 
data_06skc0067p-1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
Fumaric Acid and 2-Aminoethanol
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C6 H11 N O5'
_chemical_formula_weight          177.16
 
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                    8.1621(6)
_cell_length_b                    9.3259(5)
_cell_length_c                    21.3026(12)
_cell_angle_alpha                 86.922(4)
_cell_angle_beta                  88.863(3)
_cell_angle_gamma                 87.350(4)
_cell_volume                      1617.22(17)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     6633
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.455
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              752
_exptl_absorpt_coefficient_mu     0.128
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9848
_exptl_absorpt_correction_T_max   0.9987
_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    '10cm confocal mirrors'
_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             23933
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.1135
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -27
_diffrn_reflns_limit_l_max        27
_diffrn_reflns_theta_min          3.12
_diffrn_reflns_theta_max          27.48
_reflns_number_total              23933
_reflns_number_gt                 15565
_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)+(0.0482P)²+14.1392P] 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_number_reflns          23933
_refine_ls_number_parameters      445
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.2172
_refine_ls_R_factor_gt            0.1472
_refine_ls_wR_factor_ref          0.3410
_refine_ls_wR_factor_gt           0.2733
_refine_ls_goodness_of_fit_ref    1.191
_refine_ls_restrained_S_all       1.191
_refine_ls_shift/su_max           0.023
_refine_ls_shift/su_mean          0.001
 
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 0.8410(6) 0.0784(5) -0.0347(2) 0.0174(11) Uani 1 1 d . . .
C2 C 0.8433(6) 0.1892(5) 0.0130(2) 0.0179(11) Uani 1 1 d . . .
H2 H 0.8458 0.1582 0.0562 0.021 Uiso 1 1 calc R . .
C3 C 0.8420(6) 0.3286(5) -0.0019(2) 0.0177(11) Uani 1 1 d . . .
H3 H 0.8398 0.3584 -0.0452 0.021 Uiso 1 1 calc R . .
C4 C 0.8439(5) 0.4412(5) 0.0440(2) 0.0119(10) Uani 1 1 d . . .
O1A O 0.7937(4) -0.0436(4) -0.01985(15) 0.0212(8) Uani 1 1 d . . .
O1B O 0.8918(5) 0.1173(4) -0.09055(14) 0.0209(8) Uani 1 1 d . . .
O4A O 0.9030(5) 0.3984(4) 0.09873(14) 0.0196(8) Uani 1 1 d . . .
H4A H 0.8890 0.4647 0.1237 0.029 Uiso 1 1 calc R . .
O4B O 0.7940(5) 0.5663(4) 0.03051(15) 0.0226(8) Uani 1 1 d . . .
C22 C 1.5135(7) 0.2981(6) 0.1553(3) 0.0300(14) Uani 1 1 d . . .
H22A H 1.6348 0.2962 0.1529 0.036 Uiso 1 1 calc R . .
H22B H 1.4748 0.3734 0.1839 0.036 Uiso 1 1 calc R . .
C23 C 1.4420(6) 0.3272(6) 0.0908(2) 0.0277(13) Uani 1 1 d . . .
H23A H 1.4718 0.4237 0.0739 0.033 Uiso 1 1 calc R . .
H23B H 1.4881 0.2553 0.0620 0.033 Uiso 1 1 calc R . .
N24 N 1.2617(5) 0.3200(5) 0.09433(19) 0.0205(10) Uani 1 1 d . . .
H24A H 1.2346 0.2337 0.1126 0.031 Uiso 1 1 calc R . .
H24B H 1.2205 0.3299 0.0549 0.031 Uiso 1 1 calc R . .
H24C H 1.2189 0.3920 0.1177 0.031 Uiso 1 1 calc R . .
O21 O 1.4588(5) 0.1632(4) 0.17722(18) 0.0326(10) Uani 1 1 d . . .
H21 H 1.5116 0.1340 0.2092 0.049 Uiso 1 1 calc R . .
C31 C 1.0420(6) -0.1083(5) -0.1869(2) 0.0171(11) Uani 1 1 d . . .
C32 C 1.0450(6) -0.2225(5) -0.2340(2) 0.0168(10) Uani 1 1 d . . .
H32 H 1.1476 -0.2669 -0.2454 0.020 Uiso 1 1 calc R . .
C33 C 0.9111(6) -0.2638(5) -0.2603(2) 0.0154(10) Uani 1 1 d . . .
