# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1955539'
loop_
_audit_author_name
_audit_author_address
'Partha Pratim Das'
;NanoMEGAS SPRL
Belgium
;
_audit_update_record             
;
2020-09-28 deposited with the CCDC.	2020-10-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        Loratadine
_chemical_name_common            Claritin
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H23 Cl N2 O2'
_chemical_formula_weight         382.89

_atom_type_scat_source           
;Doyle & Turner (1968)
;

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   35.4(7)
_cell_length_b                   5.28(11)
_cell_length_c                   22.6(5)
_cell_angle_alpha                90
_cell_angle_beta                 118.2(5)
_cell_angle_gamma                90
_cell_volume                     3717(131)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       nanocrystal
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             627
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.000
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.0335

_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_source                   '120 kV electron microscope'
_diffrn_source_type              'LaB6 gun'
_diffrn_measurement_device       'transmission electron microscope'
_diffrn_measurement_device_type  'Zeiss Libra 120'
_diffrn_detector                 'single-electron detector MEDIPIX'
_diffrn_detector_type            'ASI Timepix'

_diffrn_radiation_monochromator  ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       
'stepwise energy-filtered and precession-assisted 3D electron diffraction'
_diffrn_special_details          
'data were merged from three independent experimental acquisitions'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            3350
_diffrn_reflns_av_unetI/netI     0.1862
_diffrn_reflns_av_R_equivalents  0.2497
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         0.062
_diffrn_reflns_theta_max         0.887
_diffrn_reflns_theta_full        0.887
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.862
_reflns_number_total             1320
_reflns_number_gt                1112
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SIR2014 (Burla et al. 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1320
_refine_ls_number_parameters     85
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.5758
_refine_ls_R_factor_gt           0.5807
_refine_ls_wR_factor_ref         0.8195
_refine_ls_wR_factor_gt          0.8072
_refine_ls_goodness_of_fit_ref   3.488
_refine_ls_restrained_S_all      3.424
_refine_ls_shift/su_max          2.158
_refine_ls_shift/su_mean         0.118

