# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_TPT-EN
_audit_block_doi                 10.5517/ccdc.csd.cc2j5l4g
_database_code_depnum_ccdc_archive 'CCDC 2329065'
loop_
_audit_author_name
_audit_author_address
'Kuo Zhang Kuo Zhang'
;Nankai University
China
;
_audit_update_record             
;
2024-01-29 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_date             2024-01-20
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Zn-adc-tpt
_chemical_name_systematic        Zn-adc-tpt
_chemical_formula_moiety         'C66 H39 N6 O13 Zn3'
_chemical_formula_sum            'C66 H39 N6 O13 Zn3'
_chemical_formula_weight         1320.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zn'
_chemical_oxdiff_usercomment     'C H O N Zn'
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   16.7370(2)
_cell_length_b                   16.7370(2)
_cell_length_c                   15.8689(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3849.75(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3772
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6100
_cell_measurement_theta_min      4.1050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.855
_diffrn_reflns_theta_min         4.131
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  -5.00   0.50    6.43    --    0.00 -22.00  59.00   50
  2  ω     80.00 187.00   0.50   25.73    --  101.30  19.00 -45.00  214
  3  ω     12.00 103.00   0.50   25.73    --  101.30 -43.00  41.00  182
  4  ω    -31.00  13.00   0.50    6.43    --    0.00  82.00-180.00   88
  5  ω    -33.00  37.00   0.50    6.43    --    0.00  82.00  30.00  140
  6  ω    115.00 141.00   0.50   25.73    --  101.30  82.00  90.00   52
  7  ω    163.00 191.00   0.50   25.73    --  101.30  82.00  90.00   56
  8  ω    136.00 177.00   0.50   25.73    --  101.30  82.00 150.00   82
  9  ω     82.00 123.00   0.50   25.73    --  101.30  82.00 150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0269374000
_diffrn_orient_matrix_UB_12      -0.0091718000
_diffrn_orient_matrix_UB_13      -0.0938358000
_diffrn_orient_matrix_UB_21      0.0509858000
_diffrn_orient_matrix_UB_22      -0.0537463000
_diffrn_orient_matrix_UB_23      -0.0161908000
_diffrn_orient_matrix_UB_31      -0.0892877000
_diffrn_orient_matrix_UB_32      -0.0911648000
_diffrn_orient_matrix_UB_33      0.0191951000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2271
_reflns_number_total             2633
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0815P)²+2.6535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1410
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N6(H6), C10(H10), C12(H12), C2(H2), C11(H11), C9(H9), C3(H3)
;
_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
Zn16 Zn 0.26447(2) 0.73553(2) 0.250000 0.01950(18) Uani 1 2 d S T P . .
O7 O 0.18283(13) 0.66124(12) 0.35734(11) 0.0252(4) Uani 1 1 d . . . . .
O18 O 0.15755(12) 0.51865(12) 0.33151(12) 0.0258(4) Uani 1 1 d . . . . .
O20 O 0.333333 0.666667 0.250000 0.0442(15) Uani 1 6 d S T P . .
N15 N 0.19120(10) 0.80880(10) 0.250000 0.0243(7) Uani 1 2 d S T P . .
C4 C 0.14273(17) 0.57601(18) 0.36921(16) 0.0223(5) Uani 1 1 d . . . . .
C22 C 0.06835(18) 0.53706(17) 0.43643(16) 0.0232(5) Uani 1 1 d . . . . .
C24 C 0.09103(18) 0.51960(18) 0.51684(17) 0.0242(5) Uani 1 1 d . . . . .
C13 C -0.02128(18) 0.51856(18) 0.41899(17) 0.0257(6) Uani 1 1 d . . . . .
N6 N -0.04706(12) 0.9059(2) 0.250000 0.0580(14) Uani 1 2 d S T P . .
H6 H -0.077421 0.845159 0.250000 0.070 Uiso 1 2 calc R U P . .
C10 C 0.1826(2) 0.5394(2) 0.53757(19) 0.0330(7) Uani 1 1 d . . . . .
