# Electronic Supplementary Material (ESI) for ChemComm.
# 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_f
_database_code_depnum_ccdc_archive 'CCDC 1841314'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_audit_creation_date             2018-05-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C2 H8 Cl6 K2 N4 O2 Zn2)'
_chemical_formula_sum            'C H4 Cl3 K N2 O Zn'
_chemical_formula_weight         270.88
_chemical_melting_point          408
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.8599(10)
_cell_length_b                   7.3530(12)
_cell_length_c                   8.4999(11)
_cell_angle_alpha                90
_cell_angle_beta                 99.069(13)
_cell_angle_gamma                90
_cell_volume                     423.38(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    429
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.2630
_cell_measurement_theta_min      3.5470
_shelx_estimated_absorpt_T_max   0.815
_shelx_estimated_absorpt_T_min   0.727
_exptl_absorpt_coefficient_mu    4.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (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    2.125
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1624
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.555
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  38.00   1.00  425.00    --  -16.36  77.00 -90.00   83
  2  ω     -1.00  33.00   1.00  425.00    --  -16.36  57.00-180.00   34
  3  ω    -87.00 -37.00   1.00  425.00    --  -16.36-178.00  30.00   50
  4  ω     47.00  84.00   1.00  425.00    --   17.61  57.00 -30.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0294094000
_diffrn_orient_matrix_UB_12      -0.0040676000
_diffrn_orient_matrix_UB_13      -0.0762608000
_diffrn_orient_matrix_UB_21      0.0498735000
_diffrn_orient_matrix_UB_22      -0.0830566000
_diffrn_orient_matrix_UB_23      0.0211099000
_diffrn_orient_matrix_UB_31      -0.0872836000
_diffrn_orient_matrix_UB_32      -0.0488824000
_diffrn_orient_matrix_UB_33      -0.0295743000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                559
_reflns_number_total             804
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         804
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      0.997
_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)+(0.0257P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1006
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) N2(0.5) H2A(0.5) H2B(0.5)
2.a Everything fixed:
 H1A, H1B, H2A, H2B
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_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
N1 N 0.6451(15) 0.8035(19) -0.0106(12) 0.044(6) Uani 0.5 1 d . . . A 1
H1A H 0.754550 0.835430 0.051490 0.050 Uiso 0.5 1 d . . . B 1
H1B H 0.648770 0.803570 -0.113110 0.050 Uiso 0.5 1 d . . . C 1
N2 N 0.3293(16) 0.695(2) -0.0445(12) 0.054(7) Uani 0.5 1 d . . . A 1
H2A H 0.221120 0.661290 -0.010940 0.050 Uiso 0.5 1 d . . . D 1
H2B H 0.322330 0.697080 -0.150530 0.050 Uiso 0.5 1 d . . . E 1
Zn1 Zn 0.26082(18) 0.750000 0.31180(14) 0.0358(4) Uani 1 2 d S T P . .
K1 K 0.7956(4) 0.750000 0.4560(3) 0.0577(9) Uani 1 2 d S T P . .
Cl2 Cl 0.0655(3) 0.5065(3) 0.2491(2) 0.0501(6) Uani 1 1 d . . . . .
Cl1 Cl 0.3876(5) 0.750000 0.5718(3) 0.0753(12) Uani 1 2 d S T P . .
O1 O 0.4903(9) 0.750000 0.2001(7) 0.0378(18) Uani 1 2 d S T P A .
C1 C 0.4854(15) 0.750000 0.0493(12) 0.031(3) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.045(7) 0.072(17) 0.021(5) -0.003(6) 0.016(5) -0.018(8)
N2 0.048(7) 0.09(2) 0.023(6) -0.018(7) 0.003(5) -0.021(9)
Zn1 0.0279(7) 0.0473(8) 0.0338(7) 0.000 0.0099(5) 0.000
K1 0.0364(15) 0.098(2) 0.0399(14) 0.000 0.0083(12) 0.000
Cl2 0.0480(13) 0.0464(13) 0.0564(13) -0.0039(11) 0.0099(10) -0.0118(12)
Cl1 0.0495(19) 0.148(4) 0.0305(15) 0.000 0.0110(14) 0.000
O1 0.027(4) 0.057(5) 0.031(4) 0.000 0.009(3) 0.000
C1 0.032(6) 0.029(6) 0.034(6) 0.000 0.009(5) 0.000

