 
data_04skc0003p1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Tetrabutylammonium di(DL-tartrate) dihydrate
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C24 H51 N O14'
_chemical_formula_weight          577.66
 
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            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.3454(19)
_cell_length_b                    9.3736(19)
_cell_length_c                    17.624(4)
_cell_angle_alpha                 78.41(3)
_cell_angle_beta                  78.45(3)
_cell_angle_gamma                 89.86(3)
_cell_volume                      1480.5(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3411
_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           0.12
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.296
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              628
_exptl_absorpt_coefficient_mu     0.106
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9792
_exptl_absorpt_correction_T_max   0.9968
_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             12188
_diffrn_reflns_av_R_equivalents   0.1272
_diffrn_reflns_av_sigmaI/netI     0.2821
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        22
_diffrn_reflns_theta_min          2.93
_diffrn_reflns_theta_max          27.48
_reflns_number_total              5375
_reflns_number_gt                 2266
_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 transferable hydrogens have been positioned according to the electron
 density map, bond distance and hydrogen bonding contacts, however, their
 positions cannot be conclusively determined due to the poor data.
;
 
_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)+(0.1278P)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      SHELXL
_refine_ls_extinction_coef        0.039(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          5375
_refine_ls_number_parameters      382
_refine_ls_number_restraints      6
_refine_ls_R_factor_all           0.2391
_refine_ls_R_factor_gt            0.1106
_refine_ls_wR_factor_ref          0.2993
_refine_ls_wR_factor_gt           0.2479
_refine_ls_goodness_of_fit_ref    0.982
_refine_ls_restrained_S_all       0.981
_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 0.1627(7) 0.1766(6) -0.0116(3) 0.0221(13) Uani 1 1 d . . .
C2 C 0.3259(6) 0.2104(6) -0.0294(3) 0.0224(13) Uani 1 1 d . . .
H2 H 0.3460 0.3098 -0.0638 0.027 Uiso 1 1 calc R . .
C3 C 0.3795(6) 0.2097(6) 0.0478(3) 0.0224(13) Uani 1 1 d . . .
H3 H 0.3252 0.2864 0.0725 0.027 Uiso 1 1 calc R . .
C4 C 0.5383(7) 0.2522(6) 0.0330(3) 0.0261(14) Uani 1 1 d . . .
O1A O 0.1279(5) 0.0490(4) -0.0218(2) 0.0275(10) Uani 1 1 d . . .
H1 H 0.0366 0.0354 -0.0095 0.03(4) Uiso 0.50 1 calc PR . .
O1B O 0.0788(5) 0.2661(4) 0.0119(2) 0.0265(10) Uani 1 1 d . . .
O2 O 0.4082(5) 0.1081(4) -0.0693(2) 0.0271(10) Uani 1 1 d . . .
H2A H 0.3632 0.0853 -0.1022 0.041 Uiso 1 1 calc R . .
O3 O 0.3420(4) 0.0780(4) 0.1015(2) 0.0277(10) Uani 1 1 d . . .
H3A H 0.4089 0.0193 0.0940 0.042 Uiso 1 1 calc R . .
O4A O 0.5792(5) 0.3686(5) -0.0228(3) 0.0343(11) Uani 1 1 d . . .
H4 H 0.6635 0.3971 -0.0212 0.051 Uiso 1 1 calc R . .
O4B O 0.6210(5) 0.1865(4) 0.0722(3) 0.0340(11) Uani 1 1 d . . .
C21 C 0.1748(6) 0.8439(6) 0.4892(3) 0.0205(12) Uani 1 1 d . . .
O21A O 0.0486(5) 0.8877(4) 0.4800(2) 0.0282(10) Uani 1 1 d . . .
H21 H 0.0327 0.9652 0.4967 0.042 Uiso 0.50 1 calc PR . .
O21B O 0.2661(5) 0.9086(4) 0.5132(2) 0.0279(10) Uani 1 1 d . . .
