Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Steven Langford'
_publ_contact_author_address     
;
Department of Chemistry
Monash University
Wellington Rd
Clayton
Victoria
3800
AUSTRALIA
;

_publ_contact_author_email       STEVEN.LANGFORD@SCI.MONASH.EDU.AU

_publ_section_title              
;
Supramolecular self-assembly of dihydroxy tin(IV)
porphyrin stabilized helical water chains
;
loop_
_publ_author_name
S.Langford
C.P.Woodward

data_1
_database_code_depnum_ccdc_archive 'CCDC 630949'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Trans dihydroxy (5,10,15,20-tetrakis(4-pyridyl)porphrynato)
tin(IV) tetra hydrate
;
_chemical_name_common            
;
Trans dihydroxy (5,10,15,20-tetrakis(4-pyridyl)porphrynato)
tin(IV) tetra hydrate
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H26 N8 O2 Sn, 8(H2 O)'
_chemical_formula_sum            'C40 H42 N8 O10 Sn'
_chemical_formula_weight         913.51

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'
Sn Sn -0.6537 1.4246 '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
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   12.4391(6)
_cell_length_b                   12.7200(5)
_cell_length_c                   13.2986(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.955(1)
_cell_angle_gamma                90.00
_cell_volume                     1907.73(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       tabular
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Bruker Apex II KAPPA CCD'
_diffrn_measurement_method       '0.5 deg frames in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12217
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4377
_reflns_number_gt                4035
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0176P)^2^+4.5578P] 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         4377
_refine_ls_number_parameters     304
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0480
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0963
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_restrained_S_all      1.247
_refine_ls_shift/su_max          0.004
_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
Sn1 Sn 0.5000 0.0000 0.5000 0.00946(9) Uani 1 2 d S . .
O1 O 0.3551(2) -0.02845(19) 0.3568(2) 0.0157(5) Uani 1 1 d D . .
O2 O -0.0064(3) 0.0719(2) 0.3715(3) 0.0271(6) Uani 1 1 d D . .
O3 O -0.0395(3) 0.3633(2) 0.0793(3) 0.0340(7) Uani 1 1 d D . .
O4 O 0.1621(3) 0.1126(3) 0.2951(3) 0.0329(7) Uani 1 1 d D . .
