Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002


data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'Gibson, Ashleigh E.'
'Price, Clayton'
'Clegg, William'
'Houlton, Andrew'


_publ_contact_author_name     	'Dr Andrew Houlton'  
_publ_contact_author_address 
;
Dr Andrew Houlton
Department of Chemistry
University of Newcastle upon Tyne
Newcastle upon Tyne
NE1 7RU
UNITED KINGDOM
;

_publ_contact_author_email       'ANDREW.HOULTON@NCL.AC.UK'

_publ_section_title
;
Inner-and outer-sphere binding of the minor groove site of adenine
by alkali metal ions
;

data_ah70
_database_code_CSD                167590
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C43 H54 B N6 Na O6'
_chemical_formula_weight          784.72

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'
'B'  'B'   0.0013   0.0007
'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'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/n

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

_cell_length_a                    15.1053(13)
_cell_length_b                    13.3332(12)
_cell_length_c                    22.2103(19)
_cell_angle_alpha                 90.00
_cell_angle_beta                  108.227(2)
_cell_angle_gamma                 90.00
_cell_volume                      4248.8(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     6453
_cell_measurement_theta_min       2.48
_cell_measurement_theta_max       28.20

_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.55
_exptl_crystal_size_mid           0.50
_exptl_crystal_size_min           0.28
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.227
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1672
_exptl_absorpt_coefficient_mu     0.091
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.952
_exptl_absorpt_correction_T_max   0.975
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       160(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        '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             27020
_diffrn_reflns_av_R_equivalents   0.0205
_diffrn_reflns_av_sigmaI/netI     0.0211
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        20
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -28
_diffrn_reflns_limit_l_max        29
_diffrn_reflns_theta_min          1.81
_diffrn_reflns_theta_max          28.39
_reflns_number_total              9827
_reflns_number_gt                 7982
_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^)+(0.0544P)^2^+1.0019P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0037(4)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          9827
_refine_ls_number_parameters      527
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0498
_refine_ls_R_factor_gt            0.0394
_refine_ls_wR_factor_ref          0.1103
_refine_ls_wR_factor_gt           0.1034
_refine_ls_goodness_of_fit_ref    1.039
_refine_ls_restrained_S_all       1.039
_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 0.35960(4) 0.32934(4) 0.09424(2) 0.03484(13) Uani 1 1 d . . .
N1 N 0.30606(9) 0.29998(10) 0.40260(6) 0.0456(3) Uani 1 1 d . . .
C2 C 0.29668(11) 0.28023(12) 0.34175(7) 0.0486(4) Uani 1 1 d . . .
H2 H 0.2437 0.2413 0.3199 0.058 Uiso 1 1 calc R . .
N3 N 0.35124(8) 0.30745(9) 0.30745(5) 0.0372(3) Uani 1 1 d . . .
C4 C 0.42244(8) 0.36419(9) 0.34190(5) 0.0260(2) Uani 1 1 d . . .
C5 C 0.43944(8) 0.39412(8) 0.40408(5) 0.0244(2) Uani 1 1 d . . .
C6 C 0.37826(9) 0.35750(9) 0.43549(6) 0.0313(3) Uani 1 1 d . . .
N6 N 0.39046(9) 0.37626(10) 0.49679(5) 0.0403(3) Uani 1 1 d D . .
H6A H 0.4279(11) 0.4238(12) 0.5169(8) 0.048 Uiso 1 1 d D . .
H6B H 0.3495(11) 0.3539(12) 0.5129(8) 0.048 Uiso 1 1 d D . .
N7 N 0.51724(7) 0.45542(8) 0.42345(4) 0.0265(2) Uani 1 1 d . . .
C8 C 0.54544(8) 0.46041(9) 0.37320(5) 0.0267(2) Uani 1 1 d . . .
H8 H 0.5982 0.4983 0.3722 0.032 Uiso 1 1 calc R . .
N9 N 0.49215(6) 0.40640(7) 0.32271(4) 0.0247(2) Uani 1 1 d . . .
C10 C 0.50501(8) 0.39463(9) 0.26062(5) 0.0268(2) Uani 1 1 d . . .
H10A H 0.5514 0.4440 0.2560 0.032 Uiso 1 1 calc R . .
H10B H 0.4453 0.4078 0.2270 0.032 Uiso 1 1 calc R . .
C11 C 0.53824(8) 0.28893(9) 0.25299(5) 0.0295(2) Uani 1 1 d . . .
H11A H 0.6027 0.2801 0.2817 0.035 Uiso 1 1 calc R . .
H11B H 0.4979 0.2397 0.2653 0.035 Uiso 1 1 calc R . .
N12 N 0.53609(7) 0.26943(8) 0.18756(5) 0.0295(2) Uani 1 1 d . . .
C13 C 0.54240(10) 0.16030(11) 0.17772(6) 0.0393(3) Uani 1 1 d . . .
H13A H 0.5866 0.1306 0.2163 0.047 Uiso 1 1 calc R . .
H13B H 0.5680 0.1493 0.1423 0.047 Uiso 1 1 calc R . .
