# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-h2o
_database_code_depnum_ccdc_archive 'CCDC 2114806'
loop_
_audit_author_name
_audit_author_address
'Dong-Dong Zhou'
;Sun Yat Sen University
China
;
_audit_update_record             
;
2021-10-10 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_audit_creation_date             2021-09-23
_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            1-H2O
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.25(C80 H56 K4 N32 O64), 0.25(H12 O4), 2.5(H2 O)'
_chemical_formula_sum            'C20 H22 K N8 O19.50'
_chemical_formula_weight         725.55
_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 0.0181 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'
K K 0.3868 1.0657 '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'

_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           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   27.5128(5)
_cell_length_b                   27.5128(5)
_cell_length_c                   3.52247(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2666.35(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.2940
_cell_measurement_theta_min      3.2100
_shelx_estimated_absorpt_T_max   1.0000
_shelx_estimated_absorpt_T_min   0.34664
_exptl_absorpt_coefficient_mu    2.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            9947
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.424
_diffrn_reflns_theta_max         67.424
_diffrn_reflns_theta_min         3.212
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB P300DS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1094
_reflns_number_total             1204
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.387
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1204
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0656
_refine_ls_restrained_S_all      1.028
_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)+(0.1082P)²+22.8458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1977
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H2(0.5) O5(0.25) H5A(0.25) H5B(0.25) H5C(0.25) O6(0.3125)
 H6A(0.3125) H6B(0.3125) O7(0.3125) H7A(0.3125) H7B(0.3125)
4.a Riding coordinates:
 O3(H3), N1(H1), N2(H2), O5(H5A,H5B,H5C), O6(H6A,H6B), O7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_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
K1 K 0.5000 0.2500 0.3750 0.0340(6) Uani 1 4 d S T P . .
O1 O 0.44315(9) 0.18954(9) -0.1164(8) 0.0215(7) Uani 1 1 d . . . . .
O2 O 0.37815(9) 0.14302(9) -0.0114(9) 0.0258(7) Uani 1 1 d . . . . .
O3 O 0.36008(9) 0.06209(10) 0.2583(9) 0.0312(8) Uani 1 1 d . . . . .
H3 H 0.3638 0.0904 0.1632 0.047 Uiso 1 1 d R . . . .
O4 O 0.40044(11) -0.00067(11) 0.4933(10) 0.0367(8) Uani 1 1 d . . . . .
N1 N 0.50503(10) 0.11569(11) 0.1094(8) 0.0167(7) Uani 1 1 d . . . . .
H1 H 0.5202 0.1390 0.0252 0.025 Uiso 1 1 d R . . . .
N2 N 0.49072(11) 0.04341(10) 0.3417(9) 0.0174(7) Uani 1 1 d . . . . .
H2 H 0.4994 0.0175 0.4756 0.026 Uiso 0.5 1 d R . . . .
C1 C 0.42335(13) 0.15061(12) -0.0105(10) 0.0174(8) Uani 1 1 d . . . . .
C2 C 0.45567(13) 0.11091(12) 0.1219(10) 0.0165(8) Uani 1 1 d . . . . .
C3 C 0.44681(12) 0.06558(12) 0.2688(10) 0.0166(8) Uani 1 1 d . . . . .
C4 C 0.40043(13) 0.03938(14) 0.3481(11) 0.0233(9) Uani 1 1 d . . . . .
C5 C 0.52497(13) 0.07442(12) 0.2418(10) 0.0185(8) Uani 1 1 d . . . . .
H5 H 0.5589 0.0684 0.2606 0.022 Uiso 1 1 calc R . . . .
O5 O 0.3011(5) -0.0086(4) 0.639(5) 0.031(3) Uani 0.25 1 d . U . A 3
H5A H 0.2891 -0.0187 0.8540 0.047 Uiso 0.25 1 d R . . A 3
H5B H 0.2877 0.0148 0.5302 0.047 Uiso 0.25 1 d R . . A 3
H5C H 0.3313 -0.0060 0.5935 0.047 Uiso 0.25 1 d R . . A 3
O6 O 0.3147(7) -0.0258(6) 0.996(4) 0.040(4) Uani 0.3125 1 d . U . B 2
H6A H 0.3065 -0.0297 1.2262 0.060 Uiso 0.3125 1 d R . . B 2
H6B H 0.2930 -0.0094 0.8812 0.060 Uiso 0.3125 1 d R . . B 2
O7 O 0.3127(6) -0.0187(6) 0.858(5) 0.027(3) Uani 0.3125 1 d . U . C 1
H7A H 0.3031 -0.0220 0.6301 0.041 Uiso 0.3125 1 d R . . C 1
H7B H 0.2884 -0.0203 1.0069 0.041 Uiso 0.3125 1 d R . . 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
K1 K1 3.52247(8) 1_556 ?
K1 K1 3.52247(9) 1_554 ?
K1 O1 2.865(3) 6_554 ?
K1 O1 2.902(3) 16_655 ?
K1 O1 2.865(3) 11_666 ?
K1 O1 2.865(3) . ?
K1 O1 2.902(3) 1_556 ?
K1 O1 2.902(3) 6 ?
K1 O1 2.902(3) 11_665 ?
