Supplementary Material (ESI) for Chemical Communications
This journal is © The Royal Society of Chemistry 2001

data_maaib6af 

_database_code_CSD      173157

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

_publ_contact_letter
;
Please accept this CIF submission as supplementary information to accompany
the manuscript RE499, submitted as an article to Chemical Communications.
A FAX communication was received here in Washington, DC on 19 Oct. 2001,
requesting a cif-file, and referring to it by the number B109465N. Neither 
the manuscript number nor the title was mentioned in the FAX, but this must 
the article desired.          Thank you, Isabella Karle and Richard Gilardi
;

_publ_section_title
;
Illustration of the Stacking of a Benzene Hexa Carboxylic Acid Core: 
The Crystal Structure of Benzene Hexa Carboxylic Acid-alpha-Amino Methyl
Isobutyrate Amide (MA-Aib~6~) - Sodium Nitrate Complex,
[C~6~(CONHC(CH~3~)~2~COOMe)~6~ - NaNO~3~ - (H~2~O)~2~]
;

loop_
_publ_author_name
_publ_author_address
'Subramania Ranganathan'
;     Discovery Laboratory,
Indian Institute of Chemical Technology
Hyderabad 500 007, India
;
'K. M. Muraleedharan'
;     Discovery Laboratory,
Indian Institute of Chemical Technology
Hyderabad 500 007, India
;
'CH. Chandrashekhar Rao'
;     Discovery Laboratory,
Indian Institute of Chemical Technology
Hyderabad 500 007, India
;
'M. Vairamani'
;     Mass Spectrometry Laboratory
Indian Institute of Chemical Technology
Hyderabad 500 007, India
;
'Isabella L. Karle'
;     Laboratory for the Structure of Matter
The Naval Research Laboratory, Code 6030
Washington, D. C. ; USA 20375-5341
;
'Richard Gilardi'
;     Laboratory for the Structure of Matter
The Naval Research Laboratory, Code 6030
Washington, D. C. ; USA 20375-5341
;

_publ_contact_author      'Isabella L. Karle'   
_publ_contact_author_address
;
Isabella L. Karle
Laboratory for the Structure of Matter
The Naval Research Laboratory, Code 6030
Washington, D. C. ; USA 20375-5341
;
_publ_contact_author_phone        '202 767 2624'
_publ_contact_author_fax          '202 767 6874'
_publ_contact_author_email        gilardi@nrl.navy.mil
_publ_requested_journal           'Chemical Communications'
_publ_requested_coeditor_name     'Sarah Jones?'


_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             
;
Benzene hexa carboxylic acid-alpha-amino
amide (MA-AIB6/sodium nitrate complex)
;
_chemical_formula_moiety          C42 H60 N6 O18.NaNO3.2 H2O
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C42 H60 N7 Na O23' 
_chemical_formula_weight          1053.96 
_chemical_melting_point           ? 
_chemical_compound_source         synthesized

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0181   0.0091 
'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'   0.0311   0.0180 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0492   0.0322 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Na'  'Na'   0.1353   0.1239 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            orthorhombic
_symmetry_space_group_name_H-M    Pna2(1)

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

_cell_length_a                    14.2862(5) 
_cell_length_b                    14.6144(5) 
_cell_length_c                    24.8005(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      5178.0(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        needle
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.60
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.025 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.352 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2224 
_exptl_absorpt_coefficient_mu     1.016 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        Bruker SMART CCD (with Cu source) 
_diffrn_measurement_method        omega scans
_diffrn_standards_number          NA 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             24566 
_diffrn_reflns_av_R_equivalents   0.0541 
_diffrn_reflns_av_sigmaI/netI     0.0475 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          3.51 
_diffrn_reflns_theta_max          57.22 
_reflns_number_total              6575 
_reflns_number_observed           4480 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        SMART
_computing_cell_refinement        ? 
_computing_data_reduction         SAINT 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses 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 observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     riding on C or N to which attached 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00105(10) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.17(14) 
_refine_ls_number_reflns          6575 
_refine_ls_number_parameters      659 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0774 
_refine_ls_R_factor_obs           0.0548 
_refine_ls_wR_factor_all          0.1452 
_refine_ls_wR_factor_obs          0.1342 
_refine_ls_goodness_of_fit_all    0.974 
_refine_ls_goodness_of_fit_obs    1.115 
_refine_ls_restrained_S_all       0.987 
_refine_ls_restrained_S_obs       1.133 
_refine_ls_shift/esd_max          3.997 
_refine_ls_shift/esd_mean         0.180 

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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
C1 C 0.1568(3) 0.6812(3) 0.3318(2) 0.0570(12) Uani 1 d . . 
C0 C 0.1270(5) 0.5870(3) 0.3135(2) 0.0610(13) Uani 1 d . . 
