# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 2057482'
loop_
_audit_author_name
_audit_author_address
'Peter Knipe'
;Queens University, Belfast
United Kingdom
;
_audit_update_record             
;
2021-01-20 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   8.9540(2)
_cell_length_b                   14.9196(3)
_cell_length_c                   16.0420(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2143.05(8)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C99 H90 Cl1 N9 O9 
# Dc =      1.23 Fooo =    836.00 Mu =      9.10 M =   1585.31
# Found Formula = C80 H100 Cl4 N32 O8 
# Dc =      1.38 FOOO =    936.00 Mu =     18.75 M =   1779.69

_chemical_formula_sum            'C20 H25 Cl N8 O2'
_chemical_formula_moiety         'C20 H25 Cl N8 O2'
_chemical_compound_source        synthesis
_chemical_formula_weight         444.93


_cell_measurement_reflns_used    4064
_cell_measurement_theta_min      6
_cell_measurement_theta_max      71
_cell_measurement_temperature    150

_exptl_crystal_description       needles
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.400

_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    1.875

# Sheldrick geometric approximatio 0.75 0.47 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_T_max  0.47
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_ambient_pressure         100
_diffrn_reflns_number            6522
_diffrn_reflns_av_unetI/netI     0.049
_reflns_number_total             4053
_diffrn_reflns_av_R_equivalents  0.026
# Number of reflections without Friedels Law is 4053 
# Number of reflections with Friedels Law is 2345 
# Theoretical number of reflections is about 2084 


_diffrn_reflns_theta_min         4.046
_diffrn_reflns_theta_max         71.373
_diffrn_measured_fraction_theta_max 0.988

_diffrn_reflns_theta_full        68.518
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              19

_oxford_diffrn_Wilson_B_factor   2.25
_oxford_diffrn_Wilson_scale      0.03

_atom_sites_solution_primary     other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.20
_refine_diff_density_max         0.31


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     4
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4053
_oxford_refine_ls_R_factor_ref   0.0381
_refine_ls_wR_factor_ref         0.0429
_refine_ls_goodness_of_fit_ref   1.8710
_refine_ls_shift/su_max          0.0018002
_refine_ls_shift/su_mean         0.0003283


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4053
_refine_ls_R_factor_all          0.0381
_refine_ls_wR_factor_all         0.0429

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3865
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_gt          0.0423

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661-683 
_oxford_Hooft_y                  -0.001(9) # for 1679 Friedel pairs 
_oxford_Bijvoet_difference       -0.003(10) # for 1679 Friedel pairs 
# (Similar to the Parsons(q).) 
_oxford_refined_Flack_x          0.013(16) # for 1708 Friedel pairs 
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 1679 Friedel Pairs 
;

# choose from: 
# rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 353. 469. 155. 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
O1 O 0.71036(19) 0.38551(12) 0.54740(10) 0.0296 1.0000 Uani . . . . . .
C2 C 0.8399(3) 0.36413(16) 0.54223(14) 0.0211 1.0000 Uani . . . . . .
N3 N 0.9213(2) 0.31178(12) 0.59771(11) 0.0179 1.0000 Uani . . . . . .
C4 C 0.8625(3) 0.26935(16) 0.66799(13) 0.0174 1.0000 Uani . . . . . .
N5 N 0.9612(2) 0.22032(12) 0.71130(12) 0.0214 1.0000 Uani . . . . . .
C6 C 0.9045(3) 0.17811(16) 0.77788(15) 0.0242 1.0000 Uani . . . . . .
N7 N 0.7654(2) 0.17869(13) 0.80567(11) 0.0227 1.0000 Uani . . . . . .
C8 C 0.6694(3) 0.22808(17) 0.76044(14) 0.0196 1.0000 Uani . . . . . .
C9 C 0.7123(3) 0.27693(15) 0.69065(13) 0.0177 1.0000 Uani . . . . . .
N10 N 0.5227(2) 0.22737(13) 0.78866(12) 0.0218 1.0000 Uani . . . . . .
C11 C 0.4805(3) 0.18084(17) 0.86723(14) 0.0210 1.0000 Uani . . . . . .
C12 C 0.5316(3) 0.23254(15) 0.94505(14) 0.0248 1.0000 Uani . . . . . .
C13 C 0.4919(3) 0.17893(17) 1.02316(14) 0.0342 1.0000 Uani . . . . . .
C14 C 0.4724(3) 0.32873(16) 0.94943(17) 0.0418 1.0000 Uani . . . . . .
C15 C 0.3081(3) 0.17240(18) 0.85834(15) 0.0268 1.0000 Uani D . . . . .
N16 N 0.2769(2) 0.21780(19) 0.78125(15) 0.0438 1.0000 Uani D . . . . .
C17 C 0.3985(3) 0.24604(19) 0.73950(17) 0.0342 1.0000 Uani D . . . . .
O18 O 0.4000(2) 0.28088(15) 0.67120(12) 0.0521 1.0000 Uani . . . . . .
C19 C 1.0737(3) 0.29194(15) 0.56680(14) 0.0219 1.0000 Uani . . . . . .
C20 C 1.0931(3) 0.35918(15) 0.49443(13) 0.0199 1.0000 Uani . . . . . .
N21 N 0.9376(2) 0.38823(13) 0.47883(11) 0.0209 1.0000 Uani . . . . . .
C22 C 0.8967(3) 0.43227(16) 0.40584(14) 0.0250 1.0000 Uani . . . . . .
N23 N 1.0094(2) 0.44421(14) 0.35108(11) 0.0291 1.0000 Uani . . . . . .
C24 C 0.9727(4) 0.48746(17) 0.28114(17) 0.0383 1.0000 Uani . . . . . .
N25 N 0.8391(3) 0.51831(15) 0.25851(13) 0.0372 1.0000 Uani . . . . . .
C26 C 0.7342(3) 0.50415(19) 0.31435(16) 0.0350 1.0000 Uani . . . . . .
C27 C 0.7522(3) 0.46176(17) 0.39048(14) 0.0272 1.0000 Uani . . . . . .
C28 C 1.1956(3) 0.43920(16) 0.51385(15) 0.0220 1.0000 Uani . . . . . .
C29 C 1.3596(3) 0.41060(17) 0.50693(17) 0.0307 1.0000 Uani . . . . . .
C30 C 1.1626(3) 0.48163(16) 0.59723(16) 0.0334 1.0000 Uani . . . . . .
Cl1 Cl 0.55567(9) 0.54146(5) 0.28831(5) 0.0471 1.0000 Uani . . . . . .
H61 H 0.9750 0.1428 0.8095 0.0312 1.0000 Uiso R . . . . .
H91 H 0.6425 0.3116 0.6610 0.0234 1.0000 Uiso R . . . . .
H111 H 0.5235 0.1199 0.8691 0.0281 1.0000 Uiso R . . . . .
H121 H 0.6439 0.2378 0.9411 0.0319 1.0000 Uiso R . . . . .
H132 H 0.5305 0.2076 1.0725 0.0523 1.0000 Uiso R . . . . .
H131 H 0.5323 0.1199 1.0213 0.0535 1.0000 Uiso R . . . . .
H133 H 0.3826 0.1770 1.0273 0.0532 1.0000 Uiso R . . . . .
H142 H 0.5132 0.3574 0.9990 0.0622 1.0000 Uiso R . . . . .
H141 H 0.3621 0.3264 0.9521 0.0632 1.0000 Uiso R . . . . .
H143 H 0.5013 0.3601 0.9001 0.0630 1.0000 Uiso R . . . . .
H152 H 0.2582 0.2015 0.9051 0.0331 1.0000 Uiso R . . . . .
H151 H 0.2805 0.1068 0.8533 0.0346 1.0000 Uiso R . . . . .
H192 H 1.1492 0.3013 0.6099 0.0278 1.0000 Uiso R . . . . .
H191 H 1.0793 0.2288 0.5484 0.0286 1.0000 Uiso R . . . . .
H201 H 1.1351 0.3259 0.4454 0.0251 1.0000 Uiso R . . . . .
H241 H 1.0536 0.4975 0.2414 0.0449 1.0000 Uiso R . . . . .
H271 H 0.6722 0.4546 0.4275 0.0358 1.0000 Uiso R . . . . .
H281 H 1.1779 0.4854 0.4698 0.0277 1.0000 Uiso R . . . . .
H293 H 1.4240 0.4593 0.5236 0.0474 1.0000 Uiso R . . . . .
H292 H 1.3768 0.3602 0.5425 0.0482 1.0000 Uiso R . . . . .
H291 H 1.3801 0.3920 0.4495 0.0480 1.0000 Uiso R . . . . .
H303 H 1.2193 0.5368 0.6030 0.0520 1.0000 Uiso R . . . . .
H302 H 1.1944 0.4412 0.6415 0.0515 1.0000 Uiso R . . . . .
H301 H 1.0572 0.4938 0.6033 0.0520 1.0000 Uiso R . . . . .
H161 H 0.1906(19) 0.2249(19) 0.7612(13) 0.053(2) 1.0000 Uiso D . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.53(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 . C2 . 1.205(3) yes
C2 . N3 . 1.391(3) yes
C2 . N21 . 1.389(3) yes
N3 . C4 . 1.396(3) yes
N3 . C19 . 1.482(3) yes
C4 . N5 . 1.341(3) yes
C4 . C9 . 1.397(3) yes
N5 . C6 . 1.340(3) yes
C6 . N7 . 1.323(3) yes
C6 . H61 . 0.967 no
N7 . C8 . 1.345(3) yes
C8 . C9 . 1.390(3) yes
C8 . N10 . 1.389(3) yes
C9 . H91 . 0.941 no
N10 . C11 . 1.488(3) yes
N10 . C17 . 1.392(3) yes
C11 . C12 . 1.537(3) yes
C11 . C15 . 1.555(3) yes
C11 . H111 . 0.987 no
C12 . C13 . 1.529(3) yes
C12 . C14 . 1.532(3) yes
C12 . H121 . 1.010 no
C13 . H132 . 0.964 no
C13 . H131 . 0.953 no
C13 . H133 . 0.981 no
C14 . H142 . 0.974 no
C14 . H141 . 0.989 no
C14 . H143 . 0.955 no
C15 . N16 . 1.438(3) yes
C15 . H152 . 0.976 no
C15 . H151 . 1.013 no
N16 . C17 . 1.346(3) yes
N16 . H161 . 0.843(16) no
C17 . O18 . 1.213(3) yes
C19 . C20 . 1.544(3) yes
C19 . H192 . 0.977 no
C19 . H191 . 0.988 no
C20 . N21 . 1.480(3) yes
C20 . C28 . 1.538(3) yes
C20 . H201 . 1.003 no
N21 . C22 . 1.392(3) yes
C22 . N23 . 1.349(3) yes
C22 . C27 . 1.389(4) yes
N23 . C24 . 1.335(3) yes
C24 . N25 . 1.332(4) yes
C24 . H241 . 0.977 no
N25 . C26 . 1.315(3) yes
C26 . C27 . 1.385(3) yes
C26 . Cl1 . 1.743(3) yes
C27 . H271 . 0.937 no
C28 . C29 . 1.533(3) yes
C28 . C30 . 1.509(3) yes
C28 . H281 . 1.000 no
C29 . H293 . 0.966 no
C29 . H292 . 0.956 no
C29 . H291 . 0.979 no
C30 . H303 . 0.972 no
C30 . H302 . 0.975 no
C30 . H301 . 0.966 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 . C2 . N3 . 127.5(2) yes
O1 . C2 . N21 . 126.0(2) yes
N3 . C2 . N21 . 106.47(19) yes
C2 . N3 . C4 . 124.97(19) yes
C2 . N3 . C19 . 112.40(18) yes
C4 . N3 . C19 . 121.83(19) yes
N3 . C4 . N5 . 114.6(2) yes
N3 . C4 . C9 . 122.5(2) yes
N5 . C4 . C9 . 122.9(2) yes
C4 . N5 . C6 . 114.8(2) yes
N5 . C6 . N7 . 128.5(2) yes
N5 . C6 . H61 . 115.3 no
N7 . C6 . H61 . 116.2 no
C6 . N7 . C8 . 115.1(2) yes
N7 . C8 . C9 . 123.0(2) yes
N7 . C8 . N10 . 115.1(2) yes
C9 . C8 . N10 . 121.9(2) yes
C4 . C9 . C8 . 115.7(2) yes
C4 . C9 . H91 . 123.5 no
C8 . C9 . H91 . 120.8 no
C8 . N10 . C11 . 121.32(19) yes
C8 . N10 . C17 . 124.7(2) yes
C11 . N10 . C17 . 111.72(18) yes
N10 . C11 . C12 . 112.22(19) yes
N10 . C11 . C15 . 102.26(19) yes
C12 . C11 . C15 . 114.2(2) yes
N10 . C11 . H111 . 110.8 no
C12 . C11 . H111 . 108.8 no
C15 . C11 . H111 . 108.4 no
C11 . C12 . C13 . 109.50(19) yes
C11 . C12 . C14 . 113.8(2) yes
C13 . C12 . C14 . 111.8(2) yes
C11 . C12 . H121 . 106.5 no
C13 . C12 . H121 . 108.9 no
C14 . C12 . H121 . 106.0 no
C12 . C13 . H132 . 111.0 no
C12 . C13 . H131 . 111.7 no
H132 . C13 . H131 . 107.4 no
C12 . C13 . H133 . 107.6 no
H132 . C13 . H133 . 108.4 no
H131 . C13 . H133 . 110.8 no
C12 . C14 . H142 . 108.6 no
C12 . C14 . H141 . 108.3 no
H142 . C14 . H141 . 110.8 no
C12 . C14 . H143 . 109.1 no
H142 . C14 . H143 . 111.0 no
H141 . C14 . H143 . 108.9 no
C11 . C15 . N16 . 103.53(19) yes
C11 . C15 . H152 . 110.4 no
N16 . C15 . H152 . 111.3 no
C11 . C15 . H151 . 109.1 no
N16 . C15 . H151 . 109.8 no
H152 . C15 . H151 . 112.3 no
C15 . N16 . C17 . 114.7(2) yes
C15 . N16 . H161 . 124.4(12) no
C17 . N16 . H161 . 120.8(12) no
N10 . C17 . N16 . 107.6(2) yes
N10 . C17 . O18 . 126.1(2) yes
N16 . C17 . O18 . 126.4(3) yes
N3 . C19 . C20 . 103.02(18) yes
N3 . C19 . H192 . 111.8 no
C20 . C19 . H192 . 111.2 no
N3 . C19 . H191 . 109.7 no
C20 . C19 . H191 . 112.9 no
H192 . C19 . H191 . 108.2 no
C19 . C20 . N21 . 102.23(18) yes
C19 . C20 . C28 . 114.78(19) yes
N21 . C20 . C28 . 111.63(19) yes
C19 . C20 . H201 . 108.1 no
N21 . C20 . H201 . 111.4 no
C28 . C20 . H201 . 108.6 no
C20 . N21 . C2 . 113.15(18) yes
C20 . N21 . C22 . 121.9(2) yes
C2 . N21 . C22 . 124.9(2) yes
N21 . C22 . N23 . 114.4(2) yes
N21 . C22 . C27 . 122.9(2) yes
N23 . C22 . C27 . 122.6(2) yes
C22 . N23 . C24 . 115.3(2) yes
N23 . C24 . N25 . 128.1(3) yes
N23 . C24 . H241 . 116.1 no
N25 . C24 . H241 . 115.8 no
C24 . N25 . C26 . 113.6(2) yes
N25 . C26 . C27 . 126.2(3) yes
N25 . C26 . Cl1 . 116.1(2) yes
C27 . C26 . Cl1 . 117.7(2) yes
C22 . C27 . C26 . 114.2(3) yes
C22 . C27 . H271 . 124.3 no
C26 . C27 . H271 . 121.5 no
C20 . C28 . C29 . 109.9(2) yes
C20 . C28 . C30 . 112.8(2) yes
C29 . C28 . C30 . 111.6(2) yes
C20 . C28 . H281 . 107.3 no
C29 . C28 . H281 . 107.0 no
C30 . C28 . H281 . 107.9 no
C28 . C29 . H293 . 110.0 no
C28 . C29 . H292 . 109.2 no
H293 . C29 . H292 . 109.4 no
C28 . C29 . H291 . 109.1 no
H293 . C29 . H291 . 111.2 no
H292 . C29 . H291 . 107.9 no
C28 . C30 . H303 . 109.7 no
C28 . C30 . H302 . 109.2 no
H303 . C30 . H302 . 107.6 no
C28 . C30 . H301 . 111.0 no
H303 . C30 . H301 . 110.0 no
H302 . C30 . H301 . 109.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C9 . H91 . O1 . 120 0.94 2.22 2.812(3) yes
C19 . H192 . O18 1_655 153 0.98 2.47 3.371(3) yes
C19 . H191 . O1 3_556 146 0.99 2.58 3.444(3) yes
C29 . H292 . O18 1_655 157 0.96 2.39 3.289(3) yes
C30 . H303 . N7 4_756 141 0.97 2.58 3.389(3) yes
N16 . H161 . N5 1_455 171(3) 0.843 2.206 3.042(3) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
_chemical_name_systematic        'Dimer 2d'
####################################################################### 
# 
# 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_I_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2057484'
loop_
_audit_author_name
_audit_author_address
'Peter Knipe'
;Queens University, Belfast
United Kingdom
;
_audit_update_record             
;
2021-01-20 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   12.05260(10)
_cell_length_b                   12.05260(10)
_cell_length_c                   37.0309(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5379.30(12)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2 '
_symmetry_space_group_name_Hall  'P 4abw 2nw'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y+1/2,x+1/2,z+1/4
-x,-y,z+1/2
y+1/2,-x+1/2,z+3/4
-x+1/2,y+1/2,-z+1/4
y,x,-z
x+1/2,-y+1/2,-z+3/4
-y,-x,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C1 H1 Cl1 N1 O1 
# Dc =      0.02 Fooo =     39.00 Mu =      1.27 M =     78.48
# Found Formula = C200 H272 Cl8 N64 O16 
# Dc =      1.27 FOOO =   2184.00 Mu =     15.62 M =   4112.40