H10 H 0.229185 0.563631 0.495507 0.040 Uiso 1 1 calc R U . . .
C12 C 0.0470(2) 0.4653(2) 0.66224(19) 0.0347(7) Uani 1 1 d . . . . .
H12 H 0.001570 0.439543 0.705299 0.042 Uiso 1 1 calc R U . . .
C2 C 0.2035(2) 0.5242(3) 0.6160(2) 0.0446(8) Uani 1 1 d . . . . .
H2 H 0.264978 0.539246 0.628733 0.054 Uiso 1 1 calc R U . . .
C11 C 0.1346(2) 0.4858(3) 0.6795(2) 0.0474(9) Uani 1 1 d . . . . .
H11 H 0.149903 0.474588 0.734202 0.057 Uiso 1 1 calc R U . . .
C19 C 0.09584(14) 0.90416(14) 0.250000 0.0464(13) Uani 1 2 d S T P . .
C9 C 0.2345(2) 0.8992(2) 0.2586(3) 0.0448(9) Uani 1 1 d . . . . .
H9 H 0.299561 0.931053 0.266191 0.054 Uiso 1 1 calc R U . . .
C3 C 0.1897(2) 0.9500(2) 0.2572(3) 0.0557(11) Uani 1 1 d . . . . .
H3 H 0.223687 1.015363 0.261145 0.067 Uiso 1 1 calc R U . . .
C17 C 0.04459(16) 0.95541(16) 0.250000 0.0537(15) Uani 1 2 d S T 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
Zn16 O7 2.1484(17) 4_665 ?
Zn16 O7 2.1484(17) . ?
Zn16 O18 2.1441(18) 6_565 ?
Zn16 O18 2.1441(18) 3_565 ?
Zn16 O20 1.9963(4) . ?
Zn16 N15 2.124(3) . ?
O7 C4 1.250(3) . ?
O18 C4 1.257(3) . ?
N15 C9 1.318(3) . ?
N15 C9 1.318(3) 4_665 ?
C4 C22 1.517(3) . ?
C22 C24 1.403(4) . ?
C22 C13 1.399(4) . ?
C24 C13 1.436(4) 7_566 ?
C24 C10 1.434(4) . ?
C13 C12 1.427(4) 7_566 ?
N6 H6 0.8800 . ?
N6 C17 1.330(3) . ?
N6 C17 1.330(3) 3_465 ?
C10 H10 0.9500 . ?
C10 C2 1.351(5) . ?
C12 H12 0.9500 . ?
C12 C11 1.357(5) . ?
C2 H2 0.9500 . ?
C2 C11 1.421(5) . ?
C11 H11 0.9500 . ?
C19 C3 1.366(4) 4_665 ?
C19 C3 1.366(4) . ?
C19 C17 1.486(6) . ?
C9 H9 0.9500 . ?
C9 C3 1.387(4) . ?
C3 H3 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
O7 Zn16 O7 174.31(10) . 4_665 ?
O18 Zn16 O7 90.04(7) 3_565 . ?
O18 Zn16 O7 89.56(7) 3_565 4_665 ?
O18 Zn16 O7 90.04(7) 6_565 4_665 ?
O18 Zn16 O7 89.56(7) 6_565 . ?
O18 Zn16 O18 172.02(10) 6_565 3_565 ?
O20 Zn16 O7 92.84(5) . . ?
O20 Zn16 O7 92.84(5) . 4_665 ?
O20 Zn16 O18 93.99(5) . 3_565 ?
O20 Zn16 O18 93.99(5) . 6_565 ?
O20 Zn16 N15 180.0 . . ?
N15 Zn16 O7 87.16(5) . . ?
N15 Zn16 O7 87.16(5) . 4_665 ?
N15 Zn16 O18 86.01(5) . 3_565 ?
N15 Zn16 O18 86.01(5) . 6_565 ?
C4 O7 Zn16 127.08(16) . . ?
C4 O18 Zn16 134.55(17) . 2_665 ?
Zn16 O20 Zn16 120.0 . 2_665 ?
Zn16 O20 Zn16 120.0 2_665 3_565 ?
