 
data_04mbh0601
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Heptamethyleneiminium DL-tartrate monohydrate
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C11 H23 N O7'
_chemical_formula_weight          281.30
 
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'
 'O'  'O'   0.0106   0.0060
 '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'
 
_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                    7.3930(10)
_cell_length_b                    8.215(4)
_cell_length_c                    23.323(16)
_cell_angle_alpha                 90.87(3)
_cell_angle_beta                  98.16(2)
_cell_angle_gamma                 99.94(3)
_cell_volume                      1380.0(12)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     5332
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.20
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.354
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              608
_exptl_absorpt_coefficient_mu     0.112
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9779
_exptl_absorpt_correction_T_max   0.9933
_exptl_absorpt_process_details      'SADABS V2.10 (Sheldrick, G.M., 2003)' 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             18872
_diffrn_reflns_av_R_equivalents   0.0595
_diffrn_reflns_av_sigmaI/netI     0.0835
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -30
_diffrn_reflns_limit_l_max        30
_diffrn_reflns_theta_min          3.02
_diffrn_reflns_theta_max          27.48
_reflns_number_total              6189
_reflns_number_gt                 3715
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

 The hydrogens for one of the water molecules could not be located satisfa-
 ctorily. On viewing the structure in Mercury it can be seen that there are
 a number of hydrogen bond donors and acceptors available for this molecule,
 suggesting that the molecule is rotating about its position thus making it
 difficult to locate the hydrogens from the density map. 
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0575P)²+0.8963P] where P=(Fo²+2Fc²)/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        0.0131(19)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          6189
_refine_ls_number_parameters      358
_refine_ls_number_restraints      3
_refine_ls_R_factor_all           0.1192
_refine_ls_R_factor_gt            0.0588
_refine_ls_wR_factor_ref          0.1525
_refine_ls_wR_factor_gt           0.1257
_refine_ls_goodness_of_fit_ref    1.028
_refine_ls_restrained_S_all       1.028
_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
C1 C -0.0589(3) 0.6607(3) 0.45582(12) 0.0241(6) Uani 1 1 d . . .
C2 C -0.2673(3) 0.6110(4) 0.45207(11) 0.0272(6) Uani 1 1 d . . .
H2 H -0.3002 0.4876 0.4495 0.033 Uiso 1 1 calc R . .
C3 C -0.3665(3) 0.6800(3) 0.39833(11) 0.0208(5) Uani 1 1 d . . .
H3 H -0.3282 0.6309 0.3634 0.025 Uiso 1 1 calc R . .
C4 C -0.5741(3) 0.6224(3) 0.39609(11) 0.0238(6) Uani 1 1 d . . .
O1A O 0.0387(2) 0.7274(2) 0.49983(8) 0.0317(5) Uani 1 1 d . . .
O1B O 0.0014(2) 0.6248(2) 0.40909(8) 0.0292(4) Uani 1 1 d . . .
H1 H 0.1154 0.6633 0.4120 0.044 Uiso 1 1 calc R . .
O2 O -0.3290(3) 0.6705(4) 0.50220(9) 0.0599(8) Uani 1 1 d . . .
H2A H -0.3683 0.5902 0.5216 0.090 Uiso 1 1 calc R . .
O3 O -0.3134(2) 0.8528(2) 0.39790(9) 0.0301(5) Uani 1 1 d . . .
H3O H -0.3832 0.8985 0.4159 0.045 Uiso 1 1 calc R . .
O4A O -0.6355(3) 0.4738(3) 0.38771(13) 0.0602(7) Uani 1 1 d . . .
O4B O -0.6691(2) 0.7317(2) 0.40495(8) 0.0283(4) Uani 1 1 d . . .
C22 C 0.1213(4) 0.0773(4) 0.38324(12) 0.0341(7) Uani 1 1 d . . .
H22A H 0.0636 -0.0039 0.4092 0.041 Uiso 1 1 calc R . .
H22B H 0.2563 0.1018 0.3974 0.041 Uiso 1 1 calc R . .
C23 C 0.0923(4) -0.0018(4) 0.32306(13) 0.0382(7) Uani 1 1 d . . .
