 
data_04skc0005p1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
1-Methylpiperazinium di(L-tartrate) dihydrate
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C13 H28 N2 O14'
_chemical_formula_weight          436.37
 
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   0.0000
 '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   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 
_cell_length_a                    7.4774(6)
_cell_length_b                    7.7071(7)
_cell_length_c                    16.2943(16)
_cell_angle_alpha                 88.321(8)
_cell_angle_beta                  86.355(6)
_cell_angle_gamma                 89.778(6)
_cell_volume                      936.72(15)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4219
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        lath
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.547
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              464
_exptl_absorpt_coefficient_mu     0.141
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9860
_exptl_absorpt_correction_T_max   0.9944
_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             20348
_diffrn_reflns_av_R_equivalents   0.0500
_diffrn_reflns_av_sigmaI/netI     0.0492
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          2.93
_diffrn_reflns_theta_max          27.47
_reflns_number_total              4268
_reflns_number_gt                 3622
_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 chemical_absolute_configuration could not be obtained as there are no 
 heavy atoms present in the structure.
;
 
_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)+(0.0416P)²+0.0843P] 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_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    -10(10)
_refine_ls_number_reflns          4268
_refine_ls_number_parameters      569
_refine_ls_number_restraints      15
_refine_ls_R_factor_all           0.0511
_refine_ls_R_factor_gt            0.0377
_refine_ls_wR_factor_ref          0.0800
_refine_ls_wR_factor_gt           0.0747
_refine_ls_goodness_of_fit_ref    1.040
_refine_ls_restrained_S_all       1.039
_refine_ls_shift/su_max           0.002
_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 0.4457(4) 0.2516(4) 0.31975(17) 0.0163(6) Uani 1 1 d . . .
C2 C 0.2398(4) 0.2633(4) 0.31750(17) 0.0151(6) Uani 1 1 d . . .
H2 H 0.1859 0.1589 0.3472 0.018 Uiso 1 1 calc R . .
C3 C 0.1793(4) 0.2686(4) 0.22997(17) 0.0159(6) Uani 1 1 d . . .
H3 H 0.2096 0.1551 0.2042 0.019 Uiso 1 1 calc R . .
C4 C -0.0240(4) 0.2952(4) 0.23159(18) 0.0177(6) Uani 1 1 d . . .
O1A O 0.5285(3) 0.1493(3) 0.27305(12) 0.0190(4) Uani 1 1 d . . .
O1B O 0.5179(3) 0.3435(2) 0.37132(12) 0.0176(4) Uani 1 1 d . . .
O2 O 0.1721(3) 0.4133(3) 0.35658(12) 0.0180(4) Uani 1 1 d . . .
H2O H 0.1244 0.3853 0.4031 0.027 Uiso 1 1 calc R . .
O3 O 0.2663(3) 0.4023(3) 0.18253(12) 0.0196(4) Uani 1 1 d . . .
H3O H 0.2209 0.4983 0.1955 0.029 Uiso 1 1 calc R . .
O4B O -0.1140(3) 0.1650(3) 0.26834(13) 0.0212(5) Uani 1 1 d . . .
H4 H -0.2242 0.1802 0.2635 0.032 Uiso 1 1 calc R . .
O4A O -0.0914(3) 0.4237(3) 0.20220(15) 0.0279(5) Uani 1 1 d . . .
C22 C 0.5964(4) -0.2541(4) 0.32745(17) 0.0190(6) Uani 1 1 d . . .
H22A H 0.6196 -0.3733 0.3083 0.023 Uiso 1 1 calc R . .
H22B H 0.6108 -0.1732 0.2792 0.023 Uiso 1 1 calc R . .
C23 C 0.4070(4) -0.2422(4) 0.36536(17) 0.0180(6) Uani 1 1 d . . .
H23A H 0.3805 -0.1209 0.3806 0.022 Uiso 1 1 calc R . .
