# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1451783'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-04-29 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                   9.4953(4)
_cell_length_b                   7.4545(4)
_cell_length_c                   23.2683(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.551(4)
_cell_angle_gamma                90
_cell_volume                     1645.36(13)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-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'
I -0.3257 6.8362 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C15 H17.50 I1.50 N1 O2 
# Dc =      1.75 Fooo =    840.00 Mu =    226.55 M =    434.17
# Found Formula = C15 H17.50 I1.50 N1 O2 
# Dc =      1.75 FOOO =    840.00 Mu =    226.55 M =    434.17

_chemical_formula_sum            'C15 H17.50 I1.50 N1 O2'
_chemical_formula_moiety         'C15 H17.50 I1.50 N1 O2'
_chemical_compound_source        ?
_chemical_formula_weight         434.17


_cell_measurement_reflns_used    5535
_cell_measurement_theta_min      5
_cell_measurement_theta_max      77
_cell_measurement_temperature    190

_exptl_crystal_description       needle
_exptl_crystal_colour            red-brown
_exptl_crystal_size_min          0.168
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_max          0.785

_exptl_crystal_density_diffrn    1.753
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    22.655

# Sheldrick geometric approximatio 0.02 0.02 
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_T_max  0.02
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_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       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      190
_diffrn_ambient_pressure         100
_diffrn_reflns_number            7712
_reflns_number_total             3358
_diffrn_reflns_av_R_equivalents  0.041
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3358 
# Theoretical number of reflections is about 6949 


_diffrn_reflns_theta_min         4.661
_diffrn_reflns_theta_max         76.896
_diffrn_measured_fraction_theta_max 0.966

_diffrn_reflns_theta_full        67.669
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              9
_reflns_limit_l_min              0
_reflns_limit_l_max              29

_oxford_diffrn_Wilson_B_factor   4.04
_oxford_diffrn_Wilson_scale      0.06

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.37
_refine_diff_density_max         1.41


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3355
_refine_ls_number_restraints     3
_refine_ls_number_parameters     179
_oxford_refine_ls_R_factor_ref   0.0480
_refine_ls_wR_factor_ref         0.1345
_refine_ls_goodness_of_fit_ref   0.9861
_refine_ls_shift/su_max          0.0013640
_refine_ls_shift/su_mean         0.0000213


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3355
_refine_ls_R_factor_all          0.0480
_refine_ls_wR_factor_all         0.1345

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3076
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_gt          0.1296

# 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 .


_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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.08P)² + 5.09P] 
 ,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
I1 I 0.5000 0.5000 0.5000 0.0482 1.0000 Uani S . . . . .
I2 I 0.55858(4) 0.31881(7) 0.392277(18) 0.0613 1.0000 Uani . . . . . .
O3 O 0.3754(4) 0.8647(6) 0.2627(2) 0.0562 1.0000 Uani . . . . . .
C4 C 0.4686(7) 0.7280(12) 0.2820(4) 0.0706 1.0000 Uani . . . . . .
C5 C 0.2456(5) 0.8724(7) 0.2851(2) 0.0387 1.0000 Uani . . . . . .
C6 C 0.1549(6) 1.0043(7) 0.2598(2) 0.0436 1.0000 Uani . . . . . .
C7 C 0.0230(6) 1.0218(7) 0.2781(2) 0.0412 1.0000 Uani . . . . . .
C8 C -0.0291(5) 0.9127(7) 0.3224(2) 0.0351 1.0000 Uani . . . . . .
C9 C -0.1674(6) 0.9310(8) 0.3407(2) 0.0462 1.0000 Uani . . . . . .
C10 C -0.2160(6) 0.8209(9) 0.3824(3) 0.0492 1.0000 Uani . . . . . .
C11 C -0.1286(6) 0.6882(8) 0.4068(2) 0.0446 1.0000 Uani . . . . . .
C12 C 0.0083(5) 0.6653(7) 0.3912(2) 0.0356 1.0000 Uani . . . . . .
C13 C 0.0615(5) 0.7793(6) 0.34745(19) 0.0321 1.0000 Uani . . . . . .
C14 C 0.2010(5) 0.7628(6) 0.32803(19) 0.0328 1.0000 Uani . . . . . .
C15 C 0.0971(6) 0.5176(7) 0.4180(2) 0.0386 1.0000 Uani . . . . . .
C16 C 0.0954(6) 0.3500(7) 0.3803(2) 0.0391 1.0000 Uani . . . . . .
N17 N 0.1880(5) 0.2111(6) 0.40524(19) 0.0417 1.0000 Uani . . . . . .
C18 C 0.1528(6) 0.1024(7) 0.4461(2) 0.0391 1.0000 Uani . . . . . .
O19 O 0.028033(10) 0.108279(10) 0.463417(10) 0.0483 1.0000 Uani . . . . . .
C20 C 0.2601(7) -0.0260(8) 0.4711(3) 0.0519 1.0000 Uani . . . . . .
H41 H 0.5541 0.7373 0.2614 0.1050 1.0000 Uiso R . . . . .
H43 H 0.4889 0.7417 0.3227 0.1048 1.0000 Uiso R . . . . .
H42 H 0.4242 0.6134 0.2745 0.1050 1.0000 Uiso R . . . . .
H61 H 0.1856 1.0782 0.2312 0.0519 1.0000 Uiso R . . . . .
H71 H -0.0352 1.1088 0.2612 0.0489 1.0000 Uiso R . . . . .
H91 H -0.2256 1.0199 0.3246 0.0541 1.0000 Uiso R . . . . .
H101 H -0.3076 0.8329 0.3949 0.0588 1.0000 Uiso R . . . . .
H111 H -0.1634 0.6124 0.4346 0.0530 1.0000 Uiso R . . . . .
H141 H 0.2617 0.6773 0.3446 0.0391 1.0000 Uiso R . . . . .
H151 H 0.0600 0.4888 0.4548 0.0461 1.0000 Uiso R . . . . .
H152 H 0.1936 0.5586 0.4232 0.0459 1.0000 Uiso R . . . . .
H161 H 0.0003 0.3016 0.3760 0.0467 1.0000 Uiso R . . . . .
H162 H 0.1304 0.3842 0.3430 0.0468 1.0000 Uiso R . . . . .
H203 H 0.2360 -0.0600 0.5091 0.0774 1.0000 Uiso R . . . . .
H202 H 0.3510 0.0302 0.4725 0.0774 1.0000 Uiso R . . . . .
H201 H 0.2641 -0.1308 0.4477 0.0773 1.0000 Uiso R . . . . .
H171 H 0.2755 0.2175 0.3986 0.0498 1.0000 Uiso R . . . . .
H192 H 0.0000 0.0000 0.5000 0.0712 1.0000 Uiso RS . . . . .

