# Electronic Supplementary Material (ESI) for Green Chemistry
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_lmcjma

_nottingham_internal_coll_name   LMCJMA
_nottingham_internal_coll_number 12543
_nottingham_internal_coll_client LM/CJM
_nottingham_internal_coll_type   CUSTOM
_nottingham_internal_coll_frame_time '10 and 40'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   6/06/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user WL
_nottingham_internal_process_date 7/06/2013
_nottingham_internal_solution_user WL
_nottingham_internal_solution_date 7/06/2013
_nottingham_internal_refinement_user WL
_nottingham_internal_refinement_date 7/06/2013
_nottingham_internal_validation_user WL
_nottingham_internal_validation_date 7/6/2013
_nottingham_internal_archive_date 7/6/2013

_audit_creation_date             2013-06-07
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H18 O4'
_chemical_formula_sum            'C16 H18 O4'
_chemical_formula_weight         274.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H18 O4'
_chemical_oxdiff_usercomment     
'LMCJMA #12543 IN FOMBLIN FILM ON MICROMOUNT FOR LM/CJM'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7968(2)
_cell_length_b                   21.1512(5)
_cell_length_c                   9.1046(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.189(3)
_cell_angle_gamma                90
_cell_volume                     1369.64(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6647
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1530
_cell_measurement_theta_min      4.1720
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  1.043
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       tablet
_exptl_crystal_F_000             584
_exptl_crystal_recrystallization_method 
'crystallised by vapour diffusion of cyclohexane into an ethyl acetate solution of the compound'
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.1016
_exptl_crystal_size_min          0.0629
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12604
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.564
_diffrn_reflns_theta_min         4.180
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9852
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -43.00  -18.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega  -10.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804  -99.0000 -180.0000 87

#__ type_ start__ end____ width___ exp.time_
  3 omega  -32.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804  -38.0000  -90.0000 92

#__ type_ start__ end____ width___ exp.time_
  4 omega   31.00   63.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000 -180.0000 32

#__ type_ start__ end____ width___ exp.time_
  5 omega   44.00   94.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -45.0000 -150.0000 50

#__ type_ start__ end____ width___ exp.time_
  6 omega   41.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -45.0000  120.0000 46

#__ type_ start__ end____ width___ exp.time_
  7 omega   68.00  150.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   15.0000    0.0000 82

#__ type_ start__ end____ width___ exp.time_
  8 omega  124.00  150.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   77.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega   60.00   86.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   97.00  122.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295 -125.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   30.00   90.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000    0.0000 60

#__ type_ start__ end____ width___ exp.time_
 12 omega   30.00   87.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -30.0000   60.0000 57

#__ type_ start__ end____ width___ exp.time_
 13 omega   14.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804   57.0000  -30.0000 94

#__ type_ start__ end____ width___ exp.time_
 14 omega    9.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804   77.0000   30.0000 102

#__ type_ start__ end____ width___ exp.time_
 15 omega   14.00  108.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       39.1804   57.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
 16 omega   82.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   30.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
 17 omega   23.00  109.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -94.0000  -30.0000 86

#__ type_ start__ end____ width___ exp.time_
 18 omega   82.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   30.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
 19 omega   77.00  163.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   61.0000   90.0000 86

#__ type_ start__ end____ width___ exp.time_
 20 omega   31.00  133.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295  -77.0000  120.0000 102

#__ type_ start__ end____ width___ exp.time_
 21 omega   80.00  172.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.8295   45.0000  150.0000 92
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1898122000
_diffrn_orient_matrix_UB_12      0.0081722000
_diffrn_orient_matrix_UB_13      0.0126279000
_diffrn_orient_matrix_UB_21      0.0880770000
_diffrn_orient_matrix_UB_22      0.0504799000
_diffrn_orient_matrix_UB_23      0.1315420000
_diffrn_orient_matrix_UB_31      -0.0560162000
_diffrn_orient_matrix_UB_32      0.0518452000
_diffrn_orient_matrix_UB_33      -0.1302604000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2433
_reflns_number_total             2766
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2\s(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.3480P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0941
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
2.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.69017(14) 0.46303(5) 0.50717(12) 0.0191(2) Uani 1 1 d . . . . .
C2 C 0.79946(14) 0.48869(5) 0.65696(12) 0.0191(2) Uani 1 1 d . . . . .
C3 C 0.81676(14) 0.45531(5) 0.79818(12) 0.0201(2) Uani 1 1 d . . . . .
H3 H 0.8896 0.4734 0.9005 0.024 Uiso 1 1 calc R U . . .
C4 C 0.73276(14) 0.39865(5) 0.79152(12) 0.0199(2) Uani 1 1 d . . . . .
C4A C 0.62297(14) 0.36996(5) 0.64005(12) 0.0193(2) Uani 1 1 d . . . . .
C5 C 0.54249(15) 0.30956(5) 0.63240(13) 0.0228(2) Uani 1 1 d . . . . .
H5 H 0.5572 0.2884 0.7289 0.027 Uiso 1 1 calc R U . . .
C6 C 0.44355(16) 0.28141(5) 0.48679(14) 0.0256(2) Uani 1 1 d . . . . .
H6 H 0.3933 0.2402 0.4831 0.031 Uiso 1 1 calc R U . . .
C7 C 0.41538(16) 0.31261(5) 0.34252(13) 0.0249(2) Uani 1 1 d . . . . .
H7 H 0.3461 0.2926 0.2421 0.030 Uiso 1 1 calc R U . . .
C8A C 0.59932(14) 0.40284(5) 0.49612(12) 0.0190(2) Uani 1 1 d . . . . .
C8 C 0.48820(15) 0.37222(5) 0.34667(13) 0.0212(2) Uani 1 1 d . . . . .
O9 O 0.67523(11) 0.49475(4) 0.37324(9) 0.02411(19) Uani 1 1 d . . . . .
H9 H 0.6003 0.4756 0.2912 0.036 Uiso 1 1 calc R U . . .
C10 C 0.90562(15) 0.54934(5) 0.68527(12) 0.0210(2) Uani 1 1 d . . . . .
O11 O 0.99878(13) 0.56520(4) 0.82528(9) 0.0314(2) Uani 1 1 d . . . . .
C12 C 0.90249(14) 0.59096(5) 0.55042(13) 0.0208(2) Uani 1 1 d . . . . .
H12A H 0.7710 0.6035 0.4837 0.025 Uiso 1 1 calc R U . . .
H12B H 0.9487 0.5665 0.4812 0.025 Uiso 1 1 calc R U . . .
C13 C 1.02186(16) 0.65020(5) 0.60920(14) 0.0263(3) Uani 1 1 d . . . . .
H13A H 1.1544 0.6379 0.6724 0.032 Uiso 1 1 calc R U . . .
H13B H 0.9787 0.6742 0.6811 0.032 Uiso 1 1 calc R U . . .
C14 C 1.01016(18) 0.69251(6) 0.46933(17) 0.0359(3) Uani 1 1 d . . . . .
H14A H 1.0430 0.6679 0.3933 0.054 Uiso 1 1 calc R U . . .
H14B H 1.0981 0.7279 0.5107 0.054 Uiso 1 1 calc R U . . .
H14C H 0.8819 0.7089 0.4143 0.054 Uiso 1 1 calc R U . . .
O15 O 0.74810(11) 0.36548(4) 0.92575(9) 0.02394(19) Uani 1 1 d . . . . .
H15 H 0.8201 0.3848 1.0086 0.036 Uiso 1 1 calc R U . . .
O16 O 0.46049(11) 0.40581(4) 0.20971(9) 0.02478(19) Uani 1 1 d . . . . .
C17 C 0.34628(18) 0.37865(6) 0.05445(13) 0.0294(3) Uani 1 1 d . . . . .
H17A H 0.2193 0.3685 0.0477 0.035 Uiso 1 1 calc R U . . .
H17B H 0.4045 0.3392 0.0380 0.035 Uiso 1 1 calc R U . . .
C18 C 0.33345(18) 0.42670(6) -0.07121(14) 0.0315(3) Uani 1 1 d . . . . .
H18A H 0.2564 0.4098 -0.1783 0.047 Uiso 1 1 calc R U . . .
H18B H 0.4598 0.4362 -0.0637 0.047 Uiso 1 1 calc R U . . .
H18C H 0.2758 0.4655 -0.0536 0.047 Uiso 1 1 calc R U . . .

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
C1 0.0189(5) 0.0189(5) 0.0190(5) 0.0015(4) 0.0072(4) 0.0024(4)
C2 0.0191(5) 0.0178(5) 0.0191(5) 0.0005(4) 0.0066(4) 0.0011(4)
C3 0.0203(5) 0.0201(5) 0.0168(5) -0.0008(4) 0.0044(4) 0.0002(4)
C4 0.0194(5) 0.0198(5) 0.0187(5) 0.0032(4) 0.0061(4) 0.0028(4)
C4A 0.0167(5) 0.0182(5) 0.0215(5) 0.0005(4) 0.0062(4) 0.0021(4)
C5 0.0224(5) 0.0194(5) 0.0242(5) 0.0029(4) 0.0071(4) 0.0009(4)
C6 0.0257(5) 0.0186(5) 0.0295(6) -0.0013(4) 0.0082(5) -0.0025(4)
C7 0.0254(5) 0.0218(5) 0.0236(5) -0.0050(4) 0.0060(4) -0.0023(4)
C8A 0.0174(5) 0.0180(5) 0.0202(5) -0.0004(4) 0.0063(4) 0.0017(4)
C8 0.0202(5) 0.0219(5) 0.0199(5) -0.0007(4) 0.0064(4) 0.0015(4)
O9 0.0297(4) 0.0226(4) 0.0157(4) 0.0008(3) 0.0048(3) -0.0056(3)
C10 0.0207(5) 0.0205(5) 0.0196(5) -0.0005(4) 0.0059(4) 0.0001(4)
O11 0.0402(5) 0.0268(4) 0.0192(4) -0.0004(3) 0.0042(3) -0.0110(3)
C12 0.0202(5) 0.0195(5) 0.0216(5) 0.0016(4) 0.0073(4) 0.0004(4)
C13 0.0258(5) 0.0218(5) 0.0314(6) 0.0011(4) 0.0118(5) -0.0028(4)
C14 0.0351(6) 0.0284(6) 0.0466(8) 0.0114(5) 0.0189(6) -0.0009(5)
O15 0.0287(4) 0.0209(4) 0.0178(4) 0.0022(3) 0.0051(3) -0.0043(3)
O16 0.0286(4) 0.0243(4) 0.0167(4) -0.0023(3) 0.0044(3) -0.0044(3)
C17 0.0341(6) 0.0302(6) 0.0182(5) -0.0064(4) 0.0050(5) -0.0048(5)
C18 0.0350(6) 0.0354(7) 0.0194(5) -0.0011(5) 0.0064(5) -0.0003(5)

_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 C2 1.3887(15) . ?
C1 C8A 1.4401(15) . ?
C1 O9 1.3543(13) . ?
C2 C3 1.4240(14) . ?
C2 C10 1.4906(14) . ?
C3 C4 1.3552(15) . ?
C4 C4A 1.4267(14) . ?
C4 O15 1.3712(12) . ?
C4A C5 1.4123(15) . ?
C4A C8A 1.4273(14) . ?
C5 C6 1.3672(16) . ?
C6 C7 1.4045(16) . ?
C7 C8 1.3769(16) . ?
C8A C8 1.4336(14) . ?
C8 O16 1.3732(13) . ?
C10 O11 1.2273(13) . ?
C10 C12 1.5029(14) . ?
C12 C13 1.5212(15) . ?
C13 C14 1.5284(16) . ?
O16 C17 1.4455(13) . ?
C17 C18 1.5026(17) . ?

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
C2 C1 C8A 120.03(9) . . ?
O9 C1 C2 118.84(9) . . ?
O9 C1 C8A 121.10(9) . . ?
C1 C2 C3 119.07(9) . . ?
C1 C2 C10 125.45(9) . . ?
C3 C2 C10 115.47(9) . . ?
C4 C3 C2 122.20(10) . . ?
C3 C4 C4A 120.46(10) . . ?
C3 C4 O15 123.27(9) . . ?
O15 C4 C4A 116.27(9) . . ?
C4 C4A C8A 118.74(9) . . ?
C5 C4A C4 120.72(10) . . ?
C5 C4A C8A 120.52(10) . . ?
C6 C5 C4A 120.30(10) . . ?
C5 C6 C7 120.80(10) . . ?
C8 C7 C6 119.99(10) . . ?
C4A C8A C1 119.46(9) . . ?
C4A C8A C8 116.86(9) . . ?
C8 C8A C1 123.66(10) . . ?
C7 C8 C8A 121.45(10) . . ?
O16 C8 C7 122.63(10) . . ?
O16 C8 C8A 115.92(9) . . ?
C2 C10 C12 122.74(9) . . ?
O11 C10 C2 117.72(9) . . ?
O11 C10 C12 119.53(10) . . ?
C10 C12 C13 113.10(9) . . ?
C12 C13 C14 111.72(10) . . ?
C8 O16 C17 119.15(9) . . ?
O16 C17 C18 107.33(9) . . ?

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
O9 H9 O16 0.84 1.80 2.5525(10) 147.5 .
O15 H15 O11 0.84 1.91 2.7417(11) 170.6 3_767

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
5 1 -3 0.0521 4.9967 0.9979 -3.0099 -0.9783 0.0945 0.1639
-5 4 2 0.0462 -4.9942 3.9886 2.0006 1.0058 0.0246 0.2259
0 -1 0 0.0455 -0.0006 -0.9999 0.0020 -0.0080 -0.0503 -0.0521
0 1 0 0.0455 0.0006 0.9999 -0.0020 0.0080 0.0503 0.0521
0 3 -5 0.0118 0.0000 2.9354 -5.0030 -0.0392 -0.5099 0.8039
0 1 1 0.0250 0.0009 1.0127 0.9974 0.0207 0.1824 -0.0775

loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 0 1 10.8727 11.4326 1
0 0 1 -8.33694 26.5931 15
0 0 -1 42.4401 26.7034 2
0 0 -2 33240.2 515.348 2
0 0 2 32365.6 505.853 15
0 0 3 55.9283 58.9162 15
0 0 -3 2.48035 57.7762 2
0 0 4 6883.84 307.19 15
0 0 -4 6940.23 281.285 3
0 0 5 75.6727 78.4647 15
0 0 -5 -15.6394 56.5032 3
0 0 -6 39163 531.762 4
0 0 -6 38051.6 867.516 3
0 0 6 38507.7 929.475 15
0 0 -6 37965.7 556.406 20
0 0 -6 38809.9 526.751 8
0 0 -7 25.0033 48.4595 8
0 0 -7 46.0117 65.9062 20
0 0 -7 32.5357 48.048 4
0 0 7 24.7229 104.939 13
0 0 -8 1870.46 128.418 20
0 0 -8 1970.51 132.407 5
0 0 -9 -37.0325 43.6535 20
0 0 -9 -57.6333 42.0985 5
0 0 -10 -1.46336 24.8901 5
0 1 1 101409 996.158 15
0 -1 -1 101790 928.316 1
0 1 -1 101841 918.562 3
0 -1 1 103206 945.008 15
0 -1 -1 99736.4 1005.9 14
0 1 -1 100825 991.019 2
0 -1 -2 15364 316.407 2
0 -1 2 14941.3 306.243 15
0 1 -2 14683.4 332.147 2
0 1 -2 15306.1 282.31 3
0 1 2 14528.6 329.555 15
0 -1 3 140.112 56.024 15
0 1 3 103.319 65.3794 15
0 1 -3 215.9 82.1497 2
0 1 4 1551.25 164.714 15
0 -1 4 1792.12 159.66 15
0 1 -4 1743.21 143.144 3
0 -1 -4 1762.26 151.966 3
0 1 -5 3030.41 208.686 3
0 1 5 2924.9 242.743 15
0 -1 5 2792.83 228.524 15
0 -1 -5 2981.08 220.779 3
0 -1 -6 226.857 50.0089 4
0 -1 6 -16.3604 74.9331 15
0 1 -6 121.448 54.5587 20
0 -1 6 129.925 117.023 13
0 -1 -6 284.405 65.9102 20
0 -1 -6 160.93 44.8476 8
0 1 6 159.67 65.3338 15
0 1 -6 150.396 45.1103 4
0 1 6 51.3288 110.711 13
0 -1 -6 70.2935 65.8221 3
0 1 -6 64.4558 36.3115 8
0 -1 -7 100732 1146.04 20
0 1 -7 98824.2 1083.99 4
0 1 -7 97569.5 1073.93 8
0 1 7 104559 2016.19 13
0 -1 7 100507 1981.83 13
0 1 -7 97765.8 1123.39 20
0 -1 -7 99973.5 1108.19 4
0 -1 -7 95670.9 1080.97 8
0 -1 -8 510.081 82.6173 20
0 1 -8 405.126 80.4295 20
0 -1 -8 426.473 60.7689 8
0 1 -8 357.627 72.8193 5
0 -1 -8 299.927 55.1801 4
0 1 -9 817.293 75.2907 20
0 1 -9 962.239 83.9464 5
0 -1 -9 1081.46 90.5656 5
0 -1 -10 1751.41 77.8793 5
0 1 -10 1736.8 71.0798 5
0 -2 0 233787 1979.99 14
0 2 0 235179 1944.73 2
0 2 1 27982.2 406.877 15
0 -2 -1 29293.6 380.867 1
0 2 -1 28083.7 398.189 2
0 2 -1 28155 323.195 3
0 -2 2 45353.4 597.543 15
0 -2 -2 44815.8 692.937 14
0 2 2 45744.4 675.798 15
0 2 -2 45161.6 559.008 3
0 2 -2 45810.4 666.075 2
0 -2 3 9388.6 287.945 15
0 2 -3 9111.61 320.639 2
0 2 3 8777.5 317.364 15
0 2 -3 8762.63 253.15 3
0 2 -4 1645.38 167.741 2
0 -2 4 1639.11 152.94 15
0 2 -4 1786.1 141.266 3
0 2 4 1715.26 175.852 15
0 -2 -5 4714.54 281.431 3
0 2 -5 4929.23 255.931 3
0 2 5 4664.82 298.371 15
0 -2 5 4479.01 274.965 15
0 2 6 4363.6 382.659 13
0 2 -6 5278.18 314.985 10
0 -2 -6 4912.58 168.349 4
0 -2 -6 4874.96 163.666 8
0 2 6 4583.86 327.133 15
0 -2 6 4248.35 386.415 13
0 2 -6 4632.36 149.056 4
0 2 -6 4434.52 149.357 8
0 -2 -6 5230.21 322.787 3
0 2 -6 4634.14 165.758 20
0 -2 -6 4809.91 158.263 16
0 -2 -6 4713.11 177.541 20
0 -2 -7 8880.68 226.376 16
0 -2 7 9230.37 557.531 13
0 2 -7 8872.06 255.149 20
0 -2 -7 8834.42 240.657 8
0 2 -7 8656.58 227.897 4
0 -2 -7 8814.07 251.414 4
0 2 7 9082.97 555.55 13
0 -2 -7 8815.31 264.379 20
0 2 -8 3630.52 163.932 20
0 -2 -8 3332.69 166.846 20
0 2 -8 3647.37 163.295 5
0 -2 -8 3951.33 155.859 8
0 -2 -8 3675.26 163.176 4
0 -2 -9 412.233 65.1057 5
0 2 -9 248.408 51.0507 5
0 2 -9 303.862 54.3675 20
0 -2 -10 1396.52 71.5688 5
0 3 0 -13.5536 20.4691 2
0 -3 0 19.5389 28.549 14
0 3 -1 13293.2 270.655 2
0 3 1 13988.5 287.721 15
0 -3 -1 13956.5 273.577 1
0 -3 -1 13893.4 289.384 14
0 3 -1 13986.3 210.069 3
0 3 2 27566.6 512.105 15
0 3 -2 27941.5 387.176 3
0 3 -2 27497.1 499.322 2
0 -3 -2 27598.3 442.374 1
0 -3 2 27563.8 426.856 15
0 -3 -2 26813 520.075 14
0 3 -3 12771.7 299.731 3
0 -3 3 12783.4 334.128 15
0 3 -3 12460.8 385.385 2
0 3 3 12572.9 391.209 15
0 3 -4 20820.6 460.087 3
0 3 -4 20642.2 587.627 2
0 -3 4 19871.8 504.502 15
0 3 4 20242.7 581.425 15
0 -3 5 510.944 100.012 15
0 3 -5 467.628 85.2527 3
0 3 5 474.412 112.466 15
0 -3 -5 626.03 121.515 3
0 -3 -6 415.518 58.8729 16
0 3 6 423.84 139.453 13
0 -3 -6 578.332 128.217 3
0 -3 -6 349.116 68.643 20
0 -3 6 621.611 184.38 13
0 3 -6 486.881 204.907 10
0 3 -6 466.001 67.2058 20
0 -3 -6 481.178 65.7839 4
0 3 6 601.599 142.366 15
0 -3 -7 6727.88 394.413 3
0 -3 -7 6511.04 218.368 4
0 -3 -7 6667.55 202.823 16
0 3 7 6861.47 492.189 13
0 -3 -7 6524.51 209.785 8
0 -3 7 6511.57 474.32 13
0 -3 -7 6337.68 228.175 20
0 3 -7 6521.21 216.213 20
0 -3 -8 2736.37 131.34 8
0 -3 -8 2851.93 146.435 4
0 3 -8 2759.9 141.328 20
0 3 -8 2723.78 136.27 5
0 -3 -8 2749.38 153.648 20
0 -3 -9 -24.2129 45.282 5
0 3 -9 -5.73087 39.8438 20
0 3 -9 -43.7907 38.7666 5
0 -3 -10 596.36 50.6492 5
0 4 0 194241 1697.65 2
0 -4 0 190212 1801.25 1
0 -4 0 195115 1773.35 14
0 4 1 9616.12 252.885 15
0 -4 -1 9499.9 253.144 14
0 4 -1 9151.88 233.597 2
0 -4 -1 9581.44 248.053 1
0 4 -1 8980.32 180.898 3
0 -4 -2 3231.48 183.404 14
0 4 2 3384.74 186.945 15
0 4 -2 3330.05 119.576 3
0 -4 -2 3516.16 162.682 1
0 4 -2 3307.15 176.854 2
0 -4 2 3329.22 92.6111 1
0 4 -3 179.757 82.6352 2
0 -4 -3 140.86 95.8466 14
0 4 3 51.3679 72.8156 15
0 4 -3 176.623 49.1355 3
0 -4 3 156.707 56.9253 15
0 4 4 -18.67 78.6069 15
0 4 -4 26.0521 82.8523 2
0 4 -4 81.5068 59.2902 3
0 -4 4 -62.4861 68.746 15
0 -4 -5 936.231 150.96 3
0 -4 5 814.767 123.74 15
0 4 5 903.734 148.115 15
0 4 -6 10724.9 288.49 10
0 -4 6 8961.74 545.129 13
0 4 6 9887.16 501.998 15
0 -4 -6 9824.48 249.678 16
0 4 6 9980.51 563.094 13
0 -4 -6 10434.1 258.498 4
0 -4 -6 10063.1 271.984 20
0 -4 -6 9516.19 463.916 3
0 4 -6 10260.8 250.273 20
0 -4 -7 2019.51 139.35 20
0 -4 7 2511.87 292.911 13
0 -4 -7 2085.02 235.834 3
0 -4 -7 2004.24 128.513 4
0 -4 -7 2159.73 124.066 8
0 4 -7 2067.7 126.369 20
0 4 7 2299.3 293.867 13
0 4 7 1869.03 223.936 15
0 -4 -7 2245.2 125.284 16
0 4 -7 2109.08 120.625 5
0 -4 -8 9198 246.328 8
0 -4 -8 8790.06 272.98 20
0 -4 -8 8818.21 258.49 4
0 4 -8 9019.07 241.511 5
0 4 -8 9270.18 248.808 20
0 -4 -8 8885.3 227.63 16
0 4 -9 191.215 43.2574 20
0 -4 -9 246.872 58.7916 5
0 -4 -10 603.548 49.5706 5
0 -5 0 0.88112 49.9666 1
0 5 0 -30.5977 32.8139 2
0 -5 0 -2.49602 43.141 14
0 5 1 230640 2251.81 15
0 -5 -1 230243 2242.11 1
0 5 -1 234776 2184.64 2
0 -5 -1 232963 2242.19 14
0 -5 1 234325 2133.91 1
0 5 -2 1108.73 110.832 2
0 -5 -2 1345.07 116.215 1
0 -5 2 1380.1 73.2843 1
0 5 -2 1291.44 78.8496 3
0 5 2 1361.63 132.807 15
0 -5 -2 1336.14 134.447 14
0 -5 3 89692 1082.43 15
0 -5 -3 85373.5 1282.11 14
0 5 -3 85221.3 979.76 3
0 5 -3 85044.8 1240.41 2
0 5 3 85587.7 1265.75 15
0 5 -4 2705.31 229.565 2
0 -5 4 3195.51 194.636 15
0 5 4 3010.16 239.461 15
0 5 -4 2931.25 157.23 3
0 5 5 4419.14 318.094 15
0 5 -6 4557.63 164.582 20
0 5 -6 4579.93 188.626 10
0 -5 -6 4717.07 173.708 4
0 5 6 4467.23 367.181 13
0 -5 -6 4870.12 341.582 3
0 -5 6 4569.06 373.74 13
0 5 6 4638.31 354.148 15
0 -5 -6 4676.18 174.603 16
0 -5 -6 4505.15 184.954 20
0 5 -7 820.975 396.392 10
0 -5 -7 1230.48 103.212 4
0 5 -7 1225.29 105.118 20
0 5 7 911.814 158.116 15
0 -5 7 874.015 164.478 13
0 5 7 1386.61 223.152 13
0 5 -7 1193.38 91.7027 5
0 -5 -7 1254.98 99.5317 16
0 -5 -7 1160.99 112.888 20
0 -5 -7 1131.73 176.391 3
0 -5 -7 1347.27 103.546 8
0 5 -8 48.2145 47.5068 20
0 -5 -8 -7.71154 47.1327 16
0 5 -8 114.033 45.6356 5
0 -5 -8 72.8147 50.4706 4
0 -5 -8 135.183 52.7264 8
0 -5 -9 106.018 48.7662 5
0 -5 -10 921.533 56.1929 5
0 -6 0 6202.55 214.601 14
0 6 0 6168.86 168.667 2
0 -6 0 6502.87 228.724 1
0 -6 1 56.0086 23.9182 13
0 6 1 110.043 63.5359 15
0 -6 1 93.1253 42.7778 1
0 6 1 67.3535 30.5888 13
0 -6 -1 86.0594 53.6072 14
0 6 -1 177.226 58.1428 2
0 -6 1 86.6136 41.6477 14
0 6 -2 2.77585 58.053 2
0 -6 -2 2.39163 67.9107 14
0 -6 -2 27.866 59.8946 1
0 -6 2 -13.0626 30.2833 1
0 6 2 48.7331 69.164 15
0 6 -2 -2.59868 31.9552 3
0 6 -3 6617.83 307.418 2
0 6 3 6820.22 327.32 15
0 -6 -3 6783.36 328.048 14
0 -6 3 6477.1 241.588 15
0 6 -3 6529.16 201.611 3
0 6 4 119292 1783.63 15
0 6 -4 121704 1762.44 2
0 6 5 7488.44 421.334 15
0 -6 5 7159.87 427.727 13
0 6 5 7186.35 431.103 13
0 6 -5 7855.42 428.61 2
0 -6 -6 5.46104 89.1929 3
0 6 6 99.2063 46.0576 18
0 -6 -6 53.7964 48.2304 4
0 6 6 -53.3798 108.115 15
0 6 6 -9.52027 118.762 13
0 -6 -6 117.466 62.2041 20
0 -6 6 -4.37482 110.73 13
0 6 -6 214.407 78.5811 10
0 6 -6 75.5875 46.707 20
0 -6 -6 46.8398 48.115 16
0 -6 -7 -63.2068 65.1101 20
0 -6 -7 -32.3558 48.3844 4
0 6 -7 -168.739 352.566 10
0 6 -7 0.48276 39.2853 5
0 -6 -7 153.555 113.911 3
0 6 7 32.2782 98.5226 15
0 6 -7 33.6031 50.921 20
0 -6 -7 1.98366 50.2304 8
0 -6 -7 -11.6581 45.8321 16
0 -6 -8 13579.4 303.492 16
0 -6 -8 14026.6 333.345 4
0 6 -8 14149.8 295.97 20
0 -6 -8 14454.1 314.687 8
0 -6 -9 1158.55 72.9095 8
0 -6 -9 1132.86 86.9073 5
0 -6 -10 4512.43 113.996 5
0 7 0 -17.6822 36.2947 2
0 -7 0 3.54673 57.8527 1
0 -7 0 -34.8295 53.1003 14
0 -7 -1 1241.22 128.283 1
0 7 1 1379.75 128.494 15
0 7 1 1155.93 70.9585 2
0 7 -1 1213.63 101.538 2
0 -7 1 1200.2 105.652 1
0 -7 1 1308.28 109.662 14
0 -7 -1 1122.08 113.94 14
0 7 1 1206.52 59.4857 13
0 -7 1 1152.51 46.8152 13
0 7 2 452.501 102.246 15
0 -7 -2 311.843 91.4885 14
0 -7 -2 365.683 86.3327 1
0 -7 2 346.892 57.7361 1
0 7 -2 287.403 83.6622 2
0 -7 -3 266912 2926.43 14
0 7 -3 263688 2860.76 2
0 -7 3 263030 2608.37 15
0 7 -3 264954 2429.98 3
0 7 -4 18744.6 611.578 2
0 7 4 19946.7 645.276 15
0 -7 4 19883.9 486.083 15
0 -7 -5 455.809 57.604 4
0 7 5 706.48 152.246 15
0 7 -5 391.352 117.309 2
0 -7 -5 493.913 63.9579 16
0 -7 -5 508.453 73.5596 20
0 -7 5 542.23 127.531 13
0 7 5 408.086 118.864 13
0 7 6 92.7146 94.3508 13
0 7 -6 245.525 48.0252 17
0 -7 -6 301.28 105.469 3
0 7 -6 175.821 71.0341 10
0 7 -6 224.663 50.7688 20
0 7 6 51.7156 96.5159 15
0 -7 -6 378.703 69.7765 16
0 -7 -6 327.685 63.2626 4
0 7 6 175.145 56.5349 18
0 -7 6 -86.2839 79.8516 13
0 -7 -6 124.861 60.6224 20
0 7 -7 1811.92 109.957 20
0 7 7 1953.66 119.641 18
0 -7 -7 1855.51 128.376 4
0 -7 -7 1925.14 127.389 16
0 -7 -8 2640.15 142.252 4
0 -7 -8 2805.21 136.576 16
0 -7 -8 2740.38 136.689 8
0 -7 -9 -8.99124 34.0141 8
0 -7 -9 -5.47753 41.5169 5
0 -8 0 532.665 93.2127 1
0 -8 0 622.488 87.8593 14
0 8 0 506.657 62.8999 2
0 8 1 2936.06 113.793 2
0 -8 -1 2789.48 188.994 1
0 8 -1 3046.29 165.697 2
0 -8 1 3007.19 170.608 14
0 8 1 2782.39 189.067 15
0 -8 -1 3092.33 186.731 14
0 -8 1 3137.54 175.488 1
0 8 2 9072.1 266.604 13
0 -8 2 9801.45 259.167 13
0 -8 -2 9952.27 366.161 1
0 -8 -2 10594.1 385.161 14
0 8 2 10145.7 386.395 15
0 -8 2 10142.5 287.16 1
0 8 -2 9948.6 347.924 2
0 8 3 -35.4493 84.5121 15
0 -8 -3 -54.1202 81.3958 14
0 8 3 1.78214 60.1375 13
0 8 -3 73.9332 77.2 2
0 -8 3 59.3079 53.7637 13
0 8 4 13218 500.929 13
0 8 4 13953.5 557.714 15
0 8 -4 13702.2 532.492 2
0 -8 -4 14625.5 569.683 14
0 -8 4 12663 483.105 13
0 8 5 7176.45 440.208 15
0 -8 -5 7249.25 229.197 20
0 -8 5 7523.58 412.802 13
0 -8 -5 7583.74 225.12 16
0 -8 -5 7530.27 209.826 4
0 8 5 6965.87 406.425 13
0 8 5 7609.54 221.609 18
0 8 -5 7666.97 438.25 2
0 -8 -6 6204.37 216.498 16
0 8 -6 6219.88 191.541 17
0 -8 -6 6116.49 210.999 4
0 -8 6 5396.23 376.62 13
0 8 -6 6049.03 187.186 20
0 -8 -6 5864.21 400.539 3
0 8 -6 5875.24 214.141 10
0 8 6 6426.2 435.572 15
0 8 6 5851.13 400.358 13
0 8 6 5976.55 209.579 18
0 -8 -7 4351.03 185.767 4
0 8 7 4217.83 172.835 18
0 8 -7 3979.22 273.461 10
0 8 -7 4351.73 162.236 20
0 -8 -7 4607.62 191.856 16
0 -8 -8 3455.2 151.766 16
0 -8 -8 3362.34 160.2 5
0 -8 -8 3465.26 149.444 8
0 -8 -9 359.3 45.212 8
0 -8 -9 346.323 53.5362 5
0 -9 0 -21.2517 78.7749 1
0 9 0 -28.9814 40.269 2
0 -9 0 1.19372 58.2168 14
0 -9 -1 23213.7 578.451 1
0 -9 -1 23058.2 559.74 14
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8 10 -5 -78.5139 47.4283 12
-8 10 4 12997.7 280.818 21
-8 -10 4 12777 277.358 21
8 10 -4 12692.8 294.608 12
-8 10 3 47.7462 39.2145 21
-8 -10 3 169.82 49.6939 21
8 -10 -3 99.4713 34.3079 7
8 10 -3 48.044 51.1891 12
-8 10 2 111.851 39.7582 21
-8 -10 2 135.51 44.4475 21
8 10 -2 147.505 38.2295 7
8 10 -2 116.217 42.9152 12
-8 10 1 35.5688 25.1066 21
-8 -10 1 56.2734 35.4206 21
8 10 -1 133.579 35.184 7
8 10 -1 35.1401 32.3135 12
8 10 0 594.524 45.5095 7
-8 -10 0 684.117 45.4426 21
8 -11 -7 1561.72 68.3039 16
8 11 -7 1551.14 74.2281 6
8 -11 -6 -41.092 38.5638 16
8 11 -6 4.22895 35.2854 6
8 -11 -5 2705.35 118.971 16
-8 11 5 2800.86 116.278 21
-8 -11 5 2674.81 103.988 21
8 11 -5 2542.95 120.245 12
8 11 -5 2715.87 122.088 6
-8 11 4 7273.45 197.034 21
-8 -11 4 7389.47 196.051 21
8 11 -4 7355.82 211.285 12
-8 11 3 13997.5 276.144 21
-8 -11 3 14498.4 290.644 21
-8 11 2 25.2298 30.3624 21
-8 -11 2 -10.1789 40.543 21
8 11 -2 -15.2477 37.8204 12
-8 -11 1 48.0398 33.6582 21
8 11 -1 -15.4266 25.6243 12
8 12 -7 73.9385 24.7568 6
8 -12 -6 1417.45 76.1539 16
8 12 -6 1276.09 73.2757 6
8 -12 -5 -62.4508 39.9642 16
-8 -12 5 58.5075 26.8662 21
8 12 -5 -5.60679 34.5543 6
8 -12 -4 18679.6 328.057 16
-8 12 4 19288.4 321.095 21
-8 -12 4 18182.8 307.982 21
8 12 -4 18465.9 334.166 12
-8 12 3 6177.31 166.535 21
-8 -12 3 6275.74 174.685 21
8 12 -3 6000.95 177.095 12
-8 -12 2 175.744 42.5838 21
8 12 -2 159.724 41.6936 12
-8 -12 1 14.7161 25.6157 21
8 12 -1 66.2373 27.2102 12
8 -13 -6 1663.35 74.6677 16
8 13 -6 1801.31 76.8869 6
8 -13 -5 47.8001 33.0021 16
8 13 -5 42.2943 31.7684 6
8 -13 -4 12252.8 240.021 16
-8 -13 4 11758.4 218.982 21
8 13 -4 11890.3 243.941 12
8 -13 -3 510.069 54.8312 16
-8 -13 3 448.823 50.6687 21
8 13 -3 466.868 55.3903 12
-8 -13 2 97.9235 33.4614 21
8 13 -2 4.44738 28.6619 12
-8 -13 1 106.577 25.5164 21
8 -14 -5 1766 77.1629 16
8 14 -5 1577.85 73.6053 6
8 -14 -4 91.2346 36.5366 16
-8 -14 4 54.8187 22.8797 21
8 14 -4 48.02 32.6398 12
8 -14 -3 114.226 31.6543 16
-8 -14 3 72.9936 27.3838 21
8 14 -3 131.316 33.6416 12
-8 -14 2 57.7022 24.4895 21
8 14 -2 41.18 24.3371 12
8 -15 -4 172.246 29.6788 16
8 15 -4 84.9533 24.2944 6
-9 0 8 5.22997 23.2246 18
-9 0 6 -5.28474 25.834 21
9 0 -6 -33.7038 33.2702 7
-9 0 5 60.2691 38.5907 21
9 0 -5 8.88454 35.2971 7
-9 0 4 65.1525 42.6713 21
9 0 -4 -33.838 41.1087 7
-9 0 3 131.236 42.4582 21
9 0 -3 192.72 48.4686 7
-9 0 2 32.5857 34.5028 21
9 0 -2 -28.6716 33.4007 7
-9 0 1 249.109 29.4071 21
9 0 -1 302.583 38.2579 7
-9 1 8 354.69 37.4192 18
-9 -1 8 219.675 34.3559 18
9 1 -6 742.362 59.5985 7
-9 1 6 760.432 54.9083 21
-9 -1 6 741.117 53.667 21
9 -1 -6 693.352 59.526 7
-9 1 5 299.689 48.238 21
-9 -1 5 391.408 51.4536 21
9 -1 -5 355.043 51.6288 7
9 1 -5 345.151 51.0976 7
-9 1 4 163.222 43.3593 21
-9 -1 4 157.104 44.752 21
9 -1 -4 162.043 47.3039 7
9 1 -4 221.008 48.1611 7
-9 1 3 588.72 61.3406 21
-9 -1 3 575.971 61.4653 21
9 -1 -3 567.894 61.5308 7
9 1 -3 577.881 62.8836 7
9 -1 -2 2798.92 110.749 7
9 1 -2 2851.19 112.728 7
-9 1 2 2707.16 104.36 21
-9 -1 2 2615.25 103.749 21
-9 -1 1 0.37705 20.2518 21
9 -1 -1 -4.92044 27.5425 7
9 1 -1 -2.69437 26.2081 7
-9 2 8 206.32 30.7898 18
-9 -2 8 132.645 28.9807 18
-9 2 7 678.661 51.4333 18
-9 2 6 19.1004 26.2334 21
-9 -2 6 44.134 28.5554 21
9 -2 -6 -49.3894 35.1638 7
9 2 -6 22.9284 27.6623 7
-9 2 5 49.0278 36.7341 21
-9 -2 5 78.0783 35.9191 21
9 -2 -5 79.0766 39.4313 7
9 2 -5 -13.4855 34.8434 7
9 -2 -4 10086.5 230.511 7
9 2 -4 9888.44 224.627 7
-9 2 4 9672.45 226.83 21
-9 -2 4 9657.31 227.802 21
9 -2 -3 1253.15 81.3325 7
9 2 -3 1277.93 82.5746 7
-9 2 3 1276.06 81.9158 21
-9 -2 3 1272.73 83.2162 21
-9 2 2 345.631 44.2722 21
-9 -2 2 514.591 51.9474 21
9 -2 -2 489.433 52.2085 7
9 2 -2 415.741 50.1522 7
-9 -2 1 88.2936 23.9282 21
9 -2 -1 38.5556 25.2147 7
9 2 -1 58.378 29.3852 7
9 3 -7 5395.38 117.262 6
-9 3 7 5375.88 131.319 18
9 -3 -6 129.082 39.1862 7
-9 3 6 147.209 32.0437 21
-9 -3 6 199.083 33.9275 21
9 3 -6 138.174 31.2399 7
9 3 -6 88.2838 26.9475 6
-9 3 6 190.842 36.3152 18
-9 3 5 59.904 32.8059 21
-9 -3 5 -55.4059 36.5339 21
9 -3 -5 -18.2972 38.7875 7
9 3 -5 -30.5066 33.4552 7
9 -3 -4 4093.4 141.846 7
9 3 -4 4303.39 141.007 7
-9 3 4 3996.22 141.993 21
-9 -3 4 4151.02 145.064 21
-9 3 3 173.6 39.2359 21
-9 -3 3 165.928 42.3831 21
9 -3 -3 190.462 45.3665 7
9 3 -3 176.63 43.1432 7
9 -3 -2 1108.61 68.9369 7
9 3 -2 1082.76 70.554 7
-9 3 2 1002.83 63.8309 21
-9 -3 2 1012.81 66.7606 21
9 3 -1 4616.79 123.52 7
9 4 -7 10072.6 169.811 6
-9 4 7 9417.17 169.922 18
-9 4 6 322.966 38.8215 21
-9 -4 6 271.578 33.1347 21
9 4 -6 304.24 36.8373 6
-9 4 5 132.834 39.3185 21
-9 -4 5 16.6021 29.8063 21
9 -4 -5 34.1364 34.2708 7
9 4 -5 61.4533 30.2042 7
9 -4 -4 1571.7 89.5855 7
9 4 -4 1626.33 85.8501 7
-9 4 4 1576.16 89.5187 21
-9 -4 4 1557.04 88.695 21
9 -4 -3 745.257 62.0517 7
9 4 -3 726.44 61.6683 7
-9 4 3 669.249 60.8734 21
-9 -4 3 665.583 63.9885 21
-9 4 2 430.872 43.7579 21
-9 -4 2 336.21 45.1413 21
9 -4 -2 483.238 45.8875 7
9 4 -2 429.476 50.0919 7
9 4 -1 11559.6 200.422 7
9 5 -7 8896.94 158.357 6
-9 5 6 89.633 27.8215 21
-9 -5 6 63.143 23.0516 21
9 5 -6 65.2219 25.6059 6
9 -5 -5 1250.6 77.6821 7
9 5 -5 1064.16 61.3508 7
-9 5 5 1248.96 74.4015 21
-9 -5 5 1159.49 70.337 21
9 5 -5 1123.78 59.5979 6
9 -5 -4 1700.75 88.2244 7
-9 5 4 1834.04 92.5425 21
-9 -5 4 1592.9 87.7879 21
-9 5 3 96.454 36.474 21
-9 -5 3 49.4903 36.9777 21
9 -5 -3 145.628 37.7292 7
9 5 -3 53.6985 33.24 7
-9 5 2 -4.22486 23.8265 21
-9 -5 2 -38.5408 27.4141 21
9 -5 -2 -47.6503 25.4189 7
9 5 -2 23.6686 30.3713 7
9 5 -1 1678.27 67.9829 7
9 6 -7 677.47 42.4668 6
-9 6 6 88.2784 27.6773 21
9 6 -6 -52.0944 25.9678 6
9 -6 -5 1201.52 64.3372 16
9 -6 -5 1310.43 73.6261 7
-9 6 5 1251.08 72.2082 21
-9 -6 5 1100.41 65.7152 21
9 6 -5 1058.76 59.2696 6
-9 -6 4 40.4281 34.4003 21
9 -6 -4 -14.7693 33.6067 7
9 6 -4 52.036 27.2852 7
9 6 -4 48.9408 23.8453 6
9 -6 -3 1342.19 70.0819 7
9 6 -3 1326.9 69.2263 7
-9 6 3 1304.77 73.4045 21
-9 -6 3 1367.11 77.325 21
-9 6 2 37.3387 22.2891 21
-9 -6 2 122.524 30.9204 21
9 6 -2 114.532 30.9069 7
-9 7 6 709.803 46.5146 21
9 7 -6 795.483 50.6802 6
9 -7 -5 1234.51 64.4041 16
-9 7 5 1262.53 68.9167 21
-9 -7 5 1278.84 65.8774 21
9 7 -5 1148.55 61.5436 6
9 -7 -4 837.271 56.0613 7
-9 7 4 722.952 56.9871 21
-9 -7 4 769.92 58.1243 21
9 -7 -3 494.947 41.9523 7
9 7 -3 487.073 41.4118 7
-9 7 3 468.076 46.0959 21
-9 -7 3 499.414 51.2163 21
-9 7 2 -16.8261 18.62 21
-9 -7 2 49.8355 25.5575 21
9 7 -2 19.8669 22.8423 7
9 8 -6 253.066 32.2924 6
9 -8 -5 169.858 33.0798 16
-9 8 5 185.783 32.9383 21
-9 -8 5 228.094 31.7858 21
9 8 -5 133.741 28.881 6
-9 8 4 201.56 36.4341 21
9 8 -4 146.695 27.4329 6
-9 8 3 118.428 29.3227 21
-9 -8 3 59.904 27.6836 21
-9 -8 2 310.834 34.3611 21
9 -9 -5 57.7194 23.2621 16
-9 9 5 38.2423 22.8426 21
9 9 -5 -3.60383 20.4922 6
9 -9 -4 80.1399 28.3433 16
-9 9 4 17.8074 22.7774 21
-9 -9 4 78.523 25.2888 21
-9 9 3 822.229 48.3174 21
-9 -9 3 793.901 50.7252 21

