# Electronic Supplementary Material (ESI) for ChemComm.
# 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_DY01
_database_code_depnum_ccdc_archive 'CCDC 1935565'
loop_
_audit_author_name
_audit_author_address
'Sanehiro Muromachi'
;National Institute of Advanced Industrial Science and Technology (AIST)
Japan
;
_audit_update_record             
;
2019-06-21 deposited with the CCDC.	2019-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H112 Br N O38 Xe1.17'
_chemical_formula_weight         1203.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Xe Xe -0.4205 1.9578 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_H-M_alt        'P m m a'
_space_group_name_Hall           '-P 2a 2a'

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

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

_cell_length_a                   21.088(5)
_cell_length_b                   12.630(3)
_cell_length_c                   12.063(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3212.9(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9983
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      28.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_F_000             1270
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.324
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_radiation_source         'rotating unit'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker, APEX2, CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17423
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.516
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_full        25.241
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4059
_reflns_number_gt                3869
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'Bruker SHELXTL'
_computing_molecular_graphics    ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0442P)²+2.4840P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4059
_refine_ls_number_parameters     387
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.192
_refine_ls_shift/su_mean         0.008

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 0.250000 0.500000 0.46749(2) 0.03361(3) Uani 1 4 d S T P . .
O1 O 0.18356(2) 0.000000 0.45569(4) 0.02531(12) Uani 1 2 d DS T P . .
H11 H 0.1680(7) 0.0603(6) 0.4917(11) 0.030 Uiso 0.25 1 d D U P . .
H12 H 0.2267(3) 0.000000 0.4674(12) 0.030 Uiso 0.5 2 d DS U P . .
H13 H 0.1626(5) 0.000000 0.3861(6) 0.030 Uiso 0.5 2 d DS U P . .
O2 O 0.10313(3) 0.500000 0.37376(4) 0.03041(13) Uani 1 2 d DS T P . .
H21 H 0.0902(8) 0.4322(6) 0.3939(15) 0.030 Uiso 0.25 1 d D U P . .
H22 H 0.1451(3) 0.500000 0.3774(14) 0.030 Uiso 0.5 2 d DS U P . .
O3 O 0.250000 0.28647(4) 0.61874(4) 0.03156(14) Uani 1 2 d DS T P . .
H31 H 0.250000 0.3532(6) 0.5864(10) 0.030 Uiso 0.5 2 d DS U P . .
H32 H 0.2122(4) 0.2534(10) 0.5990(15) 0.030 Uiso 0.25 1 d D U P . .
O4 O 0.07657(3) 0.500000 0.14449(5) 0.03436(14) Uani 1 2 d DS T P . .
H41 H 0.0832(8) 0.500000 0.2218(5) 0.030 Uiso 0.5 2 d DS U P . .
H42 H 0.0629(8) 0.4328(6) 0.1211(14) 0.030 Uiso 0.25 1 d D U P . .
O5 O 0.250000 0.22091(5) 0.83595(5) 0.03996(16) Uani 1 2 d DS T P . .
H51 H 0.2095(3) 0.2120(18) 0.8644(12) 0.030 Uiso 0.25 1 d D U P . .
H52 H 0.250000 0.2491(10) 0.7653(6) 0.030 Uiso 0.5 2 d DS U P . .
O6 O 0.05663(2) 0.30311(3) 0.44071(3) 0.02691(9) Uani 1 1 d D . . . .
H61 H 0.0702(8) 0.3718(6) 0.4194(15) 0.030 Uiso 0.25 1 d D U P . .
H62 H 0.0871(4) 0.2697(10) 0.4849(8) 0.006(4) Uiso 0.25 1 d D . P . .
H63 H 0.0513(10) 0.2681(10) 0.3732(6) 0.030 Uiso 0.25 1 d D U P . .
H64 H 0.0185(4) 0.2991(18) 0.4798(10) 0.030 Uiso 0.25 1 d D U P . .
O7 O 0.05598(2) 0.29852(3) 0.06031(3) 0.02892(9) Uani 1 1 d D . . . .
H71 H 0.0178(4) 0.2839(16) 0.0231(10) 0.030 Uiso 0.25 1 d D U P . .
H72 H 0.0615(10) 0.3693(6) 0.0851(14) 0.030 Uiso 0.25 1 d D U P . .
H73 H 0.0533(11) 0.2532(8) 0.1223(7) 0.030 Uiso 0.25 1 d D U P . .
H74 H 0.0888(4) 0.2640(10) 0.0210(10) 0.030 Uiso 0.25 1 d D U P . .
O8 O 0.13992(2) 0.17327(3) 0.94154(3) 0.02969(9) Uani 1 1 d D . . . .
H81 H 0.1506(9) 0.1132(7) 0.9839(9) 0.030 Uiso 0.25 1 d D U P . .
H82 H 0.1152(5) 0.1477(13) 0.8817(7) 0.030 Uiso 0.25 1 d D U P . .
H83 H 0.1128(5) 0.2182(8) 0.9826(10) 0.030 Uiso 0.25 1 d D U P . .
H84 H 0.1772(4) 0.1924(15) 0.9007(10) 0.030 Uiso 0.25 1 d D U P . .
O9 O 0.14135(2) 0.18113(3) 0.56236(3) 0.02733(9) Uani 1 1 d D . . . .
H91 H 0.1215(6) 0.1606(14) 0.6281(7) 0.030 Uiso 0.25 1 d D U P . .
H92 H 0.1126(5) 0.2264(8) 0.5269(11) 0.030 Uiso 0.25 1 d D U P . .
H93 H 0.1780(4) 0.2205(9) 0.5824(15) 0.030 Uiso 0.25 1 d D U P . .
H94 H 0.1526(9) 0.1149(6) 0.5311(12) 0.030 Uiso 0.25 1 d D U P . .
O10 O 0.11806(3) 0.000000 0.25741(4) 0.02722(13) Uani 1 2 d DS T P . .
H101 H 0.1419(5) 0.000000 0.3229(6) 0.030 Uiso 0.5 2 d DS U P . .
H102 H 0.1442(4) 0.000000 0.1959(6) 0.030 Uiso 0.6 2 d DS U P . .
H103 H 0.0992(7) 0.0672(6) 0.2654(18) 0.030 Uiso 0.25 1 d D U P . .
O11 O 0.18387(2) 0.000000 0.06064(4) 0.02794(13) Uani 1 2 d DS T P . .
H111 H 0.1644(6) 0.000000 0.1296(6) 0.030 Uiso 0.5 2 d DS U P . .
H112 H 0.2278(3) 0.000000 0.0601(14) 0.030 Uiso 0.5 2 d DS U P . .
H113 H 0.1648(7) 0.0631(6) 0.0341(13) 0.030 Uiso 0.25 1 d D U P . .
O12 O 0.08060(2) 0.10929(3) 0.74983(3) 0.02830(9) Uani 1 1 d D . . . .
H121 H 0.1019(6) 0.1307(14) 0.6838(7) 0.030 Uiso 0.25 1 d D U P . .
H122 H 0.0991(7) 0.1315(14) 0.8180(6) 0.030 Uiso 0.25 1 d D U P . .
H123 H 0.0777(11) 0.0348(5) 0.7490(16) 0.030 Uiso 0.25 1 d D U P . .
H124 H 0.0380(3) 0.1338(13) 0.7558(17) 0.030 Uiso 0.25 1 d D U P . .
O13 O 0.04234(2) 0.18054(3) 0.25205(3) 0.02757(9) Uani 1 1 d D . . . .
H131 H 0.0688(5) 0.1208(7) 0.2552(18) 0.030 Uiso 0.25 1 d D U P . .
H132 H 0.0001(3) 0.1572(14) 0.2521(17) 0.030 Uiso 0.25 1 d D U P . .
H133 H 0.0488(10) 0.2171(10) 0.3187(6) 0.030 Uiso 0.25 1 d D U P . .
H134 H 0.0489(10) 0.2196(9) 0.1865(7) 0.030 Uiso 0.25 1 d D U P . .
N1 N 0.2487(3) 0.49451(18) -0.00429(7) 0.01937(19) Uani 0.25 1 d . . P A -1
C1A C 0.19456(7) 0.45842(13) -0.07702(13) 0.0140(3) Uani 0.25 1 d . U P A -1
H1A1 H 0.161275 0.432977 -0.028335 0.017 Uiso 0.25 1 calc R U P A -1
H1A2 H 0.209503 0.397833 -0.118971 0.017 Uiso 0.25 1 calc R U P A -1
C2A C 0.16398(8) 0.53429(13) -0.15901(14) 0.0200(4) Uani 0.25 1 d . . P A -1
H2A1 H 0.148550 0.596696 -0.120666 0.024 Uiso 0.25 1 calc R U P A -1
H2A2 H 0.194725 0.556466 -0.214120 0.024 Uiso 0.25 1 calc R U P A -1
C3A C 0.10970(8) 0.47719(16) -0.21402(17) 0.0338(8) Uani 0.25 1 d . . P A -1
H3A1 H 0.076210 0.466265 -0.160104 0.041 Uiso 0.25 1 calc R U P A -1
H3A2 H 0.124160 0.408156 -0.238568 0.041 Uiso 0.25 1 calc R U P A -1
C4A C 0.08339(14) 0.5363(3) -0.3111(2) 0.0823(17) Uani 0.25 1 d . . P A -1
H4A1 H 0.066186 0.602595 -0.286495 0.123 Uiso 0.25 1 calc R U P A -1
H4A2 H 0.050525 0.495021 -0.345269 0.123 Uiso 0.25 1 calc R U P A -1
H4A3 H 0.116580 0.549108 -0.363900 0.123 Uiso 0.25 1 calc R U P A -1
C1B C 0.27281(10) 0.41487(17) 0.06261(19) 0.0325(5) Uani 0.25 1 d . . P A -1
H1B1 H 0.309638 0.444295 0.099640 0.039 Uiso 0.25 1 calc R U P A -1
H1B2 H 0.288423 0.360168 0.013209 0.039 Uiso 0.25 1 calc R U P A -1
C2B C 0.23299(8) 0.35723(13) 0.15398(13) 0.0226(5) Uani 0.25 1 d . . P A -1
H2B1 H 0.215296 0.409759 0.203828 0.027 Uiso 0.25 1 calc R U P A -1
H2B2 H 0.197947 0.320415 0.118938 0.027 Uiso 0.25 1 calc R U P A -1
C3B C 0.26974(7) 0.28191(13) 0.21792(14) 0.0176(4) Uani 0.25 1 d . . P A -1
H3B1 H 0.303696 0.318890 0.255916 0.021 Uiso 0.25 1 calc R U P A -1
H3B2 H 0.288793 0.230648 0.168153 0.021 Uiso 0.25 1 calc R U P A -1
C4B C 0.22916(9) 0.22449(14) 0.30226(16) 0.0265(5) Uani 0.25 1 d . . P A -1
H4B1 H 0.208879 0.275208 0.349775 0.040 Uiso 0.25 1 calc R U P A -1
H4B2 H 0.255372 0.178425 0.345929 0.040 Uiso 0.25 1 calc R U P A -1
H4B3 H 0.197490 0.183447 0.264554 0.040 Uiso 0.25 1 calc R U P A -1
C1C C 0.30052(10) 0.54993(19) -0.07282(19) 0.0338(5) Uani 0.25 1 d . . P A -1
H1C1 H 0.282781 0.612969 -0.106698 0.041 Uiso 0.25 1 calc R U P A -1
H1C2 H 0.334431 0.572038 -0.023662 0.041 Uiso 0.25 1 calc R U P A -1
C2C C 0.32810(8) 0.47900(17) -0.16357(17) 0.0351(8) Uani 0.25 1 d . . P A -1