C14 C 0.45108(11) 0.10676(10) 0.16328(6) 0.0406(3) Uani 1 1 d . . .
H14A H 0.4611 0.0334 0.1636 0.049 Uiso 1 1 calc R . .
H14B H 0.4211 0.1229 0.1959 0.049 Uiso 1 1 calc R . .
O15 O 0.39228(6) 0.13795(7) 0.10206(4) 0.0359(2) Uani 1 1 d . . .
C16 C 0.31229(10) 0.07523(10) 0.08091(8) 0.0439(3) Uani 1 1 d . . .
H16A H 0.2839 0.0669 0.1152 0.053 Uiso 1 1 calc R . .
H16B H 0.3306 0.0082 0.0698 0.053 Uiso 1 1 calc R . .
C17 C 0.24338(11) 0.12140(11) 0.02433(7) 0.0453(3) Uani 1 1 d . . .
H17A H 0.2712 0.1296 -0.0103 0.054 Uiso 1 1 calc R . .
H17B H 0.1875 0.0782 0.0089 0.054 Uiso 1 1 calc R . .
O18 O 0.21847(7) 0.21671(7) 0.04324(4) 0.0402(2) Uani 1 1 d . . .
C19 C 0.13578(11) 0.25638(13) -0.00056(8) 0.0533(4) Uani 1 1 d . . .
H19A H 0.0821 0.2123 -0.0028 0.064 Uiso 1 1 calc R . .
H19B H 0.1427 0.2607 -0.0434 0.064 Uiso 1 1 calc R . .
C20 C 0.12011(10) 0.35833(13) 0.02194(8) 0.0499(4) Uani 1 1 d . . .
H20A H 0.0625 0.3881 -0.0071 0.060 Uiso 1 1 calc R . .
H20B H 0.1135 0.3542 0.0648 0.060 Uiso 1 1 calc R . .
O21 O 0.19823(7) 0.41785(8) 0.02321(5) 0.0419(2) Uani 1 1 d . . .
C22 C 0.19277(11) 0.51722(12) 0.04485(8) 0.0504(4) Uani 1 1 d . . .
H22A H 0.1941 0.5165 0.0897 0.060 Uiso 1 1 calc R . .
H22B H 0.1341 0.5495 0.0191 0.060 Uiso 1 1 calc R . .
C23 C 0.27468(11) 0.57310(11) 0.03828(8) 0.0505(4) Uani 1 1 d . . .
H23A H 0.2718 0.5757 -0.0068 0.061 Uiso 1 1 calc R . .
H23B H 0.2745 0.6427 0.0538 0.061 Uiso 1 1 calc R . .
O24 O 0.35751(6) 0.52273(7) 0.07459(4) 0.0366(2) Uani 1 1 d . . .
C25 C 0.43764(10) 0.56273(10) 0.06210(7) 0.0401(3) Uani 1 1 d . . .
H25A H 0.4459 0.6341 0.0749 0.048 Uiso 1 1 calc R . .
H25B H 0.4298 0.5583 0.0162 0.048 Uiso 1 1 calc R . .
C26 C 0.52040(10) 0.50371(11) 0.09883(7) 0.0404(3) Uani 1 1 d . . .
H26A H 0.5773 0.5306 0.0916 0.048 Uiso 1 1 calc R . .
H26B H 0.5282 0.5081 0.1447 0.048 Uiso 1 1 calc R . .
O27 O 0.50640(6) 0.40197(7) 0.07831(4) 0.0338(2) Uani 1 1 d . . .
C28 C 0.58786(9) 0.34082(12) 0.10209(6) 0.0390(3) Uani 1 1 d . . .
H28A H 0.6410 0.3745 0.0934 0.047 Uiso 1 1 calc R . .
H28B H 0.5773 0.2760 0.0792 0.047 Uiso 1 1 calc R . .
C29 C 0.61279(8) 0.32087(12) 0.17268(6) 0.0366(3) Uani 1 1 d . . .
H29A H 0.6696 0.2789 0.1866 0.044 Uiso 1 1 calc R . .
H29B H 0.6262 0.3852 0.1960 0.044 Uiso 1 1 calc R . .
O30 O 0.28793(7) 0.31461(8) 0.17257(5) 0.0432(2) Uani 1 1 d D . .
H30A H 0.2431(11) 0.2746(13) 0.1602(8) 0.052 Uiso 1 1 d D . .
H30B H 0.3048(12) 0.3103(13) 0.2139(7) 0.052 Uiso 1 1 d D . .
B B 0.94002(9) 0.26145(10) 0.22889(6) 0.0284(3) Uani 1 1 d . . .
C31 C 0.94275(10) 0.37446(10) 0.19958(6) 0.0351(3) Uani 1 1 d . . .
C32 C 0.86276(13) 0.43433(12) 0.17985(7) 0.0524(4) Uani 1 1 d . . .
H32 H 0.8059 0.4088 0.1834 0.063 Uiso 1 1 calc R . .
C33 C 0.86387(18) 0.53075(14) 0.15503(8) 0.0746(7) Uani 1 1 d . . .
H33 H 0.8079 0.5686 0.1409 0.090 Uiso 1 1 calc R . .
C34 C 0.9462(2) 0.57086(13) 0.15102(8) 0.0751(7) Uani 1 1 d . . .
H34 H 0.9470 0.6361 0.1340 0.090 Uiso 1 1 calc R . .
C35 C 1.02628(17) 0.51596(12) 0.17174(8) 0.0663(5) Uani 1 1 d . . .
H35 H 1.0834 0.5436 0.1699 0.080 Uiso 1 1 calc R . .
C36 C 1.02469(13) 0.41943(11) 0.19551(7) 0.0473(4) Uani 1 1 d . . .
H36 H 1.0813 0.3826 0.2095 0.057 Uiso 1 1 calc R . .
C37 C 0.93769(9) 0.27884(9) 0.30188(6) 0.0314(3) Uani 1 1 d . . .
C38 C 0.85918(10) 0.26483(12) 0.32157(7) 0.0422(3) Uani 1 1 d . . .
H38 H 0.8036 0.2406 0.2917 0.051 Uiso 1 1 calc R . .
C39 C 0.85893(12) 0.28489(14) 0.38330(7) 0.0528(4) Uani 1 1 d . . .
H39 H 0.8042 0.2732 0.3947 0.063 Uiso 1 1 calc R . .
C40 C 0.93815(12) 0.32167(12) 0.42778(7) 0.0494(4) Uani 1 1 d . . .
H40 H 0.9385 0.3353 0.4698 0.059 Uiso 1 1 calc R . .
C41 C 1.01656(12) 0.33822(10) 0.41019(7) 0.0444(3) Uani 1 1 d . . .
H41 H 1.0712 0.3643 0.4402 0.053 Uiso 1 1 calc R . .
C42 C 1.01643(10) 0.31691(10) 0.34851(6) 0.0370(3) Uani 1 1 d . . .
H42 H 1.0717 0.3286 0.3377 0.044 Uiso 1 1 calc R . .
C43 C 0.85132(8) 0.19475(9) 0.18516(6) 0.0296(3) Uani 1 1 d . . .
C44 C 0.80697(9) 0.21342(11) 0.12053(6) 0.0349(3) Uani 1 1 d . . .
H44 H 0.8242 0.2713 0.1019 0.042 Uiso 1 1 calc R . .
C45 C 0.73839(9) 0.14983(12) 0.08267(7) 0.0431(3) Uani 1 1 d . . .
H45 H 0.7099 0.1653 0.0391 0.052 Uiso 1 1 calc R . .
C46 C 0.71155(9) 0.06457(12) 0.10804(8) 0.0474(4) Uani 1 1 d . . .
H46 H 0.6651 0.0213 0.0822 0.057 Uiso 1 1 calc R . .
C47 C 0.75330(9) 0.04337(11) 0.17159(8) 0.0442(3) Uani 1 1 d . . .
H47 H 0.7354 -0.0146 0.1898 0.053 Uiso 1 1 calc R . .
C48 C 0.82174(9) 0.10720(10) 0.20889(7) 0.0351(3) Uani 1 1 d . . .
