.033(2) 0.027(2) 0.033(2) 0.0071(17) -0.0002(18) -0.0011(18)
C8 0.043(3) 0.028(2) 0.039(2) 0.0080(18) 0.0043(19) -0.0069(19)
C9 0.049(3) 0.061(3) 0.070(3) 0.014(3) -0.010(2) -0.030(3)
C10 0.049(3) 0.061(3) 0.066(3) 0.014(2) 0.014(2) -0.001(2)
C11 0.0198(19) 0.021(2) 0.0218(19) 0.0023(15) -0.0029(15) 0.0006(16)
C12 0.0224(19) 0.028(2) 0.031(2) -0.0004(17) 0.0022(17) 0.0028(17)
C13 0.026(2) 0.035(2) 0.032(2) 0.0033(18) 0.0068(17) -0.0056(18)
C14 0.035(2) 0.026(2) 0.038(2) 0.0044(18) 0.0035(19) -0.0061(18)
C15 0.040(2) 0.021(2) 0.031(2) -0.0046(16) -0.0030(18) 0.0027(18)
C16 0.0245(19) 0.024(2) 0.0196(18) -0.0027(15) -0.0016(15) 0.0012(16)
C17 0.038(2) 0.028(2) 0.026(2) -0.0031(17) 0.0014(17) 0.0059(18)
C18 0.041(2) 0.043(3) 0.052(3) 0.014(2) 0.010(2) 0.009(2)
C19 0.029(2) 0.045(3) 0.071(3) -0.005(2) -0.003(2) 0.003(2)
C20 0.056(3) 0.035(3) 0.106(4) 0.019(3) -0.027(3) 0.009(2)
C21 0.050(3) 0.112(5) 0.100(4) -0.052(4) -0.012(3) 0.041(3)
C22 0.039(2) 0.031(2) 0.032(2) -0.0045(17) -0.0042(18) 0.0005(19)
C23 0.049(3) 0.026(2) 0.042(2) 0.0006(18) -0.002(2) -0.0030(19)
C24 0.067(3) 0.038(3) 0.044(3) -0.002(2) 0.020(2) -0.002(2)
C25 0.044(3) 0.092(4) 0.040(3) -0.009(2) -0.006(2) 0.023(3)
C26 0.033(2) 0.055(3) 0.040(3) 0.000(2) -0.002(2) 0.008(2)
C27 0.037(2) 0.052(3) 0.046(3) -0.005(2) 0.016(2) 0.003(2)
C28 0.057(3) 0.067(3) 0.045(3) -0.003(2) 0.016(2) 0.012(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
Na O1 2.335(3) . ?
Na O2 2.347(3) . ?
Na N 2.461(3) . ?
Na P 2.8796(16) . ?
P C1 1.747(4) . ?
P C2 1.861(3) . ?
P C11 1.864(3) . ?
N C10 1.462(5) . ?
N C9 1.482(5) . ?
N C8 1.484(5) . ?
O1 C18 1.428(4) . ?
O1 C17 1.443(4) . ?
O2 C27 1.433(4) . ?
O2 C26 1.436(4) . ?
Si1 C1 1.817(4) . ?
Si1 C22 1.888(4) . ?
Si1 C24 1.889(4) . ?
Si1 C23 1.889(4) . ?
Si2 C1 1.826(4) . ?
Si2 C20 1.881(5) . ?
Si2 C21 1.884(5) . ?
Si2 C19 1.888(4) . ?
C2 C3 1.397(5) . ?
C2 C7 1.416(5) . ?
C3 C4 1.387(5) . ?
C3 H3 0.950 . ?
C4 C5 1.371(5) . ?
C4 H4 0.950 . ?
C5 C6 1.385(6) . ?
C5 H5 0.950 . ?
C6 C7 1.390(5) . ?
C6 H6 0.950 . ?
C7 C8 1.517(5) . ?
C8 H8A 0.990 . ?
C8 H8B 0.990 . ?
C9 H9A 0.980 . ?
C9 H9B 0.980 . ?
C9 H9C 0.980 . ?
C10 H10A 0.980 . ?
C10 H10B 0.980 . ?
C10 H10C 0.980 . ?
C11 C12 1.390(5) . ?
C11 C16 1.415(5) . ?
C12 C13 1.388(5) . ?
C12 H12 0.950 . ?
