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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Tren-Cl-Me-nco-Ligand
_database_code_depnum_ccdc_archive 'CCDC 1840353'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 Cl3 N7 O3'
_chemical_formula_sum            'C30 H36 Cl3 N7 O3'
_chemical_formula_weight         649.01

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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.436(3)
_cell_length_b                   19.819(3)
_cell_length_c                   13.591(3)
_cell_angle_alpha                90
_cell_angle_beta                 118.29(2)
_cell_angle_gamma                90
_cell_volume                     3186.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    793
_cell_measurement_theta_min      3.517
_cell_measurement_theta_max      19.476

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             1360.0
_exptl_transmission_factor_min   0.913
_exptl_transmission_factor_max   0.939
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.331
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10707
_diffrn_reflns_av_unetI/netI     0.2972
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.000
_diffrn_reflns_theta_max         28.670
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.786
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.786
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.786
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             7465
_reflns_number_gt                3539
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0100P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7465
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3471
_refine_ls_R_factor_gt           0.1065
_refine_ls_wR_factor_ref         0.2133
_refine_ls_wR_factor_gt          0.1550
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003

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
Cl3 Cl 0.7544(2) 0.82215(13) 0.2681(2) 0.1048(11) Uani 1 1 d . . . . .
Cl1 Cl 0.26956(19) 0.53537(14) 0.3247(2) 0.0917(10) Uani 1 1 d . . . . .
Cl2 Cl 1.2638(2) 0.75725(15) 0.6796(3) 0.1177(12) Uani 1 1 d . . . . .
O3 O 0.8248(4) 0.5924(3) 0.1424(4) 0.0683(19) Uani 1 1 d . . . . .
O1 O 0.5275(4) 0.4610(3) 0.1645(4) 0.0631(18) Uani 1 1 d . . . . .
N5 N 0.9722(5) 0.6029(5) 0.3795(6) 0.077(3) Uani 1 1 d . . . . .
H5N H 0.9158 0.6077 0.3138 0.092 Uiso 1 1 calc R U . . .
O2 O 1.1128(4) 0.5309(3) 0.4940(5) 0.075(2) Uani 1 1 d . . . . .
N6 N 0.7209(6) 0.5382(4) -0.0248(6) 0.067(2) Uani 1 1 d . . . . .
H6N H 0.6544 0.5323 -0.0801 0.081 Uiso 1 1 calc R U . . .
N7 N 0.6299(5) 0.5992(4) 0.0497(6) 0.060(2) Uani 1 1 d . . . . .
H7N H 0.5688 0.5820 -0.0024 0.072 Uiso 1 1 calc R U . . .
N1 N 0.8645(6) 0.4218(4) 0.1255(6) 0.063(2) Uani 1 1 d . . . . .
N3 N 0.6574(5) 0.4904(4) 0.3444(6) 0.061(2) Uani 1 1 d . . . . .
H3N H 0.7269 0.4852 0.3939 0.074 Uiso 1 1 calc R U . . .
C29 C 0.6707(9) 0.7503(5) 0.2266(8) 0.074(3) Uani 1 1 d . . . . .
C24 C 0.6211(7) 0.6482(5) 0.1205(7) 0.055(3) Uani 1 1 d . . . . .
N2 N 0.7123(5) 0.4299(4) 0.2345(6) 0.071(2) Uani 1 1 d . . . . .
H2N H 0.7803 0.4324 0.2884 0.085 Uiso 1 1 calc R U . . .
C23 C 0.7338(8) 0.5771(5) 0.0604(8) 0.058(3) Uani 1 1 d . . . . .
C19 C 1.1245(7) 0.7322(6) 0.5975(8) 0.076(3) Uani 1 1 d . . . . .
N4 N 0.9923(6) 0.5062(5) 0.3089(7) 0.075(3) Uani 1 1 d . . . . .
H4N H 0.9446 0.5240 0.2465 0.090 Uiso 1 1 calc R U . . .
C14 C 0.9956(8) 0.6557(6) 0.4549(8) 0.070(3) Uani 1 1 d . . . . .
C12 C 1.0265(6) 0.4370(5) 0.3101(8) 0.073(3) Uani 1 1 d . . . . .
H12B H 0.9943 0.4086 0.3459 0.087 Uiso 1 1 calc R U . . .
H12A H 1.1082 0.4335 0.3519 0.087 Uiso 1 1 calc R U . . .
C2 C 0.6900(6) 0.3932(5) 0.1355(8) 0.072(3) Uani 1 1 d . . . . .
H2B H 0.6531 0.4222 0.0706 0.087 Uiso 1 1 calc R U . . .
H2A H 0.6405 0.3553 0.1260 0.087 Uiso 1 1 calc R U . . .
C17 C 1.0384(9) 0.7629(5) 0.6064(8) 0.079(3) Uani 1 1 d . . . . .
C3 C 0.6246(7) 0.4618(4) 0.2448(8) 0.057(3) Uani 1 1 d . . . . .
C25 C 0.5370(7) 0.6367(5) 0.1541(7) 0.062(3) Uani 1 1 d . . . . .
H25 H 0.4923 0.5981 0.1314 0.075 Uiso 1 1 calc R U . . .
C13 C 1.0326(7) 0.5435(6) 0.4023(8) 0.061(3) Uani 1 1 d . . . . .
C21 C 0.8299(7) 0.4313(5) 0.0088(8) 0.074(3) Uani 1 1 d . . . . .
H21A H 0.7581 0.4088 -0.0350 0.089 Uiso 1 1 calc R U . . .
H21B H 0.8850 0.4102 -0.0083 0.089 Uiso 1 1 calc R U . . .
C11 C 0.9864(7) 0.4146(5) 0.1932(8) 0.077(3) Uani 1 1 d . . . . .
H11A H 1.0238 0.4409 0.1603 0.093 Uiso 1 1 calc R U . . .
H11B H 1.0069 0.3676 0.1932 0.093 Uiso 1 1 calc R U . . .
C1 C 0.8030(7) 0.3678(5) 0.1472(8) 0.083(3) Uani 1 1 d . . . . .
H1B H 0.8490 0.3505 0.2222 0.100 Uiso 1 1 calc R U . . .
H1A H 0.7891 0.3312 0.0950 0.100 Uiso 1 1 calc R U . . .
C20 C 1.1055(7) 0.6789(5) 0.5240(7) 0.078(3) Uani 1 1 d . . . . .
H20 H 1.1663 0.6585 0.5208 0.094 Uiso 1 1 calc R U . . .
C9 C 0.4123(7) 0.5537(6) 0.3726(8) 0.072(3) Uani 1 1 d . . . . .
C30 C 0.6858(7) 0.7069(5) 0.1603(8) 0.066(3) Uani 1 1 d . . . . .
H30 H 0.7414 0.7158 0.1398 0.079 Uiso 1 1 calc R U . . .
C28 C 0.5729(7) 0.7915(5) 0.3355(8) 0.104(4) Uani 1 1 d . . . . .
H28C H 0.6426 0.7949 0.4040 0.155 Uiso 1 1 calc R U . . .
H28B H 0.5140 0.7765 0.3511 0.155 Uiso 1 1 calc R U . . .
H28A H 0.5535 0.8350 0.3000 0.155 Uiso 1 1 calc R U . . .
C16 C 0.9302(8) 0.7442(6) 0.5381(9) 0.094(4) Uani 1 1 d . . . . .
H16 H 0.8704 0.7670 0.5394 0.112 Uiso 1 1 calc R U . . .
C10 C 0.4710(6) 0.5156(4) 0.3350(7) 0.056(3) Uani 1 1 d . . . . .
H10 H 0.4352 0.4815 0.2830 0.067 Uiso 1 1 calc R U . . .
C26 C 0.5236(7) 0.6837(5) 0.2205(8) 0.069(3) Uani 1 1 d . . . . .
H26 H 0.4676 0.6755 0.2408 0.082 Uiso 1 1 calc R U . . .
C22 C 0.8177(7) 0.5056(6) -0.0259(8) 0.084(3) Uani 1 1 d . . . . .
H22A H 0.8860 0.5296 0.0244 0.101 Uiso 1 1 calc R U . . .
H22B H 0.8097 0.5087 -0.1006 0.101 Uiso 1 1 calc R U . . .
C4 C 0.5876(7) 0.5285(5) 0.3760(7) 0.060(3) Uani 1 1 d . . . . .
C15 C 0.9105(7) 0.6908(6) 0.4667(8) 0.073(3) Uani 1 1 d . . . . .
H15 H 0.8361 0.6768 0.4233 0.088 Uiso 1 1 calc R U . . .
C6 C 0.5718(10) 0.6222(6) 0.4851(9) 0.097(4) Uani 1 1 d . . . . .
H6 H 0.6073 0.6566 0.5364 0.117 Uiso 1 1 calc R U . . .
C7 C 0.4559(9) 0.6090(6) 0.4447(9) 0.079(3) Uani 1 1 d . . . . .
C5 C 0.6315(7) 0.5835(6) 0.4478(8) 0.072(3) Uani 1 1 d . . . . .
H5 H 0.7067 0.5947 0.4721 0.087 Uiso 1 1 calc R U . . .
C27 C 0.5864(9) 0.7429(5) 0.2606(8) 0.070(3) Uani 1 1 d . . . . .
C18 C 1.0621(7) 0.8160(5) 0.6932(9) 0.113(4) Uani 1 1 d . . . . .
H18C H 1.1226 0.8444 0.6991 0.169 Uiso 1 1 calc R U . . .
H18B H 1.0835 0.7948 0.7640 0.169 Uiso 1 1 calc R U . . .
H18A H 0.9955 0.8427 0.6722 0.169 Uiso 1 1 calc R U . . .
C8 C 0.3905(7) 0.6531(5) 0.4851(7) 0.106(4) Uani 1 1 d . . . . .
H8A H 0.3279 0.6734 0.4222 0.159 Uiso 1 1 calc R U . . .
H8C H 0.4393 0.6877 0.5332 0.159 Uiso 1 1 calc R U . . .
H8B H 0.3630 0.6260 0.5257 0.159 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl3 C29 1.734(10) . ?
Cl1 C9 1.747(9) . ?
Cl2 C19 1.736(9) . ?
O3 C23 1.240(8) . ?
O1 C3 1.242(8) . ?
N5 C13 1.379(10) . ?
N5 C14 1.392(11) . ?
O2 C13 1.227(9) . ?
N6 C23 1.332(10) . ?
N6 C22 1.459(10) . ?
N7 C23 1.402(10) . ?
N7 C24 1.412(10) . ?
N1 C21 1.438(10) . ?
N1 C11 1.456(8) . ?
N1 C1 1.465(10) . ?
N3 C3 1.335(10) . ?
N3 C4 1.420(10) . ?
C29 C30 1.330(12) . ?
C29 C27 1.420(13) . ?
C24 C30 1.397(11) . ?
C24 C25 1.424(11) . ?
N2 C3 1.401(10) . ?
N2 C2 1.432(10) . ?
C19 C17 1.362(12) . ?
C19 C20 1.392(12) . ?
N4 C13 1.342(10) . ?
N4 C12 1.443(10) . ?
C14 C20 1.400(10) . ?
C14 C15 1.411(12) . ?
C12 C11 1.483(10) . ?
C2 C1 1.534(10) . ?
C17 C16 1.354(11) . ?
C17 C18 1.498(11) . ?
C25 C26 1.368(11) . ?
C21 C22 1.531(11) . ?
C9 C10 1.355(11) . ?
C9 C7 1.399(12) . ?
C28 C27 1.474(12) . ?
C16 C15 1.373(12) . ?
C10 C4 1.415(9) . ?
C26 C27 1.396(11) . ?
C4 C5 1.393(11) . ?
C6 C5 1.368(11) . ?
C6 C7 1.409(12) . ?
C7 C8 1.515(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 N5 C14 124.9(8) . . ?
C23 N6 C22 121.1(8) . . ?
C23 N7 C24 123.0(7) . . ?
C21 N1 C11 112.9(7) . . ?
C21 N1 C1 113.5(8) . . ?
C11 N1 C1 111.9(7) . . ?
C3 N3 C4 125.8(8) . . ?
C30 C29 C27 123.7(10) . . ?
C30 C29 Cl3 118.0(10) . . ?
C27 C29 Cl3 118.3(9) . . ?
C30 C24 N7 126.9(10) . . ?
C30 C24 C25 116.8(9) . . ?
N7 C24 C25 116.3(9) . . ?
C3 N2 C2 120.8(7) . . ?
O3 C23 N6 126.1(9) . . ?
O3 C23 N7 121.7(9) . . ?
N6 C23 N7 112.1(8) . . ?
C17 C19 C20 121.9(9) . . ?
C17 C19 Cl2 121.1(9) . . ?
C20 C19 Cl2 116.9(8) . . ?
C13 N4 C12 122.0(9) . . ?
N5 C14 C20 122.6(10) . . ?
N5 C14 C15 122.8(9) . . ?
C20 C14 C15 114.5(10) . . ?
N4 C12 C11 108.7(8) . . ?
N2 C2 C1 108.3(7) . . ?
C19 C17 C16 119.8(10) . . ?
C19 C17 C18 120.7(10) . . ?
C16 C17 C18 119.4(10) . . ?
O1 C3 N3 126.9(9) . . ?
O1 C3 N2 119.3(9) . . ?
N3 C3 N2 113.8(8) . . ?
C26 C25 C24 118.4(9) . . ?
O2 C13 N4 127.9(10) . . ?
O2 C13 N5 122.9(10) . . ?
N4 C13 N5 109.1(9) . . ?
N1 C21 C22 113.4(8) . . ?
N1 C11 C12 112.1(7) . . ?
N1 C1 C2 111.4(7) . . ?
C14 C20 C19 120.5(10) . . ?
C10 C9 C7 125.1(9) . . ?
C10 C9 Cl1 118.4(8) . . ?
C7 C9 Cl1 116.5(8) . . ?
C29 C30 C24 122.4(10) . . ?
C17 C16 C15 118.7(10) . . ?
C9 C10 C4 118.9(9) . . ?
C25 C26 C27 125.8(10) . . ?
N6 C22 C21 112.9(8) . . ?
C5 C4 C10 116.0(9) . . ?
C5 C4 N3 120.5(9) . . ?
C10 C4 N3 123.4(9) . . ?
C16 C15 C14 124.4(9) . . ?
C5 C6 C7 119.0(11) . . ?
C9 C7 C6 115.9(10) . . ?
C9 C7 C8 125.7(10) . . ?
C6 C7 C8 118.4(11) . . ?
C6 C5 C4 124.8(9) . . ?
C26 C27 C29 112.9(10) . . ?
C26 C27 C28 124.7(11) . . ?
C29 C27 C28 122.3(10) . . ?

_refine_diff_density_max         0.523
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.076

####################################################################### 
# 
# 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_Tren-Cl-Me-nco-TBABr
_database_code_depnum_ccdc_archive 'CCDC 1840356'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 Cl3 N7 O3, C16 H36 N, Br'
_chemical_formula_sum            'C46 H72 Br Cl3 N8 O3'
_chemical_formula_weight         971.37

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'
Cl Cl 0.1484 0.1585 '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           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   16.7927(12)
_cell_length_b                   21.2995(13)
_cell_length_c                   14.8349(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5306.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1530
_cell_measurement_theta_min      3.549
_cell_measurement_theta_max      18.180

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_F_000             2056.0
_exptl_transmission_factor_min   0.774
_exptl_transmission_factor_max   0.848
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.970
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13759
_diffrn_reflns_av_unetI/netI     0.1184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.089
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 0.920
_reflns_number_total             8597
_reflns_number_gt                3437
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_max     0.835
_reflns_Friedel_fraction_full    0.835

_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0200P)²+40.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 912 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.087(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8597
_refine_ls_number_parameters     538
_refine_ls_number_restraints     149
_refine_ls_R_factor_all          0.2022
_refine_ls_R_factor_gt           0.0901
_refine_ls_wR_factor_ref         0.2352
_refine_ls_wR_factor_gt          0.1589
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002

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
C18B C 0.466(2) 0.269(3) 0.8911(8) 0.143(12) Uani 0.5 1 d D U P A 1
H18D H 0.4630 0.2266 0.9132 0.215 Uiso 0.5 1 calc R U P A 1
H18E H 0.4164 0.2897 0.8999 0.215 Uiso 0.5 1 calc R U P A 1
H18F H 0.5074 0.2910 0.9233 0.215 Uiso 0.5 1 calc R U P A 1
C18A C 0.476(2) 0.2085(10) 0.8451(19) 0.143(12) Uani 0.5 1 d D U P A 2
H18A H 0.4987 0.1742 0.8120 0.215 Uiso 0.5 1 calc R U P A 2
H18B H 0.4203 0.2008 0.8547 0.215 Uiso 0.5 1 calc R U P A 2
H18C H 0.5023 0.2123 0.9023 0.215 Uiso 0.5 1 calc R U P A 2
C24 C 0.3019(9) 0.4543(7) 0.2330(13) 0.102(7) Uani 1 1 d G . . . .
C25 C 0.2293(9) 0.4633(8) 0.1898(14) 0.131(9) Uani 1 1 d G . . . .
H25 H 0.2008 0.4289 0.1685 0.157 Uiso 1 1 calc R U . . .
C26 C 0.1994(10) 0.5236(9) 0.1783(15) 0.137(10) Uani 1 1 d G . . . .
C27 C 0.2421(14) 0.5750(7) 0.2101(18) 0.207(18) Uani 1 1 d G U . . .
C29 C 0.3147(14) 0.5660(8) 0.253(2) 0.39(5) Uani 1 1 d G . . . .
H29 H 0.3432 0.6003 0.2746 0.471 Uiso 1 1 calc R U . . .
C30 C 0.3445(10) 0.5056(10) 0.2648(16) 0.24(2) Uani 1 1 d G . . . .
H30 H 0.3931 0.4996 0.2937 0.284 Uiso 1 1 calc R U . . .
C14 C 0.5175(9) 0.2487(9) 0.6109(7) 0.147(9) Uani 1 1 d G U . . .
C15 C 0.5167(10) 0.3093(8) 0.6458(8) 0.145(8) Uani 1 1 d G U . . .
H15 H 0.5267 0.3434 0.6083 0.174 Uiso 1 1 calc R U . . .
C16 C 0.5011(11) 0.3189(7) 0.7367(9) 0.175(9) Uani 1 1 d G U . . .
C17 C 0.4861(10) 0.2680(9) 0.7928(7) 0.164(10) Uani 1 1 d DG U . . .
C19 C 0.4869(10) 0.2074(8) 0.7579(10) 0.181(9) Uani 1 1 d G U . . .
H19 H 0.4769 0.1733 0.7954 0.217 Uiso 1 1 calc R U . . .
C20 C 0.5026(11) 0.1978(7) 0.6670(10) 0.165(9) Uani 1 1 d G U . . .
H20 H 0.5031 0.1573 0.6436 0.198 Uiso 1 1 calc R U . . .
Br1 Br 0.49975(13) 0.37091(9) 0.3763(6) 0.0967(7) Uani 1 1 d . . . . .
Cl1 Cl 0.9456(4) 0.5173(3) 0.2979(8) 0.136(2) Uani 1 1 d . . . . .
Cl3 Cl 0.1093(7) 0.5322(5) 0.1350(11) 0.252(6) Uani 1 1 d . . . . .
C4 C 0.7256(11) 0.4544(8) 0.3211(13) 0.073(5) Uani 1 1 d . . . . .
N3 N 0.6734(8) 0.4105(7) 0.2821(12) 0.081(4) Uani 1 1 d . . . . .
H3N H 0.6273 0.4075 0.3070 0.097 Uiso 1 1 calc R U . . .
C9 C 0.8487(11) 0.5085(9) 0.3366(15) 0.079(5) Uani 1 1 d . . . . .
O1 O 0.7445(9) 0.3783(7) 0.1610(10) 0.104(5) Uani 1 1 d . . . . .
N8 N 0.2771(10) 0.3991(9) 0.5840(12) 0.150(8) Uani 1 1 d D U . . .
N5 N 0.5349(11) 0.2523(11) 0.5163(11) 0.109(6) Uani 1 1 d . . . . .
H5N H 0.5380 0.2881 0.4898 0.131 Uiso 1 1 calc R U . . .
C10 C 0.8015(11) 0.4636(8) 0.2930(14) 0.080(5) Uani 1 1 d . . . . .
H10 H 0.8220 0.4404 0.2453 0.096 Uiso 1 1 calc R U . . .
C5 C 0.6968(12) 0.4866(9) 0.3914(16) 0.102(7) Uani 1 1 d . . . . .
H5 H 0.6454 0.4789 0.4121 0.122 Uiso 1 1 calc R U . . .
N1 N 0.5256(10) 0.2191(7) 0.1919(12) 0.080(4) Uani 1 1 d . . . . .
N4 N 0.5463(10) 0.2045(8) 0.3801(17) 0.110(5) Uani 1 1 d . . . . .
H4N H 0.5386 0.2413 0.3579 0.132 Uiso 1 1 calc R U . . .
N2 N 0.6315(9) 0.3264(7) 0.1995(12) 0.093(5) Uani 1 1 d . . . . .
H2N H 0.5945 0.3231 0.2393 0.112 Uiso 1 1 calc R U . . .
C3 C 0.6866(13) 0.3710(10) 0.2080(15) 0.086(6) Uani 1 1 d . . . . .
C6 C 0.7443(17) 0.5319(10) 0.4338(17) 0.119(8) Uani 1 1 d . . . . .
H6 H 0.7227 0.5549 0.4812 0.142 Uiso 1 1 calc R U . . .
Cl2 Cl 0.4882(7) 0.3831(6) 0.7871(10) 0.261(6) Uani 1 1 d . . . . .
N6 N 0.3823(10) 0.2985(8) 0.2051(14) 0.104(5) Uani 1 1 d . . . . .
H6N H 0.4143 0.3027 0.2499 0.124 Uiso 1 1 calc R U . . .
C23 C 0.3278(15) 0.3455(12) 0.186(2) 0.107(8) Uani 1 1 d . . . . .
C12 C 0.5584(18) 0.1530(11) 0.318(2) 0.138(9) Uani 1 1 d . . . . .
H12A H 0.6148 0.1430 0.3170 0.166 Uiso 1 1 calc R U . . .
H12B H 0.5306 0.1166 0.3409 0.166 Uiso 1 1 calc R U . . .
O3 O 0.2812(10) 0.3415(7) 0.1258(15) 0.142(7) Uani 1 1 d . . . . .
C13 C 0.5462(14) 0.1988(13) 0.470(2) 0.107(7) Uani 1 1 d . . . . .
C31 C 0.335(2) 0.4446(14) 0.619(2) 0.172(12) Uani 1 1 d . . . . .
H31A H 0.3059 0.4731 0.6574 0.206 Uiso 1 1 calc R U . . .
H31B H 0.3714 0.4215 0.6570 0.206 Uiso 1 1 calc R U . . .
C32 C 0.3833(17) 0.4830(13) 0.560(2) 0.143(10) Uani 1 1 d . . . . .
H32A H 0.3498 0.5164 0.5364 0.172 Uiso 1 1 calc R U . . .
H32B H 0.3988 0.4573 0.5085 0.172 Uiso 1 1 calc R U . . .
C8 C 0.8769(14) 0.5883(12) 0.4622(18) 0.153(11) Uani 1 1 d . . . . .
H8A H 0.9140 0.6090 0.4229 0.230 Uiso 1 1 calc R U . . .
H8B H 0.9056 0.5646 0.5066 0.230 Uiso 1 1 calc R U . . .
H8C H 0.8442 0.6191 0.4916 0.230 Uiso 1 1 calc R U . . .
C11 C 0.535(3) 0.1620(13) 0.233(2) 0.22(2) Uani 1 1 d . . . . .
H11A H 0.4842 0.1407 0.2270 0.269 Uiso 1 1 calc R U . . .
H11B H 0.5724 0.1388 0.1955 0.269 Uiso 1 1 calc R U . . .
C7 C 0.8244(16) 0.5442(11) 0.4072(18) 0.112(8) Uani 1 1 d . . . . .
C1 C 0.591(2) 0.2302(15) 0.137(2) 0.23(2) Uani 1 1 d . . . . .
H1A H 0.6299 0.1991 0.1550 0.279 Uiso 1 1 calc R U . . .
H1B H 0.5735 0.2180 0.0771 0.279 Uiso 1 1 calc R U . . .
O2 O 0.5575(11) 0.1474(9) 0.5042(13) 0.138(6) Uani 1 1 d . . . . .
C2 C 0.6331(14) 0.2838(11) 0.1245(15) 0.118(8) Uani 1 1 d . . . . .
H2A H 0.6124 0.3053 0.0718 0.142 Uiso 1 1 calc R U . . .
H2B H 0.6880 0.2727 0.1120 0.142 Uiso 1 1 calc R U . . .
C21 C 0.457(2) 0.2163(16) 0.141(3) 0.22(2) Uani 1 1 d . . . . .
H21A H 0.4733 0.2286 0.0809 0.263 Uiso 1 1 calc R U . . .
H21B H 0.4449 0.1718 0.1369 0.263 Uiso 1 1 calc R U . . .
C22 C 0.3858(16) 0.2429(12) 0.151(2) 0.135(9) Uani 1 1 d . . . . .
H22A H 0.3500 0.2121 0.1767 0.161 Uiso 1 1 calc R U . . .
H22B H 0.3657 0.2533 0.0913 0.161 Uiso 1 1 calc R U . . .
C33 C 0.4555(15) 0.5118(12) 0.596(2) 0.183(15) Uani 1 1 d D . . . .
H33A H 0.4892 0.4771 0.6145 0.220 Uiso 1 1 calc R U . . .
H33B H 0.4391 0.5326 0.6512 0.220 Uiso 1 1 calc R U . . .
N7 N 0.3370(11) 0.3983(8) 0.2423(15) 0.114(6) Uani 1 1 d . . . . .
H7N H 0.3687 0.3941 0.2874 0.137 Uiso 1 1 calc R U . . .
C39 C 0.2231(13) 0.3731(12) 0.6591(12) 0.186(11) Uani 1 1 d D U . . .
H39A H 0.1822 0.3468 0.6325 0.223 Uiso 1 1 calc R U . . .
H39B H 0.1970 0.4077 0.6896 0.223 Uiso 1 1 calc R U . . .
C34 C 0.5112(19) 0.5585(14) 0.548(2) 0.212(16) Uani 1 1 d D . . . .
H34A H 0.4899 0.5685 0.4898 0.317 Uiso 1 1 calc R U . . .
H34B H 0.5630 0.5399 0.5412 0.317 Uiso 1 1 calc R U . . .
H34C H 0.5156 0.5961 0.5834 0.317 Uiso 1 1 calc R U . . .
C40 C 0.2709(15) 0.3345(14) 0.7282(17) 0.223(13) Uani 1 1 d D U . . .
H40A H 0.3051 0.3041 0.6988 0.268 Uiso 1 1 calc R U . . .
H40B H 0.3029 0.3613 0.7667 0.268 Uiso 1 1 calc R U . . .
C41 C 0.2038(16) 0.3022(17) 0.7816(17) 0.235(13) Uani 1 1 d D U . . .
H41A H 0.1612 0.3317 0.7937 0.282 Uiso 1 1 calc R U . . .
H41B H 0.1822 0.2674 0.7473 0.282 Uiso 1 1 calc R U . . .
C42 C 0.240(2) 0.278(2) 0.871(2) 0.294(19) Uani 1 1 d D U . . .
H42A H 0.2932 0.2639 0.8602 0.440 Uiso 1 1 calc R U . . .
H42B H 0.2081 0.2443 0.8935 0.440 Uiso 1 1 calc R U . . .
H42C H 0.2406 0.3119 0.9139 0.440 Uiso 1 1 calc R U . . .
C35 C 0.2327(16) 0.4291(11) 0.5040(15) 0.199(12) Uani 1 1 d D U . . .
H35A H 0.2698 0.4419 0.4573 0.239 Uiso 1 1 calc R U . . .
H35B H 0.1944 0.4001 0.4784 0.239 Uiso 1 1 calc R U . . .
C36 C 0.1905(16) 0.4865(12) 0.5453(19) 0.196(13) Uani 1 1 d D U . . .
H36A H 0.2298 0.5154 0.5694 0.235 Uiso 1 1 calc R U . . .
H36B H 0.1565 0.4731 0.5945 0.235 Uiso 1 1 calc R U . . .
C28 C 0.213(3) 0.6396(15) 0.185(3) 0.32(3) Uani 1 1 d . U . . .
H28A H 0.2051 0.6420 0.1214 0.480 Uiso 1 1 calc R U . . .
H28B H 0.2509 0.6704 0.2040 0.480 Uiso 1 1 calc R U . . .
H28C H 0.1628 0.6474 0.2153 0.480 Uiso 1 1 calc R U . . .
C45 C 0.3256(16) 0.2423(11) 0.459(2) 0.227(19) Uani 1 1 d D . . . .
H45A H 0.3485 0.2243 0.5127 0.273 Uiso 1 1 calc R U . . .
H45B H 0.3691 0.2576 0.4216 0.273 Uiso 1 1 calc R U . . .
C44 C 0.2733(14) 0.2986(10) 0.4857(19) 0.167(12) Uani 1 1 d D . . . .
H44A H 0.2326 0.2845 0.5276 0.201 Uiso 1 1 calc R U . . .
H44B H 0.2467 0.3149 0.4326 0.201 Uiso 1 1 calc R U . . .
C43 C 0.3219(16) 0.3516(12) 0.5299(19) 0.165(13) Uani 1 1 d D . . . .
H43A H 0.3614 0.3325 0.5688 0.198 Uiso 1 1 calc R U . . .
H43B H 0.3504 0.3737 0.4826 0.198 Uiso 1 1 calc R U . . .
C37 C 0.140(2) 0.5200(10) 0.473(2) 0.26(2) Uani 1 1 d D . . . .
H37A H 0.0897 0.4978 0.4723 0.310 Uiso 1 1 calc R U . . .
H37B H 0.1659 0.5103 0.4162 0.310 Uiso 1 1 calc R U . . .
C46 C 0.282(2) 0.1900(15) 0.407(2) 0.29(3) Uani 1 1 d D . . . .
H46A H 0.2475 0.2084 0.3624 0.431 Uiso 1 1 calc R U . . .
H46B H 0.2511 0.1654 0.4480 0.431 Uiso 1 1 calc R U . . .
H46C H 0.3204 0.1636 0.3772 0.431 Uiso 1 1 calc R U . . .
C38 C 0.118(3) 0.5901(12) 0.467(3) 0.31(3) Uani 1 1 d D . . . .
H38A H 0.1655 0.6143 0.4564 0.468 Uiso 1 1 calc R U . . .
H38B H 0.0939 0.6032 0.5223 0.468 Uiso 1 1 calc R U . . .
H38C H 0.0816 0.5963 0.4180 0.468 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C18B C17 1.4952 . ?
C18A C17 1.4952(10) . ?
C24 N7 1.34(2) . ?
C24 C25 1.3900 . ?
C24 C30 1.3900 . ?
C25 C26 1.3900 . ?
C26 C27 1.3900 . ?
C26 Cl3 1.655(17) . ?
C27 C29 1.3900 . ?
C27 C28 1.51(3) . ?
C29 C30 1.3900 . ?
C14 C15 1.3900 . ?
C14 C20 1.3900 . ?
C14 N5 1.435(18) . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C16 Cl2 1.573(16) . ?
C17 C19 1.3900 . ?
C19 C20 1.3900 . ?
Cl1 C9 1.735(19) . ?
C4 C5 1.34(2) . ?
C4 C10 1.35(2) . ?
C4 N3 1.41(2) . ?
N3 C3 1.40(2) . ?
C9 C7 1.36(3) . ?
C9 C10 1.40(2) . ?
O1 C3 1.21(2) . ?
N8 C31 1.47(3) . ?
N8 C43 1.49(3) . ?
N8 C39 1.5397(14) . ?
N8 C35 1.5400(14) . ?
N5 C13 1.35(3) . ?
C5 C6 1.40(3) . ?
N1 C11 1.37(3) . ?
N1 C21 1.39(3) . ?
N1 C1 1.38(3) . ?
N4 C13 1.33(3) . ?
N4 C12 1.45(3) . ?
N2 C3 1.33(2) . ?
N2 C2 1.44(2) . ?
C6 C7 1.43(3) . ?
N6 C23 1.39(3) . ?
N6 C22 1.43(3) . ?
C23 O3 1.19(3) . ?
C23 N7 1.41(3) . ?
C12 C11 1.33(3) . ?
C13 O2 1.22(3) . ?
C31 C32 1.45(3) . ?
C32 C33 1.46(3) . ?
C8 C7 1.52(3) . ?
C1 C2 1.36(3) . ?
C21 C22 1.32(3) . ?
C33 C34 1.5392(14) . ?
C39 C40 1.5397(14) . ?
C40 C41 1.5398(14) . ?
C41 C42 1.5399(15) . ?
C35 C36 1.5401(14) . ?
C36 C37 1.5401(14) . ?
C45 C44 1.5399(14) . ?
C45 C46 1.5394(14) . ?
C44 C43 1.5398(14) . ?
C37 C38 1.5398(14) . ?

