# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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 2401516'
loop_
_audit_author_name
_audit_author_address
'Antonios Hatzidimitriou'
;Aristotle University of Thessaloniki
Greece
;
_audit_update_record             
;
2024-11-09 deposited with the CCDC.	2025-02-27 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                   8.2408(14)
_cell_length_b                   13.887(3)
_cell_length_c                   22.884(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2618.9(9)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-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'
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            8

# Given Formula = C15 H10 N2 O2 
# Dc =      1.27 Fooo =   1040.00 Mu =      0.86 M =    250.26
# Found Formula = C15 H12 N4 O1 
# Dc =      1.34 FOOO =   1104.00 Mu =      0.89 M =    264.29

_chemical_formula_sum            'C15 H12 N4 O1'
_chemical_formula_moiety         'C15 H12 N4 O1'
_chemical_compound_source        ?
_chemical_formula_weight         264.29


_cell_measurement_reflns_used    118
_cell_measurement_theta_min      10
_cell_measurement_theta_max      15
_cell_measurement_temperature    295

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.110
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.089

# Sheldrick geometric approximatio 0.99 0.99 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_T_max  0.99
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      295
_diffrn_reflns_number            23389
_reflns_number_total             2494
_diffrn_reflns_av_R_equivalents  0.031
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 2494 
# Theoretical number of reflections is about 4991 


_diffrn_reflns_theta_min         1.780
_diffrn_reflns_theta_max         25.753
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        25.753
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_reflns_limit_h_min              0
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              27

_oxford_diffrn_Wilson_B_factor   3.94
_oxford_diffrn_Wilson_scale      64.94

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

_refine_diff_density_min         -0.11
_refine_diff_density_max         0.12


# 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>2.0\s(I)
_refine_ls_number_reflns         1844
_refine_ls_number_restraints     0
_refine_ls_number_parameters     181
_oxford_refine_ls_R_factor_ref   0.0359
_refine_ls_wR_factor_ref         0.0568
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_shift/su_max          0.0005989
_refine_ls_shift/su_mean         0.0000731


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2485
_refine_ls_R_factor_all          0.0593
_refine_ls_wR_factor_all         0.0635

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1844
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_gt          0.0568

# 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, 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: 
 2.42 3.57 1.54 0.292 
;

# 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 0.77251(13) 0.44214(8) 0.54992(4) 0.0790 1.0000 Uani . . . . . .
N1 N 0.33749(12) 0.27972(8) 0.55399(4) 0.0501 1.0000 Uani . . . . . .
N2 N 0.08448(13) 0.20740(8) 0.53513(4) 0.0556 1.0000 Uani . . . . . .
N3 N 0.44805(12) 0.29164(8) 0.64941(4) 0.0491 1.0000 Uani . . . . . .
N4 N 0.57992(12) 0.33954(8) 0.62357(4) 0.0486 1.0000 Uani . . . . . .
C1 C 0.21461(15) 0.25025(10) 0.51914(6) 0.0536 1.0000 Uani . . . . . .
C2 C 0.07231(14) 0.18854(8) 0.59521(5) 0.0445 1.0000 Uani . . . . . .
C3 C -0.06256(16) 0.13784(10) 0.61528(6) 0.0558 1.0000 Uani . . . . . .
C4 C -0.07920(17) 0.11742(10) 0.67343(6) 0.0605 1.0000 Uani . . . . . .
C5 C 0.03868(16) 0.14549(10) 0.71315(6) 0.0585 1.0000 Uani . . . . . .
C6 C 0.17250(15) 0.19469(9) 0.69392(5) 0.0495 1.0000 Uani . . . . . .
C7 C 0.19119(13) 0.21669(9) 0.63490(5) 0.0410 1.0000 Uani . . . . . .
C8 C 0.33504(13) 0.26622(8) 0.61371(5) 0.0414 1.0000 Uani . . . . . .
C9 C 0.69438(14) 0.35303(9) 0.66079(6) 0.0478 1.0000 Uani . . . . . .
C10 C 0.84533(15) 0.40195(9) 0.64849(5) 0.0454 1.0000 Uani . . . . . .
C11 C 0.88123(16) 0.44281(10) 0.59460(6) 0.0565 1.0000 Uani . . . . . .
C12 C 1.03116(19) 0.48550(11) 0.58507(7) 0.0697 1.0000 Uani . . . . . .
C13 C 1.14348(18) 0.48773(10) 0.62914(7) 0.0650 1.0000 Uani . . . . . .
C14 C 1.10967(17) 0.45125(10) 0.68330(7) 0.0610 1.0000 Uani . . . . . .
C15 C 0.96150(15) 0.40788(10) 0.69244(6) 0.0555 1.0000 Uani . . . . . .
H12 H 0.4276 0.3026 0.5369 0.0613 1.0000 Uiso R . . . . .
H11 H 0.6847 0.4152 0.5604 0.1190 1.0000 Uiso R . . . . .
H13 H 0.2289 0.2626 0.4778 0.0653 1.0000 Uiso R . . . . .
H31 H -0.1416 0.1187 0.5884 0.0656 1.0000 Uiso R . . . . .
H41 H -0.1703 0.0818 0.6868 0.0716 1.0000 Uiso R . . . . .
H51 H 0.0259 0.1306 0.7542 0.0692 1.0000 Uiso R . . . . .
H61 H 0.2572 0.2141 0.7200 0.0580 1.0000 Uiso R . . . . .
H91 H 0.6785 0.3300 0.7000 0.0590 1.0000 Uiso R . . . . .
H121 H 1.0516 0.5122 0.5487 0.0851 1.0000 Uiso R . . . . .
H131 H 1.2463 0.5159 0.6226 0.0783 1.0000 Uiso R . . . . .
H141 H 1.1884 0.4557 0.7145 0.0734 1.0000 Uiso R . . . . .
H151 H 0.9358 0.3795 0.7300 0.0657 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.12648(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
O1 . C11 . 1.3596(17) yes
O1 . H11 . 0.850 no
N1 . C1 . 1.3523(16) yes
N1 . C8 . 1.3796(15) yes
N1 . H12 . 0.897 no
N2 . C1 . 1.2798(16) yes
N2 . C2 . 1.4031(16) yes
N3 . N4 . 1.4046(14) yes
N3 . C8 . 1.2882(15) yes
N4 . C9 . 1.2847(15) yes
C1 . H13 . 0.968 no
C2 . C3 . 1.3935(17) yes
C2 . C7 . 1.3920(16) yes
C3 . C4 . 1.367(2) yes
C3 . H31 . 0.935 no
C4 . C5 . 1.3864(19) yes
C4 . H41 . 0.950 no
C5 . C6 . 1.3700(18) yes
C5 . H51 . 0.967 no
C6 . C7 . 1.3932(16) yes
C6 . H61 . 0.958 no
C7 . C8 . 1.4538(16) yes
C9 . C10 . 1.4451(17) yes
C9 . H91 . 0.961 no
C10 . C11 . 1.3893(18) yes
C10 . C15 . 1.3911(18) yes
C11 . C12 . 1.3877(19) yes
C12 . C13 . 1.369(2) yes
C12 . H121 . 0.926 no
C13 . C14 . 1.368(2) yes
C13 . H131 . 0.945 no
C14 . C15 . 1.3775(19) yes
C14 . H141 . 0.966 no
C15 . H151 . 0.968 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
C11 . O1 . H11 . 110.5 no
C1 . N1 . C8 . 122.14(11) yes
C1 . N1 . H12 . 118.1 no
C8 . N1 . H12 . 119.4 no
C1 . N2 . C2 . 115.26(11) yes
N4 . N3 . C8 . 114.97(10) yes
N3 . N4 . C9 . 110.98(10) yes
N1 . C1 . N2 . 126.84(12) yes
N1 . C1 . H13 . 115.5 no
N2 . C1 . H13 . 117.6 no
N2 . C2 . C3 . 118.31(11) yes
N2 . C2 . C7 . 122.46(11) yes
C3 . C2 . C7 . 119.22(11) yes
C2 . C3 . C4 . 120.36(13) yes
C2 . C3 . H31 . 118.8 no
C4 . C3 . H31 . 120.8 no
C3 . C4 . C5 . 120.63(13) yes
C3 . C4 . H41 . 120.1 no
C5 . C4 . H41 . 119.2 no
C4 . C5 . C6 . 119.58(12) yes
C4 . C5 . H51 . 120.0 no
C6 . C5 . H51 . 120.4 no
C5 . C6 . C7 . 120.65(12) yes
C5 . C6 . H61 . 121.8 no
C7 . C6 . H61 . 117.5 no
C6 . C7 . C2 . 119.55(11) yes
C6 . C7 . C8 . 121.15(11) yes
C2 . C7 . C8 . 119.28(10) yes
C7 . C8 . N1 . 114.00(10) yes
C7 . C8 . N3 . 120.50(10) yes
N1 . C8 . N3 . 125.49(11) yes
N4 . C9 . C10 . 124.85(12) yes
N4 . C9 . H91 . 118.1 no
C10 . C9 . H91 . 117.1 no
C9 . C10 . C11 . 123.25(12) yes
C9 . C10 . C15 . 118.64(12) yes
C11 . C10 . C15 . 118.11(12) yes
C10 . C11 . O1 . 121.63(12) yes
C10 . C11 . C12 . 120.24(13) yes
O1 . C11 . C12 . 118.13(13) yes
C11 . C12 . C13 . 119.72(14) yes
C11 . C12 . H121 . 118.3 no
C13 . C12 . H121 . 121.9 no
C12 . C13 . C14 . 121.42(14) yes
C12 . C13 . H131 . 119.9 no
C14 . C13 . H131 . 118.7 no
C13 . C14 . C15 . 118.69(14) yes
C13 . C14 . H141 . 120.6 no
C15 . C14 . H141 . 120.7 no
C10 . C15 . C14 . 121.74(14) yes
C10 . C15 . H151 . 117.8 no
C14 . C15 . H151 . 120.5 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
N1 . H12 . N2 4_556 146 0.90 2.10 2.8869(19) yes
O1 . H11 . N4 . 144 0.85 1.98 2.7185(19) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
####################################################################### 
# 
# 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 2401518'
loop_
_audit_author_name
_audit_author_address
'Antonios Hatzidimitriou'
;Aristotle University of Thessaloniki
Greece
;
_audit_update_record             
;
2024-11-09 deposited with the CCDC.	2025-02-27 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                   19.931(3)
_cell_length_b                   19.931(3)
_cell_length_c                   20.830(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8275(3)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z+1/2
-x+1/2,-y+1/2,-z+1/2
-y+3/4,x+1/4,z+1/4
y+3/4,-x+1/4,-z+1/4
-y+5/4,x+3/4,z+3/4
y+5/4,-x+3/4,-z+3/4
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
-x+1,-y+1/2,z+1
x+1,y+1/2,-z+1
y+3/4,-x+3/4,z+3/4
-y+3/4,x+3/4,-z+3/4
y+5/4,-x+5/4,z+5/4
-y+5/4,x+5/4,-z+5/4