O0 O 0.0469(3) 0.5611(2) 0.32254(14) 0.0764(10) Uani 1 d . . 
N1 N 0.1910(3) 0.5351(3) 0.2890(2) 0.0668(11) Uani 1 d . . 
H1A H 0.2477(3) 0.5606(3) 0.2838(2) 0.080 Uiso 1 d R . 
C1A C 0.1739(5) 0.4428(4) 0.2696(2) 0.083(2) Uani 1 d . . 
C1B C 0.2560(5) 0.4127(4) 0.2364(3) 0.102(2) Uani 1 d . . 
H1BA H 0.2627(5) 0.4541(4) 0.2066(3) 0.080 Uiso 1 d R . 
H1BB H 0.3113(5) 0.4152(4) 0.2584(3) 0.080 Uiso 1 d R . 
H1BC H 0.2477(5) 0.3516(4) 0.2231(3) 0.080 Uiso 1 d R . 
C1C C 0.1624(6) 0.3760(4) 0.3165(3) 0.111(2) Uani 1 d . . 
H1CA H 0.2182(6) 0.3772(4) 0.3381(3) 0.080 Uiso 1 d R . 
H1CB H 0.1099(6) 0.3945(4) 0.3381(3) 0.080 Uiso 1 d R . 
H1CC H 0.1523(6) 0.3151(4) 0.3033(3) 0.080 Uiso 1 d R . 
C1' C 0.0842(6) 0.4389(5) 0.2346(3) 0.096(2) Uani 1 d . . 
O1 O 0.0343(4) 0.3738(4) 0.2312(2) 0.144(2) Uani 1 d . . 
O2 O 0.0758(3) 0.5133(3) 0.2045(2) 0.0936(12) Uani 1 d . . 
C2 C -0.0026(6) 0.5201(6) 0.1711(3) 0.124(2) Uani 1 d . . 
H2A H -0.0006(6) 0.5765(6) 0.1512(3) 0.080 Uiso 1 d R . 
H2B H -0.0010(6) 0.4695(6) 0.1464(3) 0.080 Uiso 1 d R . 
H2C H -0.0592(6) 0.5176(6) 0.1919(3) 0.080 Uiso 1 d R . 
C11 C 0.1667(4) 0.7006(3) 0.3872(2) 0.0602(13) Uani 1 d . . 
C10 C 0.1526(5) 0.6259(4) 0.4296(2) 0.0720(15) Uani 1 d . . 
O10 O 0.0866(3) 0.6344(2) 0.46092(15) 0.0861(11) Uani 1 d . . 
N11 N 0.2145(4) 0.5591(3) 0.4319(2) 0.0805(13) Uani 1 d . . 
H11A H 0.2597(4) 0.5580(3) 0.4066(2) 0.080 Uiso 1 d R . 
C11A C 0.2161(6) 0.4872(4) 0.4742(2) 0.093(2) Uani 1 d . . 
C11B C 0.2777(7) 0.4117(5) 0.4553(3) 0.137(3) Uani 1 d . . 
H11B H 0.2519(7) 0.3840(5) 0.4235(3) 0.080 Uiso 1 d R . 
H11C H 0.3392(7) 0.4347(5) 0.4475(3) 0.080 Uiso 1 d R . 
H11D H 0.2816(7) 0.3669(5) 0.4835(3) 0.080 Uiso 1 d R . 
C11C C 0.2561(7) 0.5306(5) 0.5258(3) 0.133(3) Uani 1 d . . 
H11E H 0.2577(7) 0.4858(5) 0.5541(3) 0.080 Uiso 1 d R . 
H11F H 0.3187(7) 0.5506(5) 0.5180(3) 0.080 Uiso 1 d R . 
H11G H 0.2192(7) 0.5820(5) 0.5372(3) 0.080 Uiso 1 d R . 
C11' C 0.1228(7) 0.4535(5) 0.4829(4) 0.107(2) Uani 1 d . . 
O11 O 0.0899(5) 0.4344(6) 0.5267(3) 0.183(3) Uani 1 d . . 
O12 O 0.0747(5) 0.4410(3) 0.4383(2) 0.120(2) Uani 1 d . . 
C12 C -0.0172(8) 0.4104(6) 0.4405(4) 0.145(3) Uani 1 d . . 
H12A H -0.0417(8) 0.4060(6) 0.4045(4) 0.080 Uiso 1 d R . 
H12B H -0.0190(8) 0.3513(6) 0.4573(4) 0.080 Uiso 1 d R . 
H12C H -0.0544(8) 0.4526(6) 0.4610(4) 0.080 Uiso 1 d R . 
C21 C 0.1842(3) 0.7884(3) 0.4050(2) 0.0580(12) Uani 1 d . . 
C20 C 0.1953(5) 0.8131(3) 0.4648(2) 0.0664(14) Uani 1 d . . 
