# Supplementary Information (SI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_hexane_ex_a_pl_sq
_database_code_depnum_ccdc_archive 'CCDC 2159880'
loop_
_audit_author_name
_audit_author_address
'Younghun Kim'
;Yonsei University
South Korea
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H56 N8 O33 Zn2'
_chemical_formula_weight         2076.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2992 1.4004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   23.745(5)
_cell_length_b                   23.745(5)
_cell_length_c                   16.703(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9418(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    62994
_cell_measurement_theta_min      1.194
_cell_measurement_theta_max      32.652

_exptl_crystal_description       rod
_exptl_crystal_colour            purple-red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.732
_exptl_crystal_F_000             2120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47460
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0884
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.194
_diffrn_reflns_theta_max         32.652
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.509
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.509
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.509
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4608
_reflns_number_gt                2507
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  CIFTAB
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1287P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4608
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.2090
_refine_ls_wR_factor_gt          0.1962
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.250000 0.250000 0.11057(3) 0.0539(3) Uani 1 4 d S T P . .
O1W O 0.250000 0.250000 0.250000 0.206(5) Uani 1 8 d S T P . .
N1 N 0.16667(9) 0.27153(10) 0.10963(11) 0.0528(5) Uani 1 1 d . . . . .
O1 O -0.00430(11) 0.09606(11) -0.10958(11) 0.1131(11) Uani 1 1 d . . . . .
O2 O -0.06655(12) 0.04384(12) -0.04268(12) 0.1143(10) Uani 1 1 d . . . . .
H2 H -0.085358 0.045580 -0.085202 0.171 Uiso 1 1 calc R U . . .
O3 O -0.01324(11) 0.09828(12) 0.31555(12) 0.1278(11) Uani 1 1 d . . . . .
O4 O -0.06856(12) 0.04050(13) 0.24741(11) 0.1180(11) Uani 1 1 d . . . . .
H4 H -0.085554 0.038479 0.291427 0.177 Uiso 1 1 calc R U . . .
C1 C 0.12232(12) 0.23528(13) 0.10943(14) 0.0580(7) Uani 1 1 d . . . . .
C2 C 0.07032(13) 0.26732(15) 0.10862(15) 0.0698(8) Uani 1 1 d . . . . .
H2A H 0.033142 0.252529 0.108515 0.084 Uiso 1 1 calc R U . . .
C3 C 0.17773(14) 0.08500(13) 0.10806(16) 0.0695(9) Uani 1 1 d . . . . .
H3 H 0.146517 0.059985 0.107109 0.083 Uiso 1 1 calc R U . . .
C4 C 0.17523(13) 0.14509(12) 0.10914(14) 0.0581(7) Uani 1 1 d . . . . .
C5 C 0.12531(11) 0.17719(12) 0.10905(13) 0.0559(7) Uani 1 1 d . . . . .
C6 C 0.07095(12) 0.14427(13) 0.10661(15) 0.0622(7) Uani 1 1 d . . . . .
C7 C 0.04767(11) 0.12796(12) 0.03436(15) 0.0676(8) Uani 1 1 d . . . . .
H7 H 0.065030 0.139193 -0.014327 0.081 Uiso 1 1 calc R U . . .
C8 C -0.00084(13) 0.09531(13) 0.03227(15) 0.0751(9) Uani 1 1 d . . . . .
C9 C -0.02709(14) 0.07881(15) 0.10327(15) 0.0792(10) Uani 1 1 d . . . . .
H9 H -0.060191 0.056346 0.102117 0.095 Uiso 1 1 calc R U . . .
C10 C -0.00406(13) 0.09575(14) 0.17506(15) 0.0774(10) Uani 1 1 d . . . . .
C11 C 0.04396(12) 0.12905(13) 0.17646(15) 0.0737(9) Uani 1 1 d . . . . .
H11 H 0.058495 0.141565 0.226378 0.088 Uiso 1 1 calc R U . . .
C12 C -0.02419(15) 0.07854(14) -0.04694(17) 0.0888(11) Uani 1 1 d . . . . .
C13 C -0.02917(15) 0.07794(17) 0.25214(16) 0.0948(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.044(2) . ?
Zn1 N1 2.044(2) 4 ?
Zn1 N1 2.044(2) 2 ?
Zn1 N1 2.044(2) 3 ?
Zn1 O1W 2.3289(7) . ?
N1 C1 1.360(4) . ?
N1 C4 1.364(4) 4 ?
O1 C12 1.221(3) . ?
O2 C12 1.302(3) . ?
O2 H2 0.8400 . ?
O3 C13 1.224(3) . ?
O4 C13 1.293(3) . ?
O4 H4 0.8400 . ?
C1 C5 1.381(4) . ?
C1 C2 1.450(4) . ?
C2 C3 1.350(4) 4 ?
C2 H2A 0.9500 . ?
C3 C4 1.428(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.409(4) . ?
C5 C6 1.510(4) . ?
C6 C11 1.379(3) . ?
C6 C7 1.383(3) . ?
C7 C8 1.389(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.396(4) . ?
C8 C12 1.489(4) . ?
C9 C10 1.378(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(4) . ?
C10 C13 1.481(4) . ?
C11 H11 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N1 89.997(1) . 4 ?
N1 Zn1 N1 89.996(1) . 2 ?
N1 Zn1 N1 179.13(11) 4 2 ?
N1 Zn1 N1 179.12(11) . 3 ?
N1 Zn1 N1 89.997(1) 4 3 ?
N1 Zn1 N1 89.997(1) 2 3 ?
N1 Zn1 O1W 90.44(5) . . ?
N1 Zn1 O1W 90.44(5) 4 . ?
N1 Zn1 O1W 90.44(5) 2 . ?
N1 Zn1 O1W 90.44(5) 3 . ?
Zn1 O1W Zn1 180.0 . 5 ?
C1 N1 C4 107.2(2) . 4 ?
C1 N1 Zn1 126.3(2) . . ?
C4 N1 Zn1 126.5(2) 4 . ?
C12 O2 H2 109.5 . . ?
C13 O4 H4 109.5 . . ?
N1 C1 C5 126.3(3) . . ?
N1 C1 C2 109.1(3) . . ?
C5 C1 C2 124.6(3) . . ?
C3 C2 C1 106.7(3) 4 . ?
C3 C2 H2A 126.7 4 . ?
C1 C2 H2A 126.7 . . ?
C2 C3 C4 107.3(3) 2 . ?
C2 C3 H3 126.3 2 . ?
C4 C3 H3 126.3 . . ?
N1 C4 C5 125.2(3) 2 . ?
N1 C4 C3 109.7(3) 2 . ?
C5 C4 C3 125.1(3) . . ?
C1 C5 C4 125.7(2) . . ?
C1 C5 C6 118.2(3) . . ?
C4 C5 C6 116.1(2) . . ?
C11 C6 C7 118.6(3) . . ?
C11 C6 C5 120.7(2) . . ?
C7 C6 C5 120.7(2) . . ?
C6 C7 C8 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 120.4(2) . . ?
C7 C8 C12 118.7(2) . . ?
C9 C8 C12 120.9(3) . . ?
C10 C9 C8 118.7(3) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 C11 120.5(2) . . ?
C9 C10 C13 120.9(3) . . ?
C11 C10 C13 118.6(2) . . ?
C6 C11 C10 121.1(2) . . ?
C6 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
O1 C12 O2 124.1(3) . . ?
O1 C12 C8 121.8(3) . . ?
O2 C12 C8 114.1(3) . . ?
O3 C13 O4 123.2(3) . . ?
O3 C13 C10 121.0(3) . . ?
O4 C13 C10 115.8(2) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 C1 C5 179.4(2) 4 . . . ?
