# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_1-203K
_database_code_depnum_ccdc_archive 'CCDC 1564728'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl3 K O12, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Cl3 K N2 O12'
_chemical_formula_weight         439.63

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   9.603(3)
_cell_length_b                   14.769(5)
_cell_length_c                   20.786(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2948.0(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8674
_cell_measurement_theta_min      1.6910
_cell_measurement_theta_max      27.4662

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.981
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_absorpt_coefficient_mu    0.971
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20108
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.959
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3317
_reflns_number_gt                2917
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0533P)²+1.8273P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0055(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3317
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1321
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.20591(8) 0.23002(5) 0.12227(3) 0.0249(2) Uani 1 1 d . . . . .
Cl1 Cl 0.45696(8) 0.20840(5) 0.25448(4) 0.0197(2) Uani 1 1 d . . . . .
Cl2 Cl 0.24057(8) -0.02140(5) 0.13381(4) 0.0217(2) Uani 1 1 d . . . . .
Cl3 Cl 0.44171(8) 0.24144(5) -0.01033(4) 0.0193(2) Uani 1 1 d . . . . .
C1 C 0.6778(4) 0.4077(2) 0.16795(16) 0.0283(8) Uani 1 1 d . . . . .
H1A H 0.6559 0.3514 0.1898 0.034 Uiso 1 1 calc R U . . .
H1B H 0.6195 0.4547 0.1863 0.034 Uiso 1 1 calc R U . . .
C2 C 0.8225(4) 0.5832(2) 0.12046(15) 0.0293(8) Uani 1 1 d . . . . .
H2A H 0.8987 0.6244 0.1115 0.035 Uiso 1 1 calc R U . . .
H2B H 0.7408 0.6195 0.1297 0.035 Uiso 1 1 calc R U . . .
C3 C 0.7944(4) 0.5281(2) 0.06073(15) 0.0257(7) Uani 1 1 d . . . . .
H3A H 0.8659 0.4820 0.0570 0.031 Uiso 1 1 calc R U . . .
H3B H 0.8027 0.5675 0.0236 0.031 Uiso 1 1 calc R U . . .
C4 C 0.8283(3) 0.4309(2) 0.18033(16) 0.0241(7) Uani 1 1 d . . . . .
H4A H 0.8550 0.4065 0.2218 0.029 Uiso 1 1 calc R U . . .
H4B H 0.8853 0.4017 0.1479 0.029 Uiso 1 1 calc R U . . .
C5 C 0.6535(4) 0.4823(3) 0.05845(17) 0.0345(9) Uani 1 1 d . . . . .
H5A H 0.5835 0.5248 0.0733 0.041 Uiso 1 1 calc R U . . .
H5B H 0.6322 0.4674 0.0141 0.041 Uiso 1 1 calc R U . . .
N1 N 0.8584(3) 0.52949(19) 0.17972(14) 0.0293(7) Uani 1 1 d . . . . .
H1C H 0.9491 0.5365 0.1871 0.035 Uiso 1 1 calc R U . . .
H1D H 0.8135 0.5543 0.2127 0.035 Uiso 1 1 calc R U . . .
N2 N 0.6437(3) 0.39795(18) 0.09812(14) 0.0269(6) Uani 1 1 d . . . . .
H2C H 0.5574 0.3765 0.0948 0.032 Uiso 1 1 calc R U . . .
H2D H 0.7007 0.3568 0.0813 0.032 Uiso 1 1 calc R U . . .
O1 O 0.6066(2) 0.20369(17) 0.24741(12) 0.0287(6) Uani 1 1 d . . . . .
O2 O 0.4233(3) 0.23043(17) 0.32017(11) 0.0306(6) Uani 1 1 d . . . . .
O3 O 0.4035(3) 0.27720(17) 0.21189(12) 0.0299(6) Uani 1 1 d . . . . .
O4 O 0.3961(3) 0.12157(17) 0.23797(12) 0.0330(6) Uani 1 1 d . . . . .
O5 O 0.3110(3) 0.04505(18) 0.09511(14) 0.0438(7) Uani 1 1 d . . . . .
O6 O 0.1367(3) 0.02249(19) 0.17294(12) 0.0364(7) Uani 1 1 d . . . . .
O7 O 0.3403(3) -0.06691(19) 0.17425(13) 0.0372(6) Uani 1 1 d . . . . .
O8 O 0.1736(2) -0.08704(16) 0.09227(11) 0.0296(6) Uani 1 1 d . . . . .
O9 O 0.2932(2) 0.23698(18) -0.02099(13) 0.0338(6) Uani 1 1 d . . . . .
O10 O 0.4674(2) 0.23478(16) 0.05788(11) 0.0270(6) Uani 1 1 d . . . . .
O11 O 0.5089(2) 0.16789(15) -0.04386(12) 0.0285(6) Uani 1 1 d . . . . .
O12 O 0.4954(3) 0.32668(15) -0.03323(11) 0.0284(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O3 2.749(3) . ?
K1 O10 2.847(3) . ?
K1 O12 2.866(3) 3_455 ?
K1 O1 2.898(3) 6_556 ?
K1 O11 2.917(3) 3_455 ?
K1 O2 2.966(3) 6_556 ?
K1 O5 2.966(3) . ?
K1 O8 3.004(3) 7_665 ?
K1 O9 3.095(3) . ?
K1 O7 3.219(3) 7_665 ?
K1 O6 3.308(3) . ?
K1 O4 3.418(3) . ?
Cl1 O2 1.440(2) . ?
Cl1 O3 1.442(2) . ?
Cl1 O1 1.446(2) . ?
Cl1 O4 1.450(2) . ?
Cl1 K1 3.5186(13) 6_656 ?
Cl2 O5 1.438(3) . ?
Cl2 O7 1.441(3) . ?
Cl2 O6 1.441(2) . ?
Cl2 O8 1.449(2) . ?
Cl2 K1 3.7148(16) 7_655 ?
Cl3 O12 1.441(2) . ?
Cl3 O10 1.442(2) . ?
Cl3 O11 1.443(2) . ?
Cl3 O9 1.445(2) . ?
Cl3 K1 3.4682(13) 3 ?
C1 N2 1.495(4) . ?
C1 C4 1.507(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.505(4) . ?
C2 C3 1.508(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.513(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.484(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.497(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
O1 K1 2.898(3) 6_656 ?
O2 K1 2.966(3) 6_656 ?
O7 K1 3.219(3) 7_655 ?
O8 K1 3.004(3) 7_655 ?
O11 K1 2.917(3) 3 ?
O12 K1 2.866(3) 3 ?

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
O3 K1 O10 72.75(8) . . ?
O3 K1 O12 177.00(8) . 3_455 ?
O10 K1 O12 109.02(7) . 3_455 ?
O3 K1 O1 68.14(8) . 6_556 ?
O10 K1 O1 137.15(7) . 6_556 ?
O12 K1 O1 109.41(7) 3_455 6_556 ?
O3 K1 O11 134.05(8) . 3_455 ?
O10 K1 O11 107.26(7) . 3_455 ?
O12 K1 O11 48.14(6) 3_455 3_455 ?
O1 K1 O11 112.23(7) 6_556 3_455 ?
O3 K1 O2 110.96(8) . 6_556 ?
O10 K1 O2 175.47(7) . 6_556 ?
O12 K1 O2 67.40(7) 3_455 6_556 ?
O1 K1 O2 47.32(7) 6_556 6_556 ?
O11 K1 O2 68.34(7) 3_455 6_556 ?
O3 K1 O5 97.33(8) . . ?
O10 K1 O5 68.48(7) . . ?
O12 K1 O5 81.25(8) 3_455 . ?
O1 K1 O5 99.57(8) 6_556 . ?
O11 K1 O5 126.18(8) 3_455 . ?
O2 K1 O5 112.95(7) 6_556 . ?
O3 K1 O8 69.33(7) . 7_665 ?
O10 K1 O8 62.65(7) . 7_665 ?
O12 K1 O8 113.60(7) 3_455 7_665 ?
O1 K1 O8 116.19(7) 6_556 7_665 ?
O11 K1 O8 70.66(7) 3_455 7_665 ?
O2 K1 O8 115.73(7) 6_556 7_665 ?
O5 K1 O8 131.12(7) . 7_665 ?
O3 K1 O9 117.18(7) . . ?
O10 K1 O9 46.21(6) . . ?
O12 K1 O9 65.12(7) 3_455 . ?
O1 K1 O9 173.13(7) 6_556 . ?
O11 K1 O9 67.72(7) 3_455 . ?
O2 K1 O9 129.47(7) 6_556 . ?
O5 K1 O9 75.84(7) . . ?
O8 K1 O9 70.50(7) 7_665 . ?
O3 K1 O7 68.37(7) . 7_665 ?
O10 K1 O7 104.86(7) . 7_665 ?
O12 K1 O7 113.07(7) 3_455 7_665 ?
O1 K1 O7 76.46(7) 6_556 7_665 ?
O11 K1 O7 67.45(7) 3_455 7_665 ?
O2 K1 O7 74.73(7) 6_556 7_665 ?
O5 K1 O7 165.67(8) . 7_665 ?
O8 K1 O7 44.34(6) 7_665 7_665 ?
O9 K1 O7 109.23(7) . 7_665 ?
O3 K1 O6 99.08(7) . . ?
O10 K1 O6 110.48(7) . . ?
O12 K1 O6 78.06(7) 3_455 . ?
O1 K1 O6 60.79(7) 6_556 . ?
O11 K1 O6 121.77(7) 3_455 . ?
O2 K1 O6 71.92(7) 6_556 . ?
O5 K1 O6 43.60(7) . . ?
O8 K1 O6 167.57(7) 7_665 . ?
O9 K1 O6 113.04(7) . . ?
O7 K1 O6 136.78(7) 7_665 . ?
O3 K1 O4 43.38(7) . . ?
O10 K1 O4 82.59(7) . . ?
O12 K1 O4 133.97(7) 3_455 . ?
O1 K1 O4 57.00(7) 6_556 . ?
O11 K1 O4 169.06(7) 3_455 . ?
O2 K1 O4 101.89(7) 6_556 . ?
O5 K1 O4 61.36(7) . . ?
O8 K1 O4 111.20(7) 7_665 . ?
O9 K1 O4 123.21(7) . . ?
O7 K1 O4 105.91(7) 7_665 . ?
O6 K1 O4 56.59(6) . . ?
O2 Cl1 O3 110.06(15) . . ?
O2 Cl1 O1 109.27(15) . . ?
O3 Cl1 O1 108.98(15) . . ?
O2 Cl1 O4 109.49(15) . . ?
O3 Cl1 O4 109.53(15) . . ?
O1 Cl1 O4 109.49(15) . . ?
O2 Cl1 K1 56.06(11) . 6_656 ?
O3 Cl1 K1 128.67(11) . 6_656 ?
O1 Cl1 K1 53.36(10) . 6_656 ?
O4 Cl1 K1 121.75(11) . 6_656 ?
O5 Cl2 O7 109.41(17) . . ?
O5 Cl2 O6 109.52(17) . . ?
O7 Cl2 O6 109.91(17) . . ?
O5 Cl2 O8 109.39(16) . . ?
O7 Cl2 O8 109.30(16) . . ?
O6 Cl2 O8 109.28(15) . . ?
O5 Cl2 K1 124.99(12) . 7_655 ?
O7 Cl2 K1 58.98(11) . 7_655 ?
O6 Cl2 K1 125.22(12) . 7_655 ?
O8 Cl2 K1 50.32(10) . 7_655 ?
O12 Cl3 O10 108.85(15) . . ?
O12 Cl3 O11 109.74(15) . . ?
O10 Cl3 O11 110.29(15) . . ?
O12 Cl3 O9 110.02(15) . . ?
O10 Cl3 O9 108.46(15) . . ?
O11 Cl3 O9 109.46(15) . . ?
O12 Cl3 K1 53.88(10) . 3 ?
O10 Cl3 K1 122.85(10) . 3 ?
O11 Cl3 K1 55.96(10) . 3 ?
O9 Cl3 K1 128.66(12) . 3 ?
N2 C1 C4 113.5(3) . . ?
N2 C1 H1A 108.9 . . ?
C4 C1 H1A 108.9 . . ?
N2 C1 H1B 108.9 . . ?
C4 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C3 115.5(3) . . ?
N1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
N1 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 C5 115.3(3) . . ?
C2 C3 H3A 108.5 . . ?
C5 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
C5 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
N1 C4 C1 114.1(3) . . ?
N1 C4 H4A 108.7 . . ?
C1 C4 H4A 108.7 . . ?
N1 C4 H4B 108.7 . . ?
C1 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
N2 C5 C3 114.3(3) . . ?
N2 C5 H5A 108.7 . . ?
C3 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C3 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C4 N1 C2 118.6(3) . . ?
C4 N1 H1C 107.7 . . ?
C2 N1 H1C 107.7 . . ?
C4 N1 H1D 107.7 . . ?
C2 N1 H1D 107.7 . . ?
H1C N1 H1D 107.1 . . ?
C1 N2 C5 116.1(3) . . ?
C1 N2 H2C 108.3 . . ?
C5 N2 H2C 108.3 . . ?
C1 N2 H2D 108.3 . . ?
C5 N2 H2D 108.3 . . ?
H2C N2 H2D 107.4 . . ?
Cl1 O1 K1 103.03(12) . 6_656 ?
Cl1 O2 K1 100.18(13) . 6_656 ?
Cl1 O3 K1 118.89(14) . . ?
Cl1 O4 K1 88.13(12) . . ?
Cl2 O5 K1 111.24(15) . . ?
Cl2 O6 K1 95.62(13) . . ?
Cl2 O7 K1 98.47(13) . 7_655 ?
Cl2 O8 K1 107.90(13) . 7_655 ?
Cl3 O9 K1 96.96(13) . . ?
Cl3 O10 K1 108.22(12) . . ?
Cl3 O11 K1 99.84(12) . 3 ?
Cl3 O12 K1 102.15(12) . 3 ?