C13 C14 1.371(5) . ?
C13 H13 0.950 . ?
C14 C15 1.376(5) . ?
C14 H14 0.950 . ?
C15 C16 1.388(5) . ?
C15 H15 0.950 . ?
C16 C17 1.509(5) . ?
C17 H17A 0.990 . ?
C17 H17B 0.990 . ?
C18 H18A 0.980 . ?
C18 H18B 0.980 . ?
C18 H18C 0.980 . ?
C19 H19A 0.980 . ?
C19 H19B 0.980 . ?
C19 H19C 0.980 . ?
C20 H20A 0.980 . ?
C20 H20B 0.980 . ?
C20 H20C 0.980 . ?
C21 H21A 0.980 . ?
C21 H21B 0.980 . ?
C21 H21C 0.980 . ?
C22 H22A 0.980 . ?
C22 H22B 0.980 . ?
C22 H22C 0.980 . ?
C23 H23A 0.980 . ?
C23 H23B 0.980 . ?
C23 H23C 0.980 . ?
C24 H24A 0.980 . ?
C24 H24B 0.980 . ?
C24 H24C 0.980 . ?
C25 C26 1.494(6) . ?
C25 H25A 0.980 . ?
C25 H25B 0.980 . ?
C25 H25C 0.980 . ?
C26 H26A 0.990 . ?
C26 H26B 0.990 . ?
C27 C28 1.517(6) . ?
C27 H27A 0.990 . ?
C27 H27B 0.990 . ?
C28 H28A 0.980 . ?
C28 H28B 0.980 . ?
C28 H28C 0.980 . ?

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 Na O2 90.62(10) . . ?
O1 Na N 135.56(11) . . ?
O2 Na N 109.05(11) . . ?
O1 Na P 83.27(7) . . ?
O2 Na P 165.53(9) . . ?
N Na P 84.24(9) . . ?
C1 P C2 106.75(16) . . ?
C1 P C11 108.97(16) . . ?
C2 P C11 103.35(15) . . ?
C1 P Na 133.65(12) . . ?
C2 P Na 93.47(11) . . ?
C11 P Na 106.02(11) . . ?
C10 N C9 107.8(3) . . ?
C10 N C8 110.5(3) . . ?
C9 N C8 108.2(3) . . ?
C10 N Na 111.1(3) . . ?
C9 N Na 106.0(2) . . ?
C8 N Na 112.9(2) . . ?
C18 O1 C17 113.0(3) . . ?
C18 O1 Na 123.1(2) . . ?
C17 O1 Na 119.6(2) . . ?
C27 O2 C26 111.2(3) . . ?
C27 O2 Na 124.5(2) . . ?
C26 O2 Na 122.3(2) . . ?
C1 Si1 C22 112.43(16) . . ?
C1 Si1 C24 115.37(19) . . ?
C22 Si1 C24 103.81(19) . . ?
C1 Si1 C23 113.73(17) . . ?
C22 Si1 C23 106.41(18) . . ?
C24 Si1 C23 104.10(18) . . ?
C1 Si2 C20 113.34(19) . . ?
C1 Si2 C21 112.2(2) . . ?
C20 Si2 C21 104.6(3) . . ?
C1 Si2 C19 116.62(18) . . ?
C20 Si2 C19 105.2(2) . . ?
C21 Si2 C19 103.6(2) . . ?
P C1 Si1 115.15(19) . . ?
P C1 Si2 122.8(2) . . ?
Si1 C1 Si2 120.78(19) . . ?
C3 C2 C7 118.1(3) . . ?
C3 C2 P 123.8(3) . . ?
C7 C2 P 118.1(3) . . ?
C4 C3 C2 121.9(3) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 122.0(4) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 119.0 . . ?
C6 C7 C2 118.7(3) . . ?
C6 C7 C8 118.5(3) . . ?
C2 C7 C8 122.7(3) . . ?
N C8 C7 115.2(3) . . ?
N C8 H8A 108.5 . . ?
C7 C8 H8A 108.5 . . ?
N C8 H8B 108.5 . . ?
C7 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
N C9 H9A 109.5 . . ?
N C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N C10 H10A 109.5 . . ?
N C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 117.1(3) . . ?
C12 C11 P 117.7(3) . . ?
C16 C11 P 124.1(2) . . ?