Zn1 N1 C1 C5 -0.7(3) . . . . ?
C4 N1 C1 C2 0.1(3) 4 . . . ?
Zn1 N1 C1 C2 -179.92(15) . . . . ?
N1 C1 C2 C3 0.2(3) . . . 4 ?
C5 C1 C2 C3 -179.1(2) . . . 4 ?
C2 C3 C4 N1 0.5(3) 2 . . 2 ?
C2 C3 C4 C5 -179.9(2) 2 . . . ?
N1 C1 C5 C4 0.3(4) . . . . ?
C2 C1 C5 C4 179.4(2) . . . . ?
N1 C1 C5 C6 -178.4(2) . . . . ?
C2 C1 C5 C6 0.8(4) . . . . ?
N1 C4 C5 C1 0.0(4) 2 . . . ?
C3 C4 C5 C1 -179.4(2) . . . . ?
N1 C4 C5 C6 178.7(2) 2 . . . ?
C3 C4 C5 C6 -0.8(4) . . . . ?
C1 C5 C6 C11 -89.4(3) . . . . ?
C4 C5 C6 C11 91.8(3) . . . . ?
C1 C5 C6 C7 91.6(3) . . . . ?
C4 C5 C6 C7 -87.1(3) . . . . ?
C11 C6 C7 C8 -2.1(5) . . . . ?
C5 C6 C7 C8 176.8(3) . . . . ?
C6 C7 C8 C9 0.5(5) . . . . ?
C6 C7 C8 C12 -179.7(3) . . . . ?
C7 C8 C9 C10 0.3(5) . . . . ?
C12 C8 C9 C10 -179.5(3) . . . . ?
C8 C9 C10 C11 0.7(6) . . . . ?
C8 C9 C10 C13 -178.0(3) . . . . ?
C7 C6 C11 C10 3.1(5) . . . . ?
C5 C6 C11 C10 -175.9(3) . . . . ?
C9 C10 C11 C6 -2.4(5) . . . . ?
C13 C10 C11 C6 176.3(3) . . . . ?
C7 C8 C12 O1 -5.4(5) . . . . ?
C9 C8 C12 O1 174.4(4) . . . . ?
C7 C8 C12 O2 174.0(3) . . . . ?
C9 C8 C12 O2 -6.2(5) . . . . ?
C9 C10 C13 O3 -171.0(4) . . . . ?
C11 C10 C13 O3 10.3(6) . . . . ?
C9 C10 C13 O4 8.5(6) . . . . ?
C11 C10 C13 O4 -170.2(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O3 0.84 1.85 2.589(3) 145.5 14 yes
O4 H4 O1 0.84 1.86 2.621(3) 150.2 14_556 yes

_refine_diff_density_max         1.338
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.054




####################################################################### 
# 
# 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_YSH8Ni
_database_code_depnum_ccdc_archive 'CCDC 2324254'
loop_
_audit_author_name
_audit_author_address
'Younghun Kim'
;Yonsei University
South Korea
;
_audit_update_record             
;
2024-08-10 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_audit_creation_date             2024-01-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.75(C52 H28 N4 Ni O16)'
_chemical_formula_sum            'C39 H21 N3 Ni0.75 O12'
_chemical_formula_weight         767.62
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

_vrf_PLAT029_YSH8Ni              
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.922 Why? 
RESPONSE: low quality of crystal, thus weakly diffracted 
;

_vrf_PLAT973_YSH8Ni              
;
PROBLEM: Check Calcd Positive Resid. Density on       Ni1       2.76 eA-3 
RESPONSE: large residual density could be caused by absorption correction
;

_vrf_PLAT213_YSH8Ni              
;
PROBLEM: Atom C18             has ADP max/min Ratio .....        5.8 oblate 
RESPONSE: this alert  could be caused by large amount of disorder in the data
;

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   24.1698(19)
_cell_length_b                   24.1698(19)
_cell_length_c                   25.181(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14710(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    20460
_cell_measurement_temperature    298
_cell_measurement_theta_max      66.7310
_cell_measurement_theta_min      2.5890
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.956
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.77a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.693
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1491
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20460
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.331
_diffrn_reflns_theta_min         2.534
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2928
_reflns_number_total             6179
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         2.340
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1970
_refine_ls_R_factor_gt           0.1581
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3622
_refine_ls_wR_factor_ref         0.3923
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C9(H9), C16(H16), C17(H17), C21(H21), C23(H23), C25(H25)
2.b Idealised tetrahedral OH refined as rotating group:
 O11(H11), O29(H29), O30(H30)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2500 0.2500 0.2500 0.0380(6) Uani 1 8 d S T P . .
O11 O 0.5313(4) 0.4961(4) 0.3420(3) 0.176(5) Uani 1 1 d . . . . .
H11 H 0.5432 0.5009 0.3721 0.264 Uiso 1 1 calc R U . . .
O12 O 0.4961(3) 0.4225(3) 0.3840(2) 0.125(3) Uani 1 1 d . . . . .
N2 N 0.2500 0.3309(2) 0.2500 0.0488(17) Uani 1 2 d S T P . .
C3 C 0.2953(3) 0.3657(2) 0.2493(2) 0.0592(19) Uani 1 1 d . . . . .
C4 C 0.2771(4) 0.4184(3) 0.2502(4) 0.111(4) Uani 1 1 d . . . . .
H4 H 0.2994 0.4498 0.2511 0.133 Uiso 1 1 calc R U . . .
C5 C 0.3498(3) 0.3498(3) 0.2500 0.070(3) Uani 1 2 d S T P . .
C6 C 0.3933(3) 0.3933(3) 0.2500 0.096(5) Uani 1 2 d S T P . .
C7 C 0.4261(4) 0.4002(3) 0.2957(3) 0.088(3) Uani 1 1 d . . . . .
H7 H 0.4212 0.3774 0.3252 0.106 Uiso 1 1 calc R U . . .
C8 C 0.4679(4) 0.4439(4) 0.2960(3) 0.103(3) Uani 1 1 d . . . . .
C9 C 0.4742(4) 0.4742(4) 0.2500 0.152(8) Uani 1 2 d S T P . .
H9 H 0.5014 0.5014 0.2500 0.183 Uiso 1 2 calc R U P . .
C10 C 0.4995(5) 0.4507(5) 0.3410(3) 0.128(5) Uani 1 1 d . . . . .
Ni13 Ni 0.7500 0.7500 0.58189(8) 0.0480(6) Uani 1 4 d S T P . .
O28 O 0.6404(5) 0.4625(3) 0.7037(2) 0.184(5) Uani 1 1 d . . . . .
O29 O 0.5933(9) 0.4051(5) 0.6561(3) 0.406(15) Uani 1 1 d . . . . .
H29 H 0.5782 0.3996 0.6847 0.609 Uiso 1 1 calc R U . . .
O30 O 0.5416(4) 0.4476(3) 0.4751(3) 0.141(3) Uani 1 1 d . . . . .
H30 H 0.5260 0.4446 0.4463 0.211 Uiso 1 1 calc R U . . .
O31 O 0.5767(4) 0.5212(3) 0.4334(2) 0.151(4) Uani 1 1 d . . . . .
N14 N 0.7728(2) 0.6720(2) 0.5814(2) 0.0565(14) Uani 1 1 d . . . . .
C15 C 0.7377(3) 0.6273(3) 0.5813(3) 0.0563(17) Uani 1 1 d . . . . .
C16 C 0.7724(4) 0.5768(3) 0.5790(3) 0.080(2) Uani 1 1 d . . . . .
H16 H 0.7604 0.5402 0.5773 0.095 Uiso 1 1 calc R U . . .