Zn16 O20 Zn16 120.0 . 3_565 ?
C9 N15 Zn16 121.16(17) . . ?
C9 N15 Zn16 121.16(17) 4_665 . ?
C9 N15 C9 117.7(3) . 4_665 ?
O7 C4 O18 127.0(2) . . ?
O7 C4 C22 117.0(2) . . ?
O18 C4 C22 116.1(2) . . ?
C24 C22 C4 118.7(2) . . ?
C13 C22 C4 121.0(2) . . ?
C13 C22 C24 120.4(2) . . ?
C22 C24 C13 119.5(2) . 7_566 ?
C22 C24 C10 122.0(2) . . ?
C10 C24 C13 118.5(2) . 7_566 ?
C22 C13 C24 120.1(3) . 7_566 ?
C22 C13 C12 121.9(3) . 7_566 ?
C12 C13 C24 118.0(3) 7_566 7_566 ?
C17 N6 H6 122.7 . . ?
C17 N6 H6 122.7 3_465 . ?
C17 N6 C17 114.6(4) . 3_465 ?
C24 C10 H10 119.5 . . ?
C2 C10 C24 121.1(3) . . ?
C2 C10 H10 119.5 . . ?
C13 C12 H12 119.2 7_566 . ?
C11 C12 C13 121.6(3) . 7_566 ?
C11 C12 H12 119.2 . . ?
C10 C2 H2 119.7 . . ?
C10 C2 C11 120.6(3) . . ?
C11 C2 H2 119.7 . . ?
C12 C11 C2 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
C3 C19 C3 118.6(4) . 4_665 ?
C3 C19 C17 120.7(2) 4_665 . ?
C3 C19 C17 120.7(2) . . ?
N15 C9 H9 118.5 . . ?
N15 C9 C3 123.1(3) . . ?
C3 C9 H9 118.5 . . ?
C19 C3 C9 118.7(3) . . ?
C19 C3 H3 120.6 . . ?
C9 C3 H3 120.6 . . ?
N6 C17 N6 125.4(4) . 2_675 ?
N6 C17 C19 117.3(2) 2_675 . ?
N6 C17 C19 117.3(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
Zn16 O7 C4 O18 17.0(4) . . . . ?
Zn16 O7 C4 C22 -163.20(17) . . . . ?
Zn16 O18 C4 O7 13.0(4) 2_665 . . . ?
Zn16 O18 C4 C22 -166.75(17) 2_665 . . . ?
Zn16 N15 C9 C3 178.6(3) . . . . ?
O7 C4 C22 C24 -98.1(3) . . . . ?
O7 C4 C22 C13 82.0(3) . . . . ?
O18 C4 C22 C24 81.7(3) . . . . ?
O18 C4 C22 C13 -98.2(3) . . . . ?
N15 C9 C3 C19 2.8(6) . . . . ?
C4 C22 C24 C13 -179.1(2) . . . 7_566 ?
C4 C22 C24 C10 1.4(4) . . . . ?
C4 C22 C13 C24 179.1(2) . . . 7_566 ?
C4 C22 C13 C12 0.4(4) . . . 7_566 ?
C22 C24 C10 C2 178.4(3) . . . . ?
C24 C22 C13 C24 -0.8(4) . . . 7_566 ?
C24 C22 C13 C12 -179.4(3) . . . 7_566 ?
C24 C10 C2 C11 1.6(6) . . . . ?
C13 C22 C24 C13 0.8(4) . . . 7_566 ?
C13 C22 C24 C10 -178.7(3) . . . . ?
C13 C24 C10 C2 -1.1(5) 7_566 . . . ?
C13 C12 C11 C2 -0.2(6) 7_566 . . . ?
C10 C2 C11 C12 -0.9(6) . . . . ?
C9 N15 C9 C3 -1.4(3) 4_665 . . . ?
C3 C19 C3 C9 -1.3(3) 4_665 . . . ?
C3 C19 C17 N6 -174.4(2) . . . . ?
C3 C19 C17 N6 5.6(2) . . . 2_675 ?
C3 C19 C17 N6 5.6(2) 4_665 . . . ?
