Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Keith Izod'
'W. Clegg'
'Ross W. Harrington'
'John C. Stewart'

_publ_contact_author_name        'Keith Izod'
_publ_contact_author_address     
;
Department of Chemistry
Bedson Building
University of Newcastle
Newcastle Upon Tyne
NE1 7RU
UNITED KINGDOM
;

_publ_contact_author_email       K.J.IZOD@NCL.AC.UK

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Alkali Metal Complexes of a Naphthylamine-Substituted
Phosphanide.
;

data_ki283_2
_database_code_depnum_ccdc_archive 'CCDC 662785'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H72 Li2 N2 O P2 Si4'
_chemical_formula_sum            'C42 H72 Li2 N2 O P2 Si4'
_chemical_formula_weight         809.20

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'
Li Li -0.0003 0.0001 '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'
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'
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   'P 21/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                   17.426(4)
_cell_length_b                   11.688(3)
_cell_length_c                   25.1022(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.394(11)
_cell_angle_gamma                90.00
_cell_volume                     4973.4(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    85
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       slab
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1752
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.98
_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            38124
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         4.21
_diffrn_reflns_theta_max         24.00
_reflns_number_total             7746
_reflns_number_gt                5226
_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^)+(0.0320P)^2^+6.4283P] 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         7746
_refine_ls_number_parameters     516
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1224
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_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
P1 P 0.83817(6) 0.09363(7) 0.60774(3) 0.0295(2) Uani 1 1 d . . .
P2 P 0.74255(5) -0.12994(7) 0.70079(3) 0.0255(2) Uani 1 1 d . . .
Si1 Si 0.88543(6) 0.28372(9) 0.53166(4) 0.0368(3) Uani 1 1 d . . .
Si2 Si 0.76708(6) 0.08122(9) 0.48288(4) 0.0388(3) Uani 1 1 d . . .
Si3 Si 0.74480(6) -0.22568(9) 0.82328(4) 0.0353(3) Uani 1 1 d . . .
Si4 Si 0.63451(6) -0.01189(9) 0.77574(4) 0.0366(3) Uani 1 1 d . . .
N1 N 0.94191(15) -0.0094(2) 0.71173(10) 0.0301(7) Uani 1 1 d . . .
N2 N 0.82966(18) -0.2525(2) 0.61953(11) 0.0337(7) Uani 1 1 d . . .
Li1 Li 0.8489(3) -0.0905(5) 0.6564(2) 0.0313(13) Uani 1 1 d . . .
C1 C 0.80731(19) 0.1795(3) 0.54255(12) 0.0262(8) Uani 1 1 d . . .
H1A H 0.7617 0.2275 0.5471 0.031 Uiso 1 1 calc R . .
C2 C 0.8330(3) 0.4109(4) 0.4923(2) 0.0911(18) Uani 1 1 d . . .
H2A H 0.8720 0.4684 0.4878 0.137 Uiso 1 1 calc R . .
H2B H 0.7966 0.4443 0.5125 0.137 Uiso 1 1 calc R . .
H2C H 0.8033 0.3856 0.4561 0.137 Uiso 1 1 calc R . .
C3 C 0.9534(3) 0.2230(5) 0.4919(2) 0.0886(18) Uani 1 1 d . . .
H3A H 0.9829 0.1592 0.5123 0.133 Uiso 1 1 calc R . .
H3B H 0.9904 0.2823 0.4861 0.133 Uiso 1 1 calc R . .
H3C H 0.9229 0.1955 0.4565 0.133 Uiso 1 1 calc R . .
C4 C 0.9493(2) 0.3462(4) 0.59504(15) 0.0551(12) Uani 1 1 d . . .
H4A H 0.9779 0.2847 0.6178 0.083 Uiso 1 1 calc R . .
H4B H 0.9165 0.3873 0.6155 0.083 Uiso 1 1 calc R . .
H4C H 0.9872 0.3993 0.5850 0.083 Uiso 1 1 calc R . .
C5 C 0.8449(3) -0.0161(4) 0.46597(18) 0.0668(14) Uani 1 1 d . . .
H5A H 0.8874 -0.0273 0.4988 0.100 Uiso 1 1 calc R . .
H5B H 0.8664 0.0188 0.4370 0.100 Uiso 1 1 calc R . .
H5C H 0.8212 -0.0902 0.4534 0.100 Uiso 1 1 calc R . .
C6 C 0.7215(3) 0.1677(4) 0.42042(16) 0.0687(14) Uani 1 1 d . . .
H6A H 0.6812 0.2186 0.4288 0.103 Uiso 1 1 calc R . .
H6B H 0.6972 0.1162 0.3905 0.103 Uiso 1 1 calc R . .
H6C H 0.7625 0.2135 0.4095 0.103 Uiso 1 1 calc R . .
C7 C 0.6862(2) -0.0108(3) 0.49704(15) 0.0457(10) Uani 1 1 d . . .
H7A H 0.7075 -0.0612 0.5282 0.069 Uiso 1 1 calc R . .
H7B H 0.6638 -0.0573 0.4647 0.069 Uiso 1 1 calc R . .
H7C H 0.6448 0.0377 0.5057 0.069 Uiso 1 1 calc R . .
C8 C 0.83307(19) 0.1928(3) 0.66359(13) 0.0273(8) Uani 1 1 d . . .
C9 C 0.7960(2) 0.2993(3) 0.65130(14) 0.0360(9) Uani 1 1 d . . .
H9A H 0.7812 0.3217 0.6139 0.043 Uiso 1 1 calc R . .
C10 C 0.7793(2) 0.3744(3) 0.69024(16) 0.0424(10) Uani 1 1 d . . .
H10A H 0.7534 0.4449 0.6791 0.051 Uiso 1 1 calc R . .
C11 C 0.8004(2) 0.3461(3) 0.74462(15) 0.0457(10) Uani 1 1 d . . .
H11A H 0.7875 0.3960 0.7711 0.055 Uiso 1 1 calc R . .
C12 C 0.8410(2) 0.2435(3) 0.76142(14) 0.0354(9) Uani 1 1 d . . .
C13 C 0.8610(2) 0.2185(4) 0.81880(15) 0.0476(11) Uani 1 1 d . . .
H13A H 0.8464 0.2706 0.8437 0.057 Uiso 1 1 calc R . .
C14 C 0.9003(2) 0.1223(4) 0.83805(15) 0.0507(11) Uani 1 1 d . . .
H14A H 0.9111 0.1052 0.8760 0.061 Uiso 1 1 calc R . .
C15 C 0.9253(2) 0.0478(3) 0.80176(14) 0.0413(10) Uani 1 1 d . . .
H15A H 0.9546 -0.0184 0.8160 0.050 Uiso 1 1 calc R . .