O20 O 0.1353(3) 0.8574(3) 0.48708(14) 0.0866(12) Uani 1 d . . 
N21 N 0.2756(3) 0.7846(3) 0.4870(2) 0.0727(12) Uani 1 d . . 
H21A H 0.3130(3) 0.7468(3) 0.4682(2) 0.080 Uiso 1 d R . 
C21A C 0.3060(5) 0.8149(5) 0.5407(2) 0.086(2) Uani 1 d . . 
C21B C 0.3868(5) 0.7539(5) 0.5575(3) 0.114(2) Uani 1 d . . 
H21B H 0.3663(5) 0.6917(5) 0.5613(3) 0.080 Uiso 1 d R . 
H21C H 0.4347(5) 0.7572(5) 0.5305(3) 0.080 Uiso 1 d R . 
H21D H 0.4113(5) 0.7751(5) 0.5913(3) 0.080 Uiso 1 d R . 
C21C C 0.3391(8) 0.9137(5) 0.5376(4) 0.155(4) Uani 1 d . . 
H21E H 0.2895(8) 0.9543(5) 0.5271(4) 0.080 Uiso 1 d R . 
H21F H 0.3642(8) 0.9328(5) 0.5717(4) 0.080 Uiso 1 d R . 
H21G H 0.3876(8) 0.9150(5) 0.5108(4) 0.080 Uiso 1 d R . 
C21' C 0.2360(6) 0.8061(8) 0.5800(3) 0.115(3) Uani 1 d . . 
O21 O 0.2174(5) 0.8604(6) 0.6164(2) 0.199(4) Uani 1 d . . 
O22 O 0.1872(4) 0.7286(5) 0.5769(2) 0.126(2) Uani 1 d . . 
C22 C 0.1201(7) 0.7188(8) 0.6180(4) 0.187(5) Uani 1 d . . 
H22A H 0.0957(7) 0.6599(8) 0.6082(4) 0.080 Uiso 1 d R . 
H22B H 0.1465(7) 0.7157(8) 0.6536(4) 0.080 Uiso 1 d R . 
H22C H 0.0705(7) 0.7631(8) 0.6175(4) 0.080 Uiso 1 d R . 
C31 C 0.1935(3) 0.8597(3) 0.3676(2) 0.0574(12) Uani 1 d . . 
C30 C 0.2168(5) 0.9543(4) 0.3871(2) 0.0618(13) Uani 1 d . . 
O30 O 0.2984(3) 0.9708(3) 0.40129(15) 0.0800(10) Uani 1 d . . 
N31 N 0.1484(4) 1.0152(3) 0.3884(2) 0.0730(12) Uani 1 d . . 
H31A H 0.0925(4) 0.9983(3) 0.3749(2) 0.080 Uiso 1 d R . 
C31A C 0.1587(5) 1.1084(4) 0.4106(2) 0.088(2) Uani 1 d . . 
C31B C 0.0765(5) 1.1649(4) 0.3922(3) 0.105(2) Uani 1 d . . 
H31B H 0.0762(5) 1.1655(4) 0.3535(3) 0.080 Uiso 1 d R . 
H31C H 0.0199(5) 1.1370(4) 0.4051(3) 0.080 Uiso 1 d R . 
H31D H 0.0804(5) 1.2265(4) 0.4054(3) 0.080 Uiso 1 d R . 
C31C C 0.1667(6) 1.1041(5) 0.4718(3) 0.124(3) Uani 1 d . . 
H31E H 0.2211(6) 1.0689(5) 0.4810(3) 0.080 Uiso 1 d R . 
H31F H 0.1724(6) 1.1646(5) 0.4866(3) 0.080 Uiso 1 d R . 
H31G H 0.1119(6) 1.0751(5) 0.4863(3) 0.080 Uiso 1 d R . 
C31' C 0.2476(5) 1.1534(4) 0.3896(3) 0.084(2) Uani 1 d . . 
O31 O 0.2975(4) 1.2009(3) 0.4154(2) 0.119(2) Uani 1 d . . 
O32 O 0.2579(3) 1.1391(3) 0.3363(2) 0.0931(12) Uani 1 d . . 
C32 C 0.3400(6) 1.1745(5) 0.3121(3) 0.118(2) Uani 1 d . . 
H32A H 0.3395(6) 1.1574(5) 0.2747(3) 0.080 Uiso 1 d R . 
H32B H 0.3406(6) 1.2400(5) 0.3150(3) 0.080 Uiso 1 d R . 
H32C H 0.3948(6) 1.1498(5) 0.3291(3) 0.080 Uiso 1 d R . 
C41 C 0.1854(3) 0.8414(3) 0.3129(2) 0.0558(12) Uani 1 d . . 
