# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.
_journal_coden_Cambridge         0182
_publ_contact_author_name        'Geoff G.Z. Zhang'
_publ_contact_author_address     
;
Solid State Sciences,
Global Pharmaceutical R&D, Abbott Laboratories,
North Chicago, IL
USA 60064
;
_publ_contact_author_email       Geoff.GZ.Zhang@abbott.com
_publ_contact_author_fax         1-847-937-2417
_publ_contact_author_phone       1-847-937-4702

loop_
_publ_author_name
_publ_author_address

D.-K.Bucar
;
Solid State Sciences,
Global Pharmaceutical R&D, Abbott Laboratories,
North Chicago, IL
USA 60064

and

Department of Chemistry
University of Iowa
423E Chemistry Building
Iowa City, IA
USA 52242-1294
;
'Rodger F. Henry'
;Structural Chemistry,
Global Pharmaceutical R&D, Abbott Laboratories,
Abbott Park, IL
USA 60064
;
'Xiaochun Lou.'
;
Solid State Sciences,
Global Pharmaceutical R&D, Abbott Laboratories,
North Chicago, IL
USA 60064
;
'Thomas B. Borchardt'
;
Solid State Chemistry,
Global Pharmaceutical R&D, Abbott Laboratories,
North Chicago, IL
USA 60064
;
'Geoff G.Z. Zhang'
;
Solid State Sciences,
Global Pharmaceutical R&D, Abbott Laboratories,
North Chicago, IL
USA 60064
;
_publ_section_title              
;
A hidden co-crystal of caffeine and adipic acid
;

data_x238t
_database_code_depnum_ccdc_archive 'CCDC 616820'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
(1,3,7-trimethyl-1H-purine-2,6(3H,7H)-dione).(1,4-butanedicarboxylic acid)
;
_chemical_name_common            
;(1,3,7-trimethyl-1H-purine-2,6(3H,7H)-dione).(1,4-
butanedicarboxylic acid)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H10 N4 O2, C6 H10 O4'
_chemical_formula_sum            'C14 H20 N4 O6'
_chemical_formula_weight         340.34

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5480(16)
_cell_length_b                   9.5862(16)
_cell_length_c                   9.6682(16)
_cell_angle_alpha                82.705(3)
_cell_angle_beta                 87.649(3)
_cell_angle_gamma                67.236(2)
_cell_volume                     809.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    919
_cell_measurement_theta_min      2.9515
_cell_measurement_theta_max      28.2525

_exptl_crystal_description       paralellepiped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             360
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_type   none

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       omega-phi
_diffrn_reflns_number            9608
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         28.29
_reflns_number_total             3877
_reflns_number_gt                3433
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker 2001)'
_computing_cell_refinement       'Bruker saintplus (Bruker 1999)'
_computing_data_reduction        'Bruker saintplus (Bruker 1999)'
_computing_structure_solution    'SHELXL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2000)'
_computing_molecular_graphics    '(MS Modeling(Accelrys 2004)'

