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

_oxford_structure_analysis_title  'shelx in P2(1)'
_chemical_name_systematic         'Leucine-isoleucine co-crystal 0.40:0.60 ratio'
_chemical_melting_point           ?

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

220_ALERT_2_B Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       4.11 Ratio
222_ALERT_3_B Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       4.11 Ratio
220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...       3.51 Ratio
222_ALERT_3_C Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       3.88 Ratio
242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C31
301_ALERT_3_G Note: Main Residue  Disorder ...................      22.00 Perc.
860_ALERT_3_G Note: Number of Least-Squares Restraints .......        180
737_ALERT_1_C D...A   Calc    2.759(2), Rep    2.759(6) ......       3.00 su-Ra
              N12  -O11     1.555   2.354
737_ALERT_1_C D...A   Calc    2.974(2), Rep    2.974(6) ......       3.00 su-Ra
              N11  -O22     1.555   2.454
737_ALERT_1_C D...A   Calc    2.763(2), Rep    2.763(6) ......       3.00 su-Ra
              N11  -O12     1.555   1.555
758_ALERT_4_C D-H..A  Calc      150.00, Rep   149.84(5) ......  Senseless su
              N12  -H122 -O11     1.555   1.555   1.555
758_ALERT_4_C D-H..A  Calc      157.00, Rep   156.89(5) ......  Senseless su
              N11  -H112 -O12     1.555   1.555   1.555

Due to the disorder present in the structure there are a number of distance, thermal
and vibrational restraints used to keep the model chemically reasonable.           


910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          1
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          8
912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600        138

The data are 99.4 % complete to the Acta Min. Resolution. See below

==============================================================================
Resolution & Completeness Statistics   (Cumulative and Friedel Pairs Averaged)
===============================================================================
Theta sin(th)/Lambda Complete  Expected Measured  Missing
-------------------------------------------------------------------------------
 20.15     0.500     0.990          863      854        9
 22.27     0.550     0.991         1131     1121       10
 24.41     0.600     0.994         1468     1459        9
------------------------------------------------------------ ACTA Min. Res. ---
 26.60     0.650     0.995         1839     1830        9
 28.83     0.700     0.996         2288     2278       10
 31.11     0.750     0.982         2788     2737       51
 31.68     0.762     0.950         2929     2782      147
              
              
791_ALERT_4_G The Model has Chirality at C21     (Verify) ....          S
791_ALERT_4_G The Model has Chirality at C31     (Verify) ....          S
791_ALERT_4_G The Model has Chirality at C33     (Verify) ....          S

The solids were are supplied as teh S-hand however the main point is that both 
moelcules are of the same hand as opposed to R and S.

790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C6 H13 N O2
790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          2
              C6 H13 N O2
092_ALERT_4_G Check: Wavelength given is not Cu,Mo or Ag Ka ..       0.69 Ang.
760_ALERT_1_G CIF Contains no Torsion Angles .................          ?
795_ALERT_4_G C-Atom in CIF Coordinate List out of Sequence ..        C12
796_ALERT_4_G O-Atom in CIF Coordinate List out of Sequence ..        O12
808_ALERT_5_G No Parsable SHELXL style Weighting Scheme Found           !
811_ALERT_5_G No ADDSYM Analysis: Too Many Excluded Atoms ....          !
929_ALERT_4_G No Interpretable (SHELX) Weight Parameters found          ?

Noted. No action taken




 
# The content below is held in the file 'script/refcif.dat'. This is a text 
# file which you may edit to reflect local conditions. 
# Items which need looking at are represented by a '?'. 
# Items for which there are choices are prefixed with 'choose from'. 
 

 
data_1
_cell_length_a                    9.633(5)
_cell_length_b                    5.281(3)
_cell_length_c                    14.669(7)
_cell_angle_alpha                 90
_cell_angle_beta                  104.410(4)
_cell_angle_gamma                 90
_cell_volume                      722.8(6)
 
_symmetry_cell_setting            'monoclinic' 
_symmetry_space_group_name_H-M    'P 1 21 1 ' 
_symmetry_space_group_name_Hall   'P 2yb' 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 '-x,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                    4