C22 C 0.2081(7) 0.6930(6) 0.4716(3) 0.0243(13) Uani 1 1 d . . .
H22 H 0.3080 0.6981 0.4374 0.029 Uiso 1 1 calc R . .
O22 O 0.1078(5) 0.6436(4) 0.4316(2) 0.0268(10) Uani 1 1 d . . .
H22O H 0.0347 0.6960 0.4343 0.040 Uiso 1 1 calc R . .
C23 C 0.2084(7) 0.5839(6) 0.5500(3) 0.0243(13) Uani 1 1 d . . .
H23 H 0.2849 0.6199 0.5747 0.029 Uiso 1 1 calc R . .
O23 O 0.0759(5) 0.5780(4) 0.6030(2) 0.0289(10) Uani 1 1 d . . .
H23O H 0.0216 0.5111 0.5977 0.043 Uiso 1 1 calc R . .
C24 C 0.2516(7) 0.4315(6) 0.5347(4) 0.0259(14) Uani 1 1 d . . .
O24A O 0.3683(5) 0.4383(4) 0.4771(3) 0.0355(11) Uani 1 1 d . . .
H24O H 0.4109 0.3590 0.4833 0.053 Uiso 1 1 calc R . .
O24B O 0.1871(5) 0.3232(5) 0.5735(3) 0.0372(11) Uani 1 1 d . . .
C32A C 0.7642(6) 0.0097(6) 0.3035(3) 0.0221(12) Uani 1 1 d . . .
H32G H 0.7205 0.0715 0.3408 0.027 Uiso 1 1 calc R . .
H32H H 0.7925 -0.0817 0.3350 0.027 Uiso 1 1 calc R . .
C32B C 0.9759(6) -0.0058(5) 0.1939(3) 0.0175(12) Uani 1 1 d . . .
H32A H 1.0636 0.0493 0.1598 0.021 Uiso 1 1 calc R . .
H32B H 0.9090 -0.0222 0.1592 0.021 Uiso 1 1 calc R . .
C32C C 0.9988(6) 0.1182(6) 0.3045(3) 0.0231(13) Uani 1 1 d . . .
H32C H 1.0209 0.0241 0.3361 0.028 Uiso 1 1 calc R . .
H32D H 0.9443 0.1750 0.3418 0.028 Uiso 1 1 calc R . .
C32D C 0.8636(7) 0.2281(6) 0.1978(3) 0.0218(12) Uani 1 1 d . . .
H32E H 0.9549 0.2728 0.1621 0.026 Uiso 1 1 calc R . .
H32F H 0.7977 0.2032 0.1645 0.026 Uiso 1 1 calc R . .
C33A C 0.6491(6) -0.0270(6) 0.2599(3) 0.0216(12) Uani 1 1 d . . .
H33G H 0.6918 -0.0878 0.2219 0.026 Uiso 1 1 calc R . .
H33H H 0.6170 0.0640 0.2298 0.026 Uiso 1 1 calc R . .
C33B C 1.0223(7) -0.1535(6) 0.2340(3) 0.0268(14) Uani 1 1 d . . .
H33A H 1.0926 -0.1388 0.2672 0.032 Uiso 1 1 calc R . .
H33B H 0.9357 -0.2096 0.2688 0.032 Uiso 1 1 calc R . .
C33C C 1.1426(6) 0.2005(6) 0.2634(3) 0.0239(13) Uani 1 1 d . . .
H33C H 1.1973 0.1462 0.2249 0.029 Uiso 1 1 calc R . .
H33D H 1.1221 0.2972 0.2339 0.029 Uiso 1 1 calc R . .
C33D C 0.7927(7) 0.3378(6) 0.2426(3) 0.0235(13) Uani 1 1 d . . .
H33E H 0.8593 0.3657 0.2748 0.028 Uiso 1 1 calc R . .