C40 C 0.2060(5) 0.9203(3) 0.2747(2) 0.0578(13) Uani 1 d . . 
O40 O 0.2833(3) 0.9545(3) 0.27477(13) 0.0733(10) Uani 1 d . . 
N41 N 0.1325(3) 0.9473(3) 0.2454(2) 0.0699(11) Uani 1 d . . 
H41A H 0.0797(3) 0.9147(3) 0.2503(2) 0.080 Uiso 1 d R . 
C41A C 0.1254(4) 1.0231(4) 0.2064(2) 0.0740(15) Uani 1 d . . 
C41B C 0.2144(4) 1.0391(4) 0.1771(2) 0.089(2) Uani 1 d . . 
H41B H 0.2345(4) 0.9853(4) 0.1582(2) 0.080 Uiso 1 d R . 
H41C H 0.2038(4) 1.0877(4) 0.1518(2) 0.080 Uiso 1 d R . 
H41D H 0.2619(4) 1.0573(4) 0.2023(2) 0.080 Uiso 1 d R . 
C41C C 0.0948(5) 1.1101(4) 0.2361(3) 0.102(2) Uani 1 d . . 
H41E H 0.1434(5) 1.1303(4) 0.2600(3) 0.080 Uiso 1 d R . 
H41F H 0.0807(5) 1.1578(4) 0.2107(3) 0.080 Uiso 1 d R . 
H41G H 0.0397(5) 1.0959(4) 0.2566(3) 0.080 Uiso 1 d R . 
C41' C 0.0433(5) 0.9973(4) 0.1696(3) 0.079(2) Uani 1 d . . 
O41 O -0.0172(3) 0.9453(3) 0.1830(2) 0.1032(13) Uani 1 d . . 
O42 O 0.0448(3) 1.0415(3) 0.1236(2) 0.0902(12) Uani 1 d . . 
C42 C -0.0272(5) 1.0230(5) 0.0871(3) 0.114(2) Uani 1 d . . 
H42A H -0.0204(5) 1.0593(5) 0.0550(3) 0.080 Uiso 1 d R . 
H42B H -0.0234(5) 0.9593(5) 0.0779(3) 0.080 Uiso 1 d R . 
H42C H -0.0869(5) 1.0354(5) 0.1033(3) 0.080 Uiso 1 d R . 
C51 C 0.1690(3) 0.7525(3) 0.2947(2) 0.0545(12) Uani 1 d . . 
C50 C 0.1589(4) 0.7336(3) 0.2343(2) 0.0573(12) Uani 1 d . . 
O50 O 0.0832(3) 0.7144(2) 0.21484(13) 0.0696(9) Uani 1 d . . 
N51 N 0.2384(3) 0.7433(3) 0.2070(2) 0.0686(11) Uani 1 d . . 
H51A H 0.2901(3) 0.7610(3) 0.2249(2) 0.080 Uiso 1 d R . 
C51A C 0.2488(4) 0.7241(4) 0.1484(2) 0.0724(15) Uani 1 d . . 
C51B C 0.3386(5) 0.7722(5) 0.1307(2) 0.100(2) Uani 1 d . . 
H51B H 0.3350(5) 0.8371(5) 0.1363(2) 0.080 Uiso 1 d R . 
H51C H 0.3880(5) 0.7472(5) 0.1524(2) 0.080 Uiso 1 d R . 
H51D H 0.3511(5) 0.7600(5) 0.0933(2) 0.080 Uiso 1 d R . 
C51C C 0.2525(5) 0.6233(4) 0.1394(2) 0.093(2) Uani 1 d . . 
H51E H 0.1943(5) 0.5952(4) 0.1493(2) 0.080 Uiso 1 d R . 
H51F H 0.2652(5) 0.6112(4) 0.1020(2) 0.080 Uiso 1 d R . 
H51G H 0.3020(5) 0.5985(4) 0.1611(2) 0.080 Uiso 1 d R . 
C51' C 0.1705(4) 0.7722(5) 0.1191(2) 0.074(2) Uani 1 d . . 
O51 O 0.1475(4) 0.8494(4) 0.1256(2) 0.1090(15) Uani 1 d . . 
O52 O 0.1314(3) 0.7178(3) 0.0827(2) 0.1044(13) Uani 1 d . . 
C52 C 0.0600(6) 0.7611(6) 0.0507(4) 0.138(3) Uani 1 d . . 
H52A H 0.0369(6) 0.7176(6) 0.0249(4) 0.080 Uiso 1 d R . 
H52B H 0.0101(6) 0.7789(6) 0.0744(4) 0.080 Uiso 1 d R . 
H52C H 0.0833(6) 0.8140(6) 0.0321(4) 0.080 Uiso 1 d R . 
W3 O 0.4349(3) 0.7735(3) 0.4082(2) 0.0976(12) Uani 1 d . . 
