data_global 
_audit_creation_date        "13-09-19"
_audit_creation_method CRYSTALS_ver_14.40

_oxford_structure_analysis_title  'KAT1_0m in C2'
_chemical_name_systematic         'valine-isoleucine co-crystal 0.75:0.25 ratio'
_chemical_melting_point           ?

#looking for refcif 
 
 
# Check this file using the IUCr facility at: 
# http://checkcif.iucr.org/ 
 
;

089_ALERT_3_B Poor Data / Parameter Ratio (Zmax .LT. 18) .....       5.75
097_ALERT_2_B Large Reported Max.  (Positive) Residual Density       0.84 eA-3
094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       3.82
223_ALERT_4_C Large Solvent/Anion  H     Ueq(max)/Ueq(min) ...       3.25 Ratio
250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.04
340_ALERT_3_C Low Bond Precision on  C-C Bonds (x 1000) Ang ..          8
351_ALERT_3_C Long    C-H Bond (0.96A)   C52    -   H523   ...       1.12 Ang.
414_ALERT_2_C Short Intra D-H..H-X       H111   ..  H521    ..       1.90 Ang.
758_ALERT_4_C D-H..A  Calc      176.00, Rep  176.15(19) ......  Senseless su
              N13  -H133 -O12     1.555   1.555   1.555      #         72
231_ALERT_4_G Hirshfeld Test (Solvent)   O22    --  C12     ..       6.50 su
301_ALERT_3_G Note: Main Residue  Disorder ...................       6.00 Perc.

              
              
There are a number of distance, thermal and vibrational restraints used to keep the model 
chemically reasonable. This data was collected using the National Crystallography Service 
and is the best data that can be taken.  The decision was taken to model the anisotropic thermal
parameters for both molecules which means that the data:parameter ratio falls below the recommended
level.  This is due to the crystals being weakly diffracting. The large residual density is found 
close to the oxygen atom to make chemical sense
even as a disorder component.
             
                           
              
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          4
912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600          2

The data are complete to 99.7% complete to the Acta Min Resolution. 

             
 ===============================================================================
Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged)
===============================================================================
Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.82     0.500     0.996          794      791        3
 23.01     0.550     0.996         1041     1037        4
 25.24     0.600     0.997         1340     1336        4
------------------------------------------------------------ ACTA Min. Res. ---
 26.37     0.625     0.996         1509     1503        6             
              
                            
791_ALERT_4_G The Model has Chirality at C21     (Verify) ....          S
791_ALERT_4_G The Model has Chirality at C22     (Verify) ....          S
791_ALERT_4_G The Model has Chirality at C31     (Verify) ....          S

The solids were both S-handed but the main point of the study is that the
realtive hands were the same as each other.              
              
              
              
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C11 H24 N2 O4
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?
808_ALERT_5_G No Parsable SHELXL style Weighting Scheme Found           !
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found          ?
960_ALERT_3_G Number of Intensities with I .LT. - 2*sig(I) ..           3


Noted. No action taken.




;
data_3 
_cell_length_a                    26.142(6)
_cell_length_b                    5.2621(12)
_cell_length_c                    9.688(2)
_cell_angle_alpha                 90
_cell_angle_beta                  96.961(7)
_cell_angle_gamma                 90
_cell_volume                      1322.9(5)
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'C 1 2 1 ' 
_symmetry_space_group_name_Hall   'C 2y' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 'x+1/2,y+1/2,z'
 '-x,y,-z'
 '-x+1/2,y+1/2,-z'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 C       0.0033   0.0016   2.3100  20.8439   1.0200  10.2075   1.5886   0.5687
   0.8650  51.6512   0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 H       0.0000   0.0000   0.4930  10.5109   0.3229  26.1257   0.1402   3.1424
   0.0408  57.7998   0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 N       0.0061   0.0033  12.2126   0.0057   3.1322   9.8933   2.0125  28.9975
   1.1663   0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    2

# Given Formula = C22 H48 N4 O8 
# Dc =      1.25 Fooo =    528.00 Mu =      0.94 M =    248.32
# Found Formula = C21 H46 N4 O8 
# Dc =      1.21 FOOO =    528.00 Mu =      0.92 M =    241.31