C3 C19 C17 N6 -174.4(2) 4_665 . . 2_675 ?
C17 N6 C17 N6 0.0 3_465 . . 2_675 ?
C17 N6 C17 C19 180.0 3_465 . . . ?
C17 C19 C3 C9 178.7(3) . . . . ?

_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 0.000 0.000 -0.066 1539.2 403.5 ?
2 0.333 0.667 0.750 13.4 0.0 ?
3 0.667 0.333 0.250 13.4 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.361
_oxdiff_exptl_absorpt_empirical_full_min 0.569
####################################################################### 
# 
# 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_ni-tpt
_database_code_depnum_ccdc_archive 'CCDC 2329063'
loop_
_audit_author_name
_audit_author_address
'Kuo Zhang'
;Nankai University
China
;
_audit_update_record             
;
2024-01-29 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_audit_creation_date             2024-01-17
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            Ni-bodc-tpt
_chemical_name_systematic        Ni-bodc-tpt
_chemical_formula_moiety         'C30 H36 Ni3 O13, 2(C9 H6 N3)'
_chemical_formula_sum            'C48 H48 N6 Ni3 O13'
_chemical_formula_weight         1093.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Ni'
_chemical_oxdiff_usercomment     'C H O N Ni'
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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   16.7926(6)
_cell_length_b                   16.7926(6)
_cell_length_c                   14.6396(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3575.2(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6767
_cell_measurement_temperature    210(90)
_cell_measurement_theta_max      75.5850
_cell_measurement_theta_min      4.2940
_shelx_estimated_absorpt_T_max   0.879
_shelx_estimated_absorpt_T_min   0.778
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12516
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.057
_diffrn_reflns_theta_min         4.285
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      210(90)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -3.00  22.00   0.50    5.00    --    0.00  13.00 145.00   50
  2  ω    -45.00 -20.00   0.50    5.00    --    0.00 -13.00 -25.00   50
  3  ω     65.00  91.00   0.50   20.00    --  101.30 -13.00 -25.00   52
  4  ω    138.00 164.00   0.50   20.00    --  101.30  13.00 145.00   52
  5  ω    -35.00  23.00   0.50    5.00    --    0.00 -82.00 -30.00  116
  6  ω    -23.00  37.00   0.50    5.00    --    0.00  82.00 -90.00  120
  7  ω     -5.00  20.00   0.50    5.00    --    0.00  82.00-180.00   50
  8  ω     78.00 160.00   0.50   20.00    --  101.30  38.00-180.00  164
  9  ω     51.00 112.00   0.50   20.00    --  101.30 -77.00-150.00  122
 10  ω     52.00 123.00   0.50   20.00    --  101.30 -38.00 -60.00  142
 11  ω     17.00 117.00   0.50   20.00    --  101.30 -57.00-150.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092904000
_diffrn_orient_matrix_UB_12      0.0416952000
_diffrn_orient_matrix_UB_13      -0.0903838000
_diffrn_orient_matrix_UB_21      -0.0154354000
_diffrn_orient_matrix_UB_22      0.0699449000
_diffrn_orient_matrix_UB_23      0.0539367000
_diffrn_orient_matrix_UB_31      0.1043652000
_diffrn_orient_matrix_UB_32      0.0677130000
_diffrn_orient_matrix_UB_33      -0.0000204000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1198
_reflns_number_total             1417
_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       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     178
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0689
_refine_ls_restrained_S_all      1.157
_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)+(0.1233P)²+3.2310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2255
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C10 = O3-C10 = O2-C1 = O1-C1
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C10 \\sim C9 \\sim C8 \\sim C5 \\sim C6 \\sim C4 \\sim C3 \\sim C7
\\sim O3 \\sim C1 \\sim O2 \\sim O1 \\sim C2: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
Uanis(O4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O4(0.333333) C10(0.333333) C9(0.333333) C8(0.333333) H8A(0.333333)
 H8B(0.333333) C5(0.166667) H5A(0.166667) H5B(0.166667) C6(0.333333)
 H6A(0.333333) H6B(0.333333) C4(0.333333) H4A(0.333333) H4B(0.333333)
 C3(0.166667) H3A(0.166667) H3B(0.166667) C7(0.166667) H7A(0.166667)
 H7B(0.166667) O3(0.333333) C1(0.166667) O2(0.166667) O1(0.166667) C2(0.166667)
 Fixed X: C9(0.4603) C5(0.54023) C2(0.544439)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12)
;
_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 0.47105(6) 0.73552(3) 0.250000 0.0364(4) Uani 1 4 d S T P . .