H23B H 0.3215 -0.2759 0.3247 0.022 Uiso 1 1 calc R . .
C25 C 0.5159(4) -0.3143(4) 0.50126(18) 0.0175(6) Uani 1 1 d . . .
H25A H 0.5014 -0.3947 0.5497 0.021 Uiso 1 1 calc R . .
H25B H 0.4932 -0.1948 0.5200 0.021 Uiso 1 1 calc R . .
C26 C 0.7028(4) -0.3275(4) 0.46318(18) 0.0197(6) Uani 1 1 d . . .
H26A H 0.7889 -0.2962 0.5040 0.024 Uiso 1 1 calc R . .
H26B H 0.7272 -0.4488 0.4474 0.024 Uiso 1 1 calc R . .
C27 C 0.9152(4) -0.2194(4) 0.3527(2) 0.0294(8) Uani 1 1 d . . .
H27A H 0.9421 -0.3386 0.3366 0.044 Uiso 1 1 calc R . .
H27B H 0.9979 -0.1846 0.3935 0.044 Uiso 1 1 calc R . .
H27C H 0.9291 -0.1412 0.3042 0.044 Uiso 1 1 calc R . .
N21 N 0.7288(3) -0.2097(3) 0.38871(15) 0.0179(5) Uani 1 1 d . . .
H21 H 0.7067 -0.0964 0.4048 0.021 Uiso 1 1 calc R . .
N24 N 0.3845(3) -0.3590(3) 0.44014(14) 0.0163(5) Uani 1 1 d . . .
H24A H 0.2699 -0.3482 0.4636 0.020 Uiso 1 1 calc R . .
H24B H 0.4010 -0.4725 0.4253 0.020 Uiso 1 1 calc R . .
C31 C 0.8379(4) -0.0272(4) 0.09037(18) 0.0197(6) Uani 1 1 d . . .
C32 C 0.6470(4) 0.0274(4) 0.07451(18) 0.0169(6) Uani 1 1 d . . .
H32 H 0.5791 0.0495 0.1281 0.020 Uiso 1 1 calc R . .
C33 C 0.5596(4) -0.1205(4) 0.03233(17) 0.0167(6) Uani 1 1 d . . .
H33 H 0.5440 -0.2211 0.0723 0.020 Uiso 1 1 calc R . .
C34 C 0.3767(4) -0.0583(3) 0.00962(18) 0.0165(6) Uani 1 1 d . . .
O31A O 0.9612(3) 0.0659(3) 0.04983(15) 0.0290(5) Uani 1 1 d . . .
H31 H 1.0628 0.0253 0.0589 0.044 Uiso 1 1 calc R . .
O31B O 0.8640(3) -0.1507(3) 0.13608(13) 0.0255(5) Uani 1 1 d . . .
O32 O 0.6401(3) 0.1771(3) 0.02218(13) 0.0204(5) Uani 1 1 d . . .
H32O H 0.6276 0.2657 0.0508 0.031 Uiso 1 1 calc R . .
O33 O 0.6680(3) -0.1736(3) -0.03685(13) 0.0258(5) Uani 1 1 d . . .
H33O H 0.6294 -0.1285 -0.0798 0.039 Uiso 1 1 calc R . .
O34A O 0.2706(3) -0.0259(3) 0.07257(12) 0.0199(4) Uani 1 1 d . . .
O34B O 0.3395(3) -0.0401(3) -0.06241(12) 0.0199(4) Uani 1 1 d . . .
C42 C 0.1591(4) 0.3147(4) 0.90275(19) 0.0193(6) Uani 1 1 d . . .
H42A H 0.1582 0.2375 0.9524 0.023 Uiso 1 1 calc R . .
H42B H 0.2825 0.3162 0.8769 0.023 Uiso 1 1 calc R . .
C43 C 0.0339(4) 0.2431(4) 0.84342(19) 0.0218(7) Uani 1 1 d . . .