_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^)+(0.0648P)^2^+0.0892P] 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         3877
_refine_ls_number_parameters     222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
O1 O 1.02021(10) -0.28049(10) 0.61987(10) 0.0391(2) Uani 1 1 d . . .
O2 O 0.86986(11) 0.20139(11) 0.74834(10) 0.0404(2) Uani 1 1 d . . .
N1 N 0.73279(11) 0.17088(10) 0.57537(10) 0.0291(2) Uani 1 1 d . . .
N2 N 0.93967(10) -0.03833(11) 0.68568(10) 0.0294(2) Uani 1 1 d . . .
N3 N 0.75058(11) -0.14182(10) 0.41070(10) 0.0289(2) Uani 1 1 d . . .
N4 N 0.60049(11) 0.10550(11) 0.39898(10) 0.0291(2) Uani 1 1 d . . .
C1 C 1.05729(14) -0.09223(16) 0.79521(14) 0.0387(3) Uani 1 1 d . . .
H1A H 1.1165 -0.0303 0.7846 0.058 Uiso 1 1 calc R . .
H1B H 1.1222 -0.1963 0.7876 0.058 Uiso 1 1 calc R . .
H1C H 1.0100 -0.0853 0.8850 0.058 Uiso 1 1 calc R . .
C2 C 0.84737(13) 0.11766(13) 0.67399(12) 0.0294(2) Uani 1 1 d . . .
C3 C 0.63687(16) 0.33353(13) 0.55326(15) 0.0389(3) Uani 1 1 d . . .
H3A H 0.6324 0.3693 0.4556 0.058 Uiso 1 1 calc R . .
H3B H 0.6789 0.3887 0.6034 0.058 Uiso 1 1 calc R . .
H3C H 0.5363 0.3492 0.5863 0.058 Uiso 1 1 calc R . .
C4 C 0.71102(12) 0.07105(12) 0.49667(11) 0.0256(2) Uani 1 1 d . . .
C5 C 0.62926(13) -0.02772(13) 0.34947(12) 0.0302(2) Uani 1 1 d . . .
H5A H 0.5713 -0.0395 0.2802 0.036 Uiso 1 1 calc R . .
C6 C 0.81621(16) -0.29861(14) 0.37518(15) 0.0401(3) Uani 1 1 d . . .
H6A H 0.7537 -0.3104 0.3059 0.060 Uiso 1 1 calc R . .
H6B H 0.8212 -0.3683 0.4572 0.060 Uiso 1 1 calc R . .
H6C H 0.9166 -0.3197 0.3392 0.060 Uiso 1 1 calc R . .
C7 C 0.80585(12) -0.08038(12) 0.50742(11) 0.0265(2) Uani 1 1 d . . .
C8 C 0.92998(12) -0.14694(12) 0.60425(12) 0.0280(2) Uani 1 1 d . . .
O3 O 0.35080(9) 0.34806(9) 0.30936(9) 0.0338(2) Uani 1 1 d . . .
H3 H 0.4265 0.2726 0.3350 0.051 Uiso 1 1 calc R . .
O4 O 0.32950(10) 0.19371(9) 0.16462(9) 0.0356(2) Uani 1 1 d . . .
C9 C 0.28175(12) 0.31790(12) 0.20800(12) 0.0265(2) Uani 1 1 d . . .
C10 C 0.13986(12) 0.45066(12) 0.15560(12) 0.0292(2) Uani 1 1 d . . .
H10A H 0.1624 0.5417 0.1404 0.035 Uiso 1 1 calc R . .
H10B H 0.0633 0.4657 0.2275 0.035 Uiso 1 1 calc R . .
C11 C 0.07401(13) 0.43262(12) 0.02150(13) 0.0312(2) Uani 1 1 d . . .
H11A H 0.0551 0.3394 0.0344 0.037 Uiso 1 1 calc R . .