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'
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'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C75 H75 Cu7.50 N15 O15 
# Dc =      1.53 Fooo =   3870.00 Mu =     19.60 M =   1903.11
# Found Formula = C72 H84 Cu4 N20 O16 
# Dc =      1.40 FOOO =   3600.00 Mu =     10.88 M =   1739.77

_chemical_formula_sum            'C72 H84 Cu4 N20 O16'
_chemical_formula_moiety         'C72 H84 Cu4 N20 O16'
_chemical_compound_source        ?
_chemical_formula_weight         1739.77


_cell_measurement_reflns_used    218
_cell_measurement_theta_min      10
_cell_measurement_theta_max      20
_cell_measurement_temperature    295

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_size_min          0.120
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_max          0.180

_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3600
_exptl_absorpt_coefficient_mu    1.088

# Sheldrick geometric approximatio 0.83 0.88 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.88
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      295
_diffrn_reflns_number            13533
_reflns_number_total             3963
_diffrn_reflns_av_R_equivalents  0.040
# Number of reflections without Friedels Law is 13752 
# Number of reflections with Friedels Law is 3963 
# Theoretical number of reflections is about 3953 


_diffrn_reflns_theta_min         1.414
_diffrn_reflns_theta_max         25.741
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        25.741
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_reflns_limit_h_min              -16
_reflns_limit_h_max              17
_reflns_limit_k_min              0
_reflns_limit_k_max              24
_reflns_limit_l_min              0
_reflns_limit_l_max              25

_oxford_diffrn_Wilson_B_factor   2.90
_oxford_diffrn_Wilson_scale      655.84

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

_refine_diff_density_min         -0.49
_refine_diff_density_max         0.39


# 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>2.0\s(I)
_refine_ls_number_reflns         2721
_refine_ls_number_restraints     28
_refine_ls_number_parameters     250
_oxford_refine_ls_R_factor_ref   0.0577
_refine_ls_wR_factor_ref         0.0965
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_shift/su_max          0.0007110
_refine_ls_shift/su_mean         0.0000249


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3947
_refine_ls_R_factor_all          0.0966
_refine_ls_wR_factor_all         0.1050

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2721
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_gt          0.0965

# 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, 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: 
 3.26 3.86 1.44 
;