H23A H -0.0425 -0.0230 0.3087 0.046 Uiso 1 1 calc R . .
H23B H 0.1329 -0.1104 0.3260 0.046 Uiso 1 1 calc R . .
C24 C 0.1902(5) 0.0938(4) 0.27803(14) 0.0433(8) Uani 1 1 d . . .
H24A H 0.1734 0.0208 0.2428 0.052 Uiso 1 1 calc R . .
H24B H 0.3247 0.1173 0.2929 0.052 Uiso 1 1 calc R . .
C25 C 0.1306(4) 0.2577(4) 0.25981(13) 0.0418(8) Uani 1 1 d . . .
H25B H 0.1911 0.3443 0.2897 0.050 Uiso 1 1 calc R . .
H25A H 0.1786 0.2889 0.2232 0.050 Uiso 1 1 calc R . .
C26 C -0.0771(4) 0.2585(4) 0.25086(12) 0.0390(7) Uani 1 1 d . . .
H26A H -0.1072 0.3235 0.2165 0.047 Uiso 1 1 calc R . .
H26B H -0.1433 0.1435 0.2421 0.047 Uiso 1 1 calc R . .
C27 C -0.1514(4) 0.3288(4) 0.30168(12) 0.0365(7) Uani 1 1 d . . .
H27B H -0.0796 0.4414 0.3116 0.044 Uiso 1 1 calc R . .
H27A H -0.2816 0.3406 0.2884 0.044 Uiso 1 1 calc R . .
C28 C -0.1479(4) 0.2334(4) 0.35693(12) 0.0351(7) Uani 1 1 d . . .
H28A H -0.2196 0.2824 0.3833 0.042 Uiso 1 1 calc R . .
H28B H -0.2103 0.1177 0.3473 0.042 Uiso 1 1 calc R . .
N21 N 0.0446(3) 0.2329(3) 0.38816(9) 0.0297(5) Uani 1 1 d . . .
H21A H 0.1241 0.3175 0.3746 0.036 Uiso 1 1 calc R . .
H21B H 0.0451 0.2569 0.4269 0.036 Uiso 1 1 calc R . .
C31 C 0.5601(3) 0.1897(3) 0.04043(11) 0.0196(5) Uani 1 1 d . . .
C32 C 0.7469(3) 0.1399(3) 0.03851(10) 0.0180(5) Uani 1 1 d . . .
H32 H 0.7299 0.0165 0.0357 0.022 Uiso 1 1 calc R . .
C33 C 0.8785(3) 0.2024(3) 0.09390(10) 0.0168(5) Uani 1 1 d . . .
H33 H 0.8233 0.1478 0.1270 0.020 Uiso 1 1 calc R . .
C34 C 1.0608(3) 0.1414(3) 0.09108(10) 0.0176(5) Uani 1 1 d . . .
O31A O 0.4865(2) 0.1301(2) 0.08455(8) 0.0262(4) Uani 1 1 d . . .
H31 H 0.3928 0.1725 0.0879 0.039 Uiso 1 1 calc R . .
O31B O 0.4911(2) 0.2756(2) 0.00404(7) 0.0240(4) Uani 1 1 d . . .
O32 O 0.8238(2) 0.2046(2) -0.01064(7) 0.0197(4) Uani 1 1 d . . .
H32O H 0.8438 0.1266 -0.0312 0.030 Uiso 1 1 calc R . .
O33 O 0.9012(2) 0.3747(2) 0.10444(7) 0.0230(4) Uani 1 1 d . . .
H33O H 0.8777 0.4207 0.0730 0.034 Uiso 1 1 calc R . .
O34A O 1.0500(2) -0.0078(2) 0.07899(7) 0.0234(4) Uani 1 1 d . . .
O34B O 1.2105(2) 0.2458(2) 0.10154(7) 0.0237(4) Uani 1 1 d . . .
C42 C 0.2421(3) 0.7101(3) 0.13733(11) 0.0228(6) Uani 1 1 d . . .
H42A H 0.1170 0.7202 0.1176 0.027 Uiso 1 1 calc R . .
H42B H 0.3218 0.8203 0.1379 0.027 Uiso 1 1 calc R . .