_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
N1 N1 0.79(3) 4_575 ?
N1 C1 1.338(13) . ?
N2 N2 0.81(3) 4_575 ?
N2 C1 1.294(14) . ?
Zn1 K1 3.680(3) . ?
Zn1 K1 3.594(3) 1_455 ?
Zn1 Cl2 2.249(2) 4_575 ?
Zn1 Cl2 2.249(2) . ?
Zn1 Cl1 2.244(3) . ?
Zn1 O1 1.963(6) . ?
K1 K1 4.613(3) 3_776 ?
K1 K1 4.613(3) 3_766 ?
K1 Cl2 3.279(3) 1_655 ?
K1 Cl2 3.162(3) 2_656 ?
K1 Cl2 3.279(3) 4_675 ?
K1 Cl2 3.162(3) 3_666 ?
K1 Cl1 3.110(4) . ?
K1 O1 2.771(7) . ?
O1 C1 1.277(11) . ?

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
N1 N1 C1 72.9(6) 4_575 . ?
N2 N2 C1 71.8(7) 4_575 . ?
K1 Zn1 K1 141.13(8) 1_455 . ?
Cl2 Zn1 K1 127.17(6) 4_575 . ?
Cl2 Zn1 K1 127.17(6) . . ?
Cl2 Zn1 K1 63.45(6) 4_575 1_455 ?
Cl2 Zn1 K1 63.45(6) . 1_455 ?
Cl2 Zn1 Cl2 105.48(12) 4_575 . ?
Cl1 Zn1 K1 57.36(9) . . ?
Cl1 Zn1 K1 83.77(9) . 1_455 ?
Cl1 Zn1 Cl2 110.94(7) . . ?
Cl1 Zn1 Cl2 110.94(7) . 4_575 ?
O1 Zn1 K1 171.1(2) . 1_455 ?
O1 Zn1 K1 47.73(19) . . ?
O1 Zn1 Cl2 112.25(11) . . ?
O1 Zn1 Cl2 112.25(11) . 4_575 ?
O1 Zn1 Cl1 105.1(2) . . ?
Zn1 K1 Zn1 141.13(8) 1_655 . ?
Zn1 K1 K1 127.06(5) . 3_766 ?
Zn1 K1 K1 60.37(5) 1_655 3_776 ?
Zn1 K1 K1 127.06(5) . 3_776 ?
Zn1 K1 K1 60.37(5) 1_655 3_766 ?
K1 K1 K1 105.70(10) 3_776 3_766 ?
Cl2 K1 Zn1 115.09(7) 3_666 . ?
Cl2 K1 Zn1 37.86(4) 1_655 1_655 ?
Cl2 K1 Zn1 95.60(7) 3_666 1_655 ?
Cl2 K1 Zn1 116.03(7) 4_675 . ?
Cl2 K1 Zn1 115.09(7) 2_656 . ?
Cl2 K1 Zn1 116.03(7) 1_655 . ?
Cl2 K1 Zn1 95.60(7) 2_656 1_655 ?
Cl2 K1 Zn1 37.86(4) 4_675 1_655 ?
Cl2 K1 K1 45.28(5) 2_656 3_776 ?
Cl2 K1 K1 45.28(5) 3_666 3_766 ?
Cl2 K1 K1 43.26(5) 1_655 3_766 ?
Cl2 K1 K1 104.32(9) 3_666 3_776 ?
Cl2 K1 K1 98.17(8) 4_675 3_766 ?
Cl2 K1 K1 43.26(5) 4_675 3_776 ?
