# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 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_shelxl

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H16 Cl N O4'
_chemical_formula_weight         201.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   ' P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   8.15(3)
_cell_length_b                   8.52(4)
_cell_length_c                   8.77(3)
_cell_angle_alpha                82.77(19)
_cell_angle_beta                 65.14(13)
_cell_angle_gamma                79.9(2)
_cell_volume                     543(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1141
_cell_measurement_theta_min      3.4324
_cell_measurement_theta_max      27.7475

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.3500
_exptl_crystal_size_mid          0.3000
_exptl_crystal_size_min          0.2700
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             216
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3070
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2463
_reflns_number_gt                1244
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(2)
_refine_ls_number_reflns         2463
_refine_ls_number_parameters     217
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.1098
_refine_ls_wR_factor_ref         0.3450
_refine_ls_wR_factor_gt          0.2912
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.4862(5) 0.0745(4) 0.4598(4) 0.1097(16) Uani 1 1 d DU . .
Cl2 Cl 0.2649(5) 0.5508(4) 0.9332(4) 0.1118(17) Uani 1 1 d DU . .
O1 O 0.590(2) 0.089(2) 0.3177(14) 0.258(12) Uani 1 1 d DU . .
O2 O 0.528(4) 0.143(2) 0.553(2) 0.306(15) Uani 1 1 d DU . .
O3 O 0.454(3) -0.0628(15) 0.526(2) 0.317(19) Uani 1 1 d DU . .
O4 O 0.326(2) 0.149(3) 0.482(3) 0.44(3) Uani 1 1 d DU . .
O5 O 0.358(2) 0.6828(16) 0.869(2) 0.256(13) Uani 1 1 d DU . .
O6 O 0.249(4) 0.497(2) 1.0839(16) 0.317(17) Uani 1 1 d DU . .
O7 O 0.353(2) 0.4411(13) 0.8131(11) 0.187(8) Uani 1 1 d DU . .
O8 O 0.0919(17) 0.595(3) 0.936(3) 0.38(2) Uani 1 1 d DU . .
C1 C 0.891(3) 0.232(3) -0.078(4) 0.166(9) Uani 1 1 d . . .
H1A H 0.7677 0.2518 -0.0681 0.250 Uiso 1 1 calc R . .
H1B H 0.9693 0.2802 -0.1826 0.250 Uiso 1 1 calc R . .
H1C H 0.8978 0.2784 0.0139 0.250 Uiso 1 1 calc R . .
N1 N 1.1526(14) 0.0204(15) -0.0877(12) 0.085(3) Uani 1 1 d . . .
H1D H 1.1872 -0.0855 -0.0969 0.102 Uiso 1 1 calc R . .
H1E H 1.2210 0.0677 -0.1867 0.102 Uiso 1 1 calc R . .
C2 C 0.9523(19) 0.054(2) -0.0712(17) 0.102(6) Uani 1 1 d . . .
H2A H 0.8743 0.0081 0.0386 0.122 Uiso 1 1 calc R . .
C3 C 0.940(3) -0.032(3) -0.207(2) 0.141(7) Uani 1 1 d . . .
H3A H 0.8177 -0.0123 -0.1994 0.211 Uiso 1 1 calc R . .
H3B H 0.9744 -0.1448 -0.1918 0.211 Uiso 1 1 calc R . .
H3C H 1.0217 0.0064 -0.3157 0.211 Uiso 1 1 calc R . .
C4 C 1.096(2) -0.022(2) 0.213(2) 0.117(6) Uani 1 1 d . . .
H4A H 1.1257 0.0130 0.2974 0.176 Uiso 1 1 calc R . .
H4B H 1.1297 -0.1351 0.2056 0.176 Uiso 1 1 calc R . .
H4C H 0.9677 0.0050 0.2423 0.176 Uiso 1 1 calc R . .
C5 C 1.205(2) 0.065(2) 0.036(2) 0.100(5) Uani 1 1 d . . .
H5A H 1.1711 0.1806 0.0470 0.121 Uiso 1 1 calc R . .
C6 C 1.406(2) 0.029(2) -0.020(2) 0.106(6) Uani 1 1 d . . .
H6A H 1.4651 0.0906 -0.1221 0.159 Uiso 1 1 calc R . .
H6B H 1.4438 -0.0828 -0.0386 0.159 Uiso 1 1 calc R . .
H6C H 1.4395 0.0555 0.0659 0.159 Uiso 1 1 calc R . .
N2 N 0.5975(15) 0.5985(15) 0.4868(14) 0.090(4) Uani 1 1 d . . .
H2B H 0.5612 0.7042 0.4964 0.108 Uiso 1 1 calc R . .
H2C H 0.5294 0.5496 0.5848 0.108 Uiso 1 1 calc R . .
C7 C 0.861(3) 0.389(2) 0.459(2) 0.124(6) Uani 1 1 d . . .
H7A H 0.8499 0.3485 0.3677 0.186 Uiso 1 1 calc R . .
H7B H 0.7909 0.3344 0.5632 0.186 Uiso 1 1 calc R . .
H7C H 0.9874 0.3722 0.4425 0.186 Uiso 1 1 calc R . .
C8 C 0.792(2) 0.566(2) 0.468(3) 0.114(6) Uani 1 1 d . . .
H8A H 0.8666 0.6190 0.3604 0.137 Uiso 1 1 calc R . .
C9 C 0.810(3) 0.638(4) 0.602(4) 0.192(12) Uani 1 1 d . . .
H9A H 0.7691 0.7505 0.5986 0.287 Uiso 1 1 calc R . .
H9B H 0.9349 0.6200 0.5868 0.287 Uiso 1 1 calc R . .
H9C H 0.7360 0.5898 0.7088 0.287 Uiso 1 1 calc R . .
C10 C 0.640(3) 0.636(3) 0.1843(16) 0.163(10) Uani 1 1 d . . .
H10A H 0.6093 0.6016 0.1007 0.244 Uiso 1 1 calc R . .
H10B H 0.7699 0.6166 0.1495 0.244 Uiso 1 1 calc R . .
H10C H 0.5990 0.7485 0.1973 0.244 Uiso 1 1 calc R . .
C11 C 0.551(2) 0.5472(16) 0.3464(15) 0.079(4) Uani 1 1 d . . .
H11A H 0.5947 0.4331 0.3311 0.095 Uiso 1 1 calc R . .
C12 C 0.349(2) 0.570(2) 0.413(2) 0.102(5) Uani 1 1 d . . .
H12A H 0.3128 0.5411 0.3301 0.154 Uiso 1 1 calc R . .
H12B H 0.3032 0.6796 0.4370 0.154 Uiso 1 1 calc R . .
H12C H 0.3011 0.5031 0.5138 0.154 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 O1 1.181(11) . ?
Cl1 O2 1.248(13) . ?
Cl1 O3 1.257(13) . ?
Cl1 O4 1.298(17) . ?
Cl2 O6 1.302(14) . ?
Cl2 O7 1.368(11) . ?
Cl2 O8 1.384(15) . ?
Cl2 O5 1.391(11) . ?
C1 C2 1.52(3) . ?
N1 C5 1.44(2) . ?
N1 C2 1.555(18) . ?
C2 C3 1.52(2) . ?
C4 C5 1.59(2) . ?
C5 C6 1.48(2) . ?
N2 C8 1.50(2) . ?
N2 C11 1.562(18) . ?
C7 C8 1.52(2) . ?
C8 C9 1.46(3) . ?
C10 C11 1.48(2) . ?
C11 C12 1.48(2) . ?