_chemical_formula_sum            'C25 H34 Cl N8 O2'
_chemical_formula_moiety         'C25 H34 Cl N8 O2'
_chemical_compound_source        synthesis
_chemical_formula_weight         514.05


_cell_measurement_reflns_used    14408
_cell_measurement_theta_min      5
_cell_measurement_theta_max      71
_cell_measurement_temperature    100

_exptl_crystal_description       blocks
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_max          0.600

_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    1.562

# Sheldrick geometric approximatio 0.46 0.39 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_T_max  0.39
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_ambient_pressure         100
_diffrn_reflns_number            22811
_reflns_number_total             5157
_diffrn_reflns_av_R_equivalents  0.031
# Number of reflections without Friedels Law is 5157 
# Number of reflections with Friedels Law is 3056 
# Theoretical number of reflections is about 2611 


_diffrn_reflns_theta_min         3.857
_diffrn_reflns_theta_max         71.274
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        69.848
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       35
_reflns_limit_h_min              -9
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              45

_oxford_diffrn_Wilson_B_factor   2.89
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.22
_refine_diff_density_max         0.34


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     0
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5135
_oxford_refine_ls_R_factor_ref   0.0442
_refine_ls_wR_factor_ref         0.0581
_refine_ls_goodness_of_fit_ref   1.1707
_refine_ls_shift/su_max          0.0006647
_refine_ls_shift/su_mean         0.0000512


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        5135
_refine_ls_R_factor_all          0.0442
_refine_ls_wR_factor_all         0.0581

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4956
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_gt          0.0576

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661--683 
_oxford_Hooft_y                  0.026(4) # for 2064 Friedel pairs 
_oxford_Bijvoet_difference       0.032(5) # for 2064 Friedel pairs 
# (Similar to the Parsons(q).) 
_oxford_refined_Flack_x          0.02(2) # for 2101 Friedel pairs 
_refine_ls_abs_structure_Flack   0.032(5)
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 2064 Friedel Pairs 
;

# choose from: 
# rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 484. 595. 249. 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cl1 Cl 0.24558(6) 0.23991(6) 0.43355(2) 0.0511 1.0000 Uani . . . . . .
C2 C 0.3578(2) 0.2231(2) 0.46258(7) 0.0310 1.0000 Uani . . . . . .
N3 N 0.35753(19) 0.12945(19) 0.48158(6) 0.0404 1.0000 Uani . . . . . .
C4 C 0.4460(2) 0.1189(2) 0.50282(8) 0.0443 1.0000 Uani . . . . . .
N5 N 0.53130(18) 0.18787(17) 0.50672(6) 0.0339 1.0000 Uani . . . . . .
C6 C 0.52675(19) 0.28068(19) 0.48685(6) 0.0253 1.0000 Uani . . . . . .
C7 C 0.4381(2) 0.3029(2) 0.46336(7) 0.0299 1.0000 Uani . . . . . .
N8 N 0.61681(16) 0.35073(15) 0.49126(5) 0.0247 1.0000 Uani . . . . . .
C9 C 0.71634(18) 0.31837(17) 0.51216(6) 0.0209 1.0000 Uani . . . . . .
C10 C 0.7738(2) 0.43051(18) 0.51736(6) 0.0225 1.0000 Uani . . . . . .
N11 N 0.72603(16) 0.49824(15) 0.48853(5) 0.0214 1.0000 Uani . . . . . .
C12 C 0.6273(2) 0.4557(2) 0.47629(6) 0.0262 1.0000 Uani . . . . . .
O13 O 0.56082(14) 0.50040(14) 0.45620(5) 0.0371 1.0000 Uani . . . . . .
C14 C 0.77592(19) 0.59730(18) 0.47714(6) 0.0203 1.0000 Uani . . . . . .
N15 N 0.87347(15) 0.61728(15) 0.49348(5) 0.0234 1.0000 Uani . . . . . .
C16 C 0.9221(2) 0.7111(2) 0.48309(6) 0.0296 1.0000 Uani . . . . . .
N17 N 0.88555(16) 0.78693(16) 0.45975(5) 0.0265 1.0000 Uani . . . . . .
C18 C 0.78702(18) 0.76463(18) 0.44463(6) 0.0213 1.0000 Uani . . . . . .
C19 C 0.72838(19) 0.66733(17) 0.45178(6) 0.0201 1.0000 Uani . . . . . .
N20 N 0.74688(16) 0.84722(14) 0.42247(5) 0.0210 1.0000 Uani . . . . . .
C21 C 0.6411(2) 0.8501(2) 0.40635(6) 0.0233 1.0000 Uani . . . . . .
O22 O 0.57984(13) 0.77021(13) 0.40287(4) 0.0269 1.0000 Uani . . . . . .
N23 N 0.62214(17) 0.95549(17) 0.39561(5) 0.0265 1.0000 Uani . . . . . .
C24 C 0.5176(2) 0.9907(2) 0.37797(7) 0.0273 1.0000 Uani . . . . . .
C25 C 0.5071(3) 0.9318(3) 0.34179(7) 0.0506 1.0000 Uani . . . . . .
C26 C 0.4174(3) 0.9604(3) 0.40161(8) 0.0587 1.0000 Uani . . . . . .
C27 C 0.5188(3) 1.1162(2) 0.37256(9) 0.0530 1.0000 Uani . . . . . .
C28 C 0.7101(2) 1.03074(19) 0.40681(6) 0.0258 1.0000 Uani . . . . . .
C29 C 0.8059(2) 0.95268(19) 0.41734(6) 0.0226 1.0000 Uani . . . . . .
C30 C 0.8982(2) 0.9414(2) 0.38879(6) 0.0261 1.0000 Uani . . . . . .
C31 C 0.8538(2) 0.9106(2) 0.35107(6) 0.0334 1.0000 Uani . . . . . .
C32 C 0.9668(2) 1.0484(2) 0.38679(7) 0.0349 1.0000 Uani . . . . . .
C33 C 0.78731(19) 0.23221(19) 0.49190(6) 0.0276 1.0000 Uani . . . . . .
C34 C 0.8299(3) 0.2750(2) 0.45569(7) 0.0496 1.0000 Uani . . . . . .
C35 C 0.8828(2) 0.1933(2) 0.51730(8) 0.0397 1.0000 Uani . . . . . .
C1 C 0.9609(4) 0.1075(4) 0.50437(14) 0.0342 0.5000 Uani . . . . . .
C36 C 0.8577(5) 0.1628(4) 0.55222(17) 0.0490 0.5000 Uani . . . . . .
H41 H 0.4507 0.0523 0.5165 0.0530 1.0000 Uiso R . . . . .
H71 H 0.4359 0.3664 0.4496 0.0350 1.0000 Uiso R . . . . .
H91 H 0.6896 0.2880 0.5348 0.0245 1.0000 Uiso R . . . . .
H102 H 0.7590 0.4657 0.5411 0.0250 1.0000 Uiso R . . . . .
H101 H 0.8559 0.4278 0.5136 0.0251 1.0000 Uiso R . . . . .
H161 H 0.9939 0.7289 0.4938 0.0348 1.0000 Uiso R . . . . .
H191 H 0.6583 0.6508 0.4413 0.0237 1.0000 Uiso R . . . . .
H252 H 0.4447 0.9572 0.3285 0.0754 1.0000 Uiso R . . . . .
H251 H 0.5719 0.9410 0.3273 0.0764 1.0000 Uiso R . . . . .
H253 H 0.4968 0.8517 0.3454 0.0757 1.0000 Uiso R . . . . .
H263 H 0.3511 0.9831 0.3891 0.0920 1.0000 Uiso R . . . . .
H261 H 0.4241 0.9952 0.4251 0.0929 1.0000 Uiso R . . . . .
H262 H 0.4144 0.8791 0.4034 0.0919 1.0000 Uiso R . . . . .
H271 H 0.4479 1.1416 0.3618 0.0779 1.0000 Uiso R . . . . .
H273 H 0.5304 1.1585 0.3953 0.0776 1.0000 Uiso R . . . . .
H272 H 0.5773 1.1350 0.3549 0.0766 1.0000 Uiso R . . . . .
H282 H 0.6857 1.0734 0.4280 0.0306 1.0000 Uiso R . . . . .
H281 H 0.7344 1.0786 0.3870 0.0298 1.0000 Uiso R . . . . .
H291 H 0.8358 0.9736 0.4407 0.0259 1.0000 Uiso R . . . . .
H301 H 0.9446 0.8776 0.3972 0.0299 1.0000 Uiso R . . . . .
H312 H 0.9149 0.8973 0.3349 0.0501 1.0000 Uiso R . . . . .
H313 H 0.8024 0.9699 0.3422 0.0493 1.0000 Uiso R . . . . .
H311 H 0.8094 0.8444 0.3538 0.0497 1.0000 Uiso R . . . . .
H323 H 1.0278 1.0374 0.3716 0.0510 1.0000 Uiso R . . . . .
H321 H 0.9959 1.0684 0.4110 0.0506 1.0000 Uiso R . . . . .
H322 H 0.9184 1.1102 0.3782 0.0510 1.0000 Uiso R . . . . .
H331 H 0.7379 0.1666 0.4874 0.0314 1.0000 Uiso R . . . . .
H341 H 0.8731 0.2194 0.4428 0.0745 1.0000 Uiso R . . . . .
H343 H 0.8725 0.3424 0.4593 0.0739 1.0000 Uiso R . . . . .
H342 H 0.7676 0.2968 0.4405 0.0729 1.0000 Uiso R . . . . .
H12 H 1.0157 0.0813 0.5211 0.0624 0.5000 Uiso R . . . . .
H11 H 0.9495 0.0790 0.4799 0.0634 0.5000 Uiso R . . . . .
H14 H 0.9357 0.0320 0.5048 0.0623 0.5000 Uiso R . . . . .
H361 H 0.9279 0.1407 0.5622 0.0834 0.5000 Uiso R . . . . .
H362 H 0.8271 0.2256 0.5643 0.0832 0.5000 Uiso R . . . . .
H363 H 0.8057 0.1025 0.5502 0.0835 0.5000 Uiso R . . . . .
H13 H 1.0203 0.1439 0.4898 0.0653 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.320(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 . C2 . 1.740(2) yes
C2 . N3 . 1.330(3) yes
C2 . C7 . 1.365(3) yes
N3 . C4 . 1.331(3) yes
C4 . N5 . 1.330(3) yes
C4 . H41 . 0.951 no
N5 . C6 . 1.340(3) yes
C6 . C7 . 1.403(3) yes
C6 . N8 . 1.385(3) yes
C7 . H71 . 0.920 no
N8 . C9 . 1.480(3) yes
N8 . C12 . 1.387(3) yes
C9 . C10 . 1.531(3) yes
C9 . C33 . 1.540(3) yes
C9 . H91 . 0.972 no
C10 . N11 . 1.462(3) yes
C10 . H102 . 0.993 no
C10 . H101 . 0.999 no
N11 . C12 . 1.373(3) yes
N11 . C14 . 1.402(3) yes
C12 . O13 . 1.219(3) yes
C14 . N15 . 1.344(3) yes
C14 . C19 . 1.386(3) yes
N15 . C16 . 1.331(3) yes
C16 . N17 . 1.333(3) yes
C16 . H161 . 0.976 no
N17 . C18 . 1.340(3) yes
C18 . C19 . 1.395(3) yes
C18 . N20 . 1.378(3) yes
C19 . H191 . 0.951 no
N20 . C21 . 1.408(3) yes
N20 . C29 . 1.469(3) yes
C21 . O22 . 1.220(3) yes
C21 . N23 . 1.351(3) yes
N23 . C24 . 1.482(3) yes
N23 . C28 . 1.456(3) yes
C24 . C25 . 1.522(4) yes
C24 . C26 . 1.535(3) yes
C24 . C27 . 1.526(3) yes
C25 . H252 . 0.950 no
C25 . H251 . 0.954 no
C25 . H253 . 0.984 no
C26 . H263 . 0.963 no
C26 . H261 . 0.969 no
C26 . H262 . 0.983 no
C27 . H271 . 0.993 no
C27 . H273 . 0.993 no
C27 . H272 . 0.987 no
C28 . C29 . 1.539(3) yes
C28 . H282 . 0.984 no
C28 . H281 . 0.978 no
C29 . C30 . 1.541(3) yes
C29 . H291 . 0.971 no
C30 . C31 . 1.541(3) yes
C30 . C32 . 1.534(3) yes
C30 . H301 . 1.000 no
C31 . H312 . 0.961 no
C31 . H313 . 1.001 no
C31 . H311 . 0.965 no
C32 . H323 . 0.935 no
C32 . H321 . 0.994 no
C32 . H322 . 0.999 no
C33 . C34 . 1.526(3) yes
C33 . C35 . 1.559(3) yes
C33 . H331 . 1.004 no
C34 . H341 . 0.974 no
C34 . H343 . 0.970 no
C34 . H342 . 0.975 no
C35 . C1 . 1.477(5) yes
C35 . C36 . 1.379(6) yes
C1 . H12 . 0.960 no
C1 . H11 . 0.978 no
C1 . H14 . 0.960 no
C1 . H13 . 0.998 no
C36 . H361 . 0.961 no
C36 . H362 . 0.953 no
C36 . H363 . 0.962 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . C2 . N3 . 115.07(19) yes
Cl1 . C2 . C7 . 118.9(2) yes
N3 . C2 . C7 . 126.0(2) yes
C2 . N3 . C4 . 113.0(2) yes
N3 . C4 . N5 . 128.6(3) yes
N3 . C4 . H41 . 116.3 no
N5 . C4 . H41 . 115.1 no
C4 . N5 . C6 . 115.5(2) yes
N5 . C6 . C7 . 122.1(2) yes
N5 . C6 . N8 . 114.3(2) yes
C7 . C6 . N8 . 123.6(2) yes
C6 . C7 . C2 . 114.8(2) yes
C6 . C7 . H71 . 121.6 no
C2 . C7 . H71 . 123.7 no
C6 . N8 . C9 . 122.45(18) yes
C6 . N8 . C12 . 125.5(2) yes
C9 . N8 . C12 . 112.05(18) yes
N8 . C9 . C10 . 101.54(17) yes
N8 . C9 . C33 . 111.92(17) yes
C10 . C9 . C33 . 113.90(19) yes
N8 . C9 . H91 . 106.4 no
C10 . C9 . H91 . 112.0 no
C33 . C9 . H91 . 110.6 no
C9 . C10 . N11 . 102.85(17) yes
C9 . C10 . H102 . 114.0 no
N11 . C10 . H102 . 109.7 no
C9 . C10 . H101 . 113.7 no
N11 . C10 . H101 . 107.8 no
H102 . C10 . H101 . 108.5 no
C10 . N11 . C12 . 111.99(18) yes
C10 . N11 . C14 . 121.74(18) yes
C12 . N11 . C14 . 126.18(18) yes
N8 . C12 . N11 . 106.71(19) yes
N8 . C12 . O13 . 125.9(2) yes
N11 . C12 . O13 . 127.4(2) yes
N11 . C14 . N15 . 113.09(18) yes
N11 . C14 . C19 . 123.0(2) yes
N15 . C14 . C19 . 123.9(2) yes
C14 . N15 . C16 . 114.02(19) yes
N15 . C16 . N17 . 128.7(2) yes
N15 . C16 . H161 . 117.4 no
N17 . C16 . H161 . 113.9 no
C16 . N17 . C18 . 115.2(2) yes
N17 . C18 . C19 . 122.6(2) yes
N17 . C18 . N20 . 114.53(19) yes
C19 . C18 . N20 . 122.86(19) yes
C18 . C19 . C14 . 115.5(2) yes
C18 . C19 . H191 . 123.3 no
C14 . C19 . H191 . 121.1 no
C18 . N20 . C21 . 126.02(18) yes
C18 . N20 . C29 . 122.15(18) yes
C21 . N20 . C29 . 111.25(18) yes
N20 . C21 . O22 . 125.0(2) yes
N20 . C21 . N23 . 107.5(2) yes
O22 . C21 . N23 . 127.5(2) yes
C21 . N23 . C24 . 122.9(2) yes
C21 . N23 . C28 . 112.3(2) yes
C24 . N23 . C28 . 124.5(2) yes
N23 . C24 . C25 . 109.0(2) yes
N23 . C24 . C26 . 110.4(2) yes
C25 . C24 . C26 . 109.0(2) yes
N23 . C24 . C27 . 109.5(2) yes
C25 . C24 . C27 . 110.3(2) yes
C26 . C24 . C27 . 108.6(2) yes
C24 . C25 . H252 . 111.9 no
C24 . C25 . H251 . 111.9 no
H252 . C25 . H251 . 108.6 no
C24 . C25 . H253 . 110.4 no
H252 . C25 . H253 . 106.7 no
H251 . C25 . H253 . 107.1 no
C24 . C26 . H263 . 108.1 no
C24 . C26 . H261 . 110.1 no
H263 . C26 . H261 . 112.1 no
C24 . C26 . H262 . 107.8 no
H263 . C26 . H262 . 106.6 no
H261 . C26 . H262 . 111.9 no
C24 . C27 . H271 . 110.5 no
C24 . C27 . H273 . 113.5 no
H271 . C27 . H273 . 107.7 no
C24 . C27 . H272 . 108.8 no
H271 . C27 . H272 . 106.1 no
H273 . C27 . H272 . 110.0 no
N23 . C28 . C29 . 103.75(19) yes
N23 . C28 . H282 . 109.6 no
C29 . C28 . H282 . 109.9 no
N23 . C28 . H281 . 111.8 no
C29 . C28 . H281 . 109.1 no
H282 . C28 . H281 . 112.3 no
C28 . C29 . N20 . 101.46(18) yes
C28 . C29 . C30 . 114.9(2) yes
N20 . C29 . C30 . 111.22(19) yes
C28 . C29 . H291 . 110.2 no
N20 . C29 . H291 . 106.8 no
C30 . C29 . H291 . 111.6 no
C29 . C30 . C31 . 113.1(2) yes
C29 . C30 . C32 . 110.4(2) yes
C31 . C30 . C32 . 110.2(2) yes
C29 . C30 . H301 . 105.0 no
C31 . C30 . H301 . 106.8 no
C32 . C30 . H301 . 111.1 no
C30 . C31 . H312 . 109.7 no
C30 . C31 . H313 . 109.8 no
H312 . C31 . H313 . 112.9 no
C30 . C31 . H311 . 107.2 no
H312 . C31 . H311 . 110.7 no
H313 . C31 . H311 . 106.4 no
C30 . C32 . H323 . 109.5 no
C30 . C32 . H321 . 110.6 no
H323 . C32 . H321 . 107.5 no
C30 . C32 . H322 . 109.1 no
H323 . C32 . H322 . 111.9 no
H321 . C32 . H322 . 108.3 no
C9 . C33 . C34 . 112.78(19) yes
C9 . C33 . C35 . 108.60(18) yes
C34 . C33 . C35 . 112.5(2) yes
C9 . C33 . H331 . 106.4 no
C34 . C33 . H331 . 108.6 no
C35 . C33 . H331 . 107.6 no
C33 . C34 . H341 . 112.3 no
C33 . C34 . H343 . 109.9 no
H341 . C34 . H343 . 111.1 no
C33 . C34 . H342 . 109.9 no
H341 . C34 . H342 . 108.3 no
H343 . C34 . H342 . 105.1 no
C33 . C35 . C1 . 119.0(3) yes
C33 . C35 . C36 . 118.9(3) yes
C1 . C35 . C36 . 104.9(4) yes
C35 . C1 . H12 . 117.3 no
C35 . C1 . H11 . 117.2 no
H12 . C1 . H11 . 125.3 no
C35 . C1 . H14 . 117.2 no
H12 . C1 . H14 . 84.0 no
H11 . C1 . H14 . 68.8 no
C35 . C1 . H13 . 108.9 no
H12 . C1 . H13 . 89.9 no
H11 . C1 . H13 . 75.8 no
H14 . C1 . H13 . 130.8 no
C35 . C36 . H361 . 103.9 no
C35 . C36 . H362 . 108.3 no
H361 . C36 . H362 . 112.4 no
C35 . C36 . H363 . 105.8 no
H361 . C36 . H363 . 113.2 no
H362 . C36 . H363 . 112.6 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C7 . H71 . O13 . 122 0.92 2.22 2.815(4) yes
C10 . H102 . O22 6_556 164 0.99 2.49 3.460(4) yes
C19 . H191 . O13 . 122 0.95 2.23 2.855(4) yes
C19 . H191 . O22 . 120 0.95 2.23 2.833(4) yes
C26 . H262 . O22 . 121 0.98 2.39 3.015(4) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
_chemical_name_systematic        'N-tBu Dimer 1a'
####################################################################### 
# 
# 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_I_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2057483'
loop_
_audit_author_name
_audit_author_address
'Peter Knipe'
;Queens University, Belfast
United Kingdom
;
_audit_update_record             
;
2021-01-20 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
#--------------------------------------------------------------- 
# _oxford_ data items, April 2010: 
# There is some uncertainty about the correct way of forming local data 
# names, e.g. 

