# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_x_sq
_database_code_depnum_ccdc_archive 'CCDC 2093277'
loop_
_audit_author_name
_audit_author_address
'Yao Xiao'
;Liaoning Normal University
China
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_audit_creation_date             2022-05-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C24 H12 Cd2 N3 O9, C24 H12 Cd1 N3 O9, 4.005[H2O], 0.5[C3H7NO]'
_chemical_formula_sum            'C49.50 H35.51 Cd3 N6.50 O22.50'
_chemical_formula_weight         1418.55
_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'
Cd Cd -0.8075 1.2024 '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'

_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           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   17.118(3)
_cell_length_b                   17.118(3)
_cell_length_c                   13.766(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3493(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5801
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.408
_cell_measurement_theta_min      1.374
_shelx_estimated_absorpt_T_max   0.971
_shelx_estimated_absorpt_T_min   0.622
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (VRUKER,2016/2) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22290
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.408
_diffrn_reflns_theta_min         1.479
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3080
_reflns_number_total             5776
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         2.605
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.0082(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5776
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0965
_refine_ls_restrained_S_all      1.033
_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)+(0.1915P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2761
_refine_ls_wR_factor_ref         0.2965
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.745(4)
 0.255(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C9-C10
 1.536 with sigma of 0.002
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
Uanis(Cd2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6. Others
 Fixed Sof: Cd1(0.33333)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14), C15(H15)
;
_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
Cd1 Cd 0.3202(3) 0.6485(6) 0.52872(15) 0.0934(15) Uani 0.3333 1 d . U P . .
Cd2 Cd 0.333333 0.666667 0.79857(8) 0.0562(4) Uani 1 3 d S TU P . .
Cd3 Cd 0.666667 0.333333 0.81282(13) 0.0896(5) Uani 1 3 d S TU P . .
O2 O 0.2318(7) 0.6957(7) 0.7411(8) 0.115(3) Uani 1 1 d . U . . .
O1 O 0.2796(8) 0.7461(8) 0.5930(8) 0.125(2) Uani 1 1 d . U . . .
O3 O -0.0323(3) 0.8325(3) 0.6257(5) 0.0546(12) Uani 1 1 d . U . . .
O5 O 0.5381(5) 0.2556(8) 0.9141(6) 0.116(3) Uani 1 1 d . U . . .
O4 O 0.5281(5) 0.2362(7) 0.7649(7) 0.115(4) Uani 1 1 d . U . . .
O6 O 0.1239(4) -0.0452(3) 0.8795(5) 0.0599(14) Uani 1 1 d . U . . .
N1 N 0.0873(4) 0.0682(4) 0.8783(5) 0.0459(14) Uani 1 1 d . U . . .
N2 N 0.0715(4) 0.9854(4) 0.6256(5) 0.0422(13) Uani 1 1 d . U . . .
C1 C 0.4941(6) 0.2167(7) 0.8472(8) 0.0672(19) Uani 1 1 d . U . . .
C2 C 0.3956(6) 0.1483(6) 0.8548(8) 0.0628(17) Uani 1 1 d . U . . .
C3 C 0.3540(6) 0.1209(7) 0.9474(8) 0.069(2) Uani 1 1 d . U . . .
H3 H 0.386868 0.146605 1.003814 0.083 Uiso 1 1 calc R U . . .
C4 C 0.2645(6) 0.0559(7) 0.9521(8) 0.068(2) Uani 1 1 d . U . . .
H4 H 0.237018 0.034408 1.012111 0.081 Uiso 1 1 calc R U . . .
C5 C 0.2174(5) 0.0237(5) 0.8711(7) 0.0498(13) Uani 1 1 d . U . . .
C6 C 0.2536(6) 0.0447(7) 0.7823(8) 0.071(2) Uani 1 1 d . U . . .
H6 H 0.219060 0.019049 0.726814 0.085 Uiso 1 1 calc R U . . .
C7 C 0.3427(6) 0.1049(7) 0.7769(8) 0.075(3) Uani 1 1 d . U . . .
H7 H 0.369637 0.117537 0.715910 0.091 Uiso 1 1 calc R U . . .
