# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1atn_lt
_database_code_depnum_ccdc_archive 'CCDC 1941497'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C3 H6 O)'
_chemical_formula_sum            'C14 H14 Br4 O6'
_chemical_formula_weight         597.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   24.9223(4)
_cell_length_b                   9.0196(2)
_cell_length_c                   8.88690(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.248(2)
_cell_angle_gamma                90
_cell_volume                     1994.47(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3867
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4930
_cell_measurement_theta_min      5.2040
_shelx_estimated_absorpt_T_max   0.196
_shelx_estimated_absorpt_T_min   0.179
_exptl_absorpt_coefficient_mu    10.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5459
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.805
_diffrn_reflns_theta_min         3.553
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     82.00 134.00   1.00   15.00    --  106.99 -61.00 -30.00   52
  2  ω   -115.00 -22.00   1.00    5.00    --  -40.57 -57.00-180.00   93
  3  ω    -92.00 -11.00   1.00    5.00    --  -40.57 125.00 -60.00   81
  4  ω   -115.00 -15.00   1.00    5.00    --  -40.57 -37.00  60.00  100
  5  ω     -7.00  22.00   1.00    5.00    --   40.57 -84.00 -62.00   29
  6  ω     52.00 110.00   1.00   15.00    --  106.99 -94.00 120.00   58
  7  ω     36.00  79.00   1.00   15.00    --  106.99 -61.00 -30.00   43
  8  ω     98.00 175.00   1.00   15.00    --  106.99  84.00  57.00   77
  9  ω     41.00 110.00   1.00   15.00    --  106.99 -94.00 -30.00   69
 10  ω    107.00 178.00   1.00   15.00    --  106.99 125.00   0.00   71
 11  ω     32.00 122.00   1.00   15.00    --  106.99 -45.00  90.00   90
 12  ω     23.00  49.00   1.00   15.00    --  106.99 -94.00 120.00   26
 13  ω     24.00 165.00   1.00   15.00    --  106.99 -15.00-120.00  141
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0674271000
_diffrn_orient_matrix_UB_12      0.0326536000
_diffrn_orient_matrix_UB_13      -0.0544194000
_diffrn_orient_matrix_UB_21      -0.0580937000
_diffrn_orient_matrix_UB_22      0.1607382000
_diffrn_orient_matrix_UB_23      0.0023542000
_diffrn_orient_matrix_UB_31      0.1488815000
_diffrn_orient_matrix_UB_32      0.0479263000
_diffrn_orient_matrix_UB_33      0.0294883000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1856
_reflns_number_total             1977
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.370
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.000117(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1977
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0166
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0243P)²+0.5237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0437
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.84 with sigma of 0.02
 C7A-C5A \\sim C6A-C5A
 with sigma of 0.02
 C6B-C5B \\sim C7B-C5B
 with sigma of 0.02
 C6A-O3A \\sim O3A-C7A
 with sigma of 0.02
 O3B-C6B \\sim C6B-C7B
 with sigma of 0.02
 O3A-C5A \\sim O3B-C5B
 with sigma of 0.02
 C7A-C6A \\sim C6B-C7B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O3A, C5A, C6A, C7A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3B, C5B, C6B, C7B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(O3B)=Sof(C5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C7B)=Sof(H7BA)=
 Sof(H7BB)=Sof(H7BC)=1-FVAR(1)
 Sof(O3A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=
 Sof(H7AB)=Sof(H7AC)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,H6BC), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,
 H7BC)
;
_atom_sites_solution_hydrogens   mixed
_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
Br1 Br 0.68146(2) 0.52691(2) 0.70800(2) 0.01858(8) Uani 1 1 d . . . . .
Br2 Br 0.68347(2) 0.96958(2) 0.26253(2) 0.01996(8) Uani 1 1 d . . . . .
O1 O 0.61070(5) 0.83361(14) 0.56129(15) 0.0217(3) Uani 1 1 d D . . . .
H1 H 0.5775(7) 0.826(3) 0.553(3) 0.049(8) Uiso 1 1 d D . . . .
O2 O 0.60996(5) 0.65753(14) 0.38284(14) 0.0211(3) Uani 1 1 d . . . . .
O3A O 0.50955(11) 0.7921(4) 0.5981(4) 0.0245(7) Uani 0.507(4) 1 d D U P A 1
O3B O 0.50652(13) 0.8386(3) 0.5259(5) 0.0225(7) Uani 0.493(4) 1 d D U P A 2
C1 C 0.63351(7) 0.74070(18) 0.46998(18) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.69399(7) 0.74746(17) 0.48669(17) 0.0136(3) Uani 1 1 d . . . . .
C3 C 0.72167(6) 0.65430(17) 0.58916(18) 0.0144(3) Uani 1 1 d . . . . .
C4 C 0.72246(7) 0.84354(17) 0.39799(18) 0.0145(3) Uani 1 1 d . . . . .
C5A C 0.47318(19) 0.7989(6) 0.5007(5) 0.0226(9) Uani 0.507(4) 1 d D U P A 1
C5B C 0.47532(18) 0.7363(6) 0.5441(5) 0.0217(9) Uani 0.493(4) 1 d D U P A 2
C6A C 0.4163(3) 0.7761(16) 0.5260(19) 0.027(2) Uani 0.507(4) 1 d D U P A 1
H6AA H 0.412943 0.712285 0.611388 0.041 Uiso 0.507(4) 1 calc GR . P A 1
H6AB H 0.398800 0.731305 0.438328 0.041 Uiso 0.507(4) 1 calc GR . P A 1
H6AC H 0.399696 0.869912 0.544875 0.041 Uiso 0.507(4) 1 calc GR . P A 1
C6B C 0.4163(4) 0.7501(17) 0.543(2) 0.029(2) Uani 0.493(4) 1 d D U P A 2
H6BA H 0.405153 0.747221 0.644764 0.043 Uiso 0.493(4) 1 calc GR . P A 2
H6BB H 0.399912 0.669605 0.486778 0.043 Uiso 0.493(4) 1 calc GR . P A 2
H6BC H 0.405406 0.842491 0.497265 0.043 Uiso 0.493(4) 1 calc GR . P A 2
C7A C 0.48214(17) 0.8331(5) 0.3410(4) 0.0297(9) Uani 0.507(4) 1 d D U P A 1
H7AA H 0.464482 0.924447 0.313198 0.045 Uiso 0.507(4) 1 calc GR . P A 1
H7AB H 0.467748 0.754469 0.278044 0.045 Uiso 0.507(4) 1 calc GR . P A 1
H7AC H 0.519983 0.842421 0.328299 0.045 Uiso 0.507(4) 1 calc GR . P A 1
C7B C 0.49525(18) 0.5842(5) 0.5823(6) 0.0390(11) Uani 0.493(4) 1 d D U P A 2
H7BA H 0.475793 0.513006 0.520200 0.059 Uiso 0.493(4) 1 calc GR . P A 2
H7BB H 0.489946 0.563765 0.686441 0.059 Uiso 0.493(4) 1 calc GR . P A 2
H7BC H 0.532848 0.577850 0.564865 0.059 Uiso 0.493(4) 1 calc GR . P A 2

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
Br1 0.01519(11) 0.01954(11) 0.02119(12) 0.00738(6) 0.00258(7) -0.00268(6)
Br2 0.01562(11) 0.02128(11) 0.02261(12) 0.00930(6) -0.00211(7) 0.00124(6)
O1 0.0125(6) 0.0224(6) 0.0307(7) -0.0089(5) 0.0034(5) -0.0010(5)
O2 0.0147(6) 0.0245(6) 0.0241(6) -0.0065(5) -0.0002(5) -0.0027(5)
O3A 0.0188(14) 0.0288(16) 0.0258(15) -0.0020(14) 0.0010(12) 0.0019(11)
O3B 0.0167(16) 0.0211(14) 0.0299(19) -0.0007(13) 0.0017(13) -0.0013(12)
C1 0.0146(8) 0.0144(7) 0.0173(7) 0.0029(6) 0.0010(6) 0.0002(6)
C2 0.0128(7) 0.0138(7) 0.0142(7) -0.0027(6) 0.0009(5) 0.0001(6)
C3 0.0152(7) 0.0136(7) 0.0144(7) 0.0000(6) 0.0016(6) -0.0020(6)
C4 0.0163(8) 0.0141(7) 0.0130(7) 0.0015(6) -0.0001(6) 0.0009(6)
C5A 0.022(2) 0.020(2) 0.026(2) -0.0042(17) 0.0012(15) 0.0034(17)
C5B 0.023(2) 0.026(2) 0.0166(19) -0.0076(17) 0.0053(15) -0.0037(16)
C6A 0.019(2) 0.027(4) 0.035(4) 0.012(3) 0.001(2) -0.003(2)
C6B 0.020(2) 0.031(5) 0.035(4) 0.014(4) 0.001(2) -0.004(2)
C7A 0.029(2) 0.035(2) 0.0240(18) -0.0019(15) -0.0021(14) 0.0000(16)
C7B 0.030(2) 0.027(2) 0.061(3) -0.001(2) 0.013(2) -0.0046(16)

_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
Br1 C3 1.8869(16) . ?
Br2 C4 1.8851(16) . ?
O1 C1 1.318(2) . ?
O2 C1 1.206(2) . ?
O3A C5A 1.219(6) . ?
O3B C5B 1.224(6) . ?
C1 C2 1.507(2) . ?
C2 C3 1.393(2) . ?
C2 C4 1.393(2) . ?
C3 C4 1.391(2) 7_666 ?
C5A C6A 1.463(9) . ?
C5A C7A 1.481(6) . ?
C5B C6B 1.476(9) . ?
C5B C7B 1.492(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 112.17(14) . . ?
O2 C1 O1 125.43(16) . . ?
O2 C1 C2 122.40(15) . . ?
C3 C2 C1 119.71(14) . . ?
C4 C2 C1 120.54(14) . . ?
C4 C2 C3 119.73(15) . . ?
C2 C3 Br1 118.30(12) . . ?
C4 C3 Br1 121.58(12) 7_666 . ?
C4 C3 C2 120.12(15) 7_666 . ?
C2 C4 Br2 118.42(12) . . ?
C3 C4 Br2 121.43(12) 7_666 . ?
C3 C4 C2 120.15(15) 7_666 . ?
O3A C5A C6A 124.9(8) . . ?
O3A C5A C7A 123.0(5) . . ?
C6A C5A C7A 112.1(7) . . ?
O3B C5B C6B 125.2(7) . . ?
O3B C5B C7B 121.2(4) . . ?
C6B C5B C7B 113.4(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O3A 0.830(17) 1.79(2) 2.588(3) 161(3) . yes
O1 H1 O3B 0.830(17) 1.774(18) 2.598(4) 171(3) . yes
C7A H7AB O2 0.96 2.50 3.349(4) 147.5 2_655 yes

_shelx_res_file                  
;
TITL 1lt_a.res in C2/c
    1atn_lt.res
    created by SHELXL-2018/3 at 17:23:43 on 18-Jul-2019
REM Old TITL 1LT in C2/c #15
REM SHELXT solution in C2/c: R1 0.101, Rweak 0.003, Alpha 0.021
REM <I/s> 0.718 for 125 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 Br2 O2
CELL 1.54184 24.9223 9.0196 8.8869 90 93.248 90
ZERR 4 0.0004 0.0002 0.0001 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br O
UNIT 56 56 16 24
EQIV $1 1-X,+Y,0.5-Z
EQIV $2 +X,1-Y,0.5+Z
EQIV $3 1.5-X,-0.5+Y,1.5-Z
EQIV $4 1-X,1-Y,1-Z
DFIX 0.84 O1 H1
SADI C7A C5A C6A C5A
SADI C6B C5B C7B C5B
SADI C6A O3A O3A C7A
SADI O3B C6B C6B C7B
SADI O3A C5A O3B C5B
SADI C7A C6A C6B C7B
RIGU 0.002 0.002 O3A C5A C6A C7A
RIGU 0.002 0.002 O3B C5B C6B C7B

L.S. 8
PLAN  10
SIZE 0.26 0.24 0.24
TEMP 22.85
HTAB O1 O3A
HTAB O1 O3B
HTAB C7A O2_$1
FREE Br1 O2_$2
FREE C7A C7A_$1
FREE C7A H7Ac_$1
FREE H7Bc H7Ba_$4
FREE Br2 O1_$3
FREE C7B H7Ba_$4
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\1ATN_LT.hkl">
REM </olex2.extras>

WGHT    0.024300    0.523700
EXTI    0.000117
FVAR       0.19961   0.50657
BR1   3    0.681456    0.526908    0.708002    11.00000    0.01519    0.01954 =
         0.02119    0.00738    0.00258   -0.00268
BR2   3    0.683471    0.969584    0.262525    11.00000    0.01562    0.02128 =
         0.02261    0.00930   -0.00211    0.00124
O1    4    0.610703    0.833614    0.561291    11.00000    0.01247    0.02235 =
         0.03065   -0.00894    0.00337   -0.00105
H1    2    0.577452    0.826378    0.553273    11.00000    0.04857
O2    4    0.609957    0.657527    0.382836    11.00000    0.01470    0.02449 =
         0.02406   -0.00654   -0.00020   -0.00269
PART 1
O3A   4    0.509551    0.792109    0.598097    21.00000    0.01879    0.02884 =
         0.02579   -0.00205    0.00103    0.00191