Cl2 K1 K1 98.17(8) 1_655 3_776 ?
Cl2 K1 K1 104.32(9) 2_656 3_766 ?
Cl2 K1 Cl2 88.54(6) 3_666 1_655 ?
Cl2 K1 Cl2 128.75(8) 2_656 1_655 ?
Cl2 K1 Cl2 128.75(8) 3_666 4_675 ?
Cl2 K1 Cl2 73.24(9) 2_656 3_666 ?
Cl2 K1 Cl2 88.54(6) 2_656 4_675 ?
Cl2 K1 Cl2 66.19(8) 4_675 1_655 ?
Cl1 K1 Zn1 178.54(10) . 1_655 ?
Cl1 K1 Zn1 37.41(6) . . ?
Cl1 K1 K1 120.20(6) . 3_776 ?
Cl1 K1 K1 120.20(6) . 3_766 ?
Cl1 K1 Cl2 85.57(8) . 2_656 ?
Cl1 K1 Cl2 85.57(8) . 3_666 ?
Cl1 K1 Cl2 141.46(6) . 4_675 ?
Cl1 K1 Cl2 141.46(6) . 1_655 ?
O1 K1 Zn1 109.52(14) . 1_655 ?
O1 K1 Zn1 31.60(13) . . ?
O1 K1 K1 119.48(8) . 3_776 ?
O1 K1 K1 119.48(8) . 3_766 ?
O1 K1 Cl2 135.91(9) . 2_656 ?
O1 K1 Cl2 89.99(12) . 4_675 ?
O1 K1 Cl2 135.91(9) . 3_666 ?
O1 K1 Cl2 89.99(12) . 1_655 ?
O1 K1 Cl1 69.02(15) . . ?
Zn1 Cl2 K1 78.69(7) . 1_455 ?
Zn1 Cl2 K1 101.13(8) . 3_666 ?
K1 Cl2 K1 91.46(6) 3_666 1_455 ?
Zn1 Cl1 K1 85.23(10) . . ?
Zn1 O1 K1 100.7(2) . . ?
C1 O1 Zn1 126.1(7) . . ?
C1 O1 K1 133.2(6) . . ?
N1 C1 N1 34.2(12) . 4_575 ?
N2 C1 N1 108.8(9) . 4_575 ?
N2 C1 N1 120.3(10) 4_575 4_575 ?
N2 C1 N1 120.3(10) . . ?
N2 C1 N1 108.8(9) 4_575 . ?
N2 C1 N2 36.3(15) 4_575 . ?
O1 C1 N1 119.2(10) . 4_575 ?
O1 C1 N1 119.2(10) . . ?
O1 C1 N2 120.4(10) . . ?
O1 C1 N2 120.4(10) . 4_575 ?

_shelx_res_file                  
;
TITL urea_zncl2_kcl_1-1-2_a.res in P2(1)/m
    f.res
    created by SHELXL-2018/1 at 13:24:31 on 03-May-2018
rem ACTA
CELL 0.71073 6.8599 7.353 8.4999 90 99.069 90
ZERR 2 0.001 0.0012 0.0011 0 0.013 0
LATT 1
SYMM -X,0.5+Y,-Z
SFAC C H Cl K N O Zn
UNIT 2 8 6 2 4 2 2

L.S. 24
PLAN  20
SIZE 0.05 0.07 0.08
LIST 6
fmap 2
ACTA
MERG 2
REM <olex2.extras>
REM <HklSrc "%.\\filtered.hkl">
REM </olex2.extras>