O5 O 0.333333 0.666667 0.250000 0.063(3) Uani 1 12 d S T P . .
N1 N 0.6167(3) 0.80834(17) 0.250000 0.0489(13) Uani 1 4 d S T P . .
N2 N 0.95282(19) 1.04718(19) 0.250000 0.069(2) Uani 1 4 d S T P . .
O4 O 0.3449(14) 0.8269(12) 0.3524(15) 0.042(3) Uani 0.3333 1 d D U P A -1
C13 C 0.8088(4) 0.9044(2) 0.250000 0.0572(19) Uani 1 4 d S T P . .
C11 C 0.6642(3) 0.9000(3) 0.250000 0.0641(16) Uani 1 2 d S T P . .
H11 H 0.631584 0.932013 0.250000 0.077 Uiso 1 2 calc R U P A .
C14 C 0.9103(5) 0.9552(2) 0.250000 0.065(2) Uani 1 4 d S T P . .
C12 C 0.7592(4) 0.9501(3) 0.250000 0.074(2) Uani 1 2 d S T P . .
H12 H 0.789914 1.014714 0.250000 0.089 Uiso 1 2 calc R U P . .
C10 C 0.4287(15) 0.8589(7) 0.3648(7) 0.055(2) Uani 0.3333 1 d D U P A -1
C9 C 0.460300 0.9280(7) 0.4485(7) 0.0594(18) Uani 0.3333 1 d S U P A -1
C8 C 0.3821(10) 0.9413(10) 0.4861(11) 0.073(2) Uani 0.3333 1 d . U P A -1
H8A H 0.331984 0.883090 0.509701 0.088 Uiso 0.3333 1 calc R U P A -1
H8B H 0.357614 0.963697 0.438002 0.088 Uiso 0.3333 1 calc R U P A -1
C5 C 0.540230 1.0961(14) 0.4704(14) 0.062(3) Uani 0.1667 1 d . U P A -1
H5A H 0.595135 1.155623 0.458038 0.074 Uiso 0.1667 1 calc R U P A -1
H5B H 0.485655 1.102458 0.463154 0.074 Uiso 0.1667 1 calc R U P A -1
C6 C 0.5354(9) 1.0154(9) 0.4007(10) 0.070(2) Uani 0.3333 1 d . U P A -1
H6A H 0.517057 1.021678 0.338770 0.083 Uiso 0.3333 1 calc R U P A -1
H6B H 0.594233 1.016424 0.398285 0.083 Uiso 0.3333 1 calc R U P A -1
C4 C 0.5013(10) 0.9051(10) 0.5258(10) 0.072(2) Uani 0.3333 1 d . U P A -1
H4A H 0.538206 0.879344 0.502045 0.086 Uiso 0.3333 1 calc R U P A -1
H4B H 0.451890 0.857714 0.563149 0.086 Uiso 0.3333 1 calc R U P A -1
C3 C 0.563(2) 0.990(2) 0.587(2) 0.061(3) Uani 0.1667 1 d . U P A -1
H3A H 0.553371 0.970725 0.651721 0.073 Uiso 0.1667 1 calc R U P A -1
H3B H 0.628125 1.012030 0.573019 0.073 Uiso 0.1667 1 calc R U P A -1
C7 C 0.426(2) 1.015(2) 0.565(2) 0.065(3) Uani 0.1667 1 d . U P A -1
H7A H 0.396585 0.985551 0.623325 0.078 Uiso 0.1667 1 calc R U P A -1
H7B H 0.413636 1.064826 0.553795 0.078 Uiso 0.1667 1 calc R U P A -1
O3 O 0.4829(11) 0.8402(9) 0.3246(8) 0.053(3) Uani 0.3333 1 d D U P A -1
C1 C 0.586(2) 1.1597(17) 0.6153(16) 0.058(4) Uani 0.1667 1 d D U P A -1
O2 O 0.536(2) 1.194(3) 0.627(2) 0.049(5) Uani 0.1667 1 d D U P A -1
O1 O 0.665(3) 1.191(4) 0.643(4) 0.057(7) Uani 0.1667 1 d D U P A -1
C2 C 0.544439 1.0595(18) 0.5750(17) 0.060(3) Uani 0.1667 1 d . U P A -1


_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 O5 2.0028(9) . ?