# 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
Cu1 Cu 0.62077(5) 0.63771(6) 0.54185(5) 0.0397 1.0000 Uani . . . . . .
N1 N 0.5273(3) 0.6131(3) 0.5595(3) 0.0374 1.0000 Uani D . . . . .
N2 N 0.4283(4) 0.6091(3) 0.6210(3) 0.0382 1.0000 Uani . . . . . .
N3 N 0.5290(3) 0.5790(3) 0.4538(3) 0.0384 1.0000 Uani . . . . . .
N4 N 0.5945(3) 0.5975(3) 0.4593(3) 0.0362 1.0000 Uani . . . . . .
N5 N 0.6044(7) 0.7832(7) 0.3985(6) 0.066(5) 0.5000 Uiso D . . . 2 .
N6 N 0.6369(7) 0.7719(7) 0.3916(6) 0.057(5) 0.5000 Uiso D . . . 3 .
O1 O 0.7132(3) 0.6456(3) 0.5199(3) 0.0455 1.0000 Uani . . . . . .
O2 O 0.5672(7) 0.7505(5) 0.4964(5) 0.042(3) 0.5000 Uiso D . . . 2 .
O3 O 0.7784(3) 0.7612(3) 0.5741(3) 0.0574 1.0000 Uani . . . . . .
O4 O 1.00000(2) 0.75000(2) 0.4279(6) 0.0858 1.0000 Uani S T . . . .
O5 O 0.5964(7) 0.7546(6) 0.4892(6) 0.050(4) 0.5000 Uiso D . . . 3 .
O6 O 0.9001(9) 0.7926(8) 0.5145(8) 0.079(5) 0.5000 Uiso . . . . . .
C1 C 0.4933(4) 0.6223(4) 0.6140(4) 0.0387 1.0000 Uani . . . . . .
C2 C 0.3938(4) 0.5888(4) 0.5700(4) 0.0362 1.0000 Uani . . . . . .
C3 C 0.3236(5) 0.5799(4) 0.5757(4) 0.0433 1.0000 Uani . . . . . .
C4 C 0.2874(5) 0.5586(5) 0.5231(5) 0.0467 1.0000 Uani . . . . . .
C5 C 0.3175(4) 0.5460(4) 0.4653(4) 0.0424 1.0000 Uani . . . . . .
C6 C 0.3863(4) 0.5541(4) 0.4607(4) 0.0410 1.0000 Uani . . . . . .
C7 C 0.4246(4) 0.5756(4) 0.5110(4) 0.0359 1.0000 Uani . . . . . .
C8 C 0.4947(4) 0.5884(4) 0.5067(4) 0.0357 1.0000 Uani . . . . . .
C9 C 0.6350(4) 0.5879(4) 0.4113(4) 0.0398 1.0000 Uani . . . . . .
C10 C 0.7027(5) 0.6043(4) 0.4094(4) 0.0437 1.0000 Uani . . . . . .
C11 C 0.7391(5) 0.6296(5) 0.4647(4) 0.0443 1.0000 Uani . . . . . .
C12 C 0.8077(5) 0.6407(5) 0.4549(5) 0.0504 1.0000 Uani . . . . . .
C13 C 0.8425(5) 0.6297(5) 0.3978(5) 0.0539 1.0000 Uani . . . . . .
C14 C 0.8063(5) 0.6062(5) 0.3460(5) 0.0528 1.0000 Uani . . . . . .
C15 C 0.7382(5) 0.5929(5) 0.3532(5) 0.0474 1.0000 Uani D . . . . .
C16 C 0.5575(7) 0.7681(7) 0.4395(5) 0.068(6) 0.5000 Uiso D . . . 2 .
C17 C 0.6762(7) 0.7812(8) 0.4144(9) 0.062(6) 0.5000 Uiso D . . . 2 .
C18 C 0.5850(11) 0.8046(8) 0.3336(6) 0.075(7) 0.5000 Uiso D . . . 2 .
C19 C 0.6439(7) 0.7716(7) 0.4536(6) 0.051(5) 0.5000 Uiso D . . . 3 .
C20 C 0.5731(7) 0.7513(8) 0.3621(9) 0.064(6) 0.5000 Uiso D . . . 3 .
C21 C 0.6945(8) 0.7930(8) 0.3523(9) 0.067(6) 0.5000 Uiso D . . . 3 .
H11 H 0.5163 0.6382 0.6488 0.0471 1.0000 Uiso R . . . . .
H31 H 0.3022 0.5888 0.6138 0.0524 1.0000 Uiso R . . . . .
H32 H 0.7577 0.7287 0.5565 0.0907 1.0000 Uiso R . . . . .
H41 H 0.2411 0.5530 0.5271 0.0573 1.0000 Uiso R . . . . .
H42 H 0.9688 0.7301 0.4473 0.1041 1.0000 Uiso R . . . . .
H51 H 0.2924 0.5325 0.4306 0.0525 1.0000 Uiso R . . . . .
H61 H 0.8581 0.7932 0.5095 0.1053 0.5000 Uiso R . . . . .
H62 H 0.9149 0.7942 0.4765 0.1051 0.5000 Uiso R . . . . .
H91 H 0.6161 0.5677 0.3747 0.0491 1.0000 Uiso R . . . . .
H121 H 0.8320 0.6558 0.4903 0.0636 1.0000 Uiso R . . . . .
H131 H 0.8884 0.6388 0.3945 0.0689 1.0000 Uiso R . . . . .
H141 H 0.8269 0.5980 0.3064 0.0660 1.0000 Uiso R . . . . .
H151 H 0.7154 0.5756 0.3179 0.0585 1.0000 Uiso R . . . . .
H161 H 0.5131 0.7702 0.4242 0.0872 0.5000 Uiso R . . . 2 .
H171 H 0.7027 0.7975 0.3787 0.0999 0.5000 Uiso R . . . 2 .
H172 H 0.6895 0.7357 0.4241 0.1002 0.5000 Uiso R . . . 2 .
H173 H 0.6849 0.8091 0.4515 0.1001 0.5000 Uiso R . . . 2 .
H181 H 0.5979 0.8513 0.3272 0.1211 0.5000 Uiso R . . . 2 .
H182 H 0.5366 0.7996 0.3287 0.1211 0.5000 Uiso R . . . 2 .
H183 H 0.6085 0.7767 0.3028 0.1211 0.5000 Uiso R . . . 2 .
H191 H 0.6840 0.7851 0.4726 0.0631 0.5000 Uiso R . . . 3 .
H201 H 0.5587 0.7086 0.3789 0.0980 0.5000 Uiso R . . . 3 .
H202 H 0.5788 0.7468 0.3164 0.0982 0.5000 Uiso R . . . 3 .
H203 H 0.5380 0.7838 0.3708 0.0977 0.5000 Uiso R . . . 3 .
H211 H 0.6894 0.7765 0.3091 0.1080 0.5000 Uiso R . . . 3 .
H212 H 0.6967 0.8411 0.3520 0.1080 0.5000 Uiso R . . . 3 .
H213 H 0.7357 0.7760 0.3702 0.1078 0.5000 Uiso R . . . 3 .
H214 H 0.4075 0.5453 0.4221 0.0505 1.0000 Uiso R . . . . .
H215 H 0.8030 0.7471 0.6052 0.0908 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.051595(18)
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
Cu1 . N2 16_545 2.027(7) yes
Cu1 . N1 . 1.962(7) yes
Cu1 . N4 . 1.967(7) yes
Cu1 . O1 . 1.905(6) yes
Cu1 . O2 . 2.663(11) yes
N1 . C1 . 1.333(10) yes
N1 . C8 . 1.370(10) yes
N2 . C1 . 1.330(11) yes
N2 . C2 . 1.330(11) yes
N3 . N4 . 1.363(9) yes
N3 . C8 . 1.308(10) yes
N4 . C9 . 1.299(10) yes
N5 . C16 . 1.300(2) yes
N5 . C17 . 1.470(2) yes
N5 . C18 . 1.470(2) yes
N6 . C19 . 1.300(2) yes
N6 . C20 . 1.470(2) yes
N6 . C21 . 1.470(2) yes
O1 . C11 . 1.300(10) yes
O2 . C16 . 1.250(2) yes
O3 . H32 . 0.850 no
O3 . H215 . 0.860 no
O4 . H42 11_664 0.842 no
O4 . H42 . 0.842 no
O5 . C19 . 1.249(2) yes
O6 . H61 . 0.845 no
O6 . H62 . 0.846 no
C1 . H11 . 0.916 no
C2 . C3 . 1.416(12) yes
C2 . C7 . 1.397(11) yes
C3 . C4 . 1.378(13) yes
C3 . H31 . 0.919 no
C4 . C5 . 1.368(12) yes
C4 . H41 . 0.933 no
C5 . C6 . 1.384(12) yes
C5 . H51 . 0.920 no
C6 . C7 . 1.365(12) yes
C6 . H214 . 0.925 no
C7 . C8 . 1.423(12) yes
C9 . C10 . 1.389(12) yes
C9 . H91 . 0.941 no
C10 . C11 . 1.451(13) yes
C10 . C15 . 1.387(12) yes
C11 . C12 . 1.401(12) yes
C12 . C13 . 1.394(13) yes
C12 . H121 . 0.932 no
C13 . C14 . 1.381(14) yes
C13 . H131 . 0.934 no
C14 . C15 . 1.391(13) yes
C14 . H141 . 0.936 no
C15 . H151 . 0.931 no
C16 . H161 . 0.943 no
C17 . H171 . 0.968 no
C17 . H172 . 0.965 no
C17 . H173 . 0.968 no
C18 . H181 . 0.975 no
C18 . H182 . 0.975 no
C18 . H183 . 0.970 no
C19 . H191 . 0.932 no
C20 . H201 . 0.965 no
C20 . H202 . 0.963 no
C20 . H203 . 0.970 no
C21 . H211 . 0.963 no
C21 . H212 . 0.960 no
C21 . H213 . 0.964 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
N2 16_545 Cu1 . N1 . 96.9(3) yes
N2 16_545 Cu1 . N4 . 175.9(3) yes
N1 . Cu1 . N4 . 79.0(3) yes
N2 16_545 Cu1 . O1 . 89.5(3) yes
N1 . Cu1 . O1 . 169.9(3) yes
N4 . Cu1 . O1 . 94.6(3) yes
N2 16_545 Cu1 . O2 . 93.5(3) yes
N1 . Cu1 . O2 . 84.1(4) yes
N4 . Cu1 . O2 . 85.8(3) yes
O1 . Cu1 . O2 . 103.5(4) yes
Cu1 . N1 . C1 . 127.4(6) yes
Cu1 . N1 . C8 . 112.9(5) yes
C1 . N1 . C8 . 119.5(7) yes
Cu1 6_466 N2 . C1 . 116.7(6) yes
Cu1 6_466 N2 . C2 . 124.8(6) yes
C1 . N2 . C2 . 118.4(7) yes
N4 . N3 . C8 . 113.0(7) yes
N3 . N4 . Cu1 . 116.0(5) yes
N3 . N4 . C9 . 119.3(7) yes
Cu1 . N4 . C9 . 124.6(6) yes
C16 . N5 . C17 . 123.0(11) yes
C16 . N5 . C18 . 118.9(11) yes
C17 . N5 . C18 . 118.1(11) yes
C19 . N6 . C20 . 120.4(11) yes
C19 . N6 . C21 . 118.1(11) yes
C20 . N6 . C21 . 121.5(11) yes
Cu1 . O1 . C11 . 125.2(6) yes
Cu1 . O2 . C16 . 129.4(10) yes
H32 . O3 . H215 . 110.7 no
H42 11_664 O4 . H42 . 122.4 no
Cu1 . O5 . C19 . 110.4(9) yes
H61 . O6 . H62 . 103.3 no
N1 . C1 . N2 . 124.2(8) yes
N1 . C1 . H11 . 117.8 no
N2 . C1 . H11 . 118.0 no
N2 . C2 . C3 . 118.8(8) yes
N2 . C2 . C7 . 122.2(8) yes
C3 . C2 . C7 . 119.0(8) yes
C2 . C3 . C4 . 119.2(8) yes
C2 . C3 . H31 . 120.5 no
C4 . C3 . H31 . 120.3 no
C3 . C4 . C5 . 121.8(9) yes
C3 . C4 . H41 . 118.9 no
C5 . C4 . H41 . 119.3 no
C4 . C5 . C6 . 118.3(9) yes
C4 . C5 . H51 . 120.4 no
C6 . C5 . H51 . 121.3 no
C5 . C6 . C7 . 122.5(8) yes
C5 . C6 . H214 . 119.3 no
C7 . C6 . H214 . 118.1 no
C2 . C7 . C6 . 119.2(8) yes
C2 . C7 . C8 . 117.0(8) yes
C6 . C7 . C8 . 123.8(8) yes
C7 . C8 . N1 . 118.6(7) yes
C7 . C8 . N3 . 122.7(8) yes
N1 . C8 . N3 . 118.7(8) yes
N4 . C9 . C10 . 126.1(8) yes
N4 . C9 . H91 . 116.2 no
C10 . C9 . H91 . 117.7 no
C9 . C10 . C11 . 123.1(8) yes
C9 . C10 . C15 . 118.7(9) yes
C11 . C10 . C15 . 118.1(9) yes
C10 . C11 . O1 . 126.0(8) yes
C10 . C11 . C12 . 115.4(8) yes
O1 . C11 . C12 . 118.5(8) yes
C11 . C12 . C13 . 125.8(9) yes
C11 . C12 . H121 . 116.3 no
C13 . C12 . H121 . 117.9 no
C12 . C13 . C14 . 117.4(9) yes
C12 . C13 . H131 . 121.2 no
C14 . C13 . H131 . 121.4 no
C13 . C14 . C15 . 119.4(9) yes
C13 . C14 . H141 . 121.2 no
C15 . C14 . H141 . 119.4 no
C14 . C15 . C10 . 123.9(9) yes
C14 . C15 . H151 . 117.4 no
C10 . C15 . H151 . 118.7 no
N5 . C16 . O2 . 125.2(12) yes
N5 . C16 . H161 . 116.2 no
O2 . C16 . H161 . 118.6 no
N5 . C17 . H171 . 110.5 no
N5 . C17 . H172 . 109.9 no
H171 . C17 . H172 . 109.0 no
N5 . C17 . H173 . 109.8 no
H171 . C17 . H173 . 108.7 no
H172 . C17 . H173 . 108.8 no
N5 . C18 . H181 . 109.5 no
N5 . C18 . H182 . 109.1 no
H181 . C18 . H182 . 110.1 no
N5 . C18 . H183 . 108.3 no
H181 . C18 . H183 . 109.3 no
H182 . C18 . H183 . 110.5 no
N6 . C19 . O5 . 120.7(14) yes
N6 . C19 . H191 . 120.8 no
O5 . C19 . H191 . 118.5 no
N6 . C20 . H201 . 110.7 no
N6 . C20 . H202 . 109.7 no
H201 . C20 . H202 . 108.1 no
N6 . C20 . H203 . 111.1 no
H201 . C20 . H203 . 107.9 no
H202 . C20 . H203 . 109.3 no
N6 . C21 . H211 . 109.8 no
N6 . C21 . H212 . 109.0 no
H211 . C21 . H212 . 109.8 no
N6 . C21 . H213 . 110.5 no
H211 . C21 . H213 . 109.4 no
H212 . C21 . H213 . 108.3 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
C1 . H11 . O2 6_466 142 0.92 2.38 3.153(15) yes
C1 . H11 . O5 6_466 141 0.92 2.37 3.131(15) yes
O3 . H32 . O1 . 175 0.85 2.03 2.877(15) yes
O6 . H61 . O3 . 130 0.84 2.18 2.796(15) yes
O6 . H62 . O4 . 134 0.85 2.16 2.819(15) yes
C16 . H161 . C16 11_564 136 0.94 1.63 2.404(15) yes
C16 . H161 . C20 11_564 158 0.94 2.19 3.087(15) yes
C17 . H172 . C11 . 169 0.97 2.48 3.434(15) yes
C18 . H182 . C20 11_564 151 0.98 2.51 3.396(15) yes
O3 . H215 . N3 15_454 157 0.86 2.18 2.993(15) yes


# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
####################################################################### 
# 
# 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 2401517'
loop_
_audit_author_name
_audit_author_address
'Antonios Hatzidimitriou'
;Aristotle University of Thessaloniki
Greece
;
_audit_update_record             
;
2024-11-09 deposited with the CCDC.	2025-02-27 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                   20.8047(10)
_cell_length_b                   11.9286(8)
_cell_length_c                   26.7212(12)
_cell_angle_alpha                90
_cell_angle_beta                 111.086(7)
_cell_angle_gamma                90
_cell_volume                     6187.4(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  ?
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
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 0.0033 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'
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'
Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C57.50 H57.50 N11.50 O11.50 Zn5.75 
# Dc =      1.58 Fooo =   2990.00 Mu =     22.62 M =   1469.59
# Found Formula = C63 H58 N16 O8 Zn2 
# Dc =      1.39 FOOO =   2688.00 Mu =      8.44 M =   1298.02

_chemical_formula_sum            'C63 H58 N16 O8 Zn2'
_chemical_formula_moiety         'C63 H58 N16 O8 Zn2'
_chemical_compound_source        ?
_chemical_formula_weight         1298.02


_cell_measurement_reflns_used    274
_cell_measurement_theta_min      10
_cell_measurement_theta_max      20
_cell_measurement_temperature    295

_exptl_crystal_description       bar
_exptl_crystal_colour            colorless
_exptl_crystal_size_min          0.020
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2688
_exptl_absorpt_coefficient_mu    0.844

# Sheldrick geometric approximatio 0.97 0.98 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_T_max  0.98
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      295
_diffrn_reflns_number            65715
_reflns_number_total             11348
_diffrn_reflns_av_R_equivalents  0.062
# Number of reflections without Friedels Law is 11350 
# Number of reflections with Friedels Law is 11348 
# Theoretical number of reflections is about 11581 


_diffrn_reflns_theta_min         1.073
_diffrn_reflns_theta_max         25.548
_diffrn_measured_fraction_theta_max 0.979

_diffrn_reflns_theta_full        25.037
_diffrn_measured_fraction_theta_full 0.988


_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_reflns_limit_h_min              -25
_reflns_limit_h_max              23
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              32

_oxford_diffrn_Wilson_B_factor   2.26
_oxford_diffrn_Wilson_scale      565.57

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

_refine_diff_density_min         -0.39
_refine_diff_density_max         0.43


# 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>2.0\s(I)
_refine_ls_number_reflns         8368
_refine_ls_number_restraints     0
_refine_ls_number_parameters     802
_oxford_refine_ls_R_factor_ref   0.0497
_refine_ls_wR_factor_ref         0.0679
_refine_ls_goodness_of_fit_ref   1.0000
_refine_ls_shift/su_max          0.0009415
_refine_ls_shift/su_mean         0.0000362


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11291
_refine_ls_R_factor_all          0.0868
_refine_ls_wR_factor_all         0.0925

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8368
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_gt          0.0679

# 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

# WARNING. The IUCr will not accept pure Unit Weights for F-squared refinements 
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./4Fsq 
;