WGHT    0.025700
FVAR       0.97593
PART 1
N1    5    0.645077    0.803469   -0.010556    10.50000    0.04472    0.07166 =
         0.02057   -0.00304    0.01633   -0.01787
AFIX   1
H1A   2    0.754550    0.835430    0.051490    10.50000    0.05000
AFIX   1
H1B   2    0.648770    0.803570   -0.113110    10.50000    0.05000
AFIX   0
N2    5    0.329319    0.695125   -0.044482    10.50000    0.04798    0.09115 =
         0.02339   -0.01823    0.00345   -0.02120
AFIX   1
H2A   2    0.221120    0.661290   -0.010940    10.50000    0.05000
AFIX   1
H2B   2    0.322330    0.697080   -0.150530    10.50000    0.05000
AFIX   0
PART 0
ZN1   7    0.260822    0.750000    0.311803    10.50000    0.02787    0.04731 =
         0.03376    0.00000    0.00994    0.00000
K1    4    0.795625    0.750000    0.455971    10.50000    0.03635    0.09761 =
         0.03985    0.00000    0.00832    0.00000
CL2   3    0.065494    0.506514    0.249080    11.00000    0.04803    0.04637 =
         0.05637   -0.00388    0.00993   -0.01178
CL1   3    0.387643    0.750000    0.571780    10.50000    0.04946    0.14752 =
         0.03046    0.00000    0.01102    0.00000
O1    6    0.490341    0.750000    0.200114    10.50000    0.02688    0.05679 =
         0.03091    0.00000    0.00855    0.00000
C1    1    0.485374    0.750000    0.049278    10.50000    0.03150    0.02917 =
         0.03363    0.00000    0.00902    0.00000
HKLF 4




REM  urea_zncl2_kcl_1-1-2_a.res in P2(1)/m
REM R1 =  0.0589 for     559 Fo > 4sig(Fo)  and  0.0983 for all     804 data
REM     58 parameters refined using      0 restraints