# _atom_site_special_shape_oxford 
# or 
# _oxford_atom_site_special_shape 

# see: 
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace 

# A reserved prefix, e.g. foo, must be used in the following way 
# " If the data file contains items defined in a DDL1 dictionary, the 
# local data names assigned under the reserved prefix must contain it as 
# their first component, e.g. _foo_atom_site_my_item. " 

# However, this seems to say the opposite: 
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html 

# According to advice from the IUCr, CRYSTALS is correct 
#--------------------------------------------------------------- 
# End of 'script/refcif.dat' 
#end of refcif 
_cell_length_a                   9.69330(10)
_cell_length_b                   9.01790(10)
_cell_length_c                   13.41980(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.0868(8)
_cell_angle_gamma                90
_cell_volume                     1173.07(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21 '
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C1 H1 Cl1 N1 O1 
# Dc =      0.11 Fooo =     39.00 Mu =      5.80 M =     78.48
# Found Formula = C42 H54 Cl2 N16 O4 
# Dc =      1.30 FOOO =    484.00 Mu =     17.28 M =    917.90

_chemical_formula_sum            'C21 H27 Cl N8 O2'
_chemical_formula_moiety         'C21 H27 Cl N8 O2'
_chemical_compound_source        synthesis
_chemical_formula_weight         458.9497


_cell_measurement_reflns_used    9280
_cell_measurement_theta_min      6
_cell_measurement_theta_max      71
_cell_measurement_temperature    100

_exptl_crystal_description       needle
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_size_min          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_max          0.500

_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             484
_exptl_absorpt_coefficient_mu    1.728

# Sheldrick geometric approximatio 0.50 0.42 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_T_max  0.42
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_device       Serial
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      100
_diffrn_ambient_pressure         100
_diffrn_reflns_number            10892
_diffrn_reflns_av_unetI/netI     0.033
_reflns_number_total             3858
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 3858 
# Number of reflections with Friedels Law is 2399 
# Theoretical number of reflections is about 2282 


_diffrn_reflns_theta_min         4.562
_diffrn_reflns_theta_max         71.384
_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        69.243
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              -10
_reflns_limit_k_max              7
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.39
_oxford_diffrn_Wilson_scale      0.24

_atom_sites_solution_primary     other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.20
_refine_diff_density_max         0.22


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     5
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3842
_oxford_refine_ls_R_factor_ref   0.0342
_refine_ls_wR_factor_ref         0.0637
_refine_ls_goodness_of_fit_ref   1.9544
_refine_ls_shift/su_max          0.0003449
_refine_ls_shift/su_mean         0.0000630


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3842
_refine_ls_R_factor_all          0.0342
_refine_ls_wR_factor_all         0.0637

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3806
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_gt          0.0635

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661-683 
_oxford_Hooft_y                  -0.001(5) # for 1450 Friedel pairs 
_oxford_Bijvoet_difference       0.015(5) # for 1450 Friedel pairs 
# (Similar to the Parsons(q).) 
_oxford_refined_Flack_x          0.013(16) # for 1459 Friedel pairs 
_refine_ls_abs_structure_Flack   0.015(5)
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 1450 Friedel Pairs 
;

# choose from: 
# rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 9.59 12.4 2.85 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cl1 Cl 0.07796(7) 0.36680(11) 0.90258(5) 0.0373 1.0000 Uani . . . . . .
C2 C 0.0873(2) 0.5405(3) 0.84759(18) 0.0264 1.0000 Uani . . . . . .
N3 N 0.0592(2) 0.6556(3) 0.90592(15) 0.0316 1.0000 Uani . . . . . .
C4 C 0.0646(3) 0.7855(4) 0.85884(19) 0.0304 1.0000 Uani . . . . . .
N5 N 0.0941(2) 0.8109(3) 0.76329(15) 0.0259 1.0000 Uani . . . . . .
C6 C 0.1232(2) 0.6908(3) 0.70811(17) 0.0230 1.0000 Uani . . . . . .
C7 C 0.1210(2) 0.5475(3) 0.74764(19) 0.0248 1.0000 Uani . . . . . .
N8 N 0.15389(19) 0.7214(2) 0.60951(14) 0.0194 1.0000 Uani . . . . . .
C9 C 0.1698(2) 0.6134(3) 0.53561(17) 0.0204 1.0000 Uani . . . . . .
O10 O 0.1723(2) 0.4816(2) 0.54701(13) 0.0280 1.0000 Uani . . . . . .
N11 N 0.18047(19) 0.6912(2) 0.44649(14) 0.0175 1.0000 Uani . . . . . .
C12 C 0.1966(2) 0.6252(3) 0.35296(17) 0.0177 1.0000 Uani . . . . . .
N13 N 0.1941(2) 0.7220(2) 0.27619(15) 0.0198 1.0000 Uani . . . . . .
C14 C 0.2137(3) 0.6613(3) 0.18610(18) 0.0237 1.0000 Uani . . . . . .
N15 N 0.2360(2) 0.5211(3) 0.16337(14) 0.0210 1.0000 Uani . . . . . .
C16 C 0.2354(2) 0.4268(3) 0.24134(18) 0.0165 1.0000 Uani . . . . . .
C17 C 0.2160(2) 0.4741(3) 0.33962(17) 0.0165 1.0000 Uani . . . . . .
N18 N 0.2592(2) 0.2809(2) 0.21773(15) 0.0176 1.0000 Uani . . . . . .
C19 C 0.2224(2) 0.1591(3) 0.27741(18) 0.0222 1.0000 Uani D . . . . .
O20 O 0.1838(2) 0.1655(2) 0.36346(13) 0.0302 1.0000 Uani . . . . . .
N21 N 0.2393(2) 0.0359(3) 0.22194(15) 0.0255 1.0000 Uani D . . . . .
C22 C 0.2723(3) 0.0652(3) 0.11806(19) 0.0249 1.0000 Uani D . . . . .
C23 C 0.2982(2) 0.2336(3) 0.11550(16) 0.0181 1.0000 Uani . . . . . .
C24 C 0.4475(3) 0.2756(4) 0.0919(2) 0.0419 1.0000 Uani . . . . . .
C25 C 0.4752(4) 0.2380(4) -0.0193(3) 0.0632 1.0000 Uani . . . . . .
C26 C 0.5522(3) 0.2006(5) 0.1627(3) 0.0732 1.0000 Uani . . . . . .
C27 C 0.1601(3) 0.8516(3) 0.45824(16) 0.0229 1.0000 Uani . . . . . .
C28 C 0.1659(2) 0.8747(3) 0.57222(17) 0.0211 1.0000 Uani . . . . . .
C29 C 0.2965(3) 0.9485(3) 0.61163(19) 0.0250 1.0000 Uani . . . . . .
C30 C 0.2867(3) 1.1184(3) 0.6006(2) 0.0376 1.0000 Uani . . . . . .
C31 C 0.3970(3) 1.2005(4) 0.6596(2) 0.0499 1.0000 Uani . . . . . .
C32 C 0.4292(3) 0.8846(4) 0.5664(2) 0.0435 1.0000 Uani . . . . . .
H41 H 0.0402 0.8709 0.8981 0.0399 1.0000 Uiso R . . . . .
H71 H 0.1410 0.4581 0.7118 0.0327 1.0000 Uiso R . . . . .
H141 H 0.2109 0.7300 0.1312 0.0306 1.0000 Uiso R . . . . .
H171 H 0.2172 0.4094 0.3934 0.0223 1.0000 Uiso R . . . . .
H222 H 0.3540 0.0131 0.0990 0.0338 1.0000 Uiso R . . . . .
H221 H 0.1900 0.0445 0.0745 0.0329 1.0000 Uiso R . . . . .
H231 H 0.2317 0.2810 0.0655 0.0254 1.0000 Uiso R . . . . .
H241 H 0.4555 0.3874 0.1002 0.0524 1.0000 Uiso R . . . . .
H251 H 0.5704 0.2716 -0.0350 0.0941 1.0000 Uiso R . . . . .
H252 H 0.4065 0.2926 -0.0632 0.0950 1.0000 Uiso R . . . . .
H253 H 0.4695 0.1310 -0.0281 0.0936 1.0000 Uiso R . . . . .
H261 H 0.6432 0.2339 0.1449 0.1037 1.0000 Uiso R . . . . .
H262 H 0.5331 0.2261 0.2331 0.1040 1.0000 Uiso R . . . . .
H263 H 0.5479 0.0915 0.1521 0.1041 1.0000 Uiso R . . . . .
H272 H 0.2342 0.9077 0.4254 0.0322 1.0000 Uiso R . . . . .
H271 H 0.0659 0.8797 0.4303 0.0314 1.0000 Uiso R . . . . .
H281 H 0.0834 0.9336 0.5940 0.0289 1.0000 Uiso R . . . . .
H291 H 0.2998 0.9277 0.6847 0.0310 1.0000 Uiso R . . . . .
H301 H 0.1924 1.1475 0.6211 0.0520 1.0000 Uiso R . . . . .
H302 H 0.2961 1.1374 0.5313 0.0519 1.0000 Uiso R . . . . .
H312 H 0.3831 1.3062 0.6525 0.0761 1.0000 Uiso R . . . . .
H311 H 0.3876 1.1738 0.7311 0.0767 1.0000 Uiso R . . . . .
H313 H 0.4921 1.1722 0.6362 0.0764 1.0000 Uiso R . . . . .
H322 H 0.5112 0.9198 0.6029 0.0701 1.0000 Uiso R . . . . .
H321 H 0.4268 0.7754 0.5672 0.0695 1.0000 Uiso R . . . . .
H323 H 0.4346 0.9193 0.4975 0.0698 1.0000 Uiso R . . . . .
H211 H 0.219(3) -0.050(2) 0.2418(14) 0.032(2) 1.0000 Uiso D . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.8801(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 . C2 . 1.734(3) yes
C2 . N3 . 1.329(4) yes
C2 . C7 . 1.382(3) yes
N3 . C4 . 1.332(4) yes
C4 . N5 . 1.334(3) yes
C4 . H41 . 0.963 no
N5 . C6 . 1.342(3) yes
C6 . C7 . 1.397(4) yes
C6 . N8 . 1.384(3) yes
C7 . H71 . 0.959 no
N8 . C9 . 1.399(3) yes
N8 . C28 . 1.475(4) yes
C9 . O10 . 1.199(3) yes
C9 . N11 . 1.391(3) yes
N11 . C12 . 1.398(3) yes
N11 . C27 . 1.469(3) yes
C12 . N13 . 1.350(3) yes
C12 . C17 . 1.387(3) yes
N13 . C14 . 1.341(3) yes
C14 . N15 . 1.319(4) yes
C14 . H141 . 0.963 no
N15 . C16 . 1.348(3) yes
C16 . C17 . 1.399(3) yes
C16 . N18 . 1.373(3) yes
C17 . H171 . 0.929 no
N18 . C19 . 1.406(3) yes
N18 . C23 . 1.486(3) yes
C19 . O20 . 1.216(3) yes
C19 . N21 . 1.348(3) yes
N21 . C22 . 1.455(3) yes
N21 . H211 . 0.845(17) no
C22 . C23 . 1.539(4) yes
C22 . H222 . 0.956 no
C22 . H221 . 1.005 no
C23 . C24 . 1.529(3) yes
C23 . H231 . 1.023 no
C24 . C25 . 1.553(4) yes
C24 . C26 . 1.545(5) yes
C24 . H241 . 1.018 no
C25 . H251 . 0.994 no
C25 . H252 . 1.016 no
C25 . H253 . 0.974 no
C26 . H261 . 0.962 no
C26 . H262 . 0.990 no
C26 . H263 . 0.995 no
C27 . C28 . 1.545(3) yes
C27 . H272 . 0.983 no
C27 . H271 . 1.018 no
C28 . C29 . 1.524(3) yes
C28 . H281 . 1.004 no
C29 . C30 . 1.542(4) yes
C29 . C32 . 1.535(3) yes
C29 . H291 . 0.999 no
C30 . C31 . 1.522(4) yes
C30 . H301 . 0.991 no
C30 . H302 . 0.949 no
C31 . H312 . 0.967 no
C31 . H311 . 0.994 no
C31 . H313 . 1.007 no
C32 . H322 . 0.985 no
C32 . H321 . 0.985 no
C32 . H323 . 0.978 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . C2 . N3 . 116.36(19) yes
Cl1 . C2 . C7 . 117.8(2) yes
N3 . C2 . C7 . 125.8(3) yes
C2 . N3 . C4 . 113.5(2) yes
N3 . C4 . N5 . 128.0(3) yes
N3 . C4 . H41 . 115.7 no
N5 . C4 . H41 . 116.3 no
C4 . N5 . C6 . 116.0(3) yes
N5 . C6 . C7 . 122.2(2) yes
N5 . C6 . N8 . 114.3(2) yes
C7 . C6 . N8 . 123.4(2) yes
C6 . C7 . C2 . 114.5(3) yes
C6 . C7 . H71 . 125.7 no
C2 . C7 . H71 . 119.8 no
C6 . N8 . C9 . 124.3(2) yes
C6 . N8 . C28 . 121.9(2) yes
C9 . N8 . C28 . 113.78(19) yes
N8 . C9 . O10 . 127.0(2) yes
N8 . C9 . N11 . 105.5(2) yes
O10 . C9 . N11 . 127.5(2) yes
C9 . N11 . C12 . 124.5(2) yes
C9 . N11 . C27 . 113.25(19) yes
C12 . N11 . C27 . 122.05(19) yes
N11 . C12 . N13 . 114.1(2) yes
N11 . C12 . C17 . 123.3(2) yes
N13 . C12 . C17 . 122.6(2) yes
C12 . N13 . C14 . 114.9(2) yes
N13 . C14 . N15 . 128.6(2) yes
N13 . C14 . H141 . 115.1 no
N15 . C14 . H141 . 116.3 no
C14 . N15 . C16 . 115.1(2) yes
N15 . C16 . C17 . 122.7(2) yes
N15 . C16 . N18 . 115.1(2) yes
C17 . C16 . N18 . 122.2(2) yes
C16 . C17 . C12 . 116.1(2) yes
C16 . C17 . H171 . 122.7 no
C12 . C17 . H171 . 121.2 no
C16 . N18 . C19 . 125.1(2) yes
C16 . N18 . C23 . 122.1(2) yes
C19 . N18 . C23 . 111.5(2) yes
N18 . C19 . O20 . 125.6(3) yes
N18 . C19 . N21 . 107.4(2) yes
O20 . C19 . N21 . 127.0(3) yes
C19 . N21 . C22 . 114.0(2) yes
C19 . N21 . H211 . 123.8(12) no
C22 . N21 . H211 . 121.4(12) no
N21 . C22 . C23 . 103.7(2) yes
N21 . C22 . H222 . 110.5 no
C23 . C22 . H222 . 110.1 no
N21 . C22 . H221 . 110.3 no
C23 . C22 . H221 . 107.4 no
H222 . C22 . H221 . 114.2 no
C22 . C23 . N18 . 102.77(19) yes
C22 . C23 . C24 . 113.8(2) yes
N18 . C23 . C24 . 111.3(2) yes
C22 . C23 . H231 . 108.9 no
N18 . C23 . H231 . 108.9 no
C24 . C23 . H231 . 110.9 no
C23 . C24 . C25 . 108.1(3) yes
C23 . C24 . C26 . 112.6(3) yes
C25 . C24 . C26 . 112.4(3) yes
C23 . C24 . H241 . 107.1 no
C25 . C24 . H241 . 108.0 no
C26 . C24 . H241 . 108.4 no
C24 . C25 . H251 . 107.4 no
C24 . C25 . H252 . 109.7 no
H251 . C25 . H252 . 109.7 no
C24 . C25 . H253 . 108.8 no
H251 . C25 . H253 . 109.2 no
H252 . C25 . H253 . 111.9 no
C24 . C26 . H261 . 108.2 no
C24 . C26 . H262 . 111.2 no
H261 . C26 . H262 . 109.7 no
C24 . C26 . H263 . 108.5 no
H261 . C26 . H263 . 108.2 no
H262 . C26 . H263 . 111.0 no
N11 . C27 . C28 . 103.5(2) yes
N11 . C27 . H272 . 111.1 no
C28 . C27 . H272 . 110.4 no
N11 . C27 . H271 . 109.0 no
C28 . C27 . H271 . 111.3 no
H272 . C27 . H271 . 111.3 no
C27 . C28 . N8 . 101.9(2) yes
C27 . C28 . C29 . 115.6(2) yes
N8 . C28 . C29 . 110.9(2) yes
C27 . C28 . H281 . 109.4 no
N8 . C28 . H281 . 109.5 no
C29 . C28 . H281 . 109.2 no
C28 . C29 . C30 . 110.4(2) yes
C28 . C29 . C32 . 113.3(2) yes
C30 . C29 . C32 . 112.7(3) yes
C28 . C29 . H291 . 106.5 no
C30 . C29 . H291 . 106.4 no
C32 . C29 . H291 . 107.0 no
C29 . C30 . C31 . 113.0(3) yes
C29 . C30 . H301 . 107.0 no
C31 . C30 . H301 . 112.0 no
C29 . C30 . H302 . 105.6 no
C31 . C30 . H302 . 110.7 no
H301 . C30 . H302 . 108.3 no
C30 . C31 . H312 . 109.3 no
C30 . C31 . H311 . 108.6 no
H312 . C31 . H311 . 108.7 no
C30 . C31 . H313 . 110.9 no
H312 . C31 . H313 . 110.3 no
H311 . C31 . H313 . 109.0 no
C29 . C32 . H322 . 111.0 no
C29 . C32 . H321 . 110.6 no
H322 . C32 . H321 . 109.6 no
C29 . C32 . H323 . 107.4 no
H322 . C32 . H323 . 108.9 no
H321 . C32 . H323 . 109.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C17 . H171 . O10 . 123 0.93 2.21 2.817(4) yes
C27 . H271 . O10 2_556 151 1.02 2.50 3.429(4) yes
C30 . H302 . O20 1_565 149 0.95 2.51 3.360(4) yes
N21 . H211 . N13 1_545 171(2) 0.845 2.118 2.955(4) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
_chemical_name_systematic        'Dimer 2a'
####################################################################### 
# 
# 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_I_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2057486'
loop_
_audit_author_name
_audit_author_address
'Christopher Serpell'
;University of Kent
United Kingdom
;
_audit_update_record             
;
2021-01-22 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
Portions of the macrocyclic skeleton were found in the raw structure 
solution from Superflip. With the exception of the side chains, the rest 
of the structure was resolved by Fourier cycles. The refinement was not 
stable, and restaints were applied to bond distances following measurements
from a previous structure (CCDC #1824642) corresponding to the repeating
motif in the present structure. The first carbon of the side chains was
then resolvable in the Fourier map, and in agreement with the expected
chirality. Refinement of the anisotropic ADPs revealed that there was 
extensive disorder in the macrocycle position along the vector perpendicular
to its plane. The molecule was then modelled over two positions, and with 
competitively refined occupancy. Further side chain structure then became
visible, although it was not possible to distinguish between valine and 
isoleucine-derived monomers, with the additional methyl unit failing to 
appear or to refine to physically reasonable positions even when restrained.
The anisotropic ADPs of both sets of atoms for the macrocycle were still
prolate beyond physically reasonable limits, and so restrained refinement
from isotropic ADPs was performed to account for electron density, before
fixing the ADPs. The macrocycle could feasibly be modelled over more than 
two locations, but the qualitative description of the structure would not 
be more precise - there is extensive disorder in position perpendicular to
the plane of the macrocycle. Hydrogen atoms were added geometrically, and 
the solvent was modelled by examination of stant Fourier maps. While we are 
confident of the location and orientation of the chloroform molecules, the 
ethanol molecules are more speculative. Solvent molecules were refined 
isotropically and with partial occupancies. Weights were selected the the 
structure was refined to convergence.
This is a low-quality structure and only information about connectivity,
relative molecular position and orientation, and gross conformation of the 
main residue should be taken with any level of confidence. There are no
fully ordered portions.
;