C17 C 0.8236(4) 0.5947(4) 0.5799(3) 0.090(3) Uani 1 1 d . . . . .
H17 H 0.8548 0.5722 0.5796 0.108 Uiso 1 1 calc R U . . .
C18 C 0.6823(3) 0.6275(2) 0.5798(3) 0.0582(17) Uani 1 1 d . U . . .
C19 C 0.6528(2) 0.6756(2) 0.5814(3) 0.0534(16) Uani 1 1 d . . . . .
C20 C 0.6515(4) 0.5723(3) 0.5757(2) 0.088(3) Uani 1 1 d . . . . .
C21 C 0.6513(4) 0.5368(3) 0.6176(3) 0.087(3) Uani 1 1 d . . . . .
H21 H 0.6703 0.5452 0.6487 0.104 Uiso 1 1 calc R U . . .
C22 C 0.6207(4) 0.4857(3) 0.6123(3) 0.096(3) Uani 1 1 d . . . . .
C23 C 0.5979(5) 0.4732(4) 0.5681(3) 0.113(4) Uani 1 1 d . . . . .
H23 H 0.5797 0.4394 0.5659 0.136 Uiso 1 1 calc R U . . .
C24 C 0.5982(4) 0.5043(4) 0.5259(3) 0.111(4) Uani 1 1 d . . . . .
C25 C 0.6275(3) 0.5583(3) 0.5278(3) 0.087(3) Uani 1 1 d . . . . .
H25 H 0.6295 0.5814 0.4984 0.104 Uiso 1 1 calc R U . . .
C26 C 0.6195(7) 0.4538(6) 0.6573(4) 0.190(8) Uani 1 1 d . . . . .
C27 C 0.5724(4) 0.4923(5) 0.4752(3) 0.107(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.954(6) 4 ?
Ni1 N2 1.954(6) 2 ?
Ni1 N2 1.954(6) . ?
Ni1 N2 1.954(6) 3 ?
O11 H11 0.8200 . ?
O11 C10 1.340(10) . ?
O12 C10 1.282(10) . ?
N2 C3 1.382(7) . ?
N2 C3 1.382(7) 5 ?
C3 C4 1.349(11) . ?
C3 C5 1.371(8) . ?
C4 C4 1.31(2) 5 ?
C4 H4 0.9300 . ?
C5 C3 1.371(8) 7 ?
C5 C6 1.489(12) . ?
C6 C7 1.408(9) 7 ?
C6 C7 1.408(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.462(10) . ?
C8 C9 1.378(9) . ?
C8 C10 1.377(11) . ?
C9 C8 1.378(9) 7 ?
C9 H9 0.9300 . ?
Ni13 N14 1.965(5) 2_665 ?
Ni13 N14 1.965(5) 3_655 ?
Ni13 N14 1.965(5) 4_565 ?
Ni13 N14 1.965(5) . ?
O28 C26 1.290(11) . ?
O29 H29 0.8200 . ?
O29 C26 1.336(13) . ?
O30 H30 0.8200 . ?
O30 C27 1.314(10) . ?
O31 C27 1.268(10) . ?
N14 C15 1.373(8) . ?
N14 C19 1.330(7) 3_655 ?
C15 C16 1.482(9) . ?
C15 C18 1.340(9) . ?
C16 H16 0.9300 . ?
C16 C17 1.312(11) . ?
C17 H17 0.9300 . ?
C17 C19 1.405(10) 3_655 ?
C18 C19 1.365(9) . ?
C18 C20 1.531(8) . ?
C19 N14 1.330(7) 4_565 ?
C19 C17 1.405(10) 4_565 ?
C20 C21 1.360(9) . ?
C20 C25 1.380(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.445(10) . ?
C22 C23 1.279(10) . ?
C22 C26 1.371(13) . ?
C23 H23 0.9300 . ?
C23 C24 1.301(11) . ?
C24 C25 1.485(10) . ?
C24 C27 1.451(11) . ?
C25 H25 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N2 180.0 4 3 ?
N2 Ni1 N2 90.000(1) 4 . ?
N2 Ni1 N2 90.0 4 2 ?
N2 Ni1 N2 180.0 2 . ?
N2 Ni1 N2 90.0 3 . ?
N2 Ni1 N2 90.000(1) 3 2 ?
C10 O11 H11 109.5 . . ?
C3 N2 Ni1 127.5(3) 5 . ?
C3 N2 Ni1 127.5(3) . . ?
C3 N2 C3 104.9(7) . 5 ?
C4 C3 N2 108.4(7) . . ?
C4 C3 C5 125.4(7) . . ?
C5 C3 N2 126.1(6) . . ?
C3 C4 H4 125.5 . . ?
C4 C4 C3 109.1(5) 5 . ?
C4 C4 H4 125.5 5 . ?
C3 C5 C3 122.7(8) 7 . ?
C3 C5 C6 118.7(4) 7 . ?
C3 C5 C6 118.7(4) . . ?
C7 C6 C5 118.8(4) . . ?
C7 C6 C5 118.8(4) 7 . ?
C7 C6 C7 122.5(9) 7 . ?
C6 C7 H7 120.7 . . ?
C6 C7 C8 118.5(7) . . ?
C8 C7 H7 120.7 . . ?
C9 C8 C7 117.1(8) . . ?
C10 C8 C7 118.3(7) . . ?
C10 C8 C9 124.5(8) . . ?
C8 C9 C8 126.1(12) 7 . ?
C8 C9 H9 117.0 7 . ?
C8 C9 H9 117.0 . . ?
O11 C10 C8 115.6(8) . . ?
O12 C10 O11 117.2(7) . . ?
O12 C10 C8 126.6(7) . . ?
N14 Ni13 N14 179.2(3) 4_565 3_655 ?
N14 Ni13 N14 179.2(3) 2_665 . ?
N14 Ni13 N14 89.997(3) 3_655 . ?
N14 Ni13 N14 89.998(3) 4_565 2_665 ?
N14 Ni13 N14 89.997(3) 3_655 2_665 ?
N14 Ni13 N14 89.998(3) 4_565 . ?
C26 O29 H29 109.5 . . ?
C27 O30 H30 109.5 . . ?
C15 N14 Ni13 125.6(4) . . ?
C19 N14 Ni13 126.6(4) 3_655 . ?
C19 N14 C15 107.7(5) 3_655 . ?
N14 C15 C16 107.4(6) . . ?
C18 C15 N14 127.9(6) . . ?
C18 C15 C16 124.5(7) . . ?
C15 C16 H16 127.5 . . ?
C17 C16 C15 105.1(7) . . ?
C17 C16 H16 127.5 . . ?
C16 C17 H17 124.9 . . ?
C16 C17 C19 110.1(7) . 3_655 ?
C19 C17 H17 124.9 3_655 . ?
C15 C18 C19 121.6(5) . . ?
C15 C18 C20 119.0(7) . . ?
C19 C18 C20 119.3(6) . . ?
N14 C19 C17 109.6(6) 4_565 4_565 ?
N14 C19 C18 128.1(5) 4_565 . ?
C18 C19 C17 122.2(6) . 4_565 ?
C21 C20 C18 119.9(6) . . ?
C21 C20 C25 121.4(7) . . ?
C25 C20 C18 118.5(5) . . ?
C20 C21 H21 121.0 . . ?
C20 C21 C22 118.0(6) . . ?
C22 C21 H21 121.0 . . ?
C23 C22 C21 120.1(6) . . ?
C23 C22 C26 125.3(8) . . ?
C26 C22 C21 114.6(7) . . ?
C22 C23 H23 117.5 . . ?