H43A H 0.0469 0.3103 0.7907 0.026 Uiso 1 1 calc R . .
H43B H 0.0661 0.1209 0.8324 0.026 Uiso 1 1 calc R . .
C45 C -0.2037(4) 0.4340(4) 0.89713(19) 0.0217(6) Uani 1 1 d . . .
H45A H -0.3301 0.4396 0.9189 0.026 Uiso 1 1 calc R . .
H45B H -0.1905 0.5085 0.8466 0.026 Uiso 1 1 calc R . .
C46 C -0.0830(4) 0.4984(4) 0.96010(19) 0.0197(6) Uani 1 1 d . . .
H46A H -0.1168 0.6188 0.9742 0.024 Uiso 1 1 calc R . .
H46B H -0.0980 0.4248 1.0109 0.024 Uiso 1 1 calc R . .
C47 C 0.2272(4) 0.5539(4) 0.99094(19) 0.0253(7) Uani 1 1 d . . .
H47A H 0.2242 0.4695 1.0372 0.038 Uiso 1 1 calc R . .
H47B H 0.1855 0.6669 1.0106 0.038 Uiso 1 1 calc R . .
H47C H 0.3501 0.5647 0.9667 0.038 Uiso 1 1 calc R . .
N41 N 0.1081(3) 0.4939(3) 0.92757(15) 0.0169(5) Uani 1 1 d . . .
H41 H 0.1217 0.5682 0.8816 0.020 Uiso 1 1 calc R . .
N44 N -0.1558(3) 0.2521(3) 0.87734(15) 0.0197(5) Uani 1 1 d . . .
H44A H -0.2306 0.2121 0.8394 0.024 Uiso 1 1 calc R . .
H44B H -0.1703 0.1826 0.9241 0.024 Uiso 1 1 calc R . .
C51 C 0.1681(4) 0.0539(4) 0.56132(18) 0.0164(6) Uani 1 1 d . . .
C52 C 0.1822(4) 0.2358(3) 0.59328(17) 0.0158(6) Uani 1 1 d . . .
H52 H 0.1988 0.2280 0.6537 0.019 Uiso 1 1 calc R . .
C53 C 0.0118(4) 0.3391(4) 0.57889(17) 0.0154(6) Uani 1 1 d . . .
H53 H -0.0909 0.2846 0.6124 0.018 Uiso 1 1 calc R . .
C54 C 0.0411(4) 0.5223(4) 0.60881(18) 0.0159(6) Uani 1 1 d . . .
O51A O 0.2459(3) 0.0063(3) 0.49825(14) 0.0286(5) Uani 1 1 d . . .
O51B O 0.0609(3) -0.0445(2) 0.60885(13) 0.0235(5) Uani 1 1 d . . .
H51 H 0.0599 -0.1450 0.5903 0.035 Uiso 1 1 calc R . .
O52 O 0.3261(3) 0.3292(3) 0.55407(13) 0.0198(4) Uani 1 1 d . . .
H52O H 0.4231 0.2891 0.5699 0.030 Uiso 1 1 calc R . .
O53 O -0.0268(3) 0.3420(2) 0.49428(12) 0.0167(4) Uani 1 1 d . . .
H53O H -0.0911 0.2564 0.4852 0.025 Uiso 1 1 calc R . .
O54A O 0.0655(3) 0.6461(2) 0.55617(12) 0.0182(4) Uani 1 1 d . . .
O54B O 0.0425(3) 0.5327(3) 0.68430(13) 0.0266(5) Uani 1 1 d . . .
C61 C 0.6292(3) 0.1216(4) 0.69077(17) 0.0147(6) Uani 1 1 d . . .
C62 C 0.6566(4) -0.0649(3) 0.72184(17) 0.0144(6) Uani 1 1 d . . .
H62 H 0.7435 -0.1253 0.6831 0.017 Uiso 1 1 calc R . .
C63 C 0.4744(4) -0.1569(3) 0.72445(17) 0.0145(6) Uani 1 1 d . . .