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
O1 Cl1 O2 111.3(12) . . ?
O1 Cl1 O3 119.4(11) . . ?
O2 Cl1 O3 107.6(12) . . ?
O1 Cl1 O4 111.0(13) . . ?
O2 Cl1 O4 102.5(11) . . ?
O3 Cl1 O4 103.4(10) . . ?
O6 Cl2 O7 114.3(10) . . ?
O6 Cl2 O8 108.6(10) . . ?
O7 Cl2 O8 106.5(11) . . ?
O6 Cl2 O5 115.0(11) . . ?
O7 Cl2 O5 104.8(8) . . ?
O8 Cl2 O5 107.1(11) . . ?
C5 N1 C2 122.5(11) . . ?
C3 C2 C1 113.9(17) . . ?
C3 C2 N1 108.3(13) . . ?
C1 C2 N1 110.1(15) . . ?
N1 C5 C6 110.2(13) . . ?
N1 C5 C4 109.2(14) . . ?
C6 C5 C4 112.9(14) . . ?
C8 N2 C11 118.7(12) . . ?
C9 C8 N2 109.9(15) . . ?
C9 C8 C7 113(2) . . ?
N2 C8 C7 111.1(13) . . ?
C10 C11 C12 114.1(13) . . ?
C10 C11 N2 111.5(13) . . ?
C12 C11 N2 106.0(11) . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 1025554'
#######################################################################
#
#                 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_I_publ

_pd_block_id                     2014-09-24T17:28|I||

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2014-09-24T17:28
_audit_update_record             
; 2014-09-24T17:28  Initial CIF as created by GSAS2CIF
;

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
; ?
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      ?
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_pd_char_colour                  ? # use ICDD colour descriptions
_refine_ls_shift/su_max          1.09
_refine_ls_shift/su_mean         0.10
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     53
_refine_ls_goodness_of_fit_all   1.96
_refine_ls_number_restraints     0
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products
_symmetry_space_group_name_Hall  ?