H2C1 H 0.344395 0.414721 -0.130021 0.042 Uiso 0.25 1 calc R U P A -1
H2C2 H 0.294504 0.459120 -0.214394 0.042 Uiso 0.25 1 calc R U P A -1
C3C C 0.38038(10) 0.53181(18) -0.22757(17) 0.0351(6) Uani 0.25 1 d . . P A -1
H3C1 H 0.410070 0.563003 -0.175565 0.042 Uiso 0.25 1 calc R U P A -1
H3C2 H 0.362360 0.588811 -0.271312 0.042 Uiso 0.25 1 calc R U P A -1
C4C C 0.41738(12) 0.4556(2) -0.3065(2) 0.0425(5) Uani 0.25 1 d . U P A -1
H4C1 H 0.437434 0.401040 -0.263498 0.064 Uiso 0.25 1 calc R U P A -1
H4C2 H 0.449058 0.494811 -0.346186 0.064 Uiso 0.25 1 calc R U P A -1
H4C3 H 0.388386 0.424004 -0.358149 0.064 Uiso 0.25 1 calc R U P A -1
C1D C 0.21988(7) 0.59064(11) 0.06824(12) 0.0112(3) Uani 0.25 1 d . U P A -1
H1D1 H 0.207929 0.648182 0.019252 0.013 Uiso 0.25 1 calc R U P A -1
H1D2 H 0.182001 0.566605 0.106278 0.013 Uiso 0.25 1 calc R U P A -1
C2D C 0.26624(7) 0.62970(14) 0.15059(17) 0.0245(5) Uani 0.25 1 d . . P A -1
H2D1 H 0.305232 0.650851 0.114127 0.029 Uiso 0.25 1 calc R U P A -1
H2D2 H 0.276004 0.574675 0.204021 0.029 Uiso 0.25 1 calc R U P A -1
C3D C 0.2339(2) 0.7302(2) 0.2118(3) 0.0772(16) Uani 0.25 1 d . . P A -1
H3D1 H 0.224476 0.784072 0.156978 0.093 Uiso 0.25 1 calc R U P A -1
H3D2 H 0.194181 0.708023 0.244925 0.093 Uiso 0.25 1 calc R U P A -1
C4D C 0.27603(16) 0.7783(3) 0.3017(3) 0.0677(10) Uani 0.25 1 d . . P A -1
H4D1 H 0.279212 0.729925 0.362879 0.102 Uiso 0.25 1 calc R U P A -1
H4D2 H 0.257828 0.843694 0.326779 0.102 Uiso 0.25 1 calc R U P A -1
H4D3 H 0.317525 0.791406 0.271999 0.102 Uiso 0.25 1 calc R U P A -1
Xe11 Xe 0.250000 0.000000 0.7305(2) 0.0529(6) Uiso 0.0350(3) 4 d S . P B 2
Xe21 Xe 0.000000 0.000000 0.500000 0.02243(2) Uiso 0.42203(19) 4 d S . P C 4
Xe22 Xe 0.000000 0.01598(4) 0.500000 0.02243(2) Uiso 0.06887(11) 2 d S . P D 5
Xe31 Xe 0.000000 0.000000 0.000000 0.01932(2) Uiso 0.42579(18) 4 d S . P E 6
Xe32 Xe 0.00915(5) 0.000000 0.01843(9) 0.01932(2) Uiso 0.03236(12) 2 d S . P F
7
Xe33 Xe 0.000000 0.02298(9) 0.000000 0.01932(2) Uiso 0.02801(12) 2 d S . P G 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
O1 H11 0.936(10) . ?
O1 H12 0.921(7) . ?
O1 H13 0.950(8) . ?
O2 H21 0.931(9) . ?
O2 H22 0.886(7) . ?
O3 H31 0.929(8) . ?
O3 H32 0.932(9) . ?
O4 H41 0.943(7) . ?
O4 H42 0.940(9) . ?
O5 H51 0.928(9) . ?
O5 H52 0.923(8) . ?
O6 H61 0.949(9) . ?
O6 H62 0.935(9) . ?
O6 H63 0.934(9) . ?
O6 H64 0.933(9) . ?
O7 H71 0.940(9) . ?
O7 H72 0.950(9) . ?
O7 H73 0.943(9) . ?
O7 H74 0.944(10) . ?
O8 H81 0.942(9) . ?
O8 H82 0.948(10) . ?
O8 H83 0.946(10) . ?
O8 H84 0.958(10) . ?
O9 H91 0.934(9) . ?
O9 H92 0.937(10) . ?
O9 H93 0.950(10) . ?
O9 H94 0.947(9) . ?
O10 H101 0.936(8) . ?
O10 H102 0.925(8) . ?
O10 H103 0.942(9) . ?
O11 H111 0.927(8) . ?
O11 H112 0.927(6) . ?
O11 H113 0.948(10) . ?
O12 H121 0.954(10) . ?
O12 H122 0.952(9) . ?
O12 H123 0.943(7) . ?
O12 H124 0.953(8) . ?
O13 H131 0.940(9) . ?
O13 H132 0.937(8) . ?
O13 H133 0.937(9) . ?
O13 H134 0.942(9) . ?
N1 C1B 1.386(3) . ?
N1 C1A 1.511(4) . ?
N1 C1C 1.539(5) . ?
N1 C1D 1.615(3) . ?
C1A C2A 1.521(2) . ?
C1A H1A1 0.9700 . ?
C1A H1A2 0.9700 . ?
C2A C3A 1.507(3) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C3A C4A 1.495(4) . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C4A H4A1 0.9600 . ?
C4A H4A2 0.9600 . ?
C4A H4A3 0.9600 . ?
C1B C2B 1.565(3) . ?
C1B H1B1 0.9700 . ?
C1B H1B2 0.9700 . ?
C2B C3B 1.449(2) . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
C3B C4B 1.515(2) . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C4B H4B1 0.9600 . ?
C4B H4B2 0.9600 . ?
C4B H4B3 0.9600 . ?
C1C C2C 1.529(3) . ?
C1C H1C1 0.9700 . ?
C1C H1C2 0.9700 . ?
C2C C3C 1.502(3) . ?
C2C H2C1 0.9700 . ?
C2C H2C2 0.9700 . ?
C3C C4C 1.563(3) . ?
C3C H3C1 0.9700 . ?
C3C H3C2 0.9700 . ?
C4C H4C1 0.9600 . ?
C4C H4C2 0.9600 . ?
C4C H4C3 0.9600 . ?
C1D C2D 1.479(2) . ?
C1D H1D1 0.9700 . ?
C1D H1D2 0.9700 . ?
C2D C3D 1.619(4) . ?
C2D H2D1 0.9700 . ?
C2D H2D2 0.9700 . ?
C3D C4D 1.527(5) . ?
C3D H3D1 0.9700 . ?
C3D H3D2 0.9700 . ?
C4D H4D1 0.9600 . ?
C4D H4D2 0.9600 . ?
C4D H4D3 0.9600 . ?
Xe32 Xe32 0.589(2) 5 ?
Xe33 Xe33 0.580(2) 5 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H11 O1 H12 106.0(11) . . ?
H11 O1 H13 104.3(9) . . ?
H12 O1 H13 126.6(11) . . ?
H21 O2 H22 106.2(11) . . ?
H31 O3 H32 107.4(10) . . ?
H41 O4 H42 110.1(10) . . ?
H51 O5 H52 112.8(10) . . ?
H61 O6 H62 111.1(13) . . ?
H61 O6 H63 103.5(13) . . ?
H62 O6 H63 111.5(13) . . ?
H61 O6 H64 116.5(17) . . ?
H62 O6 H64 106.2(11) . . ?
H63 O6 H64 108.1(16) . . ?
H71 O7 H72 116.1(17) . . ?
H71 O7 H73 101.9(16) . . ?
H72 O7 H73 109.2(12) . . ?
H71 O7 H74 107.3(11) . . ?
H72 O7 H74 120.1(15) . . ?
H73 O7 H74 99.3(14) . . ?
H81 O8 H82 105.7(12) . . ?
H81 O8 H83 110.1(11) . . ?
H82 O8 H83 105.7(11) . . ?
H81 O8 H84 106.6(15) . . ?
H82 O8 H84 98.4(10) . . ?
H83 O8 H84 127.8(13) . . ?
H91 O9 H92 105.5(12) . . ?
H91 O9 H93 107.1(14) . . ?
H92 O9 H93 108.9(10) . . ?
H91 O9 H94 101.9(14) . . ?
H92 O9 H94 121.2(12) . . ?
H93 O9 H94 111.1(13) . . ?
H101 O10 H102 110.9(8) . . ?
H101 O10 H103 98.0(12) . . ?
H102 O10 H103 109.5(12) . . ?
H111 O11 H112 116.6(12) . . ?
H111 O11 H113 96.6(10) . . ?
H112 O11 H113 114.9(9) . . ?
H121 O12 H122 116.4(11) . . ?
H121 O12 H123 107.8(16) . . ?
H122 O12 H123 109.2(16) . . ?
H121 O12 H124 114.5(15) . . ?
H122 O12 H124 103.0(15) . . ?
H123 O12 H124 105.3(18) . . ?
H131 O13 H132 108.1(12) . . ?
H131 O13 H133 105.9(16) . . ?
H132 O13 H133 107.0(17) . . ?
H131 O13 H134 111.5(16) . . ?
H132 O13 H134 107.7(17) . . ?
H133 O13 H134 116.2(10) . . ?
C1B N1 C1A 113.3(2) . . ?
C1B N1 C1C 112.5(4) . . ?
C1A N1 C1C 111.23(11) . . ?
C1B N1 C1D 111.60(12) . . ?
C1A N1 C1D 104.9(3) . . ?
C1C N1 C1D 102.50(18) . . ?
N1 C1A C2A 120.55(15) . . ?
N1 C1A H1A1 107.2 . . ?
C2A C1A H1A1 107.2 . . ?
N1 C1A H1A2 107.2 . . ?
C2A C1A H1A2 107.2 . . ?
H1A1 C1A H1A2 106.8 . . ?
C3A C2A C1A 107.88(14) . . ?
C3A C2A H2A1 110.1 . . ?
C1A C2A H2A1 110.1 . . ?
C3A C2A H2A2 110.1 . . ?
C1A C2A H2A2 110.1 . . ?
H2A1 C2A H2A2 108.4 . . ?
C2A C3A C4A 112.8(2) . . ?
C2A C3A H3A1 109.0 . . ?
C4A C3A H3A1 109.0 . . ?
C2A C3A H3A2 109.0 . . ?
C4A C3A H3A2 109.0 . . ?
H3A1 C3A H3A2 107.8 . . ?
C3A C4A H4A1 109.5 . . ?
C3A C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C3A C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
N1 C1B C2B 123.4(3) . . ?
N1 C1B H1B1 106.5 . . ?
C2B C1B H1B1 106.5 . . ?
N1 C1B H1B2 106.5 . . ?
C2B C1B H1B2 106.5 . . ?
H1B1 C1B H1B2 106.5 . . ?
C3B C2B C1B 113.14(14) . . ?
C3B C2B H2B1 108.9 . . ?
C1B C2B H2B1 108.9 . . ?
C3B C2B H2B2 109.0 . . ?
C1B C2B H2B2 108.9 . . ?
H2B1 C2B H2B2 107.8 . . ?
C2B C3B C4B 111.69(14) . . ?
C2B C3B H3B1 109.3 . . ?
C4B C3B H3B1 109.3 . . ?
C2B C3B H3B2 109.3 . . ?
C4B C3B H3B2 109.3 . . ?
H3B1 C3B H3B2 107.9 . . ?
C3B C4B H4B1 109.5 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
C2C C1C N1 112.84(18) . . ?
C2C C1C H1C1 109.0 . . ?
N1 C1C H1C1 109.0 . . ?
C2C C1C H1C2 109.0 . . ?
N1 C1C H1C2 109.0 . . ?
H1C1 C1C H1C2 107.8 . . ?
C3C C2C C1C 112.76(18) . . ?
C3C C2C H2C1 109.0 . . ?
C1C C2C H2C1 109.0 . . ?
C3C C2C H2C2 109.0 . . ?
C1C C2C H2C2 109.0 . . ?
H2C1 C2C H2C2 107.8 . . ?
C2C C3C C4C 113.94(19) . . ?
C2C C3C H3C1 108.8 . . ?
C4C C3C H3C1 108.8 . . ?
C2C C3C H3C2 108.8 . . ?
C4C C3C H3C2 108.8 . . ?
H3C1 C3C H3C2 107.7 . . ?
C3C C4C H4C1 109.5 . . ?
C3C C4C H4C2 109.5 . . ?
H4C1 C4C H4C2 109.5 . . ?
C3C C4C H4C3 109.5 . . ?
H4C1 C4C H4C3 109.5 . . ?
H4C2 C4C H4C3 109.5 . . ?
C2D C1D N1 111.5(2) . . ?
C2D C1D H1D1 109.3 . . ?
N1 C1D H1D1 109.3 . . ?
C2D C1D H1D2 109.3 . . ?
N1 C1D H1D2 109.3 . . ?
H1D1 C1D H1D2 108.0 . . ?
C1D C2D C3D 106.87(18) . . ?
C1D C2D H2D1 110.3 . . ?
C3D C2D H2D1 110.3 . . ?
C1D C2D H2D2 110.3 . . ?
C3D C2D H2D2 110.3 . . ?
H2D1 C2D H2D2 108.6 . . ?
C4D C3D C2D 113.0(3) . . ?
C4D C3D H3D1 109.0 . . ?
C2D C3D H3D1 109.0 . . ?
C4D C3D H3D2 109.0 . . ?
C2D C3D H3D2 109.0 . . ?
H3D1 C3D H3D2 107.8 . . ?
C3D C4D H4D1 109.5 . . ?
C3D C4D H4D2 109.5 . . ?
H4D1 C4D H4D2 109.5 . . ?
C3D C4D H4D3 109.5 . . ?
H4D1 C4D H4D3 109.5 . . ?
H4D2 C4D H4D3 109.5 . . ?

