# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_c
_audit_block_doi                 10.5517/ccdc.csd.cc20gf75
_database_code_depnum_ccdc_archive 'CCDC 1860906'
_audit_update_record             
;
2018-08-08 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_audit_creation_date             2018-07-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        DAP-O12
_chemical_formula_moiety         '0.25(Cl12 K4 O48), 1(C6 H14 N2 O)'
_chemical_formula_sum            'C6 H14 Cl3 K N2 O13'
_chemical_formula_weight         467.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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      cubic
_space_group_IT_number           226
_space_group_name_H-M_alt        'F m -3 c'
_space_group_name_Hall           '-F 4c 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y+1/2, x+1, -z+1'
'-y+1/2, -x+1, -z+1'
'y+1/2, -x+1, z+1'
'-y+1/2, x+1, z+1'
'x+1/2, z+1, -y+1'
'-x+1/2, z+1, y+1'
'-x+1/2, -z+1, -y+1'
'x+1/2, -z+1, y+1'
'z+1/2, y+1, -x+1'
'z+1/2, -y+1, x+1'
'-z+1/2, y+1, x+1'
'-z+1/2, -y+1, -x+1'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1, x+1/2, -z+1'
'-y+1, -x+1/2, -z+1'
'y+1, -x+1/2, z+1'
'-y+1, x+1/2, z+1'
'x+1, z+1/2, -y+1'
'-x+1, z+1/2, y+1'
'-x+1, -z+1/2, -y+1'
'x+1, -z+1/2, y+1'
'z+1, y+1/2, -x+1'
'z+1, -y+1/2, x+1'
'-z+1, y+1/2, x+1'
'-z+1, -y+1/2, -x+1'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1, x+1, -z+1/2'
'-y+1, -x+1, -z+1/2'
'y+1, -x+1, z+1/2'
'-y+1, x+1, z+1/2'
'x+1, z+1, -y+1/2'
'-x+1, z+1, y+1/2'
'-x+1, -z+1, -y+1/2'
'x+1, -z+1, y+1/2'
'z+1, y+1, -x+1/2'
'z+1, -y+1, x+1/2'
'-z+1, y+1, x+1/2'
'-z+1, -y+1, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y-1/2, -x, z'
'y-1/2, x, z'
'-y-1/2, x, -z'
'y-1/2, -x, -z'
'-x-1/2, -z, y'
'x-1/2, -z, -y'
'x-1/2, z, y'
'-x-1/2, z, -y'
'-z-1/2, -y, x'
'-z-1/2, y, -x'
'z-1/2, -y, -x'
'z-1/2, y, x'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y, -x-1/2, z'
'y, x-1/2, z'
'-y, x-1/2, -z'
'y, -x-1/2, -z'
'-x, -z-1/2, y'
'x, -z-1/2, -y'
'x, z-1/2, y'
'-x, z-1/2, -y'
'-z, -y-1/2, x'
'-z, y-1/2, -x'
'z, -y-1/2, -x'
'z, y-1/2, x'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-y, x, -z-1/2'
'y, -x, -z-1/2'
'-x, -z, y-1/2'
'x, -z, -y-1/2'
'x, z, y-1/2'
'-x, z, -y-1/2'
'-z, -y, x-1/2'
'-z, y, -x-1/2'
'z, -y, -x-1/2'
'z, y, x-1/2'

_cell_length_a                   14.745(3)
_cell_length_b                   14.745(3)
_cell_length_c                   14.745(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3206(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    650
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.375
_cell_measurement_theta_min      3.909
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.915
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            650
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.375
_diffrn_reflns_theta_min         3.909
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          
;
_cell_measurement_reflns_used      650
_cell_measurement_theta_max        27.375
_cell_measurement_theta_min        3.909
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                102
_reflns_number_total             165
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         165
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0412
_refine_ls_restrained_S_all      0.953
_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)+(0.0755P)²+3.0868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1251
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C3-C4 = C6-C5 = C1-C2
 1.52 with sigma of 0.02
 O2-N1
 1.37 with sigma of 0.02
 C2-C4 = C4-C6 = C6-C2 = C1-C3 = C3-C5 = C5-C1
 2.42 with sigma of 0.02
 O2-O1_$1
 2.45 with sigma of 0.01
 N2-C2 \\sim N2-C6 \\sim N2-C4 \\sim N1-C1 \\sim N1-C5 \\sim N1-C3
 with sigma of 0.01
 O2-C1 \\sim O2-C3 \\sim O2-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(O2) = Uiso(N1) = Uiso(N2) = Uiso(C1) = Uiso(C2) = Uiso(C3) = Uiso(C4) =
Uiso(C5) = Uiso(C6)
4. Others
 Fixed Sof: O2(0.04167) H2(0.04167) N1(0.04167) N2(0.04167) H2A(0.04167)
 C1(0.04167) H1A(0.04167) H1B(0.04167) C2(0.04167) H2B(0.04167) H2C(0.04167)
 C3(0.04167) H3A(0.04167) H3B(0.04167) C4(0.04167) H4A(0.04167) H4B(0.04167)
 C5(0.04167) H5A(0.04167) H5B(0.04167) C6(0.04167) H6A(0.04167) H6B(0.04167)
5.a Riding coordinates:
 N2(H2A), C1(H1A,H1B), C2(H2B,H2C), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
 C6(H6A,H6B)
5.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.5000 0.5000 0.5000 0.0533(9) Uani 1 24 d S T P . .
Cl1 Cl 0.5000 0.5000 0.2500 0.0618(9) Uani 1 8 d S T P . .
O1 O 0.4215(3) 0.5000 0.3069(3) 0.1006(16) Uani 1 2 d DS T P . .
O2 O 0.341(3) 0.6701(18) 0.3659(14) 0.049(6) Uiso 0.0417 1 d D U . A -1
H2 H 0.3045 0.6436 0.3984 0.073 Uiso 0.0417 1 calc R . . A -1
N1 N 0.296(5) 0.713(3) 0.297(2) 0.049(6) Uiso 0.0417 1 d D U . A -1
N2 N 0.200(4) 0.803(4) 0.170(3) 0.049(6) Uiso 0.0417 1 d D U . A -1
H2A H 0.1670 0.8356 0.1269 0.059 Uiso 0.0417 1 d R . . A -1
C1 C 0.302(7) 0.662(5) 0.208(2) 0.049(6) Uiso 0.0417 1 d D U . A -1
H1A H 0.2708 0.6046 0.2166 0.059 Uiso 0.0417 1 d R . . A -1
H1B H 0.3642 0.6495 0.1921 0.059 Uiso 0.0417 1 d R . . A -1
C2 C 0.251(4) 0.719(4) 0.139(4) 0.049(6) Uiso 0.0417 1 d D U . A -1
H2B H 0.2960 0.7416 0.0961 0.059 Uiso 0.0417 1 d R . . A -1
H2C H 0.2083 0.6811 0.1066 0.059 Uiso 0.0417 1 d R . . A -1
C3 C 0.332(7) 0.807(3) 0.278(5) 0.049(6) Uiso 0.0417 1 d D U . A -1
H3A H 0.3970 0.8008 0.2673 0.059 Uiso 0.0417 1 d R . . A -1
H3B H 0.3225 0.8470 0.3292 0.059 Uiso 0.0417 1 d R . . A -1
C4 C 0.269(4) 0.862(4) 0.217(4) 0.049(6) Uiso 0.0417 1 d D U . A -1
H4A H 0.2557 0.9260 0.2256 0.059 Uiso 0.0417 1 d R . . A -1
H4B H 0.3097 0.8568 0.1657 0.059 Uiso 0.0417 1 d R . . A -1
C5 C 0.195(4) 0.726(4) 0.315(6) 0.049(6) Uiso 0.0417 1 d D U . A -1
H5A H 0.1969 0.7705 0.3635 0.059 Uiso 0.0417 1 d R . . A -1
H5B H 0.1711 0.6697 0.3400 0.059 Uiso 0.0417 1 d R . . A -1
C6 C 0.136(4) 0.771(5) 0.244(4) 0.049(6) Uiso 0.0417 1 d D U . A -1
H6A H 0.0949 0.7231 0.2240 0.059 Uiso 0.0417 1 d R . . A -1
H6B H 0.0997 0.8225 0.2629 0.059 Uiso 0.0417 1 d R . . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O1 3.073(5) 105_666 ?