O5 O 0.0364(3) 0.1598(2) 0.0719(3) 0.0245(6) Uani 1 1 d D . .
N1 N 0.5005(2) 0.1530(2) 0.4391(2) 0.0113(6) Uani 1 1 d . . .
N2 N 0.6116(2) -0.0513(2) 0.4269(2) 0.0118(6) Uani 1 1 d . . .
N3 N 0.8206(3) 0.2742(2) 0.1814(3) 0.0195(7) Uani 1 1 d . . .
N4 N 0.8366(3) -0.5178(2) 0.5118(3) 0.0180(6) Uani 1 1 d . . .
C1 C 0.4338(3) 0.2359(3) 0.4476(3) 0.0116(6) Uani 1 1 d . . .
C2 C 0.4537(3) 0.3231(3) 0.3888(3) 0.0146(7) Uani 1 1 d . . .
H2 H 0.4193 0.3910 0.3811 0.018 Uiso 1 1 calc R . .
C3 C 0.5304(3) 0.2915(3) 0.3461(3) 0.0133(7) Uani 1 1 d . . .
H3 H 0.5589 0.3331 0.3032 0.016 Uiso 1 1 calc R . .
C4 C 0.5603(3) 0.1835(3) 0.3777(3) 0.0109(6) Uani 1 1 d . . .
C5 C 0.6370(3) 0.1198(3) 0.3505(3) 0.0115(6) Uani 1 1 d . . .
C6 C 0.6619(3) 0.0131(3) 0.3750(3) 0.0120(6) Uani 1 1 d . . .
C7 C 0.7481(3) -0.0486(3) 0.3542(3) 0.0135(7) Uani 1 1 d . . .
H7 H 0.7963 -0.0243 0.3194 0.016 Uiso 1 1 calc R . .
C8 C 0.7480(3) -0.1472(3) 0.3932(3) 0.0147(7) Uani 1 1 d . . .
H8 H 0.7956 -0.2044 0.3902 0.018 Uiso 1 1 calc R . .
C9 C 0.6622(3) -0.1490(3) 0.4401(3) 0.0121(6) Uani 1 1 d . . .
C10 C 0.6407(3) -0.2345(3) 0.4969(3) 0.0110(6) Uani 1 1 d . . .
C11 C 0.6996(3) 0.1728(3) 0.2907(3) 0.0121(6) Uani 1 1 d . . .
C12 C 0.7848(3) 0.2495(3) 0.3433(3) 0.0155(7) Uani 1 1 d . . .
H12 H 0.8029 0.2691 0.4177 0.019 Uiso 1 1 calc R . .
C13 C 0.8430(3) 0.2971(3) 0.2866(3) 0.0188(7) Uani 1 1 d . . .
H13 H 0.9017 0.3484 0.3243 0.023 Uiso 1 1 calc R . .
C14 C 0.7382(3) 0.2009(3) 0.1308(3) 0.0182(7) Uani 1 1 d . . .
H14 H 0.7209 0.1841 0.0559 0.022 Uiso 1 1 calc R . .
C15 C 0.6766(3) 0.1480(3) 0.1814(3) 0.0159(7) Uani 1 1 d . . .
H15 H 0.6196 0.0958 0.1421 0.019 Uiso 1 1 calc R . .
C16 C 0.7075(3) -0.3337(3) 0.5016(3) 0.0127(7) Uani 1 1 d . . .
C17 C 0.6840(3) -0.3939(3) 0.4074(3) 0.0153(7) Uani 1 1 d . . .
H17 H 0.6235 -0.3737 0.3378 0.018 Uiso 1 1 calc R . .
C18 C 0.7503(3) -0.4838(3) 0.4168(3) 0.0161(7) Uani 1 1 d . . .
H18 H 0.7334 -0.5239 0.3516 0.019 Uiso 1 1 calc R . .
C19 C 0.8584(3) -0.4591(3) 0.6026(3) 0.0183(7) Uani 1 1 d . . .
H19 H 0.9187 -0.4819 0.6713 0.022 Uiso 1 1 calc R . .
C20 C 0.7977(3) -0.3670(3) 0.6017(3) 0.0161(7) Uani 1 1 d . . .
H20 H 0.8172 -0.3276 0.6678 0.019 Uiso 1 1 calc R . .
H1 H 0.323(4) -0.084(2) 0.358(4) 0.046(16) Uiso 1 1 d D . .
H21 H -0.005(9) 0.098(8) 0.432(5) 0.17(4) Uiso 1 1 d D . .
H22 H 0.055(3) 0.087(4) 0.360(4) 0.038(14) Uiso 1 1 d D . .
H31 H -0.087(4) 0.344(4) 0.108(4) 0.049(16) Uiso 1 1 d D . .