_chemical_formula_sum             'C21 H46 N4 O8'
_chemical_formula_moiety          'C11 H24 N2 O4, 2(C5 H11 N O2)'
_chemical_compound_source                ?
_chemical_formula_weight            482.62
 
 
_cell_measurement_reflns_used         1230
_cell_measurement_theta_min              3
_cell_measurement_theta_max             25
_cell_measurement_temperature          100
 
_exptl_crystal_description        'platelet' 
_exptl_crystal_colour             'colourless' 
_exptl_crystal_size_min           0.100 
_exptl_crystal_size_mid           0.100 
_exptl_crystal_size_max           0.200 
 
_exptl_crystal_density_diffrn     1.212 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              528 
_exptl_absorpt_coefficient_mu     0.092 
 
# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' 
_exptl_absorpt_correction_T_min   0.70 
_exptl_absorpt_correction_T_max   0.99 
_diffrn_source                          'Rotating Anode'
_diffrn_radiation_monochromator         'Confocal'
_diffrn_radiation_type                  'Molybdenum'
_diffrn_radiation_wavelength           0.71075
_diffrn_measurement_method        \w 
 
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method        \w 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_structure_solution     'SIR92 (Altomare et al., 1994)' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        100
_diffrn_reflns_number             4784 
_reflns_number_total              1504 
_diffrn_reflns_av_R_equivalents   0.071 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 1504 
# Theoretical number of reflections is about 2706 
 
 
_diffrn_reflns_theta_min          1.569 
_diffrn_reflns_theta_max          26.374 
_diffrn_measured_fraction_theta_max 0.997 
 
_diffrn_reflns_theta_full         26.374 
_diffrn_measured_fraction_theta_full 0.997 
 
 
_diffrn_reflns_limit_h_min        -32 
_diffrn_reflns_limit_h_max        32 
_diffrn_reflns_limit_k_min        -6 
_diffrn_reflns_limit_k_max        5 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        10 
_reflns_limit_h_min               -32 
_reflns_limit_h_max               32 
_reflns_limit_k_min               0 
_reflns_limit_k_max               6 
_reflns_limit_l_min               0 
_reflns_limit_l_max               12 
 
_oxford_diffrn_Wilson_B_factor    2.40 
_oxford_diffrn_Wilson_scale       33.42 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.22 
_refine_diff_density_max          0.84 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>3.0\s(I)
_refine_ls_number_reflns          885 
_refine_ls_number_restraints      0 
_refine_ls_number_parameters      154 
_oxford_refine_ls_R_factor_ref    0.0613 
_refine_ls_wR_factor_ref          0.0688 
_refine_ls_goodness_of_fit_ref    1.1644 
_refine_ls_shift/su_max           0.0001219 
_refine_ls_shift/su_mean          0.0000105 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         1496 
_refine_ls_R_factor_all           0.1033 
_refine_ls_wR_factor_all          0.1174 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0\s(I)
_reflns_number_gt                 1024 
_refine_ls_R_factor_gt            0.0687 
_refine_ls_wR_factor_gt           0.0742 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  'unk' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     constr         #undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.619 0.611 0.328 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined data collection reference 
 
User defined data reduction 
 
User defined cell refinement 
 
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., 
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, 
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. 
New York: Academic Press. 
 
Prince, E. 
Mathematical Techniques in Crystallography 
and Materials Science 
Springer-Verlag, New York, 1982. 
 