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
C1B N1 C1A C2A -177.7(2) . . . . ?
C1C N1 C1A C2A -49.7(3) . . . . ?
C1D N1 C1A C2A 60.4(2) . . . . ?
N1 C1A C2A C3A -177.0(2) . . . . ?
C1A C2A C3A C4A -169.35(18) . . . . ?
C1A N1 C1B C2B -62.4(3) . . . . ?
C1C N1 C1B C2B 170.35(17) . . . . ?
C1D N1 C1B C2B 55.8(4) . . . . ?
N1 C1B C2B C3B -176.12(19) . . . . ?
C1B C2B C3B C4B -177.67(15) . . . . ?
C1B N1 C1C C2C 69.6(2) . . . . ?
C1A N1 C1C C2C -58.8(3) . . . . ?
C1D N1 C1C C2C -170.37(18) . . . . ?
N1 C1C C2C C3C -177.8(2) . . . . ?
C1C C2C C3C C4C 169.90(18) . . . . ?
C1B N1 C1D C2D 52.6(4) . . . . ?
C1A N1 C1D C2D 175.67(14) . . . . ?
C1C N1 C1D C2D -68.1(2) . . . . ?
N1 C1D C2D C3D 176.24(18) . . . . ?
C1D C2D C3D C4D 178.8(2) . . . . ?

_refine_diff_density_max         1.362
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_DY03
_database_code_depnum_ccdc_archive 'CCDC 1935567'
loop_
_audit_author_name
_audit_author_address
'Sanehiro Muromachi'
;National Institute of Advanced Industrial Science and Technology (AIST)
Japan
;
_audit_update_record             
;
2019-06-21 deposited with the CCDC.	2019-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            
'Tetra-n-butylammonium bromide + Krypton hydrate'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H112 Br 1.05Kr N O38'
_chemical_formula_weight         1090.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Kr Kr -0.5574 2.7079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_H-M_alt        'P m m a'
_space_group_name_Hall           '-P 2a 2a'

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

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

_cell_length_a                   21.064(3)
_cell_length_b                   12.6451(19)
_cell_length_c                   12.0298(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3204.2(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9799
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.43

_exptl_crystal_description       chunk
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             1180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_min          0.15
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_max          0.2
_exptl_absorpt_coefficient_mu    1.405
_shelx_estimated_absorpt_T_min   0.763
_shelx_estimated_absorpt_T_max   0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating unit'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker, APEX2, CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17543
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.337
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.241
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4113
_reflns_number_gt                3800
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0477P)²+4.8853P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4113
_refine_ls_number_parameters     428
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1272
_refine_ls_wR_factor_gt          0.1251
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.166
_refine_ls_shift/su_mean         0.014