_refine_ls_extinction_coef       12(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          4.31(12)
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
I1 . I2 2_666 2.9224(4) yes
I1 . I2 . 2.9224(4) yes
O3 . C4 . 1.410(8) yes
O3 . C5 . 1.360(7) yes
C4 . H41 . 0.964 no
C4 . H43 . 0.964 no
C4 . H42 . 0.964 no
C5 . C6 . 1.416(7) yes
C5 . C14 . 1.373(7) yes
C6 . C7 . 1.347(8) yes
C6 . H61 . 0.922 no
C7 . C8 . 1.419(7) yes
C7 . H71 . 0.929 no
C8 . C9 . 1.405(7) yes
C8 . C13 . 1.422(6) yes
C9 . C10 . 1.367(9) yes
C9 . H91 . 0.931 no
C10 . C11 . 1.396(9) yes
C10 . H101 . 0.934 no
C11 . C12 . 1.376(7) yes
C11 . H111 . 0.930 no
C12 . C13 . 1.435(7) yes
C12 . C15 . 1.505(7) yes
C13 . C14 . 1.425(7) yes
C14 . H141 . 0.931 no
C15 . C16 . 1.526(7) yes
C15 . H151 . 0.965 no
C15 . H152 . 0.968 no
C16 . N17 . 1.461(6) yes
C16 . H161 . 0.973 no
C16 . H162 . 0.977 no
N17 . C18 . 1.304(7) yes
N17 . H171 . 0.853 no
C18 . O19 . 1.270(6) yes
C18 . C20 . 1.497(7) yes
O19 . H192 . 1.211 no
C20 . H203 . 0.957 no
C20 . H202 . 0.959 no
C20 . H201 . 0.954 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
I2 2_666 I1 . I2 . 179.996 yes
C4 . O3 . C5 . 118.4(5) yes
O3 . C4 . H41 . 108.7 no
O3 . C4 . H43 . 109.3 no
H41 . C4 . H43 . 110.2 no
O3 . C4 . H42 . 108.7 no
H41 . C4 . H42 . 110.2 no
H43 . C4 . H42 . 109.7 no
O3 . C5 . C6 . 114.5(5) yes
O3 . C5 . C14 . 124.6(5) yes
C6 . C5 . C14 . 120.9(5) yes
C5 . C6 . C7 . 119.5(5) yes
C5 . C6 . H61 . 120.6 no
C7 . C6 . H61 . 119.9 no
C6 . C7 . C8 . 122.2(5) yes
C6 . C7 . H71 . 118.5 no
C8 . C7 . H71 . 119.3 no
C7 . C8 . C9 . 121.7(5) yes
C7 . C8 . C13 . 118.3(4) yes
C9 . C8 . C13 . 120.0(5) yes
C8 . C9 . C10 . 120.5(5) yes
C8 . C9 . H91 . 119.5 no
C10 . C9 . H91 . 120.0 no
C9 . C10 . C11 . 120.0(5) yes
C9 . C10 . H101 . 120.9 no
C11 . C10 . H101 . 119.1 no
C10 . C11 . C12 . 122.1(5) yes
C10 . C11 . H111 . 119.3 no
C12 . C11 . H111 . 118.6 no
C11 . C12 . C13 . 118.7(5) yes
C11 . C12 . C15 . 120.0(5) yes
C13 . C12 . C15 . 121.3(4) yes
C12 . C13 . C8 . 118.7(4) yes
C12 . C13 . C14 . 122.4(4) yes
C8 . C13 . C14 . 119.0(4) yes
C13 . C14 . C5 . 120.1(4) yes
C13 . C14 . H141 . 119.7 no
C5 . C14 . H141 . 120.3 no
C12 . C15 . C16 . 111.7(4) yes
C12 . C15 . H151 . 108.1 no
C16 . C15 . H151 . 109.4 no
C12 . C15 . H152 . 109.3 no
C16 . C15 . H152 . 108.4 no
H151 . C15 . H152 . 109.9 no
C15 . C16 . N17 . 111.2(4) yes
C15 . C16 . H161 . 110.5 no
N17 . C16 . H161 . 108.5 no
C15 . C16 . H162 . 107.5 no
N17 . C16 . H162 . 108.3 no
H161 . C16 . H162 . 110.8 no
C16 . N17 . C18 . 124.0(5) yes
C16 . N17 . H171 . 117.6 no
C18 . N17 . H171 . 116.7 no
N17 . C18 . O19 . 118.9(4) yes
N17 . C18 . C20 . 119.3(5) yes
O19 . C18 . C20 . 121.8(5) yes
C18 . O19 . H192 . 116.0 no
C18 . C20 . H203 . 110.0 no
C18 . C20 . H202 . 109.2 no
H203 . C20 . H202 . 109.6 no
C18 . C20 . H201 . 110.2 no
H203 . C20 . H201 . 109.2 no
H202 . C20 . H201 . 108.6 no
O19 2_556 H192 . O19 . 180.0 no


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 28/01/16 at 15:50:02
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
CONT EXTPARAM 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  43,X'S) H   (  42,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE N   (  17,X'S) H   ( 171,X'S) 
RIDE O   (  19,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 202,X'S) H   ( 201,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 28/01/16 at 15:50:02
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;

# Manually omitted reflections

loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 1 7 x .
-1 0 10 x .
0 9 3 x .
_chemical_name_systematic        'agomelatine hemitriiodide '
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1451784'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-04-29 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                   13.5939(11)
_cell_length_b                   7.2782(5)
_cell_length_c                   19.7522(16)
_cell_angle_alpha                90
_cell_angle_beta                 109.567(9)
_cell_angle_gamma                90
_cell_volume                     1841.4(3)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x,-y+1/2,z+1/2
-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 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776
4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C15 H24 I1 N1 O5 
# Dc =      1.53 Fooo =    856.00 Mu =     17.59 M =    425.26
# Found Formula = C15 H24 I1 N1 O5 
# Dc =      1.53 FOOO =    856.00 Mu =     17.59 M =    425.26

_chemical_formula_sum            'C15 H24 I1 N1 O5'
_chemical_formula_moiety         'C15 H24 I1 N1 O5'
_chemical_compound_source        ?
_chemical_formula_weight         425.26


_cell_measurement_reflns_used    1814
_cell_measurement_theta_min      4
_cell_measurement_theta_max      26
_cell_measurement_temperature    301

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.120
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_max          0.440

_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    1.759

# Sheldrick geometric approximatio 0.73 0.81 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_T_max  0.81
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_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       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      301
_diffrn_ambient_pressure         100
_diffrn_reflns_number            7497
_reflns_number_total             4236
_diffrn_reflns_av_R_equivalents  0.024
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 4236 
# Theoretical number of reflections is about 9968 


_diffrn_reflns_theta_min         3.107
_diffrn_reflns_theta_max         29.189
_diffrn_measured_fraction_theta_max 0.853

_diffrn_reflns_theta_full        26.061
_diffrn_measured_fraction_theta_full 0.994


_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -18
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              9
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   4.41
_oxford_diffrn_Wilson_scale      0.09

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.41
_refine_diff_density_max         3.06


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         4236
_refine_ls_number_restraints     1
_refine_ls_number_parameters     199
_oxford_refine_ls_R_factor_ref   0.0793
_refine_ls_wR_factor_ref         0.1356
_refine_ls_goodness_of_fit_ref   0.9748
_refine_ls_shift/su_max          0.0001950
_refine_ls_shift/su_mean         0.0000442


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4236
_refine_ls_R_factor_all          0.0793
_refine_ls_wR_factor_all         0.1356

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3042
_refine_ls_R_factor_gt           0.0565
_refine_ls_wR_factor_gt          0.1201