K1 O1 3.073(5) 2_665 ?
K1 O1 3.073(5) 10_656 ?
K1 O1 3.073(5) 9 ?
K1 O1 3.073(5) 6_566 ?
K1 O1 3.073(5) 101_666 ?
K1 O1 3.073(5) 98_556 ?
K1 O1 3.073(5) 5 ?
K1 O1 3.073(5) . ?
K1 O1 3.073(5) 97_666 ?
K1 O1 3.073(5) 106_565 ?
K1 O1 3.073(5) 102_655 ?
Cl1 K1 3.6863(9) 85_445 ?
Cl1 O1 1.430(4) 86 ?
Cl1 O1 1.430(4) . ?
Cl1 O1 1.430(4) 2_665 ?
Cl1 O1 1.430(4) 85_445 ?
O2 N1 1.37(2) . ?
N1 C1 1.518(15) . ?
N1 C3 1.517(15) . ?
N1 C5 1.518(15) . ?
N2 C2 1.518(15) . ?
N2 C4 1.517(15) . ?
N2 C6 1.519(15) . ?
C1 C2 1.52(2) . ?
C3 C4 1.52(2) . ?
C5 C6 1.53(2) . ?

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 O1 180.0 105_666 9 ?
O1 K1 O1 69.58(6) . 6_566 ?
O1 K1 O1 180.0 97_666 . ?
O1 K1 O1 69.57(6) 105_666 101_666 ?
O1 K1 O1 135.74(16) 97_666 2_665 ?
O1 K1 O1 110.43(6) 9 101_666 ?
O1 K1 O1 135.74(15) 101_666 6_566 ?
O1 K1 O1 110.43(6) 105_666 5 ?
O1 K1 O1 110.43(6) 105_666 2_665 ?
O1 K1 O1 69.57(6) 9 5 ?
O1 K1 O1 180.0 98_556 2_665 ?
O1 K1 O1 180.00(17) 101_666 5 ?
O1 K1 O1 135.74(16) 98_556 . ?
O1 K1 O1 69.57(6) 105_666 97_666 ?
O1 K1 O1 110.42(6) 10_656 6_566 ?
O1 K1 O1 110.43(6) 9 97_666 ?
O1 K1 O1 69.57(6) 10_656 98_556 ?
O1 K1 O1 69.57(6) 101_666 97_666 ?
O1 K1 O1 69.57(6) 101_666 2_665 ?
O1 K1 O1 110.43(6) 5 97_666 ?
O1 K1 O1 110.43(6) 10_656 2_665 ?
O1 K1 O1 44.26(15) 105_666 106_565 ?
O1 K1 O1 69.57(6) 9 . ?
O1 K1 O1 135.74(15) 9 106_565 ?
O1 K1 O1 110.43(6) 10_656 . ?
O1 K1 O1 69.57(6) 101_666 106_565 ?
O1 K1 O1 69.58(6) 105_666 6_566 ?
O1 K1 O1 110.43(6) 5 106_565 ?
O1 K1 O1 110.43(6) 97_666 6_566 ?
O1 K1 O1 110.43(6) 97_666 106_565 ?
O1 K1 O1 69.57(6) 98_556 6_566 ?
O1 K1 O1 135.74(15) 105_666 10_656 ?
O1 K1 O1 110.43(6) 106_565 98_556 ?
O1 K1 O1 44.26(15) 9 10_656 ?
O1 K1 O1 110.43(6) 102_655 98_556 ?
O1 K1 O1 110.43(6) 101_666 10_656 ?
O1 K1 O1 69.57(6) 9 2_665 ?
O1 K1 O1 69.57(6) 5 10_656 ?
O1 K1 O1 110.43(6) 5 2_665 ?
O1 K1 O1 69.57(6) 97_666 10_656 ?
O1 K1 O1 69.57(6) 106_565 2_665 ?
O1 K1 O1 180.0 106_565 10_656 ?
O1 K1 O1 69.57(6) 102_655 2_665 ?
O1 K1 O1 110.43(6) 105_666 102_655 ?
O1 K1 O1 110.43(6) 105_666 . ?
O1 K1 O1 69.57(6) 9 102_655 ?
O1 K1 O1 110.42(6) 101_666 . ?
O1 K1 O1 44.26(15) 101_666 102_655 ?
O1 K1 O1 69.57(6) 106_565 . ?
O1 K1 O1 135.74(15) 5 102_655 ?
O1 K1 O1 110.42(6) 102_655 . ?
O1 K1 O1 69.57(6) 97_666 102_655 ?
O1 K1 O1 44.26(15) 2_665 . ?
O1 K1 O1 110.43(6) 106_565 102_655 ?
O1 K1 O1 110.42(6) 9 6_566 ?
O1 K1 O1 69.57(6) 10_656 102_655 ?
O1 K1 O1 44.26(15) 5 6_566 ?
O1 K1 O1 69.57(6) 105_666 98_556 ?
O1 K1 O1 69.58(6) 106_565 6_566 ?
O1 K1 O1 110.43(6) 9 98_556 ?
O1 K1 O1 180.0 102_655 6_566 ?
O1 K1 O1 110.43(6) 101_666 98_556 ?
O1 K1 O1 110.43(6) 2_665 6_566 ?
O1 K1 O1 69.57(6) 5 98_556 ?
O1 K1 O1 44.26(15) 97_666 98_556 ?
O1 K1 O1 69.58(6) 5 . ?
K1 Cl1 K1 180.0 85_445 . ?
O1 Cl1 K1 54.1(2) 2_665 . ?
O1 Cl1 K1 125.9(2) . 85_445 ?
O1 Cl1 K1 54.1(2) . . ?
O1 Cl1 K1 125.9(2) 85_445 . ?
O1 Cl1 K1 125.9(2) 2_665 85_445 ?
O1 Cl1 K1 125.9(2) 86 . ?
O1 Cl1 K1 54.1(2) 86 85_445 ?
O1 Cl1 K1 54.1(2) 85_445 85_445 ?
O1 Cl1 O1 110.1(2) . 86 ?
O1 Cl1 O1 108.1(4) . 2_665 ?
O1 Cl1 O1 110.1(2) . 85_445 ?
O1 Cl1 O1 108.1(4) 85_445 86 ?
O1 Cl1 O1 110.2(2) 85_445 2_665 ?
O1 Cl1 O1 110.2(2) 2_665 86 ?
Cl1 O1 K1 103.8(2) . . ?
O2 N1 C1 112.5(16) . . ?
O2 N1 C3 113.1(16) . . ?
O2 N1 C5 113.5(17) . . ?
C3 N1 C1 105.8(19) . . ?
C3 N1 C5 105.6(19) . . ?
C5 N1 C1 105.7(19) . . ?
C2 N2 C6 105.9(19) . . ?
C4 N2 C2 105.7(19) . . ?
C4 N2 C6 105.6(19) . . ?
N1 C1 C2 106(4) . . ?
N2 C2 C1 120(5) . . ?
N1 C3 C4 112(5) . . ?
N2 C4 C3 112(5) . . ?
N1 C5 C6 119(6) . . ?
N2 C6 C5 106(6) . . ?

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
K1 Cl1 O1 K1 180.000(0) 85_445 . . . ?
O1 Cl1 O1 K1 0.000(0) 2_665 . . . ?
O1 Cl1 O1 K1 120.41(12) 85_445 . . . ?
O1 Cl1 O1 K1 -120.41(12) 86 . . . ?
O2 N1 C1 C2 -178(7) . . . . ?
O2 N1 C3 C4 -167(6) . . . . ?
O2 N1 C5 C6 -179(5) . . . . ?
N1 C1 C2 N2 -6(6) . . . . ?
N1 C3 C4 N2 -16(6) . . . . ?
N1 C5 C6 N2 -6(5) . . . . ?
C1 N1 C3 C4 70(6) . . . . ?
C1 N1 C5 C6 -55(5) . . . . ?
C2 N2 C4 C3 -42(7) . . . . ?