END

WGHT      0.0259      0.0000

REM Highest difference peak  0.749,  deepest hole -0.440,  1-sigma level  0.125
Q1    1   0.6825  0.7500  0.3200  10.50000  0.05    0.71
Q2    1   0.2164  0.7500  0.4435  10.50000  0.05    0.62
Q3    1   0.3433  0.7500  0.4396  10.50000  0.05    0.62
Q4    1   0.8444  0.7500  0.3143  10.50000  0.05    0.57
Q5    1   0.0918  0.7500  0.3293  10.50000  0.05    0.54
Q6    1   0.4213  0.7500  0.2862  10.50000  0.05    0.53
Q7    1   0.7432  0.7500  0.5872  10.50000  0.05    0.49
Q8    1   0.3492  0.7500  0.1942  10.50000  0.05    0.44
Q9    1   0.9796  0.7500  0.1799  10.50000  0.05    0.43
Q10   1   0.1113  0.5364  0.3568  11.00000  0.05    0.42
Q11   1   0.1882  0.5909  0.3315  11.00000  0.05    0.42
Q12   1   0.2396  0.4746  0.2486  11.00000  0.05    0.41
Q13   1   0.5172  0.7500  0.7159  10.50000  0.05    0.38
Q14   1   0.1971  0.7500  0.1839  10.50000  0.05    0.38
Q15   1   0.9911  0.7500  0.5827  10.50000  0.05    0.37
Q16   1   0.2341  0.7500 -0.1042  10.50000  0.05    0.34
Q17   1   0.4584  0.9986  0.2601  11.00000  0.05    0.34
Q18   1   0.0766  0.6639  0.0977  11.00000  0.05    0.33
Q19   1   0.2902  0.8351  0.2050  11.00000  0.05    0.33
Q20   1   0.5104  0.8092  0.1747  11.00000  0.05    0.32
;
_shelx_res_checksum              63154
_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 1.086
_oxdiff_exptl_absorpt_empirical_full_min 0.953
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# 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_twin_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1841315'
_audit_update_record             
;
2018-05-03 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_audit_creation_date             2018-05-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H4 Cl3 K N2 O Zn'
_chemical_formula_sum            'C H4 Cl3 K N2 O Zn'
_chemical_formula_weight         270.88
_chemical_melting_point          415
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.4220(6)
_cell_length_b                   13.5530(10)
_cell_length_c                   8.4219(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.089(7)
_cell_angle_gamma                90
_cell_volume                     846.60(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2604
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8330
_cell_measurement_theta_min      5.5000
_shelx_estimated_absorpt_T_max   0.883
_shelx_estimated_absorpt_T_min   0.567
_exptl_absorpt_coefficient_mu    4.266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (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    2.125
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.894
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9911
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.442
_diffrn_reflns_theta_min         3.595
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00  -5.00   1.00   32.50    --  -16.52 137.00 -37.74   74
  2  ω    -16.00  20.00   1.00   32.50    --  -16.52 -99.00 -30.00   36