# Given Formula = C9 H18 N1 O2 
# Dc =      1.58 Fooo =    288.00 Mu =      1.10 M =    344.49
# Found Formula = C6 H13 N1 O2 
# Dc =      1.21 FOOO =    288.00 Mu =      0.89 M =    262.35

_chemical_formula_sum             'C6 H13 N1 O2'
_chemical_formula_moiety          'C6 H13 N1 O2'
_chemical_compound_source                ?
_chemical_formula_weight            131.17
 
 
_cell_measurement_reflns_used         2519
_cell_measurement_theta_min              2
_cell_measurement_theta_max             32
_cell_measurement_temperature          123
 
_exptl_crystal_description        'needle' 
_exptl_crystal_colour             'pale yellow' 
_exptl_crystal_size_min           0.010 
_exptl_crystal_size_mid           0.050 
_exptl_crystal_size_max           0.050 
 
_exptl_crystal_density_diffrn     1.205 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              288 
_exptl_absorpt_coefficient_mu     0.089 
 
# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_process_details    'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' 
_exptl_absorpt_correction_T_min   0.94 
_exptl_absorpt_correction_T_max   1.00 
_diffrn_measurement_device_type   'Rigaku Saturn724+ (2x2 bin mode)' 
_diffrn_measurement_device        'CrystalLogic Kappa (3 circle)' 
_diffrn_radiation_monochromator   'Synchrotron' 
_diffrn_radiation_type            'Synchrotron'
_diffrn_radiation_wavelength           0.68890
_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        123
_diffrn_reflns_number             15890 
_reflns_number_total              2783 
_diffrn_reflns_av_R_equivalents   0.028 
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2783 
# Theoretical number of reflections is about 5367 
 
 
_diffrn_reflns_theta_min          2.116 
_diffrn_reflns_theta_max          31.683 
_diffrn_measured_fraction_theta_max 0.950 
 
_diffrn_reflns_theta_full         27.564 
_diffrn_measured_fraction_theta_full 0.997 
 
 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        22 
_reflns_limit_h_min               -14 
_reflns_limit_h_max               14 
_reflns_limit_k_min               0 
_reflns_limit_k_max               8 
_reflns_limit_l_min               0 
_reflns_limit_l_max               22 
 
_oxford_diffrn_Wilson_B_factor    2.34 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    difmap
 
_refine_diff_density_min          -0.35 
_refine_diff_density_max          0.41 
 
 
# 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          2447 
_refine_ls_number_restraints      180 
_refine_ls_number_parameters      210 
_oxford_refine_ls_R_factor_ref    0.0548 
_refine_ls_wR_factor_ref          0.0466 
_refine_ls_goodness_of_fit_ref    1.2660 
_refine_ls_shift/su_max           0.0003438 
_refine_ls_shift/su_mean          0.0000278 
 
 
# The values computed with all filters except I/sigma 
_oxford_reflns_number_all         2776 
_refine_ls_R_factor_all           0.0624 
_refine_ls_wR_factor_all          0.0494 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0\s(I)
_reflns_number_gt                 2622 
_refine_ls_R_factor_gt            0.0586 
_refine_ls_wR_factor_gt           0.0479 
 