C16 C 0.90867(19) 0.0674(3) 0.74589(13) 0.0304(8) Uani 1 1 d . . .
C17 C 0.86173(19) 0.1651(3) 0.72263(12) 0.0280(8) Uani 1 1 d . . .
C18 C 0.9738(2) -0.1179(3) 0.73856(15) 0.0455(10) Uani 1 1 d . . .
H18A H 1.0180 -0.1012 0.7697 0.068 Uiso 1 1 calc R . .
H18B H 0.9923 -0.1662 0.7122 0.068 Uiso 1 1 calc R . .
H18C H 0.9323 -0.1581 0.7516 0.068 Uiso 1 1 calc R . .
C19 C 1.0064(2) 0.0484(3) 0.69276(14) 0.0428(10) Uani 1 1 d . . .
H19A H 1.0515 0.0599 0.7239 0.064 Uiso 1 1 calc R . .
H19B H 0.9879 0.1227 0.6767 0.064 Uiso 1 1 calc R . .
H19C H 1.0226 0.0008 0.6651 0.064 Uiso 1 1 calc R . .
C20 C 0.72033(19) -0.1063(3) 0.77036(12) 0.0269(8) Uani 1 1 d . . .
H20 H 0.7645 -0.0527 0.7862 0.032 Uiso 1 1 calc R . .
C21 C 0.6573(3) -0.2914(4) 0.84355(16) 0.0586(12) Uani 1 1 d . . .
H21A H 0.6754 -0.3387 0.8763 0.088 Uiso 1 1 calc R . .
H21B H 0.6280 -0.3390 0.8135 0.088 Uiso 1 1 calc R . .
H21C H 0.6227 -0.2306 0.8514 0.088 Uiso 1 1 calc R . .
C22 C 0.8105(2) -0.1655(4) 0.88726(14) 0.0491(11) Uani 1 1 d . . .
H22A H 0.8258 -0.2266 0.9143 0.074 Uiso 1 1 calc R . .
H22B H 0.7822 -0.1057 0.9023 0.074 Uiso 1 1 calc R . .
H22C H 0.8579 -0.1327 0.8785 0.074 Uiso 1 1 calc R . .
C23 C 0.8005(3) -0.3449(4) 0.80024(17) 0.0676(14) Uani 1 1 d . . .
H23A H 0.8165 -0.4003 0.8301 0.101 Uiso 1 1 calc R . .
H23B H 0.8475 -0.3142 0.7901 0.101 Uiso 1 1 calc R . .
H23C H 0.7668 -0.3829 0.7685 0.101 Uiso 1 1 calc R . .
C24 C 0.5343(2) -0.0765(4) 0.74915(18) 0.0639(13) Uani 1 1 d . . .
H24A H 0.5294 -0.1021 0.7113 0.096 Uiso 1 1 calc R . .
H24B H 0.4937 -0.0191 0.7502 0.096 Uiso 1 1 calc R . .
H24C H 0.5276 -0.1419 0.7720 0.096 Uiso 1 1 calc R . .
C25 C 0.6368(3) 0.1258(4) 0.73831(18) 0.0622(13) Uani 1 1 d . . .
H25A H 0.6179 0.1128 0.6989 0.093 Uiso 1 1 calc R . .
H25B H 0.6909 0.1550 0.7459 0.093 Uiso 1 1 calc R . .
H25C H 0.6026 0.1818 0.7505 0.093 Uiso 1 1 calc R . .
C26 C 0.6456(3) 0.0282(4) 0.84968(15) 0.0610(13) Uani 1 1 d . . .
H26A H 0.6093 0.0909 0.8523 0.092 Uiso 1 1 calc R . .
H26B H 0.6999 0.0527 0.8652 0.092 Uiso 1 1 calc R . .
H26C H 0.6332 -0.0382 0.8701 0.092 Uiso 1 1 calc R . .
C27 C 0.6821(2) -0.2469(3) 0.66745(13) 0.0311(8) Uani 1 1 d . . .
C28 C 0.6226(2) -0.2904(3) 0.69041(15) 0.0447(10) Uani 1 1 d . . .
H28A H 0.6244 -0.2734 0.7277 0.054 Uiso 1 1 calc R . .
C29 C 0.5607(3) -0.3576(4) 0.66168(18) 0.0658(14) Uani 1 1 d . . .
H29A H 0.5223 -0.3860 0.6796 0.079 Uiso 1 1 calc R . .
C30 C 0.5551(3) -0.3826(4) 0.60821(18) 0.0667(14) Uani 1 1 d . . .
H30A H 0.5100 -0.4215 0.5877 0.080 Uiso 1 1 calc R . .
C31 C 0.6164(3) -0.3509(3) 0.58286(15) 0.0480(11) Uani 1 1 d . . .
C32 C 0.6109(3) -0.3787(4) 0.52680(17) 0.0638(13) Uani 1 1 d . . .
H32A H 0.5646 -0.4152 0.5064 0.077 Uiso 1 1 calc R . .
C33 C 0.6697(3) -0.3543(4) 0.50202(17) 0.0679(14) Uani 1 1 d . . .
H33A H 0.6629 -0.3676 0.4639 0.081 Uiso 1 1 calc R . .
C34 C 0.7410(3) -0.3092(3) 0.53265(15) 0.0533(12) Uani 1 1 d . . .
H34A H 0.7834 -0.2975 0.5153 0.064 Uiso 1 1 calc R . .
C35 C 0.7512(2) -0.2813(3) 0.58731(14) 0.0364(9) Uani 1 1 d . . .
C36 C 0.6853(2) -0.2918(3) 0.61335(13) 0.0342(9) Uani 1 1 d . . .
C37 C 0.8570(2) -0.3453(3) 0.66069(15) 0.0438(10) Uani 1 1 d . . .
H37A H 0.8594 -0.4179 0.6416 0.066 Uiso 1 1 calc R . .
H37B H 0.8200 -0.3523 0.6845 0.066 Uiso 1 1 calc R . .
H37C H 0.9095 -0.3263 0.6828 0.066 Uiso 1 1 calc R . .
C38 C 0.8901(3) -0.2386(3) 0.58720(17) 0.0547(12) Uani 1 1 d . . .
H38A H 0.8975 -0.3115 0.5697 0.082 Uiso 1 1 calc R . .
H38B H 0.9401 -0.2150 0.6115 0.082 Uiso 1 1 calc R . .
H38C H 0.8728 -0.1801 0.5590 0.082 Uiso 1 1 calc R . .
O O 0.59991(15) 0.1098(2) 0.59671(11) 0.0494(7) Uani 1 1 d . . .
C40 C 0.5313(3) -0.0694(4) 0.58618(19) 0.0665(13) Uani 1 1 d . . .
H40A H 0.4793 -0.1050 0.5820 0.100 Uiso 1 1 calc R A .
H40B H 0.5661 -0.0947 0.6207 0.100 Uiso 1 1 calc R . .
H40C H 0.5541 -0.0920 0.5555 0.100 Uiso 1 1 calc R . .
C39 C 0.5230(3) 0.0573(4) 0.58670(19) 0.0646(13) Uani 1 1 d . A .
H39A H 0.4906 0.0836 0.5511 0.078 Uiso 1 1 calc R . .
H39B H 0.4961 0.0801 0.6157 0.078 Uiso 1 1 calc R . .
Li2 Li 0.7022(4) 0.0414(5) 0.6331(2) 0.0416(15) Uani 1 1 d . A .
C41 C 0.5950(8) 0.2220(12) 0.5770(6) 0.048(4) Uani 0.558(14) 1 d P A 1
H41A H 0.5618 0.2224 0.5392 0.058 Uiso 0.558(14) 1 calc PR A 1
H41B H 0.6485 0.2475 0.5752 0.058 Uiso 0.558(14) 1 calc PR A 1
C41A C 0.5937(15) 0.245(2) 0.5985(10) 0.085(8) Uani 0.442(14) 1 d P A 2
H41C H 0.5484 0.2671 0.6138 0.102 Uiso 0.442(14) 1 calc PR A 2
H41D H 0.6424 0.2769 0.6221 0.102 Uiso 0.442(14) 1 calc PR A 2
C42 C 0.5615(6) 0.3069(10) 0.6106(4) 0.074(4) Uani 0.558(14) 1 d P A 1
H42A H 0.5649 0.3841 0.5961 0.111 Uiso 0.558(14) 1 calc PR A 1
H42B H 0.5916 0.3038 0.6487 0.111 Uiso 0.558(14) 1 calc PR A 1
H42C H 0.5062 0.2882 0.6089 0.111 Uiso 0.558(14) 1 calc PR A 1
C42A C 0.5828(7) 0.2887(12) 0.5417(6) 0.081(5) Uani 0.442(14) 1 d P A 2
H42D H 0.5866 0.3724 0.5425 0.122 Uiso 0.442(14) 1 calc PR A 2
H42E H 0.5307 0.2659 0.5200 0.122 Uiso 0.442(14) 1 calc PR A 2
H42F H 0.6238 0.2570 0.5250 0.122 Uiso 0.442(14) 1 calc PR A 2