H33 H 0.8080 -0.2228 -0.2475 0.018 Uiso 1 1 calc R . .
C34 C 0.9151(6) -0.3718(5) -0.3090(2) 0.0175(11) Uani 1 1 d . . .
O31A O 0.9001(4) -0.0798(4) -0.16168(15) 0.0200(8) Uani 1 1 d . . .
H31A H 0.9074 -0.0136 -0.1368 0.030 Uiso 1 1 calc R . .
O31B O 1.1689(4) -0.0497(4) -0.17635(16) 0.0223(8) Uani 1 1 d . . .
O34A O 0.7890(4) -0.4133(4) -0.33005(16) 0.0250(8) Uani 1 1 d . . .
O34B O 1.0632(4) -0.4159(4) -0.32607(15) 0.0225(8) Uani 1 1 d . . .
H34B H 1.0573 -0.4806 -0.3518 0.034 Uiso 1 1 calc R . .
C42 C 0.5306(7) 0.7191(6) 0.3474(2) 0.0265(12) Uani 1 1 d . . .
H42A H 0.4654 0.7959 0.3241 0.032 Uiso 1 1 calc R . .
H42B H 0.6429 0.7522 0.3524 0.032 Uiso 1 1 calc R . .
C43 C 0.4525(6) 0.6856(6) 0.4109(2) 0.0230(12) Uani 1 1 d . . .
H43A H 0.5136 0.6035 0.4323 0.028 Uiso 1 1 calc R . .
H43B H 0.4583 0.7697 0.4371 0.028 Uiso 1 1 calc R . .
N44 N 0.2783(5) 0.6498(4) 0.40434(18) 0.0178(9) Uani 1 1 d . . .
H44A H 0.2181 0.7305 0.3918 0.027 Uiso 1 1 calc R . .
H44B H 0.2387 0.6145 0.4420 0.027 Uiso 1 1 calc R . .
H44C H 0.2715 0.5826 0.3752 0.027 Uiso 1 1 calc R . .
O41 O 0.5358(5) 0.5912(4) 0.31427(18) 0.0346(10) Uani 1 1 d . . .
H41 H 0.5499 0.6114 0.2757 0.052 Uiso 1 1 calc R . .
C51 C 1.1410(6) -0.5772(6) -0.4576(2) 0.0184(11) Uani 1 1 d . . .
C52 C 1.1510(6) -0.6866(5) -0.5046(2) 0.0150(10) Uani 1 1 d . . .
H52 H 1.1526 -0.6562 -0.5479 0.018 Uiso 1 1 calc R . .
C53 C 1.1581(6) -0.8271(5) -0.4889(2) 0.0157(10) Uani 1 1 d . . .
H53 H 1.1530 -0.8565 -0.4456 0.019 Uiso 1 1 calc R . .
C54 C 1.1733(6) -0.9394(5) -0.5351(2) 0.0151(10) Uani 1 1 d . . .
O51A O 1.0784(4) -0.6106(4) -0.40376(14) 0.0194(8) Uani 1 1 d . . .
O51B O 1.1955(4) -0.4540(4) -0.47273(15) 0.0203(8) Uani 1 1 d . . .
O54A O 1.1190(5) -0.9008(4) -0.59067(14) 0.0202(8) Uani 1 1 d . . .
H54A H 1.1169 -0.9733 -0.6124 0.030 Uiso 1 1 calc R . .
O54B O 1.2327(5) -1.0606(4) -0.52123(16) 0.0263(9) Uani 1 1 d . . .
C62 C 0.4872(7) 0.8273(6) 0.1702(3) 0.0294(13) Uani 1 1 d . . .
H62A H 0.5504 0.8779 0.2007 0.035 Uiso 1 1 calc R . .
H62B H 0.3714 0.8636 0.1726 0.035 Uiso 1 1 calc R . .
C63 C 0.5559(6) 0.8578(7) 0.1040(2) 0.0279(13) Uani 1 1 d . . .
H63A H 0.5052 0.7942 0.0748 0.034 Uiso 1 1 calc R . .
H63B H 0.5262 0.9585 0.0901 0.034 Uiso 1 1 calc R . .
N64 N 0.7362(5) 0.8345(4) 0.1007(2) 0.0203(9) Uani 1 1 d . . .
H64A H 0.7833 0.8945 0.1266 0.030 Uiso 1 1 calc R . .