# 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: 
 13.5 -10.6 8.39 
;
# 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 -0.82351(10) -0.8447(3) -0.41098(8) 0.0259 1.0000 Uani . U . . . . 
O21 O -0.73427(14) -1.2343(3) -0.38134(10) 0.0365 1.0000 Uani . U . . . . 
C11 C -0.72206(14) -0.9999(4) -0.38258(11) 0.0246 1.0000 Uani . U . . . . 
N11 N -0.55638(14) -0.6553(4) -0.39697(10) 0.0310 1.0000 Uani . U . . . . 
C21 C -0.57357(15) -0.8846(4) -0.34191(12) 0.0299 1.0000 Uani D U . . . . 
C31 C -0.5581(2) -0.8112(5) -0.23673(13) 0.0411 1.0000 Uani D U . . . . 
C12 C -0.76752(14) -0.9057(4) -0.61461(10) 0.0223 1.0000 Uani . U . . . . 
C41 C -0.4160(3) -0.6855(7) -0.19226(17) 0.0672 1.0000 Uani D U . . . . 
C61 C -0.3909(5) -0.6163(10) -0.09028(19) 0.1010 1.0000 Uani D U . . . . 
O12 O -0.66092(10) -0.7632(3) -0.58595(8) 0.0269 1.0000 Uani . U . . . . 
O22 O -0.76004(11) -1.1374(3) -0.63126(8) 0.0293 1.0000 Uani . U . . . . 
C22 C -0.91634(14) -0.7837(4) -0.63377(10) 0.0237 1.0000 Uani D U . . . . 
N12 N -0.90949(12) -0.5530(4) -0.57549(9) 0.0242 1.0000 Uani . U . . . . 
C62 C -0.9978(7) -0.7515(14) -0.9087(3) 0.0782 0.569(4) Uani D U P . 2 . 
C42 C -0.9783(4) -0.8799(8) -0.8135(2) 0.0424 0.569(4) Uani D U P . 2 . 
C52 C -1.1054(5) -1.0507(9) -0.8150(4) 0.0550 0.569(4) Uani D U P . 2 . 
C32 C -0.9587(5) -0.6779(10) -0.7374(3) 0.0325 0.569(4) Uani D U P . 2 . 
C63 C -1.1348(6) -0.9789(13) -0.8853(4) 0.0569 0.431(4) Uani D U P . 3 . 
C53 C -1.0489(5) -1.0063(10) -0.7830(3) 0.0381 0.431(4) Uani D U P . 3 . 
C43 C -0.8842(4) -0.6320(9) -0.7874(3) 0.0340 0.431(4) Uani D U P . 3 . 
C33 C -0.9870(6) -0.7545(11) -0.7377(4) 0.0270 0.431(4) Uani D U P . 3 . 
C51 C -0.5801(6) -1.0338(9) -0.1780(2) 0.0832 0.778(7) Uani D U P . 1 . 
C54 C -0.3125(11) -0.903(4) -0.1670(10) 0.0832 0.222(7) Uani D U P . 4 . 
H211 H -0.5023 -1.0080 -0.3537 0.0377 1.0000 Uiso R . . . . . 
H612 H -0.3121 -0.4991 -0.0732 0.1485 1.0000 Uiso R . . . . . 
H611 H -0.3698 -0.7618 -0.0470 0.1486 1.0000 Uiso R . . . . . 
H613 H -0.4787 -0.5405 -0.0788 0.1481 1.0000 Uiso R . . . . . 
H621 H -0.9222 -0.6303 -0.9014 0.1160 0.569(4) Uiso R . P . 2 . 
H622 H -0.9915 -0.8787 -0.9530 0.1163 0.569(4) Uiso R . P . 2 . 
H623 H -1.0894 -0.6695 -0.9242 0.1156 0.569(4) Uiso R . P . 2 . 
H421 H -0.8911 -0.9837 -0.8045 0.0478 0.569(4) Uiso R . P . 2 . 
H522 H -1.0965 -1.1260 -0.7533 0.0800 0.569(4) Uiso R . P . 2 . 
H521 H -1.1072 -1.1804 -0.8621 0.0800 0.569(4) Uiso R . P . 2 . 
H523 H -1.1912 -0.9528 -0.8326 0.0804 0.569(4) Uiso R . P . 2 . 
H321 H -1.0466 -0.5811 -0.7440 0.0397 0.569(4) Uiso R . P . 2 . 
H322 H -0.8849 -0.5640 -0.7439 0.0396 0.569(4) Uiso R . P . 2 . 
H631 H -1.1860 -1.1339 -0.9078 0.0890 0.431(4) Uiso R . P . 3 . 
H632 H -1.2023 -0.8416 -0.8930 0.0887 0.431(4) Uiso R . P . 3 . 
H633 H -1.0693 -0.9456 -0.9231 0.0889 0.431(4) Uiso R . P . 3 . 
H531 H -1.1124 -1.0729 -0.7459 0.0510 0.431(4) Uiso R . P . 3 . 