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 0.0440(6) 0.0234(5) 0.0211(4) -0.0004(4) 0.0074(4) -0.0040(4)
P2 0.0285(5) 0.0264(5) 0.0250(5) -0.0015(4) 0.0129(4) -0.0034(4)
Si1 0.0437(7) 0.0371(6) 0.0335(6) 0.0017(5) 0.0168(5) -0.0083(5)
Si2 0.0472(7) 0.0438(7) 0.0240(5) -0.0033(5) 0.0057(5) -0.0073(5)
Si3 0.0432(6) 0.0369(6) 0.0303(5) 0.0042(5) 0.0177(5) 0.0022(5)
Si4 0.0307(6) 0.0479(7) 0.0323(5) -0.0066(5) 0.0095(4) 0.0085(5)
N1 0.0245(16) 0.0381(18) 0.0276(15) 0.0036(13) 0.0056(12) -0.0022(13)
N2 0.0446(19) 0.0272(17) 0.0366(16) 0.0003(13) 0.0246(15) 0.0017(14)
Li1 0.031(3) 0.030(3) 0.036(3) -0.001(3) 0.013(3) -0.001(3)
C1 0.029(2) 0.0257(19) 0.0248(17) 0.0021(15) 0.0087(15) 0.0000(15)
C2 0.102(4) 0.052(3) 0.104(4) 0.038(3) -0.008(3) -0.018(3)
C3 0.077(4) 0.103(4) 0.104(4) -0.031(3) 0.058(3) -0.024(3)
C4 0.054(3) 0.063(3) 0.049(2) 0.002(2) 0.013(2) -0.028(2)
C5 0.083(4) 0.060(3) 0.067(3) -0.030(2) 0.039(3) -0.009(3)
C6 0.087(4) 0.076(3) 0.036(2) 0.013(2) -0.002(2) -0.013(3)
C7 0.047(3) 0.048(3) 0.039(2) -0.0070(19) 0.0035(19) -0.014(2)
C8 0.0276(19) 0.028(2) 0.0283(18) -0.0019(15) 0.0106(15) -0.0099(16)
C9 0.043(2) 0.033(2) 0.034(2) -0.0009(17) 0.0127(17) -0.0042(18)
C10 0.049(3) 0.028(2) 0.055(3) -0.0070(19) 0.024(2) -0.0006(18)
C11 0.057(3) 0.044(3) 0.044(2) -0.020(2) 0.027(2) -0.013(2)
C12 0.039(2) 0.037(2) 0.033(2) -0.0082(17) 0.0156(17) -0.0126(18)
C13 0.057(3) 0.059(3) 0.031(2) -0.014(2) 0.019(2) -0.015(2)
C14 0.059(3) 0.071(3) 0.022(2) -0.001(2) 0.0104(19) -0.014(2)
C15 0.040(2) 0.052(3) 0.030(2) 0.0011(18) 0.0052(17) -0.0086(19)
C16 0.0248(19) 0.041(2) 0.0252(18) -0.0026(16) 0.0051(15) -0.0129(17)
C17 0.0261(19) 0.034(2) 0.0255(18) -0.0048(16) 0.0102(15) -0.0156(16)
C18 0.038(2) 0.056(3) 0.040(2) 0.010(2) 0.0035(18) 0.012(2)
C19 0.028(2) 0.064(3) 0.038(2) -0.0035(19) 0.0107(17) -0.0086(19)
C20 0.0235(19) 0.035(2) 0.0245(17) -0.0031(15) 0.0106(14) 0.0002(15)
C21 0.068(3) 0.066(3) 0.045(2) 0.010(2) 0.021(2) -0.018(2)
C22 0.051(3) 0.057(3) 0.037(2) 0.0094(19) 0.0060(19) 0.004(2)
C23 0.110(4) 0.048(3) 0.053(3) 0.016(2) 0.035(3) 0.038(3)
C24 0.034(2) 0.086(4) 0.071(3) -0.019(3) 0.012(2) 0.006(2)
C25 0.067(3) 0.052(3) 0.071(3) 0.002(2) 0.023(2) 0.023(2)
C26 0.051(3) 0.086(3) 0.045(2) -0.017(2) 0.008(2) 0.026(2)
C27 0.035(2) 0.030(2) 0.0304(18) -0.0014(15) 0.0118(16) -0.0032(16)
C28 0.048(3) 0.051(3) 0.040(2) -0.0050(19) 0.0192(19) -0.021(2)
C29 0.065(3) 0.078(3) 0.059(3) -0.006(3) 0.023(2) -0.042(3)
C30 0.070(3) 0.068(3) 0.061(3) -0.015(2) 0.012(2) -0.046(3)
C31 0.064(3) 0.035(2) 0.043(2) -0.0096(19) 0.009(2) -0.014(2)
C32 0.087(4) 0.053(3) 0.047(3) -0.023(2) 0.009(3) -0.017(3)
C33 0.104(4) 0.067(3) 0.032(2) -0.018(2) 0.014(3) -0.005(3)
C34 0.081(3) 0.048(3) 0.038(2) -0.012(2) 0.027(2) -0.001(2)
C35 0.058(3) 0.022(2) 0.035(2) -0.0025(16) 0.0217(19) 0.0003(18)
C36 0.051(2) 0.0208(19) 0.0331(19) -0.0031(16) 0.0141(18) -0.0039(17)
C37 0.053(3) 0.033(2) 0.050(2) 0.0075(19) 0.021(2) 0.0135(19)
C38 0.070(3) 0.049(3) 0.061(3) -0.003(2) 0.046(2) 0.002(2)
O 0.0321(16) 0.054(2) 0.0606(17) 0.0022(15) 0.0080(13) 0.0060(13)
C40 0.054(3) 0.068(3) 0.069(3) 0.004(3) -0.002(2) -0.005(3)
C39 0.041(3) 0.076(4) 0.072(3) 0.002(3) 0.002(2) -0.004(2)
Li2 0.033(4) 0.048(4) 0.045(4) 0.007(3) 0.012(3) 0.008(3)
C41 0.034(5) 0.033(8) 0.078(11) -0.002(8) 0.015(6) 0.004(5)
C41A 0.080(12) 0.059(13) 0.11(2) -0.052(13) 0.012(12) 0.010(9)
C42 0.076(7) 0.055(7) 0.089(7) -0.002(6) 0.013(6) 0.018(6)
C42A 0.072(9) 0.058(9) 0.105(12) 0.018(9) 0.003(7) 0.012(7)