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
N1 C2 C3 C5 76.6(4) . . . . ?
N2 C1 C4 N1 87.7(4) . . . . ?
C2 C3 C5 N2 -78.2(4) . . . . ?
C1 C4 N1 C2 -57.1(4) . . . . ?
C3 C2 N1 C4 -15.6(5) . . . . ?
C4 C1 N2 C5 -66.3(4) . . . . ?
C3 C5 N2 C1 56.6(4) . . . . ?
O2 Cl1 O1 K1 4.30(16) . . . 6_656 ?
O3 Cl1 O1 K1 124.59(13) . . . 6_656 ?
O4 Cl1 O1 K1 -115.62(14) . . . 6_656 ?
O3 Cl1 O2 K1 -123.79(13) . . . 6_656 ?
O1 Cl1 O2 K1 -4.16(16) . . . 6_656 ?
O4 Cl1 O2 K1 115.76(13) . . . 6_656 ?
O2 Cl1 O3 K1 -117.46(16) . . . . ?
O1 Cl1 O3 K1 122.74(15) . . . . ?
O4 Cl1 O3 K1 2.97(19) . . . . ?
K1 Cl1 O3 K1 -179.48(5) 6_656 . . . ?
O2 Cl1 O4 K1 118.68(13) . . . . ?
O3 Cl1 O4 K1 -2.09(14) . . . . ?
O1 Cl1 O4 K1 -121.54(12) . . . . ?
K1 Cl1 O4 K1 -179.84(5) 6_656 . . . ?
O7 Cl2 O5 K1 -118.86(16) . . . . ?
O6 Cl2 O5 K1 1.68(19) . . . . ?
O8 Cl2 O5 K1 121.43(14) . . . . ?
K1 Cl2 O5 K1 176.00(4) 7_655 . . . ?
O5 Cl2 O6 K1 -1.41(16) . . . . ?
O7 Cl2 O6 K1 118.82(14) . . . . ?
O8 Cl2 O6 K1 -121.23(13) . . . . ?
K1 Cl2 O6 K1 -175.71(4) 7_655 . . . ?
O5 Cl2 O7 K1 -119.84(14) . . . 7_655 ?
O6 Cl2 O7 K1 119.86(14) . . . 7_655 ?
O8 Cl2 O7 K1 -0.07(15) . . . 7_655 ?
O5 Cl2 O8 K1 119.85(15) . . . 7_655 ?
O7 Cl2 O8 K1 0.08(17) . . . 7_655 ?
O6 Cl2 O8 K1 -120.24(14) . . . 7_655 ?
O12 Cl3 O9 K1 -115.55(12) . . . . ?
O10 Cl3 O9 K1 3.41(15) . . . . ?
O11 Cl3 O9 K1 123.79(12) . . . . ?
K1 Cl3 O9 K1 -174.75(4) 3 . . . ?
O12 Cl3 O10 K1 115.82(13) . . . . ?
O11 Cl3 O10 K1 -123.73(13) . . . . ?
O9 Cl3 O10 K1 -3.87(17) . . . . ?
K1 Cl3 O10 K1 174.42(3) 3 . . . ?
O12 Cl3 O11 K1 3.29(16) . . . 3 ?
O10 Cl3 O11 K1 -116.62(13) . . . 3 ?
O9 Cl3 O11 K1 124.12(13) . . . 3 ?
O10 Cl3 O12 K1 117.42(13) . . . 3 ?
O11 Cl3 O12 K1 -3.37(16) . . . 3 ?
O9 Cl3 O12 K1 -123.86(13) . . . 3 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1A O1 0.97 2.53 3.504(4) 178.2 .
C2 H2A O10 0.97 2.36 3.282(4) 159.5 7_765
C2 H2B O2 0.97 2.50 3.439(5) 162.7 4_655
C3 H3A O11 0.97 2.62 3.570(4) 166.6 3
C4 H4A O3 0.97 2.40 3.271(4) 149.1 6_656
C5 H5A O12 0.97 2.46 3.206(4) 133.0 5_665
C5 H5B O12 0.97 2.65 3.350(4) 129.6 .
N1 H1C O4 0.89 2.22 2.979(4) 143.6 7_765
N1 H1C O7 0.89 2.55 3.227(4) 133.5 7_765
N1 H1D O1 0.89 2.44 2.952(4) 116.6 7_765
N1 H1D O4 0.89 2.47 3.279(4) 151.8 4_655
N1 H1D O6 0.89 2.47 3.065(4) 124.7 4_655
N2 H2C O8 0.89 2.28 3.058(4) 145.3 7_665
N2 H2C O10 0.89 2.39 3.061(4) 132.3 .
N2 H2D O9 0.89 2.07 2.933(4) 163.8 3

_refine_diff_density_max         0.746
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_1-378K
_database_code_depnum_ccdc_archive 'CCDC 1564731'
_audit_update_record             
;
2017-10-31 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl3 K O12, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Cl3 K N2 O12'
_chemical_formula_weight         439.63

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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'

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

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

_cell_length_a                   10.739(11)
_cell_length_b                   9.967(11)
_cell_length_c                   14.350(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1536(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4434
_cell_measurement_theta_min      2.3683
_cell_measurement_theta_max      27.3968

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_absorpt_coefficient_mu    0.932
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6072
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10597
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.788
_diffrn_reflns_theta_max         27.374
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measured_fraction_theta_full 0.888
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_Laue_measured_fraction_full 0.888
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_point_group_measured_fraction_full 0.888
_reflns_number_total             1556
_reflns_number_gt                1459
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1404P)²+3.9824P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1556
_refine_ls_number_parameters     143
_refine_ls_number_restraints     185
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.1210
_refine_ls_wR_factor_ref         0.3286
_refine_ls_wR_factor_gt          0.3235
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_restrained_S_all      1.259
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.24705(19) 0.2146(2) 0.7500 0.0552(8) Uani 1 2 d S TU P . .
Cl1 Cl 0.5114(3) 0.4538(3) 0.7500 0.0752(10) Uani 1 2 d S TU P . .
Cl2 Cl 0.2468(2) 0.2500 1.0000 0.0733(10) Uani 1 2 d S TU P . .
Cl3 Cl -0.0180(3) 0.4490(2) 0.7500 0.0619(8) Uani 1 2 d S TU P . .
C1 C 0.895(2) 0.223(3) -0.016(2) 0.114(5) Uani 0.5 1 d D U P . .
H1A H 0.9046 0.1572 0.0326 0.137 Uiso 0.5 1 d R U P . .
H1B H 0.9756 0.2343 -0.0440 0.137 Uiso 0.5 1 d R U P . .
C2 C 0.661(3) 0.177(3) -0.072(2) 0.122(5) Uani 0.5 1 d D U P . .
H2A H 0.6340 0.2069 -0.1320 0.146 Uiso 0.5 1 d R U P . .
H2B H 0.6334 0.0859 -0.0653 0.146 Uiso 0.5 1 d R U P . .
C3 C 0.6011(15) 0.2500 0.0000 0.125(4) Uani 1 2 d DS TU P . .
H3A H 0.5825 0.1898 0.0503 0.150 Uiso 0.5 1 d R U P . .
H3B H 0.5227 0.2723 -0.0282 0.150 Uiso 0.5 1 d R U P . .
C4 C 0.865(2) 0.331(2) 0.029(2) 0.110(5) Uani 0.5 1 d D U P . .
H4A H 0.8529 0.3975 -0.0184 0.133 Uiso 0.5 1 d R U P . .
H4B H 0.9353 0.3589 0.0659 0.133 Uiso 0.5 1 d R U P . .
C5 C 0.646(2) 0.365(2) 0.0239(19) 0.118(5) Uani 0.5 1 d D U P . .
H5A H 0.5865 0.3644 0.0738 0.141 Uiso 0.5 1 d R U P . .
H5B H 0.6200 0.4526 -0.0008 0.141 Uiso 0.5 1 d R U P . .
N1 N 0.817(2) 0.156(2) -0.0774(16) 0.123(5) Uani 0.5 1 d D U P . .
H1C H 0.8382 0.0689 -0.0815 0.148 Uiso 0.5 1 d R U P . .
H1D H 0.8395 0.1940 -0.1319 0.148 Uiso 0.5 1 d R U P . .
N2 N 0.7424(16) 0.334(3) 0.0936(16) 0.107(4) Uani 0.5 1 d D U P . .
H2C H 0.7439 0.4039 0.1336 0.129 Uiso 0.5 1 d R U P . .
H2D H 0.7402 0.2577 0.1267 0.129 Uiso 0.5 1 d R U P . .
O1 O 0.5008(11) 0.5953(8) 0.7500 0.114(3) Uani 1 2 d S TU P . .
O2 O 0.6397(10) 0.4221(13) 0.7500 0.127(4) Uani 1 2 d S TU P . .
O3 O 0.4528(7) 0.3978(8) 0.8289(6) 0.115(2) Uani 1 1 d . U . . .
O4 O 0.3243(6) 0.1589(7) 0.9485(4) 0.0902(19) Uani 1 1 d . U . . .
O5 O 0.1705(6) 0.3211(8) 0.9345(4) 0.103(2) Uani 1 1 d . U . . .
O6 O 0.1149(8) 0.4782(8) 0.7500 0.075(2) Uani 1 2 d S TU P . .
O7 O -0.0337(9) 0.3084(8) 0.7500 0.093(2) Uani 1 2 d S TU P . .
O8 O -0.0749(6) 0.5083(6) 0.8309(4) 0.0872(19) 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
K1 O1 2.957(11) 7_655 ?
K1 O5 2.968(7) . ?
K1 O5 2.969(7) 6_557 ?
K1 O6 2.986(9) . ?
K1 O8 2.999(7) 4_546 ?
K1 O8 2.999(7) 7 ?
K1 O4 3.018(7) . ?
K1 O4 3.018(7) 6_557 ?
K1 O3 3.082(8) . ?
K1 O3 3.082(8) 6_557 ?
K1 O7 3.156(10) . ?
K1 O2 3.159(13) 7_655 ?
Cl1 O3 1.410(7) . ?
Cl1 O3 1.410(7) 6_557 ?
Cl1 O2 1.414(11) . ?
Cl1 O1 1.414(8) . ?
Cl1 K1 3.672(4) 7_665 ?
Cl2 O5 1.433(6) 3_557 ?
Cl2 O5 1.433(6) . ?
Cl2 O4 1.437(6) . ?
Cl2 O4 1.437(6) 3_557 ?
Cl2 K1 3.605(4) 3_557 ?
Cl3 O7 1.411(8) . ?
Cl3 O8 1.439(6) . ?
Cl3 O8 1.439(6) 6_557 ?
Cl3 O6 1.456(9) . ?
Cl3 K1 3.614(4) 7_565 ?
C1 C4 0.65(3) 3 ?
C1 C1 0.70(4) 3 ?
C1 C4 1.293(19) . ?
C1 N1 1.39(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9599 . ?
C2 C5 0.82(4) 3 ?
C2 N2 0.93(3) 3 ?
C2 C3 1.42(3) . ?
C2 N1 1.69(3) . ?
C2 H2A 0.9599 . ?
C2 H2B 0.9600 . ?
C3 C5 1.293(19) . ?
C3 C5 1.293(19) 3 ?
C3 C2 1.42(3) 3 ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C4 C1 0.65(3) 3 ?
C4 N1 0.87(3) 3 ?
C4 N2 1.61(3) . ?
C4 C4 1.82(4) 3 ?
C4 H4A 0.9600 . ?
C4 H4B 0.9601 . ?
C5 C2 0.82(4) 3 ?
C5 N2 1.47(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9800 . ?
N1 N2 0.84(2) 3 ?
N1 C4 0.87(3) 3 ?
N1 H1C 0.9000 . ?
N1 H1D 0.9001 . ?
N2 N1 0.84(2) 3 ?
N2 C2 0.93(3) 3 ?
N2 H2C 0.8999 . ?
N2 H2D 0.9000 . ?
O1 K1 2.957(11) 7_665 ?
O2 K1 3.159(13) 7_665 ?
O8 K1 2.999(7) 7_565 ?