C43 C 0.2270(3) 0.6644(3) 0.19913(11) 0.0265(6) Uani 1 1 d . . .
H43A H 0.1585 0.5494 0.1982 0.032 Uiso 1 1 calc R . .
H43B H 0.1496 0.7363 0.2148 0.032 Uiso 1 1 calc R . .
C44 C 0.4063(4) 0.6751(4) 0.24233(12) 0.0356(7) Uani 1 1 d . . .
H44A H 0.3751 0.6847 0.2820 0.043 Uiso 1 1 calc R . .
H44B H 0.4530 0.5700 0.2391 0.043 Uiso 1 1 calc R . .
C45 C 0.5634(4) 0.8175(4) 0.23522(12) 0.0351(7) Uani 1 1 d . . .
H45A H 0.6257 0.8606 0.2742 0.042 Uiso 1 1 calc R . .
H45B H 0.5087 0.9078 0.2158 0.042 Uiso 1 1 calc R . .
C46 C 0.7101(4) 0.7726(4) 0.20053(12) 0.0318(7) Uani 1 1 d . . .
H46A H 0.8151 0.8668 0.2048 0.038 Uiso 1 1 calc R . .
H46B H 0.7577 0.6772 0.2187 0.038 Uiso 1 1 calc R . .
C47 C 0.6520(3) 0.7292(3) 0.13581(11) 0.0266(6) Uani 1 1 d . . .
H47A H 0.5965 0.8208 0.1177 0.032 Uiso 1 1 calc R . .
H47B H 0.7649 0.7223 0.1182 0.032 Uiso 1 1 calc R . .
C48 C 0.5144(3) 0.5683(3) 0.12083(12) 0.0252(6) Uani 1 1 d . . .
H48A H 0.5546 0.5075 0.0893 0.030 Uiso 1 1 calc R . .
H48B H 0.5175 0.4989 0.1552 0.030 Uiso 1 1 calc R . .
N41 N 0.3185(3) 0.5925(3) 0.10216(9) 0.0214(5) Uani 1 1 d . . .
H41A H 0.3101 0.6275 0.0647 0.026 Uiso 1 1 calc R . .
H41B H 0.2426 0.4909 0.1013 0.026 Uiso 1 1 calc R . .
O1W O -0.4134(3) 1.1198(3) 0.46607(11) 0.0641(7) Uani 1 1 d . . .
O2W O 0.8352(2) 0.5787(2) 0.01625(8) 0.0246(4) Uani 1 1 d D . .
H21W H 0.745(3) 0.628(4) 0.0127(15) 0.057(11) Uiso 1 1 d D . .
H22W H 0.932(3) 0.643(3) 0.0110(15) 0.057(11) Uiso 1 1 d D . .
 
 
_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 O1A 1.229(3) . ?
C1 O1B 1.284(3) . ?
C1 C2 1.514(3) . ?
C2 O2 1.423(3) . ?
C2 C3 1.528(4) . ?
C2 H2 1.0000 . ?
C3 O3 1.407(3) . ?
C3 C4 1.519(3) . ?
C3 H3 1.0000 . ?
C4 O4A 1.229(3) . ?
C4 O4B 1.263(3) . ?
O1B H1 0.8400 . ?
O2 H2A 0.8400 . ?
O3 H3O 0.8400 . ?
C22 N21 1.495(4) . ?
C22 C23 1.509(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.513(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.535(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.522(4) . ?
C25 H25B 0.9900 . ?
C25 H25A 0.9900 . ?
C26 C27 1.521(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.517(4) . ?
C27 H27B 0.9900 . ?
C27 H27A 0.9900 . ?
C28 N21 1.504(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
N21 H21A 0.9200 . ?
N21 H21B 0.9200 . ?
C31 O31B 1.224(3) . ?
C31 O31A 1.295(3) . ?
C31 C32 1.513(3) . ?
C32 O32 1.421(3) . ?
C32 C33 1.526(3) . ?
C32 H32 1.0000 . ?
C33 O33 1.410(3) . ?
C33 C34 1.526(3) . ?
C33 H33 1.0000 . ?
C34 O34A 1.240(3) . ?
C34 O34B 1.268(3) . ?
O31A H31 0.8400 . ?