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
N7 C24 C25 123.8(15) . . ?
N7 C24 C30 116.1(15) . . ?
C25 C24 C30 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C27 120.0 . . ?
C25 C26 Cl3 118.7(14) . . ?
C27 C26 Cl3 121.1(14) . . ?
C29 C27 C26 120.0 . . ?
C29 C27 C28 122(2) . . ?
C26 C27 C28 118(2) . . ?
C27 C29 C30 120.0 . . ?
C29 C30 C24 120.0 . . ?
C15 C14 C20 120.0 . . ?
C15 C14 N5 108.4(15) . . ?
C20 C14 N5 131.6(15) . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 Cl2 128.0(11) . . ?
C17 C16 Cl2 111.7(11) . . ?
C16 C17 C19 120.0 . . ?
C16 C17 C18A 173.0(17) . . ?
C19 C17 C18A 53.7(15) . . ?
C16 C17 C18B 128(3) . . ?
C19 C17 C18B 112(3) . . ?
C20 C19 C17 120.0 . . ?
C19 C20 C14 120.0 . . ?
C5 C4 C10 120.4(19) . . ?
C5 C4 N3 115.8(18) . . ?
C10 C4 N3 123.8(17) . . ?
C3 N3 C4 128.5(16) . . ?
C7 C9 C10 125(2) . . ?
C7 C9 Cl1 118.5(18) . . ?
C10 C9 Cl1 116.9(16) . . ?
C31 N8 C43 107.6(17) . . ?
C31 N8 C39 112.0(19) . . ?
C43 N8 C39 116.2(19) . . ?
C31 N8 C35 108(2) . . ?
C43 N8 C35 96.4(17) . . ?
C39 N8 C35 114.9(19) . . ?
C13 N5 C14 119(2) . . ?
C4 C10 C9 119.4(18) . . ?
C4 C5 C6 120(2) . . ?
C11 N1 C21 107(3) . . ?
C11 N1 C1 109(3) . . ?
C21 N1 C1 110(2) . . ?
C13 N4 C12 125(2) . . ?
C3 N2 C2 120.8(18) . . ?
O1 C3 N2 127(2) . . ?
O1 C3 N3 120(2) . . ?
N2 C3 N3 113.1(17) . . ?
C5 C6 C7 123(2) . . ?
C23 N6 C22 121(2) . . ?
O3 C23 N6 122(3) . . ?
O3 C23 N7 125(3) . . ?
N6 C23 N7 113(2) . . ?
C11 C12 N4 117(2) . . ?
O2 C13 N4 120(3) . . ?
O2 C13 N5 124(3) . . ?
N4 C13 N5 116(2) . . ?
C32 C31 N8 122(3) . . ?
C31 C32 C33 119(3) . . ?
C12 C11 N1 125(2) . . ?
C9 C7 C6 113(2) . . ?
C9 C7 C8 126(2) . . ?
C6 C7 C8 121(2) . . ?
C2 C1 N1 130(2) . . ?
C1 C2 N2 115(2) . . ?
C22 C21 N1 132(3) . . ?
C21 C22 N6 117(2) . . ?
C32 C33 C34 127(3) . . ?
C24 N7 C23 127(2) . . ?
N8 C39 C40 111.5(19) . . ?
C41 C40 C39 101.5(19) . . ?
C42 C41 C40 108(2) . . ?
C36 C35 N8 104(2) . . ?
C35 C36 C37 110(2) . . ?
C44 C45 C46 115(2) . . ?
C45 C44 C43 112(2) . . ?
N8 C43 C44 117(2) . . ?
C36 C37 C38 128(3) . . ?

_refine_diff_density_max         0.505
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.061


# start Validation Reply Form
_vrf_PLAT234_Tren-Cl-Me-nco-TBABr 
;
PROBLEM: Large Hirshfeld Difference C18A     --C19              0.32 Ang. 
RESPONSE: This may be due to disorder in the model.
;
_vrf_PLAT241_Tren-Cl-Me-nco-TBABr 
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C29 Check  
RESPONSE: This may be due to mismatching of U(eq) values.
;
_vrf_PLAT410_Tren-Cl-Me-nco-TBABr 
;
PROBLEM: Short Intra H...H Contact  H1B      ..H21A             1.70 Ang.   
RESPONSE: This may be due to short distances between adjacent H atoms.
;
####################################################################### 
# 
# 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_Tren-Br-Me-nco_TBAF
_database_code_depnum_ccdc_archive 'CCDC 1840359'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 Br3 N7 O3, C16 H36 N, F'
_chemical_formula_sum            'C46 H72 Br3 F N8 O3'
_chemical_formula_weight         1043.82

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'
F F 0.0171 0.0103 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   8.9493(5)
_cell_length_b                   22.5028(14)
_cell_length_c                   25.721(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.732(6)
_cell_angle_gamma                90
_cell_volume                     5179.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3914
_cell_measurement_theta_min      3.5950
_cell_measurement_theta_max      21.5820

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_F_000             2168.0
_exptl_transmission_factor_min   0.494
_exptl_transmission_factor_max   0.621
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    2.385
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21566
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.901
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9120
_reflns_number_gt                4053
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0600P)²+0.6677P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9120
_refine_ls_number_parameters     557
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1564
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.003

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 0.66762(8) 0.48497(4) 0.81153(3) 0.1023(3) Uani 1 1 d . . . . .
Br3 Br 0.06738(9) 0.40590(4) 0.58306(4) 0.1175(4) Uani 1 1 d . . . . .
Br2 Br 0.77495(16) 0.43702(4) 0.35427(4) 0.1599(5) Uani 1 1 d . . . . .
F1 F 0.1810(3) 0.77311(14) 0.40423(11) 0.0596(8) Uani 1 1 d . . . . .
O3 O 0.3834(5) 0.1206(2) 0.60920(18) 0.0849(14) Uani 1 1 d . . . . .
N1 N 0.9231(5) 0.06936(19) 0.61396(17) 0.0504(11) Uani 1 1 d . . . . .
O1 O 1.0031(4) 0.2114(2) 0.76122(17) 0.0795(13) Uani 1 1 d . . . . .
O2 O 0.9977(5) 0.15520(19) 0.44005(17) 0.0826(13) Uani 1 1 d . . . . .
N6 N 0.6345(5) 0.1172(2) 0.60529(19) 0.0663(14) Uani 1 1 d . . . . .
H6N H 0.7144 0.1363 0.5976 0.080 Uiso 1 1 calc R U . . .
C23 C 0.5042(7) 0.1465(3) 0.6036(2) 0.0675(17) Uani 1 1 d . . . . .
N2 N 0.9715(5) 0.1730(2) 0.68032(19) 0.0698(14) Uani 1 1 d . . . . .
H2N H 0.9329 0.1788 0.6499 0.084 Uiso 1 1 calc R U . . .
N3 N 0.8800(5) 0.2643(2) 0.69835(18) 0.0655(13) Uani 1 1 d . . . . .
H3N H 0.8571 0.2640 0.6658 0.079 Uiso 1 1 calc R U . . .
C8 C 0.7461(8) 0.4168(3) 0.7224(3) 0.086(2) Uani 1 1 d . . . . .
N5 N 0.8791(5) 0.2229(2) 0.49240(18) 0.0662(14) Uani 1 1 d . . . . .
H5N H 0.8438 0.2266 0.5232 0.079 Uiso 1 1 calc R U . . .
N7 N 0.5197(5) 0.2057(2) 0.5942(2) 0.0723(15) Uani 1 1 d . . . . .
H7N H 0.6092 0.2178 0.5886 0.087 Uiso 1 1 calc R U . . .
C10 C 0.7928(7) 0.3649(3) 0.6979(3) 0.082(2) Uani 1 1 d . . . . .
H10 H 0.7961 0.3641 0.6618 0.099 Uiso 1 1 calc R U . . .
N4 N 0.9789(5) 0.1391(2) 0.52649(19) 0.0644(13) Uani 1 1 d . . . . .
H4N H 0.9598 0.1554 0.5559 0.077 Uiso 1 1 calc R U . . .
C3 C 0.9548(6) 0.2162(3) 0.7159(3) 0.0632(16) Uani 1 1 d . . . . .
C4 C 0.8348(6) 0.3142(3) 0.7255(2) 0.0619(16) Uani 1 1 d . . . . .
C7 C 0.7386(7) 0.4170(3) 0.7757(3) 0.074(2) Uani 1 1 d . . . . .
N8 N 0.3577(6) 0.2278(3) 0.3581(2) 0.0862(18) Uani 1 1 d . . . . .
C14 C 0.8514(6) 0.2704(3) 0.4586(2) 0.0580(15) Uani 1 1 d . . . . .
C1 C 0.9602(7) 0.0653(3) 0.6693(2) 0.0639(16) Uani 1 1 d . . . . .
H1A H 1.0161 0.0290 0.6754 0.077 Uiso 1 1 calc R U . . .
H1B H 0.8683 0.0627 0.6887 0.077 Uiso 1 1 calc R U . . .
C24 C 0.4097(7) 0.2490(3) 0.5926(2) 0.0652(17) Uani 1 1 d . . . . .
C20 C 0.8045(7) 0.3237(3) 0.4802(3) 0.0757(19) Uani 1 1 d . . . . .
H20 H 0.7897 0.3257 0.5159 0.091 Uiso 1 1 calc R U . . .
C22 C 0.6483(6) 0.0552(3) 0.6193(3) 0.0758(19) Uani 1 1 d . . . . .
H21A H 0.5662 0.0329 0.6039 0.091 Uiso 1 1 calc R U . . .
H21B H 0.6438 0.0510 0.6568 0.091 Uiso 1 1 calc R U . . .
C11 C 1.0540(6) 0.0569(3) 0.5816(2) 0.0625(16) Uani 1 1 d . . . . .
H11A H 1.0720 0.0144 0.5813 0.075 Uiso 1 1 calc R U . . .
H11B H 1.1411 0.0759 0.5970 0.075 Uiso 1 1 calc R U . . .
C13 C 0.9564(7) 0.1706(3) 0.4827(3) 0.0620(16) Uani 1 1 d . . . . .
C12 C 1.0341(7) 0.0786(3) 0.5262(2) 0.0650(16) Uani 1 1 d . . . . .
H12A H 1.1290 0.0770 0.5084 0.078 Uiso 1 1 calc R U . . .
H12B H 0.9638 0.0532 0.5077 0.078 Uiso 1 1 calc R U . . .
C15 C 0.8711(6) 0.2665(3) 0.4052(2) 0.0674(17) Uani 1 1 d . . . . .
H15 H 0.8995 0.2310 0.3897 0.081 Uiso 1 1 calc R U . . .
C17 C 0.8000(8) 0.3692(3) 0.3983(3) 0.083(2) Uani 1 1 d . . . . .
C5 C 0.8328(7) 0.3170(3) 0.7797(2) 0.0734(18) Uani 1 1 d . . . . .
H5 H 0.8649 0.2847 0.7996 0.088 Uiso 1 1 calc R U . . .
C6 C 0.7824(7) 0.3682(3) 0.8037(3) 0.079(2) Uani 1 1 d . . . . .
H6 H 0.7783 0.3695 0.8397 0.095 Uiso 1 1 calc R U . . .
C21 C 0.7957(6) 0.0309(3) 0.6000(3) 0.0709(18) Uani 1 1 d . . . . .
H20A H 0.8120 -0.0083 0.6146 0.085 Uiso 1 1 calc R U . . .
H20B H 0.7903 0.0269 0.5624 0.085 Uiso 1 1 calc R U . . .
C30 C 0.4562(7) 0.3072(3) 0.5917(2) 0.0765(19) Uani 1 1 d . . . . .
H30 H 0.5585 0.3145 0.5929 0.092 Uiso 1 1 calc R U . . .
C27 C 0.2112(7) 0.3423(3) 0.5872(3) 0.079(2) Uani 1 1 d . . . . .
C28 C 0.3613(7) 0.3559(3) 0.5892(3) 0.0764(19) Uani 1 1 d . . . . .
C2 C 1.0503(7) 0.1172(3) 0.6894(2) 0.0723(18) Uani 1 1 d . . . . .
H2A H 1.0691 0.1122 0.7264 0.087 Uiso 1 1 calc R U . . .
H2B H 1.1460 0.1182 0.6721 0.087 Uiso 1 1 calc R U . . .
C43 C 0.4626(7) 0.1945(4) 0.3934(3) 0.105(3) Uani 1 1 d . . . . .
H43A H 0.5308 0.2226 0.4096 0.126 Uiso 1 1 calc R U . . .
H43B H 0.5215 0.1675 0.3726 0.126 Uiso 1 1 calc R U . . .
C35 C 0.4558(7) 0.2589(4) 0.3187(3) 0.120(3) Uani 1 1 d . . . . .
H35B H 0.5210 0.2867 0.3369 0.144 Uiso 1 1 calc R U . . .
H35A H 0.5183 0.2296 0.3019 0.144 Uiso 1 1 calc R U . . .
C26 C 0.1599(7) 0.2855(3) 0.5879(3) 0.089(2) Uani 1 1 d . . . . .
H26 H 0.0575 0.2786 0.5875 0.107 Uiso 1 1 calc R U . . .
C44 C 0.3859(9) 0.1593(5) 0.4355(3) 0.149(4) Uani 1 1 d D . . . .
H44A H 0.3230 0.1291 0.4195 0.179 Uiso 1 1 calc R U . . .
H44B H 0.3222 0.1856 0.4552 0.179 Uiso 1 1 calc R U . . .
C18 C 0.7789(8) 0.3741(3) 0.4506(3) 0.089(2) Uani 1 1 d . . . . .
C25 C 0.2570(7) 0.2382(3) 0.5891(3) 0.082(2) Uani 1 1 d . . . . .
H25 H 0.2210 0.1995 0.5877 0.098 Uiso 1 1 calc R U . . .
C16 C 0.8468(8) 0.3174(3) 0.3758(3) 0.086(2) Uani 1 1 d . . . . .
H16 H 0.8626 0.3163 0.3401 0.103 Uiso 1 1 calc R U . . .
C31 C 0.2482(7) 0.1856(4) 0.3324(3) 0.089(2) Uani 1 1 d . . . . .
H31A H 0.1878 0.1677 0.3593 0.107 Uiso 1 1 calc R U . . .
H31B H 0.1818 0.2086 0.3101 0.107 Uiso 1 1 calc R U . . .
C29 C 0.4212(8) 0.4188(3) 0.5877(4) 0.114(3) Uani 1 1 d . . . . .
H29A H 0.5284 0.4179 0.5887 0.171 Uiso 1 1 calc R U . . .
H29B H 0.3853 0.4406 0.6171 0.171 Uiso 1 1 calc R U . . .
H29C H 0.3878 0.4379 0.5562 0.171 Uiso 1 1 calc R U . . .
C32 C 0.3154(8) 0.1373(4) 0.3010(3) 0.127(3) Uani 1 1 d D . . . .
H32A H 0.3719 0.1106 0.3233 0.153 Uiso 1 1 calc R U . . .
H32B H 0.3827 0.1540 0.2756 0.153 Uiso 1 1 calc R U . . .
C19 C 0.7353(11) 0.4320(3) 0.4774(3) 0.132(3) Uani 1 1 d . . . . .
H19A H 0.7307 0.4256 0.5143 0.199 Uiso 1 1 calc R U . . .
H19C H 0.6393 0.4447 0.4646 0.199 Uiso 1 1 calc R U . . .
H19B H 0.8084 0.4619 0.4702 0.199 Uiso 1 1 calc R U . . .
C39 C 0.2635(8) 0.2712(4) 0.3880(3) 0.106(3) Uani 1 1 d . . . . .
H39B H 0.2001 0.2930 0.3638 0.128 Uiso 1 1 calc R U . . .
H39A H 0.1994 0.2495 0.4114 0.128 Uiso 1 1 calc R U . . .
C9 C 0.7104(11) 0.4711(4) 0.6907(3) 0.140(3) Uani 1 1 d . . . . .
H9A H 0.6040 0.4762 0.6886 0.209 Uiso 1 1 calc R U . . .
H9B H 0.7494 0.4664 0.6563 0.209 Uiso 1 1 calc R U . . .
H9C H 0.7548 0.5053 0.7069 0.209 Uiso 1 1 calc R U . . .
C33 C 0.1900(10) 0.1037(5) 0.2736(4) 0.166(4) Uani 1 1 d D . . . .
H33A H 0.1269 0.1322 0.2554 0.199 Uiso 1 1 calc R U . . .
H33B H 0.1293 0.0846 0.2997 0.199 Uiso 1 1 calc R U . . .
C34 C 0.2396(15) 0.0562(6) 0.2344(5) 0.253(7) Uani 1 1 d D . . . .
H34A H 0.2832 0.0752 0.2048 0.379 Uiso 1 1 calc R U . . .
H34C H 0.1545 0.0332 0.2233 0.379 Uiso 1 1 calc R U . . .
H34B H 0.3120 0.0304 0.2506 0.379 Uiso 1 1 calc R U . . .
C36 C 0.3673(9) 0.2920(5) 0.2778(4) 0.166(5) Uani 1 1 d D . . . .
H36A H 0.2844 0.2675 0.2660 0.199 Uiso 1 1 calc R U . . .
H36B H 0.3265 0.3280 0.2928 0.199 Uiso 1 1 calc R U . . .
C37 C 0.4629(12) 0.3078(6) 0.2324(4) 0.263(9) Uani 1 1 d D . . . .
H37B H 0.4006 0.3247 0.2050 0.315 Uiso 1 1 calc R U . . .
H37A H 0.5091 0.2721 0.2189 0.315 Uiso 1 1 calc R U . . .
C38 C 0.5853(16) 0.3527(6) 0.2477(5) 0.233(7) Uani 1 1 d D . . . .
H38B H 0.5409 0.3860 0.2651 0.350 Uiso 1 1 calc R U . . .
H38A H 0.6350 0.3662 0.2171 0.350 Uiso 1 1 calc R U . . .
H38C H 0.6565 0.3340 0.2707 0.350 Uiso 1 1 calc R U . . .
C40 C 0.3572(13) 0.3146(6) 0.4189(5) 0.183(5) Uani 1 1 d . . . . .
H40A H 0.4153 0.2936 0.4452 0.220 Uiso 1 1 calc R U . . .
H40B H 0.4257 0.3351 0.3961 0.220 Uiso 1 1 calc R U . . .
C41 C 0.2560(18) 0.3585(6) 0.4443(5) 0.238(8) Uani 1 1 d D . . . .
H41A H 0.3009 0.3705 0.4772 0.286 Uiso 1 1 calc R U . . .
H41B H 0.1622 0.3390 0.4518 0.286 Uiso 1 1 calc R U . . .
C42 C 0.223(2) 0.4146(7) 0.4120(7) 0.306(11) Uani 1 1 d D . . . .
H42A H 0.3103 0.4392 0.4110 0.459 Uiso 1 1 calc R U . . .
H42B H 0.1424 0.4363 0.4275 0.459 Uiso 1 1 calc R U . . .
H42C H 0.1946 0.4034 0.3772 0.459 Uiso 1 1 calc R U . . .
C46 C 0.611(2) 0.0842(6) 0.4512(5) 0.275(10) Uani 1 1 d D . . . .
H46B H 0.5637 0.0605 0.4248 0.412 Uiso 1 1 calc R U . . .
H46C H 0.6467 0.0590 0.4789 0.412 Uiso 1 1 calc R U . . .
H46A H 0.6942 0.1052 0.4365 0.412 Uiso 1 1 calc R U . . .
C45 C 0.4985(12) 0.1292(7) 0.4729(4) 0.222(7) Uani 1 1 d D . . . .
H45B H 0.5550 0.1604 0.4901 0.267 Uiso 1 1 calc R U . . .
H45A H 0.4416 0.1090 0.4994 0.267 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C7 1.899(6) . ?
Br3 C27 1.927(6) . ?
Br2 C17 1.912(7) . ?
O3 C23 1.239(6) . ?
N1 C1 1.459(7) . ?
N1 C21 1.472(7) . ?
N1 C11 1.472(6) . ?
O1 C3 1.242(7) . ?
O2 C13 1.213(6) . ?
N6 C23 1.340(7) . ?
N6 C22 1.444(7) . ?
C23 N7 1.362(8) . ?
N2 C3 1.345(7) . ?
N2 C2 1.459(7) . ?
N3 C3 1.349(7) . ?
N3 C4 1.386(7) . ?
C8 C7 1.374(9) . ?
C8 C10 1.393(9) . ?
C8 C9 1.501(10) . ?
N5 C13 1.389(7) . ?
N5 C14 1.396(7) . ?
N7 C24 1.386(7) . ?
C10 C4 1.393(9) . ?
N4 C13 1.345(7) . ?
N4 C12 1.447(7) . ?
C4 C5 1.396(8) . ?
C7 C6 1.367(9) . ?
N8 C43 1.497(8) . ?
N8 C39 1.507(8) . ?
N8 C31 1.509(8) . ?
N8 C35 1.521(8) . ?
C14 C20 1.389(8) . ?
C14 C15 1.391(7) . ?
C1 C2 1.508(8) . ?
C24 C30 1.375(8) . ?
C24 C25 1.389(8) . ?
C20 C18 1.382(9) . ?
C22 C21 1.518(7) . ?
C11 C12 1.517(8) . ?
C15 C16 1.389(8) . ?
C17 C18 1.366(9) . ?
C17 C16 1.368(9) . ?
C5 C6 1.386(8) . ?
C30 C28 1.388(8) . ?
C27 C26 1.358(9) . ?
C27 C28 1.378(8) . ?
C28 C29 1.514(9) . ?
C43 C44 1.514(9) . ?
C35 C36 1.506(10) . ?
C26 C25 1.374(8) . ?
C44 C45 1.5392(10) . ?
C18 C19 1.527(9) . ?
C31 C32 1.487(9) . ?
C32 C33 1.5198(7) . ?
C39 C40 1.507(12) . ?
C33 C34 1.5388(10) . ?
C36 C37 1.4997(10) . ?
C37 C38 1.5387(10) . ?
C40 C41 1.495(14) . ?
C41 C42 1.5392(10) . ?
C46 C45 1.5386(10) . ?