H64B H 0.7723 0.8530 0.0605 0.030 Uiso 1 1 calc R . .
H64C H 0.7639 0.7417 0.1129 0.030 Uiso 1 1 calc R . .
O61 O 0.4969(5) 0.6758(4) 0.18589(19) 0.0304(9) Uani 1 1 d . . .
H61 H 0.4067 0.6406 0.1788 0.046 Uiso 1 1 calc R . .
C71 C 0.9765(6) 0.8854(5) 0.3175(2) 0.0150(10) Uani 1 1 d . . .
C72 C 0.9587(6) 0.7796(5) 0.2682(2) 0.0169(11) Uani 1 1 d . . .
H72 H 0.8514 0.7531 0.2585 0.020 Uiso 1 1 calc R . .
C73 C 1.0840(6) 0.7211(5) 0.2374(2) 0.0181(11) Uani 1 1 d . . .
H73 H 1.1911 0.7463 0.2479 0.022 Uiso 1 1 calc R . .
C74 C 1.0687(6) 0.6181(5) 0.1871(2) 0.0151(10) Uani 1 1 d . . .
O71A O 1.1211(4) 0.8986(4) 0.33852(14) 0.0177(8) Uani 1 1 d . . .
O71B O 0.8533(4) 0.9578(4) 0.33436(15) 0.0208(8) Uani 1 1 d . . .
O74A O 1.1955(4) 0.5602(4) 0.16501(15) 0.0200(8) Uani 1 1 d . . .
O74B O 0.9224(4) 0.5923(4) 0.17175(15) 0.0189(8) Uani 1 1 d . . .
C82 C 0.5054(7) 0.1273(7) 0.3525(3) 0.0302(13) Uani 1 1 d . . .
H82A H 0.5149 0.0397 0.3808 0.036 Uiso 1 1 calc R . .
H82B H 0.3872 0.1501 0.3456 0.036 Uiso 1 1 calc R . .
C83 C 0.5758(7) 0.2471(6) 0.3834(3) 0.0280(13) Uani 1 1 d . . .
H83A H 0.5043 0.2730 0.4195 0.034 Uiso 1 1 calc R . .
H83B H 0.5775 0.3318 0.3534 0.034 Uiso 1 1 calc R . .
N84 N 0.7455(5) 0.2128(5) 0.40615(19) 0.0227(10) Uani 1 1 d . . .
H84A H 0.7419 0.1490 0.4400 0.034 Uiso 1 1 calc R . .
H84B H 0.7907 0.2948 0.4175 0.034 Uiso 1 1 calc R . .
H84C H 0.8075 0.1737 0.3749 0.034 Uiso 1 1 calc R . .
O81 O 0.5834(5) 0.0982(5) 0.29362(16) 0.0342(10) Uani 1 1 d . . .
H81 H 0.6649 0.0412 0.2997 0.051 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 O1A 1.241(6) . ?
C1 O1B 1.292(6) . ?
C1 C2 1.487(7) . ?
C2 C3 1.322(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.473(7) . ?
C3 H3 0.9500 . ?
C4 O4B 1.239(6) . ?
C4 O4A 1.306(5) . ?
O4A H4A 0.8400 . ?
C22 O21 1.407(6) . ?
C22 C23 1.511(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.477(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N24 H24A 0.9100 . ?
N24 H24B 0.9100 . ?
N24 H24C 0.9100 . ?
O21 H21 0.8400 . ?
C31 O31B 1.224(6) . ?
C31 O31A 1.289(6) . ?
C31 C32 1.501(7) . ?
C32 C33 1.320(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.483(7) . ?
C33 H33 0.9500 . ?
C34 O34A 1.219(6) . ?
C34 O34B 1.310(6) . ?
O31A H31A 0.8400 . ?
O34B H34B 0.8400 . ?
C42 O41 1.417(6) . ?
C42 C43 1.508(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 N44 1.487(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
N44 H44A 0.9100 . ?
N44 H44B 0.9100 . ?
N44 H44C 0.9100 . ?
O41 H41 0.8400 . ?
C51 O51A 1.275(6) . ?
C51 O51B 1.274(6) . ?
C51 C52 1.465(7) . ?
C52 C53 1.333(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.474(7) . ?
C53 H53 0.9500 . ?
C54 O54B 1.233(6) . ?
C54 O54A 1.299(5) . ?
O54A H54A 0.8400 . ?