# 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
Zn1 Zn 0.71967(2) 0.56796(3) 0.657219(16) 0.0352 1.0000 Uani . . . . . .
Zn2 Zn 0.83244(2) 0.34551(3) 0.333291(15) 0.0370 1.0000 Uani . . . . . .
N1 N 0.67834(15) 0.6686(2) 0.71126(10) 0.0362 1.0000 Uani . . . . . .
N2 N 0.65554(14) 0.8270(2) 0.75404(10) 0.0378 1.0000 Uani . . . . . .
N3 N 0.63525(15) 0.4927(2) 0.72517(11) 0.0367 1.0000 Uani . . . . . .
N4 N 0.66844(14) 0.4531(2) 0.68941(10) 0.0339 1.0000 Uani . . . . . .
N5 N 0.62985(15) 0.6358(2) 0.58938(11) 0.0387 1.0000 Uani . . . . . .
N6 N 0.51606(17) 0.6499(3) 0.52834(11) 0.0499 1.0000 Uani . . . . . .
N7 N 0.70931(16) 0.7804(2) 0.58989(11) 0.0397 1.0000 Uani . . . . . .
N8 N 0.75808(15) 0.7143(2) 0.63236(10) 0.0341 1.0000 Uani . . . . . .
N9 N 0.82129(15) 0.2410(2) 0.26000(10) 0.0347 1.0000 Uani . . . . . .
N10 N 0.80422(14) 0.0783(2) 0.20483(10) 0.0348 1.0000 Uani . . . . . .
N11 N 0.82769(15) 0.4171(2) 0.22104(10) 0.0356 1.0000 Uani . . . . . .
N12 N 0.83817(15) 0.4573(2) 0.27361(10) 0.0341 1.0000 Uani . . . . . .
N13 N 0.93962(15) 0.2940(2) 0.37515(10) 0.0367 1.0000 Uani . . . . . .
N14 N 1.06284(16) 0.3206(2) 0.41028(11) 0.0399 1.0000 Uani . . . . . .
N15 N 0.89280(16) 0.1392(2) 0.40283(10) 0.0380 1.0000 Uani . . . . . .
N16 N 0.82977(16) 0.1988(2) 0.37876(10) 0.0360 1.0000 Uani . . . . . .
O1 O 0.73111(12) 0.43439(18) 0.60908(8) 0.0375 1.0000 Uani . . . . . .
O2 O 0.81888(12) 0.54930(18) 0.71567(9) 0.0389 1.0000 Uani . . . . . .
O3 O 0.85504(13) 0.48136(17) 0.38673(8) 0.0382 1.0000 Uani . . . . . .
O4 O 0.72654(12) 0.35645(18) 0.31570(8) 0.0390 1.0000 Uani . . . . . .
O5 O 0.83053(16) 0.5273(3) 0.56799(11) 0.0738 1.0000 Uani . . . . . .
O6 O 0.85615(13) 0.4131(2) 0.48598(10) 0.0541 1.0000 Uani . . . . . .
O8 O 0.46650(13) 0.4264(2) 0.58749(10) 0.0559 1.0000 Uani . . . . . .
O88 O 0.62467(12) 0.4348(2) 0.50180(10) 0.0517 1.0000 Uani . . . . . .
C1 C 0.68528(18) 0.7770(3) 0.72352(13) 0.0359 1.0000 Uani . . . . . .
C2 C 0.61710(19) 0.7666(3) 0.77845(13) 0.0388 1.0000 Uani . . . . . .
C3 C 0.58718(18) 0.8215(3) 0.81077(13) 0.0418 1.0000 Uani . . . . . .
C4 C 0.54814(19) 0.7600(3) 0.83405(14) 0.0448 1.0000 Uani . . . . . .
C5 C 0.53870(19) 0.6451(3) 0.82305(13) 0.0442 1.0000 Uani . . . . . .
C6 C 0.56972(18) 0.5919(3) 0.79094(13) 0.0422 1.0000 Uani . . . . . .
C7 C 0.61062(18) 0.6508(3) 0.76828(13) 0.0375 1.0000 Uani . . . . . .
C8 C 0.64196(18) 0.6013(3) 0.73488(13) 0.0367 1.0000 Uani . . . . . .
C9 C 0.66456(17) 0.3457(3) 0.68367(12) 0.0359 1.0000 Uani . . . . . .
C10 C 0.69629(18) 0.2794(3) 0.65134(13) 0.0371 1.0000 Uani . . . . . .
C11 C 0.72681(19) 0.3253(3) 0.61688(13) 0.0383 1.0000 Uani . . . . . .
C12 C 0.75624(19) 0.2491(3) 0.59131(14) 0.0410 1.0000 Uani . . . . . .
C13 C 0.7560(2) 0.1332(3) 0.59812(14) 0.0461 1.0000 Uani . . . . . .
C14 C 0.72167(19) 0.0898(3) 0.63021(14) 0.0462 1.0000 Uani . . . . . .
C15 C 0.69272(19) 0.1631(3) 0.65730(13) 0.0429 1.0000 Uani . . . . . .
C16 C 0.5656(2) 0.5986(3) 0.56800(14) 0.0462 1.0000 Uani . . . . . .
C17 C 0.5283(2) 0.7498(3) 0.50557(15) 0.0504 1.0000 Uani . . . . . .
C18 C 0.4750(2) 0.8018(3) 0.46365(15) 0.0563 1.0000 Uani . . . . . .
C19 C 0.4852(2) 0.9016(3) 0.44029(16) 0.0578 1.0000 Uani . . . . . .
C20 C 0.5512(2) 0.9487(4) 0.46133(15) 0.0579 1.0000 Uani . . . . . .
C21 C 0.6028(2) 0.8970(3) 0.50437(15) 0.0537 1.0000 Uani . . . . . .
C22 C 0.5945(2) 0.7957(3) 0.52781(15) 0.0496 1.0000 Uani . . . . . .
C23 C 0.6453(2) 0.7364(3) 0.56905(13) 0.0404 1.0000 Uani . . . . . .
C24 C 0.81972(17) 0.7577(3) 0.65383(13) 0.0346 1.0000 Uani . . . . . .
C25 C 0.87843(18) 0.7086(3) 0.69663(13) 0.0352 1.0000 Uani . . . . . .
C26 C 0.87619(19) 0.6099(3) 0.72425(14) 0.0389 1.0000 Uani . . . . . .
C27 C 0.93807(18) 0.5780(3) 0.76493(14) 0.0450 1.0000 Uani . . . . . .
C28 C 0.9999(2) 0.6355(3) 0.77602(16) 0.0509 1.0000 Uani . . . . . .
C29 C 1.0012(2) 0.7323(3) 0.74696(15) 0.0491 1.0000 Uani . . . . . .
C30 C 0.93982(18) 0.7684(3) 0.70732(14) 0.0423 1.0000 Uani . . . . . .
C31 C 0.81214(18) 0.1322(3) 0.25148(12) 0.0355 1.0000 Uani . . . . . .
C32 C 0.80118(18) 0.1399(3) 0.15934(13) 0.0373 1.0000 Uani . . . . . .
C33 C 0.79119(18) 0.0840(3) 0.11091(13) 0.0413 1.0000 Uani . . . . . .
C34 C 0.79125(19) 0.1460(3) 0.06667(13) 0.0422 1.0000 Uani . . . . . .
C35 C 0.79619(19) 0.2633(3) 0.06975(13) 0.0413 1.0000 Uani . . . . . .
C36 C 0.80684(19) 0.3150(3) 0.11906(13) 0.0406 1.0000 Uani . . . . . .
C37 C 0.80899(19) 0.2562(3) 0.16523(13) 0.0371 1.0000 Uani . . . . . .
C38 C 0.81984(19) 0.3043(3) 0.21578(13) 0.0349 1.0000 Uani . . . . . .
C39 C 0.84983(17) 0.5656(3) 0.27836(12) 0.0351 1.0000 Uani . . . . . .
C40 C 0.86232(18) 0.6336(3) 0.32837(12) 0.0360 1.0000 Uani . . . . . .
C41 C 0.86631(19) 0.5902(3) 0.37817(13) 0.0385 1.0000 Uani . . . . . .
C42 C 0.87947(19) 0.6652(3) 0.42101(13) 0.0429 1.0000 Uani . . . . . .
C43 C 0.88617(19) 0.7803(3) 0.41475(13) 0.0399 1.0000 Uani . . . . . .
C44 C 0.8816(2) 0.8235(3) 0.36484(13) 0.0441 1.0000 Uani . . . . . .
C45 C 0.86910(19) 0.7488(3) 0.32180(13) 0.0401 1.0000 Uani . . . . . .
C46 C 0.99757(19) 0.3551(3) 0.38217(12) 0.0384 1.0000 Uani . . . . . .
C47 C 1.0726(2) 0.2114(3) 0.43084(13) 0.0404 1.0000 Uani . . . . . .
C48 C 1.1407(2) 0.1732(3) 0.45695(13) 0.0443 1.0000 Uani . . . . . .
C49 C 1.1508(2) 0.0630(3) 0.47527(13) 0.0463 1.0000 Uani . . . . . .
C50 C 1.0963(2) -0.0100(3) 0.47049(14) 0.0438 1.0000 Uani . . . . . .
C51 C 1.0299(2) 0.0340(3) 0.44544(14) 0.0440 1.0000 Uani . . . . . .
C52 C 1.01608(19) 0.1432(3) 0.42522(13) 0.0393 1.0000 Uani . . . . . .
C53 C 0.9499(2) 0.1904(3) 0.40048(13) 0.0375 1.0000 Uani . . . . . .