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 N1 C21 111.5(4) . . ?
C1 N1 C11 111.5(4) . . ?
C21 N1 C11 111.7(4) . . ?
C23 N6 C22 123.7(5) . . ?
O3 C23 N6 121.7(7) . . ?
O3 C23 N7 124.9(6) . . ?
N6 C23 N7 113.4(5) . . ?
C3 N2 C2 124.8(5) . . ?
C3 N3 C4 129.0(5) . . ?
C7 C8 C10 118.3(7) . . ?
C7 C8 C9 121.7(7) . . ?
C10 C8 C9 119.9(8) . . ?
C13 N5 C14 128.4(5) . . ?
C23 N7 C24 128.3(5) . . ?
C8 C10 C4 122.3(7) . . ?
C13 N4 C12 122.6(5) . . ?
O1 C3 N2 122.5(6) . . ?
O1 C3 N3 123.3(6) . . ?
N2 C3 N3 114.3(6) . . ?
N3 C4 C10 119.0(6) . . ?
N3 C4 C5 123.1(6) . . ?
C10 C4 C5 117.9(6) . . ?
C6 C7 C8 120.3(7) . . ?
C6 C7 Br1 119.1(6) . . ?
C8 C7 Br1 120.6(6) . . ?
C43 N8 C39 111.5(6) . . ?
C43 N8 C31 110.5(6) . . ?
C39 N8 C31 105.5(5) . . ?
C43 N8 C35 105.7(5) . . ?
C39 N8 C35 111.8(6) . . ?
C31 N8 C35 112.0(6) . . ?
C20 C14 C15 119.4(6) . . ?
C20 C14 N5 117.7(5) . . ?
C15 C14 N5 122.8(6) . . ?
N1 C1 C2 113.6(5) . . ?
C30 C24 N7 117.1(5) . . ?
C30 C24 C25 117.6(6) . . ?
N7 C24 C25 125.2(6) . . ?
C18 C20 C14 122.5(6) . . ?
N6 C22 C21 109.8(5) . . ?
N1 C11 C12 112.7(5) . . ?
O2 C13 N4 124.2(6) . . ?
O2 C13 N5 124.3(6) . . ?
N4 C13 N5 111.5(5) . . ?
N4 C12 C11 109.5(5) . . ?
C16 C15 C14 117.7(6) . . ?
C18 C17 C16 122.2(6) . . ?
C18 C17 Br2 120.1(6) . . ?
C16 C17 Br2 117.6(5) . . ?
C6 C5 C4 119.2(6) . . ?
C7 C6 C5 121.9(7) . . ?
N1 C21 C22 112.5(5) . . ?
C24 C30 C28 124.6(6) . . ?
C26 C27 C28 122.6(6) . . ?
C26 C27 Br3 118.3(5) . . ?
C28 C27 Br3 119.2(6) . . ?
C27 C28 C30 115.0(6) . . ?
C27 C28 C29 123.5(7) . . ?
C30 C28 C29 121.5(6) . . ?
N2 C2 C1 110.9(5) . . ?
N8 C43 C44 114.1(6) . . ?
C36 C35 N8 113.0(6) . . ?
C27 C26 C25 121.0(6) . . ?
C43 C44 C45 112.2(7) . . ?
C17 C18 C20 116.9(7) . . ?
C17 C18 C19 123.6(7) . . ?
C20 C18 C19 119.5(7) . . ?
C26 C25 C24 119.2(6) . . ?
C17 C16 C15 121.3(6) . . ?
C32 C31 N8 115.6(6) . . ?
C31 C32 C33 108.4(7) . . ?
C40 C39 N8 112.2(7) . . ?
C32 C33 C34 115.6(9) . . ?
C37 C36 C35 111.2(7) . . ?
C36 C37 C38 111.6(10) . . ?
C41 C40 C39 108.8(10) . . ?
C40 C41 C42 114.9(13) . . ?
C46 C45 C44 119.4(12) . . ?

_refine_diff_density_max         0.620
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.065


# start Validation Reply Form
_vrf_PLAT234_Tren-Br-Me-nco_TBAF 
;
PROBLEM: Large Hirshfeld Difference C36      --C37              0.32 Ang.  
RESPONSE: This may be due to disorder in the model.
;
####################################################################### 
# 
# 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_T-Br-Me-TEASiF6
_database_code_depnum_ccdc_archive 'CCDC 1840361'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C30 H35 Br3 N7 O3), F6 Si'
_chemical_formula_sum            'C60 H70 Br6 F6 N14 O6 Si'
_chemical_formula_weight         1704.79

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'
F F 0.0171 0.0103 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+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                   15.372(6)
_cell_length_b                   21.983(6)
_cell_length_c                   26.797(9)
_cell_angle_alpha                90
_cell_angle_beta                 92.632(10)
_cell_angle_gamma                90
_cell_volume                     9046(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1487
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      12.91

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_F_000             3416.0
_exptl_transmission_factor_min   0.434
_exptl_transmission_factor_max   0.533
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_absorpt_coefficient_mu    2.734
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22832
_diffrn_reflns_av_unetI/netI     0.3982
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.521
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             7890
_reflns_number_gt                5341
_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-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0500P)²+0.3670P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7890
_refine_ls_number_parameters     380
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.3126
_refine_ls_R_factor_gt           0.0927
_refine_ls_wR_factor_ref         0.2246
_refine_ls_wR_factor_gt          0.2090
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.002

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
C24 C 0.2973(7) 0.0732(3) 0.6939(3) 0.094(5) Uani 1 1 d G U . . .
C30 C 0.3870(7) 0.0671(4) 0.6915(4) 0.123(5) Uani 1 1 d G U . . .
H30 H 0.4228 0.0717 0.7202 0.147 Uiso 1 1 calc R U . . .
C29 C 0.4233(4) 0.0540(4) 0.6461(5) 0.177(7) Uani 1 1 d G U . . .
H29 H 0.4833 0.0499 0.6445 0.212 Uiso 1 1 calc R U . . .
C28 C 0.3699(8) 0.0471(4) 0.6032(3) 0.209(11) Uani 1 1 d G U . . .
C26 C 0.2802(8) 0.0532(4) 0.6057(3) 0.153(6) Uani 1 1 d G U . . .
C25 C 0.2439(4) 0.0663(4) 0.6510(5) 0.121(5) Uani 1 1 d G U . . .
H25 H 0.1839 0.0704 0.6527 0.145 Uiso 1 1 calc R U . . .
C14 C -0.0578(5) 0.2357(3) 0.8291(4) 0.100(5) Uani 1 1 d G U . . .
C15 C -0.0398(5) 0.2874(5) 0.8576(3) 0.109(5) Uani 1 1 d G U . . .
H15 H -0.0135 0.2837 0.8894 0.131 Uiso 1 1 calc R U . . .
C16 C -0.0610(5) 0.3446(4) 0.8385(4) 0.127(6) Uani 1 1 d G U . . .
C18 C -0.1002(5) 0.3501(3) 0.7910(4) 0.118(6) Uani 1 1 d G U . . .
C19 C -0.1183(5) 0.2984(5) 0.7625(2) 0.120(5) Uani 1 1 d G U . . .
C20 C -0.0971(5) 0.2412(4) 0.7815(3) 0.110(5) Uani 1 1 d G U . . .
H20 H -0.1092 0.2066 0.7624 0.132 Uiso 1 1 calc R U . . .
C4 C -0.0627(6) -0.1030(4) 0.8804(4) 0.119(5) Uani 1 1 d G U . . .
C10 C -0.1427(8) -0.0858(3) 0.8585(3) 0.157(7) Uani 1 1 d G U . . .
H10 H -0.1454 -0.0553 0.8344 0.189 Uiso 1 1 calc R U . . .
C9 C -0.2186(5) -0.1141(5) 0.8726(4) 0.206(9) Uani 1 1 d G U . . .
H9 H -0.2721 -0.1026 0.8579 0.247 Uiso 1 1 calc R U . . .
C8 C -0.2145(6) -0.1597(5) 0.9086(4) 0.138(6) Uani 1 1 d G U . . .
C6 C -0.1346(8) -0.1769(4) 0.9305(3) 0.134(5) Uani 1 1 d G U . . .
C5 C -0.0587(6) -0.1485(4) 0.9164(4) 0.115(5) Uani 1 1 d G U . . .
H5 H -0.0052 -0.1601 0.9311 0.138 Uiso 1 1 calc R U . . .
Br2 Br -0.13060(11) 0.42590(7) 0.76179(7) 0.1855(9) Uani 1 1 d . . . . .
Br1 Br -0.32004(12) -0.19511(8) 0.92799(8) 0.2243(11) Uani 1 1 d . . . . .
Si1 Si 0.0000 0.9589(3) 0.2500 0.123(2) Uani 1 2 d S T P . .
Br3 Br 0.42367(14) 0.02446(9) 0.54502(7) 0.2462(12) Uani 1 1 d . . . . .
C13 C -0.0059(10) 0.1594(9) 0.8914(6) 0.102(5) Uani 1 1 d . U . . .
N3 N 0.0130(9) -0.0728(6) 0.8592(5) 0.157(5) Uani 1 1 d . U . . .
H3N H 0.0014 -0.0522 0.8325 0.188 Uiso 1 1 calc R U . . .
N2 N 0.1590(12) -0.0382(6) 0.8591(6) 0.153(5) Uani 1 1 d . U . . .
H2N H 0.1454 -0.0174 0.8327 0.184 Uiso 1 1 calc R U . . .
N6 N 0.2237(8) 0.1262(4) 0.8118(4) 0.127(4) Uani 1 1 d . U . . .
H6N H 0.1707 0.1147 0.8057 0.152 Uiso 1 1 calc R U . . .
N1 N 0.2128(9) 0.0673(7) 0.9108(4) 0.110(5) Uani 1 1 d . . . . .
O3 O 0.3533(6) 0.1354(4) 0.7810(3) 0.146(4) Uani 1 1 d . . . . .
C23 C 0.2837(15) 0.1176(9) 0.7793(8) 0.146(4) Uani 1 1 d . U . . .
C2 C 0.2463(13) -0.0317(9) 0.8818(7) 0.164(9) Uani 1 1 d . . . . .
H2A H 0.2698 -0.0712 0.8914 0.197 Uiso 1 1 calc R U . . .
H2B H 0.2847 -0.0129 0.8586 0.197 Uiso 1 1 calc R U . . .
C12 C 0.0707(12) 0.0802(5) 0.9448(4) 0.134(7) Uani 1 1 d . . . . .
H12A H 0.0652 0.0363 0.9470 0.161 Uiso 1 1 calc R U . . .
H12B H 0.0450 0.0974 0.9741 0.161 Uiso 1 1 calc R U . . .
C22 C 0.2492(8) 0.1546(6) 0.8566(5) 0.146(4) Uani 1 1 d . . . . .
H22A H 0.2000 0.1765 0.8693 0.175 Uiso 1 1 calc R U . . .
H22B H 0.2946 0.1840 0.8505 0.175 Uiso 1 1 calc R U . . .
C21 C 0.2841(10) 0.1070(6) 0.8971(4) 0.146(4) Uani 1 1 d . . . . .
H21A H 0.3304 0.0829 0.8837 0.175 Uiso 1 1 calc R U . . .
H21B H 0.3074 0.1283 0.9265 0.175 Uiso 1 1 calc R U . . .
C1 C 0.2384(9) 0.0059(8) 0.9248(6) 0.134(7) Uani 1 1 d . . . . .
H1A H 0.2937 0.0070 0.9437 0.161 Uiso 1 1 calc R U . . .
H1B H 0.1953 -0.0114 0.9460 0.161 Uiso 1 1 calc R U . . .
C11 C 0.1680(9) 0.0964(7) 0.9467(6) 0.136(7) Uani 1 1 d . . . . .
H11A H 0.1742 0.1400 0.9425 0.163 Uiso 1 1 calc R U . . .
H11B H 0.1935 0.0857 0.9793 0.163 Uiso 1 1 calc R U . . .
N7 N 0.2528(6) 0.0873(4) 0.7374(4) 0.096(3) Uani 1 1 d . U . . .
H7N H 0.1996 0.0753 0.7377 0.115 Uiso 1 1 calc R U . . .
C27 C 0.2294(12) 0.0384(7) 0.5553(5) 0.262(10) Uani 1 1 d . . . . .
H27A H 0.2421 0.0687 0.5309 0.393 Uiso 1 1 calc R U . . .
H27B H 0.1679 0.0382 0.5605 0.393 Uiso 1 1 calc R U . . .
H27C H 0.2467 -0.0009 0.5437 0.393 Uiso 1 1 calc R U . . .
C17A C -0.0362(14) 0.4047(9) 0.8699(10) 0.170(9) Uani 0.5 1 d . U P . .
H17A H 0.0124 0.3963 0.8926 0.255 Uiso 0.5 1 calc R U P . .
H17B H -0.0851 0.4172 0.8883 0.255 Uiso 0.5 1 calc R U P . .
H17C H -0.0208 0.4366 0.8474 0.255 Uiso 0.5 1 calc R U P . .
N5 N -0.0301(7) 0.1788(5) 0.8476(4) 0.112(4) Uani 1 1 d . U . . .
H5N H -0.0291 0.1511 0.8249 0.134 Uiso 1 1 calc R U . . .
C7 C -0.1315(11) -0.2311(8) 0.9634(6) 0.250(9) Uani 1 1 d . . . . .
H7A H -0.1020 -0.2210 0.9946 0.375 Uiso 1 1 calc R U . . .
H7B H -0.1008 -0.2632 0.9475 0.375 Uiso 1 1 calc R U . . .
H7C H -0.1898 -0.2441 0.9692 0.375 Uiso 1 1 calc R U . . .
N4 N 0.0198(6) 0.1015(5) 0.8996(4) 0.095(3) Uani 1 1 d . U . . .
H4N H 0.0057 0.0749 0.8771 0.114 Uiso 1 1 calc R U . . .
O2 O -0.0094(5) 0.1948(4) 0.9302(3) 0.124(3) Uani 1 1 d . . . . .
C3 C 0.1031(16) -0.0724(8) 0.8762(8) 0.134(7) Uani 1 1 d . U . . .
O1 O 0.1159(5) -0.1127(4) 0.9124(4) 0.162(4) Uani 1 1 d . . . . .
C17B C -0.1512(15) 0.2895(9) 0.7100(11) 0.170(9) Uani 0.5 1 d . U P . .
H17D H -0.1047 0.2753 0.6903 0.255 Uiso 0.5 1 calc R U P . .
H17E H -0.1730 0.3274 0.6967 0.255 Uiso 0.5 1 calc R U P . .
H17F H -0.1973 0.2599 0.7091 0.255 Uiso 0.5 1 calc R U P . .
F1 F 0.0717(6) 0.9558(4) 0.3001(3) 0.204(4) Uani 1 1 d . . . . .
F2 F -0.0645(7) 0.9557(7) 0.2905(4) 0.323(10) Uani 1 1 d . . . . .
F3 F 0.0000 0.8931(7) 0.2500 0.365(14) Uani 1 2 d S T P . .
F4 F 0.0000 1.0286(6) 0.2500 0.377(14) Uani 1 2 d S T P . .


_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
C24 C30 1.3900 . ?
C24 C25 1.3900 . ?
C24 N7 1.412(9) . ?
C30 C29 1.3900 . ?
C29 C28 1.3900 . ?
C28 C26 1.3900 . ?
C28 Br3 1.866(7) . ?
C26 C25 1.3900 . ?
C26 C27 1.562(13) . ?
C14 C15 1.3900 . ?
C14 C20 1.3900 . ?
C14 N5 1.406(11) . ?
C15 C16 1.3900 . ?
C16 C18 1.3900 . ?
C16 C17A 1.60(2) . ?
C18 C19 1.3900 . ?
C18 Br2 1.890(6) . ?
C19 C20 1.3900 . ?
C19 C17B 1.49(3) . ?
C4 C10 1.3900 . ?
C4 C5 1.3900 . ?
C4 N3 1.477(13) . ?
C10 C9 1.3900 . ?
C9 C8 1.3900 . ?
C8 C6 1.3900 . ?
C8 Br1 1.893(7) . ?
C6 C5 1.3900 . ?
C6 C7 1.480(15) . ?
Si1 F3 1.445(14) . ?
Si1 F2 1.505(12) . ?
Si1 F2 1.505(12) 2 ?
Si1 F4 1.533(14) . ?
Si1 F1 1.699(9) 2 ?
Si1 F1 1.699(9) . ?
C13 N5 1.287(15) . ?
C13 O2 1.302(14) . ?
C13 N4 1.347(16) . ?
N3 C3 1.44(2) . ?
N2 C3 1.25(2) . ?
N2 C2 1.454(18) . ?
N6 C23 1.311(18) . ?
N6 C22 1.393(12) . ?
N1 C11 1.367(15) . ?
N1 C1 1.451(14) . ?
N1 C21 1.460(14) . ?
O3 C23 1.138(17) . ?
C23 N7 1.370(17) . ?
C2 C1 1.426(17) . ?
C12 N4 1.488(12) . ?
C12 C11 1.536(15) . ?
C22 C21 1.584(15) . ?
C3 O1 1.322(18) . ?

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
C30 C24 C25 120.0 . . ?
C30 C24 N7 125.4(10) . . ?
C25 C24 N7 114.6(10) . . ?
C24 C30 C29 120.0 . . ?
C28 C29 C30 120.0 . . ?
C26 C28 C29 120.0 . . ?
C26 C28 Br3 122.9(8) . . ?
C29 C28 Br3 116.9(8) . . ?
C25 C26 C28 120.0 . . ?
C25 C26 C27 126.4(11) . . ?
C28 C26 C27 113.4(11) . . ?
C26 C25 C24 120.0 . . ?
C15 C14 C20 120.0 . . ?
C15 C14 N5 118.9(9) . . ?
C20 C14 N5 120.9(9) . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C18 120.0 . . ?
C15 C16 C17A 120.5(12) . . ?
C18 C16 C17A 119.4(12) . . ?
C19 C18 C16 120.0 . . ?
C19 C18 Br2 117.0(7) . . ?
C16 C18 Br2 123.0(7) . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C17B 132.8(12) . . ?
C20 C19 C17B 106.9(11) . . ?
C19 C20 C14 120.0 . . ?
C10 C4 C5 120.0 . . ?
C10 C4 N3 114.4(11) . . ?
C5 C4 N3 125.4(11) . . ?
C9 C10 C4 120.0 . . ?
C10 C9 C8 120.0 . . ?
C6 C8 C9 120.0 . . ?
C6 C8 Br1 121.6(8) . . ?
C9 C8 Br1 118.4(8) . . ?
C8 C6 C5 120.0 . . ?
C8 C6 C7 118.3(12) . . ?
C5 C6 C7 121.2(12) . . ?
C6 C5 C4 120.0 . . ?
F3 Si1 F2 87.3(7) . . ?
F3 Si1 F2 87.3(7) . 2 ?
F2 Si1 F2 174.6(13) . 2 ?
F3 Si1 F4 180.0 . . ?
F2 Si1 F4 92.7(7) . . ?
F2 Si1 F4 92.7(7) 2 . ?
F3 Si1 F1 87.7(4) . 2 ?
F2 Si1 F1 98.2(5) . 2 ?
F2 Si1 F1 81.5(5) 2 2 ?
F4 Si1 F1 92.3(4) . 2 ?
F3 Si1 F1 87.7(4) . . ?
F2 Si1 F1 81.5(5) . . ?
F2 Si1 F1 98.3(5) 2 . ?
F4 Si1 F1 92.3(4) . . ?
F1 Si1 F1 175.3(8) 2 . ?
N5 C13 O2 120.6(19) . . ?
N5 C13 N4 122.2(17) . . ?
O2 C13 N4 117.2(16) . . ?
C3 N3 C4 130.2(17) . . ?
C3 N2 C2 123(2) . . ?
C23 N6 C22 117.2(15) . . ?
C11 N1 C1 113.1(15) . . ?
C11 N1 C21 107.8(13) . . ?
C1 N1 C21 115.0(14) . . ?
O3 C23 N6 128(2) . . ?
O3 C23 N7 119(2) . . ?
N6 C23 N7 112.7(18) . . ?
C1 C2 N2 106.4(18) . . ?
N4 C12 C11 115.4(12) . . ?
N6 C22 C21 111.5(12) . . ?
N1 C21 C22 109.4(13) . . ?
C2 C1 N1 111.3(16) . . ?
N1 C11 C12 113.0(16) . . ?
C23 N7 C24 128.3(14) . . ?
C13 N5 C14 133.4(14) . . ?
C13 N4 C12 124.7(13) . . ?
N2 C3 O1 126(2) . . ?
N2 C3 N3 124(2) . . ?
O1 C3 N3 110(2) . . ?

_refine_diff_density_max         0.435
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.077

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.202 0.250 0.048 1169 404 ' '
2 0.184 0.750 -0.066 1169 404 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_Tren-Cl-Me-TBASO4
_database_code_depnum_ccdc_archive 'CCDC 1840358'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C30 H35 Cl3 N7 O3, C30 H36 Cl3 N7 O3, 2(C16 H36 N), O4 S'
_chemical_formula_sum            'C92 H143 Cl6 N16 O10 S'
_chemical_formula_weight         1877.98
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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.6203(7)
_cell_length_b                   16.4617(6)
_cell_length_c                   25.0998(13)
_cell_angle_alpha                108.871(4)
_cell_angle_beta                 95.521(4)
_cell_angle_gamma                91.523(4)
_cell_volume                     5290.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7319
_cell_measurement_theta_min      3.1340
_cell_measurement_theta_max      20.9870

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_F_000             2010.0
_exptl_transmission_factor_min   0.935
_exptl_transmission_factor_max   0.955
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.241
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51128
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.941
_diffrn_reflns_theta_max         28.752
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             26177
_reflns_number_gt                9388
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.1100P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         26177
_refine_ls_number_parameters     1150
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2075
_refine_ls_R_factor_gt           0.0964
_refine_ls_wR_factor_ref         0.3120
_refine_ls_wR_factor_gt          0.2502
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003