C13 C12 C11 122.4(3) . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C14 C15 C16 122.2(3) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C11 119.4(3) . . ?
C15 C16 C17 118.9(3) . . ?
C11 C16 C17 121.7(3) . . ?
O1 C17 C16 113.0(3) . . ?
O1 C17 H17A 109.0 . . ?
C16 C17 H17A 109.0 . . ?
O1 C17 H17B 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
O1 C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si2 C19 H19A 109.5 . . ?
Si2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O2 C26 C25 108.5(3) . . ?
O2 C26 H26A 110.0 . . ?
C25 C26 H26A 110.0 . . ?
O2 C26 H26B 110.0 . . ?
C25 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
O2 C27 C28 108.8(3) . . ?
O2 C27 H27A 109.9 . . ?
C28 C27 H27A 109.9 . . ?
O2 C27 H27B 109.9 . . ?
C28 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        22.50
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.057

#===END

data_ki165_compound13
_database_code_depnum_ccdc_archive 'CCDC 720587'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H78 K2 N2 O2 P2 Si4'
_chemical_formula_sum            'C48 H78 K2 N2 O2 P2 Si4'
_chemical_formula_weight         967.62

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'
Si Si 0.0817 0.0704 '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'

_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                   9.8748(15)
_cell_length_b                   10.9613(19)
_cell_length_c                   14.189(4)
_cell_angle_alpha                86.361(18)
_cell_angle_beta                 88.243(18)
_cell_angle_gamma                66.81(2)
_cell_volume                     1408.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6390
_cell_measurement_theta_min      4.7
_cell_measurement_theta_max      25

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19414
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.65
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4905
_reflns_number_gt                3356
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Nonius COLLECT'
_computing_cell_refinement       EvalCCD
_computing_data_reduction        EvalCCD
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_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^)+(0.0415P)^2^+0.6680P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4905
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0508
_refine_ls_wR_factor_ref         0.1077
_refine_ls_wR_factor_gt          0.0960
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K K -0.09497(7) 1.05738(6) 0.36297(5) 0.0317(2) Uani 1 1 d . . .
P P 0.22700(8) 0.85498(7) 0.30569(5) 0.02004(19) Uani 1 1 d . . .
Si1 Si 0.12966(10) 0.64545(8) 0.23987(6) 0.0296(2) Uani 1 1 d . . .
Si2 Si 0.45993(9) 0.61073(8) 0.20410(6) 0.0296(2) Uani 1 1 d . . .
O O 0.0762(2) 1.13251(17) 0.47859(14) 0.0289(5) Uani 1 1 d . . .
N N -0.0292(3) 1.1255(2) 0.17396(18) 0.0316(6) Uani 1 1 d . . .
C1 C 0.2798(3) 0.6980(3) 0.2595(2) 0.0241(7) Uani 1 1 d . . .
C2 C 0.3173(3) 0.9498(2) 0.23258(19) 0.0196(6) Uani 1 1 d . . .
C3 C 0.4576(3) 0.9437(3) 0.2540(2) 0.0244(7) Uani 1 1 d . . .
H3 H 0.5065 0.8930 0.3088 0.029 Uiso 1 1 calc R . .
C4 C 0.5269(3) 1.0104(3) 0.1967(2) 0.0317(8) Uani 1 1 d . . .
H4 H 0.6221 1.0045 0.2126 0.038 Uiso 1 1 calc R . .
C5 C 0.4573(3) 1.0847(3) 0.1173(2) 0.0351(8) Uani 1 1 d . . .
H5 H 0.5040 1.1304 0.0782 0.042 Uiso 1 1 calc R . .
C6 C 0.3188(3) 1.0923(3) 0.0950(2) 0.0309(7) Uani 1 1 d . . .
H6 H 0.2710 1.1435 0.0401 0.037 Uiso 1 1 calc R . .
C7 C 0.2475(3) 1.0262(3) 0.1516(2) 0.0219(7) Uani 1 1 d . . .
C8 C 0.0980(3) 1.0361(3) 0.1203(2) 0.0267(7) Uani 1 1 d . . .
H8A H 0.0852 1.0671 0.0528 0.032 Uiso 1 1 calc R . .
H8B H 0.0970 0.9460 0.1254 0.032 Uiso 1 1 calc R . .
C9 C -0.1642(3) 1.1278(3) 0.1312(3) 0.0448(9) Uani 1 1 d . . .