# 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 .


_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= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 7.06P] 
 ,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
I1 I 0.42314(3) 0.37412(7) 0.60875(2) 0.0635 1.0000 Uani D . . . . .
O20 O 0.8258(3) 0.2033(7) 0.4600(2) 0.0681 1.0000 Uani . . . . . .
O3 O 0.9609(3) 0.6926(6) 0.9525(2) 0.0595 1.0000 Uani . . . . . .
C4 C 0.8971(5) 0.8290(10) 0.9680(3) 0.0686 1.0000 Uani . . . . . .
C5 C 0.9348(4) 0.6336(7) 0.8825(3) 0.0457 1.0000 Uani . . . . . .
C6 C 0.8527(4) 0.6990(7) 0.8270(3) 0.0397 1.0000 Uani . . . . . .
C7 C 0.8316(4) 0.6298(7) 0.7566(3) 0.0398 1.0000 Uani . . . . . .
C8 C 0.8979(4) 0.4893(7) 0.7457(3) 0.0494 1.0000 Uani . . . . . .
C9 C 0.9824(4) 0.4274(8) 0.8063(4) 0.0599 1.0000 Uani . . . . . .
C10 C 1.0002(4) 0.4960(8) 0.8718(4) 0.0558 1.0000 Uani . . . . . .
C11 C 0.8790(6) 0.4192(8) 0.6763(4) 0.0645 1.0000 Uani . . . . . .
C12 C 0.7975(6) 0.4814(9) 0.6203(4) 0.0688 1.0000 Uani . . . . . .
C13 C 0.7309(5) 0.6190(8) 0.6303(3) 0.0561 1.0000 Uani . . . . . .
C14 C 0.7468(4) 0.6944(7) 0.6967(3) 0.0417 1.0000 Uani . . . . . .
C15 C 0.6772(4) 0.8474(7) 0.7053(3) 0.0433 1.0000 Uani . . . . . .
C16 C 0.7258(4) 1.0346(7) 0.7024(3) 0.0468 1.0000 Uani . . . . . .
N17 N 0.6692(3) 1.1811(6) 0.7251(2) 0.0459 1.0000 Uani . . . . . .
C18 C 0.6943(4) 1.2437(7) 0.7891(3) 0.0409 1.0000 Uani . . . . . .
O19 O 0.7769(3) 1.1788(5) 0.83626(19) 0.0502 1.0000 Uani . . . . . .
C20 C 0.6296(4) 1.3850(8) 0.8085(3) 0.0513 1.0000 Uani . . . . . .
O21 O 0.7048(4) 1.0012(8) 0.5079(3) 0.0921 1.0000 Uani . . . . . .
O22 O 0.5413(5) 0.2274(9) 0.4826(4) 0.1253 1.0000 Uani D . . . . .
H41 H 0.9232 0.8549 1.0173 0.1081 1.0000 Uiso R . . . . .
H43 H 0.8270 0.7832 0.9546 0.1079 1.0000 Uiso R . . . . .
H42 H 0.8996 0.9390 0.9409 0.1079 1.0000 Uiso R . . . . .
H61 H 0.8106 0.7905 0.8352 0.0488 1.0000 Uiso R . . . . .
H91 H 1.0247 0.3354 0.7996 0.0740 1.0000 Uiso R . . . . .
H111 H 0.9226 0.3296 0.6688 0.0800 1.0000 Uiso R . . . . .
H121 H 0.7843 0.4321 0.5746 0.0809 1.0000 Uiso R . . . . .
H131 H 0.6750 0.6595 0.5912 0.0699 1.0000 Uiso R . . . . .
H152 H 0.6120 0.8405 0.6667 0.0542 1.0000 Uiso R . . . . .
H151 H 0.6649 0.8351 0.7499 0.0537 1.0000 Uiso R . . . . .
H161 H 0.7223 1.0591 0.6544 0.0544 1.0000 Uiso R . . . . .
H162 H 0.7981 1.0364 0.7336 0.0535 1.0000 Uiso R . . . . .
H203 H 0.6720 1.4854 0.8321 0.0750 1.0000 Uiso R . . . . .
H204 H 0.5986 1.3320 0.8397 0.0752 1.0000 Uiso R . . . . .
H205 H 0.5755 1.4290 0.7667 0.0751 1.0000 Uiso R . . . . .
H171 H 0.6167 1.2259 0.6941 0.0538 1.0000 Uiso R . . . . .
H211 H 0.6547 1.0775 0.5010 0.1435 1.0000 Uiso R . . . . .
H201 H 0.7897 0.1338 0.4742 0.1006 1.0000 Uiso R . . . . .
H191 H 0.7881 1.2207 0.8771 0.0744 1.0000 Uiso R . . . . .
H202 H 0.8844 0.1885 0.4881 0.1011 1.0000 Uiso R . . . . .
H212 H 0.6688 0.9190 0.4825 0.1439 1.0000 Uiso R . . . . .
H222 H 0.5236 0.2688 0.5170 0.1913 1.0000 Uiso DR . . . . .
H221 H 0.5567 0.3196 0.4634 0.1912 1.0000 Uiso DR . . . . .
H101 H 1.0576 0.4531 0.9111 0.0681 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          3.59(5)
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
O20 . H201 . 0.817 no
O20 . H202 . 0.811 no
O3 . C4 . 1.417(7) yes
O3 . C5 . 1.376(7) yes
C4 . H41 . 0.937 no
C4 . H43 . 0.960 no
C4 . H42 . 0.969 no
C5 . C6 . 1.362(7) yes
C5 . C10 . 1.401(8) yes
C6 . C7 . 1.415(7) yes
C6 . H61 . 0.928 no
C7 . C8 . 1.426(7) yes
C7 . C14 . 1.427(7) yes
C8 . C9 . 1.427(8) yes
C8 . C11 . 1.403(9) yes
C9 . C10 . 1.332(9) yes
C9 . H91 . 0.921 no
C10 . H101 . 0.950 no
C11 . C12 . 1.355(9) yes
C11 . H111 . 0.926 no
C12 . C13 . 1.408(9) yes
C12 . H121 . 0.930 no
C13 . C14 . 1.370(7) yes
C13 . H131 . 0.931 no
C14 . C15 . 1.507(7) yes
C15 . C16 . 1.523(7) yes
C15 . H152 . 0.957 no
C15 . H151 . 0.956 no
C16 . N17 . 1.471(7) yes
C16 . H161 . 0.950 no
C16 . H162 . 0.969 no
N17 . C18 . 1.278(6) yes
N17 . H171 . 0.835 no
C18 . O19 . 1.285(6) yes
C18 . C20 . 1.484(7) yes
O19 . H191 . 0.827 no
C20 . H203 . 0.950 no
C20 . H204 . 0.938 no
C20 . H205 . 0.959 no
O21 . H211 . 0.853 no
O21 . H212 . 0.827 no
O22 . H222 . 0.847 no
O22 . H221 . 0.832 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
H201 . O20 . H202 . 104.3 no
C4 . O3 . C5 . 117.7(4) yes
O3 . C4 . H41 . 108.6 no
O3 . C4 . H43 . 108.7 no
H41 . C4 . H43 . 110.6 no
O3 . C4 . H42 . 108.8 no
H41 . C4 . H42 . 109.6 no
H43 . C4 . H42 . 110.5 no
O3 . C5 . C6 . 124.5(5) yes
O3 . C5 . C10 . 114.3(5) yes
C6 . C5 . C10 . 121.2(5) yes
C5 . C6 . C7 . 120.6(5) yes
C5 . C6 . H61 . 119.8 no
C7 . C6 . H61 . 119.6 no
C6 . C7 . C8 . 118.2(5) yes
C6 . C7 . C14 . 122.6(4) yes
C8 . C7 . C14 . 119.1(5) yes
C7 . C8 . C9 . 118.2(5) yes
C7 . C8 . C11 . 119.3(6) yes
C9 . C8 . C11 . 122.5(5) yes
C8 . C9 . C10 . 122.0(5) yes
C8 . C9 . H91 . 118.4 no
C10 . C9 . H91 . 119.6 no
C5 . C10 . C9 . 119.8(6) yes
C5 . C10 . H101 . 120.1 no
C9 . C10 . H101 . 120.2 no
C8 . C11 . C12 . 120.5(6) yes
C8 . C11 . H111 . 119.7 no
C12 . C11 . H111 . 119.7 no
C11 . C12 . C13 . 120.8(6) yes
C11 . C12 . H121 . 120.1 no
C13 . C12 . H121 . 119.1 no
C12 . C13 . C14 . 121.1(6) yes
C12 . C13 . H131 . 119.6 no
C14 . C13 . H131 . 119.3 no
C7 . C14 . C13 . 119.1(5) yes
C7 . C14 . C15 . 120.9(4) yes
C13 . C14 . C15 . 120.0(5) yes
C14 . C15 . C16 . 111.1(4) yes
C14 . C15 . H152 . 108.7 no
C16 . C15 . H152 . 108.3 no
C14 . C15 . H151 . 110.2 no
C16 . C15 . H151 . 109.3 no
H152 . C15 . H151 . 109.2 no
C15 . C16 . N17 . 111.0(4) yes
C15 . C16 . H161 . 109.2 no
N17 . C16 . H161 . 108.2 no
C15 . C16 . H162 . 110.4 no
N17 . C16 . H162 . 108.5 no
H161 . C16 . H162 . 109.5 no
C16 . N17 . C18 . 124.6(4) yes
C16 . N17 . H171 . 117.7 no
C18 . N17 . H171 . 117.7 no
N17 . C18 . O19 . 117.7(5) yes
N17 . C18 . C20 . 121.2(5) yes
O19 . C18 . C20 . 121.2(5) yes
C18 . O19 . H191 . 113.7 no
C18 . C20 . H203 . 110.2 no
C18 . C20 . H204 . 108.7 no
H203 . C20 . H204 . 109.0 no
C18 . C20 . H205 . 111.0 no
H203 . C20 . H205 . 109.2 no
H204 . C20 . H205 . 108.7 no
H211 . O21 . H212 . 95.5 no
H222 . O22 . H221 . 105.2 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
O21 . H211 . O22 1_565 175.8(3) 0.853 1.824 2.676(8) yes
O20 . H201 . O21 1_545 174.2(2) 0.817 1.795 2.609(8) yes
O19 . H191 . O20 3_565 172.81(19) 0.827 1.639 2.462(8) yes
O20 . H202 . O3 4_746 168.51(17) 0.811 2.037 2.836(8) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 02/02/16 at 11:06:51
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE O   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) H   (  43,X'S) H   (  42,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE N   (  17,X'S) H   ( 171,X'S) 
RIDE O   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 204,X'S) H   ( 205,X'S) 
RIDE O   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE O   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
END                                                                             
;


