 
data_ssg0302
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Glutaric acid & 1,1,3,3-tetramethylbutylamine
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C47 H100 N4 O12'
_chemical_formula_weight          913.31
 
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            Monoclinic
_symmetry_space_group_name_H-M    C2
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 
_cell_length_a                    23.089(7)
_cell_length_b                    6.403(2)
_cell_length_c                    18.496(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.025(3)
_cell_angle_gamma                 90.00
_cell_volume                      2727.7(15)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     958
_cell_measurement_theta_min       3.21
_cell_measurement_theta_max       26.99
 
_exptl_crystal_description        needle
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.112
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1012
_exptl_absorpt_coefficient_mu     0.079
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.6911
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator   'silicon 111'
_diffrn_measurement_device_type   'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method        'fine-slice ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         5
_diffrn_reflns_number             12018
_diffrn_reflns_av_R_equivalents   0.0492
_diffrn_reflns_av_sigmaI/netI     0.0747
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        29
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          2.84
_diffrn_reflns_theta_max          26.66
_reflns_number_total              6130
_reflns_number_gt                 5380
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Bruker APEX2'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_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.
;
 
_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)+(0.0653P)²+0.4011P] where P=(Fo²+2Fc²)/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_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    1.7(9)
_refine_ls_number_reflns          6130
_refine_ls_number_parameters      305
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0581
_refine_ls_R_factor_gt            0.0498
_refine_ls_wR_factor_ref          0.1331
_refine_ls_wR_factor_gt           0.1268
_refine_ls_goodness_of_fit_ref    1.029
_refine_ls_restrained_S_all       1.029
_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
C1 C 0.26584(7) 0.6667(3) 0.14482(9) 0.0212(4) Uani 1 1 d . . .
C2 C 0.27904(8) 0.7678(3) 0.21836(10) 0.0228(4) Uani 1 1 d . . .
H2A H 0.2474 0.7353 0.2501 0.027 Uiso 1 1 calc R . .
H2B H 0.2806 0.9213 0.2125 0.027 Uiso 1 1 calc R . .
C3 C 0.33677(8) 0.6903(4) 0.25412(9) 0.0247(4) Uani 1 1 d . . .
H3A H 0.3688 0.7379 0.2253 0.030 Uiso 1 1 calc R . .
H3B H 0.3369 0.5357 0.2544 0.030 Uiso 1 1 calc R . .
C4 C 0.34718(8) 0.7707(4) 0.33229(10) 0.0262(4) Uani 1 1 d . . .
H4A H 0.3882 0.7464 0.3495 0.031 Uiso 1 1 calc R . .
H4B H 0.3399 0.9230 0.3333 0.031 Uiso 1 1 calc R . .
C5 C 0.30792(8) 0.6617(3) 0.38246(9) 0.0221(4) Uani 1 1 d . . .
O1A O 0.26567(6) 0.7824(2) 0.08855(7) 0.0276(3) Uani 1 1 d . . .
O1B O 0.25639(6) 0.4758(2) 0.14314(7) 0.0270(3) Uani 1 1 d . . .
O5A O 0.27356(6) 0.7673(2) 0.41772(7) 0.0250(3) Uani 1 1 d . . .
O5B O 0.31222(6) 0.4650(2) 0.38745(7) 0.0246(3) Uani 1 1 d . . .
C21 C 0.45377(9) 0.1608(5) 0.22203(11) 0.0363(5) Uani 1 1 d . . .
H21A H 0.4943 0.1327 0.2383 0.055 Uiso 1 1 calc R . .
H21B H 0.4287 0.0569 0.2430 0.055 Uiso 1 1 calc R . .
H21C H 0.4430 0.3007 0.2378 0.055 Uiso 1 1 calc R . .
C22 C 0.44638(8) 0.1483(3) 0.13861(10) 0.0248(4) Uani 1 1 d . . .
C23 C 0.38049(8) 0.1766(3) 0.11815(9) 0.0231(4) Uani 1 1 d . . .
H23A H 0.3609 0.0525 0.1372 0.028 Uiso 1 1 calc R . .