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    383

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

#==============================================================================

# 8. Phase information from GSAS

_pd_phase_name                   'from K:/gsas/MyWork/DIPA-ClO4/70C/bc3050.cif'
_cell_length_a                   17.662(9)
_cell_length_b                   8.7860(5)
_cell_length_c                   16.671(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 118.590(24)
_cell_angle_gamma                90.0
_cell_volume                     2271.6(13)
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
2 -x,+y+1/2,-z+1/2
-1 -x,-y,-z
-2 +x,-y+1/2,+z+1/2

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
Cl Cl2 0.60921 0.20439 0.26584 1.0 Uani 0.20661 4
O O21 0.57452 0.0819 0.2987 1.0 Uani 0.31199 4
O O22 0.6889 0.2498 0.3304 1.0 Uani 0.31199 4
O O23 0.6161 0.1435 0.1871 1.0 Uani 0.31199 4
O O24 0.55388 0.3388 0.2396 1.0 Uani 0.31199 4
Cl Cl1 0.1078 0.28299 0.34991 1.0 Uani 0.20661 4
O O11 0.07405 0.41 0.28279 1.0 Uani 0.31199 4
O O12 0.0543 0.1454 0.31697 1.0 Uani 0.31199 4
O O13 0.11082 0.3366 0.43558 1.0 Uani 0.31199 4
O O14 0.19014 0.2426 0.36572 1.0 Uani 0.31199 4
N N1 0.09458 0.7607 0.3628 1.0 Uani 0.23537 4
H H1A 0.0584 0.824 0.329 1.0 Uiso 0.56(9) 4
H H1B 0.0812 0.665 0.338 1.0 Uiso 0.56(9) 4
C C11 0.0929 0.7492 0.4552 1.0 Uani 0.29827 4
H H11 0.1313 0.6622 0.491 1.0 Uiso 0.56(9) 4
C C12 0.0049 0.703 0.4375 1.0 Uani 0.29827 4
H H12A -0.0114 0.6055 0.4012 1.0 Uiso 0.56(9) 4
H H12B -0.0333 0.7889 0.4044 1.0 Uiso 0.56(9) 4
H H12C 0.0032 0.6852 0.4958 1.0 Uiso 0.56(9) 4
C C13 0.1219 0.9042 0.5087 1.0 Uani 0.29827 4
H H13A 0.1778 0.9291 0.5172 1.0 Uiso 0.56(9) 4
H H13B 0.122 0.8922 0.5683 1.0 Uiso 0.56(9) 4
H H13C 0.0844 0.9904 0.475 1.0 Uiso 0.56(9) 4
C C14 0.1752 0.8031 0.3579 1.0 Uani 0.29827 4
H H14 0.1918 0.9127 0.3831 1.0 Uiso 0.56(9) 4
C C15 0.157 0.806 0.2562 1.0 Uani 0.29827 4
H H15A 0.1167 0.8897 0.2246 1.0 Uiso 0.56(9) 4
H H15B 0.1345 0.703 0.2284 1.0 Uiso 0.56(9) 4
H H15C 0.2082 0.8269 0.2513 1.0 Uiso 0.56(9) 4
C C16 0.2454 0.6886 0.4154 1.0 Uani 0.29827 4
H H16A 0.2541 0.6916 0.4788 1.0 Uiso 0.56(9) 4
H H16B 0.2963 0.7207 0.4124 1.0 Uiso 0.56(9) 4
H H16C 0.2306 0.5804 0.3916 1.0 Uiso 0.56(9) 4
N N2 0.40327 0.2296 0.27392 1.0 Uani 0.23537 4
H H2A 0.4432 0.167 0.276 1.0 Uiso 0.56(9) 4
H H2B 0.418 0.319 0.264 1.0 Uiso 0.56(9) 4
C C21 0.32467 0.1813 0.1909 1.0 Uani 0.29827 4
H H21 0.3116 0.0693 0.2004 1.0 Uiso 0.56(9) 4
C C22 0.2512 0.2844 0.179 1.0 Uani 0.29827 4
H H22A 0.2428 0.2783 0.234 1.0 Uiso 0.56(9) 4
H H22B 0.2015 0.2464 0.1266 1.0 Uiso 0.56(9) 4
H H22C 0.262 0.3948 0.1686 1.0 Uiso 0.56(9) 4
C C23 0.3428 0.1828 0.1076 1.0 Uani 0.29827 4
H H23A 0.392 0.1186 0.1205 1.0 Uiso 0.56(9) 4
H H23B 0.3524 0.2923 0.0943 1.0 Uiso 0.56(9) 4
H H23C 0.2955 0.1385 0.0549 1.0 Uiso 0.56(9) 4
C C24 0.4043 0.2392 0.3673 1.0 Uani 0.29827 4
H H24 0.363 0.3208 0.3644 1.0 Uiso 0.56(9) 4
C C25 0.4913 0.297 0.4363 1.0 Uani 0.29827 4
H H25A 0.5042 0.397 0.4148 1.0 Uiso 0.56(9) 4
H H25B 0.5325 0.2167 0.4418 1.0 Uiso 0.56(9) 4
H H25C 0.492 0.3139 0.4958 1.0 Uiso 0.56(9) 4
C C26 0.3802 0.0803 0.3943 1.0 Uani 0.29827 4
H H26A 0.3231 0.0546 0.352 1.0 Uiso 0.56(9) 4
H H26B 0.3853 0.0881 0.4562 1.0 Uiso 0.56(9) 4
H H26C 0.417 -0.0034 0.3921 1.0 Uiso 0.56(9) 4


# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C6 H16 Cl N O4'
_chemical_formula_weight         201.65
_cell_formula_units_Z            8

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
? ? ? ? ? ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
? ? ? ? ? ? ? ?