K1 O1 2.865(3) 16_656 ?
O1 K1 2.902(3) 1_554 ?
O1 C1 1.258(4) . ?
O2 C1 1.261(4) . ?
O3 H3 0.8533 . ?
O3 C4 1.312(5) . ?
O4 C4 1.215(5) . ?
N1 H1 0.8211 . ?
N1 C2 1.365(4) . ?
N1 C5 1.345(5) . ?
N2 H2 0.8878 . ?
N2 C3 1.378(4) . ?
N2 C5 1.319(5) . ?
C1 C2 1.484(5) . ?
C2 C3 1.372(5) . ?
C3 C4 1.492(5) . ?
C5 H5 0.9500 . ?
O5 H5A 0.8715 . ?
O5 H5B 0.8331 . ?
O5 H5C 0.8504 . ?
O6 H6A 0.8498 . ?
O6 H6B 0.8506 . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8500 . ?

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
K1 K1 K1 180.0 1_554 1_556 ?
O1 K1 K1 51.88(5) 1_556 1_556 ?
O1 K1 K1 52.84(5) 11_666 1_556 ?
O1 K1 K1 51.88(5) 11_665 1_554 ?
O1 K1 K1 128.12(5) 1_556 1_554 ?
O1 K1 K1 128.12(5) 11_665 1_556 ?
O1 K1 K1 127.16(5) . 1_556 ?
O1 K1 K1 127.16(5) 16_656 1_554 ?
O1 K1 K1 51.88(5) 16_655 1_554 ?
O1 K1 K1 127.16(5) 11_666 1_554 ?
O1 K1 K1 52.84(5) 16_656 1_556 ?
O1 K1 K1 52.84(5) 6_554 1_554 ?
O1 K1 K1 127.16(5) 6_554 1_556 ?
O1 K1 K1 52.84(5) . 1_554 ?
O1 K1 K1 51.88(5) 6 1_556 ?
O1 K1 K1 128.12(5) 6 1_554 ?
O1 K1 K1 128.12(5) 16_655 1_556 ?
O1 K1 O1 68.11(3) 6_554 16_655 ?
O1 K1 O1 179.04(9) . 6 ?
O1 K1 O1 105.68(10) 6_554 . ?
O1 K1 O1 68.11(3) . 16_655 ?
O1 K1 O1 68.10(3) . 11_665 ?
O1 K1 O1 112.40(6) 6 16_655 ?
O1 K1 O1 68.11(3) 11_666 6 ?
O1 K1 O1 111.40(5) 16_656 6_554 ?
O1 K1 O1 105.68(10) 16_656 11_666 ?
O1 K1 O1 111.40(5) 11_666 6_554 ?
O1 K1 O1 75.28(6) 16_656 16_655 ?
O1 K1 O1 68.11(3) 11_666 1_556 ?
O1 K1 O1 68.11(3) 16_656 6 ?
O1 K1 O1 179.04(9) 6_554 1_556 ?
O1 K1 O1 75.28(6) 6_554 6 ?
O1 K1 O1 75.28(6) . 1_556 ?
O1 K1 O1 179.04(9) 16_656 11_665 ?
O1 K1 O1 103.76(10) 6 1_556 ?
O1 K1 O1 68.11(3) 6_554 11_665 ?
O1 K1 O1 112.40(6) 11_665 1_556 ?
O1 K1 O1 112.40(5) 6 11_665 ?
O1 K1 O1 111.40(5) 16_656 . ?
O1 K1 O1 179.04(9) 11_666 16_655 ?
O1 K1 O1 111.40(5) 11_666 . ?
O1 K1 O1 103.76(10) 11_665 16_655 ?
O1 K1 O1 75.28(6) 11_666 11_665 ?
O1 K1 O1 68.11(3) 16_656 1_556 ?
O1 K1 O1 112.40(5) 16_655 1_556 ?
K1 O1 K1 75.28(6) . 1_554 ?
C1 O1 K1 154.7(2) . 1_554 ?
C1 O1 K1 123.5(2) . . ?
C4 O3 H3 115.3 . . ?
C2 N1 H1 126.3 . . ?
C5 N1 H1 125.3 . . ?
C5 N1 C2 108.3(3) . . ?
C3 N2 H2 133.6 . . ?
C5 N2 H2 118.0 . . ?
C5 N2 C3 106.9(3) . . ?
O1 C1 O2 124.6(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 C2 118.0(3) . . ?
N1 C2 C1 121.0(3) . . ?
N1 C2 C3 106.1(3) . . ?
C3 C2 C1 132.9(3) . . ?
N2 C3 C4 120.1(3) . . ?
C2 C3 N2 108.5(3) . . ?
C2 C3 C4 131.4(3) . . ?
O3 C4 C3 116.6(3) . . ?
O4 C4 O3 122.2(3) . . ?
O4 C4 C3 121.1(3) . . ?
N1 C5 H5 124.8 . . ?
N2 C5 N1 110.3(3) . . ?
N2 C5 H5 124.8 . . ?
H5A O5 H5B 118.7 . . ?
H5A O5 H5C 124.2 . . ?
H5B O5 H5C 106.2 . . ?
H6A O6 H6B 109.5 . . ?
H7A O7 H7B 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