C54 C 0.77790(19) 0.1560(3) 0.38636(12) 0.0388 1.0000 Uani . . . . . .
C55 C 0.70649(19) 0.1986(3) 0.36529(13) 0.0388 1.0000 Uani . . . . . .
C56 C 0.6841(2) 0.2925(3) 0.33173(13) 0.0411 1.0000 Uani . . . . . .
C57 C 0.6142(2) 0.3215(3) 0.31331(14) 0.0431 1.0000 Uani . . . . . .
C58 C 0.5669(2) 0.2583(3) 0.32786(14) 0.0468 1.0000 Uani . . . . . .
C59 C 0.5869(2) 0.1628(3) 0.36015(14) 0.0476 1.0000 Uani . . . . . .
C60 C 0.6574(2) 0.1386(3) 0.37958(14) 0.0457 1.0000 Uani . . . . . .
C61 C 0.9218(2) 0.3662(4) 0.50997(16) 0.0595 1.0000 Uani . . . . . .
C63 C 0.4748(2) 0.3771(4) 0.63909(16) 0.0656 1.0000 Uani . . . . . .
C64 C 0.6535(2) 0.3653(4) 0.47103(16) 0.0658 1.0000 Uani . . . . . .
H11 H 0.7120 0.8202 0.7097 0.0428 1.0000 Uiso R . . . . .
H21 H 0.6593 0.8976 0.7582 0.0445 1.0000 Uiso R . . . . .
H31 H 0.5930 0.8986 0.8164 0.0497 1.0000 Uiso R . . . . .
H41 H 0.5283 0.7951 0.8560 0.0531 1.0000 Uiso R . . . . .
H51 H 0.8004 0.4990 0.5772 0.1078 1.0000 Uiso R . . . . .
H52 H 0.8244 0.5180 0.5363 0.1099 1.0000 Uiso R . . . . .
H61 H 0.4771 0.6200 0.5159 0.0597 1.0000 Uiso R . . . . .
H71 H 0.6966 0.3964 0.4714 0.0986 1.0000 Uiso R . . . . .
H72 H 0.6608 0.2913 0.4858 0.0987 1.0000 Uiso R . . . . .
H73 H 0.6210 0.3613 0.4349 0.0989 1.0000 Uiso R . . . . .
H81 H 0.4365 0.4685 0.5697 0.0839 1.0000 Uiso R . . . . .
H91 H 0.6402 0.3067 0.7008 0.0420 1.0000 Uiso R . . . . .
H101 H 0.8013 0.0069 0.2035 0.0419 1.0000 Uiso R . . . . .
H121 H 0.7772 0.2776 0.5686 0.0481 1.0000 Uiso R . . . . .
H131 H 0.7785 0.0853 0.5818 0.0546 1.0000 Uiso R . . . . .
H141 H 0.7175 0.0125 0.6332 0.0552 1.0000 Uiso R . . . . .
H151 H 0.6709 0.1345 0.6797 0.0502 1.0000 Uiso R . . . . .
H161 H 0.5546 0.5329 0.5820 0.0543 1.0000 Uiso R . . . . .
H181 H 0.4313 0.7687 0.4515 0.0663 1.0000 Uiso R . . . . .
H191 H 0.4500 0.9353 0.4119 0.0689 1.0000 Uiso R . . . . .
H201 H 0.5611 1.0144 0.4466 0.0685 1.0000 Uiso R . . . . .
H211 H 0.6454 0.9316 0.5181 0.0632 1.0000 Uiso R . . . . .
H241 H 0.8268 0.8268 0.6400 0.0409 1.0000 Uiso R . . . . .
H271 H 0.9377 0.5154 0.7853 0.0533 1.0000 Uiso R . . . . .
H281 H 1.0397 0.6093 0.8020 0.0607 1.0000 Uiso R . . . . .
H291 H 1.0415 0.7726 0.7539 0.0580 1.0000 Uiso R . . . . .
H301 H 0.9398 0.8335 0.6883 0.0504 1.0000 Uiso R . . . . .
H311 H 0.8124 0.0880 0.2803 0.0428 1.0000 Uiso R . . . . .
H331 H 0.7842 0.0065 0.1081 0.0496 1.0000 Uiso R . . . . .
H341 H 0.7876 0.1094 0.0354 0.0502 1.0000 Uiso R . . . . .
H351 H 0.7925 0.3053 0.0399 0.0494 1.0000 Uiso R . . . . .
H361 H 0.8131 0.3926 0.1215 0.0486 1.0000 Uiso R . . . . .
H391 H 0.8502 0.6040 0.2480 0.0415 1.0000 Uiso R . . . . .
H421 H 0.8828 0.6374 0.4541 0.0503 1.0000 Uiso R . . . . .
H431 H 0.8937 0.8285 0.4434 0.0473 1.0000 Uiso R . . . . .
H441 H 0.8867 0.9002 0.3603 0.0522 1.0000 Uiso R . . . . .
H451 H 0.8649 0.7765 0.2888 0.0474 1.0000 Uiso R . . . . .
H461 H 0.9922 0.4257 0.3662 0.0454 1.0000 Uiso R . . . . .
H481 H 1.1778 0.2210 0.4619 0.0528 1.0000 Uiso R . . . . .
H491 H 1.1957 0.0360 0.4912 0.0544 1.0000 Uiso R . . . . .
H501 H 1.1034 -0.0827 0.4833 0.0523 1.0000 Uiso R . . . . .
H511 H 0.9927 -0.0128 0.4414 0.0521 1.0000 Uiso R . . . . .
H541 H 0.7858 0.0916 0.4073 0.0452 1.0000 Uiso R . . . . .
H571 H 0.5992 0.3835 0.2914 0.0514 1.0000 Uiso R . . . . .
H581 H 0.5215 0.2811 0.3159 0.0561 1.0000 Uiso R . . . . .
H591 H 0.5552 0.1173 0.3681 0.0564 1.0000 Uiso R . . . . .
H601 H 0.6730 0.0790 0.4033 0.0543 1.0000 Uiso R . . . . .
H611 H 0.9554 0.4223 0.5128 0.0883 1.0000 Uiso R . . . . .
H612 H 0.9272 0.3391 0.5449 0.0889 1.0000 Uiso R . . . . .
H613 H 0.9271 0.3060 0.4884 0.0887 1.0000 Uiso R . . . . .
H631 H 0.4760 0.4359 0.6637 0.0976 1.0000 Uiso R . . . . .
H632 H 0.5172 0.3375 0.6514 0.0977 1.0000 Uiso R . . . . .
H633 H 0.4379 0.3270 0.6357 0.0979 1.0000 Uiso R . . . . .
H881 H 0.6544 0.4325 0.5316 0.0764 1.0000 Uiso R . . . . .
H882 H 0.5116 0.6040 0.8371 0.0523 1.0000 Uiso R . . . . .
H883 H 0.5623 0.5154 0.7843 0.0507 1.0000 Uiso R . . . . .
H884 H 0.8558 0.4330 0.4566 0.0804 1.0000 Uiso R . . . . .
H885 H 1.0965 0.3647 0.4148 0.0476 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.063227(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
Zn1 . N1 . 2.271(3) yes
Zn1 . N4 . 2.101(3) yes
Zn1 . N5 . 2.235(3) yes
Zn1 . N8 . 2.123(3) yes
Zn1 . O1 . 2.114(2) yes
Zn1 . O2 . 2.105(2) yes
Zn2 . N9 . 2.262(3) yes
Zn2 . N12 . 2.115(2) yes
Zn2 . N13 . 2.193(3) yes
Zn2 . N16 . 2.143(3) yes
Zn2 . O3 . 2.098(2) yes
Zn2 . O4 . 2.085(2) yes
N1 . C1 . 1.329(4) yes
N1 . C8 . 1.400(4) yes
N2 . C1 . 1.329(4) yes
N2 . C2 . 1.400(4) yes
N2 . H21 . 0.849 no
N3 . N4 . 1.445(4) yes
N3 . C8 . 1.319(4) yes
N4 . C9 . 1.290(4) yes
N5 . C16 . 1.327(4) yes
N5 . C23 . 1.402(4) yes
N6 . C16 . 1.332(4) yes
N6 . C17 . 1.403(5) yes
N6 . H61 . 0.837 no
N7 . N8 . 1.453(4) yes
N7 . C23 . 1.351(4) yes
N8 . C24 . 1.308(4) yes
N9 . C31 . 1.320(4) yes
N9 . C38 . 1.393(4) yes
N10 . C31 . 1.359(4) yes
N10 . C32 . 1.402(4) yes
N10 . H101 . 0.854 no
N11 . N12 . 1.425(3) yes
N11 . C38 . 1.356(4) yes
N12 . C39 . 1.312(4) yes
N13 . C46 . 1.363(4) yes
N13 . C53 . 1.387(4) yes
N14 . C46 . 1.358(4) yes
N14 . C47 . 1.399(4) yes
N14 . H885 . 0.849 no
N15 . N16 . 1.426(4) yes
N15 . C53 . 1.357(4) yes
N16 . C54 . 1.274(4) yes
O1 . C11 . 1.327(4) yes
O2 . C26 . 1.342(4) yes
O3 . C41 . 1.353(4) yes
O4 . C56 . 1.348(4) yes
O5 . H51 . 0.823 no
O5 . H52 . 0.817 no
O6 . C61 . 1.400(4) yes
O6 . H884 . 0.817 no
O8 . C63 . 1.451(4) yes
O8 . H81 . 0.809 no
O88 . C64 . 1.442(5) yes
O88 . H881 . 0.814 no
C1 . H11 . 0.927 no
C2 . C3 . 1.396(5) yes
C2 . C7 . 1.406(5) yes
C3 . C4 . 1.396(5) yes
C3 . H31 . 0.934 no