# Powder diffraction data for histogram  1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      383
_diffrn_source                   ?
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_measurement_device_type  ?
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'


loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
Cl 8.0 0.000 0.000 11.4604 0.01040 7.19640 1.16620 6.25560 18.5194 1.64550
47.7784 -9.5574 International_Tables_Vol_C
O 32.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
N 8.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
H 128.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081
57.7997 0.00304 International_Tables_Vol_C
C 48.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
_diffrn_radiation_probe          x-ray
_diffrn_radiation_polarisn_ratio 0.7

loop_
_diffrn_radiation_wavelength
1.540500
_diffrn_radiation_type           CuK\a

_pd_proc_ls_prof_R_factor        0.0848
_pd_proc_ls_prof_wR_factor       0.1210
_pd_proc_ls_prof_wR_expected     0.0621
_refine_ls_R_Fsqd_factor         0.30115

_pd_proc_ls_background_function  
;   GSAS Background function number 2 with  9 terms.
 Cosine Fourier series
      1:    154.044     2:    48.8714     3:    7.56067     4:   -22.6652    
      5:    17.3925     6:   -9.94049     7:   -15.1558     8:    15.1855    
      9:   -18.7188    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
# Extinction correction
_gsas_exptl_extinct_corr_T_min   1.00000
_gsas_exptl_extinct_corr_T_max   1.00000
_pd_proc_ls_pref_orient_corr     
;   March-Dollase
 AXIS  1 Ratio=     0.060 Frac     0.000  h= 0.000  k= 0.000  l= 2.000
 AXIS  2 Ratio=     8.560 Frac     0.058  h= 2.000  k= 0.000  l=-2.000
 AXIS  3 Ratio=     0.076 Frac     0.011  h= 0.000  k= 2.000  l= 2.000
 AXIS  4 Ratio=     0.099 Frac     0.011  h= 0.000  k= 1.000  l= 2.000
 AXIS  5 Ratio=     0.278 Frac     0.646  h= 1.000  k= 1.000  l= 3.000
 AXIS  6 Ratio=     0.079 Frac     0.035  h= 2.000  k= 2.000  l=-1.000
 AXIS  7 Ratio=     8.354 Frac     0.017  h= 0.000  k= 0.000  l= 4.000
 AXIS  8 Ratio=     1.058 Frac     0.221  h= 0.000  k= 1.000  l= 4.000
 Prefered orientation correction range: Min=   0.33237, Max=  35.47228
;

_pd_proc_ls_profile_function     
;
 CW Profile function number 2 with  18 terms
 Profile coefficients for Simpson's rule integration of pseudovoigt function
 C.J. Howard (1982). J. Appl. Cryst.,15,615-620.
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 #1(GU)   =  752.528 #2(GV)   = -260.757 #3(GW)   =   16.339
 #4(LX)   =    0.000 #5(LY)   =    4.774 #6(trns) =   13.825
 #7(asym) =   4.5163 #8(shft) =  -9.7733 #9(GP)   =   11.341
 #10(stec)=    16.97 #11(ptec)=     0.00 #12(sfec)=     0.00
 #13(L11) =    0.037 #14(L22) =    0.017 #15(L33) =    0.000
 #16(L12) =    0.012 #17(L13) =    0.010 #18(L23) =   -0.005
 Peak tails are ignored  where the intensity is below 0.0050 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff          0.00500
_pd_proc_info_datetime           2014-09-24T17:28:19
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        5.0
_pd_meas_2theta_range_max        69.98
_pd_meas_2theta_range_inc        0.02
_pd_proc_2theta_range_min        5.0
_pd_proc_2theta_range_max        69.98
_pd_proc_2theta_range_inc        0.02