H63 H 0.4316 -0.1520 0.6675 0.017 Uiso 1 1 calc R . .
C64 C 0.4927(4) -0.3472(3) 0.75027(17) 0.0152(6) Uani 1 1 d . . .
O61A O 0.5845(3) 0.1377(3) 0.61815(12) 0.0194(4) Uani 1 1 d . . .
O61B O 0.6534(3) 0.2440(2) 0.73798(12) 0.0198(4) Uani 1 1 d . . .
O62 O 0.7215(3) -0.0693(2) 0.80178(12) 0.0159(4) Uani 1 1 d . . .
H62O H 0.8112 -0.1352 0.8027 0.024 Uiso 1 1 calc R . .
O63 O 0.3467(2) -0.0700(2) 0.77622(12) 0.0159(4) Uani 1 1 d . . .
H63O H 0.3836 -0.0660 0.8238 0.024 Uiso 1 1 calc R . .
O64A O 0.4216(3) -0.4107(3) 0.81267(13) 0.0214(5) Uani 1 1 d . . .
O64B O 0.5961(3) -0.4320(2) 0.69620(12) 0.0210(5) Uani 1 1 d . . .
H64 H 0.6001 -0.5373 0.7107 0.032 Uiso 1 1 calc R . .
O1W O 0.7103(3) 0.1135(3) 0.45918(13) 0.0183(4) Uani 1 1 d D . .
H1W H 0.651(4) 0.189(4) 0.4327(17) 0.031(10) Uiso 1 1 d D . .
H2W H 0.663(5) 0.110(5) 0.5074(12) 0.041(12) Uiso 1 1 d D . .
O2W O 0.0305(3) 0.7527(3) 0.80215(12) 0.0170(4) Uani 1 1 d D . .
H21W H 0.030(6) 0.689(5) 0.761(2) 0.070(16) Uiso 1 1 d D . .
H22W H 0.128(4) 0.812(4) 0.793(2) 0.028(9) Uiso 1 1 d D . .
O3W O 0.5997(3) 0.4562(3) 0.11254(13) 0.0227(5) Uani 1 1 d D . .
H31W H 0.506(3) 0.436(5) 0.142(2) 0.040(11) Uiso 1 1 d D . .
H32W H 0.687(3) 0.464(6) 0.142(2) 0.055(14) Uiso 1 1 d D . .
O4W O 0.1821(3) 0.7393(3) 0.19930(13) 0.0226(5) Uani 1 1 d D . .
H41W H 0.075(3) 0.754(6) 0.190(3) 0.070(16) Uiso 1 1 d D . .
H42W H 0.245(4) 0.811(4) 0.171(2) 0.040(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 1.247(4) . ?
C1 O1B 1.263(3) . ?
C1 C2 1.544(4) . ?
C2 O2 1.413(3) . ?
C2 C3 1.523(4) . ?
C2 H2 1.0000 . ?
C3 O3 1.406(3) . ?
C3 C4 1.532(4) . ?
C3 H3 1.0000 . ?
C4 O4A 1.209(4) . ?
C4 O4B 1.318(3) . ?
O2 H2O 0.8400 . ?
O3 H3O 0.8400 . ?
O4B H4 0.8400 . ?
C22 N21 1.497(4) . ?
C22 C23 1.512(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.495(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 N24 1.491(4) . ?
C25 C26 1.497(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N21 1.497(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 N21 1.480(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
N21 H21 0.9300 . ?
N24 H24A 0.9200 . ?
N24 H24B 0.9200 . ?
C31 O31B 1.214(4) . ?
C31 O31A 1.304(4) . ?
C31 C32 1.522(4) . ?
C32 O32 1.417(3) . ?
C32 C33 1.519(4) . ?
C32 H32 1.0000 . ?
C33 O33 1.415(3) . ?
C33 C34 1.512(4) . ?
C33 H33 1.0000 . ?