W4 O 0.4144(3) 0.7666(3) 0.2717(2) 0.0852(11) Uani 1 d . . 
Na1 Na -0.09977(14) 0.61311(14) 0.33752(9) 0.0862(6) Uani 1 d . . 
N1S N -0.0789(3) 0.9282(2) 0.34382(14) 0.0433(8) Uani 1 d D . 
O1S O -0.0044(4) 0.9002(5) 0.3489(5) 0.240(4) Uani 1 d D . 
O2S O -0.1387(6) 0.8906(5) 0.3204(6) 0.286(6) Uani 1 d D . 
O3S O -0.0906(7) 1.0126(4) 0.3506(7) 0.363(8) Uani 1 d 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 
C1 0.076(3) 0.054(3) 0.041(3) -0.002(2) 0.002(2) 0.001(2) 
C0 0.090(4) 0.058(3) 0.035(3) -0.001(2) -0.007(3) 0.004(3) 
O0 0.092(3) 0.067(2) 0.071(3) -0.001(2) 0.002(2) -0.007(2) 
N1 0.085(3) 0.065(3) 0.050(2) -0.009(2) 0.004(2) 0.007(2) 
C1A 0.134(5) 0.057(3) 0.058(4) -0.005(3) 0.013(4) 0.017(3) 
C1B 0.151(6) 0.085(4) 0.069(4) -0.010(3) 0.005(4) 0.034(4) 
C1C 0.187(7) 0.060(3) 0.086(5) -0.005(3) 0.014(5) 0.020(4) 
C1' 0.124(6) 0.073(4) 0.091(5) -0.028(4) 0.007(4) -0.009(4) 
O1 0.179(5) 0.101(4) 0.151(5) -0.008(3) -0.023(4) -0.039(4) 
O2 0.113(3) 0.089(3) 0.079(3) -0.005(2) -0.024(2) -0.003(2) 
C2 0.120(6) 0.141(6) 0.111(6) -0.014(5) -0.022(5) 0.009(5) 
C11 0.084(4) 0.050(3) 0.046(3) 0.002(2) 0.003(2) 0.010(2) 
C10 0.105(5) 0.069(4) 0.042(3) 0.003(3) 0.001(3) 0.004(3) 
O10 0.116(3) 0.086(3) 0.056(2) 0.014(2) 0.019(2) 0.004(2) 
N11 0.124(4) 0.058(3) 0.060(3) 0.006(2) -0.010(3) 0.014(3) 
C11A 0.151(6) 0.061(4) 0.066(4) 0.010(3) -0.019(4) 0.011(4) 
C11B 0.206(9) 0.101(6) 0.105(6) 0.031(4) -0.045(6) 0.035(6) 
C11C 0.224(9) 0.101(5) 0.074(5) 0.012(4) -0.049(5) 0.004(5) 
C11' 0.139(7) 0.093(5) 0.090(6) 0.043(4) -0.017(5) -0.005(4) 
O11 0.214(7) 0.217(7) 0.119(5) 0.089(5) -0.004(5) -0.033(5) 
O12 0.147(5) 0.094(3) 0.119(4) 0.005(3) -0.024(4) -0.017(3) 
C12 0.190(11) 0.121(6) 0.124(7) 0.014(6) -0.031(7) 0.019(7) 
C21 0.080(3) 0.056(3) 0.038(3) -0.003(2) 0.003(2) 0.008(2) 
C20 0.108(5) 0.058(3) 0.033(3) -0.001(2) -0.001(3) 0.006(3) 
O20 0.121(3) 0.093(3) 0.046(2) -0.008(2) 0.011(2) 0.031(2) 
N21 0.091(3) 0.091(3) 0.036(2) -0.008(2) -0.009(2) 0.016(2) 
C21A 0.108(5) 0.099(5) 0.050(4) -0.005(3) -0.021(4) 0.000(4) 
C21B 0.128(6) 0.142(6) 0.070(4) 0.010(4) -0.035(4) 0.000(5) 
C21C 0.236(11) 0.106(6) 0.124(7) -0.017(5) -0.089(7) -0.015(6) 
C21' 0.110(6) 0.179(9) 0.056(5) 0.011(5) -0.008(4) 0.024(6) 
O21 0.224(7) 0.300(10) 0.071(4) -0.079(5) 0.003(4) 0.063(6) 
O22 0.118(4) 0.179(6) 0.082(3) 0.054(4) 0.027(3) 0.007(4) 
C22 0.109(7) 0.264(13) 0.189(11) 0.115(10) -0.020(7) 0.009(7) 
C31 0.079(4) 0.050(3) 0.043(3) -0.003(2) 0.004(2) 0.003(2) 
C30 0.092(4) 0.055(3) 0.039(3) 0.003(2) 0.005(3) -0.001(3) 
