 
data_ssf1328
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
maleic acid and 1,1,3,3-tetramethylbutylamine
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C13 H25 N O4'
_chemical_formula_weight          259.34
 
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            monoclinic
_symmetry_space_group_name_H-M    P21/c
 
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                    6.6154(15)
_cell_length_b                    30.477(7)
_cell_length_c                    15.282(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.924(2)
_cell_angle_gamma                 90.00
_cell_volume                      3080.7(12)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     924
_cell_measurement_theta_min       2.60
_cell_measurement_theta_max       19.23
 
_exptl_crystal_description        lath
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.118
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1136
_exptl_absorpt_coefficient_mu     0.082
_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      0.6905
_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             19088
_diffrn_reflns_av_R_equivalents   0.1059
_diffrn_reflns_av_sigmaI/netI     0.0846
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -33
_diffrn_reflns_limit_k_max        33
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          2.90
_diffrn_reflns_theta_max          22.54
_reflns_number_total              4405
_reflns_number_gt                 2532
_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)+(0.0645P)²+0.0000P] 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      SHELXL
_refine_ls_extinction_coef        0.028(2)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          4405
_refine_ls_number_parameters      346
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1103
_refine_ls_R_factor_gt            0.0498
_refine_ls_wR_factor_ref          0.1323
_refine_ls_wR_factor_gt           0.1073
_refine_ls_goodness_of_fit_ref    0.971
_refine_ls_restrained_S_all       0.971
_refine_ls_shift/su_max           0.000
_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 0.7271(5) 0.20612(10) 0.98248(19) 0.0337(8) Uani 1 1 d . . .
C2 C 0.6135(4) 0.18288(11) 1.05199(19) 0.0386(8) Uani 1 1 d . . .
H2 H 0.5485 0.2012 1.0933 0.046 Uiso 1 1 calc R . .
C3 C 0.5908(4) 0.13980(11) 1.0640(2) 0.0390(8) Uani 1 1 d . . .
H3 H 0.5141 0.1304 1.1125 0.047 Uiso 1 1 calc R . .
C4 C 0.6758(5) 0.10647(11) 1.0077(2) 0.0387(8) Uani 1 1 d . . .
C5 C 0.7392(5) 0.03030(12) 0.9956(2) 0.0604(11) Uani 1 1 d . . .
H5A H 0.6651 0.0260 0.9402 0.091 Uiso 1 1 calc R . .
H5B H 0.7317 0.0035 1.0308 0.091 Uiso 1 1 calc R . .
H5C H 0.8810 0.0370 0.9836 0.091 Uiso 1 1 calc R . .
O1A O 0.6204(3) 0.22459(7) 0.92304(12) 0.0385(6) Uani 1 1 d . . .
O1B O 0.9145(3) 0.20892(7) 0.99116(12) 0.0382(6) Uani 1 1 d . . .
O4A O 0.6510(3) 0.06614(7) 1.04279(14) 0.0457(6) Uani 1 1 d . . .
O4B O 0.7609(3) 0.11234(7) 0.93875(14) 0.0457(6) Uani 1 1 d . . .
C21 C 0.1029(5) 0.10076(11) 0.7087(2) 0.0526(10) Uani 1 1 d . . .
H21A H 0.1220 0.1232 0.6636 0.079 Uiso 1 1 calc R . .
H21B H -0.0332 0.1034 0.7326 0.079 Uiso 1 1 calc R . .
H21C H 0.1191 0.0716 0.6828 0.079 Uiso 1 1 calc R . .
C22 C 0.2598(5) 0.10713(10) 0.78203(19) 0.0372(8) Uani 1 1 d . . .
C23 C 0.2274(4) 0.14939(10) 0.83593(18) 0.0338(8) Uani 1 1 d . . .
H23A H 0.1103 0.1438 0.8739 0.041 Uiso 1 1 calc R . .
H23B H 0.3469 0.1525 0.8753 0.041 Uiso 1 1 calc R . .
C24 C 0.1923(4) 0.19433(10) 0.79344(18) 0.0332(8) Uani 1 1 d . . .