C34 O34B 1.227(3) . ?
C34 O34A 1.286(3) . ?
O31A H31 0.8400 . ?
O32 H32O 0.8400 . ?
O33 H33O 0.8400 . ?
C42 N41 1.492(4) . ?
C42 C43 1.506(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 N44 1.491(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C45 N44 1.485(4) . ?
C45 C46 1.505(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 N41 1.493(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 N41 1.490(4) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
N41 H41 0.9300 . ?
N44 H44A 0.9200 . ?
N44 H44B 0.9200 . ?
C51 O51A 1.214(4) . ?
C51 O51B 1.307(4) . ?
C51 C52 1.517(4) . ?
C52 O52 1.405(3) . ?
C52 C53 1.527(4) . ?
C52 H52 1.0000 . ?
C53 O53 1.426(3) . ?
C53 C54 1.529(4) . ?
C53 H53 1.0000 . ?
C54 O54B 1.236(4) . ?
C54 O54A 1.270(3) . ?
O51B H51 0.8400 . ?
O52 H52O 0.8400 . ?
O53 H53O 0.8400 . ?
C61 O61A 1.253(3) . ?
C61 O61B 1.255(3) . ?
C61 C62 1.527(4) . ?
C62 O62 1.418(3) . ?
C62 C63 1.536(4) . ?
C62 H62 1.0000 . ?
C63 O63 1.413(3) . ?
C63 C64 1.522(4) . ?
C63 H63 1.0000 . ?
C64 O64A 1.208(3) . ?
C64 O64B 1.321(3) . ?
O62 H62O 0.8400 . ?
O63 H63O 0.8400 . ?
O64B H64 0.8400 . ?
O1W H1W 0.851(18) . ?
O1W H2W 0.842(18) . ?
O2W H21W 0.844(19) . ?
O2W H22W 0.863(18) . ?
O3W H31W 0.831(18) . ?
O3W H32W 0.834(19) . ?
O4W H41W 0.836(19) . ?
O4W H42W 0.838(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
O1A C1 O1B 124.5(3) . . ?
O1A C1 C2 118.5(2) . . ?
O1B C1 C2 116.9(2) . . ?
O2 C2 C3 107.7(2) . . ?
O2 C2 C1 111.3(2) . . ?
C3 C2 C1 112.2(2) . . ?
O2 C2 H2 108.5 . . ?
C3 C2 H2 108.5 . . ?
C1 C2 H2 108.5 . . ?
O3 C3 C2 111.0(2) . . ?
O3 C3 C4 109.9(2) . . ?
C2 C3 C4 109.7(2) . . ?
O3 C3 H3 108.7 . . ?
C2 C3 H3 108.7 . . ?
C4 C3 H3 108.7 . . ?
O4A C4 O4B 124.8(3) . . ?
O4A C4 C3 122.4(3) . . ?
O4B C4 C3 112.8(2) . . ?
C2 O2 H2O 109.5 . . ?
C3 O3 H3O 109.5 . . ?
C4 O4B H4 109.5 . . ?
N21 C22 C23 110.6(2) . . ?
N21 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
N21 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
N24 C23 C22 110.3(2) . . ?
N24 C23 H23A 109.6 . . ?
C22 C23 H23A 109.6 . . ?
N24 C23 H23B 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
N24 C25 C26 110.0(2) . . ?
N24 C25 H25A 109.7 . . ?
C26 C25 H25A 109.7 . . ?
N24 C25 H25B 109.7 . . ?
C26 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
N21 C26 C25 111.2(2) . . ?
N21 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
N21 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
N21 C27 H27A 109.5 . . ?
N21 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N21 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C27 N21 C26 110.9(2) . . ?
C27 N21 C22 111.6(2) . . ?
C26 N21 C22 109.7(2) . . ?
C27 N21 H21 108.2 . . ?
C26 N21 H21 108.2 . . ?
C22 N21 H21 108.2 . . ?