_iucr_refine_instruction_details_restraints 
;
#
# Punched on 02/02/16 at 11:06:51
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
ANGLE 104.500000 , 1.000000 = H(222) TO O(22) TO H(221) 
DISTANCE 0.820000 , 0.001000 = O(22) TO H(222) 
DISTANCE 0.820000 , 0.0010000 = O(22) TO H(221) 
ANGLE 180.000000 , 1.000000 = I(1) TO H(222) TO O(22) 
END                                                                             
;
_chemical_name_systematic        'agomelatine hydriodide trihydrate '
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_chemical_properties_physical    'Air-sensitive, Oxygen-sensitive'
####################################################################### 
# 
# 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 1451785'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-04-29 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        'agomelatine hemitriiodide iodine '
_chemical_name_common            'agomelatine iodine -- triiodide '
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C60 H68 I8 N4 O8'
_chemical_formula_weight         1988.5
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

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

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   13.1828(4)
_cell_length_b                   14.6064(5)
_cell_length_c                   18.7024(12)
_cell_angle_alpha                89.990(4)
_cell_angle_beta                 75.962(4)
_cell_angle_gamma                73.901(3)
_cell_volume                     3347.9(3)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.8856(7) 1 0 0 0 1 0 0 0 1
2 0.1144(7) -1 0 0 0.5005 1 0 0 0 -1

_cell_formula_units_Z            2

_cell_measurement_reflns_used    23385
_cell_measurement_theta_min      3.48
_cell_measurement_theta_max      28.09
_cell_measurement_temperature    100.01(10)
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.9725
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1892

_exptl_absorpt_coefficient_mu    3.758
_exptl_crystal_description       'prolongated parallelepiped'
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.044
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'redish black'
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_T_max  0.865
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      100.01
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2027
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            39722
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_full        27.16
_diffrn_measured_fraction_theta_max 0.91
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

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

# 8. REFINEMENT DATA

_refine_special_details          
;
The refinement was carried out against all reflections.  The conventional
R-factor is always based on F. The goodness of fit as well as the weighted
R-factor are based on F and F² for refinement carried out on F and F²,
respectively. The threshold expression is used only for calculating
R-factors etc. and it is not relevant to the choice of reflections for
refinement.

The program used for refinement, Jana2006, uses the weighting scheme
based on the experimental expectations, see _refine_ls_weighting_details,
that does not force S to be one. Therefore the values of S are usually larger
than the ones from the SHELX program.

;

_reflns_number_total             15068
_reflns_number_gt                13213
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0181
_refine_ls_wR_factor_gt          0.0443
_refine_ls_R_factor_all          0.0229
_refine_ls_wR_factor_ref         0.0467
_refine_ls_goodness_of_fit_ref   1.15
_refine_ls_goodness_of_fit_gt    1.17
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         15068
_refine_ls_number_parameters     737
_refine_ls_number_restraints     4
_refine_ls_number_constraints    263
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0500
_refine_ls_shift/su_mean         0.0014
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
I -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_structure_solution    
;
Superflip, version February 2014
;
_computing_structure_refinement  Jana2006
_computing_molecular_graphics    Diamond
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
N1 . H1n1 . 1 0.001
N2 . H1n2 . 1 0.001
N3 . H1n3 . 1 0.001
N4 . H1n4 . 1 0.001
O3 . H1o3o5 . 2 0.001
O5 . H1o3o5 . 2 0.001