H32 H -0.036(6) 0.4306(16) 0.084(6) 0.07(2) Uiso 1 1 d D . .
H41 H 0.224(3) 0.074(4) 0.314(5) 0.059(18) Uiso 1 1 d D . .
H42 H 0.133(4) 0.121(4) 0.2251(18) 0.045(16) Uiso 1 1 d D . .
H51 H 0.010(5) 0.222(2) 0.071(5) 0.07(2) Uiso 1 1 d D . .
H52 H -0.025(3) 0.122(4) 0.050(4) 0.052(17) Uiso 1 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
Sn1 0.01075(15) 0.00736(15) 0.01117(15) 0.00075(12) 0.00549(12) 0.00071(12)
O1 0.0154(12) 0.0116(12) 0.0173(12) 0.0000(10) 0.0043(10) -0.0025(10)
O2 0.0282(16) 0.0239(15) 0.0295(16) 0.0000(13) 0.0124(13) 0.0018(12)
O3 0.048(2) 0.0205(15) 0.049(2) -0.0059(15) 0.0355(17) -0.0074(15)
O4 0.0248(16) 0.045(2) 0.0239(16) 0.0013(15) 0.0059(13) 0.0117(14)
O5 0.0196(14) 0.0200(15) 0.0334(16) 0.0012(13) 0.0105(13) -0.0013(12)
N1 0.0141(13) 0.0074(13) 0.0138(14) 0.0026(11) 0.0071(11) 0.0022(11)
N2 0.0147(13) 0.0085(13) 0.0133(14) 0.0000(11) 0.0070(11) 0.0004(11)
N3 0.0219(16) 0.0169(15) 0.0258(17) 0.0070(13) 0.0160(14) 0.0034(13)
N4 0.0218(15) 0.0094(14) 0.0283(16) 0.0038(13) 0.0158(13) 0.0031(12)
C1 0.0118(15) 0.0078(15) 0.0144(16) -0.0009(13) 0.0048(13) -0.0007(12)
C2 0.0189(17) 0.0086(15) 0.0172(17) 0.0027(13) 0.0083(14) 0.0011(13)
C3 0.0146(16) 0.0101(16) 0.0160(16) 0.0026(13) 0.0074(14) 0.0000(13)
C4 0.0102(15) 0.0107(15) 0.0121(15) 0.0024(12) 0.0049(13) -0.0002(12)
C5 0.0131(15) 0.0131(16) 0.0075(14) -0.0006(12) 0.0034(13) -0.0012(13)
C6 0.0130(15) 0.0101(16) 0.0124(15) -0.0009(13) 0.0047(12) -0.0003(13)
C7 0.0149(16) 0.0128(16) 0.0159(17) 0.0016(13) 0.0095(14) 0.0020(13)
C8 0.0144(16) 0.0147(17) 0.0171(17) -0.0013(14) 0.0089(14) 0.0016(13)
C9 0.0127(15) 0.0129(16) 0.0119(15) -0.0017(13) 0.0064(13) 0.0005(13)
C10 0.0103(14) 0.0098(15) 0.0113(15) -0.0008(13) 0.0031(12) 0.0005(12)
C11 0.0147(16) 0.0074(15) 0.0175(17) 0.0029(13) 0.0100(14) 0.0036(13)
C12 0.0171(17) 0.0128(16) 0.0160(17) -0.0007(14) 0.0064(14) 0.0006(14)
C13 0.0163(17) 0.0133(17) 0.029(2) 0.0012(15) 0.0114(16) -0.0016(14)
C14 0.0270(19) 0.0146(17) 0.0176(17) 0.0044(14) 0.0137(16) 0.0045(15)
C15 0.0196(17) 0.0113(16) 0.0180(17) -0.0010(14) 0.0091(14) 0.0008(14)
C16 0.0146(16) 0.0080(15) 0.0198(17) 0.0008(13) 0.0115(14) 0.0016(13)
C17 0.0173(17) 0.0140(17) 0.0153(17) 0.0012(14) 0.0076(14) 0.0005(14)
C18 0.0217(17) 0.0089(16) 0.0206(17) -0.0004(14) 0.0117(14) 0.0004(14)
C19 0.0191(17) 0.0167(17) 0.0185(18) 0.0039(14) 0.0075(15) 0.0036(14)
C20 0.0181(17) 0.0146(17) 0.0162(17) -0.0001(14) 0.0078(14) 0.0043(14)