C25 N24 C23 110.6(2) . . ?
C25 N24 H24A 109.5 . . ?
C23 N24 H24A 109.5 . . ?
C25 N24 H24B 109.5 . . ?
C23 N24 H24B 109.5 . . ?
H24A N24 H24B 108.1 . . ?
O31B C31 O31A 125.9(3) . . ?
O31B C31 C32 119.9(3) . . ?
O31A C31 C32 114.2(2) . . ?
O32 C32 C33 107.7(2) . . ?
O32 C32 C31 112.7(2) . . ?
C33 C32 C31 107.9(2) . . ?
O32 C32 H32 109.5 . . ?
C33 C32 H32 109.5 . . ?
C31 C32 H32 109.5 . . ?
O33 C33 C34 112.4(2) . . ?
O33 C33 C32 110.9(2) . . ?
C34 C33 C32 107.3(2) . . ?
O33 C33 H33 108.7 . . ?
C34 C33 H33 108.7 . . ?
C32 C33 H33 108.7 . . ?
O34B C34 O34A 125.3(3) . . ?
O34B C34 C33 121.6(3) . . ?
O34A C34 C33 113.1(2) . . ?
C31 O31A H31 109.5 . . ?
C32 O32 H32O 109.5 . . ?
C33 O33 H33O 109.5 . . ?
N41 C42 C43 112.1(2) . . ?
N41 C42 H42A 109.2 . . ?
C43 C42 H42A 109.2 . . ?
N41 C42 H42B 109.2 . . ?
C43 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
N44 C43 C42 110.9(2) . . ?
N44 C43 H43A 109.5 . . ?
C42 C43 H43A 109.5 . . ?
N44 C43 H43B 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 108.0 . . ?
N44 C45 C46 109.6(2) . . ?
N44 C45 H45A 109.7 . . ?
C46 C45 H45A 109.7 . . ?
N44 C45 H45B 109.7 . . ?
C46 C45 H45B 109.7 . . ?
H45A C45 H45B 108.2 . . ?
N41 C46 C45 110.5(2) . . ?
N41 C46 H46A 109.6 . . ?
C45 C46 H46A 109.6 . . ?
N41 C46 H46B 109.6 . . ?
C45 C46 H46B 109.6 . . ?
H46A C46 H46B 108.1 . . ?
N41 C47 H47A 109.5 . . ?
N41 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N41 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C47 N41 C42 110.1(2) . . ?
C47 N41 C46 110.2(2) . . ?
C42 N41 C46 110.3(2) . . ?
C47 N41 H41 108.7 . . ?
C42 N41 H41 108.7 . . ?
C46 N41 H41 108.7 . . ?
C45 N44 C43 110.0(2) . . ?
C45 N44 H44A 109.7 . . ?
C43 N44 H44A 109.7 . . ?
C45 N44 H44B 109.7 . . ?
C43 N44 H44B 109.7 . . ?
H44A N44 H44B 108.2 . . ?
O51A C51 O51B 124.1(3) . . ?
O51A C51 C52 123.7(2) . . ?
O51B C51 C52 112.3(2) . . ?
O52 C52 C51 112.4(2) . . ?
O52 C52 C53 107.2(2) . . ?
C51 C52 C53 110.5(2) . . ?
O52 C52 H52 108.9 . . ?
C51 C52 H52 108.9 . . ?
C53 C52 H52 108.9 . . ?
O53 C53 C52 111.3(2) . . ?
O53 C53 C54 111.3(2) . . ?
C52 C53 C54 107.0(2) . . ?
O53 C53 H53 109.1 . . ?
C52 C53 H53 109.1 . . ?
C54 C53 H53 109.1 . . ?
O54B C54 O54A 126.4(3) . . ?
O54B C54 C53 114.5(2) . . ?
O54A C54 C53 119.1(2) . . ?
C51 O51B H51 109.5 . . ?
C52 O52 H52O 109.5 . . ?