PART 0
PART 2
O3B   4    0.506516    0.838644    0.525892   -21.00000    0.01668    0.02107 =
         0.02991   -0.00066    0.00167   -0.00131

PART 0
C1    1    0.633510    0.740701    0.469980    11.00000    0.01459    0.01441 =
         0.01728    0.00289    0.00095    0.00018
C2    1    0.693986    0.747456    0.486692    11.00000    0.01276    0.01384 =
         0.01418   -0.00269    0.00095    0.00005
C3    1    0.721675    0.654298    0.589159    11.00000    0.01523    0.01356 =
         0.01436    0.00004    0.00161   -0.00200
C4    1    0.722463    0.843538    0.397992    11.00000    0.01626    0.01410 =
         0.01299    0.00150   -0.00009    0.00092

PART 1
C5A   1    0.473181    0.798934    0.500711    21.00000    0.02162    0.01974 =
         0.02649   -0.00421    0.00119    0.00338

PART 0
PART 2
C5B   1    0.475325    0.736287    0.544129   -21.00000    0.02346    0.02551 =
         0.01659   -0.00764    0.00526   -0.00371

PART 0
PART 1
C6A   1    0.416260    0.776150    0.526000    21.00000    0.01938    0.02713 =
         0.03475    0.01186    0.00110   -0.00287
AFIX 137
H6AA  2    0.412943    0.712285    0.611388    21.00000   -1.50000
H6AB  2    0.398800    0.731305    0.438328    21.00000   -1.50000
H6AC  2    0.399696    0.869912    0.544875    21.00000   -1.50000
AFIX   0

PART 0
PART 2
C6B   1    0.416288    0.750109    0.543148   -21.00000    0.02035    0.03079 =
         0.03475    0.01369    0.00139   -0.00396
AFIX 137
H6BA  2    0.405153    0.747221    0.644764   -21.00000   -1.50000
H6BB  2    0.399912    0.669605    0.486778   -21.00000   -1.50000
H6BC  2    0.405406    0.842491    0.497265   -21.00000   -1.50000
AFIX   0

PART 0
PART 1
C7A   1    0.482137    0.833072    0.341009    21.00000    0.02940    0.03527 =
         0.02396   -0.00190   -0.00210   -0.00004
AFIX 137
H7AA  2    0.464482    0.924447    0.313198    21.00000   -1.50000
H7AB  2    0.467748    0.754469    0.278044    21.00000   -1.50000
H7AC  2    0.519983    0.842421    0.328299    21.00000   -1.50000
AFIX   0

PART 0
PART 2
C7B   1    0.495254    0.584172    0.582311   -21.00000    0.03017    0.02667 =
         0.06148   -0.00101    0.01306   -0.00461
AFIX 137
H7BA  2    0.475793    0.513006    0.520200   -21.00000   -1.50000
H7BB  2    0.489946    0.563765    0.686441   -21.00000   -1.50000
H7BC  2    0.532848    0.577850    0.564865   -21.00000   -1.50000
AFIX   0
HKLF 4




REM  1lt_a.res in C2/c
REM wR2 = 0.0437, GooF = S = 1.095, Restrained GooF = 1.094 for all data
REM R1 = 0.0166 for 1856 Fo > 4sig(Fo) and 0.0182 for all 1977 data
REM 155 parameters refined using 44 restraints

END

WGHT      0.0243      0.5237

REM Highest difference peak  0.370,  deepest hole -0.292,  1-sigma level  0.065
Q1    1   0.7476  0.6671  0.6189  11.00000  0.05    0.37
Q2    1   0.7079  0.8985  0.3505  11.00000  0.05    0.32
Q3    1   0.6860  0.9851  0.1153  11.00000  0.05    0.31
Q4    1   0.6674  0.7475  0.4748  11.00000  0.05    0.28
Q5    1   0.7075  0.8121  0.4504  11.00000  0.05    0.28
Q6    1   0.6792  0.5150  0.8595  11.00000  0.05    0.27
Q7    1   0.7098  0.5942  0.6225  11.00000  0.05    0.26
Q8    1   0.7106  0.6693  0.5171  11.00000  0.05    0.25
Q9    1   0.6487  0.9873  0.3543  11.00000  0.05    0.25
Q10   1   0.6797  0.5366  0.5599  11.00000  0.05    0.25
;
_shelx_res_checksum              65518
_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 1.180
_oxdiff_exptl_absorpt_empirical_full_min 0.820
####################################################################### 
# 
# 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_1rt
_database_code_depnum_ccdc_archive 'CCDC 1941498'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C3 H6 O)'
_chemical_formula_sum            'C14 H14 Br4 O6'
_chemical_formula_weight         597.89
_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'
Br Br -0.2901 2.4595 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.174(5)
_cell_length_b                   9.1572(18)
_cell_length_c                   8.9838(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.250(7)
_cell_angle_gamma                90
_cell_volume                     2067.7(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7982
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.546
_cell_measurement_theta_min      3.243
_shelx_estimated_absorpt_T_max   0.236
_shelx_estimated_absorpt_T_min   0.203
_exptl_absorpt_coefficient_mu    7.809
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1287 before and 0.0688 after correction. The Ratio of minimum to maximum transmission is 0.6169. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23666
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.757
_diffrn_reflns_theta_min         3.242
_diffrn_ambient_temperature      296.0
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 CMOS PHOTON II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1521
_reflns_number_total             1973
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         0.489
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.00068(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1973
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0306
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+5.3796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0655
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.84 with sigma of 0.02
 C7A-C5A \\sim C6A-C5A
 with sigma of 0.02
 C6B-C5B \\sim C7B-C5B
 with sigma of 0.02
 C6A-O3A \\sim O3A-C7A
 with sigma of 0.02
 O3B-C6B \\sim C6B-C7B
 with sigma of 0.02
 O3A-C5A \\sim O3B-C5B
 with sigma of 0.02
 C7A-C6A \\sim C6B-C7B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O3A, C5A, C6A, C7A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3B, C5B, C6B, C7B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Sof(O3B)=Sof(C5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=Sof(C7B)=Sof(H7BA)=
 Sof(H7BB)=Sof(H7BC)=1-FVAR(1)
 Sof(O3A)=Sof(C5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7AA)=
 Sof(H7AB)=Sof(H7AC)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,H6BC), C7A(H7AA,H7AB,H7AC), C7B(H7BA,H7BB,
 H7BC)
;
_atom_sites_solution_hydrogens   mixed
_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
Br1 Br 0.68239(2) 0.52812(5) 0.70311(5) 0.05175(16) Uani 1 1 d . . . . .
Br2 Br 0.68440(2) 0.96719(5) 0.26663(5) 0.05437(17) Uani 1 1 d . . . . .
O1 O 0.61227(10) 0.8290(3) 0.5610(3) 0.0495(7) Uani 1 1 d D . . . .
H1 H 0.5798(8) 0.829(5) 0.553(5) 0.058(13) Uiso 1 1 d D . . . .
O2 O 0.61182(10) 0.6602(3) 0.3821(3) 0.0515(7) Uani 1 1 d . . . . .
O3A O 0.5107(4) 0.7925(13) 0.5930(10) 0.066(3) Uani 0.517(7) 1 d D U P A 1
O3B O 0.5082(4) 0.8294(11) 0.5303(12) 0.056(2) Uani 0.483(7) 1 d D U P A 2
C1 C 0.63477(13) 0.7401(4) 0.4698(4) 0.0341(8) Uani 1 1 d . . . . .
C2 C 0.69451(12) 0.7474(4) 0.4870(4) 0.0295(7) Uani 1 1 d . . . . .
C3 C 0.72218(13) 0.6551(4) 0.5863(3) 0.0307(7) Uani 1 1 d . . . . .
C4 C 0.72306(12) 0.8423(4) 0.4003(3) 0.0307(7) Uani 1 1 d . . . . .
C5A C 0.4744(4) 0.8011(14) 0.4996(11) 0.055(2) Uani 0.517(7) 1 d D U P A 1
C5B C 0.4752(4) 0.7325(12) 0.5406(13) 0.053(3) Uani 0.483(7) 1 d D U P A 2
C6A C 0.4194(5) 0.785(3) 0.531(3) 0.083(5) Uani 0.517(7) 1 d D U P A 1
H6AA H 0.415443 0.704519 0.597231 0.125 Uiso 0.517(7) 1 calc GR . P A 1
H6AB H 0.398695 0.767903 0.439391 0.125 Uiso 0.517(7) 1 calc GR . P A 1
H6AC H 0.407232 0.873129 0.576304 0.125 Uiso 0.517(7) 1 calc GR . P A 1
C6B C 0.4176(6) 0.746(3) 0.540(4) 0.090(7) Uani 0.483(7) 1 d D U P A 2
H6BA H 0.406701 0.742917 0.640794 0.135 Uiso 0.483(7) 1 calc GR . P A 2
H6BB H 0.401253 0.667788 0.483873 0.135 Uiso 0.483(7) 1 calc GR . P A 2
H6BC H 0.406931 0.837937 0.495679 0.135 Uiso 0.483(7) 1 calc GR . P A 2
C7A C 0.4828(4) 0.8380(12) 0.3443(9) 0.081(3) Uani 0.517(7) 1 d D U P A 1
H7AA H 0.464342 0.926957 0.318380 0.122 Uiso 0.517(7) 1 calc GR . P A 1
H7AB H 0.469461 0.760595 0.280590 0.122 Uiso 0.517(7) 1 calc GR . P A 1
H7AC H 0.520171 0.850758 0.331976 0.122 Uiso 0.517(7) 1 calc GR . P A 1
C7B C 0.4931(5) 0.5833(12) 0.5789(19) 0.122(6) Uani 0.483(7) 1 d D U P A 2
H7BA H 0.503628 0.534591 0.490739 0.183 Uiso 0.483(7) 1 calc GR . P A 2
H7BB H 0.464485 0.530407 0.620314 0.183 Uiso 0.483(7) 1 calc GR . P A 2
H7BC H 0.522758 0.587809 0.650761 0.183 Uiso 0.483(7) 1 calc GR . P A 2

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
Br1 0.0392(2) 0.0571(3) 0.0596(3) 0.0260(2) 0.00863(18) -0.00790(18)
Br2 0.0402(2) 0.0621(3) 0.0599(3) 0.0301(2) -0.00527(18) 0.00538(19)
O1 0.0259(14) 0.0572(18) 0.0657(18) -0.0186(14) 0.0070(13) 0.0019(13)
O2 0.0318(14) 0.0622(18) 0.0600(18) -0.0216(14) -0.0017(12) -0.0030(13)
O3A 0.041(4) 0.098(8) 0.059(5) 0.000(4) 0.005(3) 0.005(4)
O3B 0.039(5) 0.059(5) 0.071(7) 0.000(4) 0.012(5) 0.000(3)
C1 0.0288(19) 0.036(2) 0.037(2) 0.0027(16) 0.0031(16) 0.0014(15)
C2 0.0225(17) 0.0337(19) 0.0326(18) -0.0012(14) 0.0035(14) -0.0004(14)
C3 0.0315(18) 0.0303(19) 0.0306(18) 0.0041(14) 0.0061(14) -0.0031(14)
C4 0.0298(18) 0.0309(19) 0.0310(18) 0.0068(14) -0.0030(14) 0.0029(14)
C5A 0.042(4) 0.060(7) 0.063(4) -0.013(4) 0.000(3) 0.007(5)
C5B 0.043(5) 0.070(5) 0.049(6) -0.013(5) 0.019(5) -0.008(4)
C6A 0.039(5) 0.099(12) 0.111(14) 0.012(10) 0.001(6) 0.007(6)
C6B 0.041(5) 0.117(15) 0.113(17) 0.022(12) 0.015(7) -0.020(5)
C7A 0.076(7) 0.105(8) 0.062(4) -0.006(5) -0.005(4) 0.003(6)
C7B 0.098(9) 0.057(6) 0.216(16) -0.002(7) 0.040(10) -0.007(5)

_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
Br1 C3 1.891(3) . ?
Br2 C4 1.888(3) . ?
O1 C1 1.307(4) . ?
O2 C1 1.199(4) . ?
O3A C5A 1.207(11) . ?
O3B C5B 1.222(11) . ?
C1 C2 1.505(4) . ?
C2 C3 1.387(4) . ?
C2 C4 1.394(4) . ?
C3 C4 1.377(4) 7_666 ?
C5A C6A 1.436(12) . ?
C5A C7A 1.463(11) . ?
C5B C6B 1.455(13) . ?
C5B C7B 1.473(13) . ?