O30 0.104(3) 0.075(2) 0.060(2) -0.009(2) -0.005(2) -0.005(2) 
N31 0.105(4) 0.052(3) 0.062(3) -0.004(2) 0.010(2) 0.010(2) 
C31A 0.140(6) 0.063(4) 0.061(4) -0.013(3) 0.027(4) 0.017(4) 
C31B 0.127(6) 0.076(4) 0.111(5) -0.002(4) 0.037(4) 0.019(4) 
C31C 0.211(8) 0.099(5) 0.063(4) -0.007(3) 0.035(5) 0.012(5) 
C31' 0.119(6) 0.059(4) 0.075(5) -0.006(3) -0.004(4) 0.011(4) 
O31 0.163(5) 0.086(3) 0.108(4) -0.032(3) -0.008(3) -0.004(3) 
O32 0.120(3) 0.086(3) 0.073(3) 0.008(2) 0.011(2) -0.014(2) 
C32 0.148(7) 0.107(5) 0.100(5) 0.012(4) 0.002(5) -0.001(5) 
C41 0.075(3) 0.053(3) 0.039(3) 0.003(2) -0.001(2) 0.005(2) 
C40 0.085(4) 0.050(3) 0.038(3) 0.000(2) 0.003(3) 0.002(3) 
O40 0.081(3) 0.082(2) 0.056(2) 0.013(2) -0.003(2) -0.013(2) 
N41 0.078(3) 0.077(3) 0.054(3) 0.017(2) 0.002(2) -0.005(2) 
C41A 0.097(4) 0.070(4) 0.055(3) 0.022(3) -0.002(3) 0.001(3) 
C41B 0.116(5) 0.083(4) 0.068(4) 0.025(3) -0.017(4) -0.022(3) 
C41C 0.126(5) 0.095(5) 0.084(5) 0.012(4) -0.023(4) 0.012(4) 
C41' 0.081(4) 0.072(4) 0.084(5) 0.011(3) 0.001(3) -0.002(3) 
O41 0.095(3) 0.118(3) 0.097(3) 0.036(3) -0.026(3) -0.014(3) 
O42 0.106(3) 0.101(3) 0.064(2) 0.033(2) -0.030(2) -0.008(2) 
C42 0.130(6) 0.129(6) 0.083(5) 0.024(4) -0.025(5) 0.003(4) 
C51 0.076(4) 0.053(3) 0.034(3) 0.000(2) 0.004(2) 0.004(2) 
C50 0.077(4) 0.055(3) 0.040(3) 0.004(2) 0.004(3) 0.001(2) 
O50 0.073(3) 0.092(3) 0.043(2) -0.004(2) -0.004(2) -0.004(2) 
N51 0.076(3) 0.092(3) 0.038(2) -0.008(2) 0.002(2) 0.001(2) 
C51A 0.088(4) 0.087(4) 0.042(3) -0.005(3) 0.013(3) 0.001(3) 
C51B 0.106(5) 0.131(5) 0.063(4) 0.008(4) 0.023(3) -0.006(4) 
C51C 0.109(5) 0.105(5) 0.065(4) -0.019(3) 0.009(3) 0.017(4) 
C51' 0.089(4) 0.095(5) 0.039(3) 0.001(3) 0.008(3) -0.008(4) 
O51 0.147(4) 0.094(3) 0.086(3) 0.002(3) -0.029(3) 0.010(3) 
O52 0.125(4) 0.118(3) 0.070(3) -0.020(2) -0.025(3) 0.000(3) 
C52 0.124(7) 0.188(9) 0.102(6) -0.001(6) -0.032(5) -0.031(6) 
W3 0.104(3) 0.112(3) 0.077(3) -0.002(2) 0.015(2) 0.005(2) 
W4 0.086(3) 0.096(3) 0.073(2) -0.010(2) -0.003(2) 0.002(2) 
Na1 0.092(2) 0.0959(15) 0.0713(14) 0.0025(12) 0.0034(12) -0.0017(11) 
N1S 0.052(2) 0.035(2) 0.042(2) -0.007(2) 0.001(2) 0.000(2) 
O1S 0.248(9) 0.169(7) 0.305(12) 0.013(8) -0.021(10) -0.006(7) 
O2S 0.252(10) 0.160(7) 0.447(19) -0.024(9) -0.022(12) 0.022(7) 
O3S 0.315(14) 0.390(19) 0.384(20) -0.094(16) -0.098(15) -0.064(13) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
C1 C51 1.401(6) . ? 
C1 C11 1.409(7) . ? 
C1 C0 1.512(7) . ? 
C0 O0 1.226(6) . ? 
C0 N1 1.334(7) . ? 
O0 Na1 2.260(5) . ? 
N1 C1A 1.453(7) . ? 
C1A C1B 1.501(8) . ? 
C1A C1C 1.528(8) . ? 