H23B H 0.3679 0.2978 0.1463 0.028 Uiso 1 1 calc R . .
C24 C 0.35455(8) 0.2082(3) 0.03953(10) 0.0217(4) Uani 1 1 d . . .
C26 C 0.48396(10) 0.3194(4) 0.10837(13) 0.0357(5) Uani 1 1 d . . .
H26A H 0.5243 0.3021 0.1279 0.054 Uiso 1 1 calc R . .
H26B H 0.4696 0.4564 0.1225 0.054 Uiso 1 1 calc R . .
H26C H 0.4821 0.3093 0.0554 0.054 Uiso 1 1 calc R . .
C27 C 0.46770(10) -0.0651(4) 0.11588(13) 0.0366(5) Uani 1 1 d . . .
H27A H 0.4673 -0.0716 0.0629 0.055 Uiso 1 1 calc R . .
H27B H 0.4422 -0.1738 0.1332 0.055 Uiso 1 1 calc R . .
H27C H 0.5074 -0.0875 0.1368 0.055 Uiso 1 1 calc R . .
C28 C 0.37093(9) 0.0428(4) -0.01454(10) 0.0279(4) Uani 1 1 d . . .
H28A H 0.3651 -0.0963 0.0058 0.042 Uiso 1 1 calc R . .
H28B H 0.4118 0.0598 -0.0245 0.042 Uiso 1 1 calc R . .
H28C H 0.3465 0.0586 -0.0597 0.042 Uiso 1 1 calc R . .
C29 C 0.36416(9) 0.4273(3) 0.01005(11) 0.0275(4) Uani 1 1 d . . .
H29A H 0.4053 0.4457 0.0018 0.041 Uiso 1 1 calc R . .
H29B H 0.3526 0.5311 0.0452 0.041 Uiso 1 1 calc R . .
H29C H 0.3407 0.4456 -0.0358 0.041 Uiso 1 1 calc R . .
N25 N 0.28967(6) 0.1883(3) 0.04567(8) 0.0218(3) Uani 1 1 d . . .
H25A H 0.2830 0.0828 0.0633 0.043(8) Uiso 1 1 calc R . .
H25B H 0.2672 0.2042 0.0026 0.051(8) Uiso 1 1 d R . .
H25C H 0.2742 0.2925 0.0796 0.044(7) Uiso 1 1 d R . .
C31 C -0.04279(10) -0.1961(4) 0.41504(12) 0.0348(5) Uani 1 1 d . . .
C32 C 0.00448(10) -0.3518(4) 0.43163(13) 0.0376(5) Uani 1 1 d . . .
H32A H 0.0420 -0.2762 0.4359 0.045 Uiso 1 1 calc R . .
H32B H 0.0055 -0.4479 0.3898 0.045 Uiso 1 1 calc R . .
C33 C 0.0000 -0.4831(5) 0.5000 0.0336(7) Uani 1 2 d S . .
H33A H 0.0346 -0.5742 0.5065 0.040 Uiso 0.50 1 calc PR . .
H33B H -0.0346 -0.5742 0.4935 0.040 Uiso 0.50 1 calc PR . .
O31A O -0.03419(8) -0.0120(3) 0.40338(13) 0.0576(5) Uani 1 1 d . . .
O31B O -0.09467(7) -0.2791(3) 0.41421(10) 0.0417(4) Uani 1 1 d . . .
H31 H -0.1198 -0.1841 0.4108 0.14(2) Uiso 1 1 calc R . .
C41 C 0.14497(10) 0.1134(4) 0.18765(11) 0.0360(5) Uani 1 1 d . . .
H41A H 0.1446 -0.0383 0.1945 0.054 Uiso 1 1 calc R . .
H41B H 0.1838 0.1579 0.1759 0.054 Uiso 1 1 calc R . .
H41C H 0.1167 0.1515 0.1479 0.054 Uiso 1 1 calc R . .
C42 C 0.12893(8) 0.2222(3) 0.25790(10) 0.0249(4) Uani 1 1 d . . .
C43 C 0.17826(8) 0.1680(3) 0.31612(9) 0.0229(4) Uani 1 1 d . . .