loop_
_pd_meas_counts_total
_pd_proc_ls_weight
_pd_proc_intensity_bkg_calc
_pd_calc_intensity_total
191.0 0.00524 180.59129 180.62396
200.0 0.00500 180.62230 180.65553
206.0 0.00485 180.65343 180.68710
204.0 0.00490 180.68462 180.71887
177.0 0.00565 180.71594 180.75072
199.0 0.00503 180.74738 180.78270
206.0 0.00485 180.77892 180.81473
180.0 0.00556 180.81053 180.84695
192.0 0.00521 180.84225 180.87923
189.0 0.00529 180.87411 180.91161
198.0 0.00505 180.90607 180.94411
196.0 0.00510 180.93811 180.97668
202.0 0.00495 180.97025 181.00935
189.0 0.00529 181.00250 181.04219
200.0 0.00500 181.03488 181.07507
181.0 0.00552 181.06732 181.10809
179.0 0.00559 181.09988 181.14114
198.0 0.00505 181.13254 181.17433
202.0 0.00495 181.16530 181.20757
195.0 0.00513 181.19817 181.24092
193.0 0.00518 181.23114 181.27434
187.0 0.00535 181.26418 181.30780
202.0 0.00495 181.29738 181.34138
211.0 0.00474 181.33060 181.37508
199.0 0.00503 181.36400 181.40884
203.0 0.00493 181.39745 181.44266
181.0 0.00552 181.43100 181.47656
193.0 0.00518 181.46468 181.51051
186.0 0.00538 181.49843 181.54448
196.0 0.00510 181.53230 181.57857
203.0 0.00493 181.56625 181.61267
202.0 0.00495 181.60033 181.64688
184.0 0.00543 181.63448 181.68109
173.0 0.00578 181.66872 181.71550
193.0 0.00518 181.70306 181.74988
193.0 0.00518 181.73753 181.78427
205.0 0.00488 181.77206 181.81880
186.0 0.00538 181.80672 181.85335
199.0 0.00503 181.84143 181.88797
199.0 0.00503 181.87628 181.92261
197.0 0.00508 181.91122 181.95738
186.0 0.00538 181.94626 181.99219
188.0 0.00532 181.98135 182.02702
180.0 0.00556 182.01660 182.06195
192.0 0.00521 182.05190 182.09692
187.0 0.00535 182.08733 182.13203
206.0 0.00485 182.12283 182.16716
187.0 0.00535 182.15840 182.20236
200.0 0.00500 182.19412 182.23770
211.0 0.00474 182.22987 182.27307
196.0 0.00510 182.26575 182.30853
204.0 0.00490 182.30176 182.34407
203.0 0.00493 182.33781 182.37973
193.0 0.00518 182.37398 182.41545
186.0 0.00538 182.41025 182.45129
198.0 0.00505 182.44656 182.48720
191.0 0.00524 182.48299 182.52318
198.0 0.00505 182.51955 182.55931
208.0 0.00481 182.55615 182.59547
200.0 0.00500 182.59286 182.63184
181.0 0.00552 182.62965 182.66820
196.0 0.00510 182.66656 182.70473
189.0 0.00529 182.70355 182.74129
185.0 0.00541 182.74063 182.77800
193.0 0.00518 182.77777 182.81479
179.0 0.00559 182.81505 182.85168
169.0 0.00592 182.85239 182.88866
187.0 0.00535 182.88983 182.92578
189.0 0.00529 182.92735 182.96292
190.0 0.00526 182.96497 183.00027
180.0 0.00556 183.00269 183.03770
184.0 0.00543 183.04045 183.07516
184.0 0.00543 183.07832 183.11276
168.0 0.00595 183.11630 183.15045
195.0 0.00513 183.15433 183.18825
191.0 0.00524 183.19249 183.22615
177.0 0.00565 183.23070 183.26413
187.0 0.00535 183.26901 183.30226
176.0 0.00568 183.30743 183.34044
189.0 0.00529 183.34589 183.37872
186.0 0.00538 183.38449 183.41710
183.0 0.00546 183.42313 183.45555
185.0 0.00541 183.46187 183.49416
171.0 0.00585 183.50070 183.53281
196.0 0.00510 183.53961 183.57156
169.0 0.00592 183.57861 183.61046
189.0 0.00529 183.61768 183.64935
184.0 0.00543 183.65685 183.68846
199.0 0.00503 183.69612 183.72755
184.0 0.00543 183.73544 183.76675
181.0 0.00552 183.77487 183.80606
176.0 0.00568 183.81435 183.84546
177.0 0.00565 183.85393 183.88498
184.0 0.00543 183.89362 183.92455
182.0 0.00549 183.93336 183.96423
167.0 0.00599 183.97318 184.00401
166.0 0.00602 184.01309 184.04385
179.0 0.00559 184.05309 184.08380
187.0 0.00535 184.09315 184.12376
183.0 0.00546 184.13332 184.16391
195.0 0.00513 184.17352 184.20416
186.0 0.00538 184.21384 184.32095
185.0 0.00541 184.25423 184.39999
175.0 0.00571 184.29469 184.44150