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 0.250000 0.500000 0.52978(2) 0.03463(4) Uani 1 4 d S T P . .
O1 O 0.18351(3) 0.000000 0.54351(6) 0.02569(17) Uani 1 2 d DS T P . .
H11 H 0.1646(7) 0.0589(7) 0.5112(11) 0.074(8) Uiso 0.5 1 d D . P . .
H12 H 0.1524(5) 0.000000 0.6005(8) 0.21(3) Uiso 0.5 2 d DS . P . .
H13 H 0.2278(3) 0.000000 0.539(2) 0.058(10) Uiso 0.5 2 d DS . P . .
O2 O 0.10351(4) 0.500000 0.62598(6) 0.0314(2) Uani 1 2 d DS T P . .
H21 H 0.0927(6) 0.4375(6) 0.5964(9) 0.020(4) Uiso 0.5 1 d D . P . .
O3 O 0.250000 0.28517(6) 0.37982(6) 0.0330(2) Uani 1 2 d DS T P . .
H31 H 0.2155(4) 0.2518(10) 0.4134(11) 0.061(7) Uiso 0.5 1 d D . P . .
H32 H 0.250000 0.3510(6) 0.4164(9) 0.073(5) Uiso 1 2 d DS . P . .
O4 O 0.07641(4) 0.500000 0.85598(7) 0.0350(2) Uani 1 2 d DS T P . .
H41 H 0.0829(8) 0.500000 0.7784(5) 0.065(5) Uiso 1 2 d DS . P . .
H42 H 0.0708(8) 0.4355(6) 0.8924(9) 0.036(5) Uiso 0.5 1 d D . P . .
O5 O 0.05659(2) 0.30336(4) 0.55920(4) 0.02761(13) Uani 1 1 d D . . . .
H51 H 0.0489(7) 0.2681(9) 0.6257(6) 0.023(4) Uiso 0.5 1 d D . P . .
H52 H 0.0196(3) 0.3089(11) 0.5149(8) 0.018(4) Uiso 0.5 1 d D . P . .
H53 H 0.0683(6) 0.3718(5) 0.5815(11) 0.023(4) Uiso 0.5 1 d D . P . .
H54 H 0.0788(7) 0.2751(13) 0.5318(12) 0.021(4) Uiso 0.5 1 d . . P . .
O6 O 0.14103(2) 0.18050(4) 0.43708(4) 0.02766(13) Uani 1 1 d D . . . .
H61 H 0.1769(4) 0.2135(11) 0.4071(12) 0.076(8) Uiso 0.5 1 d D . P . .
H62 H 0.1190(5) 0.1464(9) 0.3791(7) 0.026(4) Uiso 0.5 1 d D . P . .
H63 H 0.1088(4) 0.2203(8) 0.4739(9) 0.021(4) Uiso 0.5 1 d D . P . .
H64 H 0.1524(7) 0.1189(6) 0.4757(9) 0.039(5) Uiso 0.5 1 d D . P . .
O7 O 0.11810(4) 0.000000 0.74175(6) 0.02729(18) Uani 1 2 d DS T P . .
H71 H 0.1425(5) 0.000000 0.6766(7) 0.028(6) Uiso 0.5 2 d DS . P . .
H72 H 0.1035(7) 0.0695(6) 0.7402(15) 0.046(6) Uiso 0.5 1 d D . P . .
H73 H 0.1448(5) 0.000000 0.8045(7) 0.099(14) Uiso 0.5 2 d DS . P . .
O8 O 0.18373(3) 0.000000 0.93903(6) 0.02839(18) Uani 1 2 d DS T P . .
H81 H 0.1529(5) 0.000000 0.8821(8) 0.120(17) Uiso 0.5 2 d DS . P . .
H82 H 0.2283(3) 0.000000 0.935(3) 0.091(13) Uiso 0.5 2 d DS . P . .
H83 H 0.1686(8) 0.0649(6) 0.9665(14) 0.018(7) Uiso 0.25 1 d D . P . .
O9 O 0.250000 0.22128(8) 0.16175(7) 0.0411(2) Uani 1 2 d DS T P . .
H91 H 0.250000 0.2555(11) 0.2310(6) 0.036(7) Uiso 0.5 2 d DS . P . .
H92 H 0.2107(4) 0.2103(16) 0.1301(11) 0.062(7) Uiso 0.5 1 d D . P . .
O10 O 0.05595(2) 0.29846(4) 0.93947(4) 0.02954(13) Uani 1 1 d D . . . .
H101 H 0.0499(6) 0.2569(7) 0.8765(6) 0.009(3) Uiso 0.5 1 d D . P . .
H102 H 0.0876(4) 0.2569(8) 0.9710(10) 0.029(4) Uiso 0.5 1 d D . P . .
H103 H 0.01824(10) 0.2997(11) 0.9828(3) 0.017(4) Uiso 0.5 1 d D . P . .
H104 H 0.0582(9) 0.3671(6) 0.9109(11) 0.045(5) Uiso 0.5 1 d D . P . .
O11 O 0.13946(2) 0.17203(4) 0.05817(4) 0.03023(13) Uani 1 1 d D . . . .
H111 H 0.1513(6) 0.1150(6) 0.0138(8) 0.015(3) Uiso 0.5 1 d D . P . .
H112 H 0.1093(4) 0.2137(8) 0.0214(9) 0.022(4) Uiso 0.5 1 d D . P . .
H113 H 0.1753(4) 0.1879(16) 0.1013(9) 0.005(6) Uiso 0.25 1 d D . P . .
H114 H 0.1164(5) 0.1375(9) 0.1154(7) 0.036(5) Uiso 0.5 1 d D . P . .
O12 O 0.07968(3) 0.10885(4) 0.25001(4) 0.02839(13) Uani 1 1 d D . . . .
H121 H 0.0880(8) 0.0363(5) 0.2522(13) 0.045(6) Uiso 0.5 1 d D . P . .
H122 H 0.0972(6) 0.1341(10) 0.1840(6) 0.026(4) Uiso 0.5 1 d D . P . .
H123 H 0.0357(3) 0.1112(18) 0.2480(15) 0.048(6) Uiso 0.5 1 d D . P . .
H124 H 0.0997(6) 0.1361(11) 0.3129(7) 0.046(5) Uiso 0.5 1 d D . P . .
O13 O 0.04276(3) 0.18030(4) 0.74762(4) 0.02819(13) Uani 1 1 d D . . . .
H131 H 0.0656(5) 0.1169(6) 0.7453(10) 0.006(3) Uiso 0.5 1 d D . P . .
H132 H -0.0010(3) 0.1678(13) 0.7480(11) 0.021(4) Uiso 0.5 1 d D . P . .
H133 H 0.0420(17) 0.2189(10) 0.6800(7) 0.142(14) Uiso 0.5 1 d D . P . .
H134 H 0.0429(14) 0.2173(10) 0.8166(7) 0.110(11) Uiso 0.5 1 d D . P . .
N1 N 0.2509(2) 0.5030(3) 0.00328(9) 0.0199(3) Uani 0.25 1 d D U P A -1
C1A C 0.30403(11) 0.4604(2) 0.0736(2) 0.0296(7) Uani 0.25 1 d D . P A -1
H1A1 H 0.337911 0.438354 0.024138 0.036 Uiso 0.25 1 calc R U P A -1
H1A2 H 0.288578 0.397364 0.110829 0.036 Uiso 0.25 1 calc R U P A -1
C2A C 0.33273(10) 0.53246(18) 0.16136(17) 0.0203(6) Uani 0.25 1 d D U P A -1
H2A1 H 0.299482 0.558131 0.210179 0.024 Uiso 0.25 1 calc R U P A -1
H2A2 H 0.352238 0.593039 0.125576 0.024 Uiso 0.25 1 calc R U P A -1
C3A C 0.38298(12) 0.4729(2) 0.23027(19) 0.0302(9) Uani 0.25 1 d D . P A -1
H3A1 H 0.362411 0.419743 0.275916 0.036 Uiso 0.25 1 calc R U P A -1
H3A2 H 0.412448 0.437328 0.180846 0.036 Uiso 0.25 1 calc R U P A -1
C4A C 0.41936(14) 0.5509(3) 0.3049(2) 0.0406(8) Uani 0.25 1 d D . P A -1
H4A1 H 0.436337 0.607077 0.260227 0.061 Uiso 0.25 1 calc R U P A -1
H4A2 H 0.453436 0.514507 0.341576 0.061 Uiso 0.25 1 calc R U P A -1
H4A3 H 0.390995 0.579777 0.359500 0.061 Uiso 0.25 1 calc R U P A -1
C1B C 0.19821(10) 0.54871(19) 0.07418(17) 0.0191(5) Uani 0.25 1 d D U P A -1
H1B1 H 0.164998 0.573860 0.024982 0.023 Uiso 0.25 1 calc R U P A -1
H1B2 H 0.214928 0.609719 0.113319 0.023 Uiso 0.25 1 calc R U P A -1
C2B C 0.16829(12) 0.4757(2) 0.1588(2) 0.0427(12) Uani 0.25 1 d D . P A -1
H2B1 H 0.198895 0.459205 0.216488 0.051 Uiso 0.25 1 calc R U P A -1
H2B2 H 0.155946 0.410064 0.123052 0.051 Uiso 0.25 1 calc R U P A -1
C3B C 0.10964(13) 0.5284(3) 0.2108(2) 0.0425(12) Uani 0.25 1 d D . P A -1
H3B1 H 0.120230 0.600416 0.231608 0.051 Uiso 0.25 1 calc R U P A -1
H3B2 H 0.075984 0.531503 0.155845 0.051 Uiso 0.25 1 calc R U P A -1
C4B C 0.08575(17) 0.4694(3) 0.3129(3) 0.0588(15) Uani 0.25 1 d D . P A -1
H4B1 H 0.070624 0.400860 0.291178 0.088 Uiso 0.25 1 calc R U P A -1
H4B2 H 0.051770 0.508636 0.346479 0.088 Uiso 0.25 1 calc R U P A -1
H4B3 H 0.119794 0.461625 0.365271 0.088 Uiso 0.25 1 calc R U P A -1
C1C C 0.27751(12) 0.58939(19) -0.0674(2) 0.0256(2) Uani 0.25 1 d D U P A -1
H1C1 H 0.315306 0.562582 -0.103815 0.031 Uiso 0.25 1 calc R U P A -1
H1C2 H 0.290735 0.646513 -0.018811 0.031 Uiso 0.25 1 calc R U P A -1
C2C C 0.23441(10) 0.63539(19) -0.15577(16) 0.0231(7) Uani 0.25 1 d D . P A -1
H2C1 H 0.198060 0.668845 -0.120927 0.028 Uiso 0.25 1 calc R U P A -1
H2C2 H 0.219031 0.579327 -0.203763 0.028 Uiso 0.25 1 calc R U P A -1
C3C C 0.27108(12) 0.7172(2) -0.2250(2) 0.0234(6) Uani 0.25 1 d D . P A -1
H3C1 H 0.292062 0.766887 -0.175753 0.028 Uiso 0.25 1 calc R U P A -1
H3C2 H 0.303423 0.681669 -0.268580 0.028 Uiso 0.25 1 calc R U P A -1
C4C C 0.22626(16) 0.7771(2) -0.3026(3) 0.0427(9) Uani 0.25 1 d D . P A -1
H4C1 H 0.205388 0.727919 -0.351154 0.064 Uiso 0.25 1 calc R U P A -1
H4C2 H 0.250132 0.826866 -0.346016 0.064 Uiso 0.25 1 calc R U P A -1
H4C3 H 0.195093 0.814188 -0.259317 0.064 Uiso 0.25 1 calc R U P A -1
C1D C 0.22375(11) 0.41377(17) -0.06442(18) 0.0197(6) Uani 0.25 1 d D . P A -1
H1D1 H 0.186500 0.439854 -0.103091 0.024 Uiso 0.25 1 calc R U P A -1
H1D2 H 0.209710 0.358891 -0.013724 0.024 Uiso 0.25 1 calc R U P A -1
C2D C 0.26757(11) 0.36405(19) -0.1491(2) 0.0310(7) Uani 0.25 1 d D U P A -1
H2D1 H 0.305927 0.339515 -0.112665 0.037 Uiso 0.25 1 calc R U P A -1
H2D2 H 0.279467 0.416207 -0.204419 0.037 Uiso 0.25 1 calc R U P A -1
C3D C 0.23401(15) 0.2705(2) -0.2058(2) 0.0438(12) Uani 0.25 1 d D . P A -1
H3D1 H 0.227667 0.214618 -0.151696 0.053 Uiso 0.25 1 calc R U P A -1
H3D2 H 0.192551 0.293328 -0.231418 0.053 Uiso 0.25 1 calc R U P A -1
C4D C 0.27117(17) 0.2270(3) -0.3035(3) 0.0481(10) Uani 0.25 1 d D . P A -1
H4D1 H 0.279977 0.282980 -0.355102 0.072 Uiso 0.25 1 calc R U P A -1
H4D2 H 0.246686 0.173061 -0.339790 0.072 Uiso 0.25 1 calc R U P A -1
H4D3 H 0.310394 0.197296 -0.277425 0.072 Uiso 0.25 1 calc R U P A -1
Kr11 Kr 0.000000 0.000000 0.000000 0.02873(7) Uiso 0.2639(4) 4 d S . P B 2
Kr12 Kr 0.01014(8) 0.000000 -0.01763(13) 0.02873(7) Uiso 0.0591(2) 2 d S . P C
3
Kr13 Kr 0.000000 0.02241(12) 0.000000 0.02873(7) Uiso 0.0557(2) 2 d S . P D 4
Kr21 Kr 0.000000 0.000000 0.500000 0.03001(7) Uiso 0.3217(4) 4 d S . P E 5
Kr22 Kr 0.000000 0.02705(11) 0.500000 0.03001(7) Uiso 0.0601(2) 2 d S . P F 6
Kr23 Kr -0.01430(15) 0.000000 0.4894(3) 0.03001(7) Uiso 0.0279(2) 2 d S . P G 7
Kr31 Kr 0.250000 0.000000 0.2761(7) 0.0514(8) Uiso 0.0248(6) 4 d S . P H 8
Kr32 Kr 0.250000 0.000000 0.2723(6) 0.0514(8) Uiso 0.0298(6) 4 d S . P I 9


