 
data_06skc0065p21n
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Glutaric Acid & TEMED
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C16 H32 N2 O8'
_chemical_formula_weight          380.44
 
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/n
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    17.308(2)
_cell_length_b                    9.0088(14)
_cell_length_c                    18.932(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  105.305(7)
_cell_angle_gamma                 90.00
_cell_volume                      2847.2(7)
_cell_formula_units_Z             6
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6289
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.18
_exptl_crystal_size_mid           0.11
_exptl_crystal_size_min           0.07
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.331
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1236
_exptl_absorpt_coefficient_mu     0.106
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9812
_exptl_absorpt_correction_T_max   0.9926
_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             51188
_diffrn_reflns_av_R_equivalents   0.3562
_diffrn_reflns_av_sigmaI/netI     0.3075
_diffrn_reflns_limit_h_min        -22
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -24
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          2.93
_diffrn_reflns_theta_max          27.48
_reflns_number_total              6444
_reflns_number_gt                 1866
_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.
;
 
_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)+(0.2000P)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     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          6444
_refine_ls_number_parameters      363
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.3760
_refine_ls_R_factor_gt            0.1472
_refine_ls_wR_factor_ref          0.4538
_refine_ls_wR_factor_gt           0.3334
_refine_ls_goodness_of_fit_ref    1.014
_refine_ls_restrained_S_all       1.014
_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 0.1754(5) 0.0411(9) 0.1583(4) 0.043(2) Uani 1 1 d . . .
C2 C 0.2511(5) -0.0342(10) 0.1961(5) 0.058(3) Uani 1 1 d . . .
H2A H 0.2651 -0.1035 0.1609 0.069 Uiso 1 1 calc R . .
H2B H 0.2938 0.0421 0.2084 0.069 Uiso 1 1 calc R . .
C3 C 0.2533(6) -0.1159(10) 0.2619(5) 0.072(3) Uani 1 1 d . . .
H3A H 0.3038 -0.1734 0.2761 0.087 Uiso 1 1 calc R . .
H3B H 0.2083 -0.1874 0.2517 0.087 Uiso 1 1 calc R . .
C4 C 0.2478(5) -0.0163(10) 0.3261(5) 0.061(3) Uani 1 1 d . . .
H4A H 0.2033 0.0545 0.3080 0.073 Uiso 1 1 calc R . .
H4B H 0.2332 -0.0796 0.3633 0.073 Uiso 1 1 calc R . .
C5 C 0.3198(6) 0.0698(11) 0.3630(5) 0.061(3) Uani 1 1 d . . .
O1A O 0.1115(3) 0.0224(6) 0.1764(3) 0.0476(15) Uani 1 1 d . . .
O1B O 0.1782(3) 0.1303(6) 0.1056(3) 0.0568(17) Uani 1 1 d . . .
O5A O 0.3837(3) 0.0593(7) 0.3479(4) 0.074(2) Uani 1 1 d . . .
O5B O 0.3143(3) 0.1638(7) 0.4190(3) 0.0619(17) Uani 1 1 d . . .
H5 H 0.2678 0.1595 0.4247 0.093 Uiso 1 1 calc R . .
C21 C 0.4629(5) -0.2210(9) 0.5261(5) 0.065(3) Uani 1 1 d . . .
H21A H 0.4404 -0.2881 0.5563 0.097 Uiso 1 1 calc R . .
H21B H 0.4252 -0.1399 0.5079 0.097 Uiso 1 1 calc R . .
H21C H 0.5137 -0.1801 0.5556 0.097 Uiso 1 1 calc R . .
C23 C 0.5246(4) -0.4433(8) 0.4863(4) 0.0376(19) Uani 1 1 d . . .
H23A H 0.5732 -0.4194 0.5258 0.045 Uiso 1 1 calc R . .
H23B H 0.5418 -0.4851 0.4446 0.045 Uiso 1 1 calc R . .
C24 C 0.5183(4) -0.2085(8) 0.4183(4) 0.048(2) Uani 1 1 d . . .
H24A H 0.5292 -0.2671 0.3784 0.071 Uiso 1 1 calc R . .
H24B H 0.5688 -0.1709 0.4499 0.071 Uiso 1 1 calc R . .
H24C H 0.4833 -0.1248 0.3978 0.071 Uiso 1 1 calc R . .
N22 N 0.4774(4) -0.3050(7) 0.4627(4) 0.0472(18) Uani 1 1 d . . .
H22 H 0.4278 -0.3325 0.4325 0.09(3) Uiso 1 1 calc R . .