C2 N2 C6 C5 57(5) . . . . ?
C3 N1 C1 C2 -55(7) . . . . ?
C3 N1 C5 C6 57(6) . . . . ?
C4 N2 C2 C1 57(7) . . . . ?
C4 N2 C6 C5 -55(5) . . . . ?
C5 N1 C1 C2 57(7) . . . . ?
C5 N1 C3 C4 -42(7) . . . . ?
C6 N2 C2 C1 -55(7) . . . . ?
C6 N2 C4 C3 70(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_18072303
_audit_block_doi                 10.5517/ccdc.csd.cc20gf86
_database_code_depnum_ccdc_archive 'CCDC 1860907'
_audit_update_record             
;
2018-08-08 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_audit_creation_date             2018-07-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        PAP-1
_chemical_formula_moiety         'Cl3 Na O12, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Cl3 N2 Na O12'
_chemical_formula_weight         409.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         NHONaCl
_chemical_oxdiff_usercomment     PAP-1
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1521(2)
_cell_length_b                   9.7195(2)
_cell_length_c                   13.1621(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.900(2)
_cell_angle_gamma                90
_cell_volume                     1298.03(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4026
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      40.2570
_cell_measurement_theta_min      3.7390
_shelx_estimated_absorpt_T_max   0.923
_shelx_estimated_absorpt_T_min   0.842
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13462
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.173
_diffrn_reflns_theta_min         3.258
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5826
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00   4.00   1.00   14.35    --  -37.75  77.00  60.00   49
  2  ω     -4.00  79.00   1.00   14.35    --   38.69 -99.00 150.00   83
  3  ω     15.00 108.00   1.00   14.35    --   38.69  57.00 -60.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0457128000
_diffrn_orient_matrix_UB_12      0.0345291000
_diffrn_orient_matrix_UB_13      0.0306610000
_diffrn_orient_matrix_UB_21      0.0429096000
_diffrn_orient_matrix_UB_22      0.0575578000
_diffrn_orient_matrix_UB_23      0.0036808000
_diffrn_orient_matrix_UB_31      -0.0309455000
_diffrn_orient_matrix_UB_32      0.0286968000
_diffrn_orient_matrix_UB_33      -0.0441692000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5644
_reflns_number_total             8275
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     40.15
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         8275
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0505
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0532P)²+0.0699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1403
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl01 Cl 0.97100(3) 1.03448(3) 0.23385(2) 0.01873(7) Uani 1 1 d . . . . .
Cl02 Cl 0.48705(3) 0.53834(3) 0.23709(2) 0.01784(7) Uani 1 1 d . . . . .
Cl03 Cl 0.75805(3) 0.75469(3) 0.50435(2) 0.01872(7) Uani 1 1 d . . . . .
Na1 Na 0.74986(8) 0.76536(9) 0.25464(5) 0.03867(19) Uani 1 1 d . . . . .
O1 O 0.83500(13) 0.67894(14) 0.43443(10) 0.0368(3) Uani 1 1 d . . . . .
O2 O 0.67773(12) 0.85268(13) 0.44865(9) 0.0340(3) Uani 1 1 d . . . . .
O3 O 0.84482(13) 0.82489(13) 0.57537(10) 0.0399(3) Uani 1 1 d . . . . .
O4 O 0.67620(13) 0.66466(14) 0.56008(12) 0.0419(3) Uani 1 1 d . . . . .
O5 O 0.90419(13) 0.94663(12) 0.30315(10) 0.0349(3) Uani 1 1 d . . . . .
O6 O 0.92848(13) 1.00067(13) 0.13083(9) 0.0336(3) Uani 1 1 d . . . . .
O7 O 0.93932(12) 1.17541(11) 0.25461(10) 0.0319(3) Uani 1 1 d . . . . .
O8 O 1.11020(12) 1.01397(13) 0.24559(9) 0.0317(3) Uani 1 1 d . . . . .
O9 O 0.58007(15) 0.59670(14) 0.30875(12) 0.0479(4) Uani 1 1 d . . . . .
O10 O 0.51959(14) 0.57796(14) 0.13559(10) 0.0401(3) Uani 1 1 d . . . . .
O11 O 0.35872(14) 0.58697(17) 0.25726(12) 0.0475(4) Uani 1 1 d . . . . .
O12 O 0.49170(15) 0.39137(11) 0.24509(9) 0.0372(3) Uani 1 1 d . . . . .
N1 N 0.62026(12) 0.20520(14) 0.53851(10) 0.0243(2) Uani 1 1 d . . . . .
H1A H 0.5565 0.2101 0.5843 0.029 Uiso 1 1 calc R . . . .
H1B H 0.5942 0.1451 0.4899 0.029 Uiso 1 1 calc R . . . .
N2 N 0.87397(12) 0.29063(13) 0.46899(10) 0.0240(2) Uani 1 1 d . . . . .
H2A H 0.8993 0.3512 0.5175 0.029 Uiso 1 1 calc R . . . .
H2B H 0.9380 0.2860 0.4234 0.029 Uiso 1 1 calc R . . . .
C1 C 0.74476(14) 0.15541(15) 0.58941(11) 0.0223(3) Uani 1 1 d . . . . .
H1C H 0.7309 0.0629 0.6167 0.027 Uiso 1 1 calc R . . . .
H1D H 0.7688 0.2164 0.6463 0.027 Uiso 1 1 calc R . . . .
C2 C 0.85540(16) 0.15182(16) 0.51596(14) 0.0285(3) Uani 1 1 d . . . . .
H2C H 0.9371 0.1236 0.5518 0.034 Uiso 1 1 calc R . . . .
H2D H 0.8353 0.0841 0.4625 0.034 Uiso 1 1 calc R . . . .
C3 C 0.74909(15) 0.33927(16) 0.41740(12) 0.0249(3) Uani 1 1 d . . . . .
H3A H 0.7247 0.2769 0.3614 0.030 Uiso 1 1 calc R . . . .
H3B H 0.7625 0.4312 0.3889 0.030 Uiso 1 1 calc R . . . .
C4 C 0.63969(15) 0.34407(16) 0.49197(13) 0.0281(3) Uani 1 1 d . . . . .
H4A H 0.6615 0.4111 0.5455 0.034 Uiso 1 1 calc R . . . .
H4B H 0.5578 0.3736 0.4570 0.034 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
Cl01 O5 1.4360(12) . ?
Cl01 O6 1.4472(11) . ?
Cl01 O7 1.4353(11) . ?
Cl01 O8 1.4304(12) . ?
Cl02 O9 1.4298(13) . ?
Cl02 O10 1.4392(13) . ?
Cl02 O11 1.4192(14) . ?
Cl02 O12 1.4330(11) . ?
Cl03 Na1 3.2866(7) . ?
Cl03 Na1 3.3039(7) 4_576 ?
Cl03 O1 1.4307(12) . ?
Cl03 O2 1.4387(12) . ?
Cl03 O3 1.4355(11) . ?
Cl03 O4 1.4264(13) . ?
Na1 Cl03 3.3039(7) 4_575 ?
Na1 O1 2.6301(15) . ?
Na1 O2 2.8109(15) . ?
Na1 O3 2.7235(17) 4_575 ?
Na1 O4 2.7299(18) 4_575 ?
Na1 O5 2.4290(15) . ?
Na1 O8 2.8265(16) 2_745 ?
Na1 O9 2.4995(17) . ?
Na1 O12 2.7412(16) 2_655 ?
O3 Na1 2.7235(17) 4_576 ?
O4 Na1 2.7299(18) 4_576 ?
O8 Na1 2.8265(16) 2_755 ?
O12 Na1 2.7412(16) 2_645 ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 C1 1.4915(18) . ?
N1 C4 1.4979(19) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N2 C2 1.4986(19) . ?
N2 C3 1.4949(19) . ?
C1 H1C 0.9800 . ?
C1 H1D 0.9800 . ?
C1 C2 1.506(2) . ?
C2 H2C 0.9800 . ?
C2 H2D 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 C4 1.507(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Cl01 O6 109.12(8) . . ?
O7 Cl01 O5 109.45(8) . . ?
O7 Cl01 O6 109.47(7) . . ?