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
O1 K1 O5 113.41(14) 7_655 . ?
O1 K1 O5 113.41(14) 7_655 6_557 ?
O5 K1 O5 126.2(3) . 6_557 ?
O1 K1 O6 142.1(3) 7_655 . ?
O5 K1 O6 63.51(14) . . ?
O5 K1 O6 63.51(14) 6_557 . ?
O1 K1 O8 106.8(2) 7_655 4_546 ?
O5 K1 O8 114.8(2) . 4_546 ?
O5 K1 O8 74.3(2) 6_557 4_546 ?
O6 K1 O8 108.1(2) . 4_546 ?
O1 K1 O8 106.8(2) 7_655 7 ?
O5 K1 O8 74.3(2) . 7 ?
O5 K1 O8 114.8(2) 6_557 7 ?
O6 K1 O8 108.1(2) . 7 ?
O8 K1 O8 45.5(2) 4_546 7 ?
O1 K1 O4 71.00(13) 7_655 . ?
O5 K1 O4 45.57(19) . . ?
O5 K1 O4 169.6(2) 6_557 . ?
O6 K1 O4 107.00(14) . . ?
O8 K1 O4 114.12(18) 4_546 . ?
O8 K1 O4 71.22(18) 7 . ?
O1 K1 O4 71.00(13) 7_655 6_557 ?
O5 K1 O4 169.6(2) . 6_557 ?
O5 K1 O4 45.57(19) 6_557 6_557 ?
O6 K1 O4 107.00(14) . 6_557 ?
O8 K1 O4 71.22(18) 4_546 6_557 ?
O8 K1 O4 114.12(18) 7 6_557 ?
O4 K1 O4 141.4(3) . 6_557 ?
O1 K1 O3 65.3(2) 7_655 . ?
O5 K1 O3 70.1(2) . . ?
O5 K1 O3 108.3(2) 6_557 . ?
O6 K1 O3 79.6(2) . . ?
O8 K1 O3 172.1(2) 4_546 . ?
O8 K1 O3 134.9(2) 7 . ?
O4 K1 O3 64.24(19) . . ?
O4 K1 O3 105.0(2) 6_557 . ?
O1 K1 O3 65.3(2) 7_655 6_557 ?
O5 K1 O3 108.3(2) . 6_557 ?
O5 K1 O3 70.1(2) 6_557 6_557 ?
O6 K1 O3 79.6(2) . 6_557 ?
O8 K1 O3 134.9(2) 4_546 6_557 ?
O8 K1 O3 172.1(2) 7 6_557 ?
O4 K1 O3 105.0(2) . 6_557 ?
O4 K1 O3 64.24(19) 6_557 6_557 ?
O3 K1 O3 43.1(3) . 6_557 ?
O1 K1 O7 173.5(2) 7_655 . ?
O5 K1 O7 68.26(14) . . ?
O5 K1 O7 68.26(14) 6_557 . ?
O6 K1 O7 44.4(2) . . ?
O8 K1 O7 67.3(2) 4_546 . ?
O8 K1 O7 67.3(2) 7 . ?
O4 K1 O7 108.48(13) . . ?
O4 K1 O7 108.48(13) 6_557 . ?
O3 K1 O7 120.6(2) . . ?
O3 K1 O7 120.6(2) 6_557 . ?
O1 K1 O2 43.6(3) 7_655 7_655 ?
O5 K1 O2 115.88(15) . 7_655 ?
O5 K1 O2 115.88(15) 6_557 7_655 ?
O6 K1 O2 174.3(3) . 7_655 ?
O8 K1 O2 66.7(2) 4_546 7_655 ?
O8 K1 O2 66.7(2) 7 7_655 ?
O4 K1 O2 74.01(14) . 7_655 ?
O4 K1 O2 74.01(14) 6_557 7_655 ?
O3 K1 O2 105.7(2) . 7_655 ?
O3 K1 O2 105.7(2) 6_557 7_655 ?
O7 K1 O2 129.9(3) . 7_655 ?
O3 Cl1 O3 106.7(7) . 6_557 ?
O3 Cl1 O2 110.3(5) . . ?
O3 Cl1 O2 110.3(5) 6_557 . ?
O3 Cl1 O1 111.0(4) . . ?
O3 Cl1 O1 111.0(4) 6_557 . ?
O2 Cl1 O1 107.5(7) . . ?
O3 Cl1 K1 126.6(3) . 7_665 ?
O3 Cl1 K1 126.6(3) 6_557 7_665 ?
O2 Cl1 K1 58.0(5) . 7_665 ?
O1 Cl1 K1 49.5(5) . 7_665 ?
O5 Cl2 O5 110.4(6) 3_557 . ?
O5 Cl2 O4 110.9(4) 3_557 . ?
O5 Cl2 O4 107.8(4) . . ?
O5 Cl2 O4 107.8(4) 3_557 3_557 ?
O5 Cl2 O4 110.9(4) . 3_557 ?
O4 Cl2 O4 109.2(6) . 3_557 ?
O5 Cl2 K1 52.9(3) 3_557 3_557 ?
O5 Cl2 K1 127.2(3) . 3_557 ?
O4 Cl2 K1 125.0(3) . 3_557 ?
O4 Cl2 K1 54.9(2) 3_557 3_557 ?
O7 Cl3 O8 110.9(4) . . ?
O7 Cl3 O8 110.9(4) . 6_557 ?
O8 Cl3 O8 107.6(5) . 6_557 ?
O7 Cl3 O6 108.4(5) . . ?
O8 Cl3 O6 109.5(4) . . ?
O8 Cl3 O6 109.5(4) 6_557 . ?
O7 Cl3 K1 130.2(4) . 7_565 ?
O8 Cl3 K1 53.8(3) . 7_565 ?
O8 Cl3 K1 53.8(3) 6_557 7_565 ?
O6 Cl3 K1 121.4(4) . 7_565 ?
C4 C1 C1 145(6) 3 3 ?
C4 C1 C4 135(6) 3 . ?
C1 C1 C4 17(3) 3 . ?
C4 C1 N1 29(4) 3 . ?
C1 C1 N1 141(2) 3 . ?
C4 C1 N1 125(3) . . ?
C4 C1 H1A 72.6 3 . ?
C1 C1 H1A 93.3 3 . ?
C4 C1 H1A 103.6 . . ?
N1 C1 H1A 101.3 . . ?
C4 C1 H1B 114.4 3 . ?
C1 C1 H1B 100.5 3 . ?
C4 C1 H1B 109.6 . . ?
N1 C1 H1B 109.2 . . ?
H1A C1 H1B 106.8 . . ?
C5 C2 N2 114(5) 3 3 ?
C5 C2 C3 64(2) 3 . ?
N2 C2 C3 137(3) 3 . ?
C5 C2 N1 100(3) 3 . ?
N2 C2 N1 17(2) 3 . ?
C3 C2 N1 123.3(19) . . ?
C5 C2 H2A 148.4 3 . ?
N2 C2 H2A 91.2 3 . ?
C3 C2 H2A 110.8 . . ?
N1 C2 H2A 107.3 . . ?
C5 C2 H2B 51.2 3 . ?
N2 C2 H2B 102.1 3 . ?
C3 C2 H2B 105.8 . . ?
N1 C2 H2B 101.4 . . ?
H2A C2 H2B 106.7 . . ?
C5 C3 C5 136(3) . 3 ?
C5 C3 C2 118.6(18) . . ?
C5 C3 C2 34.9(17) 3 . ?
C5 C3 C2 34.9(17) . 3 ?
C5 C3 C2 118.6(18) 3 3 ?
C2 C3 C2 126(2) . 3 ?
C5 C3 H3A 115.7 . . ?
C5 C3 H3A 73.8 3 . ?
C2 C3 H3A 108.7 . . ?
C2 C3 H3A 82.5 3 . ?
C5 C3 H3B 103.5 . . ?
C5 C3 H3B 114.9 3 . ?
C2 C3 H3B 102.2 . . ?
C2 C3 H3B 126.0 3 . ?
H3A C3 H3B 106.3 . . ?
C5 C3 H5A 37.8 . . ?
C5 C3 H5A 149.9 3 . ?
C2 C3 H5A 155.8 . . ?
C2 C3 H5A 34.8 3 . ?
H3A C3 H5A 85.7 . . ?
H3B C3 H5A 91.7 . . ?
C1 C4 N1 130(7) 3 3 ?
C1 C4 C1 18(3) 3 . ?
N1 C4 C1 132(3) 3 . ?
C1 C4 N2 126(5) 3 . ?
N1 C4 N2 20(2) 3 . ?
C1 C4 N2 120(2) . . ?
C1 C4 C4 30(4) 3 3 ?
N1 C4 C4 120(3) 3 3 ?
C1 C4 C4 14.8(18) . 3 ?
N2 C4 C4 106.4(17) . 3 ?
C1 C4 H4A 115.4 3 . ?
N1 C4 H4A 112.3 3 . ?
C1 C4 H4A 104.9 . . ?
N2 C4 H4A 106.2 . . ?
C4 C4 H4A 106.7 3 . ?
C1 C4 H4B 91.0 3 . ?
N1 C4 H4B 89.0 3 . ?
C1 C4 H4B 108.8 . . ?
N2 C4 H4B 108.5 . . ?
C4 C4 H4B 120.7 3 . ?
H4A C4 H4B 107.4 . . ?
C2 C5 C3 81(3) 3 . ?
C2 C5 N2 35(2) 3 . ?
C3 C5 N2 105(2) . . ?
C2 C5 H5A 60.3 3 . ?
C3 C5 H5A 86.6 . . ?
N2 C5 H5A 87.7 . . ?
C2 C5 H5B 144.4 3 . ?
C3 C5 H5B 125.9 . . ?
N2 C5 H5B 129.2 . . ?
H5A C5 H5B 95.0 . . ?
N2 N1 C4 140(4) 3 3 ?
N2 N1 C1 134(3) 3 . ?
C4 N1 C1 21(3) 3 . ?
N2 N1 C2 19(2) 3 . ?
C4 N1 C2 122(3) 3 . ?
C1 N1 C2 120.6(17) . . ?
N2 N1 H1C 109.2 3 . ?
C4 N1 H1C 92.7 3 . ?
C1 N1 H1C 110.8 . . ?
C2 N1 H1C 111.7 . . ?
N2 N1 H1D 88.1 3 . ?
C4 N1 H1D 118.0 3 . ?
C1 N1 H1D 101.1 . . ?
C2 N1 H1D 104.7 . . ?
H1C N1 H1D 106.3 . . ?
N1 N2 C2 144(4) 3 3 ?
N1 N2 C5 117(3) 3 . ?
C2 N2 C5 31(3) 3 . ?
N1 N2 C4 20(2) 3 . ?
C2 N2 C4 125(3) 3 . ?
C5 N2 C4 101(2) . . ?
N1 N2 H2C 94.2 3 . ?
C2 N2 H2C 108.9 3 . ?
C5 N2 H2C 106.5 . . ?
C4 N2 H2C 111.6 . . ?
N1 N2 H2D 105.5 3 . ?
C2 N2 H2D 92.8 3 . ?
C5 N2 H2D 121.1 . . ?
C4 N2 H2D 107.9 . . ?
H2C N2 H2D 108.5 . . ?
Cl1 O1 K1 109.1(6) . 7_665 ?
Cl1 O2 K1 99.7(6) . 7_665 ?
Cl1 O3 K1 105.1(4) . . ?
Cl2 O4 K1 102.1(3) . . ?
Cl2 O5 K1 104.5(4) . . ?
Cl3 O6 K1 106.9(4) . . ?
Cl3 O7 K1 100.4(5) . . ?
Cl3 O8 K1 103.4(3) . 7_565 ?