H48 H 0.8498 0.0909 0.2523 0.042 Uiso 1 1 calc R . .
C49 C 1.03082(8) 0.19539(9) 0.22636(6) 0.0276(2) Uani 1 1 d . . .
C50 C 1.05398(9) 0.19004(10) 0.16971(6) 0.0329(3) Uani 1 1 d . . .
H50 H 1.0185 0.2283 0.1343 0.039 Uiso 1 1 calc R . .
C51 C 1.12640(9) 0.13116(10) 0.16349(7) 0.0365(3) Uani 1 1 d . . .
H51 H 1.1397 0.1301 0.1244 0.044 Uiso 1 1 calc R . .
C52 C 1.17941(9) 0.07380(10) 0.21410(7) 0.0378(3) Uani 1 1 d . . .
H52 H 1.2297 0.0342 0.2103 0.045 Uiso 1 1 calc R . .
C53 C 1.15761(8) 0.07529(10) 0.27015(7) 0.0350(3) Uani 1 1 d . . .
H53 H 1.1925 0.0354 0.3050 0.042 Uiso 1 1 calc R . .
C54 C 1.08474(8) 0.13496(9) 0.27584(6) 0.0295(2) Uani 1 1 d . . .
H54 H 1.0712 0.1346 0.3148 0.035 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 0.0380(3) 0.0357(3) 0.0312(3) -0.0030(2) 0.0114(2) -0.0003(2)
N1 0.0513(7) 0.0514(7) 0.0430(6) -0.0162(6) 0.0276(6) -0.0285(6)
C2 0.0495(8) 0.0577(9) 0.0445(8) -0.0203(7) 0.0232(7) -0.0321(7)
N3 0.0387(6) 0.0429(6) 0.0327(5) -0.0122(5) 0.0151(5) -0.0185(5)
C4 0.0273(5) 0.0267(6) 0.0255(5) -0.0004(4) 0.0102(4) -0.0031(4)
C5 0.0248(5) 0.0246(5) 0.0237(5) 0.0000(4) 0.0077(4) -0.0025(4)
C6 0.0370(6) 0.0302(6) 0.0311(6) -0.0031(5) 0.0168(5) -0.0083(5)
N6 0.0513(7) 0.0457(7) 0.0326(6) -0.0094(5) 0.0257(5) -0.0216(6)
N7 0.0250(5) 0.0317(5) 0.0231(5) -0.0007(4) 0.0078(4) -0.0047(4)
C8 0.0231(5) 0.0319(6) 0.0249(5) -0.0009(5) 0.0074(4) -0.0044(4)
N9 0.0261(5) 0.0277(5) 0.0220(4) -0.0011(4) 0.0098(4) -0.0031(4)
C10 0.0306(6) 0.0306(6) 0.0213(5) -0.0002(4) 0.0112(4) -0.0022(5)
C11 0.0299(6) 0.0354(6) 0.0241(5) 0.0015(5) 0.0099(4) 0.0051(5)
N12 0.0273(5) 0.0379(6) 0.0252(5) -0.0018(4) 0.0107(4) 0.0061(4)
C13 0.0421(7) 0.0431(8) 0.0311(6) -0.0021(6) 0.0093(5) 0.0207(6)
C14 0.0591(9) 0.0291(6) 0.0332(7) 0.0019(5) 0.0140(6) 0.0098(6)
O15 0.0404(5) 0.0333(5) 0.0336(5) -0.0004(4) 0.0111(4) -0.0006(4)
C16 0.0466(8) 0.0302(7) 0.0585(9) -0.0066(6) 0.0216(7) -0.0036(6)
C17 0.0439(8) 0.0425(8) 0.0475(8) -0.0156(6) 0.0114(6) -0.0092(6)
O18 0.0389(5) 0.0375(5) 0.0371(5) -0.0046(4) 0.0017(4) -0.0027(4)
C19 0.0388(8) 0.0583(10) 0.0490(9) -0.0063(7) -0.0062(6) -0.0027(7)
C20 0.0295(7) 0.0609(10) 0.0510(9) -0.0002(7) 0.0009(6) 0.0039(6)
O21 0.0411(5) 0.0429(6) 0.0409(5) -0.0005(4) 0.0117(4) 0.0077(4)
C22 0.0457(8) 0.0464(9) 0.0590(9) -0.0024(7) 0.0162(7) 0.0169(7)
C23 0.0559(9) 0.0342(7) 0.0620(10) 0.0064(7) 0.0191(8) 0.0160(7)
O24 0.0435(5) 0.0323(5) 0.0379(5) 0.0022(4) 0.0185(4) 0.0045(4)
C25 0.0568(8) 0.0322(7) 0.0397(7) 0.0001(6) 0.0273(6) -0.0021(6)
C26 0.0442(7) 0.0441(8) 0.0375(7) -0.0067(6) 0.0195(6) -0.0085(6)
O27 0.0336(5) 0.0398(5) 0.0281(4) -0.0010(4) 0.0099(3) 0.0051(4)
C28 0.0313(6) 0.0590(9) 0.0298(6) 0.0034(6) 0.0140(5) 0.0110(6)
C29 0.0243(6) 0.0596(9) 0.0277(6) 0.0019(6) 0.0106(5) 0.0057(6)
O30 0.0409(5) 0.0564(7) 0.0309(5) -0.0100(5) 0.0096(4) -0.0173(5)
B 0.0292(6) 0.0277(6) 0.0268(6) -0.0014(5) 0.0069(5) 0.0019(5)
C31 0.0486(7) 0.0288(6) 0.0247(6) -0.0035(5) 0.0068(5) 0.0021(5)
C32 0.0638(10) 0.0371(8) 0.0432(8) -0.0046(6) -0.0022(7) 0.0121(7)
C33 0.1155(18) 0.0401(9) 0.0444(9) -0.0013(8) -0.0093(10) 0.0292(11)
C34 0.156(2) 0.0305(8) 0.0364(9) 0.0023(7) 0.0261(11) 0.0010(12)
C35 0.1260(17) 0.0344(8) 0.0526(10) -0.0047(7) 0.0481(11) -0.0149(10)
C36 0.0713(10) 0.0326(7) 0.0435(8) -0.0020(6) 0.0260(7) -0.0053(7)
C37 0.0392(7) 0.0249(6) 0.0288(6) 0.0002(5) 0.0086(5) 0.0072(5)
C38 0.0382(7) 0.0528(9) 0.0353(7) -0.0062(6) 0.0110(5) 0.0111(6)
C39 0.0527(9) 0.0678(11) 0.0437(8) -0.0059(8) 0.0234(7) 0.0132(8)
C40 0.0714(10) 0.0469(9) 0.0303(7) -0.0041(6) 0.0163(7) 0.0137(8)
C41 0.0624(9) 0.0307(7) 0.0322(7) -0.0042(5) 0.0032(6) 0.0001(6)
C42 0.0481(8) 0.0273(6) 0.0333(6) -0.0018(5) 0.0093(6) -0.0030(5)
C43 0.0251(5) 0.0318(6) 0.0335(6) -0.0072(5) 0.0112(5) 0.0056(5)
C44 0.0286(6) 0.0444(7) 0.0330(6) -0.0092(6) 0.0115(5) 0.0045(5)
C45 0.0283(6) 0.0623(9) 0.0380(7) -0.0216(7) 0.0094(5) 0.0043(6)
C46 0.0256(6) 0.0537(9) 0.0647(10) -0.0299(8) 0.0168(6) -0.0042(6)
C47 0.0310(7) 0.0370(7) 0.0707(10) -0.0132(7) 0.0246(7) -0.0007(5)
C48 0.0292(6) 0.0338(7) 0.0454(7) -0.0047(6) 0.0159(5) 0.0057(5)
C49 0.0255(5) 0.0249(6) 0.0311(6) -0.0027(5) 0.0071(4) -0.0042(4)
C50 0.0320(6) 0.0337(6) 0.0331(6) -0.0007(5) 0.0103(5) -0.0018(5)
C51 0.0331(6) 0.0371(7) 0.0440(7) -0.0066(6) 0.0188(6) -0.0061(5)
C52 0.0262(6) 0.0328(7) 0.0559(8) -0.0056(6) 0.0150(6) -0.0022(5)
C53 0.0267(6) 0.0292(6) 0.0452(7) 0.0022(5) 0.0057(5) -0.0020(5)
C54 0.0268(6) 0.0271(6) 0.0337(6) -0.0007(5) 0.0081(5) -0.0056(5)