O8 Cl01 O5 109.53(8) . . ?
O8 Cl01 O6 109.42(7) . . ?
O8 Cl01 O7 109.83(8) . . ?
O9 Cl02 O10 109.83(9) . . ?
O9 Cl02 O12 109.12(8) . . ?
O11 Cl02 O9 109.56(10) . . ?
O11 Cl02 O10 108.96(9) . . ?
O11 Cl02 O12 110.27(9) . . ?
O12 Cl02 O10 109.08(8) . . ?
Na1 Cl03 Na1 176.71(3) . 4_576 ?
O1 Cl03 Na1 130.04(6) . 4_576 ?
O1 Cl03 Na1 50.90(6) . . ?
O1 Cl03 O2 108.99(8) . . ?
O1 Cl03 O3 109.09(8) . . ?
O2 Cl03 Na1 120.97(6) . 4_576 ?
O2 Cl03 Na1 58.29(6) . . ?
O3 Cl03 Na1 129.11(7) . . ?
O3 Cl03 Na1 54.12(7) . 4_576 ?
O3 Cl03 O2 110.02(8) . . ?
O4 Cl03 Na1 54.32(7) . 4_576 ?
O4 Cl03 Na1 122.53(7) . . ?
O4 Cl03 O1 110.78(9) . . ?
O4 Cl03 O2 109.76(8) . . ?
O4 Cl03 O3 108.19(9) . . ?
Cl03 Na1 Cl03 174.06(3) . 4_575 ?
O1 Na1 Cl03 149.31(4) . 4_575 ?
O1 Na1 Cl03 24.97(3) . . ?
O1 Na1 O2 50.71(4) . . ?
O1 Na1 O3 124.15(5) . 4_575 ?
O1 Na1 O4 174.40(5) . 4_575 ?
O1 Na1 O8 64.83(4) . 2_745 ?
O1 Na1 O12 114.13(4) . 2_655 ?
O2 Na1 Cl03 25.81(2) . . ?
O2 Na1 Cl03 159.98(4) . 4_575 ?
O2 Na1 O8 114.08(4) . 2_745 ?
O3 Na1 Cl03 25.28(3) 4_575 4_575 ?
O3 Na1 Cl03 149.12(4) 4_575 . ?
O3 Na1 O2 174.08(5) 4_575 . ?
O3 Na1 O4 50.31(4) 4_575 4_575 ?
O3 Na1 O8 61.85(4) 4_575 2_745 ?
O3 Na1 O12 119.18(4) 4_575 2_655 ?
O4 Na1 Cl03 25.11(3) 4_575 4_575 ?
O4 Na1 Cl03 160.56(4) 4_575 . ?
O4 Na1 O2 134.87(5) 4_575 . ?
O4 Na1 O8 109.66(4) 4_575 2_745 ?
O4 Na1 O12 70.90(4) 4_575 2_655 ?
O5 Na1 Cl03 105.52(4) . 4_575 ?
O5 Na1 Cl03 76.43(4) . . ?
O5 Na1 O1 78.77(5) . . ?
O5 Na1 O2 74.18(4) . . ?
O5 Na1 O3 102.57(5) . 4_575 ?
O5 Na1 O4 102.71(5) . 4_575 ?
O5 Na1 O8 107.90(5) . 2_745 ?
O5 Na1 O9 147.75(6) . . ?
O5 Na1 O12 104.17(5) . 2_655 ?
O8 Na1 Cl03 85.33(3) 2_745 4_575 ?
O8 Na1 Cl03 88.72(3) 2_745 . ?
O9 Na1 Cl03 71.89(4) . . ?
O9 Na1 Cl03 106.61(4) . 4_575 ?
O9 Na1 O1 75.13(5) . . ?
O9 Na1 O2 74.71(5) . . ?
O9 Na1 O3 107.63(5) . 4_575 ?
O9 Na1 O4 105.11(5) . 4_575 ?
O9 Na1 O8 77.57(5) . 2_745 ?
O9 Na1 O12 70.56(5) . 2_655 ?
O12 Na1 Cl03 94.58(3) 2_655 4_575 ?
O12 Na1 Cl03 90.33(3) 2_655 . ?
O12 Na1 O2 66.66(4) 2_655 . ?
O12 Na1 O8 146.72(5) 2_655 2_745 ?
Cl03 O1 Na1 104.13(7) . . ?
Cl03 O2 Na1 95.90(7) . . ?
Cl03 O3 Na1 100.59(8) . 4_576 ?
Cl03 O4 Na1 100.57(8) . 4_576 ?
Cl01 O5 Na1 125.34(8) . . ?
Cl01 O8 Na1 111.98(7) . 2_755 ?
Cl02 O9 Na1 121.26(9) . . ?
Cl02 O12 Na1 114.72(8) . 2_645 ?
H1A N1 H1B 108.1 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 C4 110.79(11) . . ?
C4 N1 H1A 109.5 . . ?
C4 N1 H1B 109.5 . . ?
H2A N2 H2B 108.1 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
C3 N2 H2A 109.5 . . ?
C3 N2 H2B 109.5 . . ?
C3 N2 C2 110.83(11) . . ?
N1 C1 H1C 109.4 . . ?
N1 C1 H1D 109.4 . . ?
N1 C1 C2 110.98(12) . . ?
H1C C1 H1D 108.0 . . ?
C2 C1 H1C 109.4 . . ?
C2 C1 H1D 109.4 . . ?
N2 C2 C1 110.52(12) . . ?
N2 C2 H2C 109.5 . . ?
N2 C2 H2D 109.5 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2C C2 H2D 108.1 . . ?
N2 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
N2 C3 C4 110.25(12) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
N1 C4 C3 110.38(13) . . ?
N1 C4 H4A 109.6 . . ?
N1 C4 H4B 109.6 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?

_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 1.718
_oxdiff_exptl_absorpt_empirical_full_min 0.696
####################################################################### 
# 
# 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_dap-o2
_database_code_depnum_ccdc_archive 'CCDC 1872410'
_audit_update_record             
;
2018-10-10 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_audit_creation_date             2018-10-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl3 K O12, C6 H14 N2 O'
_chemical_formula_sum            'C6 H14 Cl3 K N2 O13'
_chemical_formula_weight         467.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.6921(5)
_cell_length_b                   10.4526(4)
_cell_length_c                   10.0448(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.171(3)
_cell_angle_gamma                90
_cell_volume                     1542.26(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4150
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      34.2290
_cell_measurement_theta_min      3.9080
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.813
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13406
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.629
_diffrn_reflns_theta_min         3.390
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  Mo
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4466
_reflns_number_total             6075
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.191
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         6075
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0759
_refine_ls_restrained_S_all      1.086
_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)+(0.1091P)²+1.1589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2241
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B), C6(H6A,H6B), C5(H5A,H5B)
2.c Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.0000 0.5000 0.5000 0.0265(2) Uani 1 2 d S T P . .
Cl1 Cl -0.00309(5) 0.25391(7) 0.75533(7) 0.01949(16) Uani 1 1 d . . . . .
K2 K 0.5000 0.5000 0.5000 0.0323(3) Uani 1 2 d S T P . .
Cl3 Cl 0.51996(5) 0.75347(7) 0.24756(8) 0.02227(17) Uani 1 1 d . . . . .
Cl2 Cl 0.24348(5) 0.48671(7) 0.53222(8) 0.02108(17) Uani 1 1 d . . . . .
O3 O 0.01174(19) 0.2141(3) 0.6207(2) 0.0321(6) Uani 1 1 d . . . . .
O6 O 0.18309(18) 0.5671(2) 0.4551(3) 0.0309(5) Uani 1 1 d . . . . .
O2 O 0.07575(18) 0.2248(3) 0.8376(3) 0.0308(5) Uani 1 1 d . . . . .
O4 O -0.0195(2) 0.3897(2) 0.7569(3) 0.0344(6) Uani 1 1 d . . . . .
O8 O 0.31251(18) 0.4383(3) 0.4469(3) 0.0334(6) Uani 1 1 d . . . . .
O11 O 0.5131(2) 0.7330(3) 0.1048(3) 0.0406(7) Uani 1 1 d . . . . .