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_res_file                  
;
TITL
CELL 1.54184 7.796837 21.151208 9.104618 90 114.1889 90
ZERR 4 0.00022 0.000467 0.000255 0 0.0033 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
 
SFAC C H O
UNIT 64 72 16
EQIV $1 2-X,1-Y,2-Z
 
L.S. 10
PLAN  20
TEMP -153(2)
HTAB O15 O11_$1
HTAB O9 O16
fmap 2
acta
REM <HKL>C:/Users/pczwl/Dropbox/Organic/LMCJMA/LMCJMA.hkl</HKL>
 
WGHT    0.049800    0.348000
FVAR       5.23697
C1    1    0.690166    0.463028    0.507165    11.00000    0.01888    0.01894 =
         0.01902    0.00147    0.00721    0.00241
C2    1    0.799464    0.488694    0.656965    11.00000    0.01908    0.01782 =
         0.01905    0.00047    0.00660    0.00114
C3    1    0.816759    0.455313    0.798181    11.00000    0.02034    0.02009 =
         0.01682   -0.00082    0.00436    0.00017
AFIX  43
H3    2    0.889612    0.473371    0.900483    11.00000   -1.20000
AFIX   0
C4    1    0.732764    0.398646    0.791522    11.00000    0.01944    0.01985 =
         0.01872    0.00317    0.00615    0.00283
C4A   1    0.622974    0.369958    0.640050    11.00000    0.01672    0.01816 =
         0.02149    0.00049    0.00622    0.00206
C5    1    0.542487    0.309562    0.632398    11.00000    0.02241    0.01940 =
         0.02420    0.00293    0.00713    0.00090
AFIX  43
H5    2    0.557159    0.288405    0.728871    11.00000   -1.20000
AFIX   0
C6    1    0.443555    0.281407    0.486788    11.00000    0.02568    0.01864 =
         0.02947   -0.00134    0.00822   -0.00250
AFIX  43
H6    2    0.393254    0.240238    0.483144    11.00000   -1.20000
AFIX   0
C7    1    0.415385    0.312611    0.342523    11.00000    0.02539    0.02184 =
         0.02363   -0.00496    0.00604   -0.00233
AFIX  43
H7    2    0.346101    0.292590    0.242088    11.00000   -1.20000
AFIX   0
C8A   1    0.599316    0.402843    0.496115    11.00000    0.01745    0.01804 =
         0.02022   -0.00042    0.00626    0.00165
C8    1    0.488196    0.372224    0.346674    11.00000    0.02021    0.02186 =
         0.01987   -0.00074    0.00639    0.00151
O9    3    0.675232    0.494745    0.373238    11.00000    0.02969    0.02256 =
         0.01570    0.00084    0.00485   -0.00560
AFIX 147
H9    2    0.600290    0.475591    0.291222    11.00000   -1.50000
AFIX   0
C10   1    0.905617    0.549336    0.685274    11.00000    0.02065    0.02048 =
         0.01956   -0.00049    0.00588    0.00011
O11   3    0.998776    0.565198    0.825278    11.00000    0.04018    0.02681 =
         0.01920   -0.00042    0.00417   -0.01102
C12   1    0.902488    0.590964    0.550422    11.00000    0.02018    0.01948 =
         0.02161    0.00163    0.00730    0.00042
AFIX  23
H12A  2    0.771031    0.603543    0.483698    11.00000   -1.20000
H12B  2    0.948664    0.566488    0.481250    11.00000   -1.20000
AFIX   0
C13   1    1.021860    0.650195    0.609202    11.00000    0.02580    0.02182 =
         0.03139    0.00113    0.01177   -0.00279
AFIX  23
H13A  2    1.154433    0.637864    0.672386    11.00000   -1.20000
H13B  2    0.978659    0.674200    0.681075    11.00000   -1.20000
AFIX   0
C14   1    1.010163    0.692513    0.469329    11.00000    0.03506    0.02836 =
         0.04656    0.01139    0.01890   -0.00086
AFIX 137
H14A  2    1.042975    0.667892    0.393337    11.00000   -1.50000
H14B  2    1.098103    0.727894    0.510717    11.00000   -1.50000
H14C  2    0.881911    0.708887    0.414250    11.00000   -1.50000
AFIX   0
O15   3    0.748100    0.365481    0.925747    11.00000    0.02873    0.02092 =
         0.01779    0.00224    0.00508   -0.00432
AFIX 147
H15   2    0.820147    0.384849    1.008647    11.00000   -1.50000
AFIX   0
O16   3    0.460486    0.405814    0.209709    11.00000    0.02856    0.02433 =
         0.01667   -0.00233    0.00443   -0.00435
C17   1    0.346285    0.378652    0.054452    11.00000    0.03413    0.03018 =
         0.01817   -0.00641    0.00499   -0.00484
AFIX  23
H17A  2    0.219296    0.368540    0.047722    11.00000   -1.20000
H17B  2    0.404502    0.339216    0.037975    11.00000   -1.20000
AFIX   0
C18   1    0.333450    0.426698   -0.071205    11.00000    0.03495    0.03540 =
         0.01937   -0.00109    0.00642   -0.00035
AFIX 137
H18A  2    0.256353    0.409783   -0.178349    11.00000   -1.50000
H18B  2    0.459843    0.436155   -0.063659    11.00000   -1.50000
H18C  2    0.275781    0.465490   -0.053562    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM
REM R1 =  0.0329 for    2433 Fo > 4sig(Fo)  and  0.0378 for all    2766 data
REM    185 parameters refined using      0 restraints
 
END  
     
WGHT      0.0498      0.3481 

REM Highest difference peak  0.279,  deepest hole -0.180,  1-sigma level  0.038
Q1    1   0.8460  0.5176  0.6588  11.00000  0.05    0.28
Q2    1   0.6494  0.4318  0.4986  11.00000  0.05    0.24
Q3    1   0.5930  0.3393  0.6369  11.00000  0.05    0.24
Q4    1   0.6777  0.3848  0.7142  11.00000  0.05    0.23
Q5    1   0.9634  0.6188  0.5797  11.00000  0.05    0.22
Q6    1   0.6154  0.3869  0.5685  11.00000  0.05    0.21
Q7    1   0.7380  0.4801  0.5867  11.00000  0.05    0.21
Q8    1   0.4712  0.3368  0.3470  11.00000  0.05    0.20
Q9    1   0.5565  0.3864  0.4241  11.00000  0.05    0.20
Q10   1   0.8102  0.4700  0.7202  11.00000  0.05    0.19
Q11   1   0.9014  0.5701  0.6150  11.00000  0.05    0.18
Q12   1   0.3357  0.4009 -0.0157  11.00000  0.05    0.18
Q13   1   0.8022  0.4240  0.7924  11.00000  0.05    0.17
Q14   1   0.4439  0.3007  0.4191  11.00000  0.05    0.15
Q15   1   0.4803  0.3004  0.5572  11.00000  0.05    0.14
Q16   1   1.0049  0.6716  0.5403  11.00000  0.05    0.11
Q17   1   0.9417  0.6826  0.3367  11.00000  0.05    0.11
Q18   1   0.0677  0.3648  0.0935  11.00000  0.05    0.10
Q19   1   0.5242  0.4319  0.2172  11.00000  0.05    0.10
Q20   1   0.7441  0.5184  0.3722  11.00000  0.05    0.10

REM The information below was added by Olex2.
REM
REM R1 = 0.0329 for 2433 Fo > 4sig(Fo) and 0.0378 for all 12831 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.28, deepest hole -0.18
REM Mean Shift 0, Max Shift 0.

REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0378
REM R1_gt = 0.0329
REM wR_ref = 0.0941
REM GOOF = 1.044
REM Shift_max = 0
REM Shift_mean = 0
REM Reflections_all = 12831
REM Reflections_gt = 2433
REM Parameters = n/a
REM Hole = 0.28
REM Peak = -0.18
REM Flack = n/a

;
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 952121'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_lmcjmm

_nottingham_internal_coll_name   LMCJMM
_nottingham_internal_coll_number 12611
_nottingham_internal_coll_client LM/CJM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '80 and 320s'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   28/6/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user WL
_nottingham_internal_process_date 1/7/2013
_nottingham_internal_solution_user WL
_nottingham_internal_solution_date 1/7/2013
_nottingham_internal_refinement_user WL
_nottingham_internal_refinement_date 1/7/2013
_nottingham_internal_validation_user WL
_nottingham_internal_validation_date 4/7/2013
_nottingham_internal_archive_date 4/7/2013

_audit_creation_date             2013-07-04
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H16 O4'
_chemical_formula_sum            'C15 H16 O4'
_chemical_formula_weight         260.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H16 O4'
_chemical_oxdiff_usercomment     
'LMCJMM #12611 IN FOMBLIN FIML ON MICROMOUNT FOR LM/CJM'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.8287(3)
_cell_length_b                   7.9789(3)
_cell_length_c                   24.2643(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2483.67(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5510
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2240
_cell_measurement_theta_min      3.6340
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  1.018
_exptl_absorpt_correction_T_min  0.931
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.1243
_exptl_crystal_size_mid          0.0791
_exptl_crystal_size_min          0.0316
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13106
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.782
_diffrn_reflns_theta_min         3.643
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.9822
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -46.00   28.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000    0.0000 74

#__ type_ start__ end____ width___ exp.time_
  2 omega   18.00  105.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573   57.0000  120.0000 87

#__ type_ start__ end____ width___ exp.time_
  3 omega   30.00   75.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000   90.0000 45

#__ type_ start__ end____ width___ exp.time_
  4 omega   66.00  109.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -94.0000  -60.0000 43

#__ type_ start__ end____ width___ exp.time_
  5 omega   82.00  170.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   45.0000    0.0000 88

#__ type_ start__ end____ width___ exp.time_
  6 omega   30.00   89.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -30.0000 -180.0000 59

#__ type_ start__ end____ width___ exp.time_
  7 omega  133.00  172.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   77.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
  8 omega   10.00  112.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573   77.0000 -120.0000 102

#__ type_ start__ end____ width___ exp.time_
  9 omega  -28.00   65.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573  -57.0000  120.0000 93

#__ type_ start__ end____ width___ exp.time_
 10 omega   81.00  173.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   45.0000  150.0000 92

#__ type_ start__ end____ width___ exp.time_
 11 omega   63.00  167.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526   15.0000  -90.0000 104

#__ type_ start__ end____ width___ exp.time_
 12 omega   23.00  109.00   1.0000  320.0000
omega____ theta____ kappa____ phi______ frames
    -      103.2526  -94.0000  120.0000 86
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0989630000
_diffrn_orient_matrix_UB_12      -0.1015532000
_diffrn_orient_matrix_UB_13      -0.0133929000
_diffrn_orient_matrix_UB_21      0.0267683000
_diffrn_orient_matrix_UB_22      0.0080701000
_diffrn_orient_matrix_UB_23      -0.0618470000
_diffrn_orient_matrix_UB_31      0.0625415000
_diffrn_orient_matrix_UB_32      -0.1639833000
_diffrn_orient_matrix_UB_33      0.0052578000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2126
_reflns_number_total             2494
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2\s(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+1.0941P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1191
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C7(H7), C5(H5)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O16 O 0.67725(8) 0.76409(15) 0.25196(5) 0.0262(3) Uani 1 1 d . . . . .
O9 O 0.90276(8) 0.41491(15) 0.05269(5) 0.0266(3) Uani 1 1 d . . . . .
H9 H 0.9078(17) 0.357(3) 0.0221(10) 0.040 Uiso 1 1 d . U . . .
O11 O 0.85646(8) 0.24904(15) -0.03394(5) 0.0261(3) Uani 1 1 d . . . . .
O15 O 0.48170(8) 0.46262(15) 0.09914(5) 0.0251(3) Uani 1 1 d . . . . .
C8A C 0.76583(11) 0.5102(2) 0.10977(6) 0.0206(3) Uani 1 1 d . . . . .
C3 C 0.61745(11) 0.3702(2) 0.03803(6) 0.0215(3) Uani 1 1 d . . . . .
H3 H 0.5673 0.3237 0.0136 0.026 Uiso 1 1 calc R U . . .
C1 C 0.79890(11) 0.4243(2) 0.06140(6) 0.0214(3) Uani 1 1 d . . . . .
C2 C 0.72617(11) 0.3548(2) 0.02517(6) 0.0210(3) Uani 1 1 d . . . . .
C4 C 0.58477(10) 0.4500(2) 0.08440(6) 0.0212(3) Uani 1 1 d . . . . .
C4A C 0.65770(10) 0.52515(19) 0.12140(6) 0.0201(3) Uani 1 1 d . . . . .
C10 C 0.76079(11) 0.2656(2) -0.02394(6) 0.0220(3) Uani 1 1 d . . . . .
C8 C 0.83859(11) 0.5810(2) 0.14698(7) 0.0240(3) Uani 1 1 d . . . . .
H8 H 0.9111 0.5721 0.1395 0.029 Uiso 1 1 calc R U . . .
C7 C 0.80599(11) 0.6616(2) 0.19327(7) 0.0242(3) Uani 1 1 d . . . . .
H7 H 0.8558 0.7071 0.2181 0.029 Uiso 1 1 calc R U . . .
C12 C 0.68161(11) 0.1946(2) -0.06330(6) 0.0230(3) Uani 1 1 d . . . . .
H12A H 0.6303 0.2832 -0.0722 0.028 Uiso 1 1 calc R U . . .
H12B H 0.6436 0.1029 -0.0445 0.028 Uiso 1 1 calc R U . . .
C5 C 0.62491(11) 0.6106(2) 0.16948(6) 0.0218(3) Uani 1 1 d . . . . .
H5 H 0.5527 0.6215 0.1775 0.026 Uiso 1 1 calc R U . . .
C6 C 0.69810(11) 0.6781(2) 0.20470(6) 0.0220(3) Uani 1 1 d . . . . .
C13 C 0.72672(11) 0.1271(2) -0.11684(7) 0.0257(4) Uani 1 1 d . . . . .
H13A H 0.7737 0.0318 -0.1087 0.031 Uiso 1 1 calc R U . . .
H13B H 0.7683 0.2158 -0.1350 0.031 Uiso 1 1 calc R U . . .
C17 C 0.57050(12) 0.7921(2) 0.26512(7) 0.0291(4) Uani 1 1 d . . . . .
H17A H 0.5379 0.8588 0.2359 0.044 Uiso 1 1 calc R U . . .
H17B H 0.5656 0.8526 0.3002 0.044 Uiso 1 1 calc R U . . .
H17C H 0.5345 0.6842 0.2683 0.044 Uiso 1 1 calc R U . . .
C14 C 0.64057(13) 0.0693(3) -0.15560(8) 0.0366(4) Uani 1 1 d . . . . .
H14A H 0.6714 0.0302 -0.1903 0.055 Uiso 1 1 calc R U . . .
H14B H 0.5932 0.1629 -0.1631 0.055 Uiso 1 1 calc R U . . .
H14C H 0.6016 -0.0226 -0.1384 0.055 Uiso 1 1 calc R U . . .
H15 H 0.444(2) 0.397(3) 0.0777(10) 0.055 Uiso 1 1 d . U . . .

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
O16 0.0193(5) 0.0331(6) 0.0264(5) -0.0041(5) -0.0010(4) -0.0002(4)
O9 0.0131(5) 0.0344(7) 0.0322(6) -0.0058(5) 0.0010(4) 0.0013(4)
O11 0.0154(5) 0.0311(6) 0.0318(6) -0.0048(5) 0.0018(4) 0.0022(4)
O15 0.0122(5) 0.0330(6) 0.0300(6) -0.0061(5) 0.0011(4) -0.0009(4)
C8A 0.0161(7) 0.0206(8) 0.0250(7) 0.0031(6) -0.0005(5) 0.0006(5)
C3 0.0155(7) 0.0229(7) 0.0260(7) 0.0002(6) -0.0016(5) -0.0001(5)
C1 0.0139(6) 0.0229(8) 0.0274(7) 0.0034(7) 0.0003(5) 0.0013(5)
C2 0.0157(7) 0.0212(8) 0.0262(7) 0.0014(6) 0.0002(5) 0.0014(5)
C4 0.0132(6) 0.0233(7) 0.0270(7) 0.0035(6) 0.0005(5) 0.0008(5)
C4A 0.0165(7) 0.0192(7) 0.0246(7) 0.0045(6) -0.0006(5) 0.0002(5)
C10 0.0168(7) 0.0219(8) 0.0274(7) 0.0031(7) 0.0002(5) 0.0022(6)
C8 0.0150(6) 0.0268(8) 0.0301(8) 0.0032(7) -0.0017(5) -0.0004(6)
C7 0.0188(7) 0.0268(8) 0.0269(7) 0.0007(7) -0.0033(6) -0.0015(6)
C12 0.0166(6) 0.0250(8) 0.0275(7) -0.0011(7) -0.0008(5) 0.0019(6)
C5 0.0151(6) 0.0233(8) 0.0269(7) 0.0030(7) 0.0009(5) 0.0007(5)
C6 0.0204(7) 0.0222(8) 0.0235(7) 0.0020(6) -0.0002(5) -0.0003(6)
C13 0.0190(7) 0.0285(9) 0.0296(8) -0.0033(7) 0.0001(6) 0.0010(6)
C17 0.0222(8) 0.0366(9) 0.0285(8) -0.0043(8) 0.0003(6) 0.0062(7)
C14 0.0249(8) 0.0496(12) 0.0354(9) -0.0130(9) -0.0047(7) 0.0057(7)

_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
O16 C6 1.3629(19) . ?
O16 C17 1.4239(18) . ?
O9 H9 0.88(2) . ?
O9 C1 1.3511(17) . ?
O11 C10 1.2580(18) . ?
O15 C4 1.3734(16) . ?
O15 H15 0.88(3) . ?
C8A C1 1.424(2) . ?
C8A C4A 1.4205(18) . ?
C8A C8 1.416(2) . ?
C3 H3 0.9500 . ?
C3 C2 1.4344(19) . ?
C3 C4 1.359(2) . ?
C1 C2 1.397(2) . ?
C2 C10 1.457(2) . ?
C4 C4A 1.429(2) . ?
C4A C5 1.415(2) . ?
C10 C12 1.505(2) . ?
C8 H8 0.9500 . ?
C8 C7 1.360(2) . ?
C7 H7 0.9500 . ?
C7 C6 1.418(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.521(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.523(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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
C6 O16 C17 117.17(12) . . ?
C1 O9 H9 103.5(15) . . ?
C4 O15 H15 109.3(16) . . ?
C4A C8A C1 119.68(13) . . ?
C8 C8A C1 121.41(13) . . ?
C8 C8A C4A 118.91(14) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C4 C3 C2 121.34(14) . . ?
O9 C1 C8A 116.71(13) . . ?
O9 C1 C2 122.57(14) . . ?
C2 C1 C8A 120.72(13) . . ?
C3 C2 C10 121.07(13) . . ?
C1 C2 C3 118.60(14) . . ?
C1 C2 C10 120.32(13) . . ?
O15 C4 C4A 115.85(13) . . ?
C3 C4 O15 123.15(13) . . ?
C3 C4 C4A 120.99(13) . . ?
C8A C4A C4 118.64(14) . . ?
C5 C4A C8A 119.64(13) . . ?
C5 C4A C4 121.71(13) . . ?
O11 C10 C2 120.42(14) . . ?
O11 C10 C12 119.77(14) . . ?
C2 C10 C12 119.81(12) . . ?
C8A C8 H8 119.6 . . ?
C7 C8 C8A 120.82(13) . . ?
C7 C8 H8 119.6 . . ?
C8 C7 H7 119.8 . . ?
C8 C7 C6 120.37(14) . . ?
C6 C7 H7 119.8 . . ?
C10 C12 H12A 108.6 . . ?
C10 C12 H12B 108.6 . . ?
C10 C12 C13 114.75(12) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.6 . . ?
C13 C12 H12B 108.6 . . ?
C4A C5 H5 120.1 . . ?
C6 C5 C4A 119.77(13) . . ?
C6 C5 H5 120.1 . . ?
O16 C6 C7 113.76(13) . . ?
O16 C6 C5 125.75(13) . . ?
C5 C6 C7 120.49(14) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.02(12) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
O16 C17 H17A 109.5 . . ?
O16 C17 H17B 109.5 . . ?
O16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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
O9 H9 O11 0.88(2) 1.74(2) 2.5540(16) 154(2) .
O15 H15 O11 0.88(3) 1.94(3) 2.8171(16) 177(2) 3_455

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O9 C1 C2 C3 179.64(14) . . . . ?
O9 C1 C2 C10 0.9(2) . . . . ?
O11 C10 C12 C13 -7.8(2) . . . . ?
O15 C4 C4A C8A 177.32(14) . . . . ?
O15 C4 C4A C5 -1.5(2) . . . . ?
C8A C1 C2 C3 -0.7(2) . . . . ?
C8A C1 C2 C10 -179.37(14) . . . . ?
C8A C4A C5 C6 -0.2(2) . . . . ?
C8A C8 C7 C6 -0.8(2) . . . . ?
C3 C2 C10 O11 -178.04(14) . . . . ?
C3 C2 C10 C12 2.7(2) . . . . ?
C3 C4 C4A C8A -2.1(2) . . . . ?
C3 C4 C4A C5 179.14(15) . . . . ?
C1 C8A C4A C4 1.2(2) . . . . ?
C1 C8A C4A C5 -179.96(14) . . . . ?
C1 C8A C8 C7 -179.49(15) . . . . ?
C1 C2 C10 O11 0.6(2) . . . . ?
C1 C2 C10 C12 -178.66(14) . . . . ?
C2 C3 C4 O15 -177.78(14) . . . . ?
C2 C3 C4 C4A 1.6(2) . . . . ?
C2 C10 C12 C13 171.51(14) . . . . ?
C4 C3 C2 C1 -0.2(2) . . . . ?
C4 C3 C2 C10 178.53(15) . . . . ?
C4 C4A C5 C6 178.53(14) . . . . ?
C4A C8A C1 O9 179.83(14) . . . . ?
C4A C8A C1 C2 0.1(2) . . . . ?
C4A C8A C8 C7 0.2(2) . . . . ?
C4A C5 C6 O16 179.50(14) . . . . ?
C4A C5 C6 C7 -0.3(2) . . . . ?
C10 C12 C13 C14 -176.03(15) . . . . ?
C8 C8A C1 O9 -0.4(2) . . . . ?
C8 C8A C1 C2 179.84(15) . . . . ?
C8 C8A C4A C4 -178.51(14) . . . . ?
C8 C8A C4A C5 0.3(2) . . . . ?
C8 C7 C6 O16 -178.96(14) . . . . ?
C8 C7 C6 C5 0.9(2) . . . . ?
C17 O16 C6 C7 177.44(14) . . . . ?
C17 O16 C6 C5 -2.4(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3 -5 2 0.0572 2.9994 -5.0056 2.0516 0.1840 -0.0870 1.0192
8 -2 0 0.0364 7.9999 -2.0098 0.0327 -0.5880 0.1959 0.8301
8 1 -2 0.0410 8.0003 0.9911 -1.9952 -0.8657 0.3456 0.3273
-1 5 -2 0.0433 -0.9994 5.0035 -2.0480 -0.3818 0.1403 -0.8938
-7 3 0 0.0337 -6.9998 3.0095 -0.0401 0.3876 -0.1606 -0.9315
-1 0 -16 0.0248 -0.9989 -0.0086 -16.0053 0.3141 0.9631 -0.1452
1 0 16 0.0068 0.9989 0.0086 16.0053 -0.3141 -0.9631 0.1452
3 -4 -9 0.0476 3.0003 -4.0115 -8.9600 0.2305 0.6021 0.7983
-7 -3 2 0.0526 -7.0005 -2.9936 2.0153 0.9698 -0.3362 0.0637
3 0 -15 0.0281 3.0011 -0.0122 -14.9979 -0.0949 1.0078 0.1108

loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 0 2 135900 669.042 2
0 0 -2 144315 973.244 1
0 0 3 22.4597 44.1716 2
0 0 -3 -0.46918 64.375 8
0 0 4 1044.4 100.327 2
0 0 -4 932.285 130.107 8
0 0 5 -17.6441 62.6403 2
0 0 -5 40.7293 104.545 8
0 0 6 69044.3 848.261 2
0 0 -6 69012.9 1065.36 8
0 0 7 41.1476 101.303 2
0 0 -7 -495.658 248.072 8
0 0 8 30.6491 83.5354 2
0 0 -8 46.9 140.51 8
0 0 -9 -111.573 180.571 8
0 0 9 23.4498 85.0794 2
0 0 -10 85369 1629.29 8
0 0 10 88572.3 1295.86 2
0 0 11 133.896 140.859 2
0 0 -11 2952.68 628.775 8
0 0 12 32178.1 880.97 2
0 0 -12 34828.3 1238.61 8
0 0 -13 478.579 349.804 8
0 0 13 -43.3431 97.2089 2
0 0 14 124616 1860.38 2
0 0 -14 120977 2483.42 8
0 0 15 -8.13377 95.2759 2
0 0 -15 -13.1511 229.156 8
0 0 16 917.601 196.718 2
0 0 -16 606.171 295.078 8
0 0 17 13.0289 64.9985 6
0 0 -17 41.0346 101.459 11
0 0 -17 -141.238 228.837 8
0 0 -18 3497.85 628.923 8
0 0 18 3664.35 215.229 6
0 0 -18 3678.62 252.037 11
0 0 -19 -79.0778 242.701 8
0 0 19 -59.3421 81.3514 6
0 0 -19 -24.4283 106.083 11
0 0 20 5657.4 265.008 6
0 0 -20 5532.13 328.097 11
0 0 -20 4717.88 736.56 8
0 0 21 -27.3586 90.0199 6
0 0 -21 -4.94828 116.372 11
0 0 -21 -90.8883 250.927 8
0 0 22 33718.4 653.879 6
0 0 -22 34528.8 780.614 11
0 0 23 -16.7604 86.4754 6
0 0 -23 14.5835 125.58 11
0 0 24 867.675 135.311 6
0 0 -24 906.7 173.31 11
0 0 25 29.1444 74.4808 6
0 0 -25 -8.26252 133.816 11
0 0 26 -2.5057 70.8212 6
0 0 -26 -46.6194 121.543 11
0 0 27 -48.0432 65.7595 6
0 0 -27 107.588 117.34 11
0 0 28 315.196 76.0231 6
0 0 -28 237.967 108.336 11
0 0 -29 156.091 92.1056 11
0 0 -30 228.37 73.4318 11
1 0 0 -25.4494 47.5615 9
-1 0 0 -11.5465 26.1301 2
-1 0 -1 7.01815 23.446 2
1 0 1 7.73719 39.4288 9
-1 0 1 19.636 38.9277 2
-1 0 1 22.4723 22.0161 1
1 0 -2 144294 763.55 1
-1 0 -2 145535 967.107 8
-1 0 2 149688 934.069 2
1 0 2 145998 946.102 9
-1 0 2 143194 794.765 1
1 0 -2 138935 987.583 8
-1 0 3 15.1001 51.8117 1
1 0 3 0.05169 53.5655 9
-1 0 -3 -39.1774 76.113 8
1 0 -3 -11.8574 78.797 8
-1 0 3 11.4306 56.2278 2
-1 0 4 20819.2 448.626 2
1 0 -4 20226 493.534 8
-1 0 -4 20867.6 485.14 8
-1 0 4 20679.1 487.121 1
1 0 -5 -16.2869 124.288 8
-1 0 5 27.661 109.016 1
-1 0 -5 62.8158 119.904 8
-1 0 5 -12.8098 78.4511 2
-1 0 -6 19822 645.38 8
-1 0 6 18846.7 639.506 1
-1 0 6 18759.3 516.073 2
1 0 6 19952.4 409.977 2
-1 0 7 19.5614 125.828 2
-1 0 -7 350.667 374.325 8
-1 0 -8 5368.07 382.929 8
1 0 8 5717.29 267.678 2
1 0 -8 5373.96 397.959 8
-1 0 8 5081.39 324.857 2
-1 0 -9 110.828 203.236 8
-1 0 9 -86.9746 116.088 2
1 0 9 -18.393 81.0246 2
-1 0 10 10262.1 487.324 2
1 0 10 10420.9 419.506 2
-1 0 -10 9844.27 589.265 8
1 0 -10 10677 624.516 8
-1 0 11 39.9422 114.34 2
1 0 11 -87.6588 96.8357 2
1 0 -12 2921.24 381.653 8
-1 0 12 3672.99 347.602 2
-1 0 -12 3180.64 370.408 8
1 0 12 3978.69 296.253 2
1 0 13 -40.5669 90.6093 2
-1 0 13 24.7018 107.831 2
-1 0 -13 51.7929 359.376 8
-1 0 -14 35652.5 1330.96 8
1 0 14 36318.1 922.166 2
1 0 -14 35413.8 1396.09 8
-1 0 14 36554.5 1085.29 2
-1 0 -15 112.876 211.718 8
-1 0 15 47.3981 134.769 2
1 0 -15 61.9525 204.525 8
1 0 -16 2322.01 481.593 8
-1 0 16 1749.82 280.175 2
1 0 -17 0.4692 240.451 8
-1 0 -17 6.06519 85.3973 11
-1 0 17 -156.156 126.319 2
1 0 17 -0.69005 71.2182 6
-1 0 -17 100.223 245.769 8
1 0 -17 40.3368 97.3812 11
-1 0 17 4.14851 65.3557 6
1 0 17 -21.0286 76.8007 5
-1 0 -18 3216.87 231.042 11
-1 0 -18 3275.93 604.256 8
1 0 18 3393.17 202.406 6
1 0 -18 3298.44 239.197 11
-1 0 18 3387.63 197.151 6
1 0 -18 2506.39 541.472 8
1 0 18 3130.77 260.2 5
-1 0 19 19.2183 70.7541 6
1 0 19 53.7389 119.216 5
-1 0 -19 -192.875 112.276 11
1 0 -19 14.403 108.059 11
1 0 -19 0.41235 293.45 8
1 0 19 75.5203 87.1845 6
-1 0 -19 -246.679 338.134 8
-1 0 20 1397.18 147.49 6
1 0 20 1294.02 149.012 6
1 0 -20 1028.05 377.109 8
-1 0 -20 1131.85 405.611 8
1 0 -20 1045.44 170.458 11
-1 0 -20 1190.62 165.535 11
-1 0 -21 132.976 133.793 11
1 0 -21 122.939 135.136 11
-1 0 21 51.2438 85.4052 6
1 0 21 -46.9751 87.2139 6
1 0 -21 48.2328 256.222 8
-1 0 -21 -103.072 239.119 8
1 0 22 560.851 121.431 6
-1 0 22 615.589 120.031 6
1 0 -22 618.572 161.037 11
-1 0 -22 785.9 170.878 11
-1 0 23 29.9189 78.7487 6
-1 0 -23 -49.1396 146.544 11
1 0 -23 25.959 122.853 11
1 0 23 69.6746 93.2458 6
1 0 24 1540.51 162.346 6
-1 0 24 1675.14 159.408 6
-1 0 -24 1480.93 191.191 11
1 0 -24 1511.55 205.203 11
1 0 25 -111.742 84.2716 6
1 0 -25 140.407 138.096 11
-1 0 25 50.8737 77.2749 6
-1 0 -25 -5.02951 121.455 11
1 0 26 833.637 113.203 6
-1 0 -26 841.223 153.25 11
-1 0 26 727.248 105.652 6
1 0 -26 889.579 180.868 11
1 0 -27 34.3587 107.471 11
-1 0 -27 -103.923 119.285 11
1 0 27 8.76969 62.2908 6
-1 0 27 37.563 63.8963 6
-1 0 -28 51.6613 92.1831 11
1 0 -28 260.826 114.542 11
1 0 28 229.539 67.5497 6
-1 0 -29 -35.2156 79.4472 11
1 0 -29 -41.2083 82.0566 11
1 0 29 -2.86365 43.8853 6
1 0 -30 238.931 73.4707 11
-1 0 -30 130.969 67.5296 11
-2 0 0 657651 2098.07 2
2 0 0 673603 3061.27 9
2 0 -1 43.6894 114.613 9
-2 0 1 -31.3859 62.3535 2
2 0 1 84.6225 92.3961 9
-2 0 -1 25.7207 52.0803 2
-2 0 2 14035.1 288.476 1
-2 0 2 13792.4 362.77 2
2 0 2 14509.8 406.33 9
2 0 -2 15260.6 546.26 9
2 0 -3 -12.2361 118.475 8
-2 0 3 -55.7972 88.3764 2
-2 0 3 6.93982 54.7639 1
2 0 3 -0.3586 75.625 9
-2 0 4 5096.46 265.165 2
2 0 -4 5192.92 307.911 8
2 0 4 5334.61 274.414 9
-2 0 -4 5243.1 279.204 8
-2 0 4 5127.69 231.29 1
2 0 -5 393.363 256.195 8
2 0 5 235.997 141.463 9
-2 0 -5 68.0625 132.96 8
-2 0 5 0.24311 82.2449 1
-2 0 5 2.27557 87.5473 2
-2 0 6 38903.5 829.667 1
-2 0 -6 39926.2 874.943 8
-2 0 6 40317.9 829.743 2
2 0 -7 -30.4319 154.827 8
-2 0 7 50.9062 110.057 2
-2 0 7 11.6671 117.326 1
-2 0 -7 10.8371 136 8
-2 0 8 7416.98 477.73 1
-2 0 -8 6648.83 427.738 8
2 0 -8 6902.45 461.645 8
-2 0 8 7079.09 407.98 2
2 0 8 7392.98 280.954 2
-2 0 -9 -36.2423 157.513 8
2 0 9 -27.2956 84.2123 2
-2 0 9 -111.615 137.347 2
2 0 10 2343.76 190.039 2
2 0 -10 1572.28 209.553 8
-2 0 10 2223.69 268.714 2
2 0 11 -34.412 78.8895 2
2 0 -11 -302.751 287.014 8
-2 0 -11 -230.432 275.881 8
-2 0 11 -40.0762 127.842 2
-2 0 -12 66323.7 1663.58 8
2 0 -12 68312.5 1834.61 8
2 0 12 69913.2 1067.13 2
-2 0 12 69466.2 1505.78 2
-2 0 13 48.6471 124.533 2
2 0 -13 96.2341 214.659 8
-2 0 -13 100.935 183.797 8
-2 0 14 5081.54 453.719 2
2 0 -14 4586.87 558.458 8
-2 0 -14 4874.48 521.672 8
-2 0 15 -39.07 117.35 2
2 0 -15 -33.8699 235.066 8
-2 0 -15 17.7038 206.942 8
-2 0 -16 20944.8 1137.21 8
2 0 -16 21212.8 1271.1 8
-2 0 -16 20012.4 481.083 11
2 0 -16 19339.3 503.999 11
-2 0 -17 -1.9678 243.775 8
2 0 -17 107.027 216.418 8
2 0 17 101.432 112.817 5
-2 0 17 -53.6092 67.7839 6
-2 0 17 -108.752 145.93 2
-2 0 -17 22.5573 91.1323 11
2 0 -17 -17.3584 106.341 11
-2 0 -18 4082.55 655.09 8
2 0 18 4169.37 304.748 5
-2 0 18 4278.95 218.026 6
-2 0 18 4980.61 496.736 2
2 0 -18 3848.87 257.074 11
-2 0 -18 3977.63 255.494 11
2 0 -18 3751.46 654.434 8
2 0 19 33.4661 80.3266 6
-2 0 19 26.3532 70.6241 6
2 0 19 25.1102 91.0535 5
-2 0 19 11.6697 136.998 2
2 0 -19 82.1274 279.415 8
2 0 -19 58.7012 111.758 11
2 0 -20 1889.17 218.982 11
2 0 20 1936.26 221.977 5
-2 0 -20 2091.32 205.649 11
-2 0 20 2016.26 164.61 6
2 0 20 2009.9 172.409 6
-2 0 -20 1717.79 448.415 8
2 0 -20 1310.77 433.404 8
-2 0 -21 -106.381 237.676 8
-2 0 21 -96.1586 91.398 6
2 0 -21 10.6002 262.75 8
2 0 -21 18.6268 129.303 11
2 0 21 44.7468 85.6216 6
-2 0 -21 172.6 123.827 11
-2 0 -22 65627.3 1043.89 11
2 0 22 64354 925.087 6
-2 0 22 63348.2 865.468 6
2 0 -22 64649.5 1089.8 11
2 0 23 95.873 94.8021 6
2 0 -23 36.9646 132.668 11
-2 0 -23 -18.1967 123.866 11
-2 0 23 -12.9903 82.469 6
-2 0 -24 1702.34 205.75 11
-2 0 24 1488.18 144.886 6
2 0 -24 1487.6 206.261 11
2 0 24 1601.09 161.513 6
-2 0 25 236.561 95.5126 6
2 0 25 -56.2235 87.8538 6
2 0 -25 -173.628 137.906 11
-2 0 -25 19.3597 117.646 11
2 0 -26 -33.2051 114.693 11
2 0 26 -55.585 78.2845 6
-2 0 26 153.873 86.417 6
2 0 27 52.034 72.6939 6
-2 0 -27 107.963 131.12 11
2 0 -27 3.81753 113.244 11
2 0 28 337.267 76.4704 6
-2 0 -28 598.598 120.854 11
2 0 -28 485.812 116.436 11
2 0 29 147.34 56.4142 6
2 0 -29 7.98109 78.9902 11
-2 0 -30 741.541 89.3051 11
2 0 -30 844.529 96.8055 11
-3 0 0 18.2791 77.1052 2
3 0 0 12.8652 136.982 9
3 0 1 51.0109 117.512 9
-3 0 1 -4.55898 78.8951 2
-3 0 -1 -25.1374 83.363 2
3 0 -1 -30.923 144.235 9
-3 0 2 9777.53 356.783 2
-3 0 2 9386.24 284.351 1
3 0 -2 9915.34 521.495 9
-3 0 -2 9313.16 288.242 2
3 0 2 9630.81 406.952 9
3 0 -3 -131.945 201.031 9
-3 0 3 -37.6178 63.3772 1
3 0 3 -97.029 104.761 9
-3 0 3 -37.4047 90.4954 2
3 0 4 82580.9 1203.26 9
-3 0 4 83993.8 971.529 1
-3 0 4 82827.2 1157.27 2
-3 0 5 26.7872 96.81 2
3 0 -5 -28.7084 138.234 8
3 0 5 -26.7322 104.372 9
-3 0 -5 27.9641 126.9 8
-3 0 5 -25.1794 85.2742 1
-3 0 6 175.401 114.29 2
-3 0 -6 292.917 159.498 8
3 0 -6 248.703 185.722 8
3 0 6 214.796 106.707 9
-3 0 6 192.329 96.9777 1
-3 0 7 12.4566 101.2 1
-3 0 -7 25.1311 127.378 8
3 0 -7 2.59509 198.23 8
-3 0 7 52.0102 104.561 2
3 0 7 43.0145 104.52 9
3 0 -8 41441.3 1185.12 8
-3 0 8 40446.2 997.155 2
-3 0 -8 38929.4 1032.63 8
-3 0 9 -23.3474 124.59 1
3 0 9 -1.08105 60.1446 2
-3 0 9 25.3541 122.757 2
3 0 -9 -53.4511 197.169 8
3 0 -10 6854.33 572.332 8
-3 0 10 6424.12 467.214 2
-3 0 -10 6205.75 485.414 8
3 0 10 6730.37 268.406 2
-3 0 10 6714.31 538.917 1
3 0 -11 1.99025 198.478 8
-3 0 -11 -478.251 310.514 8
-3 0 11 48.2359 126.526 2
3 0 -12 2848.85 423.519 8
-3 0 12 2667.11 330.806 2
-3 0 -12 1935.92 293.944 8
3 0 -13 -11.9717 204.345 8
-3 0 13 -66.8869 154.679 2
-3 0 -13 -19.6767 196.294 8
-3 0 -14 2884.97 414.993 8
-3 0 14 3080.63 376.054 2
3 0 -14 2818.42 478.558 8
-3 0 -15 115.542 228.527 8
-3 0 15 -137.935 154.142 2
3 0 -15 434.374 562.918 8
-3 0 16 1043.77 249.963 2
3 0 16 898.921 141.447 5
-3 0 -16 959.335 329.923 8
-3 0 -16 859.361 134.098 11
3 0 -16 1391.34 428.673 8
3 0 -16 1067.82 162.445 11
-3 0 -17 -81.6832 104.175 11
3 0 -17 -88.4374 281.409 8
3 0 -17 -57.6105 105.952 11
3 0 17 5.44922 77.1984 5
-3 0 17 58.0597 79.2544 6
-3 0 -17 475.99 446.561 8
-3 0 17 248.804 193.348 2
-3 0 18 1121.55 130.722 6
3 0 -18 932.786 209.087 11
3 0 -18 924.708 403.687 8
-3 0 -18 926.728 146.39 11
-3 0 -18 1049.67 383.506 8
3 0 18 984.339 174.082 5
-3 0 18 836.723 235.296 2
-3 0 19 34.4186 72.742 6
-3 0 19 58.4202 160.749 2
3 0 -19 157.873 176.175 11
3 0 19 69.6366 103.731 5
3 0 -19 73.5674 331.505 8
-3 0 -19 322.953 136.394 11
-3 0 -19 -297.418 332.282 8
3 0 20 89.9193 106.247 5
-3 0 20 60.6096 76.7158 6
3 0 -20 52.0052 298.946 8
3 0 -20 -16.8051 128.071 11
3 0 20 127.138 94.7598 6
-3 0 20 -53.9343 159.372 2
-3 0 -20 27.6289 252.898 8
-3 0 -20 46.3572 110.947 11
-3 0 -21 -24.0465 114.182 11
3 0 21 99.3706 109.311 5
-3 0 -21 303.998 334.602 8
3 0 -21 -7.26538 125.029 11
-3 0 21 33.4782 83.3298 6
3 0 21 119.832 89.8168 6
3 0 -22 11053 489.092 11
-3 0 22 10786.5 360.306 6
-3 0 -22 11641.9 457.644 11
3 0 22 11194.9 396.035 6
3 0 23 156.529 99.8094 6
-3 0 -23 -16.0354 118.03 11
-3 0 23 174.441 97.519 6
3 0 -23 -94.731 137.731 11
3 0 -24 8334.81 419.072 11
-3 0 24 7426.04 293.987 6
3 0 24 7954.51 326.928 6
-3 0 -24 8198.76 389.74 11
3 0 25 54.7564 84.9697 6
3 0 -25 -53.1404 127.128 11
-3 0 -25 65.8715 115.977 11
-3 0 -26 3642.25 244.737 11
3 0 -26 3795.36 269.615 11
3 0 26 3902.85 207.716 6
3 0 27 74.6401 63.585 6
3 0 -27 114.678 111.628 11
-3 0 -27 61.6053 97.2767 11
3 0 -28 2481.59 200.269 11
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4 -9 3 984.725 104.667 4
4 -9 -3 821.072 107.013 4
4 -9 -4 84.8125 69.5371 4
4 -9 4 27.4693 58.2733 4
4 -9 5 86.6158 57.6025 4
4 -9 6 501.935 78.7408 4
4 -9 7 37.5058 48.3327 4
4 -9 8 474.218 67.0057 4
4 -9 9 869.204 77.4479 4
4 -9 10 5943.41 165.287 4
5 -9 0 24.5508 64.2468 4
5 -9 -1 385.851 76.5288 4
5 -9 1 369.768 71.2722 4
5 -9 -2 133.35 65.4525 4
5 -9 2 179.029 66.7924 4
5 -9 3 229.174 62.4666 4
5 -9 4 -1.97705 48.8006 4
5 -9 5 228.502 57.2732 4
5 -9 6 806.626 77.003 4
5 -9 7 761.112 68.2971 4

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_res_file                  
;
TITL
CELL 1.54184 12.82865 7.978927 24.264303 90 90 90
ZERR 8 0.000349 0.0003 0.000875 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
 
SFAC C H O
UNIT 120 128 32
EQIV $1 -0.5+X,0.5-Y,-Z
 
L.S. 9
PLAN  20
TEMP -153(2)
HTAB O9 O11
HTAB O15 O11_$1
fmap 2
bond $h
conf
wpdb -1
htab
acta
REM <HKL>C:\Dropbox\Organic\LMCJMM\LMCJMM.hkl</HKL>
 