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
C5 C2 C3 C5 131(3) 3 . . . ?
N2 C2 C3 C5 33(6) 3 . . . ?
N1 C2 C3 C5 46(3) . . . . ?
N2 C2 C3 C5 -98(6) 3 . . 3 ?
N1 C2 C3 C5 -85(3) . . . 3 ?
C5 C2 C3 C2 90(3) 3 . . 3 ?
N2 C2 C3 C2 -8(5) 3 . . 3 ?
N1 C2 C3 C2 5.0(16) . . . 3 ?
C4 C1 C4 C1 133(22) 3 . . 3 ?
N1 C1 C4 C1 168(17) . . . 3 ?
C4 C1 C4 N1 40(8) 3 . . 3 ?
C1 C1 C4 N1 -93(16) 3 . . 3 ?
N1 C1 C4 N1 75(6) . . . 3 ?
C4 C1 C4 N2 20(7) 3 . . . ?
C1 C1 C4 N2 -113(15) 3 . . . ?
N1 C1 C4 N2 55(4) . . . . ?
C1 C1 C4 C4 -133(22) 3 . . 3 ?
N1 C1 C4 C4 35(6) . . . 3 ?
C5 C3 C5 C2 -74(3) 3 . . 3 ?
C2 C3 C5 C2 -112(4) . . . 3 ?
C5 C3 C5 N2 -47.4(13) 3 . . . ?
C2 C3 C5 N2 -86(2) . . . . ?
C2 C3 C5 N2 26(2) 3 . . . ?
C4 C1 N1 N2 117(9) 3 . . 3 ?
C1 C1 N1 N2 0(13) 3 . . 3 ?
C4 C1 N1 N2 -5(6) . . . 3 ?
C1 C1 N1 C4 -117(14) 3 . . 3 ?
C4 C1 N1 C4 -122(9) . . . 3 ?
C4 C1 N1 C2 100(8) 3 . . . ?
C1 C1 N1 C2 -16(12) 3 . . . ?
C4 C1 N1 C2 -22(4) . . . . ?
C5 C2 N1 N2 146(10) 3 . . 3 ?
C3 C2 N1 N2 -148(9) . . . 3 ?
C5 C2 N1 C4 -48(4) 3 . . 3 ?
N2 C2 N1 C4 166(10) 3 . . 3 ?
C3 C2 N1 C4 18(5) . . . 3 ?
C5 C2 N1 C1 -72(4) 3 . . . ?
N2 C2 N1 C1 141(9) 3 . . . ?
C3 C2 N1 C1 -7(4) . . . . ?
C2 C5 N2 N1 157(6) 3 . . 3 ?
C3 C5 N2 N1 108(3) . . . 3 ?
C3 C5 N2 C2 -49(4) . . . 3 ?
C2 C5 N2 C4 144(5) 3 . . . ?
C3 C5 N2 C4 95(2) . . . . ?
C1 C4 N2 N1 109(11) 3 . . 3 ?
C1 C4 N2 N1 130(8) . . . 3 ?
C4 C4 N2 N1 135(8) 3 . . 3 ?
C1 C4 N2 C2 -84(8) 3 . . 3 ?
N1 C4 N2 C2 167(10) 3 . . 3 ?
C1 C4 N2 C2 -63(5) . . . 3 ?
C4 C4 N2 C2 -58(5) 3 . . 3 ?
C1 C4 N2 C5 -105(6) 3 . . . ?
N1 C4 N2 C5 146(8) 3 . . . ?
C1 C4 N2 C5 -84(3) . . . . ?
C4 C4 N2 C5 -79(3) 3 . . . ?
O3 Cl1 O1 K1 120.7(4) . . . 7_665 ?
O3 Cl1 O1 K1 -120.7(4) 6_557 . . 7_665 ?
O2 Cl1 O1 K1 0.0 . . . 7_665 ?
O3 Cl1 O2 K1 -121.2(4) . . . 7_665 ?
O3 Cl1 O2 K1 121.2(4) 6_557 . . 7_665 ?
O1 Cl1 O2 K1 0.0 . . . 7_665 ?
O3 Cl1 O3 K1 -2.0(7) 6_557 . . . ?
O2 Cl1 O3 K1 -121.7(5) . . . . ?
O1 Cl1 O3 K1 119.2(5) . . . . ?
K1 Cl1 O3 K1 173.73(15) 7_665 . . . ?
O5 Cl2 O4 K1 121.5(3) 3_557 . . . ?
O5 Cl2 O4 K1 0.6(4) . . . . ?
O4 Cl2 O4 K1 -119.9(3) 3_557 . . . ?
K1 Cl2 O4 K1 -179.91(9) 3_557 . . . ?
O5 Cl2 O5 K1 -121.9(4) 3_557 . . . ?
O4 Cl2 O5 K1 -0.7(4) . . . . ?
O4 Cl2 O5 K1 118.8(4) 3_557 . . . ?
K1 Cl2 O5 K1 179.91(9) 3_557 . . . ?
O7 Cl3 O6 K1 0.0 . . . . ?
O8 Cl3 O6 K1 121.1(3) . . . . ?
O8 Cl3 O6 K1 -121.1(3) 6_557 . . . ?
K1 Cl3 O6 K1 180.0 7_565 . . . ?
O8 Cl3 O7 K1 -120.3(3) . . . . ?
O8 Cl3 O7 K1 120.3(3) 6_557 . . . ?
O6 Cl3 O7 K1 0.0 . . . . ?
K1 Cl3 O7 K1 180.0 7_565 . . . ?
O7 Cl3 O8 K1 -125.2(4) . . . 7_565 ?
O8 Cl3 O8 K1 -3.8(6) 6_557 . . 7_565 ?
O6 Cl3 O8 K1 115.2(4) . . . 7_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1A O8 0.96 2.57 3.53(4) 176.5 3_656
C1 H1B O5 0.96 2.29 3.19(2) 157.6 1_654
C1 H1B O5 0.96 2.67 3.21(2) 115.6 3_656
C2 H2A O1 0.96 2.49 3.20(3) 130.5 7_654
C2 H2B O3 0.96 2.58 3.36(3) 137.8 7_654
C3 H3A O3 0.96 2.39 3.277(11) 153.6 3_556
C3 H3B O3 0.96 2.52 3.277(11) 136.1 1_554
C3 H3B O4 0.96 2.44 3.195(16) 135.8 1_554
C3 H3B O4 0.96 2.51 3.195(16) 127.9 3_556
C4 H4A O8 0.96 2.55 3.41(3) 149.2 1_654
C4 H4B O8 0.96 2.49 3.42(3) 162.5 5_666
C5 H5A O1 0.96 2.73 3.63(3) 156.8 5_666
C5 H5B O4 0.98 2.26 3.14(3) 148.0 7_664
N1 H1C O5 0.90 2.48 3.35(3) 161.0 7_654
N1 H1C O6 0.90 2.63 3.13(2) 116.2 7_654
N1 H1D O7 0.90 2.46 3.32(3) 160.3 1_654
N2 H2C O6 0.90 2.54 3.30(2) 141.7 5_666

_refine_diff_density_max         0.627
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.104

####################################################################### 
# 
# 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_1-293K
_database_code_depnum_ccdc_archive 'CCDC 1564729'
_audit_update_record             
;
2017-07-26 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl3 K O12, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Cl3 K N2 O12'
_chemical_formula_weight         439.63

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   9.640(4)
_cell_length_b                   14.793(7)
_cell_length_c                   20.947(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2987(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8184
_cell_measurement_theta_min      1.9445
_cell_measurement_theta_max      27.7672