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
Cl1 Cl 0.7001(9) 0.724(5) 0.0074(13) 0.071(13) Uiso 1 1 d D . . . .
C2 C 0.6765(7) 0.664(4) 0.0577(9) 0.006(14) Uiso 1 1 d DG . . . .
C3 C 0.6932(8) 0.477(5) 0.1068(10) 0.30(10) Uiso 1 1 d DG . . . .
H3 H 0.717012 0.384533 0.112645 0.355 Uiso 1 1 calc R U . . .
C4 C 0.6741(8) 0.429(5) 0.1473(10) 0.006(14) Uiso 1 1 d DG . . . .
C5 C 0.6385(7) 0.567(4) 0.1386(9) 0.027(16) Uiso 1 1 d DG . . . .
C6 C 0.6218(7) 0.754(5) 0.0894(13) 0.22(7) Uiso 1 1 d DG . . . .
H6 H 0.597990 0.846443 0.083605 0.267 Uiso 1 1 calc R U . . .
C7 C 0.6409(8) 0.802(5) 0.0490(13) 0.13(4) Uiso 1 1 d DG . . . .
H7 H 0.629718 0.927316 0.016090 0.157 Uiso 1 1 calc R U . . .
C8 C 0.6163(7) 0.521(3) 0.1819(8) -0.001(13) Uiso 1 1 d D . . . .
C9 C 0.6464(6) 0.612(4) 0.2541(9) 2(2) Uiso 1 1 d DG . . . .
N10 N 0.6333(8) 0.821(5) 0.2772(12) 2(3) Uiso 1 1 d DG . . . .
C11 C 0.6590(11) 0.913(6) 0.3418(13) 0.14(4) Uiso 1 1 d G . . . .
H11 H 0.650246 1.052262 0.357340 0.170 Uiso 1 1 calc R U . . .
C12 C 0.6978(9) 0.795(5) 0.3833(10) -0.001(13) Uiso 1 1 d G . . . .
H12 H 0.714998 0.856202 0.426555 -0.001 Uiso 1 1 calc R U . . .
C13 C 0.7109(7) 0.586(5) 0.3602(9) -0.001(13) Uiso 1 1 d DG . . . .
H13 H 0.736846 0.507701 0.387906 -0.001 Uiso 1 1 calc R U . . .
C14 C 0.6852(7) 0.495(4) 0.2955(9) -0.001(13) Uiso 1 1 d DG . . . .
C15 C 0.5807(8) 0.428(5) 0.1629(10) 0.6(3) Uiso 1 1 d D . . . .
C16 C 0.5605(13) 0.388(7) 0.2104(19) 2(2) Uiso 1 1 d D . . . .
H16A H 0.537785 0.510525 0.199716 2.400 Uiso 1 1 calc R U . . .
H16B H 0.582094 0.414014 0.256694 2.400 Uiso 1 1 calc R U . . .
C17 C 0.5421(14) 0.118(8) 0.2021(14) 0.036(18) Uiso 1 1 d D . . . .
H17A H 0.564664 -0.006276 0.212979 0.043 Uiso 1 1 calc R U . . .
H17B H 0.530002 0.092482 0.232323 0.043 Uiso 1 1 calc R U . . .
N18 N 0.5098(13) 0.087(13) 0.1343(15) 0.07(2) Uiso 1 1 d D . . . .
C19 C 0.5235(13) 0.103(7) 0.0854(18) 0.003(13) Uiso 1 1 d D . . . .
H19A H 0.498429 0.102921 0.041386 0.004 Uiso 1 1 calc R U . . .
H19B H 0.539986 -0.047867 0.088407 0.004 Uiso 1 1 calc R U . . .
C20 C 0.5508(10) 0.337(6) 0.0911(11) -0.001(13) Uiso 1 1 d D . . . .
H20A H 0.568026 0.299505 0.069193 -0.001 Uiso 1 1 calc R U . . .
H20B H 0.531700 0.475102 0.066574 -0.001 Uiso 1 1 calc R U . . .
C21 C 0.4714(12) -0.036(7) 0.1206(19) 0.10(3) Uiso 1 1 d D . . . .
O22 O 0.4489(14) -0.125(11) 0.0647(19) 0.054(19) Uiso 1 1 d D . . . .
O23 O 0.458(3) -0.060(18) 0.170(3) 2(3) Uiso 1 1 d D . . . .
C24 C 0.4239(13) -0.238(7) 0.1586(19) -0.001(12) Uiso 1 1 d D . . . .
H24A H 0.397875 -0.140576 0.145226 -0.001 Uiso 1 1 calc R U . . .
H24B H 0.430820 -0.316166 0.201408 -0.001 Uiso 1 1 calc R U . . .
C25 C 0.4132(15) -0.454(8) 0.1065(19) -0.001(13) Uiso 1 1 d D . . . .
H25A H 0.390065 -0.553724 0.104926 -0.002 Uiso 1 1 calc R U . . .
H25B H 0.404817 -0.382051 0.062975 -0.002 Uiso 1 1 calc R U . . .
H25C H 0.437954 -0.558671 0.119487 -0.002 Uiso 1 1 calc R U . . .
C26 C 0.7017(15) 0.262(7) 0.2732(16) 0.06(2) Uiso 1 1 d D . . . .
H26A H 0.690431 0.114420 0.284889 0.076 Uiso 1 1 calc R U . . .
H26B H 0.732547 0.258664 0.301587 0.076 Uiso 1 1 calc R U . . .
C27 C 0.6938(18) 0.220(7) 0.2008(16) 0.14(4) Uiso 1 1 d D . . . .
H27A H 0.675561 0.072533 0.183580 0.171 Uiso 1 1 calc R U . . .
H27B H 0.721203 0.175785 0.203516 0.171 Uiso 1 1 calc R U . . .