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
S1 S 0.88447(8) 0.18707(6) 0.75405(4) 0.0541(3) Uani 1 1 d . . . . .
Cl1 Cl -0.43636(15) 0.57568(12) 0.04493(10) 0.1706(10) Uani 1 1 d . . . . .
Cl2 Cl 0.31950(14) 0.52049(11) 0.46241(7) 0.1282(6) Uani 1 1 d . . . . .
Cl6 Cl -0.08188(18) 0.72294(11) 0.00755(8) 0.1613(8) Uani 1 1 d . . . . .
Cl5 Cl 0.58273(18) 1.18121(13) 0.35343(11) 0.1831(10) Uani 1 1 d . . . . .
Cl3 Cl 0.51476(18) 1.05713(14) 0.07845(10) 0.1701(9) Uani 1 1 d . . . . .
Cl4 Cl -0.07871(19) 0.60174(18) 0.47824(10) 0.1861(10) Uani 1 1 d . . . . .
O10 O 0.8535(2) 0.11056(18) 0.76767(14) 0.0840(9) Uani 1 1 d . . . . .
O8 O 0.8391(2) 0.18109(18) 0.69768(12) 0.0835(9) Uani 1 1 d . . . . .
O9 O 0.9920(2) 0.1937(2) 0.75676(14) 0.0879(9) Uani 1 1 d . . . . .
O7 O 0.8509(3) 0.26485(18) 0.79560(13) 0.0893(10) Uani 1 1 d . . . . .
O5 O 0.3040(3) 1.07805(19) 0.43518(13) 0.0845(9) Uani 1 1 d . . . . .
O6 O -0.0818(3) 1.10059(19) 0.22769(13) 0.0901(10) Uani 1 1 d . . . . .
O1 O -0.1075(3) 0.5005(2) 0.11387(18) 0.1124(13) Uani 1 1 d . . . . .
N8 N -0.0117(3) 1.0706(2) 0.39349(14) 0.0659(9) Uani 1 1 d . . . . .
O2 O 0.3770(2) 0.5692(2) 0.28279(14) 0.0877(10) Uani 1 1 d . . . . .
N16 N 0.4083(3) 0.3053(2) 0.57814(15) 0.0721(10) Uani 1 1 d . . . . .
N1 N 0.2345(3) 0.5565(2) 0.10811(15) 0.0675(9) Uani 1 1 d . . . . .
O3 O 0.2979(3) 0.7936(2) 0.04734(14) 0.0927(10) Uani 1 1 d . . . . .
N5 N 0.2609(3) 0.6671(2) 0.31150(16) 0.0756(11) Uani 1 1 d . . . . .
H5N H 0.2242 0.7017 0.3005 0.091 Uiso 1 1 calc R U . . .
O4 O -0.1619(3) 0.8410(2) 0.40471(16) 0.0982(11) Uani 1 1 d . . . . .
N3 N -0.0924(3) 0.6461(2) 0.15615(16) 0.0761(10) Uani 1 1 d . . . . .
H3N H -0.0513 0.6869 0.1774 0.091 Uiso 1 1 calc R U . . .
N15 N 0.8503(3) 0.2440(2) 0.12542(15) 0.0691(10) Uani 1 1 d . . . . .
N11 N 0.1743(3) 0.9807(2) 0.40450(16) 0.0752(10) Uani 1 1 d . . . . .
H11N H 0.1504 0.9331 0.3797 0.090 Uiso 1 1 calc R U . . .
N12 N 0.3035(3) 0.9673(2) 0.35147(16) 0.0793(11) Uani 1 1 d . . . . .
H12N H 0.2702 0.9208 0.3308 0.095 Uiso 1 1 calc R U . . .
N14 N -0.0256(3) 0.9660(2) 0.19269(15) 0.0817(12) Uani 1 1 d . . . . .
H14N H 0.0199 0.9338 0.1988 0.098 Uiso 1 1 calc R U . . .
N13 N 0.0421(3) 1.0576(2) 0.27789(15) 0.0775(11) Uani 1 1 d . . . . .
H13N H 0.0818 1.0180 0.2782 0.093 Uiso 1 1 calc R U . . .
N7 N 0.2709(3) 0.8683(2) 0.13931(16) 0.0781(11) Uani 1 1 d . . . . .
H7N H 0.2431 0.8634 0.1675 0.094 Uiso 1 1 calc R U . . .
N2 N 0.0402(3) 0.5666(2) 0.1561(2) 0.0931(13) Uani 1 1 d . . . . .
H2N H 0.0708 0.6135 0.1782 0.112 Uiso 1 1 calc R U . . .
C14 C 0.2497(3) 0.6630(3) 0.36542(18) 0.0615(11) Uani 1 1 d . . . . .
C43 C 0.2634(4) 1.0141(3) 0.39965(19) 0.0665(11) Uani 1 1 d . . . . .
C4 C -0.1877(3) 0.6700(3) 0.14301(18) 0.0644(11) Uani 1 1 d . . . . .
N6 N 0.2044(3) 0.7318(3) 0.09471(16) 0.0915(13) Uani 1 1 d . . . . .
H6N H 0.1759 0.7393 0.1249 0.110 Uiso 1 1 calc R U . . .
N9 N -0.1143(3) 0.8955(3) 0.33729(17) 0.0854(11) Uani 1 1 d . . . . .
H9N H -0.0826 0.8866 0.3081 0.103 Uiso 1 1 calc R U . . .
N4 N 0.3217(3) 0.6465(3) 0.22683(17) 0.0820(11) Uani 1 1 d . . . . .
H4N H 0.2856 0.6875 0.2243 0.098 Uiso 1 1 calc R U . . .
C81 C 0.4491(3) 0.3981(2) 0.59526(19) 0.0694(12) Uani 1 1 d . . . . .
H81A H 0.4929 0.4102 0.6301 0.083 Uiso 1 1 calc R U . . .
H81B H 0.4890 0.4030 0.5663 0.083 Uiso 1 1 calc R U . . .
C13 C 0.3236(4) 0.6226(3) 0.27381(19) 0.0712(12) Uani 1 1 d . . . . .
C53 C -0.0257(4) 1.0452(3) 0.23248(19) 0.0720(13) Uani 1 1 d . . . . .
C20 C 0.2825(3) 0.5976(3) 0.3850(2) 0.0723(12) Uani 1 1 d . . . . .
H20 H 0.3127 0.5518 0.3614 0.087 Uiso 1 1 calc R U . . .
N10 N -0.0682(3) 0.7650(3) 0.33664(18) 0.0889(12) Uani 1 1 d . . . . .
H10N H -0.0431 0.7665 0.3068 0.107 Uiso 1 1 calc R U . . .
C15 C 0.1991(4) 0.7266(3) 0.4017(2) 0.0776(13) Uani 1 1 d . . . . .
H15 H 0.1739 0.7703 0.3895 0.093 Uiso 1 1 calc R U . . .
C44 C 0.3904(4) 0.9853(3) 0.3319(2) 0.0769(13) Uani 1 1 d . . . . .
C3 C -0.0574(4) 0.5666(3) 0.1396(2) 0.0793(13) Uani 1 1 d . . . . .
C23 C 0.2608(4) 0.7983(3) 0.0911(2) 0.0762(13) Uani 1 1 d . . . . .
C19 C 0.2704(4) 0.6005(3) 0.4395(2) 0.0770(13) Uani 1 1 d . . . . .
C61 C 0.7895(4) 0.3014(3) 0.0990(2) 0.0796(14) Uani 1 1 d . . . . .
H61A H 0.8069 0.3610 0.1215 0.095 Uiso 1 1 calc R U . . .
H61B H 0.8087 0.2930 0.0614 0.095 Uiso 1 1 calc R U . . .
C6 C -0.3492(4) 0.6464(3) 0.0935(2) 0.0876(14) Uani 1 1 d . . . . .
C77 C 0.3346(3) 0.2826(3) 0.52576(18) 0.0757(13) Uani 1 1 d . . . . .
H77A H 0.2779 0.3168 0.5351 0.091 Uiso 1 1 calc R U . . .
H77B H 0.3118 0.2227 0.5162 0.091 Uiso 1 1 calc R U . . .
C7 C -0.3727(4) 0.7306(3) 0.1185(2) 0.0764(13) Uani 1 1 d . . . . .
C54 C -0.0902(4) 0.9305(3) 0.14312(19) 0.0745(13) Uani 1 1 d . . . . .
C41 C 0.0651(4) 1.0975(3) 0.44187(18) 0.0771(13) Uani 1 1 d . . . . .
H41A H 0.0352 1.1274 0.4758 0.093 Uiso 1 1 calc R U . . .
H41B H 0.1128 1.1375 0.4358 0.093 Uiso 1 1 calc R U . . .
C85 C 0.3511(4) 0.2921(4) 0.6242(2) 0.1054(19) Uani 1 1 d . . . . .
H85A H 0.3219 0.2337 0.6107 0.127 Uiso 1 1 calc R U . . .
H85B H 0.2974 0.3304 0.6295 0.127 Uiso 1 1 calc R U . . .
C73 C 0.8355(4) 0.1514(3) 0.0880(2) 0.0788(13) Uani 1 1 d . . . . .
H73A H 0.7653 0.1352 0.0822 0.095 Uiso 1 1 calc R U . . .
H73B H 0.8676 0.1164 0.1082 0.095 Uiso 1 1 calc R U . . .
C34 C -0.0530(4) 0.6910(4) 0.3518(2) 0.0824(14) Uani 1 1 d . . . . .
C24 C 0.3215(4) 0.9465(3) 0.1475(2) 0.0749(13) Uani 1 1 d . . . . .
C51 C -0.0261(4) 1.1356(3) 0.3657(2) 0.0845(14) Uani 1 1 d . . . . .
H51A H -0.0227 1.1919 0.3945 0.101 Uiso 1 1 calc R U . . .
H51B H -0.0916 1.1257 0.3451 0.101 Uiso 1 1 calc R U . . .
C10 C -0.2103(4) 0.7531(3) 0.17028(19) 0.0740(12) Uani 1 1 d . . . . .
H10 H -0.1640 0.7904 0.1973 0.089 Uiso 1 1 calc R U . . .
C17 C 0.2219(4) 0.6622(3) 0.4757(2) 0.0787(13) Uani 1 1 d . . . . .
C89 C 0.4950(4) 0.2508(3) 0.5690(2) 0.0933(17) Uani 1 1 d . . . . .
H89A H 0.5405 0.2700 0.6035 0.112 Uiso 1 1 calc R U . . .
H89B H 0.5286 0.2617 0.5394 0.112 Uiso 1 1 calc R U . . .
C33 C -0.1176(4) 0.8343(3) 0.3633(2) 0.0782(13) Uani 1 1 d . . . . .
C42 C 0.1179(4) 1.0239(3) 0.4510(2) 0.0820(14) Uani 1 1 d . . . . .
H42A H 0.1623 1.0449 0.4858 0.098 Uiso 1 1 calc R U . . .
H42B H 0.0699 0.9826 0.4554 0.098 Uiso 1 1 calc R U . . .
C52 C 0.0491(4) 1.1353(3) 0.32551(19) 0.0775(13) Uani 1 1 d . . . . .
H52A H 0.0403 1.1838 0.3119 0.093 Uiso 1 1 calc R U . . .
H52B H 0.1148 1.1426 0.3458 0.093 Uiso 1 1 calc R U . . .
C65 C 0.8181(4) 0.2492(3) 0.1833(2) 0.0818(14) Uani 1 1 d . . . . .
H65A H 0.7496 0.2275 0.1776 0.098 Uiso 1 1 calc R U . . .
H65B H 0.8570 0.2109 0.1979 0.098 Uiso 1 1 calc R U . . .
C78 C 0.3710(4) 0.2955(3) 0.47311(19) 0.0796(13) Uani 1 1 d . . . . .
H78A H 0.3989 0.3539 0.4824 0.096 Uiso 1 1 calc R U . . .
H78B H 0.4224 0.2564 0.4601 0.096 Uiso 1 1 calc R U . . .
C45 C 0.4411(4) 1.0645(3) 0.3514(2) 0.0948(16) Uani 1 1 d . . . . .
H45 H 0.4195 1.1089 0.3806 0.114 Uiso 1 1 calc R U . . .
C60 C -0.0630(5) 0.8561(3) 0.1024(2) 0.0883(15) Uani 1 1 d . . . . .
H60 H -0.0019 0.8346 0.1084 0.106 Uiso 1 1 calc R U . . .
C31 C -0.1051(4) 1.0400(3) 0.4078(2) 0.0842(14) Uani 1 1 d . . . . .
H31A H -0.1449 1.0886 0.4224 0.101 Uiso 1 1 calc R U . . .
H31B H -0.0906 1.0149 0.4375 0.101 Uiso 1 1 calc R U . . .
C16 C 0.1857(4) 0.7260(3) 0.4556(2) 0.0886(15) Uani 1 1 d . . . . .
H16 H 0.1516 0.7694 0.4788 0.106 Uiso 1 1 calc R U . . .
C1 C 0.1547(4) 0.4892(3) 0.0898(3) 0.0983(17) Uani 1 1 d . . . . .
H1A H 0.1825 0.4338 0.0750 0.118 Uiso 1 1 calc R U . . .
H1B H 0.1112 0.4979 0.0594 0.118 Uiso 1 1 calc R U . . .
C69 C 0.9578(4) 0.2755(3) 0.1325(2) 0.0812(13) Uani 1 1 d . . . . .
H69A H 0.9760 0.2737 0.0957 0.097 Uiso 1 1 calc R U . . .
H69B H 0.9643 0.3352 0.1567 0.097 Uiso 1 1 calc R U . . .
C9 C -0.3021(4) 0.7815(3) 0.1577(2) 0.0809(14) Uani 1 1 d . . . . .
H9 H -0.3156 0.8378 0.1769 0.097 Uiso 1 1 calc R U . . .
C12 C 0.3787(4) 0.6049(4) 0.1809(2) 0.0913(15) Uani 1 1 d . . . . .
H12A H 0.4380 0.5850 0.1960 0.110 Uiso 1 1 calc R U . . .
H12B H 0.3988 0.6466 0.1635 0.110 Uiso 1 1 calc R U . . .
C82 C 0.3758(4) 0.4667(3) 0.6042(2) 0.0883(14) Uani 1 1 d . . . . .
H82A H 0.3351 0.4629 0.6330 0.106 Uiso 1 1 calc R U . . .
H82B H 0.3330 0.4572 0.5693 0.106 Uiso 1 1 calc R U . . .
C11 C 0.3216(4) 0.5298(3) 0.1363(2) 0.0895(15) Uani 1 1 d . . . . .
H11A H 0.3646 0.5014 0.1082 0.107 Uiso 1 1 calc R U . . .
H11B H 0.3003 0.4887 0.1538 0.107 Uiso 1 1 calc R U . . .
C79 C 0.2862(4) 0.2787(3) 0.4268(2) 0.0949(16) Uani 1 1 d . . . . .
H79A H 0.2562 0.2215 0.4197 0.114 Uiso 1 1 calc R U . . .
H79B H 0.2366 0.3195 0.4398 0.114 Uiso 1 1 calc R U . . .
C40 C -0.0752(4) 0.6830(4) 0.4033(2) 0.0928(15) Uani 1 1 d . . . . .
H40 H -0.1057 0.7261 0.4291 0.111 Uiso 1 1 calc R U . . .
C74 C 0.8729(4) 0.1288(3) 0.0307(2) 0.0851(15) Uani 1 1 d . . . . .
H74A H 0.9444 0.1369 0.0354 0.102 Uiso 1 1 calc R U . . .
H74B H 0.8465 0.1668 0.0110 0.102 Uiso 1 1 calc R U . . .
C21 C 0.2587(4) 0.5841(3) 0.0611(2) 0.0876(15) Uani 1 1 d . . . . .
H21A H 0.2557 0.5344 0.0271 0.105 Uiso 1 1 calc R U . . .
H21B H 0.3257 0.6097 0.0692 0.105 Uiso 1 1 calc R U . . .
C55 C -0.1817(4) 0.9612(3) 0.1337(2) 0.0872(15) Uani 1 1 d . . . . .
H55 H -0.2028 1.0099 0.1599 0.105 Uiso 1 1 calc R U . . .
C5 C -0.2591(4) 0.6162(3) 0.1047(2) 0.0833(14) Uani 1 1 d . . . . .
H5 H -0.2466 0.5592 0.0862 0.100 Uiso 1 1 calc R U . . .
C32 C -0.1631(4) 0.9747(3) 0.3579(2) 0.0937(15) Uani 1 1 d . . . . .
H32A H -0.2269 0.9621 0.3685 0.112 Uiso 1 1 calc R U . . .
H32B H -0.1745 0.9989 0.3276 0.112 Uiso 1 1 calc R U . . .
C86 C 0.4103(5) 0.3070(5) 0.6821(3) 0.146(3) Uani 1 1 d . . . . .
H86A H 0.4508 0.2588 0.6802 0.175 Uiso 1 1 calc R U . . .
H86B H 0.4539 0.3584 0.6918 0.175 Uiso 1 1 calc R U . . .
C70 C 1.0295(5) 0.2265(4) 0.1569(3) 0.1137(19) Uani 1 1 d . . . . .
H70A H 1.0276 0.1678 0.1314 0.136 Uiso 1 1 calc R U . . .
H70B H 1.0093 0.2247 0.1926 0.136 Uiso 1 1 calc R U . . .
C90 C 0.4753(5) 0.1533(3) 0.5531(3) 0.125(2) Uani 1 1 d . . . . .
H90A H 0.4294 0.1325 0.5189 0.150 Uiso 1 1 calc R U . . .
H90B H 0.4454 0.1404 0.5832 0.150 Uiso 1 1 calc R U . . .
C46 C 0.5231(5) 1.0772(4) 0.3275(3) 0.1026(17) Uani 1 1 d . . . . .
C84 C 0.4849(5) 0.5867(4) 0.6798(3) 0.135(2) Uani 1 1 d . . . . .
H84A H 0.4433 0.5809 0.7074 0.202 Uiso 1 1 calc R U . . .
H84B H 0.5070 0.6459 0.6890 0.202 Uiso 1 1 calc R U . . .
H84C H 0.5410 0.5527 0.6801 0.202 Uiso 1 1 calc R U . . .
C59 C -0.1231(6) 0.8151(4) 0.0548(2) 0.0983(17) Uani 1 1 d . . . . .
C35 C -0.0084(4) 0.6232(4) 0.3149(2) 0.0959(16) Uani 1 1 d . . . . .
H35 H 0.0050 0.6273 0.2802 0.115 Uiso 1 1 calc R U . . .
C83 C 0.4279(5) 0.5562(3) 0.6224(3) 0.1084(19) Uani 1 1 d . . . . .
H83A H 0.4728 0.5571 0.5948 0.130 Uiso 1 1 calc R U . . .
H83B H 0.3785 0.5971 0.6210 0.130 Uiso 1 1 calc R U . . .
C62 C 0.6799(5) 0.2864(4) 0.0940(3) 0.1093(19) Uani 1 1 d . . . . .
H62A H 0.6608 0.2864 0.1303 0.131 Uiso 1 1 calc R U . . .
H62B H 0.6606 0.2302 0.0665 0.131 Uiso 1 1 calc R U . . .
C57 C -0.2126(6) 0.8417(5) 0.0427(3) 0.1079(19) Uani 1 1 d . . . . .
C22 C 0.1890(5) 0.6484(3) 0.0506(2) 0.0957(16) Uani 1 1 d . . . . .
H22A H 0.1983 0.6553 0.0145 0.115 Uiso 1 1 calc R U . . .
H22B H 0.1215 0.6264 0.0485 0.115 Uiso 1 1 calc R U . . .
C50 C 0.4270(4) 0.9213(3) 0.2889(2) 0.0933(16) Uani 1 1 d . . . . .
H50 H 0.3955 0.8666 0.2761 0.112 Uiso 1 1 calc R U . . .
C30 C 0.3881(4) 0.9613(4) 0.1119(2) 0.0902(15) Uani 1 1 d . . . . .
H30 H 0.4009 0.9174 0.0796 0.108 Uiso 1 1 calc R U . . .
C91 C 0.5726(6) 0.1069(4) 0.5432(4) 0.151(4) Uani 1 1 d . . . . .
H91A H 0.6217 0.1363 0.5747 0.181 Uiso 1 1 calc R U . . .
H91B H 0.5610 0.0490 0.5441 0.181 Uiso 1 1 calc R U . . .
C66 C 0.8273(5) 0.3377(3) 0.2284(2) 0.112(2) Uani 1 1 d . . . . .
H66A H 0.8966 0.3568 0.2379 0.134 Uiso 1 1 calc R U . . .
H66B H 0.7945 0.3779 0.2127 0.134 Uiso 1 1 calc R U . . .
C8 C -0.4716(4) 0.7648(4) 0.1051(3) 0.1105(18) Uani 1 1 d . . . . .
H8A H -0.5200 0.7491 0.1260 0.166 Uiso 1 1 calc R U . . .
H8B H -0.4927 0.7406 0.0653 0.166 Uiso 1 1 calc R U . . .
H8C H -0.4646 0.8264 0.1156 0.166 Uiso 1 1 calc R U . . .
C39 C -0.0498(4) 0.6070(5) 0.4150(3) 0.109(2) Uani 1 1 d . . . . .
C2 C 0.0956(4) 0.4886(3) 0.1373(3) 0.116(2) Uani 1 1 d . . . . .
H2C H 0.0497 0.4383 0.1248 0.139 Uiso 1 1 calc R U . . .
H2D H 0.1398 0.4848 0.1690 0.139 Uiso 1 1 calc R U . . .
C36 C 0.0166(5) 0.5506(4) 0.3275(3) 0.1086(19) Uani 1 1 d . . . . .
C48 C 0.6469(5) 1.0335(5) 0.2531(3) 0.144(3) Uani 1 1 d . . . . .
H48A H 0.6837 1.0850 0.2770 0.216 Uiso 1 1 calc R U . . .
H48B H 0.6236 1.0406 0.2176 0.216 Uiso 1 1 calc R U . . .
H48C H 0.6888 0.9860 0.2464 0.216 Uiso 1 1 calc R U . . .
C25 C 0.3075(5) 1.0148(4) 0.1950(2) 0.0992(17) Uani 1 1 d . . . . .
H25 H 0.2631 1.0070 0.2191 0.119 Uiso 1 1 calc R U . . .
C76 C 0.8829(5) 0.0066(3) -0.0596(2) 0.113(2) Uani 1 1 d . . . . .
H76A H 0.8697 0.0472 -0.0792 0.169 Uiso 1 1 calc R U . . .
H76B H 0.8526 -0.0488 -0.0821 0.169 Uiso 1 1 calc R U . . .
H76C H 0.9530 0.0026 -0.0534 0.169 Uiso 1 1 calc R U . . .
C29 C 0.4351(4) 1.0437(4) 0.1258(3) 0.0995(17) Uani 1 1 d . . . . .
C47 C 0.5584(5) 1.0157(4) 0.2821(3) 0.1059(18) Uani 1 1 d . . . . .
C75 C 0.8419(4) 0.0357(3) -0.0046(2) 0.0977(16) Uani 1 1 d . . . . .
H75A H 0.8632 -0.0013 0.0170 0.117 Uiso 1 1 calc R U . . .
H75B H 0.7704 0.0293 -0.0114 0.117 Uiso 1 1 calc R U . . .
C49 C 0.5064(5) 0.9364(4) 0.2651(3) 0.116(2) Uani 1 1 d . . . . .
H49 H 0.5276 0.8916 0.2359 0.139 Uiso 1 1 calc R U . . .
C27 C 0.4211(6) 1.1096(4) 0.1717(3) 0.120(2) Uani 1 1 d . . . . .
C26 C 0.3572(6) 1.0946(4) 0.2079(3) 0.124(2) Uani 1 1 d . . . . .
H26 H 0.3477 1.1383 0.2411 0.148 Uiso 1 1 calc R U . . .
C56 C -0.2419(5) 0.9163(4) 0.0828(3) 0.1078(19) Uani 1 1 d . . . . .
H56 H -0.3031 0.9367 0.0756 0.129 Uiso 1 1 calc R U . . .
C37 C -0.0046(5) 0.5406(4) 0.3787(3) 0.1107(19) Uani 1 1 d . . . . .
C18 C 0.2061(5) 0.6652(4) 0.5351(2) 0.128(2) Uani 1 1 d . . . . .
H18A H 0.1759 0.6112 0.5339 0.192 Uiso 1 1 calc R U . . .
H18B H 0.1637 0.7105 0.5509 0.192 Uiso 1 1 calc R U . . .
H18C H 0.2685 0.6758 0.5581 0.192 Uiso 1 1 calc R U . . .
C28 C 0.4727(7) 1.1995(5) 0.1842(4) 0.187(4) Uani 1 1 d . . . . .
H28A H 0.5415 1.1938 0.1791 0.280 Uiso 1 1 calc R U . . .
H28B H 0.4663 1.2341 0.2226 0.280 Uiso 1 1 calc R U . . .
H28C H 0.4425 1.2266 0.1587 0.280 Uiso 1 1 calc R U . . .
C38 C 0.0274(7) 0.4645(5) 0.3960(4) 0.071(2) Uani 0.5 1 d . . P . .
H38A H 0.0748 0.4841 0.4290 0.107 Uiso 0.5 1 calc R U P . .
H38B H 0.0568 0.4247 0.3656 0.107 Uiso 0.5 1 calc R U P . .
H38C H -0.0291 0.4365 0.4043 0.107 Uiso 0.5 1 calc R U P . .
C87 C 0.3407(9) 0.3171(8) 0.7288(4) 0.204(6) Uani 1 1 d . . . . .
H87A H 0.3769 0.3078 0.7613 0.244 Uiso 1 1 calc R U . . .
H87B H 0.2868 0.2733 0.7146 0.244 Uiso 1 1 calc R U . . .
C80 C 0.3158(6) 0.2853(4) 0.3721(2) 0.131(2) Uani 1 1 d . . . . .
H80A H 0.3296 0.3446 0.3762 0.197 Uiso 1 1 calc R U . . .
H80B H 0.2629 0.2613 0.3424 0.197 Uiso 1 1 calc R U . . .
H80C H 0.3739 0.2541 0.3628 0.197 Uiso 1 1 calc R U . . .
C63 C 0.6261(6) 0.3529(5) 0.0764(3) 0.136(3) Uani 1 1 d . . . . .
H63A H 0.6619 0.4081 0.0951 0.164 Uiso 1 1 calc R U . . .
H63B H 0.6277 0.3398 0.0360 0.164 Uiso 1 1 calc R U . . .
C58 C -0.2846(6) 0.7957(6) -0.0086(3) 0.183(4) Uani 1 1 d . . . . .
H58A H -0.2574 0.7972 -0.0422 0.275 Uiso 1 1 calc R U . . .
H58B H -0.3458 0.8237 -0.0057 0.275 Uiso 1 1 calc R U . . .
H58C H -0.2964 0.7371 -0.0105 0.275 Uiso 1 1 calc R U . . .
C71 C 1.1346(6) 0.2652(6) 0.1671(4) 0.164(3) Uani 1 1 d D . . . .
H71A H 1.1404 0.2989 0.1420 0.197 Uiso 1 1 calc R U . . .
H71B H 1.1782 0.2185 0.1559 0.197 Uiso 1 1 calc R U . . .
C92 C 0.6150(7) 0.1010(6) 0.4902(4) 0.172(4) Uani 1 1 d . . . . .
H92A H 0.5648 0.0791 0.4587 0.258 Uiso 1 1 calc R U . . .
H92B H 0.6681 0.0630 0.4855 0.258 Uiso 1 1 calc R U . . .
H92C H 0.6397 0.1571 0.4920 0.258 Uiso 1 1 calc R U . . .
C67 C 0.7844(7) 0.3399(5) 0.2808(3) 0.149(3) Uani 1 1 d . . . . .
H67A H 0.7998 0.3973 0.3076 0.179 Uiso 1 1 calc R U . . .
H67B H 0.7132 0.3337 0.2716 0.179 Uiso 1 1 calc R U . . .
C68 C 0.8081(8) 0.2848(5) 0.3085(3) 0.198(5) Uani 1 1 d . . . . .
H68A H 0.7492 0.2540 0.3116 0.298 Uiso 1 1 calc R U . . .
H68B H 0.8397 0.3160 0.3457 0.298 Uiso 1 1 calc R U . . .
H68C H 0.8523 0.2448 0.2880 0.298 Uiso 1 1 calc R U . . .
C64 C 0.5350(11) 0.3607(11) 0.0869(7) 0.368(11) Uani 1 1 d . . . . .
H64A H 0.5120 0.3116 0.0961 0.552 Uiso 1 1 calc R U . . .
H64B H 0.4950 0.3641 0.0542 0.552 Uiso 1 1 calc R U . . .
H64C H 0.5303 0.4120 0.1184 0.552 Uiso 1 1 calc R U . . .
C88 C 0.2978(10) 0.4059(10) 0.7476(5) 0.244(7) Uani 1 1 d . . . . .
H88A H 0.3501 0.4498 0.7553 0.365 Uiso 1 1 calc R U . . .
H88B H 0.2663 0.4131 0.7813 0.365 Uiso 1 1 calc R U . . .
H88C H 0.2503 0.4106 0.7181 0.365 Uiso 1 1 calc R U . . .
C72 C 1.1729(13) 0.3228(11) 0.2276(4) 0.67(3) Uani 1 1 d D . . . .
H72A H 1.1316 0.3703 0.2394 1.012 Uiso 1 1 calc R U . . .
H72B H 1.2395 0.3441 0.2283 1.012 Uiso 1 1 calc R U . . .
H72C H 1.1715 0.2899 0.2529 1.012 Uiso 1 1 calc R U . . .
C38B C 0.0676(10) 0.4765(6) 0.2987(5) 0.112(4) Uani 0.5 1 d . . P . .
H38D H 0.0346 0.4495 0.2612 0.167 Uiso 0.5 1 calc R U P . .
H38E H 0.0679 0.4365 0.3193 0.167 Uiso 0.5 1 calc R U P . .
H38F H 0.1344 0.4939 0.2963 0.167 Uiso 0.5 1 calc R U P . .