_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na O30 2.3271(11) . ?
Na O27 2.5437(10) . ?
Na O18 2.5636(11) . ?
Na O15 2.5947(11) . ?
Na O24 2.6137(11) . ?
Na O21 2.7235(11) . ?
Na N12 2.9299(11) . ?
N1 C2 1.3403(18) . ?
N1 C6 1.3463(17) . ?
C2 N3 1.3358(17) . ?
N3 C4 1.3415(15) . ?
C4 N9 1.3739(14) . ?
C4 C5 1.3823(15) . ?
C5 N7 1.3849(14) . ?
C5 C6 1.4082(15) . ?
C6 N6 1.3390(16) . ?
N7 C8 1.3148(15) . ?
C8 N9 1.3636(14) . ?
N9 C10 1.4602(14) . ?
C10 C11 1.5232(17) . ?
C11 N12 1.4666(14) . ?
N12 C29 1.4702(16) . ?
N12 C13 1.4789(17) . ?
C13 C14 1.496(2) . ?
C14 O15 1.4335(16) . ?
O15 C16 1.4230(17) . ?
C16 C17 1.491(2) . ?
C17 O18 1.4254(17) . ?
O18 C19 1.4235(17) . ?
C19 C20 1.492(2) . ?
C20 O21 1.4149(19) . ?
O21 C22 1.4205(18) . ?
C22 C23 1.490(2) . ?
C23 O24 1.4268(18) . ?
O24 C25 1.4270(16) . ?
C25 C26 1.486(2) . ?
C26 O27 1.4256(17) . ?
O27 C28 1.4322(15) . ?
C28 C29 1.5170(17) . ?
B C49 1.6457(17) . ?
B C31 1.6470(19) . ?
B C43 1.6478(18) . ?
B C37 1.6489(18) . ?
C31 C32 1.399(2) . ?
C31 C36 1.403(2) . ?
C32 C33 1.401(3) . ?
C33 C34 1.382(3) . ?
C34 C35 1.365(3) . ?
C35 C36 1.394(2) . ?
C37 C38 1.3990(19) . ?
C37 C42 1.4051(18) . ?
C38 C39 1.398(2) . ?
C39 C40 1.382(2) . ?
C40 C41 1.376(2) . ?
C41 C42 1.3984(19) . ?
C43 C44 1.4035(18) . ?
C43 C48 1.4097(19) . ?
C44 C45 1.3980(19) . ?
C45 C46 1.385(2) . ?
C46 C47 1.383(2) . ?
C47 C48 1.394(2) . ?
C49 C54 1.4001(17) . ?
C49 C50 1.4092(17) . ?
C50 C51 1.3881(18) . ?
C51 C52 1.388(2) . ?
C52 C53 1.384(2) . ?
C53 C54 1.3955(18) . ?