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 1.003308(11) 0.340138(11) -0.155052(8) Uani 0.01944(5) 2 1 d . . .
I2 I -0.001241(11) 0.844325(11) 0.654623(9) Uani 0.01962(5) 2 1 d . . .
I3 I 0.007197(12) 0.853225(12) 0.803393(9) Uani 0.02322(6) 2 1 d . . .
I4 I 0.991938(12) 0.352570(12) -0.303232(9) Uani 0.02331(6) 2 1 d . . .
I5 I 0.995657(12) 0.328763(12) 0.011478(9) Uani 0.02351(6) 2 1 d . . .
I6 I 0.007972(12) 0.826218(12) 0.488059(9) Uani 0.02337(6) 2 1 d . . .
I7 I 1.000549(12) 0.094964(12) -0.002902(9) Uani 0.02538(6) 2 1 d . . .
I8 I 0.000792(12) 0.594845(12) 0.503256(8) Uani 0.02494(6) 2 1 d . . .
O1 O 0.27418(12) 0.84173(11) 0.16037(9) Uani 0.0212(6) 2 1 d . . .
O2 O 0.26871(13) 0.34564(11) 0.16083(9) Uani 0.0215(6) 2 1 d . . .
O3 O 0.56369(12) 0.79839(11) 0.50466(9) Uani 0.0171(6) 2 1 d . . .
O4 O 0.72981(12) 0.47827(11) 0.33913(9) Uani 0.0212(6) 2 1 d . . .
O5 O 0.44978(12) 0.69551(11) 0.49557(9) Uani 0.0164(6) 2 1 d . . .
O6 O 0.55825(12) 0.92056(11) 0.00441(9) Uani 0.0171(6) 2 1 d . . .
N1 N 0.72645(15) 0.32709(13) -0.01128(10) Uani 0.0143(6) 2 1 d . . .
O8 O 0.27362(12) 1.01840(12) 0.66016(9) Uani 0.0212(6) 2 1 d . . .
O7 O 0.55586(12) 0.41982(11) 0.00441(9) Uani 0.0168(6) 2 1 d . . .
N3 N 0.72924(15) 0.82795(13) -0.01596(11) Uani 0.0148(6) 2 1 d . . .
N4 N 0.27783(15) 0.69173(13) 0.51023(10) Uani 0.0145(6) 2 1 d . . .
N2 N 0.73395(15) 0.80795(13) 0.48284(11) Uani 0.0147(6) 2 1 d . . .
C1 C 0.30964(17) 0.59141(15) 0.48352(12) Uani 0.0145(7) 2 1 d . . .
C2 C 0.69923(17) 0.90802(15) 0.51174(12) Uani 0.0142(7) 2 1 d . . .
C3 C 0.72371(19) 0.56993(16) 0.12947(12) Uani 0.0165(8) 2 1 d . . .
C4 C 0.72113(19) 1.06901(16) 0.62995(12) Uani 0.0166(8) 2 1 d . . .
C5 C 0.68945(17) 0.73870(15) 0.09527(12) Uani 0.0145(7) 2 1 d . . .
C6 C 0.34825(17) 0.73926(16) 0.51361(12) Uani 0.0137(7) 2 1 d . . .
C7 C 0.64816(18) 1.02007(16) 0.62425(12) Uani 0.0143(7) 2 1 d . . .
C8 C 0.28314(19) 0.42813(17) 0.36562(12) Uani 0.0171(8) 2 1 d . . .
C9 C 0.35592(18) 0.47690(15) 0.37246(12) Uani 0.0140(7) 2 1 d . . .
C10 C 0.50177(18) 0.58201(15) 0.17219(12) Uani 0.0143(8) 2 1 d . . .
C11 C 0.69687(17) 0.74401(15) 0.01254(12) Uani 0.0152(8) 2 1 d . . .
C12 C 0.64189(18) 0.15517(16) 0.12748(12) Uani 0.0152(8) 2 1 d . . .
C13 C 0.38882(18) 0.59149(16) 0.19606(12) Uani 0.0171(8) 2 1 d . . .
C14 C 0.71429(19) 0.06945(16) 0.13420(12) Uani 0.0169(8) 2 1 d . . .
C15 C 0.61811(18) 0.28341(16) 0.30383(12) Uani 0.0174(8) 2 1 d . . .
C16 C 0.38558(18) 1.21249(16) 0.69675(12) Uani 0.0167(8) 2 1 d . . .
C17 C 0.64963(18) 0.65521(16) 0.12443(12) Uani 0.0143(7) 2 1 d . . .
C18 C 0.30909(19) 1.16672(16) 0.69377(12) Uani 0.0178(8) 2 1 d . . .
C19 C 0.31476(17) 0.58072(16) 0.40128(12) Uani 0.0153(8) 2 1 d . . .
C20 C 0.65723(17) 0.41074(15) -0.01432(12) Uani 0.0139(7) 2 1 d . . .
C21 C 0.69286(17) 0.24359(15) 0.01582(12) Uani 0.0145(7) 2 1 d . . .
C22 C 0.68456(17) 0.23725(16) 0.09867(12) Uani 0.0155(8) 2 1 d . . .
C23 C 0.49237(19) 0.08378(16) 0.17364(12) Uani 0.0156(8) 2 1 d . . .
C24 C 0.30298(19) 0.17942(17) 0.19400(13) Uani 0.0192(8) 2 1 d . . .
C25 C 0.37851(19) 0.09520(16) 0.19742(12) Uani 0.0175(8) 2 1 d . . .
C26 C 0.68927(17) 0.91654(16) 0.59480(12) Uani 0.0152(8) 2 1 d . . .
C27 C 0.57039(19) -0.00339(16) 0.17777(12) Uani 0.0177(8) 2 1 d . . .
C28 C 0.58180(19) 0.49565(16) 0.17577(12) Uani 0.0168(8) 2 1 d . . .
C29 C 0.67881(19) -0.01082(16) 0.15808(12) Uani 0.0182(8) 2 1 d . . .
C30 C 0.66508(18) 0.75803(16) 0.48113(12) Uani 0.0137(7) 2 1 d . . .
C31 C 0.65928(18) 0.91126(15) -0.01782(12) Uani 0.0140(7) 2 1 d . . .
C32 C 0.47029(18) 0.42801(16) 0.35372(12) Uani 0.0143(7) 2 1 d . . .
C33 C 0.57757(19) 1.21338(16) 0.67669(12) Uani 0.0174(8) 2 1 d . . .
C34 C 0.53583(18) 0.66328(15) 0.14457(11) Uani 0.0129(7) 2 1 d . . .
C35 C 0.68622(20) 1.16649(17) 0.65508(13) Uani 0.0194(8) 2 1 d . . .
C36 C 0.31201(19) 0.67523(17) 0.19298(13) Uani 0.0183(8) 2 1 d . . .
C37 C 0.68999(19) 0.48927(16) 0.15446(12) Uani 0.0180(8) 2 1 d . . .
C38 C 0.42652(19) 0.28266(17) 0.32243(12) Uani 0.0178(8) 2 1 d . . .
C39 C 0.69420(19) 0.32961(17) 0.30691(13) Uani 0.0187(8) 2 1 d . . .
C40 C 0.31770(19) 0.33004(17) 0.34215(13) Uani 0.0193(8) 2 1 d . . .
C41 C 0.34378(18) 1.07052(16) 0.66499(12) Uani 0.0160(8) 2 1 d . . .
C42 C 0.50508(18) 0.32994(16) 0.32676(12) Uani 0.0145(7) 2 1 d . . .
C43 C 0.70799(18) 0.65614(16) 0.45188(13) Uani 0.0189(8) 2 1 d . . .
C44 C 0.52788(18) 0.16435(16) 0.14618(12) Uani 0.0145(7) 2 1 d . . .
C45 C 0.49852(18) 1.16622(16) 0.67268(12) Uani 0.0147(8) 2 1 d . . .
C46 C 0.45417(18) 0.74841(16) 0.14066(12) Uani 0.0153(8) 2 1 d . . .
C47 C 0.65953(18) 0.42588(16) 0.33453(12) Uani 0.0167(8) 2 1 d . . .
C48 C 0.69997(18) 0.49259(16) -0.04071(13) Uani 0.0184(8) 2 1 d . . .
C49 C 0.30740(18) 0.84239(16) 0.53949(13) Uani 0.0184(8) 2 1 d . . .
C50 C 0.70017(18) 0.99302(16) -0.04621(13) Uani 0.0187(8) 2 1 d . . .