_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
O1 H11 0.930(10) . ?
O1 H12 0.949(9) . ?
O1 H13 0.935(7) . ?
O2 H21 0.896(8) . ?
O2 H21 0.896(8) 7_565 ?
O3 H31 0.932(10) . ?
O3 H32 0.941(8) . ?
O4 H41 0.944(7) . ?
O4 H42 0.933(8) . ?
O5 H51 0.930(8) . ?
O5 H52 0.948(8) . ?
O5 H53 0.939(8) . ?
O5 H54 0.675(16) . ?
O6 H61 0.936(10) . ?
O6 H62 0.942(9) . ?
O6 H63 0.953(9) . ?
O6 H64 0.938(9) . ?
O7 H71 0.936(9) . ?
O7 H72 0.931(8) . ?
O7 H73 0.942(9) . ?
O8 H81 0.943(9) . ?
O8 H82 0.940(7) . ?
O8 H83 0.940(10) . ?
O9 H91 0.939(9) . ?
O9 H92 0.921(9) . ?
O10 H101 0.931(8) . ?
O10 H102 0.929(9) . ?
O10 H103 0.950(2) . ?
O10 H104 0.934(8) . ?
O11 H111 0.931(8) . ?
O11 H112 0.936(9) . ?
O11 H113 0.939(10) . ?
O11 H114 0.949(9) . ?
O12 H121 0.934(7) . ?
O12 H122 0.932(9) . ?
O12 H123 0.928(7) . ?
O12 H124 0.932(9) . ?
O13 H131 0.936(8) . ?
O13 H132 0.936(7) . ?
O13 H133 0.949(9) . ?
O13 H134 0.953(9) . ?
N1 C1D 1.505(4) . ?
N1 C1C 1.493(4) . ?
N1 C1A 1.502(4) . ?
N1 C1B 1.515(4) . ?
C1A C2A 1.520(3) . ?
C1A H1A1 0.9700 . ?
C1A H1A2 0.9700 . ?
C2A C3A 1.541(3) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C3A C4A 1.538(4) . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C4A H4A1 0.9600 . ?
C4A H4A2 0.9600 . ?
C4A H4A3 0.9600 . ?
C1B C2B 1.512(4) . ?
C1B H1B1 0.9700 . ?
C1B H1B2 0.9700 . ?
C2B C3B 1.537(4) . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
C3B C4B 1.522(5) . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C4B H4B1 0.9600 . ?
C4B H4B2 0.9600 . ?
C4B H4B3 0.9600 . ?
C1C C2C 1.514(3) . ?
C1C H1C1 0.9700 . ?
C1C H1C2 0.9700 . ?
C2C C3C 1.537(3) . ?
C2C H2C1 0.9700 . ?
C2C H2C2 0.9700 . ?
C3C C4C 1.528(4) . ?
C3C H3C1 0.9700 . ?
C3C H3C2 0.9700 . ?
C4C H4C1 0.9600 . ?
C4C H4C2 0.9600 . ?
C4C H4C3 0.9600 . ?
C1D C2D 1.512(3) . ?
C1D H1D1 0.9700 . ?
C1D H1D2 0.9700 . ?
C2D C3D 1.537(4) . ?
C2D H2D1 0.9700 . ?
C2D H2D2 0.9700 . ?
C3D C4D 1.516(4) . ?
C3D H3D1 0.9700 . ?
C3D H3D2 0.9700 . ?
C4D H4D1 0.9600 . ?
C4D H4D2 0.9600 . ?
C4D H4D3 0.9600 . ?
Kr12 Kr12 0.602(3) 5 ?
Kr13 Kr13 0.567(3) 5 ?
Kr22 Kr22 0.684(3) 5_556 ?
Kr23 Kr23 0.655(7) 5_556 ?

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
H11 O1 H12 90.3(10) . . ?
H11 O1 H13 113.8(12) . . ?
H12 O1 H13 137.1(18) . . ?
H21 O2 H21 123.7(14) . 7_565 ?
H31 O3 H32 101.4(9) . . ?
H41 O4 H42 118.9(7) . . ?
H51 O5 H52 112.0(11) . . ?
H51 O5 H53 104.0(10) . . ?
H52 O5 H53 108.0(12) . . ?
H51 O5 H54 106.6(15) . . ?
H52 O5 H54 109.6(14) . . ?
H53 O5 H54 116.5(16) . . ?
H61 O6 H62 108.5(11) . . ?
H61 O6 H63 121.2(10) . . ?
H62 O6 H63 103.6(9) . . ?
H61 O6 H64 110.8(12) . . ?
H62 O6 H64 96.5(10) . . ?
H63 O6 H64 112.9(10) . . ?
H71 O7 H72 99.4(11) . . ?
H71 O7 H73 110.1(9) . . ?
H72 O7 H73 102.3(10) . . ?
H81 O8 H82 130(2) . . ?
H81 O8 H83 91.2(11) . . ?
H82 O8 H83 110.9(13) . . ?
H91 O9 H92 115.9(9) . . ?
H101 O10 H102 96.3(10) . . ?
H101 O10 H103 110.0(9) . . ?
H102 O10 H103 112.6(9) . . ?
H101 O10 H104 103.4(10) . . ?
H102 O10 H104 129.7(13) . . ?
H103 O10 H104 103.2(13) . . ?
H111 O11 H112 110.3(9) . . ?
H111 O11 H113 105.5(13) . . ?
H112 O11 H113 133.3(14) . . ?
H111 O11 H114 101.4(9) . . ?
H112 O11 H114 104.7(9) . . ?
H113 O11 H114 96.3(10) . . ?
H121 O12 H122 106.7(13) . . ?
H121 O12 H123 102.6(17) . . ?
H122 O12 H123 111.3(13) . . ?
H121 O12 H124 104.8(13) . . ?
H122 O12 H124 112.7(10) . . ?
H123 O12 H124 117.5(14) . . ?
H131 O13 H132 111.3(11) . . ?
H131 O13 H133 115.1(15) . . ?
H132 O13 H133 94(2) . . ?
H131 O13 H134 116.4(14) . . ?
H132 O13 H134 95(2) . . ?
H133 O13 H134 119.7(11) . . ?
C1D N1 C1C 112.52(14) . . ?
C1D N1 C1A 108.6(3) . . ?
C1C N1 C1A 107.7(3) . . ?
C1D N1 C1B 108.1(3) . . ?
C1C N1 C1B 108.5(3) . . ?
C1A N1 C1B 111.45(14) . . ?
N1 C1A C2A 118.1(2) . . ?
N1 C1A H1A1 107.8 . . ?
C2A C1A H1A1 107.8 . . ?
N1 C1A H1A2 107.8 . . ?
C2A C1A H1A2 107.8 . . ?
H1A1 C1A H1A2 107.1 . . ?
C1A C2A C3A 110.70(19) . . ?
C1A C2A H2A1 109.5 . . ?
C3A C2A H2A1 109.5 . . ?
C1A C2A H2A2 109.5 . . ?
C3A C2A H2A2 109.5 . . ?
H2A1 C2A H2A2 108.1 . . ?
C4A C3A C2A 110.0(2) . . ?
C4A C3A H3A1 109.6 . . ?
C2A C3A H3A1 109.7 . . ?
C4A C3A H3A2 109.7 . . ?
C2A C3A H3A2 109.7 . . ?
H3A1 C3A H3A2 108.2 . . ?
C3A C4A H4A1 109.5 . . ?
C3A C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C3A C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
N1 C1B C2B 116.9(2) . . ?
N1 C1B H1B1 108.1 . . ?
C2B C1B H1B1 108.1 . . ?
N1 C1B H1B2 108.1 . . ?
C2B C1B H1B2 108.1 . . ?
H1B1 C1B H1B2 107.3 . . ?
C1B C2B C3B 110.1(2) . . ?
C1B C2B H2B1 109.6 . . ?
C3B C2B H2B1 109.6 . . ?
C1B C2B H2B2 109.6 . . ?
C3B C2B H2B2 109.6 . . ?
H2B1 C2B H2B2 108.2 . . ?
C4B C3B C2B 112.4(3) . . ?
C4B C3B H3B1 109.1 . . ?
C2B C3B H3B1 109.1 . . ?
C4B C3B H3B2 109.1 . . ?
C2B C3B H3B2 109.1 . . ?
H3B1 C3B H3B2 107.9 . . ?
C3B C4B H4B1 109.5 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
N1 C1C C2C 117.1(2) . . ?
N1 C1C H1C1 108.0 . . ?
C2C C1C H1C1 108.0 . . ?
N1 C1C H1C2 108.0 . . ?
C2C C1C H1C2 108.0 . . ?
H1C1 C1C H1C2 107.3 . . ?
C1C C2C C3C 109.75(19) . . ?
C1C C2C H2C1 109.7 . . ?
C3C C2C H2C1 109.7 . . ?
C1C C2C H2C2 109.7 . . ?
C3C C2C H2C2 109.7 . . ?
H2C1 C2C H2C2 108.2 . . ?
C4C C3C C2C 110.7(2) . . ?
C4C C3C H3C1 109.5 . . ?
C2C C3C H3C1 109.5 . . ?
C4C C3C H3C2 109.5 . . ?
C2C C3C H3C2 109.5 . . ?
H3C1 C3C H3C2 108.1 . . ?
C3C C4C H4C1 109.5 . . ?
C3C C4C H4C2 109.5 . . ?
H4C1 C4C H4C2 109.5 . . ?
C3C C4C H4C3 109.5 . . ?
H4C1 C4C H4C3 109.5 . . ?
H4C2 C4C H4C3 109.5 . . ?
N1 C1D C2D 116.4(2) . . ?
N1 C1D H1D1 108.2 . . ?
C2D C1D H1D1 108.2 . . ?
N1 C1D H1D2 108.2 . . ?
C2D C1D H1D2 108.2 . . ?
H1D1 C1D H1D2 107.3 . . ?
C1D C2D C3D 109.8(2) . . ?
C1D C2D H2D1 109.7 . . ?
C3D C2D H2D1 109.7 . . ?
C1D C2D H2D2 109.7 . . ?
C3D C2D H2D2 109.7 . . ?
H2D1 C2D H2D2 108.2 . . ?
C4D C3D C2D 112.7(3) . . ?
C4D C3D H3D1 109.1 . . ?
C2D C3D H3D1 109.1 . . ?
C4D C3D H3D2 109.0 . . ?
C2D C3D H3D2 109.0 . . ?
H3D1 C3D H3D2 107.8 . . ?
C3D C4D H4D1 109.5 . . ?
C3D C4D H4D2 109.5 . . ?
H4D1 C4D H4D2 109.5 . . ?
C3D C4D H4D3 109.5 . . ?
H4D1 C4D H4D3 109.5 . . ?
H4D2 C4D H4D3 109.5 . . ?