178.0 0.00562 184.33525 184.48308
186.0 0.00538 184.37585 184.52481
185.0 0.00541 184.41658 184.56664
186.0 0.00538 184.45737 184.60849
187.0 0.00535 184.49823 184.65053
175.0 0.00571 184.53920 184.69264
190.0 0.00526 184.58022 184.73482
196.0 0.00510 184.62131 184.77705
179.0 0.00559 184.66251 184.81953
181.0 0.00552 184.70374 184.86200
179.0 0.00559 184.74504 184.90457
182.0 0.00549 184.78647 184.94730
191.0 0.00524 184.82797 184.99004
182.0 0.00549 184.86949 185.03291
174.0 0.00575 184.91113 185.07590
188.0 0.00532 184.95284 185.11897
184.0 0.00543 184.99463 185.16214
183.0 0.00546 185.03650 185.20543
181.0 0.00552 185.07843 185.24876
187.0 0.00535 185.12041 185.29230
179.0 0.00559 185.16249 185.33585
172.0 0.00581 185.20464 185.37952
192.0 0.00521 185.24687 185.42326
182.0 0.00549 185.28917 185.46713
205.0 0.00488 185.33154 185.51114
182.0 0.00549 185.37396 185.55518
184.0 0.00543 185.41649 185.59929
180.0 0.00556 185.45906 185.64355
173.0 0.00578 185.50172 185.68791
183.0 0.00546 185.54445 185.73236
176.0 0.00568 185.58722 185.77692
184.0 0.00543 185.63008 185.82156
174.0 0.00575 185.67307 185.86635
186.0 0.00538 185.71603 185.91119
190.0 0.00526 185.75912 185.95616
175.0 0.00571 185.80226 186.00121
165.0 0.00606 185.84549 186.04636
180.0 0.00556 185.88876 186.09160
186.0 0.00538 185.93213 186.13701
191.0 0.00524 185.97554 186.18243
173.0 0.00578 186.01903 186.22801
184.0 0.00543 186.06258 186.27367
181.0 0.00552 186.10617 186.31947
180.0 0.00556 186.14987 186.36536
183.0 0.00546 186.19365 186.41133
190.0 0.00526 186.23746 186.45743
166.0 0.00602 186.28134 186.50360
169.0 0.00592 186.32526 186.54984
171.0 0.00585 186.36926 186.59627
160.0 0.00625 186.41339 186.64282
182.0 0.00549 186.45753 186.68939
177.0 0.00565 186.50174 186.73616
178.0 0.00562 186.54604 186.78299
157.0 0.00637 186.59035 186.82991
183.0 0.00546 186.63475 186.87694
173.0 0.00578 186.67920 186.92416
166.0 0.00602 186.72374 186.97144
180.0 0.00556 186.76834 187.01881
173.0 0.00578 186.81296 187.06630
194.0 0.00515 186.85770 187.11395
184.0 0.00543 186.90247 187.16165
189.0 0.00529 186.94730 187.20953
194.0 0.00515 186.99220 187.25748
183.0 0.00546 187.03716 187.30556
180.0 0.00556 187.08215 187.35379
177.0 0.00565 187.12724 187.40208
200.0 0.00500 187.17238 187.45062
179.0 0.00559 187.21758 187.49916
188.0 0.00532 187.26286 187.54788
185.0 0.00541 187.30814 187.59668
174.0 0.00575 187.35352 187.64566
188.0 0.00532 187.39894 187.69478
179.0 0.00559 187.44443 187.74399
197.0 0.00508 187.48997 187.79329
180.0 0.00556 187.53558 187.84282
193.0 0.00518 187.58125 187.89247
182.0 0.00549 187.62695 187.94220
179.0 0.00559 187.67270 187.99211
175.0 0.00571 187.71857 188.04213
183.0 0.00546 187.76442 188.09229
204.0 0.00490 187.81038 188.14268
186.0 0.00538 187.85638 188.19313
173.0 0.00578 187.90242 188.24377
170.0 0.00588 187.94853 188.29457
172.0 0.00581 187.99467 188.34549
188.0 0.00532 188.04088 188.39664
181.0 0.00552 188.08714 188.44789
181.0 0.00552 188.13345 188.49933
172.0 0.00581 188.17984 188.55096
168.0 0.00595 188.22624 188.60275
171.0 0.00585 188.27272 188.65466
194.0 0.00515 188.31923 188.70679
199.0 0.00503 188.36583 188.75908
182.0 0.00549 188.41246 188.81157
181.0 0.00552 188.45914 188.86426
188.0 0.00532 188.50584 188.91707
183.0 0.00546 188.55264 188.97018
173.0 0.00578 188.59946 189.02350
198.0 0.00505 188.64633 189.07689
187.0 0.00535 188.69325 189.13058
186.0 0.00538 188.74022 189.18452
197.0 0.00508 188.78728 189.23865
178.0 0.00562 188.83434 189.30299
184.0 0.00543 188.88145 189.35760
178.0 0.00562 188.92862 189.41740
196.0 0.00510 188.97583 189.47253
197.0 0.00508 189.02309 189.52786