H33F H 0.7021 0.2935 0.2791 0.028 Uiso 1 1 calc R . .
C34A C 0.5175(7) -0.1090(7) 0.3180(3) 0.0270(13) Uani 1 1 d . . .
H34C H 0.5493 -0.2012 0.3470 0.032 Uiso 1 1 calc R . .
H34D H 0.4769 -0.0493 0.3571 0.032 Uiso 1 1 calc R . .
C34B C 1.0923(7) -0.2384(6) 0.1726(3) 0.0285(14) Uani 1 1 d . . .
H34E H 1.1779 -0.1814 0.1374 0.034 Uiso 1 1 calc R . .
H34F H 1.0214 -0.2536 0.1399 0.034 Uiso 1 1 calc R . .
C34C C 1.2355(7) 0.2203(7) 0.3218(4) 0.0300(14) Uani 1 1 d . . .
H34A H 1.1808 0.2745 0.3604 0.036 Uiso 1 1 calc R . .
H34B H 1.2562 0.1236 0.3513 0.036 Uiso 1 1 calc R . .
C34D C 0.7560(7) 0.4732(6) 0.1879(3) 0.0257(13) Uani 1 1 d . . .
H34G H 0.8464 0.5161 0.1506 0.031 Uiso 1 1 calc R . .
H34H H 0.6878 0.4455 0.1564 0.031 Uiso 1 1 calc R . .
C35A C 0.4003(7) -0.1421(7) 0.2757(4) 0.0305(14) Uani 1 1 d . . .
H35D H 0.3694 -0.0509 0.2465 0.037 Uiso 1 1 calc R . .
H35E H 0.3164 -0.1921 0.3144 0.037 Uiso 1 1 calc R . .
H35F H 0.4390 -0.2048 0.2387 0.037 Uiso 1 1 calc R . .
C35B C 1.1416(8) -0.3867(6) 0.2117(4) 0.0354(16) Uani 1 1 d . . .
H35J H 1.2096 -0.3719 0.2454 0.043 Uiso 1 1 calc R . .
H35K H 1.1903 -0.4374 0.1707 0.043 Uiso 1 1 calc R . .
H35L H 1.0561 -0.4456 0.2441 0.043 Uiso 1 1 calc R . .
C35C C 1.3775(8) 0.3021(7) 0.2810(4) 0.0351(15) Uani 1 1 d . . .
H35G H 1.4358 0.2445 0.2462 0.042 Uiso 1 1 calc R . .
H35H H 1.4319 0.3191 0.3207 0.042 Uiso 1 1 calc R . .
H35I H 1.3574 0.3957 0.2495 0.042 Uiso 1 1 calc R . .
C35D C 0.6871(8) 0.5861(6) 0.2327(4) 0.0356(16) Uani 1 1 d . . .
H35A H 0.5921 0.5479 0.2653 0.043 Uiso 1 1 calc R . .
H35B H 0.6734 0.6749 0.1951 0.043 Uiso 1 1 calc R . .
H35C H 0.7511 0.6087 0.2668 0.043 Uiso 1 1 calc R . .
N31 N 0.9000(5) 0.0877(5) 0.2505(3) 0.0212(11) Uani 1 1 d . . .
O1W O 0.4537(5) 0.1762(4) 0.4649(3) 0.0309(10) Uani 1 1 d D . .
H11W H 0.381(3) 0.118(4) 0.484(3) 0.009(14) Uiso 1 1 d D . .
H12W H 0.529(3) 0.144(5) 0.477(3) 0.011 Uiso 1 1 d D . .
O2W O 0.1534(5) 0.5459(5) 0.0292(3) 0.0344(11) Uani 1 1 d D . .
H21W H 0.126(8) 0.478(5) 0.010(5) 0.06(3) Uiso 1 1 d D . .
H22W H 0.111(7) 0.622(4) 0.014(4) 0.031(18) 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 O1B 1.223(7) . ?