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
O30 Na O27 139.97(4) . . ?
O30 Na O18 76.34(4) . . ?
O27 Na O18 143.33(4) . . ?
O30 Na O15 89.44(4) . . ?
O27 Na O15 103.17(3) . . ?
O18 Na O15 64.40(3) . . ?
O30 Na O24 102.94(4) . . ?
O27 Na O24 64.32(3) . . ?
O18 Na O24 122.63(4) . . ?
O15 Na O24 166.79(4) . . ?
O30 Na O21 85.89(4) . . ?
O27 Na O21 114.56(4) . . ?
O18 Na O21 61.84(3) . . ?
O15 Na O21 125.59(4) . . ?
O24 Na O21 60.92(3) . . ?
O30 Na N12 88.93(4) . . ?
O27 Na N12 64.04(3) . . ?
O18 Na N12 126.85(4) . . ?
O15 Na N12 64.69(3) . . ?
O24 Na N12 110.36(3) . . ?
O21 Na N12 168.34(4) . . ?
C2 N1 C6 118.12(11) . . ?
N3 C2 N1 129.22(12) . . ?
C2 N3 C4 110.83(11) . . ?
N3 C4 N9 127.56(10) . . ?
N3 C4 C5 126.72(11) . . ?
N9 C4 C5 105.71(10) . . ?
C4 C5 N7 110.80(9) . . ?
C4 C5 C6 116.70(10) . . ?
N7 C5 C6 132.49(10) . . ?
N6 C6 N1 119.25(11) . . ?
N6 C6 C5 122.41(11) . . ?
N1 C6 C5 118.32(11) . . ?
C8 N7 C5 103.59(9) . . ?
N7 C8 N9 114.00(10) . . ?
C8 N9 C4 105.89(9) . . ?
C8 N9 C10 127.94(9) . . ?
C4 N9 C10 126.17(9) . . ?
N9 C10 C11 110.50(9) . . ?
N12 C11 C10 111.61(9) . . ?
C11 N12 C29 111.43(10) . . ?
C11 N12 C13 109.77(10) . . ?
C29 N12 C13 109.51(10) . . ?
C11 N12 Na 112.70(7) . . ?
C29 N12 Na 108.69(7) . . ?
C13 N12 Na 104.49(7) . . ?
N12 C13 C14 113.79(10) . . ?
O15 C14 C13 108.73(11) . . ?
C16 O15 C14 110.66(11) . . ?
C16 O15 Na 115.58(8) . . ?
C14 O15 Na 113.41(7) . . ?
O15 C16 C17 109.42(12) . . ?
O18 C17 C16 107.38(11) . . ?
C19 O18 C17 112.70(11) . . ?
C19 O18 Na 121.00(9) . . ?
C17 O18 Na 113.13(8) . . ?
O18 C19 C20 107.87(12) . . ?
O21 C20 C19 107.40(13) . . ?
C20 O21 C22 113.18(11) . . ?
C20 O21 Na 110.99(8) . . ?
C22 O21 Na 110.14(8) . . ?
O21 C22 C23 107.19(12) . . ?
O24 C23 C22 108.52(12) . . ?
C23 O24 C25 111.19(11) . . ?
C23 O24 Na 121.43(9) . . ?
C25 O24 Na 115.75(8) . . ?
O24 C25 C26 108.32(11) . . ?
O27 C26 C25 108.24(11) . . ?
C26 O27 C28 113.54(10) . . ?
C26 O27 Na 111.49(7) . . ?
C28 O27 Na 114.70(8) . . ?
O27 C28 C29 112.82(10) . . ?
N12 C29 C28 110.84(10) . . ?
C49 B C31 110.61(10) . . ?
C49 B C43 102.94(9) . . ?
C31 B C43 112.15(10) . . ?
C49 B C37 112.53(10) . . ?
C31 B C37 105.71(10) . . ?
C43 B C37 113.07(10) . . ?
C32 C31 C36 115.38(14) . . ?
C32 C31 B 121.32(13) . . ?
C36 C31 B 123.22(12) . . ?
C31 C32 C33 122.10(19) . . ?
C34 C33 C32 120.15(19) . . ?
C35 C34 C33 119.43(16) . . ?
C34 C35 C36 120.3(2) . . ?
C35 C36 C31 122.60(17) . . ?
C38 C37 C42 115.00(12) . . ?
C38 C37 B 124.72(11) . . ?
C42 C37 B 120.14(11) . . ?
C39 C38 C37 122.93(14) . . ?
C40 C39 C38 120.11(15) . . ?
C41 C40 C39 118.93(13) . . ?
C40 C41 C42 120.53(14) . . ?
C41 C42 C37 122.48(14) . . ?
C44 C43 C48 115.05(12) . . ?
C44 C43 B 123.17(12) . . ?
C48 C43 B 121.40(11) . . ?
C45 C44 C43 122.32(14) . . ?
C46 C45 C44 120.62(14) . . ?
C47 C46 C45 119.01(13) . . ?
C46 C47 C48 119.89(14) . . ?
C47 C48 C43 123.11(14) . . ?
C54 C49 C50 115.20(11) . . ?
C54 C49 B 124.58(11) . . ?
C50 C49 B 119.99(11) . . ?
C51 C50 C49 122.76(12) . . ?
C52 C51 C50 120.25(12) . . ?
C53 C52 C51 118.78(12) . . ?
C52 C53 C54 120.40(12) . . ?
C53 C54 C49 122.59(12) . . ?