C62 O61 1.433(6) . ?
C62 C63 1.525(7) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 N64 1.478(6) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
N64 H64A 0.9100 . ?
N64 H64B 0.9100 . ?
N64 H64C 0.9100 . ?
O61 H61 0.8400 . ?
C71 O71B 1.242(5) . ?
C71 O71A 1.284(6) . ?
C71 C72 1.493(7) . ?
C72 C73 1.318(7) . ?
C72 H72 0.9500 . ?
C73 C74 1.486(7) . ?
C73 H73 0.9500 . ?
C74 O74A 1.242(5) . ?
C74 O74B 1.281(6) . ?
C82 O81 1.429(6) . ?
C82 C83 1.472(8) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 N84 1.492(7) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
N84 H84A 0.9100 . ?
N84 H84B 0.9100 . ?
N84 H84C 0.9100 . ?
O81 H81 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 123.5(5) . . ?
O1A C1 C2 120.4(4) . . ?
O1B C1 C2 116.1(4) . . ?
C3 C2 C1 123.2(4) . . ?
C3 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
C2 C3 C4 124.6(4) . . ?
C2 C3 H3 117.7 . . ?
C4 C3 H3 117.7 . . ?
O4B C4 O4A 123.6(4) . . ?
O4B C4 C3 121.6(4) . . ?
O4A C4 C3 114.8(4) . . ?
C4 O4A H4A 109.5 . . ?
O21 C22 C23 106.1(5) . . ?
O21 C22 H22A 110.5 . . ?
C23 C22 H22A 110.5 . . ?
O21 C22 H22B 110.5 . . ?
C23 C22 H22B 110.5 . . ?
H22A C22 H22B 108.7 . . ?
N24 C23 C22 110.0(4) . . ?
N24 C23 H23A 109.7 . . ?
C22 C23 H23A 109.7 . . ?
N24 C23 H23B 109.7 . . ?
C22 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C23 N24 H24A 109.5 . . ?
C23 N24 H24B 109.5 . . ?
H24A N24 H24B 109.5 . . ?
C23 N24 H24C 109.5 . . ?
H24A N24 H24C 109.5 . . ?
H24B N24 H24C 109.5 . . ?
C22 O21 H21 109.5 . . ?
O31B C31 O31A 126.0(5) . . ?
O31B C31 C32 119.1(5) . . ?
O31A C31 C32 114.9(4) . . ?
C33 C32 C31 122.8(5) . . ?
C33 C32 H32 118.6 . . ?
C31 C32 H32 118.6 . . ?
C32 C33 C34 122.7(5) . . ?
C32 C33 H33 118.6 . . ?
C34 C33 H33 118.6 . . ?
O34A C34 O34B 124.8(5) . . ?
O34A C34 C33 121.2(5) . . ?
O34B C34 C33 114.0(5) . . ?
C31 O31A H31A 109.5 . . ?
C34 O34B H34B 109.5 . . ?
O41 C42 C43 107.4(4) . . ?
O41 C42 H42A 110.2 . . ?
C43 C42 H42A 110.2 . . ?
O41 C42 H42B 110.2 . . ?
C43 C42 H42B 110.2 . . ?
H42A C42 H42B 108.5 . . ?
N44 C43 C42 110.7(4) . . ?
N44 C43 H43A 109.5 . . ?
C42 C43 H43A 109.5 . . ?
N44 C43 H43B 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
C43 N44 H44A 109.5 . . ?
C43 N44 H44B 109.5 . . ?
H44A N44 H44B 109.5 . . ?
C43 N44 H44C 109.5 . . ?
H44A N44 H44C 109.5 . . ?
H44B N44 H44C 109.5 . . ?
C42 O41 H41 109.5 . . ?
O51A C51 O51B 123.5(5) . . ?
O51A C51 C52 118.2(5) . . ?
O51B C51 C52 118.2(4) . . ?
C53 C52 C51 122.6(4) . . ?
C53 C52 H52 118.7 . . ?
C51 C52 H52 118.7 . . ?
C52 C53 C54 123.8(4) . . ?
C52 C53 H53 118.1 . . ?
C54 C53 H53 118.1 . . ?
O54B C54 O54A 123.2(5) . . ?
O54B C54 C53 121.8(4) . . ?
O54A C54 C53 115.0(4) . . ?
C54 O54A H54A 109.5 . . ?
O61 C62 C63 110.1(5) . . ?