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_absorpt_coefficient_mu    0.959
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7060
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20406
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.944
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             3317
_reflns_number_gt                2894
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0683P)²+2.3309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0071(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3317
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1618
_refine_ls_wR_factor_gt          0.1483
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.20821(9) 0.23110(6) 0.12269(4) 0.0372(3) Uani 1 1 d . . . . .
Cl1 Cl 0.45890(9) 0.20907(6) 0.25428(4) 0.0312(3) Uani 1 1 d . . . . .
Cl2 Cl 0.23992(10) -0.02094(6) 0.13326(5) 0.0346(3) Uani 1 1 d . . . . .
Cl3 Cl 0.44352(9) 0.24150(6) -0.01018(4) 0.0302(3) Uani 1 1 d . . . . .
C1 C 0.6799(5) 0.4071(3) 0.1667(2) 0.0492(11) Uani 1 1 d . . . . .
H1A H 0.6200 0.4527 0.1854 0.059 Uiso 1 1 calc R U . . .
H1B H 0.6596 0.3501 0.1876 0.059 Uiso 1 1 calc R U . . .
C2 C 0.8238(5) 0.5827(3) 0.1207(2) 0.0466(11) Uani 1 1 d . . . . .
H2A H 0.9018 0.6224 0.1122 0.056 Uiso 1 1 calc R U . . .
H2B H 0.7439 0.6207 0.1291 0.056 Uiso 1 1 calc R U . . .
C3 C 0.7952(5) 0.5289(3) 0.06139(19) 0.0420(10) Uani 1 1 d . . . . .
H3A H 0.8665 0.4830 0.0572 0.050 Uiso 1 1 calc R U . . .
H3B H 0.8030 0.5688 0.0248 0.050 Uiso 1 1 calc R U . . .
C4 C 0.8268(5) 0.4318(3) 0.1801(2) 0.0447(10) Uani 1 1 d . . . . .
H4A H 0.8522 0.4080 0.2216 0.054 Uiso 1 1 calc R U . . .
H4B H 0.8857 0.4028 0.1486 0.054 Uiso 1 1 calc R U . . .
C5 C 0.6557(5) 0.4831(3) 0.0589(2) 0.0535(12) Uani 1 1 d . . . . .
H5A H 0.5860 0.5253 0.0741 0.064 Uiso 1 1 calc R U . . .
H5B H 0.6342 0.4692 0.0148 0.064 Uiso 1 1 calc R U . . .
N1 N 0.8547(4) 0.5297(2) 0.17935(17) 0.0472(9) Uani 1 1 d . . . . .
H1C H 0.9441 0.5374 0.1883 0.057 Uiso 1 1 calc R U . . .
H1D H 0.8068 0.5544 0.2112 0.057 Uiso 1 1 calc R U . . .
N2 N 0.6456(4) 0.3986(2) 0.09698(18) 0.0442(9) Uani 1 1 d . . . . .
H2C H 0.7023 0.3577 0.0798 0.053 Uiso 1 1 calc R U . . .
H2D H 0.5596 0.3773 0.0935 0.053 Uiso 1 1 calc R U . . .
O1 O 0.6074(3) 0.2052(2) 0.24729(15) 0.0458(8) Uani 1 1 d . . . . .
O2 O 0.4254(3) 0.2299(2) 0.31934(14) 0.0481(8) Uani 1 1 d . . . . .
O3 O 0.4055(3) 0.2782(2) 0.21300(15) 0.0494(8) Uani 1 1 d . . . . .
O4 O 0.3991(3) 0.1231(2) 0.23709(16) 0.0523(9) Uani 1 1 d . . . . .
O5 O 0.3084(4) 0.0456(2) 0.09467(18) 0.0653(10) Uani 1 1 d . . . . .
O6 O 0.1384(3) 0.0218(2) 0.17338(16) 0.0553(9) Uani 1 1 d . . . . .
O7 O 0.3408(3) -0.0664(3) 0.17208(17) 0.0594(9) Uani 1 1 d . . . . .
O8 O 0.1721(3) -0.0860(2) 0.09249(15) 0.0465(8) Uani 1 1 d . . . . .
O9 O 0.2958(3) 0.2378(2) -0.02039(17) 0.0517(9) Uani 1 1 d . . . . .
O10 O 0.4700(3) 0.2351(2) 0.05729(14) 0.0419(7) Uani 1 1 d . . . . .
O11 O 0.5094(3) 0.16803(19) -0.04343(14) 0.0445(7) Uani 1 1 d . . . . .
O12 O 0.4984(3) 0.32579(18) -0.03299(14) 0.0422(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O3 2.771(3) . ?
K1 O10 2.872(3) . ?
K1 O12 2.886(3) 3_455 ?
K1 O1 2.917(3) 6_556 ?
K1 O11 2.942(3) 3_455 ?
K1 O5 2.968(4) . ?
K1 O2 2.984(4) 6_556 ?
K1 O8 3.008(4) 7_665 ?
K1 O9 3.115(4) . ?
K1 O7 3.204(4) 7_665 ?
K1 O6 3.342(4) . ?
K1 O4 3.418(4) . ?
Cl1 O2 1.434(3) . ?
Cl1 O3 1.435(3) . ?
Cl1 O1 1.440(3) . ?
Cl1 O4 1.443(3) . ?
Cl1 K1 3.5388(16) 6_656 ?
Cl2 O5 1.434(3) . ?
Cl2 O7 1.435(3) . ?
Cl2 O6 1.436(3) . ?
Cl2 O8 1.443(3) . ?
Cl2 K1 3.709(2) 7_655 ?
Cl3 O12 1.436(3) . ?
Cl3 O11 1.439(3) . ?
Cl3 O10 1.439(3) . ?
Cl3 O9 1.441(3) . ?
Cl3 K1 3.4970(16) 3 ?
C1 C4 1.489(6) . ?
C1 N2 1.503(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.488(5) . ?
C2 C3 1.501(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C5 1.506(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.473(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.487(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
O1 K1 2.917(3) 6_656 ?
O2 K1 2.984(4) 6_656 ?
O7 K1 3.204(4) 7_655 ?
O8 K1 3.008(4) 7_655 ?
O11 K1 2.942(3) 3 ?
O12 K1 2.886(3) 3 ?

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
O3 K1 O10 73.60(10) . . ?
O3 K1 O12 176.96(10) . 3_455 ?
O10 K1 O12 108.13(9) . 3_455 ?
O3 K1 O1 67.93(10) . 6_556 ?
O10 K1 O1 137.80(9) . 6_556 ?
O12 K1 O1 109.64(9) 3_455 6_556 ?
O3 K1 O11 134.79(10) . 3_455 ?
O10 K1 O11 107.03(9) . 3_455 ?
O12 K1 O11 47.47(8) 3_455 3_455 ?
O1 K1 O11 112.11(9) 6_556 3_455 ?
O3 K1 O5 98.30(11) . . ?
O10 K1 O5 68.81(9) . . ?
O12 K1 O5 80.19(10) 3_455 . ?
O1 K1 O5 99.89(10) 6_556 . ?
O11 K1 O5 124.70(10) 3_455 . ?
O3 K1 O2 110.52(10) . 6_556 ?
O10 K1 O2 175.44(9) . 6_556 ?
O12 K1 O2 67.85(9) 3_455 6_556 ?
O1 K1 O2 46.76(8) 6_556 6_556 ?
O11 K1 O2 68.75(9) 3_455 6_556 ?
O5 K1 O2 111.86(10) . 6_556 ?
O3 K1 O8 69.76(9) . 7_665 ?
O10 K1 O8 62.90(8) . 7_665 ?
O12 K1 O8 113.21(9) 3_455 7_665 ?
O1 K1 O8 116.24(9) 6_556 7_665 ?
O11 K1 O8 71.04(9) 3_455 7_665 ?
O5 K1 O8 131.69(9) . 7_665 ?
O2 K1 O8 116.18(9) 6_556 7_665 ?
O3 K1 O9 117.56(10) . . ?
O10 K1 O9 45.76(8) . . ?
O12 K1 O9 64.71(8) 3_455 . ?
O1 K1 O9 173.09(9) 6_556 . ?
O11 K1 O9 67.51(9) 3_455 . ?
O5 K1 O9 75.58(10) . . ?
O2 K1 O9 129.73(8) 6_556 . ?
O8 K1 O9 70.43(8) 7_665 . ?
O3 K1 O7 69.23(10) . 7_665 ?
O10 K1 O7 105.33(9) . 7_665 ?
O12 K1 O7 112.31(9) 3_455 7_665 ?
O1 K1 O7 76.83(9) 6_556 7_665 ?
O11 K1 O7 67.18(9) 3_455 7_665 ?
O5 K1 O7 167.49(10) . 7_665 ?
O2 K1 O7 74.91(9) 6_556 7_665 ?
O8 K1 O7 44.24(8) 7_665 7_665 ?
O9 K1 O7 108.70(9) . 7_665 ?
O3 K1 O6 98.89(9) . . ?
O10 K1 O6 110.32(8) . . ?
O12 K1 O6 78.20(8) 3_455 . ?
O1 K1 O6 60.97(8) 6_556 . ?
O11 K1 O6 121.20(8) 3_455 . ?
O5 K1 O6 43.25(9) . . ?
O2 K1 O6 71.42(9) 6_556 . ?
O8 K1 O6 167.76(9) 7_665 . ?
O9 K1 O6 112.94(9) . . ?
O7 K1 O6 137.23(9) 7_665 . ?
O3 K1 O4 43.09(9) . . ?
O10 K1 O4 82.58(9) . . ?
O12 K1 O4 134.21(8) 3_455 . ?
O1 K1 O4 57.55(8) 6_556 . ?
O11 K1 O4 169.57(9) 3_455 . ?
O5 K1 O4 62.04(9) . . ?
O2 K1 O4 101.75(9) 6_556 . ?
O8 K1 O4 111.19(8) 7_665 . ?
O9 K1 O4 122.92(9) . . ?
O7 K1 O4 106.87(9) 7_665 . ?
O6 K1 O4 56.80(8) . . ?
O2 Cl1 O3 109.8(2) . . ?
O2 Cl1 O1 109.18(19) . . ?
O3 Cl1 O1 108.9(2) . . ?
O2 Cl1 O4 109.7(2) . . ?
O3 Cl1 O4 109.6(2) . . ?
O1 Cl1 O4 109.71(19) . . ?
O2 Cl1 K1 56.00(14) . 6_656 ?
O3 Cl1 K1 128.08(14) . 6_656 ?
O1 Cl1 K1 53.31(13) . 6_656 ?
O4 Cl1 K1 122.30(15) . 6_656 ?
O5 Cl2 O7 109.2(2) . . ?
O5 Cl2 O6 110.0(2) . . ?
O7 Cl2 O6 109.6(2) . . ?
O5 Cl2 O8 109.4(2) . . ?
O7 Cl2 O8 109.2(2) . . ?
O6 Cl2 O8 109.33(19) . . ?
O5 Cl2 K1 125.65(16) . 7_655 ?
O7 Cl2 K1 58.60(15) . 7_655 ?
O6 Cl2 K1 124.18(16) . 7_655 ?
O8 Cl2 K1 50.66(13) . 7_655 ?
O12 Cl3 O11 109.41(18) . . ?
O12 Cl3 O10 108.60(18) . . ?
O11 Cl3 O10 110.31(19) . . ?
O12 Cl3 O9 110.3(2) . . ?
O11 Cl3 O9 109.62(19) . . ?
O10 Cl3 O9 108.6(2) . . ?
O12 Cl3 K1 53.59(12) . 3 ?
O11 Cl3 K1 55.90(13) . 3 ?
O10 Cl3 K1 122.69(13) . 3 ?
O9 Cl3 K1 128.71(16) . 3 ?
C4 C1 N2 114.4(4) . . ?
C4 C1 H1A 108.7 . . ?
N2 C1 H1A 108.7 . . ?
C4 C1 H1B 108.7 . . ?
N2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
N1 C2 C3 116.1(4) . . ?
N1 C2 H2A 108.3 . . ?
C3 C2 H2A 108.3 . . ?
N1 C2 H2B 108.3 . . ?
C3 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
C2 C3 C5 115.5(4) . . ?
C2 C3 H3A 108.4 . . ?
C5 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
C5 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
N1 C4 C1 114.3(4) . . ?
N1 C4 H4A 108.7 . . ?
C1 C4 H4A 108.7 . . ?
N1 C4 H4B 108.7 . . ?
C1 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
N2 C5 C3 114.7(4) . . ?
N2 C5 H5A 108.6 . . ?
C3 C5 H5A 108.6 . . ?
N2 C5 H5B 108.6 . . ?
C3 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
C4 N1 C2 119.4(3) . . ?
C4 N1 H1C 107.5 . . ?
C2 N1 H1C 107.5 . . ?
C4 N1 H1D 107.5 . . ?
C2 N1 H1D 107.5 . . ?
H1C N1 H1D 107.0 . . ?
C5 N2 C1 115.8(3) . . ?
C5 N2 H2C 108.3 . . ?
C1 N2 H2C 108.3 . . ?
C5 N2 H2D 108.3 . . ?
C1 N2 H2D 108.3 . . ?
H2C N2 H2D 107.4 . . ?
Cl1 O1 K1 103.37(16) . 6_656 ?
Cl1 O2 K1 100.52(16) . 6_656 ?
Cl1 O3 K1 118.56(19) . . ?
Cl1 O4 K1 88.72(16) . . ?
Cl2 O5 K1 111.9(2) . . ?
Cl2 O6 K1 94.85(17) . . ?
Cl2 O7 K1 98.94(17) . 7_655 ?
Cl2 O8 K1 107.56(16) . 7_655 ?
Cl3 O9 K1 97.25(17) . . ?
Cl3 O10 K1 108.30(16) . . ?
Cl3 O11 K1 100.22(15) . 3 ?
Cl3 O12 K1 102.80(15) . 3 ?