H11B H 0.1475 0.4239 -0.0526 0.037 Uiso 1 1 calc R . .
O5 O 0.30384(10) -0.01859(9) 0.01261(10) 0.0373(2) Uani 1 1 d . . .
H5 H 0.3173 0.0461 0.0521 0.056 Uiso 1 1 calc R . .
O6 O 0.48637(11) -0.17898(10) 0.16086(10) 0.0417(2) Uani 1 1 d . . .
C12 C 0.40026(13) -0.15734(12) 0.06498(12) 0.0285(2) Uani 1 1 d . . .
C13 C 0.38653(12) -0.28133(11) -0.00804(12) 0.0271(2) Uani 1 1 d . . .
H13B H 0.3994 -0.2596 -0.1074 0.033 Uiso 1 1 calc R . .
H13A H 0.2852 -0.2809 0.0063 0.033 Uiso 1 1 calc R . .
C14 C 0.50253(13) -0.43939(11) 0.04304(11) 0.0275(2) Uani 1 1 d . . .
H14B H 0.4827 -0.4662 0.1399 0.033 Uiso 1 1 calc R . .
H14A H 0.6035 -0.4375 0.0379 0.033 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
O1 0.0362(5) 0.0306(4) 0.0434(5) -0.0023(4) -0.0048(4) -0.0052(3)
O2 0.0489(5) 0.0429(5) 0.0376(5) -0.0127(4) -0.0066(4) -0.0236(4)
N1 0.0333(5) 0.0244(4) 0.0303(5) -0.0064(3) -0.0044(4) -0.0104(4)
N2 0.0287(5) 0.0331(5) 0.0275(5) -0.0021(4) -0.0048(4) -0.0129(4)
N3 0.0330(5) 0.0265(5) 0.0293(5) -0.0080(4) -0.0003(4) -0.0123(4)
N4 0.0306(5) 0.0281(5) 0.0287(5) -0.0049(4) -0.0046(4) -0.0106(4)
C1 0.0341(6) 0.0487(7) 0.0338(6) -0.0003(5) -0.0110(5) -0.0166(5)
C2 0.0324(5) 0.0325(5) 0.0276(5) -0.0057(4) -0.0004(4) -0.0164(4)
C3 0.0484(7) 0.0235(5) 0.0420(7) -0.0078(5) -0.0076(5) -0.0088(5)
C4 0.0272(5) 0.0261(5) 0.0250(5) -0.0047(4) -0.0006(4) -0.0114(4)
C5 0.0321(5) 0.0319(5) 0.0289(5) -0.0065(4) -0.0029(4) -0.0136(4)
C6 0.0467(7) 0.0298(6) 0.0449(7) -0.0168(5) 0.0009(6) -0.0123(5)
C7 0.0287(5) 0.0257(5) 0.0267(5) -0.0064(4) 0.0009(4) -0.0115(4)
C8 0.0276(5) 0.0292(5) 0.0272(5) -0.0023(4) 0.0008(4) -0.0114(4)
O3 0.0352(4) 0.0273(4) 0.0359(5) -0.0091(3) -0.0087(3) -0.0062(3)
O4 0.0395(5) 0.0243(4) 0.0416(5) -0.0100(3) -0.0070(4) -0.0081(3)
C9 0.0291(5) 0.0247(5) 0.0278(5) -0.0046(4) 0.0004(4) -0.0122(4)
C10 0.0299(5) 0.0243(5) 0.0328(6) -0.0070(4) -0.0022(4) -0.0085(4)
C11 0.0290(5) 0.0286(5) 0.0364(6) -0.0083(4) -0.0039(4) -0.0095(5)
O5 0.0439(5) 0.0233(4) 0.0448(5) -0.0081(3) -0.0111(4) -0.0107(4)
O6 0.0518(5) 0.0325(4) 0.0437(5) -0.0088(4) -0.0167(4) -0.0165(4)
C12 0.0311(5) 0.0255(5) 0.0315(6) -0.0069(4) 0.0000(4) -0.0127(4)
C13 0.0296(5) 0.0248(5) 0.0295(5) -0.0068(4) -0.0034(4) -0.0119(4)
C14 0.0315(5) 0.0251(5) 0.0285(5) -0.0062(4) -0.0041(4) -0.0125(4)