C8 C 0.0632(5) -0.0189(5) 0.8760(6) 0.0459(15) Uani 1 1 d . U . . .
C9 C 0.2362(11) 0.7347(14) 0.6660(10) 0.123(4) Uani 1 1 d D U . . .
C10 C 0.1621(7) 0.7599(7) 0.6554(10) 0.084(2) Uani 1 1 d D U . . .
C11 C 0.1166(9) 0.7649(9) 0.7292(9) 0.094(3) Uani 1 1 d . U . . .
H11 H 0.130045 0.751406 0.790201 0.113 Uiso 1 1 calc R U . . .
C12 C 0.0498(8) 0.7888(7) 0.7244(8) 0.077(2) Uani 1 1 d . U . . .
H12 H 0.016435 0.787363 0.778368 0.093 Uiso 1 1 calc R U . . .
C13 C 0.0373(6) 0.8141(5) 0.6358(7) 0.0546(15) Uani 1 1 d . U . . .
C14 C 0.0810(7) 0.8136(7) 0.5571(9) 0.079(3) Uani 1 1 d . U . . .
H14 H 0.068195 0.828751 0.496682 0.094 Uiso 1 1 calc R U . . .
C15 C 0.1492(8) 0.7887(8) 0.5684(9) 0.088(3) Uani 1 1 d . U . . .
H15 H 0.184670 0.792295 0.515568 0.105 Uiso 1 1 calc R U . . .
C16 C -0.0137(5) 0.9203(5) 0.6250(6) 0.0406(14) Uani 1 1 d . U . . .


_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
Cd1 Cd1 0.482(12) 3_565 ?
Cd1 Cd1 0.482(12) 2_665 ?
Cd1 O1 1.927(13) 2_665 ?
Cd1 O1 2.286(15) . ?
Cd1 O1 2.343(11) 3_565 ?
Cd2 O2 2.181(8) . ?
Cd2 O2 2.181(8) 3_565 ?
Cd2 O2 2.181(8) 2_665 ?
Cd3 O5 2.373(8) . ?
Cd3 O5 2.373(8) 3_665 ?
Cd3 O5 2.373(8) 2_655 ?
Cd3 O4 2.210(8) 2_655 ?
Cd3 O4 2.210(8) . ?
Cd3 O4 2.209(8) 3_665 ?
O2 C9 1.213(17) . ?
O1 C9 1.205(16) . ?
O3 C13 1.383(9) . ?
O3 C16 1.373(9) . ?
O5 C1 1.165(12) . ?
O4 C1 1.241(13) . ?
O6 C5 1.442(9) . ?
O6 C8 1.323(9) . ?
N1 C8 1.307(9) 2 ?
N1 C8 1.335(9) . ?
N2 C16 1.315(9) 2_675 ?
N2 C16 1.320(8) . ?
C1 C2 1.500(12) . ?
C2 C3 1.420(15) . ?
C2 C7 1.360(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.374(13) . ?
C4 H4 0.9300 . ?
C4 C5 1.325(13) . ?
C5 C6 1.336(14) . ?
C6 H6 0.9300 . ?
C6 C7 1.350(13) . ?
C7 H7 0.9300 . ?
C9 C10 1.537(2) . ?
C10 C11 1.308(17) . ?
C10 C15 1.354(17) . ?
C11 H11 0.9300 . ?
C11 C12 1.395(16) . ?
C12 H12 0.9300 . ?
C12 C13 1.347(14) . ?
C13 C14 1.318(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.437(13) . ?
C15 H15 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
Cd1 Cd1 Cd1 59.999(17) 3_565 2_665 ?
Cd1 Cd1 O1 90.8(19) 2_665 . ?
Cd1 Cd1 O1 37.7(17) 3_565 . ?
Cd1 Cd1 O1 146.1(15) 3_565 2_665 ?
Cd1 Cd1 O1 77.3(17) 3_565 3_565 ?
Cd1 Cd1 O1 133.5(18) 2_665 2_665 ?
Cd1 Cd1 O1 27.3(11) 2_665 3_565 ?
O1 Cd1 O1 107.0(5) 2_665 3_565 ?
O1 Cd1 O1 96.1(4) . 3_565 ?