O1 O -0.08035(19) 0.1877(3) 0.8073(3) 0.0376(6) Uani 1 1 d . . . . .
O7 O 0.2842(2) 0.5560(3) 0.6404(3) 0.0404(7) Uani 1 1 d . . . . .
O5 O 0.1913(2) 0.3806(3) 0.5855(3) 0.0352(6) Uani 1 1 d . . . . .
O13 O 0.33679(19) 0.7044(2) 0.0126(3) 0.0357(6) Uani 1 1 d . . . . .
H13 H 0.3906 0.6902 0.0347 0.054 Uiso 1 1 calc GR . . . .
O12 O 0.5140(2) 0.8877(3) 0.2735(3) 0.0437(7) Uani 1 1 d . . . . .
O9 O 0.4472(2) 0.6871(3) 0.3092(3) 0.0415(7) Uani 1 1 d . . . . .
O10 O 0.6054(2) 0.7044(3) 0.2965(3) 0.0459(8) Uani 1 1 d . . . . .
N1 N 0.28658(18) 0.5901(2) 0.0194(3) 0.0199(5) Uani 1 1 d . . . . .
N2 N 0.19040(18) 0.3942(3) 0.0208(3) 0.0221(5) Uani 1 1 d . . . . .
H2 H 0.1521 0.3163 0.0218 0.027 Uiso 1 1 calc R . . . .
C1 C 0.3366(2) 0.4831(3) -0.0470(4) 0.0256(6) Uani 1 1 d . . . . .
H1A H 0.3887 0.4561 0.0086 0.031 Uiso 1 1 calc R . . . .
H1B H 0.3591 0.5114 -0.1333 0.031 Uiso 1 1 calc R . . . .
C2 C 0.2695(2) 0.3717(3) -0.0663(4) 0.0272(6) Uani 1 1 d . . . . .
H2A H 0.2491 0.3668 -0.1596 0.033 Uiso 1 1 calc R . . . .
H2B H 0.2992 0.2907 -0.0424 0.033 Uiso 1 1 calc R . . . .
C4 C 0.1345(2) 0.5041(3) -0.0311(4) 0.0265(7) Uani 1 1 d . . . . .
H4A H 0.0885 0.5280 0.0336 0.032 Uiso 1 1 calc R . . . .
H4B H 0.1033 0.4801 -0.1146 0.032 Uiso 1 1 calc R . . . .
C3 C 0.1994(2) 0.6167(3) -0.0546(4) 0.0254(6) Uani 1 1 d . . . . .
H3A H 0.2108 0.6258 -0.1500 0.030 Uiso 1 1 calc R . . . .
H3B H 0.1724 0.6964 -0.0226 0.030 Uiso 1 1 calc R . . . .
C6 C 0.2230(3) 0.4231(3) 0.1606(3) 0.0281(7) Uani 1 1 d . . . . .
H6A H 0.2673 0.3586 0.1904 0.034 Uiso 1 1 calc R . . . .
H6B H 0.1717 0.4221 0.2213 0.034 Uiso 1 1 calc R . . . .
C5 C 0.2673(2) 0.5558(3) 0.1602(3) 0.0273(7) Uani 1 1 d . . . . .
H5A H 0.2262 0.6189 0.1988 0.033 Uiso 1 1 calc R . . . .
H5B H 0.3240 0.5546 0.2133 0.033 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 O3 3.228(3) . ?
K1 O3 3.228(3) 3_566 ?
K1 O6 2.825(3) 3_566 ?
K1 O6 2.825(3) . ?
K1 O2 3.082(3) 4_565 ?
K1 O2 3.082(3) 2_556 ?
K1 O4 2.847(3) 3_566 ?
K1 O4 2.847(3) . ?
K1 O1 2.982(3) 2_556 ?
K1 O1 2.982(3) 4_565 ?
K1 O5 3.177(3) 3_566 ?
K1 O5 3.177(3) . ?
Cl1 K1 3.6168(7) 2_546 ?
Cl1 O3 1.436(2) . ?
Cl1 O2 1.441(2) . ?
Cl1 O4 1.440(3) . ?
Cl1 O1 1.437(3) . ?
K2 Cl3 3.5888(7) 4_576 ?
K2 Cl3 3.5888(7) 2_645 ?
K2 O8 2.869(3) 3_666 ?
K2 O8 2.869(3) . ?
K2 O11 2.987(3) 4_576 ?
K2 O11 2.987(3) 2_645 ?
K2 O12 2.991(3) 4_576 ?
K2 O12 2.991(3) 2_645 ?
K2 O9 2.836(3) . ?
K2 O9 2.836(3) 3_666 ?
K2 O10 3.357(4) . ?
K2 O10 3.357(4) 3_666 ?
Cl3 K2 3.5888(7) 2_655 ?
Cl3 O11 1.451(3) . ?
Cl3 O12 1.430(3) . ?
Cl3 O9 1.426(3) . ?
Cl3 O10 1.434(3) . ?
Cl2 O6 1.437(2) . ?
Cl2 O8 1.434(3) . ?
Cl2 O7 1.427(3) . ?
Cl2 O5 1.456(3) . ?
O2 K1 3.082(3) 2_546 ?
O11 K2 2.987(3) 2_655 ?
O1 K1 2.982(3) 2_546 ?
O13 H13 0.8300 . ?
O13 N1 1.406(3) . ?
O12 K2 2.991(3) 2_655 ?
N1 C1 1.502(4) . ?
N1 C3 1.494(4) . ?
N1 C5 1.491(4) . ?
N2 H2 0.9900 . ?
N2 C2 1.488(4) . ?
N2 C4 1.499(4) . ?
N2 C6 1.505(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 C2 1.536(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 C3 1.537(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 C5 1.532(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?

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 O3 180.0 3_566 . ?
O6 K1 O3 75.76(7) 3_566 . ?
O6 K1 O3 104.24(7) . . ?
O6 K1 O3 104.23(7) 3_566 3_566 ?
O6 K1 O3 75.76(7) . 3_566 ?
O6 K1 O6 180.0 3_566 . ?
O6 K1 O2 75.49(7) . 4_565 ?
O6 K1 O2 75.49(7) 3_566 2_556 ?
O6 K1 O2 104.51(7) . 2_556 ?
O6 K1 O2 104.51(7) 3_566 4_565 ?
O6 K1 O4 68.96(8) 3_566 . ?
O6 K1 O4 111.04(8) 3_566 3_566 ?
O6 K1 O4 111.04(8) . . ?
O6 K1 O4 68.96(8) . 3_566 ?
O6 K1 O1 115.17(8) 3_566 2_556 ?
O6 K1 O1 64.83(8) 3_566 4_565 ?
O6 K1 O1 115.17(8) . 4_565 ?
O6 K1 O1 64.83(8) . 2_556 ?
O6 K1 O5 45.62(7) 3_566 3_566 ?
O6 K1 O5 45.62(7) . . ?
O6 K1 O5 134.38(7) . 3_566 ?
O6 K1 O5 134.38(7) 3_566 . ?
O2 K1 O3 121.63(7) 2_556 . ?
O2 K1 O3 58.37(7) 4_565 . ?
O2 K1 O3 58.37(7) 2_556 3_566 ?
O2 K1 O3 121.63(7) 4_565 3_566 ?
O2 K1 O2 180.00(8) 4_565 2_556 ?
O2 K1 O5 61.09(7) 2_556 3_566 ?
O2 K1 O5 118.91(7) 2_556 . ?
O2 K1 O5 118.91(7) 4_565 3_566 ?
O2 K1 O5 61.09(7) 4_565 . ?
O4 K1 O3 44.78(7) 3_566 3_566 ?
O4 K1 O3 135.22(7) 3_566 . ?
O4 K1 O3 135.22(7) . 3_566 ?
O4 K1 O3 44.78(7) . . ?
O4 K1 O2 102.42(7) 3_566 2_556 ?
O4 K1 O2 77.58(7) . 2_556 ?
O4 K1 O2 77.58(7) 3_566 4_565 ?
O4 K1 O2 102.42(7) . 4_565 ?
O4 K1 O4 180.0 3_566 . ?