C4 . C5 . 1.400(5) yes
C4 . H41 . 0.930 no
C5 . C6 . 1.398(5) yes
C5 . H882 . 0.923 no
C6 . C7 . 1.398(5) yes
C6 . H883 . 0.932 no
C7 . C8 . 1.410(5) yes
C9 . C10 . 1.489(5) yes
C9 . H91 . 0.921 no
C10 . C11 . 1.404(5) yes
C10 . C15 . 1.401(5) yes
C11 . C12 . 1.403(5) yes
C12 . C13 . 1.394(5) yes
C12 . H121 . 0.931 no
C13 . C14 . 1.397(5) yes
C13 . H131 . 0.939 no
C14 . C15 . 1.402(5) yes
C14 . H141 . 0.932 no
C15 . H151 . 0.936 no
C16 . H161 . 0.931 no
C17 . C18 . 1.406(5) yes
C17 . C22 . 1.400(5) yes
C18 . C19 . 1.395(5) yes
C18 . H181 . 0.935 no
C19 . C20 . 1.401(6) yes
C19 . H191 . 0.935 no
C20 . C21 . 1.403(5) yes
C20 . H201 . 0.933 no
C21 . C22 . 1.400(5) yes
C21 . H211 . 0.927 no
C22 . C23 . 1.412(5) yes
C24 . C25 . 1.462(5) yes
C24 . H241 . 0.936 no
C25 . C26 . 1.399(4) yes
C25 . C30 . 1.400(5) yes
C26 . C27 . 1.406(5) yes
C27 . C28 . 1.393(5) yes
C27 . H271 . 0.926 no
C28 . C29 . 1.397(5) yes
C28 . H281 . 0.922 no
C29 . C30 . 1.401(5) yes
C29 . H291 . 0.926 no
C30 . H301 . 0.928 no
C31 . H311 . 0.931 no
C32 . C33 . 1.403(4) yes
C32 . C37 . 1.399(4) yes
C33 . C34 . 1.395(4) yes
C33 . H331 . 0.935 no
C34 . C35 . 1.403(5) yes
C34 . H341 . 0.922 no
C35 . C36 . 1.399(4) yes
C35 . H351 . 0.921 no
C36 . C37 . 1.406(4) yes
C36 . H361 . 0.933 no
C37 . C38 . 1.409(4) yes
C39 . C40 . 1.504(4) yes
C39 . H391 . 0.934 no
C40 . C41 . 1.402(4) yes
C40 . C45 . 1.400(4) yes
C41 . C42 . 1.400(4) yes
C42 . C43 . 1.396(5) yes
C42 . H421 . 0.923 no
C43 . C44 . 1.401(4) yes
C43 . H431 . 0.925 no
C44 . C45 . 1.403(4) yes
C44 . H441 . 0.933 no
C45 . H451 . 0.916 no
C46 . H461 . 0.932 no
C47 . C48 . 1.411(5) yes
C47 . C52 . 1.393(5) yes
C48 . C49 . 1.392(5) yes
C48 . H481 . 0.929 no
C49 . C50 . 1.399(5) yes
C49 . H491 . 0.932 no
C50 . C51 . 1.403(5) yes
C50 . H501 . 0.924 no
C51 . C52 . 1.400(5) yes
C51 . H511 . 0.928 no
C52 . C53 . 1.412(5) yes
C54 . C55 . 1.477(5) yes
C54 . H541 . 0.929 no
C55 . C56 . 1.406(4) yes
C55 . C60 . 1.407(5) yes
C56 . C57 . 1.400(5) yes
C57 . C58 . 1.401(5) yes
C57 . H571 . 0.925 no
C58 . C59 . 1.400(5) yes
C58 . H581 . 0.923 no
C59 . C60 . 1.399(5) yes
C59 . H591 . 0.937 no
C60 . H601 . 0.929 no
C61 . H611 . 0.951 no
C61 . H612 . 0.955 no
C61 . H613 . 0.951 no
C63 . H631 . 0.955 no
C63 . H632 . 0.948 no
C63 . H633 . 0.952 no
C64 . H71 . 0.967 no
C64 . H72 . 0.956 no
C64 . H73 . 0.961 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
N1 . Zn1 . N4 . 73.77(10) yes
N1 . Zn1 . N5 . 85.81(10) yes
N4 . Zn1 . N5 . 99.72(10) yes
N1 . Zn1 . N8 . 92.04(10) yes
N4 . Zn1 . N8 . 165.41(10) yes
N5 . Zn1 . N8 . 75.38(11) yes
N1 . Zn1 . O1 . 159.43(9) yes
N4 . Zn1 . O1 . 86.69(9) yes
N5 . Zn1 . O1 . 91.35(9) yes
N8 . Zn1 . O1 . 106.97(9) yes
N1 . Zn1 . O2 . 94.51(9) yes
N4 . Zn1 . O2 . 97.69(10) yes
N5 . Zn1 . O2 . 161.95(10) yes
N8 . Zn1 . O2 . 86.57(10) yes
O1 . Zn1 . O2 . 94.41(9) yes
N9 . Zn2 . N12 . 73.18(9) yes
N9 . Zn2 . N13 . 93.20(10) yes
N12 . Zn2 . N13 . 103.80(10) yes
N9 . Zn2 . N16 . 91.45(10) yes
N12 . Zn2 . N16 . 164.29(10) yes
N13 . Zn2 . N16 . 73.18(11) yes
N9 . Zn2 . O3 . 160.53(9) yes
N12 . Zn2 . O3 . 88.08(9) yes
N13 . Zn2 . O3 . 86.08(10) yes
N16 . Zn2 . O3 . 106.87(9) yes
N9 . Zn2 . O4 . 93.92(9) yes
N12 . Zn2 . O4 . 97.60(10) yes
N13 . Zn2 . O4 . 158.58(9) yes
N16 . Zn2 . O4 . 86.46(10) yes
O3 . Zn2 . O4 . 93.73(9) yes
Zn1 . N1 . C1 . 129.7(2) yes
Zn1 . N1 . C8 . 111.9(2) yes
C1 . N1 . C8 . 118.4(3) yes
C1 . N2 . C2 . 121.7(3) yes
C1 . N2 . H21 . 119.0 no
C2 . N2 . H21 . 119.3 no
N4 . N3 . C8 . 114.2(3) yes
N3 . N4 . Zn1 . 119.40(18) yes
N3 . N4 . C9 . 112.3(3) yes
Zn1 . N4 . C9 . 128.2(2) yes
Zn1 . N5 . C16 . 130.3(2) yes
Zn1 . N5 . C23 . 112.5(2) yes
C16 . N5 . C23 . 117.1(3) yes
C16 . N6 . C17 . 121.8(3) yes
C16 . N6 . H61 . 118.7 no
C17 . N6 . H61 . 119.4 no
N8 . N7 . C23 . 114.8(3) yes
N7 . N8 . Zn1 . 117.0(2) yes
N7 . N8 . C24 . 115.3(3) yes
Zn1 . N8 . C24 . 127.4(2) yes
Zn2 . N9 . C31 . 130.9(2) yes
Zn2 . N9 . C38 . 113.57(19) yes
C31 . N9 . C38 . 115.4(3) yes
C31 . N10 . C32 . 120.0(3) yes
C31 . N10 . H101 . 119.5 no
C32 . N10 . H101 . 120.5 no
N12 . N11 . C38 . 114.0(2) yes
N11 . N12 . Zn2 . 120.04(18) yes
N11 . N12 . C39 . 112.6(2) yes
Zn2 . N12 . C39 . 127.3(2) yes
Zn2 . N13 . C46 . 127.4(2) yes
Zn2 . N13 . C53 . 116.6(2) yes
C46 . N13 . C53 . 115.8(3) yes
C46 . N14 . C47 . 118.3(3) yes
C46 . N14 . H885 . 120.0 no
C47 . N14 . H885 . 121.7 no
N16 . N15 . C53 . 115.6(3) yes
N15 . N16 . Zn2 . 117.1(2) yes
N15 . N16 . C54 . 115.0(3) yes
Zn2 . N16 . C54 . 127.9(2) yes
Zn1 . O1 . C11 . 128.0(2) yes
Zn1 . O2 . C26 . 130.1(2) yes
Zn2 . O3 . C41 . 129.49(19) yes
Zn2 . O4 . C56 . 130.8(2) yes
H51 . O5 . H52 . 113.6 no
C61 . O6 . H884 . 103.0 no
C63 . O8 . H81 . 127.8 no
C64 . O88 . H881 . 102.3 no
N2 . C1 . N1 . 123.7(3) yes
N2 . C1 . H11 . 118.2 no
N1 . C1 . H11 . 118.1 no
N2 . C2 . C3 . 120.3(3) yes
N2 . C2 . C7 . 116.6(3) yes
C3 . C2 . C7 . 123.2(3) yes
C2 . C3 . C4 . 119.3(3) yes
C2 . C3 . H31 . 120.0 no
C4 . C3 . H31 . 120.7 no
C3 . C4 . C5 . 118.7(3) yes
C3 . C4 . H41 . 120.4 no
C5 . C4 . H41 . 120.9 no
C4 . C5 . C6 . 120.8(4) yes
C4 . C5 . H882 . 119.6 no
C6 . C5 . H882 . 119.5 no
C5 . C6 . C7 . 121.6(3) yes
C5 . C6 . H883 . 118.7 no
C7 . C6 . H883 . 119.6 no
C2 . C7 . C6 . 116.2(3) yes
C2 . C7 . C8 . 120.0(3) yes
C6 . C7 . C8 . 123.8(3) yes
C7 . C8 . N1 . 119.6(3) yes
C7 . C8 . N3 . 119.7(3) yes
N1 . C8 . N3 . 120.7(3) yes
N4 . C9 . C10 . 125.1(3) yes
N4 . C9 . H91 . 117.7 no
C10 . C9 . H91 . 117.3 no
C9 . C10 . C11 . 124.9(3) yes
C9 . C10 . C15 . 114.0(3) yes
C11 . C10 . C15 . 121.0(3) yes
C10 . C11 . O1 . 123.9(3) yes
C10 . C11 . C12 . 116.5(3) yes
O1 . C11 . C12 . 119.6(3) yes
C11 . C12 . C13 . 123.8(3) yes