  3  ω    -68.00   5.00   1.00   32.50    --  -16.52 119.00  64.63   73
  4  ω    -34.00  52.00   1.00   32.50    --  -16.52  57.00-150.00   86
  5  ω    -85.00 -23.00   1.00   32.50    --  -16.52 -57.00  60.00   62
  6  ω    -85.00   1.00   1.00   32.50    --  -16.52 -77.00 150.00   86
  7  ω     -2.00  88.00   1.00   32.50    --   17.61  38.00   0.00   90
  8  ω    -17.00  58.00   1.00   32.50    --   17.61 -99.00 -60.00   75
  9  ω     -5.00  87.00   1.00   32.50    --   17.61  38.00 -90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0948538000
_diffrn_orient_matrix_UB_12      0.0065162000
_diffrn_orient_matrix_UB_13      -0.0006657000
_diffrn_orient_matrix_UB_21      -0.0008890000
_diffrn_orient_matrix_UB_22      -0.0152711000
_diffrn_orient_matrix_UB_23      0.0805309000
_diffrn_orient_matrix_UB_31      0.0121682000
_diffrn_orient_matrix_UB_32      0.0496333000
_diffrn_orient_matrix_UB_33      0.0248179000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1326
_reflns_number_total             1867
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1867
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      0.600
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0920
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2.a X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.73751(5) 0.37606(3) 0.64056(5) 0.02937(15) Uani 1 1 d . . . . .
K1 K 0.80695(10) 0.64768(6) 0.57787(10) 0.0373(2) Uani 1 1 d . . . . .
Cl1 Cl 0.96790(10) 0.27233(7) 0.70815(11) 0.0382(2) Uani 1 1 d . . . . .
Cl2 Cl 0.48147(10) 0.29626(6) 0.69108(11) 0.0380(2) Uani 1 1 d . . . . .
Cl3 Cl 0.76712(14) 0.44577(8) 0.40239(11) 0.0485(3) Uani 1 1 d . . . . .
O1 O 0.7568(3) 0.49365(17) 0.7854(3) 0.0333(5) Uani 1 1 d . . . . .
N1 N 0.8161(4) 0.4124(3) 1.0158(4) 0.0457(8) Uani 1 1 d . . . . .
H1A H 0.857198 0.362389 0.965675 0.055 Uiso 1 1 calc R . . . .
H1B H 0.814142 0.411626 1.117804 0.055 Uiso 1 1 calc R . . . .
N2 N 0.6965(4) 0.5680(3) 1.0142(4) 0.0492(8) Uani 1 1 d . . . . .
H2A H 0.659631 0.619628 0.963235 0.059 Uiso 1 1 calc R . . . .
H2B H 0.695123 0.566713 1.116211 0.059 Uiso 1 1 calc R . . . .
C1 C 0.7555(4) 0.4907(3) 0.9356(4) 0.0308(7) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0384(2) 0.0263(2) 0.0234(2) 0.00016(16) 0.00150(14) -0.00025(14)
K1 0.0500(4) 0.0318(4) 0.0302(5) -0.0007(3) 0.0037(3) 0.0002(3)
Cl1 0.0363(4) 0.0383(5) 0.0404(5) 0.0065(4) 0.0061(3) 0.0067(3)
Cl2 0.0334(4) 0.0393(5) 0.0412(6) 0.0023(4) -0.0013(3) -0.0033(3)
Cl3 0.0878(7) 0.0377(5) 0.0200(5) 0.0002(4) 0.0032(4) 0.0028(4)
O1 0.0527(14) 0.0263(13) 0.0209(13) 0.0005(10) 0.0022(9) 0.0006(9)
N1 0.070(2) 0.047(2) 0.0203(17) 0.0035(15) -0.0010(13) 0.0111(15)
N2 0.071(2) 0.046(2) 0.031(2) -0.0088(16) 0.0092(14) 0.0131(15)
C1 0.0357(16) 0.0336(19) 0.0231(18) -0.0029(15) 0.0021(12) -0.0046(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 K1 3.7572(9) . ?
Zn1 K1 3.9203(9) 2_646 ?
Zn1 K1 3.9208(9) 3_766 ?
Zn1 Cl1 2.2701(9) . ?