H43A H 0.1870 0.0177 0.3105 0.027 Uiso 1 1 calc R . .
H43B H 0.2131 0.2454 0.3031 0.027 Uiso 1 1 calc R . .
C44 C 0.17230(7) 0.2061(3) 0.39760(10) 0.0204(4) Uani 1 1 d . . .
C46 C 0.12574(9) 0.4577(4) 0.24255(12) 0.0322(5) Uani 1 1 d . . .
H46A H 0.0985 0.4837 0.2005 0.048 Uiso 1 1 calc R . .
H46B H 0.1643 0.5093 0.2325 0.048 Uiso 1 1 calc R . .
H46C H 0.1124 0.5306 0.2849 0.048 Uiso 1 1 calc R . .
C47 C 0.06898(9) 0.1423(4) 0.27606(12) 0.0326(5) Uani 1 1 d . . .
H47A H 0.0562 0.2189 0.3179 0.049 Uiso 1 1 calc R . .
H47B H 0.0714 -0.0070 0.2875 0.049 Uiso 1 1 calc R . .
H47C H 0.0411 0.1639 0.2343 0.049 Uiso 1 1 calc R . .
C48 C 0.13427(9) 0.0440(4) 0.43182(11) 0.0289(4) Uani 1 1 d . . .
H48A H 0.1488 -0.0963 0.4222 0.043 Uiso 1 1 calc R . .
H48B H 0.0942 0.0571 0.4110 0.043 Uiso 1 1 calc R . .
H48C H 0.1353 0.0671 0.4843 0.043 Uiso 1 1 calc R . .
C49 C 0.15417(9) 0.4263(3) 0.41706(11) 0.0277(4) Uani 1 1 d . . .
H49A H 0.1564 0.4417 0.4699 0.041 Uiso 1 1 calc R . .
H49B H 0.1142 0.4515 0.3976 0.041 Uiso 1 1 calc R . .
H49C H 0.1802 0.5274 0.3963 0.041 Uiso 1 1 calc R . .
N45 N 0.23307(6) 0.1759(3) 0.43304(8) 0.0203(3) Uani 1 1 d . . .
H45A H 0.2462 0.0465 0.4221 0.020(5) Uiso 1 1 calc R . .
H45B H 0.2322 0.1886 0.4820 0.044(7) Uiso 1 1 calc R . .
H45C H 0.2572 0.2744 0.4163 0.033(6) Uiso 1 1 calc R . .
 
 
_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 O1B 1.242(3) . ?
C1 O1A 1.277(2) . ?
C1 C2 1.518(3) . ?
C2 C3 1.529(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.538(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.513(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O5A 1.259(2) . ?
C5 O5B 1.266(3) . ?
C21 C22 1.543(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C27 1.522(3) . ?
C22 C26 1.528(3) . ?
C22 C23 1.552(3) . ?
C23 C24 1.547(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N25 1.516(2) . ?
C24 C28 1.523(3) . ?
C24 C29 1.526(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
N25 H25A 0.7700 . ?
N25 H25B 0.9255 . ?
N25 H25C 0.9983 . ?
C31 O31A 1.217(3) . ?
C31 O31B 1.310(3) . ?
C31 C32 1.494(3) . ?
C32 C33 1.528(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C32 1.528(3) 2_556 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O31B H31 0.8400 . ?
C41 C42 1.542(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C47 1.535(3) . ?
C42 C46 1.536(3) . ?
C42 C43 1.551(3) . ?
C43 C44 1.542(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N45 1.519(2) . ?
C44 C49 1.521(3) . ?
C44 C48 1.525(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
N45 H45A 0.9100 . ?
N45 H45B 0.9100 . ?
N45 H45C 0.9100 . ?
 
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
O1B C1 O1A 124.07(17) . . ?
O1B C1 C2 117.79(17) . . ?
O1A C1 C2 118.15(18) . . ?
C1 C2 C3 111.31(16) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C2 C3 C4 111.86(16) . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C3 111.19(16) . . ?
C5 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O5A C5 O5B 123.06(18) . . ?