O32 H32O 0.8400 . ?
O33 H33O 0.8400 . ?
C42 N41 1.490(3) . ?
C42 C43 1.509(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.535(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.528(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.532(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.529(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.525(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 N41 1.500(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N41 H41A 0.9200 . ?
N41 H41B 0.9200 . ?
O2W H21W 0.829(17) . ?
O2W H22W 0.838(17) . ?
 
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
O1A C1 O1B 125.0(2) . . ?
O1A C1 C2 122.1(2) . . ?
O1B C1 C2 113.0(2) . . ?
O2 C2 C1 110.6(2) . . ?
O2 C2 C3 109.0(2) . . ?
C1 C2 C3 110.7(2) . . ?
O2 C2 H2 108.9 . . ?
C1 C2 H2 108.9 . . ?
C3 C2 H2 108.9 . . ?
O3 C3 C4 113.9(2) . . ?
O3 C3 C2 110.9(2) . . ?
C4 C3 C2 108.2(2) . . ?
O3 C3 H3 107.9 . . ?
C4 C3 H3 107.9 . . ?
C2 C3 H3 107.9 . . ?
O4A C4 O4B 125.2(2) . . ?
O4A C4 C3 118.0(2) . . ?
O4B C4 C3 116.8(2) . . ?
C1 O1B H1 109.5 . . ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3O 109.5 . . ?
N21 C22 C23 115.4(2) . . ?
N21 C22 H22A 108.4 . . ?
C23 C22 H22A 108.4 . . ?
N21 C22 H22B 108.4 . . ?
C23 C22 H22B 108.4 . . ?
H22A C22 H22B 107.5 . . ?
C22 C23 C24 117.1(3) . . ?
C22 C23 H23A 108.0 . . ?
C24 C23 H23A 108.0 . . ?
C22 C23 H23B 108.0 . . ?
C24 C23 H23B 108.0 . . ?
H23A C23 H23B 107.3 . . ?
C23 C24 C25 117.7(3) . . ?
C23 C24 H24A 107.9 . . ?
C25 C24 H24A 107.9 . . ?
C23 C24 H24B 107.9 . . ?
C25 C24 H24B 107.9 . . ?
H24A C24 H24B 107.2 . . ?
C26 C25 C24 116.2(3) . . ?
C26 C25 H25B 108.2 . . ?
C24 C25 H25B 108.2 . . ?
C26 C25 H25A 108.2 . . ?
C24 C25 H25A 108.2 . . ?
H25B C25 H25A 107.4 . . ?
C27 C26 C25 115.5(2) . . ?
C27 C26 H26A 108.4 . . ?
C25 C26 H26A 108.4 . . ?
C27 C26 H26B 108.4 . . ?
C25 C26 H26B 108.4 . . ?
H26A C26 H26B 107.5 . . ?
C28 C27 C26 118.0(3) . . ?
C28 C27 H27B 107.8 . . ?
C26 C27 H27B 107.8 . . ?
C28 C27 H27A 107.8 . . ?
C26 C27 H27A 107.8 . . ?
H27B C27 H27A 107.1 . . ?
N21 C28 C27 113.7(2) . . ?
N21 C28 H28A 108.8 . . ?
C27 C28 H28A 108.8 . . ?
N21 C28 H28B 108.8 . . ?
C27 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C22 N21 C28 117.0(2) . . ?
C22 N21 H21A 108.0 . . ?
C28 N21 H21A 108.0 . . ?
C22 N21 H21B 108.0 . . ?
C28 N21 H21B 108.0 . . ?
H21A N21 H21B 107.3 . . ?
O31B C31 O31A 125.8(2) . . ?
O31B C31 C32 122.7(2) . . ?
O31A C31 C32 111.5(2) . . ?
O32 C32 C31 110.55(19) . . ?
O32 C32 C33 110.02(19) . . ?
C31 C32 C33 109.83(19) . . ?
O32 C32 H32 108.8 . . ?
C31 C32 H32 108.8 . . ?
C33 C32 H32 108.8 . . ?
O33 C33 C32 113.55(19) . . ?
O33 C33 C34 113.43(18) . . ?
C32 C33 C34 107.65(19) . . ?