C22 C23 C24 124.9(8) . . ?
C24 C23 H23 117.5 . . ?
C23 C24 C25 118.9(7) . . ?
C23 C24 C27 127.0(8) . . ?
C27 C24 C25 114.1(7) . . ?
C20 C25 C24 116.4(6) . . ?
C20 C25 H25 121.8 . . ?
C24 C25 H25 121.8 . . ?
O28 C26 O29 110.5(11) . . ?
O28 C26 C22 130.4(10) . . ?
O29 C26 C22 119.1(8) . . ?
O30 C27 C24 114.2(8) . . ?
O31 C27 O30 120.0(7) . . ?
O31 C27 C24 125.9(8) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N2 C3 C4 -179.2(5) . . . . ?
Ni1 N2 C3 C5 -2.1(7) . . . . ?
N2 C3 C4 C4 -2.1(13) . . . 5 ?
N2 C3 C5 C3 1.1(4) . . . 7 ?
N2 C3 C5 C6 -178.9(4) . . . . ?
C3 N2 C3 C4 0.8(5) 5 . . . ?
C3 N2 C3 C5 177.9(7) 5 . . . ?
C3 C5 C6 C7 111.9(5) . . . . ?
C3 C5 C6 C7 111.9(5) 7 . . 7 ?
C3 C5 C6 C7 -68.1(5) . . . 7 ?
C3 C5 C6 C7 -68.1(5) 7 . . . ?
C4 C3 C5 C3 177.7(8) . . . 7 ?
C4 C3 C5 C6 -2.3(8) . . . . ?
C5 C3 C4 C4 -179.2(9) . . . 5 ?
C5 C6 C7 C8 -178.5(7) . . . . ?
C6 C7 C8 C9 -2.9(14) . . . . ?
C6 C7 C8 C10 179.6(10) . . . . ?
C7 C6 C7 C8 1.5(7) 7 . . . ?
C7 C8 C9 C8 1.5(7) . . . 7 ?
C7 C8 C10 O11 -170.7(12) . . . . ?
C7 C8 C10 O12 -1(2) . . . . ?
C9 C8 C10 O11 12.0(19) . . . . ?
C9 C8 C10 O12 -177.9(11) . . . . ?
C10 C8 C9 C8 178.8(14) . . . 7 ?
Ni13 N14 C15 C16 178.1(4) . . . . ?
Ni13 N14 C15 C18 2.4(10) . . . . ?
N14 C15 C16 C17 2.2(8) . . . . ?
N14 C15 C18 C19 -4.2(11) . . . . ?
N14 C15 C18 C20 175.4(6) . . . . ?
C15 C16 C17 C19 -1.3(9) . . . 3_655 ?
C15 C18 C19 N14 4.3(12) . . . 4_565 ?
C15 C18 C19 C17 -179.9(7) . . . 4_565 ?
C15 C18 C20 C21 69.7(11) . . . . ?
C15 C18 C20 C25 -106.0(9) . . . . ?
C16 C15 C18 C19 -179.2(7) . . . . ?
C16 C15 C18 C20 0.3(10) . . . . ?
C18 C15 C16 C17 178.1(7) . . . . ?
C18 C20 C21 C22 178.8(8) . . . . ?
C18 C20 C25 C24 179.8(9) . . . . ?
C19 N14 C15 C16 -2.2(7) 3_655 . . . ?
C19 N14 C15 C18 -178.0(7) 3_655 . . . ?
C19 C18 C20 C21 -110.8(10) . . . . ?
C19 C18 C20 C25 73.5(11) . . . . ?
C20 C18 C19 N14 -175.2(6) . . . 4_565 ?
C20 C18 C19 C17 0.6(11) . . . 4_565 ?
C20 C21 C22 C23 4.6(16) . . . . ?
C20 C21 C22 C26 -175.9(12) . . . . ?
C21 C20 C25 C24 4.1(14) . . . . ?
C21 C22 C23 C24 -2.1(19) . . . . ?
C21 C22 C26 O28 1(3) . . . . ?
C21 C22 C26 O29 -178.4(18) . . . . ?
C22 C23 C24 C25 0.6(19) . . . . ?
C22 C23 C24 C27 -179.1(12) . . . . ?
C23 C22 C26 O28 -179.3(17) . . . . ?
C23 C22 C26 O29 1(3) . . . . ?
C23 C24 C25 C20 -1.5(16) . . . . ?
C23 C24 C27 O30 6.7(19) . . . . ?
C23 C24 C27 O31 -174.4(13) . . . . ?
C25 C20 C21 C22 -5.6(15) . . . . ?
C25 C24 C27 O30 -173.0(10) . . . . ?
C25 C24 C27 O31 5.9(17) . . . . ?
C26 C22 C23 C24 178.4(15) . . . . ?
C27 C24 C25 C20 178.2(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.528 -0.125 -0.214 9869.2 3561.6 ?
2 0.000 0.058 0.160 0.0 0.0 ?
3 0.000 0.083 0.207 0.0 0.0 ?
4 0.000 0.417 0.293 0.0 0.0 ?
5 0.000 0.442 0.340 0.0 0.0 ?
6 0.000 0.558 0.660 0.0 0.0 ?
7 0.000 0.583 0.707 0.0 0.0 ?
8 0.000 0.917 0.793 0.0 0.0 ?
9 0.000 0.942 0.840 0.0 0.0 ?
10 0.008 0.050 0.117 0.0 0.0 ?
11 0.008 0.092 0.215 0.0 0.0 ?
12 0.008 0.408 0.285 0.0 0.0 ?
13 0.008 0.450 0.383 0.0 0.0 ?
14 0.008 0.575 0.703 0.0 0.0 ?
15 0.008 0.592 0.742 0.0 0.0 ?
16 0.008 0.600 0.750 0.0 0.0 ?
17 0.008 0.900 0.750 0.0 0.0 ?
18 0.008 0.908 0.758 0.0 0.0 ?
19 0.008 0.925 0.797 0.0 0.0 ?
20 0.017 0.167 0.234 0.0 0.0 ?
21 0.017 0.333 0.266 0.0 0.0 ?
22 0.017 0.575 0.711 0.0 0.0 ?
23 0.017 0.925 0.789 0.0 0.0 ?
24 0.033 0.075 0.148 0.0 0.0 ?
25 0.033 0.083 0.156 0.0 0.0 ?
26 0.033 0.092 0.164 0.0 0.0 ?
27 0.033 0.408 0.336 0.0 0.0 ?
28 0.033 0.417 0.344 0.0 0.0 ?
29 0.033 0.425 0.352 0.0 0.0 ?
30 0.046 0.083 0.148 0.0 0.0 ?
31 0.046 0.417 0.352 0.0 0.0 ?
32 0.050 0.008 0.383 0.0 0.0 ?
33 0.050 0.492 0.117 0.0 0.0 ?
34 0.058 0.000 0.340 0.0 0.0 ?
35 0.058 0.500 0.160 0.0 0.0 ?
36 0.075 0.033 0.352 0.0 0.0 ?
37 0.075 0.142 0.180 0.0 0.0 ?
38 0.075 0.358 0.320 0.0 0.0 ?
39 0.075 0.467 0.148 0.0 0.0 ?
40 0.075 0.508 0.203 0.0 0.0 ?
41 0.075 0.517 0.211 0.0 0.0 ?
42 0.075 0.983 0.289 0.0 0.0 ?
43 0.075 0.992 0.297 0.0 0.0 ?
44 0.083 0.000 0.293 0.0 0.0 ?
45 0.083 0.033 0.344 0.0 0.0 ?
46 0.083 0.046 0.352 0.0 0.0 ?
47 0.083 0.454 0.148 0.0 0.0 ?