O61 C62 H62A 109.6 . . ?
C63 C62 H62A 109.6 . . ?
O61 C62 H62B 109.6 . . ?
C63 C62 H62B 109.6 . . ?
H62A C62 H62B 108.2 . . ?
N64 C63 C62 112.1(4) . . ?
N64 C63 H63A 109.2 . . ?
C62 C63 H63A 109.2 . . ?
N64 C63 H63B 109.2 . . ?
C62 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C63 N64 H64A 109.5 . . ?
C63 N64 H64B 109.5 . . ?
H64A N64 H64B 109.5 . . ?
C63 N64 H64C 109.5 . . ?
H64A N64 H64C 109.5 . . ?
H64B N64 H64C 109.5 . . ?
C62 O61 H61 109.5 . . ?
O71B C71 O71A 124.1(5) . . ?
O71B C71 C72 118.8(4) . . ?
O71A C71 C72 117.1(4) . . ?
C73 C72 C71 123.4(5) . . ?
C73 C72 H72 118.3 . . ?
C71 C72 H72 118.3 . . ?
C72 C73 C74 124.2(5) . . ?
C72 C73 H73 117.9 . . ?
C74 C73 H73 117.9 . . ?
O74A C74 O74B 125.0(4) . . ?
O74A C74 C73 118.7(4) . . ?
O74B C74 C73 116.3(4) . . ?
O81 C82 C83 113.2(5) . . ?
O81 C82 H82A 108.9 . . ?
C83 C82 H82A 108.9 . . ?
O81 C82 H82B 108.9 . . ?
C83 C82 H82B 108.9 . . ?
H82A C82 H82B 107.8 . . ?
C82 C83 N84 113.1(5) . . ?
C82 C83 H83A 109.0 . . ?
N84 C83 H83A 109.0 . . ?
C82 C83 H83B 109.0 . . ?
N84 C83 H83B 109.0 . . ?
H83A C83 H83B 107.8 . . ?
C83 N84 H84A 109.5 . . ?
C83 N84 H84B 109.5 . . ?
H84A N84 H84B 109.5 . . ?
C83 N84 H84C 109.5 . . ?
H84A N84 H84C 109.5 . . ?
H84B N84 H84C 109.5 . . ?
C82 O81 H81 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
N24 H24C O74A  0.91 1.91 2.791(5) 162.8 .
O31A H31A O1B  0.84 1.61 2.441(5) 171.3 .
O31A H31A O1A  0.84 2.65 3.158(5) 120.7 .
O34B H34B O51A  0.84 1.69 2.519(5) 170.8 .
O41 H41 O61  0.84 2.02 2.825(6) 159.5 .
N64 H64C O74B  0.91 2.21 3.019(5) 147.2 .
N64 H64C O4B  0.91 2.46 2.996(5) 117.6 .
O4A H4A O74B  0.84 1.65 2.460(5) 162.7 .
N24 H24A O31A  0.91 2.07 2.945(5) 159.9 2_755
N84 H84B O51B  0.91 1.95 2.788(6) 151.9 2_755
N84 H84B O34B  0.91 2.51 2.959(6) 111.1 2_755
N24 H24B O4B  0.91 2.02 2.847(5) 150.9 2_765
N64 H64A O31B  0.91 1.90 2.786(6) 165.0 2_765
O21 H21 O81  0.84 1.91 2.726(5) 163.8 1_655
N44 H44A O71A  0.91 2.03 2.905(5) 162.2 1_455
O61 H61 O74A  0.84 1.95 2.785(5) 178.2 1_455
N44 H44B O51B  0.91 1.92 2.823(5) 169.2 1_466
N44 H44C O34A  0.91 1.98 2.863(6) 163.3 2_655
N64 H64B O1A  0.91 1.93 2.792(5) 157.8 1_565
O54A H54A O71A  0.84 1.63 2.465(5) 173.1 1_534
O54A H54A O71B  0.84 2.58 3.101(5) 121.8 1_534
N84 H84A O54B  0.91 1.89 2.770(5) 162.8 2_745
N84 H84C O71B  0.91 2.25 2.985(6) 138.1 1_545
O81 H81 O71B  0.84 1.84 2.647(5) 160.6 1_545
 
_diffrn_measured_fraction_theta_max    0.914
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.914
_refine_diff_density_max    0.838
_refine_diff_density_min   -0.631
_refine_diff_density_rms    0.153