O4 K1 O1 73.98(8) 3_566 4_565 ?
O4 K1 O1 73.98(8) . 2_556 ?
O4 K1 O1 106.02(8) . 4_565 ?
O4 K1 O1 106.02(8) 3_566 2_556 ?
O4 K1 O5 72.59(8) . . ?
O4 K1 O5 107.42(8) 3_566 . ?
O4 K1 O5 107.41(8) . 3_566 ?
O4 K1 O5 72.58(8) 3_566 3_566 ?
O1 K1 O3 110.36(7) 4_565 3_566 ?
O1 K1 O3 110.36(7) 2_556 . ?
O1 K1 O3 69.64(7) 2_556 3_566 ?
O1 K1 O3 69.64(7) 4_565 . ?
O1 K1 O2 45.36(7) 4_565 4_565 ?
O1 K1 O2 134.64(7) 4_565 2_556 ?
O1 K1 O2 45.36(7) 2_556 2_556 ?
O1 K1 O2 134.64(7) 2_556 4_565 ?
O1 K1 O1 180.00(9) 4_565 2_556 ?
O1 K1 O5 75.32(7) 2_556 . ?
O1 K1 O5 104.68(7) 2_556 3_566 ?
O1 K1 O5 104.68(7) 4_565 . ?
O1 K1 O5 75.32(7) 4_565 3_566 ?
O5 K1 O3 120.35(7) 3_566 . ?
O5 K1 O3 59.65(7) 3_566 3_566 ?
O5 K1 O3 120.35(7) . 3_566 ?
O5 K1 O3 59.65(7) . . ?
O5 K1 O5 180.0 3_566 . ?
K1 Cl1 K1 177.43(2) 2_546 . ?
O3 Cl1 K1 62.36(12) . . ?
O3 Cl1 K1 115.30(13) . 2_546 ?
O3 Cl1 O2 110.08(16) . . ?
O3 Cl1 O4 108.96(17) . . ?
O3 Cl1 O1 109.81(17) . . ?
O2 Cl1 K1 57.10(12) . 2_546 ?
O2 Cl1 K1 122.18(12) . . ?
O4 Cl1 K1 135.68(12) . 2_546 ?
O4 Cl1 K1 46.73(12) . . ?
O4 Cl1 O2 109.54(16) . . ?
O1 Cl1 K1 128.24(13) . . ?
O1 Cl1 K1 53.03(12) . 2_546 ?
O1 Cl1 O2 108.75(17) . . ?
O1 Cl1 O4 109.68(19) . . ?
Cl3 K2 Cl3 180.0 4_576 2_645 ?
O8 K2 Cl3 69.21(6) 3_666 4_576 ?
O8 K2 Cl3 69.21(6) . 2_645 ?
O8 K2 Cl3 110.79(6) . 4_576 ?
O8 K2 Cl3 110.79(6) 3_666 2_645 ?
O8 K2 O8 180.0 . 3_666 ?
O8 K2 O11 109.30(9) . 4_576 ?
O8 K2 O11 70.70(9) 3_666 4_576 ?
O8 K2 O11 70.70(9) . 2_645 ?
O8 K2 O11 109.30(9) 3_666 2_645 ?
O8 K2 O12 72.14(9) . 2_645 ?
O8 K2 O12 107.86(9) . 4_576 ?
O8 K2 O12 107.86(9) 3_666 2_645 ?
O8 K2 O12 72.14(9) 3_666 4_576 ?
O8 K2 O10 61.11(7) . 3_666 ?
O8 K2 O10 118.89(7) . . ?
O8 K2 O10 61.11(7) 3_666 . ?
O8 K2 O10 118.89(7) 3_666 3_666 ?
O11 K2 Cl3 23.27(6) 2_645 2_645 ?
O11 K2 Cl3 23.27(6) 4_576 4_576 ?
O11 K2 Cl3 156.73(6) 2_645 4_576 ?
O11 K2 Cl3 156.73(6) 4_576 2_645 ?
O11 K2 O11 180.0 4_576 2_645 ?
O11 K2 O12 133.88(8) 4_576 2_645 ?
O11 K2 O12 133.88(8) 2_645 4_576 ?
O11 K2 O12 46.12(8) 4_576 4_576 ?
O11 K2 O12 46.12(8) 2_645 2_645 ?
O11 K2 O10 114.04(8) 4_576 3_666 ?
O11 K2 O10 65.96(8) 4_576 . ?
O11 K2 O10 114.04(8) 2_645 . ?
O11 K2 O10 65.96(8) 2_645 3_666 ?
O12 K2 Cl3 157.13(6) 2_645 4_576 ?
O12 K2 Cl3 22.87(6) 4_576 4_576 ?
O12 K2 Cl3 157.13(6) 4_576 2_645 ?
O12 K2 Cl3 22.87(6) 2_645 2_645 ?
O12 K2 O12 180.0 4_576 2_645 ?
O12 K2 O10 106.59(8) 2_645 3_666 ?
O12 K2 O10 73.41(8) 2_645 . ?
O12 K2 O10 73.41(8) 4_576 3_666 ?
O12 K2 O10 106.59(8) 4_576 . ?
O9 K2 Cl3 90.54(6) 3_666 4_576 ?
O9 K2 Cl3 90.54(6) . 2_645 ?
O9 K2 Cl3 89.46(6) . 4_576 ?
O9 K2 Cl3 89.46(6) 3_666 2_645 ?
O9 K2 O8 102.65(8) . 3_666 ?
O9 K2 O8 102.65(8) 3_666 . ?
O9 K2 O8 77.35(8) . . ?
O9 K2 O8 77.35(8) 3_666 3_666 ?
O9 K2 O11 66.98(8) . 4_576 ?
O9 K2 O11 66.98(8) 3_666 2_645 ?
O9 K2 O11 113.02(8) . 2_645 ?
O9 K2 O11 113.02(8) 3_666 4_576 ?
O9 K2 O12 111.29(8) . 4_576 ?
O9 K2 O12 68.71(8) 3_666 4_576 ?
O9 K2 O12 68.71(8) . 2_645 ?
O9 K2 O12 111.29(8) 3_666 2_645 ?
O9 K2 O9 180.0 3_666 . ?
O9 K2 O10 43.34(8) . . ?
O9 K2 O10 43.34(8) 3_666 3_666 ?
O9 K2 O10 136.66(8) 3_666 . ?
O9 K2 O10 136.66(8) . 3_666 ?
O10 K2 Cl3 86.13(6) . 4_576 ?
O10 K2 Cl3 93.87(6) 3_666 4_576 ?
O10 K2 Cl3 93.87(6) . 2_645 ?
O10 K2 Cl3 86.13(6) 3_666 2_645 ?
O10 K2 O10 180.0 . 3_666 ?
K2 Cl3 K2 170.75(2) 2_655 . ?
O11 Cl3 K2 124.71(14) . . ?
O11 Cl3 K2 54.42(13) . 2_655 ?
O12 Cl3 K2 125.05(14) . . ?
O12 Cl3 K2 54.36(14) . 2_655 ?
O12 Cl3 O11 108.74(19) . . ?
O12 Cl3 O10 110.2(2) . . ?
O9 Cl3 K2 126.76(14) . 2_655 ?
O9 Cl3 K2 43.98(14) . . ?
O9 Cl3 O11 108.65(19) . . ?
O9 Cl3 O12 110.4(2) . . ?
O9 Cl3 O10 109.6(2) . . ?
O10 Cl3 K2 123.57(15) . 2_655 ?
O10 Cl3 K2 65.68(15) . . ?
O10 Cl3 O11 109.2(2) . . ?
O6 Cl2 K1 47.56(11) . . ?
O6 Cl2 O5 108.60(17) . . ?
O8 Cl2 K1 132.53(12) . . ?
O8 Cl2 O6 108.72(17) . . ?
O8 Cl2 O5 109.59(17) . . ?
O7 Cl2 K1 116.79(15) . . ?
O7 Cl2 O6 111.01(18) . . ?
O7 Cl2 O8 110.11(19) . . ?
O7 Cl2 O5 108.78(18) . . ?
O5 Cl2 K1 62.03(12) . . ?
Cl1 O3 K1 94.43(14) . . ?