48 0.083 0.467 0.156 0.0 0.0 ?
49 0.083 0.500 0.207 0.0 0.0 ?
50 0.092 0.008 0.285 0.0 0.0 ?
51 0.092 0.033 0.336 0.0 0.0 ?
52 0.092 0.467 0.164 0.0 0.0 ?
53 0.092 0.492 0.215 0.0 0.0 ?
54 0.092 0.508 0.242 0.0 0.0 ?
55 0.092 0.992 0.258 0.0 0.0 ?
56 0.100 0.508 0.250 0.0 0.0 ?
57 0.100 0.992 0.250 0.0 0.0 ?
58 0.142 0.075 0.320 0.0 0.0 ?
59 0.142 0.425 0.180 0.0 0.0 ?
60 0.167 0.017 0.266 0.0 0.0 ?
61 0.167 0.483 0.234 0.0 0.0 ?
62 0.333 0.017 0.234 0.0 0.0 ?
63 0.333 0.483 0.266 0.0 0.0 ?
64 0.358 0.075 0.180 0.0 0.0 ?
65 0.358 0.425 0.320 0.0 0.0 ?
66 0.400 0.508 0.250 0.0 0.0 ?
67 0.400 0.992 0.250 0.0 0.0 ?
68 0.408 0.008 0.215 0.0 0.0 ?
69 0.408 0.033 0.164 0.0 0.0 ?
70 0.408 0.467 0.336 0.0 0.0 ?
71 0.408 0.492 0.285 0.0 0.0 ?
72 0.408 0.508 0.258 0.0 0.0 ?
73 0.408 0.992 0.242 0.0 0.0 ?
74 0.417 0.000 0.207 0.0 0.0 ?
75 0.417 0.033 0.156 0.0 0.0 ?
76 0.417 0.046 0.148 0.0 0.0 ?
77 0.417 0.454 0.352 0.0 0.0 ?
78 0.417 0.467 0.344 0.0 0.0 ?
79 0.417 0.500 0.293 0.0 0.0 ?
80 0.425 0.033 0.148 0.0 0.0 ?
81 0.425 0.142 0.320 0.0 0.0 ?
82 0.425 0.358 0.180 0.0 0.0 ?
83 0.425 0.467 0.352 0.0 0.0 ?
84 0.425 0.508 0.297 0.0 0.0 ?
85 0.425 0.517 0.289 0.0 0.0 ?
86 0.425 0.983 0.211 0.0 0.0 ?
87 0.425 0.992 0.203 0.0 0.0 ?
88 0.442 0.000 0.160 0.0 0.0 ?
89 0.442 0.500 0.340 0.0 0.0 ?
90 0.450 0.008 0.117 0.0 0.0 ?
91 0.454 0.083 0.352 0.0 0.0 ?
92 0.454 0.417 0.148 0.0 0.0 ?
93 0.450 0.492 0.383 0.0 0.0 ?
94 0.467 0.075 0.352 0.0 0.0 ?
95 0.467 0.083 0.344 0.0 0.0 ?
96 0.467 0.092 0.336 0.0 0.0 ?
97 0.467 0.408 0.164 0.0 0.0 ?
98 0.467 0.417 0.156 0.0 0.0 ?
99 0.467 0.425 0.148 0.0 0.0 ?
100 0.483 0.167 0.266 0.0 0.0 ?
101 0.483 0.333 0.234 0.0 0.0 ?
102 0.483 0.575 0.789 0.0 0.0 ?
103 0.483 0.925 0.711 0.0 0.0 ?
104 0.492 0.050 0.383 0.0 0.0 ?
105 0.492 0.092 0.285 0.0 0.0 ?
106 0.492 0.408 0.215 0.0 0.0 ?
107 0.492 0.450 0.117 0.0 0.0 ?
108 0.492 0.575 0.797 0.0 0.0 ?
109 0.492 0.592 0.758 0.0 0.0 ?
110 0.492 0.600 0.750 0.0 0.0 ?
111 0.492 0.900 0.750 0.0 0.0 ?
112 0.492 0.908 0.742 0.0 0.0 ?
113 0.492 0.925 0.703 0.0 0.0 ?
114 0.500 0.058 0.340 0.0 0.0 ?
115 0.500 0.083 0.293 0.0 0.0 ?
116 0.500 0.417 0.207 0.0 0.0 ?
117 0.500 0.442 0.160 0.0 0.0 ?
118 0.500 0.558 0.840 0.0 0.0 ?
119 0.500 0.583 0.793 0.0 0.0 ?
120 0.500 0.917 0.707 0.0 0.0 ?
121 0.500 0.942 0.660 0.0 0.0 ?
122 0.508 0.075 0.297 0.0 0.0 ?
123 0.508 0.092 0.258 0.0 0.0 ?
124 0.508 0.100 0.250 0.0 0.0 ?
125 0.508 0.400 0.250 0.0 0.0 ?
126 0.508 0.408 0.242 0.0 0.0 ?
127 0.508 0.425 0.203 0.0 0.0 ?
128 0.508 0.550 0.883 0.0 0.0 ?
129 0.508 0.592 0.785 0.0 0.0 ?
130 0.508 0.908 0.715 0.0 0.0 ?
131 0.508 0.950 0.617 0.0 0.0 ?
132 0.517 0.075 0.289 0.0 0.0 ?
133 0.517 0.425 0.211 0.0 0.0 ?
134 0.517 0.667 0.766 0.0 0.0 ?
135 0.517 0.833 0.734 0.0 0.0 ?
136 0.533 0.575 0.852 0.0 0.0 ?
137 0.533 0.583 0.844 0.0 0.0 ?
138 0.533 0.592 0.836 0.0 0.0 ?
139 0.533 0.908 0.664 0.0 0.0 ?
140 0.533 0.917 0.656 0.0 0.0 ?
141 0.533 0.925 0.648 0.0 0.0 ?
142 0.546 0.583 0.852 0.0 0.0 ?
143 0.546 0.917 0.648 0.0 0.0 ?
144 0.550 0.508 0.617 0.0 0.0 ?
145 0.550 0.992 0.883 0.0 0.0 ?
146 0.558 0.000 0.840 0.0 0.0 ?
147 0.558 0.500 0.660 0.0 0.0 ?
148 0.575 0.008 0.797 0.0 0.0 ?
149 0.575 0.017 0.789 0.0 0.0 ?
150 0.575 0.483 0.711 0.0 0.0 ?
151 0.575 0.492 0.703 0.0 0.0 ?
152 0.575 0.533 0.648 0.0 0.0 ?
153 0.575 0.642 0.820 0.0 0.0 ?
154 0.575 0.858 0.680 0.0 0.0 ?
155 0.575 0.967 0.852 0.0 0.0 ?
156 0.583 0.000 0.793 0.0 0.0 ?
157 0.583 0.500 0.707 0.0 0.0 ?
158 0.583 0.533 0.656 0.0 0.0 ?
159 0.583 0.546 0.648 0.0 0.0 ?
160 0.583 0.954 0.852 0.0 0.0 ?
161 0.583 0.967 0.844 0.0 0.0 ?
162 0.592 0.008 0.758 0.0 0.0 ?
163 0.592 0.492 0.742 0.0 0.0 ?
164 0.592 0.508 0.715 0.0 0.0 ?
165 0.592 0.533 0.664 0.0 0.0 ?
166 0.592 0.967 0.836 0.0 0.0 ?
167 0.592 0.992 0.785 0.0 0.0 ?
168 0.600 0.008 0.750 0.0 0.0 ?
169 0.600 0.492 0.750 0.0 0.0 ?
170 0.642 0.575 0.680 0.0 0.0 ?