C31 C 0.8322(5) 1.0006(11) 0.1685(5) 0.054(2) Uani 1 1 d . . .
C32 C 0.7757(5) 1.1215(10) 0.1296(5) 0.058(3) Uani 1 1 d . . .
H32A H 0.7561 1.1787 0.1660 0.069 Uiso 1 1 calc R . .
H32B H 0.8052 1.1905 0.1054 0.069 Uiso 1 1 calc R . .
C33 C 0.7060(5) 1.0580(10) 0.0736(4) 0.057(3) Uani 1 1 d . . .
H33A H 0.6658 1.1370 0.0557 0.069 Uiso 1 1 calc R . .
H33B H 0.6805 0.9798 0.0966 0.069 Uiso 1 1 calc R . .
C34 C 0.7313(4) 0.9921(9) 0.0092(4) 0.047(2) Uani 1 1 d . . .
H34A H 0.7468 1.0734 -0.0195 0.056 Uiso 1 1 calc R . .
H34B H 0.7788 0.9282 0.0279 0.056 Uiso 1 1 calc R . .
C35 C 0.6650(5) 0.9009(10) -0.0408(5) 0.056(2) Uani 1 1 d . . .
O31A O 0.9012(3) 1.0013(7) 0.1598(3) 0.0673(18) Uani 1 1 d . . .
O31B O 0.8129(3) 0.9081(7) 0.2103(3) 0.0589(17) Uani 1 1 d . . .
O35A O 0.6847(3) 0.8227(8) -0.0910(3) 0.0640(18) Uani 1 1 d . . .
H35 H 0.7333 0.8365 -0.0887 0.096 Uiso 1 1 calc R . .
O35B O 0.5971(3) 0.9047(7) -0.0345(3) 0.0629(18) Uani 1 1 d . . .
C41 C 0.5154(4) 0.7885(9) 0.0787(4) 0.046(2) Uani 1 1 d . . .
H41A H 0.5685 0.8191 0.1083 0.070 Uiso 1 1 calc R . .
H41B H 0.4834 0.8767 0.0600 0.070 Uiso 1 1 calc R . .
H41C H 0.5214 0.7277 0.0375 0.070 Uiso 1 1 calc R . .
C43 C 0.5206(4) 0.5609(8) 0.1509(4) 0.0379(19) Uani 1 1 d . . .
H43A H 0.5372 0.5147 0.1098 0.045 Uiso 1 1 calc R . .
H43B H 0.5697 0.5861 0.1895 0.045 Uiso 1 1 calc R . .
C44 C 0.4721(4) 0.4520(9) 0.1808(4) 0.044(2) Uani 1 1 d . . .
H44A H 0.4503 0.5014 0.2181 0.053 Uiso 1 1 calc R . .
H44B H 0.4264 0.4174 0.1408 0.053 Uiso 1 1 calc R . .
C46 C 0.4763(5) 0.2294(9) 0.2535(5) 0.055(2) Uani 1 1 d . . .
H46A H 0.5102 0.1463 0.2766 0.082 Uiso 1 1 calc R . .
H46B H 0.4280 0.1909 0.2189 0.082 Uiso 1 1 calc R . .
H46C H 0.4612 0.2884 0.2912 0.082 Uiso 1 1 calc R . .
C47 C 0.4623(5) 0.7897(9) 0.1872(4) 0.051(2) Uani 1 1 d . . .
H47A H 0.5143 0.8199 0.2189 0.076 Uiso 1 1 calc R . .
H47B H 0.4339 0.7294 0.2154 0.076 Uiso 1 1 calc R . .
H47C H 0.4305 0.8781 0.1685 0.076 Uiso 1 1 calc R . .
C48 C 0.5538(5) 0.2367(9) 0.1635(5) 0.054(2) Uani 1 1 d . . .
H48A H 0.5099 0.1986 0.1238 0.081 Uiso 1 1 calc R . .
H48B H 0.5849 0.1534 0.1899 0.081 Uiso 1 1 calc R . .
H48C H 0.5886 0.2998 0.1430 0.081 Uiso 1 1 calc R . .
N42 N 0.4747(3) 0.7007(7) 0.1245(3) 0.0382(17) Uani 1 1 d . . .
H42 H 0.4245 0.6735 0.0954 0.12(4) Uiso 1 1 calc R . .
N45 N 0.5211(3) 0.3237(7) 0.2140(3) 0.0385(16) Uani 1 1 d . . .
H45 H 0.5647 0.3617 0.2491 0.05(2) Uiso 1 1 calc R . .