Cl2 O6 K1 110.40(14) . . ?
Cl1 O2 K1 99.77(13) . 2_546 ?
Cl1 O4 K1 111.67(15) . . ?
Cl2 O8 K2 119.85(15) . . ?
Cl3 O11 K2 102.32(16) . 2_655 ?
Cl1 O1 K1 104.33(15) . 2_546 ?
Cl2 O5 K1 94.09(13) . . ?
N1 O13 H13 109.5 . . ?
Cl3 O12 K2 102.77(16) . 2_655 ?
Cl3 O9 K2 115.57(18) . . ?
Cl3 O10 K2 91.42(16) . . ?
O13 N1 C1 110.4(3) . . ?
O13 N1 C3 105.3(2) . . ?
O13 N1 C5 111.1(2) . . ?
C3 N1 C1 109.8(3) . . ?
C5 N1 C1 110.2(3) . . ?
C5 N1 C3 109.8(3) . . ?
C2 N2 H2 109.0 . . ?
C2 N2 C4 110.3(3) . . ?
C2 N2 C6 110.0(3) . . ?
C4 N2 H2 109.0 . . ?
C4 N2 C6 109.4(3) . . ?
C6 N2 H2 109.0 . . ?
N1 C1 H1A 110.2 . . ?
N1 C1 H1B 110.2 . . ?
N1 C1 C2 107.6(3) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
N2 C2 C1 108.2(2) . . ?
N2 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2A 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N2 C4 H4A 110.2 . . ?
N2 C4 H4B 110.2 . . ?
N2 C4 C3 107.6(2) . . ?
H4A C4 H4B 108.5 . . ?
C3 C4 H4A 110.2 . . ?
C3 C4 H4B 110.2 . . ?
N1 C3 C4 108.0(2) . . ?
N1 C3 H3A 110.1 . . ?
N1 C3 H3B 110.1 . . ?
C4 C3 H3A 110.1 . . ?
C4 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
N2 C6 H6A 110.1 . . ?
N2 C6 H6B 110.1 . . ?
N2 C6 C5 107.8(2) . . ?
H6A C6 H6B 108.5 . . ?
C5 C6 H6A 110.1 . . ?
C5 C6 H6B 110.1 . . ?
N1 C5 C6 108.0(2) . . ?
N1 C5 H5A 110.1 . . ?
N1 C5 H5B 110.1 . . ?
C6 C5 H5A 110.1 . . ?
C6 C5 H5B 110.1 . . ?
H5A C5 H5B 108.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_CSL_Cu
_database_code_depnum_ccdc_archive 'CCDC 1872452'
_audit_update_record             
;
2018-10-10 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_audit_creation_date             2018-04-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r5381)
;
_chemical_formula_moiety         'Cl3 Na O12, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Cl3 N2 Na O12'
_chemical_formula_weight         409.49
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cl 0.36843 0.69943 11.46040 7.19640 6.25560 1.64550 0.01040 1.16620 18.51940
47.77840 -9.55739974976
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Na 0.13799 0.12245 4.76260 3.17360 1.26740 1.11280 3.28500 8.84220 0.31360
129.42400 0.675999999046
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   10.1689(4)
_cell_length_b                   9.7312(4)
_cell_length_c                   13.2985(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.993(4)
_cell_angle_gamma                90
_cell_volume                     1315.17(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.0990
_cell_measurement_theta_min      4.3390
_exptl_absorpt_coefficient_mu    7.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.0679
_exptl_crystal_description       block
_exptl_crystal_F_000             840.0138
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11329
_diffrn_reflns_theta_full        77.3376
_diffrn_reflns_theta_max         77.34
_diffrn_reflns_theta_min         4.35
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9742
_diffrn_measured_fraction_theta_max 0.9742
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  58.00   1.00   30.00    --  -32.00   0.00-180.00  127
  2  ω    -47.00  14.00   1.00   30.00    --  -32.00  72.00  36.00   61
  3  ω    -78.00 -18.00   1.00   30.00    --  -32.00 -72.00-180.00   60
  4  ω    -78.00 -18.00   1.00   30.00    --  -32.00 -72.00 108.00   60
  5  ω    -79.00  17.00   1.00   30.00    --  -32.00   0.00 108.00   96
  6  ω    -47.00  15.00   1.00   30.00    --  -32.00  72.00 108.00   62
  7  ω    -78.00 -18.00   1.00   30.00    --  -32.00 -72.00  36.00   60
  8  ω   -200.00 -20.00   1.00   80.00    -- -110.00   0.00-180.00  180
  9  ω   -125.00 -34.00   1.00   80.00    -- -110.00  72.00 108.00   91
 10  ω   -114.00 -35.00   1.00   80.00    -- -110.00  72.00-180.00   79
 11  ω   -104.00 -23.00   1.00   80.00    -- -110.00  72.00 -36.00   81
 12  ω   -200.00 -38.00   1.00   80.00    -- -110.00   0.00-108.00  162
 13  ω   -200.00-105.00   1.00   80.00    -- -110.00 -72.00 -36.00   95
 14  ω    -89.00 -23.00   1.00   80.00    -- -110.00  72.00  36.00   66
 15  ω   -125.00 -64.00   1.00   80.00    -- -110.00  72.00-108.00   61
 16  ω   -169.00-109.00   1.00   80.00    -- -110.00 -72.00-180.00   60
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1357929000
_diffrn_orient_matrix_UB_12      -0.0583044000
_diffrn_orient_matrix_UB_13      -0.0251896000
_diffrn_orient_matrix_UB_21      -0.0618640000
_diffrn_orient_matrix_UB_22      -0.1428638000
_diffrn_orient_matrix_UB_23      -0.0172088000
_diffrn_orient_matrix_UB_31      -0.0265235000
_diffrn_orient_matrix_UB_32      0.0351022000
_diffrn_orient_matrix_UB_33      -0.1119021000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2379
_reflns_number_total             2722
_reflns_odcompleteness_completeness 97.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.13
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.2025
_refine_diff_density_min         -0.6800
_refine_diff_density_rms         0.2511
_refine_ls_d_res_high            0.7901
_refine_ls_d_res_low             10.1627
_refine_ls_goodness_of_fit_ref   1.0292
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2722
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0731
_refine_ls_restrained_S_all      1.0292
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1743P)²+0.0644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2103
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N00F(H00a,H00b), N00G(H00c,H00d), C00J(H00e,H00f), C00K(H00g,H00h), C00L(H00i,
 H00j), C00M(H00k,H00l)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
Cl01 Cl 0.75715(5) 0.25512(6) 1.00413(4) 0.0323(3) Uani 1.000000 .
Cl02 Cl 0.97197(6) 0.53508(6) 0.73390(5) 0.0320(3) Uani 1.000000 .
Cl03 Cl 0.48768(6) 0.03869(7) 0.73769(5) 0.0312(3) Uani 1.000000 .
Na00 Na 0.75108(13) 0.2667(2) 0.75445(9) 0.0569(5) Uani 1.000000 .
O005 O 1.1112(2) 0.5142(3) 0.74540(17) 0.0503(6) Uani 1.000000 .
O006 O 0.8433(3) 0.3248(3) 1.0739(2) 0.0602(7) Uani 1.000000 .
O007 O 0.6768(2) 0.3525(3) 0.94931(18) 0.0540(6) Uani 1.000000 .
O008 O 0.9417(3) 0.6764(2) 0.7523(2) 0.0548(6) Uani 1.000000 .
O009 O 0.9294(3) 0.4992(3) 0.63280(18) 0.0570(7) Uani 1.000000 .
O00A O 0.9057(3) 0.4498(3) 0.8038(2) 0.0570(7) Uani 1.000000 .
O00B O 0.4892(3) -0.1071(2) 0.74557(19) 0.0613(7) Uani 1.000000 .
O00C O 0.8338(2) 0.1796(3) 0.93508(19) 0.0596(7) Uani 1.000000 .
O00D O 0.6760(3) 0.1647(3) 1.0592(2) 0.0642(8) Uani 1.000000 .
O00E O 0.5790(3) 0.0964(3) 0.8081(3) 0.0788(10) Uani 1.000000 .