171 0.642 0.925 0.820 0.0 0.0 ?
172 0.667 0.517 0.734 0.0 0.0 ?
173 0.667 0.983 0.766 0.0 0.0 ?
174 0.833 0.517 0.766 0.0 0.0 ?
175 0.833 0.983 0.734 0.0 0.0 ?
176 0.858 0.575 0.820 0.0 0.0 ?
177 0.858 0.925 0.680 0.0 0.0 ?
178 0.900 0.008 0.750 0.0 0.0 ?
179 0.900 0.492 0.750 0.0 0.0 ?
180 0.908 0.008 0.742 0.0 0.0 ?
181 0.908 0.492 0.758 0.0 0.0 ?
182 0.908 0.508 0.785 0.0 0.0 ?
183 0.908 0.533 0.836 0.0 0.0 ?
184 0.908 0.967 0.664 0.0 0.0 ?
185 0.908 0.992 0.715 0.0 0.0 ?
186 0.917 0.000 0.707 0.0 0.0 ?
187 0.917 0.500 0.793 0.0 0.0 ?
188 0.917 0.533 0.844 0.0 0.0 ?
189 0.917 0.546 0.852 0.0 0.0 ?
190 0.917 0.954 0.648 0.0 0.0 ?
191 0.917 0.967 0.656 0.0 0.0 ?
192 0.925 0.008 0.703 0.0 0.0 ?
193 0.925 0.017 0.711 0.0 0.0 ?
194 0.925 0.483 0.789 0.0 0.0 ?
195 0.925 0.492 0.797 0.0 0.0 ?
196 0.925 0.533 0.852 0.0 0.0 ?
197 0.925 0.642 0.680 0.0 0.0 ?
198 0.925 0.858 0.820 0.0 0.0 ?
199 0.925 0.967 0.648 0.0 0.0 ?
200 0.942 0.000 0.660 0.0 0.0 ?
201 0.942 0.500 0.840 0.0 0.0 ?
202 0.950 0.508 0.883 0.0 0.0 ?
203 0.954 0.583 0.648 0.0 0.0 ?
204 0.954 0.917 0.852 0.0 0.0 ?
205 0.950 0.992 0.617 0.0 0.0 ?
206 0.967 0.575 0.648 0.0 0.0 ?
207 0.967 0.583 0.656 0.0 0.0 ?
208 0.967 0.592 0.664 0.0 0.0 ?
209 0.967 0.908 0.836 0.0 0.0 ?
210 0.967 0.917 0.844 0.0 0.0 ?
211 0.967 0.925 0.852 0.0 0.0 ?
212 0.983 0.075 0.211 0.0 0.0 ?
213 0.983 0.425 0.289 0.0 0.0 ?
214 0.983 0.667 0.734 0.0 0.0 ?
215 0.983 0.833 0.766 0.0 0.0 ?
216 0.992 0.075 0.203 0.0 0.0 ?
217 0.992 0.092 0.242 0.0 0.0 ?
218 0.992 0.100 0.250 0.0 0.0 ?
219 0.992 0.400 0.250 0.0 0.0 ?
220 0.992 0.408 0.258 0.0 0.0 ?
221 0.992 0.425 0.297 0.0 0.0 ?
222 0.992 0.550 0.617 0.0 0.0 ?
223 0.992 0.592 0.715 0.0 0.0 ?
224 0.992 0.908 0.785 0.0 0.0 ?
225 0.992 0.950 0.883 0.0 0.0 ?

_smtbx_masks_void_probe_radius   0.1
_smtbx_masks_void_truncation_radius 0.1
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_a19132o_112_sq
_database_code_depnum_ccdc_archive 'CCDC 2159884'
loop_
_audit_author_name
_audit_author_address
'Younghun Kim'
;Yonsei University
South Korea
;
_audit_update_record             
;
2022-03-18 deposited with the CCDC.	2024-09-03 downloaded from the CCDC.
;
_audit_creation_date             2020-11-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C52 H28 N4 O16.5 Zn), O'
_chemical_formula_sum            'C104 H60 N8 O34 Zn2'
_chemical_formula_weight         2096.34
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           112
_space_group_name_H-M_alt        'P -4 2 c'
_space_group_name_Hall           'P -4 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'-y, -x, z+1/2'
'y, x, z+1/2'

_cell_length_a                   23.881(5)
_cell_length_b                   23.881(5)
_cell_length_c                   16.664(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9503(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.96
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.912
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.7336
_exptl_absorpt_correction_T_min  0.5450
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1403 before and 0.1137 after correction.
The Ratio of minimum to maximum transmission is 0.7429.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.733
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.109
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1267
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50510
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.296
_diffrn_reflns_theta_max         24.296
_diffrn_reflns_theta_min         2.961
_diffrn_ambient_temperature      172.85
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4958
_reflns_number_total             7724
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker APEXIII'
_computing_data_collection       'Bruker APEXIII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    SHELXS
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.680
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7724
_refine_ls_number_restraints     369
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.1076
_refine_ls_restrained_S_all      1.785
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.2975
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.53(5)
 0.47(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(N2) \\sim Ueq, Uanis(N20) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: O40(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C11(H11), C13(H13), C22(H22), C23(H23), C27(H27),
 C29(H29), C31(H31)
6.b Fitted pentagon refined as free rotating group:
 N2(C3,C4,C5,C6), N20(C21,C22,C23,C24)
6.c Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C26(C27,C28,C29,C30,C31)
6.d Tetrahedral OH refined with riding coordinates:
 O15(H15), O19(H19), O34(H34), O36(H36)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.5000 0.0000 0.05626(9) 0.0513(5) Uani 1 2 d S TU P . .
N2 N 0.5829(2) 0.0186(2) 0.0611(6) 0.082(2) Uani 1 1 d . U . . .
C3 C 0.6265(3) -0.0193(2) 0.0408(6) 0.089(2) Uani 1 1 d G U . . .
C4 C 0.6774(2) 0.0114(3) 0.0371(7) 0.096(3) Uani 1 1 d G U . . .
H4 H 0.7133 -0.0034 0.0247 0.116 Uiso 1 1 calc R . . . .
C5 C 0.6652(2) 0.0683(2) 0.0551(7) 0.099(3) Uani 1 1 d G U . . .
H5 H 0.6915 0.0981 0.0569 0.119 Uiso 1 1 calc R . . . .
C6 C 0.6068(3) 0.0727(2) 0.0699(6) 0.085(2) Uani 1 1 d G U . . .
C7 C 0.5716(4) 0.1239(4) 0.0803(8) 0.0723(19) Uani 1 1 d . U . . .
C8 C 0.6057(3) 0.1792(2) 0.0827(4) 0.0584(18) Uani 1 1 d . U . . .
C9 C 0.6244(3) 0.2022(3) 0.0109(3) 0.062(2) Uani 1 1 d G U . . .
H9 H 0.6137 0.1859 -0.0387 0.075 Uiso 1 1 calc R . . . .
C10 C 0.6589(3) 0.2491(3) 0.0118(3) 0.067(2) Uani 1 1 d G U . . .
C11 C 0.6747(3) 0.2730(2) 0.0845(3) 0.066(2) Uani 1 1 d G U . . .
H11 H 0.6982 0.3050 0.0851 0.079 Uiso 1 1 calc R . . . .
C12 C 0.6559(3) 0.2500(3) 0.1562(3) 0.0643(19) Uani 1 1 d G U . . .
C13 C 0.6214(3) 0.2031(3) 0.1553(3) 0.058(2) Uani 1 1 d G U . . .
H13 H 0.6086 0.1874 0.2043 0.069 Uiso 1 1 calc R . . . .