_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 Li1 2.461(6) . ?
P1 C1 1.889(3) . ?
P1 C8 1.837(3) . ?
P1 Li2 2.662(6) . ?
P2 Li1 2.417(5) . ?
P2 C20 1.895(3) . ?
P2 C27 1.809(3) . ?
P2 Li2 2.616(6) . ?
Si1 C1 1.893(3) . ?
Si1 C2 1.898(5) . ?
Si1 C3 1.857(4) . ?
Si1 C4 1.867(4) . ?
Si2 C1 1.889(3) . ?
Si2 C5 1.891(4) . ?
Si2 C6 1.880(4) . ?
Si2 C7 1.872(4) . ?
Si3 C20 1.905(3) . ?
Si3 C21 1.880(4) . ?
Si3 C22 1.880(4) . ?
Si3 C23 1.865(4) . ?
Si4 C20 1.888(3) . ?
Si4 C24 1.877(4) . ?
Si4 C25 1.868(4) . ?
Si4 C26 1.880(4) . ?
N1 Li1 2.100(6) . ?
N1 C16 1.451(4) . ?
N1 C18 1.483(4) . ?
N1 C19 1.481(4) . ?
N2 Li1 2.100(6) . ?
N2 C35 1.458(5) . ?
N2 C37 1.498(4) . ?
N2 C38 1.480(4) . ?
C1 H1A 1.000 . ?
C2 H2A 0.980 . ?
C2 H2B 0.980 . ?
C2 H2C 0.980 . ?
C3 H3A 0.980 . ?
C3 H3B 0.980 . ?
C3 H3C 0.980 . ?
C4 H4A 0.980 . ?
C4 H4B 0.980 . ?
C4 H4C 0.980 . ?
C5 H5A 0.980 . ?
C5 H5B 0.980 . ?
C5 H5C 0.980 . ?
C6 H6A 0.980 . ?
C6 H6B 0.980 . ?
C6 H6C 0.980 . ?
C7 H7A 0.980 . ?
C7 H7B 0.980 . ?
C7 H7C 0.980 . ?
C8 C9 1.403(5) . ?
C8 C17 1.486(4) . ?
C9 H9A 0.950 . ?
C9 C10 1.393(5) . ?
C10 H10A 0.950 . ?
C10 C11 1.369(5) . ?
C11 H11A 0.950 . ?
C11 C12 1.407(5) . ?
C12 C13 1.432(5) . ?
C12 C17 1.442(5) . ?
C13 H13A 0.950 . ?
C13 C14 1.346(6) . ?
C14 H14A 0.950 . ?
C14 C15 1.401(5) . ?
C15 H15A 0.950 . ?
C15 C16 1.384(4) . ?
C16 C17 1.447(5) . ?
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 H20 1.000 . ?
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 H25A 0.980 . ?
C25 H25B 0.980 . ?
C25 H25C 0.980 . ?
C26 H26A 0.980 . ?
C26 H26B 0.980 . ?
C26 H26C 0.980 . ?
C27 C28 1.393(5) . ?
C27 C36 1.469(4) . ?
C28 H28A 0.950 . ?
C28 C29 1.393(5) . ?
C29 H29A 0.950 . ?
C29 C30 1.355(6) . ?
C30 H30A 0.950 . ?
C30 C31 1.413(6) . ?
C31 C32 1.425(5) . ?
C31 C36 1.442(5) . ?
C32 H32A 0.950 . ?
C32 C33 1.347(6) . ?
C33 H33A 0.950 . ?
C33 C34 1.404(6) . ?
C34 H34A 0.950 . ?
C34 C35 1.381(5) . ?
C35 C36 1.451(5) . ?
C37 H37A 0.980 . ?
C37 H37B 0.980 . ?
C37 H37C 0.980 . ?
C38 H38A 0.980 . ?
C38 H38B 0.980 . ?
C38 H38C 0.980 . ?
O C39 1.442(5) . ?
O Li2 1.974(6) . ?
O C41 1.397(15) . ?
O C41A 1.58(2) . ?
C40 H40A 0.980 . ?
C40 H40B 0.980 . ?
C40 H40C 0.980 . ?
C40 C39 1.488(6) . ?
C39 H39A 0.990 . ?
C39 H39B 0.990 . ?
C41 H41A 0.990 . ?
C41 H41B 0.990 . ?
C41 C42 1.506(16) . ?
C41A H41C 0.990 . ?
C41A H41D 0.990 . ?
C41A C42A 1.49(3) . ?
C42 H42A 0.980 . ?
C42 H42B 0.980 . ?
C42 H42C 0.980 . ?
C42A H42D 0.980 . ?
C42A H42E 0.980 . ?
C42A H42F 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
Li1 P1 C1 150.33(17) . . ?
Li1 P1 C8 100.63(16) . . ?
Li1 P1 Li2 69.53(19) . . ?
C1 P1 C8 105.74(15) . . ?
C1 P1 Li2 103.78(17) . . ?
C8 P1 Li2 76.08(17) . . ?
Li1 P2 C20 137.65(17) . . ?
Li1 P2 C27 110.97(17) . . ?
Li1 P2 Li2 70.96(19) . . ?
C20 P2 C27 108.36(15) . . ?
C20 P2 Li2 113.95(17) . . ?
C27 P2 Li2 103.76(18) . . ?
C1 Si1 C2 107.7(2) . . ?
C1 Si1 C3 113.7(2) . . ?
C1 Si1 C4 115.82(15) . . ?
C2 Si1 C3 108.0(3) . . ?
C2 Si1 C4 104.9(2) . . ?
C3 Si1 C4 106.1(2) . . ?
C1 Si2 C5 112.96(18) . . ?
C1 Si2 C6 109.97(18) . . ?
C1 Si2 C7 110.89(15) . . ?
C5 Si2 C6 108.8(2) . . ?
C5 Si2 C7 107.9(2) . . ?
C6 Si2 C7 106.1(2) . . ?
C20 Si3 C21 115.04(18) . . ?
C20 Si3 C22 108.37(17) . . ?
C20 Si3 C23 112.30(16) . . ?
C21 Si3 C22 107.08(18) . . ?
C21 Si3 C23 107.0(2) . . ?
C22 Si3 C23 106.7(2) . . ?
C20 Si4 C24 115.23(18) . . ?
C20 Si4 C25 110.99(17) . . ?
C20 Si4 C26 108.33(16) . . ?
C24 Si4 C25 107.1(2) . . ?
C24 Si4 C26 109.0(2) . . ?
C25 Si4 C26 105.8(2) . . ?
Li1 N1 C16 108.5(2) . . ?
Li1 N1 C18 93.7(3) . . ?
Li1 N1 C19 121.4(2) . . ?
C16 N1 C18 114.8(3) . . ?
C16 N1 C19 110.2(3) . . ?
C18 N1 C19 107.6(3) . . ?
Li1 N2 C35 119.1(3) . . ?
Li1 N2 C37 110.8(3) . . ?
Li1 N2 C38 94.7(3) . . ?
C35 N2 C37 108.8(3) . . ?
C35 N2 C38 114.6(3) . . ?
C37 N2 C38 107.8(3) . . ?
P1 Li1 P2 114.7(2) . . ?
P1 Li1 N1 83.8(2) . . ?
P1 Li1 N2 125.7(3) . . ?
P2 Li1 N1 109.8(2) . . ?
P2 Li1 N2 88.3(2) . . ?
N1 Li1 N2 135.9(3) . . ?
P1 C1 Si1 113.40(17) . . ?
P1 C1 Si2 110.03(16) . . ?
P1 C1 H1A 105.8 . . ?
Si1 C1 Si2 115.08(16) . . ?
Si1 C1 H1A 105.8 . . ?
Si2 C1 H1A 105.8 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 C9 119.5(2) . . ?
P1 C8 C17 124.0(3) . . ?
C9 C8 C17 116.4(3) . . ?
C8 C9 H9A 117.8 . . ?
C8 C9 C10 124.4(3) . . ?
H9A C9 C10 117.8 . . ?
C9 C10 H10A 120.1 . . ?
C9 C10 C11 119.7(4) . . ?
H10A C10 C11 120.1 . . ?
C10 C11 H11A 119.8 . . ?
C10 C11 C12 120.3(3) . . ?
H11A C11 C12 119.8 . . ?
C11 C12 C13 117.7(3) . . ?
C11 C12 C17 121.8(3) . . ?
C13 C12 C17 120.6(4) . . ?
C12 C13 H13A 119.4 . . ?
C12 C13 C14 121.1(4) . . ?
H13A C13 C14 119.4 . . ?
C13 C14 H14A 120.2 . . ?
C13 C14 C15 119.7(3) . . ?
H14A C14 C15 120.2 . . ?
C14 C15 H15A 118.9 . . ?
C14 C15 C16 122.1(4) . . ?
H15A C15 C16 118.9 . . ?
N1 C16 C15 118.5(3) . . ?
N1 C16 C17 121.0(3) . . ?
C15 C16 C17 120.4(3) . . ?
C8 C17 C12 117.1(3) . . ?
C8 C17 C16 127.1(3) . . ?
C12 C17 C16 115.8(3) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P2 C20 Si3 118.39(17) . . ?
P2 C20 Si4 119.04(17) . . ?
P2 C20 H20 98.9 . . ?
Si3 C20 Si4 115.54(15) . . ?
Si3 C20 H20 98.9 . . ?
Si4 C20 H20 98.9 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si4 C25 H25A 109.5 . . ?
Si4 C25 H25B 109.5 . . ?
Si4 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si4 C26 H26A 109.5 . . ?
Si4 C26 H26B 109.5 . . ?
Si4 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
P2 C27 C28 119.6(3) . . ?
P2 C27 C36 123.7(2) . . ?
C28 C27 C36 116.3(3) . . ?
C27 C28 H28A 118.2 . . ?
C27 C28 C29 123.6(3) . . ?
H28A C28 C29 118.2 . . ?
C28 C29 H29A 119.9 . . ?
C28 C29 C30 120.2(4) . . ?
H29A C29 C30 119.9 . . ?
C29 C30 H30A 119.9 . . ?
C29 C30 C31 120.1(4) . . ?
H30A C30 C31 119.9 . . ?
C30 C31 C32 120.0(4) . . ?
C30 C31 C36 120.6(3) . . ?
C32 C31 C36 119.4(4) . . ?
C31 C32 H32A 119.2 . . ?
C31 C32 C33 121.5(4) . . ?
H32A C32 C33 119.2 . . ?
C32 C33 H33A 120.0 . . ?
C32 C33 C34 119.9(4) . . ?
H33A C33 C34 120.0 . . ?
C33 C34 H34A 119.1 . . ?
C33 C34 C35 121.8(4) . . ?
H34A C34 C35 119.1 . . ?
N2 C35 C34 119.6(3) . . ?
N2 C35 C36 120.5(3) . . ?
C34 C35 C36 119.7(4) . . ?
C27 C36 C31 117.1(3) . . ?
C27 C36 C35 126.2(3) . . ?
C31 C36 C35 116.7(3) . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N2 C38 H38A 109.5 . . ?
N2 C38 H38B 109.5 . . ?
N2 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C39 O Li2 127.7(3) . . ?
C39 O C41 111.0(6) . . ?
C39 O C41A 111.2(10) . . ?
Li2 O C41 121.2(6) . . ?
Li2 O C41A 116.8(10) . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40A C40 C39 109.5 . . ?
H40B C40 H40C 109.5 . . ?
H40B C40 C39 109.5 . . ?
H40C C40 C39 109.5 . . ?
O C39 C40 109.7(4) . . ?
O C39 H39A 109.7 . . ?
O C39 H39B 109.7 . . ?
C40 C39 H39A 109.7 . . ?
C40 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
P1 Li2 P2 102.2(2) . . ?
P1 Li2 O 123.7(3) . . ?
P2 Li2 O 133.5(3) . . ?
O C41 H41A 108.6 . . ?
O C41 H41B 108.6 . . ?
O C41 C42 114.8(11) . . ?
H41A C41 H41B 107.5 . . ?
H41A C41 C42 108.6 . . ?
H41B C41 C42 108.6 . . ?
O C41A H41C 110.0 . . ?
O C41A H41D 110.0 . . ?
O C41A C42A 108.3(13) . . ?
H41C C41A H41D 108.4 . . ?
H41C C41A C42A 110.0 . . ?
H41D C41A C42A 110.0 . . ?
C41A C42A H42D 109.5 . . ?
C41A C42A H42E 109.5 . . ?
C41A C42A H42F 109.5 . . ?
H42D C42A H42E 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.054