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 C1 C2 112.0(3) . . ?
O2 C1 O1 125.6(3) . . ?
O2 C1 C2 122.4(3) . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 C4 118.9(3) . . ?
C4 C2 C1 120.9(3) . . ?
C2 C3 Br1 118.0(2) . . ?
C4 C3 Br1 121.4(2) 7_666 . ?
C4 C3 C2 120.6(3) 7_666 . ?
C2 C4 Br2 118.0(2) . . ?
C3 C4 Br2 121.5(2) 7_666 . ?
C3 C4 C2 120.4(3) 7_666 . ?
O3A C5A C6A 124.0(14) . . ?
O3A C5A C7A 122.2(10) . . ?
C6A C5A C7A 113.7(13) . . ?
O3B C5B C6B 128.2(12) . . ?
O3B C5B C7B 119.4(11) . . ?
C6B C5B C7B 111.9(10) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O3A 0.816(19) 1.83(2) 2.610(9) 161(4) . yes
O1 H1 O3B 0.816(19) 1.80(2) 2.618(10) 178(4) . yes
C7A H7AB O2 0.96 2.61 3.452(10) 146.1 2_655 yes

_shelx_res_file                  
;
TITL KCKS7_0m_a.res in C2/c
    1rt.res
    created by SHELXL-2018/3 at 17:27:34 on 18-Jul-2019
REM Old TITL KCKS7_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.214, Rweak 0.029, Alpha 0.044, Orientation as input
REM Formula found by SHELXT: C6 Br2 O3
CELL 0.71073 25.1742 9.1572 8.9838 90 93.25 90
ZERR 4 0.0048 0.0018 0.0017 0 0.007 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Br O
UNIT 56 56 16 24
EQIV $1 1-X,+Y,0.5-Z
EQIV $2 +X,1-Y,0.5+Z
EQIV $3 1.5-X,-0.5+Y,1.5-Z
EQIV $4 1-X,1-Y,1-Z
DFIX 0.84 O1 H1
SADI C7A C5A C6A C5A
SADI C6B C5B C7B C5B
SADI C6A O3A O3A C7A
SADI O3B C6B C6B C7B
SADI O3A C5A O3B C5B
SADI C7A C6A C6B C7B
RIGU 0.002 0.002 O3A C5A C6A C7A
RIGU 0.002 0.002 O3B C5B C6B C7B

L.S. 8
PLAN  10
SIZE 0.26 0.26 0.3
TEMP 22.85
HTAB O1 O3A
HTAB O1 O3B
HTAB C7A O2_$1
FREE Br2 O1_$3
FREE C7A C7A_$1
FREE C7A H7Ac_$1
FREE H7Bc H7Ba_$4
FREE Br1 O2_$2
FREE H7Ba H7Ba_$4
FREE C7B H7Ba_$4
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\1RT.hkl">
REM </olex2.extras>

WGHT    0.023800    5.379600
EXTI    0.000676
FVAR       0.20957   0.51685
BR1   3    0.682393    0.528116    0.703110    11.00000    0.03917    0.05712 =
         0.05963    0.02596    0.00863   -0.00790
BR2   3    0.684395    0.967189    0.266629    11.00000    0.04020    0.06207 =
         0.05991    0.03010   -0.00527    0.00538
O1    4    0.612269    0.828979    0.561045    11.00000    0.02595    0.05724 =
         0.06575   -0.01863    0.00704    0.00192
H1    2    0.579832    0.829014    0.553349    11.00000    0.05768
O2    4    0.611816    0.660239    0.382111    11.00000    0.03184    0.06218 =
         0.06002   -0.02162   -0.00169   -0.00302
PART 1
O3A   4    0.510722    0.792538    0.593010    21.00000    0.04069    0.09761 =
         0.05874    0.00036    0.00500    0.00469

PART 0
PART 2
O3B   4    0.508229    0.829373    0.530323   -21.00000    0.03902    0.05891 =
         0.07102   -0.00031    0.01194    0.00018

PART 0
C1    1    0.634765    0.740126    0.469757    11.00000    0.02879    0.03615 =
         0.03745    0.00273    0.00314    0.00145
C2    1    0.694505    0.747365    0.487036    11.00000    0.02252    0.03371 =
         0.03263   -0.00122    0.00353   -0.00037
C3    1    0.722175    0.655089    0.586280    11.00000    0.03152    0.03030 =
         0.03063    0.00409    0.00609   -0.00313
C4    1    0.723056    0.842329    0.400259    11.00000    0.02983    0.03088 =
         0.03096    0.00679   -0.00300    0.00295

PART 1
C5A   1    0.474437    0.801088    0.499636    21.00000    0.04163    0.05965 =
         0.06282   -0.01295   -0.00040    0.00663

PART 0
PART 2
C5B   1    0.475218    0.732545    0.540585   -21.00000    0.04317    0.06986 =
         0.04890   -0.01267    0.01917   -0.00825

PART 0
PART 1
C6A   1    0.419387    0.785356    0.530717    21.00000    0.03941    0.09943 =
         0.11068    0.01215    0.00133    0.00655
AFIX 137
H6AA  2    0.415443    0.704519    0.597231    21.00000   -1.50000
H6AB  2    0.398695    0.767903    0.439391    21.00000   -1.50000
H6AC  2    0.407232    0.873129    0.576304    21.00000   -1.50000
AFIX   0

PART 0
PART 2
C6B   1    0.417626    0.746483    0.540200   -21.00000    0.04084    0.11685 =
         0.11301    0.02235    0.01508   -0.01994
AFIX 137
H6BA  2    0.406701    0.742917    0.640794   -21.00000   -1.50000
H6BB  2    0.401253    0.667788    0.483873   -21.00000   -1.50000
H6BC  2    0.406931    0.837937    0.495679   -21.00000   -1.50000
AFIX   0

PART 0
PART 1
C7A   1    0.482824    0.838024    0.344296    21.00000    0.07607    0.10484 =
         0.06151   -0.00627   -0.00479    0.00290
AFIX 137
H7AA  2    0.464342    0.926957    0.318380    21.00000   -1.50000
H7AB  2    0.469461    0.760595    0.280590    21.00000   -1.50000
H7AC  2    0.520171    0.850758    0.331976    21.00000   -1.50000
AFIX   0

PART 0
PART 2
C7B   1    0.493077    0.583347    0.578939   -21.00000    0.09769    0.05654 =
         0.21560   -0.00232    0.04039   -0.00690
AFIX 137
H7BA  2    0.503628    0.534591    0.490739   -21.00000   -1.50000
H7BB  2    0.464485    0.530407    0.620314   -21.00000   -1.50000
H7BC  2    0.522758    0.587809    0.650761   -21.00000   -1.50000
AFIX   0
HKLF 4




REM  KCKS7_0m_a.res in C2/c
REM wR2 = 0.0655, GooF = S = 1.020, Restrained GooF = 1.013 for all data
REM R1 = 0.0306 for 1521 Fo > 4sig(Fo) and 0.0488 for all 1973 data
REM 155 parameters refined using 44 restraints

END

WGHT      0.0238      5.3794

REM Highest difference peak  0.489,  deepest hole -0.398,  1-sigma level  0.075
Q1    1   0.6928  0.8823  0.2179  11.00000  0.05    0.49
Q2    1   0.7003  0.4731  0.6464  11.00000  0.05    0.47
Q3    1   0.6814  0.5235  0.5697  11.00000  0.05    0.36
Q4    1   0.6959  0.5991  0.7551  11.00000  0.05    0.36
Q5    1   0.7047  1.0151  0.3346  11.00000  0.05    0.32
Q6    1   0.6807  0.9671  0.1120  11.00000  0.05    0.30
Q7    1   0.7111  0.8918  0.3335  11.00000  0.05    0.29
Q8    1   0.6898  0.6831  0.3023  11.00000  0.05    0.27
Q9    1   0.7086  0.7212  0.5521  11.00000  0.05    0.26
Q10   1   0.6703  0.5143  0.7147  11.00000  0.05    0.25
;
_shelx_res_checksum              55186
_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_4eg_lt
_database_code_depnum_ccdc_archive 'CCDC 1941503'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C2 H6 O2)'
_chemical_formula_sum            'C12 H14 Br4 O8'
_chemical_formula_weight         605.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   7.96170(10)
_cell_length_b                   9.93120(10)
_cell_length_c                   23.5837(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1864.75(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1114
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.842
_cell_measurement_theta_min      3.749
_shelx_estimated_absorpt_T_max   0.220
_shelx_estimated_absorpt_T_min   0.139
_exptl_absorpt_coefficient_mu    10.880
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.158
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9715
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.842
_diffrn_reflns_theta_min         3.749
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1608
_reflns_number_total             1875
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1875
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0188
_refine_ls_restrained_S_all      1.058
_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)+(0.0249P)²+0.4146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0520
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O1-H1 = O3-H3 = O4-H4
 0.82 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
;
_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
Br1 Br 0.26368(3) 0.70873(2) 0.42775(2) 0.01452(8) Uani 1 1 d . . . . .
Br2 Br 0.73487(3) 0.28593(2) 0.43002(2) 0.01462(8) Uani 1 1 d . . . . .
O1 O 0.41616(17) 0.41433(13) 0.35173(5) 0.0160(3) Uani 1 1 d D . . . .
H1 H 0.445(4) 0.403(3) 0.3186(6) 0.041(8) Uiso 1 1 d D . . . .
O2 O 0.60778(16) 0.57998(13) 0.35362(5) 0.0149(3) Uani 1 1 d . . . . .
O3 O 0.53652(19) 0.35586(14) 0.25565(5) 0.0207(3) Uani 1 1 d D . . . .
H3 H 0.567(4) 0.2773(14) 0.2597(12) 0.036(8) Uiso 1 1 d D . . . .
O4 O 0.36839(18) 0.60200(13) 0.22550(6) 0.0194(3) Uani 1 1 d D . . . .
H4 H 0.2738(18) 0.591(3) 0.2127(12) 0.039(9) Uiso 1 1 d D . . . .
C1 C 0.5126(2) 0.50251(16) 0.37685(7) 0.0113(3) Uani 1 1 d . . . . .
C2 C 0.5009(2) 0.49919(16) 0.44077(8) 0.0110(3) Uani 1 1 d . . . . .
C3 C 0.3990(2) 0.58907(17) 0.47002(7) 0.0111(3) Uani 1 1 d . . . . .
C4 C 0.6019(2) 0.40957(17) 0.47107(7) 0.0114(3) Uani 1 1 d . . . . .
C5 C 0.4828(3) 0.38410(19) 0.19880(8) 0.0186(4) Uani 1 1 d . . . . .
H5A H 0.367326 0.349857 0.192866 0.022 Uiso 1 1 calc R . . . .
H5B H 0.558152 0.338964 0.171350 0.022 Uiso 1 1 calc R . . . .
C6 C 0.4872(2) 0.5336(2) 0.18981(8) 0.0193(4) Uani 1 1 d . . . . .
H6A H 0.601542 0.567529 0.198019 0.023 Uiso 1 1 calc R . . . .
H6B H 0.461564 0.553756 0.149610 0.023 Uiso 1 1 calc R . . . .

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
Br1 0.01587(13) 0.01655(12) 0.01115(12) 0.00240(6) -0.00033(6) 0.00688(7)
Br2 0.01741(13) 0.01534(12) 0.01112(12) -0.00088(6) 0.00258(7) 0.00689(7)
O1 0.0196(7) 0.0186(6) 0.0099(6) -0.0017(5) -0.0003(5) -0.0064(5)
O2 0.0173(7) 0.0150(6) 0.0125(6) -0.0002(5) 0.0023(5) -0.0026(5)
O3 0.0324(8) 0.0159(7) 0.0137(6) 0.0000(5) -0.0017(6) 0.0062(6)
O4 0.0194(7) 0.0181(7) 0.0207(6) -0.0030(5) -0.0047(6) 0.0000(5)
C1 0.0101(8) 0.0117(8) 0.0123(8) -0.0002(6) -0.0001(6) 0.0029(7)
C2 0.0107(8) 0.0113(8) 0.0110(8) -0.0007(6) 0.0004(6) -0.0025(7)
C3 0.0105(8) 0.0107(8) 0.0121(8) 0.0019(6) -0.0001(6) 0.0000(6)
C4 0.0111(8) 0.0111(8) 0.0119(8) -0.0025(6) 0.0017(6) 0.0000(6)
C5 0.0225(10) 0.0224(10) 0.0109(8) -0.0031(7) -0.0022(7) 0.0028(8)
C6 0.0181(10) 0.0250(10) 0.0149(8) 0.0029(7) 0.0002(7) -0.0031(8)

_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
Br1 C3 1.8886(17) . ?
Br2 C4 1.8884(17) . ?
O1 H1 0.822(10) . ?
O1 C1 1.307(2) . ?
O2 C1 1.211(2) . ?
O3 H3 0.823(10) . ?
O3 C5 1.435(2) . ?
O4 H4 0.818(10) . ?
O4 C6 1.436(2) . ?
C1 C2 1.511(2) . ?
C2 C3 1.389(2) . ?
C2 C4 1.396(2) . ?
C3 C4 1.390(3) 5_666 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.501(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?