N00F N 0.3781(2) 0.2048(3) 0.4633(2) 0.0427(6) Uani 1.000000 .
H00a H 0.4027(2) 0.1433(3) 0.5109(2) 0.0512(8) Uiso 1.000000 R
H00b H 0.4425(2) 0.2097(3) 0.4187(2) 0.0512(8) Uiso 1.000000 R
N00G N 0.1258(2) 0.2916(3) 0.5305(2) 0.0408(6) Uani 1.000000 .
H00c H 0.0609(2) 0.2870(3) 0.5747(2) 0.0490(8) Uiso 1.000000 R
H00d H 0.1020(2) 0.3532(3) 0.4827(2) 0.0490(8) Uiso 1.000000 R
O00H O 0.3600(3) 0.0894(4) 0.7563(3) 0.0810(10) Uani 1.000000 .
O00I O 0.5192(3) 0.0773(3) 0.6369(2) 0.0726(9) Uani 1.000000 .
C00J C 0.2547(3) 0.1576(3) 0.4113(2) 0.0392(7) Uani 1.000000 .
H00e H 0.2324(3) 0.2191(3) 0.3559(2) 0.0471(8) Uiso 1.000000 R
H00f H 0.2675(3) 0.0664(3) 0.3839(2) 0.0471(8) Uiso 1.000000 R
C00K C 0.2497(3) 0.3376(4) 0.5832(2) 0.0423(7) Uani 1.000000 .
H00g H 0.2371(3) 0.4282(4) 0.6117(2) 0.0507(9) Uiso 1.000000 R
H00h H 0.2720(3) 0.2748(4) 0.6379(2) 0.0507(9) Uiso 1.000000 R
C00L C 0.3606(3) 0.3420(4) 0.5109(3) 0.0481(8) Uani 1.000000 .
H00i H 0.4414(3) 0.3687(4) 0.5465(3) 0.0577(10) Uiso 1.000000 R
H00j H 0.3413(3) 0.4100(4) 0.4591(3) 0.0577(10) Uiso 1.000000 R
C00M C 0.1439(3) 0.1548(4) 0.4835(3) 0.0466(8) Uani 1.000000 .
H00k H 0.1630(3) 0.0872(4) 0.5356(3) 0.0559(9) Uiso 1.000000 R
H00l H 0.0632(3) 0.1278(4) 0.4479(3) 0.0559(9) Uiso 1.000000 R


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
Cl01 O006 1.426(2) . ?
Cl01 O007 1.433(2) . ?
Cl01 O00C 1.429(2) . ?
Cl01 O00D 1.426(2) . ?
Cl02 O005 1.433(2) . ?
Cl02 O008 1.432(2) . ?
Cl02 O009 1.441(2) . ?
Cl02 O00A 1.432(2) . ?
Cl03 O00B 1.422(3) . ?
Cl03 O00E 1.412(3) . ?
Cl03 O00H 1.419(3) . ?
Cl03 O00I 1.439(3) . ?
Na00 O006 2.755(3) 4_565 ?
Na00 O00A 2.451(3) . ?
Na00 O00B 2.735(3) 2_656 ?
Na00 O00C 2.656(3) . ?
Na00 O00D 2.763(3) 4_565 ?
Na00 O00E 2.530(4) . ?
N00F H00a 0.9000 . ?
N00F H00b 0.9000 . ?
N00F C00J 1.485(4) . ?
N00F C00L 1.491(4) . ?
N00G H00c 0.9000 . ?
N00G H00d 0.9000 . ?
N00G C00K 1.490(4) . ?
N00G C00M 1.484(4) . ?
C00J H00e 0.9700 . ?
C00J H00f 0.9700 . ?
C00J C00M 1.506(4) . ?
C00K H00g 0.9700 . ?
C00K H00h 0.9700 . ?
C00K C00L 1.508(4) . ?
C00L H00i 0.9700 . ?
C00L H00j 0.9700 . ?
C00M H00k 0.9700 . ?
C00M H00l 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
O007 Cl01 O006 110.06(16) . . ?
O00C Cl01 O006 109.05(16) . . ?
O00C Cl01 O007 109.10(16) . . ?
O00D Cl01 O006 108.22(18) . . ?
O00D Cl01 O007 109.82(15) . . ?
O00D Cl01 O00C 110.58(18) . . ?
O008 Cl02 O005 109.60(17) . . ?
O009 Cl02 O005 109.20(15) . . ?
O009 Cl02 O008 109.42(16) . . ?
O00A Cl02 O005 109.52(15) . . ?
O00A Cl02 O008 109.67(15) . . ?
O00A Cl02 O009 109.43(16) . . ?
O00E Cl03 O00B 110.05(16) . . ?
O00H Cl03 O00B 110.0(2) . . ?
O00H Cl03 O00E 109.3(2) . . ?
O00I Cl03 O00B 109.10(17) . . ?
O00I Cl03 O00E 110.5(2) . . ?
O00I Cl03 O00H 107.8(2) . . ?
O00A Na00 O006 103.52(9) . 4_565 ?
O00B Na00 O006 118.45(8) 2_656 4_565 ?
O00B Na00 O00A 103.77(11) 2_656 . ?
O00C Na00 O006 125.31(10) . 4_565 ?
O00C Na00 O00A 79.02(9) . . ?
O00C Na00 O00B 113.48(8) . 2_656 ?
O00D Na00 O006 49.51(7) 4_565 4_565 ?
O00D Na00 O00A 103.29(10) 4_565 . ?
O00D Na00 O00B 70.94(8) 4_565 2_656 ?
O00D Na00 O00C 174.57(11) 4_565 . ?
O00E Na00 O006 107.08(12) . 4_565 ?
O00E Na00 O00A 147.57(11) . . ?
O00E Na00 O00B 70.58(10) . 2_656 ?
O00E Na00 O00C 74.74(9) . . ?
O00E Na00 O00D 104.58(10) . 4_565 ?
Na00 O006 Cl01 101.14(15) 4_566 . ?
Na00 O00A Cl02 123.99(17) . . ?
Na00 O00B Cl03 116.14(18) 2_646 . ?
Na00 O00C Cl01 104.73(15) . . ?
Na00 O00D Cl01 100.81(16) 4_566 . ?
Na00 O00E Cl03 121.3(2) . . ?
H00b N00F H00a 108.0 . . ?
C00J N00F H00a 109.38(18) . . ?
C00J N00F H00b 109.38(15) . . ?
C00L N00F H00a 109.4(2) . . ?
C00L N00F H00b 109.38(18) . . ?
C00L N00F C00J 111.3(2) . . ?
H00d N00G H00c 108.1 . . ?
C00K N00G H00c 109.53(16) . . ?
C00K N00G H00d 109.53(18) . . ?
C00M N00G H00c 109.53(17) . . ?
C00M N00G H00d 109.53(19) . . ?
C00M N00G C00K 110.6(2) . . ?
H00e C00J N00F 109.59(18) . . ?
H00f C00J N00F 109.59(16) . . ?
H00f C00J H00e 108.1 . . ?
C00M C00J N00F 110.3(2) . . ?
C00M C00J H00e 109.6(2) . . ?
C00M C00J H00f 109.59(18) . . ?
H00g C00K N00G 109.60(17) . . ?
H00h C00K N00G 109.60(18) . . ?
H00h C00K H00g 108.1 . . ?
C00L C00K N00G 110.3(3) . . ?
C00L C00K H00g 109.60(19) . . ?
C00L C00K H00h 109.6(2) . . ?
C00K C00L N00F 110.4(3) . . ?
H00i C00L N00F 109.57(16) . . ?
H00i C00L C00K 109.57(17) . . ?
H00j C00L N00F 109.6(2) . . ?
H00j C00L C00K 109.6(2) . . ?
H00j C00L H00i 108.1 . . ?
C00J C00M N00G 111.0(3) . . ?
H00k C00M N00G 109.43(19) . . ?
H00k C00M C00J 109.4(2) . . ?
H00l C00M N00G 109.43(17) . . ?
H00l C00M C00J 109.43(17) . . ?
H00l C00M H00k 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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.769
_oxdiff_exptl_absorpt_empirical_full_min 0.212