C51 C 0.53330(17) 1.06848(15) 0.64458(12) Uani 0.0133(7) 2 1 d . . .
C52 C 0.55035(18) 0.47396(16) 0.35820(12) Uani 0.0149(8) 2 1 d . . .
C53 C 0.45302(17) 1.02304(16) 0.64032(12) Uani 0.0147(7) 2 1 d . . .
C54 C 0.44756(18) 0.25032(16) 0.14183(12) Uani 0.0157(8) 2 1 d . . .
C55 C 0.34545(18) 0.75464(16) 0.16468(12) Uani 0.0157(8) 2 1 d . . .
C56 C 0.16063(18) 0.85424(18) 0.19048(15) Uani 0.0264(9) 2 1 d . . .
C57 C 0.33834(18) 0.25807(16) 0.16562(12) Uani 0.0167(8) 2 1 d . . .
C58 C 0.15457(19) 0.35976(18) 0.18985(15) Uani 0.0280(9) 2 1 d . . .
C59 C 0.15935(19) 1.06180(18) 0.68949(15) Uani 0.0270(9) 2 1 d . . .
C60 C 0.84395(19) 0.43440(19) 0.30923(15) Uani 0.0284(10) 2 1 d . . .
H1c1 H 0.258211 0.560981 0.511174 Uiso 0.0174 2 1 d . . .
H2c1 H 0.379662 0.559569 0.491647 Uiso 0.0174 2 1 d . . .
H1c2 H 0.630198 0.939737 0.502061 Uiso 0.017 2 1 d . . .
H2c2 H 0.750885 0.939761 0.486405 Uiso 0.017 2 1 d . . .
H1c3 H 0.800181 0.565014 0.115684 Uiso 0.0198 2 1 d . . .
H1c4 H 0.79776 1.036223 0.616541 Uiso 0.0199 2 1 d . . .
H1c5 H 0.640318 0.796885 0.121387 Uiso 0.0174 2 1 d . . .
H2c5 H 0.760003 0.732147 0.10375 Uiso 0.0174 2 1 d . . .
H1c8 H 0.206727 0.461566 0.377106 Uiso 0.0205 2 1 d . . .
H1c11 H 0.748708 0.687163 -0.013825 Uiso 0.0182 2 1 d . . .
H2c11 H 0.627522 0.746184 0.003684 Uiso 0.0182 2 1 d . . .
H1c13 H 0.365454 0.537582 0.214969 Uiso 0.0205 2 1 d . . .
H1c14 H 0.79087 0.064009 0.122368 Uiso 0.0203 2 1 d . . .
H1c15 H 0.642165 0.217526 0.285578 Uiso 0.0208 2 1 d . . .
H1c16 H 0.361802 1.278064 0.715777 Uiso 0.02 2 1 d . . .
H1c18 H 0.232746 1.199499 0.711023 Uiso 0.0213 2 1 d . . .
H1c19 H 0.243429 0.608287 0.393665 Uiso 0.0184 2 1 d . . .
H2c19 H 0.362091 0.615126 0.374006 Uiso 0.0184 2 1 d . . .
H1c21 H 0.744553 0.18679 -0.010721 Uiso 0.0174 2 1 d . . .
H2c21 H 0.623451 0.246955 0.006557 Uiso 0.0174 2 1 d . . .
H1c22 H 0.755218 0.228991 0.107484 Uiso 0.0186 2 1 d . . .
H2c22 H 0.636809 0.29589 0.124885 Uiso 0.0186 2 1 d . . .
H1c24 H 0.226487 0.185192 0.210735 Uiso 0.0231 2 1 d . . .
H1c25 H 0.353902 0.041938 0.216521 Uiso 0.021 2 1 d . . .
H1c26 H 0.639784 0.88267 0.61995 Uiso 0.0182 2 1 d . . .
H2c26 H 0.759266 0.888005 0.604209 Uiso 0.0182 2 1 d . . .
H1c27 H 0.546607 -0.057879 0.194632 Uiso 0.0213 2 1 d . . .
H1c28 H 0.559421 0.440818 0.193476 Uiso 0.0202 2 1 d . . .
H1c29 H 0.731224 -0.070598 0.160409 Uiso 0.0219 2 1 d . . .
H1c33 H 0.5544 1.279264 0.694867 Uiso 0.0208 2 1 d . . .
H1c35 H 0.738993 1.199799 0.656952 Uiso 0.0232 2 1 d . . .
H1c36 H 0.235796 0.679998 0.209962 Uiso 0.022 2 1 d . . .
H1c37 H 0.743365 0.429945 0.156431 Uiso 0.0217 2 1 d . . .
H1c38 H 0.449887 0.216345 0.305415 Uiso 0.0214 2 1 d . . .
H1c39 H 0.770607 0.296709 0.2904 Uiso 0.0225 2 1 d . . .
H1c40 H 0.264935 0.296802 0.340049 Uiso 0.0231 2 1 d . . .
H1c43 H 0.786001 0.639557 0.43453 Uiso 0.0227 2 1 d . . .
H2c43 H 0.688394 0.616156 0.490463 Uiso 0.0227 2 1 d . . .
H3c43 H 0.677237 0.647021 0.411794 Uiso 0.0227 2 1 d . . .
H1c46 H 0.475378 0.802853 0.120792 Uiso 0.0184 2 1 d . . .
H1c48 H 0.776217 0.476788 -0.042272 Uiso 0.022 2 1 d . . .
H2c48 H 0.69012 0.505468 -0.089297 Uiso 0.022 2 1 d . . .
H3c48 H 0.661048 0.548141 -0.007527 Uiso 0.022 2 1 d . . .
H1c49 H 0.231778 0.866219 0.539587 Uiso 0.0221 2 1 d . . .
H2c49 H 0.315376 0.850045 0.588631 Uiso 0.0221 2 1 d . . .
H3c49 H 0.348693 0.877383 0.506949 Uiso 0.0221 2 1 d . . .
H1c50 H 0.778427 0.974036 -0.057445 Uiso 0.0225 2 1 d . . .
H2c50 H 0.676948 1.012105 -0.090158 Uiso 0.0225 2 1 d . . .
H3c50 H 0.671498 1.045632 -0.009341 Uiso 0.0225 2 1 d . . .
H1c52 H 0.528216 0.539152 0.37792 Uiso 0.0179 2 1 d . . .
H1c53 H 0.47504 0.958154 0.619933 Uiso 0.0176 2 1 d . . .
H1c54 H 0.470014 0.304189 0.121861 Uiso 0.0188 2 1 d . . .
H1c56 H 0.120864 0.919581 0.188089 Uiso 0.0316 2 1 d . . .
H2c56 H 0.136224 0.813296 0.162588 Uiso 0.0316 2 1 d . . .
H3c56 H 0.148318 0.83827 0.241047 Uiso 0.0316 2 1 d . . .
H1c58 H 0.116 0.425159 0.186402 Uiso 0.0336 2 1 d . . .
H2c58 H 0.130217 0.318718 0.162008 Uiso 0.0336 2 1 d . . .
H3c58 H 0.140645 0.344928 0.240675 Uiso 0.0336 2 1 d . . .
H1c59 H 0.120374 1.016266 0.685296 Uiso 0.0324 2 1 d . . .
H2c59 H 0.145602 1.082419 0.740554 Uiso 0.0324 2 1 d . . .
H3c59 H 0.135308 1.115868 0.662314 Uiso 0.0324 2 1 d . . .
H1c60 H 0.883377 0.479711 0.313 Uiso 0.0341 2 1 d . . .
H2c60 H 0.868117 0.380334 0.336372 Uiso 0.0341 2 1 d . . .
H3c60 H 0.85699 0.413713 0.258257 Uiso 0.0341 2 1 d . . .
H1n1 H 0.7920(11) 0.3247(17) -0.0181(13) Uiso 0.0172 2 1 d . . .
H1n4 H 0.2123(11) 0.7232(15) 0.5209(13) Uiso 0.0173 2 1 d . . .
H1n3 H 0.7958(10) 0.8228(17) -0.0276(13) Uiso 0.0178 2 1 d . . .
H1n2 H 0.7998(10) 0.7795(15) 0.4659(13) Uiso 0.0176 2 1 d . . .
H1o7 H 0.5 0.5 0 Uiso 0.0202 1 1 d . . .
H1o3o5 H 0.5056(14) 0.7474(12) 0.5019(12) Uiso 0.0205 2 1 d . . .
H1o6 H 0.5 1 0 Uiso 0.0206 1 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