C1 O1A 1.296(7) . ?
C1 C2 1.515(9) . ?
C2 O2 1.434(7) . ?
C2 C3 1.540(8) . ?
C2 H2 1.0000 . ?
C3 O3 1.393(7) . ?
C3 C4 1.496(9) . ?
C3 H3 1.0000 . ?
C4 O4B 1.223(7) . ?
C4 O4A 1.313(7) . ?
O1A H1 0.8400 . ?
O2 H2A 0.8400 . ?
O3 H3A 0.8400 . ?
O4A H4 0.8400 . ?
C21 O21B 1.235(7) . ?
C21 O21A 1.278(7) . ?
C21 C22 1.526(8) . ?
O21A H21 0.8400 . ?
C22 O22 1.409(7) . ?
C22 C23 1.546(8) . ?
C22 H22 1.0000 . ?
O22 H22O 0.8400 . ?
C23 O23 1.387(7) . ?
C23 C24 1.544(8) . ?
C23 H23 1.0000 . ?
O23 H23O 0.8400 . ?
C24 O24B 1.192(7) . ?
C24 O24A 1.324(8) . ?
O24A H24O 0.8400 . ?
C32A N31 1.507(7) . ?
C32A C33A 1.517(8) . ?
C32A H32G 0.9900 . ?
C32A H32H 0.9900 . ?
C32B N31 1.527(6) . ?
C32B C33B 1.527(7) . ?
C32B H32A 0.9900 . ?
C32B H32B 0.9900 . ?
C32C N31 1.517(7) . ?
C32C C33C 1.521(8) . ?
C32C H32C 0.9900 . ?
C32C H32D 0.9900 . ?
C32D C33D 1.494(7) . ?
C32D N31 1.531(6) . ?
C32D H32E 0.9900 . ?
C32D H32F 0.9900 . ?
C33A C34A 1.528(8) . ?
C33A H33G 0.9900 . ?
C33A H33H 0.9900 . ?
C33B C34B 1.514(8) . ?
C33B H33A 0.9900 . ?
C33B H33B 0.9900 . ?
C33C C34C 1.511(8) . ?
C33C H33C 0.9900 . ?
C33C H33D 0.9900 . ?
C33D C34D 1.515(7) . ?
C33D H33E 0.9900 . ?
C33D H33F 0.9900 . ?
C34A C35A 1.507(8) . ?
C34A H34C 0.9900 . ?
C34A H34D 0.9900 . ?
C34B C35B 1.536(8) . ?
C34B H34E 0.9900 . ?
C34B H34F 0.9900 . ?
C34C C35C 1.506(9) . ?
C34C H34A 0.9900 . ?
C34C H34B 0.9900 . ?
C34D C35D 1.513(8) . ?
C34D H34G 0.9900 . ?
C34D H34H 0.9900 . ?
C35A H35D 0.9800 . ?
C35A H35E 0.9800 . ?
C35A H35F 0.9800 . ?
C35B H35J 0.9800 . ?
C35B H35K 0.9800 . ?
C35B H35L 0.9800 . ?
C35C H35G 0.9800 . ?
C35C H35H 0.9800 . ?
C35C H35I 0.9800 . ?
C35D H35A 0.9800 . ?
C35D H35B 0.9800 . ?
C35D H35C 0.9800 . ?
O1W H11W 0.838(19) . ?
O1W H12W 0.816(19) . ?
O2W H21W 0.84(2) . ?
O2W H22W 0.836(19) . ?
 
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 126.8(6) . . ?
O1B C1 C2 119.4(5) . . ?
O1A C1 C2 113.8(5) . . ?
O2 C2 C1 112.8(5) . . ?
O2 C2 C3 108.2(4) . . ?
C1 C2 C3 110.2(4) . . ?
O2 C2 H2 108.5 . . ?
C1 C2 H2 108.5 . . ?