O1 Cd1 O1 109.3(4) 2_665 . ?
O2 Cd2 O2 107.6(3) . 2_665 ?
O2 Cd2 O2 107.6(3) 3_565 2_665 ?
O2 Cd2 O2 107.6(3) . 3_565 ?
O5 Cd3 O5 89.0(3) 2_655 3_665 ?
O5 Cd3 O5 89.0(3) . 3_665 ?
O5 Cd3 O5 89.0(3) 2_655 . ?
O4 Cd3 O5 53.7(3) 2_655 2_655 ?
O4 Cd3 O5 119.2(4) 3_665 . ?
O4 Cd3 O5 119.2(4) 2_655 3_665 ?
O4 Cd3 O5 129.2(4) 3_665 2_655 ?
O4 Cd3 O5 53.7(3) . . ?
O4 Cd3 O5 119.2(4) . 2_655 ?
O4 Cd3 O5 53.7(3) 3_665 3_665 ?
O4 Cd3 O5 129.2(4) 2_655 . ?
O4 Cd3 O5 129.2(4) . 3_665 ?
O4 Cd3 O4 111.5(2) 2_655 3_665 ?
O4 Cd3 O4 111.5(2) 2_655 . ?
O4 Cd3 O4 111.5(2) 3_665 . ?
C9 O2 Cd2 126.7(9) . . ?
Cd1 O1 Cd1 6.6(4) 3_565 2_665 ?
Cd1 O1 Cd1 11.9(3) . 2_665 ?
Cd1 O1 Cd1 8.8(2) 3_565 . ?
C9 O1 Cd1 134.5(12) . 3_565 ?
C9 O1 Cd1 132.5(10) . 2_665 ?
C9 O1 Cd1 126.4(11) . . ?
C16 O3 C13 119.7(6) . . ?
C1 O5 Cd3 90.5(7) . . ?
C1 O4 Cd3 96.5(7) . . ?
C8 O6 C5 117.2(5) . . ?
C8 N1 C8 113.5(7) 2 . ?
C16 N2 C16 112.3(7) 2_675 . ?
O5 C1 O4 119.1(9) . . ?
O5 C1 C2 123.0(10) . . ?
O4 C1 C2 117.8(10) . . ?
C3 C2 C1 120.1(9) . . ?
C7 C2 C1 123.6(10) . . ?
C7 C2 C3 116.2(8) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(9) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.8(10) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 O6 117.9(8) . . ?
C4 C5 C6 123.7(8) . . ?
C6 C5 O6 118.0(8) . . ?
C5 C6 H6 121.6 . . ?
C5 C6 C7 116.8(10) . . ?
C7 C6 H6 121.6 . . ?
C2 C7 H7 117.8 . . ?
C6 C7 C2 124.3(10) . . ?
C6 C7 H7 117.8 . . ?
O6 C8 N1 121.5(6) . . ?
N1 C8 O6 111.9(6) 3 . ?
N1 C8 N1 126.4(7) 3 . ?
O2 C9 C10 113.8(13) . . ?
O1 C9 O2 131.5(11) . . ?
O1 C9 C10 113.8(12) . . ?
C11 C10 C9 123.1(12) . . ?
C11 C10 C15 116.9(9) . . ?
C15 C10 C9 119.6(12) . . ?
C10 C11 H11 117.1 . . ?
C10 C11 C12 125.8(11) . . ?
C12 C11 H11 117.1 . . ?
C11 C12 H12 122.5 . . ?
C13 C12 C11 115.0(12) . . ?
C13 C12 H12 122.5 . . ?
C12 C13 O3 117.2(9) . . ?
C14 C13 O3 118.4(8) . . ?
C14 C13 C12 124.0(9) . . ?
C13 C14 H14 121.3 . . ?
C13 C14 C15 117.4(11) . . ?
C15 C14 H14 121.3 . . ?
C10 C15 C14 120.5(11) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
N2 C16 O3 113.7(6) 3_465 . ?
N2 C16 O3 118.6(6) . . ?
N2 C16 N2 127.7(7) 3_465 . ?

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
Cd1 O1 C9 O2 28(3) 3_565 . . . ?
Cd1 O1 C9 O2 33(3) . . . . ?