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
C1 O1 H1 111(2) . . ?
C5 O3 H3 112(2) . . ?
C6 O4 H4 109(2) . . ?
O1 C1 C2 113.66(14) . . ?
O2 C1 O1 126.05(17) . . ?
O2 C1 C2 120.27(15) . . ?
C3 C2 C1 121.16(15) . . ?
C3 C2 C4 119.45(17) . . ?
C4 C2 C1 119.28(15) . . ?
C2 C3 Br1 118.38(13) . . ?
C2 C3 C4 120.38(16) . 5_666 ?
C4 C3 Br1 121.24(13) 5_666 . ?
C2 C4 Br2 118.36(13) . . ?
C3 C4 Br2 121.46(13) 5_666 . ?
C3 C4 C2 120.17(16) 5_666 . ?
O3 C5 H5A 110.0 . . ?
O3 C5 H5B 110.0 . . ?
O3 C5 C6 108.57(15) . . ?
H5A C5 H5B 108.4 . . ?
C6 C5 H5A 110.0 . . ?
C6 C5 H5B 110.0 . . ?
O4 C6 C5 111.69(15) . . ?
O4 C6 H6A 109.3 . . ?
O4 C6 H6B 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O3 0.822(10) 1.719(12) 2.5277(18) 167(3) . yes
O3 H3 O4 0.823(10) 1.848(10) 2.6697(19) 176(3) 3_645 yes
O4 H4 O2 0.818(10) 2.052(17) 2.7991(19) 152(3) 6_556 yes

_shelx_res_file                  
;
TITL kcnj12cult_a.res in Pbca
    4eg_lt.res
    created by SHELXL-2018/3 at 18:22:57 on 18-Jul-2019
REM Old TITL
REM SHELXT solution in Pbca
REM R1 0.076, Rweak 0.001, Alpha 0.025, Orientation as input
REM Formula found by SHELXT: C6 O4 Br2
CELL 1.54184 7.9617 9.9312 23.5837 90 90 90
ZERR 4 0.0001 0.0001 0.0003 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br O
UNIT 48 56 16 32
EQIV $1 1-X,-0.5+Y,0.5-Z
EQIV $2 -0.5+X,+Y,0.5-Z
DFIX 0.82 0.01 O1 H1 O3 H3 O4 H4

L.S. 10
PLAN  10
SIZE 0.3 0.2 0.2
TEMP -173(2)
HTAB O1 O3
HTAB O3 O4_$1
HTAB O4 O2_$2
BOND $H
list 4
more -3
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\4EG_LT.hkl">
REM </olex2.extras>

WGHT    0.024900    0.414600
FVAR       0.20603
BR1   3    0.263681    0.708727    0.427749    11.00000    0.01587    0.01655 =
         0.01115    0.00240   -0.00033    0.00688
BR2   3    0.734873    0.285931    0.430017    11.00000    0.01741    0.01534 =
         0.01112   -0.00088    0.00258    0.00689
O1    4    0.416156    0.414332    0.351726    11.00000    0.01964    0.01859 =
         0.00992   -0.00172   -0.00030   -0.00637
H1    2    0.444872    0.403126    0.318565    11.00000    0.04148
O2    4    0.607778    0.579980    0.353621    11.00000    0.01728    0.01500 =
         0.01249   -0.00023    0.00233   -0.00258
O3    4    0.536516    0.355864    0.255653    11.00000    0.03244    0.01588 =
         0.01369   -0.00003   -0.00167    0.00617
H3    2    0.567056    0.277274    0.259720    11.00000    0.03640
O4    4    0.368394    0.601999    0.225497    11.00000    0.01940    0.01807 =
         0.02074   -0.00299   -0.00472    0.00001
H4    2    0.273764    0.591447    0.212747    11.00000    0.03948
C1    1    0.512643    0.502509    0.376846    11.00000    0.01009    0.01168 =
         0.01226   -0.00022   -0.00007    0.00291
C2    1    0.500904    0.499189    0.440767    11.00000    0.01072    0.01130 =
         0.01097   -0.00074    0.00038   -0.00248
C3    1    0.399028    0.589071    0.470017    11.00000    0.01052    0.01071 =
         0.01207    0.00188   -0.00013    0.00003
C4    1    0.601882    0.409571    0.471067    11.00000    0.01110    0.01109 =
         0.01194   -0.00249    0.00175    0.00004
C5    1    0.482774    0.384104    0.198796    11.00000    0.02248    0.02236 =
         0.01089   -0.00309   -0.00222    0.00285
AFIX  23
H5A   2    0.367326    0.349857    0.192866    11.00000   -1.20000
H5B   2    0.558152    0.338964    0.171350    11.00000   -1.20000
AFIX   0
C6    1    0.487161    0.533641    0.189806    11.00000    0.01805    0.02498 =
         0.01487    0.00295    0.00024   -0.00313
AFIX  23
H6A   2    0.601542    0.567529    0.198019    11.00000   -1.20000
H6B   2    0.461564    0.553756    0.149610    11.00000   -1.20000
AFIX   0
HKLF 4




REM  kcnj12cult_a.res in Pbca
REM wR2 = 0.0520, GooF = S = 1.059, Restrained GooF = 1.058 for all data
REM R1 = 0.0188 for 1608 Fo > 4sig(Fo) and 0.0234 for all 1875 data
REM 121 parameters refined using 3 restraints

END

WGHT      0.0249      0.4146

REM Highest difference peak  0.358,  deepest hole -0.331,  1-sigma level  0.071
Q1    1   0.8150  0.3597  0.4303  11.00000  0.05    0.36
Q2    1   0.5565  0.4674  0.4525  11.00000  0.05    0.35
Q3    1   0.3709  0.5746  0.4989  11.00000  0.05    0.34
Q4    1   0.1725  0.6386  0.4288  11.00000  0.05    0.34
Q5    1   0.5813  0.3884  0.4997  11.00000  0.05    0.33
Q6    1   0.4980  0.4993  0.4131  11.00000  0.05    0.31
Q7    1   0.4495  0.5333  0.4560  11.00000  0.05    0.30
Q8    1   0.6954  0.4065  0.4326  11.00000  0.05    0.30
Q9    1   0.7289  0.3073  0.3919  11.00000  0.05    0.26
Q10   1   0.4988  0.4615  0.1895  11.00000  0.05    0.26
;
_shelx_res_checksum              40252
_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_4lt
_database_code_depnum_ccdc_archive 'CCDC 1941501'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C2 H6 O S)'
_chemical_formula_sum            'C12 H14 Br4 O6 S2'
_chemical_formula_weight         637.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.24933(17)
_cell_length_b                   25.7601(6)
_cell_length_c                   8.66218(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2063.88(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3078
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.500
_cell_measurement_theta_min      5.388
_shelx_estimated_absorpt_T_max   0.184
_shelx_estimated_absorpt_T_min   0.152
_exptl_absorpt_coefficient_mu    11.639
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    2.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10378
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.473
_diffrn_reflns_theta_min         5.388
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1809
_reflns_number_total             1901
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1901
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0453
_refine_ls_restrained_S_all      1.121
_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)+(0.0378P)²+19.5076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1093
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.01
3.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   mixed
_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
Br1 Br 0.97147(6) 0.31523(2) 0.27940(6) 0.01516(19) Uani 1 1 d . . . . .
Br2 Br 0.52371(6) 0.31534(2) 0.71941(6) 0.01654(19) Uani 1 1 d . . . . .
S1 S 0.70934(14) 0.51505(5) 0.54164(14) 0.0180(3) Uani 1 1 d . . . . .
O1 O 0.8296(4) 0.38396(13) 0.5974(4) 0.0156(7) Uani 1 1 d D . . . .
O2 O 0.6660(4) 0.38577(13) 0.4071(4) 0.0166(8) Uani 1 1 d . . . . .
O3 O 0.8237(4) 0.48094(14) 0.6176(5) 0.0252(9) Uani 1 1 d . . . . .
C1 C 0.7445(4) 0.36284(18) 0.4987(5) 0.0102(9) Uani 1 1 d . . . . .
C2 C 0.7480(4) 0.30398(19) 0.5000(5) 0.0085(9) Uani 1 1 d . . . . .
C3 C 0.8428(5) 0.27702(17) 0.4056(5) 0.0103(9) Uani 1 1 d . . . . .
C4 C 0.6524(5) 0.27687(18) 0.5937(5) 0.0114(9) Uani 1 1 d . . . . .
C5 C 0.8013(8) 0.5740(2) 0.4973(8) 0.0358(15) Uani 1 1 d . . . . .
H5A H 0.840228 0.589149 0.592403 0.054 Uiso 1 1 calc GR . . . .
H5B H 0.733545 0.598462 0.449614 0.054 Uiso 1 1 calc GR . . . .
H5C H 0.880712 0.566815 0.425512 0.054 Uiso 1 1 calc GR . . . .
C6 C 0.6012(6) 0.5387(2) 0.6968(7) 0.0246(12) Uani 1 1 d . . . . .
H6A H 0.547868 0.509796 0.743337 0.037 Uiso 1 1 calc GR . . . .
H6B H 0.532766 0.564551 0.657560 0.037 Uiso 1 1 calc GR . . . .
H6C H 0.663671 0.554727 0.774781 0.037 Uiso 1 1 calc GR . . . .
H1 H 0.824(12) 0.4158(5) 0.600(12) 0.09(3) Uiso 1 1 d 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
Br1 0.0179(3) 0.0081(3) 0.0195(3) 0.00129(18) 0.0085(2) -0.00167(18)
Br2 0.0190(3) 0.0099(3) 0.0207(3) -0.00198(18) 0.0096(2) 0.00194(18)
S1 0.0234(6) 0.0148(6) 0.0158(6) -0.0011(5) -0.0036(5) -0.0008(5)
O1 0.0187(18) 0.0078(16) 0.0204(18) -0.0011(14) -0.0041(15) 0.0018(14)
O2 0.0205(18) 0.0111(16) 0.0183(17) 0.0003(14) -0.0067(15) 0.0016(14)
O3 0.0192(19) 0.0163(18) 0.040(2) -0.0086(17) -0.0044(18) 0.0035(15)
C1 0.009(2) 0.008(2) 0.014(2) -0.0031(17) 0.0025(19) -0.0004(16)
C2 0.008(2) 0.009(2) 0.009(2) -0.0043(16) -0.0024(18) -0.0002(16)
C3 0.010(2) 0.009(2) 0.011(2) 0.0017(18) 0.0008(18) -0.0037(18)
C4 0.012(2) 0.012(2) 0.010(2) -0.0017(18) 0.0003(19) 0.0031(19)
C5 0.048(4) 0.026(3) 0.033(3) 0.008(3) -0.004(3) -0.011(3)
C6 0.020(3) 0.026(3) 0.028(3) -0.004(2) -0.003(2) 0.005(2)

_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
Br1 C3 1.892(4) . ?
Br2 C4 1.893(5) . ?
S1 O3 1.524(4) . ?
S1 C5 1.782(6) . ?
S1 C6 1.782(6) . ?
O1 C1 1.284(6) . ?
O1 H1 0.821(10) . ?
O2 C1 1.227(6) . ?
C1 C2 1.516(7) . ?
C2 C3 1.386(6) . ?
C2 C4 1.388(7) . ?
C3 C3 1.392(9) 7_565 ?
C4 C4 1.385(9) 7_565 ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 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 S1 C5 104.7(3) . . ?
O3 S1 C6 105.1(3) . . ?
C6 S1 C5 98.0(3) . . ?
C1 O1 H1 114(8) . . ?
O1 C1 C2 113.9(4) . . ?
O2 C1 O1 126.1(5) . . ?
O2 C1 C2 119.9(4) . . ?
C3 C2 C1 120.7(4) . . ?
C3 C2 C4 119.7(4) . . ?
C4 C2 C1 119.6(4) . . ?
C2 C3 Br1 118.6(3) . . ?
C2 C3 C3 120.1(3) . 7_565 ?
C3 C3 Br1 121.35(14) 7_565 . ?
C2 C4 Br2 118.2(3) . . ?
C4 C4 Br2 121.55(14) 7_565 . ?
C4 C4 C2 120.2(3) 7_565 . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S1 C6 H6A 109.5 . . ?
S1 C6 H6B 109.5 . . ?
S1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C6 H6B O2 0.98 2.31 3.272(6) 167.3 5_666 yes
O1 H1 O3 0.821(10) 1.686(15) 2.505(5) 175(11) . yes

_shelx_res_file                  
;
TITL
    4lt.res
    created by SHELXL-2018/3 at 18:07:33 on 18-Jul-2019
CELL 1.54184 9.249328 25.760111 8.662184 90 90 90
ZERR 4 0.000168 0.000564 0.00018 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Br O S
UNIT 48 56 16 24 8
EQIV $1 0.5+X,+Y,0.5-Z
EQIV $2 -0.5+X,+Y,1.5-Z
EQIV $3 1-X,1-Y,1-Z
DFIX 0.82 0.01 O1 H1

L.S. 4
PLAN  10
SIZE 0.26 0.26 0.22
TEMP -173(2)
RTAB CBrO C3 Br1 O2_$1
RTAB BrO Br1 O2_$1
RTAB CBrO C4 Br2 O1_$2
RTAB BrO Br2 O1_$2
HTAB O1 O3
HTAB C6 O2_$3
BOND $H
LIST 4
fmap 2
acta 133
OMIT 0 135
REM <olex2.extras>
REM <HklSrc "%.\\4LT.hkl">
REM </olex2.extras>

WGHT    0.037800   19.507601
FVAR       2.01973
BR1   3    0.971466    0.315234    0.279395    11.00000    0.01795    0.00807 =
         0.01948    0.00129    0.00848   -0.00167
BR2   3    0.523711    0.315336    0.719411    11.00000    0.01897    0.00995 =
         0.02070   -0.00198    0.00956    0.00194
S1    5    0.709341    0.515052    0.541637    11.00000    0.02343    0.01475 =
         0.01584   -0.00106   -0.00358   -0.00077
O1    4    0.829647    0.383961    0.597436    11.00000    0.01871    0.00783 =
         0.02036   -0.00112   -0.00412    0.00184
O2    4    0.666042    0.385769    0.407057    11.00000    0.02052    0.01109 =
         0.01832    0.00034   -0.00673    0.00157
O3    4    0.823677    0.480941    0.617640    11.00000    0.01921    0.01629 =
         0.04014   -0.00860   -0.00442    0.00347
C1    1    0.744525    0.362837    0.498688    11.00000    0.00851    0.00822 =
         0.01390   -0.00313    0.00246   -0.00045
C2    1    0.747993    0.303985    0.499985    11.00000    0.00781    0.00888 =
         0.00869   -0.00433   -0.00244   -0.00016
C3    1    0.842811    0.277017    0.405593    11.00000    0.01047    0.00943 =
         0.01098    0.00174    0.00082   -0.00368
C4    1    0.652442    0.276873    0.593700    11.00000    0.01223    0.01184 =
         0.01010   -0.00171    0.00031    0.00313
C5    1    0.801308    0.574005    0.497301    11.00000    0.04830    0.02590 =
         0.03328    0.00828   -0.00367   -0.01137
AFIX 137
H5A   2    0.840228    0.589149    0.592403    11.00000   -1.50000
H5B   2    0.733545    0.598462    0.449614    11.00000   -1.50000
H5C   2    0.880712    0.566815    0.425512    11.00000   -1.50000
AFIX   0
C6    1    0.601247    0.538692    0.696790    11.00000    0.02026    0.02588 =
         0.02780   -0.00408   -0.00263    0.00518
AFIX 137
H6A   2    0.547868    0.509796    0.743337    11.00000   -1.50000
H6B   2    0.532766    0.564551    0.657560    11.00000   -1.50000
H6C   2    0.663671    0.554727    0.774781    11.00000   -1.50000
AFIX   0