_vrf_PLAT027_I                   
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      41.63 Degree
RESPONSE: The crystal was extremely weakly diffracting and high-angle data
were absent.
;
_vrf_PLAT084_I                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.52 Report
RESPONSE: This reflects the poor quality of the diffraction data and the
disordered nature of the crystal.
;
_vrf_PLAT707_I                   
;
PROBLEM: D...A   Calc 2.23330(10), Rep   2.232(18), Dev..      13.00 Sigma 
RESPONSE: This is between two disordered residues and is unlikely to occur
in any one instance.
;


_cell_length_a                   12.00486(4)
_cell_length_b                   18.58877(3)
_cell_length_c                   23.79439(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.150(5)
_cell_angle_gamma                90
_cell_volume                     5279.29(6)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2'
_symmetry_space_group_name_Hall  'I 2y'
loop_
_symmetry_equiv_pos_as_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

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0492 0.0322 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C5.25 H6.50 Cl0.75 N2 O0.50 
# Dc =      0.17 Fooo =    275.00 Mu =      4.28 M =    132.21
# Found Formula = C42.64 H56.23 Cl3.11 N16 O5.46 
# Dc =      1.25 FOOO =   2082.26 Mu =     20.98 M =    990.44

_chemical_formula_sum            'C42.64 H56.23 Cl3.11 N16 O5.46'
_chemical_formula_moiety         'C42.64 H56.23 Cl3.11 N16 O5.46'
_chemical_compound_source        .
_chemical_formula_weight         990.44


_cell_measurement_reflns_used    4657
_cell_measurement_theta_min      3
_cell_measurement_theta_max      68
_cell_measurement_temperature    100(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.005
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_max          0.220

_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2082.261
_exptl_absorpt_coefficient_mu    2.098

# Sheldrick geometric approximatio 0.75 0.99 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
# 
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_T_max  0.99
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter χ goniometer'
_diffrn_measurement_device_type  
;
Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'


_diffrn_radiation_collimation    0.3
_diffrn_radiation_collimation_monochromator 'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'

_diffrn_source                   'Rotating anode'
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_source_current           30.0
_diffrn_source_target            Cu
_diffrn_radiation_wavelength     1.54178

_diffrn_ambient_temperature      100(2)

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_reflns_number            31995
_diffrn_reflns_av_unetI/netI     0.181
_reflns_number_total             9165
_diffrn_reflns_av_R_equivalents  0.114
# Number of reflections without Friedels Law is 9165 
# Number of reflections with Friedels Law is 4908 
# Theoretical number of reflections is about 4834 


_diffrn_reflns_theta_min         3.023
_diffrn_reflns_theta_max         68.242
_diffrn_measured_fraction_theta_max 0.981

_diffrn_reflns_theta_full        41.627
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -14
_reflns_limit_h_max              14
_reflns_limit_k_min              -22
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   5.11
_oxford_diffrn_Wilson_scale      0.96

_atom_sites_solution_primary     other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.69
_refine_diff_density_max         0.71


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_restraints     675
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6744
_oxford_refine_ls_R_factor_ref   0.2252
_refine_ls_wR_factor_ref         0.4983
_refine_ls_goodness_of_fit_ref   1.7645
_refine_ls_shift/su_max          0.0370659
_refine_ls_shift/su_mean         0.0040268


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        9165
_refine_ls_R_factor_all          0.2533
_refine_ls_wR_factor_all         0.5199

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3801
_refine_ls_R_factor_gt           0.1864
_refine_ls_wR_factor_gt          0.4695

# For an explanation, see Cooper & Watkin, Acta Cryst. (2016). B72, 661-683 
_oxford_Hooft_y                  0.19(5) # for 1818 Friedel pairs 
_oxford_Bijvoet_difference       0.22(4) # for 1818 Friedel pairs 
# (Similar to the Parsons(q).) 
_refine_ls_abs_structure_Flack   0.22(4)
_refine_ls_abs_structure_details 
; 
 Parsons, Flack & Wagner (2013), 
 1818 Friedel Pairs 
;