Watkin D.J. (1994). 
Acta Cryst, A50, 411-437. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O11 O 0.29652(15) -0.0312(8) 1.3870(3) 0.0301 1.0000 Uani . . . . . . 
O21 O 0.32358(16) -0.4067(9) 1.3180(3) 0.0312 1.0000 Uani . . . . . . 
C11 C 0.3116(2) -0.1753(11) 1.2972(5) 0.0254 1.0000 Uani . . . . . . 
C21 C 0.3202(2) -0.0638(10) 1.1570(5) 0.0272 1.0000 Uani . . . . . . 
C31 C 0.3782(2) -0.0218(12) 1.1402(5) 0.0305 1.0000 Uani . . . . . . 
C41 C 0.4082(2) 0.0854(14) 1.2749(6) 0.0350 1.0000 Uani . . . . . . 
C51 C 0.4018(3) -0.2710(13) 1.0968(6) 0.0395 1.0000 Uani . . . . . . 
C61 C 0.4579(5) -0.256(3) 1.0746(14) 0.0489 0.5000 Uani . . . . 1 . 
O12 O 0.29930(16) 0.3790(8) 0.8730(4) 0.0282 1.0000 Uani . . . . . . 
C12 C 0.3146(2) 0.2211(14) 0.7895(5) 0.0320 1.0000 Uani . . . . . . 
O22 O 0.31350(17) -0.0148(9) 0.7981(4) 0.0334 1.0000 Uani . . . . . . 
C22 C 0.3388(2) 0.3435(11) 0.6647(5) 0.0292 1.0000 Uani . . . . . . 
N12 N 0.30737(19) 0.5645(10) 0.6106(4) 0.0310 1.0000 Uani . . . . . . 
C32 C 0.3943(2) 0.4307(12) 0.7122(6) 0.0340 1.0000 Uani . . . . . . 
C52 C 0.4192(3) 0.5504(17) 0.5946(6) 0.0569 1.0000 Uani . . . . . . 
C42 C 0.4285(3) 0.2085(18) 0.7763(9) 0.0622 1.0000 Uani . . . . . . 
N11 N 0.29143(18) 0.1807(10) 1.1365(4) 0.0258 1.0000 Uani . . . . . . 
H211 H 0.3055 -0.1848 1.0848 0.0313 1.0000 Uiso R . . . . . 
H311 H 0.3799 0.1052 1.0651 0.0312 1.0000 Uiso R . . . . . 
H413 H 0.4418 0.1471 1.2551 0.0540 1.0000 Uiso R . . . . . 
H412 H 0.3890 0.2200 1.3127 0.0540 1.0000 Uiso R . . . . . 
H411 H 0.4135 -0.0485 1.3441 0.0539 1.0000 Uiso R . . . . . 
H511 H 0.3807 -0.3354 1.0133 0.0491 1.0000 Uiso R . . . . . 
H512 H 0.4012 -0.3949 1.1721 0.0492 1.0000 Uiso R . . . . . 
H613 H 0.4670 -0.4127 1.0269 0.0790 0.5000 Uiso R . . . 1 . 
H612 H 0.4602 -0.1165 1.0056 0.0790 0.5000 Uiso R . . . 1 . 
H611 H 0.4794 -0.2276 1.1540 0.0790 0.5000 Uiso R . . . 1 . 
H221 H 0.3389 0.2145 0.5910 0.0321 1.0000 Uiso R . . . . . 
H321 H 0.3938 0.5617 0.7863 0.0394 1.0000 Uiso R . . . . . 
H523 H 0.4576 0.6302 0.6373 0.0925 1.0000 Uiso R . . . . . 
H522 H 0.4213 0.4083 0.5162 0.0931 1.0000 Uiso R . . . . . 
H521 H 0.3941 0.6993 0.5563 0.0933 1.0000 Uiso R . . . . . 
H421 H 0.4645 0.2516 0.7875 0.1040 1.0000 Uiso R . . . . . 
H422 H 0.4229 0.0619 0.7167 0.1039 1.0000 Uiso R . . . . . 
H423 H 0.4189 0.1620 0.8690 0.1042 1.0000 Uiso R . . . . . 
H113 H 0.2955 0.2466 1.0523 0.0361 1.0000 Uiso R . . . . . 
H112 H 0.2571 0.1573 1.1387 0.0363 1.0000 Uiso R . . . . . 
H114 H 0.3035 0.2943 1.2018 0.0360 1.0000 Uiso R . . . . . 
H513 H 0.4364 -0.2437 1.0783 0.0487 0.5000 Uiso R . . . 2 . 
H121 H 0.3220 0.6391 0.5349 0.0351 1.0000 Uiso R . . . . . 
H122 H 0.2732 0.5081 0.5796 0.0351 1.0000 Uiso R . . . . . 
H123 H 0.3064 0.6872 0.6824 0.0351 1.0000 Uiso R . . . . . 
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O11 0.047(2) 0.023(2) 0.0212(17) 0.0038(17) 0.0084(15) 0.001(2) 
O21 0.057(3) 0.016(2) 0.0213(17) 0.0016(17) 0.0067(17) -0.002(2) 