H1    2    0.824249    0.415765    0.599616    11.00000    0.08745
HKLF 4




REM
REM wR2 = 0.1093, GooF = S = 1.121, Restrained GooF = 1.121 for all data
REM R1 = 0.0453 for 1809 Fo > 4sig(Fo) and 0.0467 for all 1901 data
REM 115 parameters refined using 1 restraints

END

WGHT      0.0378     19.5077

REM Highest difference peak  1.713,  deepest hole -1.153,  1-sigma level  0.141
Q1    1   1.0385  0.3157  0.2208  11.00000  0.05    1.71
Q2    1   0.4838  0.3145  0.7934  11.00000  0.05    1.23
Q3    1   0.8010  0.5178  0.4733  11.00000  0.05    1.05
Q4    1   0.6074  0.3131  0.7299  11.00000  0.05    0.60
Q5    1   0.6875  0.4806  0.3853  11.00000  0.05    0.58
Q6    1   0.7502  0.4778  0.5356  11.00000  0.05    0.57
Q7    1   0.6967  0.5688  0.5321  11.00000  0.05    0.51
Q8    1   0.6296  0.2500  0.5735  10.50000  0.05    0.49
Q9    1   0.8734  0.2500  0.4236  10.50000  0.05    0.47
Q10   1   0.9235  0.2500  0.2831  10.50000  0.05    0.44
;
_shelx_res_checksum              98857
_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_2etoh_rt
_database_code_depnum_ccdc_archive 'CCDC 1941500'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT415_2etoh_rt            
;
PROBLEM: Short Inter D-H..H-X       H1       ..H5BB     .       1.28 Ang.
RESPONSE: Because of disordered ethanol molecules
;
_vrf_PLAT431_2etoh_rt            
;
PROBLEM: Short Inter HL..A Contact  Br1      ..O2       .       3.06 Ang.
RESPONSE: Because of strong Br...O halogen bonding
;
# Added during the CSD deposition process: Thursday 18 July 2019 01:04 PM
# end Validation Reply Form

_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C2 H6 O)'
_chemical_formula_sum            'C12 H14 Br4 O6'
_chemical_formula_weight         573.87
_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'
Br Br -0.2901 2.4595 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   9.1624(5)
_cell_length_b                   23.4820(12)
_cell_length_c                   8.9930(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1934.86(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    296
_cell_measurement_theta_max      29.114
_cell_measurement_theta_min      3.29
_shelx_estimated_absorpt_T_max   0.204
_shelx_estimated_absorpt_T_min   0.169
_exptl_absorpt_coefficient_mu    8.340
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.3986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1512 before and 0.0488 after correction. The Ratio of minimum to maximum transmission is 0.5345. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            32805
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.983
_diffrn_reflns_theta_min         3.291
_diffrn_ambient_temperature      296
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 CMOS PHOTON II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1630
_reflns_number_total             1938
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1938
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.054
_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)+(0.0366P)²+1.9856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0730
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.01
 O3A-C5A \\sim O3B-C5B
 with sigma of 0.01
 C5A-C6A \\sim C5B-C6B
 with sigma of 0.01
 O3A-C6A \\sim O3B-C6B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6B) \\sim Ueq, Uanis(O3B) \\sim Ueq, Uanis(C5B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O3A, C5A, C6A
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 O3B, C5B, C6B
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
5. Others
 Sof(O3B)=Sof(H3B)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=
 Sof(H6BC)=1-FVAR(1)
 Sof(O3A)=Sof(H3A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C5A(H5AA,H5AB), C5B(H5BA,H5BB)
6.b Idealised Me refined as rotating group:
 C6A(H6AA,H6AB,H6AC), C6B(H6BA,H6BB,H6BC)
6.c Idealised tetrahedral OH refined as rotating group:
 O3A(H3A), O3B(H3B)
;
_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
Br1 Br 0.68276(4) 0.67886(2) 0.28900(4) 0.05115(13) Uani 1 1 d . . . . .
Br2 Br 1.12361(5) 0.67876(2) 0.72319(4) 0.06221(15) Uani 1 1 d . . . . .
O1 O 0.8265(2) 0.60182(9) 0.5890(3) 0.0533(6) Uani 1 1 d D . . . .
O2 O 0.9974(2) 0.60290(8) 0.4133(2) 0.0459(5) Uani 1 1 d . . . . .
O3A O 0.8249(4) 0.49367(13) 0.5823(6) 0.0701(12) Uani 0.816(6) 1 d D U P A 1
H3A H 0.888985 0.469328 0.585020 0.105 Uiso 0.816(6) 1 calc GR . P A 1
C1 C 0.9149(3) 0.62669(10) 0.4968(3) 0.0325(5) Uani 1 1 d . . . . .
C2 C 0.9066(3) 0.69085(10) 0.5033(3) 0.0298(5) Uani 1 1 d . . . . .
C3 C 0.8111(3) 0.72048(10) 0.4116(3) 0.0311(5) Uani 1 1 d . . . . .
C4 C 0.9992(3) 0.72068(11) 0.5969(3) 0.0345(6) Uani 1 1 d . . . . .
C5A C 0.6896(6) 0.4693(2) 0.6288(8) 0.0916(16) Uani 0.816(6) 1 d D U P A 1
H5AA H 0.705696 0.448009 0.719797 0.110 Uiso 0.816(6) 1 calc R . P A 1
H5AB H 0.621624 0.499769 0.651109 0.110 Uiso 0.816(6) 1 calc R . P A 1
C6A C 0.6255(6) 0.4328(3) 0.5228(8) 0.0987(18) Uani 0.816(6) 1 d D U P A 1
H6AA H 0.613584 0.452869 0.430615 0.148 Uiso 0.816(6) 1 calc GR . P A 1
H6AB H 0.531922 0.420359 0.558128 0.148 Uiso 0.816(6) 1 calc GR . P A 1
H6AC H 0.687411 0.400340 0.507536 0.148 Uiso 0.816(6) 1 calc GR . P A 1
O3B O 0.7023(16) 0.4664(6) 0.4573(16) 0.072(4) Uani 0.184(6) 1 d D U P A 2
H3B H 0.724959 0.442921 0.393861 0.108 Uiso 0.184(6) 1 calc GR . P A 2
C5B C 0.828(3) 0.4961(14) 0.504(2) 0.074(5) Uani 0.184(6) 1 d D U P A 2
H5BA H 0.911930 0.480357 0.452590 0.089 Uiso 0.184(6) 1 calc R . P A 2
H5BB H 0.818703 0.535579 0.473572 0.089 Uiso 0.184(6) 1 calc R . P A 2
C6B C 0.856(3) 0.4947(12) 0.656(2) 0.064(5) Uani 0.184(6) 1 d D U P A 2
H6BA H 0.765374 0.490148 0.709090 0.097 Uiso 0.184(6) 1 calc GR . P A 2
H6BB H 0.901363 0.529688 0.686018 0.097 Uiso 0.184(6) 1 calc GR . P A 2
H6BC H 0.919186 0.463353 0.678508 0.097 Uiso 0.184(6) 1 calc GR . P A 2
H1 H 0.841(4) 0.5674(5) 0.587(5) 0.088(15) Uiso 1 1 d 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
Br1 0.0563(2) 0.03059(18) 0.0666(2) -0.00737(13) -0.02757(16) -0.00378(12)
Br2 0.0745(3) 0.0408(2) 0.0714(3) 0.00606(15) -0.03954(19) 0.00905(15)
O1 0.0655(14) 0.0234(11) 0.0711(14) 0.0057(10) 0.0280(12) 0.0034(10)
O2 0.0511(12) 0.0268(9) 0.0599(12) -0.0002(9) 0.0145(10) 0.0062(9)
O3A 0.0714(19) 0.0266(15) 0.112(3) 0.020(2) 0.018(2) 0.0118(13)
C1 0.0358(13) 0.0206(12) 0.0411(14) 0.0019(11) -0.0003(11) 0.0022(11)
C2 0.0322(12) 0.0215(12) 0.0357(12) 0.0013(10) 0.0012(11) 0.0017(10)
C3 0.0318(13) 0.0251(12) 0.0363(13) -0.0028(10) -0.0046(11) -0.0016(10)
C4 0.0375(13) 0.0285(13) 0.0374(13) 0.0031(11) -0.0072(11) 0.0031(11)
C5A 0.081(2) 0.058(2) 0.136(4) 0.018(2) 0.022(2) -0.0059(17)
C6A 0.081(3) 0.065(3) 0.150(4) 0.014(3) 0.011(3) -0.006(2)
O3B 0.087(6) 0.059(7) 0.070(6) 0.008(5) -0.009(5) 0.014(5)
C5B 0.089(7) 0.067(9) 0.068(6) 0.010(6) -0.008(5) 0.009(6)
C6B 0.081(9) 0.045(11) 0.067(6) 0.009(6) -0.005(5) 0.018(7)

_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
Br1 C3 1.885(2) . ?
Br2 C4 1.886(2) . ?
O1 C1 1.298(3) . ?
O2 C1 1.203(3) . ?
O3A C5A 1.428(6) . ?
C1 C2 1.510(3) . ?
C2 C3 1.389(3) . ?
C2 C4 1.386(3) . ?
C3 C3 1.386(5) 8_575 ?
C4 C4 1.377(5) 8_575 ?
C5A C6A 1.409(9) . ?
O3B C5B 1.411(11) . ?
C5B C6B 1.392(13) . ?

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 C1 C2 113.1(2) . . ?
O2 C1 O1 125.6(2) . . ?
O2 C1 C2 121.3(2) . . ?
C3 C2 C1 120.6(2) . . ?
C4 C2 C1 119.8(2) . . ?
C4 C2 C3 119.5(2) . . ?
C2 C3 Br1 118.70(19) . . ?
C3 C3 Br1 121.23(7) 8_575 . ?
C3 C3 C2 120.07(15) 8_575 . ?
C2 C4 Br2 118.17(19) . . ?
C4 C4 Br2 121.46(8) 8_575 . ?
C4 C4 C2 120.37(15) 8_575 . ?
C6A C5A O3A 114.0(6) . . ?
C6B C5B O3B 115.4(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3A H3A O2 0.82 1.99 2.792(4) 165.7 5_766 yes
O1 H1 O3A 0.819(10) 1.737(15) 2.541(4) 166(4) . yes

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
O1 C1 C2 C3 -90.9(3) . . . . ?
O1 C1 C2 C4 91.8(3) . . . . ?
O2 C1 C2 C3 89.5(3) . . . . ?
O2 C1 C2 C4 -87.8(3) . . . . ?
C1 C2 C3 Br1 4.3(3) . . . . ?
C1 C2 C3 C3 -175.83(16) . . . 8_575 ?
C1 C2 C4 Br2 -4.2(3) . . . . ?
C1 C2 C4 C4 175.85(15) . . . 8_575 ?
C3 C2 C4 Br2 178.4(2) . . . . ?
C3 C2 C4 C4 -1.5(3) . . . 8_575 ?
C4 C2 C3 Br1 -178.38(19) . . . . ?
C4 C2 C3 C3 1.5(3) . . . 8_575 ?