Cd1 O1 C9 O2 19(3) 2_665 . . . ?
Cd1 O1 C9 C10 -135.4(11) . . . . ?
Cd1 O1 C9 C10 -148.6(10) 2_665 . . . ?
Cd1 O1 C9 C10 -139.9(12) 3_565 . . . ?
Cd2 O2 C9 O1 23(3) . . . . ?
Cd2 O2 C9 C10 -169.2(9) . . . . ?
Cd3 O5 C1 O4 -4.8(12) . . . . ?
Cd3 O5 C1 C2 179.6(8) . . . . ?
Cd3 O4 C1 O5 5.2(12) . . . . ?
Cd3 O4 C1 C2 -179.0(7) . . . . ?
O2 C9 C10 C11 20(2) . . . . ?
O2 C9 C10 C15 -168.0(14) . . . . ?
O1 C9 C10 C11 -169.8(15) . . . . ?
O1 C9 C10 C15 2(2) . . . . ?
O3 C13 C14 C15 -176.1(9) . . . . ?
O5 C1 C2 C3 -6.9(16) . . . . ?
O5 C1 C2 C7 177.5(12) . . . . ?
O4 C1 C2 C3 177.5(10) . . . . ?
O4 C1 C2 C7 1.8(16) . . . . ?
O6 C5 C6 C7 -175.6(9) . . . . ?
C1 C2 C3 C4 -177.8(9) . . . . ?
C1 C2 C7 C6 -178.4(10) . . . . ?
C2 C3 C4 C5 -3.9(15) . . . . ?
C3 C2 C7 C6 5.8(17) . . . . ?
C3 C4 C5 O6 179.3(8) . . . . ?
C3 C4 C5 C6 6.4(15) . . . . ?
C4 C5 C6 C7 -2.7(15) . . . . ?
C5 O6 C8 N1 176.1(7) . . . 3 ?
C5 O6 C8 N1 -9.2(13) . . . . ?
C5 C6 C7 C2 -3.7(17) . . . . ?
C7 C2 C3 C4 -1.8(15) . . . . ?
C8 O6 C5 C4 96.9(9) . . . . ?
C8 O6 C5 C6 -89.8(10) . . . . ?
C8 N1 C8 O6 -178.8(4) 2 . . . ?
C8 N1 C8 N1 -4.9(19) 2 . . 3 ?
C9 C10 C11 C12 178.9(14) . . . . ?
C9 C10 C15 C14 -179.3(13) . . . . ?
C10 C11 C12 C13 -4.6(19) . . . . ?
C11 C10 C15 C14 -6.7(18) . . . . ?
C11 C12 C13 O3 175.7(9) . . . . ?
C11 C12 C13 C14 2.7(15) . . . . ?
C12 C13 C14 C15 -3.2(16) . . . . ?
C13 O3 C16 N2 -173.1(8) . . . 3_465 ?
C13 O3 C16 N2 5.8(12) . . . . ?
C13 C14 C15 C10 5.2(18) . . . . ?
C15 C10 C11 C12 7(2) . . . . ?
C16 O3 C13 C12 100.8(9) . . . . ?
C16 O3 C13 C14 -85.8(10) . . . . ?
C16 N2 C16 O3 -179.9(4) 2_675 . . . ?