C14 C 0.6767(5) 0.2741(5) -0.0606(7) 0.080(2) Uani 1 1 d . U . . .
O15 O 0.6563(4) 0.2582(5) -0.1287(5) 0.121(3) Uani 1 1 d . U . . .
H15 H 0.6700 0.2778 -0.1657 0.181 Uiso 1 1 calc R . . . .
O16 O 0.7114(4) 0.3163(4) -0.0628(5) 0.092(3) Uani 1 1 d . U . . .
C17 C 0.6715(5) 0.2744(5) 0.2304(6) 0.075(2) Uani 1 1 d . U . . .
O18 O 0.7072(4) 0.3155(4) 0.2322(4) 0.098(3) Uani 1 1 d . U . . .
O19 O 0.6499(3) 0.2571(3) 0.2975(4) 0.087(3) Uani 1 1 d . U . . .
H19 H 0.6636 0.2754 0.3358 0.130 Uiso 1 1 calc R . . . .
N20 N 0.4790(2) 0.0835(2) 0.0600(6) 0.084(2) Uani 1 1 d . U . . .
C21 C 0.5165(2) 0.1275(3) 0.0801(6) 0.082(2) Uani 1 1 d G U . . .
C22 C 0.4859(3) 0.1785(2) 0.0795(7) 0.093(2) Uani 1 1 d G U . . .
H22 H 0.5005 0.2147 0.0908 0.112 Uiso 1 1 calc R . . . .
C23 C 0.4295(2) 0.1661(2) 0.0591(7) 0.097(2) Uani 1 1 d G U . . .
H23 H 0.3998 0.1924 0.0544 0.116 Uiso 1 1 calc R . . . .
C24 C 0.4253(2) 0.1073(2) 0.0471(7) 0.085(2) Uani 1 1 d G U . . .
C25 C 0.3783(4) 0.0777(4) 0.0444(8) 0.075(2) Uani 1 1 d . U . . .
C26 C 0.3242(2) 0.1103(3) 0.0428(5) 0.076(2) Uani 1 1 d . U . . .
C27 C 0.3005(3) 0.1256(3) -0.0302(4) 0.077(2) Uani 1 1 d G U . . .
H27 H 0.3177 0.1146 -0.0790 0.093 Uiso 1 1 calc R . . . .
C28 C 0.2515(3) 0.1571(3) -0.0317(4) 0.082(2) Uani 1 1 d G U . . .
C29 C 0.2263(2) 0.1734(3) 0.0398(5) 0.083(2) Uani 1 1 d G U . . .
H29 H 0.1929 0.1949 0.0388 0.100 Uiso 1 1 calc R . . . .
C30 C 0.2500(3) 0.1581(3) 0.1128(4) 0.084(2) Uani 1 1 d G U . . .
C31 C 0.2989(3) 0.1265(3) 0.1143(4) 0.080(2) Uani 1 1 d G U . . .
H31 H 0.3151 0.1161 0.1641 0.096 Uiso 1 1 calc R . . . .
C32 C 0.2326(6) 0.1764(6) -0.1060(9) 0.095(3) Uani 1 1 d . U . . .
O33 O 0.2514(5) 0.1553(4) -0.1733(6) 0.118(3) Uani 1 1 d . U . . .
O34 O 0.1861(4) 0.2070(4) -0.1104(6) 0.113(3) Uani 1 1 d . U . . .
H34 H 0.1804 0.2162 -0.1583 0.169 Uiso 1 1 calc R . . . .
C35 C 0.2288(6) 0.1745(7) 0.1841(9) 0.096(3) Uani 1 1 d . U . . .
O36 O 0.1876(4) 0.2127(4) 0.1850(6) 0.118(3) Uani 1 1 d . U . . .
H36 H 0.1768 0.2178 0.2324 0.176 Uiso 1 1 calc R . . . .
O37 O 0.2481(4) 0.1583(4) 0.2516(7) 0.119(3) Uani 1 1 d . U . . .
O39 O 0.5000 0.0000 0.2500 0.189(11) Uani 1 4 d S TU P . .
O40 O 0.5000 0.0000 -0.0858(16) 0.146(7) Uani 0.5 2 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N2 2.030(4) 2_655 ?
Zn1 N2 2.030(4) . ?
Zn1 N20 2.058(5) 2_655 ?
Zn1 N20 2.058(5) . ?
Zn1 O40 2.37(3) . ?
N2 C3 1.4200 . ?
N2 C6 1.4200 . ?
C3 C4 1.4200 . ?
C3 C25 1.402(10) 2_655 ?
C4 H4 0.9500 . ?
C4 C5 1.4200 . ?
C5 H5 0.9500 . ?
C5 C6 1.4200 . ?
C6 C7 1.493(12) . ?
C7 C8 1.553(8) . ?
C7 C21 1.319(11) . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 H9 0.9500 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C10 C14 1.412(12) . ?
C11 H11 0.9500 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C17 1.417(10) . ?
C13 H13 0.9500 . ?
C14 O15 1.293(13) . ?
C14 O16 1.306(11) . ?
O15 H15 0.8400 . ?
C17 O18 1.299(11) . ?
C17 O19 1.300(12) . ?
O19 H19 0.8400 . ?
N20 C21 1.4200 . ?
N20 C24 1.4200 . ?
C21 C22 1.4200 . ?
C22 H22 0.9500 . ?
C22 C23 1.4200 . ?
C23 H23 0.9500 . ?
C23 C24 1.4200 . ?
C24 C25 1.326(9) . ?
C25 C3 1.40(2) 2_655 ?
C25 C26 1.511(12) . ?
C26 C27 1.3900 . ?
C26 C31 1.3900 . ?
C27 H27 0.9500 . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C28 C32 1.396(16) . ?
C29 H29 0.9500 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C30 C35 1.350(15) . ?
C31 H31 0.9500 . ?
C32 O33 1.310(16) . ?
C32 O34 1.330(16) . ?
O34 H34 0.8400 . ?
C35 O36 1.341(16) . ?
C35 O37 1.276(17) . ?
O36 H36 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Zn1 N2 175.5(5) 2_655 . ?
N2 Zn1 N20 88.5(2) . 2_655 ?
N2 Zn1 N20 88.5(2) 2_655 . ?
N2 Zn1 N20 91.4(2) 2_655 2_655 ?
N2 Zn1 N20 91.4(2) . . ?
N2 Zn1 O40 92.3(3) 2_655 . ?
N2 Zn1 O40 92.3(3) . . ?
N20 Zn1 N20 176.5(5) 2_655 . ?
N20 Zn1 O40 91.7(3) . . ?
N20 Zn1 O40 91.7(3) 2_655 . ?
C3 N2 Zn1 124.5(4) . . ?
C3 N2 C6 108.0 . . ?
C6 N2 Zn1 126.5(4) . . ?
C4 C3 N2 108.0 . . ?
C25 C3 N2 124.3(6) 2_655 . ?
C25 C3 C4 125.9(6) 2_655 . ?
C3 C4 H4 126.0 . . ?
C3 C4 C5 108.0 . . ?
C5 C4 H4 126.0 . . ?
C4 C5 H5 126.0 . . ?
C4 C5 C6 108.0 . . ?
C6 C5 H5 126.0 . . ?
N2 C6 C5 108.0 . . ?
N2 C6 C7 122.0(5) . . ?
C5 C6 C7 129.4(5) . . ?
C6 C7 C8 113.8(7) . . ?
C21 C7 C6 128.0(7) . . ?
C21 C7 C8 117.8(8) . . ?
C9 C8 C7 118.9(6) . . ?
C9 C8 C13 120.0 . . ?