Ni1 N1 2.118(5) . ?
Ni1 O3 1.993(14) . ?
N1 C11 1.333(5) . ?
N1 C11 1.333(5) 21_565 ?
N2 C14 1.339(4) 3_675 ?
N2 C14 1.339(4) . ?
O4 C10 1.243(17) . ?
C13 C14 1.476(9) . ?
C13 C12 1.387(6) . ?
C13 C12 1.387(6) 21_565 ?
C11 H11 0.9400 . ?
C11 C12 1.382(7) . ?
C12 H12 0.9400 . ?
C10 C9 1.586(16) . ?
C10 O3 1.249(16) . ?
C9 C8 1.539(16) . ?
C9 C6 1.544(15) . ?
C9 C4 1.472(17) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 C7 1.58(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 C6 1.67(2) . ?
C5 C2 1.66(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 C3 1.56(3) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C2 1.37(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 C2 1.75(3) . ?
C1 O2 1.236(19) . ?
C1 O1 1.24(2) . ?
C1 C2 1.58(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ni1 N1 180.00(6) . . ?
O3 Ni1 O5 95.0(4) . . ?
O3 Ni1 N1 85.0(4) . . ?
Ni1 O5 Ni1 120.0 . 3_565 ?
Ni1 O5 Ni1 120.002(1) 2_665 3_565 ?
Ni1 O5 Ni1 120.001(1) 2_665 . ?
C11 N1 Ni1 121.2(3) . . ?
C11 N1 Ni1 121.2(3) 21_565 . ?
C11 N1 C11 117.6(5) 21_565 . ?
C14 N2 C14 114.9(7) 3_675 . ?
C12 C13 C14 121.4(3) . . ?
C12 C13 C14 121.4(3) 21_565 . ?
C12 C13 C12 117.2(6) . 21_565 ?
N1 C11 H11 118.5 . . ?
N1 C11 C12 123.0(4) . . ?
C12 C11 H11 118.5 . . ?
N2 C14 N2 125.1(7) 2_765 . ?
N2 C14 C13 117.5(3) 2_765 . ?
N2 C14 C13 117.5(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
O4 C10 C9 108.8(14) . . ?
O4 C10 O3 129.1(13) . . ?
O3 C10 C9 122.0(17) . . ?
C8 C9 C10 112.6(11) . . ?
C8 C9 C6 112.0(12) . . ?
C6 C9 C10 99.2(9) . . ?
C4 C9 C10 115.6(12) . . ?
C4 C9 C8 107.9(12) . . ?
C4 C9 C6 109.3(8) . . ?
C9 C8 H8A 110.5 . . ?
C9 C8 H8B 110.5 . . ?
C9 C8 C7 106.0(15) . . ?
H8A C8 H8B 108.7 . . ?
C7 C8 H8A 110.5 . . ?
C7 C8 H8B 110.5 . . ?
H5A C5 H5B 108.8 . . ?
C6 C5 H5A 110.8 . . ?
C6 C5 H5B 110.8 . . ?
C2 C5 H5A 110.8 . . ?
C2 C5 H5B 110.8 . . ?
C2 C5 C6 104.9(16) . . ?
C9 C6 C5 100.3(10) . . ?
C9 C6 H6A 111.7 . . ?
C9 C6 H6B 111.7 . . ?
C5 C6 H6A 111.7 . . ?