#===END

data_ki285_3
_database_code_depnum_ccdc_archive 'CCDC 662786'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H47 N3 Na P Si2'
_chemical_formula_sum            'C25 H47 N3 Na P Si2'
_chemical_formula_weight         499.80

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'
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                   9.795(3)
_cell_length_b                   26.617(9)
_cell_length_c                   12.301(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.430(5)
_cell_angle_gamma                90.00
_cell_volume                     3042.5(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5082
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      28.14

_exptl_crystal_description       lath
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_T_max  0.995
_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  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \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            22487
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5938
_reflns_number_gt                4575
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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^)+(0.1597P)^2^+1.7287P] 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         5938
_refine_ls_number_parameters     301
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.2461
_refine_ls_wR_factor_gt          0.2263
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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
P P 0.23118(10) 0.10304(3) 0.36614(7) 0.0180(3) Uani 1 1 d . . .
Si1 Si 0.28313(11) 0.09513(4) 0.13057(8) 0.0257(3) Uani 1 1 d . . .
Si2 Si -0.03294(11) 0.10920(4) 0.15502(8) 0.0243(3) Uani 1 1 d . . .
Na Na 0.09602(15) 0.12233(5) 0.52659(12) 0.0256(4) Uani 1 1 d . . .
N1 N 0.3363(3) 0.07353(11) 0.6098(2) 0.0217(6) Uani 1 1 d . . .
N2 N 0.0604(3) 0.20499(11) 0.5983(2) 0.0252(7) Uani 1 1 d . . .
N3 N -0.1171(3) 0.11121(11) 0.5905(3) 0.0261(7) Uani 1 1 d . . .
C1 C 0.1662(4) 0.12270(12) 0.2100(3) 0.0185(7) Uani 1 1 d . . .
H1A H 0.1774 0.1600 0.2084 0.022 Uiso 1 1 calc R . .
C2 C 0.2464(5) 0.02655(17) 0.1056(4) 0.0464(12) Uani 1 1 d . . .
H2A H 0.2599 0.0097 0.1791 0.070 Uiso 1 1 calc R . .
H2B H 0.3130 0.0123 0.0688 0.070 Uiso 1 1 calc R . .
H2C H 0.1472 0.0217 0.0558 0.070 Uiso 1 1 calc R . .
C3 C 0.4803(5) 0.10169(19) 0.2090(4) 0.0429(11) Uani 1 1 d . . .
H3A H 0.5018 0.0875 0.2861 0.064 Uiso 1 1 calc R . .
H3B H 0.5068 0.1373 0.2146 0.064 Uiso 1 1 calc R . .
H3C H 0.5354 0.0837 0.1672 0.064 Uiso 1 1 calc R . .
C4 C 0.2518(6) 0.1280(2) -0.0113(4) 0.0518(13) Uani 1 1 d . . .
H4A H 0.1553 0.1199 -0.0624 0.078 Uiso 1 1 calc R . .
H4B H 0.3237 0.1168 -0.0462 0.078 Uiso 1 1 calc R . .
H4C H 0.2602 0.1644 0.0011 0.078 Uiso 1 1 calc R . .
C5 C -0.0820(5) 0.04681(15) 0.2013(4) 0.0370(10) Uani 1 1 d . . .
H5A H -0.0446 0.0443 0.2850 0.055 Uiso 1 1 calc R . .
H5B H -0.0402 0.0200 0.1672 0.055 Uiso 1 1 calc R . .
H5C H -0.1870 0.0433 0.1760 0.055 Uiso 1 1 calc R . .
C6 C -0.1063(5) 0.11017(17) -0.0060(4) 0.0398(10) Uani 1 1 d . . .
H6A H -0.2095 0.1026 -0.0304 0.060 Uiso 1 1 calc R . .
H6B H -0.0563 0.0849 -0.0374 0.060 Uiso 1 1 calc R . .
H6C H -0.0914 0.1435 -0.0341 0.060 Uiso 1 1 calc R . .
C7 C -0.1286(5) 0.15947(17) 0.2087(4) 0.0420(11) Uani 1 1 d . . .
H7A H -0.0833 0.1635 0.2916 0.063 Uiso 1 1 calc R . .
H7B H -0.2298 0.1500 0.1928 0.063 Uiso 1 1 calc R . .
H7C H -0.1229 0.1912 0.1700 0.063 Uiso 1 1 calc R . .
C8 C 0.3514(4) 0.15343(12) 0.4395(3) 0.0169(7) Uani 1 1 d . . .
C9 C 0.3815(4) 0.19391(13) 0.3753(3) 0.0224(7) Uani 1 1 d . . .
H9A H 0.3436 0.1922 0.2941 0.027 Uiso 1 1 calc R . .
C10 C 0.4624(4) 0.23588(14) 0.4231(3) 0.0261(8) Uani 1 1 d . . .
H10A H 0.4766 0.2617 0.3745 0.031 Uiso 1 1 calc R . .
C11 C 0.5223(4) 0.24050(14) 0.5401(3) 0.0270(8) Uani 1 1 d . . .
H11A H 0.5753 0.2697 0.5725 0.032 Uiso 1 1 calc R . .
C12 C 0.5039(4) 0.20119(13) 0.6112(3) 0.0207(7) Uani 1 1 d . . .
C13 C 0.5691(4) 0.20686(14) 0.7317(3) 0.0267(8) Uani 1 1 d . . .
H13A H 0.6200 0.2369 0.7608 0.032 Uiso 1 1 calc R . .
C14 C 0.5599(4) 0.17004(15) 0.8060(3) 0.0297(9) Uani 1 1 d . . .
H14A H 0.6049 0.1742 0.8861 0.036 Uiso 1 1 calc R . .
C15 C 0.4839(4) 0.12617(14) 0.7637(3) 0.0277(8) Uani 1 1 d . . .
H15A H 0.4791 0.1004 0.8159 0.033 Uiso 1 1 calc R . .
C16 C 0.4150(4) 0.11907(13) 0.6477(3) 0.0188(7) Uani 1 1 d . . .
C17 C 0.4217(3) 0.15687(12) 0.5644(3) 0.0173(7) Uani 1 1 d . . .
C18 C 0.4215(4) 0.03677(14) 0.5692(3) 0.0273(8) Uani 1 1 d . . .
H18A H 0.5007 0.0243 0.6344 0.041 Uiso 1 1 calc R . .
H18B H 0.4608 0.0529 0.5139 0.041 Uiso 1 1 calc R . .
H18C H 0.3598 0.0086 0.5323 0.041 Uiso 1 1 calc R . .
C19 C 0.2765(5) 0.04934(17) 0.6928(3) 0.0367(10) Uani 1 1 d . . .
H19A H 0.3541 0.0329 0.7529 0.055 Uiso 1 1 calc R . .
H19B H 0.2048 0.0242 0.6533 0.055 Uiso 1 1 calc R . .
H19C H 0.2309 0.0748 0.7274 0.055 Uiso 1 1 calc R . .
C20 C 0.1679(4) 0.21409(16) 0.7111(3) 0.0315(9) Uani 1 1 d . . .
H20A H 0.1478 0.2463 0.7415 0.047 Uiso 1 1 calc R . .
H20B H 0.2642 0.2150 0.7031 0.047 Uiso 1 1 calc R . .
H20C H 0.1632 0.1870 0.7638 0.047 Uiso 1 1 calc R . .
C21 C 0.0752(5) 0.24499(16) 0.5202(4) 0.0407(11) Uani 1 1 d . . .
H21A H 0.0564 0.2776 0.5495 0.061 Uiso 1 1 calc R . .
H21B H 0.0059 0.2394 0.4440 0.061 Uiso 1 1 calc R . .
H21C H 0.1730 0.2446 0.5152 0.061 Uiso 1 1 calc R . .
C22 C -0.0863(4) 0.20454(14) 0.6069(3) 0.0297(8) Uani 1 1 d . . .
H22A H -0.1563 0.2090 0.5293 0.036 Uiso 1 1 calc R . .
H22B H -0.0971 0.2334 0.6544 0.036 Uiso 1 1 calc R . .
C23 C -0.1214(4) 0.15634(14) 0.6588(3) 0.0283(8) Uani 1 1 d . . .
H23A H -0.0519 0.1521 0.7366 0.034 Uiso 1 1 calc R . .
H23B H -0.2186 0.1594 0.6666 0.034 Uiso 1 1 calc R . .
C24 C -0.1279(5) 0.06659(16) 0.6581(4) 0.0426(11) Uani 1 1 d . . .
H24A H -0.2156 0.0688 0.6801 0.064 Uiso 1 1 calc R . .
H24B H -0.0438 0.0650 0.7272 0.064 Uiso 1 1 calc R . .
H24C H -0.1316 0.0363 0.6120 0.064 Uiso 1 1 calc R . .
C25 C -0.2400(5) 0.11131(17) 0.4838(4) 0.0369(10) Uani 1 1 d . . .
H25A H -0.3299 0.1137 0.5024 0.055 Uiso 1 1 calc R . .
H25B H -0.2396 0.0802 0.4414 0.055 Uiso 1 1 calc R . .
H25C H -0.2320 0.1402 0.4367 0.055 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
P 0.0247(5) 0.0270(5) 0.0005(4) -0.0003(3) 0.0014(3) -0.0034(3)
Si1 0.0305(6) 0.0431(6) 0.0030(5) -0.0034(4) 0.0045(4) 0.0005(4)
Si2 0.0231(5) 0.0313(5) 0.0133(5) 0.0050(4) -0.0019(4) -0.0026(4)
Na 0.0283(8) 0.0396(8) 0.0111(7) -0.0009(5) 0.0095(6) 0.0033(6)
N1 0.0264(16) 0.0334(16) 0.0058(13) 0.0042(11) 0.0057(12) 0.0019(12)
N2 0.0345(17) 0.0349(16) 0.0072(14) 0.0035(11) 0.0079(12) 0.0005(13)
N3 0.0239(16) 0.0354(17) 0.0174(17) 0.0042(12) 0.0042(13) 0.0001(12)
C1 0.0246(17) 0.0274(17) 0.0009(15) 0.0008(12) 0.0002(12) -0.0027(13)
C2 0.054(3) 0.052(3) 0.030(2) -0.0167(19) 0.010(2) 0.003(2)
C3 0.032(2) 0.073(3) 0.026(2) -0.011(2) 0.0128(19) 0.000(2)
C4 0.057(3) 0.092(4) 0.014(2) 0.009(2) 0.021(2) 0.007(3)
C5 0.032(2) 0.041(2) 0.030(2) 0.0087(17) -0.0008(17) -0.0085(17)
C6 0.036(2) 0.052(3) 0.017(2) 0.0063(17) -0.0119(17) -0.0069(19)
C7 0.033(2) 0.046(2) 0.047(3) 0.013(2) 0.014(2) 0.0035(19)
C8 0.0194(17) 0.0285(17) 0.0031(15) -0.0022(11) 0.0038(13) 0.0012(12)
C9 0.0286(19) 0.0341(19) 0.0050(16) -0.0010(13) 0.0062(14) -0.0061(14)
C10 0.034(2) 0.0342(19) 0.0117(18) -0.0013(14) 0.0096(15) -0.0075(15)
C11 0.031(2) 0.0329(19) 0.0165(19) -0.0086(14) 0.0060(15) -0.0088(15)
C12 0.0224(18) 0.0313(18) 0.0081(16) -0.0057(13) 0.0043(13) 0.0012(13)
C13 0.0244(19) 0.039(2) 0.0124(18) -0.0114(14) -0.0003(14) 0.0008(15)
C14 0.035(2) 0.045(2) 0.0024(16) -0.0056(14) -0.0040(14) 0.0088(17)
C15 0.039(2) 0.038(2) 0.0037(16) 0.0016(13) 0.0036(15) 0.0090(16)
C16 0.0209(17) 0.0320(18) 0.0018(15) -0.0010(12) 0.0011(12) 0.0044(13)
C17 0.0177(16) 0.0298(17) 0.0035(15) -0.0014(12) 0.0019(12) 0.0032(13)
C18 0.032(2) 0.0296(19) 0.0166(19) 0.0010(14) 0.0019(15) 0.0026(15)
C19 0.038(2) 0.054(3) 0.018(2) 0.0115(17) 0.0093(17) -0.0064(19)
C20 0.034(2) 0.049(2) 0.0119(18) -0.0005(15) 0.0066(16) 0.0012(17)
C21 0.065(3) 0.041(2) 0.018(2) 0.0053(16) 0.015(2) -0.006(2)
C22 0.031(2) 0.039(2) 0.0176(19) 0.0004(15) 0.0048(15) 0.0078(16)
C23 0.0246(19) 0.045(2) 0.0163(19) 0.0002(15) 0.0088(15) 0.0031(15)
C24 0.039(2) 0.048(3) 0.037(3) 0.0159(19) 0.007(2) -0.0039(19)
C25 0.035(2) 0.053(3) 0.018(2) 0.0011(17) 0.0022(17) -0.0030(18)