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
N1 C2 C3 C5 74.3(6) . . . . ?
N2 C1 C4 N1 86.0(5) . . . . ?
C2 C3 C5 N2 -78.4(5) . . . . ?
C1 C4 N1 C2 -58.2(6) . . . . ?
C3 C2 N1 C4 -12.9(6) . . . . ?
C3 C5 N2 C1 56.6(5) . . . . ?
C4 C1 N2 C5 -65.0(5) . . . . ?
O2 Cl1 O1 K1 4.1(2) . . . 6_656 ?
O3 Cl1 O1 K1 123.92(17) . . . 6_656 ?
O4 Cl1 O1 K1 -116.17(18) . . . 6_656 ?
O3 Cl1 O2 K1 -123.23(17) . . . 6_656 ?
O1 Cl1 O2 K1 -3.9(2) . . . 6_656 ?
O4 Cl1 O2 K1 116.31(17) . . . 6_656 ?
O2 Cl1 O3 K1 -117.9(2) . . . . ?
O1 Cl1 O3 K1 122.6(2) . . . . ?
O4 Cl1 O3 K1 2.6(3) . . . . ?
K1 Cl1 O3 K1 -179.66(6) 6_656 . . . ?
O2 Cl1 O4 K1 118.72(16) . . . . ?
O3 Cl1 O4 K1 -1.87(18) . . . . ?
O1 Cl1 O4 K1 -121.36(15) . . . . ?
K1 Cl1 O4 K1 -179.74(6) 6_656 . . . ?
O7 Cl2 O5 K1 -118.6(2) . . . . ?
O6 Cl2 O5 K1 1.8(3) . . . . ?
O8 Cl2 O5 K1 121.89(18) . . . . ?
K1 Cl2 O5 K1 176.84(5) 7_655 . . . ?
O5 Cl2 O6 K1 -1.5(2) . . . . ?
O7 Cl2 O6 K1 118.61(18) . . . . ?
O8 Cl2 O6 K1 -121.65(16) . . . . ?
K1 Cl2 O6 K1 -176.62(5) 7_655 . . . ?
O5 Cl2 O7 K1 -120.69(19) . . . 7_655 ?
O6 Cl2 O7 K1 118.75(18) . . . 7_655 ?
O8 Cl2 O7 K1 -1.0(2) . . . 7_655 ?
O5 Cl2 O8 K1 120.7(2) . . . 7_655 ?
O7 Cl2 O8 K1 1.1(2) . . . 7_655 ?
O6 Cl2 O8 K1 -118.84(19) . . . 7_655 ?
O12 Cl3 O9 K1 -115.72(16) . . . . ?
O11 Cl3 O9 K1 123.73(16) . . . . ?
O10 Cl3 O9 K1 3.17(19) . . . . ?
K1 Cl3 O9 K1 -174.77(5) 3 . . . ?
O12 Cl3 O10 K1 116.39(16) . . . . ?
O11 Cl3 O10 K1 -123.72(16) . . . . ?
O9 Cl3 O10 K1 -3.6(2) . . . . ?
K1 Cl3 O10 K1 174.50(4) 3 . . . ?
O12 Cl3 O11 K1 3.0(2) . . . 3 ?
O10 Cl3 O11 K1 -116.42(16) . . . 3 ?
O9 Cl3 O11 K1 124.09(18) . . . 3 ?
O11 Cl3 O12 K1 -3.1(2) . . . 3 ?
O10 Cl3 O12 K1 117.38(16) . . . 3 ?
O9 Cl3 O12 K1 -123.74(18) . . . 3 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1B O1 0.97 2.53 3.501(6) 177.2 .
C2 H2A O10 0.97 2.37 3.285(5) 156.4 7_765
C2 H2B O2 0.97 2.54 3.477(6) 163.3 4_655
C3 H3A O11 0.97 2.64 3.590(5) 166.3 3
C4 H4A O3 0.97 2.41 3.278(5) 148.3 6_656
C5 H5A O12 0.97 2.50 3.239(6) 132.7 5_665
N1 H1C O4 0.89 2.22 3.001(5) 146.0 7_765
N1 H1C O7 0.89 2.60 3.266(5) 132.0 7_765
N1 H1D O1 0.89 2.50 2.984(5) 114.9 7_765
N1 H1D O4 0.89 2.48 3.310(5) 155.6 4_655
N1 H1D O6 0.89 2.52 3.088(5) 122.2 4_655
N2 H2C O9 0.89 2.09 2.957(5) 164.8 3
N2 H2D O8 0.89 2.30 3.073(5) 145.4 7_665
N2 H2D O10 0.89 2.40 3.067(4) 132.2 .

_refine_diff_density_max         0.784
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.132

####################################################################### 
# 
# 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_1-328K
_database_code_depnum_ccdc_archive 'CCDC 1564730'
_audit_update_record             
;
2017-10-31 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl3 K O12, C5 H14 N2'
_chemical_formula_sum            'C5 H14 Cl3 K N2 O12'
_chemical_formula_weight         439.63

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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'

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

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

_cell_length_a                   10.682(10)
_cell_length_b                   9.876(10)
_cell_length_c                   14.264(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1505(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4067
_cell_measurement_theta_min      1.9065
_cell_measurement_theta_max      27.5165

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_absorpt_coefficient_mu    0.951
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5917
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10356
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.906
_diffrn_reflns_theta_max         27.440
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1793
_reflns_number_gt                1273
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1180P)²+1.5084P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1793
_refine_ls_number_parameters     143
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0896
_refine_ls_wR_factor_ref         0.2758
_refine_ls_wR_factor_gt          0.2411
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.259
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.25213(13) 0.71439(17) 0.2500 0.0459(5) Uani 1 2 d S TU P . .
Cl1 Cl 0.48142(19) 0.44825(19) 0.2500 0.0548(6) Uani 1 2 d S TU P . .
Cl2 Cl 0.25275(17) 0.7500 0.0000 0.0680(8) Uani 1 2 d S TU P . .
Cl3 Cl 0.0105(2) 0.4550(2) 0.2500 0.0658(7) Uani 1 2 d S TU P . .
C1 C 0.3934(17) 0.215(2) 1.0135(18) 0.098(4) Uani 0.5 1 d D U P . .
H1A H 0.4764 0.2174 1.0391 0.118 Uiso 0.5 1 d R U P . .
H1B H 0.3925 0.1455 0.9663 0.118 Uiso 0.5 1 d R U P . .
C2 C 0.1506(18) 0.182(2) 1.0673(14) 0.110(4) Uani 0.5 1 d D U P . .
H2A H 0.1208 0.0921 1.0549 0.131 Uiso 0.5 1 d R U P . .
H2B H 0.1105 0.2100 1.1244 0.131 Uiso 0.5 1 d R U P . .
C3 C 0.1006(12) 0.2500 1.0000 0.117(3) Uani 1 2 d DS TU P . .
H3A H 0.0156 0.2669 1.0183 0.141 Uiso 0.5 1 d R U P . .
H3B H 0.0984 0.1991 0.9427 0.141 Uiso 0.5 1 d R U P . .
C4 C 0.373(2) 0.328(2) 0.9686(17) 0.099(4) Uani 0.5 1 d D U P . .
H4A H 0.4426 0.3493 0.9284 0.119 Uiso 0.5 1 d R U P . .
H4B H 0.3676 0.3984 1.0151 0.119 Uiso 0.5 1 d R U P . .
C5 C 0.1484(18) 0.3677(17) 0.9775(15) 0.109(4) Uani 0.5 1 d D U P . .
H5A H 0.1841 0.4105 1.0317 0.131 Uiso 0.5 1 d R U P . .
H5B H 0.0814 0.4238 0.9550 0.131 Uiso 0.5 1 d R U P . .
N1 N 0.3154(13) 0.1592(19) 1.0746(13) 0.115(4) Uani 0.5 1 d D U P . .
H1C H 0.3323 0.2104 1.1252 0.139 Uiso 0.5 1 d R U P . .
H1D H 0.3339 0.0730 1.0898 0.139 Uiso 0.5 1 d R U P . .
N2 N 0.2420(10) 0.332(2) 0.9033(12) 0.098(3) Uani 0.5 1 d D U P . .
H2C H 0.2334 0.2538 0.8717 0.117 Uiso 0.5 1 d R U P . .
H2D H 0.2395 0.4017 0.8626 0.117 Uiso 0.5 1 d R U P . .
O1 O 0.4653(7) 0.3061(6) 0.2500 0.094(2) Uani 1 2 d S TU P . .
O2 O 0.6140(5) 0.4774(6) 0.2500 0.0645(15) Uani 1 2 d S TU P . .
O3 O 0.4239(4) 0.5074(5) 0.1693(3) 0.0789(13) Uani 1 1 d . U . . .
O4 O 0.3296(4) 0.8209(6) 0.0663(3) 0.0878(15) Uani 1 1 d . U . . .
O5 O 0.1759(4) 0.6577(6) 0.0515(3) 0.0839(15) Uani 1 1 d . U . . .
O6 O 0.1388(6) 0.4232(8) 0.2500 0.099(2) Uani 1 2 d S TU P . .
O7 O -0.0013(7) 0.5980(6) 0.2500 0.0877(19) Uani 1 2 d S TU P . .
O8 O -0.0501(5) 0.3979(6) 0.3295(4) 0.112(2) 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
K1 O7 2.941(7) . ?
K1 O4 2.943(5) . ?
K1 O4 2.943(5) 6_556 ?
K1 O2 2.965(6) 7_665 ?
K1 O3 2.978(5) 6_556 ?
K1 O3 2.978(5) . ?
K1 O5 2.999(5) . ?
K1 O5 2.999(5) 6_556 ?
K1 O8 3.038(6) 4 ?
K1 O8 3.038(6) 7_565 ?
K1 O6 3.120(8) . ?
K1 O1 3.151(8) 7_665 ?
Cl1 O1 1.414(6) . ?
Cl1 O3 1.429(4) . ?
Cl1 O3 1.429(4) 6_556 ?
Cl1 O2 1.445(6) . ?
Cl1 K1 3.665(3) 7_655 ?
Cl2 O5 1.429(5) . ?
Cl2 O5 1.429(5) 3_565 ?
Cl2 O4 1.434(5) 3_565 ?
Cl2 O4 1.434(5) . ?
Cl2 K1 3.583(3) 3_565 ?
Cl3 O6 1.406(7) . ?
Cl3 O7 1.418(6) . ?
Cl3 O8 1.422(5) 6_556 ?
Cl3 O8 1.422(5) . ?
Cl3 K1 3.677(3) 7 ?
C1 C4 0.54(3) 3_557 ?
C1 C1 0.79(3) 3_557 ?
C1 C4 1.309(15) . ?
C1 N1 1.32(2) . ?
C1 N1 1.95(2) 3_557 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C2 C5 0.81(3) 3_557 ?
C2 N2 1.07(2) 3_557 ?
C2 C3 1.288(19) . ?
C2 N1 1.78(2) . ?
C2 H2A 0.9601 . ?
C2 H2B 0.9600 . ?
C3 C2 1.29(2) 3_557 ?
C3 C5 1.309(15) 3_557 ?
C3 C5 1.309(15) . ?
C3 H3A 0.9599 . ?
C3 H3B 0.9599 . ?
C4 C1 0.54(3) 3_557 ?
C4 N1 0.88(2) 3_557 ?
C4 N2 1.68(2) . ?
C4 C4 1.79(3) 3_557 ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C5 C2 0.81(3) 3_557 ?
C5 N2 1.50(2) . ?
C5 N1 1.95(3) 3_557 ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
N1 N2 0.849(17) 3_557 ?
N1 C4 0.88(2) 3_557 ?
N1 C5 1.95(3) 3_557 ?
N1 C1 1.95(2) 3_557 ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 N1 0.849(17) 3_557 ?
N2 C2 1.07(2) 3_557 ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
O1 K1 3.151(8) 7_655 ?
O2 K1 2.965(6) 7_655 ?
O8 K1 3.037(6) 7 ?