_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
S1 O9 1.460(3) . ?
S1 O8 1.460(3) . ?
S1 O10 1.469(3) . ?
S1 O7 1.482(3) . ?
Cl1 C6 1.726(5) . ?
Cl2 C19 1.725(5) . ?
Cl6 C59 1.741(6) . ?
Cl5 C46 1.766(6) . ?
Cl3 C29 1.745(6) . ?
Cl4 C39 1.700(6) . ?
O5 C43 1.215(5) . ?
O6 C53 1.234(5) . ?
O1 C3 1.220(5) . ?
N8 C51 1.462(5) . ?
N8 C41 1.466(5) . ?
N8 C31 1.473(6) . ?
O2 C13 1.219(5) . ?
N16 C89 1.493(6) . ?
N16 C81 1.519(5) . ?
N16 C77 1.512(5) . ?
N16 C85 1.522(6) . ?
N1 C21 1.456(6) . ?
N1 C1 1.459(6) . ?
N1 C11 1.473(6) . ?
O3 C23 1.234(5) . ?
N5 C13 1.378(6) . ?
N5 C14 1.400(5) . ?
O4 C33 1.227(6) . ?
N3 C3 1.353(6) . ?
N3 C4 1.406(5) . ?
N15 C73 1.507(5) . ?
N15 C69 1.515(6) . ?
N15 C61 1.536(5) . ?
N15 C65 1.535(5) . ?
N11 C43 1.352(6) . ?
N11 C42 1.456(6) . ?
N12 C43 1.379(6) . ?
N12 C44 1.383(6) . ?
N14 C53 1.362(5) . ?
N14 C54 1.399(6) . ?
N13 C53 1.352(6) . ?
N13 C52 1.433(5) . ?
N7 C23 1.367(6) . ?
N7 C24 1.389(6) . ?
N2 C3 1.354(6) . ?
N2 C2 1.472(6) . ?
C14 C20 1.387(5) . ?
C14 C15 1.395(6) . ?
C4 C5 1.372(6) . ?
C4 C10 1.375(6) . ?
N6 C23 1.353(6) . ?
N6 C22 1.452(6) . ?
N9 C33 1.368(6) . ?
N9 C32 1.444(6) . ?
N4 C13 1.357(5) . ?
N4 C12 1.445(6) . ?
C81 C82 1.503(6) . ?
C20 C19 1.379(6) . ?
N10 C33 1.355(6) . ?
N10 C34 1.403(6) . ?
C15 C16 1.384(6) . ?
C44 C50 1.386(7) . ?
C44 C45 1.375(6) . ?
C19 C17 1.360(6) . ?
C61 C62 1.494(7) . ?
C6 C7 1.386(6) . ?
C6 C5 1.373(7) . ?
C77 C78 1.530(6) . ?
C7 C9 1.354(6) . ?
C7 C8 1.524(7) . ?
C54 C55 1.385(7) . ?
C54 C60 1.403(6) . ?
C41 C42 1.492(6) . ?
C85 C86 1.537(7) . ?
C73 C74 1.506(6) . ?
C34 C40 1.402(7) . ?
C34 C35 1.396(7) . ?
C24 C25 1.382(7) . ?
C24 C30 1.403(7) . ?
C51 C52 1.505(7) . ?
C10 C9 1.390(6) . ?
C17 C16 1.388(6) . ?
C17 C18 1.510(6) . ?
C89 C90 1.532(6) . ?
C65 C66 1.522(7) . ?
C78 C79 1.510(6) . ?
C45 C46 1.360(8) . ?
C60 C59 1.348(7) . ?
C31 C32 1.497(7) . ?
C1 C2 1.505(8) . ?
C69 C70 1.493(7) . ?
C12 C11 1.507(7) . ?
C82 C83 1.527(7) . ?
C79 C80 1.502(7) . ?
C40 C39 1.418(8) . ?
C74 C75 1.525(7) . ?
C21 C22 1.508(6) . ?
C55 C56 1.416(7) . ?
C86 C87 1.547(12) . ?
C70 C71 1.516(9) . ?
C90 C91 1.548(10) . ?
C46 C47 1.392(8) . ?
C84 C83 1.493(8) . ?
C59 C57 1.347(8) . ?
C35 C36 1.374(7) . ?
C62 C63 1.492(7) . ?
C57 C56 1.407(8) . ?
C57 C58 1.510(9) . ?
C50 C49 1.339(8) . ?
C30 C29 1.406(7) . ?
C91 C92 1.476(11) . ?
C66 C67 1.481(8) . ?
C39 C37 1.379(9) . ?
C36 C37 1.404(8) . ?
C36 C38B 1.437(13) . ?
C48 C47 1.536(8) . ?
C25 C26 1.387(8) . ?
C76 C75 1.478(7) . ?
C29 C27 1.336(8) . ?
C47 C49 1.386(8) . ?
C27 C26 1.389(9) . ?
C27 C28 1.544(8) . ?
C37 C38 1.513(9) . ?
C87 C88 1.534(15) . ?
C63 C64 1.294(12) . ?
C71 C72 1.5388(10) . ?
C67 C68 1.338(9) . ?

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
O9 S1 O8 110.6(2) . . ?
O9 S1 O10 109.36(18) . . ?
O8 S1 O10 109.72(19) . . ?
O9 S1 O7 109.3(2) . . ?
O8 S1 O7 108.34(18) . . ?
O10 S1 O7 109.42(19) . . ?
C51 N8 C41 112.8(4) . . ?
C51 N8 C31 112.5(4) . . ?
C41 N8 C31 112.6(4) . . ?
C89 N16 C81 106.6(3) . . ?
C89 N16 C77 112.0(4) . . ?
C81 N16 C77 111.3(3) . . ?
C89 N16 C85 111.4(4) . . ?
C81 N16 C85 110.4(4) . . ?
C77 N16 C85 105.3(3) . . ?
C21 N1 C1 111.0(4) . . ?
C21 N1 C11 112.3(4) . . ?
C1 N1 C11 111.6(4) . . ?
C13 N5 C14 128.0(3) . . ?
C3 N3 C4 128.0(4) . . ?
C73 N15 C69 110.7(3) . . ?
C73 N15 C61 110.4(3) . . ?
C69 N15 C61 107.5(3) . . ?
C73 N15 C65 107.4(3) . . ?
C69 N15 C65 109.7(4) . . ?
C61 N15 C65 111.1(3) . . ?
C43 N11 C42 121.2(4) . . ?
C43 N12 C44 128.5(4) . . ?
C53 N14 C54 128.1(4) . . ?
C53 N13 C52 121.6(4) . . ?
C23 N7 C24 126.9(4) . . ?
C3 N2 C2 122.0(4) . . ?
C20 C14 C15 116.8(4) . . ?
C20 C14 N5 124.5(4) . . ?
C15 C14 N5 118.6(4) . . ?
O5 C43 N11 122.5(5) . . ?
O5 C43 N12 124.2(5) . . ?
N11 C43 N12 113.3(4) . . ?
C5 C4 C10 118.0(4) . . ?
C5 C4 N3 124.3(4) . . ?
C10 C4 N3 117.7(4) . . ?
C23 N6 C22 123.9(4) . . ?
C33 N9 C32 121.2(4) . . ?
C13 N4 C12 121.7(4) . . ?
C82 C81 N16 117.4(4) . . ?
O2 C13 N4 123.8(5) . . ?
O2 C13 N5 123.1(4) . . ?
N4 C13 N5 113.0(4) . . ?
O6 C53 N13 122.9(4) . . ?
O6 C53 N14 123.4(4) . . ?
N13 C53 N14 113.6(4) . . ?
C19 C20 C14 120.2(4) . . ?
C33 N10 C34 127.9(4) . . ?
C16 C15 C14 121.4(4) . . ?
C50 C44 N12 118.7(5) . . ?
C50 C44 C45 117.6(5) . . ?
N12 C44 C45 123.7(5) . . ?
O1 C3 N2 122.2(5) . . ?
O1 C3 N3 124.7(5) . . ?
N2 C3 N3 113.1(4) . . ?
O3 C23 N6 121.1(5) . . ?
O3 C23 N7 125.0(5) . . ?
N6 C23 N7 113.8(4) . . ?
C17 C19 C20 123.8(4) . . ?
C17 C19 Cl2 118.6(4) . . ?
C20 C19 Cl2 117.6(4) . . ?
C62 C61 N15 115.7(4) . . ?
C7 C6 C5 123.3(5) . . ?
C7 C6 Cl1 118.7(4) . . ?
C5 C6 Cl1 118.0(4) . . ?
N16 C77 C78 116.6(4) . . ?
C9 C7 C6 115.4(5) . . ?
C9 C7 C8 121.2(5) . . ?
C6 C7 C8 123.4(5) . . ?
C55 C54 C60 118.4(5) . . ?
C55 C54 N14 123.8(4) . . ?
C60 C54 N14 117.6(5) . . ?
N8 C41 C42 113.0(4) . . ?
N16 C85 C86 116.4(5) . . ?
N15 C73 C74 117.0(4) . . ?
N10 C34 C40 123.8(5) . . ?
N10 C34 C35 118.3(5) . . ?
C40 C34 C35 117.8(5) . . ?
C25 C24 N7 118.0(5) . . ?
C25 C24 C30 117.0(5) . . ?
N7 C24 C30 124.9(5) . . ?
N8 C51 C52 113.2(4) . . ?
C4 C10 C9 120.4(4) . . ?
C19 C17 C16 116.2(4) . . ?
C19 C17 C18 124.5(5) . . ?
C16 C17 C18 119.3(5) . . ?
N16 C89 C90 117.7(4) . . ?
O4 C33 N10 124.7(5) . . ?
O4 C33 N9 123.9(5) . . ?
N10 C33 N9 111.4(5) . . ?
N11 C42 C41 112.9(4) . . ?
N13 C52 C51 112.9(4) . . ?
C66 C65 N15 116.5(4) . . ?
C79 C78 C77 109.9(4) . . ?
C46 C45 C44 119.3(5) . . ?
C59 C60 C54 121.6(6) . . ?
N8 C31 C32 112.5(4) . . ?
C17 C16 C15 121.5(5) . . ?
N1 C1 C2 112.2(5) . . ?
C70 C69 N15 115.7(4) . . ?
C7 C9 C10 122.8(4) . . ?
N4 C12 C11 112.5(4) . . ?
C81 C82 C83 111.3(4) . . ?
N1 C11 C12 112.1(4) . . ?
C80 C79 C78 113.8(5) . . ?
C34 C40 C39 118.0(6) . . ?
C73 C74 C75 110.6(4) . . ?
N1 C21 C22 112.0(4) . . ?
C54 C55 C56 117.9(5) . . ?
C4 C5 C6 120.0(4) . . ?
N9 C32 C31 113.1(4) . . ?
C87 C86 C85 111.0(6) . . ?
C69 C70 C71 113.0(5) . . ?
C89 C90 C91 110.7(5) . . ?
C45 C46 C47 124.3(6) . . ?
C45 C46 Cl5 116.8(5) . . ?
C47 C46 Cl5 118.7(5) . . ?
C60 C59 C57 123.1(6) . . ?
C60 C59 Cl6 117.5(6) . . ?
C57 C59 Cl6 119.4(5) . . ?
C36 C35 C34 123.1(6) . . ?
C84 C83 C82 116.4(5) . . ?
C61 C62 C63 112.5(5) . . ?
C59 C57 C56 116.6(6) . . ?
C59 C57 C58 125.0(7) . . ?
C56 C57 C58 118.3(8) . . ?
N6 C22 C21 112.4(4) . . ?
C49 C50 C44 121.7(5) . . ?
C24 C30 C29 118.8(5) . . ?
C92 C91 C90 116.8(6) . . ?
C67 C66 C65 113.7(5) . . ?
C37 C39 C40 124.0(6) . . ?
C37 C39 Cl4 120.6(6) . . ?
C40 C39 Cl4 115.4(6) . . ?
N2 C2 C1 111.5(4) . . ?
C35 C36 C37 120.4(6) . . ?
C35 C36 C38B 133.0(8) . . ?
C37 C36 C38B 106.5(7) . . ?
C24 C25 C26 122.3(6) . . ?
C27 C29 C30 124.0(6) . . ?
C27 C29 Cl3 120.2(5) . . ?
C30 C29 Cl3 115.8(5) . . ?
C49 C47 C46 114.0(6) . . ?
C49 C47 C48 122.6(6) . . ?
C46 C47 C48 123.4(6) . . ?
C76 C75 C74 113.8(5) . . ?
C50 C49 C47 122.8(6) . . ?
C29 C27 C26 117.4(6) . . ?
C29 C27 C28 121.8(7) . . ?
C26 C27 C28 120.8(7) . . ?
C25 C26 C27 120.5(6) . . ?
C57 C56 C55 122.4(6) . . ?
C39 C37 C36 116.7(6) . . ?
C39 C37 C38 121.0(7) . . ?
C36 C37 C38 122.2(7) . . ?
C86 C87 C88 112.8(8) . . ?
C64 C63 C62 116.5(8) . . ?
C70 C71 C72 117.5(9) . . ?
C68 C67 C66 122.1(7) . . ?

_refine_diff_density_max         0.815
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.060


# start Validation Reply Form
_vrf_PLAT242_Tren-Cl-Me-TBASO4   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C71 Check  
RESPONSE: This may be due to mismatching of U(eq) values.
;
_vrf_PLAT413_Tren-Cl-Me-TBASO4   
;
PROBLEM: Short Inter XH3 .. XHn     H38D     ..H72A             1.87 Ang.   
RESPONSE: This may be due to short distances between adjacent H atoms.
;
####################################################################### 
# 
# 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_T-Cl-Me-TEACO3
_database_code_depnum_ccdc_archive 'CCDC 1840357'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C30 H35 Cl3 N7 O3), 2(C8 H20 N), C O3'
_chemical_formula_sum            'C77 H110 Cl6 N16 O9'
_chemical_formula_weight         1616.51

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

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

_cell_length_a                   19.3717(13)
_cell_length_b                   22.5639(14)
_cell_length_c                   19.5218(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.140(6)
_cell_angle_gamma                90
_cell_volume                     8527.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1866
_cell_measurement_theta_min      3.0720
_cell_measurement_theta_max      18.9180

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_F_000             3432.0
_exptl_transmission_factor_min   0.921
_exptl_transmission_factor_max   0.939
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    0.264
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20037
_diffrn_reflns_av_unetI/netI     0.1505
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.074
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             14622
_reflns_number_gt                8683
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0200P)²+3.5552P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00026(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14622
_refine_ls_number_parameters     1012
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.2546
_refine_ls_R_factor_gt           0.0973
_refine_ls_wR_factor_ref         0.2015
_refine_ls_wR_factor_gt          0.1486
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003