# choose from: 
# rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.20P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C815 C -0.0000 0.124(2) 0.0000 0.114(9) 0.3791 Uiso DS U . 1 6 .
O816 O 0.0000 0.047(2) 0.0000 0.114(9) 0.3791 Uiso DS U . 1 6 .
Cl820 Cl 0.8919(9) 0.2708(12) 0.4619(7) 0.375(8) 0.8733 Uiso D U . 1 9 .
N10 N 0.5232(7) 0.3342(6) 0.3103(3) 0.0814 0.486(3) Uani D U P 1 1 .
N11 N 0.4764(6) 0.3338(6) 0.3123(3) 0.0799 0.514(3) Uani D U P 1 2 .
C20 C 0.554(2) 0.4103(6) 0.3180(7) 0.0816 0.486(3) Uani D U P 1 1 .
C21 C 0.488(2) 0.4106(6) 0.3263(7) 0.0803 0.514(3) Uani D U P 1 2 .
C30 C 0.6161(14) 0.4092(6) 0.3763(6) 0.0815 0.486(3) Uani D U P 1 1 .
C31 C 0.5592(12) 0.4121(6) 0.3822(6) 0.0799 0.514(3) Uani D U P 1 2 .
N40 N 0.6092(7) 0.3350(6) 0.3971(3) 0.0804 0.486(3) Uani D U P 1 1 .
N41 N 0.5566(7) 0.3369(5) 0.4012(3) 0.0792 0.514(3) Uani D U P 1 2 .
C50 C 0.5633(8) 0.2901(6) 0.3545(4) 0.0804 0.486(3) Uani D U P 1 1 .
C51 C 0.5110(7) 0.2918(5) 0.3587(4) 0.0795 0.514(3) Uani D U P 1 2 .
O60 O 0.5591(7) 0.2257(6) 0.3568(5) 0.0799 0.486(3) Uani D U P 1 1 .
O61 O 0.5032(7) 0.2276(5) 0.3616(5) 0.0797 0.514(3) Uani D U P 1 2 .
C70 C 0.6442(6) 0.3140(6) 0.4527(3) 0.0802 0.486(3) Uani D U P 1 1 .
C71 C 0.5866(7) 0.3130(5) 0.4565(3) 0.0780 0.514(3) Uani D U P 1 2 .
N80 N 0.6663(6) 0.3660(4) 0.4914(4) 0.0810 0.486(3) Uani D U P 1 1 .
N81 N 0.6111(7) 0.3661(4) 0.4939(4) 0.0784 0.514(3) Uani D U P 1 2 .
C90 C 0.6968(7) 0.3426(5) 0.5440(3) 0.0810 0.486(3) Uani D U P 1 1 .
C91 C 0.6442(7) 0.3445(5) 0.5467(3) 0.0782 0.514(3) Uani D U P 1 2 .
N100 N 0.7001(7) 0.2748(6) 0.5629(3) 0.0807 0.486(3) Uani D U P 1 1 .
N101 N 0.6551(7) 0.2770(6) 0.5663(3) 0.0785 0.514(3) Uani D U P 1 2 .
C110 C 0.6723(7) 0.2247(4) 0.5235(4) 0.0798 0.486(3) Uani D U P 1 1 .
C111 C 0.6299(8) 0.2255(4) 0.5275(4) 0.0785 0.514(3) Uani D U P 1 2 .
C120 C 0.6388(7) 0.2409(5) 0.4667(4) 0.0796 0.486(3) Uani D U P 1 1 .
C121 C 0.5947(8) 0.2399(5) 0.4707(4) 0.0784 0.514(3) Uani D U P 1 2 .
N210 N 0.6986(7) 0.1544(4) 0.5414(4) 0.0801 0.486(3) Uani D U P 1 1 .
N211 N 0.6413(8) 0.1538(4) 0.5451(4) 0.0798 0.514(3) Uani D U P 1 2 .
C220 C 0.722(2) 0.1325(9) 0.6008(4) 0.0808 0.486(3) Uani D U P 1 1 .
C221 C 0.667(2) 0.1323(9) 0.6045(5) 0.0804 0.514(3) Uani D U P 1 2 .
C230 C 0.7532(11) 0.0547(9) 0.5963(5) 0.0808 0.486(3) Uani D U P 1 1 .
C231 C 0.6960(11) 0.0538(9) 0.6036(5) 0.0807 0.514(3) Uani D U P 1 2 .
N240 N 0.6913(7) 0.0370(4) 0.5414(4) 0.0808 0.486(3) Uani D U P 1 1 .
N241 N 0.6487(8) 0.0330(4) 0.5464(4) 0.0806 0.514(3) Uani D U P 1 2 .
C250 C 0.6745(7) 0.0961(6) 0.5063(3) 0.0803 0.486(3) Uani D U P 1 1 .
C251 C 0.6157(7) 0.0923(6) 0.5139(3) 0.0805 0.514(3) Uani D U P 1 2 .
O260 O 0.6461(7) 0.0906(8) 0.4566(3) 0.0825 0.486(3) Uani D U P 1 1 .
O261 O 0.5717(7) 0.0904(8) 0.4662(3) 0.0819 0.514(3) Uani D U P 1 2 .
C270 C 0.7044(6) -0.0330(4) 0.5215(4) 0.0818 0.486(3) Uani D U P 1 1 .
C271 C 0.6465(6) -0.0370(4) 0.5245(4) 0.0800 0.514(3) Uani D U P 1 2 .
N280 N 0.7314(6) -0.0847(6) 0.5599(3) 0.0829 0.486(3) Uani D U P 1 1 .
N281 N 0.6730(6) -0.0873(5) 0.5641(3) 0.0803 0.514(3) Uani D U P 1 2 .
C290 C 0.7146(6) -0.1521(5) 0.5409(3) 0.0829 0.486(3) Uani D U P 1 1 .
C291 C 0.6615(6) -0.1553(5) 0.5459(3) 0.0803 0.514(3) Uani D U P 1 2 .
N300 N 0.6668(7) -0.1734(5) 0.4903(4) 0.0830 0.486(3) Uani D U P 1 1 .
N301 N 0.6197(7) -0.1787(4) 0.4948(4) 0.0805 0.514(3) Uani D U P 1 2 .
C310 C 0.6369(7) -0.1201(6) 0.4539(3) 0.0825 0.486(3) Uani D U P 1 1 .
C311 C 0.5912(7) -0.1268(6) 0.4569(3) 0.0803 0.514(3) Uani D U P 1 2 .
C320 C 0.6490(7) -0.0471(5) 0.4677(4) 0.0819 0.486(3) Uani D U P 1 1 .
C321 C 0.5970(7) -0.0533(5) 0.4700(4) 0.0800 0.514(3) Uani D U P 1 2 .
N410 N 0.5856(7) -0.1463(6) 0.4023(3) 0.0831 0.486(3) Uani D U P 1 1 .
N411 N 0.5380(7) -0.1495(6) 0.4047(3) 0.0820 0.514(3) Uani D U P 1 2 .
C420 C 0.575(2) -0.2235(6) 0.3894(7) 0.0841 0.486(3) Uani D U P 1 1 .
C421 C 0.516(2) -0.2261(6) 0.3930(7) 0.0830 0.514(3) Uani D U P 1 2 .
C430 C 0.5289(16) -0.2227(6) 0.3282(6) 0.0840 0.486(3) Uani D U P 1 1 .
C431 C 0.4619(14) -0.2273(5) 0.3332(6) 0.0832 0.514(3) Uani D U P 1 2 .
N440 N 0.4932(7) -0.1481(6) 0.3162(3) 0.0835 0.486(3) Uani D U P 1 1 .
N441 N 0.4393(7) -0.1507(5) 0.3215(3) 0.0828 0.514(3) Uani D U P 1 2 .
C450 C 0.5406(8) -0.1033(5) 0.3584(4) 0.0834 0.486(3) Uani D U P 1 1 .
C451 C 0.4873(8) -0.1051(5) 0.3630(4) 0.0819 0.514(3) Uani D U P 1 2 .
O460 O 0.5395(8) -0.0388(5) 0.3554(5) 0.0869 0.486(3) Uani D U P 1 1 .
O461 O 0.4834(8) -0.0406(5) 0.3625(5) 0.0789 0.514(3) Uani D U P 1 2 .
C470 C 0.4312(6) -0.1262(6) 0.2659(3) 0.0834 0.486(3) Uani D U P 1 1 .
C471 C 0.3817(6) -0.1285(6) 0.2702(3) 0.0827 0.514(3) Uani D U P 1 2 .
N480 N 0.4052(6) -0.1778(4) 0.2273(4) 0.0842 0.486(3) Uani D U P 1 1 .
N481 N 0.3382(7) -0.1799(4) 0.2348(4) 0.0838 0.514(3) Uani D U P 1 2 .
C490 C 0.3499(7) -0.1550(5) 0.1787(3) 0.0845 0.486(3) Uani D U P 1 1 .
C491 C 0.2738(6) -0.1559(5) 0.1892(3) 0.0841 0.514(3) Uani D U P 1 2 .
N500 N 0.3249(7) -0.0873(5) 0.1629(3) 0.0845 0.486(3) Uani D U P 1 1 .
N501 N 0.2543(7) -0.0877(5) 0.1731(3) 0.0840 0.514(3) Uani D U P 1 2 .
C510 C 0.3562(8) -0.0372(4) 0.2018(4) 0.0841 0.486(3) Uani D U P 1 1 .
C511 C 0.3022(8) -0.0380(4) 0.2086(4) 0.0830 0.514(3) Uani D U P 1 2 .
C520 C 0.4155(7) -0.0528(5) 0.2543(4) 0.0835 0.486(3) Uani D U P 1 1 .
C521 C 0.3731(7) -0.0550(5) 0.2575(4) 0.0825 0.514(3) Uani D U P 1 2 .
N610 N 0.3367(7) 0.0345(4) 0.1856(4) 0.0842 0.486(3) Uani D U P 1 1 .
N611 N 0.2835(7) 0.0318(4) 0.1878(4) 0.0839 0.514(3) Uani D U P 1 2 .
C620 C 0.282(2) 0.0533(10) 0.1291(7) 0.0855 0.486(3) Uani D U P 1 1 .
C621 C 0.230(2) 0.0565(9) 0.1328(7) 0.0848 0.514(3) Uani D U P 1 2 .
C630 C 0.3259(15) 0.1281(8) 0.1222(4) 0.0855 0.486(3) Uani D U P 1 1 .
C631 C 0.2585(14) 0.1347(9) 0.1289(4) 0.0847 0.514(3) Uani D U P 1 2 .
N640 N 0.3489(7) 0.1512(4) 0.1814(4) 0.0848 0.486(3) Uani D U P 1 1 .
N641 N 0.2932(7) 0.1523(4) 0.1884(4) 0.0829 0.514(3) Uani D U P 1 2 .
C650 C 0.3638(7) 0.0942(6) 0.2187(3) 0.0839 0.486(3) Uani D U P 1 1 .
C651 C 0.3074(7) 0.0914(6) 0.2216(3) 0.0828 0.514(3) Uani D U P 1 2 .
O661 O 0.3372(7) 0.0939(9) 0.2713(3) 0.0849 0.514(3) Uani D U P 1 2 .
O660 O 0.3941(7) 0.0998(8) 0.2682(3) 0.0834 0.486(3) Uani D U P 1 1 .
C670 C 0.3712(8) 0.2217(4) 0.1999(4) 0.0845 0.486(3) Uani D U P 1 1 .
C671 C 0.3154(8) 0.2239(4) 0.2040(4) 0.0811 0.514(3) Uani D U P 1 2 .
N680 N 0.3250(7) 0.2736(5) 0.1660(3) 0.0845 0.486(3) Uani D U P 1 1 .
N681 N 0.2686(7) 0.2755(5) 0.1699(3) 0.0816 0.514(3) Uani D U P 1 2 .
C690 C 0.3538(7) 0.3408(5) 0.1821(3) 0.0846 0.486(3) Uani D U P 1 1 .
C691 C 0.2928(7) 0.3429(5) 0.1869(3) 0.0808 0.514(3) Uani D U P 1 2 .
N700 N 0.4231(7) 0.3616(4) 0.2270(4) 0.0841 0.486(3) Uani D U P 1 1 .
N701 N 0.3574(7) 0.3644(4) 0.2333(4) 0.0808 0.514(3) Uani D U P 1 2 .
C710 C 0.4676(7) 0.3080(5) 0.2596(3) 0.0832 0.486(3) Uani D U P 1 1 .
C711 C 0.4028(7) 0.3111(5) 0.2660(3) 0.0796 0.514(3) Uani D U P 1 2 .
C720 C 0.4449(7) 0.2352(5) 0.2485(4) 0.0838 0.486(3) Uani D U P 1 1 .
C721 C 0.3845(8) 0.2381(5) 0.2540(4) 0.0803 0.514(3) Uani D U P 1 2 .
C330 C 0.8819(11) 0.0485(6) 0.6028(5) 0.0833 0.486(3) Uani D U P 1 1 .
C331 C 0.8227(11) 0.0388(5) 0.6136(4) 0.0835 0.514(3) Uani D U P 1 2 .
C530 C 0.6113(14) -0.2532(6) 0.2890(4) 0.0867 0.486(3) Uani D U P 1 1 .
C531 C 0.5400(14) -0.2639(5) 0.2946(4) 0.0854 0.514(3) Uani D U P 1 2 .
C730 C 0.4338(14) 0.1296(6) 0.0926(4) 0.0877 0.486(3) Uani D U P 1 1 .
C731 C 0.3572(13) 0.1441(6) 0.0932(4) 0.0889 0.514(3) Uani D U P 1 2 .
C130 C 0.7406(13) 0.4213(6) 0.3691(5) 0.0865 0.486(3) Uani D U P 1 1 .
C131 C 0.6798(12) 0.4371(5) 0.3767(5) 0.0835 0.514(3) Uani D U P 1 2 .
Cl804 Cl 0.6412(10) 0.0956(8) 0.2653(4) 0.224(3) 0.5923 Uiso D U . 1 3 .
Cl803 Cl 0.7909(11) 0.1588(6) 0.3620(5) 0.223(3) 0.5923 Uiso D U . 1 3 .
Cl802 Cl 0.7813(12) -0.0013(6) 0.3454(5) 0.227(3) 0.5923 Uiso D U . 1 3 .
C801 C 0.7127(7) 0.0831(6) 0.3341(4) 0.224(3) 0.5923 Uiso D U . 1 3 .
C751 C 0.4493(15) 0.0880(12) 0.1095(7) 0.0937 0.514(3) Uani D U P 1 2 .
C741 C 0.3169(16) 0.1403(11) 0.0296(4) 0.0916 0.514(3) Uani D U P 1 2 .
C341 C 0.8722(13) 0.0661(11) 0.6721(5) 0.0890 0.514(3) Uani D U P 1 2 .
C541 C 0.5512(18) -0.3449(5) 0.3075(7) 0.0877 0.514(3) Uani D U P 1 2 .
C740 C 0.4066(16) 0.1313(11) 0.0279(4) 0.0910 0.486(3) Uani D U P 1 1 .
C351 C 0.8843(14) 0.0722(11) 0.5664(6) 0.0923 0.514(3) Uani D U P 1 2 .
C150 C 0.7804(18) 0.3691(9) 0.3252(8) 0.0968 0.486(3) Uani D U P 1 1 .
C140 C 0.7621(17) 0.5000(7) 0.3530(9) 0.0923 0.486(3) Uani D U P 1 1 .
C750 C 0.5100(16) 0.0653(10) 0.1111(7) 0.0923 0.486(3) Uani D U P 1 1 .
C540 C 0.6366(17) -0.3331(5) 0.3020(7) 0.0875 0.486(3) Uani D U P 1 1 .
C350 C 0.9339(16) 0.1031(12) 0.5646(7) 0.0945 0.486(3) Uani D U P 1 1 .
C340 C 0.9302(13) 0.0577(12) 0.6650(5) 0.0860 0.486(3) Uani D U P 1 1 .
C141 C 0.6847(15) 0.5192(6) 0.3687(8) 0.0879 0.514(3) Uani D U P 1 2 .
C550 C 0.7200(16) -0.2087(9) 0.2931(9) 0.0927 0.486(3) Uani D U P 1 1 .
C151 C 0.7290(16) 0.3974(9) 0.3282(7) 0.0911 0.514(3) Uani D U P 1 2 .
C551 C 0.6557(14) -0.2272(9) 0.2997(8) 0.0919 0.514(3) Uani D U P 1 2 .
O824 O 0.106(3) 0.0183(18) 0.0122(12) 0.211(9) 0.6209 Uiso D U . 1 7 .
C823 C 0.055(4) 0.067(2) -0.0294(18) 0.212(9) 0.6209 Uiso D U . 1 7 .
C826 C 0.8912 -0.2035 0.4757 0.2595 0.3000 Uiso D U . 1 5 .
O825 O 1.0570 -0.1478 0.6005 0.3504 0.5000 Uiso D U . 1 4 .
C819 C 1.0000 0.3222(12) 0.5000 0.375(8) 0.8733 Uiso DS U . 1 9 .
Cl821 Cl 0.9532(11) 0.3977(12) 0.5370(4) 0.375(8) 0.4570 Uiso D U . 1 9 .
H201 H 0.5970 0.4280 0.2896 0.0980 0.486(3) Uiso R . P 1 1 .
H203 H 0.4885 0.4384 0.3187 0.0980 0.486(3) Uiso R . P 1 1 .
H211 H 0.5240 0.4351 0.2980 0.0963 0.514(3) Uiso R . P 1 2 .
H212 H 0.4172 0.4316 0.3293 0.0963 0.514(3) Uiso R . P 1 2 .
H301 H 0.5874 0.4426 0.4013 0.0978 0.486(3) Uiso R . P 1 1 .
H311 H 0.5243 0.4412 0.4081 0.0959 0.514(3) Uiso R . P 1 2 .
H901 H 0.7189 0.3786 0.5713 0.0973 0.486(3) Uiso R . P 1 1 .
H911 H 0.6619 0.3813 0.5739 0.0939 0.514(3) Uiso R . P 1 2 .
H1201 H 0.6139 0.2051 0.4398 0.0955 0.486(3) Uiso R . P 1 1 .
H1211 H 0.5789 0.2030 0.4433 0.0940 0.514(3) Uiso R . P 1 2 .
H2202 H 0.7818 0.1597 0.6197 0.0970 0.486(3) Uiso R . P 1 1 .
H2203 H 0.6574 0.1375 0.6202 0.0970 0.486(3) Uiso R . P 1 1 .
H2211 H 0.7277 0.1594 0.6226 0.0965 0.514(3) Uiso R . P 1 2 .
H2212 H 0.6028 0.1388 0.6241 0.0965 0.514(3) Uiso R . P 1 2 .
H2301 H 0.7240 0.0277 0.6253 0.0969 0.486(3) Uiso R . P 1 1 .
H2311 H 0.6594 0.0286 0.6311 0.0969 0.514(3) Uiso R . P 1 2 .
H2901 H 0.7394 -0.1892 0.5667 0.0994 0.486(3) Uiso R . P 1 1 .
H2911 H 0.6849 -0.1918 0.5725 0.0963 0.514(3) Uiso R . P 1 2 .
H3201 H 0.6219 -0.0100 0.4424 0.0983 0.486(3) Uiso R . P 1 1 .
H3212 H 0.5703 -0.0169 0.4439 0.0960 0.514(3) Uiso R . P 1 2 .
H4201 H 0.6455 -0.2467 0.3954 0.1009 0.486(3) Uiso R . P 1 1 .
H4202 H 0.5239 -0.2460 0.4118 0.1009 0.486(3) Uiso R . P 1 1 .
H4211 H 0.5841 -0.2529 0.3969 0.0996 0.514(3) Uiso R . P 1 2 .
H4212 H 0.4665 -0.2453 0.4176 0.0996 0.514(3) Uiso R . P 1 2 .
H4301 H 0.4628 -0.2512 0.3239 0.1008 0.486(3) Uiso R . P 1 1 .
H4311 H 0.3923 -0.2518 0.3314 0.0998 0.514(3) Uiso R . P 1 2 .
H4901 H 0.3245 -0.1909 0.1520 0.1013 0.486(3) Uiso R . P 1 1 .
H4911 H 0.2380 -0.1918 0.1653 0.1009 0.514(3) Uiso R . P 1 2 .
H5202 H 0.4444 -0.0167 0.2801 0.1002 0.486(3) Uiso R . P 1 1 .