_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
Sn1 O1 2.027(2) . ?
Sn1 O1 2.027(2) 3_656 ?
Sn1 N2 2.106(3) . ?
Sn1 N2 2.106(3) 3_656 ?
Sn1 N1 2.109(3) . ?
Sn1 N1 2.109(3) 3_656 ?
O1 H1 0.819(19) . ?
O2 H21 0.86(2) . ?
O2 H22 0.862(19) . ?
O3 H31 0.858(19) . ?
O3 H32 0.86(2) . ?
O4 H41 0.86(2) . ?
O4 H42 0.851(19) . ?
O5 H51 0.85(2) . ?
O5 H52 0.847(19) . ?
N1 C4 1.373(4) . ?
N1 C1 1.375(4) . ?
N2 C9 1.371(4) . ?
N2 C6 1.379(4) . ?
N3 C14 1.339(5) . ?
N3 C13 1.339(5) . ?
N4 C18 1.338(5) . ?
N4 C19 1.347(5) . ?
C1 C10 1.408(4) 3_656 ?
C1 C2 1.437(4) . ?
C2 C3 1.361(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.439(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.410(4) . ?
C5 C6 1.400(5) . ?
C5 C11 1.489(4) . ?
C6 C7 1.446(4) . ?
C7 C8 1.358(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.446(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.412(5) . ?
C10 C1 1.408(4) 3_656 ?
C10 C16 1.499(4) . ?
C11 C12 1.392(5) . ?
C11 C15 1.394(5) . ?
C12 C13 1.385(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.389(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.389(5) . ?
C16 C20 1.397(5) . ?
C17 C18 1.383(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.391(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sn1 O1 180.000(1) . 3_656 ?
O1 Sn1 N2 90.50(11) . . ?
O1 Sn1 N2 89.50(11) 3_656 . ?
O1 Sn1 N2 89.50(11) . 3_656 ?
O1 Sn1 N2 90.50(11) 3_656 3_656 ?
N2 Sn1 N2 180.0 . 3_656 ?
O1 Sn1 N1 87.10(10) . . ?
O1 Sn1 N1 92.90(10) 3_656 . ?
N2 Sn1 N1 89.97(10) . . ?
N2 Sn1 N1 90.03(10) 3_656 . ?
O1 Sn1 N1 92.90(10) . 3_656 ?
O1 Sn1 N1 87.10(10) 3_656 3_656 ?
N2 Sn1 N1 90.03(10) . 3_656 ?
N2 Sn1 N1 89.97(10) 3_656 3_656 ?
N1 Sn1 N1 180.00(6) . 3_656 ?
Sn1 O1 H1 112(4) . . ?
H21 O2 H22 114(7) . . ?
H31 O3 H32 105(5) . . ?
H41 O4 H42 108(5) . . ?
H51 O5 H52 103(5) . . ?
C4 N1 C1 109.2(3) . . ?
C4 N1 Sn1 125.4(2) . . ?
C1 N1 Sn1 125.2(2) . . ?
C9 N2 C6 108.7(3) . . ?
C9 N2 Sn1 125.3(2) . . ?
C6 N2 Sn1 125.0(2) . . ?
C14 N3 C13 117.0(3) . . ?
C18 N4 C19 116.4(3) . . ?
N1 C1 C10 125.9(3) . 3_656 ?
N1 C1 C2 107.4(3) . . ?
C10 C1 C2 126.7(3) 3_656 . ?
C3 C2 C1 108.1(3) . . ?
C3 C2 H2 125.9 . . ?
C1 C2 H2 125.9 . . ?
C2 C3 C4 107.5(3) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
N1 C4 C5 125.8(3) . . ?
N1 C4 C3 107.8(3) . . ?
C5 C4 C3 126.4(3) . . ?
C6 C5 C4 127.2(3) . . ?
C6 C5 C11 116.7(3) . . ?
C4 C5 C11 116.0(3) . . ?
N2 C6 C5 126.1(3) . . ?
N2 C6 C7 107.7(3) . . ?
C5 C6 C7 126.2(3) . . ?
C8 C7 C6 107.9(3) . . ?
C8 C7 H7 126.1 . . ?
C6 C7 H7 126.1 . . ?
C7 C8 C9 107.5(3) . . ?
C7 C8 H8 126.3 . . ?
C9 C8 H8 126.3 . . ?
N2 C9 C10 125.9(3) . . ?
N2 C9 C8 108.2(3) . . ?
C10 C9 C8 125.8(3) . . ?
C1 C10 C9 127.3(3) 3_656 . ?
C1 C10 C16 116.4(3) 3_656 . ?
C9 C10 C16 116.3(3) . . ?
C12 C11 C15 117.5(3) . . ?
C12 C11 C5 120.5(3) . . ?
C15 C11 C5 122.0(3) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
N3 C13 C12 123.3(3) . . ?
N3 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
N3 C14 C15 123.8(3) . . ?
N3 C14 H14 118.1 . . ?
C15 C14 H14 118.1 . . ?
C14 C15 C11 118.9(3) . . ?
C14 C15 H15 120.6 . . ?
C11 C15 H15 120.6 . . ?
C17 C16 C20 118.1(3) . . ?
C17 C16 C10 121.7(3) . . ?
C20 C16 C10 120.2(3) . . ?
C18 C17 C16 118.9(3) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
N4 C18 C17 124.2(3) . . ?
N4 C18 H18 117.9 . . ?
C17 C18 H18 117.9 . . ?
N4 C19 C20 123.8(3) . . ?
N4 C19 H19 118.1 . . ?
C20 C19 H19 118.1 . . ?
C19 C20 C16 118.5(3) . . ?
C19 C20 H20 120.7 . . ?
C16 C20 H20 120.7 . . ?

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
O4 H41 O1 0.86(2) 1.97(2) 2.828(4) 174(6) .
O4 H42 O5 0.851(19) 1.94(2) 2.774(4) 166(5) .
O2 H21 O3 0.86(2) 2.24(3) 3.073(5) 165(10) 4_566
O2 H22 O4 0.862(19) 1.89(2) 2.737(5) 165(5) .
O3 H32 O2 0.86(2) 1.90(3) 2.734(4) 165(7) 2
O3 H31 N3 0.858(19) 2.01(2) 2.854(4) 169(5) 1_455
O5 H51 O3 0.85(2) 1.92(2) 2.772(4) 176(7) .
O5 H52 N4 0.847(19) 2.06(2) 2.899(4) 174(5) 4_455
O1 H1 N3 0.819(19) 2.43(2) 3.225(4) 163(5) 2_645

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.853
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.100