_diffrn_measured_fraction_theta_max    0.923
_diffrn_reflns_theta_full              26.00
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    0.627
_refine_diff_density_min   -0.225
_refine_diff_density_rms    0.037

#===END


data_ah73
_database_code_CSD                167591
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C19 H32 F6 K N6 O5 P'
_chemical_formula_weight          608.58

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'
'F'  'F'   0.0171   0.0103
'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            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c

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

_cell_length_a                    8.5521(7)
_cell_length_b                    18.2322(16)
_cell_length_c                    17.0228(15)
_cell_angle_alpha                 90.00
_cell_angle_beta                  99.177(2)
_cell_angle_gamma                 90.00
_cell_volume                      2620.3(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     5693
_cell_measurement_theta_min       2.54
_cell_measurement_theta_max       28.26

_exptl_crystal_description        needle
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.45
_exptl_crystal_size_mid           0.24
_exptl_crystal_size_min           0.18
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.543
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1264
_exptl_absorpt_coefficient_mu     0.349
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.859
_exptl_absorpt_correction_T_max   0.940
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       160(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        '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             22262
_diffrn_reflns_av_R_equivalents   0.0295
_diffrn_reflns_av_sigmaI/netI     0.0215
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          1.65
_diffrn_reflns_theta_max          28.52
_reflns_number_total              6119
_reflns_number_gt                 5337
_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^)+(0.0388P)^2^+2.3688P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          6119
_refine_ls_number_parameters      349
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0523
_refine_ls_R_factor_gt            0.0452
_refine_ls_wR_factor_ref          0.1056
_refine_ls_wR_factor_gt           0.1021
_refine_ls_goodness_of_fit_ref    1.116
_refine_ls_restrained_S_all       1.116
_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
K K 0.66986(5) 0.60109(2) 0.77539(2) 0.02175(10) Uani 1 1 d . . .
N1 N 0.4064(2) 0.41641(9) 0.62615(11) 0.0281(4) Uani 1 1 d . . .
C2 C 0.5403(2) 0.45578(12) 0.64251(13) 0.0295(4) Uani 1 1 d . . .
H2 H 0.6275 0.4306 0.6722 0.035 Uiso 1 1 calc R . .
N3 N 0.5698(2) 0.52489(9) 0.62351(10) 0.0258(4) Uani 1 1 d . . .
C4 C 0.4404(2) 0.55545(10) 0.58032(11) 0.0199(4) Uani 1 1 d . . .
C5 C 0.2932(2) 0.52230(11) 0.55894(11) 0.0199(4) Uani 1 1 d . . .
C6 C 0.2776(2) 0.44924(11) 0.58388(12) 0.0225(4) Uani 1 1 d . . .
N6 N 0.1425(2) 0.41136(10) 0.56960(13) 0.0320(4) Uani 1 1 d D . .
H6A H 0.144(3) 0.3667(12) 0.5824(16) 0.038 Uiso 1 1 d D . .
H6B H 0.057(3) 0.4274(14) 0.5418(15) 0.038 Uiso 1 1 d D . .
N7 N 0.18751(19) 0.57000(9) 0.51455(10) 0.0246(4) Uani 1 1 d . . .
C8 C 0.2719(2) 0.62969(11) 0.51005(12) 0.0243(4) Uani 1 1 d . . .
H8 H 0.2303 0.6725 0.4824 0.029 Uiso 1 1 calc R . .
N9 N 0.42507(19) 0.62496(9) 0.54865(10) 0.0210(3) Uani 1 1 d . . .
C10 C 0.5526(2) 0.67912(11) 0.54774(12) 0.0222(4) Uani 1 1 d . . .
H10A H 0.5620 0.6906 0.4918 0.027 Uiso 1 1 calc R . .
H10B H 0.6541 0.6573 0.5732 0.027 Uiso 1 1 calc R . .
C11 C 0.5248(2) 0.75021(11) 0.59071(11) 0.0227(4) Uani 1 1 d . . .
H11A H 0.6012 0.7876 0.5784 0.027 Uiso 1 1 calc R . .
H11B H 0.4169 0.7684 0.5703 0.027 Uiso 1 1 calc R . .
N12 N 0.54173(18) 0.74143(9) 0.67804(9) 0.0204(3) Uani 1 1 d . . .
C13 C 0.6827(2) 0.77935(11) 0.72070(12) 0.0234(4) Uani 1 1 d . . .
H13A H 0.6894 0.7698 0.7784 0.028 Uiso 1 1 calc R . .
H13B H 0.6686 0.8328 0.7124 0.028 Uiso 1 1 calc R . .
C14 C 0.8381(2) 0.75679(11) 0.69541(12) 0.0260(4) Uani 1 1 d . . .
H14A H 0.8423 0.7751 0.6410 0.031 Uiso 1 1 calc R . .
H14B H 0.9277 0.7786 0.7320 0.031 Uiso 1 1 calc R . .
O15 O 0.85121(16) 0.67908(8) 0.69683(9) 0.0251(3) Uani 1 1 d . . .
C16 C 1.0033(2) 0.65367(14) 0.68408(14) 0.0322(5) Uani 1 1 d . . .
H16A H 1.0855 0.6697 0.7284 0.039 Uiso 1 1 calc R . .
H16B H 1.0292 0.6744 0.6340 0.039 Uiso 1 1 calc R . .
C17 C 0.9997(3) 0.57150(14) 0.67945(13) 0.0343(5) Uani 1 1 d . . .
H17A H 0.9175 0.5554 0.6352 0.041 Uiso 1 1 calc R . .
H17B H 1.1034 0.5527 0.6696 0.041 Uiso 1 1 calc R . .
O18 O 0.96527(17) 0.54367(8) 0.75299(9) 0.0281(3) Uani 1 1 d . . .
C19 C 0.9705(3) 0.46574(12) 0.75737(14) 0.0317(5) Uani 1 1 d . . .
H19A H 1.0795 0.4482 0.7556 0.038 Uiso 1 1 calc R . .
H19B H 0.8990 0.4443 0.7117 0.038 Uiso 1 1 calc R . .
C20 C 0.9194(3) 0.44292(12) 0.83379(14) 0.0320(5) Uani 1 1 d . . .
H20A H 0.9362 0.3896 0.8420 0.038 Uiso 1 1 calc R . .
H20B H 0.9831 0.4690 0.8789 0.038 Uiso 1 1 calc R . .
O21 O 0.75549(17) 0.46005(8) 0.83054(9) 0.0271(3) Uani 1 1 d . . .
C22 C 0.7032(3) 0.44764(12) 0.90502(13) 0.0302(5) Uani 1 1 d . . .
H22A H 0.7615 0.4802 0.9462 0.036 Uiso 1 1 calc R . .
H22B H 0.7243 0.3962 0.9219 0.036 Uiso 1 1 calc R . .
C23 C 0.5292(3) 0.46306(12) 0.89592(14) 0.0317(5) Uani 1 1 d . . .
H23A H 0.4726 0.4369 0.8489 0.038 Uiso 1 1 calc R . .
H23B H 0.4869 0.4460 0.9436 0.038 Uiso 1 1 calc R . .
O24 O 0.50649(16) 0.54016(8) 0.88633(9) 0.0267(3) Uani 1 1 d . . .
C25 C 0.3436(2) 0.56114(13) 0.87383(14) 0.0331(5) Uani 1 1 d . . .
H25A H 0.2914 0.5428 0.9179 0.040 Uiso 1 1 calc R . .
H25B H 0.2884 0.5400 0.8234 0.040 Uiso 1 1 calc R . .
C26 C 0.3360(3) 0.64337(14) 0.87045(13) 0.0330(5) Uani 1 1 d . . .
H26A H 0.2263 0.6601 0.8717 0.040 Uiso 1 1 calc R . .
H26B H 0.4059 0.6646 0.9168 0.040 Uiso 1 1 calc R . .
O27 O 0.38628(16) 0.66684(8) 0.79824(8) 0.0245(3) Uani 1 1 d . . .
C28 C 0.3864(2) 0.74489(11) 0.79193(13) 0.0277(4) Uani 1 1 d . . .
H28A H 0.4774 0.7654 0.8286 0.033 Uiso 1 1 calc R . .
H28B H 0.2878 0.7650 0.8071 0.033 Uiso 1 1 calc R . .
C29 C 0.3977(2) 0.76646(11) 0.70736(13) 0.0261(4) Uani 1 1 d . . .
H29A H 0.3043 0.7465 0.6719 0.031 Uiso 1 1 calc R . .
H29B H 0.3924 0.8206 0.7033 0.031 Uiso 1 1 calc R . .
P P 0.91148(6) 0.69157(3) 0.95783(3) 0.02253(12) Uani 1 1 d . . .
F1 F 0.9484(2) 0.62174(9) 0.90804(10) 0.0563(4) Uani 1 1 d . . .
F2 F 0.73540(17) 0.69468(9) 0.90779(9) 0.0483(4) Uani 1 1 d . . .
F3 F 0.87045(18) 0.76240(7) 1.00568(8) 0.0409(3) Uani 1 1 d . . .
F4 F 1.08599(17) 0.69048(9) 1.00699(10) 0.0522(4) Uani 1 1 d . . .
F5 F 0.97252(17) 0.74430(8) 0.89312(8) 0.0426(3) Uani 1 1 d . . .
F6 F 0.84891(17) 0.64007(7) 1.02216(8) 0.0368(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K 0.0215(2) 0.0215(2) 0.0234(2) 0.00207(16) 0.00732(15) 0.00146(15)
N1 0.0264(9) 0.0224(9) 0.0331(10) -0.0003(7) -0.0024(7) -0.0007(7)
C2 0.0259(10) 0.0267(10) 0.0325(11) -0.0002(9) -0.0057(8) 0.0021(8)
N3 0.0217(8) 0.0256(9) 0.0279(9) -0.0017(7) -0.0029(7) -0.0010(7)
C4 0.0198(9) 0.0231(9) 0.0169(8) -0.0046(7) 0.0033(7) -0.0013(7)
C5 0.0167(8) 0.0228(9) 0.0203(9) -0.0035(7) 0.0029(7) 0.0004(7)
C6 0.0227(9) 0.0212(9) 0.0234(9) -0.0055(8) 0.0034(7) -0.0004(7)
N6 0.0253(9) 0.0189(8) 0.0490(12) 0.0017(8) -0.0027(8) -0.0026(7)
N7 0.0200(8) 0.0241(8) 0.0285(9) 0.0010(7) 0.0003(7) 0.0002(6)
C8 0.0203(9) 0.0253(10) 0.0261(10) 0.0015(8) 0.0001(8) 0.0007(7)
N9 0.0195(8) 0.0226(8) 0.0207(8) -0.0008(6) 0.0027(6) -0.0021(6)
C10 0.0192(9) 0.0266(10) 0.0210(9) 0.0016(8) 0.0038(7) -0.0053(7)
C11 0.0248(9) 0.0223(9) 0.0198(9) 0.0025(7) 0.0000(7) -0.0021(7)
N12 0.0212(8) 0.0204(8) 0.0194(8) 0.0020(6) 0.0021(6) -0.0005(6)
C13 0.0253(10) 0.0214(9) 0.0219(9) 0.0013(7) -0.0014(7) -0.0024(7)
C14 0.0230(9) 0.0304(11) 0.0243(10) 0.0067(8) 0.0026(8) -0.0064(8)
O15 0.0178(6) 0.0294(7) 0.0290(7) 0.0038(6) 0.0070(5) 0.0001(5)
C16 0.0179(9) 0.0490(14) 0.0312(11) 0.0101(10) 0.0088(8) 0.0042(9)
C17 0.0291(11) 0.0486(14) 0.0273(11) 0.0022(10) 0.0114(9) 0.0131(10)
O18 0.0283(8) 0.0306(8) 0.0261(7) -0.0007(6) 0.0071(6) 0.0077(6)
C19 0.0252(10) 0.0298(11) 0.0396(12) -0.0084(9) 0.0033(9) 0.0070(8)
C20 0.0298(11) 0.0247(10) 0.0383(12) 0.0012(9) -0.0044(9) 0.0081(8)
O21 0.0280(7) 0.0266(7) 0.0254(7) 0.0024(6) 0.0002(6) 0.0045(6)
C22 0.0407(12) 0.0236(10) 0.0250(10) 0.0064(8) 0.0010(9) 0.0012(9)
C23 0.0399(12) 0.0239(10) 0.0318(11) 0.0052(9) 0.0076(9) -0.0060(9)
O24 0.0243(7) 0.0248(7) 0.0313(8) 0.0051(6) 0.0053(6) -0.0020(6)
C25 0.0237(10) 0.0452(13) 0.0315(11) 0.0135(10) 0.0076(9) -0.0048(9)
C26 0.0277(11) 0.0462(13) 0.0285(11) 0.0103(10) 0.0143(9) 0.0095(9)
O27 0.0249(7) 0.0270(7) 0.0235(7) 0.0048(6) 0.0099(6) 0.0035(5)
C28 0.0276(10) 0.0266(10) 0.0307(11) -0.0015(8) 0.0105(8) 0.0043(8)
C29 0.0231(9) 0.0240(10) 0.0316(11) 0.0053(8) 0.0054(8) 0.0040(8)
P 0.0232(2) 0.0245(3) 0.0197(2) -0.00250(19) 0.00306(19) 0.00455(19)
F1 0.0742(11) 0.0401(8) 0.0616(10) -0.0209(8) 0.0324(9) 0.0040(8)
F2 0.0346(8) 0.0676(11) 0.0381(8) 0.0074(7) -0.0085(6) -0.0041(7)
F3 0.0613(9) 0.0275(7) 0.0370(7) -0.0042(6) 0.0173(7) 0.0093(6)
F4 0.0309(7) 0.0554(10) 0.0632(10) 0.0138(8) -0.0138(7) 0.0034(7)
F5 0.0482(8) 0.0483(9) 0.0350(7) 0.0068(6) 0.0178(6) -0.0022(7)
F6 0.0485(8) 0.0313(7) 0.0316(7) 0.0061(6) 0.0099(6) 0.0007(6)