_shelx_res_file                  
;
TITL KCNJ1_0m_a.res in Pnma
    2etoh_rt.res
    created by SHELXL-2018/3 at 18:04:52 on 18-Jul-2019
REM Old TITL KCNJ1_0m in Pnma
REM SHELXT solution in Pnma
REM R1 0.285, Rweak 0.012, Alpha 0.045, Orientation a'=b, b'=c, c'=a
REM Formula found by SHELXT: C7 Br2 O2
CELL 0.71073 9.1624 23.482 8.993 90 90 90
ZERR 4 0.0005 0.0012 0.0004 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H Br O
UNIT 48 56 16 24
EQIV $1 0.5+X,+Y,1.5-Z
EQIV $2 -0.5+X,+Y,0.5-Z
EQIV $3 2-X,1-Y,1-Z
DFIX 0.82 0.01 O1 H1
SADI 0.01 O3A C5A O3B C5B
SADI 0.01 C5A C6A C5B C6B
SADI O3A C6A O3B C6B
RIGU 0.0002 0.0002 O3A C5A C6A
RIGU 0.0002 0.0002 O3B C5B C6B
ISOR 0.01 0.02 O3A C5A C6A
ISOR 0.01 0.02 C6B O3B C5B

L.S. 5
PLAN  10
SIZE 0.33 0.28 0.28
TEMP 22.85
RTAB CBrO C3 Br1 O2_$2
RTAB BrO Br1 O2_$2
RTAB CBrO C4 Br2 O1_$1
RTAB BrO Br2 O1_$1
HTAB O1 O3A
HTAB O3A O2_$3
LIST 4
CONF
fmap 2
acta
OMIT -3 52
OMIT 0 1 1
REM <olex2.extras>
REM <HklSrc "%.\\2EtOH_RT.hkl">
REM </olex2.extras>

WGHT    0.036600    1.985600
FVAR       0.26948   0.81583
BR1   3    0.682760    0.678856    0.288995    11.00000    0.05629    0.03059 =
         0.06657   -0.00737   -0.02757   -0.00378
BR2   3    1.123613    0.678757    0.723190    11.00000    0.07450    0.04076 =
         0.07136    0.00606   -0.03954    0.00905
O1    4    0.826517    0.601825    0.589048    11.00000    0.06551    0.02338 =
         0.07108    0.00572    0.02802    0.00336
O2    4    0.997357    0.602895    0.413341    11.00000    0.05106    0.02679 =
         0.05994   -0.00018    0.01453    0.00617
PART 1
O3A   4    0.824865    0.493666    0.582251    21.00000    0.07138    0.02657 =
         0.11223    0.01958    0.01757    0.01179
AFIX 147
H3A   2    0.888985    0.469328    0.585020    21.00000   -1.50000
AFIX   0

PART 0
C1    1    0.914879    0.626694    0.496769    11.00000    0.03580    0.02060 =
         0.04107    0.00189   -0.00026    0.00219
C2    1    0.906597    0.690848    0.503262    11.00000    0.03224    0.02152 =
         0.03568    0.00129    0.00123    0.00174
C3    1    0.811095    0.720484    0.411611    11.00000    0.03181    0.02508 =
         0.03627   -0.00285   -0.00464   -0.00164
C4    1    0.999189    0.720682    0.596918    11.00000    0.03745    0.02850 =
         0.03742    0.00309   -0.00718    0.00305

PART 1
C5A   1    0.689566    0.469265    0.628784    21.00000    0.08054    0.05825 =
         0.13593    0.01760    0.02174   -0.00592
AFIX  23
H5AA  2    0.705696    0.448009    0.719797    21.00000   -1.20000
H5AB  2    0.621624    0.499769    0.651109    21.00000   -1.20000
AFIX   0
C6A   1    0.625518    0.432803    0.522823    21.00000    0.08075    0.06536 =
         0.14993    0.01365    0.01084   -0.00587
AFIX 137
H6AA  2    0.613584    0.452869    0.430615    21.00000   -1.50000
H6AB  2    0.531922    0.420359    0.558128    21.00000   -1.50000
H6AC  2    0.687411    0.400340    0.507536    21.00000   -1.50000
AFIX   0
PART 0
PART 2
O3B   4    0.702343    0.466402    0.457295   -21.00000    0.08669    0.05898 =
         0.06961    0.00827   -0.00857    0.01368
AFIX 147
H3B   2    0.724959    0.442921    0.393861   -21.00000   -1.50000
AFIX   0
C5B   1    0.828089    0.496119    0.504006   -21.00000    0.08857    0.06652 =
         0.06759    0.01019   -0.00754    0.00878
AFIX  23
H5BA  2    0.911930    0.480357    0.452590   -21.00000   -1.20000
H5BB  2    0.818703    0.535579    0.473572   -21.00000   -1.20000
AFIX   0
C6B   1    0.855642    0.494719    0.656222   -21.00000    0.08069    0.04534 =
         0.06713    0.00878   -0.00546    0.01789
AFIX 137
H6BA  2    0.765374    0.490148    0.709090   -21.00000   -1.50000
H6BB  2    0.901363    0.529688    0.686018   -21.00000   -1.50000
H6BC  2    0.919186    0.463353    0.678508   -21.00000   -1.50000
AFIX   0

PART 0
H1    2    0.840568    0.567372    0.586941    11.00000    0.08762
HKLF 4




REM  KCNJ1_0m_a.res in Pnma
REM wR2 = 0.0730, GooF = S = 1.037, Restrained GooF = 1.054 for all data
REM R1 = 0.0275 for 1630 Fo > 4sig(Fo) and 0.0344 for all 1938 data
REM 136 parameters refined using 58 restraints

END

WGHT      0.0366      1.9856

REM Highest difference peak  0.398,  deepest hole -0.647,  1-sigma level  0.086
Q1    1   1.1736  0.6950  0.6404  11.00000  0.05    0.40
Q2    1   0.7602  0.6884  0.2406  11.00000  0.05    0.37
Q3    1   0.7681  0.4796  0.4345  11.00000  0.05    0.37
Q4    1   0.9142  0.6617  0.4960  11.00000  0.05    0.36
Q5    1   0.6693  0.4988  0.4050  11.00000  0.05    0.31
Q6    1   0.8033  0.5001  0.5431  11.00000  0.05    0.27
Q7    1   0.6583  0.6884  0.3757  11.00000  0.05    0.27
Q8    1   0.5724  0.4402  0.5981  11.00000  0.05    0.25
Q9    1   0.8344  0.6980  0.4882  11.00000  0.05    0.25
Q10   1   0.9493  0.7016  0.5506  11.00000  0.05    0.24
;
_shelx_res_checksum              25454
_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_4eg_rt
_database_code_depnum_ccdc_archive 'CCDC 1941504'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C16 H4 Br8 O8), 2(C2 H6 O2)'
_chemical_formula_sum            'C12 H14 Br4 O8'
_chemical_formula_weight         605.87
_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'
Br Br -0.2901 2.4595 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   8.134(2)
_cell_length_b                   9.964(3)
_cell_length_c                   23.849(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1933.0(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9675
_cell_measurement_temperature    296
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      3.031
_shelx_estimated_absorpt_T_max   0.286
_shelx_estimated_absorpt_T_min   0.261
_exptl_absorpt_coefficient_mu    8.362
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1808 before and 0.0987 after correction. The Ratio of minimum to maximum transmission is 0.4953. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.22
_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  0.0724
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30880
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.032
_diffrn_ambient_temperature      296
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 CMOS PHOTON II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\mus'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1544
_reflns_number_total             1968
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         1.501
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0034(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1968
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.032
_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)+(0.0494P)²+6.4579P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1122
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O1-H1 = O3-H3 = O4-H4
 0.82 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(Br2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(Br1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1, C2, C4, Br2, C3, Br1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C1, C2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
;
_atom_sites_solution_hydrogens   mixed
_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
Br1 Br 0.27281(6) 0.70906(5) 0.42733(2) 0.0410(2) Uani 1 1 d . U . . .
Br2 Br 0.72846(7) 0.28337(5) 0.43199(2) 0.0422(2) Uani 1 1 d . U . . .
O1 O 0.4163(4) 0.4161(3) 0.35374(12) 0.0387(8) Uani 1 1 d D . . . .
H1 H 0.435(7) 0.404(5) 0.3202(7) 0.053(16) Uiso 1 1 d D . . . .
O2 O 0.6115(4) 0.5737(3) 0.35468(12) 0.0370(7) Uani 1 1 d . . . . .
O3 O 0.5189(7) 0.3508(4) 0.25648(14) 0.0689(14) Uani 1 1 d D . . . .
H3 H 0.563(7) 0.277(3) 0.258(2) 0.046(16) Uiso 1 1 d D . . . .
O4 O 0.3738(5) 0.6000(4) 0.22381(17) 0.0522(10) Uani 1 1 d D . . . .
H4 H 0.290(5) 0.588(9) 0.206(3) 0.10(3) Uiso 1 1 d D . . . .
C1 C 0.5158(5) 0.5001(3) 0.37813(16) 0.0234(7) Uani 1 1 d . U . . .
C2 C 0.5025(4) 0.4982(3) 0.44115(16) 0.0217(6) Uani 1 1 d . U . . .
C3 C 0.4034(5) 0.5891(4) 0.46982(15) 0.0230(7) Uani 1 1 d . U . . .
C4 C 0.5991(5) 0.4085(4) 0.47215(16) 0.0235(7) Uani 1 1 d . U . . .
C5 C 0.4778(8) 0.3805(5) 0.20043(19) 0.0510(14) Uani 1 1 d . . . . .
H5A H 0.366744 0.350144 0.192683 0.061 Uiso 1 1 calc R . . . .
H5B H 0.551977 0.333635 0.175330 0.061 Uiso 1 1 calc R . . . .
C6 C 0.4894(7) 0.5273(5) 0.1905(2) 0.0550(14) Uani 1 1 d . . . . .
H6A H 0.599748 0.557470 0.199418 0.066 Uiso 1 1 calc R . . . .
H6B H 0.469327 0.545753 0.151197 0.066 Uiso 1 1 calc R . . . .

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
Br1 0.0459(3) 0.0479(3) 0.0291(3) 0.00841(18) -0.00073(18) 0.0236(2)
Br2 0.0524(4) 0.0441(3) 0.0302(3) -0.00256(18) 0.00887(19) 0.0253(2)
O1 0.052(2) 0.0450(18) 0.0188(15) -0.0042(14) -0.0016(14) -0.0183(16)
O2 0.0456(19) 0.0377(16) 0.0276(16) 0.0013(13) 0.0071(14) -0.0117(14)
O3 0.130(4) 0.047(2) 0.0300(19) -0.0055(16) -0.009(2) 0.038(2)
O4 0.058(2) 0.0391(19) 0.060(2) -0.0075(16) -0.019(2) -0.0017(18)
C1 0.0268(17) 0.0230(16) 0.0204(8) -0.0006(8) 0.0020(8) 0.0030(12)
C2 0.0224(11) 0.0222(10) 0.0204(9) -0.0007(7) 0.0017(7) 0.0009(10)
C3 0.0245(12) 0.0243(11) 0.0201(9) -0.0007(8) 0.0013(8) 0.0032(11)
C4 0.0246(13) 0.0252(11) 0.0206(9) 0.0002(8) 0.0029(8) 0.0038(11)
C5 0.070(4) 0.054(3) 0.029(3) -0.011(2) -0.001(2) 0.006(3)
C6 0.056(3) 0.065(4) 0.043(3) 0.012(3) 0.003(2) -0.010(3)

_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
Br1 O1 3.115(3) 8_665 ?
Br1 C3 1.893(4) . ?
Br2 O2 9.597(3) 4_466 ?
Br2 C4 1.892(4) . ?
O1 H1 0.823(10) . ?
O1 C1 1.301(5) . ?
O2 C1 1.207(5) . ?
O3 H3 0.818(10) . ?
O3 C5 1.409(6) . ?
O4 H4 0.820(10) . ?
O4 C6 1.428(7) . ?
C1 C2 1.507(5) . ?
C2 C3 1.392(5) . ?
C2 C4 1.401(5) . ?
C3 C4 1.384(5) 5_666 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.484(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 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
C3 Br1 O1 175.45(14) . 8_665 ?
C4 Br2 O2 2.40(12) . 4_466 ?
C1 O1 H1 115(4) . . ?
C5 O3 H3 110(4) . . ?
C6 O4 H4 101(6) . . ?
O1 C1 C2 113.2(3) . . ?
O2 C1 O1 125.8(4) . . ?
O2 C1 C2 121.0(3) . . ?
C3 C2 C1 121.6(3) . . ?
C3 C2 C4 118.7(4) . . ?
C4 C2 C1 119.6(3) . . ?
C2 C3 Br1 118.2(3) . . ?
C4 C3 Br1 121.1(3) 5_666 . ?
C4 C3 C2 120.7(3) 5_666 . ?
C2 C4 Br2 117.7(3) . . ?
C3 C4 Br2 121.7(3) 5_666 . ?
C3 C4 C2 120.5(3) 5_666 . ?
O3 C5 H5A 109.7 . . ?
O3 C5 H5B 109.7 . . ?
O3 C5 C6 110.0(4) . . ?
H5A C5 H5B 108.2 . . ?
C6 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
O4 C6 C5 111.7(4) . . ?
O4 C6 H6A 109.3 . . ?
O4 C6 H6B 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O3 0.823(10) 1.748(18) 2.550(5) 164(6) . yes
O3 H3 O4 0.818(10) 1.887(17) 2.688(5) 166(5) 3_645 yes
O4 H4 O2 0.820(10) 2.05(2) 2.851(5) 167(8) 6_556 yes

_shelx_res_file                  
;
TITL KCKS9_0m_a.res in Pbca
    4eg_rt.res
    created by SHELXL-2018/3 at 18:55:58 on 18-Jul-2019
REM Old TITL KCKS9_0m in Pbca
REM SHELXT solution in Pbca
REM R1 0.254, Rweak 0.005, Alpha 0.053, Orientation as input
REM Formula found by SHELXT: C8 Br2 O2
CELL 0.71073 8.1339 9.9645 23.849 90 90 90
ZERR 4 0.0023 0.0027 0.0061 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Br O
UNIT 48 56 16 32
EQIV $1 0.5-X,0.5+Y,+Z
EQIV $2 -0.5+X,1.5-Y,1-Z
EQIV $3 1-X,-0.5+Y,0.5-Z
EQIV $4 -0.5+X,+Y,0.5-Z
DFIX 0.82 0.01 O1 H1 O3 H3 O4 H4
RIGU 0.0001 0.0001 C1 C2 C4 Br2 C3 Br1
RIGU 0.0001 0.0001 C1 C2
ISOR 0.01 0.02 C2 C4 Br2 C3 Br1
ISOR 0.01 0.02 C2