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
Cl3A Cl 0.1501(2) 0.39220(17) 0.7579(2) 0.1340(15) Uani 0.7 1 d . . P A 1
Cl6A Cl 0.33788(18) 0.55597(19) 0.55083(17) 0.1453(15) Uani 0.8 1 d . . P B 1
Cl3B Cl 0.2533(6) 0.2456(5) 0.9473(6) 0.176(5) Uani 0.3 1 d . . P C 2
Cl6B Cl 0.1368(6) 0.4878(6) 0.6461(5) 0.110(5) Uani 0.2 1 d . . P D 2
Cl2 Cl 0.55541(12) -0.02904(11) 0.83484(9) 0.1016(9) Uani 1 1 d . . . . .
Cl5 Cl 0.25572(16) 0.88966(13) 0.14223(15) 0.1493(12) Uani 1 1 d . . . . .
Cl4 Cl 0.3131(2) 0.16032(14) 0.13312(17) 0.1949(17) Uani 1 1 d . . . . .
Cl1 Cl 0.1257(2) -0.32965(14) 0.80882(16) 0.219(2) Uani 1 1 d . . . . .
N1 N 0.1435(4) 0.0269(3) 0.5323(3) 0.0689(19) Uani 1 1 d . . . . .
O2 O 0.3939(3) 0.0356(3) 0.5259(2) 0.0890(19) Uani 1 1 d . . . . .
N8 N 0.0347(3) 0.5018(3) 0.1515(3) 0.0693(19) Uani 1 1 d . . . . .
O1 O 0.1073(4) -0.1723(3) 0.6376(3) 0.110(2) Uani 1 1 d . . . . .
N5 N 0.3865(3) 0.0147(3) 0.6398(3) 0.075(2) Uani 1 1 d . . . . .
H5N H 0.3575 0.0104 0.6716 0.090 Uiso 1 1 calc R U . . .
N3 N 0.1514(4) -0.1165(3) 0.7272(4) 0.087(2) Uani 1 1 d . . . . .
H3N H 0.1592 -0.0804 0.7391 0.105 Uiso 1 1 calc R U . . .
N13 N 0.0685(4) 0.4832(3) 0.2968(3) 0.082(2) Uani 1 1 d . . . . .
H13N H 0.0998 0.4995 0.2730 0.099 Uiso 1 1 calc R U . . .
O6 O 0.0319(3) 0.4666(3) 0.4033(2) 0.109(2) Uani 1 1 d . . . . .
O5 O 0.1230(3) 0.7053(3) 0.1123(3) 0.107(2) Uani 1 1 d . . . . .
N7 N 0.1546(4) 0.1665(3) 0.7348(4) 0.085(2) Uani 1 1 d . . . . .
H7N H 0.1776 0.1354 0.7467 0.102 Uiso 1 1 calc R U . . .
O4 O 0.1778(4) 0.3394(3) 0.0774(3) 0.115(2) Uani 1 1 d . . . . .
O3 O 0.0737(3) 0.2011(3) 0.6568(3) 0.109(2) Uani 1 1 d . . . . .
N12 N 0.2229(5) 0.6665(4) 0.1604(4) 0.093(3) Uani 1 1 d . . . . .
H12N H 0.2414 0.6330 0.1711 0.112 Uiso 1 1 calc R U . . .
N6 N 0.1116(4) 0.1071(3) 0.6503(3) 0.085(2) Uani 1 1 d . . . . .
H6N H 0.1412 0.0817 0.6661 0.102 Uiso 1 1 calc R U . . .
N14 N 0.1356(3) 0.5130(3) 0.3881(3) 0.081(2) Uani 1 1 d . . . . .
H14N H 0.1594 0.5288 0.3566 0.098 Uiso 1 1 calc R U . . .
C61 C 0.2500 0.0274(5) 0.7500 0.052(3) Uani 1 2 d S T P . .
N10 N 0.2531(5) 0.3782(4) 0.1589(4) 0.096(3) Uani 1 1 d . . . . .
H10N H 0.2637 0.4114 0.1782 0.116 Uiso 1 1 calc R U . . .
N9 N 0.1594(4) 0.4313(4) 0.1179(3) 0.092(2) Uani 1 1 d . . . . .
H9N H 0.1711 0.4574 0.1482 0.110 Uiso 1 1 calc R U . . .
N4 N 0.2927(4) 0.0477(3) 0.5752(3) 0.090(3) Uani 1 1 d . . . . .
H4N H 0.2693 0.0432 0.6114 0.107 Uiso 1 1 calc R U . . .
N2 N 0.1398(4) -0.0775(3) 0.6193(4) 0.103(3) Uani 1 1 d . . . . .
H2N H 0.1517 -0.0444 0.6382 0.123 Uiso 1 1 calc R U . . .
N11 N 0.1197(4) 0.6156(3) 0.1600(4) 0.096(2) Uani 1 1 d . . . . .
H11N H 0.1431 0.5864 0.1770 0.115 Uiso 1 1 calc R U . . .
C20 C 0.4711(4) -0.0056(3) 0.7260(3) 0.060(2) Uani 1 1 d . . . . .
H20 H 0.4370 -0.0020 0.7580 0.072 Uiso 1 1 calc R U . . .
C14 C 0.4548(4) 0.0024(3) 0.6580(3) 0.057(2) Uani 1 1 d . . . . .
C19 C 0.5384(4) -0.0189(3) 0.7474(3) 0.062(2) Uani 1 1 d . . . . .
C13 C 0.3595(4) 0.0329(4) 0.5778(4) 0.064(2) Uani 1 1 d . . . . .
N16 N 0.4935(5) 0.1948(4) 0.5096(5) 0.103(3) Uani 1 1 d . . . . .
C11 C 0.2013(5) 0.0305(4) 0.4861(3) 0.083(3) Uani 1 1 d . . . . .
H11C H 0.1844 0.0448 0.4417 0.099 Uiso 1 1 calc R U . . .
H11D H 0.2202 -0.0089 0.4798 0.099 Uiso 1 1 calc R U . . .
C62 C 0.2500 0.5246(6) 0.2500 0.103(6) Uani 1 2 d S T P . .
C17 C 0.5919(4) -0.0229(3) 0.7022(4) 0.066(2) Uani 1 1 d . . . . .
C23 C 0.1097(5) 0.1621(5) 0.6783(5) 0.081(3) Uani 1 1 d . . . . .
C15 C 0.5052(4) -0.0040(4) 0.6110(3) 0.073(3) Uani 1 1 d . . . . .
H15 H 0.4943 -0.0014 0.5643 0.088 Uiso 1 1 calc R U . . .
C16 C 0.5725(4) -0.0142(4) 0.6344(4) 0.072(2) Uani 1 1 d . . . . .
H16 H 0.6067 -0.0153 0.6023 0.086 Uiso 1 1 calc R U . . .
C33 C 0.1958(6) 0.3793(5) 0.1168(5) 0.087(3) Uani 1 1 d . . . . .
C51 C -0.0162(4) 0.4921(4) 0.2031(4) 0.084(3) Uani 1 1 d . . . . .
H51A H -0.0562 0.4726 0.1818 0.101 Uiso 1 1 calc R U . . .
H51B H -0.0311 0.5301 0.2202 0.101 Uiso 1 1 calc R U . . .
C4 C 0.1607(5) -0.1589(4) 0.7786(5) 0.082(3) Uani 1 1 d . . . . .
C53 C 0.0751(5) 0.4846(4) 0.3664(4) 0.077(3) Uani 1 1 d . . . . .
C25 C 0.1497(5) 0.2745(5) 0.7524(5) 0.097(3) Uani 1 1 d . . . . .
H25 H 0.1293 0.2801 0.7090 0.116 Uiso 1 1 calc R U . . .
C31 C 0.0351(5) 0.4505(4) 0.1066(4) 0.089(3) Uani 1 1 d . . . . .
H31A H -0.0024 0.4540 0.0725 0.107 Uiso 1 1 calc R U . . .
H31B H 0.0272 0.4150 0.1333 0.107 Uiso 1 1 calc R U . . .
C54 C 0.1624(5) 0.5189(4) 0.4563(4) 0.076(3) Uani 1 1 d . . . . .
C12 C 0.2578(4) 0.0711(4) 0.5133(4) 0.088(3) Uani 1 1 d . . . . .
H12A H 0.2914 0.0767 0.4782 0.105 Uiso 1 1 calc R U . . .
H12B H 0.2381 0.1095 0.5234 0.105 Uiso 1 1 calc R U . . .
C3 C 0.1310(5) -0.1255(5) 0.6588(6) 0.090(3) Uani 1 1 d . . . . .
C43 C 0.1549(7) 0.6663(4) 0.1404(5) 0.086(3) Uani 1 1 d . . . . .
C49 C 0.2883(7) 0.8187(5) 0.1602(5) 0.092(3) Uani 1 1 d . . . . .
O8 O 0.1993(4) 0.0060(3) 0.7236(4) 0.161(3) Uani 1 1 d . . . . .
C21 C 0.1015(4) 0.0797(4) 0.5288(4) 0.083(3) Uani 1 1 d . . . . .
H21A H 0.0679 0.0761 0.4910 0.099 Uiso 1 1 calc R U . . .
H21B H 0.1307 0.1135 0.5198 0.099 Uiso 1 1 calc R U . . .
C52 C 0.0105(4) 0.4551(4) 0.2623(4) 0.090(3) Uani 1 1 d . . . . .
H52A H -0.0260 0.4493 0.2944 0.108 Uiso 1 1 calc R U . . .
H52B H 0.0242 0.4165 0.2457 0.108 Uiso 1 1 calc R U . . .
C24 C 0.1656(5) 0.2181(5) 0.7745(5) 0.082(3) Uani 1 1 d . . . . .
C1 C 0.1018(5) -0.0259(4) 0.5173(4) 0.109(3) Uani 1 1 d . . . . .
H1A H 0.0560 -0.0197 0.5346 0.130 Uiso 1 1 calc R U . . .
H1B H 0.0968 -0.0303 0.4679 0.130 Uiso 1 1 calc R U . . .
C50 C 0.2412(5) 0.7731(5) 0.1481(4) 0.098(3) Uani 1 1 d . . . . .
H50 H 0.1968 0.7798 0.1300 0.118 Uiso 1 1 calc R U . . .
C32 C 0.1025(6) 0.4443(4) 0.0709(4) 0.103(3) Uani 1 1 d . . . . .
H32A H 0.0983 0.4129 0.0371 0.123 Uiso 1 1 calc R U . . .
H32B H 0.1120 0.4809 0.0469 0.123 Uiso 1 1 calc R U . . .
C34 C 0.2978(6) 0.3310(5) 0.1756(5) 0.085(3) Uani 1 1 d . . . . .
C26 C 0.1638(5) 0.3234(5) 0.7940(6) 0.106(3) Uani 1 1 d . . . . .
C44 C 0.2652(7) 0.7166(6) 0.1650(4) 0.091(3) Uani 1 1 d . . . . .
O9 O 0.2105(4) 0.5580(4) 0.2802(4) 0.180(4) Uani 1 1 d . . . . .
C41 C 0.0211(5) 0.5575(4) 0.1144(4) 0.100(3) Uani 1 1 d . . . . .
H41A H -0.0282 0.5613 0.1049 0.120 Uiso 1 1 calc R U . . .
H41B H 0.0436 0.5561 0.0708 0.120 Uiso 1 1 calc R U . . .
C47 C 0.3554(7) 0.8139(6) 0.1863(5) 0.098(3) Uani 1 1 d . . . . .
C10 C 0.1947(5) -0.1432(5) 0.8392(5) 0.098(3) Uani 1 1 d . . . . .
H10 H 0.2079 -0.1040 0.8461 0.118 Uiso 1 1 calc R U . . .
C45 C 0.3333(6) 0.7088(5) 0.1882(5) 0.096(3) Uani 1 1 d . . . . .
H45 H 0.3494 0.6708 0.1981 0.116 Uiso 1 1 calc R U . . .
C42 C 0.0460(6) 0.6103(4) 0.1530(5) 0.112(3) Uani 1 1 d . . . . .
H42A H 0.0279 0.6455 0.1302 0.135 Uiso 1 1 calc R U . . .
H42B H 0.0274 0.6091 0.1985 0.135 Uiso 1 1 calc R U . . .
C55 C 0.2295(5) 0.5367(4) 0.4680(5) 0.099(3) Uani 1 1 d . . . . .
H55 H 0.2579 0.5454 0.4319 0.119 Uiso 1 1 calc R U . . .
C39 C 0.3287(7) 0.2301(5) 0.1685(5) 0.105(3) Uani 1 1 d . . . . .
C22 C 0.0642(4) 0.0906(4) 0.5939(4) 0.091(3) Uani 1 1 d . . . . .
H22A H 0.0307 0.1220 0.5862 0.109 Uiso 1 1 calc R U . . .
H22B H 0.0394 0.0550 0.6061 0.109 Uiso 1 1 calc R U . . .
C29 C 0.2105(5) 0.2600(6) 0.8789(5) 0.096(3) Uani 1 1 d . . . . .
C30 C 0.1972(5) 0.2106(5) 0.8382(5) 0.096(3) Uani 1 1 d . . . . .
H30 H 0.2095 0.1729 0.8537 0.115 Uiso 1 1 calc R U . . .
C40 C 0.2846(5) 0.2740(5) 0.1488(4) 0.097(3) Uani 1 1 d . . . . .
H40 H 0.2471 0.2669 0.1187 0.117 Uiso 1 1 calc R U . . .
C27 C 0.1935(6) 0.3178(6) 0.8583(6) 0.108(4) Uani 1 1 d . . . . .
C9 C 0.2097(5) -0.1852(7) 0.8908(5) 0.110(4) Uani 1 1 d . . . . .
H9 H 0.2327 -0.1734 0.9312 0.132 Uiso 1 1 calc R U . . .
C35 C 0.3539(6) 0.3388(5) 0.2189(5) 0.103(3) Uani 1 1 d . . . . .
H35 H 0.3618 0.3765 0.2368 0.124 Uiso 1 1 calc R U . . .
C37 C 0.3865(6) 0.2384(5) 0.2101(5) 0.095(3) Uani 1 1 d . . . . .
C2 C 0.1295(6) -0.0806(4) 0.5460(5) 0.132(4) Uani 1 1 d . . . . .
H2C H 0.0980 -0.1128 0.5346 0.158 Uiso 1 1 calc R U . . .
H2D H 0.1733 -0.0892 0.5256 0.158 Uiso 1 1 calc R U . . .
C7 C 0.1905(6) -0.2440(6) 0.8819(6) 0.109(4) Uani 1 1 d . . . . .
C60 C 0.1218(5) 0.5077(4) 0.5116(4) 0.096(3) Uani 1 1 d . . . . .
H60 H 0.0764 0.4956 0.5035 0.115 Uiso 1 1 calc R U . . .
C5 C 0.1405(5) -0.2179(5) 0.7702(5) 0.106(3) Uani 1 1 d . . . . .
H5 H 0.1174 -0.2305 0.7301 0.128 Uiso 1 1 calc R U . . .
C56 C 0.2540(5) 0.5413(5) 0.5369(6) 0.110(4) Uani 1 1 d . . . . .
C6 C 0.1555(6) -0.2574(5) 0.8230(6) 0.120(4) Uani 1 1 d . . . . .
C46 C 0.3764(6) 0.7557(6) 0.1967(5) 0.109(4) Uani 1 1 d . . . . .
H46 H 0.4223 0.7486 0.2100 0.131 Uiso 1 1 calc R U . . .
C18 C 0.6661(4) -0.0332(4) 0.7264(4) 0.108(3) Uani 1 1 d . . . . .
H18A H 0.6962 -0.0256 0.6895 0.162 Uiso 1 1 calc R U . . .
H18B H 0.6716 -0.0736 0.7413 0.162 Uiso 1 1 calc R U . . .
H18C H 0.6775 -0.0070 0.7639 0.162 Uiso 1 1 calc R U . . .
C57 C 0.2127(7) 0.5307(5) 0.5917(5) 0.110(4) Uani 1 1 d . . . . .
C36 C 0.4011(6) 0.2931(5) 0.2383(5) 0.119(4) Uani 1 1 d . . . . .
H36 H 0.4391 0.2996 0.2679 0.142 Uiso 1 1 calc R U . . .
C38 C 0.4365(5) 0.1871(4) 0.2280(5) 0.141(4) Uani 1 1 d . . . . .
H38A H 0.4744 0.2017 0.2562 0.211 Uiso 1 1 calc R U . . .
H38B H 0.4536 0.1707 0.1866 0.211 Uiso 1 1 calc R U . . .
H38C H 0.4125 0.1569 0.2524 0.211 Uiso 1 1 calc R U . . .
O10 O 0.2500 0.4777(5) 0.2500 0.236(9) Uani 1 2 d S T P . .
C48 C 0.4039(5) 0.8656(5) 0.1980(5) 0.141(4) Uani 1 1 d . . . . .
H48A H 0.4506 0.8514 0.2021 0.212 Uiso 1 1 calc R U . . .
H48B H 0.3926 0.8859 0.2394 0.212 Uiso 1 1 calc R U . . .
H48C H 0.3995 0.8925 0.1600 0.212 Uiso 1 1 calc R U . . .
C59 C 0.1461(7) 0.5137(5) 0.5781(6) 0.123(4) Uani 1 1 d . . . . .
O7 O 0.2317(6) 0.0718(5) 0.7828(4) 0.092(4) Uani 0.5 1 d . . P . .
C28 C 0.2086(5) 0.3706(5) 0.9041(5) 0.156(5) Uani 1 1 d . . . . .
H28A H 0.2542 0.3851 0.8964 0.234 Uiso 1 1 calc R U . . .
H28B H 0.2055 0.3590 0.9512 0.234 Uiso 1 1 calc R U . . .
H28C H 0.1755 0.4014 0.8938 0.234 Uiso 1 1 calc R U . . .
C8 C 0.2080(5) -0.2885(5) 0.9383(5) 0.155(5) Uani 1 1 d . . . . .
H8A H 0.2445 -0.3139 0.9241 0.232 Uiso 1 1 calc R U . . .
H8B H 0.1678 -0.3119 0.9471 0.232 Uiso 1 1 calc R U . . .
H8C H 0.2226 -0.2678 0.9793 0.232 Uiso 1 1 calc R U . . .
C78 C 0.5941(7) 0.1213(6) 0.5154(7) 0.193(7) Uani 1 1 d . . . . .
H78A H 0.5735 0.0995 0.5516 0.289 Uiso 1 1 calc R U . . .
H78B H 0.6418 0.1289 0.5274 0.289 Uiso 1 1 calc R U . . .
H78C H 0.5910 0.0986 0.4738 0.289 Uiso 1 1 calc R U . . .
C72 C 0.3855(7) 0.1842(7) 0.4324(10) 0.240(9) Uani 1 1 d D . . . .
H72A H 0.3716 0.2037 0.4733 0.360 Uiso 1 1 calc R U . . .
H72B H 0.3564 0.1504 0.4236 0.360 Uiso 1 1 calc R U . . .
H72C H 0.3812 0.2111 0.3944 0.360 Uiso 1 1 calc R U . . .
C58 C 0.2456(6) 0.5386(5) 0.6648(5) 0.189(6) Uani 1 1 d . . . . .
H58A H 0.2948 0.5417 0.6621 0.283 Uiso 1 1 calc R U . . .
H58B H 0.2344 0.5051 0.6925 0.283 Uiso 1 1 calc R U . . .
H58C H 0.2279 0.5741 0.6850 0.283 Uiso 1 1 calc R U . . .
C77 C 0.5628(10) 0.1697(10) 0.5066(6) 0.298(14) Uani 1 1 d . . . . .
H77A H 0.5757 0.1805 0.4607 0.357 Uiso 1 1 calc R U . . .
H77B H 0.5895 0.1960 0.5366 0.357 Uiso 1 1 calc R U . . .
N15 N 0.5032(6) 0.3106(5) -0.0020(4) 0.127(4) Uani 1 1 d D . . . .
C76 C 0.4889(7) 0.1820(7) 0.6312(7) 0.225(8) Uani 1 1 d D . . . .
H76A H 0.5350 0.1665 0.6347 0.338 Uiso 1 1 calc R U . . .
H76B H 0.4619 0.1648 0.6663 0.338 Uiso 1 1 calc R U . . .
H76C H 0.4902 0.2243 0.6368 0.338 Uiso 1 1 calc R U . . .
C74 C 0.4977(8) 0.2990(6) 0.4639(9) 0.272(10) Uani 1 1 d . . . . .
H74A H 0.5061 0.2842 0.4189 0.408 Uiso 1 1 calc R U . . .
H74B H 0.5343 0.3254 0.4782 0.408 Uiso 1 1 calc R U . . .
H74C H 0.4545 0.3199 0.4631 0.408 Uiso 1 1 calc R U . . .
C70 C 0.5530(10) 0.3171(8) 0.1156(7) 0.288(11) Uani 1 1 d . . . . .
H70A H 0.5168 0.2906 0.1278 0.432 Uiso 1 1 calc R U . . .
H70B H 0.5568 0.3487 0.1485 0.432 Uiso 1 1 calc R U . . .
H70C H 0.5960 0.2960 0.1150 0.432 Uiso 1 1 calc R U . . .
C75 C 0.4562(8) 0.1666(8) 0.5604(7) 0.39(2) Uani 1 1 d D . . . .
H75A H 0.4570 0.1240 0.5535 0.463 Uiso 1 1 calc R U . . .
H75B H 0.4084 0.1796 0.5577 0.463 Uiso 1 1 calc R U . . .
C67 C 0.5230(10) 0.2494(12) -0.0121(11) 0.41(2) Uani 1 1 d . . . . .
H67A H 0.5027 0.2346 -0.0549 0.491 Uiso 1 1 calc R U . . .
H67B H 0.5071 0.2250 0.0251 0.491 Uiso 1 1 calc R U . . .
C68 C 0.6054(10) 0.2479(8) -0.0138(6) 0.320(12) Uani 1 1 d . . . . .
H68A H 0.6209 0.2780 -0.0444 0.480 Uiso 1 1 calc R U . . .
H68B H 0.6200 0.2098 -0.0295 0.480 Uiso 1 1 calc R U . . .
H68C H 0.6248 0.2550 0.0314 0.480 Uiso 1 1 calc R U . . .
C73 C 0.4952(10) 0.2551(7) 0.5064(10) 0.305(13) Uani 1 1 d . . . . .
H73A H 0.4549 0.2655 0.5320 0.366 Uiso 1 1 calc R U . . .
H73B H 0.5341 0.2640 0.5374 0.366 Uiso 1 1 calc R U . . .
C69 C 0.539(2) 0.3382(8) 0.0576(11) 0.48(3) Uani 1 1 d . . . . .
H69A H 0.5837 0.3508 0.0409 0.570 Uiso 1 1 calc R U . . .
H69B H 0.5140 0.3743 0.0660 0.570 Uiso 1 1 calc R U . . .
C64 C 0.3837(11) 0.3395(8) 0.0075(10) 0.346(16) Uani 1 1 d D . . . .
H64A H 0.4039 0.3698 -0.0198 0.519 Uiso 1 1 calc R U . . .
H64B H 0.3785 0.3541 0.0532 0.519 Uiso 1 1 calc R U . . .
H64C H 0.3393 0.3289 -0.0122 0.519 Uiso 1 1 calc R U . . .
C63 C 0.4311(7) 0.2847(8) 0.0097(12) 0.345(17) Uani 1 1 d D . . . .
H63A H 0.4177 0.2568 -0.0261 0.414 Uiso 1 1 calc R U . . .
H63B H 0.4298 0.2649 0.0538 0.414 Uiso 1 1 calc R U . . .
C71 C 0.4611(7) 0.1638(7) 0.4417(10) 0.279(11) Uani 1 1 d D . . . .
H71A H 0.4869 0.1752 0.4021 0.335 Uiso 1 1 calc R U . . .
H71B H 0.4631 0.1210 0.4463 0.335 Uiso 1 1 calc R U . . .
C65 C 0.5331(12) 0.3693(7) -0.0280(8) 0.75(6) Uani 1 1 d D . . . .
H65A H 0.5178 0.4042 -0.0039 0.896 Uiso 1 1 calc R U . . .
H65B H 0.5828 0.3692 -0.0325 0.896 Uiso 1 1 calc R U . . .
C66 C 0.4914(7) 0.3557(9) -0.0949(7) 0.230(9) Uani 1 1 d D . . . .
H66A H 0.4791 0.3145 -0.0959 0.345 Uiso 1 1 calc R U . . .
H66B H 0.5189 0.3647 -0.1334 0.345 Uiso 1 1 calc R U . . .
H66C H 0.4502 0.3794 -0.0970 0.345 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl3A C26 1.722(11) . ?
Cl6A C56 1.671(10) . ?
Cl3B C29 1.579(13) . ?
Cl6B C59 1.468(13) . ?
Cl2 C19 1.741(6) . ?
Cl5 C49 1.751(10) . ?
Cl4 C39 1.741(10) . ?
Cl1 C6 1.749(11) . ?
N1 C21 1.443(9) . ?
N1 C1 1.462(9) . ?
N1 C11 1.467(8) . ?
O2 C13 1.234(7) . ?
N8 C31 1.452(8) . ?
N8 C51 1.451(8) . ?
N8 C41 1.471(9) . ?
O1 C3 1.218(10) . ?
N5 C13 1.365(8) . ?
N5 C14 1.384(8) . ?
N5 H5N 0.8600 . ?
N3 C3 1.392(10) . ?
N3 C4 1.394(10) . ?
N3 H3N 0.8600 . ?
N13 C53 1.360(8) . ?
N13 C52 1.437(8) . ?
N13 H13N 0.8600 . ?
O6 C53 1.195(8) . ?
O5 C43 1.197(10) . ?
N7 C23 1.383(10) . ?
N7 C24 1.410(10) . ?
N7 H7N 0.8600 . ?
O4 C33 1.227(11) . ?
O3 C23 1.190(10) . ?
N12 C43 1.360(11) . ?
N12 C44 1.396(11) . ?
N12 H12N 0.8600 . ?
N6 C23 1.356(10) . ?
N6 C22 1.455(9) . ?
N6 H6N 0.8600 . ?
N14 C53 1.388(9) . ?
N14 C54 1.417(9) . ?
N14 H14N 0.8600 . ?
C61 O7 1.248(11) . ?
C61 O7 1.248(11) 2_556 ?
C61 O8 1.194(6) 2_556 ?
C61 O8 1.194(6) . ?
N10 C33 1.356(11) . ?
N10 C34 1.403(11) . ?
N10 H10N 0.8600 . ?
N9 C33 1.369(11) . ?
N9 C32 1.437(10) . ?
N9 H9N 0.8600 . ?
N4 C13 1.335(8) . ?
N4 C12 1.461(8) . ?
N4 H4N 0.8600 . ?
N2 C3 1.345(10) . ?
N2 C2 1.439(9) . ?
N2 H2N 0.8600 . ?
N11 C43 1.392(11) . ?
N11 C42 1.434(10) . ?
N11 H11N 0.8600 . ?
C20 C14 1.364(8) . ?
C20 C19 1.388(9) . ?
C20 H20 0.9300 . ?
C14 C15 1.371(8) . ?
C19 C17 1.390(9) . ?
N16 C73 1.362(15) . ?
N16 C75 1.402(16) . ?
N16 C77 1.462(15) . ?
N16 C71 1.606(16) . ?
C11 C12 1.508(9) . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C62 O10 1.058(12) . ?
C62 O9 1.238(9) . ?
C62 O9 1.239(9) 2 ?
C17 C16 1.376(9) . ?
C17 C18 1.515(9) . ?
C15 C16 1.385(9) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C51 C52 1.502(9) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C4 C10 1.378(11) . ?
C4 C5 1.396(11) . ?
C25 C24 1.376(11) . ?
C25 C26 1.391(12) . ?
C25 H25 0.9300 . ?
C31 C32 1.511(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C54 C60 1.383(9) . ?
C54 C55 1.373(10) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C49 C50 1.390(12) . ?
C49 C47 1.384(12) . ?
C21 C22 1.505(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C24 C30 1.375(11) . ?
C1 C2 1.451(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C50 C44 1.392(12) . ?
C50 H50 0.9300 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C34 C35 1.363(11) . ?
C34 C40 1.408(11) . ?
C26 C27 1.367(12) . ?
C44 C45 1.389(12) . ?
C41 C42 1.481(11) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C47 C46 1.387(13) . ?
C47 C48 1.511(12) . ?
C10 C9 1.405(12) . ?
C10 H10 0.9300 . ?
C45 C46 1.356(12) . ?
C45 H45 0.9300 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C55 C56 1.413(11) . ?
C55 H55 0.9300 . ?
C39 C40 1.355(12) . ?
C39 C37 1.372(12) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C29 C30 1.388(12) . ?
C29 C27 1.401(13) . ?
C30 H30 0.9300 . ?
C40 H40 0.9300 . ?
C27 C28 1.513(12) . ?
C9 C7 1.387(13) . ?
C9 H9 0.9300 . ?
C35 C36 1.421(12) . ?
C35 H35 0.9300 . ?
C37 C36 1.376(12) . ?
C37 C38 1.541(12) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C7 C6 1.348(12) . ?
C7 C8 1.519(13) . ?
C60 C59 1.369(11) . ?
C60 H60 0.9300 . ?
C5 C6 1.384(11) . ?
C5 H5 0.9300 . ?
C56 C57 1.380(12) . ?
C46 H46 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C57 C59 1.363(13) . ?
C57 C58 1.551(11) . ?
C36 H36 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
O7 O7 1.487(16) 2_556 ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C78 C77 1.257(17) . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C72 C71 1.5398(11) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C58 H58A 0.9601 . ?
C58 H58B 0.9601 . ?
C58 H58C 0.9601 . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
N15 C69 1.47(3) . ?
N15 C67 1.45(2) . ?
N15 C65 1.5396(11) . ?
N15 C63 1.5400(11) . ?
C76 C75 1.5393(11) . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C74 C73 1.293(17) . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C70 C69 1.25(2) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C67 C68 1.60(2) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C64 C63 1.5396(11) . ?
C64 H64A 0.9601 . ?
C64 H64B 0.9601 . ?
C64 H64C 0.9601 . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C65 C66 1.5399(11) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 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
C21 N1 C1 110.9(7) . . ?
C21 N1 C11 111.5(6) . . ?
C1 N1 C11 110.5(7) . . ?
C31 N8 C51 108.5(6) . . ?
C31 N8 C41 112.9(6) . . ?
C51 N8 C41 110.9(7) . . ?
C13 N5 C14 128.3(6) . . ?
C13 N5 H5N 115.9 . . ?
C14 N5 H5N 115.8 . . ?
C3 N3 C4 128.0(8) . . ?
C3 N3 H3N 116.0 . . ?
C4 N3 H3N 116.0 . . ?
C53 N13 C52 121.4(7) . . ?
C53 N13 H13N 119.3 . . ?
C52 N13 H13N 119.3 . . ?
C23 N7 C24 125.2(8) . . ?
C23 N7 H7N 117.4 . . ?
C24 N7 H7N 117.4 . . ?
C43 N12 C44 125.6(10) . . ?
C43 N12 H12N 117.2 . . ?
C44 N12 H12N 117.2 . . ?
C23 N6 C22 120.9(9) . . ?
C23 N6 H6N 119.6 . . ?
C22 N6 H6N 119.5 . . ?
C53 N14 C54 127.2(7) . . ?
C53 N14 H14N 116.4 . . ?
C54 N14 H14N 116.4 . . ?
O7 C61 O7 73.1(11) . 2_556 ?
O7 C61 O8 110.4(7) . 2_556 ?
O7 C61 O8 107.5(7) 2_556 2_556 ?
O7 C61 O8 107.5(7) . . ?
O7 C61 O8 110.4(7) 2_556 . ?
O8 C61 O8 132.4(13) 2_556 . ?
C33 N10 C34 129.7(9) . . ?
C33 N10 H10N 115.1 . . ?
C34 N10 H10N 115.1 . . ?
C33 N9 C32 123.2(9) . . ?
C33 N9 H9N 118.4 . . ?
C32 N9 H9N 118.4 . . ?
C13 N4 C12 122.7(6) . . ?
C13 N4 H4N 118.7 . . ?
C12 N4 H4N 118.7 . . ?
C3 N2 C2 121.0(8) . . ?
C3 N2 H2N 119.5 . . ?
C2 N2 H2N 119.5 . . ?
C43 N11 C42 122.6(9) . . ?
C43 N11 H11N 118.6 . . ?
C42 N11 H11N 118.8 . . ?
C14 C20 C19 120.2(6) . . ?
C14 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C20 C14 C15 119.5(7) . . ?
C20 C14 N5 117.4(6) . . ?
C15 C14 N5 123.1(7) . . ?
C17 C19 C20 122.4(7) . . ?
C17 C19 Cl2 119.8(6) . . ?
C20 C19 Cl2 117.8(6) . . ?
O2 C13 N4 120.5(7) . . ?
O2 C13 N5 122.8(8) . . ?
N4 C13 N5 116.6(7) . . ?
C73 N16 C75 120.0(14) . . ?
C73 N16 C77 111.3(14) . . ?
C75 N16 C77 110.5(12) . . ?
C73 N16 C71 114.0(11) . . ?
C75 N16 C71 100.9(10) . . ?
C77 N16 C71 97.4(9) . . ?
N1 C11 C12 112.2(6) . . ?
N1 C11 H11C 109.2 . . ?
C12 C11 H11C 109.2 . . ?
N1 C11 H11D 109.1 . . ?
C12 C11 H11D 109.1 . . ?
H11C C11 H11D 107.9 . . ?
O10 C62 O9 127.4(6) . . ?
O10 C62 O9 127.4(6) . 2 ?
O9 C62 O9 105.1(13) . 2 ?
C16 C17 C19 114.8(7) . . ?
C16 C17 C18 123.0(7) . . ?
C19 C17 C18 122.2(7) . . ?
O3 C23 N6 123.9(11) . . ?
O3 C23 N7 124.8(10) . . ?
N6 C23 N7 111.3(9) . . ?
C14 C15 C16 118.8(7) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 124.1(7) . . ?
C17 C16 H16 117.9 . . ?
C15 C16 H16 118.0 . . ?
O4 C33 N10 124.9(11) . . ?
O4 C33 N9 120.3(11) . . ?
N10 C33 N9 114.7(11) . . ?
N8 C51 C52 113.2(7) . . ?
N8 C51 H51A 109.0 . . ?
C52 C51 H51A 109.0 . . ?
N8 C51 H51B 108.9 . . ?
C52 C51 H51B 108.9 . . ?
H51A C51 H51B 107.8 . . ?
C10 C4 N3 119.1(10) . . ?
C10 C4 C5 118.0(9) . . ?
N3 C4 C5 122.8(10) . . ?
O6 C53 N13 123.5(8) . . ?
O6 C53 N14 125.2(8) . . ?
N13 C53 N14 111.1(7) . . ?
C24 C25 C26 120.9(10) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.6 . . ?
N8 C31 C32 112.1(7) . . ?
N8 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
N8 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C60 C54 C55 119.0(8) . . ?
C60 C54 N14 121.3(9) . . ?
C55 C54 N14 119.7(8) . . ?
N4 C12 C11 112.2(7) . . ?
N4 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
N4 C12 H12B 109.2 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
O1 C3 N2 124.0(10) . . ?
O1 C3 N3 122.8(9) . . ?
N2 C3 N3 113.2(9) . . ?
O5 C43 N12 127.4(11) . . ?
O5 C43 N11 118.7(12) . . ?
N12 C43 N11 113.8(10) . . ?
C50 C49 C47 127.2(10) . . ?
C50 C49 Cl5 114.5(10) . . ?
C47 C49 Cl5 118.2(11) . . ?
N1 C21 C22 112.5(7) . . ?
N1 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
N1 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
N13 C52 C51 111.0(7) . . ?
N13 C52 H52A 109.5 . . ?
C51 C52 H52A 109.5 . . ?
N13 C52 H52B 109.4 . . ?
C51 C52 H52B 109.4 . . ?
H52A C52 H52B 108.0 . . ?
C30 C24 C25 119.0(9) . . ?
C30 C24 N7 116.6(9) . . ?
C25 C24 N7 124.3(9) . . ?
C2 C1 N1 114.9(8) . . ?
C2 C1 H1A 108.6 . . ?
N1 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
N1 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
C49 C50 C44 115.4(10) . . ?
C49 C50 H50 122.3 . . ?
C44 C50 H50 122.3 . . ?
N9 C32 C31 112.3(7) . . ?
N9 C32 H32A 109.2 . . ?
C31 C32 H32A 109.2 . . ?
N9 C32 H32B 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
C35 C34 N10 121.2(10) . . ?
C35 C34 C40 118.6(11) . . ?
N10 C34 C40 120.2(11) . . ?
C27 C26 C25 122.0(11) . . ?
C27 C26 Cl3A 120.9(10) . . ?
C25 C26 Cl3A 116.8(9) . . ?
C45 C44 C50 119.8(11) . . ?
C45 C44 N12 117.8(12) . . ?
C50 C44 N12 122.4(12) . . ?
N8 C41 C42 112.8(7) . . ?
N8 C41 H41A 109.0 . . ?
C42 C41 H41A 109.0 . . ?
N8 C41 H41B 109.1 . . ?
C42 C41 H41B 109.0 . . ?
H41A C41 H41B 107.8 . . ?
C49 C47 C46 113.3(11) . . ?
C49 C47 C48 124.4(12) . . ?
C46 C47 C48 122.1(12) . . ?
C4 C10 C9 121.5(10) . . ?
C4 C10 H10 119.2 . . ?
C9 C10 H10 119.3 . . ?
C46 C45 C44 121.0(11) . . ?
C46 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
N11 C42 C41 114.8(9) . . ?
N11 C42 H42A 108.6 . . ?
C41 C42 H42A 108.6 . . ?
N11 C42 H42B 108.5 . . ?
C41 C42 H42B 108.5 . . ?
H42A C42 H42B 107.5 . . ?
C54 C55 C56 117.5(9) . . ?
C54 C55 H55 121.3 . . ?
C56 C55 H55 121.2 . . ?
C40 C39 C37 124.1(10) . . ?
C40 C39 Cl4 116.8(9) . . ?
C37 C39 Cl4 119.0(10) . . ?
N6 C22 C21 111.8(7) . . ?
N6 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
N6 C22 H22B 109.2 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
C30 C29 C27 123.2(10) . . ?
C30 C29 Cl3B 113.6(11) . . ?
C27 C29 Cl3B 122.9(12) . . ?
C24 C30 C29 119.0(10) . . ?
C24 C30 H30 120.6 . . ?
C29 C30 H30 120.4 . . ?
C39 C40 C34 117.3(10) . . ?
C39 C40 H40 121.4 . . ?
C34 C40 H40 121.3 . . ?
C26 C27 C29 115.9(10) . . ?
C26 C27 C28 122.4(12) . . ?
C29 C27 C28 121.8(12) . . ?
C7 C9 C10 120.5(11) . . ?
C7 C9 H9 119.8 . . ?
C10 C9 H9 119.7 . . ?
C34 C35 C36 124.2(10) . . ?
C34 C35 H35 117.9 . . ?
C36 C35 H35 117.9 . . ?
C39 C37 C36 120.7(11) . . ?
C39 C37 C38 121.6(11) . . ?
C36 C37 C38 117.7(11) . . ?
N2 C2 C1 112.2(8) . . ?
N2 C2 H2C 109.2 . . ?
C1 C2 H2C 109.1 . . ?
N2 C2 H2D 109.2 . . ?
C1 C2 H2D 109.2 . . ?
H2C C2 H2D 107.9 . . ?
C6 C7 C9 116.4(12) . . ?
C6 C7 C8 124.1(13) . . ?
C9 C7 C8 119.4(12) . . ?
C59 C60 C54 122.5(10) . . ?
C59 C60 H60 118.8 . . ?
C54 C60 H60 118.7 . . ?
C6 C5 C4 118.4(10) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.9 . . ?
C57 C56 C55 122.8(10) . . ?
C57 C56 Cl6A 119.8(10) . . ?
C55 C56 Cl6A 117.3(10) . . ?
C7 C6 C5 125.2(11) . . ?
C7 C6 Cl1 119.8(10) . . ?
C5 C6 Cl1 115.0(9) . . ?
C45 C46 C47 123.0(12) . . ?
C45 C46 H46 118.5 . . ?
C47 C46 H46 118.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C59 C57 C56 118.0(10) . . ?
C59 C57 C58 124.5(11) . . ?
C56 C57 C58 117.6(12) . . ?
C37 C36 C35 115.0(11) . . ?
C37 C36 H36 122.5 . . ?
C35 C36 H36 122.5 . . ?
C37 C38 H38A 109.4 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.4 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C57 C59 C60 120.1(11) . . ?
C57 C59 Cl6B 94.7(10) . . ?
C60 C59 Cl6B 140.2(12) . . ?
C61 O7 O7 53.4(5) . 2_556 ?
C27 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.6 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.4 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C77 C78 H78A 109.3 . . ?
C77 C78 H78B 109.9 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.3 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.6 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.3 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.4 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.6 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C78 C77 N16 140(2) . . ?
C78 C77 H77A 102.0 . . ?
N16 C77 H77A 102.0 . . ?
C78 C77 H77B 101.8 . . ?
N16 C77 H77B 101.9 . . ?
H77A C77 H77B 104.8 . . ?
C69 N15 C67 113.0(15) . . ?
C69 N15 C65 73.9(11) . . ?
C67 N15 C65 132.2(17) . . ?
C69 N15 C63 116.9(15) . . ?
C67 N15 C63 84.5(12) . . ?
C65 N15 C63 136.8(15) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.4 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
N16 C75 C76 109.1(15) . . ?
N16 C75 H75A 109.9 . . ?
C76 C75 H75A 109.9 . . ?
N16 C75 H75B 109.8 . . ?
C76 C75 H75B 109.9 . . ?
H75A C75 H75B 108.3 . . ?
N15 C67 C68 107.0(19) . . ?
N15 C67 H67A 110.3 . . ?
C68 C67 H67A 110.3 . . ?
N15 C67 H67B 110.4 . . ?
C68 C67 H67B 110.3 . . ?
H67A C67 H67B 108.5 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.4 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C74 C73 N16 143(2) . . ?
C74 C73 H73A 101.3 . . ?
N16 C73 H73A 101.3 . . ?
C74 C73 H73B 101.3 . . ?
N16 C73 H73B 101.3 . . ?
H73A C73 H73B 104.5 . . ?
C70 C69 N15 129(2) . . ?
C70 C69 H69A 105.0 . . ?
N15 C69 H69A 104.8 . . ?
C70 C69 H69B 105.0 . . ?
N15 C69 H69B 105.1 . . ?
H69A C69 H69B 105.8 . . ?
C63 C64 H64A 109.2 . . ?
C63 C64 H64B 109.3 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.9 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C64 C63 N15 103.5(14) . . ?
C64 C63 H63A 110.8 . . ?
N15 C63 H63A 111.1 . . ?
C64 C63 H63B 111.1 . . ?
N15 C63 H63B 111.1 . . ?
H63A C63 H63B 109.1 . . ?
C72 C71 N16 107.9(14) . . ?
C72 C71 H71A 110.3 . . ?
N16 C71 H71A 110.1 . . ?
C72 C71 H71B 110.0 . . ?
N16 C71 H71B 110.1 . . ?
H71A C71 H71B 108.4 . . ?
C66 C65 N15 85.2(9) . . ?
C66 C65 H65A 114.4 . . ?
N15 C65 H65A 114.4 . . ?
C66 C65 H65B 114.5 . . ?
N15 C65 H65B 114.5 . . ?
H65A C65 H65B 111.6 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.4 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?