Zn1 Cl2 2.2407(9) . ?
Zn1 Cl3 2.2353(11) . ?
Zn1 O1 2.009(2) . ?
K1 Cl1 3.1723(11) 3_766 ?
K1 Cl1 3.2452(11) 2_656 ?
K1 Cl2 3.1522(12) 3_666 ?
K1 Cl2 3.1756(12) 2_656 ?
K1 Cl3 3.1190(13) . ?
K1 Cl3 3.4040(13) 3_766 ?
K1 O1 2.757(2) . ?
O1 C1 1.266(4) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.328(5) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C1 1.322(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
K1 Zn1 K1 83.651(19) . 3_766 ?
K1 Zn1 K1 108.183(17) 2_646 3_766 ?
K1 Zn1 K1 150.877(14) . 2_646 ?
Cl1 Zn1 K1 54.00(3) . 3_766 ?
Cl1 Zn1 K1 55.85(2) . 2_646 ?
Cl1 Zn1 K1 122.42(3) . . ?
Cl2 Zn1 K1 143.25(3) . 3_766 ?
Cl2 Zn1 K1 128.41(3) . . ?
Cl2 Zn1 K1 54.09(3) . 2_646 ?
Cl2 Zn1 Cl1 106.85(3) . . ?
Cl3 Zn1 K1 59.93(3) . 3_766 ?
Cl3 Zn1 K1 56.03(3) . . ?
Cl3 Zn1 K1 152.84(3) . 2_646 ?
Cl3 Zn1 Cl1 112.89(4) . . ?
Cl3 Zn1 Cl2 119.09(4) . . ?
O1 Zn1 K1 45.64(7) . . ?
O1 Zn1 K1 107.84(7) . 3_766 ?
O1 Zn1 K1 105.35(7) . 2_646 ?
O1 Zn1 Cl1 107.62(7) . . ?
O1 Zn1 Cl2 108.05(7) . . ?
O1 Zn1 Cl3 101.68(7) . . ?
Zn1 K1 Zn1 96.349(19) . 3_766 ?
Zn1 K1 Zn1 116.21(2) 2_656 3_766 ?
Zn1 K1 Zn1 132.34(2) . 2_656 ?
Cl1 K1 Zn1 104.35(3) 3_766 2_656 ?
Cl1 K1 Zn1 121.35(3) 3_766 . ?
Cl1 K1 Zn1 35.376(17) 2_656 2_656 ?
Cl1 K1 Zn1 150.88(3) 2_656 3_766 ?
Cl1 K1 Zn1 35.378(17) 3_766 3_766 ?
Cl1 K1 Zn1 109.86(3) 2_656 . ?
Cl1 K1 Cl1 127.08(3) 3_766 2_656 ?
Cl1 K1 Cl2 89.21(3) 3_766 2_656 ?
Cl1 K1 Cl3 140.18(4) 2_656 3_766 ?
Cl1 K1 Cl3 69.53(3) 3_766 3_766 ?
Cl2 K1 Zn1 127.05(3) 2_656 . ?
Cl2 K1 Zn1 34.852(17) 2_656 2_656 ?
Cl2 K1 Zn1 85.64(2) 2_656 3_766 ?
Cl2 K1 Zn1 104.91(3) 3_666 3_766 ?
Cl2 K1 Zn1 104.13(3) 3_666 . ?
Cl2 K1 Zn1 100.04(3) 3_666 2_656 ?
Cl2 K1 Cl1 68.68(3) 2_656 2_656 ?
Cl2 K1 Cl1 74.62(3) 3_666 3_766 ?
Cl2 K1 Cl1 81.34(3) 3_666 2_656 ?
Cl2 K1 Cl2 126.52(3) 3_666 2_656 ?
Cl2 K1 Cl3 136.88(3) 3_666 3_766 ?
Cl2 K1 Cl3 76.61(3) 2_656 3_766 ?
Cl3 K1 Zn1 76.95(3) . 3_766 ?
Cl3 K1 Zn1 36.47(2) . . ?
Cl3 K1 Zn1 111.27(3) 3_766 2_656 ?
Cl3 K1 Zn1 34.634(18) 3_766 3_766 ?
Cl3 K1 Zn1 166.09(3) . 2_656 ?
Cl3 K1 Zn1 76.14(2) 3_766 . ?
Cl3 K1 Cl1 132.01(3) . 2_656 ?
Cl3 K1 Cl1 89.05(3) . 3_766 ?
Cl3 K1 Cl2 152.00(4) . 2_656 ?
Cl3 K1 Cl2 79.68(3) . 3_666 ?
Cl3 K1 Cl3 76.62(3) . 3_766 ?
O1 K1 Zn1 111.96(5) . 3_766 ?
O1 K1 Zn1 31.40(5) . . ?
O1 K1 Zn1 101.43(5) . 2_656 ?
O1 K1 Cl1 145.82(6) . 3_766 ?
O1 K1 Cl1 86.56(5) . 2_656 ?
O1 K1 Cl2 122.30(6) . 3_666 ?
O1 K1 Cl2 99.61(6) . 2_656 ?
O1 K1 Cl3 67.87(5) . . ?
O1 K1 Cl3 80.43(5) . 3_766 ?
Zn1 Cl1 K1 88.77(3) . 2_646 ?
Zn1 Cl1 K1 90.62(3) . 3_766 ?
K1 Cl1 K1 163.49(4) 3_766 2_646 ?
Zn1 Cl2 K1 91.06(3) . 2_646 ?
Zn1 Cl2 K1 107.80(4) . 3_666 ?
K1 Cl2 K1 154.26(3) 3_666 2_646 ?
Zn1 Cl3 K1 85.43(3) . 3_766 ?
Zn1 Cl3 K1 87.50(4) . . ?
K1 Cl3 K1 103.39(3) . 3_766 ?
Zn1 O1 K1 102.95(9) . . ?
C1 O1 Zn1 125.4(2) . . ?
C1 O1 K1 131.6(2) . . ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
O1 C1 N1 121.2(3) . . ?
O1 C1 N2 119.3(3) . . ?
N2 C1 N1 119.4(3) . . ?