C5 C6 H6B 111.7 . . ?
H6A C6 H6B 109.5 . . ?
C9 C4 H4A 108.9 . . ?
C9 C4 H4B 108.9 . . ?
C9 C4 C3 113.2(15) . . ?
H4A C4 H4B 107.8 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C2 C3 C4 111(2) . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C8 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
C8 C7 C2 112.5(19) . . ?
H7A C7 H7B 107.8 . . ?
C2 C7 H7A 109.1 . . ?
C2 C7 H7B 109.1 . . ?
C10 O3 Ni1 135.8(12) . . ?
O2 C1 C2 120(3) . . ?
O1 C1 O2 126(3) . . ?
O1 C1 C2 113(3) . . ?
C5 C2 C7 80.6(14) . . ?
C3 C2 C5 121(2) . . ?
C3 C2 C7 110(2) . . ?
C3 C2 C1 134(2) . . ?
C1 C2 C5 91.6(18) . . ?
C1 C2 C7 107(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
Ni1 N1 C11 C12 180.0 . . . . ?
N1 C11 C12 C13 0.0 . . . . ?
O4 C10 C9 C8 -3.9(17) . . . . ?
O4 C10 C9 C6 -122.6(13) . . . . ?
O4 C10 C9 C4 120.7(15) . . . . ?
O4 C10 O3 Ni1 -20(3) . . . . ?
C11 N1 C11 C12 0.0 21_565 . . . ?
C14 N2 C14 N2 0.0 3_675 . . 2_765 ?
C14 N2 C14 C13 180.0 3_675 . . . ?
C14 C13 C12 C11 180.0 . . . . ?
C12 C13 C14 N2 180.0 . . . 2_765 ?
C12 C13 C14 N2 180.0 21_565 . . . ?
C12 C13 C14 N2 0.0 . . . . ?
C12 C13 C14 N2 0.0 21_565 . . 2_765 ?
C12 C13 C12 C11 0.0 21_565 . . . ?
C10 C9 C8 C7 -177.6(18) . . . . ?
C10 C9 C6 C5 158.4(12) . . . . ?
C10 C9 C4 C3 158.1(16) . . . . ?
C9 C10 O3 Ni1 155.6(10) . . . . ?
C9 C8 C7 C2 5(3) . . . . ?
C9 C4 C3 C2 19(3) . . . . ?
C8 C9 C6 C5 39.3(12) . . . . ?
C8 C9 C4 C3 -74.8(19) . . . . ?
C8 C7 C2 C5 63(3) . . . . ?
C8 C7 C2 C3 -56(3) . . . . ?
C8 C7 C2 C1 152(2) . . . . ?
C6 C9 C8 C7 -67(2) . . . . ?
C6 C9 C4 C3 47.3(18) . . . . ?
C6 C5 C2 C3 14.1(15) . . . . ?
C6 C5 C2 C7 -93.6(14) . . . . ?
C6 C5 C2 C1 159.6(15) . . . . ?
C4 C9 C8 C7 54(2) . . . . ?
C4 C9 C6 C5 -80.3(12) . . . . ?
C4 C3 C2 C5 -50(2) . . . . ?
C4 C3 C2 C7 41(3) . . . . ?
C4 C3 C2 C1 -178(2) . . . . ?
O3 C10 C9 C8 179.3(12) . . . . ?
O3 C10 C9 C6 60.6(14) . . . . ?
O3 C10 C9 C4 -56.1(14) . . . . ?
O2 C1 C2 C5 76(3) . . . . ?
O2 C1 C2 C3 -147(3) . . . . ?
O2 C1 C2 C7 -5(3) . . . . ?
O1 C1 C2 C5 -114(3) . . . . ?
O1 C1 C2 C3 23(5) . . . . ?
O1 C1 C2 C7 165(4) . . . . ?
C2 C5 C6 C9 47.0(8) . . . . ?

_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 -0.034 -0.770 -0.742 1543.6 440.8 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.255
_oxdiff_exptl_absorpt_empirical_full_min 0.228
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dimethylacetamide?DI water'