_refine_diff_density_max         0.347
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.045


# start Validation Reply Form
_vrf_PLAT234_T-Cl-Me-TEACO3      
;
PROBLEM: Large Hirshfeld Difference N15      --C65              0.57 Ang. 
RESPONSE: This may be due to disorder in the model.
;
_vrf_PLAT410_T-Cl-Me-TEACO3      
;
PROBLEM: Short Intra H...H Contact  H65A     ..H69B             1.53 Ang.   
RESPONSE: This may be due to short distances between adjacent H atoms.
;
####################################################################### 
# 
# 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_T-Br-Me-TBASO4
_database_code_depnum_ccdc_archive 'CCDC 1840360'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C30 H36 Br3 N7 O3), 2(C16 H36 N), O4 S'
_chemical_formula_sum            'C92 H144 Br6 N16 O10 S'
_chemical_formula_weight         2145.69

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'
S S 0.1246 0.1234 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.738(2)
_cell_length_b                   16.583(3)
_cell_length_c                   25.631(4)
_cell_angle_alpha                108.151(15)
_cell_angle_beta                 97.637(12)
_cell_angle_gamma                93.047(14)
_cell_volume                     5471.6(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2146
_cell_measurement_theta_min      3.2390
_cell_measurement_theta_max      18.6060

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_F_000             2228.0
_exptl_transmission_factor_min   0.498
_exptl_transmission_factor_max   0.592
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_exptl_absorpt_coefficient_mu    2.278
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19808
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.868
_diffrn_reflns_theta_max         24.253
_diffrn_reflns_theta_full        24.253
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             16564
_reflns_number_gt                10364
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.1600P)²+3.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16564
_refine_ls_number_parameters     1140
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0990
_refine_ls_wR_factor_ref         0.3247
_refine_ls_wR_factor_gt          0.2657
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.004