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 K1 O4 113.49(9) . . ?
O7 K1 O4 113.49(9) . 6_556 ?
O4 K1 O4 125.9(2) . 6_556 ?
O7 K1 O2 141.84(18) . 7_665 ?
O4 K1 O2 63.33(11) . 7_665 ?
O4 K1 O2 63.33(11) 6_556 7_665 ?
O7 K1 O3 107.39(17) . 6_556 ?
O4 K1 O3 114.60(14) . 6_556 ?
O4 K1 O3 74.22(15) 6_556 6_556 ?
O2 K1 O3 107.70(16) 7_665 6_556 ?
O7 K1 O3 107.39(17) . . ?
O4 K1 O3 74.22(15) . . ?
O4 K1 O3 114.60(14) 6_556 . ?
O2 K1 O3 107.70(16) 7_665 . ?
O3 K1 O3 45.46(18) 6_556 . ?
O7 K1 O5 71.17(9) . . ?
O4 K1 O5 45.75(15) . . ?
O4 K1 O5 169.70(15) 6_556 . ?
O2 K1 O5 107.12(11) 7_665 . ?
O3 K1 O5 113.83(14) 6_556 . ?
O3 K1 O5 70.99(13) . . ?
O7 K1 O5 71.17(9) . 6_556 ?
O4 K1 O5 169.70(15) . 6_556 ?
O4 K1 O5 45.75(15) 6_556 6_556 ?
O2 K1 O5 107.12(11) 7_665 6_556 ?
O3 K1 O5 70.99(13) 6_556 6_556 ?
O3 K1 O5 113.83(14) . 6_556 ?
O5 K1 O5 141.54(19) . 6_556 ?
O7 K1 O8 65.11(17) . 4 ?
O4 K1 O8 69.77(15) . 4 ?
O4 K1 O8 108.59(16) 6_556 4 ?
O2 K1 O8 79.64(18) 7_665 4 ?
O3 K1 O8 172.49(16) 6_556 4 ?
O3 K1 O8 134.68(15) . 4 ?
O5 K1 O8 64.29(14) . 4 ?
O5 K1 O8 105.71(15) 6_556 4 ?
O7 K1 O8 65.11(17) . 7_565 ?
O4 K1 O8 108.59(16) . 7_565 ?
O4 K1 O8 69.77(15) 6_556 7_565 ?
O2 K1 O8 79.64(18) 7_665 7_565 ?
O3 K1 O8 134.68(15) 6_556 7_565 ?
O3 K1 O8 172.49(16) . 7_565 ?
O5 K1 O8 105.71(15) . 7_565 ?
O5 K1 O8 64.29(14) 6_556 7_565 ?
O8 K1 O8 43.8(2) 4 7_565 ?
O7 K1 O6 44.17(18) . . ?
O4 K1 O6 116.02(11) . . ?
O4 K1 O6 116.02(11) 6_556 . ?
O2 K1 O6 173.99(18) 7_665 . ?
O3 K1 O6 66.82(17) 6_556 . ?
O3 K1 O6 66.82(17) . . ?
O5 K1 O6 73.90(11) . . ?
O5 K1 O6 73.90(11) 6_556 . ?
O8 K1 O6 105.91(18) 4 . ?
O8 K1 O6 105.91(18) 7_565 . ?
O7 K1 O1 173.70(17) . 7_665 ?
O4 K1 O1 68.16(10) . 7_665 ?
O4 K1 O1 68.16(10) 6_556 7_665 ?
O2 K1 O1 44.45(16) 7_665 7_665 ?
O3 K1 O1 66.87(15) 6_556 7_665 ?
O3 K1 O1 66.87(15) . 7_665 ?
O5 K1 O1 108.28(9) . 7_665 ?
O5 K1 O1 108.28(9) 6_556 7_665 ?
O8 K1 O1 120.60(17) 4 7_665 ?
O8 K1 O1 120.60(17) 7_565 7_665 ?
O6 K1 O1 129.53(18) . 7_665 ?
O1 Cl1 O3 110.7(3) . . ?
O1 Cl1 O3 110.7(3) . 6_556 ?
O3 Cl1 O3 107.2(4) . 6_556 ?
O1 Cl1 O2 108.5(4) . . ?
O3 Cl1 O2 109.9(3) . . ?
O3 Cl1 O2 109.9(3) 6_556 . ?
O1 Cl1 K1 130.0(3) . . ?
O3 Cl1 K1 53.67(19) . . ?
O3 Cl1 K1 53.67(19) 6_556 . ?
O2 Cl1 K1 121.5(3) . . ?
O1 Cl1 K1 57.9(3) . 7_655 ?
O3 Cl1 K1 126.3(2) . 7_655 ?
O3 Cl1 K1 126.3(2) 6_556 7_655 ?
O2 Cl1 K1 50.5(3) . 7_655 ?
K1 Cl1 K1 172.04(7) . 7_655 ?
O5 Cl2 O5 109.9(4) . 3_565 ?
O5 Cl2 O4 110.8(3) . 3_565 ?
O5 Cl2 O4 107.6(3) 3_565 3_565 ?
O5 Cl2 O4 107.6(3) . . ?
O5 Cl2 O4 110.8(3) 3_565 . ?
O4 Cl2 O4 110.2(4) 3_565 . ?
O5 Cl2 K1 54.93(18) . . ?
O5 Cl2 K1 124.93(19) 3_565 . ?
O4 Cl2 K1 127.5(2) 3_565 . ?
O4 Cl2 K1 52.7(2) . . ?
O5 Cl2 K1 124.93(19) . 3_565 ?
O5 Cl2 K1 54.93(18) 3_565 3_565 ?
O4 Cl2 K1 52.7(2) 3_565 3_565 ?
O4 Cl2 K1 127.5(2) . 3_565 ?
K1 Cl2 K1 179.79(8) . 3_565 ?
O6 Cl3 O7 108.0(4) . . ?
O6 Cl3 O8 110.8(3) . 6_556 ?
O7 Cl3 O8 110.8(3) . 6_556 ?
O6 Cl3 O8 110.8(3) . . ?
O7 Cl3 O8 110.8(3) . . ?
O8 Cl3 O8 105.7(5) 6_556 . ?
O6 Cl3 K1 57.7(3) . . ?
O7 Cl3 K1 50.3(3) . . ?
O8 Cl3 K1 127.1(3) 6_556 . ?
O8 Cl3 K1 127.1(3) . . ?
O6 Cl3 K1 126.8(3) . 7 ?
O7 Cl3 K1 125.1(3) . 7 ?
O8 Cl3 K1 52.8(3) 6_556 7 ?
O8 Cl3 K1 52.8(3) . 7 ?
K1 Cl3 K1 175.48(8) . 7 ?
C4 C1 C1 157(4) 3_557 3_557 ?
C4 C1 C4 147(6) 3_557 . ?
C1 C1 C4 9.5(16) 3_557 . ?
C4 C1 N1 28(4) 3_557 . ?
C1 C1 N1 133(3) 3_557 . ?
C4 C1 N1 125(2) . . ?
C4 C1 N1 129(5) 3_557 3_557 ?
C1 C1 N1 29.7(19) 3_557 3_557 ?
C4 C1 N1 21.6(12) . 3_557 ?
N1 C1 N1 114.8(15) . 3_557 ?
C4 C1 H1A 102.0 3_557 . ?
C1 C1 H1A 99.3 3_557 . ?
C4 C1 H1A 108.4 . . ?
N1 C1 H1A 110.0 . . ?
N1 C1 H1A 128.5 3_557 . ?
C4 C1 H1B 76.3 3_557 . ?
C1 C1 H1B 106.5 3_557 . ?
C4 C1 H1B 105.5 . . ?
N1 C1 H1B 99.1 . . ?
N1 C1 H1B 90.0 3_557 . ?
H1A C1 H1B 107.1 . . ?
C5 C2 N2 105(3) 3_557 3_557 ?
C5 C2 C3 73.4(19) 3_557 . ?
N2 C2 C3 138(2) 3_557 . ?
C5 C2 N1 90(2) 3_557 . ?
N2 C2 N1 19.7(12) 3_557 . ?
C3 C2 N1 121.3(14) . . ?
C5 C2 H2A 44.0 3_557 . ?
N2 C2 H2A 104.7 3_557 . ?
C3 C2 H2A 102.0 . . ?
N1 C2 H2A 102.8 . . ?
C5 C2 H2B 146.4 3_557 . ?
N2 C2 H2B 96.5 3_557 . ?
C3 C2 H2B 107.3 . . ?
N1 C2 H2B 115.4 . . ?
H2A C2 H2B 105.9 . . ?
C2 C3 C2 131(2) 3_557 . ?
C2 C3 C5 119.0(14) 3_557 3_557 ?
C2 C3 C5 36.2(13) . 3_557 ?
C2 C3 C5 36.2(13) 3_557 . ?
C2 C3 C5 119.0(14) . . ?
C5 C3 C5 134(2) 3_557 . ?
C2 C3 H3A 120.3 3_557 . ?
C2 C3 H3A 106.3 . . ?
C5 C3 H3A 117.1 3_557 . ?
C5 C3 H3A 106.3 . . ?
C2 C3 H3B 69.4 3_557 . ?
C2 C3 H3B 111.8 . . ?
C5 C3 H3B 75.7 3_557 . ?
C5 C3 H3B 105.4 . . ?
H3A C3 H3B 107.4 . . ?
C1 C4 N1 136(6) 3_557 3_557 ?
C1 C4 C1 14(3) 3_557 . ?
N1 C4 C1 125(3) 3_557 . ?
C1 C4 N2 127(5) 3_557 . ?
N1 C4 N2 13.1(15) 3_557 . ?
C1 C4 N2 115.2(19) . . ?
C1 C4 C4 23(4) 3_557 3_557 ?
N1 C4 C4 118(2) 3_557 3_557 ?
C1 C4 C4 9.5(16) . 3_557 ?
N2 C4 C4 107.2(13) . 3_557 ?
C1 C4 H4A 98.3 3_557 . ?
N1 C4 H4A 95.4 3_557 . ?
C1 C4 H4A 110.5 . . ?
N2 C4 H4A 107.9 . . ?
C4 C4 H4A 119.0 3_557 . ?
C1 C4 H4B 105.5 3_557 . ?
N1 C4 H4B 109.8 3_557 . ?
C1 C4 H4B 106.8 . . ?
N2 C4 H4B 108.4 . . ?
C4 C4 H4B 106.1 3_557 . ?
H4A C4 H4B 107.9 . . ?
C2 C5 C3 70.5(19) 3_557 . ?
C2 C5 N2 44(2) 3_557 . ?
C3 C5 N2 103.0(15) . . ?
C2 C5 N1 66(2) 3_557 3_557 ?
C3 C5 N1 109.2(14) . 3_557 ?
N2 C5 N1 24.3(8) . 3_557 ?
C2 C5 H5A 153.4 3_557 . ?
C3 C5 H5A 110.4 . . ?
N2 C5 H5A 114.0 . . ?
N1 C5 H5A 90.2 3_557 . ?
C2 C5 H5B 96.2 3_557 . ?
C3 C5 H5B 107.7 . . ?
N2 C5 H5B 113.4 . . ?
N1 C5 H5B 129.2 3_557 . ?
H5A C5 H5B 108.2 . . ?
N2 N1 C4 153(3) 3_557 3_557 ?
N2 N1 C1 141(2) 3_557 . ?
C4 N1 C1 17(2) 3_557 . ?
N2 N1 C2 25.2(16) 3_557 . ?
C4 N1 C2 130(2) 3_557 . ?
C1 N1 C2 122.1(13) . . ?
N2 N1 C5 46.5(18) 3_557 3_557 ?
C4 N1 C5 113(3) 3_557 3_557 ?
C1 N1 C5 112.4(15) . 3_557 ?
C2 N1 C5 24.4(9) . 3_557 ?
N2 N1 C1 125(2) 3_557 3_557 ?
C4 N1 C1 33.2(16) 3_557 3_557 ?
C1 N1 C1 17.3(12) . 3_557 ?
C2 N1 C1 107.7(10) . 3_557 ?
C5 N1 C1 103.4(11) 3_557 3_557 ?
N2 N1 H1C 80.2 3_557 . ?
C4 N1 H1C 110.0 3_557 . ?
C1 N1 H1C 99.7 . . ?
C2 N1 H1C 100.0 . . ?
C5 N1 H1C 124.4 3_557 . ?
C1 N1 H1C 94.2 3_557 . ?
N2 N1 H1D 102.1 3_557 . ?
C4 N1 H1D 98.3 3_557 . ?
C1 N1 H1D 114.3 . . ?
C2 N1 H1D 110.6 . . ?
C5 N1 H1D 99.5 3_557 . ?
C1 N1 H1D 131.5 3_557 . ?
H1C N1 H1D 107.1 . . ?
N1 N2 C2 135(3) 3_557 3_557 ?
N1 N2 C5 109(2) 3_557 . ?
C2 N2 C5 31.3(15) 3_557 . ?
N1 N2 C4 13.6(16) 3_557 . ?
C2 N2 C4 122.6(19) 3_557 . ?
C5 N2 C4 99.8(16) . . ?
N1 N2 H2C 111.6 3_557 . ?
C2 N2 H2C 89.5 3_557 . ?
C5 N2 H2C 119.2 . . ?
C4 N2 H2C 110.1 . . ?
N1 N2 H2D 100.9 3_557 . ?
C2 N2 H2D 109.0 3_557 . ?
C5 N2 H2D 104.9 . . ?
C4 N2 H2D 113.4 . . ?
H2C N2 H2D 109.3 . . ?
Cl1 O1 K1 99.7(4) . 7_655 ?
Cl1 O2 K1 107.4(3) . 7_655 ?
Cl1 O3 K1 103.6(2) . . ?
Cl2 O4 K1 104.5(3) . . ?
Cl2 O5 K1 102.1(2) . . ?
Cl3 O6 K1 99.9(4) . . ?
Cl3 O7 K1 107.9(4) . . ?
Cl3 O8 K1 105.2(3) . 7 ?