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
C1D N1 C1A C2A -171.5(2) . . . . ?
C1C N1 C1A C2A 66.4(3) . . . . ?
C1B N1 C1A C2A -52.4(3) . . . . ?
N1 C1A C2A C3A 176.0(2) . . . . ?
C1A C2A C3A C4A 170.5(2) . . . . ?
C1D N1 C1B C2B 62.4(3) . . . . ?
C1C N1 C1B C2B -175.3(2) . . . . ?
C1A N1 C1B C2B -56.9(3) . . . . ?
N1 C1B C2B C3B -171.5(2) . . . . ?
C1B C2B C3B C4B -168.0(2) . . . . ?
C1D N1 C1C C2C 53.0(4) . . . . ?
C1A N1 C1C C2C 172.6(2) . . . . ?
C1B N1 C1C C2C -66.6(3) . . . . ?
N1 C1C C2C C3C -176.1(2) . . . . ?
C1C C2C C3C C4C -171.2(2) . . . . ?
C1C N1 C1D C2D 54.7(4) . . . . ?
C1A N1 C1D C2D -64.5(3) . . . . ?
C1B N1 C1D C2D 174.5(2) . . . . ?
N1 C1D C2D C3D 176.7(2) . . . . ?
C1D C2D C3D C4D 171.4(2) . . . . ?

_refine_diff_density_max         1.451
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_dy02
_database_code_depnum_ccdc_archive 'CCDC 1935566'
loop_
_audit_author_name
_audit_author_address
'Sanehiro Muromachi'
;National Institute of Advanced Industrial Science and Technology (AIST)
Japan
;
_audit_update_record             
;
2019-06-21 deposited with the CCDC.	2019-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H112 Ar1.23 Br N O38'
_chemical_formula_weight         1055.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ar Ar 0.1743 0.2003 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           51
_space_group_name_H-M_alt        'P m m a'
_space_group_name_Hall           '-P 2a 2a'

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

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

_cell_length_a                   21.041(3)
_cell_length_b                   12.6523(15)
_cell_length_c                   12.0228(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3200.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9950
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.54

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.784
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker, APEX2, CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17732
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.337
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_full        25.241
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4166
_reflns_number_gt                3859
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0747P)²+1.6167P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4166
_refine_ls_number_parameters     386
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1278
_refine_ls_wR_factor_gt          0.1264
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.125
_refine_ls_shift/su_mean         0.008