C51 C 0.3260(5) 0.5491(10) 0.0023(5) 0.049(2) Uani 1 1 d . . .
C52 C 0.2453(5) 0.4700(10) -0.0350(5) 0.053(2) Uani 1 1 d . . .
H52A H 0.2284 0.4116 0.0027 0.064 Uiso 1 1 calc R . .
H52B H 0.2040 0.5470 -0.0532 0.064 Uiso 1 1 calc R . .
C53 C 0.2471(5) 0.3721(10) -0.0953(5) 0.056(2) Uani 1 1 d . . .
H53A H 0.1984 0.3095 -0.1062 0.067 Uiso 1 1 calc R . .
H53B H 0.2939 0.3054 -0.0795 0.067 Uiso 1 1 calc R . .
C54 C 0.2515(4) 0.4491(10) -0.1649(4) 0.049(2) Uani 1 1 d . . .
H54A H 0.2630 0.3743 -0.1991 0.059 Uiso 1 1 calc R . .
H54B H 0.2967 0.5203 -0.1533 0.059 Uiso 1 1 calc R . .
C55 C 0.1744(5) 0.5326(10) -0.2033(4) 0.049(2) Uani 1 1 d . . .
O51A O 0.3211(3) 0.6411(6) 0.0533(3) 0.0467(15) Uani 1 1 d . . .
O51B O 0.3850(3) 0.5308(6) -0.0179(3) 0.0543(16) Uani 1 1 d . . .
O55A O 0.1767(3) 0.6024(7) -0.2643(3) 0.0642(18) Uani 1 1 d . . .
H55 H 0.2220 0.5909 -0.2719 0.096 Uiso 1 1 calc R . .
O55B O 0.1153(3) 0.5303(7) -0.1828(3) 0.0629(18) Uani 1 1 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 1.253(9) . ?
C1 O1B 1.291(9) . ?
C1 C2 1.481(10) . ?
C2 C3 1.437(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.534(12) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.477(13) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 O5A 1.217(9) . ?
C5 O5B 1.379(11) . ?
O5B H5 0.8400 . ?
C21 N22 1.495(10) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C23 N22 1.492(9) . ?
C23 C23 1.506(13) 3_646 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 N22 1.508(9) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N22 H22 0.9300 . ?
C31 O31A 1.249(9) . ?
C31 O31B 1.254(10) . ?
C31 C32 1.518(12) . ?
C32 C33 1.494(11) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.522(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.521(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O35B 1.213(9) . ?
C35 O35A 1.300(9) . ?
O35A H35 0.8400 . ?
C41 N42 1.484(8) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C43 C44 1.497(10) . ?
C43 N42 1.502(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N45 1.473(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C46 N45 1.479(9) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 N42 1.494(9) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 N45 1.460(9) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N42 H42 0.9300 . ?
N45 H45 0.9300 . ?
C51 O51B 1.192(8) . ?
C51 O51A 1.292(9) . ?
C51 C52 1.562(11) . ?
C52 C53 1.449(11) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.509(11) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.537(11) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 O55B 1.186(8) . ?
C55 O55A 1.326(9) . ?
O55A H55 0.8400 . ?
 
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 120.7(7) . . ?
O1A C1 C2 122.5(8) . . ?
O1B C1 C2 116.8(8) . . ?
C3 C2 C1 118.1(8) . . ?
C3 C2 H2A 107.8 . . ?
C1 C2 H2A 107.8 . . ?
C3 C2 H2B 107.8 . . ?
C1 C2 H2B 107.8 . . ?
H2A C2 H2B 107.1 . . ?
C2 C3 C4 113.2(7) . . ?
C2 C3 H3A 108.9 . . ?
C4 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
C4 C3 H3B 108.9 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 117.4(8) . . ?
C5 C4 H4A 107.9 . . ?
C3 C4 H4A 107.9 . . ?
C5 C4 H4B 107.9 . . ?
C3 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
O5A C5 O5B 118.7(10) . . ?
O5A C5 C4 123.6(9) . . ?
O5B C5 C4 117.7(7) . . ?
C5 O5B H5 109.5 . . ?
N22 C21 H21A 109.5 . . ?
N22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N22 C23 C23 110.8(7) . 3_646 ?
N22 C23 H23A 109.5 . . ?
C23 C23 H23A 109.5 3_646 . ?
N22 C23 H23B 109.5 . . ?
C23 C23 H23B 109.5 3_646 . ?
H23A C23 H23B 108.1 . . ?
N22 C24 H24A 109.5 . . ?
N22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 N22 C21 112.1(6) . . ?