H5211 H 0.4121 -0.0192 0.2803 0.0990 0.514(3) Uiso R . P 1 2 .
H6201 H 0.3079 0.0234 0.1008 0.1026 0.486(3) Uiso R . P 1 1 .
H6202 H 0.2032 0.0498 0.1278 0.1026 0.486(3) Uiso R . P 1 1 .
H6211 H 0.2582 0.0296 0.1036 0.1017 0.514(3) Uiso R . P 1 2 .
H6212 H 0.1505 0.0509 0.1302 0.1017 0.514(3) Uiso R . P 1 2 .
H6301 H 0.2678 0.1566 0.1032 0.1026 0.486(3) Uiso R . P 1 1 .
H6311 H 0.1938 0.1616 0.1156 0.1017 0.514(3) Uiso R . P 1 2 .
H6901 H 0.3224 0.3784 0.1584 0.1015 0.486(3) Uiso R . P 1 1 .
H6912 H 0.2622 0.3804 0.1628 0.0970 0.514(3) Uiso R . P 1 2 .
H7201 H 0.4758 0.1976 0.2723 0.1006 0.486(3) Uiso R . P 1 1 .
H7211 H 0.4149 0.2007 0.2781 0.0963 0.514(3) Uiso R . P 1 2 .
H3301 H 0.9021 0.0016 0.5916 0.1000 0.486(3) Uiso R . P 1 1 .
H3311 H 0.8322 -0.0118 0.6111 0.1002 0.514(3) Uiso R . P 1 2 .
H5301 H 0.5799 -0.2472 0.2509 0.1041 0.486(3) Uiso R . P 1 1 .
H5311 H 0.5079 -0.2569 0.2567 0.1025 0.514(3) Uiso R . P 1 2 .
H7301 H 0.4695 0.1750 0.0986 0.1052 0.486(3) Uiso R . P 1 1 .
H7311 H 0.3789 0.1929 0.0988 0.1067 0.514(3) Uiso R . P 1 2 .
H1302 H 0.7825 0.4109 0.4043 0.1038 0.486(3) Uiso R . P 1 1 .
H1311 H 0.7216 0.4245 0.4115 0.1001 0.514(3) Uiso R . P 1 2 .
H8011 H 0.6542 0.0799 0.3579 0.1743 0.5923 Uiso R . . 1 3 .
H7511 H 0.5053 0.0989 0.0855 0.1125 0.514(3) Uiso R . P 1 2 .
H7512 H 0.4776 0.0972 0.1476 0.1125 0.514(3) Uiso R . P 1 2 .
H7513 H 0.4291 0.0387 0.1054 0.1125 0.514(3) Uiso R . P 1 2 .
H7411 H 0.3754 0.1505 0.0069 0.1099 0.514(3) Uiso R . P 1 2 .
H7412 H 0.2561 0.1723 0.0200 0.1099 0.514(3) Uiso R . P 1 2 .
H7413 H 0.2922 0.0921 0.0231 0.1099 0.514(3) Uiso R . P 1 2 .
H3412 H 0.9500 0.0555 0.6774 0.1068 0.514(3) Uiso R . P 1 2 .
H3413 H 0.8352 0.0412 0.6996 0.1068 0.514(3) Uiso R . P 1 2 .
H3414 H 0.8614 0.1164 0.6760 0.1068 0.514(3) Uiso R . P 1 2 .
H5411 H 0.5978 -0.3674 0.2829 0.1052 0.514(3) Uiso R . P 1 2 .
H5412 H 0.5807 -0.3532 0.3456 0.1052 0.514(3) Uiso R . P 1 2 .
H5413 H 0.4778 -0.3643 0.3012 0.1052 0.514(3) Uiso R . P 1 2 .
H7401 H 0.4715 0.1320 0.0083 0.1092 0.486(3) Uiso R . P 1 1 .
H7402 H 0.3584 0.1698 0.0150 0.1092 0.486(3) Uiso R . P 1 1 .
H7403 H 0.3684 0.0869 0.0210 0.1092 0.486(3) Uiso R . P 1 1 .
H3512 H 0.9619 0.0614 0.5735 0.1108 0.514(3) Uiso R . P 1 2 .
H3513 H 0.8740 0.1228 0.5671 0.1108 0.514(3) Uiso R . P 1 2 .
H3514 H 0.8562 0.0541 0.5303 0.1108 0.514(3) Uiso R . P 1 2 .
H1501 H 0.8571 0.3792 0.3222 0.1162 0.486(3) Uiso R . P 1 1 .
H1502 H 0.7726 0.3202 0.3358 0.1162 0.486(3) Uiso R . P 1 1 .
H1503 H 0.7379 0.3774 0.2897 0.1162 0.486(3) Uiso R . P 1 1 .
H1401 H 0.8393 0.5079 0.3495 0.1107 0.486(3) Uiso R . P 1 1 .
H1402 H 0.7398 0.5291 0.3826 0.1107 0.486(3) Uiso R . P 1 1 .
H1403 H 0.7189 0.5122 0.3185 0.1107 0.486(3) Uiso R . P 1 1 .
H7502 H 0.5728 0.0669 0.0900 0.1107 0.486(3) Uiso R . P 1 1 .
H7503 H 0.5340 0.0735 0.1500 0.1107 0.486(3) Uiso R . P 1 1 .
H7504 H 0.4753 0.0194 0.1068 0.1107 0.486(3) Uiso R . P 1 1 .
H5401 H 0.6881 -0.3511 0.2778 0.1050 0.486(3) Uiso R . P 1 1 .
H5402 H 0.6656 -0.3406 0.3403 0.1050 0.486(3) Uiso R . P 1 1 .
H5403 H 0.5671 -0.3575 0.2945 0.1050 0.486(3) Uiso R . P 1 1 .
H3501 H 1.0132 0.0990 0.5700 0.1134 0.486(3) Uiso R . P 1 1 .
H3502 H 0.9127 0.1505 0.5741 0.1134 0.486(3) Uiso R . P 1 1 .
H3503 H 0.9083 0.0937 0.5261 0.1134 0.486(3) Uiso R . P 1 1 .
H3402 H 1.0096 0.0543 0.6687 0.1032 0.486(3) Uiso R . P 1 1 .
H3403 H 0.9006 0.0215 0.6872 0.1032 0.486(3) Uiso R . P 1 1 .
H3404 H 0.9088 0.1038 0.6775 0.1032 0.486(3) Uiso R . P 1 1 .
H1411 H 0.7603 0.5338 0.3675 0.1054 0.514(3) Uiso R . P 1 2 .
H1412 H 0.6555 0.5413 0.4000 0.1054 0.514(3) Uiso R . P 1 2 .
H1413 H 0.6413 0.5332 0.3347 0.1054 0.514(3) Uiso R . P 1 2 .
H5501 H 0.7699 -0.2289 0.2690 0.1113 0.486(3) Uiso R . P 1 1 .
H5502 H 0.7519 -0.2125 0.3313 0.1113 0.486(3) Uiso R . P 1 1 .
H5503 H 0.7076 -0.1594 0.2838 0.1113 0.486(3) Uiso R . P 1 1 .
H1512 H 0.8036 0.4142 0.3277 0.1094 0.514(3) Uiso R . P 1 2 .
H1513 H 0.7297 0.3469 0.3344 0.1094 0.514(3) Uiso R . P 1 2 .
H1514 H 0.6871 0.4079 0.2930 0.1094 0.514(3) Uiso R . P 1 2 .
H5511 H 0.7003 -0.2517 0.2752 0.1103 0.514(3) Uiso R . P 1 2 .
H5512 H 0.6887 -0.2321 0.3376 0.1103 0.514(3) Uiso R . P 1 2 .
H5513 H 0.6513 -0.1777 0.2898 0.1103 0.514(3) Uiso R . P 1 2 .
H8151 H -0.0746 0.1413 -0.0081 0.2693 0.3791 Uiso R . . 1 6 .
H8152 H 0.0304 0.1413 0.0361 0.2693 0.3791 Uiso R . . 1 6 .
H8153 H 0.0443 0.1413 -0.0280 0.2693 0.3791 Uiso R . . 1 6 .
H8231 H 0.0269 0.0413 -0.0625 0.3693 0.6149 Uiso R . . 1 7 .
H8232 H 0.1140 0.0976 -0.0376 0.3693 0.6149 Uiso R . . 1 7 .
H8233 H -0.0040 0.0950 -0.0167 0.3693 0.6149 Uiso R . . 1 7 .
H8241 H 0.0527 -0.0091 0.0196 0.1823 0.6149 Uiso R . . 1 7 .
H8161 H -0.0396 0.0321 0.0251 0.1757 0.3791 Uiso R . . 1 6 .
H8191 H 1.0370 0.3442 0.4711 0.6066 0.4569 Uiso R . . 1 9 .
O828 O 1.0000 -0.2256 0.5000 0.2596 0.3000 Uiso D U . 1 5 .
C827 C 1.0036 -0.1259 0.5466 0.3504 0.5000 Uiso D U . 1 4 .
H8261 H 0.8449 -0.2523 0.4635 0.3792 0.3000 Uiso . . . 1 5 .
H8262 H 0.8388 -0.1816 0.4977 0.3792 0.3000 Uiso . . . 1 5 .
H8263 H 0.8941 -0.1816 0.4417 0.3792 0.3000 Uiso . . . 1 5 .
H8281 H 0.9899 -0.2396 0.5293 0.3792 0.3000 Uiso . . . 1 5 .
H8271 H 1.0129 -0.0686 0.5383 0.3827 0.5000 Uiso . . . 1 4 .
H8272 H 1.0614 -0.1372 0.5129 0.3827 0.5000 Uiso . . . 1 4 .
H8273 H 0.9463 -0.1402 0.5369 0.3827 0.5000 Uiso . . . 1 4 .
H8251 H 1.0609 -0.2029 0.6005 0.3828 0.5000 Uiso . . . 1 4 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.624(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C815 . H8152 3_555 0.950 no
C815 . H8151 3_555 0.950 no
C815 . H8153 3_555 0.950 no
C815 . O816 . 1.43000(10) yes
C815 . H8151 . 0.950 no
C815 . H8152 . 0.950 no
C815 . H8153 . 0.950 no
O816 . H8161 3_555 0.850 no
O816 . H8161 . 0.850 no
Cl820 . C819 . 1.7797(6) yes
N10 . C20 . 1.4700(10) yes
N10 . C50 . 1.3800(10) yes
N10 . C710 . 1.4000(10) yes
N11 . C21 . 1.4699(10) yes
N11 . C51 . 1.3800(10) yes
N11 . C711 . 1.3998(10) yes
C20 . C30 . 1.5000(10) yes
C20 . H201 . 0.950 no
C20 . H203 . 0.950 no
C21 . C31 . 1.5000(10) yes
C21 . H211 . 0.950 no
C21 . H212 . 0.950 no
C30 . N40 . 1.4700(10) yes
C30 . C130 . 1.5401(10) yes
C30 . H301 . 0.950 no
C31 . N41 . 1.4701(10) yes
C31 . C131 . 1.5400(10) yes
C31 . H311 . 0.950 no
N40 . C50 . 1.3801(10) yes
N40 . C70 . 1.4000(10) yes
N41 . C51 . 1.3801(10) yes
N41 . C71 . 1.4002(10) yes
C50 . O60 . 1.2000(10) yes
C51 . O61 . 1.20000(10) yes
C70 . N80 . 1.3416(9) yes
C70 . C120 . 1.4017(9) yes
C71 . N81 . 1.3402(10) yes
C71 . C121 . 1.4001(9) yes
N80 . C90 . 1.3394(9) yes
N81 . C91 . 1.3399(8) yes
C90 . N100 . 1.3381(9) yes
C90 . H901 . 0.950 no
C91 . N101 . 1.3397(8) yes
C91 . H911 . 0.950 no
N100 . C110 . 1.3384(9) yes
N101 . C111 . 1.3400(10) yes
C110 . C120 . 1.4000(9) yes
C110 . N210 . 1.3997(10) yes
C111 . C121 . 1.4000(9) yes
C111 . N211 . 1.3999(10) yes
C120 . H1201 . 0.950 no
C121 . H1211 . 0.950 no
N210 . C220 . 1.4700(10) yes
N210 . C250 . 1.3799(10) yes
N211 . C221 . 1.4699(10) yes
N211 . C251 . 1.3800(10) yes
C220 . C230 . 1.5000(10) yes
C220 . H2202 . 0.950 no
C220 . H2203 . 0.950 no
C221 . C231 . 1.5001(10) yes
C221 . H2211 . 0.950 no
C221 . H2212 . 0.950 no
C230 . N240 . 1.4700(10) yes
C230 . C330 . 1.5401(10) yes
C230 . H2301 . 0.950 no
C231 . N241 . 1.4700(10) yes
C231 . C331 . 1.5400(10) yes
C231 . H2311 . 0.950 no
N240 . C250 . 1.3799(10) yes
N240 . C270 . 1.4000(10) yes
N241 . C251 . 1.3799(10) yes
N241 . C271 . 1.4000(10) yes
C250 . O260 . 1.1999(10) yes
C251 . O261 . 1.20000(11) yes
C270 . N280 . 1.3413(9) yes
C270 . C320 . 1.4017(9) yes
C271 . N281 . 1.3414(9) yes
C271 . C321 . 1.4018(9) yes
N280 . C290 . 1.3393(9) yes
N281 . C291 . 1.3395(9) yes
C290 . N300 . 1.3380(9) yes
C290 . H2901 . 0.950 no
C291 . N301 . 1.3382(9) yes
C291 . H2911 . 0.950 no
N300 . C310 . 1.3385(9) yes
N301 . C311 . 1.3386(9) yes
C310 . C320 . 1.4004(9) yes
C310 . N410 . 1.3999(10) yes
C311 . C321 . 1.4004(9) yes
C311 . N411 . 1.4001(10) yes
C320 . H3201 . 0.950 no
C321 . H3212 . 0.950 no
N410 . C420 . 1.4699(10) yes
N410 . C450 . 1.3800(10) yes
N411 . C421 . 1.4700(10) yes
N411 . C451 . 1.3801(10) yes
C420 . C430 . 1.5001(10) yes
C420 . H4201 . 0.950 no
C420 . H4202 . 0.950 no
C421 . C431 . 1.5000(10) yes
C421 . H4211 . 0.950 no
C421 . H4212 . 0.950 no
C430 . N440 . 1.4700(10) yes
C430 . C530 . 1.5401(10) yes
C430 . H4301 . 0.950 no
C431 . N441 . 1.4699(10) yes
C431 . C531 . 1.5399(10) yes
C431 . H4311 . 0.950 no
N440 . C450 . 1.3800(10) yes
N440 . C470 . 1.4000(10) yes
N441 . C451 . 1.3799(10) yes
N441 . C471 . 1.3999(10) yes
C450 . O460 . 1.2000(10) yes
C451 . O461 . 1.20000(10) yes
C470 . N480 . 1.3413(9) yes
C470 . C520 . 1.4016(9) yes
C471 . N481 . 1.3413(9) yes
C471 . C521 . 1.4015(9) yes
N480 . C490 . 1.3394(9) yes
N481 . C491 . 1.3393(9) yes
C490 . N500 . 1.3383(9) yes
C490 . H4901 . 0.950 no
C491 . N501 . 1.3382(9) yes
C491 . H4911 . 0.950 no
N500 . C510 . 1.3386(9) yes
N501 . C511 . 1.3386(9) yes
C510 . C520 . 1.4001(9) yes
C510 . N610 . 1.3999(10) yes
C511 . C521 . 1.4000(9) yes
C511 . N611 . 1.3998(10) yes
C520 . H5202 . 0.950 no
C521 . H5211 . 0.950 no
N610 . C620 . 1.4699(10) yes
N610 . C650 . 1.3800(10) yes
N611 . C621 . 1.4700(10) yes
N611 . C651 . 1.3800(10) yes
C620 . C630 . 1.5001(10) yes
C620 . H6201 . 0.950 no
C620 . H6202 . 0.950 no
C621 . C631 . 1.5002(10) yes
C621 . H6211 . 0.950 no
C621 . H6212 . 0.950 no
C630 . N640 . 1.4700(10) yes
C630 . C730 . 1.5401(10) yes
C630 . H6301 . 0.950 no
C631 . N641 . 1.4699(10) yes
C631 . C731 . 1.5402(10) yes
C631 . H6311 . 0.950 no
N640 . C650 . 1.3801(10) yes
N640 . C670 . 1.4000(10) yes
N641 . C651 . 1.3800(10) yes
N641 . C671 . 1.4000(10) yes
C650 . O660 . 1.2000(10) yes
C651 . O661 . 1.20000(10) yes
C670 . N680 . 1.3399(10) yes
C670 . C720 . 1.4002(9) yes
C671 . N681 . 1.3400(10) yes
C671 . C721 . 1.4002(9) yes
N680 . C690 . 1.3398(8) yes
N681 . C691 . 1.3398(8) yes
C690 . N700 . 1.3398(8) yes
C690 . H6901 . 0.950 no
C691 . N701 . 1.3398(8) yes
C691 . H6912 . 0.950 no
N700 . C710 . 1.3399(10) yes
N701 . C711 . 1.3399(10) yes
C710 . C720 . 1.4000(9) yes
C711 . C721 . 1.4000(9) yes
C720 . H7201 . 0.950 no
C721 . H7211 . 0.950 no
C330 . C350 . 1.5400(8) yes
C330 . C340 . 1.5399(8) yes
C330 . H3301 . 0.950 no
C331 . C341 . 1.5400(8) yes
C331 . C351 . 1.5400(8) yes
C331 . H3311 . 0.950 no
C530 . C540 . 1.5400(8) yes
C530 . C550 . 1.5400(8) yes
C530 . H5301 . 0.950 no
C531 . C541 . 1.5400(8) yes
C531 . C551 . 1.5400(8) yes
C531 . H5311 . 0.950 no
C730 . C740 . 1.5400(8) yes
C730 . C750 . 1.5401(8) yes
C730 . H7301 . 0.950 no
C731 . C751 . 1.5400(8) yes
C731 . C741 . 1.5399(8) yes
C731 . H7311 . 0.950 no
C130 . C150 . 1.5400(8) yes
C130 . C140 . 1.5400(8) yes
C130 . H1302 . 0.950 no
C131 . C141 . 1.5399(8) yes
C131 . C151 . 1.5399(8) yes
C131 . H1311 . 0.950 no
Cl804 . C801 . 1.7797(8) yes
Cl803 . C801 . 1.7797(8) yes
Cl802 . C801 . 1.7798(8) yes
C801 . H8011 . 0.950 no
C751 . H7511 . 0.950 no
C751 . H7512 . 0.950 no
C751 . H7513 . 0.950 no
C741 . H7411 . 0.950 no
C741 . H7412 . 0.950 no
C741 . H7413 . 0.950 no
C341 . H3412 . 0.950 no
C341 . H3413 . 0.950 no
C341 . H3414 . 0.950 no
C541 . H5411 . 0.950 no
C541 . H5412 . 0.950 no
C541 . H5413 . 0.950 no
C740 . H7401 . 0.950 no
C740 . H7402 . 0.950 no
C740 . H7403 . 0.950 no
C351 . H3512 . 0.950 no
C351 . H3513 . 0.950 no
C351 . H3514 . 0.950 no
C150 . H1501 . 0.950 no