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 0.250000 0.000000 0.47138(2) 0.03188(3) Uani 1 4 d S T P . .
O1 O 0.18361(2) 0.500000 0.45692(4) 0.02411(12) Uani 1 2 d DS T P . .
H11 H 0.1672(5) 0.4462(5) 0.4927(8) 0.027(3) Uiso 0.5 1 d D . P . .
H12 H 0.1542(4) 0.500000 0.4033(7) 0.036(5) Uiso 0.5 2 d DS . P . .
H13 H 0.2253(3) 0.500000 0.4621(11) 0.015(4) Uiso 0.5 2 d DS . P . .
O2 O 0.250000 0.21498(4) 0.62044(4) 0.03108(13) Uani 1 2 d DS T P . .
H21 H 0.250000 0.1534(5) 0.5833(8) 0.019(4) Uiso 0.5 2 d DS . P . .
H22 H 0.2135(3) 0.2403(8) 0.5941(9) 0.032(3) Uiso 0.5 1 d D . P . .
O3 O 0.10337(3) 0.000000 0.37422(4) 0.02937(13) Uani 1 2 d S T P . .
O4 O 0.05688(2) 0.19651(3) 0.44098(3) 0.02544(8) Uani 1 1 d D . . . .
H41 H 0.0740(5) 0.1319(5) 0.4271(11) 0.042(4) Uiso 0.5 1 d D . P . .
H42 H 0.0849(4) 0.2323(8) 0.4814(8) 0.048(4) Uiso 0.5 1 d D . P . .
H43 H 0.0575(7) 0.2247(8) 0.3744(5) 0.040(4) Uiso 0.5 1 d D . P . .
H44 H 0.0205(3) 0.1905(12) 0.4791(8) 0.051(4) Uiso 0.5 1 d D . P . .
O5 O 0.11798(2) 0.500000 0.25844(4) 0.02569(12) Uani 1 2 d DS T P . .
H51 H 0.1415(5) 0.500000 0.3207(6) 0.045(6) Uiso 0.5 2 d DS . P . .
H52 H 0.0932(4) 0.4454(6) 0.2621(11) 0.049(4) Uiso 0.5 1 d D . P . .
H53 H 0.1570(3) 0.500000 0.2282(13) 0.15(3) Uiso 0.25 2 d DS . P . .
O6 O 0.07609(3) 0.000000 0.14442(4) 0.03268(14) Uani 1 2 d DS T P . .
H61 H 0.0870(6) 0.000000 0.2165(5) 0.006(3) Uiso 0.5 2 d DS . P . .
O7 O 0.18367(2) 0.500000 0.06124(4) 0.02702(12) Uani 1 2 d DS T P . .
H71 H 0.1593(4) 0.500000 0.1204(6) 0.024(4) Uiso 0.5 2 d DS . P . .
H72 H 0.2260(3) 0.500000 0.0631(19) 0.061(7) Uiso 0.5 2 d DS . P . .
O8 O 0.04296(2) 0.31940(3) 0.25249(3) 0.02665(9) Uani 1 1 d D . . . .
H81 H 0.0439(7) 0.2937(9) 0.3212(5) 0.051(4) Uiso 0.5 1 d D . P . .
H82 H 0.0033(3) 0.3427(8) 0.2517(7) 0.015(3) Uiso 0.5 1 d D . P . .
H83 H 0.0696(4) 0.3737(6) 0.2609(12) 0.070(6) Uiso 0.5 1 d D . P . .
O9 O 0.14093(2) 0.31977(3) 0.56292(3) 0.02631(9) Uani 1 1 d D . . . .
H91 H 0.1740(4) 0.2845(9) 0.5921(11) 0.108(8) Uiso 0.5 1 d D . P . .
H92 H 0.1151(4) 0.3376(12) 0.6207(6) 0.068(5) Uiso 0.5 1 d D . P . .
H93 H 0.1086(4) 0.2870(8) 0.5277(8) 0.041(4) Uiso 0.5 1 d D . P . .
O10 O 0.05599(2) 0.20116(3) 0.06087(3) 0.02754(9) Uani 1 1 d D . . . .
H101 H 0.0540(5) 0.2409(6) 0.1232(5) 0.020(3) Uiso 0.5 1 d D . P . .
H102 H 0.0186(3) 0.2044(11) 0.0257(8) 0.041(4) Uiso 0.5 1 d D . P . .
H103 H 0.0858(4) 0.2361(8) 0.0228(8) 0.041(4) Uiso 0.5 1 d D . P . .
O11 O 0.13918(2) 0.32820(3) 0.94203(3) 0.02886(9) Uani 1 1 d D . . . .
H111 H 0.1468(9) 0.3873(6) 0.9804(9) 0.090(7) Uiso 0.5 1 d D . P . .
H112 H 0.1100(3) 0.2877(6) 0.9776(7) 0.019(3) Uiso 0.5 1 d D . P . .
H113 H 0.1098(4) 0.3511(12) 0.8930(7) 0.015(5) Uiso 0.25 1 d D . P . .
O12 O 0.250000 0.27800(5) 0.83939(5) 0.03860(15) Uani 1 2 d DS T P . .
H121 H 0.250000 0.2527(7) 0.7696(5) 0.036(2) Uiso 1 2 d DS . P . .
O13 O 0.07951(2) 0.39151(3) 0.74993(3) 0.02665(7) Uiso 1 1 d D . . . .
H131 H 0.0410(3) 0.3648(9) 0.7457(9) 0.031(3) Uiso 0.5 1 d D . P . .
H132 H 0.0899(6) 0.3763(10) 0.8215(5) 0.038(4) Uiso 0.5 1 d D . P . .
N1 N 0.24778(14) -0.00482(19) -0.00285(7) 0.01675(17) Uani 0.25 1 d D . P A -1
C1A C 0.27297(9) 0.08778(17) 0.06632(17) 0.0301(5) Uani 0.25 1 d D . P A -1
H1A1 H 0.312712 0.065559 0.099845 0.036 Uiso 0.25 1 calc R U P A -1
H1A2 H 0.282870 0.144949 0.015431 0.036 Uiso 0.25 1 calc R U P A -1
C2A C 0.23320(10) 0.13092(16) 0.15431(18) 0.0381(7) Uani 0.25 1 d D . P A -1
H2A1 H 0.226756 0.077303 0.210860 0.046 Uiso 0.25 1 calc R U P A -1
H2A2 H 0.191972 0.149115 0.123721 0.046 Uiso 0.25 1 calc R U P A -1
C3A C 0.26354(10) 0.23274(17) 0.21014(18) 0.0391(7) Uani 0.25 1 d D . P A -1
H3A1 H 0.305183 0.215432 0.239586 0.047 Uiso 0.25 1 calc R U P A -1
H3A2 H 0.268775 0.287568 0.154496 0.047 Uiso 0.25 1 calc R U P A -1
C4A C 0.22016(9) 0.27429(16) 0.30600(17) 0.0300(5) Uani 0.25 1 d D . P A -1
H4A1 H 0.182796 0.306279 0.274915 0.045 Uiso 0.25 1 calc R U P A -1
H4A2 H 0.242980 0.325740 0.348998 0.045 Uiso 0.25 1 calc R U P A -1
H4A3 H 0.208026 0.216385 0.353036 0.045 Uiso 0.25 1 calc R U P A -1
C1B C 0.30360(10) -0.0495(2) -0.07444(19) 0.0393(6) Uani 0.25 1 d D . P A -1
H1B1 H 0.336823 -0.072000 -0.023761 0.047 Uiso 0.25 1 calc R U P A -1
H1B2 H 0.288205 -0.112287 -0.112048 0.047 Uiso 0.25 1 calc R U P A -1
C2B C 0.33352(11) 0.01998(12) -0.16000(18) 0.0369(7) Uani 0.25 1 d D . P A -1
H2B1 H 0.300629 0.046733 -0.209026 0.044 Uiso 0.25 1 calc R U P A -1
H2B2 H 0.352886 0.080071 -0.123090 0.044 Uiso 0.25 1 calc R U P A -1
C3B C 0.38230(9) -0.03424(15) -0.22756(16) 0.0266(4) Uani 0.25 1 d D . P A -1
H3B1 H 0.361937 -0.091570 -0.267549 0.032 Uiso 0.25 1 calc R U P A -1
H3B2 H 0.413151 -0.065513 -0.177449 0.032 Uiso 0.25 1 calc R U P A -1
C4B C 0.41751(12) 0.0332(2) -0.31044(19) 0.0455(7) Uani 0.25 1 d D . P A -1
H4B1 H 0.389906 0.049876 -0.371531 0.068 Uiso 0.25 1 calc R U P A -1
H4B2 H 0.453883 -0.004764 -0.337490 0.068 Uiso 0.25 1 calc R U P A -1
H4B3 H 0.431183 0.097291 -0.275127 0.068 Uiso 0.25 1 calc R U P A -1
C1C C 0.19674(7) 0.04259(13) -0.07496(12) 0.0124(3) Uani 0.25 1 d D . P A -1
H1C1 H 0.214361 0.102747 -0.114347 0.015 Uiso 0.25 1 calc R U P A -1
H1C2 H 0.162825 0.068461 -0.027589 0.015 Uiso 0.25 1 calc R U P A -1
C2C C 0.16808(7) -0.03562(13) -0.16135(12) 0.0154(3) Uani 0.25 1 d D U P A -1
H2C1 H 0.199087 -0.051083 -0.218785 0.019 Uiso 0.25 1 calc R U P A -1
H2C2 H 0.156513 -0.101357 -0.125107 0.019 Uiso 0.25 1 calc R U P A -1
C3C C 0.10885(8) 0.0160(3) -0.21309(16) 0.0436(7) Uani 0.25 1 d D . P A -1
H3C1 H 0.076488 0.025040 -0.156411 0.052 Uiso 0.25 1 calc R U P A -1
H3C2 H 0.119840 0.085361 -0.241705 0.052 Uiso 0.25 1 calc R U P A -1
C4C C 0.08281(12) -0.0519(2) -0.3069(2) 0.0513(7) Uani 0.25 1 d D . P A -1
H4C1 H 0.117055 -0.073745 -0.354378 0.077 Uiso 0.25 1 calc R U P A -1
H4C2 H 0.052587 -0.011827 -0.349260 0.077 Uiso 0.25 1 calc R U P A -1
H4C3 H 0.062341 -0.113165 -0.276200 0.077 Uiso 0.25 1 calc R U P A -1
C1D C 0.21998(7) -0.08919(12) 0.06773(12) 0.0122(3) Uani 0.25 1 d D U P A -1
H1D1 H 0.203944 -0.144732 0.019715 0.015 Uiso 0.25 1 calc R U P A -1
H1D2 H 0.184066 -0.059999 0.107913 0.015 Uiso 0.25 1 calc R U P A -1
C2D C 0.26702(6) -0.13956(12) 0.15379(12) 0.0132(3) Uani 0.25 1 d D . P A -1
H2D1 H 0.300875 -0.176961 0.115725 0.016 Uiso 0.25 1 calc R U P A -1
H2D2 H 0.285707 -0.085332 0.200508 0.016 Uiso 0.25 1 calc R U P A -1
C3D C 0.22751(8) -0.21591(13) 0.22352(15) 0.0187(4) Uani 0.25 1 d D . P A -1
H3D1 H 0.196184 -0.176094 0.265339 0.022 Uiso 0.25 1 calc R U P A -1
H3D2 H 0.204880 -0.263610 0.174309 0.022 Uiso 0.25 1 calc R U P A -1
C4D C 0.26526(8) -0.27663(17) 0.29921(18) 0.0320(6) Uani 0.25 1 d D . P A -1
H4D1 H 0.300711 -0.306717 0.260188 0.048 Uiso 0.25 1 calc R U P A -1
H4D2 H 0.239863 -0.332224 0.330481 0.048 Uiso 0.25 1 calc R U P A -1
H4D3 H 0.280509 -0.231661 0.357725 0.048 Uiso 0.25 1 calc R U P A -1
Ar11 Ar 0.000000 0.500000 0.500000 0.04168(17) Uiso 0.2393(6) 4 d S . P B 2
Ar12 Ar 0.000000 0.47331(15) 0.500000 0.04168(17) Uiso 0.0923(3) 2 d S . P C 3
Ar13 Ar 0.0168(2) 0.500000 0.4872(5) 0.04168(17) Uiso 0.0365(3) 2 d S . P D 4
Ar21 Ar 0.250000 0.500000 0.7191(4) 0.0402(7) Uiso 0.0671(8) 4 d S . P E 5
Ar22 Ar 0.2288(4) 0.500000 0.7218(8) 0.0402(7) Uiso 0.0219(6) 2 d S . P F 6
Ar31 Ar 0.000000 0.500000 1.000000 0.03754(17) Uiso 0.2002(6) 4 d S . P G 7
Ar32 Ar 0.0165(6) 0.500000 1.0260(9) 0.03754(17) Uiso 0.0158(3) 2 d S . P H 8
Ar33 Ar 0.00752(9) 0.48164(12) 1.01432(14) 0.03754(17) Uiso 0.06597(17) 1 d . .
P I 9