_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 C2 1.73(3) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C27 1.54(3) . ?
C5 C6 1.3900 . ?
C5 C8 1.53(2) . ?
C6 C7 1.3900 . ?
C8 C15 1.23(3) . ?
C8 C9 1.54(3) . ?
C9 N10 1.3900 . ?
C9 C14 1.3900 . ?
N10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C26 1.54(3) . ?
C15 C20 1.53(3) . ?
C15 C16 1.56(3) . ?
C16 C17 1.54(3) . ?
C17 N18 1.42(3) . ?
N18 C21 1.40(3) . ?
N18 C19 1.40(3) . ?
C19 C20 1.54(3) . ?
C21 O22 1.22(3) . ?
C21 O23 1.42(3) . ?
O23 C24 1.45(3) . ?
C24 C25 1.55(3) . ?
C26 C27 1.54(4) . ?

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
C3 C2 C7 120.0 . . ?
C3 C2 Cl1 120.0(11) . . ?
C7 C2 Cl1 120.0(10) . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C27 122.2(17) . . ?
C3 C4 C27 117.8(19) . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C8 122.1(15) . . ?
C6 C5 C8 117.9(16) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C2 120.0 . . ?
C15 C8 C9 125.2(10) . . ?
C15 C8 C5 126.2(13) . . ?
C9 C8 C5 108.5(18) . . ?
N10 C9 C14 120.0 . . ?
N10 C9 C8 117.3(13) . . ?
C14 C9 C8 122.7(13) . . ?
C11 N10 C9 120.0 . . ?
C12 C11 N10 120.0 . . ?
C11 C12 C13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 C26 117.2(17) . . ?
C9 C14 C26 122.8(17) . . ?
C8 C15 C20 125.3(16) . . ?
C8 C15 C16 123.0(19) . . ?
C20 C15 C16 112(3) . . ?
C15 C16 C17 110(2) . . ?
N18 C17 C16 108(3) . . ?
C21 N18 C19 120.9(19) . . ?
C21 N18 C17 120(2) . . ?
C19 N18 C17 116(3) . . ?
N18 C19 C20 115(3) . . ?
C15 C20 C19 116(2) . . ?
O22 C21 N18 119.8(19) . . ?
O22 C21 O23 119(2) . . ?
N18 C21 O23 121.5(19) . . ?
C21 O23 C24 118.5(19) . . ?
O23 C24 C25 120(2) . . ?
C14 C26 C27 124(3) . . ?
C26 C27 C4 121(3) . . ?

_refine_diff_density_max         0.657
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.134