C11 0.037(3) 0.023(3) 0.017(2) -0.002(2) 0.006(2) -0.005(3) 
C21 0.049(4) 0.013(3) 0.020(2) 0.004(2) 0.005(2) -0.002(3) 
C31 0.043(3) 0.028(3) 0.021(2) 0.005(2) 0.006(2) 0.001(3) 
C41 0.047(4) 0.028(3) 0.031(3) 0.004(3) 0.006(2) 0.002(3) 
C51 0.056(4) 0.036(4) 0.029(3) 0.000(3) 0.013(3) 0.011(4) 
C61 0.053(8) 0.048(9) 0.048(7) -0.010(6) 0.016(6) 0.021(8) 
O12 0.044(2) 0.021(2) 0.0223(17) 0.0032(16) 0.0130(15) 0.0032(18) 
C12 0.039(3) 0.041(5) 0.018(2) 0.000(3) 0.007(2) 0.003(3) 
O22 0.053(3) 0.015(2) 0.034(2) 0.0016(18) 0.0114(19) 0.000(2) 
C22 0.050(4) 0.021(3) 0.017(2) -0.001(2) 0.006(2) 0.001(3) 
N12 0.041(3) 0.027(3) 0.026(2) 0.008(2) 0.006(2) -0.008(3) 
C32 0.045(3) 0.029(4) 0.030(3) 0.002(2) 0.013(2) 0.002(3) 
C52 0.061(4) 0.076(6) 0.036(3) 0.000(4) 0.016(3) -0.023(5) 
C42 0.045(4) 0.062(5) 0.083(5) 0.025(5) 0.022(4) 0.007(4) 
N11 0.042(3) 0.020(3) 0.0174(19) 0.0029(17) 0.0089(19) -0.008(2) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.1824(11) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
O11 . C11 . 1.254(7)    yes
O21 . C11 . 1.268(7)    yes
C11 . C21 . 1.521(7)    yes
C21 . C31 . 1.561(8)    yes
C21 . N11 . 1.491(8)    yes
C21 . H211 . 0.988    no
C31 . C41 . 1.545(8)    yes
C31 . C51 . 1.529(9)    yes
C31 . H311 . 0.993    no
C41 . H413 . 0.977    no
C41 . H412 . 0.966    no
C41 . H411 . 0.971    no
C51 . C61 . 1.511(15)    yes
C51 . H511 . 0.983    no
C51 . H512 . 0.980    no
C61 . H613 . 0.986    no
C61 . H612 . 1.001    no
C61 . H611 . 0.909    no
O12 . C12 . 1.258(7)    yes
C12 . O22 . 1.244(8)    yes
C12 . C22 . 1.569(7)    yes
C22 . N12 . 1.482(8)    yes
C22 . C32 . 1.538(9)    yes
C22 . H221 . 0.985    no
N12 . H121 . 0.951    no
N12 . H122 . 0.954    no
N12 . H123 . 0.952    no
C32 . C52 . 1.517(8)    yes
C32 . C42 . 1.555(11)    yes
C32 . H321 . 0.996    no
C52 . H523 . 1.119    no
C52 . H522 . 1.072    no
C52 . H521 . 1.060    no
C42 . H421 . 0.962    no
C42 . H422 . 0.964    no
C42 . H423 . 0.993    no
N11 . H113 . 0.904    no
N11 . H112 . 0.908    no
N11 . H114 . 0.900    no
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O21 . C11 . O11 . 124.2(5)    yes
O21 . C11 . C21 . 116.9(5)    yes
O11 . C11 . C21 . 118.7(5)    yes
C11 . C21 . C31 . 113.4(4)    yes
C11 . C21 . N11 . 109.0(4)    yes
C31 . C21 . N11 . 110.2(4)    yes
C11 . C21 . H211 . 107.2    no
C31 . C21 . H211 . 108.6    no
N11 . C21 . H211 . 108.3    no
C21 . C31 . C41 . 111.4(4)    yes
C21 . C31 . C51 . 109.6(5)    yes
C41 . C31 . C51 . 111.4(5)    yes
C21 . C31 . H311 . 107.4    no
C41 . C31 . H311 . 108.1    no
C51 . C31 . H311 . 108.7    no
C31 . C41 . H413 . 109.4    no
C31 . C41 . H412 . 110.7    no
H413 . C41 . H412 . 110.7    no
C31 . C41 . H411 . 109.5    no
H413 . C41 . H411 . 108.7    no
H412 . C41 . H411 . 107.9    no
C31 . C51 . C61 . 115.2(8)    yes
C31 . C51 . H511 . 108.5    no
C61 . C51 . H511 . 111.0    no
C31 . C51 . H512 . 108.8    no
C61 . C51 . H512 . 104.1    no
H511 . C51 . H512 . 109.0    no