C16 N2 C16 N2 -1.2(18) 2_675 . . 3_465 ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  
;
A solvent mask was calculated and 120 electrons were 
found in a volume of 1472Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
8.01[H2O], 1[C3H7NO] per Asymmetric Unit 
which account for 120 electrons 
per unit cell.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 -0.013 491 40 '4.005 H2O'
2 0.500 1.000 -0.014 491 40 '4.005 H2O'
3 0.500 0.500 -0.016 490 40 '1.0 C3H7NO'

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.745(4)
2 0.255(4)

####################################################################### 
# 
# 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_k1_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 2093279'
loop_
_audit_author_name
_audit_author_address
'Yao Xiao'
;Liaoning Normal University
China
;
_audit_update_record             
;
2022-05-19 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C24 H14.007 N3 O11.013 Zn2, 0.498[C3H7NO], 1.002[H3O], 1.002[H2O], 2.002[H2O]'
_chemical_formula_sum            'C25.49 H26.51 N3.50 O15.52 Zn2'
_chemical_formula_weight         760.95
_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      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
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'
'-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'

_cell_length_a                   16.8223(18)
_cell_length_b                   16.8223(18)
_cell_length_c                   6.8892(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1688.4(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    885
_cell_measurement_temperature    301.26
_cell_measurement_theta_max      23.747
_cell_measurement_theta_min      2.796
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.493
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (VRUKER,2016/2) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.0
_exptl_crystal_size_min          0.0
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0911
_diffrn_reflns_Laue_measured_fraction_full 0.651
_diffrn_reflns_Laue_measured_fraction_max 0.651
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2538
_diffrn_reflns_point_group_measured_fraction_full 0.651
_diffrn_reflns_point_group_measured_fraction_max 0.651
_diffrn_reflns_theta_full        25.131
_diffrn_reflns_theta_max         25.131
_diffrn_reflns_theta_min         4.071
_diffrn_ambient_temperature      301.26
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.651
_diffrn_measured_fraction_theta_max 0.651
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                413
_reflns_number_total             715
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         715
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0740
_refine_ls_restrained_S_all      0.913
_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)+(0.1318P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.2067
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O4-C2 \\sim C2-O2
 with sigma of 0.001
 Zn1-O1 \\sim Zn1-O1A
 with sigma of 0.02
 C7-C1 \\sim C1-C3
 with sigma of 0.001
 C8-O3 \\sim O3-C4
 with sigma of 0.001
3. Restrained planarity
 O4, C1, O2, C2, C7, C3, C4, C5, O3, C8
 with sigma of 0.001
4. Rigid bond restraints
 H1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Zn1 \\sim O1 \\sim O1A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(C1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uiso(O1A) = Uiso(O1)
6. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C8, C7, O2, O4, O3, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: C1(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C8(0.5)
 H8(0.5) C7(0.5) H7(0.5) O2(0.5) O1(0.16777) O4(0.5) O1A(0.16777) H1A(0.16777)
 H1(0.16667)
8.a Everything fixed:
 H1A, H1
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C7(H7)
8.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C8,C7)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.666667 0.333333 0.4983(2) 0.0468(7) Uani 1 3 d DS T P . .
C1 C 0.50524(13) 0.21732(9) 0.2210(13) 0.036(3) Uani 0.5 1 d D U P A -1
C2 C 0.4047(3) 0.1477(2) 0.2287(10) 0.035(3) Uani 0.5 1 d DG . P A -1
C3 C 0.3609(3) 0.1180(3) 0.4069(8) 0.044(6) Uani 0.5 1 d DG . P A -1
H3 H 0.393823 0.141251 0.521363 0.053 Uiso 0.5 1 calc R U P A -1
C4 C 0.2678(4) 0.0535(4) 0.4140(5) 0.044(8) Uani 0.5 1 d DG . P A -1
H4 H 0.238468 0.033664 0.533260 0.053 Uiso 0.5 1 calc R U P A -1
C5 C 0.2186(3) 0.0188(3) 0.2430(3) 0.031(2) Uani 0.5 1 d G . P A -1
C8 C 0.2624(3) 0.0485(4) 0.0648(5) 0.061(12) Uani 0.5 1 d DG . P A -1
H8 H 0.229492 0.025252 -0.049634 0.073 Uiso 0.5 1 calc R U P A -1
C7 C 0.3555(3) 0.1130(3) 0.0577(8) 0.048(7) Uani 0.5 1 d DG . P A -1
H7 H 0.384847 0.132839 -0.061535 0.058 Uiso 0.5 1 calc R U P A -1
C6 C 0.0650(8) -0.0189(7) 0.250000 0.027(2) Uani 1 2 d S T P A .
O2 O 0.5493(3) 0.2484(2) 0.3771(15) 0.059(4) Uani 0.5 1 d D U P A -1
O3 O 0.1271(5) -0.0446(5) 0.250000 0.0382(16) Uani 1 2 d DS T P . .
N1 N -0.0207(6) -0.0910(5) 0.250000 0.021(2) Uani 1 2 d S T P . .