_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
P Na 2.7503(17) . ?
P C1 1.896(3) . ?
P C8 1.824(3) . ?
Si1 C1 1.874(4) . ?
Si1 C2 1.867(5) . ?
Si1 C3 1.874(5) . ?
Si1 C4 1.889(4) . ?
Si2 C1 1.886(4) . ?
Si2 C5 1.867(4) . ?
Si2 C6 1.881(4) . ?
Si2 C7 1.870(5) . ?
Na N1 2.599(3) . ?
Na N2 2.436(3) . ?
Na N3 2.470(3) . ?
Na C8 3.129(4) . ?
Na C16 3.008(4) . ?
N1 C16 1.433(5) . ?
N1 C18 1.472(5) . ?
N1 C19 1.476(5) . ?
N2 C20 1.473(5) . ?
N2 C21 1.472(5) . ?
N2 C22 1.473(5) . ?
N3 C23 1.474(5) . ?
N3 C24 1.472(5) . ?
N3 C25 1.474(5) . ?
C1 H1A 1.000 . ?
C2 H2A 0.980 . ?
C2 H2B 0.980 . ?
C2 H2C 0.980 . ?
C3 H3A 0.980 . ?
C3 H3B 0.980 . ?
C3 H3C 0.980 . ?
C4 H4A 0.980 . ?
C4 H4B 0.980 . ?
C4 H4C 0.980 . ?
C5 H5A 0.980 . ?
C5 H5B 0.980 . ?
C5 H5C 0.980 . ?
C6 H6A 0.980 . ?
C6 H6B 0.980 . ?
C6 H6C 0.980 . ?
C7 H7A 0.980 . ?
C7 H7B 0.980 . ?
C7 H7C 0.980 . ?
C8 C9 1.420(5) . ?
C8 C17 1.475(4) . ?
C9 H9A 0.950 . ?
C9 C10 1.388(5) . ?
C10 H10A 0.950 . ?
C10 C11 1.377(5) . ?
C11 H11A 0.950 . ?
C11 C12 1.412(5) . ?
C12 C13 1.424(5) . ?
C12 C17 1.441(5) . ?
C13 H13A 0.950 . ?
C13 C14 1.362(6) . ?
C14 H14A 0.950 . ?
C14 C15 1.394(6) . ?
C15 H15A 0.950 . ?
C15 C16 1.385(5) . ?
C16 C17 1.453(5) . ?
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 0.990 . ?
C22 H22B 0.990 . ?
C22 C23 1.520(5) . ?
C23 H23A 0.990 . ?
C23 H23B 0.990 . ?
C24 H24A 0.980 . ?
C24 H24B 0.980 . ?
C24 H24C 0.980 . ?
C25 H25A 0.980 . ?
C25 H25B 0.980 . ?
C25 H25C 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
Na P C1 126.28(12) . . ?
Na P C8 83.69(11) . . ?
C1 P C8 104.79(15) . . ?
C1 Si1 C2 110.55(19) . . ?
C1 Si1 C3 113.30(17) . . ?
C1 Si1 C4 110.64(19) . . ?
C2 Si1 C3 106.8(2) . . ?
C2 Si1 C4 109.5(2) . . ?
C3 Si1 C4 105.8(2) . . ?
C1 Si2 C5 113.39(17) . . ?
C1 Si2 C6 112.48(18) . . ?
C1 Si2 C7 108.30(18) . . ?
C5 Si2 C6 106.48(19) . . ?
C5 Si2 C7 108.8(2) . . ?
C6 Si2 C7 107.2(2) . . ?
P Na N1 66.91(7) . . ?
P Na N2 125.81(9) . . ?
P Na N3 148.55(10) . . ?
N1 Na N2 121.62(11) . . ?
N1 Na N3 124.47(11) . . ?
N2 Na N3 76.14(11) . . ?
Na N1 C16 91.86(19) . . ?
Na N1 C18 137.6(2) . . ?
Na N1 C19 89.0(2) . . ?
C16 N1 C18 111.6(3) . . ?
C16 N1 C19 115.8(3) . . ?
C18 N1 C19 109.7(3) . . ?
Na N2 C20 110.4(2) . . ?
Na N2 C21 111.2(2) . . ?
Na N2 C22 105.9(2) . . ?
C20 N2 C21 107.9(3) . . ?
C20 N2 C22 110.9(3) . . ?
C21 N2 C22 110.6(3) . . ?
Na N3 C23 105.3(2) . . ?
Na N3 C24 119.7(2) . . ?
Na N3 C25 104.5(2) . . ?
C23 N3 C24 108.4(3) . . ?
C23 N3 C25 110.1(3) . . ?
C24 N3 C25 108.7(3) . . ?
P C1 Si1 110.78(17) . . ?
P C1 Si2 106.77(16) . . ?
P C1 H1A 106.8 . . ?
Si1 C1 Si2 118.16(17) . . ?
Si1 C1 H1A 106.8 . . ?
Si2 C1 H1A 106.8 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P C8 C9 119.9(2) . . ?
P C8 C17 125.2(2) . . ?
C9 C8 C17 114.9(3) . . ?
C8 C9 H9A 117.8 . . ?
C8 C9 C10 124.4(3) . . ?
H9A C9 C10 117.8 . . ?
C9 C10 H10A 119.6 . . ?
C9 C10 C11 120.8(3) . . ?
H10A C10 C11 119.6 . . ?
C10 C11 H11A 120.5 . . ?
C10 C11 C12 119.1(3) . . ?
H11A C11 C12 120.5 . . ?
C11 C12 C13 117.6(3) . . ?
C11 C12 C17 121.6(3) . . ?
C13 C12 C17 120.9(3) . . ?
C12 C13 H13A 119.4 . . ?
C12 C13 C14 121.2(3) . . ?
H13A C13 C14 119.4 . . ?
C13 C14 H14A 120.2 . . ?
C13 C14 C15 119.5(3) . . ?
H14A C14 C15 120.2 . . ?
C14 C15 H15A 119.1 . . ?
C14 C15 C16 121.9(3) . . ?
H15A C15 C16 119.1 . . ?
N1 C16 C15 119.1(3) . . ?
N1 C16 C17 119.8(3) . . ?
C15 C16 C17 121.1(3) . . ?
C8 C17 C12 119.0(3) . . ?
C8 C17 C16 125.6(3) . . ?
C12 C17 C16 115.4(3) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.0 . . ?
N2 C22 H22B 109.0 . . ?
N2 C22 C23 113.1(3) . . ?
H22A C22 H22B 107.8 . . ?
H22A C22 C23 109.0 . . ?
H22B C22 C23 109.0 . . ?
N3 C23 C22 113.4(3) . . ?
N3 C23 H23A 108.9 . . ?
N3 C23 H23B 108.9 . . ?
C22 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.148

#===END

data_ki292_4
_database_code_depnum_ccdc_archive 'CCDC 662787'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H54 K N4 P Si2'
_chemical_formula_sum            'C28 H54 K N4 P Si2'
_chemical_formula_weight         573.00

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'
K K 0.2009 0.2494 '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'
Si Si 0.0817 0.0704 '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/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                   9.814(2)
_cell_length_b                   16.820(4)
_cell_length_c                   21.700(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.932(4)
_cell_angle_gamma                90.00
_cell_volume                     3491.3(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9200
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.2