H9A H -0.2499 1.1803 0.1688 0.067 Uiso 1 1 calc R . .
H9B H -0.1588 1.0367 0.1297 0.067 Uiso 1 1 calc R . .
H9C H -0.1737 1.1677 0.0667 0.067 Uiso 1 1 calc R . .
C10 C -0.0320(4) 1.2614(3) 0.1705(3) 0.0431(9) Uani 1 1 d . . .
H10A H 0.0565 1.2599 0.2008 0.065 Uiso 1 1 calc R . .
H10B H -0.1197 1.3198 0.2038 0.065 Uiso 1 1 calc R . .
H10C H -0.0347 1.2947 0.1045 0.065 Uiso 1 1 calc R . .
C11 C 0.3234(3) 0.8418(3) 0.4195(2) 0.0209(6) Uani 1 1 d . . .
C12 C 0.3985(3) 0.7161(3) 0.4645(2) 0.0256(7) Uani 1 1 d . . .
H12 H 0.4038 0.6393 0.4344 0.031 Uiso 1 1 calc R . .
C13 C 0.4652(3) 0.7004(3) 0.5514(2) 0.0308(7) Uani 1 1 d . . .
H13 H 0.5144 0.6139 0.5801 0.037 Uiso 1 1 calc R . .
C14 C 0.4606(3) 0.8104(3) 0.5967(2) 0.0301(7) Uani 1 1 d . . .
H14 H 0.5089 0.7998 0.6554 0.036 Uiso 1 1 calc R . .
C15 C 0.3842(3) 0.9362(3) 0.5549(2) 0.0256(7) Uani 1 1 d . . .
H15 H 0.3804 1.0120 0.5856 0.031 Uiso 1 1 calc R . .
C16 C 0.3132(3) 0.9537(3) 0.4688(2) 0.0217(7) Uani 1 1 d . . .
C17 C 0.2206(3) 1.0959(3) 0.4345(2) 0.0256(7) Uani 1 1 d . . .
H17A H 0.2671 1.1562 0.4526 0.031 Uiso 1 1 calc R . .
H17B H 0.2117 1.1024 0.3649 0.031 Uiso 1 1 calc R . .
C18 C -0.0097(4) 1.2728(3) 0.4653(3) 0.0411(9) Uani 1 1 d . . .
H18A H 0.0439 1.3221 0.4904 0.062 Uiso 1 1 calc R . .
H18B H -0.1041 1.2953 0.4987 0.062 Uiso 1 1 calc R . .
H18C H -0.0277 1.2968 0.3978 0.062 Uiso 1 1 calc R . .
C19 C -0.0572(3) 0.7687(3) 0.2773(3) 0.0411(9) Uani 1 1 d . . .
H19A H -0.0555 0.7832 0.3446 0.062 Uiso 1 1 calc R . .
H19B H -0.1322 0.7335 0.2662 0.062 Uiso 1 1 calc R . .
H19C H -0.0808 0.8531 0.2405 0.062 Uiso 1 1 calc R . .
C20 C 0.0984(4) 0.6249(4) 0.1122(3) 0.0541(10) Uani 1 1 d . . .
H20A H 0.0634 0.7119 0.0776 0.081 Uiso 1 1 calc R . .
H20B H 0.0245 0.5865 0.1086 0.081 Uiso 1 1 calc R . .
H20C H 0.1911 0.5658 0.0840 0.081 Uiso 1 1 calc R . .
C21 C 0.1489(4) 0.4833(3) 0.3046(3) 0.0487(10) Uani 1 1 d . . .
H21A H 0.2342 0.4105 0.2797 0.073 Uiso 1 1 calc R . .
H21B H 0.0596 0.4669 0.2957 0.073 Uiso 1 1 calc R . .
H21C H 0.1627 0.4885 0.3721 0.073 Uiso 1 1 calc R . .
C22 C 0.4899(4) 0.6915(3) 0.0882(2) 0.0429(9) Uani 1 1 d . . .
H22A H 0.4088 0.7048 0.0452 0.064 Uiso 1 1 calc R . .
H22B H 0.5833 0.6341 0.0599 0.064 Uiso 1 1 calc R . .
H22C H 0.4931 0.7777 0.0993 0.064 Uiso 1 1 calc R . .