O1 O 0.661(3) 0.265(3) 0.757(7) 0.071(10) Uiso 0.1678 1 d D U P A -1
O4 O 0.5420(3) 0.2421(2) 0.0495(15) 0.052(4) Uani 0.5 1 d D U P A -1
O1A O 0.686(7) 0.326(9) 0.797(4) 0.071(10) Uiso 0.1678 1 d D U P A -2
H1A H 0.632210 0.303290 0.841440 0.107 Uiso 0.1678 1 d . U P B -2
H1 H 0.653130 0.210470 0.852670 0.071 Uiso 0.1667 1 d . . P C -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
Zn1 O2 1.953(5) . ?
Zn1 O1 2.09(3) . ?
Zn1 O1A 2.10(2) . ?
C1 C2 1.501(5) . ?
C1 O2 1.261(9) . ?
C1 O4 1.302(8) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 H3 0.9300 . ?
C3 C4 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 C8 1.3900 . ?
C5 O3 1.366(9) . ?
C8 H8 0.9300 . ?
C8 C7 1.3900 . ?
C7 H7 0.9300 . ?
C6 O3 1.314(13) . ?
C6 N1 1.338(13) 2 ?
C6 N1 1.342(13) . ?
O1 H1 1.0884 . ?
O1A H1A 0.8376 . ?

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
O2 Zn1 O1 102.2(13) . . ?
O2 C1 C2 119.5(4) . . ?
O2 C1 O4 123.7(4) . . ?
O4 C1 C2 116.8(3) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 C7 120.0 . . ?
C7 C2 C1 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C8 C5 C4 120.0 . . ?
O3 C5 C4 120.0 . . ?
O3 C5 C8 120.0 . . ?
C5 C8 H8 120.0 . . ?
C7 C8 C5 120.0 . . ?
C7 C8 H8 120.0 . . ?
C2 C7 H7 120.0 . . ?
C8 C7 C2 120.0 . . ?
C8 C7 H7 120.0 . . ?
O3 C6 N1 120.1(10) . 2 ?
O3 C6 N1 112.0(9) . . ?
N1 C6 N1 128.0(12) 2 . ?
C1 O2 Zn1 146.8(6) . . ?
C6 O3 C5 120.9(6) . . ?
C6 N1 C6 112.0(12) 3 . ?
Zn1 O1 H1 158.7 . . ?
Zn1 O1A H1A 103.0 . . ?

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
C1 C2 C3 C4 180.0 . . . . ?
C1 C2 C7 C8 180.0 . . . . ?
C2 C1 O2 Zn1 -177.2(4) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C2 C7 C8 0.0 . . . . ?
C3 C4 C5 C8 0.0 . . . . ?
C3 C4 C5 O3 179.99(6) . . . . ?
C4 C5 C8 C7 0.0 . . . . ?
C4 C5 O3 C6 90.71(18) . . . . ?
C5 C8 C7 C2 0.0 . . . . ?
C8 C5 O3 C6 -89.31(18) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
O2 C1 C2 C3 0.00(4) . . . . ?
O2 C1 C2 C7 180.00(2) . . . . ?
O3 C5 C8 C7 -179.99(6) . . . . ?
O3 C6 N1 C6 180.0 . . . 3 ?
N1 C6 O3 C5 177.64(11) . . . . ?
N1 C6 O3 C5 -2.36(11) 2 . . . ?
N1 C6 N1 C6 0.0 2 . . 3 ?
O4 C1 C2 C3 180.00(2) . . . . ?
O4 C1 C2 C7 0.00(4) . . . . ?
O4 C1 O2 Zn1 2.8(4) . . . . ?

_platon_squeeze_details          ?
_platon_squeeze_special_details  
;
A solvent mask was calculated and 126 electrons were 
found in a volume of 596Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C3H7NO], 2[H3O], 6[H20] per Asymmetric Unit 
which account for 124 electrons 
per unit cell.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 -0.027 199 42 '0.498 DMF,1.002 H3O,1.002 H2O'
2 0.500 1.000 -0.033 199 43 '0.498 DMF,1.002 H3O,1.002 H2O'
3 0.500 0.500 -0.037 198 42 '4.004 H2O'

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