H532 H -0.9722 -1.1255 -0.7795 0.0511 0.431(4) Uiso R . P . 3 . 
H431 H -0.9343 -0.5508 -0.8463 0.0569 0.431(4) Uiso R . P . 3 . 
H432 H -0.8226 -0.7603 -0.8033 0.0573 0.431(4) Uiso R . P . 3 . 
H433 H -0.8247 -0.5101 -0.7477 0.0574 0.431(4) Uiso R . P . 3 . 
H331 H -1.0687 -0.6384 -0.7412 0.0372 0.431(4) Uiso R . P . 3 . 
H511 H -0.5816 -0.9818 -0.1154 0.1351 0.778(7) Uiso R . P . 1 . 
H512 H -0.6657 -1.1185 -0.2069 0.1349 0.778(7) Uiso R . P . 1 . 
H513 H -0.5028 -1.1493 -0.1756 0.1349 0.778(7) Uiso R . P . 1 . 
H541 H -0.2266 -0.8521 -0.1221 0.1530 0.222(7) Uiso R . P . 4 . 
H543 H -0.2887 -0.9564 -0.2238 0.1531 0.222(7) Uiso R . P . 4 . 
H542 H -0.3559 -1.0418 -0.1424 0.1530 0.222(7) Uiso R . P . 4 . 
H123 H -0.9980 -0.4942 -0.5798 0.0387 1.0000 Uiso R . . . . . 
H122 H -0.8693 -0.5929 -0.5128 0.0381 1.0000 Uiso R . . . . . 
H221 H -0.9904 -0.9021 -0.6231 0.0300 1.0000 Uiso R . . . . . 
H121 H -0.8549 -0.4380 -0.5965 0.0392 1.0000 Uiso R . . . . . 
H311 H -0.5696 -0.9591 -0.2025 0.0498 0.222(7) Uiso R . P . 4 . 
H312 H -0.6315 -0.6932 -0.2343 0.0498 1.0000 Uiso R . . . . . 
H411 H -0.3437 -0.8052 -0.1955 0.0876 0.778(7) Uiso R . P . 1 . 
H412 H -0.4054 -0.5394 -0.2277 0.0876 1.0000 Uiso R . . . . . 
H111 H -0.4642 -0.5840 -0.3719 0.0373 1.0000 Uiso R . . . . . 
H112 H -0.5660 -0.7003 -0.4610 0.0373 1.0000 Uiso R . . . . . 
H113 H -0.6279 -0.5349 -0.3931 0.0373 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 0.0163(4) 0.0274(5) 0.0334(5) 0.0056(4) 0.0047(3) -0.0031(3) 
O21 0.0339(6) 0.0252(6) 0.0511(7) 0.0035(5) 0.0118(5) -0.0028(5) 
C11 0.0195(5) 0.0263(6) 0.0286(6) 0.0022(5) 0.0072(4) -0.0015(4) 
N11 0.0243(5) 0.0351(7) 0.0359(6) -0.0095(6) 0.0120(5) -0.0145(5) 
C21 0.0187(5) 0.0312(8) 0.0387(7) -0.0035(6) 0.0048(5) 0.0003(5) 
C31 0.0397(8) 0.0473(11) 0.0335(7) 0.0020(7) 0.0037(6) 0.0025(7) 
C12 0.0183(5) 0.0232(6) 0.0266(6) 0.0032(5) 0.0077(4) 0.0048(4) 
C41 0.0563(12) 0.089(2) 0.0482(10) -0.0111(13) -0.0014(9) -0.0187(12) 
C61 0.130(3) 0.116(3) 0.0398(10) -0.0024(16) -0.0114(14) -0.034(3) 
O12 0.0182(4) 0.0296(6) 0.0340(5) 0.0001(4) 0.0085(4) 0.0026(4) 
O22 0.0254(5) 0.0233(5) 0.0398(6) -0.0006(5) 0.0092(4) 0.0051(4) 
C22 0.0180(4) 0.0250(7) 0.0281(5) 0.0014(5) 0.0059(4) 0.0049(5) 
N12 0.0195(4) 0.0213(5) 0.0341(6) 0.0035(4) 0.0108(4) 0.0055(4) 
C62 0.113(4) 0.089(4) 0.0299(14) 0.0112(18) 0.013(2) 0.020(3) 
C42 0.0474(15) 0.0471(19) 0.0302(11) 0.0022(10) 0.0047(12) 0.0169(13) 
C52 0.054(2) 0.046(2) 0.054(2) -0.0122(18) -0.0065(18) 0.0049(15) 
C32 0.033(2) 0.032(2) 0.0314(10) 0.0080(10) 0.0048(13) 0.0077(13) 
C63 0.060(3) 0.064(4) 0.0366(18) -0.012(2) -0.0059(18) 0.008(3) 
C53 0.0342(19) 0.039(2) 0.0372(17) -0.0040(16) 0.0003(15) 0.0012(16) 
C43 0.0359(17) 0.038(2) 0.0315(15) 0.0030(16) 0.0143(13) 0.0044(15) 
C33 0.0211(19) 0.030(2) 0.0288(16) 0.0035(16) 0.0048(11) 0.0073(15) 
C51 0.131(4) 0.069(2) 0.0381(14) 0.0099(14) -0.0015(17) -0.038(2) 
C54 0.035(3) 0.137(8) 0.071(7) 0.028(5) -0.001(4) -0.004(5) 