WGHT    0.063600    1.094100
FVAR       3.34036
O16   3    0.677247    0.764091    0.251960    11.00000    0.01931    0.03307 =
         0.02637   -0.00410   -0.00105   -0.00020
O9    3    0.902760    0.414908    0.052690    11.00000    0.01307    0.03440 =
         0.03224   -0.00581    0.00105    0.00127
H9    2    0.907772    0.357205    0.022106    11.00000   -1.50000
O11   3    0.856459    0.249044   -0.033940    11.00000    0.01544    0.03110 =
         0.03179   -0.00478    0.00182    0.00221
O15   3    0.481703    0.462624    0.099135    11.00000    0.01225    0.03303 =
         0.03004   -0.00610    0.00111   -0.00088
C8A   1    0.765827    0.510183    0.109774    11.00000    0.01609    0.02057 =
         0.02503    0.00305   -0.00047    0.00058
C3    1    0.617448    0.370182    0.038030    11.00000    0.01550    0.02294 =
         0.02596    0.00022   -0.00162   -0.00010
AFIX  43
H3    2    0.567269    0.323664    0.013636    11.00000   -1.20000
AFIX   0
C1    1    0.798903    0.424291    0.061398    11.00000    0.01388    0.02285 =
         0.02740    0.00338    0.00026    0.00127
C2    1    0.726165    0.354780    0.025173    11.00000    0.01569    0.02119 =
         0.02616    0.00137    0.00017    0.00144
C4    1    0.584771    0.449971    0.084401    11.00000    0.01319    0.02334 =
         0.02699    0.00349    0.00051    0.00082
C4A   1    0.657703    0.525154    0.121404    11.00000    0.01649    0.01920 =
         0.02463    0.00450   -0.00059    0.00017
C10   1    0.760787    0.265612   -0.023942    11.00000    0.01681    0.02192 =
         0.02741    0.00314    0.00021    0.00223
C8    1    0.838595    0.580985    0.146983    11.00000    0.01502    0.02680 =
         0.03014    0.00323   -0.00168   -0.00035
AFIX  43
H8    2    0.911078    0.572061    0.139522    11.00000   -1.20000
AFIX   0
C7    1    0.805991    0.661605    0.193273    11.00000    0.01882    0.02684 =
         0.02694    0.00072   -0.00333   -0.00152
AFIX  43
H7    2    0.855796    0.707127    0.218081    11.00000   -1.20000
AFIX   0
C12   1    0.681610    0.194570   -0.063296    11.00000    0.01662    0.02497 =
         0.02752   -0.00108   -0.00078    0.00194
AFIX  23
H12A  2    0.630316    0.283195   -0.072237    11.00000   -1.20000
H12B  2    0.643634    0.102870   -0.044527    11.00000   -1.20000
AFIX   0
C5    1    0.624908    0.610649    0.169480    11.00000    0.01514    0.02329 =
         0.02690    0.00304    0.00087    0.00066
AFIX  43
H5    2    0.552726    0.621544    0.177457    11.00000   -1.20000
AFIX   0
C6    1    0.698102    0.678077    0.204702    11.00000    0.02036    0.02225 =
         0.02351    0.00202   -0.00015   -0.00032
C13   1    0.726721    0.127088   -0.116843    11.00000    0.01903    0.02848 =
         0.02960   -0.00334    0.00013    0.00102
AFIX  23
H13A  2    0.773706    0.031834   -0.108687    11.00000   -1.20000
H13B  2    0.768324    0.215773   -0.135021    11.00000   -1.20000
AFIX   0
C17   1    0.570496    0.792100    0.265123    11.00000    0.02218    0.03661 =
         0.02851   -0.00427    0.00034    0.00615
AFIX 137
H17A  2    0.537905    0.858798    0.235912    11.00000   -1.50000
H17B  2    0.565623    0.852560    0.300184    11.00000   -1.50000
H17C  2    0.534487    0.684218    0.268331    11.00000   -1.50000
AFIX   0
C14   1    0.640573    0.069258   -0.155601    11.00000    0.02486    0.04956 =
         0.03536   -0.01303   -0.00467    0.00574
AFIX 137
H14A  2    0.671399    0.030212   -0.190253    11.00000   -1.50000
H14B  2    0.593227    0.162915   -0.163094    11.00000   -1.50000
H14C  2    0.601649   -0.022572   -0.138400    11.00000   -1.50000
AFIX   0
H15   2    0.443995    0.397216    0.077661    11.00000   -1.50000
HKLF 4
 
REM
REM R1 =  0.0438 for    2126 Fo > 4sig(Fo)  and  0.0525 for all    2494 data
REM    180 parameters refined using      0 restraints
 
END  
     
WGHT      0.0636      1.0941 

REM Instructions for potential hydrogen bonds
HTAB O9 O11
EQIV $2 -x+1, -y+1, -z
HTAB C12 O15_$2
HTAB O15 O11_$1

REM Highest difference peak  0.224,  deepest hole -0.271,  1-sigma level  0.049
Q1    1   0.5974  0.4487  0.0501  11.00000  0.05    0.22
Q2    1   0.7440  0.2855  0.0088  11.00000  0.05    0.22
Q3    1   0.7602  0.3379  0.0530  11.00000  0.05    0.20
Q4    1   0.7085  0.5573  0.1097  11.00000  0.05    0.19
Q5    1   0.8553  0.6643  0.2317  11.00000  0.05    0.19
Q6    1   0.7975  0.5113  0.1407  11.00000  0.05    0.19
Q7    1   0.7079  0.1368 -0.0855  11.00000  0.05    0.18
Q8    1   0.7201  0.4750  0.1222  11.00000  0.05    0.18
Q9    1   0.7861  0.4386  0.0954  11.00000  0.05    0.18
Q10   1   0.8274  0.5755  0.1843  11.00000  0.05    0.18
Q11   1   0.7792  0.5114  0.0796  11.00000  0.05    0.17
Q12   1   0.6075  0.3593  0.0718  11.00000  0.05    0.17
Q13   1   0.4769  0.4779  0.1421  11.00000  0.05    0.17
Q14   1   0.7633  0.4240  0.0344  11.00000  0.05    0.17
Q15   1   0.8233  0.7415  0.2723  11.00000  0.05    0.17
Q16   1   0.6605  0.6064  0.1969  11.00000  0.05    0.17
Q17   1   0.6234  0.5087  0.1000  11.00000  0.05    0.16
Q18   1   0.8467  0.7802  0.2227  11.00000  0.05    0.16
Q19   1   0.7182  0.2552 -0.0483  11.00000  0.05    0.16
Q20   1   0.6402  0.5903  0.1388  11.00000  0.05    0.15

REM The information below was added by Olex2.
REM
REM R1 = 0.0438 for 2126 Fo > 4sig(Fo) and 0.0525 for all 14325 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.22, deepest hole -0.27
REM Mean Shift 0, Max Shift 0.

REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0525
REM R1_gt = 0.0438
REM wR_ref = 0.1191
REM GOOF = 1.032
REM Shift_max = 0
REM Shift_mean = 0
REM Reflections_all = 14325
REM Reflections_gt = 2126
REM Parameters = n/a
REM Hole = 0.22
REM Peak = -0.27
REM Flack = n/a

;
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 952122'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_lmcjmg

_nottingham_internal_coll_name   LMCJMG
_nottingham_internal_coll_number 12560
_nottingham_internal_coll_client LM/CJM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '3 and 12'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   14/6/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_NCS_number  ?
_nottingham_internal_process_user WL
_nottingham_internal_process_date 14/6/2013
_nottingham_internal_solution_user WL
_nottingham_internal_solution_date 14/6/2013
_nottingham_internal_refinement_user WL
_nottingham_internal_refinement_date 14/6/2013
_nottingham_internal_validation_user WL
_nottingham_internal_validation_date 17/6/2013
_nottingham_internal_archive_date 17/6/2013

_audit_creation_date             2013-06-17
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H18 O5'
_chemical_formula_sum            'C16 H18 O5'
_chemical_formula_weight         290.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16 H18 O5'
_chemical_oxdiff_usercomment     
'LMCJMG #12560 IN FOMBLIN FILM ON A MICROMOUNT FOR LM/CJM'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.7243(11)
_cell_length_b                   5.0123(3)
_cell_length_c                   18.5815(12)
_cell_angle_alpha                90
_cell_angle_beta                 107.285(7)
_cell_angle_gamma                90
_cell_volume                     1398.35(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2283
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4140
_cell_measurement_theta_min      3.2290
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1.555
_exptl_absorpt_correction_T_min  1.146
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             616
_exptl_crystal_recrystallization_method 
'crystallised by slow cooling of a hot cyclohexane solution'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.0864
_exptl_crystal_size_min          0.0426
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5181
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.350
_diffrn_reflns_theta_min         4.980
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.9986
_diffrn_measured_fraction_theta_max 0.9548
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -38.00   24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 62

#__ type_ start__ end____ width___ exp.time_
  2 omega  -44.00   26.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   45.0000 -120.0000 70

#__ type_ start__ end____ width___ exp.time_
  3 omega  -33.00   31.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 64

#__ type_ start__ end____ width___ exp.time_
  4 omega  -91.00  -63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000   60.0000 28

#__ type_ start__ end____ width___ exp.time_
  5 omega  132.00  161.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  125.0000 -180.0000 29

#__ type_ start__ end____ width___ exp.time_
  6 omega   85.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000  -90.0000 93

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   90.0000 54

#__ type_ start__ end____ width___ exp.time_
  8 omega   37.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -90.0000 57

#__ type_ start__ end____ width___ exp.time_
  9 omega  126.00  174.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  114.0000   55.0000 48

#__ type_ start__ end____ width___ exp.time_
 10 omega   42.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   33.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  150.0000 37

#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00   96.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -125.0000   60.0000 57
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova-Duo, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0124119000
_diffrn_orient_matrix_UB_12      0.0578073000
_diffrn_orient_matrix_UB_13      0.0839032000
_diffrn_orient_matrix_UB_21      0.1017703000
_diffrn_orient_matrix_UB_22      -0.0183051000
_diffrn_orient_matrix_UB_23      0.0162722000
_diffrn_orient_matrix_UB_31      0.0036068000
_diffrn_orient_matrix_UB_32      0.3015111000
_diffrn_orient_matrix_UB_33      -0.0150741000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2328
_reflns_number_total             2731
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2\s(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.2158P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1048
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C8(H8)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.72020(8) 0.7636(2) 0.33355(7) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.81186(8) 0.7919(2) 0.36335(6) 0.0178(3) Uani 1 1 d . . . . .
C3 C 0.85857(8) 0.6197(2) 0.42314(7) 0.0179(3) Uani 1 1 d . . . . .
H3 H 0.9212 0.6393 0.4440 0.022 Uiso 1 1 calc R U . . .
C4 C 0.81579(8) 0.4275(2) 0.45122(6) 0.0175(3) Uani 1 1 d . . . . .
C4A C 0.72060(8) 0.3976(2) 0.42243(7) 0.0171(3) Uani 1 1 d . . . . .
C5 C 0.66919(8) 0.2113(2) 0.45034(7) 0.0184(3) Uani 1 1 d . . . . .
C6 C 0.57790(9) 0.2014(3) 0.42214(7) 0.0216(3) Uani 1 1 d . . . . .
H6 H 0.5452 0.0793 0.4427 0.026 Uiso 1 1 calc R U . . .
C7 C 0.53291(9) 0.3717(3) 0.36293(7) 0.0229(3) Uani 1 1 d . . . . .
H7 H 0.4699 0.3615 0.3431 0.027 Uiso 1 1 calc R U . . .
C8 C 0.57904(9) 0.5520(3) 0.33362(7) 0.0217(3) Uani 1 1 d . . . . .
H8 H 0.5480 0.6660 0.2936 0.026 Uiso 1 1 calc R U . . .
C8A C 0.67274(8) 0.5690(2) 0.36279(6) 0.0183(3) Uani 1 1 d . . . . .
O9 O 0.67121(6) 0.91764(19) 0.27683(5) 0.0232(2) Uani 1 1 d . . . . .
H9 H 0.7109(14) 1.026(4) 0.2676(10) 0.035 Uiso 1 1 d . U . . .
C10 C 0.85832(9) 0.9952(2) 0.33208(7) 0.0189(3) Uani 1 1 d . . . . .
O11 O 0.81641(6) 1.13952(19) 0.27906(5) 0.0240(2) Uani 1 1 d . . . . .
C12 C 0.95752(9) 1.0269(2) 0.36388(7) 0.0200(3) Uani 1 1 d . . . . .
H12A H 0.9861 0.8521 0.3620 0.024 Uiso 1 1 calc R U . . .
H12B H 0.9718 1.0799 0.4175 0.024 Uiso 1 1 calc R U . . .
C13 C 0.99699(9) 1.2322(2) 0.32250(7) 0.0212(3) Uani 1 1 d . . . . .
H13A H 0.9785 1.1896 0.2680 0.025 Uiso 1 1 calc R U . . .
H13B H 0.9735 1.4111 0.3287 0.025 Uiso 1 1 calc R U . . .
C14 C 1.09821(9) 1.2369(3) 0.35213(8) 0.0275(3) Uani 1 1 d . . . . .
H14A H 1.1213 1.3743 0.3254 0.041 Uiso 1 1 calc R U . . .
H14B H 1.1218 1.0623 0.3438 0.041 Uiso 1 1 calc R U . . .
H14C H 1.1167 1.2769 0.4062 0.041 Uiso 1 1 calc R U . . .
O15 O 0.86749(6) 0.26839(18) 0.50732(5) 0.0222(2) Uani 1 1 d . . . . .
H15 H 0.8350(13) 0.156(4) 0.5217(11) 0.033 Uiso 1 1 d . U . . .
O16 O 0.71727(6) 0.04683(18) 0.50808(5) 0.0209(2) Uani 1 1 d . . . . .
C17 C 0.66940(9) -0.1466(3) 0.53782(7) 0.0213(3) Uani 1 1 d . . . . .
H17A H 0.6300 -0.2504 0.4956 0.026 Uiso 1 1 calc R U . . .
H17B H 0.7124 -0.2722 0.5706 0.026 Uiso 1 1 calc R U . . .
O18 O 0.61855(6) -0.0318(2) 0.57876(5) 0.0247(2) Uani 1 1 d . . . . .
C19 C 0.66974(10) 0.0931(3) 0.64667(8) 0.0317(3) Uani 1 1 d . . . . .
H19A H 0.7014 0.2469 0.6345 0.048 Uiso 1 1 calc R U . . .
H19B H 0.7129 -0.0346 0.6769 0.048 Uiso 1 1 calc R U . . .
H19C H 0.6301 0.1531 0.6754 0.048 Uiso 1 1 calc R U . . .

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
C1 0.0206(6) 0.0178(6) 0.0158(5) -0.0007(4) 0.0046(5) 0.0021(5)
C2 0.0202(6) 0.0173(6) 0.0165(5) -0.0010(4) 0.0063(5) -0.0005(5)
C3 0.0147(6) 0.0205(6) 0.0184(5) -0.0013(4) 0.0046(4) -0.0007(4)
C4 0.0181(6) 0.0177(6) 0.0164(5) -0.0005(4) 0.0048(4) 0.0015(4)
C4A 0.0175(6) 0.0174(6) 0.0174(5) -0.0027(4) 0.0065(5) -0.0006(4)
C5 0.0195(6) 0.0183(6) 0.0180(5) -0.0010(4) 0.0065(4) 0.0001(5)
C6 0.0204(6) 0.0230(6) 0.0224(6) -0.0019(5) 0.0080(5) -0.0042(5)
C7 0.0154(6) 0.0276(7) 0.0240(6) -0.0029(5) 0.0034(5) -0.0024(5)
C8 0.0201(6) 0.0246(6) 0.0190(6) 0.0000(5) 0.0036(5) 0.0013(5)
C8A 0.0187(6) 0.0190(6) 0.0171(5) -0.0027(4) 0.0054(5) 0.0000(5)
O9 0.0204(5) 0.0252(5) 0.0217(4) 0.0059(4) 0.0026(4) -0.0007(4)
C10 0.0225(6) 0.0169(6) 0.0184(5) -0.0014(4) 0.0077(5) 0.0006(5)
O11 0.0238(5) 0.0245(5) 0.0232(4) 0.0065(4) 0.0064(4) 0.0009(4)
C12 0.0207(6) 0.0185(6) 0.0217(6) 0.0019(4) 0.0078(5) -0.0004(5)
C13 0.0241(6) 0.0189(6) 0.0227(6) 0.0005(5) 0.0102(5) -0.0022(5)
C14 0.0253(7) 0.0297(7) 0.0289(7) 0.0035(5) 0.0100(6) -0.0051(5)
O15 0.0168(4) 0.0232(5) 0.0248(5) 0.0085(4) 0.0034(4) -0.0010(4)
O16 0.0173(4) 0.0224(5) 0.0236(4) 0.0062(3) 0.0069(4) -0.0014(3)
C17 0.0215(6) 0.0207(6) 0.0234(6) 0.0014(5) 0.0094(5) -0.0031(5)
O18 0.0214(5) 0.0326(5) 0.0219(4) -0.0042(4) 0.0090(4) -0.0055(4)
C19 0.0337(8) 0.0379(8) 0.0243(6) -0.0068(6) 0.0097(6) -0.0085(6)

_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 C2 1.3892(18) . ?
C1 C8A 1.4301(17) . ?
C1 O9 1.3482(15) . ?
C2 C3 1.4263(17) . ?
C2 C10 1.4703(17) . ?
C3 H3 0.9500 . ?
C3 C4 1.3643(17) . ?
C4 C4A 1.4399(17) . ?
C4 O15 1.3710(15) . ?
C4A C5 1.4295(17) . ?
C4A C8A 1.4273(17) . ?
C5 C6 1.3749(18) . ?
C5 O16 1.3857(15) . ?
C6 H6 0.9500 . ?
C6 C7 1.4059(19) . ?
C7 H7 0.9500 . ?
C7 C8 1.3690(19) . ?
C8 H8 0.9500 . ?
C8 C8A 1.4132(18) . ?
O9 H9 0.88(2) . ?
C10 O11 1.2418(16) . ?
C10 C12 1.5034(18) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.5230(16) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.5218(18) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O15 H15 0.85(2) . ?
O16 C17 1.4351(14) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 O18 1.3821(15) . ?
O18 C19 1.4244(17) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