C26 C 0.4724(5) 0.10464(12) 0.7439(2) 0.0523(10) Uani 1 1 d . . .
H26A H 0.4907 0.0761 0.7155 0.078 Uiso 1 1 calc R . .
H26B H 0.5733 0.1081 0.7910 0.078 Uiso 1 1 calc R . .
H26C H 0.4889 0.1281 0.7007 0.078 Uiso 1 1 calc R . .
C27 C 0.2394(5) 0.06880(11) 0.8472(2) 0.0476(9) Uani 1 1 d . . .
H27A H 0.1039 0.0692 0.8722 0.071 Uiso 1 1 calc R . .
H27B H 0.3409 0.0719 0.8941 0.071 Uiso 1 1 calc R . .
H27C H 0.2602 0.0410 0.8165 0.071 Uiso 1 1 calc R . .
C28 C 0.3499(5) 0.20774(11) 0.72661(19) 0.0416(8) Uani 1 1 d . . .
H28A H 0.4855 0.2043 0.7524 0.062 Uiso 1 1 calc R . .
H28B H 0.3286 0.2385 0.7099 0.062 Uiso 1 1 calc R . .
H28C H 0.3366 0.1891 0.6746 0.062 Uiso 1 1 calc R . .
C29 C -0.0212(5) 0.20071(11) 0.7560(2) 0.0422(9) Uani 1 1 d . . .
H29A H -0.0409 0.2316 0.7400 0.063 Uiso 1 1 calc R . .
H29B H -0.1202 0.1923 0.8000 0.063 Uiso 1 1 calc R . .
H29C H -0.0396 0.1823 0.7039 0.063 Uiso 1 1 calc R . .
N25 N 0.2116(4) 0.22657(8) 0.86838(15) 0.0338(7) Uani 1 1 d . . .
H25A H 0.3375 0.2245 0.8929 0.065(11) Uiso 1 1 calc R . .
H25B H 0.1175 0.2203 0.9093 0.051(10) Uiso 1 1 calc R . .
H25C H 0.1913 0.2543 0.8480 0.041(9) Uiso 1 1 calc R . .
C31 C 1.2085(5) 0.17435(10) 1.2415(2) 0.0349(8) Uani 1 1 d . . .
C32 C 1.1015(4) 0.15176(11) 1.16763(19) 0.0386(8) Uani 1 1 d . . .
H32 H 1.0361 0.1700 1.1255 0.046 Uiso 1 1 calc R . .
C33 C 1.0878(5) 0.10873(12) 1.1546(2) 0.0448(9) Uani 1 1 d . . .
H33 H 1.0173 0.0987 1.1037 0.054 Uiso 1 1 calc R . .
C34 C 1.1745(5) 0.07611(11) 1.2136(2) 0.0409(9) Uani 1 1 d . . .
C35 C 1.2302(5) 0.00044(11) 1.2362(2) 0.0598(11) Uani 1 1 d . . .
H35A H 1.3780 0.0017 1.2337 0.090 Uiso 1 1 calc R . .
H35B H 1.1831 -0.0280 1.2142 0.090 Uiso 1 1 calc R . .
H35C H 1.1880 0.0042 1.2969 0.090 Uiso 1 1 calc R . .
O31A O 1.1012(3) 0.19026(7) 1.30139(13) 0.0381(6) Uani 1 1 d . . .
O31B O 1.3952(3) 0.17892(7) 1.23579(12) 0.0374(6) Uani 1 1 d . . .
O34A O 1.2641(3) 0.08358(7) 1.28146(14) 0.0480(6) Uani 1 1 d . . .
O34B O 1.1442(3) 0.03503(8) 1.18295(14) 0.0516(7) Uani 1 1 d . . .
C41 C 0.7354(5) 0.03387(11) 1.3676(2) 0.0503(9) Uani 1 1 d . . .
H41A H 0.7735 0.0058 1.3944 0.075 Uiso 1 1 calc R . .
H41B H 0.8211 0.0394 1.3170 0.075 Uiso 1 1 calc R . .
