# Supplementary Information (SI) for Dalton Transactions.
# 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_5-27-1
_database_code_depnum_ccdc_archive 'CCDC 2354198'
loop_
_audit_author_name
_audit_author_address
'Kai Li'
;Jinzhong University
China
;
_audit_update_record             
;
2024-05-09 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_audit_creation_date             2019-06-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.13(Cl24 K8), 0.5(H4 O2), C4 H12 N2'
_chemical_formula_sum            'C4 H14 Cl3 K N2 O'
_chemical_formula_weight         251.62
_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'
Cl Cl 0.3639 0.7018 '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      orthorhombic
_space_group_IT_number           57
_space_group_name_H-M_alt        'P b c m'
_space_group_name_Hall           '-P 2c 2b'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, z'

_cell_length_a                   6.41538(13)
_cell_length_b                   12.7348(3)
_cell_length_c                   12.7219(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1039.35(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2496
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      72.8650
_cell_measurement_theta_min      3.4750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.214
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3008
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.087
_diffrn_reflns_theta_min         6.902
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  87.00   0.50    0.50    --    0.00  77.00-180.00  104
  2  ω    -37.00  10.00   0.50    0.50    --    0.00  57.00 -30.00   94
  3  ω     48.00 171.00   0.50    0.50    --   98.20  30.00 120.00  246
  4  ω     46.00 118.00   0.50    0.50    --   98.20 -82.00  90.00  144
  5  ω     10.00  43.00   0.50    0.50    --   98.20 -82.00  90.00   66
  6  ω     74.00 156.00   0.50    0.50    --   98.20  61.00-180.00  164
  7  ω     85.00 141.00   0.50    0.50    --   98.20 -82.00  30.00  112
;
_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      -0.1216081000
_diffrn_orient_matrix_UB_12      -0.1007857000
_diffrn_orient_matrix_UB_13      0.0265222000
_diffrn_orient_matrix_UB_21      -0.2061069000
_diffrn_orient_matrix_UB_22      0.0620109000
_diffrn_orient_matrix_UB_23      -0.0034665000
_diffrn_orient_matrix_UB_31      -0.0209936000
_diffrn_orient_matrix_UB_32      -0.0246969000
_diffrn_orient_matrix_UB_33      -0.1181485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                1041
_reflns_number_total             1066
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.484
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.207
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         1066
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.207
_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)+(0.0589P)²+0.5465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0964
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H1E(0.5) H1F(0.5)
3.a Free rotating group:
 O1(H1E,H1F)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.00396(8) 0.76217(5) 0.250000 0.0087(2) Uani 1 2 d S T P . .
Cl3 Cl -0.06110(9) 0.750000 0.500000 0.0072(2) Uani 1 2 d S T P . .
Cl2 Cl 0.49985(9) 0.74649(5) 0.250000 0.0084(2) Uani 1 2 d S T P . .
Cl1 Cl -0.01924(9) 0.51405(5) 0.250000 0.0080(2) Uani 1 2 d S T P . .
O1 O 0.4542(3) 0.48446(15) 0.250000 0.0077(4) Uani 1 2 d S T P . .
H1E H 0.325886 0.492757 0.264383 0.012 Uiso 0.5 1 d G . . . .
H1F H 0.467119 0.419391 0.237825 0.012 Uiso 0.5 1 d G . . . .
N1 N 0.6225(2) 0.56947(10) 0.43493(10) 0.0054(3) Uani 1 1 d . . . . .
H1A H 0.588192 0.548931 0.370344 0.007 Uiso 1 1 calc R . . . .
H1B H 0.713800 0.621798 0.429311 0.007 Uiso 1 1 calc R . . . .
C1 C 0.5679(3) 0.39216(14) 0.50943(13) 0.0069(4) Uani 1 1 d . . . . .
H1C H 0.528407 0.362403 0.442124 0.008 Uiso 1 1 calc R . . . .
H1D H 0.633219 0.337238 0.550733 0.008 Uiso 1 1 calc R . . . .
C2 C 0.7213(3) 0.48002(15) 0.49218(12) 0.0066(4) Uani 1 1 d . . . . .
H2A H 0.773011 0.504376 0.559557 0.008 Uiso 1 1 calc R . . . .
H2B H 0.838925 0.454094 0.451922 0.008 Uiso 1 1 calc R . . . .


_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 Cl3 3.21147(13) 6_556 ?
K1 Cl3 3.21147(13) . ?
K1 Cl2 3.1876(8) . ?
K1 Cl2 3.2402(8) 1_455 ?
K1 Cl1 3.1633(7) . ?
K1 Cl1 3.2092(7) 3 ?
O1 H1E 0.85(2) 6_556 ?
O1 H1E 0.8500 . ?
O1 H1F 0.8470 . ?
O1 H1F 0.85(2) 6_556 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C1 1.494(2) 5_666 ?
N1 C2 1.493(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.506(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?

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
Cl3 K1 Cl3 164.06(3) 6_556 . ?
Cl3 K1 Cl2 82.375(14) 6_556 1_455 ?
Cl3 K1 Cl2 82.375(14) . 1_455 ?
Cl2 K1 Cl3 97.278(14) . 6_556 ?
Cl2 K1 Cl3 97.278(14) . . ?
Cl2 K1 Cl2 172.87(4) . 1_455 ?
Cl2 K1 Cl1 91.84(2) . 3 ?
Cl1 K1 Cl3 86.886(11) . . ?
Cl1 K1 Cl3 92.992(11) 3 6_556 ?
Cl1 K1 Cl3 92.992(11) 3 . ?
Cl1 K1 Cl3 86.886(11) . 6_556 ?
Cl1 K1 Cl2 89.10(2) . . ?
Cl1 K1 Cl2 95.28(2) 3 1_455 ?
Cl1 K1 Cl2 83.77(2) . 1_455 ?
Cl1 K1 Cl1 179.054(19) . 3 ?
K1 Cl3 K1 165.07(3) 7_576 . ?
K1 Cl2 K1 172.87(4) . 1_655 ?
K1 Cl1 K1 175.55(2) . 3_545 ?
H1E O1 H1E 24.9 . 6_556 ?
H1E O1 H1F 104.8 6_556 6_556 ?
H1E O1 H1F 104.8 . . ?
H1E O1 H1F 100.2 . 6_556 ?
H1F O1 H1E 100.2 . 6_556 ?
H1F O1 H1F 21.1 . 6_556 ?
H1A N1 H1B 108.0 . . ?
C1 N1 H1A 109.3 5_666 . ?
C1 N1 H1B 109.3 5_666 . ?
C2 N1 H1A 109.3 . . ?
C2 N1 H1B 109.3 . . ?
C2 N1 C1 111.43(12) . 5_666 ?
N1 C1 H1C 109.4 5_666 . ?
N1 C1 H1D 109.4 5_666 . ?
N1 C1 C2 111.12(14) 5_666 . ?
H1C C1 H1D 108.0 . . ?
C2 C1 H1C 109.4 . . ?
C2 C1 H1D 109.4 . . ?
N1 C2 C1 111.13(16) . . ?
N1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?

_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 3.257
_oxdiff_exptl_absorpt_empirical_full_min 0.507