C1A C1' 1.550(10) . ? 
C1' O1 1.192(7) . ? 
C1' O2 1.325(8) . ? 
O2 C2 1.397(8) . ? 
C11 C21 1.380(7) . ? 
C11 C10 1.529(7) . ? 
C10 O10 1.228(6) . ? 
C10 N11 1.319(7) . ? 
N11 C11A 1.484(7) . ? 
C11A C11' 1.438(10) . ? 
C11A C11B 1.488(10) . ? 
C11A C11C 1.541(9) . ? 
C11' O11 1.216(10) . ? 
C11' O12 1.314(9) . ? 
O12 C12 1.388(10) . ? 
C21 C31 1.402(6) . ? 
C21 C20 1.534(7) . ? 
C20 O20 1.209(6) . ? 
C20 N21 1.338(7) . ? 
N21 C21A 1.469(7) . ? 
C21A C21' 1.402(10) . ? 
C21A C21C 1.520(10) . ? 
C21A C21B 1.517(9) . ? 
C21' O21 1.230(10) . ? 
C21' O22 1.332(10) . ? 
O22 C22 1.406(10) . ? 
C31 C41 1.387(6) . ? 
C31 C30 1.503(7) . ? 
C30 O30 1.242(6) . ? 
C30 N31 1.322(7) . ? 
O30 Na1 2.474(4) 3_565 ? 
N31 C31A 1.477(7) . ? 
C31A C31B 1.506(9) . ? 
C31A C31C 1.521(9) . ? 
C31A C31' 1.523(9) . ? 
C31' O31 1.182(7) . ? 
C31' O32 1.348(8) . ? 
O32 C32 1.416(8) . ? 
C41 C51 1.396(6) . ? 
C41 C40 1.520(7) . ? 
C40 O40 1.214(6) . ? 
C40 N41 1.337(6) . ? 
N41 C41A 1.472(6) . ? 
C41A C41B 1.484(8) . ? 
C41A C41C 1.534(8) . ? 
C41A C41' 1.534(8) . ? 
C41' O41 1.198(6) . ? 
C41' O42 1.310(7) . ? 
O42 C42 1.398(7) . ? 
C51 C50 1.529(7) . ? 
C50 O50 1.217(6) . ? 
C50 N51 1.330(6) . ? 
N51 C51A 1.489(6) . ? 
C51A C51C 1.492(8) . ? 
C51A C51' 1.507(8) . ? 
C51A C51B 1.527(8) . ? 
C51' O51 1.187(7) . ? 
C51' O52 1.326(7) . ? 
O52 C52 1.439(9) . ? 
Na1 W4 2.407(4) 3_465 ? 
Na1 W3 2.462(5) 3_465 ? 
Na1 O30 2.474(4) 3_465 ? 
Na1 O40 2.487(4) 3_465 ? 
N1S O1S 1.147(4) . ? 
N1S O2S 1.169(4) . ? 
N1S O3S 1.258(4) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C51 C1 C11 118.6(4) . . ? 
C51 C1 C0 121.0(4) . . ? 
C11 C1 C0 120.3(4) . . ? 
O0 C0 N1 123.2(5) . . ? 
O0 C0 C1 119.3(5) . . ? 
N1 C0 C1 117.4(5) . . ? 
C0 O0 Na1 142.3(3) . . ? 
C0 N1 C1A 124.2(5) . . ? 
N1 C1A C1B 108.8(5) . . ? 
N1 C1A C1C 111.1(5) . . ? 
C1B C1A C1C 108.3(5) . . ? 
N1 C1A C1' 111.1(5) . . ? 
C1B C1A C1' 109.1(5) . . ? 
C1C C1A C1' 108.3(6) . . ? 
O1 C1' O2 124.2(7) . . ? 
O1 C1' C1A 124.3(7) . . ? 
O2 C1' C1A 111.1(6) . . ? 
C1' O2 C2 117.8(6) . . ? 
C21 C11 C1 121.1(4) . . ? 
C21 C11 C10 117.8(4) . . ? 
C1 C11 C10 120.9(4) . . ? 
O10 C10 N11 124.3(5) . . ? 
O10 C10 C11 117.6(5) . . ? 
N11 C10 C11 118.1(5) . . ? 
C10 N11 C11A 124.4(5) . . ? 
C11' C11A C11B 110.0(6) . . ? 
C11' C11A N11 109.5(6) . . ? 
C11B C11A N11 108.2(6) . . ? 
C11' C11A C11C 111.1(7) . . ? 
C11B C11A C11C 110.3(6) . . ? 
N11 C11A C11C 107.6(5) . . ? 
O11 C11' O12 121.2(9) . . ? 
O11 C11' C11A 124.8(8) . . ? 
O12 C11' C11A 114.0(7) . . ? 
C11' O12 C12 120.4(7) . . ? 