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 20.64(4) 
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 . 1.2641(19)    yes
O21 . C11 . 1.244(2)    yes
C11 . C21 . 1.532(2)    yes
N11 . C21 . 1.488(2)    yes
N11 . H111 . 0.950    no
N11 . H112 . 0.950    no
N11 . H113 . 0.950    no
C21 . C31 . 1.562(3)    yes
C21 . H211 . 0.992    no
C31 . C41 . 1.515(3)    yes
C31 . C51 . 1.503(4)    yes
C31 . H312 . 0.950    no
C12 . O12 . 1.2582(19)    yes
C12 . O22 . 1.253(2)    yes
C12 . C22 . 1.5327(19)    yes
C41 . C61 . 1.500(4)    yes
C41 . H411 . 0.950    no
C41 . H412 . 0.950    no
C61 . H612 . 0.962    no
C61 . H611 . 0.986    no
C61 . H613 . 0.987    no
C22 . N12 . 1.480(2)    yes
C22 . C32 . 1.575(5)    yes
C22 . H221 . 0.990    no
N12 . H123 . 0.895    no
N12 . H122 . 0.929    no
N12 . H121 . 0.906    no
C62 . C42 . 1.522(6)    yes
C62 . H621 . 0.955    no
C62 . H622 . 0.947    no
C62 . H623 . 0.958    no
C42 . C52 . 1.516(6)    yes
C42 . C32 . 1.521(6)    yes
C42 . H421 . 0.984    no
C52 . H522 . 0.973    no
C52 . H521 . 0.971    no
C52 . H523 . 0.955    no
C32 . H321 . 0.973    no
C32 . H322 . 0.954    no
C63 . C53 . 1.529(7)    yes
C63 . H631 . 0.970    no
C63 . H632 . 0.961    no
C63 . H633 . 0.955    no
C53 . C33 . 1.539(8)    yes
C53 . H531 . 0.980    no
C53 . H532 . 0.962    no
C43 . C33 . 1.514(7)    yes
C43 . H431 . 0.978    no
C43 . H432 . 0.967    no
C43 . H433 . 0.957    no
C33 . H331 . 0.989    no
C51 . H511 . 0.962    no
C51 . H512 . 0.941    no
C51 . H513 . 0.957    no
C54 . H541 . 0.959    no
C54 . H543 . 0.960    no
C54 . H542 . 0.959    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
O11 . C11 . O21 . 125.59(15)    yes
O11 . C11 . C21 . 116.16(14)    yes
O21 . C11 . C21 . 118.17(14)    yes
C21 . N11 . H111 . 109.4    no
C21 . N11 . H112 . 109.6    no
H111 . N11 . H112 . 109.5    no
C21 . N11 . H113 . 109.4    no
H111 . N11 . H113 . 109.5    no
H112 . N11 . H113 . 109.5    no
C11 . C21 . N11 . 109.35(12)    yes
C11 . C21 . C31 . 109.50(13)    yes
N11 . C21 . C31 . 109.76(15)    yes
C11 . C21 . H211 . 106.9    no
N11 . C21 . H211 . 105.4    no
C31 . C21 . H211 . 115.8    no
C21 . C31 . C41 . 112.85(17)    yes
C21 . C31 . C51 . 112.3(2)    yes
C41 . C31 . C51 . 109.7(2)    yes
C21 . C31 . H312 . 108.1    no
C41 . C31 . H312 . 107.3    no
C51 . C31 . H312 . 106.2    no
O12 . C12 . O22 . 124.57(13)    yes
O12 . C12 . C22 . 117.26(14)    yes
O22 . C12 . C22 . 118.12(13)    yes
C31 . C41 . C61 . 116.1(3)    yes
C31 . C41 . H411 . 106.4    no
C61 . C41 . H411 . 105.9    no
C31 . C41 . H412 . 109.2    no
C61 . C41 . H412 . 109.6    no
H411 . C41 . H412 . 109.5    no
C41 . C61 . H612 . 109.7    no
C41 . C61 . H611 . 114.1    no
H612 . C61 . H611 . 108.1    no
C41 . C61 . H613 . 109.6    no
H612 . C61 . H613 . 110.4    no
H611 . C61 . H613 . 104.7    no
C12 . C22 . N12 . 109.57(12)    yes
C12 . C22 . C32 . 109.4(2)    yes
N12 . C22 . C32 . 103.3(2)    yes
C12 . C22 . H221 . 112.5    no