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
C2 C1 C8A 120.99(11) . . ?
O9 C1 C2 122.51(11) . . ?
O9 C1 C8A 116.50(11) . . ?
C1 C2 C3 118.81(11) . . ?
C1 C2 C10 119.44(11) . . ?
C3 C2 C10 121.74(11) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.80(11) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C4A 120.51(11) . . ?
C3 C4 O15 116.94(11) . . ?
O15 C4 C4A 122.55(11) . . ?
C5 C4A C4 124.80(11) . . ?
C8A C4A C4 118.42(11) . . ?
C8A C4A C5 116.77(11) . . ?
C6 C5 C4A 121.60(11) . . ?
C6 C5 O16 122.78(11) . . ?
O16 C5 C4A 115.60(11) . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.14(12) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.61(12) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C8A 120.15(12) . . ?
C8A C8 H8 119.9 . . ?
C4A C8A C1 119.43(11) . . ?
C8 C8A C1 119.84(11) . . ?
C8 C8A C4A 120.71(11) . . ?
C1 O9 H9 103.4(12) . . ?
C2 C10 C12 119.81(11) . . ?
O11 C10 C2 120.56(11) . . ?
O11 C10 C12 119.63(11) . . ?
C10 C12 H12A 108.8 . . ?
C10 C12 H12B 108.8 . . ?
C10 C12 C13 113.81(10) . . ?
H12A C12 H12B 107.7 . . ?
C13 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
C12 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 C12 111.53(11) . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 O15 H15 110.3(13) . . ?
C5 O16 C17 118.17(10) . . ?
O16 C17 H17A 109.0 . . ?
O16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
O18 C17 O16 112.71(10) . . ?
O18 C17 H17A 109.0 . . ?
O18 C17 H17B 109.0 . . ?
C17 O18 C19 113.80(10) . . ?
O18 C19 H19A 109.5 . . ?
O18 C19 H19B 109.5 . . ?
O18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
O9 H9 O11 0.88(2) 1.71(2) 2.5289(13) 154.0(18) .
O15 H15 O16 0.85(2) 1.88(2) 2.6139(12) 144.0(18) .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.54(18) . . . . ?
C1 C2 C10 O11 -0.58(18) . . . . ?
C1 C2 C10 C12 -179.89(11) . . . . ?
C2 C1 C8A C4A -1.32(17) . . . . ?
C2 C1 C8A C8 177.30(11) . . . . ?
C2 C3 C4 C4A -1.84(18) . . . . ?
C2 C3 C4 O15 178.30(11) . . . . ?
C2 C10 C12 C13 176.17(10) . . . . ?
C3 C2 C10 O11 178.65(11) . . . . ?
C3 C2 C10 C12 -0.66(17) . . . . ?
C3 C4 C4A C5 -176.96(11) . . . . ?
C3 C4 C4A C8A 1.52(17) . . . . ?
C4 C4A C5 C6 177.23(11) . . . . ?
C4 C4A C5 O16 -1.65(17) . . . . ?
C4 C4A C8A C1 0.04(16) . . . . ?
C4 C4A C8A C8 -178.57(11) . . . . ?
C4A C5 C6 C7 1.87(19) . . . . ?
C4A C5 O16 C17 -179.26(10) . . . . ?
C5 C4A C8A C1 178.64(10) . . . . ?
C5 C4A C8A C8 0.03(17) . . . . ?
C5 C6 C7 C8 -1.2(2) . . . . ?
C5 O16 C17 O18 -70.19(14) . . . . ?
C6 C5 O16 C17 1.88(17) . . . . ?
C6 C7 C8 C8A -0.06(19) . . . . ?
C7 C8 C8A C1 -177.99(11) . . . . ?
C7 C8 C8A C4A 0.62(19) . . . . ?
C8A C1 C2 C3 1.06(17) . . . . ?
C8A C1 C2 C10 -179.69(10) . . . . ?
C8A C4A C5 C6 -1.28(17) . . . . ?
C8A C4A C5 O16 179.84(10) . . . . ?
O9 C1 C2 C3 -179.73(11) . . . . ?
O9 C1 C2 C10 -0.48(18) . . . . ?
O9 C1 C8A C4A 179.42(10) . . . . ?
O9 C1 C8A C8 -1.95(17) . . . . ?
C10 C2 C3 C4 -178.70(11) . . . . ?
C10 C12 C13 C14 -174.53(11) . . . . ?
O11 C10 C12 C13 -3.14(16) . . . . ?
O15 C4 C4A C5 2.89(18) . . . . ?
O15 C4 C4A C8A -178.63(10) . . . . ?
O16 C5 C6 C7 -179.34(11) . . . . ?
O16 C17 O18 C19 -66.63(14) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 0 0 0.0213 1.0012 0.0003 -0.0010 0.0124 0.1019 0.0037
-1 0 0 0.0213 -1.0012 -0.0003 0.0010 -0.0124 -0.1019 -0.0037
0 3 1 0.2200 -0.0070 2.9998 1.0074 0.2578 -0.0392 0.8893
1 0 -4 0.0320 0.9951 0.0005 -3.9980 -0.3231 0.0362 0.0640
-3 -1 12 0.0949 -2.9824 -1.0016 11.9914 0.9112 -0.0901 -0.4935
3 -1 -12 0.0739 2.9881 -0.9983 -11.9969 -1.0272 0.1272 -0.1094
6 3 -2 0.1864 5.9957 3.0020 -1.9962 0.0805 0.5228 0.9568
5 0 8 0.0396 5.0184 0.0013 7.9893 0.7327 0.6407 -0.1019
-8 0 10 0.0429 -7.9944 -0.0032 10.0005 0.7397 -0.6508 -0.1806
-6 0 -7 0.0331 -6.0181 -0.0017 -6.9890 -0.6612 -0.7262 0.0831

loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_scale_group_code
0 0 -2 46668.5 698.282 2
0 0 -3 -36.666 77.5565 2
0 0 -4 103020 1530.95 2
0 0 -5 1.11886 112.13 2
0 0 -6 127843 2162.8 2
0 0 -7 -37.6575 130.761 2
0 0 -8 979.88 243.746 2
0 0 -9 7.97066 149.046 2
0 0 -10 77547.5 2287.75 2
0 0 -11 -6.73825 113.793 2
0 0 -12 42403.1 1881.81 2
0 0 -12 41980.1 886.597 7
0 0 -13 3.77843 66.6255 7
0 0 -13 -166.393 177.722 2
0 0 -14 119664 3398.07 2
0 0 -14 119463 1695.73 7
0 0 -15 -119.004 90.2438 10
0 0 -15 121.133 93.9294 7
0 0 -16 1716.31 220.471 7
0 0 -16 2065.55 235.957 10
0 0 -17 -22.8475 81.3993 7
0 0 -17 -58.9568 74.2169 10
0 0 -18 205.383 101.019 10
0 0 -18 204.031 105.058 7
0 0 -19 -38.6175 80.1523 10
0 0 -19 0.42122 75.6692 7
0 0 -20 8427.96 388.12 10
0 0 -21 -58.1719 58.4585 11
0 0 -22 22568.4 402.466 11
0 1 0 -28.6651 72.5967 4
0 1 0 -16.0547 30.7802 2
0 1 0 34.6916 33.9241 3
0 1 -1 71378.9 937.881 2
0 1 1 70608.5 1048.13 4
0 1 1 72165.5 688.632 3
0 1 -1 70517.6 1080.38 4
0 1 -1 71111.8 746.765 1
0 1 -1 72772.9 923.093 3
0 1 -2 42366.2 869.745 2
0 1 2 41497.2 790.976 4
0 1 -2 42866.6 699.605 1
0 1 3 4192.8 248.299 4
0 1 -3 4179.74 324.428 2
0 -1 -3 4156.69 186.309 2
0 -1 -4 56600 917.273 2
0 1 -4 58907.1 1015.53 4
0 1 -4 57848.3 1337 2
0 1 -5 79671.7 1174.67 4
0 -1 -5 76982.4 1280.28 2
0 1 -5 80109.4 1723.71 2
0 -1 -6 55742.1 1198.33 2
0 1 -6 54913.9 1556.14 2
0 1 -6 55589.9 959.563 4
0 1 -7 1178.46 294.248 2
0 1 -7 1026.87 124.84 4
0 -1 -7 1026.69 193.107 2
0 1 -8 10850.9 377.59 4
0 -1 -8 10786.4 651.231 2
0 1 -8 10352.9 804.878 2
0 1 -9 39319.9 1649.24 2
0 -1 -9 41224.6 1371.56 2
0 1 -10 9883.78 881.323 2
0 -1 -10 11191.3 766.984 2
0 1 -11 1231.95 373.62 2
0 -1 -11 562.422 147.414 2
0 1 12 4075.52 232.038 8
0 1 -12 4137.73 630.785 2
0 -1 -12 4290.91 271.051 7
0 1 -12 4840.47 324.927 7
0 -1 -12 5085.7 576.749 2
0 -1 -13 19422.9 608.195 7
0 1 13 18406 534.002 8
0 1 -13 18826 1411.54 2
0 1 -13 18820.5 673.834 7
0 1 -14 6008.94 403.111 7
0 -1 -14 5429.77 340.216 10
0 -1 -14 5884.6 355.465 7
0 1 14 5611.38 303.664 8
0 1 -15 1092.08 181.584 7
0 1 15 1171.85 141.962 8
0 -1 -15 1242.02 160.932 10
0 -1 -15 990.745 156.648 7
0 1 -15 1092.51 191.909 10
0 1 -16 3856.59 335.546 10
0 -1 -16 4046.38 300.861 7
0 -1 -16 3557.83 277.478 10
0 1 -16 3361.72 322.865 7
0 -1 -17 18.7447 69.4495 7
0 1 -17 -32.4623 98.7073 10
0 -1 -17 41.448 63.3335 10
0 1 -17 8.87934 108.648 7
0 1 -18 2435.72 259.125 10
0 1 -18 2725.68 268.867 7
0 -1 -18 2689.59 217.563 10
0 1 -19 15.5482 85.4101 7
0 -1 -19 12.9698 47.0578 10
0 1 -19 33.9461 67.5551 10
0 1 -20 4422.87 278.529 10
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-14 4 8 1882.25 129.895 8
-14 4 8 1960.65 126.021 9
-14 4 7 19002.3 408.979 8
-14 4 7 18851.5 408.311 9
-14 4 6 17734.2 388.583 8
-14 4 6 18702.1 420.125 9
-14 4 5 1432.78 108.319 8
-14 4 5 1730.14 134.168 9
-14 4 4 1999.95 119.142 8
-14 4 4 2122.55 148.401 9
-14 4 3 6051.39 239.9 9
-14 4 2 9106.71 274.889 9
-14 4 1 981.998 86.1627 9
15 0 -19 -65.7592 36.238 7
15 0 -18 4164.39 241.026 7
15 0 -17 6.45924 47.8212 7
15 0 -16 285.416 115.14 6
15 0 -15 -115.851 105.361 6
15 0 -14 20296.9 714.114 6
15 0 -13 -48.3545 131.552 6
15 0 -12 725.268 195.956 6
15 0 -11 -144.812 149.309 6
15 0 -10 105712 1800.92 6
15 0 -9 -32.8961 127.936 6
15 0 -8 480.628 173.174 6
15 0 -7 -22.9639 120.308 6
15 0 -6 3437.63 341.702 6
15 0 -5 22.0612 115.224 6
15 0 -4 7478.56 487.155 6
15 0 -3 -4.10313 130.051 6
15 0 -2 9121.34 530.73 6
15 0 -1 -122.415 150.004 6
15 0 0 40839.6 1095.84 6
15 0 1 -82.9589 125.06 6
15 0 2 987.543 190.251 6
15 0 3 146.005 103.178 6
15 0 4 -20.4253 92.4431 6
15 0 5 -20.2694 88.4419 6
15 0 6 2315.86 214.045 6
15 0 7 -6.49056 59.9564 6
15 0 8 720.623 96.2359 6
15 1 -19 197.668 51.8086 7
15 1 -18 4607.99 247.463 7
15 -1 -17 61.0227 36.996 7
15 1 -17 160.231 65.2332 7
15 -1 -16 20148.4 534.497 7
15 1 -15 25389.6 745.961 6
15 -1 -15 26878 719.37 6
15 1 -14 12609.2 543.073 6
15 -1 -14 12548.9 524.551 6
15 1 -13 350.306 139.367 6
15 -1 -13 383.773 132.38 6
15 1 -12 1579.26 224.574 6
15 -1 -12 1245.42 186.776 6
15 1 -11 1866.15 236.397 6
15 -1 -11 1689.56 234.178 6
15 1 -10 2683.83 285.348 6
15 -1 -10 2864.81 298.496 6
15 1 -9 1428.61 221.965 6
15 -1 -9 1722.49 233.132 6
15 1 -8 75.0195 101.674 6
15 -1 -8 -5.27054 112.891 6
15 1 -7 -86.8809 118.195 6
15 -1 -7 136.437 133.242 6
15 1 -6 6368.07 427.559 6
15 -1 -6 6280.48 444.885 6
15 1 -5 8416.3 480.123 6
15 -1 -5 8449.58 511.53 6
15 -1 -4 2036.14 265.569 6
15 1 -4 2430.16 265.005 6
15 -1 -3 1872.8 258.762 6
15 1 -3 1893.47 235.493 6
15 1 -2 4113.75 330.482 6
15 -1 -2 3685.92 360.997 6
15 1 -1 2522.13 254.275 6
15 -1 -1 2489.05 294.292 6
15 1 0 46.2994 105.922 6
15 -1 0 69.7947 137.339 6
15 1 1 -14.8783 94.0121 6
15 -1 1 -19.3251 120.355 6
15 1 2 307.4 111.841 6
15 -1 2 -69.2647 145.889 6
15 -1 3 1403.71 216.062 6
15 1 3 1726.36 180.613 6
15 1 4 18.2678 57.909 6
15 -1 4 42.0553 97.4674 6
15 -1 5 5461.31 347.394 6
15 -1 6 149.434 82.266 6
15 -1 7 1675.77 164.412 6
15 -1 8 2178.72 159.127 6
15 2 -17 339.704 57.2645 7
15 2 -16 1940.03 155.854 7
-15 2 15 3079.51 157.263 8
15 2 -15 2438.04 196.541 7
-15 2 14 3596.54 199.401 8
-15 2 13 701.189 100.427 8
15 -2 -13 703.861 106.523 6
-15 2 12 400.906 80.5828 9
15 2 -12 520.91 113.781 6
15 -2 -12 651.111 111.218 6
15 2 -11 -60.8043 84.2051 6
15 -2 -11 -41.0862 74.0183 6
15 2 -10 4375.92 285.383 6
15 -2 -10 3834.59 277.636 6
15 2 -9 384.169 102.379 6
15 -2 -9 480.895 119.227 6
15 2 -8 340.878 88.2945 6
15 -2 -8 419.885 129.203 6
15 2 -7 2035.98 200.116 6
15 -2 -7 2260.79 230.859 6
15 -2 -6 3684.52 297.934 6
15 -2 -5 3908.56 310.524 6
15 -2 -4 2083.88 229.75 6
15 -2 -3 432.787 104.645 6
15 -2 -2 1995.7 231.633 6
15 -2 -1 10630 506.966 6
15 -2 0 1383.4 204.856 6
15 -2 1 -1.51793 83.668 6
15 -2 2 3729.63 283.626 6
-15 2 -2 3334.83 190.794 9
15 -2 3 3984.65 278.805 6
15 -2 4 738.023 125.823 6
15 -2 5 2436.85 190.287 6
15 -2 6 374.859 73.2425 6
-15 3 14 7.25774 19.2563 8
-15 3 13 1415.35 113.97 8
-15 3 12 897.141 104.112 8
-15 3 11 2029.89 162.128 8
-15 3 11 1977.8 134.179 9
-15 3 10 2348.2 181.668 8
-15 3 10 2154.44 160.279 9
-15 3 9 409.636 86.0867 9
-15 3 8 134.199 66.6101 9
-15 3 7 125.012 70.5986 9
-15 3 6 1243.21 156.825 9
-15 3 5 593.821 112.62 9
-15 3 4 -40.8105 65.4071 9
-15 3 3 70.4435 62.3027 9
-15 3 2 1393.92 138.803 9
15 3 -1 1114.39 93.1363 5
-15 3 1 1213.27 126.609 9
-15 3 0 -43.7648 46.158 9
15 3 0 34.4825 27.756 5
15 3 1 1140.93 93.6736 5
-15 3 -1 1097.19 95.9872 9
15 3 2 45.6166 27.6857 5
15 3 3 593.861 61.4064 5
-15 4 6 10455.4 247.603 9
-15 4 5 14619.8 297.479 9
-15 4 4 23.3943 31.0878 9
16 0 -18 2337.44 148.674 7
16 0 -17 -11.5043 41.4624 7
16 0 -16 806.227 129.29 6
16 0 -15 -80.0726 95.061 6
16 0 -14 1898.42 210.466 6
16 0 -13 101.425 98.6415 6
16 0 -12 6152.46 398.279 6
16 0 -11 -30.9121 110.147 6
16 0 -10 1407.61 229.453 6
16 0 -9 21.1787 115.095 6
16 0 -8 3675.8 329.058 6
16 0 -7 68.1125 117.005 6
16 0 -6 2648.63 309.221 6
16 0 -5 -92.8756 149.35 6
16 0 -4 63.4051 115.167 6
16 0 -3 8.5755 108.207 6
16 0 -2 119.477 110.084 6
16 0 -1 -55.5917 107.874 6
16 0 0 131.683 127.946 6
16 0 1 -33.6095 108.43 6
16 0 2 377.74 122.716 6
16 0 3 102.973 94.3004 6
16 0 4 7096.73 357.12 6
16 0 5 -36.8728 52.778 6
16 0 6 2352.22 165.615 6
16 1 -17 26067.6 557.64 7
16 -1 -16 15091 376.346 7
16 1 -16 17066.2 516.237 7
16 1 -15 2571.43 221.454 6
16 -1 -15 2525.78 203.195 6
16 1 -14 3863.01 276.593 6
16 -1 -14 3701.88 263.261 6
16 1 -13 14226.5 543.55 6
16 -1 -13 13680.6 524.124 6
16 1 -12 1003.67 164.57 6
16 -1 -12 1298.84 179.949 6
16 1 -11 178.138 107.223 6
16 -1 -11 334.97 113.365 6
16 1 -10 2314.57 253.782 6
16 -1 -10 2069.46 246.788 6
16 1 -9 221.141 114.608 6
16 -1 -9 72.5637 93.3005 6
16 1 -8 3293.92 304.294 6
16 -1 -8 3002.08 291.927 6
16 1 -7 278.041 113.503 6
16 -1 -7 290.564 140.033 6
16 1 -6 202.134 108.468 6
16 -1 -6 104.289 108.354 6
16 1 -5 4567.54 339.374 6
16 -1 -5 5093.19 387.18 6
16 1 -4 1685.88 223.498 6
16 -1 -4 1972.35 257.448 6
16 1 -3 24249.3 756.002 6
16 -1 -3 25305.2 842.627 6
16 -1 -2 1225.8 213.491 6
16 1 -2 1144.56 172.548 6
16 -1 -1 389.175 157.19 6
16 1 -1 484.083 111.117 6
16 -1 0 608.334 156.777 6
16 1 0 444.478 95.9996 6
16 -1 1 10.5557 97.0877 6
16 1 1 96.3797 70.6241 6
16 -1 2 284.917 123.575 6
16 1 2 27.0344 61.2995 6
16 -1 3 726.614 137.119 6
16 -1 4 1126.62 156.329 6
16 -1 5 2610.99 198.654 6
16 -1 6 18653.3 460.446 6
16 2 -15 613.204 85.7696 7
-16 2 14 147.7 35.7013 8
16 2 -14 121.12 44.6882 7
-16 2 13 468.562 70.5127 8
-16 2 12 151.904 48.3243 9
-16 2 12 221.641 60.3646 8
16 -2 -12 175.291 63.372 6
-16 2 11 -4.65343 43.5635 9
16 -2 -11 87.5929 51.0307 6
16 -2 -10 2762.49 215.908 6
16 -2 -9 389.946 93.9318 6
16 -2 -8 12930 490.014 6
16 -2 -7 2407.95 218.083 6
16 -2 -6 1857.82 198.07 6
16 -2 -5 2859.22 255.275 6
16 -2 -4 2676.62 243.06 6
16 -2 -3 59.831 76.4609 6
16 -2 -2 1896.59 199.08 6
16 -2 -1 3547.02 268.015 6
-16 2 0 921.693 113.918 9
16 -2 0 1181.65 154.792 6
16 -2 1 1666.24 172.544 6
-16 2 -1 1486.87 123.755 9
16 -2 2 39.9791 56.2139 6
16 2 2 51.429 25.9122 5
16 -2 3 -0.77374 45.4625 6
16 2 3 1.49121 19.7544 5
16 -2 4 1033.74 112.445 6
-16 3 12 5280.22 192.031 8
-16 3 11 225.787 52.917 8
-16 3 10 5020.48 222.806 8
-16 3 10 5091.5 198.556 9
-16 3 9 6496.01 263.179 8
-16 3 9 5996.77 239.467 9
-16 3 8 1468.41 125.999 9
-16 3 7 8.53924 42.1263 9
-16 3 6 113 44.4711 9
-16 3 5 11.2662 51.4277 9
-16 3 4 6029.88 258.897 9
-16 3 3 1378.96 124.185 9
-16 3 2 460.053 73.5666 9
-16 3 1 -87.2483 48.3651 9
17 0 -16 1167.76 122.353 7
17 0 -15 -31.4163 66.8651 6
17 0 -14 218.204 85.3638 6
17 0 -13 -154.395 102.338 6
17 0 -12 350.106 125.133 6
17 0 -11 148.989 99.8978 6
17 0 -10 744.053 162.805 6
17 0 -9 68.1188 106.284 6
17 0 -8 3833.89 321.464 6
17 0 -7 55.3074 110.182 6
17 0 -6 6228.47 406.458 6
17 0 -5 111.07 119.845 6
17 0 -4 296.75 118.405 6
17 0 -3 -43.4439 91.7359 6
17 0 -2 204.283 99.4904 6
17 0 -1 0.20528 83.7269 6
17 0 0 2247.44 225.072 6
17 0 1 -44.3147 79.2073 6
17 0 2 3755.04 251.241 6
17 0 3 91.698 66.0234 6
17 0 4 449.604 73.3297 6
17 1 -16 3603.7 193.276 7
17 1 -14 1024.83 127.476 6
17 -1 -14 906.363 116.71 6
17 1 -13 501.765 103.876 6
17 -1 -13 377.528 93.4121 6
17 1 -12 3923.04 264.943 6
17 -1 -12 3878.79 263.444 6
17 1 -11 1668.33 187.177 6
17 -1 -11 1464.3 178.363 6
17 1 -10 1090.04 158.09 6
17 -1 -10 896.878 154.19 6
17 1 -9 5007.47 326.637 6
17 -1 -9 4661.13 325.643 6
17 1 -8 1963.18 218.397 6
17 -1 -8 1847.34 215.377 6
17 1 -7 340.3 110.204 6
17 -1 -7 247.689 112.246 6
17 1 -6 1733.64 198.14 6
17 -1 -6 1642.39 216.061 6
17 1 -5 -146.838 116.03 6
17 -1 -5 12.1725 97.8084 6
17 1 -4 8915.77 414.015 6
17 -1 -4 8601.64 454.493 6
17 1 -3 1874.43 192.702 6
17 -1 -3 1769.12 217.716 6
17 1 -2 2488.27 209.213 6
17 -1 -2 2728.12 258.402 6
17 1 -1 2356.93 196.867 6
17 -1 -1 2402.4 239.026 6
17 1 0 2473.49 187.398 6
17 -1 0 2482.25 228.651 6
17 -1 1 2267.31 209.963 6
17 -1 2 697.179 119.269 6
17 -1 3 326.832 77.438 6
17 -1 4 252.686 62.3981 6
17 2 -13 132.751 46.0165 7
-17 2 12 154.726 33.7582 9
-17 2 12 393.447 57.0718 8
-17 2 11 173.427 50.7662 9
17 -2 -11 28.1475 26.7859 6
17 -2 -10 2166.25 160.608 6
-17 2 10 2280.04 162.812 9
-17 2 9 476.819 97.7545 9
17 -2 -9 556.814 91.9132 6
17 -2 -8 4434.44 252.432 6
17 -2 -7 5882.78 296.255 6
17 -2 -6 5304.37 286.115 6
17 -2 -5 22.3098 53.5131 6
17 -2 -4 2984.66 219.008 6
17 -2 -3 5681.63 295.858 6
-17 2 2 417.033 93.925 9
17 -2 -2 423.334 94.301 6
-17 2 1 -67.2331 47.938 9
17 -2 -1 59.9385 46.833 6
17 -2 0 3183.92 196.363 6
-17 2 0 2503.28 133.448 9
17 -2 1 71.5274 45.0136 6
-17 3 9 316.194 50.0173 8
-17 3 8 137.678 37.626 9
-17 3 8 184.295 43.6985 8
-17 3 7 4079.05 170.17 9
-17 3 6 3050.45 148.731 9
-17 3 5 393.707 56.2093 9
-17 3 4 1148.44 86.6119 9
18 0 -14 1242.19 125.353 6
18 0 -13 -7.11946 51.2339 6
18 0 -12 4085.97 258.284 6
18 0 -11 48.14 63.7328 6
18 0 -10 320.886 92.07 6
18 0 -9 -180.446 110.437 6
18 0 -8 899.056 153.359 6
18 0 -7 15.5712 82.1598 6
18 0 -6 261.559 111.706 6
18 0 -5 132.863 90.3 6
18 0 -4 1483.73 183.637 6
18 0 -3 74.3546 77.9045 6
18 0 -2 1532.9 168.376 6
18 0 -1 -38.1933 56.4664 6
18 0 0 2134.81 174.194 6
18 0 1 66.4272 50.7182 6
18 1 -13 1957.58 154.725 6
18 -1 -13 1873.7 144.049 6
18 1 -12 497.594 85.7647 6
18 -1 -12 526.735 80.925 6
18 1 -11 893.335 117.574 6
18 -1 -11 650.185 102.521 6
18 1 -10 1055.05 124.572 6
18 -1 -10 1008.81 130.498 6
18 1 -9 767.759 118.276 6
18 -1 -9 787.283 127.273 6
18 1 -8 -91.4936 76.6238 6
18 -1 -8 19.0771 71.3597 6
18 1 -7 213.475 80.4983 6
18 -1 -7 249.33 93.8143 6
18 1 -6 107.715 61.6028 6
18 -1 -6 170.783 96.4314 6
18 1 -5 976.731 124.586 6
18 -1 -5 736.219 131.749 6
18 1 -4 546.267 99.244 6
18 -1 -4 331.629 103.63 6
18 1 -3 364.173 81.4184 6
18 -1 -3 472.145 113.273 6
18 -1 -2 322.847 90.5761 6
18 -1 -1 4338.57 261.424 6
18 -1 0 4986.84 256.367 6
18 -1 1 3225.75 191.244 6
-18 2 10 388.786 51.6729 9
-18 2 10 518.64 59.1741 8
-18 2 9 632.638 73.7829 9
-18 2 8 1287.48 112.82 9
18 -2 -7 4099.53 189.58 6
-18 2 7 4820.76 218.766 9
-18 2 6 69.9363 40.0296 9
18 -2 -6 10.9331 37.8841 6
18 -2 -5 6742.44 252.1 6
-18 2 5 8235.6 266.364 9
18 -2 -4 14365.2 359.195 6
-18 2 4 14544.1 339.517 9
-18 2 3 54.4246 33.8211 9
19 0 -12 36.9344 41.2927 6
19 0 -11 -63.0436 45.3222 6
19 0 -10 767.218 106.123 6
19 0 -9 44.4451 63.8478 6
19 0 -8 3501.56 222.272 6
19 0 -7 -9.43272 57.5495 6
19 0 -6 1544.4 155.87 6
19 0 -5 58.2792 55.9684 6
19 0 -4 19762.1 485.341 6
19 0 -3 -67.1121 51.1848 6
19 0 -2 7869.24 271.87 6
19 -1 -10 306.163 58.3658 6
19 -1 -9 3257.08 184.606 6
19 -1 -8 5760.65 255.858 6
19 -1 -7 6795.31 281.899 6
19 -1 -6 213.437 58.7986 6
19 -1 -5 102.902 47.2963 6
19 -1 -4 28.2551 39.199 6
19 -1 -3 952.948 99.6759 6