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
C5 C2 C3 C2 -84(2) 3_557 . . 3_557 ?
N2 C2 C3 C2 10(3) 3_557 . . 3_557 ?
N1 C2 C3 C2 -4.8(12) . . . 3_557 ?
N2 C2 C3 C5 94(4) 3_557 . . 3_557 ?
N1 C2 C3 C5 79(2) . . . 3_557 ?
C5 C2 C3 C5 -126(3) 3_557 . . . ?
N2 C2 C3 C5 -32(4) 3_557 . . . ?
N1 C2 C3 C5 -47(2) . . . . ?
C4 C1 C4 C1 174(33) 3_557 . . 3_557 ?
N1 C1 C4 C1 149(24) . . . 3_557 ?
N1 C1 C4 C1 -143(24) 3_557 . . 3_557 ?
C4 C1 C4 N1 -43(9) 3_557 . . 3_557 ?
C1 C1 C4 N1 143(24) 3_557 . . 3_557 ?
N1 C1 C4 N1 -68(4) . . . 3_557 ?
C4 C1 C4 N2 -33(10) 3_557 . . . ?
C1 C1 C4 N2 153(23) 3_557 . . . ?
N1 C1 C4 N2 -58(3) . . . . ?
N1 C1 C4 N2 10(2) 3_557 . . . ?
C1 C1 C4 C4 -174(33) 3_557 . . 3_557 ?
N1 C1 C4 C4 -25(9) . . . 3_557 ?
N1 C1 C4 C4 43(9) 3_557 . . 3_557 ?
C2 C3 C5 C2 121(3) . . . 3_557 ?
C5 C3 C5 C2 79(2) 3_557 . . 3_557 ?
C2 C3 C5 N2 -29.6(17) 3_557 . . . ?
C2 C3 C5 N2 91.3(17) . . . . ?
C5 C3 C5 N2 49.7(10) 3_557 . . . ?
C2 C3 C5 N1 -54(2) 3_557 . . 3_557 ?
C2 C3 C5 N1 66.8(18) . . . 3_557 ?
C5 C3 C5 N1 25.3(9) 3_557 . . 3_557 ?
C4 C1 N1 N2 -144(10) 3_557 . . 3_557 ?
C1 C1 N1 N2 14(9) 3_557 . . 3_557 ?
C4 C1 N1 N2 7(6) . . . 3_557 ?
N1 C1 N1 N2 -15(5) 3_557 . . 3_557 ?
C1 C1 N1 C4 157(13) 3_557 . . 3_557 ?
C4 C1 N1 C4 151(10) . . . 3_557 ?
N1 C1 N1 C4 129(10) 3_557 . . 3_557 ?
C4 C1 N1 C2 -122(9) 3_557 . . . ?
C1 C1 N1 C2 36(7) 3_557 . . . ?
C4 C1 N1 C2 29(3) . . . . ?
N1 C1 N1 C2 7(3) 3_557 . . . ?
C4 C1 N1 C5 -96(9) 3_557 . . 3_557 ?
C1 C1 N1 C5 61(7) 3_557 . . 3_557 ?
C4 C1 N1 C5 55(3) . . . 3_557 ?
N1 C1 N1 C5 33(2) 3_557 . . 3_557 ?
C4 C1 N1 C1 -157(13) 3_557 . . 3_557 ?
C4 C1 N1 C1 -7(5) . . . 3_557 ?
N1 C1 N1 C1 -29(5) 3_557 . . 3_557 ?
C5 C2 N1 N2 -140(6) 3_557 . . 3_557 ?
C3 C2 N1 N2 149(5) . . . 3_557 ?
C5 C2 N1 C4 55(4) 3_557 . . 3_557 ?
N2 C2 N1 C4 -165(6) 3_557 . . 3_557 ?
C3 C2 N1 C4 -16(4) . . . 3_557 ?
C5 C2 N1 C1 73(3) 3_557 . . . ?
N2 C2 N1 C1 -147(5) 3_557 . . . ?
C3 C2 N1 C1 3(3) . . . . ?
N2 C2 N1 C5 140(6) 3_557 . . 3_557 ?
C3 C2 N1 C5 -70(2) . . . 3_557 ?
C5 C2 N1 C1 83(2) 3_557 . . 3_557 ?
N2 C2 N1 C1 -136(5) 3_557 . . 3_557 ?
C3 C2 N1 C1 13(2) . . . 3_557 ?
C2 C5 N2 N1 -150(4) 3_557 . . 3_557 ?
C3 C5 N2 N1 -108(3) . . . 3_557 ?
C3 C5 N2 C2 42(2) . . . 3_557 ?
N1 C5 N2 C2 150(4) 3_557 . . 3_557 ?
C2 C5 N2 C4 -140(3) 3_557 . . . ?
C3 C5 N2 C4 -97.9(17) . . . . ?
N1 C5 N2 C4 10.1(18) 3_557 . . . ?
C1 C4 N2 N1 -134(13) 3_557 . . 3_557 ?
C1 C4 N2 N1 -142(9) . . . 3_557 ?
C4 C4 N2 N1 -147(9) 3_557 . . 3_557 ?
C1 C4 N2 C2 68(8) 3_557 . . 3_557 ?
N1 C4 N2 C2 -158(10) 3_557 . . 3_557 ?
C1 C4 N2 C2 60(3) . . . 3_557 ?
C4 C4 N2 C2 54(3) 3_557 . . 3_557 ?
C1 C4 N2 C5 91(7) 3_557 . . . ?
N1 C4 N2 C5 -135(9) 3_557 . . . ?
C1 C4 N2 C5 83(2) . . . . ?
C4 C4 N2 C5 78(2) 3_557 . . . ?
O3 Cl1 O1 K1 120.6(2) . . . 7_655 ?
O3 Cl1 O1 K1 -120.6(2) 6_556 . . 7_655 ?
O2 Cl1 O1 K1 0.0 . . . 7_655 ?
K1 Cl1 O1 K1 180.0 . . . 7_655 ?
O1 Cl1 O2 K1 0.0 . . . 7_655 ?
O3 Cl1 O2 K1 -121.1(2) . . . 7_655 ?
O3 Cl1 O2 K1 121.1(2) 6_556 . . 7_655 ?
K1 Cl1 O2 K1 180.0 . . . 7_655 ?
O1 Cl1 O3 K1 125.1(3) . . . . ?
O3 Cl1 O3 K1 4.3(4) 6_556 . . . ?
O2 Cl1 O3 K1 -115.1(3) . . . . ?
K1 Cl1 O3 K1 -170.12(9) 7_655 . . . ?
O5 Cl2 O4 K1 -1.5(3) . . . . ?
O5 Cl2 O4 K1 118.7(3) 3_565 . . . ?
O4 Cl2 O4 K1 -122.4(3) 3_565 . . . ?
K1 Cl2 O4 K1 179.81(7) 3_565 . . . ?
O5 Cl2 O5 K1 -119.3(3) 3_565 . . . ?
O4 Cl2 O5 K1 121.9(2) 3_565 . . . ?
O4 Cl2 O5 K1 1.4(3) . . . . ?
K1 Cl2 O5 K1 -179.82(7) 3_565 . . . ?
O7 Cl3 O6 K1 0.0 . . . . ?
O8 Cl3 O6 K1 121.5(3) 6_556 . . . ?
O8 Cl3 O6 K1 -121.5(3) . . . . ?
K1 Cl3 O6 K1 180.0 7 . . . ?
O6 Cl3 O7 K1 0.0 . . . . ?
O8 Cl3 O7 K1 -121.5(3) 6_556 . . . ?
O8 Cl3 O7 K1 121.5(3) . . . . ?
K1 Cl3 O7 K1 180.0 7 . . . ?
O6 Cl3 O8 K1 -121.1(3) . . . 7 ?
O7 Cl3 O8 K1 119.0(3) . . . 7 ?
O8 Cl3 O8 K1 -1.0(5) 6_556 . . 7 ?
K1 Cl3 O8 K1 174.33(10) . . . 7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1 H1A Cl2 0.96 2.96 3.801(19) 146.4 5_666
C1 H1A O4 0.96 2.59 3.19(2) 121.0 5_666
C1 H1A O4 0.96 2.34 3.23(2) 153.1 7_656
C1 H1B O3 0.96 2.48 3.42(3) 168.8 3_556
C2 H2A O8 0.96 2.64 3.35(2) 130.7 4_546
C2 H2B O7 0.96 2.41 3.166(18) 135.7 7_556
C3 H3A Cl2 0.96 2.88 3.775(13) 155.0 5_566
C3 H3A O5 0.96 2.39 3.177(12) 138.6 5_566
C3 H3A O5 0.96 2.36 3.177(12) 142.7 7_556
C3 H3A O8 0.96 2.62 3.262(9) 124.3 6_557
C3 H3B O8 0.96 2.46 3.262(9) 141.2 8_566
C4 H4A O3 0.96 2.44 3.35(2) 156.3 5_666
C4 H4B O3 0.96 2.52 3.41(3) 153.6 1_556
C5 H5A O5 0.96 2.46 3.067(19) 121.0 1_556
C5 H5B O8 0.96 2.53 3.30(2) 137.4 2_565
N1 H1C O1 0.90 2.47 3.31(2) 155.6 1_556
N1 H1D O2 0.90 2.54 3.171(17) 128.1 7_656
N1 H1D O4 0.90 2.51 3.35(2) 154.2 1_546
N2 H2D O2 0.90 2.54 3.269(15) 138.5 5_666

_refine_diff_density_max         0.497
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.100