N12 . C22 . H221 . 111.0    no
C32 . C22 . H221 . 110.7    no
C22 . N12 . H123 . 109.9    no
C22 . N12 . H122 . 109.5    no
H123 . N12 . H122 . 107.7    no
C22 . N12 . H121 . 107.6    no
H123 . N12 . H121 . 111.5    no
H122 . N12 . H121 . 110.7    no
C42 . C62 . H621 . 106.2    no
C42 . C62 . H622 . 107.4    no
H621 . C62 . H622 . 112.0    no
C42 . C62 . H623 . 108.4    no
H621 . C62 . H623 . 110.8    no
H622 . C62 . H623 . 111.7    no
C62 . C42 . C52 . 109.7(4)    yes
C62 . C42 . C32 . 109.0(4)    yes
C52 . C42 . C32 . 112.4(3)    yes
C62 . C42 . H421 . 106.1    no
C52 . C42 . H421 . 109.2    no
C32 . C42 . H421 . 110.2    no
C42 . C52 . H522 . 110.2    no
C42 . C52 . H521 . 107.6    no
H522 . C52 . H521 . 110.9    no
C42 . C52 . H523 . 108.9    no
H522 . C52 . H523 . 110.1    no
H521 . C52 . H523 . 109.2    no
C42 . C32 . C22 . 114.5(4)    yes
C42 . C32 . H321 . 110.4    no
C22 . C32 . H321 . 107.0    no
C42 . C32 . H322 . 109.2    no
C22 . C32 . H322 . 107.4    no
H321 . C32 . H322 . 108.1    no
C53 . C63 . H631 . 111.1    no
C53 . C63 . H632 . 111.8    no
H631 . C63 . H632 . 109.0    no
C53 . C63 . H633 . 108.2    no
H631 . C63 . H633 . 108.1    no
H632 . C63 . H633 . 108.6    no
C63 . C53 . C33 . 113.5(5)    yes
C63 . C53 . H531 . 108.6    no
C33 . C53 . H531 . 107.3    no
C63 . C53 . H532 . 109.6    no
C33 . C53 . H532 . 109.4    no
H531 . C53 . H532 . 108.2    no
C33 . C43 . H431 . 112.1    no
C33 . C43 . H432 . 109.4    no
H431 . C43 . H432 . 107.0    no
C33 . C43 . H433 . 111.0    no
H431 . C43 . H433 . 109.4    no
H432 . C43 . H433 . 107.8    no
C53 . C33 . C22 . 112.1(4)    yes
C53 . C33 . C43 . 112.9(4)    yes
C22 . C33 . C43 . 110.1(4)    yes
C53 . C33 . H331 . 107.2    no
C22 . C33 . H331 . 105.6    no
C43 . C33 . H331 . 108.5    no
C31 . C51 . H511 . 111.2    no
C31 . C51 . H512 . 110.2    no
H511 . C51 . H512 . 110.3    no
C31 . C51 . H513 . 107.4    no
H511 . C51 . H513 . 110.1    no
H512 . C51 . H513 . 107.5    no
C41 . C54 . H541 . 111.3    no
C41 . C54 . H543 . 107.4    no
H541 . C54 . H543 . 109.1    no
C41 . C54 . H542 . 110.6    no
H541 . C54 . H542 . 109.7    no
H543 . C54 . H542 . 108.7    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
C21 . H211 . O12 2_444 167.83(5) 0.992 2.401 3.378(6)    yes
C62 . H621 . C54 2_454 160.3(4) 0.955 2.537 3.452(6)    yes
C43 . H322 . N12 . 151.6(6) 0.734 2.540 3.205(6)    yes
C43 . H433 . O22 1_565 157.75(9) 0.957 2.579 3.484(6)    yes
C51 . H512 . O21 . 123.02(11) 0.941 2.552 3.165(6)    yes
N12 . H123 . O11 2_354 175.26(5) 0.895 1.866 2.759(6)    yes
N12 . H122 . O11 . 149.84(5) 0.929 1.966 2.808(6)    yes
N12 . H121 . O22 1_565 168.06(5) 0.906 1.962 2.854(6)    yes
N11 . H111 . C12 2_454 153.40(5) 0.950 2.476 3.352(6)    yes
N11 . H111 . O12 2_454 134.77(5) 0.950 2.253 2.999(6)    yes
N11 . H111 . O22 2_454 141.91(5) 0.950 2.168 2.974(6)    yes
N11 . H112 . O12 . 156.89(5) 0.950 1.864 2.763(6)    yes
N11 . H113 . O21 1_565 165.95(5) 0.950 1.920 2.851(6)    yes