_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
O1 H11 0.876(8) . ?
O1 H12 0.893(8) . ?
O1 H13 0.879(6) . ?
O1 H11 0.876(8) 7_565 ?
O2 H21 0.898(7) . ?
O2 H22 0.891(7) . ?
O2 H22 0.891(7) 8_655 ?
O4 H41 0.909(7) . ?
O4 H42 0.887(8) . ?
O4 H43 0.877(7) . ?
O4 H44 0.895(7) . ?
O5 H51 0.897(8) . ?
O5 H52 0.867(8) . ?
O5 H53 0.897(9) . ?
O5 H52 0.867(8) 7_565 ?
O6 H61 0.896(6) . ?
O7 H71 0.877(8) . ?
O7 H72 0.892(6) . ?
O8 H81 0.888(7) . ?
O8 H82 0.885(6) . ?
O8 H83 0.893(8) . ?
O9 H91 0.898(9) . ?
O9 H92 0.910(8) . ?
O9 H93 0.903(8) . ?
O10 H101 0.904(7) . ?
O10 H102 0.894(7) . ?
O10 H103 0.893(8) . ?
O11 H111 0.893(8) . ?
O11 H112 0.907(8) . ?
O11 H113 0.902(9) . ?
O12 H121 0.898(6) . ?
O13 H131 0.880(7) . ?
O13 H132 0.908(7) . ?
N1 C1D 1.484(3) . ?
N1 C1C 1.505(3) . ?
N1 C1A 1.531(3) . ?
N1 C1B 1.562(3) . ?
C1A C2A 1.455(3) . ?
C1A H1A1 0.9700 . ?
C1A H1A2 0.9700 . ?
C2A C3A 1.587(3) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?
C3A C4A 1.561(3) . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C4A H4A1 0.9600 . ?
C4A H4A2 0.9600 . ?
C4A H4A3 0.9600 . ?
C1B C2B 1.492(3) . ?
C1B H1B1 0.9700 . ?
C1B H1B2 0.9700 . ?
C2B C3B 1.478(3) . ?
C2B H2B1 0.9700 . ?
C2B H2B2 0.9700 . ?
C3B C4B 1.506(3) . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C4B H4B1 0.9600 . ?
C4B H4B2 0.9600 . ?
C4B H4B3 0.9600 . ?
C1C C2C 1.556(2) . ?
C1C H1C1 0.9700 . ?
C1C H1C2 0.9700 . ?
C2C C3C 1.539(3) . ?
C2C H2C1 0.9700 . ?
C2C H2C2 0.9700 . ?
C3C C4C 1.520(4) . ?
C3C H3C1 0.9700 . ?
C3C H3C2 0.9700 . ?
C4C H4C1 0.9600 . ?
C4C H4C2 0.9600 . ?
C4C H4C3 0.9600 . ?
C1D C2D 1.567(2) . ?
C1D H1D1 0.9700 . ?
C1D H1D2 0.9700 . ?
C2D C3D 1.526(2) . ?
C2D H2D1 0.9700 . ?
C2D H2D2 0.9700 . ?
C3D C4D 1.431(3) . ?
C3D H3D1 0.9700 . ?
C3D H3D2 0.9700 . ?
C4D H4D1 0.9600 . ?
C4D H4D2 0.9600 . ?
C4D H4D3 0.9600 . ?
Ar12 Ar12 0.675(4) 5_566 ?
Ar13 Ar13 0.770(11) 5_566 ?
Ar22 Ar22 0.890(17) 2_565 ?
Ar32 Ar32 0.93(2) 5_567 ?
Ar33 Ar33 0.659(3) 5_567 ?

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
H11 O1 H12 94.7(7) . . ?
H11 O1 H13 110.9(8) . . ?
H12 O1 H13 137.9(10) . . ?
H11 O1 H11 102.0(11) . 7_565 ?
H12 O1 H11 94.7(7) . 7_565 ?
H13 O1 H11 110.9(8) . 7_565 ?
H21 O2 H22 97.8(8) . . ?
H21 O2 H22 97.8(7) . 8_655 ?
H22 O2 H22 119.2(13) . 8_655 ?
H41 O4 H42 107.3(9) . . ?
H41 O4 H43 101.1(11) . . ?
H42 O4 H43 106.4(10) . . ?
H41 O4 H44 110.9(12) . . ?
H42 O4 H44 109.3(9) . . ?
H43 O4 H44 121.0(11) . . ?
H51 O5 H52 106.9(9) . . ?
H51 O5 H53 80.4(11) . . ?
H52 O5 H53 124.8(7) . . ?
H51 O5 H52 106.9(9) . 7_565 ?
H52 O5 H52 105.8(11) . 7_565 ?
H53 O5 H52 124.8(7) . 7_565 ?
H71 O7 H72 124.4(16) . . ?
H81 O8 H82 98.7(11) . . ?
H81 O8 H83 99.3(12) . . ?
H82 O8 H83 109.7(9) . . ?
H91 O9 H92 106.7(10) . . ?
H91 O9 H93 122.6(10) . . ?
H92 O9 H93 91.2(9) . . ?
H101 O10 H102 109.0(10) . . ?
H101 O10 H103 100.4(9) . . ?
H102 O10 H103 110.6(9) . . ?
H111 O11 H112 110.6(11) . . ?
H111 O11 H113 101.1(13) . . ?
H112 O11 H113 91.4(9) . . ?
H131 O13 H132 101.3(10) . . ?
C1D N1 C1C 109.6(2) . . ?
C1D N1 C1A 112.10(11) . . ?
C1C N1 C1A 104.77(18) . . ?
C1D N1 C1B 110.56(19) . . ?
C1C N1 C1B 111.31(11) . . ?
C1A N1 C1B 108.4(2) . . ?
C2A C1A N1 118.87(18) . . ?
C2A C1A H1A1 107.6 . . ?
N1 C1A H1A1 107.6 . . ?
C2A C1A H1A2 107.6 . . ?
N1 C1A H1A2 107.6 . . ?
H1A1 C1A H1A2 107.0 . . ?
C1A C2A C3A 112.38(17) . . ?
C1A C2A H2A1 109.1 . . ?
C3A C2A H2A1 109.1 . . ?
C1A C2A H2A2 109.1 . . ?
C3A C2A H2A2 109.1 . . ?
H2A1 C2A H2A2 107.9 . . ?
C4A C3A C2A 110.51(17) . . ?
C4A C3A H3A1 109.5 . . ?
C2A C3A H3A1 109.5 . . ?
C4A C3A H3A2 109.5 . . ?
C2A C3A H3A2 109.5 . . ?
H3A1 C3A H3A2 108.1 . . ?
C3A C4A H4A1 109.5 . . ?
C3A C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C3A C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C2B C1B N1 118.9(2) . . ?
C2B C1B H1B1 107.6 . . ?
N1 C1B H1B1 107.6 . . ?
C2B C1B H1B2 107.6 . . ?
N1 C1B H1B2 107.6 . . ?
H1B1 C1B H1B2 107.0 . . ?
C3B C2B C1B 113.48(16) . . ?
C3B C2B H2B1 108.9 . . ?
C1B C2B H2B1 108.9 . . ?
C3B C2B H2B2 108.9 . . ?
C1B C2B H2B2 108.9 . . ?
H2B1 C2B H2B2 107.7 . . ?
C2B C3B C4B 116.26(17) . . ?
C2B C3B H3B1 108.2 . . ?
C4B C3B H3B1 108.2 . . ?
C2B C3B H3B2 108.2 . . ?
C4B C3B H3B2 108.2 . . ?
H3B1 C3B H3B2 107.4 . . ?
C3B C4B H4B1 109.5 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
N1 C1C C2C 114.06(14) . . ?
N1 C1C H1C1 108.7 . . ?
C2C C1C H1C1 108.7 . . ?
N1 C1C H1C2 108.7 . . ?
C2C C1C H1C2 108.7 . . ?
H1C1 C1C H1C2 107.6 . . ?
C3C C2C C1C 108.28(15) . . ?
C3C C2C H2C1 110.0 . . ?
C1C C2C H2C1 110.0 . . ?
C3C C2C H2C2 110.0 . . ?
C1C C2C H2C2 110.0 . . ?
H2C1 C2C H2C2 108.4 . . ?
C4C C3C C2C 110.6(2) . . ?
C4C C3C H3C1 109.5 . . ?
C2C C3C H3C1 109.5 . . ?
C4C C3C H3C2 109.5 . . ?
C2C C3C H3C2 109.5 . . ?
H3C1 C3C H3C2 108.1 . . ?
C3C C4C H4C1 109.5 . . ?
C3C C4C H4C2 109.5 . . ?
H4C1 C4C H4C2 109.5 . . ?
C3C C4C H4C3 109.5 . . ?
H4C1 C4C H4C3 109.5 . . ?
H4C2 C4C H4C3 109.5 . . ?
N1 C1D C2D 114.91(14) . . ?
N1 C1D H1D1 108.5 . . ?
C2D C1D H1D1 108.5 . . ?
N1 C1D H1D2 108.5 . . ?
C2D C1D H1D2 108.5 . . ?
H1D1 C1D H1D2 107.5 . . ?
C3D C2D C1D 106.03(11) . . ?
C3D C2D H2D1 110.5 . . ?
C1D C2D H2D1 110.5 . . ?
C3D C2D H2D2 110.5 . . ?
C1D C2D H2D2 110.5 . . ?
H2D1 C2D H2D2 108.7 . . ?
C4D C3D C2D 112.75(14) . . ?
C4D C3D H3D1 109.0 . . ?
C2D C3D H3D1 109.0 . . ?
C4D C3D H3D2 109.0 . . ?
C2D C3D H3D2 109.0 . . ?
H3D1 C3D H3D2 107.8 . . ?
C3D C4D H4D1 109.5 . . ?
C3D C4D H4D2 109.5 . . ?
H4D1 C4D H4D2 109.5 . . ?
C3D C4D H4D3 109.5 . . ?
H4D1 C4D H4D3 109.5 . . ?
H4D2 C4D H4D3 109.5 . . ?

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
C1D N1 C1A C2A -46.9(3) . . . . ?
C1C N1 C1A C2A 71.8(2) . . . . ?
C1B N1 C1A C2A -169.24(18) . . . . ?
N1 C1A C2A C3A -174.69(17) . . . . ?
C1A C2A C3A C4A -178.46(17) . . . . ?
C1D N1 C1B C2B 173.59(18) . . . . ?
C1C N1 C1B C2B 51.6(3) . . . . ?
C1A N1 C1B C2B -63.2(2) . . . . ?
N1 C1B C2B C3B -175.61(18) . . . . ?
C1B C2B C3B C4B -176.08(19) . . . . ?
C1D N1 C1C C2C -64.89(17) . . . . ?
C1A N1 C1C C2C 174.67(14) . . . . ?
C1B N1 C1C C2C 57.7(2) . . . . ?
N1 C1C C2C C3C 169.45(15) . . . . ?
C1C C2C C3C C4C 174.05(17) . . . . ?
C1C N1 C1D C2D -175.53(12) . . . . ?
C1A N1 C1D C2D -59.7(2) . . . . ?
C1B N1 C1D C2D 61.43(18) . . . . ?
N1 C1D C2D C3D 174.97(14) . . . . ?
C1D C2D C3D C4D 174.03(15) . . . . ?

_refine_diff_density_max         1.562
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.068