C3 C2 H2 108.5 . . ?
O3 C3 C4 113.2(4) . . ?
O3 C3 C2 111.3(5) . . ?
C4 C3 C2 112.4(5) . . ?
O3 C3 H3 106.5 . . ?
C4 C3 H3 106.5 . . ?
C2 C3 H3 106.5 . . ?
O4B C4 O4A 123.3(6) . . ?
O4B C4 C3 122.2(6) . . ?
O4A C4 C3 114.5(5) . . ?
C1 O1A H1 109.5 . . ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3A 109.5 . . ?
C4 O4A H4 109.5 . . ?
O21B C21 O21A 126.6(5) . . ?
O21B C21 C22 118.9(5) . . ?
O21A C21 C22 114.5(5) . . ?
C21 O21A H21 109.5 . . ?
O22 C22 C21 112.6(4) . . ?
O22 C22 C23 110.0(5) . . ?
C21 C22 C23 109.1(4) . . ?
O22 C22 H22 108.3 . . ?
C21 C22 H22 108.3 . . ?
C23 C22 H22 108.3 . . ?
C22 O22 H22O 109.5 . . ?
O23 C23 C24 111.7(5) . . ?
O23 C23 C22 111.9(4) . . ?
C24 C23 C22 111.1(5) . . ?
O23 C23 H23 107.3 . . ?
C24 C23 H23 107.3 . . ?
C22 C23 H23 107.3 . . ?
C23 O23 H23O 109.5 . . ?
O24B C24 O24A 126.1(5) . . ?
O24B C24 C23 121.8(5) . . ?
O24A C24 C23 112.0(5) . . ?
C24 O24A H24O 109.5 . . ?
N31 C32A C33A 114.4(4) . . ?
N31 C32A H32G 108.7 . . ?
C33A C32A H32G 108.7 . . ?
N31 C32A H32H 108.7 . . ?
C33A C32A H32H 108.7 . . ?
H32G C32A H32H 107.6 . . ?
N31 C32B C33B 114.8(4) . . ?
N31 C32B H32A 108.6 . . ?
C33B C32B H32A 108.6 . . ?
N31 C32B H32B 108.6 . . ?
C33B C32B H32B 108.6 . . ?
H32A C32B H32B 107.5 . . ?
N31 C32C C33C 115.8(4) . . ?
N31 C32C H32C 108.3 . . ?
C33C C32C H32C 108.3 . . ?
N31 C32C H32D 108.3 . . ?
C33C C32C H32D 108.3 . . ?
H32C C32C H32D 107.4 . . ?
C33D C32D N31 114.0(4) . . ?
C33D C32D H32E 108.8 . . ?
N31 C32D H32E 108.8 . . ?
C33D C32D H32F 108.8 . . ?
N31 C32D H32F 108.8 . . ?
H32E C32D H32F 107.7 . . ?
C32A C33A C34A 110.8(4) . . ?
C32A C33A H33G 109.5 . . ?
C34A C33A H33G 109.5 . . ?
C32A C33A H33H 109.5 . . ?
C34A C33A H33H 109.5 . . ?
H33G C33A H33H 108.1 . . ?
C34B C33B C32B 110.4(4) . . ?
C34B C33B H33A 109.6 . . ?
C32B C33B H33A 109.6 . . ?
C34B C33B H33B 109.6 . . ?
C32B C33B H33B 109.6 . . ?
H33A C33B H33B 108.1 . . ?
C34C C33C C32C 111.8(5) . . ?
C34C C33C H33C 109.3 . . ?
C32C C33C H33C 109.3 . . ?
C34C C33C H33D 109.3 . . ?
C32C C33C H33D 109.3 . . ?
H33C C33C H33D 107.9 . . ?
C32D C33D C34D 111.9(4) . . ?
C32D C33D H33E 109.2 . . ?
C34D C33D H33E 109.2 . . ?