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_shelx_res_file                  
;
TITL
CELL 1.54184 15.724286 5.012273 18.581499 90 107.2855 90
ZERR 4 0.001076 0.000349 0.001173 0 0.0072 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
 
SFAC C H O
UNIT 64 72 20
 
L.S. 9
PLAN  20
TEMP -153(2)
HTAB O15 O16
HTAB O9 O11
bond $h
conf
wpdb -1
htab
fmap 2
acta
REM <HKL>C:/Users/pczwl/Dropbox/Organic/LMCJMG/LMCJMG.hkl</HKL>
 
WGHT    0.055700    0.215800
FVAR       5.73848
C1    1    0.720201    0.763645    0.333550    11.00000    0.02056    0.01778 =
         0.01584   -0.00069    0.00455    0.00207
C2    1    0.811864    0.791910    0.363350    11.00000    0.02022    0.01732 =
         0.01650   -0.00096    0.00626   -0.00053
C3    1    0.858574    0.619667    0.423144    11.00000    0.01467    0.02050 =
         0.01842   -0.00130    0.00458   -0.00066
AFIX  43
H3    2    0.921190    0.639301    0.443989    11.00000   -1.20000
AFIX   0
C4    1    0.815788    0.427478    0.451223    11.00000    0.01805    0.01769 =
         0.01644   -0.00050    0.00477    0.00148
C4A   1    0.720598    0.397555    0.422428    11.00000    0.01748    0.01738 =
         0.01738   -0.00265    0.00646   -0.00056
C5    1    0.669187    0.211281    0.450343    11.00000    0.01949    0.01831 =
         0.01799   -0.00104    0.00653    0.00012
C6    1    0.577901    0.201447    0.422137    11.00000    0.02036    0.02303 =
         0.02236   -0.00186    0.00797   -0.00420
AFIX  43
H6    2    0.545158    0.079349    0.442699    11.00000   -1.20000
AFIX   0
C7    1    0.532915    0.371712    0.362930    11.00000    0.01536    0.02761 =
         0.02404   -0.00288    0.00340   -0.00240
AFIX  43
H7    2    0.469928    0.361541    0.343078    11.00000   -1.20000
AFIX   0
C8    1    0.579038    0.552030    0.333620    11.00000    0.02008    0.02464 =
         0.01902   -0.00002    0.00362    0.00125
AFIX  43
H8    2    0.547985    0.666023    0.293581    11.00000   -1.20000
AFIX   0
C8A   1    0.672737    0.568986    0.362788    11.00000    0.01871    0.01901 =
         0.01711   -0.00275    0.00543   -0.00004
O9    3    0.671212    0.917635    0.276828    11.00000    0.02044    0.02520 =
         0.02172    0.00593    0.00264   -0.00066
H9    2    0.710939    1.026360    0.267639    11.00000   -1.50000
C10   1    0.858315    0.995196    0.332076    11.00000    0.02245    0.01690 =
         0.01838   -0.00140    0.00767    0.00061
O11   3    0.816412    1.139518    0.279063    11.00000    0.02379    0.02451 =
         0.02322    0.00654    0.00642    0.00092
C12   1    0.957524    1.026859    0.363884    11.00000    0.02066    0.01850 =
         0.02174    0.00185    0.00776   -0.00036
AFIX  23
H12A  2    0.986143    0.852132    0.361998    11.00000   -1.20000
H12B  2    0.971783    1.079865    0.417484    11.00000   -1.20000
AFIX   0
C13   1    0.996995    1.232194    0.322496    11.00000    0.02413    0.01886 =
         0.02267    0.00050    0.01022   -0.00221
AFIX  23
H13A  2    0.978521    1.189588    0.268014    11.00000   -1.20000
H13B  2    0.973465    1.411139    0.328712    11.00000   -1.20000
AFIX   0
C14   1    1.098208    1.236852    0.352126    11.00000    0.02526    0.02974 =
         0.02886    0.00353    0.01000   -0.00508
AFIX 137
H14A  2    1.121349    1.374301    0.325428    11.00000   -1.50000
H14B  2    1.121791    1.062316    0.343845    11.00000   -1.50000
H14C  2    1.116665    1.276938    0.406186    11.00000   -1.50000
AFIX   0
O15   3    0.867487    0.268390    0.507316    11.00000    0.01676    0.02323 =
         0.02483    0.00848    0.00340   -0.00105
H15   2    0.835041    0.156263    0.521707    11.00000   -1.50000
O16   3    0.717271    0.046827    0.508079    11.00000    0.01731    0.02242 =
         0.02355    0.00624    0.00694   -0.00137
C17   1    0.669397   -0.146627    0.537821    11.00000    0.02151    0.02072 =
         0.02337    0.00144    0.00937   -0.00308
AFIX  23
H17A  2    0.630009   -0.250398    0.495634    11.00000   -1.20000
H17B  2    0.712394   -0.272178    0.570646    11.00000   -1.20000
AFIX   0
O18   3    0.618550   -0.031838    0.578757    11.00000    0.02135    0.03260 =
         0.02185   -0.00417    0.00899   -0.00552
C19   1    0.669741    0.093129    0.646665    11.00000    0.03369    0.03787 =
         0.02433   -0.00678    0.00965   -0.00850
AFIX 137
H19A  2    0.701396    0.246941    0.634476    11.00000   -1.50000
H19B  2    0.712947   -0.034649    0.676889    11.00000   -1.50000
H19C  2    0.630101    0.153074    0.675353    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM
REM R1 =  0.0362 for    2328 Fo > 4sig(Fo)  and  0.0436 for all    2731 data
REM    198 parameters refined using      0 restraints
 
END  
     
WGHT      0.0557      0.2158 

REM Instructions for potential hydrogen bonds
HTAB C6 O18
EQIV $1 -x+1, -y, -z+1
HTAB C6 O18_$1
HTAB O9 O11
HTAB O15 O16

REM Highest difference peak  0.289,  deepest hole -0.189,  1-sigma level  0.043
Q1    1   0.8352  0.8932  0.3508  11.00000  0.05    0.29
Q2    1   0.6943  0.3177  0.4381  11.00000  0.05    0.28
Q3    1   0.9748  1.1291  0.3409  11.00000  0.05    0.26
Q4    1   0.7662  0.4178  0.4396  11.00000  0.05    0.26
Q5    1   0.6975  0.6394  0.3437  11.00000  0.05    0.26
Q6    1   0.8280  0.5711  0.4502  11.00000  0.05    0.23
Q7    1   0.7644  0.8173  0.3583  11.00000  0.05    0.21
Q8    1   0.8294  0.7116  0.3880  11.00000  0.05    0.21
Q9    1   0.7749  0.7281  0.3405  11.00000  0.05    0.20
Q10   1   0.6256  0.1848  0.4277  11.00000  0.05    0.20
Q11   1   0.6993  0.4635  0.3886  11.00000  0.05    0.19
Q12   1   0.7301 -0.2233  0.5659  11.00000  0.05    0.19
Q13   1   0.6275  0.5335  0.3446  11.00000  0.05    0.19
Q14   1   0.9099  1.0082  0.3498  11.00000  0.05    0.18
Q15   1   0.5562  0.4212  0.3372  11.00000  0.05    0.18
Q16   1   1.0473  1.2215  0.3312  11.00000  0.05    0.17
Q17   1   0.5598  0.2993  0.4009  11.00000  0.05    0.13
Q18   1   0.5714 -0.0381  0.5610  11.00000  0.05    0.13
Q19   1   0.6698  0.3204  0.6343  11.00000  0.05    0.12
Q20   1   0.6877 -0.0435  0.5115  11.00000  0.05    0.12

REM The information below was added by Olex2.
REM
REM R1 = 0.0362 for 2328 Fo > 4sig(Fo) and 0.0436 for all 5600 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.29, deepest hole -0.19
REM Mean Shift 0, Max Shift 0.

REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0436
REM R1_gt = 0.0362
REM wR_ref = 0.1048
REM GOOF = 1.048
REM Shift_max = 0
REM Shift_mean = 0
REM Reflections_all = 5600
REM Reflections_gt = 2328
REM Parameters = n/a
REM Hole = 0.29
REM Peak = -0.19
REM Flack = n/a

;
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
_database_code_depnum_ccdc_archive 'CCDC 952123'