H41C H 0.5935 0.0327 1.3484 0.075 Uiso 1 1 calc R . .
C42 C 0.7640(5) 0.07093(10) 1.43483(19) 0.0380(8) Uani 1 1 d . . .
C43 C 0.7228(4) 0.11402(10) 1.38462(18) 0.0349(8) Uani 1 1 d . . .
H43A H 0.8369 0.1180 1.3442 0.042 Uiso 1 1 calc R . .
H43B H 0.6010 0.1089 1.3476 0.042 Uiso 1 1 calc R . .
C44 C 0.6913(4) 0.15838(10) 1.43039(18) 0.0322(8) Uani 1 1 d . . .
C46 C 0.6206(6) 0.06265(12) 1.5096(2) 0.0591(11) Uani 1 1 d . . .
H46A H 0.6421 0.0330 1.5325 0.089 Uiso 1 1 calc R . .
H46B H 0.4807 0.0656 1.4884 0.089 Uiso 1 1 calc R . .
H46C H 0.6465 0.0841 1.5563 0.089 Uiso 1 1 calc R . .
C47 C 0.9840(5) 0.06833(11) 1.4694(2) 0.0507(10) Uani 1 1 d . . .
H47A H 1.0046 0.0900 1.5160 0.076 Uiso 1 1 calc R . .
H47B H 1.0768 0.0744 1.4215 0.076 Uiso 1 1 calc R . .
H47C H 1.0105 0.0389 1.4926 0.076 Uiso 1 1 calc R . .
C48 C 0.8557(5) 0.17070(11) 1.49759(19) 0.0429(9) Uani 1 1 d . . .
H48A H 0.9889 0.1675 1.4712 0.064 Uiso 1 1 calc R . .
H48B H 0.8466 0.1513 1.5485 0.064 Uiso 1 1 calc R . .
H48C H 0.8368 0.2012 1.5161 0.064 Uiso 1 1 calc R . .
C49 C 0.4803(5) 0.16370(11) 1.4688(2) 0.0427(9) Uani 1 1 d . . .
H49A H 0.4603 0.1943 1.4863 0.064 Uiso 1 1 calc R . .
H49B H 0.4677 0.1446 1.5201 0.064 Uiso 1 1 calc R . .
H49C H 0.3779 0.1556 1.4247 0.064 Uiso 1 1 calc R . .
N45 N 0.7033(4) 0.19173(8) 1.35783(15) 0.0339(7) Uani 1 1 d . . .
H45A H 0.8245 0.1893 1.3310 0.033(9) Uiso 1 1 calc R . .
H45B H 0.6909 0.2192 1.3805 0.044(10) Uiso 1 1 calc R . .
H45C H 0.6017 0.1869 1.3182 0.050(10) 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 1.247(3) . ?
C1 O1A 1.273(3) . ?
C1 C2 1.490(4) . ?
C2 C3 1.334(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.451(5) . ?
C3 H3 0.9500 . ?
C4 O4B 1.215(4) . ?
C4 O4A 1.352(4) . ?
C5 O4A 1.438(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C21 C22 1.528(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C26 1.533(4) . ?
C22 C27 1.542(4) . ?
C22 C23 1.546(4) . ?
C23 C24 1.532(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N25 1.513(4) . ?
C24 C28 1.527(4) . ?
C24 C29 1.528(4) . ?
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 0.9100 . ?
N25 H25B 0.9100 . ?
N25 H25C 0.9100 . ?
C31 O31B 1.247(3) . ?
C31 O31A 1.265(4) . ?
C31 C32 1.491(4) . ?
C32 C33 1.329(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.454(4) . ?
C33 H33 0.9500 . ?
C34 O34A 1.208(3) . ?
C34 O34B 1.350(4) . ?
C35 O34B 1.443(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C41 C42 1.537(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C46 1.518(4) . ?
C42 C47 1.542(4) . ?
C42 C43 1.543(4) . ?
C43 C44 1.538(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N45 1.507(4) . ?
C44 C48 1.530(4) . ?
C44 C49 1.532(4) . ?