C11 C21 C31 119.8(4) . . ? 
C11 C21 C20 123.1(4) . . ? 
C31 C21 C20 117.1(4) . . ? 
O20 C20 N21 125.9(5) . . ? 
O20 C20 C21 119.6(5) . . ? 
N21 C20 C21 114.4(5) . . ? 
C20 N21 C21A 122.2(5) . . ? 
C21' C21A N21 113.0(6) . . ? 
C21' C21A C21C 110.1(8) . . ? 
N21 C21A C21C 109.4(5) . . ? 
C21' C21A C21B 107.3(6) . . ? 
N21 C21A C21B 107.3(5) . . ? 
C21C C21A C21B 109.6(6) . . ? 
O21 C21' O22 118.5(9) . . ? 
O21 C21' C21A 127.2(11) . . ? 
O22 C21' C21A 114.3(8) . . ? 
C21' O22 C22 113.7(8) . . ? 
C41 C31 C21 119.7(4) . . ? 
C41 C31 C30 120.8(4) . . ? 
C21 C31 C30 119.4(4) . . ? 
O30 C30 N31 123.9(5) . . ? 
O30 C30 C31 118.5(5) . . ? 
N31 C30 C31 117.6(5) . . ? 
C30 O30 Na1 106.0(3) . 3_565 ? 
C30 N31 C31A 123.8(5) . . ? 
N31 C31A C31B 108.3(6) . . ? 
N31 C31A C31C 109.9(5) . . ? 
C31B C31A C31C 112.6(5) . . ? 
N31 C31A C31' 110.7(5) . . ? 
C31B C31A C31' 108.0(5) . . ? 
C31C C31A C31' 107.2(6) . . ? 
O31 C31' O32 123.8(7) . . ? 
O31 C31' C31A 124.9(6) . . ? 
O32 C31' C31A 111.1(6) . . ? 
C31' O32 C32 116.7(6) . . ? 
C31 C41 C51 120.6(4) . . ? 
C31 C41 C40 116.5(4) . . ? 
C51 C41 C40 122.5(4) . . ? 
O40 C40 N41 126.4(4) . . ? 
O40 C40 C41 119.2(5) . . ? 
N41 C40 C41 114.3(5) . . ? 
C40 O40 Na1 116.6(3) . 3_565 ? 
C40 N41 C41A 129.3(4) . . ? 
N41 C41A C41B 112.4(5) . . ? 
N41 C41A C41C 109.2(4) . . ? 
C41B C41A C41C 110.4(5) . . ? 
N41 C41A C41' 105.0(4) . . ? 
C41B C41A C41' 113.7(5) . . ? 
C41C C41A C41' 105.8(5) . . ? 
O41 C41' O42 124.4(6) . . ? 
O41 C41' C41A 122.8(5) . . ? 
O42 C41' C41A 112.6(5) . . ? 
C41' O42 C42 117.2(5) . . ? 
C41 C51 C1 120.0(4) . . ? 
C41 C51 C50 120.0(4) . . ? 
C1 C51 C50 119.8(4) . . ? 
O50 C50 N51 125.5(4) . . ? 
O50 C50 C51 121.0(5) . . ? 
N51 C50 C51 113.4(5) . . ? 
C50 N51 C51A 124.2(4) . . ? 
C51C C51A N51 109.6(5) . . ? 
C51C C51A C51' 114.5(5) . . ? 
N51 C51A C51' 108.0(4) . . ? 
C51C C51A C51B 112.4(5) . . ? 
N51 C51A C51B 106.1(5) . . ? 
C51' C51A C51B 105.7(5) . . ? 
O51 C51' O52 123.1(6) . . ? 
O51 C51' C51A 125.7(6) . . ? 
O52 C51' C51A 111.1(6) . . ? 
C51' O52 C52 114.2(6) . . ? 
O0 Na1 W4 93.22(15) . 3_465 ? 
O0 Na1 W3 99.0(2) . 3_465 ? 
W4 Na1 W3 88.52(14) 3_465 3_465 ? 
O0 Na1 O30 118.9(2) . 3_465 ? 
W4 Na1 O30 147.7(2) 3_465 3_465 ? 
W3 Na1 O30 89.79(15) 3_465 3_465 ? 
O0 Na1 O40 112.7(2) . 3_465 ? 
W4 Na1 O40 85.57(14) 3_465 3_465 ? 
W3 Na1 O40 148.0(2) 3_465 3_465 ? 
O30 Na1 O40 78.96(14) 3_465 3_465 ? 
O1S N1S O2S 124.4(5) . . ? 
O1S N1S O3S 117.3(4) . . ? 
O2S N1S O3S 115.5(5) . . ? 

_refine_diff_density_max    0.315 
_refine_diff_density_min   -0.310 
_refine_diff_density_rms    0.046