C150 . H1502 . 0.950 no
C150 . H1503 . 0.950 no
C140 . H1401 . 0.950 no
C140 . H1402 . 0.950 no
C140 . H1403 . 0.950 no
C750 . H7502 . 0.950 no
C750 . H7503 . 0.950 no
C750 . H7504 . 0.950 no
C540 . H5401 . 0.950 no
C540 . H5402 . 0.950 no
C540 . H5403 . 0.950 no
C350 . H3501 . 0.950 no
C350 . H3502 . 0.950 no
C350 . H3503 . 0.950 no
C340 . H3402 . 0.950 no
C340 . H3403 . 0.950 no
C340 . H3404 . 0.950 no
C141 . H1411 . 0.950 no
C141 . H1412 . 0.950 no
C141 . H1413 . 0.950 no
C550 . H5501 . 0.950 no
C550 . H5502 . 0.950 no
C550 . H5503 . 0.950 no
C151 . H1512 . 0.950 no
C151 . H1513 . 0.950 no
C151 . H1514 . 0.950 no
C551 . H5511 . 0.950 no
C551 . H5512 . 0.950 no
C551 . H5513 . 0.950 no
O824 . C823 . 1.43000(11) yes
O824 . H8241 . 0.850 no
C823 . H8231 . 0.950 no
C823 . H8232 . 0.950 no
C823 . H8233 . 0.950 no
C826 . O828 . 1.431 yes
C826 . H8261 . 1.086 no
C826 . H8262 . 0.953 no
C826 . H8263 . 0.908 no
O825 . C827 . 1.43034(5) yes
O825 . H8251 . 1.026 no
C819 . Cl821 3_756 1.7797(9) yes
C819 . H8191 3_756 0.951 no
C819 . Cl821 . 1.7797(8) yes
C819 . H8191 . 0.951 no
Cl821 . Cl821 3_756 2.187(8) yes
Cl821 . H8191 3_756 1.022 no
O828 . H8281 3_756 0.765 no
O828 . H8281 . 0.765 no
C827 . H8271 . 1.092 no
C827 . H8272 . 1.135 no
C827 . H8273 . 0.750 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
H8152 3_555 C815 . H8151 3_555 109.5 no
H8152 3_555 C815 . H8153 3_555 109.5 no
H8151 3_555 C815 . H8153 3_555 109.5 no
H8152 3_555 C815 . O816 . 109.5 no
H8151 3_555 C815 . O816 . 109.5 no
H8153 3_555 C815 . O816 . 109.5 no
H8152 3_555 C815 . H8151 . 56.3 no
H8151 3_555 C815 . H8151 . 141.1 no
H8153 3_555 C815 . H8151 . 56.3 no
O816 . C815 . H8151 . 109.5 no
H8152 3_555 C815 . H8152 . 141.1 no
H8151 3_555 C815 . H8152 . 56.3 no
H8153 3_555 C815 . H8152 . 56.3 no
O816 . C815 . H8152 . 109.5 no
H8151 . C815 . H8152 . 109.5 no
H8152 3_555 C815 . H8153 . 56.3 no
H8151 3_555 C815 . H8153 . 56.3 no
H8153 3_555 C815 . H8153 . 141.1 no
O816 . C815 . H8153 . 109.5 no
H8151 . C815 . H8153 . 109.5 no
H8152 . C815 . H8153 . 109.5 no
C815 . O816 . H8161 3_555 109.5 no
C815 . O816 . H8161 . 109.5 no
H8161 3_555 O816 . H8161 . 141.1 no
C20 . N10 . C50 . 114.3(7) yes
C20 . N10 . C710 . 122.3(9) yes
C50 . N10 . C710 . 123.0(9) yes
C21 . N11 . C51 . 110.7(8) yes
C21 . N11 . C711 . 120.5(9) yes
C51 . N11 . C711 . 124.8(9) yes
N10 . C20 . C30 . 101.4(9) yes
N10 . C20 . H201 . 113.2 no
C30 . C20 . H201 . 114.3 no
N10 . C20 . H203 . 109.4 no
C30 . C20 . H203 . 108.7 no
H201 . C20 . H203 . 109.5 no
N11 . C21 . C31 . 104.6(9) yes
N11 . C21 . H211 . 110.3 no
C31 . C21 . H211 . 111.3 no
N11 . C21 . H212 . 110.5 no
C31 . C21 . H212 . 110.7 no
H211 . C21 . H212 . 109.5 no
C20 . C30 . N40 . 106.5(9) yes
C20 . C30 . C130 . 106.5(14) yes
N40 . C30 . C130 . 105.4(10) yes
C20 . C30 . H301 . 113.2 no
N40 . C30 . H301 . 111.4 no
C130 . C30 . H301 . 113.3 no
C21 . C31 . N41 . 103.1(9) yes
C21 . C31 . C131 . 112.3(13) yes
N41 . C31 . C131 . 111.3(9) yes
C21 . C31 . H311 . 109.8 no
N41 . C31 . H311 . 108.5 no
C131 . C31 . H311 . 111.5 no
C30 . N40 . C50 . 110.7(8) yes
C30 . N40 . C70 . 123.9(10) yes
C50 . N40 . C70 . 125.5(10) yes
C31 . N41 . C51 . 111.9(8) yes
C31 . N41 . C71 . 125.4(10) yes
C51 . N41 . C71 . 122.5(9) yes
N40 . C50 . N10 . 106.3(6) yes
N40 . C50 . O60 . 125.8(11) yes
N10 . C50 . O60 . 127.9(10) yes
N41 . C51 . N11 . 107.7(7) yes
N41 . C51 . O61 . 126.2(10) yes
N11 . C51 . O61 . 126.1(10) yes
N40 . C70 . N80 . 117.7(8) yes
N40 . C70 . C120 . 118.6(8) yes
N80 . C70 . C120 . 123.003(7) yes
N41 . C71 . N81 . 113.9(8) yes
N41 . C71 . C121 . 122.6(8) yes
N81 . C71 . C121 . 123.49(4) yes
C70 . N80 . C90 . 115.003(10) yes
C71 . N81 . C91 . 115.000(10) yes
N80 . C90 . N100 . 127.999(10) yes
N80 . C90 . H901 . 116.0 no
N100 . C90 . H901 . 116.0 no
N81 . C91 . N101 . 128.000(10) yes
N81 . C91 . H911 . 116.3 no
N101 . C91 . H911 . 115.7 no
C90 . N100 . C110 . 114.997(10) yes
C91 . N101 . C111 . 115.000(10) yes
N100 . C110 . C120 . 123.48(6) yes
N100 . C110 . N210 . 113.8(8) yes
C120 . C110 . N210 . 121.8(9) yes
N101 . C111 . C121 . 123.51(4) yes
N101 . C111 . N211 . 117.8(8) yes
C121 . C111 . N211 . 118.7(8) yes
C70 . C120 . C110 . 115.005(10) yes
C70 . C120 . H1201 . 122.5 no
C110 . C120 . H1201 . 122.4 no
C71 . C121 . C111 . 115.000(10) yes
C71 . C121 . H1211 . 122.1 no
C111 . C121 . H1211 . 122.9 no
C110 . N210 . C220 . 124.5(11) yes
C110 . N210 . C250 . 121.6(10) yes
C220 . N210 . C250 . 111.7(9) yes
C111 . N211 . C221 . 123.4(10) yes
C111 . N211 . C251 . 128.3(10) yes
C221 . N211 . C251 . 107.7(8) yes
N210 . C220 . C230 . 102.9(11) yes
N210 . C220 . H2202 . 111.4 no
C230 . C220 . H2202 . 111.6 no
N210 . C220 . H2203 . 110.8 no
C230 . C220 . H2203 . 110.6 no
H2202 . C220 . H2203 . 109.5 no
N211 . C221 . C231 . 106.0(11) yes
N211 . C221 . H2211 . 111.2 no
C231 . C221 . H2211 . 110.8 no
N211 . C221 . H2212 . 109.8 no
C231 . C221 . H2212 . 109.4 no
H2211 . C221 . H2212 . 109.5 no
C220 . C230 . N240 . 99.9(10) yes
C220 . C230 . C330 . 108.6(13) yes
N240 . C230 . C330 . 118.5(10) yes
C220 . C230 . H2301 . 110.1 no
N240 . C230 . H2301 . 109.7 no
C330 . C230 . H2301 . 109.4 no
C221 . C231 . N241 . 101.7(10) yes
C221 . C231 . C331 . 113.6(13) yes
N241 . C231 . C331 . 111.8(9) yes
C221 . C231 . H2311 . 110.2 no
N241 . C231 . H2311 . 110.3 no
C331 . C231 . H2311 . 109.0 no
C230 . N240 . C250 . 112.8(9) yes
C230 . N240 . C270 . 116.3(10) yes
C250 . N240 . C270 . 123.4(9) yes
C231 . N241 . C251 . 111.6(8) yes
C231 . N241 . C271 . 125.3(10) yes
C251 . N241 . C271 . 122.8(9) yes
N240 . C250 . N210 . 104.6(5) yes
N240 . C250 . O260 . 122.4(12) yes
N210 . C250 . O260 . 133.0(12) yes
N211 . C251 . N241 . 109.0(5) yes
N211 . C251 . O261 . 125.7(11) yes
N241 . C251 . O261 . 125.3(11) yes
N240 . C270 . N280 . 117.6(8) yes
N240 . C270 . C320 . 115.0(7) yes
N280 . C270 . C320 . 123.006(10) yes
N241 . C271 . N281 . 113.2(8) yes
N241 . C271 . C321 . 122.3(8) yes
N281 . C271 . C321 . 123.006(10) yes
C270 . N280 . C290 . 115.003(10) yes
C271 . N281 . C291 . 115.003(10) yes
N280 . C290 . N300 . 127.998(10) yes
N280 . C290 . H2901 . 115.8 no
N300 . C290 . H2901 . 116.2 no
N281 . C291 . N301 . 127.999(10) yes
N281 . C291 . H2911 . 116.5 no
N301 . C291 . H2911 . 115.5 no
C290 . N300 . C310 . 114.997(10) yes
C291 . N301 . C311 . 114.997(10) yes
N300 . C310 . C320 . 123.43(7) yes
N300 . C310 . N410 . 111.8(8) yes
C320 . C310 . N410 . 124.6(8) yes
N301 . C311 . C321 . 123.38(8) yes
N301 . C311 . N411 . 116.1(8) yes
C321 . C311 . N411 . 119.9(8) yes
C270 . C320 . C310 . 115.005(10) yes
C270 . C320 . H3201 . 122.6 no
C310 . C320 . H3201 . 122.4 no
C271 . C321 . C311 . 115.005(10) yes
C271 . C321 . H3212 . 122.0 no
C311 . C321 . H3212 . 123.0 no
C310 . N410 . C420 . 123.0(9) yes
C310 . N410 . C450 . 124.2(10) yes
C420 . N410 . C450 . 112.8(7) yes
C311 . N411 . C421 . 121.0(9) yes
C311 . N411 . C451 . 125.5(9) yes
C421 . N411 . C451 . 112.8(8) yes
N410 . C420 . C430 . 102.1(9) yes
N410 . C420 . H4201 . 110.7 no
C430 . C420 . H4201 . 112.3 no
N410 . C420 . H4202 . 111.2 no
C430 . C420 . H4202 . 111.0 no
H4201 . C420 . H4202 . 109.5 no
N411 . C421 . C431 . 104.1(9) yes
N411 . C421 . H4211 . 110.8 no
C431 . C421 . H4211 . 111.5 no
N411 . C421 . H4212 . 110.9 no
C431 . C421 . H4212 . 110.1 no
H4211 . C421 . H4212 . 109.5 no
C420 . C430 . N440 . 105.5(9) yes
C420 . C430 . C530 . 113.1(14) yes
N440 . C430 . C530 . 114.9(10) yes
C420 . C430 . H4301 . 108.4 no
N440 . C430 . H4301 . 106.4 no
C530 . C430 . H4301 . 108.2 no
C421 . C431 . N441 . 102.6(8) yes
C421 . C431 . C531 . 110.0(13) yes
N441 . C431 . C531 . 115.3(10) yes
C421 . C431 . H4311 . 109.9 no
N441 . C431 . H4311 . 108.3 no
C531 . C431 . H4311 . 110.5 no
C430 . N440 . C450 . 109.8(8) yes
C430 . N440 . C470 . 123.9(10) yes
C450 . N440 . C470 . 125.8(9) yes
C431 . N441 . C451 . 113.9(7) yes
C431 . N441 . C471 . 120.9(9) yes
C451 . N441 . C471 . 125.0(9) yes
N410 . C450 . N440 . 107.4(6) yes
N410 . C450 . O460 . 128.6(10) yes
N440 . C450 . O460 . 124.0(10) yes
N411 . C451 . N441 . 105.4(6) yes
N411 . C451 . O461 . 128.2(10) yes
N441 . C451 . O461 . 126.4(10) yes
N440 . C470 . N480 . 116.1(8) yes
N440 . C470 . C520 . 120.0(8) yes
N480 . C470 . C520 . 123.003(7) yes
N441 . C471 . N481 . 117.4(8) yes
N441 . C471 . C521 . 119.6(8) yes
N481 . C471 . C521 . 123.003(7) yes
C470 . N480 . C490 . 115.003(10) yes
C471 . N481 . C491 . 115.003(10) yes
N480 . C490 . N500 . 127.998(10) yes
N480 . C490 . H4901 . 116.7 no
N500 . C490 . H4901 . 115.3 no
N481 . C491 . N501 . 127.999(10) yes
N481 . C491 . H4911 . 115.9 no
N501 . C491 . H4911 . 116.1 no
C490 . N500 . C510 . 114.997(10) yes
C491 . N501 . C511 . 114.997(10) yes
N500 . C510 . C520 . 123.42(7) yes
N500 . C510 . N610 . 116.4(8) yes
C520 . C510 . N610 . 119.9(8) yes
N501 . C511 . C521 . 123.39(8) yes
N501 . C511 . N611 . 112.0(8) yes
C521 . C511 . N611 . 124.2(8) yes
C470 . C520 . C510 . 115.004(10) yes
C470 . C520 . H5202 . 121.8 no
C510 . C520 . H5202 . 123.1 no
C471 . C521 . C511 . 115.004(10) yes
C471 . C521 . H5211 . 122.6 no
C511 . C521 . H5211 . 122.4 no
C510 . N610 . C620 . 121.5(10) yes
C510 . N610 . C650 . 125.8(9) yes
C620 . N610 . C650 . 112.6(9) yes
C511 . N611 . C621 . 130.0(10) yes
C511 . N611 . C651 . 121.5(9) yes
C621 . N611 . C651 . 108.2(9) yes
N610 . C620 . C630 . 101.3(10) yes
N610 . C620 . H6201 . 111.4 no
C630 . C620 . H6201 . 108.8 no
N610 . C620 . H6202 . 111.0 no
C630 . C620 . H6202 . 114.7 no
H6201 . C620 . H6202 . 109.5 no
N611 . C621 . C631 . 105.9(10) yes
N611 . C621 . H6211 . 109.1 no
C631 . C621 . H6211 . 111.1 no
N611 . C621 . H6212 . 111.5 no
C631 . C621 . H6212 . 109.7 no
H6211 . C621 . H6212 . 109.5 no
C620 . C630 . N640 . 101.4(11) yes
C620 . C630 . C730 . 112.7(15) yes
N640 . C630 . C730 . 110.6(10) yes
C620 . C630 . H6301 . 108.8 no
N640 . C630 . H6301 . 110.2 no
C730 . C630 . H6301 . 112.5 no
C621 . C631 . N641 . 101.5(11) yes
C621 . C631 . C731 . 110.0(15) yes
N641 . C631 . C731 . 110.6(10) yes
C621 . C631 . H6311 . 110.1 no
N641 . C631 . H6311 . 110.0 no
C731 . C631 . H6311 . 114.0 no
C630 . N640 . C650 . 113.0(8) yes
C630 . N640 . C670 . 125.8(10) yes
C650 . N640 . C670 . 120.6(9) yes
C631 . N641 . C651 . 111.9(8) yes
C631 . N641 . C671 . 119.5(10) yes
C651 . N641 . C671 . 128.4(9) yes
N640 . C650 . N610 . 104.1(5) yes
N640 . C650 . O660 . 124.7(11) yes
N610 . C650 . O660 . 131.2(12) yes
N641 . C651 . N611 . 108.7(5) yes
N641 . C651 . O661 . 122.5(12) yes
N611 . C651 . O661 . 128.8(11) yes
N640 . C670 . N680 . 115.6(7) yes
N640 . C670 . C720 . 120.7(7) yes
N680 . C670 . C720 . 123.50(4) yes
N641 . C671 . N681 . 117.7(8) yes
N641 . C671 . C721 . 118.8(8) yes
N681 . C671 . C721 . 123.49(4) yes
C670 . N680 . C690 . 114.999(10) yes
C671 . N681 . C691 . 115.000(10) yes
N680 . C690 . N700 . 127.999(10) yes
N680 . C690 . H6901 . 116.3 no
N700 . C690 . H6901 . 115.7 no
N681 . C691 . N701 . 127.999(10) yes
N681 . C691 . H6912 . 116.5 no
N701 . C691 . H6912 . 115.5 no
C690 . N700 . C710 . 114.999(10) yes
C691 . N701 . C711 . 114.999(10) yes
N10 . C710 . N700 . 111.3(8) yes
N10 . C710 . C720 . 124.4(8) yes
N700 . C710 . C720 . 123.50(4) yes
N11 . C711 . N701 . 114.8(8) yes
N11 . C711 . C721 . 121.6(8) yes
N701 . C711 . C721 . 123.50(4) yes
C670 . C720 . C710 . 115.000(10) yes
C670 . C720 . H7201 . 122.2 no
C710 . C720 . H7201 . 122.8 no