C51 . C61 . H613 . 108.5    no
C51 . C61 . H612 . 105.6    no
H613 . C61 . H612 . 105.3    no
C51 . C61 . H611 . 113.5    no
H613 . C61 . H611 . 112.1    no
H612 . C61 . H611 . 111.3    no
O12 . C12 . O22 . 127.2(6)    yes
O12 . C12 . C22 . 114.4(6)    yes
O22 . C12 . C22 . 118.4(5)    yes
C12 . C22 . N12 . 109.7(5)    yes
C12 . C22 . C32 . 110.2(4)    yes
N12 . C22 . C32 . 109.5(5)    yes
C12 . C22 . H221 . 108.2    no
N12 . C22 . H221 . 109.5    no
C32 . C22 . H221 . 109.6    no
C22 . N12 . H121 . 109.9    no
C22 . N12 . H122 . 108.9    no
H121 . N12 . H122 . 109.5    no
C22 . N12 . H123 . 109.6    no
H121 . N12 . H123 . 109.4    no
H122 . N12 . H123 . 109.5    no
C22 . C32 . C52 . 112.0(5)    yes
C22 . C32 . C42 . 111.8(6)    yes
C52 . C32 . C42 . 109.5(6)    yes
C22 . C32 . H321 . 109.1    no
C52 . C32 . H321 . 107.3    no
C42 . C32 . H321 . 106.9    no
C32 . C52 . H523 . 109.0    no
C32 . C52 . H522 . 107.8    no
H523 . C52 . H522 . 113.8    no
C32 . C52 . H521 . 105.4    no
H523 . C52 . H521 . 110.0    no
H522 . C52 . H521 . 110.5    no
C32 . C42 . H421 . 112.1    no
C32 . C42 . H422 . 108.9    no
H421 . C42 . H422 . 109.4    no
C32 . C42 . H423 . 110.5    no
H421 . C42 . H423 . 107.9    no
H422 . C42 . H423 . 107.9    no
C21 . N11 . H113 . 109.8    no
C21 . N11 . H112 . 111.3    no
H113 . N11 . H112 . 107.4    no
C21 . N11 . H114 . 110.5    no
H113 . N11 . H114 . 108.0    no
H112 . N11 . H114 . 109.7    no
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_site_symmetry_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_site_symmetry_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_A
 _geom_hbond_angle_DHA
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_publ_flag
C22 . H221 . O11 1_554 152.53(16) 0.985 2.505 3.410(10)    yes
N11 . H113 . O12 . 176.15(19) 0.904 1.885 2.788(10)    yes
N11 . H112 . O12 4_547 142.47(17) 0.908 2.072 2.847(10)    yes
N11 . H114 . O21 1_565 168.50(17) 0.900 1.968 2.856(10)    yes
N12 . H121 . O11 1_564 132.83(15) 0.951 2.296 3.025(10)    yes
N12 . H121 . O21 1_564 140.78(18) 0.951 2.121 2.920(10)    yes
N12 . H121 . C11 1_564 150.16(17) 0.951 2.486 3.345(10)    yes
N12 . H122 . O11 4_557 149.35(18) 0.954 1.901 2.765(10)    yes
N12 . H123 . O22 1_565 165.89(18) 0.952 1.924 2.856(10)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/09/13 at 17:37:13
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  41,X'S) H   ( 413,X'S) H   ( 412,X'S) H   ( 411,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  61,X'S) H   ( 613,X'S) H   ( 612,X'S) H   ( 611,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE N   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  52,X'S) H   ( 523,X'S) H   ( 522,X'S) H   ( 521,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) H   ( 423,X'S) 
RIDE N   (  13,X'S) H   ( 133,X'S) H   ( 132,X'S) H   ( 134,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/09/13 at 17:37:13
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
  -4   0   4  x   .
END