_exptl_crystal_description       rod
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_T_max  0.975
_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  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \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            22770
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         0.96
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6856
_reflns_number_gt                5143
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR97
_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^)+(0.0280P)^2^+2.0832P] 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         6856
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.0999
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.003
_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 0.78795(8) 0.08892(4) 0.27969(4) 0.02822(18) Uani 1 1 d . . .
P P 1.03709(10) 0.15066(5) 0.38732(4) 0.02162(19) Uani 1 1 d . . .
Si1 Si 0.87073(11) 0.27648(6) 0.43633(5) 0.0280(2) Uani 1 1 d . . .
Si2 Si 1.20831(11) 0.27571(5) 0.47460(5) 0.0262(2) Uani 1 1 d . . .
N1 N 1.0466(3) -0.01218(15) 0.35033(13) 0.0267(7) Uani 1 1 d . . .
N2 N 0.6729(3) 0.18756(16) 0.17388(14) 0.0313(7) Uani 1 1 d . . .
N3 N 0.6040(3) 0.01224(16) 0.17902(14) 0.0312(7) Uani 1 1 d . . .
N4 N 0.5568(3) 0.01709(17) 0.31241(15) 0.0371(8) Uani 1 1 d . . .
C1 C 1.0433(4) 0.25826(17) 0.41461(15) 0.0228(7) Uani 1 1 d . . .
H1A H 1.0461 0.2924 0.3772 0.027 Uiso 1 1 calc R . .
C2 C 0.8166(4) 0.1934(2) 0.48382(18) 0.0389(10) Uani 1 1 d . . .
H2A H 0.8125 0.1435 0.4602 0.058 Uiso 1 1 calc R . .
H2B H 0.7243 0.2051 0.4918 0.058 Uiso 1 1 calc R . .
H2C H 0.8849 0.1884 0.5242 0.058 Uiso 1 1 calc R . .
C3 C 0.8671(5) 0.3705(2) 0.48324(18) 0.0430(11) Uani 1 1 d . . .
H3A H 0.7723 0.3794 0.4892 0.065 Uiso 1 1 calc R . .
H3B H 0.8953 0.4155 0.4603 0.065 Uiso 1 1 calc R . .
H3C H 0.9320 0.3653 0.5246 0.065 Uiso 1 1 calc R . .
C4 C 0.7334(4) 0.2890(2) 0.36227(18) 0.0394(10) Uani 1 1 d . . .
H4A H 0.7413 0.2461 0.3327 0.059 Uiso 1 1 calc R . .
H4B H 0.7459 0.3404 0.3430 0.059 Uiso 1 1 calc R . .
H4C H 0.6409 0.2871 0.3722 0.059 Uiso 1 1 calc R . .
C5 C 1.2319(4) 0.3842(2) 0.49534(18) 0.0395(10) Uani 1 1 d . . .
H5A H 1.1571 0.4017 0.5155 0.059 Uiso 1 1 calc R . .
H5B H 1.2281 0.4153 0.4568 0.059 Uiso 1 1 calc R . .
H5C H 1.3226 0.3923 0.5245 0.059 Uiso 1 1 calc R . .
C6 C 1.2045(4) 0.2178(2) 0.54784(15) 0.0356(9) Uani 1 1 d . . .
H6A H 1.1922 0.1612 0.5373 0.053 Uiso 1 1 calc R . .
H6B H 1.1266 0.2363 0.5656 0.053 Uiso 1 1 calc R . .
H6C H 1.2927 0.2255 0.5790 0.053 Uiso 1 1 calc R . .
C7 C 1.3687(4) 0.2421(2) 0.44801(18) 0.0386(9) Uani 1 1 d . . .
H7A H 1.3541 0.1880 0.4310 0.058 Uiso 1 1 calc R . .
H7B H 1.4492 0.2426 0.4841 0.058 Uiso 1 1 calc R . .
H7C H 1.3863 0.2780 0.4151 0.058 Uiso 1 1 calc R . .
C8 C 1.1077(3) 0.15302(18) 0.31720(15) 0.0206(7) Uani 1 1 d . . .
C9 C 1.1642(3) 0.22274(18) 0.29614(15) 0.0247(7) Uani 1 1 d . . .
H9A H 1.1767 0.2676 0.3234 0.030 Uiso 1 1 calc R . .
C10 C 1.2027(4) 0.23041(19) 0.23858(15) 0.0280(8) Uani 1 1 d . . .
H10A H 1.2418 0.2791 0.2286 0.034 Uiso 1 1 calc R . .
C11 C 1.1853(4) 0.16893(19) 0.19589(16) 0.0272(8) Uani 1 1 d . . .
H11A H 1.2082 0.1755 0.1559 0.033 Uiso 1 1 calc R . .
C12 C 1.1325(3) 0.09556(19) 0.21254(15) 0.0230(7) Uani 1 1 d . . .
C13 C 1.1048(4) 0.0343(2) 0.16709(17) 0.0289(8) Uani 1 1 d . . .
H13A H 1.1228 0.0430 0.1264 0.035 Uiso 1 1 calc R . .
C14 C 1.0528(4) -0.0371(2) 0.18047(18) 0.0357(9) Uani 1 1 d . . .
H14A H 1.0276 -0.0761 0.1482 0.043 Uiso 1 1 calc R . .
C15 C 1.0364(4) -0.0532(2) 0.24164(18) 0.0323(9) Uani 1 1 d . . .
H15A H 1.0067 -0.1045 0.2514 0.039 Uiso 1 1 calc R . .
C16 C 1.0628(3) 0.00471(18) 0.28831(16) 0.0230(7) Uani 1 1 d . . .
C17 C 1.1031(3) 0.08384(18) 0.27424(15) 0.0198(7) Uani 1 1 d . . .
C18 C 0.9550(4) -0.0780(2) 0.3580(2) 0.0414(10) Uani 1 1 d . . .
H18A H 0.8651 -0.0722 0.3277 0.062 Uiso 1 1 calc R . .
H18B H 0.9397 -0.0776 0.4011 0.062 Uiso 1 1 calc R . .
H18C H 0.9986 -0.1284 0.3503 0.062 Uiso 1 1 calc R . .
C19 C 1.1784(4) -0.0170(2) 0.39713(17) 0.0333(9) Uani 1 1 d . . .
H19A H 1.2363 0.0292 0.3929 0.050 Uiso 1 1 calc R . .
H19B H 1.2277 -0.0657 0.3903 0.050 Uiso 1 1 calc R . .
H19C H 1.1597 -0.0178 0.4396 0.050 Uiso 1 1 calc R . .
C20 C 0.8100(4) 0.1941(3) 0.1567(2) 0.0490(11) Uani 1 1 d . . .
H20A H 0.8747 0.2240 0.1895 0.074 Uiso 1 1 calc R . .
H20B H 0.7985 0.2218 0.1161 0.074 Uiso 1 1 calc R . .
H20C H 0.8477 0.1408 0.1531 0.074 Uiso 1 1 calc R . .
C21 C 0.6191(5) 0.2671(2) 0.1815(2) 0.0535(12) Uani 1 1 d . . .
H21A H 0.5307 0.2628 0.1952 0.080 Uiso 1 1 calc R . .
H21B H 0.6033 0.2955 0.1411 0.080 Uiso 1 1 calc R . .
H21C H 0.6871 0.2964 0.2134 0.080 Uiso 1 1 calc R . .
C22 C 0.5720(4) 0.1451(2) 0.12482(17) 0.0396(10) Uani 1 1 d . . .
H22A H 0.5721 0.1696 0.0833 0.047 Uiso 1 1 calc R . .
H22B H 0.4774 0.1523 0.1329 0.047 Uiso 1 1 calc R . .
C23 C 0.5998(5) 0.0573(2) 0.12090(18) 0.0432(10) Uani 1 1 d . . .
H23A H 0.5262 0.0342 0.0868 0.052 Uiso 1 1 calc R . .
H23B H 0.6903 0.0503 0.1086 0.052 Uiso 1 1 calc R . .
C24 C 0.6533(4) -0.0689(2) 0.1704(2) 0.0454(11) Uani 1 1 d . . .
H24A H 0.6625 -0.0988 0.2099 0.068 Uiso 1 1 calc R . .
H24B H 0.7443 -0.0662 0.1590 0.068 Uiso 1 1 calc R . .
H24C H 0.5858 -0.0956 0.1366 0.068 Uiso 1 1 calc R . .
C25 C 0.4666(4) 0.0094(2) 0.19573(18) 0.0378(10) Uani 1 1 d . . .
H25A H 0.4021 -0.0221 0.1632 0.045 Uiso 1 1 calc R . .
H25B H 0.4290 0.0642 0.1942 0.045 Uiso 1 1 calc R . .
C26 C 0.4665(4) -0.0254(2) 0.2596(2) 0.0409(10) Uani 1 1 d . . .
H26A H 0.3696 -0.0252 0.2658 0.049 Uiso 1 1 calc R . .
H26B H 0.4975 -0.0815 0.2603 0.049 Uiso 1 1 calc R . .
C27 C 0.5777(5) -0.0297(3) 0.3709(2) 0.0571(13) Uani 1 1 d . . .
H27A H 0.6183 -0.0814 0.3644 0.086 Uiso 1 1 calc R . .
H27B H 0.4876 -0.0377 0.3824 0.086 Uiso 1 1 calc R . .
H27C H 0.6413 -0.0012 0.4050 0.086 Uiso 1 1 calc R . .
C28 C 0.4959(4) 0.0946(2) 0.32326(19) 0.0420(10) Uani 1 1 d . . .
H28A H 0.4886 0.1282 0.2858 0.063 Uiso 1 1 calc R . .
H28B H 0.5559 0.1207 0.3598 0.063 Uiso 1 1 calc R . .
H28C H 0.4026 0.0865 0.3314 0.063 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 0.0217(4) 0.0294(4) 0.0314(4) 0.0014(3) 0.0014(3) -0.0026(4)
P 0.0256(5) 0.0193(4) 0.0203(4) -0.0003(4) 0.0058(4) -0.0010(4)
Si1 0.0310(6) 0.0265(5) 0.0287(5) 0.0005(4) 0.0115(5) 0.0034(5)
Si2 0.0313(6) 0.0240(5) 0.0220(5) -0.0019(4) 0.0029(4) -0.0036(4)
N1 0.0268(18) 0.0202(14) 0.0361(17) 0.0052(12) 0.0132(14) -0.0004(12)
N2 0.0310(18) 0.0269(15) 0.0341(17) 0.0033(13) 0.0031(15) 0.0018(14)