C23 N22 C24 110.4(5) . . ?
C21 N22 C24 111.0(6) . . ?
C23 N22 H22 107.7 . . ?
C21 N22 H22 107.7 . . ?
C24 N22 H22 107.7 . . ?
O31A C31 O31B 120.7(8) . . ?
O31A C31 C32 116.6(9) . . ?
O31B C31 C32 122.6(8) . . ?
C33 C32 C31 111.4(7) . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C32 C33 C34 111.6(7) . . ?
C32 C33 H33A 109.3 . . ?
C34 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
C34 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
C35 C34 C33 112.3(7) . . ?
C35 C34 H34A 109.1 . . ?
C33 C34 H34A 109.1 . . ?
C35 C34 H34B 109.1 . . ?
C33 C34 H34B 109.1 . . ?
H34A C34 H34B 107.9 . . ?
O35B C35 O35A 122.3(8) . . ?
O35B C35 C34 121.1(8) . . ?
O35A C35 C34 116.6(7) . . ?
C35 O35A H35 109.5 . . ?
N42 C41 H41A 109.5 . . ?
N42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C44 C43 N42 112.0(6) . . ?
C44 C43 H43A 109.2 . . ?
N42 C43 H43A 109.2 . . ?
C44 C43 H43B 109.2 . . ?
N42 C43 H43B 109.2 . . ?
H43A C43 H43B 107.9 . . ?
N45 C44 C43 111.0(6) . . ?
N45 C44 H44A 109.4 . . ?
C43 C44 H44A 109.4 . . ?
N45 C44 H44B 109.4 . . ?
C43 C44 H44B 109.4 . . ?
H44A C44 H44B 108.0 . . ?
N45 C46 H46A 109.5 . . ?
N45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N42 C47 H47A 109.5 . . ?
N42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N45 C48 H48A 109.5 . . ?
N45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C41 N42 C47 111.6(6) . . ?
C41 N42 C43 110.5(5) . . ?
C47 N42 C43 111.1(6) . . ?
C41 N42 H42 107.8 . . ?
C47 N42 H42 107.8 . . ?
C43 N42 H42 107.8 . . ?
C48 N45 C44 114.9(6) . . ?
C48 N45 C46 111.6(6) . . ?
C44 N45 C46 110.3(6) . . ?
C48 N45 H45 106.5 . . ?
C44 N45 H45 106.5 . . ?
C46 N45 H45 106.5 . . ?
O51B C51 O51A 124.0(8) . . ?
O51B C51 C52 122.1(8) . . ?
O51A C51 C52 113.8(7) . . ?
C53 C52 C51 115.5(7) . . ?
C53 C52 H52A 108.4 . . ?
C51 C52 H52A 108.4 . . ?
C53 C52 H52B 108.4 . . ?
C51 C52 H52B 108.4 . . ?
H52A C52 H52B 107.5 . . ?
C52 C53 C54 115.2(8) . . ?
C52 C53 H53A 108.5 . . ?
C54 C53 H53A 108.5 . . ?
C52 C53 H53B 108.5 . . ?
C54 C53 H53B 108.5 . . ?
H53A C53 H53B 107.5 . . ?
C53 C54 C55 113.5(6) . . ?
C53 C54 H54A 108.9 . . ?
C55 C54 H54A 108.9 . . ?
C53 C54 H54B 108.9 . . ?
C55 C54 H54B 108.9 . . ?
H54A C54 H54B 107.7 . . ?
O55B C55 O55A 121.3(8) . . ?
O55B C55 C54 123.6(8) . . ?
O55A C55 C54 115.0(6) . . ?
C55 O55A H55 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
N42 H42 O51A  0.93 1.78 2.697(8) 168.2 .
N42 H42 O51B  0.93 2.44 3.133(8) 131.5 .
O5B H5 O51A  0.84 1.71 2.542(7) 172.8 2_545
N22 H22 O1B  0.93 1.82 2.725(9) 164.7 2_545
N22 H22 O1A  0.93 2.38 3.095(8) 133.1 2_545
O35A H35 O1B  0.84 1.67 2.498(7) 166.2 3_665
N45 H45 O31A  0.93 2.09 2.895(8) 144.2 2_645
N45 H45 O31B  0.93 2.10 2.953(8) 152.4 2_645
O55A H55 O31B  0.84 1.69 2.528(8) 172.4 4_575
 
_diffrn_measured_fraction_theta_max    0.985
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.985
_refine_diff_density_max    0.583
_refine_diff_density_min   -0.387
_refine_diff_density_rms    0.084