L.S. 12
PLAN  8
SIZE 0.22 0.22 0.2
TEMP 22.85
HTAB O1 O3
HTAB O3 O4_$3
HTAB O4 O2_$4
BIND Br2 O2_$2
BIND Br1 O1_$1
BOND $H
list 4
more -3
fmap 2
acta
OMIT 0 2 2
REM <olex2.extras>
REM <HklSrc "%.\\4EG_RT.hkl">
REM </olex2.extras>

WGHT    0.049400    6.457900
EXTI    0.003359
FVAR       0.28153
BR1   3    0.272807    0.709055    0.427331    11.00000    0.04591    0.04792 =
         0.02912    0.00841   -0.00073    0.02359
BR2   3    0.728456    0.283369    0.431990    11.00000    0.05237    0.04408 =
         0.03017   -0.00256    0.00887    0.02534
O1    4    0.416288    0.416060    0.353737    11.00000    0.05222    0.04497 =
         0.01876   -0.00417   -0.00156   -0.01831
H1    2    0.434821    0.403565    0.320204    11.00000    0.05343
O2    4    0.611459    0.573726    0.354683    11.00000    0.04562    0.03773 =
         0.02756    0.00134    0.00706   -0.01170
O3    4    0.518917    0.350797    0.256476    11.00000    0.12993    0.04664 =
         0.03002   -0.00545   -0.00947    0.03815
H3    2    0.562766    0.277007    0.258228    11.00000    0.04624
O4    4    0.373841    0.600019    0.223811    11.00000    0.05768    0.03905 =
         0.05988   -0.00745   -0.01859   -0.00170
H4    2    0.289580    0.588480    0.205553    11.00000    0.10471
C1    1    0.515766    0.500054    0.378133    11.00000    0.02680    0.02304 =
         0.02040   -0.00060    0.00200    0.00303
C2    1    0.502488    0.498238    0.441152    11.00000    0.02242    0.02216 =
         0.02038   -0.00071    0.00171    0.00092
C3    1    0.403397    0.589145    0.469822    11.00000    0.02451    0.02428 =
         0.02009   -0.00071    0.00132    0.00322
C4    1    0.599066    0.408461    0.472145    11.00000    0.02462    0.02524 =
         0.02060    0.00024    0.00287    0.00379
C5    1    0.477752    0.380494    0.200432    11.00000    0.07028    0.05389 =
         0.02883   -0.01060   -0.00095    0.00609
AFIX  23
H5A   2    0.366744    0.350144    0.192683    11.00000   -1.20000
H5B   2    0.551977    0.333635    0.175330    11.00000   -1.20000
AFIX   0
C6    1    0.489414    0.527259    0.190537    11.00000    0.05617    0.06533 =
         0.04347    0.01163    0.00342   -0.01013
AFIX  23
H6A   2    0.599748    0.557470    0.199418    11.00000   -1.20000
H6B   2    0.469327    0.545753    0.151197    11.00000   -1.20000
AFIX   0
HKLF 4




REM  KCKS9_0m_a.res in Pbca
REM wR2 = 0.1122, GooF = S = 1.037, Restrained GooF = 1.032 for all data
REM R1 = 0.0417 for 1544 Fo > 4sig(Fo) and 0.0549 for all 1968 data
REM 122 parameters refined using 59 restraints

END

WGHT      0.0494      6.4578

REM Highest difference peak  1.501,  deepest hole -1.135,  1-sigma level  0.117
Q1    1   0.7984  0.3443  0.4388  11.00000  0.05    1.50
Q2    1   0.2184  0.6394  0.4322  11.00000  0.05    0.87
Q3    1   0.6066  0.4009  0.5000  11.00000  0.05    0.49
Q4    1   0.4477  0.5249  0.4492  11.00000  0.05    0.45
Q5    1   0.5267  0.4260  0.4431  11.00000  0.05    0.44
Q6    1   0.9286  0.3798  0.4241  11.00000  0.05    0.38
Q7    1   0.4117  0.3200  0.2512  11.00000  0.05    0.34
Q8    1   0.6993  0.2596  0.4589  11.00000  0.05    0.33
;
_shelx_res_checksum              59978
_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_2etoh_lt
_database_code_depnum_ccdc_archive 'CCDC 1941499'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C2 H6 O)'
_chemical_formula_sum            'C12 H14 Br4 O6'
_chemical_formula_weight         573.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   9.27849(19)
_cell_length_b                   23.5754(5)
_cell_length_c                   8.6023(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1881.71(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4308
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      73.5200
_cell_measurement_theta_min      5.4400
_shelx_estimated_absorpt_T_max   0.281
_shelx_estimated_absorpt_T_min   0.203
_exptl_absorpt_coefficient_mu    10.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31048
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.584
_oxdiff_exptl_absorpt_empirical_full_max 2.711
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9416
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.483
_diffrn_reflns_theta_max         67.483
_diffrn_reflns_theta_min         3.750
_diffrn_ambient_temperature      100.02(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1595
_reflns_number_total             1747
_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         1.010
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1747
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²+0.1889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0809
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1 = O3-H3
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_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
Br1 Br 0.69564(3) 0.67863(2) 0.28531(3) 0.01807(14) Uani 1 1 d . . . . .
Br2 Br 1.14708(3) 0.67862(2) 0.72161(3) 0.02135(14) Uani 1 1 d . . . . .
O1 O 0.84539(18) 0.60320(7) 0.59898(19) 0.0209(4) Uani 1 1 d D . . . .
H1 H 0.851(4) 0.5683(8) 0.598(4) 0.034(9) Uiso 1 1 d D . . . .
O2 O 1.00826(17) 0.60218(7) 0.40626(17) 0.0177(3) Uani 1 1 d . . . . .
O3 O 0.8349(2) 0.49657(7) 0.6012(3) 0.0334(5) Uani 1 1 d D . . . .
H3 H 0.888(3) 0.4689(11) 0.592(4) 0.042(10) Uiso 1 1 d D . . . .
C1 C 0.9300(2) 0.62708(10) 0.4968(2) 0.0137(4) Uani 1 1 d . . . . .
C2 C 0.9238(2) 0.69105(10) 0.5009(2) 0.0146(4) Uani 1 1 d . . . . .
C3 C 0.8269(2) 0.72047(9) 0.4081(2) 0.0131(4) Uani 1 1 d . . . . .
C4 C 1.0189(2) 0.72048(9) 0.5956(2) 0.0147(4) Uani 1 1 d . . . . .
C5 C 0.6982(3) 0.47493(11) 0.6551(3) 0.0293(6) Uani 1 1 d . . . . .
H5A H 0.635291 0.507067 0.684897 0.035 Uiso 1 1 calc R . . . .
H5B H 0.713923 0.451250 0.748638 0.035 Uiso 1 1 calc R . . . .
C6 C 0.6245(3) 0.44022(12) 0.5326(3) 0.0339(6) Uani 1 1 d . . . . .
H6A H 0.608538 0.463592 0.440009 0.051 Uiso 1 1 calc GR . . . .
H6B H 0.531579 0.426733 0.572352 0.051 Uiso 1 1 calc GR . . . .
H6C H 0.685057 0.407647 0.505502 0.051 Uiso 1 1 calc GR . . . .

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
Br1 0.0187(2) 0.01204(19) 0.0235(2) -0.00215(8) -0.00828(9) -0.00134(8)
Br2 0.0246(2) 0.0148(2) 0.0247(2) 0.00142(8) -0.01220(10) 0.00293(8)
O1 0.0261(9) 0.0109(8) 0.0256(9) 0.0024(7) 0.0091(7) 0.0004(7)
O2 0.0173(8) 0.0149(7) 0.0209(8) -0.0009(6) 0.0038(7) 0.0019(6)
O3 0.0258(10) 0.0120(8) 0.0624(14) 0.0062(8) 0.0173(10) 0.0034(7)
C1 0.0113(10) 0.0130(10) 0.0167(10) 0.0016(8) -0.0032(10) 0.0006(7)
C2 0.0161(11) 0.0122(10) 0.0155(10) 0.0002(8) 0.0056(10) -0.0002(8)
C3 0.0123(10) 0.0129(11) 0.0140(10) -0.0022(8) -0.0010(9) -0.0001(8)
C4 0.0144(10) 0.0151(11) 0.0146(10) 0.0020(9) -0.0014(9) 0.0013(9)
C5 0.0268(14) 0.0227(13) 0.0385(15) 0.0054(11) 0.0117(12) -0.0010(10)
C6 0.0327(14) 0.0289(13) 0.0401(17) 0.0005(12) 0.0009(12) 0.0036(12)

_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
Br1 C3 1.890(2) . ?
Br2 C4 1.888(2) . ?
O1 C1 1.306(3) . ?
O2 C1 1.216(3) . ?
O3 C5 1.444(3) . ?
C1 C2 1.510(3) . ?
C2 C3 1.388(3) . ?
C2 C4 1.387(3) . ?
C3 C3 1.393(4) 8_575 ?
C4 C4 1.392(4) 8_575 ?
C5 C6 1.499(4) . ?

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 C1 C2 113.09(18) . . ?
O2 C1 O1 125.6(2) . . ?
O2 C1 C2 121.31(19) . . ?
C3 C2 C1 120.7(2) . . ?
C4 C2 C1 119.30(19) . . ?
C4 C2 C3 120.0(2) . . ?
C2 C3 Br1 118.56(17) . . ?
C2 C3 C3 119.97(13) . 8_575 ?
C3 C3 Br1 121.47(7) 8_575 . ?
C2 C4 Br2 118.46(17) . . ?
C2 C4 C4 120.03(13) . 8_575 ?
C4 C4 Br2 121.51(7) 8_575 . ?
O3 C5 C6 111.6(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O3 0.824(18) 1.699(19) 2.516(2) 171(3) . yes
O3 H3 O2 0.825(18) 1.930(19) 2.746(2) 170(3) 5_766 yes

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
O1 C1 C2 C3 -90.9(2) . . . . ?
O1 C1 C2 C4 90.8(2) . . . . ?
O2 C1 C2 C3 89.6(3) . . . . ?
O2 C1 C2 C4 -88.7(3) . . . . ?
C1 C2 C3 Br1 3.5(3) . . . . ?
C1 C2 C3 C3 -177.16(13) . . . 8_575 ?
C1 C2 C4 Br2 -2.5(3) . . . . ?
C1 C2 C4 C4 177.19(13) . . . 8_575 ?
C3 C2 C4 Br2 179.22(16) . . . . ?
C3 C2 C4 C4 -1.1(2) . . . 8_575 ?
C4 C2 C3 Br1 -178.25(16) . . . . ?
C4 C2 C3 C3 1.1(2) . . . 8_575 ?

_shelx_res_file                  
;
TITL kcnj10CuLT in Pnma
    2etoh_lt.res
    created by SHELXL-2018/3 at 17:55:18 on 18-Jul-2019
CELL 1.54184 9.278496 23.575417 8.602326 90 90 90
ZERR 4 0.000193 0.0005 0.000198 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H Br O
UNIT 48 56 16 24
EQIV $1 2-X,1-Y,1-Z
DFIX 0.84 O1 H1 O3 H3

L.S. 4
PLAN  8
SIZE 0.22 0.22 0.16
TEMP -173.13(10)
HTAB O1 O3
HTAB O3 O2_$1
CONF
fmap 2
ACTA
OMIT 0 135
REM <olex2.extras>
REM <HklSrc "%.\\2EtOH_LT.hkl">
REM </olex2.extras>

WGHT    0.054600    0.188900
FVAR       2.35008
BR1   3    0.695636    0.678627    0.285313    11.00000    0.01871    0.01204 =
         0.02345   -0.00215   -0.00828   -0.00134
BR2   3    1.147084    0.678621    0.721615    11.00000    0.02456    0.01478 =
         0.02472    0.00142   -0.01220    0.00293
O1    4    0.845390    0.603204    0.598980    11.00000    0.02612    0.01088 =
         0.02556    0.00236    0.00908    0.00037
H1    2    0.850824    0.568339    0.597987    11.00000    0.03353
O2    4    1.008259    0.602184    0.406255    11.00000    0.01733    0.01492 =
         0.02085   -0.00085    0.00384    0.00190
O3    4    0.834942    0.496573    0.601198    11.00000    0.02584    0.01203 =
         0.06237    0.00616    0.01728    0.00340
H3    2    0.888481    0.468855    0.591883    11.00000    0.04171
C1    1    0.929977    0.627077    0.496817    11.00000    0.01131    0.01300 =
         0.01673    0.00163   -0.00320    0.00057
C2    1    0.923807    0.691049    0.500898    11.00000    0.01614    0.01217 =
         0.01547    0.00020    0.00561   -0.00019
C3    1    0.826851    0.720468    0.408083    11.00000    0.01230    0.01288 =
         0.01405   -0.00222   -0.00105   -0.00012
C4    1    1.018887    0.720481    0.595551    11.00000    0.01442    0.01515 =
         0.01459    0.00199   -0.00140    0.00133
C5    1    0.698180    0.474930    0.655126    11.00000    0.02679    0.02272 =
         0.03848    0.00536    0.01168   -0.00104
AFIX  23
H5A   2    0.635291    0.507067    0.684897    11.00000   -1.20000
H5B   2    0.713923    0.451250    0.748638    11.00000   -1.20000
AFIX   0
C6    1    0.624455    0.440220    0.532642    11.00000    0.03275    0.02892 =
         0.04012    0.00049    0.00087    0.00356
AFIX 137
H6A   2    0.608538    0.463592    0.440009    11.00000   -1.50000
H6B   2    0.531579    0.426733    0.572352    11.00000   -1.50000
H6C   2    0.685057    0.407647    0.505502    11.00000   -1.50000
AFIX   0
HKLF 4