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

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
I5 N1 . . 3.682(2) ?
I5 N3 . 2_765 3.7340(18) ?
I6 N4 . . 3.6778(19) ?
I6 N2 . 1_455 3.720(2) ?
I7 I7 . 2_755 2.7802(3) ?
I8 I8 . 2_566 2.7795(3) ?
O1 C55 . . 1.372(3) ?
O1 C56 . . 1.425(3) ?
O2 C57 . . 1.369(3) ?
O2 C58 . . 1.426(3) ?
O3 C30 . . 1.267(2) ?
O3 H1o3o5 . . 1.22(2) ?
O4 C47 . . 1.372(3) ?
O4 C60 . . 1.430(3) ?
O5 C6 . . 1.273(2) ?
O5 H1o3o5 . . 1.22(2) ?
O6 C31 . . 1.263(3) ?
O6 H1o6 . . 1.2163(14) ?
N1 C20 . . 1.317(3) ?
N1 C21 . . 1.460(3) ?
N1 H1n1 . . 0.833(16) ?
O8 C41 . . 1.369(3) ?
O8 C59 . . 1.429(3) ?
O7 C20 . . 1.265(3) ?
O7 H1o7 . . 1.2132(14) ?
N3 C11 . . 1.466(3) ?
N3 C31 . . 1.314(3) ?
N3 H1n3 . . 0.833(14) ?
N4 C1 . . 1.460(3) ?
N4 C6 . . 1.317(3) ?
N4 H1n4 . . 0.833(13) ?
N2 C2 . . 1.465(3) ?
N2 C30 . . 1.318(3) ?
N2 H1n2 . . 0.833(13) ?
C1 C19 . . 1.529(3) ?
C1 H1c1 . . 0.96 ?
C1 H2c1 . . 0.96 ?
C2 C26 . . 1.529(3) ?
C2 H1c2 . . 0.96 ?
C2 H2c2 . . 0.96 ?
C3 C17 . . 1.373(3) ?
C3 C37 . . 1.412(4) ?
C3 H1c3 . . 0.96 ?
C4 C7 . . 1.371(4) ?
C4 C35 . . 1.411(3) ?
C4 H1c4 . . 0.96 ?
C5 C11 . . 1.530(3) ?
C5 C17 . . 1.509(3) ?
C5 H1c5 . . 0.96 ?
C5 H2c5 . . 0.96 ?
C6 C49 . . 1.489(3) ?
C7 C26 . . 1.512(3) ?
C7 C51 . . 1.437(3) ?
C8 C9 . . 1.372(4) ?
C8 C40 . . 1.412(3) ?
C8 H1c8 . . 0.96 ?
C9 C19 . . 1.512(3) ?
C9 C32 . . 1.433(3) ?
C10 C13 . . 1.414(3) ?
C10 C28 . . 1.416(3) ?
C10 C34 . . 1.435(3) ?
C11 H1c11 . . 0.96 ?
C11 H2c11 . . 0.96 ?
C12 C14 . . 1.375(3) ?
C12 C22 . . 1.507(3) ?
C12 C44 . . 1.426(3) ?
C13 C36 . . 1.366(3) ?
C13 H1c13 . . 0.96 ?
C14 C29 . . 1.413(4) ?
C14 H1c14 . . 0.96 ?
C15 C39 . . 1.367(4) ?
C15 C42 . . 1.412(3) ?
C15 H1c15 . . 0.96 ?
C16 C18 . . 1.367(4) ?
C16 C45 . . 1.412(3) ?
C16 H1c16 . . 0.96 ?
C17 C34 . . 1.426(3) ?
C18 C41 . . 1.413(3) ?
C18 H1c18 . . 0.96 ?
C19 H1c19 . . 0.96 ?
C19 H2c19 . . 0.96 ?
C20 C48 . . 1.493(3) ?
C21 C22 . . 1.531(3) ?
C21 H1c21 . . 0.96 ?
C21 H2c21 . . 0.96 ?
C22 H1c22 . . 0.96 ?
C22 H2c22 . . 0.96 ?
C23 C25 . . 1.420(3) ?
C23 C27 . . 1.413(3) ?
C23 C44 . . 1.434(3) ?
C24 C25 . . 1.364(3) ?
C24 C57 . . 1.413(4) ?
C24 H1c24 . . 0.96 ?
C25 H1c25 . . 0.96 ?
C26 H1c26 . . 0.96 ?
C26 H2c26 . . 0.96 ?
C27 C29 . . 1.360(3) ?
C27 H1c27 . . 0.96 ?
C28 C37 . . 1.361(3) ?
C28 H1c28 . . 0.96 ?
C29 H1c29 . . 0.96 ?
C30 C43 . . 1.489(3) ?
C31 C50 . . 1.489(3) ?
C32 C42 . . 1.428(3) ?
C32 C52 . . 1.417(4) ?
C33 C35 . . 1.363(3) ?
C33 C45 . . 1.415(4) ?
C33 H1c33 . . 0.96 ?
C34 C46 . . 1.416(3) ?
C35 H1c35 . . 0.96 ?
C36 C55 . . 1.411(4) ?
C36 H1c36 . . 0.96 ?
C37 H1c37 . . 0.96 ?
C38 C40 . . 1.366(3) ?
C38 C42 . . 1.412(4) ?
C38 H1c38 . . 0.96 ?
C39 C47 . . 1.408(3) ?
C39 H1c39 . . 0.96 ?
C40 H1c40 . . 0.96 ?
C41 C53 . . 1.375(3) ?
C43 H1c43 . . 0.96 ?
C43 H2c43 . . 0.96 ?
C43 H3c43 . . 0.96 ?
C44 C54 . . 1.417(3) ?
C45 C51 . . 1.430(3) ?
C46 C55 . . 1.371(3) ?
C46 H1c46 . . 0.96 ?
C47 C52 . . 1.375(3) ?
C48 H1c48 . . 0.96 ?
C48 H2c48 . . 0.96 ?
C48 H3c48 . . 0.96 ?
C49 H1c49 . . 0.96 ?
C49 H2c49 . . 0.96 ?
C49 H3c49 . . 0.96 ?
C50 H1c50 . . 0.96 ?
C50 H2c50 . . 0.96 ?
C50 H3c50 . . 0.96 ?
C51 C53 . . 1.413(4) ?
C52 H1c52 . . 0.96 ?
C53 H1c53 . . 0.96 ?
C54 C57 . . 1.372(3) ?
C54 H1c54 . . 0.96 ?
C56 H1c56 . . 0.96 ?
C56 H2c56 . . 0.96 ?
C56 H3c56 . . 0.96 ?
C58 H1c58 . . 0.96 ?
C58 H2c58 . . 0.96 ?
C58 H3c58 . . 0.96 ?
C59 H1c59 . . 0.96 ?
C59 H2c59 . . 0.96 ?
C59 H3c59 . . 0.96 ?
C60 H1c60 . . 0.96 ?
C60 H2c60 . . 0.96 ?
C60 H3c60 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 I5 N3 . . 2_765 143.62(4) ?
N4 I6 N2 . . 1_455 144.31(4) ?
C55 O1 C56 . . . 118.04(19) ?
C57 O2 C58 . . . 118.19(19) ?
C30 O3 H1o3o5 . . . 114.8(7) ?
C47 O4 C60 . . . 117.83(18) ?
C6 O5 H1o3o5 . . . 112.4(7) ?
C31 O6 H1o6 . . . 114.52(16) ?
I5 N1 C20 . . . 116.70(16) ?
I5 N1 C21 . . . 114.14(13) ?
I5 N1 H1n1 . . . 15.1(17) ?
C20 N1 C21 . . . 123.53(19) ?
C20 N1 H1n1 . . . 117.4(17) ?
C21 N1 H1n1 . . . 118.1(17) ?
C41 O8 C59 . . . 118.27(18) ?
C20 O7 H1o7 . . . 113.56(16) ?
I5 N3 C11 2_765 . . 81.58(11) ?
I5 N3 C31 2_765 . . 153.07(17) ?
I5 N3 H1n3 2_765 . . 35.6(17) ?
C11 N3 C31 . . . 123.50(19) ?
C11 N3 H1n3 . . . 116.9(17) ?
C31 N3 H1n3 . . . 119.3(17) ?
I6 N4 C1 . . . 113.03(14) ?
I6 N4 C6 . . . 118.25(13) ?
I6 N4 H1n4 . . . 19.7(17) ?
C1 N4 C6 . . . 123.55(17) ?
C1 N4 H1n4 . . . 120.0(16) ?
C6 N4 H1n4 . . . 116.3(16) ?
I6 N2 C2 1_655 . . 82.80(13) ?
I6 N2 C30 1_655 . . 151.87(13) ?
I6 N2 H1n2 1_655 . . 39.7(16) ?
C2 N2 C30 . . . 123.22(17) ?
C2 N2 H1n2 . . . 120.7(16) ?
C30 N2 H1n2 . . . 116.1(16) ?
N4 C1 C19 . . . 111.44(18) ?
N4 C1 H1c1 . . . 109.47 ?
N4 C1 H2c1 . . . 109.47 ?
C19 C1 H1c1 . . . 109.47 ?
C19 C1 H2c1 . . . 109.47 ?
H1c1 C1 H2c1 . . . 107.43 ?
N2 C2 C26 . . . 111.56(18) ?
N2 C2 H1c2 . . . 109.47 ?
N2 C2 H2c2 . . . 109.47 ?
C26 C2 H1c2 . . . 109.47 ?
C26 C2 H2c2 . . . 109.47 ?
H1c2 C2 H2c2 . . . 107.3 ?
C17 C3 C37 . . . 121.5(2) ?
C17 C3 H1c3 . . . 119.25 ?
C37 C3 H1c3 . . . 119.25 ?
C7 C4 C35 . . . 121.5(2) ?
C7 C4 H1c4 . . . 119.24 ?
C35 C4 H1c4 . . . 119.24 ?
C11 C5 C17 . . . 110.9(2) ?
C11 C5 H1c5 . . . 109.47 ?
C11 C5 H2c5 . . . 109.47 ?
C17 C5 H1c5 . . . 109.47 ?
C17 C5 H2c5 . . . 109.47 ?
H1c5 C5 H2c5 . . . 107.99 ?
O5 C6 N4 . . . 119.10(19) ?
O5 C6 C49 . . . 121.5(2) ?
N4 C6 C49 . . . 119.36(18) ?
C4 C7 C26 . . . 119.78(19) ?
C4 C7 C51 . . . 119.6(2) ?
C26 C7 C51 . . . 120.6(2) ?
C9 C8 C40 . . . 121.7(2) ?
C9 C8 H1c8 . . . 119.14 ?
C40 C8 H1c8 . . . 119.14 ?
C8 C9 C19 . . . 119.87(19) ?
C8 C9 C32 . . . 119.4(2) ?
C19 C9 C32 . . . 120.7(2) ?
C13 C10 C28 . . . 122.1(2) ?
C13 C10 C34 . . . 118.62(19) ?
C28 C10 C34 . . . 119.2(2) ?
N3 C11 C5 . . . 111.7(2) ?
N3 C11 H1c11 . . . 109.47 ?
N3 C11 H2c11 . . . 109.47 ?
C5 C11 H1c11 . . . 109.47 ?
C5 C11 H2c11 . . . 109.47 ?
H1c11 C11 H2c11 . . . 107.1 ?
C14 C12 C22 . . . 119.4(2) ?