_shelx_res_file                  
;
TITL twin_twin1_hklf4_a.res in P2(1)/n
    twin_twin1_hklf4.res
    created by SHELXL-2018/1 at 11:32:17 on 03-May-2018
REM Old TITL twin_twin1_hklf4 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.116, Rweak 0.011, Alpha 0.023, Orientation as input
REM Formula found by SHELXT: C3 O Zn Cl4
CELL 0.71073 7.422 13.553 8.4219 90 92.089 90
ZERR 4 0.0006 0.001 0.0005 0 0.007 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N O Zn K Cl
UNIT 4 16 8 4 4 4 12

L.S. 24
PLAN  20
SIZE 0.15 0.08 0.03
BOND $H
list 4
fmap 2 53
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\twin_twin1_hklf4.hkl">
REM </olex2.extras>

WGHT    0.100000
FVAR       0.49245
ZN1   5    0.737508    0.376058    0.640563    11.00000    0.03836    0.02634 =
         0.02343    0.00016    0.00150   -0.00025
K1    6    0.806954    0.647683    0.577869    11.00000    0.05002    0.03175 =
         0.03022   -0.00073    0.00367    0.00017
CL1   7    0.967903    0.272327    0.708148    11.00000    0.03628    0.03835 =
         0.04036    0.00647    0.00606    0.00669
CL2   7    0.481469    0.296263    0.691081    11.00000    0.03344    0.03932 =
         0.04117    0.00234   -0.00132   -0.00328
CL3   7    0.767115    0.445773    0.402389    11.00000    0.08776    0.03774 =
         0.01998    0.00016    0.00325    0.00279
O1    4    0.756821    0.493648    0.785395    11.00000    0.05270    0.02626 =
         0.02095    0.00047    0.00216    0.00057
N1    3    0.816053    0.412374    1.015772    11.00000    0.06997    0.04673 =
         0.02026    0.00350   -0.00101    0.01109
AFIX  93
H1A   2    0.857198    0.362389    0.965675    11.00000   -1.20000
H1B   2    0.814142    0.411626    1.117804    11.00000   -1.20000
AFIX   0
N2    3    0.696542    0.568026    1.014172    11.00000    0.07096    0.04583 =
         0.03148   -0.00880    0.00917    0.01307
AFIX  93
H2A   2    0.659631    0.619628    0.963235    11.00000   -1.20000
H2B   2    0.695123    0.566713    1.116211    11.00000   -1.20000
AFIX   0
C1    1    0.755481    0.490700    0.935591    11.00000    0.03573    0.03358 =
         0.02308   -0.00294    0.00210   -0.00457
HKLF 4




REM  twin_twin1_hklf4_a.res in P2(1)/n
REM R1 =  0.0305 for    1326 Fo > 4sig(Fo)  and  0.0523 for all    1867 data
REM     82 parameters refined using      0 restraints

END

WGHT      0.0302      0.0000

REM Highest difference peak  0.785,  deepest hole -0.375,  1-sigma level  0.088
Q1    1   0.6541  0.4564  0.4024  11.00000  0.05    0.79
Q2    1   0.6065  0.3784  0.6513  11.00000  0.05    0.60
Q3    1   0.7000  0.6432  0.5805  11.00000  0.05    0.48
Q4    1   0.8569  0.3764  0.6172  11.00000  0.05    0.44
Q5    1   0.9452  0.2611  0.6132  11.00000  0.05    0.40
Q6    1   0.4999  0.3627  0.6782  11.00000  0.05    0.39
Q7    1   0.7297  0.4449  0.5171  11.00000  0.05    0.34
Q8    1   0.4043  0.3810  0.6967  11.00000  0.05    0.34
Q9    1   0.9321  0.3752  0.6042  11.00000  0.05    0.33
Q10   1   0.6617  0.4577  0.6611  11.00000  0.05    0.32
Q11   1   0.5778  0.2450  0.6666  11.00000  0.05    0.30
Q12   1   0.6886  0.5120  0.4373  11.00000  0.05    0.28
Q13   1   0.6110  0.3045  0.7450  11.00000  0.05    0.28
Q14   1   0.9360  0.3831  0.9360  11.00000  0.05    0.27
Q15   1   0.7756  0.4546  0.6473  11.00000  0.05    0.27
Q16   1   0.6690  0.4979  0.8176  11.00000  0.05    0.25
Q17   1   0.9260  0.6227  0.4243  11.00000  0.05    0.25
Q18   1   0.7256  0.3168  0.6286  11.00000  0.05    0.24
Q19   1   0.8818  0.6407  0.4341  11.00000  0.05    0.24
Q20   1   0.8281  0.3162  0.7364  11.00000  0.05    0.24
;
_shelx_res_checksum              44141
_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 2.948
_oxdiff_exptl_absorpt_empirical_full_min 0.898
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6153 7205 4938 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3847 7204 4938 nmt 0.9999 -0.0000 0.0001 -0.0004 -1.0001 0.0001 -0.0813
-0.0001 -0.9995

_twin_special_details            
;
Component 2 rotated by -179.9939° 
 around [1.00 -0.00 -0.04] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