REM  kcnj10CuLT in Pnma
REM wR2 = 0.0809, GooF = S = 1.057, Restrained GooF = 1.056 for all data
REM R1 = 0.0294 for 1595 Fo > 4sig(Fo) and 0.0316 for all 1747 data
REM 109 parameters refined using 2 restraints

END

WGHT      0.0546      0.1889

REM Highest difference peak  1.010,  deepest hole -0.653,  1-sigma level  0.134
Q1    1   0.6978  0.6369  0.2826  11.00000  0.05    1.01
Q2    1   1.1428  0.6340  0.7238  11.00000  0.05    1.01
Q3    1   0.6899  0.7194  0.2841  11.00000  0.05    0.97
Q4    1   1.1435  0.7197  0.7239  11.00000  0.05    0.97
Q5    1   0.9234  0.6777  0.4966  11.00000  0.05    0.54
Q6    1   1.1016  0.7500  0.5828  10.50000  0.05    0.50
Q7    1   0.7452  0.7500  0.4176  10.50000  0.05    0.50
Q8    1   0.6957  0.7500  0.1405  10.50000  0.05    0.47
;
_shelx_res_checksum              79299
_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_4rt
_database_code_depnum_ccdc_archive 'CCDC 1941502'
loop_
_audit_author_name
_audit_author_address
'Kittipong Chainok'
;Thammasat University
Thailand
;
_audit_update_record             
;
2019-07-18 deposited with the CCDC.	2019-10-28 downloaded from the CCDC.
;
_audit_creation_date             2019-07-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H2 Br4 O4, 2(C2 H6 O S)'
_chemical_formula_sum            'C12 H14 Br4 O6 S2'
_chemical_formula_weight         637.99
_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'
Br Br -0.2901 2.4595 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   9.2133(2)
_cell_length_b                   25.7139(6)
_cell_length_c                   8.9323(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2116.15(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.839
_cell_measurement_theta_min      3.169
_shelx_estimated_absorpt_T_max   0.304
_shelx_estimated_absorpt_T_min   0.255
_exptl_absorpt_coefficient_mu    7.827
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0895 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.7972. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            52655
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         2.414
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'PHOTON area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle KAPPA diffractometer'
_diffrn_measurement_device_type  'BRUKER D8 CMOS PHOTON II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_monochromator  'graphiteDouble Bounce Multilayer Mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1927
_reflns_number_total             2683
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         1.408
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2683
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0446
_refine_ls_restrained_S_all      1.098
_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)+(0.0401P)²+7.5398P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1229
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.82 with sigma of 0.01
3.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   mixed
_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
Br1 Br 0.96244(6) 0.31500(2) 0.28090(6) 0.05080(19) Uani 1 1 d . . . . .
Br2 Br 0.52512(6) 0.31517(2) 0.72008(7) 0.0560(2) Uani 1 1 d . . . . .
S1 S 0.70616(16) 0.51568(5) 0.54426(16) 0.0520(3) Uani 1 1 d . . . . .
O1 O 0.8283(4) 0.38426(13) 0.5906(4) 0.0460(8) Uani 1 1 d D . . . .
O2 O 0.6582(4) 0.38576(12) 0.4143(4) 0.0488(9) Uani 1 1 d . . . . .
O3 O 0.8225(4) 0.48150(15) 0.6086(5) 0.0688(12) Uani 1 1 d . . . . .
C1 C 0.7397(4) 0.36285(15) 0.4989(5) 0.0312(8) Uani 1 1 d . . . . .
C2 C 0.7444(4) 0.30409(15) 0.5004(4) 0.0278(8) Uani 1 1 d . . . . .
C3 C 0.8367(4) 0.27706(15) 0.4072(5) 0.0310(8) Uani 1 1 d . . . . .
C4 C 0.6514(4) 0.27690(15) 0.5941(5) 0.0315(9) Uani 1 1 d . . . . .
C5 C 0.7922(10) 0.5749(3) 0.5021(9) 0.100(3) Uani 1 1 d . . . . .
H5A H 0.844508 0.586936 0.588390 0.150 Uiso 1 1 calc GR . . . .
H5B H 0.720544 0.600269 0.474461 0.150 Uiso 1 1 calc GR . . . .
H5C H 0.858515 0.569914 0.420485 0.150 Uiso 1 1 calc GR . . . .
C6 C 0.6028(7) 0.5363(3) 0.6995(7) 0.0695(17) Uani 1 1 d . . . . .
H6A H 0.556474 0.506781 0.744789 0.104 Uiso 1 1 calc GR . . . .
H6B H 0.530238 0.560607 0.666941 0.104 Uiso 1 1 calc GR . . . .
H6C H 0.665279 0.552741 0.771288 0.104 Uiso 1 1 calc GR . . . .
H1 H 0.833(13) 0.4160(6) 0.598(13) 0.19(5) Uiso 1 1 d 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
Br1 0.0593(3) 0.0325(3) 0.0606(4) 0.0052(2) 0.0290(3) -0.0046(2)
Br2 0.0626(4) 0.0393(3) 0.0660(4) -0.0063(2) 0.0327(3) 0.0069(2)
S1 0.0633(8) 0.0368(6) 0.0559(8) -0.0073(6) -0.0116(6) -0.0001(6)
O1 0.053(2) 0.0260(15) 0.059(2) -0.0037(15) -0.0201(17) 0.0042(14)
O2 0.055(2) 0.0300(16) 0.061(2) 0.0044(15) -0.0212(17) 0.0053(15)
O3 0.056(2) 0.0370(18) 0.113(4) -0.025(2) -0.017(2) 0.0056(18)
C1 0.033(2) 0.0222(18) 0.039(2) -0.0001(16) 0.0003(18) 0.0021(16)
C2 0.0313(18) 0.0213(17) 0.0308(18) -0.0030(15) -0.0015(16) 0.0012(15)
C3 0.033(2) 0.0256(19) 0.035(2) -0.0001(16) 0.0056(17) -0.0011(16)
C4 0.033(2) 0.0263(19) 0.035(2) -0.0022(16) 0.0065(17) 0.0019(16)
C5 0.130(7) 0.059(4) 0.112(7) 0.018(4) 0.020(6) -0.020(5)
C6 0.061(4) 0.074(4) 0.074(4) -0.007(3) -0.002(3) 0.018(3)

_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
Br1 C3 1.889(4) . ?
Br2 C4 1.894(4) . ?
S1 O3 1.501(4) . ?
S1 C5 1.758(7) . ?
S1 C6 1.764(6) . ?
O1 C1 1.280(5) . ?
O1 H1 0.821(10) . ?
O2 C1 1.218(5) . ?
C1 C2 1.512(5) . ?
C2 C3 1.378(5) . ?
C2 C4 1.387(5) . ?
C3 C3 1.392(8) 7_565 ?
C4 C4 1.384(8) 7_565 ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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 S1 C5 105.5(4) . . ?
O3 S1 C6 105.1(3) . . ?
C5 S1 C6 98.7(4) . . ?
C1 O1 H1 121(8) . . ?
O1 C1 C2 114.0(4) . . ?
O2 C1 O1 125.6(4) . . ?
O2 C1 C2 120.4(4) . . ?
C3 C2 C1 121.1(4) . . ?
C3 C2 C4 119.4(4) . . ?
C4 C2 C1 119.5(3) . . ?
C2 C3 Br1 118.6(3) . . ?
C2 C3 C3 120.3(2) . 7_565 ?
C3 C3 Br1 121.10(12) 7_565 . ?
C2 C4 Br2 118.4(3) . . ?
C4 C4 Br2 121.30(12) 7_565 . ?
C4 C4 C2 120.3(2) 7_565 . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S1 C6 H6A 109.5 . . ?
S1 C6 H6B 109.5 . . ?
S1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C6 H6B O2 0.96 2.33 3.291(7) 175.6 5_666 yes
O1 H1 O3 0.821(10) 1.689(18) 2.506(5) 173(12) . yes

_shelx_res_file                  
;
TITL KCNJ3_0m_a.res in Pnma
    4rt.res
    created by SHELXL-2018/3 at 18:18:38 on 18-Jul-2019
REM Old TITL KCNJ3_0m in Pnma
REM SHELXT solution in Pnma
REM R1 0.241, Rweak 0.010, Alpha 0.035, Orientation a'=b, b'=c, c'=a
REM Formula found by SHELXT: C6 Br2 O3 S
CELL 0.71073 9.2133 25.7139 8.9323 90 90 90
ZERR 4 0.0002 0.0006 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Br O S
UNIT 48 56 16 24 8
EQIV $1 0.5+X,+Y,0.5-Z
EQIV $2 -0.5+X,+Y,1.5-Z
EQIV $3 1-X,1-Y,1-Z
DFIX 0.82 0.01 O1 H1

L.S. 4
PLAN  10
SIZE 0.24 0.24 0.2
TEMP 23(2)
RTAB CBrO C3 Br1 O2_$1
RTAB BrO Br1 O2_$1
RTAB CBrO C4 Br2 O1_$2
RTAB BrO Br2 O1_$2
HTAB O1 O3
HTAB C6 O2_$3
BOND $H
LIST 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\4RT.hkl">
REM </olex2.extras>

WGHT    0.040100    7.539800
FVAR       0.21938
BR1   3    0.962437    0.314997    0.280899    11.00000    0.05931    0.03252 =
         0.06056    0.00518    0.02903   -0.00459
BR2   3    0.525118    0.315166    0.720081    11.00000    0.06259    0.03926 =
         0.06602   -0.00625    0.03267    0.00688
S1    5    0.706156    0.515677    0.544255    11.00000    0.06330    0.03680 =
         0.05594   -0.00731   -0.01156   -0.00012
O1    4    0.828282    0.384255    0.590636    11.00000    0.05281    0.02596 =
         0.05923   -0.00374   -0.02013    0.00424
O2    4    0.658184    0.385757    0.414266    11.00000    0.05522    0.02996 =
         0.06108    0.00442   -0.02119    0.00529
O3    4    0.822491    0.481499    0.608646    11.00000    0.05636    0.03697 =
         0.11320   -0.02548   -0.01721    0.00558
C1    1    0.739726    0.362850    0.498938    11.00000    0.03255    0.02221 =
         0.03871   -0.00011    0.00033    0.00208
C2    1    0.744358    0.304094    0.500417    11.00000    0.03126    0.02126 =
         0.03084   -0.00299   -0.00149    0.00121
C3    1    0.836719    0.277063    0.407239    11.00000    0.03259    0.02559 =
         0.03476   -0.00009    0.00557   -0.00113
C4    1    0.651362    0.276902    0.594136    11.00000    0.03310    0.02625 =
         0.03518   -0.00219    0.00655    0.00189
C5    1    0.792195    0.574923    0.502115    11.00000    0.12972    0.05897 =
         0.11189    0.01844    0.01972   -0.01998
AFIX 137
H5A   2    0.844508    0.586936    0.588390    11.00000   -1.50000
H5B   2    0.720544    0.600269    0.474461    11.00000   -1.50000
H5C   2    0.858515    0.569914    0.420485    11.00000   -1.50000
AFIX   0
C6    1    0.602754    0.536302    0.699510    11.00000    0.06067    0.07372 =
         0.07423   -0.00690   -0.00201    0.01754
AFIX 137
H6A   2    0.556474    0.506781    0.744789    11.00000   -1.50000
H6B   2    0.530238    0.560607    0.666941    11.00000   -1.50000
H6C   2    0.665279    0.552741    0.771288    11.00000   -1.50000
AFIX   0

H1    2    0.833181    0.416038    0.598139    11.00000    0.19095
HKLF 4




REM  KCNJ3_0m_a.res in Pnma
REM wR2 = 0.1229, GooF = S = 1.098, Restrained GooF = 1.098 for all data
REM R1 = 0.0446 for 1927 Fo > 4sig(Fo) and 0.0650 for all 2683 data
REM 115 parameters refined using 1 restraints

END

WGHT      0.0401      7.5399

REM Highest difference peak  1.408,  deepest hole -0.550,  1-sigma level  0.101
Q1    1   1.0423  0.3169  0.2085  11.00000  0.05    1.41
Q2    1   0.4765  0.3177  0.7829  11.00000  0.05    1.15
Q3    1   0.5963  0.3079  0.7605  11.00000  0.05    0.90
Q4    1   0.7957  0.5171  0.4545  11.00000  0.05    0.70
Q5    1   0.8847  0.3096  0.2443  11.00000  0.05    0.69
Q6    1   0.4896  0.2996  0.6702  11.00000  0.05    0.55
Q7    1   1.0000  0.3021  0.3384  11.00000  0.05    0.45
Q8    1   0.8166  0.5131  0.5547  11.00000  0.05    0.44
Q9    1   0.8484  0.2500  0.3958  10.50000  0.05    0.41
Q10   1   0.6428  0.2500  0.5994  10.50000  0.05    0.40
;
_shelx_res_checksum              51985
_olex2_submission_special_instructions 'No special instructions were received'