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 125.8(3) . . ?
O1B C1 C2 117.9(3) . . ?
O1A C1 C2 116.0(3) . . ?
C3 C2 C1 128.7(3) . . ?
C3 C2 H2 115.7 . . ?
C1 C2 H2 115.7 . . ?
C2 C3 C4 124.2(3) . . ?
C2 C3 H3 117.9 . . ?
C4 C3 H3 117.9 . . ?
O4B C4 O4A 122.6(3) . . ?
O4B C4 C3 126.9(3) . . ?
O4A C4 C3 110.5(3) . . ?
O4A C5 H5A 109.5 . . ?
O4A C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O4A C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 O4A C5 116.0(3) . . ?
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 . . ?
C21 C22 C26 109.3(3) . . ?
C21 C22 C27 108.2(3) . . ?
C26 C22 C27 107.4(3) . . ?
C21 C22 C23 113.5(3) . . ?
C26 C22 C23 112.3(3) . . ?
C27 C22 C23 105.8(2) . . ?
C24 C23 C22 122.7(2) . . ?
C24 C23 H23A 106.6 . . ?
C22 C23 H23A 106.6 . . ?
C24 C23 H23B 106.6 . . ?
C22 C23 H23B 106.6 . . ?
H23A C23 H23B 106.6 . . ?
N25 C24 C28 106.4(2) . . ?
N25 C24 C29 105.5(2) . . ?
C28 C24 C29 110.6(2) . . ?
N25 C24 C23 104.4(2) . . ?
C28 C24 C23 115.0(3) . . ?
C29 C24 C23 113.9(3) . . ?
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 109.5 . . ?
H25A N25 H25B 109.5 . . ?
C24 N25 H25C 109.5 . . ?
H25A N25 H25C 109.5 . . ?
H25B N25 H25C 109.5 . . ?
O31B C31 O31A 125.1(3) . . ?
O31B C31 C32 117.3(3) . . ?
O31A C31 C32 117.4(3) . . ?
C33 C32 C31 126.8(3) . . ?
C33 C32 H32 116.6 . . ?
C31 C32 H32 116.6 . . ?
C32 C33 C34 123.8(3) . . ?
C32 C33 H33 118.1 . . ?
C34 C33 H33 118.1 . . ?
O34A C34 O34B 122.7(3) . . ?
O34A C34 C33 125.9(3) . . ?
O34B C34 C33 111.3(3) . . ?
O34B C35 H35A 109.5 . . ?
O34B C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O34B C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 O34B C35 115.3(2) . . ?
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 . . ?
C46 C42 C41 108.0(3) . . ?
C46 C42 C47 109.3(3) . . ?
C41 C42 C47 107.2(3) . . ?
C46 C42 C43 114.1(3) . . ?
C41 C42 C43 105.9(2) . . ?
C47 C42 C43 111.9(3) . . ?
C44 C43 C42 123.1(2) . . ?
C44 C43 H43A 106.6 . . ?
C42 C43 H43A 106.6 . . ?
C44 C43 H43B 106.6 . . ?
C42 C43 H43B 106.6 . . ?
H43A C43 H43B 106.5 . . ?
N45 C44 C48 106.4(2) . . ?
N45 C44 C49 105.7(2) . . ?
C48 C44 C49 111.0(2) . . ?
N45 C44 C43 104.4(2) . . ?
C48 C44 C43 114.9(2) . . ?
C49 C44 C43 113.5(3) . . ?
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
N45 H45A O31A  0.91 1.89 2.783(3) 165.7 .
N25 H25A O1A  0.91 1.92 2.818(3) 168.7 .
N45 H45B O1A  0.91 1.89 2.795(3) 170.8 4_566
N45 H45C O31B  0.91 1.86 2.768(3) 178.0 1_455
N25 H25B O1B  0.91 1.88 2.791(3) 177.3 1_455
N25 H25C O31A  0.91 1.92 2.825(3) 170.1 4_465
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              22.54
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    0.190
_refine_diff_density_min   -0.183
_refine_diff_density_rms    0.045