177.0 0.00565 189.07040 189.58350
182.0 0.00549 189.11772 189.63936
186.0 0.00538 189.16516 189.69554
196.0 0.00510 189.21260 189.75194
187.0 0.00535 189.26010 189.80870
207.0 0.00483 189.30763 189.86571
180.0 0.00556 189.35519 189.92303
188.0 0.00532 189.40280 189.98067
183.0 0.00546 189.45050 190.03867
181.0 0.00552 189.49821 190.09695
189.0 0.00529 189.54596 190.15555
184.0 0.00543 189.59378 190.21458
171.0 0.00585 189.64159 190.27390
195.0 0.00513 189.68945 190.33475
188.0 0.00532 189.73741 190.39488
186.0 0.00538 189.78537 190.45546
187.0 0.00535 189.83337 190.51695
196.0 0.00510 189.88144 190.57840
199.0 0.00503 189.92952 190.64026
183.0 0.00546 189.97765 190.70262
178.0 0.00562 190.02583 190.76550
181.0 0.00552 190.07402 190.82883
188.0 0.00532 190.12225 190.89273
182.0 0.00549 190.17058 190.95717
190.0 0.00526 190.21889 191.02222
194.0 0.00515 190.26724 191.08778
182.0 0.00549 190.31564 191.15404
175.0 0.00571 190.36407 191.22090
192.0 0.00521 190.41257 191.28841
203.0 0.00493 190.46109 191.35666
190.0 0.00526 190.50963 191.42564
173.0 0.00578 190.55824 191.49539
194.0 0.00515 190.60683 191.56587
180.0 0.00556 190.65552 191.63730
185.0 0.00541 190.70419 191.70952
169.0 0.00592 190.75291 191.78268
174.0 0.00575 190.80170 191.85684
176.0 0.00568 190.85046 192.87155
196.0 0.00510 190.89928 193.42943
190.0 0.00526 190.94818 193.53508
199.0 0.00503 190.99706 193.64265
192.0 0.00521 191.04601 193.75244
189.0 0.00529 191.09496 193.86449
199.0 0.00503 191.14397 193.97878
180.0 0.00556 191.19301 194.09555
185.0 0.00541 191.24203 194.21483
198.0 0.00505 191.29114 194.33684
186.0 0.00538 191.34026 194.46158
181.0 0.00552 191.38940 194.58932
188.0 0.00532 191.43858 194.72026
201.0 0.00498 191.48782 194.85446
195.0 0.00513 191.53705 194.99229
176.0 0.00568 191.58632 195.13361
196.0 0.00510 191.63559 195.27872
180.0 0.00556 191.68495 195.42805
190.0 0.00526 191.73428 195.58157
205.0 0.00488 191.78371 195.73964
194.0 0.00515 191.83310 195.90254
198.0 0.00505 191.88252 196.07051
195.0 0.00513 191.93198 196.24393
202.0 0.00495 191.98151 196.42308
181.0 0.00552 192.03102 196.60837
223.0 0.00448 192.08057 196.80014
176.0 0.00568 192.13014 196.99876
202.0 0.00495 192.17970 197.20468
209.0 0.00478 192.22934 197.41846
193.0 0.00518 192.27899 197.64055
189.0 0.00529 192.32866 197.87143
183.0 0.00546 192.37837 198.11191
190.0 0.00526 192.42807 198.36243
197.0 0.00508 192.47780 198.62378
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175.0 0.00571 181.43758 182.11182
175.0 0.00571 181.41499 182.07297
187.0 0.00535 181.39238 182.03412
196.0 0.00510 181.36969 181.99466
196.0 0.00510 181.34697 181.95502
179.0 0.00559 181.32414 181.91513
202.0 0.00495 181.30133 181.87515
185.0 0.00541 181.27838 181.83540
194.0 0.00515 181.25543 181.79602
170.0 0.00588 181.23242 181.75717
183.0 0.00546 181.20930 181.71919
175.0 0.00571 181.18617 181.68262
185.0 0.00541 181.16295 181.64766
201.0 0.00498 181.13971 181.61449
196.0 0.00510 181.11638 181.58359
200.0 0.00500 181.09297 181.55492
181.0 0.00552 181.06958 181.52856
179.0 0.00559 181.04607 181.50452
191.0 0.00524 181.02251 181.48355
174.0 0.00575 180.99889 181.46439
197.0 0.00508 180.97523 181.44783
175.0 0.00571 180.95152 181.43381
173.0 0.00578 180.92772 181.42245
183.0 0.00546 180.90390 181.41336
173.0 0.00578 180.88000 181.40666
192.0 0.00521 180.85603 181.40233
187.0 0.00535 180.83202 181.40036
195.0 0.00513 180.80794 181.40021
199.0 0.00503 180.78381 181.40137
191.0 0.00524 180.75966 181.40334
191.0 0.00524 180.73541 181.40579
180.0 0.00556 180.71112 181.40805
189.0 0.00529 180.68677 181.40927
200.0 0.00500 180.66235 181.40895
178.0 0.00562 180.63789 181.40686