_shelx_res_file                  
;
TITL    global
    shelx.res
    created by SHELXL-2018/3 at 13:01:56 on 29-May-2019
CELL    0.0335 35.41     5.28     22.56      90    118.21   90
ZERR     8      0.71     0.11      0.45       0.0    0.5     0.0
LATT 7
SYMM -x,y,1/2-z
SFAC C      0.73070  36.99510   1.19510  11.29660   0.45630   2.81390 =
            0.12470   0.34560   0.00000   0.000   0.000   0.000   0.770  12.011
SFAC N      0.57170  28.84650   1.04250   9.05420   0.46470   2.42130 =
            0.13110   0.31670   0.00000   0.000   0.000   0.000   0.750  14.007
SFAC O      0.45480  23.78030   0.91730   7.62200   0.47190   2.14400 =
            0.13840   0.29590   0.00000   0.000   0.000   0.000   0.730  15.999
SFAC CL     1.45240  30.93520   2.29260   9.97980   0.78740   2.33360 =
            0.32170   0.32280   0.00000   0.000   0.000   0.000   0.990  35.453
SFAC H      0.37540  15.49460   0.14080   4.12610   0.02160   0.02460 =
           -0.10120  46.88400   0.00000   0.000   0.000   0.000   0.320   1.008
UNIT 176 16 16 8 184
L.S.      60
ACTA
BOND
FMAP     -2
PLAN     25
WGHT    0.100000
FVAR       0.17379
CL1   4    0.700109    0.724057    0.007449    11.00000    0.07145
AFIX  66
C2    1    0.676511    0.663941    0.057674    11.00000    0.00584
C3    1    0.693156    0.477116    0.106824    11.00000    0.29553
AFIX  43
H3    5    0.717012    0.384533    0.112645    11.00000   -1.20000
AFIX  65
C4    1    0.674146    0.428664    0.147275    11.00000    0.00604
C5    1    0.638492    0.567038    0.138575    11.00000    0.02709
C6    1    0.621846    0.753864    0.089426    11.00000    0.22241
AFIX  43
H6    5    0.597990    0.846443    0.083605    11.00000   -1.20000
AFIX  65
C7    1    0.640855    0.802317    0.048975    11.00000    0.13114
AFIX  43
H7    5    0.629718    0.927316    0.016090    11.00000   -1.20000
AFIX   0
C8    1    0.616333    0.521219    0.181924    11.00000   -0.00100
AFIX  66
C9    1    0.646387    0.612433    0.254063    11.00000    1.86335
N10   2    0.633298    0.821232    0.277220    11.00000    1.99530
C11   1    0.659004    0.912562    0.341846    11.00000    0.14196
AFIX  43
H11   5    0.650246    1.052262    0.357340    11.00000   -1.20000
AFIX  65
C12   1    0.697799    0.795094    0.383316    11.00000   -0.00100
AFIX  43
H12   5    0.714998    0.856202    0.426555    11.00000   -1.20000
AFIX  65
C13   1    0.710889    0.586295    0.360160    11.00000   -0.00100
AFIX  43
H13   5    0.736846    0.507701    0.387906    11.00000   -1.20000
AFIX  65
C14   1    0.685183    0.494963    0.295534    11.00000   -0.00100
AFIX   0
C15   1    0.580749    0.427965    0.162936    11.00000    0.59636
C16   1    0.560479    0.387785    0.210372    11.00000    2.00000
AFIX  23
H16A  5    0.537785    0.510525    0.199716    11.00000   -1.20000
H16B  5    0.582094    0.414014    0.256694    11.00000   -1.20000
AFIX   0
C17   1    0.542092    0.117509    0.202118    11.00000    0.03563
AFIX  23
H17A  5    0.564664   -0.006276    0.212979    11.00000   -1.20000
H17B  5    0.530002    0.092482    0.232323    11.00000   -1.20000
AFIX   0
N18   2    0.509788    0.086628    0.134320    11.00000    0.06753
C19   1    0.523467    0.102609    0.085445    11.00000    0.00299
AFIX  23
H19A  5    0.498429    0.102921    0.041386    11.00000   -1.20000
H19B  5    0.539986   -0.047867    0.088407    11.00000   -1.20000
AFIX   0
C20   1    0.550806    0.337116    0.091114    11.00000   -0.00100
AFIX  23
H20A  5    0.568026    0.299505    0.069193    11.00000   -1.20000
H20B  5    0.531700    0.475102    0.066574    11.00000   -1.20000
AFIX   0
C21   1    0.471381   -0.036309    0.120615    11.00000    0.10279
O22   3    0.448884   -0.125477    0.064733    11.00000    0.05390
O23   3    0.457799   -0.060291    0.170206    11.00000    2.00000
C24   1    0.423885   -0.237909    0.158564    11.00000   -0.00100
AFIX  23
H24A  5    0.397875   -0.140576    0.145226    11.00000   -1.20000
H24B  5    0.430820   -0.316166    0.201408    11.00000   -1.20000
AFIX   0
C25   1    0.413162   -0.453570    0.106548    11.00000   -0.00100
AFIX  33
H25A  5    0.390065   -0.553724    0.104926    11.00000   -1.50000
H25B  5    0.404817   -0.382051    0.062975    11.00000   -1.50000
H25C  5    0.437954   -0.558671    0.119487    11.00000   -1.50000
AFIX   0
C26   1    0.701729    0.262420    0.273156    11.00000    0.06342
AFIX  23
H26A  5    0.690431    0.114420    0.284889    11.00000   -1.20000
H26B  5    0.732547    0.258664    0.301587    11.00000   -1.20000
AFIX   0
C27   1    0.693843    0.220305    0.200768    11.00000    0.14272
AFIX  23
H27A  5    0.675561    0.072533    0.183580    11.00000   -1.20000
H27B  5    0.721203    0.175785    0.203516    11.00000   -1.20000
FLAT 0.01 Cl1 C2 C3 C4 C5 C6 C7 C8 C27
FLAT 0.01 C8 C9 N10 C11 C12 C13 C14 C26
FLAT 0.01 C5 C8 C9 C15 C16 C20
FLAT 0.01 N18 C21 O22 O23
DFIX 1.75 0.02 Cl1 C2
DFIX 2.91 0.02 C16 C19
DFIX 2.91 0.02 C17 C20
SADI 0.01 C16 C19 C17 C20
DFIX 1.54 0.02 C5 C8
DFIX 1.54 0.02 C9 C8
SADI 0.010 C5 C8 C9 C8
DFIX 1.54 0.02 C4 C27
DFIX 1.54 0.02 C14 C26
DFIX 1.54 0.02 C26 C27
DFIX 1.54 0.02 C15 C16
DFIX 1.54 0.02 C15 C20
DFIX 1.54 0.02 C19 C20
DFIX 1.54 0.02 C16 C17
DFIX 1.43 0.02 C17 N18
DFIX 1.43 0.02 N18 C19
DFIX 1.43 0.02 N18 C21
DFIX 1.23 0.02 C21 O22
DFIX 1.43 0.02 C21 O23
DFIX 1.43 0.02 O23 C24
DFIX 1.54 0.02 C24 C25
DANG 2.70 0.02 Cl1 C3
DANG 2.70 0.02 Cl1 C7
SADI 0.01 Cl1 C3 Cl1 C7
DANG 2.52 0.02 C8 N10
DANG 2.46 0.02 C8 C20
DANG 2.46 0.02 C8 C16
SADI 0.010 C8 C20 C8 C16
DANG 2.27 0.02 N18 O22
DANG 2.44 0.02 N18 O23
DANG 2.27 0.02 O22 O23
DANG 2.47 0.02 C21 C24
DANG 2.60 0.02 O23 C25
DANG 2.50 0.02 C3 C27
DANG 2.50 0.02 C13 C26
SADI 0.01 C3 C27 C13 C26
DANG 2.50 0.02 C6 C8
DANG 2.50 0.02 N10 C8
DANG 2.46 0.02 C5 C15
DANG 2.46 0.02 C15 C9
SADI 0.01 C5 C15 C15 C9
DANG 2.43 0.02 C21 C19
DANG 2.43 0.02 C21 C17
SADI 0.01 C21 C19 C21 C17
AFIX   0
HKLF      4