N3 0.0275(18) 0.0244(15) 0.0384(18) -0.0029(14) 0.0007(15) 0.0031(13)
N4 0.0277(17) 0.0345(17) 0.049(2) 0.0113(15) 0.0093(17) 0.0013(15)
C1 0.0288(19) 0.0196(16) 0.0203(17) 0.0009(13) 0.0063(16) -0.0020(15)
C2 0.042(2) 0.039(2) 0.041(2) 0.0076(18) 0.021(2) 0.0040(18)
C3 0.052(3) 0.040(2) 0.042(2) -0.0088(18) 0.020(2) 0.0081(19)
C4 0.033(2) 0.034(2) 0.050(3) 0.0038(18) 0.0049(19) 0.0054(17)
C5 0.045(3) 0.031(2) 0.037(2) -0.0059(16) -0.001(2) -0.0074(18)
C6 0.046(3) 0.036(2) 0.0215(19) 0.0014(16) -0.0001(17) -0.0054(19)
C7 0.032(2) 0.043(2) 0.037(2) -0.0003(17) -0.0006(19) -0.0024(18)
C8 0.0187(18) 0.0197(15) 0.0220(17) 0.0031(13) 0.0017(14) 0.0012(14)
C9 0.0280(19) 0.0184(15) 0.0275(18) -0.0009(15) 0.0058(16) 0.0008(15)
C10 0.032(2) 0.0229(16) 0.0294(19) 0.0074(15) 0.0089(17) -0.0008(16)
C11 0.031(2) 0.0306(18) 0.0232(18) 0.0038(14) 0.0118(17) 0.0023(16)
C12 0.0203(17) 0.0268(17) 0.0225(18) 0.0013(14) 0.0064(15) 0.0049(15)
C13 0.023(2) 0.036(2) 0.028(2) -0.0066(15) 0.0057(16) 0.0055(16)
C14 0.032(2) 0.036(2) 0.038(2) -0.0153(17) 0.0055(19) -0.0013(17)
C15 0.028(2) 0.0230(17) 0.047(2) -0.0044(16) 0.0103(19) 0.0003(16)
C16 0.0177(18) 0.0189(15) 0.033(2) -0.0007(14) 0.0057(16) 0.0009(13)
C17 0.0159(16) 0.0188(15) 0.0235(18) -0.0005(13) 0.0021(15) 0.0014(14)
C18 0.043(2) 0.027(2) 0.058(3) 0.0070(18) 0.021(2) -0.0072(18)
C19 0.037(2) 0.0299(18) 0.034(2) 0.0121(16) 0.0097(19) 0.0073(17)
C20 0.039(3) 0.054(3) 0.054(3) 0.011(2) 0.009(2) -0.003(2)
C21 0.068(3) 0.034(2) 0.057(3) 0.004(2) 0.011(3) 0.011(2)
C22 0.040(2) 0.039(2) 0.034(2) 0.0063(18) -0.0030(19) 0.0037(19)
C23 0.047(3) 0.040(2) 0.036(2) -0.0060(19) -0.004(2) 0.000(2)
C24 0.042(3) 0.033(2) 0.061(3) -0.0083(19) 0.011(2) 0.0096(18)
C25 0.021(2) 0.035(2) 0.053(3) -0.0094(18) 0.0003(19) -0.0016(16)
C26 0.025(2) 0.0311(19) 0.068(3) -0.0020(19) 0.015(2) -0.0042(17)
C27 0.042(3) 0.063(3) 0.070(3) 0.031(2) 0.020(2) 0.004(2)
C28 0.036(2) 0.040(2) 0.050(3) 0.0009(19) 0.010(2) 0.0026(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
K N4 2.799(3) . ?
K N3 2.816(3) . ?
K N2 2.853(3) . ?
K N1 3.154(3) . ?
K P 3.1552(13) . ?
P C8 1.808(3) . ?
P C1 1.901(3) . ?
Si1 C4 1.864(4) . ?
Si1 C2 1.882(4) . ?
Si1 C1 1.882(4) . ?
Si1 C3 1.885(4) . ?
Si2 C1 1.860(4) . ?
Si2 C6 1.872(3) . ?
Si2 C7 1.881(4) . ?
Si2 C5 1.882(4) . ?
N1 C16 1.419(4) . ?
N1 C19 1.457(4) . ?
N1 C18 1.459(4) . ?
N2 C21 1.462(5) . ?
N2 C22 1.467(4) . ?
N2 C20 1.478(5) . ?
N3 C23 1.464(5) . ?
N3 C24 1.473(4) . ?
N3 C25 1.474(5) . ?
N4 C26 1.468(5) . ?
N4 C27 1.468(5) . ?
N4 C28 1.475(5) . ?
C1 H1A 1.000 . ?
C2 H2A 0.980 . ?
C2 H2B 0.980 . ?
C2 H2C 0.980 . ?
C3 H3A 0.980 . ?
C3 H3B 0.980 . ?
C3 H3C 0.980 . ?
C4 H4A 0.980 . ?
C4 H4B 0.980 . ?
C4 H4C 0.980 . ?
C5 H5A 0.980 . ?
C5 H5B 0.980 . ?
C5 H5C 0.980 . ?
C6 H6A 0.980 . ?
C6 H6B 0.980 . ?
C6 H6C 0.980 . ?
C7 H7A 0.980 . ?
C7 H7B 0.980 . ?
C7 H7C 0.980 . ?
C8 C9 1.416(4) . ?
C8 C17 1.485(4) . ?
C9 C10 1.390(5) . ?
C9 H9A 0.950 . ?
C10 C11 1.373(5) . ?
C10 H10A 0.950 . ?
C11 C12 1.416(5) . ?
C11 H11A 0.950 . ?
C12 C13 1.411(4) . ?
C12 C17 1.445(4) . ?
C13 C14 1.361(5) . ?
C13 H13A 0.950 . ?
C14 C15 1.399(5) . ?
C14 H14A 0.950 . ?
C15 C16 1.387(5) . ?
C15 H15A 0.950 . ?
C16 C17 1.441(4) . ?
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 C23 1.508(5) . ?
C22 H22A 0.990 . ?
C22 H22B 0.990 . ?
C23 H23A 0.990 . ?
C23 H23B 0.990 . ?
C24 H24A 0.980 . ?
C24 H24B 0.980 . ?
C24 H24C 0.980 . ?
C25 C26 1.504(5) . ?
C25 H25A 0.990 . ?
C25 H25B 0.990 . ?
C26 H26A 0.990 . ?
C26 H26B 0.990 . ?
C27 H27A 0.980 . ?
C27 H27B 0.980 . ?
C27 H27C 0.980 . ?
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
N4 K N3 65.40(9) . . ?
N4 K N2 104.96(9) . . ?
N3 K N2 64.69(8) . . ?
N4 K N1 104.71(8) . . ?
N3 K N1 115.89(8) . . ?
N2 K N1 146.65(9) . . ?
N4 K P 119.49(7) . . ?
N3 K P 168.82(7) . . ?
N2 K P 120.39(7) . . ?
N1 K P 53.95(5) . . ?
C8 P C1 104.45(14) . . ?
C8 P K 76.35(11) . . ?
C1 P K 120.63(11) . . ?
C4 Si1 C2 108.55(18) . . ?
C4 Si1 C1 108.66(17) . . ?
C2 Si1 C1 113.35(16) . . ?
C4 Si1 C3 105.87(18) . . ?
C2 Si1 C3 106.57(17) . . ?
C1 Si1 C3 113.49(17) . . ?
C1 Si2 C6 109.41(16) . . ?
C1 Si2 C7 113.28(16) . . ?
C6 Si2 C7 106.31(17) . . ?
C1 Si2 C5 111.19(16) . . ?
C6 Si2 C5 109.08(17) . . ?
C7 Si2 C5 107.39(18) . . ?
C16 N1 C19 113.7(3) . . ?
C16 N1 C18 117.5(3) . . ?
C19 N1 C18 110.6(3) . . ?
C16 N1 K 71.33(17) . . ?
C19 N1 K 149.5(2) . . ?
C18 N1 K 90.8(2) . . ?
C21 N2 C22 109.0(3) . . ?
C21 N2 C20 109.4(3) . . ?
C22 N2 C20 111.0(3) . . ?
C21 N2 K 122.0(2) . . ?
C22 N2 K 112.5(2) . . ?
C20 N2 K 91.6(2) . . ?
C23 N3 C24 108.5(3) . . ?
C23 N3 C25 112.2(3) . . ?
C24 N3 C25 110.2(3) . . ?
C23 N3 K 108.7(2) . . ?
C24 N3 K 110.6(2) . . ?
C25 N3 K 106.7(2) . . ?
C26 N4 C27 110.9(3) . . ?
C26 N4 C28 111.1(3) . . ?
C27 N4 C28 108.6(3) . . ?
C26 N4 K 113.2(2) . . ?
C27 N4 K 119.1(2) . . ?
C28 N4 K 92.3(2) . . ?
Si2 C1 Si1 119.37(17) . . ?
Si2 C1 P 109.29(16) . . ?
Si1 C1 P 105.37(16) . . ?
Si2 C1 H1A 107.4 . . ?
Si1 C1 H1A 107.4 . . ?
P C1 H1A 107.4 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C17 113.9(3) . . ?
C9 C8 P 122.8(2) . . ?
C17 C8 P 123.2(2) . . ?
C10 C9 C8 124.9(3) . . ?
C10 C9 H9A 117.6 . . ?
C8 C9 H9A 117.6 . . ?
C11 C10 C9 121.2(3) . . ?
C11 C10 H10A 119.4 . . ?
C9 C10 H10A 119.4 . . ?
C10 C11 C12 118.8(3) . . ?
C10 C11 H11A 120.6 . . ?
C12 C11 H11A 120.6 . . ?
C13 C12 C11 118.9(3) . . ?
C13 C12 C17 120.1(3) . . ?
C11 C12 C17 121.0(3) . . ?
C14 C13 C12 121.2(3) . . ?
C14 C13 H13A 119.4 . . ?
C12 C13 H13A 119.4 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15A 119.5 . . ?
C14 C15 H15A 119.5 . . ?
C15 C16 N1 120.7(3) . . ?
C15 C16 C17 120.6(3) . . ?
N1 C16 C17 118.7(3) . . ?
C16 C17 C12 116.3(3) . . ?
C16 C17 C8 124.2(3) . . ?
C12 C17 C8 119.4(3) . . ?
N1 C18 H18A 109.5 . . ?
N1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 C23 114.6(3) . . ?
N2 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
N2 C22 H22B 108.6 . . ?
C23 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
N3 C23 C22 115.4(3) . . ?
N3 C23 H23A 108.4 . . ?
C22 C23 H23A 108.4 . . ?
N3 C23 H23B 108.4 . . ?
C22 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 C26 115.4(3) . . ?
N3 C25 H25A 108.4 . . ?
C26 C25 H25A 108.4 . . ?
K C25 H25A 157.7 . . ?
N3 C25 H25B 108.4 . . ?
C26 C25 H25B 108.4 . . ?
K C25 H25B 87.0 . . ?
H25A C25 H25B 107.5 . . ?
N4 C26 C25 113.9(3) . . ?
N4 C26 H26A 108.8 . . ?
C25 C26 H26A 108.8 . . ?
N4 C26 H26B 108.8 . . ?
C25 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N4 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.070

#===END