O5A C5 C4 119.78(19) . . ?
O5B C5 C4 117.15(17) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C27 C22 C26 109.86(18) . . ?
C27 C22 C21 107.93(19) . . ?
C26 C22 C21 107.65(18) . . ?
C27 C22 C23 111.59(17) . . ?
C26 C22 C23 113.53(17) . . ?
C21 C22 C23 105.99(15) . . ?
C24 C23 C22 123.55(15) . . ?
C24 C23 H23A 106.4 . . ?
C22 C23 H23A 106.4 . . ?
C24 C23 H23B 106.4 . . ?
C22 C23 H23B 106.4 . . ?
H23A C23 H23B 106.5 . . ?
N25 C24 C28 106.44(15) . . ?
N25 C24 C29 105.87(15) . . ?
C28 C24 C29 110.82(16) . . ?
N25 C24 C23 103.77(14) . . ?
C28 C24 C23 115.38(16) . . ?
C29 C24 C23 113.57(16) . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C29 H29A 109.5 . . ?
C24 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C24 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C24 N25 H25A 109.5 . . ?
C24 N25 H25B 115.0 . . ?
H25A N25 H25B 110.2 . . ?
C24 N25 H25C 112.9 . . ?
H25A N25 H25C 103.3 . . ?
H25B N25 H25C 105.3 . . ?
O31A C31 O31B 123.5(2) . . ?
O31A C31 C32 123.8(2) . . ?
O31B C31 C32 112.7(2) . . ?
C31 C32 C33 116.50(18) . . ?
C31 C32 H32A 108.2 . . ?
C33 C32 H32A 108.2 . . ?
C31 C32 H32B 108.2 . . ?
C33 C32 H32B 108.2 . . ?
H32A C32 H32B 107.3 . . ?
C32 C33 C32 113.3(3) . 2_556 ?
C32 C33 H33A 108.9 . . ?
C32 C33 H33A 108.9 2_556 . ?
C32 C33 H33B 108.9 . . ?
C32 C33 H33B 108.9 2_556 . ?
H33A C33 H33B 107.7 . . ?
C31 O31B H31 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C46 109.60(18) . . ?
C47 C42 C41 107.91(17) . . ?
C46 C42 C41 107.40(18) . . ?
C47 C42 C43 113.77(16) . . ?
C46 C42 C43 111.80(17) . . ?
C41 C42 C43 106.02(16) . . ?
C44 C43 C42 122.11(15) . . ?
C44 C43 H43A 106.8 . . ?
C42 C43 H43A 106.8 . . ?
C44 C43 H43B 106.8 . . ?
C42 C43 H43B 106.8 . . ?
H43A C43 H43B 106.7 . . ?
N45 C44 C49 106.10(15) . . ?
N45 C44 C48 105.99(15) . . ?
C49 C44 C48 110.88(17) . . ?
N45 C44 C43 104.98(14) . . ?
C49 C44 C43 115.01(16) . . ?
C48 C44 C43 113.03(16) . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C44 C48 H48A 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C44 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C49 H49A 109.5 . . ?
C44 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C44 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 N45 H45A 109.5 . . ?
C44 N45 H45B 109.5 . . ?
H45A N45 H45B 109.5 . . ?
C44 N45 H45C 109.5 . . ?
H45A N45 H45C 109.5 . . ?
H45B N45 H45C 109.5 . . ?
 
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
N25 H25C O1B  1.00 1.73 2.725(2) 172.8 .
N45 H45C O5B  0.91 1.87 2.774(2) 174.6 .
N25 H25A O1A  0.77 2.03 2.784(2) 168.2 1_545
N45 H45A O5A  0.91 1.90 2.799(2) 169.6 1_545
N25 H25B O1A  0.93 1.87 2.777(2) 167.1 4_545
O31B H31 O5B  0.84 1.86 2.676(2) 162.9 3_445
N45 H45B O5A  0.91 1.94 2.836(2) 169.7 4_546
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              26.66
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    0.527
_refine_diff_density_min   -0.209
_refine_diff_density_rms    0.043