REM     global
REM wR2 = 0.8195, GooF = S = 3.488, Restrained GooF = 3.424 for all data
REM R1 = 0.5807 for 1112 Fo > 4sig(Fo) and 0.5758 for all 1320 data
REM 85 parameters refined using 59 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  0.657,  deepest hole -0.382,  1-sigma level  0.134
Q1    1   0.5220  0.1233  0.1186  11.00000  0.05    0.66
Q2    1   0.6867  0.6789  0.0309  11.00000  0.05    0.64
Q3    1   0.6270  0.5435  0.1611  11.00000  0.05    0.57
Q4    1   0.5450  0.1257  0.1673  11.00000  0.05    0.44
Q5    1   0.6409  0.5935  0.0887  11.00000  0.05    0.40
Q6    1   0.7026  0.2480  0.2439  11.00000  0.05    0.39
Q7    1   0.4875 -0.3489  0.1252  11.00000  0.05   -0.38
Q8    1   0.5125  0.6830  0.0630  11.00000  0.05   -0.36
Q9    1   0.5231  0.1265  0.0420  11.00000  0.05    0.35
Q10   1   0.6829  0.4534  0.1216  11.00000  0.05    0.35
Q11   1   0.6706  1.0544  0.0722  11.00000  0.05   -0.35
Q12   1   0.4209 -0.4243  0.0851  11.00000  0.05    0.34
Q13   1   0.5065  0.5749  0.0423  11.00000  0.05   -0.34
Q14   1   0.3962 -0.4281  0.1221  11.00000  0.05    0.34
Q15   1   0.6052  0.5560  0.2068  11.00000  0.05    0.33
Q16   1   0.4354 -0.2190  0.1271  11.00000  0.05    0.32
Q17   1   0.6763  1.0058 -0.0225  11.00000  0.05   -0.32
Q18   1   0.6908  0.7852  0.4230  11.00000  0.05    0.32
Q19   1   0.4288 -0.7826  0.0604  11.00000  0.05   -0.31
Q20   1   0.5351  0.7194  0.1729  11.00000  0.05   -0.30
Q21   1   0.4246  0.1677  0.1427  11.00000  0.05   -0.30
Q22   1   0.4558 -0.6468  0.0775  11.00000  0.05   -0.30
Q23   1   0.4568 -0.0819  0.0380  11.00000  0.05    0.29
Q24   1   0.5413  0.7041  0.0915  11.00000  0.05   -0.29
Q25   1   0.7010  1.1733  0.3721  11.00000  0.05   -0.28
;
_shelx_res_checksum              60000