_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
O1 C8 1.2296(14) . ?
O2 C2 1.2246(14) . ?
N1 C4 1.3747(14) . ?
N1 C2 1.3771(16) . ?
N1 C3 1.4635(14) . ?
N2 C2 1.4039(15) . ?
N2 C8 1.4147(14) . ?
N2 C1 1.4695(15) . ?
N3 C5 1.3416(15) . ?
N3 C7 1.3858(14) . ?
N3 C6 1.4678(14) . ?
N4 C5 1.3448(14) . ?
N4 C4 1.3593(15) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C7 1.3748(14) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.4291(16) . ?
O3 C9 1.3233(14) . ?
O3 H3 0.8200 . ?
O4 C9 1.2215(13) . ?
C9 C10 1.5066(15) . ?
C10 C11 1.5213(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C11 1.529(2) 2_565 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O5 C12 1.3389(14) . ?
O5 H5 0.8200 . ?
O6 C12 1.2083(14) . ?
C12 C13 1.5065(14) . ?
C13 C14 1.5240(14) . ?
C13 H13B 0.9700 . ?
C13 H13A 0.9700 . ?
C14 C14 1.5291(19) 2_645 ?
C14 H14B 0.9700 . ?
C14 H14A 0.9700 . ?

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
C4 N1 C2 119.68(10) . . ?
C4 N1 C3 120.45(10) . . ?
C2 N1 C3 119.86(10) . . ?
C2 N2 C8 126.83(10) . . ?
C2 N2 C1 115.59(10) . . ?
C8 N2 C1 117.57(10) . . ?
C5 N3 C7 106.66(9) . . ?
C5 N3 C6 126.14(10) . . ?
C7 N3 C6 127.11(10) . . ?
C5 N4 C4 103.94(9) . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 N1 122.23(11) . . ?
O2 C2 N2 120.72(11) . . ?
N1 C2 N2 117.04(9) . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 C4 N1 126.44(10) . . ?
N4 C4 C7 111.52(10) . . ?
N1 C4 C7 122.02(10) . . ?
N3 C5 N4 112.74(10) . . ?
N3 C5 H5A 123.6 . . ?
N4 C5 H5A 123.6 . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 N3 105.14(10) . . ?
C4 C7 C8 122.87(10) . . ?
N3 C7 C8 131.98(10) . . ?
O1 C8 N2 121.65(11) . . ?
O1 C8 C7 126.92(11) . . ?
N2 C8 C7 111.43(9) . . ?
C9 O3 H3 109.5 . . ?
O4 C9 O3 122.31(10) . . ?
O4 C9 C10 124.75(10) . . ?
O3 C9 C10 112.93(9) . . ?
C9 C10 C11 114.66(9) . . ?
C9 C10 H10A 108.6 . . ?
C11 C10 H10A 108.6 . . ?
C9 C10 H10B 108.6 . . ?
C11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C10 C11 C11 111.88(11) . 2_565 ?
C10 C11 H11A 109.2 . . ?
C11 C11 H11A 109.2 2_565 . ?
C10 C11 H11B 109.2 . . ?
C11 C11 H11B 109.2 2_565 . ?
H11A C11 H11B 107.9 . . ?
C12 O5 H5 109.5 . . ?
O6 C12 O5 123.26(10) . . ?
O6 C12 C13 124.59(10) . . ?
O5 C12 C13 112.14(10) . . ?
C12 C13 C14 113.11(9) . . ?
C12 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C12 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
H13B C13 H13A 107.8 . . ?
C13 C14 C14 112.05(11) . 2_645 ?
C13 C14 H14B 109.2 . . ?
C14 C14 H14B 109.2 2_645 . ?
C13 C14 H14A 109.2 . . ?
C14 C14 H14A 109.2 2_645 . ?
H14B C14 H14A 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 C2 O2 -178.76(10) . . . . ?
C3 N1 C2 O2 2.36(17) . . . . ?
C4 N1 C2 N2 1.72(15) . . . . ?
C3 N1 C2 N2 -177.17(10) . . . . ?
C8 N2 C2 O2 -177.89(10) . . . . ?
C1 N2 C2 O2 2.54(16) . . . . ?
C8 N2 C2 N1 1.65(16) . . . . ?
C1 N2 C2 N1 -177.93(10) . . . . ?
C5 N4 C4 N1 178.43(10) . . . . ?
C5 N4 C4 C7 -0.12(12) . . . . ?
C2 N1 C4 N4 177.84(10) . . . . ?
C3 N1 C4 N4 -3.28(17) . . . . ?
C2 N1 C4 C7 -3.75(16) . . . . ?
C3 N1 C4 C7 175.13(10) . . . . ?
C7 N3 C5 N4 0.11(12) . . . . ?
C6 N3 C5 N4 -176.57(11) . . . . ?
C4 N4 C5 N3 0.00(12) . . . . ?
N4 C4 C7 N3 0.19(13) . . . . ?
N1 C4 C7 N3 -178.44(9) . . . . ?
N4 C4 C7 C8 -178.85(10) . . . . ?
N1 C4 C7 C8 2.52(17) . . . . ?
C5 N3 C7 C4 -0.18(12) . . . . ?
C6 N3 C7 C4 176.46(10) . . . . ?
C5 N3 C7 C8 178.74(11) . . . . ?
C6 N3 C7 C8 -4.6(2) . . . . ?
C2 N2 C8 O1 177.44(10) . . . . ?
C1 N2 C8 O1 -2.99(16) . . . . ?
C2 N2 C8 C7 -2.73(15) . . . . ?
C1 N2 C8 C7 176.84(9) . . . . ?
C4 C7 C8 O1 -179.56(11) . . . . ?
N3 C7 C8 O1 1.7(2) . . . . ?
C4 C7 C8 N2 0.62(15) . . . . ?
N3 C7 C8 N2 -178.14(10) . . . . ?
O4 C9 C10 C11 -12.26(16) . . . . ?
O3 C9 C10 C11 168.62(9) . . . . ?
C9 C10 C11 C11 177.01(11) . . . 2_565 ?
O6 C12 C13 C14 -4.77(16) . . . . ?
O5 C12 C13 C14 176.07(9) . . . . ?
C12 C13 C14 C14 -173.91(11) . . . 2_645 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5 O4 0.82 1.93 2.7453(12) 171.9 .
O3 H3 N4 0.82 1.87 2.6850(12) 177.5 .
C5 H5a O4 0.93 2.68 3.263 121.8 .
C5 H5a O6 0.93 2.26 3.114 153.2 .

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.048