_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 O15 2.6224(14) . ?
K O24 2.7557(15) . ?
K O27 2.7876(14) . ?
K O21 2.7948(15) . ?
K F2 2.8112(17) . ?
K O18 2.8163(14) . ?
K N3 2.9394(18) . ?
K F1 3.033(2) . ?
K N12 3.1488(16) . ?
N1 C2 1.343(3) . ?
N1 C6 1.355(3) . ?
C2 N3 1.335(3) . ?
N3 C4 1.348(2) . ?
C4 N9 1.375(2) . ?
C4 C5 1.391(3) . ?
C5 N7 1.388(2) . ?
C5 C6 1.411(3) . ?
C6 N6 1.335(3) . ?
N7 C8 1.315(3) . ?
C8 N9 1.371(2) . ?
N9 C10 1.473(2) . ?
C10 C11 1.525(3) . ?
C11 N12 1.479(2) . ?
N12 C29 1.473(2) . ?
N12 C13 1.476(2) . ?
C13 C14 1.517(3) . ?
C14 O15 1.421(2) . ?
O15 C16 1.429(2) . ?
C16 C17 1.500(3) . ?
C17 O18 1.424(3) . ?
O18 C19 1.423(3) . ?
C19 C20 1.496(3) . ?
C20 O21 1.429(3) . ?
O21 C22 1.428(3) . ?
C22 C23 1.498(3) . ?
C23 O24 1.425(3) . ?
O24 C25 1.427(3) . ?
C25 C26 1.501(3) . ?
C26 O27 1.431(2) . ?
O27 C28 1.427(2) . ?
C28 C29 1.510(3) . ?
P F1 1.5887(15) . ?
P F4 1.5905(15) . ?
P F3 1.5955(14) . ?
P F6 1.5981(14) . ?
P F2 1.6085(15) . ?
P F5 1.6105(14) . ?