C11 . C12 . H121 . 118.0 no
C13 . C12 . H121 . 118.2 no
C12 . C13 . C14 . 118.3(4) yes
C12 . C13 . H131 . 121.1 no
C14 . C13 . H131 . 120.6 no
C13 . C14 . C15 . 119.7(3) yes
C13 . C14 . H141 . 120.1 no
C15 . C14 . H141 . 120.2 no
C14 . C15 . C10 . 120.6(3) yes
C14 . C15 . H151 . 120.0 no
C10 . C15 . H151 . 119.4 no
N6 . C16 . N5 . 124.1(3) yes
N6 . C16 . H161 . 118.4 no
N5 . C16 . H161 . 117.5 no
N6 . C17 . C18 . 120.4(4) yes
N6 . C17 . C22 . 116.9(3) yes
C18 . C17 . C22 . 122.6(4) yes
C17 . C18 . C19 . 122.0(4) yes
C17 . C18 . H181 . 118.7 no
C19 . C18 . H181 . 119.4 no
C18 . C19 . C20 . 116.6(4) yes
C18 . C19 . H191 . 122.0 no
C20 . C19 . H191 . 121.4 no
C19 . C20 . C21 . 120.2(4) yes
C19 . C20 . H201 . 120.2 no
C21 . C20 . H201 . 119.6 no
C20 . C21 . C22 . 124.4(4) yes
C20 . C21 . H211 . 118.1 no
C22 . C21 . H211 . 117.5 no
C17 . C22 . C21 . 114.1(4) yes
C17 . C22 . C23 . 118.8(4) yes
C21 . C22 . C23 . 127.1(4) yes
C22 . C23 . N5 . 121.3(3) yes
C22 . C23 . N7 . 118.5(3) yes
N5 . C23 . N7 . 120.1(3) yes
N8 . C24 . C25 . 126.6(3) yes
N8 . C24 . H241 . 116.4 no
C25 . C24 . H241 . 117.0 no
C24 . C25 . C26 . 124.9(3) yes
C24 . C25 . C30 . 113.6(3) yes
C26 . C25 . C30 . 121.5(3) yes
C25 . C26 . O2 . 124.0(3) yes
C25 . C26 . C27 . 116.2(3) yes
O2 . C26 . C27 . 119.7(3) yes
C26 . C27 . C28 . 123.3(3) yes
C26 . C27 . H271 . 118.4 no
C28 . C27 . H271 . 118.3 no
C27 . C28 . C29 . 119.3(4) yes
C27 . C28 . H281 . 120.2 no
C29 . C28 . H281 . 120.5 no
C28 . C29 . C30 . 118.7(4) yes
C28 . C29 . H291 . 121.0 no
C30 . C29 . H291 . 120.3 no
C29 . C30 . C25 . 120.9(3) yes
C29 . C30 . H301 . 119.5 no
C25 . C30 . H301 . 119.6 no
N10 . C31 . N9 . 125.9(3) yes
N10 . C31 . H311 . 116.9 no
N9 . C31 . H311 . 117.2 no
N10 . C32 . C33 . 119.7(3) yes
N10 . C32 . C37 . 117.1(3) yes
C33 . C32 . C37 . 123.2(3) yes
C32 . C33 . C34 . 119.0(3) yes
C32 . C33 . H331 . 120.7 no
C34 . C33 . H331 . 120.3 no
C33 . C34 . C35 . 120.1(3) yes
C33 . C34 . H341 . 119.5 no
C35 . C34 . H341 . 120.4 no
C34 . C35 . C36 . 118.6(3) yes
C34 . C35 . H351 . 120.7 no
C36 . C35 . H351 . 120.7 no
C35 . C36 . C37 . 123.4(3) yes
C35 . C36 . H361 . 118.4 no
C37 . C36 . H361 . 118.2 no
C36 . C37 . C32 . 115.5(3) yes
C36 . C37 . C38 . 125.6(3) yes
C32 . C37 . C38 . 118.9(3) yes
C37 . C38 . N9 . 122.6(3) yes
C37 . C38 . N11 . 118.4(3) yes
N9 . C38 . N11 . 119.0(3) yes
N12 . C39 . C40 . 125.7(3) yes
N12 . C39 . H391 . 117.3 no
C40 . C39 . H391 . 117.0 no
C39 . C40 . C41 . 125.2(3) yes
C39 . C40 . C45 . 114.3(3) yes
C41 . C40 . C45 . 120.5(3) yes
C40 . C41 . O3 . 124.0(3) yes
C40 . C41 . C42 . 117.9(3) yes
O3 . C41 . C42 . 118.0(3) yes
C41 . C42 . C43 . 121.9(3) yes
C41 . C42 . H421 . 118.6 no
C43 . C42 . H421 . 119.4 no
C42 . C43 . C44 . 120.1(3) yes
C42 . C43 . H431 . 120.5 no
C44 . C43 . H431 . 119.5 no
C43 . C44 . C45 . 118.4(3) yes
C43 . C44 . H441 . 120.8 no
C45 . C44 . H441 . 120.8 no
C44 . C45 . C40 . 121.2(3) yes
C44 . C45 . H451 . 119.1 no
C40 . C45 . H451 . 119.7 no
N13 . C46 . N14 . 125.0(3) yes
N13 . C46 . H461 . 117.7 no
N14 . C46 . H461 . 117.3 no
N14 . C47 . C48 . 118.2(3) yes
N14 . C47 . C52 . 120.2(3) yes
C48 . C47 . C52 . 121.5(3) yes
C47 . C48 . C49 . 118.5(4) yes
C47 . C48 . H481 . 120.4 no
C49 . C48 . H481 . 121.1 no
C48 . C49 . C50 . 122.7(4) yes
C48 . C49 . H491 . 119.1 no
C50 . C49 . H491 . 118.2 no
C49 . C50 . C51 . 116.0(3) yes
C49 . C50 . H501 . 122.3 no
C51 . C50 . H501 . 121.7 no
C50 . C51 . C52 . 124.2(4) yes
C50 . C51 . H511 . 117.8 no
C52 . C51 . H511 . 118.0 no
C51 . C52 . C47 . 117.0(3) yes
C51 . C52 . C53 . 125.6(3) yes
C47 . C52 . C53 . 117.4(3) yes
C52 . C53 . N13 . 122.4(3) yes
C52 . C53 . N15 . 121.4(3) yes
N13 . C53 . N15 . 116.1(3) yes
N16 . C54 . C55 . 126.5(3) yes
N16 . C54 . H541 . 116.8 no
C55 . C54 . H541 . 116.7 no
C54 . C55 . C56 . 125.1(3) yes
C54 . C55 . C60 . 116.7(3) yes
C56 . C55 . C60 . 118.2(3) yes
C55 . C56 . O4 . 123.3(3) yes
C55 . C56 . C57 . 119.0(3) yes
O4 . C56 . C57 . 117.7(3) yes
C56 . C57 . C58 . 120.9(3) yes
C56 . C57 . H571 . 119.4 no
C58 . C57 . H571 . 119.7 no
C57 . C58 . C59 . 121.8(4) yes
C57 . C58 . H581 . 118.6 no
C59 . C58 . H581 . 119.6 no
C58 . C59 . C60 . 115.9(4) yes
C58 . C59 . H591 . 122.3 no
C60 . C59 . H591 . 121.8 no
C55 . C60 . C59 . 124.1(3) yes
C55 . C60 . H601 . 117.7 no
C59 . C60 . H601 . 118.2 no
O6 . C61 . H611 . 108.8 no
O6 . C61 . H612 . 109.6 no
H611 . C61 . H612 . 109.5 no
O6 . C61 . H613 . 109.3 no
H611 . C61 . H613 . 109.8 no
H612 . C61 . H613 . 109.8 no
O8 . C63 . H631 . 108.7 no
O8 . C63 . H632 . 108.1 no
H631 . C63 . H632 . 109.6 no
O8 . C63 . H633 . 110.5 no
H631 . C63 . H633 . 110.2 no
H632 . C63 . H633 . 109.8 no
O88 . C64 . H71 . 110.4 no
O88 . C64 . H72 . 109.5 no
H71 . C64 . H72 . 109.9 no
O88 . C64 . H73 . 108.5 no
H71 . C64 . H73 . 110.0 no
H72 . C64 . H73 . 108.6 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
N2 . H21 . O2 3_656 167 0.85 1.93 2.767(5) yes
O5 . H51 . O1 . 173 0.82 2.07 2.889(5) yes
O5 . H52 . O6 . 141 0.82 2.11 2.789(5) yes
N6 . H61 . O88 2_666 167 0.84 2.10 2.923(5) yes
O8 . H81 . O88 2_666 157 0.81 2.20 2.962(5) yes
N10 . H101 . O4 3_645 165 0.85 1.90 2.732(5) yes
C16 . H161 . O8 . 144 0.93 2.28 3.084(5) yes
O88 . H881 . O1 . 177 0.81 2.11 2.925(5) yes
O88 . H881 . C11 . 152 0.81 2.58 3.314(5) yes
O6 . H884 . O3 . 180 0.82 1.95 2.766(5) yes
N14 . H885 . O5 2_766 173 0.85 1.92 2.761(5) yes



# 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
9 4 16 x .
13 3 16 x .
13 1 17 x .
18 3 9 x .
15 8 10 x .
11 3 19 x .
15 5 10 x .
15 8 9 x .
13 0 9 x .
17 5 7 x .
14 9 9 x .
14 3 11 x .
# looking for ARCHIVE-HKL.CIF 

# end of ARCHIVE-HKL.CIF 