C53 O53 H53O 109.5 . . ?
O61A C61 O61B 125.6(3) . . ?
O61A C61 C62 115.3(2) . . ?
O61B C61 C62 119.1(2) . . ?
O62 C62 C61 111.2(2) . . ?
O62 C62 C63 109.4(2) . . ?
C61 C62 C63 107.7(2) . . ?
O62 C62 H62 109.5 . . ?
C61 C62 H62 109.5 . . ?
C63 C62 H62 109.5 . . ?
O63 C63 C64 111.8(2) . . ?
O63 C63 C62 110.7(2) . . ?
C64 C63 C62 110.9(2) . . ?
O63 C63 H63 107.8 . . ?
C64 C63 H63 107.8 . . ?
C62 C63 H63 107.8 . . ?
O64A C64 O64B 124.9(3) . . ?
O64A C64 C63 123.7(3) . . ?
O64B C64 C63 111.3(2) . . ?
C62 O62 H62O 109.5 . . ?
C63 O63 H63O 109.5 . . ?
C64 O64B H64 109.5 . . ?
H1W O1W H2W 106(3) . . ?
H21W O2W H22W 104(3) . . ?
H31W O3W H32W 110(3) . . ?
H41W O4W H42W 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
N21 H21 O1W  0.93 1.87 2.772(3) 163.5 .
N41 H41 O2W  0.93 2.04 2.897(3) 152.7 .
O32 H32O O3W  0.84 1.81 2.648(3) 179.8 .
O2 H2O O53  0.84 1.83 2.657(3) 166.8 .
O3 H3O O4W  0.84 1.88 2.687(3) 160.6 .
O52 H52O O61A  0.84 1.87 2.673(3) 159.9 .
O1W H1W O1B  0.851(18) 1.862(19) 2.712(3) 177(3) .
O1W H2W O61A  0.842(18) 1.88(2) 2.710(3) 169(4) .
O2W H21W O54B  0.844(19) 1.76(2) 2.596(3) 172(5) .
O3W H31W O3  0.831(18) 1.890(19) 2.702(3) 165(4) .
N44 H44A O61B  0.92 1.92 2.760(3) 150.1 1_455
N44 H44A O62  0.92 2.31 2.973(3) 128.9 1_455
O4B H4 O1A  0.84 1.86 2.673(3) 161.9 1_455
O53 H53O O1W  0.84 1.93 2.742(3) 163.0 1_455
N44 H44B O32  0.92 2.07 2.775(3) 132.8 1_456
N44 H44B O31A  0.92 2.47 3.285(3) 147.4 1_456
N41 H41 O64A  0.93 2.45 2.986(3) 116.9 1_565
O2W H22W O63  0.863(18) 1.877(19) 2.739(3) 177(4) 1_565
O4W H42W O34A  0.838(19) 2.01(3) 2.756(3) 149(3) 1_565
N24 H24A O54A  0.92 2.08 2.949(3) 157.4 1_545
N24 H24B O1B  0.92 1.87 2.739(3) 155.5 1_545
N24 H24B O2  0.92 2.30 2.809(3) 114.8 1_545
O51B H51 O54A  0.84 1.72 2.557(3) 177.0 1_545
O64B H64 O61B  0.84 1.78 2.610(3) 169.1 1_545
O31A H31 O34A  0.84 1.63 2.463(3) 171.8 1_655
O3W H32W O4A  0.834(19) 2.00(2) 2.817(3) 166(4) 1_655
O33 H33O O62  0.84 2.05 2.732(3) 138.5 1_554
O62 H62O O2W  0.84 1.85 2.683(3) 170.6 1_645
O63 H63O O34B  0.84 1.88 2.643(3) 150.6 1_556
O4W H41W O31B  0.836(19) 1.98(3) 2.771(3) 159(4) 1_465
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    0.214
_refine_diff_density_min   -0.242
_refine_diff_density_rms    0.055