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
O15 K O24 166.84(5) . . ?
O15 K O27 115.88(4) . . ?
O24 K O27 61.98(4) . . ?
O15 K O21 121.71(5) . . ?
O24 K O21 62.17(4) . . ?
O27 K O21 122.41(4) . . ?
O15 K F2 91.22(5) . . ?
O24 K F2 75.72(5) . . ?
O27 K F2 72.17(4) . . ?
O21 K F2 106.32(5) . . ?
O15 K O18 61.07(4) . . ?
O24 K O18 120.45(4) . . ?
O27 K O18 176.33(5) . . ?
O21 K O18 60.71(4) . . ?
F2 K O18 105.41(5) . . ?
O15 K N3 85.44(5) . . ?
O24 K N3 107.70(5) . . ?
O27 K N3 100.86(5) . . ?
O21 K N3 83.37(5) . . ?
F2 K N3 170.03(5) . . ?
O18 K N3 81.18(5) . . ?
O15 K F1 81.62(5) . . ?
O24 K F1 87.92(5) . . ?
O27 K F1 116.11(4) . . ?
O21 K F1 74.42(4) . . ?
F2 K F1 45.19(4) . . ?
O18 K F1 62.10(4) . . ?
N3 K F1 142.87(5) . . ?
O15 K N12 58.37(4) . . ?
O24 K N12 121.09(4) . . ?
O27 K N12 59.11(4) . . ?
O21 K N12 167.17(4) . . ?
F2 K N12 86.38(4) . . ?
O18 K N12 118.38(4) . . ?
N3 K N12 83.87(5) . . ?
F1 K N12 117.19(4) . . ?
C2 N1 C6 117.90(18) . . ?
N3 C2 N1 129.98(19) . . ?
C2 N3 C4 110.58(17) . . ?
C2 N3 K 105.84(13) . . ?
C4 N3 K 112.51(12) . . ?
N3 C4 N9 127.84(17) . . ?
N3 C4 C5 126.37(18) . . ?
N9 C4 C5 105.79(16) . . ?
N7 C5 C4 110.71(17) . . ?
N7 C5 C6 132.13(17) . . ?
C4 C5 C6 117.16(17) . . ?
N6 C6 N1 118.34(18) . . ?
N6 C6 C5 123.65(18) . . ?
N1 C6 C5 117.99(17) . . ?
C8 N7 C5 103.56(16) . . ?
N7 C8 N9 114.28(18) . . ?
C8 N9 C4 105.66(16) . . ?
C8 N9 C10 127.23(16) . . ?
C4 N9 C10 126.68(16) . . ?
N9 C10 C11 113.07(16) . . ?
N12 C11 C10 113.10(16) . . ?
C29 N12 C13 110.47(16) . . ?
C29 N12 C11 110.72(15) . . ?
C13 N12 C11 112.65(15) . . ?
C29 N12 K 108.24(11) . . ?
C13 N12 K 86.18(10) . . ?
C11 N12 K 125.94(11) . . ?
N12 C13 C14 114.64(16) . . ?
O15 C14 C13 109.62(15) . . ?
C14 O15 C16 113.06(16) . . ?
C14 O15 K 119.85(11) . . ?
C16 O15 K 121.88(12) . . ?
O15 C16 C17 108.67(17) . . ?
O18 C17 C16 108.37(18) . . ?
C19 O18 C17 113.12(17) . . ?
C19 O18 K 112.68(12) . . ?
C17 O18 K 107.58(11) . . ?
O18 C19 C20 108.19(17) . . ?
O21 C20 C19 109.06(17) . . ?
C22 O21 C20 112.05(16) . . ?
C22 O21 K 109.98(11) . . ?
C20 O21 K 114.65(12) . . ?
O21 C22 C23 108.96(17) . . ?
O24 C23 C22 108.20(17) . . ?
C23 O24 C25 113.18(16) . . ?
C23 O24 K 113.66(12) . . ?
C25 O24 K 112.28(11) . . ?
O24 C25 C26 107.98(17) . . ?
O27 C26 C25 108.33(18) . . ?
C28 O27 C26 111.52(16) . . ?
C28 O27 K 114.04(11) . . ?
C26 O27 K 112.24(11) . . ?
O27 C28 C29 109.41(17) . . ?
N12 C29 C28 115.26(16) . . ?
F1 P F4 91.21(10) . . ?
F1 P F3 178.29(10) . . ?
F4 P F3 90.33(9) . . ?
F1 P F6 90.66(8) . . ?
F4 P F6 91.19(8) . . ?
F3 P F6 90.05(8) . . ?
F1 P F2 89.69(10) . . ?
F4 P F2 178.67(9) . . ?
F3 P F2 88.75(9) . . ?
F6 P F2 89.78(8) . . ?
F1 P F5 89.99(9) . . ?
F4 P F5 89.31(9) . . ?
F3 P F5 89.29(8) . . ?
F6 P F5 179.17(8) . . ?
F2 P F5 89.71(8) . . ?
P F1 K 107.30(9) . . ?
P F2 K 116.95(8) . . ?

_diffrn_measured_fraction_theta_max    0.918
_diffrn_reflns_theta_full              26.00
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.680
_refine_diff_density_min   -0.375
_refine_diff_density_rms    0.057

#===END