C14 C12 C44 . . . 119.5(2) ?
C22 C12 C44 . . . 121.03(18) ?
C10 C13 C36 . . . 121.8(2) ?
C10 C13 H1c13 . . . 119.08 ?
C36 C13 H1c13 . . . 119.08 ?
C12 C14 C29 . . . 121.6(2) ?
C12 C14 H1c14 . . . 119.18 ?
C29 C14 H1c14 . . . 119.18 ?
C39 C15 C42 . . . 121.8(2) ?
C39 C15 H1c15 . . . 119.09 ?
C42 C15 H1c15 . . . 119.09 ?
C18 C16 C45 . . . 122.0(2) ?
C18 C16 H1c16 . . . 119.02 ?
C45 C16 H1c16 . . . 119.02 ?
C3 C17 C5 . . . 119.7(2) ?
C3 C17 C34 . . . 119.7(2) ?
C5 C17 C34 . . . 120.52(18) ?
C16 C18 C41 . . . 119.2(2) ?
C16 C18 H1c18 . . . 120.41 ?
C41 C18 H1c18 . . . 120.41 ?
C1 C19 C9 . . . 111.30(18) ?
C1 C19 H1c19 . . . 109.47 ?
C1 C19 H2c19 . . . 109.47 ?
C9 C19 H1c19 . . . 109.47 ?
C9 C19 H2c19 . . . 109.47 ?
H1c19 C19 H2c19 . . . 107.58 ?
N1 C20 O7 . . . 119.3(2) ?
N1 C20 C48 . . . 119.4(2) ?
O7 C20 C48 . . . 121.32(18) ?
N1 C21 C22 . . . 111.4(2) ?
N1 C21 H1c21 . . . 109.47 ?
N1 C21 H2c21 . . . 109.47 ?
C22 C21 H1c21 . . . 109.47 ?
C22 C21 H2c21 . . . 109.47 ?
H1c21 C21 H2c21 . . . 107.49 ?
C12 C22 C21 . . . 111.1(2) ?
C12 C22 H1c22 . . . 109.47 ?
C12 C22 H2c22 . . . 109.47 ?
C21 C22 H1c22 . . . 109.47 ?
C21 C22 H2c22 . . . 109.47 ?
H1c22 C22 H2c22 . . . 107.75 ?
C25 C23 C27 . . . 121.9(2) ?
C25 C23 C44 . . . 118.31(19) ?
C27 C23 C44 . . . 119.7(2) ?
C25 C24 C57 . . . 119.4(2) ?
C25 C24 H1c24 . . . 120.3 ?
C57 C24 H1c24 . . . 120.3 ?
C23 C25 C24 . . . 122.1(2) ?
C23 C25 H1c25 . . . 118.95 ?
C24 C25 H1c25 . . . 118.95 ?
C2 C26 C7 . . . 110.78(18) ?
C2 C26 H1c26 . . . 109.47 ?
C2 C26 H2c26 . . . 109.47 ?
C7 C26 H1c26 . . . 109.47 ?
C7 C26 H2c26 . . . 109.47 ?
H1c26 C26 H2c26 . . . 108.13 ?
C23 C27 C29 . . . 120.6(2) ?
C23 C27 H1c27 . . . 119.68 ?
C29 C27 H1c27 . . . 119.68 ?
C10 C28 C37 . . . 120.9(2) ?
C10 C28 H1c28 . . . 119.53 ?
C37 C28 H1c28 . . . 119.53 ?
C14 C29 C27 . . . 120.0(2) ?
C14 C29 H1c29 . . . 120.02 ?
C27 C29 H1c29 . . . 120.02 ?
O3 C30 N2 . . . 118.80(19) ?
O3 C30 C43 . . . 121.7(2) ?
N2 C30 C43 . . . 119.46(18) ?
O6 C31 N3 . . . 119.3(2) ?
O6 C31 C50 . . . 121.09(18) ?
N3 C31 C50 . . . 119.6(2) ?
C9 C32 C42 . . . 118.6(2) ?
C9 C32 C52 . . . 122.6(2) ?
C42 C32 C52 . . . 118.75(19) ?
C35 C33 C45 . . . 120.9(2) ?
C35 C33 H1c33 . . . 119.57 ?
C45 C33 H1c33 . . . 119.57 ?
C10 C34 C17 . . . 118.54(18) ?
C10 C34 C46 . . . 118.1(2) ?
C17 C34 C46 . . . 123.3(2) ?
C4 C35 C33 . . . 120.0(3) ?
C4 C35 H1c35 . . . 119.98 ?
C33 C35 H1c35 . . . 119.98 ?
C13 C36 C55 . . . 119.5(2) ?
C13 C36 H1c36 . . . 120.23 ?
C55 C36 H1c36 . . . 120.22 ?
C3 C37 C28 . . . 120.0(2) ?
C3 C37 H1c37 . . . 120.01 ?
C28 C37 H1c37 . . . 120.01 ?
C40 C38 C42 . . . 120.9(2) ?
C40 C38 H1c38 . . . 119.57 ?
C42 C38 H1c38 . . . 119.56 ?
C15 C39 C47 . . . 119.4(2) ?
C15 C39 H1c39 . . . 120.29 ?
C47 C39 H1c39 . . . 120.29 ?
C8 C40 C38 . . . 119.7(3) ?
C8 C40 H1c40 . . . 120.14 ?
C38 C40 H1c40 . . . 120.14 ?
O8 C41 C18 . . . 123.57(19) ?
O8 C41 C53 . . . 115.7(2) ?
C18 C41 C53 . . . 120.7(2) ?
C15 C42 C32 . . . 118.6(2) ?
C15 C42 C38 . . . 121.8(2) ?
C32 C42 C38 . . . 119.60(19) ?
C30 C43 H1c43 . . . 109.47 ?
C30 C43 H2c43 . . . 109.47 ?
C30 C43 H3c43 . . . 109.47 ?
H1c43 C43 H2c43 . . . 109.47 ?
H1c43 C43 H3c43 . . . 109.47 ?
H2c43 C43 H3c43 . . . 109.47 ?
C12 C44 C23 . . . 118.37(19) ?
C12 C44 C54 . . . 123.3(2) ?
C23 C44 C54 . . . 118.3(2) ?
C16 C45 C33 . . . 121.9(2) ?
C16 C45 C51 . . . 118.7(2) ?
C33 C45 C51 . . . 119.44(19) ?
C34 C46 C55 . . . 121.3(2) ?
C34 C46 H1c46 . . . 119.33 ?
C55 C46 H1c46 . . . 119.33 ?
O4 C47 C39 . . . 123.55(19) ?
O4 C47 C52 . . . 115.5(2) ?
C39 C47 C52 . . . 120.9(2) ?
C20 C48 H1c48 . . . 109.47 ?
C20 C48 H2c48 . . . 109.47 ?
C20 C48 H3c48 . . . 109.47 ?
H1c48 C48 H2c48 . . . 109.47 ?
H1c48 C48 H3c48 . . . 109.47 ?
H2c48 C48 H3c48 . . . 109.47 ?
C6 C49 H1c49 . . . 109.47 ?
C6 C49 H2c49 . . . 109.47 ?
C6 C49 H3c49 . . . 109.47 ?
H1c49 C49 H2c49 . . . 109.47 ?
H1c49 C49 H3c49 . . . 109.47 ?
H2c49 C49 H3c49 . . . 109.47 ?
C31 C50 H1c50 . . . 109.47 ?
C31 C50 H2c50 . . . 109.47 ?
C31 C50 H3c50 . . . 109.47 ?
H1c50 C50 H2c50 . . . 109.47 ?
H1c50 C50 H3c50 . . . 109.47 ?
H2c50 C50 H3c50 . . . 109.47 ?
C7 C51 C45 . . . 118.5(2) ?
C7 C51 C53 . . . 123.0(2) ?
C45 C51 C53 . . . 118.52(19) ?
C32 C52 C47 . . . 120.5(2) ?
C32 C52 H1c52 . . . 119.75 ?
C47 C52 H1c52 . . . 119.75 ?
C41 C53 C51 . . . 120.9(2) ?
C41 C53 H1c53 . . . 119.56 ?
C51 C53 H1c53 . . . 119.56 ?
C44 C54 C57 . . . 121.3(2) ?
C44 C54 H1c54 . . . 119.35 ?
C57 C54 H1c54 . . . 119.35 ?
O1 C55 C36 . . . 123.5(2) ?
O1 C55 C46 . . . 115.9(2) ?
C36 C55 C46 . . . 120.5(2) ?
O1 C56 H1c56 . . . 109.47 ?
O1 C56 H2c56 . . . 109.47 ?
O1 C56 H3c56 . . . 109.47 ?
H1c56 C56 H2c56 . . . 109.47 ?
H1c56 C56 H3c56 . . . 109.47 ?
H2c56 C56 H3c56 . . . 109.47 ?
O2 C57 C24 . . . 123.6(2) ?
O2 C57 C54 . . . 115.9(2) ?
C24 C57 C54 . . . 120.6(2) ?
O2 C58 H1c58 . . . 109.47 ?
O2 C58 H2c58 . . . 109.47 ?
O2 C58 H3c58 . . . 109.47 ?
H1c58 C58 H2c58 . . . 109.47 ?
H1c58 C58 H3c58 . . . 109.47 ?
H2c58 C58 H3c58 . . . 109.47 ?
O8 C59 H1c59 . . . 109.47 ?
O8 C59 H2c59 . . . 109.47 ?
O8 C59 H3c59 . . . 109.47 ?
H1c59 C59 H2c59 . . . 109.47 ?
H1c59 C59 H3c59 . . . 109.47 ?
H2c59 C59 H3c59 . . . 109.47 ?
O4 C60 H1c60 . . . 109.47 ?
O4 C60 H2c60 . . . 109.47 ?
O4 C60 H3c60 . . . 109.47 ?
H1c60 C60 H2c60 . . . 109.47 ?
H1c60 C60 H3c60 . . . 109.47 ?
H2c60 C60 H3c60 . . . 109.47 ?
O7 H1o7 O7 . . 2_665 180.0(5) ?
O3 H1o3o5 O5 . . . 177(2) ?
O6 H1o6 O6 . . 2_675 180.0(5) ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?

# start Validation Reply Form
_vrf_PLAT902_I                   
;
PROBLEM: No (Interpretable) Reflections found in FCF ....     Please Check
RESPONSE: Platon cannot read reflection files for twins
;
_vrf_PLAT434_I                   
;
PROBLEM: Short Inter HL..HL Contact I5     ..  I7      ..       3.41 Ang.  
RESPONSE: verified
;
# end Validation Reply Form