# start Validation Reply Form
_vrf_ATOM007_shelx               
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: All atoms were refined with one isotropic displacement parameter.
;
_vrf_SHFSU01_shelx               
;
PROBLEM: The absolute value of parameter shift to su ratio > 0.20
RESPONSE: The accuracy of the refinement is poor, even for electron 
diffraction standards. The structure was later validate with DFT+D.
;
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: All suitable data were used for the refinemet.
;
_vrf_RINTA01_shelx               
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: High Rint is expected fror electron diffraction.
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.862 Why?  
RESPONSE: All suitable data were used for the refinemet.
;
_vrf_PLAT080_shelx               
;
PROBLEM: Maximum Shift/Error ............................       2.16 Why ? 
RESPONSE: The accuracy of the refinement is poor, even for electron 
diffraction standards. The structure was later validate with DFT+D.
;
_vrf_PLAT082_shelx               
;
PROBLEM: High R1 Value ..................................       0.58 Report
RESPONSE: High agreement parameters are expected fror electron diffraction.
The solution was later validate with DFT+D.
;
_vrf_PLAT084_shelx               
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.82 Report
RESPONSE: High agreement parameters are expected fror electron diffraction.
The solution was later validate with DFT+D.
;
_vrf_PLAT183_shelx               
;
PROBLEM: Missing _cell_measurement_reflns_used Value ....     Please Do !  
RESPONSE: Cell parameters were determined by the software PETS. No output 
information for this parameter was given.
;
_vrf_PLAT184_shelx               
;
PROBLEM: Missing _cell_measurement_theta_min Value ......     Please Do !  
RESPONSE: Cell parameters were determined by the software PETS. No output 
information for this parameter was given.
;
_vrf_PLAT185_shelx               
;
PROBLEM: Missing _cell_measurement_theta_max Value ......     Please Do !  
RESPONSE: Cell parameters were determined by the software PETS. No output 
information for this parameter was given.
;
_vrf_PLAT201_shelx               
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         27 Report
RESPONSE: All atoms were refined with one isotropic displacement parameter.
;
_vrf_PLAT203_shelx               
;
PROBLEM: Negative Isotropic ADP for C8        ...........     -0.001 Report
RESPONSE: Negative thermal factors may result from not fully modeled dynamical
effects.
;
_vrf_PLAT241_shelx               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O23 Check 
RESPONSE: Thermal factors could not be refined properly. The molecule 
connectivity is known a priori.
;
_vrf_PLAT242_shelx               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C2 Check 
RESPONSE: Thermal factors could not be refined properly. The molecule 
connectivity is known a priori.
;
_vrf_PLAT340_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.05143 Ang.  
RESPONSE: The accuracy of the refinement is poor, even for electron 
diffraction standards. The structure was later validate with DFT+D.
;
_vrf_PLAT020_shelx               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.250 Report
RESPONSE: High Rint is expected fror electron diffraction.
;
_vrf_PLAT149_shelx               
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.50 Degree
RESPONSE: The accuracy of the refinement is poor, even for electron 
diffraction standards. The structure was later validate with DFT+D.
;
_vrf_PLAT411_shelx               
;
PROBLEM: Short Inter H...H Contact  H11      ..H24A     .       1.96 Ang.  
RESPONSE: The accuracy of the refinement is poor, even for electron 
diffraction standards. The structure was later validate with DFT+D.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene/TBME'