C13 C8 C7 120.8(6) . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 C14 120.6(6) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 C14 119.3(6) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 C17 120.1(5) . . ?
C13 C12 C17 119.9(5) . . ?
C8 C13 H13 120.0 . . ?
C12 C13 C8 120.0 . . ?
C12 C13 H13 120.0 . . ?
O15 C14 C10 120.9(8) . . ?
O15 C14 O16 116.2(10) . . ?
O16 C14 C10 122.8(9) . . ?
C14 O15 H15 109.5 . . ?
O18 C17 C12 120.3(8) . . ?
O18 C17 O19 118.7(8) . . ?
O19 C17 C12 121.0(8) . . ?
C17 O19 H19 109.5 . . ?
C21 N20 Zn1 124.8(3) . . ?
C24 N20 Zn1 127.1(3) . . ?
C24 N20 C21 108.0 . . ?
C7 C21 N20 125.4(6) . . ?
C7 C21 C22 124.8(6) . . ?
C22 C21 N20 108.0 . . ?
C21 C22 H22 126.0 . . ?
C21 C22 C23 108.0 . . ?
C23 C22 H22 126.0 . . ?
C22 C23 H23 126.0 . . ?
C24 C23 C22 108.0 . . ?
C24 C23 H23 126.0 . . ?
C23 C24 N20 108.0 . . ?
C25 C24 N20 123.7(7) . . ?
C25 C24 C23 126.3(7) . . ?
C3 C25 C26 116.2(7) 2_655 . ?
C24 C25 C3 127.1(9) . 2_655 ?
C24 C25 C26 116.7(8) . . ?
C27 C26 C25 120.0(7) . . ?
C27 C26 C31 120.0 . . ?
C31 C26 C25 120.0(7) . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C32 117.8(8) . . ?
C29 C28 C27 120.0 . . ?
C29 C28 C32 121.8(8) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C31 120.0 . . ?
C35 C30 C29 122.7(9) . . ?
C35 C30 C31 117.2(9) . . ?
C26 C31 H31 120.0 . . ?
C30 C31 C26 120.0 . . ?
C30 C31 H31 120.0 . . ?
O33 C32 C28 121.5(13) . . ?
O33 C32 O34 116.7(13) . . ?
O34 C32 C28 120.0(13) . . ?
C32 O34 H34 109.5 . . ?
O36 C35 C30 118.9(13) . . ?
O37 C35 C30 123.4(14) . . ?
O37 C35 O36 117.5(13) . . ?
C35 O36 H36 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O15 H15 O18 0.84 1.77 2.551(11) 153.2 7_664
O19 H19 O16 0.84 1.79 2.577(10) 156.3 7_665
O34 H34 O37 0.84 1.76 2.588(15) 166.3 8_554
O36 H36 O33 0.84 1.84 2.650(14) 162.4 8

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 N2 C3 C4 169.3(7) . . . . ?
Zn1 N2 C3 C25 -25.3(12) . . . 2_655 ?
Zn1 N2 C6 C5 -169.0(8) . . . . ?
Zn1 N2 C6 C7 2.6(11) . . . . ?
Zn1 N20 C21 C7 17.2(13) . . . . ?
Zn1 N20 C21 C22 -177.4(8) . . . . ?
Zn1 N20 C24 C23 177.3(8) . . . . ?
Zn1 N20 C24 C25 12.5(13) . . . . ?
N2 C3 C4 C5 0.0 . . . . ?
N2 C6 C7 C8 -175.8(7) . . . . ?
N2 C6 C7 C21 -2.7(17) . . . . ?
C3 N2 C6 C5 0.0 . . . . ?
C3 N2 C6 C7 171.6(11) . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C25 C26 C27 -88(2) 2_655 . . . ?
C3 C25 C26 C31 94(2) 2_655 . . . ?
C4 C5 C6 N2 0.0 . . . . ?
C4 C5 C6 C7 -170.8(12) . . . . ?
C5 C6 C7 C8 -6.1(14) . . . . ?
C5 C6 C7 C21 167.0(10) . . . . ?
C6 N2 C3 C4 0.0 . . . . ?
C6 N2 C3 C25 165.4(11) . . . 2_655 ?
C6 C7 C8 C9 78.9(10) . . . . ?
C6 C7 C8 C13 -95.7(10) . . . . ?
C6 C7 C21 N20 -8.0(18) . . . . ?
C6 C7 C21 C22 -171.0(10) . . . . ?
C7 C8 C9 C10 -174.6(8) . . . . ?
C7 C8 C13 C12 174.5(8) . . . . ?
C7 C21 C22 C23 165.5(12) . . . . ?
C8 C7 C21 N20 164.9(8) . . . . ?
C8 C7 C21 C22 1.8(15) . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C8 C9 C10 C14 -177.8(10) . . . . ?
C9 C8 C13 C12 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C9 C10 C14 O15 8.3(18) . . . . ?
C9 C10 C14 O16 -176.4(10) . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C17 -179.6(10) . . . . ?
C11 C10 C14 O15 -169.5(11) . . . . ?
C11 C10 C14 O16 5.8(17) . . . . ?
C11 C12 C13 C8 0.0 . . . . ?
C11 C12 C17 O18 -5.8(17) . . . . ?
C11 C12 C17 O19 172.9(10) . . . . ?
C13 C8 C9 C10 0.0 . . . . ?
C13 C12 C17 O18 174.7(10) . . . . ?
C13 C12 C17 O19 -6.7(17) . . . . ?
C14 C10 C11 C12 177.8(10) . . . . ?
C17 C12 C13 C8 179.6(10) . . . . ?
N20 C21 C22 C23 0.0 . . . . ?
N20 C24 C25 C3 -11(3) . . . 2_655 ?
N20 C24 C25 C26 171.0(8) . . . . ?
C21 C7 C8 C9 -95.0(11) . . . . ?
C21 C7 C8 C13 90.4(11) . . . . ?
C21 N20 C24 C23 0.0 . . . . ?
C21 N20 C24 C25 -164.9(12) . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C22 C23 C24 N20 0.0 . . . . ?
C22 C23 C24 C25 164.4(12) . . . . ?
C23 C24 C25 C3 -173(2) . . . 2_655 ?
C23 C24 C25 C26 8.9(16) . . . . ?
C24 N20 C21 C7 -165.4(12) . . . . ?
C24 N20 C21 C22 0.0 . . . . ?
C24 C25 C26 C27 90.6(11) . . . . ?
C24 C25 C26 C31 -87.4(12) . . . . ?
C25 C3 C4 C5 -165.1(12) 2_655 . . . ?
C25 C26 C27 C28 -178.0(6) . . . . ?
C25 C26 C31 C30 178.0(6) . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C26 C27 C28 C32 173.5(9) . . . . ?
C27 C26 C31 C30 0.0 . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
C27 C28 C32 O33 16.0(16) . . . . ?
C27 C28 C32 O34 -179.6(9) . . . . ?
C28 C29 C30 C31 0.0 . . . . ?
C28 C29 C30 C35 177.1(10) . . . . ?
C29 C28 C32 O33 -170.6(10) . . . . ?
C29 C28 C32 O34 -6.3(16) . . . . ?
C29 C30 C31 C26 0.0 . . . . ?
C29 C30 C35 O36 -8.5(16) . . . . ?
C29 C30 C35 O37 175.9(11) . . . . ?
C31 C26 C27 C28 0.0 . . . . ?
C31 C30 C35 O36 168.7(9) . . . . ?
C31 C30 C35 O37 -6.9(18) . . . . ?
C32 C28 C29 C30 -173.2(10) . . . . ?
C35 C30 C31 C26 -177.2(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.53(5)
2 0.47(5)