C32D C33D H33F 109.2 . . ?
C34D C33D H33F 109.2 . . ?
H33E C33D H33F 107.9 . . ?
C35A C34A C33A 111.3(5) . . ?
C35A C34A H34C 109.4 . . ?
C33A C34A H34C 109.4 . . ?
C35A C34A H34D 109.4 . . ?
C33A C34A H34D 109.4 . . ?
H34C C34A H34D 108.0 . . ?
C33B C34B C35B 111.2(5) . . ?
C33B C34B H34E 109.4 . . ?
C35B C34B H34E 109.4 . . ?
C33B C34B H34F 109.4 . . ?
C35B C34B H34F 109.4 . . ?
H34E C34B H34F 108.0 . . ?
C35C C34C C33C 111.6(5) . . ?
C35C C34C H34A 109.3 . . ?
C33C C34C H34A 109.3 . . ?
C35C C34C H34B 109.3 . . ?
C33C C34C H34B 109.3 . . ?
H34A C34C H34B 108.0 . . ?
C35D C34D C33D 112.2(5) . . ?
C35D C34D H34G 109.2 . . ?
C33D C34D H34G 109.2 . . ?
C35D C34D H34H 109.2 . . ?
C33D C34D H34H 109.2 . . ?
H34G C34D H34H 107.9 . . ?
C34A C35A H35D 109.5 . . ?
C34A C35A H35E 109.5 . . ?
H35D C35A H35E 109.5 . . ?
C34A C35A H35F 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 109.5 . . ?
C34B C35B H35J 109.5 . . ?
C34B C35B H35K 109.5 . . ?
H35J C35B H35K 109.5 . . ?
C34B C35B H35L 109.5 . . ?
H35J C35B H35L 109.5 . . ?
H35K C35B H35L 109.5 . . ?
C34C C35C H35G 109.5 . . ?
C34C C35C H35H 109.5 . . ?
H35G C35C H35H 109.5 . . ?
C34C C35C H35I 109.5 . . ?
H35G C35C H35I 109.5 . . ?
H35H C35C H35I 109.5 . . ?
C34D C35D H35A 109.5 . . ?
C34D C35D H35B 109.5 . . ?
H35A C35D H35B 109.5 . . ?
C34D C35D H35C 109.5 . . ?
H35A C35D H35C 109.5 . . ?
H35B C35D H35C 109.5 . . ?
C32A N31 C32C 106.6(4) . . ?
C32A N31 C32B 110.9(4) . . ?
C32C N31 C32B 110.8(4) . . ?
C32A N31 C32D 111.5(4) . . ?
C32C N31 C32D 111.6(4) . . ?
C32B N31 C32D 105.6(4) . . ?
H11W O1W H12W 113(3) . . ?
H21W O2W H22W 109(3) . . ?
 
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
O24A H24O O1W  0.84 1.84 2.617(5) 154.3 .
O2W H21W O1B  0.84(2) 2.03(3) 2.806(6) 153(6) .
O2 H2A O4B  0.84 2.51 2.787(6) 100.7 2_655
O4A H4 O2W  0.84 1.76 2.600(6) 173.4 2_665
O21A H21 O21A  0.84 1.66 2.468(7) 161.4 2_576
O22 H22O O24B  0.84 2.11 2.791(6) 137.3 2_566
O23 H23O O22  0.84 2.10 2.931(6) 172.5 2_566
O1W H11W O21B  0.838(19) 2.16(3) 2.943(6) 155(5) 1_545
O1W H12W O21B  0.816(19) 2.01(2) 2.812(6) 168(5) 2_666
O2W H22W O1B  0.836(19) 2.14(4) 2.905(6) 152(6) 2_565
 
_diffrn_measured_fraction_theta_max    0.793
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.800
_refine_diff_density_max    0.546
_refine_diff_density_min   -0.393
_refine_diff_density_rms    0.116