_iucr_refine_instruction_details_constraints
;
#
# Punched on 19/09/13 at 11:36:11
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
EQUIV PART(1, OCC) PART(4,OCC) 
WEIGHT -1 PART(4, OCC) 
EQUIV PART(2, OCC) PART(3,OCC) 
WEIGHT -1 PART(3, OCC) 
RIDE N   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) H   ( 613,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE N   (  12,X'S) H   ( 123,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) H   ( 622,X'S) H   ( 623,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  52,X'S) H   ( 522,X'S) H   ( 521,X'S) H   ( 523,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) H   ( 632,X'S) H   ( 633,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) H   ( 532,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) H   ( 433,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) H   ( 543,X'S) H   ( 542,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints
;
#
# Punched on 19/09/13 at 11:36:11
#
#LIST     16                                                                    
DISTANCE 1.540000 , 0.030000 = C(21) TO C(31) 
DISTANCE 1.510000 , 0.030000 = C(31) TO C(51) 
DISTANCE 1.540000 , 0.030000 = C(31) TO C(41) 
DISTANCE 1.510000 , 0.030000 = C(41) TO C(54) 
DISTANCE 1.510000 , 0.030000 = C(41) TO C(61) 
DISTANCE 1.540000 , 0.030000 = C(22) TO C(32) 
DISTANCE 1.510000 , 0.030000 = C(32) TO C(42) 
DISTANCE 1.510000 , 0.030000 = C(42) TO C(52) 
DISTANCE 1.510000 , 0.030000 = C(42) TO C(62) 
DISTANCE 1.540000 , 0.030000 = C(22) TO C(33) 
DISTANCE 1.510000 , 0.030000 = C(33) TO C(43) 
DISTANCE 1.510000 , 0.030000 = C(33) TO C(53) 
DISTANCE 1.510000 , 0.030000 = C(53) TO C(63) 
REM   DELU   START (DO NOT REMOVE THIS LINE) 
VIBR .0, 0.00100 = O(11) TO C(11) 
VIBR .0, 0.00100 = O(21) TO C(11) 
VIBR .0, 0.00100 = C(11) TO C(21) 
VIBR .0, 0.00300 = O(11) TO O(21) 
VIBR .0, 0.00300 = C(21) TO O(21) 
VIBR .0, 0.00300 = C(21) TO O(11) 
VIBR .0, 0.00100 = N(11) TO C(21) 
VIBR .0, 0.00100 = C(21) TO C(31) 
VIBR .0, 0.00300 = N(11) TO C(11) 
VIBR .0, 0.00300 = C(31) TO C(11) 
VIBR .0, 0.00300 = C(31) TO N(11) 
VIBR .0, 0.00100 = C(31) TO C(41) 