C23 C 0.4886(4) 0.4368(3) 0.1743(3) 0.0453(9) Uani 1 1 d . . .
H23A H 0.4946 0.3823 0.2327 0.068 Uiso 1 1 calc R . .
H23B H 0.5804 0.3979 0.1382 0.068 Uiso 1 1 calc R . .
H23C H 0.4058 0.4400 0.1365 0.068 Uiso 1 1 calc R . .
C24 C 0.6266(3) 0.5851(3) 0.2777(2) 0.0406(9) Uani 1 1 d . . .
H24A H 0.6163 0.6699 0.3022 0.061 Uiso 1 1 calc R . .
H24B H 0.7157 0.5514 0.2384 0.061 Uiso 1 1 calc R . .
H24C H 0.6342 0.5206 0.3305 0.061 Uiso 1 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
K 0.0261(4) 0.0336(4) 0.0339(4) 0.0010(3) 0.0079(3) -0.0112(3)
P 0.0211(4) 0.0187(4) 0.0212(4) 0.0005(3) 0.0008(3) -0.0090(3)
Si1 0.0391(5) 0.0259(5) 0.0297(5) 0.0023(4) -0.0067(4) -0.0191(4)
Si2 0.0345(5) 0.0225(5) 0.0267(5) -0.0024(4) 0.0032(4) -0.0058(4)
O 0.0276(11) 0.0188(11) 0.0382(14) -0.0008(9) 0.0107(10) -0.0079(9)
N 0.0273(14) 0.0265(14) 0.0338(16) 0.0050(12) 0.0010(12) -0.0039(11)
C1 0.0311(16) 0.0203(15) 0.0217(17) -0.0028(13) 0.0004(13) -0.0109(13)
C2 0.0236(15) 0.0170(14) 0.0188(17) -0.0052(12) 0.0043(13) -0.0083(12)
C3 0.0258(16) 0.0276(16) 0.0213(17) -0.0030(13) 0.0029(13) -0.0121(13)
C4 0.0302(17) 0.0402(19) 0.033(2) -0.0050(16) 0.0059(15) -0.0226(15)
C5 0.042(2) 0.041(2) 0.030(2) 0.0026(16) 0.0103(16) -0.0261(16)
C6 0.0397(19) 0.0314(18) 0.0227(18) 0.0053(14) 0.0021(15) -0.0162(15)
C7 0.0240(15) 0.0202(15) 0.0206(17) -0.0048(13) 0.0019(13) -0.0072(12)
C8 0.0301(17) 0.0244(16) 0.0203(17) 0.0019(13) -0.0005(13) -0.0055(13)
C9 0.0289(18) 0.044(2) 0.053(2) 0.0097(18) -0.0028(17) -0.0073(16)
C10 0.047(2) 0.0299(19) 0.041(2) -0.0029(16) 0.0008(17) -0.0026(16)
C11 0.0190(14) 0.0247(16) 0.0215(17) -0.0003(13) 0.0043(12) -0.0118(12)
C12 0.0284(16) 0.0247(16) 0.0241(18) -0.0009(13) 0.0006(14) -0.0109(13)
C13 0.0342(18) 0.0270(17) 0.029(2) 0.0058(14) -0.0009(15) -0.0106(14)
C14 0.0298(17) 0.0397(19) 0.0227(18) 0.0001(15) -0.0037(14) -0.0158(15)
C15 0.0277(16) 0.0317(18) 0.0239(18) -0.0062(14) 0.0055(14) -0.0184(14)
C16 0.0208(15) 0.0256(16) 0.0225(18) -0.0010(13) 0.0067(13) -0.0136(12)
C17 0.0295(16) 0.0252(16) 0.0256(18) -0.0031(13) 0.0095(14) -0.0147(13)
C18 0.0405(19) 0.0224(17) 0.051(2) 0.0006(16) 0.0111(17) -0.0036(15)
C19 0.0369(19) 0.043(2) 0.053(2) 0.0028(17) -0.0067(17) -0.0269(16)
C20 0.066(2) 0.061(3) 0.042(2) -0.004(2) -0.015(2) -0.031(2)
C21 0.060(2) 0.035(2) 0.062(3) 0.0082(18) -0.010(2) -0.0299(18)
C22 0.054(2) 0.0353(19) 0.032(2) -0.0038(16) 0.0112(17) -0.0091(17)
C23 0.058(2) 0.0284(18) 0.041(2) -0.0063(16) -0.0009(18) -0.0067(16)
C24 0.0302(17) 0.0349(19) 0.047(2) -0.0025(16) 0.0070(16) -0.0031(15)

_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
K P 3.1947(13) . ?