C671 . C721 . C711 . 115.000(10) yes
C671 . C721 . H7211 . 122.0 no
C711 . C721 . H7211 . 123.0 no
C230 . C330 . C350 . 110.98(9) yes
C230 . C330 . C340 . 110.99(9) yes
C350 . C330 . C340 . 111.000(10) yes
C230 . C330 . H3301 . 108.9 no
C350 . C330 . H3301 . 108.0 no
C340 . C330 . H3301 . 106.8 no
C231 . C331 . C341 . 111.00(9) yes
C231 . C331 . C351 . 111.00(9) yes
C341 . C331 . C351 . 111.000(10) yes
C231 . C331 . H3311 . 107.0 no
C341 . C331 . H3311 . 110.1 no
C351 . C331 . H3311 . 106.6 no
C430 . C530 . C540 . 110.99(9) yes
C430 . C530 . C550 . 110.99(9) yes
C540 . C530 . C550 . 111.000(10) yes
C430 . C530 . H5301 . 108.7 no
C540 . C530 . H5301 . 110.8 no
C550 . C530 . H5301 . 104.2 no
C431 . C531 . C541 . 111.00(9) yes
C431 . C531 . C551 . 111.00(9) yes
C541 . C531 . C551 . 111.000(10) yes
C431 . C531 . H5311 . 107.1 no
C541 . C531 . H5311 . 110.0 no
C551 . C531 . H5311 . 106.6 no
C630 . C730 . C740 . 110.99(9) yes
C630 . C730 . C750 . 110.97(9) yes
C740 . C730 . C750 . 111.000(10) yes
C630 . C730 . H7301 . 109.6 no
C740 . C730 . H7301 . 100.1 no
C750 . C730 . H7301 . 113.7 no
C631 . C731 . C751 . 110.98(9) yes
C631 . C731 . C741 . 110.98(9) yes
C751 . C731 . C741 . 111.000(10) yes
C631 . C731 . H7311 . 104.2 no
C751 . C731 . H7311 . 115.6 no
C741 . C731 . H7311 . 103.7 no
C30 . C130 . C150 . 110.98(9) yes
C30 . C130 . C140 . 110.99(9) yes
C150 . C130 . C140 . 111.000(10) yes
C30 . C130 . H1302 . 107.5 no
C150 . C130 . H1302 . 107.2 no
C140 . C130 . H1302 . 109.0 no
C31 . C131 . C141 . 111.00(9) yes
C31 . C131 . C151 . 111.00(9) yes
C141 . C131 . C151 . 111.000(10) yes
C31 . C131 . H1311 . 105.4 no
C141 . C131 . H1311 . 109.2 no
C151 . C131 . H1311 . 109.1 no
Cl802 . C801 . Cl804 . 115.05(6) yes
Cl802 . C801 . Cl803 . 115.04(6) yes
Cl804 . C801 . Cl803 . 115.04(6) yes
Cl802 . C801 . H8011 . 102.3 no
Cl804 . C801 . H8011 . 104.0 no
Cl803 . C801 . H8011 . 102.9 no
C731 . C751 . H7511 . 103.8 no
C731 . C751 . H7512 . 107.0 no
H7511 . C751 . H7512 . 109.5 no
C731 . C751 . H7513 . 117.3 no
H7511 . C751 . H7513 . 109.5 no
H7512 . C751 . H7513 . 109.5 no
C731 . C741 . H7411 . 112.0 no
C731 . C741 . H7412 . 111.1 no
H7411 . C741 . H7412 . 109.5 no
C731 . C741 . H7413 . 105.2 no
H7411 . C741 . H7413 . 109.5 no
H7412 . C741 . H7413 . 109.5 no
C331 . C341 . H3412 . 109.3 no
C331 . C341 . H3413 . 107.5 no
H3412 . C341 . H3413 . 109.5 no
C331 . C341 . H3414 . 111.6 no
H3412 . C341 . H3414 . 109.5 no
H3413 . C341 . H3414 . 109.5 no
C531 . C541 . H5411 . 110.6 no
C531 . C541 . H5412 . 111.5 no
H5411 . C541 . H5412 . 109.5 no
C531 . C541 . H5413 . 106.3 no
H5411 . C541 . H5413 . 109.5 no
H5412 . C541 . H5413 . 109.5 no
C730 . C740 . H7401 . 113.2 no
C730 . C740 . H7402 . 113.3 no
H7401 . C740 . H7402 . 109.5 no
C730 . C740 . H7403 . 101.6 no
H7401 . C740 . H7403 . 109.5 no
H7402 . C740 . H7403 . 109.5 no
C331 . C351 . H3512 . 108.8 no
C331 . C351 . H3513 . 108.2 no
H3512 . C351 . H3513 . 109.5 no
C331 . C351 . H3514 . 111.4 no
H3512 . C351 . H3514 . 109.5 no
H3513 . C351 . H3514 . 109.5 no
C130 . C150 . H1501 . 107.4 no
C130 . C150 . H1502 . 112.1 no
H1501 . C150 . H1502 . 109.5 no
C130 . C150 . H1503 . 108.9 no
H1501 . C150 . H1503 . 109.5 no
H1502 . C150 . H1503 . 109.5 no
C130 . C140 . H1401 . 111.1 no
C130 . C140 . H1402 . 106.8 no
H1401 . C140 . H1402 . 109.5 no
C130 . C140 . H1403 . 110.5 no
H1401 . C140 . H1403 . 109.5 no
H1402 . C140 . H1403 . 109.5 no
C730 . C750 . H7502 . 107.8 no
C730 . C750 . H7503 . 105.2 no
H7502 . C750 . H7503 . 109.5 no
C730 . C750 . H7504 . 115.3 no
H7502 . C750 . H7504 . 109.5 no
H7503 . C750 . H7504 . 109.5 no
C530 . C540 . H5401 . 110.2 no
C530 . C540 . H5402 . 112.3 no
H5401 . C540 . H5402 . 109.5 no
C530 . C540 . H5403 . 105.8 no
H5401 . C540 . H5403 . 109.5 no
H5402 . C540 . H5403 . 109.5 no
C330 . C350 . H3501 . 109.2 no
C330 . C350 . H3502 . 109.5 no
H3501 . C350 . H3502 . 109.5 no
C330 . C350 . H3503 . 109.6 no
H3501 . C350 . H3503 . 109.5 no
H3502 . C350 . H3503 . 109.5 no
C330 . C340 . H3402 . 110.7 no
C330 . C340 . H3403 . 109.4 no
H3402 . C340 . H3403 . 109.5 no
C330 . C340 . H3404 . 108.4 no
H3402 . C340 . H3404 . 109.5 no
H3403 . C340 . H3404 . 109.5 no
C131 . C141 . H1411 . 109.7 no
C131 . C141 . H1412 . 108.0 no
H1411 . C141 . H1412 . 109.5 no
C131 . C141 . H1413 . 110.7 no
H1411 . C141 . H1413 . 109.5 no
H1412 . C141 . H1413 . 109.5 no
C530 . C550 . H5501 . 109.4 no
C530 . C550 . H5502 . 105.8 no
H5501 . C550 . H5502 . 109.5 no
C530 . C550 . H5503 . 113.1 no
H5501 . C550 . H5503 . 109.5 no
H5502 . C550 . H5503 . 109.5 no
C131 . C151 . H1512 . 106.8 no
C131 . C151 . H1513 . 110.8 no
H1512 . C151 . H1513 . 109.5 no
C131 . C151 . H1514 . 110.8 no
H1512 . C151 . H1514 . 109.5 no
H1513 . C151 . H1514 . 109.5 no
C531 . C551 . H5511 . 107.5 no
C531 . C551 . H5512 . 108.2 no
H5511 . C551 . H5512 . 109.5 no
C531 . C551 . H5513 . 112.6 no
H5511 . C551 . H5513 . 109.5 no
H5512 . C551 . H5513 . 109.5 no
C823 . O824 . H8241 . 104.1 no
O824 . C823 . H8231 . 110.1 no
O824 . C823 . H8232 . 104.1 no
H8231 . C823 . H8232 . 109.5 no
O824 . C823 . H8233 . 114.1 no
H8231 . C823 . H8233 . 109.5 no
H8232 . C823 . H8233 . 109.5 no
O828 . C826 . H8261 . 106.6 no
O828 . C826 . H8262 . 121.8 no
H8261 . C826 . H8262 . 98.9 no
O828 . C826 . H8263 . 111.6 no
H8261 . C826 . H8263 . 101.8 no
H8262 . C826 . H8263 . 112.9 no
C827 . O825 . H8251 . 107.5 no
Cl820 3_756 C819 . Cl820 . 115.06(6) yes
Cl820 3_756 C819 . Cl821 3_756 115.07(6) yes
Cl820 . C819 . Cl821 3_756 115.06(6) yes
Cl820 3_756 C819 . H8191 3_756 103.6 no
Cl820 . C819 . H8191 3_756 103.2 no
Cl821 3_756 C819 . H8191 3_756 102.4 no
Cl820 3_756 C819 . Cl821 . 115.06(6) yes
Cl820 . C819 . Cl821 . 115.07(6) yes
Cl821 3_756 C819 . Cl821 . 75.8(3) yes
H8191 3_756 C819 . Cl821 . 26.6 no
Cl820 3_756 C819 . H8191 . 103.2 no
Cl820 . C819 . H8191 . 103.6 no
Cl821 3_756 C819 . H8191 . 26.6 no
H8191 3_756 C819 . H8191 . 128.9 no
Cl821 . C819 . H8191 . 102.4 no
Cl821 3_756 Cl821 . C819 . 52.09(16) yes
Cl821 3_756 Cl821 . H8191 3_756 76.7 no
C819 . Cl821 . H8191 3_756 24.6 no
C819 . H8191 . Cl821 3_756 128.9 no
C826 . O828 . C826 3_756 146.57 yes
C826 . O828 . H8281 3_756 87.5 no
C826 3_756 O828 . H8281 3_756 103.8 no
C826 . O828 . H8281 . 103.8 no
C826 3_756 O828 . H8281 . 87.5 no
H8281 3_756 O828 . H8281 . 140.4 no
O825 . C827 . H8271 . 113.2 no
O825 . C827 . H8272 . 109.4 no
H8271 . C827 . H8272 . 88.3 no
O825 . C827 . H8273 . 119.0 no
H8271 . C827 . H8273 . 113.5 no
H8272 . C827 . H8273 . 109.0 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C21 . H212 . N501 4_555 145 0.95 2.08 2.915(18) yes
C31 . H301 . C141 . 121 0.78 2.05 2.538(18) yes
C90 . H901 . N500 2_555 149 0.95 2.49 3.337(18) yes
C91 . H901 . N500 2_555 148 1.20 2.49 3.560(18) yes
C90 . H901 . N501 2_555 148 0.95 2.50 3.337(18) yes
C91 . H901 . N501 2_555 130 1.20 2.50 3.396(18) yes
C90 . H911 . N501 2_555 125 1.12 2.56 3.337(18) yes
C91 . H911 . N501 2_555 146 0.95 2.56 3.396(18) yes
C120 . H1201 . O60 . 124 0.95 2.05 2.701(18) yes
C120 . H1201 . O61 . 124 0.95 2.21 2.846(18) yes
C120 . H1201 . O260 . 121 0.95 2.19 2.807(18) yes
C121 . H1201 . O260 . 122 1.02 2.19 2.870(18) yes
C120 . H1201 . O261 . 122 0.95 2.29 2.911(18) yes
C120 . H1211 . O61 . 121 1.11 2.11 2.846(18) yes
C121 . H1211 . O60 . 121 0.95 2.09 2.709(18) yes
C121 . H1211 . O61 . 121 0.95 2.11 2.717(18) yes
C121 . H1211 . O260 . 122 0.95 2.25 2.870(18) yes
C120 . H1211 . O261 . 122 1.11 2.17 2.911(18) yes
C121 . H1211 . O261 . 122 0.95 2.17 2.792(18) yes
C221 . H2212 . O61 3_656 135 0.95 2.13 2.884(18) yes
C231 . H2311 . O461 3_656 140 0.95 2.16 2.956(18) yes
C290 . H2901 . N680 2_545 149 0.95 2.57 3.418(18) yes
C291 . H2901 . N680 2_545 138 1.19 2.57 3.544(18) yes
C290 . H2901 . N681 2_545 145 0.95 2.53 3.350(18) yes
C291 . H2901 . N681 2_545 124 1.19 2.53 3.345(18) yes
C290 . H2911 . N681 2_545 130 1.14 2.50 3.350(18) yes
C291 . H2911 . N681 2_545 148 0.95 2.50 3.345(18) yes
C320 . H3201 . O260 . 124 0.95 1.92 2.573(18) yes
C321 . H3201 . O260 . 131 1.10 1.92 2.765(18) yes
C320 . H3201 . O261 . 125 0.95 2.06 2.719(18) yes
C321 . H3212 . O261 . 122 0.95 2.07 2.690(18) yes
C321 . H3212 . O460 . 121 0.95 2.14 2.752(18) yes
C320 . H3212 . O461 . 128 1.19 2.14 3.029(18) yes
C321 . H3212 . O461 . 123 0.95 2.14 2.776(18) yes
C431 . H4311 . C671 4_545 156 0.95 2.58 3.473(18) yes
C431 . H4311 . N681 4_545 136 0.95 1.99 2.762(18) yes
C490 . H4901 . N100 2_444 149 0.95 2.54 3.386(18) yes
C491 . H4911 . N100 2_444 141 0.95 2.51 3.302(18) yes
C491 . H4911 . N101 2_444 146 0.95 2.52 3.354(18) yes
C520 . H5202 . O460 . 124 0.95 2.06 2.703(18) yes
C520 . H5202 . O461 . 120 0.95 2.02 2.626(18) yes
C521 . H5202 . O460 . 125 1.20 2.06 2.919(18) yes
C520 . H5202 . O660 . 121 0.95 2.26 2.870(18) yes
C521 . H5211 . O460 . 126 0.95 2.26 2.919(18) yes
C521 . H5211 . O461 . 122 0.95 2.09 2.714(18) yes
C520 . H5211 . O661 . 129 0.88 2.29 2.927(18) yes
C520 . H5211 . O660 . 128 0.88 2.24 2.870(18) yes
C521 . H5211 . O660 . 126 0.95 2.24 2.897(18) yes
C631 . H6301 . C741 . 138 0.75 1.93 2.538(18) yes
C690 . H6901 . N280 2_454 147 0.95 2.57 3.407(18) yes
C691 . H6901 . N280 2_454 129 1.04 2.57 3.318(18) yes
C691 . H6912 . N280 2_454 141 0.95 2.52 3.318(18) yes
C691 . H6912 . N281 2_454 146 0.95 2.55 3.375(18) yes
C720 . H7211 . O661 . 133 1.04 2.19 3.002(18) yes
C721 . H7211 . O60 . 121 0.95 2.46 3.056(18) yes
C720 . H7211 . O660 . 125 1.04 1.90 2.643(18) yes
C721 . H7211 . O660 . 128 0.95 1.90 2.594(18) yes
C331 . H3311 . N280 . 127 0.95 2.11 2.793(18) yes
C530 . H5301 . N480 . 121 0.95 2.48 3.076(18) yes
C531 . H5311 . N480 . 127 0.95 2.00 2.681(18) yes
C531 . H5311 . N481 . 121 0.95 2.50 3.097(18) yes
C731 . H7311 . N680 . 128 0.95 2.33 3.016(18) yes
C130 . H1311 . N80 . 149 1.06 2.35 3.299(18) yes
C131 . H1311 . N80 . 131 0.95 2.35 3.052(18) yes
C801 . H8011 . O260 . 134 0.95 2.37 3.109(18) yes
C750 . H7511 . C740 . 139 0.87 1.82 2.538(18) yes
C751 . H7512 . C650 . 121 0.95 2.29 2.897(18) yes
C750 . H7512 . N640 . 150 1.15 2.08 3.127(18) yes
C750 . H7512 . C650 . 145 1.15 2.29 3.298(18) yes
C750 . H7513 . C620 . 137 1.08 1.93 2.819(18) yes
C750 . H7513 . C621 . 139 1.08 2.57 3.464(18) yes
C740 . H7401 . C740 3_655 179 0.95 1.78 2.727(18) yes
C741 . H7402 . C826 2_454 150 0.84 2.58 3.335(18) yes
C740 . H7402 . C826 2_454 134 0.95 2.58 3.310(18) yes
C350 . H3513 . N210 . 157 0.82 2.21 2.977(18) yes
C350 . H3513 . C220 . 152 0.82 2.08 2.824(18) yes
C351 . H3514 . C270 . 120 0.95 2.43 3.023(18) yes
C140 . H1401 . C750 4_655 143 0.95 2.22 3.031(18) yes
C141 . H1412 . C823 2_555 164 0.95 2.23 3.151(18) yes
C141 . H1413 . C541 1_565 129 0.95 2.56 3.252(18) yes
C150 . H1512 . C140 . 140 0.89 1.79 2.538(18) yes
C150 . H1513 . N10 . 140 0.78 2.50 3.137(18) yes
C150 . H1513 . N40 . 146 0.78 2.20 2.881(18) yes
C150 . H1513 . C50 . 173 0.78 2.35 3.134(18) yes
C550 . H5511 . C540 . 130 0.93 1.84 2.538(18) yes
C550 . H5513 . N440 . 151 1.00 2.13 3.050(18) yes
C826 . H8261 . C741 2_545 125 1.09 2.59 3.335(18) yes
C826 . H8262 . C290 . 170 0.95 1.98 2.919(18) yes
C826 . H8262 . C291 . 163 0.95 2.57 3.491(18) yes
C826 . H8262 . N300 . 134 0.95 2.06 2.809(18) yes
C826 . H8263 . O825 3_756 157 0.91 1.37 2.232(18) yes
C827 . H8273 . C826 . 133 0.75 1.93 2.502(18) yes


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: chloroform, methanol'