VIBR .0, 0.00100 = C(31) TO C(51) 
VIBR .0, 0.00300 = C(41) TO C(21) 
VIBR .0, 0.00300 = C(51) TO C(21) 
VIBR .0, 0.00300 = C(51) TO C(41) 
VIBR .0, 0.00100 = C(12) TO O(12) 
VIBR .0, 0.00100 = C(12) TO O(22) 
VIBR .0, 0.00100 = C(12) TO C(22) 
VIBR .0, 0.00300 = O(22) TO O(12) 
VIBR .0, 0.00300 = C(22) TO O(12) 
VIBR .0, 0.00300 = C(22) TO O(22) 
VIBR .0, 0.00100 = C(41) TO C(61) 
VIBR .0, 0.00100 = C(41) TO C(54) 
VIBR .0, 0.00300 = C(61) TO C(31) 
VIBR .0, 0.00300 = C(54) TO C(31) 
VIBR .0, 0.00300 = C(54) TO C(61) 
VIBR .0, 0.00100 = C(22) TO N(12) 
VIBR .0, 0.00100 = C(22) TO C(32) 
VIBR .0, 0.00300 = N(12) TO C(12) 
VIBR .0, 0.00300 = C(32) TO C(12) 
VIBR .0, 0.00300 = C(32) TO N(12) 
VIBR .0, 0.00100 = C(62) TO C(42) 
VIBR .0, 0.00100 = C(42) TO C(52) 
VIBR .0, 0.00100 = C(42) TO C(32) 
VIBR .0, 0.00300 = C(52) TO C(62) 
VIBR .0, 0.00300 = C(32) TO C(62) 
VIBR .0, 0.00300 = C(32) TO C(52) 
VIBR .0, 0.00300 = C(42) TO C(22) 
VIBR .0, 0.00100 = C(63) TO C(53) 
VIBR .0, 0.00100 = C(53) TO C(33) 
VIBR .0, 0.00300 = C(33) TO C(63) 
VIBR .0, 0.00100 = C(43) TO C(33) 
VIBR .0, 0.00300 = C(43) TO C(22) 
VIBR .0, 0.00300 = C(53) TO C(22) 
VIBR .0, 0.00300 = C(53) TO C(43) 
REM   DELU   END (DO NOT REMOVE THIS LINE) 
REM   THERMSIM   START (DO NOT REMOVE THIS LINE) 
U(IJ) .0, 0.04000 = O(11) TO C(11) 
U(IJ) .0, 0.04000 = O(21) TO C(11) 
U(IJ) .0, 0.02000 = C(11) TO C(21) 
U(IJ) .0, 0.04000 = N(11) TO C(21) 
U(IJ) .0, 0.02000 = C(21) TO C(31) 
U(IJ) .0, 0.02000 = C(31) TO C(41) 
U(IJ) .0, 0.04000 = C(31) TO C(51) 
U(IJ) .0, 0.04000 = C(12) TO O(12) 
U(IJ) .0, 0.04000 = C(12) TO O(22) 
U(IJ) .0, 0.02000 = C(12) TO C(22) 
U(IJ) .0, 0.04000 = C(41) TO C(61) 
U(IJ) .0, 0.04000 = C(41) TO C(54) 
U(IJ) .0, 0.04000 = C(22) TO N(12) 
U(IJ) .0, 0.02000 = C(22) TO C(32) 
U(IJ) .0, 0.04000 = C(62) TO C(42) 
U(IJ) .0, 0.04000 = C(42) TO C(52) 
U(IJ) .0, 0.02000 = C(42) TO C(32) 
U(IJ) .0, 0.04000 = C(63) TO C(53) 
U(IJ) .0, 0.02000 = C(53) TO C(33) 
U(IJ) .0, 0.04000 = C(43) TO C(33) 
REM   THERMSIM   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
   2   1   0  x   .
   
END