K O 2.769(2) . ?
K O 2.924(2) 2_576 ?
K N 2.862(3) . ?
K C14 3.365(3) 2_576 ?
K C15 3.028(3) 2_576 ?
K C16 3.195(3) 2_576 ?
P C1 1.754(3) . ?
P C2 1.867(3) . ?
P C11 1.868(3) . ?
Si1 C1 1.824(3) . ?
Si1 C19 1.892(3) . ?
Si1 C20 1.889(4) . ?
Si1 C21 1.891(3) . ?
Si2 C1 1.835(3) . ?
Si2 C22 1.889(3) . ?
Si2 C23 1.887(3) . ?
Si2 C24 1.893(3) . ?
O K 2.924(2) 2_576 ?
O C17 1.453(3) . ?
O C18 1.438(3) . ?
N C8 1.478(4) . ?
N C9 1.472(4) . ?
N C10 1.476(4) . ?
C2 C3 1.402(4) . ?
C2 C7 1.404(4) . ?
C3 H3 0.950 . ?
C3 C4 1.396(4) . ?
C4 H4 0.950 . ?
C4 C5 1.377(4) . ?
C5 H5 0.950 . ?
C5 C6 1.382(4) . ?
C6 H6 0.950 . ?
C6 C7 1.399(4) . ?
C7 C8 1.515(4) . ?
C8 H8A 0.990 . ?
C8 H8B 0.990 . ?
C9 H9A 0.980 . ?
C9 H9B 0.980 . ?
C9 H9C 0.980 . ?
C10 H10A 0.980 . ?
C10 H10B 0.980 . ?
C10 H10C 0.980 . ?
C11 C12 1.403(4) . ?
C11 C16 1.419(4) . ?
C12 H12 0.950 . ?
C12 C13 1.385(4) . ?
C13 H13 0.950 . ?
C13 C14 1.386(4) . ?
C14 K 3.365(3) 2_576 ?
C14 H14 0.950 . ?
C14 C15 1.388(4) . ?
C15 K 3.028(3) 2_576 ?
C15 H15 0.950 . ?
C15 C16 1.392(4) . ?
C16 K 3.195(3) 2_576 ?
C16 C17 1.520(4) . ?
C17 H17A 0.990 . ?
C17 H17B 0.990 . ?
C18 H18A 0.980 . ?
C18 H18B 0.980 . ?
C18 H18C 0.980 . ?
C19 H19A 0.980 . ?
C19 H19B 0.980 . ?
C19 H19C 0.980 . ?
C20 H20A 0.980 . ?
C20 H20B 0.980 . ?
C20 H20C 0.980 . ?
C21 H21A 0.980 . ?
C21 H21B 0.980 . ?
C21 H21C 0.980 . ?
C22 H22A 0.980 . ?
C22 H22B 0.980 . ?
C22 H22C 0.980 . ?
C23 H23A 0.980 . ?
C23 H23B 0.980 . ?
C23 H23C 0.980 . ?
C24 H24A 0.980 . ?
C24 H24B 0.980 . ?
C24 H24C 0.980 . ?

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
P K O 79.49(5) . . ?
P K O 86.21(5) . 2_576 ?
P K N 70.74(5) . . ?
P K C14 161.61(6) . 2_576 ?
P K C15 141.62(6) . 2_576 ?
P K C16 132.03(6) . 2_576 ?
O K O 82.99(6) . 2_576 ?
O K N 105.72(7) . . ?
O K N 152.92(6) 2_576 . ?
O K C14 116.44(7) . 2_576 ?
O K C14 86.79(7) 2_576 2_576 ?
O K C15 116.59(7) . 2_576 ?
O K C15 63.45(7) 2_576 2_576 ?
O K C16 93.10(7) . 2_576 ?
O K C16 45.82(6) 2_576 2_576 ?
N K C14 110.67(8) . 2_576 ?
N K C15 128.96(8) . 2_576 ?
N K C16 153.69(8) . 2_576 ?
C14 K C15 24.36(7) 2_576 2_576 ?