177.0 0.00565 180.61337 181.40269
195.0 0.00513 180.58881 181.39583
202.0 0.00495 180.56418 181.38669
171.0 0.00585 180.53951 181.37494
201.0 0.00498 180.51476 181.36046
193.0 0.00518 180.48994 181.34325
203.0 0.00493 180.46510 181.32304
187.0 0.00535 180.44020 181.29976
178.0 0.00562 180.41524 181.27354
198.0 0.00505 180.39021 181.24367
183.0 0.00546 180.36514 181.21013
193.0 0.00518 180.34003 181.17349
190.0 0.00526 180.31487 181.13390
197.0 0.00508 180.28963 181.09148
179.0 0.00559 180.26436 181.04660
190.0 0.00526 180.23898 180.99988
209.0 0.00478 180.21359 180.95187
182.0 0.00549 180.18813 180.90273
183.0 0.00546 180.16263 180.85341
202.0 0.00495 180.13710 180.80341
191.0 0.00524 180.11148 180.75388
172.0 0.00581 180.08585 180.70474
199.0 0.00503 180.06010 180.65630
186.0 0.00538 180.03433 180.60889
193.0 0.00518 180.00850 180.56273
204.0 0.00490 179.98262 180.51796
173.0 0.00578 179.95670 180.47501
189.0 0.00529 179.93071 180.43431
173.0 0.00578 179.90469 180.39546
184.0 0.00543 179.87860 180.35927
196.0 0.00510 179.85246 180.32550
175.0 0.00571 179.82626 180.29425
178.0 0.00562 179.80002 180.26613
179.0 0.00559 179.77376 180.24048
167.0 0.00599 179.74738 180.21776
186.0 0.00538 179.72099 180.19740
186.0 0.00538 179.69455 180.17986
187.0 0.00535 179.66805 180.16454
198.0 0.00505 179.64151 180.15134
170.0 0.00588 179.61490 180.13992
194.0 0.00515 179.58826 180.12994
187.0 0.00535 179.56152 180.12088
194.0 0.00515 179.53477 180.11253
176.0 0.00568 179.50798 180.10410
184.0 0.00543 179.48114 180.09558
197.0 0.00508 179.45422 180.08646
187.0 0.00535 179.42726 180.07588
180.0 0.00556 179.40027 180.06502
193.0 0.00518 179.37321 180.05281
178.0 0.00562 179.34612 180.03957
178.0 0.00562 179.31897 180.02481
188.0 0.00532 179.29175 180.00844
183.0 0.00546 179.26450 179.99059
177.0 0.00565 179.23721 179.97079
184.0 0.00543 179.20985 179.94897
202.0 0.00495 179.18243 179.92525
200.0 0.00500 179.15503 179.89969
194.0 0.00515 179.12750 179.87189
189.0 0.00529 179.09998 179.84216
191.0 0.00524 179.07236 179.81091
193.0 0.00518 179.04472 179.77803
169.0 0.00592 179.01704 179.74391
185.0 0.00541 178.98929 179.70880
189.0 0.00529 178.96155 179.67281
173.0 0.00578 178.93370 179.63666
179.0 0.00559 178.90582 179.60080
181.0 0.00552 178.87788 179.56551
194.0 0.00515 178.84995 179.53186
188.0 0.00532 178.82190 179.49994
181.0 0.00552 178.79382 179.47067
186.0 0.00538 178.76573 179.44449
184.0 0.00543 178.73758 179.42191
192.0 0.00521 178.70937 179.40407
183.0 0.00546 178.68112 179.39087
193.0 0.00518 178.65280 179.38316
179.0 0.00559 178.62448 179.38156
204.0 0.00490 178.59608 179.38631
181.0 0.00552 178.56769 179.39775
176.0 0.00568 178.53917 179.41615
184.0 0.00543 178.51067 179.44121
189.0 0.00529 178.48207 179.47307
187.0 0.00535 178.45348 179.51120
186.0 0.00538 178.42482 179.55511
181.0 0.00552 178.39610 179.60432
211.0 0.00474 178.36736 179.65739
180.0 0.00556 178.33859 179.71332
169.0 0.00592 178.30974 179.77043
180.0 0.00556 178.28087 179.82648
199.0 0.00503 178.25194 179.87947
190.0 0.00526 178.22299 179.92741
194.0 0.00515 178.19398 179.96733
210.0 0.00476 178.16490 179.99762
192.0 0.00521 178.13582 180.01614
205.0 . . .
_pd_meas_number_of_points        3250
_pd_proc_number_of_points        3250

_reflns_number_total             1961
_reflns_limit_h_min              0
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              6
_reflns_limit_l_min              -12
_reflns_limit_l_max              10
_reflns_d_resolution_high        1.343
_reflns_d_resolution_low         15.509
#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
_database_code_depnum_ccdc_archive 'CCDC 1025820'