O33 C33 H33 107.3 . . ?
C32 C33 H33 107.3 . . ?
C34 C33 H33 107.3 . . ?
O34A C34 O34B 125.3(2) . . ?
O34A C34 C33 116.8(2) . . ?
O34B C34 C33 118.0(2) . . ?
C31 O31A H31 109.5 . . ?
C32 O32 H32O 109.5 . . ?
C33 O33 H33O 109.5 . . ?
N41 C42 C43 115.7(2) . . ?
N41 C42 H42A 108.3 . . ?
C43 C42 H42A 108.3 . . ?
N41 C42 H42B 108.3 . . ?
C43 C42 H42B 108.3 . . ?
H42A C42 H42B 107.4 . . ?
C42 C43 C44 118.5(2) . . ?
C42 C43 H43A 107.7 . . ?
C44 C43 H43A 107.7 . . ?
C42 C43 H43B 107.7 . . ?
C44 C43 H43B 107.7 . . ?
H43A C43 H43B 107.1 . . ?
C45 C44 C43 116.3(2) . . ?
C45 C44 H44A 108.2 . . ?
C43 C44 H44A 108.2 . . ?
C45 C44 H44B 108.2 . . ?
C43 C44 H44B 108.2 . . ?
H44A C44 H44B 107.4 . . ?
C44 C45 C46 115.0(2) . . ?
C44 C45 H45A 108.5 . . ?
C46 C45 H45A 108.5 . . ?
C44 C45 H45B 108.5 . . ?
C46 C45 H45B 108.5 . . ?
H45A C45 H45B 107.5 . . ?
C47 C46 C45 117.9(2) . . ?
C47 C46 H46A 107.8 . . ?
C45 C46 H46A 107.8 . . ?
C47 C46 H46B 107.8 . . ?
C45 C46 H46B 107.8 . . ?
H46A C46 H46B 107.2 . . ?
C48 C47 C46 115.5(2) . . ?
C48 C47 H47A 108.4 . . ?
C46 C47 H47A 108.4 . . ?
C48 C47 H47B 108.4 . . ?
C46 C47 H47B 108.4 . . ?
H47A C47 H47B 107.5 . . ?
N41 C48 C47 113.9(2) . . ?
N41 C48 H48A 108.8 . . ?
C47 C48 H48A 108.8 . . ?
N41 C48 H48B 108.8 . . ?
C47 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
C42 N41 C48 118.04(19) . . ?
C42 N41 H41A 107.8 . . ?
C48 N41 H41A 107.8 . . ?
C42 N41 H41B 107.8 . . ?
C48 N41 H41B 107.8 . . ?
H41A N41 H41B 107.1 . . ?
H21W O2W H22W 110(2) . . ?
 
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
O3 H3O O1W  0.84 2.21 2.945(4) 146.4 .
O33 H33O O2W  0.84 1.90 2.716(3) 163.7 .
O1B H1 O4B  0.84 1.63 2.459(2) 169.7 1_655
N21 H21A O4A  0.92 1.99 2.811(3) 148.2 1_655
N21 H21B O1A  0.92 1.91 2.795(3) 160.8 2_566
N21 H21B O2  0.92 2.46 3.070(3) 123.9 2_566
O31A H31 O34B  0.84 1.64 2.472(2) 173.5 1_455
N41 H41B O34B  0.92 1.99 2.822(3) 150.1 1_455
N41 H41B O33  0.92 2.55 3.297(3) 138.4 1_455
O32 H32O O34A  0.84 1.81 2.625(3) 161.6 2_755
N41 H41A O32  0.92 2.16 2.918(3) 139.7 2_665
N41 H41A O31B  0.92 2.38 3.136(3) 139.2 2_665
N41 H41A O2W  0.92 2.51 3.055(3) 118.5 2_665
O2W H21W O31B  0.829(17) 2.033(17) 2.857(2) 173(3) 2_665
O2W H22W O32  0.838(17) 2.013(18) 2.845(2) 172(3) 2_765
 
_diffrn_measured_fraction_theta_max    0.977
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.977
_refine_diff_density_max    0.688
_refine_diff_density_min   -0.455
_refine_diff_density_rms    0.063