C14 K C16 43.29(8) 2_576 2_576 ?
C15 K C16 25.66(7) 2_576 2_576 ?
K P C1 128.66(10) . . ?
K P C2 108.21(9) . . ?
K P C11 99.02(9) . . ?
C1 P C2 107.75(13) . . ?
C1 P C11 110.56(13) . . ?
C2 P C11 98.38(12) . . ?
C1 Si1 C19 113.71(14) . . ?
C1 Si1 C20 114.85(16) . . ?
C1 Si1 C21 114.61(15) . . ?
C19 Si1 C20 102.33(17) . . ?
C19 Si1 C21 104.56(16) . . ?
C20 Si1 C21 105.47(17) . . ?
C1 Si2 C22 114.54(14) . . ?
C1 Si2 C23 112.21(15) . . ?
C1 Si2 C24 116.09(14) . . ?
C22 Si2 C23 104.21(15) . . ?
C22 Si2 C24 104.97(16) . . ?
C23 Si2 C24 103.54(16) . . ?
K O K 97.01(6) . 2_576 ?
K O C17 107.58(16) . . ?
K O C17 109.00(15) 2_576 . ?
K O C18 95.32(18) . . ?
K O C18 131.59(17) 2_576 . ?
C17 O C18 111.3(2) . . ?
K N C8 122.23(17) . . ?
K N C9 96.22(18) . . ?
K N C10 108.58(19) . . ?
C8 N C9 107.8(2) . . ?
C8 N C10 110.9(2) . . ?
C9 N C10 109.7(2) . . ?
P C1 Si1 115.31(15) . . ?
P C1 Si2 123.23(15) . . ?
Si1 C1 Si2 119.46(15) . . ?
P C2 C3 121.9(2) . . ?
P C2 C7 120.2(2) . . ?
C3 C2 C7 117.9(2) . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.5(3) . . ?
H3 C3 C4 119.3 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0(3) . . ?
H4 C4 C5 120.0 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.4(3) . . ?
H5 C5 C6 120.3 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.4(3) . . ?
H6 C6 C7 119.3 . . ?
C2 C7 C6 119.8(3) . . ?
C2 C7 C8 122.2(2) . . ?
C6 C7 C8 118.0(3) . . ?
N C8 C7 115.4(2) . . ?
N C8 H8A 108.4 . . ?
N C8 H8B 108.4 . . ?
C7 C8 H8A 108.4 . . ?
C7 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
N C9 H9A 109.5 . . ?
N C9 H9B 109.5 . . ?
N C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N C10 H10A 109.5 . . ?
N C10 H10B 109.5 . . ?
N C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P C11 C12 119.4(2) . . ?
P C11 C16 123.3(2) . . ?
C12 C11 C16 117.0(3) . . ?
C11 C12 H12 119.0 . . ?
C11 C12 C13 122.1(3) . . ?
H12 C12 C13 119.0 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.4(3) . . ?
H13 C13 C14 119.8 . . ?
K C14 C13 97.02(19) 2_576 . ?
K C14 H14 108.0 2_576 . ?
K C14 C15 64.11(15) 2_576 . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.9(3) . . ?
H14 C14 C15 120.6 . . ?
K C15 C14 91.53(16) 2_576 . ?
K C15 H15 94.7 2_576 . ?
K C15 C16 83.87(16) 2_576 . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.4(3) . . ?
H15 C15 C16 119.3 . . ?
K C16 C11 100.52(16) 2_576 . ?
K C16 C15 70.46(15) 2_576 . ?
K C16 C17 95.38(15) 2_576 . ?
C11 C16 C15 120.2(3) . . ?
C11 C16 C17 123.0(3) . . ?
C15 C16 C17 116.8(3) . . ?
O C17 C16 107.3(2) . . ?
O C17 H17A 110.2 . . ?
O C17 H17B 110.2 . . ?
C16 C17 H17A 110.2 . . ?
C16 C17 H17B 110.2 . . ?
H17A C17 H17B 108.5 . . ?
O C18 H18A 109.5 . . ?
O C18 H18B 109.5 . . ?
O C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C19 H19A 109.5 . . ?
Si1 C19 H19B 109.5 . . ?
Si1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
Si1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C23 H23A 109.5 . . ?
Si2 C23 H23B 109.5 . . ?
Si2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.059

#===END