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
Br4 Br 0.27214(18) 0.87070(17) -0.03148(7) 0.1627(10) Uani 1 1 d . . . . .
Br1 Br -0.17286(14) 0.45549(17) 0.24137(11) 0.1584(10) Uani 1 1 d . . . . .
Br6 Br 0.98297(13) 0.7566(2) 0.40837(10) 0.1802(12) Uani 1 1 d . . . . .
Br3 Br 0.46953(18) 1.07387(17) 0.08950(10) 0.1702(10) Uani 1 1 d . . . . .
Br2 Br 0.78909(17) 0.73107(19) 0.53019(8) 0.1791(11) Uani 1 1 d . . . . .
Br5 Br 0.01021(18) 0.30325(17) 0.31914(11) 0.1759(10) Uani 1 1 d . . . . .
S1 S 0.3747(2) 0.6915(2) 0.25011(11) 0.0620(9) Uani 1 1 d . . . . .
O7 O 0.3216(7) 0.6821(6) 0.1945(3) 0.093(3) Uani 1 1 d . . . . .
O3 O 0.6299(6) 0.6773(6) 0.0907(4) 0.089(3) Uani 1 1 d . . . . .
O2 O 0.5915(8) 0.4168(7) 0.2772(4) 0.100(3) Uani 1 1 d . . . . .
O9 O 0.3551(7) 0.6132(7) 0.2654(4) 0.102(3) Uani 1 1 d . . . . .
N15 N 0.8705(7) 0.8323(7) 0.0928(4) 0.073(3) Uani 1 1 d . . . . .
O5 O 0.2228(7) 0.7262(7) 0.4536(4) 0.108(3) Uani 1 1 d . . . . .
O4 O 0.1019(7) 0.9246(7) 0.2207(4) 0.102(3) Uani 1 1 d . . . . .
O8 O 0.3391(7) 0.7653(6) 0.2914(3) 0.094(3) Uani 1 1 d . . . . .
O10 O 0.4787(7) 0.7113(6) 0.2524(3) 0.101(3) Uani 1 1 d . . . . .
N4 N 0.4645(9) 0.4511(7) 0.2244(5) 0.084(3) Uani 1 1 d . . . . .
H4N H 0.4239 0.4884 0.2231 0.101 Uiso 1 1 calc R U . . .
N8 N 0.2656(8) 0.9512(7) 0.3865(4) 0.078(3) Uani 1 1 d . . . . .
N12 N 0.2405(9) 0.6507(10) 0.3642(5) 0.092(4) Uani 1 1 d . . . . .
H12N H 0.2682 0.6533 0.3365 0.111 Uiso 1 1 calc R U . . .
N1 N 0.5094(7) 0.4420(7) 0.1105(4) 0.072(3) Uani 1 1 d . . . . .
N5 N 0.5313(8) 0.5445(8) 0.3073(5) 0.087(3) Uani 1 1 d . . . . .
H5N H 0.4859 0.5738 0.2985 0.105 Uiso 1 1 calc R U . . .
N9 N 0.1606(7) 0.8452(8) 0.2739(4) 0.087(3) Uani 1 1 d . . . . .
H9N H 0.1949 0.8036 0.2748 0.105 Uiso 1 1 calc R U . . .
N14 N 0.5795(9) 0.8635(9) 0.3408(4) 0.084(3) Uani 1 1 d . . . . .
H14 H 0.5405 0.8201 0.3195 0.100 Uiso 1 1 calc R U . . .
N16 N 0.3425(8) 0.7290(7) 0.6216(4) 0.077(3) Uani 1 1 d . . . . .
N13 N 0.4461(9) 0.9381(8) 0.3301(4) 0.089(3) Uani 1 1 d . . . . .
H13N H 0.4167 0.8911 0.3067 0.107 Uiso 1 1 calc R U . . .
O1 O 0.1956(8) 0.4063(8) 0.0663(4) 0.114(4) Uani 1 1 d . . . . .
N6 N 0.5887(9) 0.6281(8) 0.1591(5) 0.088(3) Uani 1 1 d . . . . .
H6N H 0.5550 0.6352 0.1859 0.106 Uiso 1 1 calc R U . . .
O6 O 0.5911(7) 1.0102(8) 0.3813(5) 0.115(3) Uani 1 1 d . . . . .
N2 N 0.3171(9) 0.5162(8) 0.0930(4) 0.088(3) Uani 1 1 d . . . . .
H2N H 0.3386 0.5660 0.1159 0.106 Uiso 1 1 calc R U . . .
C13 C 0.5328(12) 0.4651(11) 0.2691(6) 0.077(4) Uani 1 1 d . . . . .
N11 N 0.3171(10) 0.7855(10) 0.4060(4) 0.091(3) Uani 1 1 d . . . . .
H11N H 0.3461 0.7754 0.3772 0.109 Uiso 1 1 calc R U . . .
N7 N 0.5231(9) 0.7460(9) 0.1473(4) 0.093(3) Uani 1 1 d . . . . .
H7N H 0.4855 0.7390 0.1702 0.112 Uiso 1 1 calc R U . . .
N10 N 0.2062(8) 0.8247(7) 0.1892(4) 0.087(3) Uani 1 1 d . . . . .
H10N H 0.2358 0.7843 0.1966 0.104 Uiso 1 1 calc R U . . .
C44 C 0.1831(10) 0.5741(13) 0.3564(6) 0.085(4) Uani 1 1 d . . . . .
C23 C 0.5852(9) 0.6820(10) 0.1299(6) 0.074(4) Uani 1 1 d . . . . .
C43 C 0.2581(11) 0.7231(12) 0.4112(6) 0.078(4) Uani 1 1 d . . . . .
C73 C 0.7971(8) 0.8169(9) 0.0404(5) 0.079(4) Uani 1 1 d . . . . .
H73A H 0.7552 0.7649 0.0345 0.095 Uiso 1 1 calc R U . . .
H73B H 0.7554 0.8633 0.0467 0.095 Uiso 1 1 calc R U . . .
C42 C 0.3339(12) 0.8687(11) 0.4466(5) 0.102(5) Uani 1 1 d . . . . .
H42A H 0.3989 0.8943 0.4463 0.123 Uiso 1 1 calc R U . . .
H42B H 0.3329 0.8635 0.4832 0.123 Uiso 1 1 calc R U . . .
N3 N 0.1930(9) 0.5240(9) 0.1444(5) 0.099(4) Uani 1 1 d . . . . .
H3N H 0.2258 0.5720 0.1636 0.119 Uiso 1 1 calc R U . . .
C61 C 0.9364(9) 0.7596(9) 0.0875(5) 0.077(4) Uani 1 1 d . . . . .
H61A H 0.9836 0.7733 0.1215 0.092 Uiso 1 1 calc R U . . .
H61B H 0.9733 0.7566 0.0574 0.092 Uiso 1 1 calc R U . . .
C1 C 0.4328(11) 0.4073(10) 0.0618(5) 0.099(5) Uani 1 1 d . . . . .
H1A H 0.3880 0.3654 0.0683 0.118 Uiso 1 1 calc R U . . .
H1B H 0.4632 0.3785 0.0299 0.118 Uiso 1 1 calc R U . . .
C69 C 0.9378(9) 0.9163(10) 0.1078(6) 0.090(4) Uani 1 1 d . . . . .
H69A H 0.9786 0.9252 0.1434 0.108 Uiso 1 1 calc R U . . .
H69B H 0.9816 0.9097 0.0803 0.108 Uiso 1 1 calc R U . . .
C34 C 0.2174(8) 0.8384(10) 0.1376(5) 0.073(4) Uani 1 1 d . . . . .
C54 C 0.6767(14) 0.8490(13) 0.3605(7) 0.092(5) Uani 1 1 d . . . . .
C35 C 0.2020(9) 0.9146(10) 0.1261(6) 0.088(4) Uani 1 1 d . . . . .
H35 H 0.1809 0.9599 0.1525 0.106 Uiso 1 1 calc R U . . .
C33 C 0.1516(10) 0.8710(10) 0.2282(5) 0.071(4) Uani 1 1 d . . . . .
C15 C 0.6837(12) 0.5591(10) 0.3731(7) 0.090(4) Uani 1 1 d . . . . .
H15 H 0.7072 0.5126 0.3489 0.107 Uiso 1 1 calc R U . . .
C62 C 0.8823(10) 0.6717(9) 0.0769(6) 0.089(4) Uani 1 1 d . . . . .
H62A H 0.8485 0.6727 0.1079 0.107 Uiso 1 1 calc R U . . .
H62B H 0.8330 0.6580 0.0437 0.107 Uiso 1 1 calc R U . . .
C53 C 0.5438(13) 0.9407(14) 0.3532(6) 0.088(4) Uani 1 1 d . . . . .
C40 C 0.2444(9) 0.7712(10) 0.0976(5) 0.085(4) Uani 1 1 d . . . . .
H40 H 0.2523 0.7201 0.1047 0.102 Uiso 1 1 calc R U . . .
C41 C 0.2564(11) 0.9275(10) 0.4360(5) 0.091(4) Uani 1 1 d . . . . .
H41A H 0.1911 0.8988 0.4318 0.109 Uiso 1 1 calc R U . . .
H41B H 0.2636 0.9787 0.4681 0.109 Uiso 1 1 calc R U . . .
C55 C 0.6989(11) 0.7698(15) 0.3309(7) 0.104(6) Uani 1 1 d . . . . .
H55 H 0.6505 0.7367 0.3022 0.125 Uiso 1 1 calc R U . . .
C14 C 0.5922(12) 0.5846(10) 0.3583(6) 0.083(4) Uani 1 1 d . . . . .
C74 C 0.8388(10) 0.8092(10) -0.0125(5) 0.095(4) Uani 1 1 d . . . . .
H74A H 0.8704 0.7569 -0.0235 0.114 Uiso 1 1 calc R U . . .
H74B H 0.8881 0.8567 -0.0061 0.114 Uiso 1 1 calc R U . . .
C24 C 0.5141(9) 0.8197(11) 0.1324(6) 0.084(4) Uani 1 1 d . . . . .
C85 C 0.4491(9) 0.7657(9) 0.6338(6) 0.086(4) Uani 1 1 d . . . . .
H85A H 0.4545 0.8241 0.6584 0.103 Uiso 1 1 calc R U . . .
H85B H 0.4704 0.7666 0.5994 0.103 Uiso 1 1 calc R U . . .
C11 C 0.5345(10) 0.3797(8) 0.1399(5) 0.082(4) Uani 1 1 d . . . . .
H11A H 0.5992 0.3978 0.1625 0.099 Uiso 1 1 calc R U . . .
H11B H 0.5374 0.3243 0.1129 0.099 Uiso 1 1 calc R U . . .
C65 C 0.8095(9) 0.8386(9) 0.1405(5) 0.077(4) Uani 1 1 d . . . . .
H65A H 0.7707 0.8866 0.1436 0.093 Uiso 1 1 calc R U . . .
H65B H 0.7634 0.7876 0.1291 0.093 Uiso 1 1 calc R U . . .
C32 C 0.1131(10) 0.8871(13) 0.3209(6) 0.109(6) Uani 1 1 d . . . . .
H32A H 0.1051 0.8490 0.3424 0.130 Uiso 1 1 calc R U . . .
H32B H 0.0479 0.8993 0.3075 0.130 Uiso 1 1 calc R U . . .
C12 C 0.4582(10) 0.3720(10) 0.1772(5) 0.090(4) Uani 1 1 d . . . . .
H12A H 0.3925 0.3608 0.1556 0.108 Uiso 1 1 calc R U . . .
H12B H 0.4701 0.3245 0.1909 0.108 Uiso 1 1 calc R U . . .
C30 C 0.4805(9) 0.8915(12) 0.1705(6) 0.095(5) Uani 1 1 d . . . . .
H30 H 0.4671 0.8888 0.2046 0.114 Uiso 1 1 calc R U . . .
C18 C 0.6179(14) 0.7010(10) 0.4462(6) 0.096(4) Uani 1 1 d . . . . .
C38 C 0.2606(11) 0.7777(13) 0.0456(6) 0.101(5) Uani 1 1 d . . . . .
C77 C 0.2864(12) 0.7881(9) 0.5957(5) 0.094(5) Uani 1 1 d . . . . .
H77A H 0.3117 0.7872 0.5620 0.113 Uiso 1 1 calc R U . . .
H77B H 0.2998 0.8460 0.6213 0.113 Uiso 1 1 calc R U . . .
C31 C 0.1733(11) 0.9710(11) 0.3588(6) 0.100(5) Uani 1 1 d . . . . .
H31A H 0.1883 1.0068 0.3367 0.120 Uiso 1 1 calc R U . . .
H31B H 0.1350 1.0018 0.3864 0.120 Uiso 1 1 calc R U . . .
C81 C 0.3032(11) 0.7219(11) 0.6737(6) 0.100(5) Uani 1 1 d . . . . .
H81A H 0.3410 0.6839 0.6885 0.120 Uiso 1 1 calc R U . . .
H81B H 0.2348 0.6977 0.6635 0.120 Uiso 1 1 calc R U . . .
C90 C 0.3692(11) 0.6235(10) 0.5289(6) 0.094(4) Uani 1 1 d . . . . .
H90A H 0.4405 0.6343 0.5379 0.112 Uiso 1 1 calc R U . . .
H90B H 0.3455 0.6636 0.5107 0.112 Uiso 1 1 calc R U . . .
C51 C 0.3429(11) 1.0178(10) 0.3953(5) 0.092(4) Uani 1 1 d . . . . .
H51A H 0.3932 1.0157 0.4251 0.110 Uiso 1 1 calc R U . . .
H51B H 0.3161 1.0723 0.4075 0.110 Uiso 1 1 calc R U . . .
C21 C 0.5974(11) 0.4808(10) 0.0975(6) 0.098(5) Uani 1 1 d . . . . .
H21A H 0.5787 0.4986 0.0652 0.118 Uiso 1 1 calc R U . . .
H21B H 0.6437 0.4384 0.0880 0.118 Uiso 1 1 calc R U . . .
C25 C 0.5373(9) 0.8300(12) 0.0824(6) 0.092(4) Uani 1 1 d . . . . .
H25 H 0.5614 0.7851 0.0572 0.111 Uiso 1 1 calc R U . . .
C46 C 0.1391(14) 0.4252(14) 0.2996(7) 0.115(6) Uani 1 1 d . . . . .
H46 H 0.1444 0.3797 0.2682 0.138 Uiso 1 1 calc R U . . .
C2 C 0.3743(11) 0.4759(9) 0.0490(5) 0.089(4) Uani 1 1 d . . . . .
H2C H 0.4195 0.5193 0.0443 0.107 Uiso 1 1 calc R U . . .
H2D H 0.3297 0.4508 0.0142 0.107 Uiso 1 1 calc R U . . .
C45 C 0.1934(12) 0.5026(14) 0.3092(7) 0.101(5) Uani 1 1 d . . . . .
H45 H 0.2364 0.5082 0.2851 0.121 Uiso 1 1 calc R U . . .
C60 C 0.7464(13) 0.9010(13) 0.4027(6) 0.118(6) Uani 1 1 d . . . . .
H60 H 0.7360 0.9555 0.4242 0.142 Uiso 1 1 calc R U . . .
C22 C 0.6484(10) 0.5583(11) 0.1461(6) 0.101(5) Uani 1 1 d . . . . .
H22A H 0.6643 0.5409 0.1788 0.121 Uiso 1 1 calc R U . . .
H22B H 0.7098 0.5773 0.1369 0.121 Uiso 1 1 calc R U . . .
C89 C 0.3267(9) 0.6377(9) 0.5813(6) 0.085(4) Uani 1 1 d . . . . .
H89A H 0.3552 0.6004 0.6005 0.102 Uiso 1 1 calc R U . . .
H89B H 0.2563 0.6206 0.5715 0.102 Uiso 1 1 calc R U . . .
C50 C 0.1222(12) 0.5619(14) 0.3910(8) 0.121(6) Uani 1 1 d . . . . .
H50 H 0.1154 0.6075 0.4220 0.145 Uiso 1 1 calc R U . . .
C20 C 0.5606(11) 0.6565(10) 0.3961(6) 0.088(4) Uani 1 1 d . . . . .
H20 H 0.4994 0.6742 0.3869 0.106 Uiso 1 1 calc R U . . .
C28 C 0.4674(10) 0.9671(12) 0.1564(7) 0.095(5) Uani 1 1 d . . . . .
C37 C 0.2468(12) 0.8557(16) 0.0377(6) 0.108(5) Uani 1 1 d . . . . .
C4 C 0.1064(12) 0.5026(13) 0.1638(7) 0.088(4) Uani 1 1 d . . . . .
C75 C 0.7563(11) 0.8086(11) -0.0588(6) 0.113(5) Uani 1 1 d . . . . .
H75A H 0.7263 0.8617 -0.0478 0.136 Uiso 1 1 calc R U . . .
H75B H 0.7060 0.7625 -0.0636 0.136 Uiso 1 1 calc R U . . .
C58 C 0.8404(10) 0.8619(16) 0.4111(7) 0.108(7) Uani 1 1 d . . . . .
C3 C 0.2307(13) 0.4771(14) 0.0987(7) 0.090(4) Uani 1 1 d . . . . .
C36 C 0.2179(10) 0.9225(11) 0.0760(7) 0.092(4) Uani 1 1 d . . . . .
H36 H 0.2089 0.9732 0.0685 0.111 Uiso 1 1 calc R U . . .
C91 C 0.3413(11) 0.5322(12) 0.4888(7) 0.120(6) Uani 1 1 d . . . . .
H91A H 0.3598 0.4928 0.5087 0.144 Uiso 1 1 calc R U . . .
H91B H 0.2701 0.5236 0.4783 0.144 Uiso 1 1 calc R U . . .
C57 C 0.850(2) 0.7841(18) 0.3793(13) 0.143(11) Uani 1 1 d . . . . .
C56 C 0.7882(18) 0.7328(18) 0.3397(9) 0.154(12) Uani 1 1 d . . . . .
H56 H 0.8002 0.6783 0.3192 0.185 Uiso 1 1 calc R U . . .
C16 C 0.7400(12) 0.6036(13) 0.4246(8) 0.107(5) Uani 1 1 d . . . . .
H16 H 0.8010 0.5865 0.4347 0.128 Uiso 1 1 calc R U . . .
C26 C 0.5256(13) 0.9029(18) 0.0703(8) 0.132(7) Uani 1 1 d . . . . .
H26 H 0.5410 0.9084 0.0373 0.158 Uiso 1 1 calc R U . . .
C48 C 0.0694(13) 0.4837(19) 0.3821(7) 0.121(7) Uani 1 1 d . . . . .
C17 C 0.7068(15) 0.6717(13) 0.4601(6) 0.102(5) Uani 1 1 d . . . . .
C63 C 0.9534(13) 0.6042(12) 0.0694(7) 0.119(5) Uani 1 1 d . . . . .
H63A H 1.0000 0.6163 0.1034 0.143 Uiso 1 1 calc R U . . .
H63B H 0.9904 0.6063 0.0400 0.143 Uiso 1 1 calc R U . . .
C66 C 0.8618(11) 0.8485(12) 0.1967(6) 0.111(5) Uani 1 1 d . . . . .
H66A H 0.8930 0.7970 0.1957 0.134 Uiso 1 1 calc R U . . .
H66B H 0.9135 0.8953 0.2072 0.134 Uiso 1 1 calc R U . . .
C70 C 0.8868(11) 0.9938(11) 0.1109(7) 0.117(5) Uani 1 1 d . . . . .
H70A H 0.8452 1.0034 0.1396 0.140 Uiso 1 1 calc R U . . .
H70B H 0.8451 0.9861 0.0758 0.140 Uiso 1 1 calc R U . . .
C10 C 0.0768(14) 0.5675(13) 0.2051(8) 0.110(5) Uani 1 1 d . . . . .
H10 H 0.1146 0.6200 0.2174 0.131 Uiso 1 1 calc R U . . .
C5 C 0.0559(12) 0.4258(13) 0.1451(6) 0.100(5) Uani 1 1 d . . . . .
H5 H 0.0751 0.3814 0.1172 0.120 Uiso 1 1 calc R U . . .
C6 C -0.0329(14) 0.4141(17) 0.1709(11) 0.123(8) Uani 1 1 d . . . . .
C64 C 0.9000(14) 0.5138(12) 0.0546(7) 0.138(6) Uani 1 1 d . . . . .
H64A H 0.8761 0.5075 0.0868 0.207 Uiso 1 1 calc R U . . .
H64B H 0.9452 0.4722 0.0427 0.207 Uiso 1 1 calc R U . . .
H64C H 0.8455 0.5056 0.0253 0.207 Uiso 1 1 calc R U . . .
C9 C -0.0065(16) 0.5595(15) 0.2299(10) 0.128(8) Uani 1 1 d . . . . .
H9 H -0.0267 0.6046 0.2568 0.154 Uiso 1 1 calc R U . . .
C67 C 0.7956(14) 0.8650(15) 0.2395(7) 0.127(6) Uani 1 1 d . . . . .
H67A H 0.7423 0.8194 0.2275 0.153 Uiso 1 1 calc R U . . .
H67B H 0.8327 0.8621 0.2737 0.153 Uiso 1 1 calc R U . . .
C78 C 0.1731(13) 0.7648(13) 0.5815(7) 0.138(7) Uani 1 1 d . . . . .
H78A H 0.1480 0.7570 0.6134 0.166 Uiso 1 1 calc R U . . .
H78B H 0.1580 0.7117 0.5509 0.166 Uiso 1 1 calc R U . . .
C86 C 0.5185(11) 0.7144(13) 0.6610(7) 0.126(6) Uani 1 1 d . . . . .
H86A H 0.5001 0.7151 0.6964 0.151 Uiso 1 1 calc R U . . .
H86B H 0.5137 0.6557 0.6371 0.151 Uiso 1 1 calc R U . . .
C39 C 0.2938(14) 0.7026(12) 0.0030(6) 0.138(7) Uani 1 1 d . . . . .
H39A H 0.2497 0.6888 -0.0316 0.207 Uiso 1 1 calc R U . . .
H39B H 0.2934 0.6543 0.0161 0.207 Uiso 1 1 calc R U . . .
H39C H 0.3594 0.7171 -0.0024 0.207 Uiso 1 1 calc R U . . .
C92 C 0.3868(14) 0.5093(13) 0.4366(7) 0.154(8) Uani 1 1 d . . . . .
H92A H 0.3715 0.5491 0.4171 0.231 Uiso 1 1 calc R U . . .
H92B H 0.3608 0.4528 0.4133 0.231 Uiso 1 1 calc R U . . .
H92C H 0.4571 0.5114 0.4461 0.231 Uiso 1 1 calc R U . . .
C82 C 0.3108(14) 0.8110(14) 0.7190(7) 0.132(6) Uani 1 1 d . . . . .
H82A H 0.2692 0.8488 0.7064 0.158 Uiso 1 1 calc R U . . .
H82B H 0.3784 0.8373 0.7294 0.158 Uiso 1 1 calc R U . . .
C8 C -0.0507(16) 0.487(2) 0.2128(8) 0.121(8) Uani 1 1 d . . . . .
C87 C 0.6243(15) 0.7565(15) 0.6697(9) 0.159(7) Uani 1 1 d . . . . .
H87A H 0.6469 0.7449 0.6341 0.191 Uiso 1 1 calc R U . . .
H87B H 0.6249 0.8178 0.6859 0.191 Uiso 1 1 calc R U . . .
C79 C 0.1245(17) 0.8348(17) 0.5657(8) 0.215(13) Uani 1 1 d D . . . .
H79A H 0.1755 0.8727 0.5601 0.258 Uiso 1 1 calc R U . . .
H79B H 0.0819 0.8093 0.5302 0.258 Uiso 1 1 calc R U . . .
C76 C 0.7919(15) 0.7978(13) -0.1139(6) 0.149(7) Uani 1 1 d . . . . .
H76A H 0.8089 0.8528 -0.1169 0.224 Uiso 1 1 calc R U . . .
H76B H 0.7405 0.7670 -0.1438 0.224 Uiso 1 1 calc R U . . .
H76C H 0.8490 0.7665 -0.1158 0.224 Uiso 1 1 calc R U . . .
C71 C 0.9660(15) 1.0734(13) 0.1248(11) 0.163(8) Uani 1 1 d . . . . .
H71A H 1.0172 1.0580 0.1018 0.196 Uiso 1 1 calc R U . . .
H71B H 0.9346 1.1195 0.1159 0.196 Uiso 1 1 calc R U . . .
C19 C 0.5821(17) 0.7779(14) 0.4845(7) 0.171(9) Uani 1 1 d . . . . .
H19A H 0.5835 0.7715 0.5205 0.257 Uiso 1 1 calc R U . . .
H19B H 0.5158 0.7837 0.4699 0.257 Uiso 1 1 calc R U . . .
H19C H 0.6241 0.8279 0.4877 0.257 Uiso 1 1 calc R U . . .
C68 C 0.7526(16) 0.9457(16) 0.2519(8) 0.161(8) Uani 1 1 d . . . . .
H68A H 0.8040 0.9918 0.2674 0.241 Uiso 1 1 calc R U . . .
H68B H 0.7081 0.9480 0.2781 0.241 Uiso 1 1 calc R U . . .
H68C H 0.7170 0.9506 0.2183 0.241 Uiso 1 1 calc R U . . .
C80 C 0.063(2) 0.8893(19) 0.6068(11) 0.31(2) Uani 1 1 d D . . . .
H80A H 0.0870 0.8892 0.6437 0.464 Uiso 1 1 calc R U . . .
H80B H -0.0050 0.8659 0.5966 0.464 Uiso 1 1 calc R U . . .
H80C H 0.0681 0.9467 0.6058 0.464 Uiso 1 1 calc R U . . .
C72 C 1.013(2) 1.1042(17) 0.1870(12) 0.216(12) Uani 1 1 d . . . . .
H72A H 0.9665 1.0924 0.2089 0.324 Uiso 1 1 calc R U . . .
H72B H 1.0324 1.1645 0.1989 0.324 Uiso 1 1 calc R U . . .
H72C H 1.0706 1.0748 0.1918 0.324 Uiso 1 1 calc R U . . .
C88 C 0.6887(17) 0.726(2) 0.7049(12) 0.245(14) Uani 1 1 d . . . . .
H88A H 0.6538 0.7132 0.7320 0.367 Uiso 1 1 calc R U . . .
H88B H 0.7430 0.7684 0.7235 0.367 Uiso 1 1 calc R U . . .
H88C H 0.7131 0.6749 0.6833 0.367 Uiso 1 1 calc R U . . .
C59 C 0.9105(16) 0.9264(15) 0.4593(10) 0.181(9) Uani 1 1 d . . . . .
H59A H 0.9016 0.9169 0.4935 0.271 Uiso 1 1 calc R U . . .
H59B H 0.8962 0.9832 0.4613 0.271 Uiso 1 1 calc R U . . .
H59C H 0.9774 0.9195 0.4533 0.271 Uiso 1 1 calc R U . . .
C27 C 0.4908(11) 0.9674(14) 0.1074(9) 0.109(6) Uani 1 1 d . . . . .
C47 C 0.0768(11) 0.4139(13) 0.3360(9) 0.114(6) Uani 1 1 d . . . . .
C83 C 0.2728(17) 0.7881(15) 0.7690(8) 0.178(10) Uani 1 1 d D . . . .
H83A H 0.2036 0.7663 0.7591 0.214 Uiso 1 1 calc R U . . .
H83B H 0.3103 0.7453 0.7784 0.214 Uiso 1 1 calc R U . . .
C29 C 0.4283(15) 1.0375(12) 0.2000(7) 0.141(6) Uani 1 1 d . . . . .
H29A H 0.4784 1.0846 0.2160 0.212 Uiso 1 1 calc R U . . .
H29B H 0.4106 1.0161 0.2286 0.212 Uiso 1 1 calc R U . . .
H29C H 0.3711 1.0561 0.1829 0.212 Uiso 1 1 calc R U . . .
C49 C -0.0076(18) 0.4644(19) 0.4164(12) 0.213(12) Uani 1 1 d . . . . .
H49A H 0.0211 0.4815 0.4549 0.320 Uiso 1 1 calc R U . . .
H49B H -0.0283 0.4043 0.4035 0.320 Uiso 1 1 calc R U . . .
H49C H -0.0637 0.4953 0.4121 0.320 Uiso 1 1 calc R U . . .
C52 C 0.3917(12) 1.0136(10) 0.3445(7) 0.111(5) Uani 1 1 d . . . . .
H52A H 0.3417 1.0110 0.3134 0.133 Uiso 1 1 calc R U . . .
H52B H 0.4366 1.0645 0.3525 0.133 Uiso 1 1 calc R U . . .
C84 C 0.288(3) 0.8718(18) 0.8183(12) 0.66(8) Uani 1 1 d D . . . .
H84A H 0.2625 0.8620 0.8492 0.994 Uiso 1 1 calc R U . . .
H84B H 0.2528 0.9143 0.8076 0.994 Uiso 1 1 calc R U . . .
H84C H 0.3567 0.8911 0.8286 0.994 Uiso 1 1 calc R U . . .
C7 C -0.081(2) 0.329(2) 0.1486(11) 0.234(15) Uani 1 1 d . . . . .
H7A H -0.1462 0.3285 0.1578 0.350 Uiso 1 1 calc R U . . .
H7B H -0.0438 0.2923 0.1642 0.350 Uiso 1 1 calc R U . . .
H7C H -0.0843 0.3095 0.1090 0.350 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br4 C37 1.939(16) . ?
Br1 C8 2.03(3) . ?
Br6 C57 2.01(3) . ?
Br3 C27 1.984(18) . ?
Br2 C17 1.928(15) . ?
Br5 C47 1.901(19) . ?
S1 O10 1.438(9) . ?
S1 O7 1.470(8) . ?
S1 O9 1.489(10) . ?
S1 O8 1.501(9) . ?
O3 C23 1.229(14) . ?
O2 C13 1.209(15) . ?
N15 C73 1.511(14) . ?
N15 C61 1.529(15) . ?
N15 C69 1.543(16) . ?
N15 C65 1.551(13) . ?
O5 C43 1.236(15) . ?
O4 C33 1.196(15) . ?
N4 C13 1.332(16) . ?
N4 C12 1.471(16) . ?
N4 H4N 0.8600 . ?
N8 C51 1.433(17) . ?
N8 C41 1.461(16) . ?
N8 C31 1.473(16) . ?
N12 C43 1.394(18) . ?
N12 C44 1.402(18) . ?
N12 H12N 0.8600 . ?
N1 C21 1.464(17) . ?
N1 C1 1.461(15) . ?
N1 C11 1.487(15) . ?
N5 C13 1.377(16) . ?
N5 C14 1.399(17) . ?
N5 H5N 0.8600 . ?
N9 C33 1.360(16) . ?
N9 C32 1.449(15) . ?
N9 H9N 0.8600 . ?
N14 C53 1.355(19) . ?
N14 C54 1.42(2) . ?
N14 H14 0.8600 . ?
N16 C85 1.509(16) . ?
N16 C77 1.532(15) . ?
N16 C81 1.539(15) . ?
N16 C89 1.530(17) . ?
N13 C53 1.386(17) . ?
N13 C52 1.465(17) . ?
N13 H13N 0.8600 . ?
O1 C3 1.236(18) . ?
N6 C23 1.332(16) . ?
N6 C22 1.434(17) . ?
N6 H6N 0.8600 . ?
O6 C53 1.244(17) . ?
N2 C3 1.369(19) . ?
N2 C2 1.469(15) . ?
N2 H2N 0.8600 . ?
N11 C43 1.331(17) . ?
N11 C42 1.431(18) . ?
N11 H11N 0.8600 . ?
N7 C23 1.398(16) . ?
N7 C24 1.397(17) . ?
N7 H7N 0.8600 . ?
N10 C33 1.389(14) . ?
N10 C34 1.437(16) . ?
N10 H10N 0.8600 . ?
C44 C50 1.35(2) . ?
C44 C45 1.44(2) . ?
C73 C74 1.514(16) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C42 C41 1.535(19) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
N3 C3 1.372(18) . ?
N3 C4 1.42(2) . ?
N3 H3N 0.8600 . ?
C61 C62 1.527(18) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C1 C2 1.520(19) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C69 C70 1.48(2) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C34 C40 1.364(16) . ?
C34 C35 1.404(19) . ?
C54 C55 1.37(2) . ?
C54 C60 1.37(2) . ?
C35 C36 1.376(18) . ?
C35 H35 0.9300 . ?
C15 C16 1.39(2) . ?
C15 C14 1.392(18) . ?
C15 H15 0.9300 . ?
C62 C63 1.509(19) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C40 C38 1.42(2) . ?
C40 H40 0.9300 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C55 C56 1.42(3) . ?
C55 H55 0.9300 . ?
C14 C20 1.413(18) . ?
C74 C75 1.524(17) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C24 C25 1.418(19) . ?
C24 C30 1.427(19) . ?
C85 C86 1.548(19) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C11 C12 1.534(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C65 C66 1.478(17) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C32 C31 1.54(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C30 C28 1.42(2) . ?
C30 H30 0.9300 . ?
C18 C17 1.38(2) . ?
C18 C20 1.375(18) . ?
C18 C19 1.50(2) . ?
C38 C37 1.39(2) . ?
C38 C39 1.52(2) . ?
C77 C78 1.55(2) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C81 C82 1.56(2) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C90 C89 1.491(17) . ?
C90 C91 1.54(2) . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
C51 C52 1.526(19) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C21 C22 1.541(19) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C25 C26 1.35(2) . ?
C25 H25 0.9300 . ?
C46 C47 1.39(2) . ?
C46 C45 1.39(2) . ?
C46 H46 0.9300 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C45 H45 0.9300 . ?
C60 C58 1.49(2) . ?
C60 H60 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C89 H89A 0.9700 . ?
C89 H89B 0.9700 . ?
C50 C48 1.39(3) . ?
C50 H50 0.9300 . ?
C20 H20 0.9300 . ?
C28 C27 1.34(2) . ?
C28 C29 1.52(2) . ?
C37 C36 1.35(2) . ?
C4 C5 1.33(2) . ?
C4 C10 1.38(2) . ?
C75 C76 1.516(19) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C58 C57 1.32(3) . ?
C58 C59 1.53(3) . ?
C36 H36 0.9300 . ?
C91 C92 1.50(2) . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C57 C56 1.28(3) . ?
C56 H56 0.9300 . ?
C16 C17 1.35(2) . ?
C16 H16 0.9300 . ?
C26 C27 1.35(2) . ?
C26 H26 0.9300 . ?
C48 C47 1.39(2) . ?
C48 C49 1.54(3) . ?
C63 C64 1.54(2) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C66 C67 1.487(19) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C70 C71 1.58(2) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C10 C9 1.40(2) . ?
C10 H10 0.9300 . ?
C5 C6 1.49(3) . ?
C5 H5 0.9300 . ?
C6 C8 1.41(3) . ?
C6 C7 1.43(4) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C9 C8 1.23(3) . ?
C9 H9 0.9300 . ?
C67 C68 1.45(2) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C78 C79 1.50(2) . ?
C78 H78A 0.9700 . ?
C78 H78B 0.9700 . ?
C86 C87 1.54(2) . ?
C86 H86A 0.9700 . ?
C86 H86B 0.9700 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C92 H92A 0.9600 . ?
C92 H92B 0.9600 . ?
C92 H92C 0.9600 . ?
C82 C83 1.59(2) . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C87 C88 1.41(3) . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C79 C80 1.5399(12) . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C71 C72 1.55(3) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C80 H80A 0.9609 . ?
C80 H80B 0.9608 . ?
C80 H80C 0.9609 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C83 C84 1.5402(12) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C84 H84A 0.9985 . ?
C84 H84B 0.9974 . ?
C84 H84C 0.9961 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 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
O10 S1 O7 110.1(5) . . ?
O10 S1 O9 111.1(6) . . ?
O7 S1 O9 110.9(6) . . ?
O10 S1 O8 107.5(6) . . ?
O7 S1 O8 108.4(5) . . ?
O9 S1 O8 108.8(5) . . ?
C73 N15 C61 111.5(9) . . ?
C73 N15 C69 112.3(10) . . ?
C61 N15 C69 108.0(10) . . ?
C73 N15 C65 106.7(8) . . ?
C61 N15 C65 109.9(9) . . ?
C69 N15 C65 108.4(9) . . ?
C13 N4 C12 120.2(12) . . ?
C13 N4 H4N 119.9 . . ?
C12 N4 H4N 120.0 . . ?
C51 N8 C41 113.5(11) . . ?
C51 N8 C31 110.3(12) . . ?
C41 N8 C31 115.1(11) . . ?
C43 N12 C44 128.0(13) . . ?
C43 N12 H12N 116.0 . . ?
C44 N12 H12N 116.0 . . ?
C21 N1 C1 112.2(10) . . ?
C21 N1 C11 111.8(10) . . ?
C1 N1 C11 113.3(11) . . ?
C13 N5 C14 129.9(12) . . ?
C13 N5 H5N 115.0 . . ?
C14 N5 H5N 115.1 . . ?
C33 N9 C32 120.6(11) . . ?
C33 N9 H9N 119.7 . . ?
C32 N9 H9N 119.7 . . ?
C53 N14 C54 124.8(14) . . ?
C53 N14 H14 117.6 . . ?
C54 N14 H14 117.6 . . ?
C85 N16 C77 105.0(10) . . ?
C85 N16 C81 112.8(10) . . ?
C77 N16 C81 112.5(9) . . ?
C85 N16 C89 112.5(9) . . ?
C77 N16 C89 110.1(9) . . ?
C81 N16 C89 104.1(11) . . ?
C53 N13 C52 121.4(14) . . ?
C53 N13 H13N 119.3 . . ?
C52 N13 H13N 119.3 . . ?
C23 N6 C22 120.4(11) . . ?
C23 N6 H6N 119.8 . . ?
C22 N6 H6N 119.8 . . ?
C3 N2 C2 122.2(14) . . ?
C3 N2 H2N 118.9 . . ?
C2 N2 H2N 119.0 . . ?
O2 C13 N4 126.6(14) . . ?
O2 C13 N5 121.5(14) . . ?
N4 C13 N5 111.8(14) . . ?
C43 N11 C42 122.3(13) . . ?
C43 N11 H11N 118.9 . . ?
C42 N11 H11N 118.8 . . ?
C23 N7 C24 128.4(12) . . ?
C23 N7 H7N 115.8 . . ?
C24 N7 H7N 115.8 . . ?
C33 N10 C34 125.8(11) . . ?
C33 N10 H10N 117.1 . . ?
C34 N10 H10N 117.2 . . ?
C50 C44 N12 125.0(18) . . ?
C50 C44 C45 118(2) . . ?
N12 C44 C45 117.2(14) . . ?
O3 C23 N6 125.0(13) . . ?
O3 C23 N7 121.6(15) . . ?
N6 C23 N7 113.4(12) . . ?
O5 C43 N11 124.6(16) . . ?
O5 C43 N12 121.6(16) . . ?
N11 C43 N12 113.8(14) . . ?
C74 C73 N15 117.0(10) . . ?
C74 C73 H73A 108.0 . . ?
N15 C73 H73A 108.0 . . ?
C74 C73 H73B 108.0 . . ?
N15 C73 H73B 108.1 . . ?
H73A C73 H73B 107.3 . . ?
N11 C42 C41 112.5(12) . . ?
N11 C42 H42A 109.1 . . ?
C41 C42 H42A 109.1 . . ?
N11 C42 H42B 109.1 . . ?
C41 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?
C3 N3 C4 127.8(16) . . ?
C3 N3 H3N 116.1 . . ?
C4 N3 H3N 116.2 . . ?
N15 C61 C62 115.3(10) . . ?
N15 C61 H61A 108.5 . . ?
C62 C61 H61A 108.4 . . ?
N15 C61 H61B 108.4 . . ?
C62 C61 H61B 108.5 . . ?
H61A C61 H61B 107.5 . . ?
N1 C1 C2 112.3(11) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
C70 C69 N15 115.9(11) . . ?
C70 C69 H69A 108.3 . . ?
N15 C69 H69A 108.3 . . ?
C70 C69 H69B 108.4 . . ?
N15 C69 H69B 108.2 . . ?
H69A C69 H69B 107.4 . . ?
C40 C34 C35 119.2(12) . . ?
C40 C34 N10 116.1(14) . . ?
C35 C34 N10 124.6(12) . . ?
C55 C54 C60 118.9(17) . . ?
C55 C54 N14 111.1(16) . . ?
C60 C54 N14 130.0(16) . . ?
C36 C35 C34 120.3(13) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.8 . . ?
O4 C33 N9 125.7(12) . . ?
O4 C33 N10 123.1(12) . . ?
N9 C33 N10 111.1(13) . . ?
C16 C15 C14 119.5(14) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.3 . . ?
C63 C62 C61 110.9(12) . . ?
C63 C62 H62A 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C63 C62 H62B 109.4 . . ?
C61 C62 H62B 109.4 . . ?
H62A C62 H62B 108.1 . . ?
O6 C53 N14 125.9(15) . . ?
O6 C53 N13 120.1(17) . . ?
N14 C53 N13 113.9(16) . . ?
C34 C40 C38 121.4(16) . . ?
C34 C40 H40 119.3 . . ?
C38 C40 H40 119.3 . . ?
N8 C41 C42 112.4(10) . . ?
N8 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
N8 C41 H41B 109.2 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C54 C55 C56 126.7(18) . . ?
C54 C55 H55 116.6 . . ?
C56 C55 H55 116.6 . . ?
C15 C14 N5 123.5(14) . . ?
C15 C14 C20 118.1(14) . . ?
N5 C14 C20 118.5(13) . . ?
C73 C74 C75 110.0(11) . . ?
C73 C74 H74A 109.7 . . ?
C75 C74 H74A 109.6 . . ?
C73 C74 H74B 109.7 . . ?
C75 C74 H74B 109.7 . . ?
H74A C74 H74B 108.2 . . ?
N7 C24 C25 125.2(14) . . ?
N7 C24 C30 118.1(14) . . ?
C25 C24 C30 116.6(17) . . ?
N16 C85 C86 112.8(12) . . ?
N16 C85 H85A 109.0 . . ?
C86 C85 H85A 108.9 . . ?
N16 C85 H85B 109.0 . . ?
C86 C85 H85B 109.1 . . ?
H85A C85 H85B 107.8 . . ?
N1 C11 C12 111.4(10) . . ?
N1 C11 H11A 109.4 . . ?
C12 C11 H11A 109.3 . . ?
N1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C66 C65 N15 119.0(10) . . ?
C66 C65 H65A 107.5 . . ?
N15 C65 H65A 107.6 . . ?
C66 C65 H65B 107.6 . . ?
N15 C65 H65B 107.6 . . ?
H65A C65 H65B 107.0 . . ?
N9 C32 C31 111.9(11) . . ?
N9 C32 H32A 109.2 . . ?
C31 C32 H32A 109.2 . . ?
N9 C32 H32B 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?
N4 C12 C11 110.4(12) . . ?
N4 C12 H12A 109.6 . . ?
C11 C12 H12A 109.5 . . ?
N4 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C24 C30 C28 120.1(14) . . ?
C24 C30 H30 120.0 . . ?
C28 C30 H30 119.9 . . ?
C17 C18 C20 118.2(13) . . ?
C17 C18 C19 121.9(17) . . ?
C20 C18 C19 119.8(17) . . ?
C37 C38 C40 116.2(14) . . ?
C37 C38 C39 123.9(16) . . ?
C40 C38 C39 119.8(19) . . ?
N16 C77 C78 114.5(12) . . ?
N16 C77 H77A 108.6 . . ?
C78 C77 H77A 108.6 . . ?
N16 C77 H77B 108.7 . . ?
C78 C77 H77B 108.6 . . ?
H77A C77 H77B 107.6 . . ?
N8 C31 C32 109.3(12) . . ?
N8 C31 H31A 109.8 . . ?
C32 C31 H31A 109.8 . . ?
N8 C31 H31B 109.8 . . ?
C32 C31 H31B 109.8 . . ?
H31A C31 H31B 108.3 . . ?
N16 C81 C82 110.9(13) . . ?
N16 C81 H81A 109.5 . . ?
C82 C81 H81A 109.4 . . ?
N16 C81 H81B 109.4 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 108.0 . . ?
C89 C90 C91 112.0(13) . . ?
C89 C90 H90A 109.3 . . ?
C91 C90 H90A 109.3 . . ?
C89 C90 H90B 109.1 . . ?
C91 C90 H90B 109.2 . . ?
H90A C90 H90B 107.9 . . ?
N8 C51 C52 114.9(12) . . ?
N8 C51 H51A 108.5 . . ?
C52 C51 H51A 108.4 . . ?
N8 C51 H51B 108.6 . . ?
C52 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
N1 C21 C22 112.5(10) . . ?
N1 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
N1 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C26 C25 C24 122.1(16) . . ?
C26 C25 H25 118.8 . . ?
C24 C25 H25 119.1 . . ?
C47 C46 C45 121.5(18) . . ?
C47 C46 H46 119.3 . . ?
C45 C46 H46 119.2 . . ?
N2 C2 C1 112.4(10) . . ?
N2 C2 H2C 109.1 . . ?
C1 C2 H2C 109.1 . . ?
N2 C2 H2D 109.1 . . ?
C1 C2 H2D 109.2 . . ?
H2C C2 H2D 107.9 . . ?
C46 C45 C44 119.7(16) . . ?
C46 C45 H45 120.2 . . ?
C44 C45 H45 120.1 . . ?
C54 C60 C58 113.9(17) . . ?
C54 C60 H60 123.1 . . ?
C58 C60 H60 123.0 . . ?
N6 C22 C21 113.0(12) . . ?
N6 C22 H22A 109.0 . . ?
C21 C22 H22A 109.0 . . ?
N6 C22 H22B 109.0 . . ?
C21 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C90 C89 N16 115.8(12) . . ?
C90 C89 H89A 108.3 . . ?
N16 C89 H89A 108.3 . . ?
C90 C89 H89B 108.4 . . ?
N16 C89 H89B 108.3 . . ?
H89A C89 H89B 107.4 . . ?
C44 C50 C48 122.4(19) . . ?
C44 C50 H50 118.7 . . ?
C48 C50 H50 118.9 . . ?
C18 C20 C14 121.8(14) . . ?
C18 C20 H20 119.1 . . ?
C14 C20 H20 119.1 . . ?
C27 C28 C30 116.8(15) . . ?
C27 C28 C29 129(2) . . ?
C30 C28 C29 114.5(16) . . ?
C36 C37 C38 123.6(14) . . ?
C36 C37 Br4 117.8(16) . . ?
C38 C37 Br4 118.6(14) . . ?
C5 C4 C10 120.6(18) . . ?
C5 C4 N3 124.2(18) . . ?
C10 C4 N3 115.3(19) . . ?
C74 C75 C76 113.1(13) . . ?
C74 C75 H75A 109.0 . . ?
C76 C75 H75A 109.0 . . ?
C74 C75 H75B 109.0 . . ?
C76 C75 H75B 108.9 . . ?
H75A C75 H75B 107.8 . . ?
C57 C58 C60 119.8(17) . . ?
C57 C58 C59 132(2) . . ?
C60 C58 C59 108(2) . . ?
O1 C3 N2 121.5(17) . . ?
O1 C3 N3 126.2(16) . . ?
N2 C3 N3 112.2(17) . . ?
C37 C36 C35 119.2(16) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C92 C91 C90 116.1(15) . . ?
C92 C91 H91A 108.3 . . ?
C90 C91 H91A 108.2 . . ?
C92 C91 H91B 108.2 . . ?
C90 C91 H91B 108.3 . . ?
H91A C91 H91B 107.4 . . ?
C56 C57 C58 129(3) . . ?
C56 C57 Br6 125.0(19) . . ?
C58 C57 Br6 106(3) . . ?
C57 C56 C55 111(3) . . ?
C57 C56 H56 124.3 . . ?
C55 C56 H56 124.3 . . ?
C17 C16 C15 120.8(14) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C25 C26 C27 118.2(17) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 120.8 . . ?
C47 C48 C50 120.7(16) . . ?
C47 C48 C49 112(2) . . ?
C50 C48 C49 127(2) . . ?
C16 C17 C18 121.6(14) . . ?
C16 C17 Br2 118.5(16) . . ?
C18 C17 Br2 119.8(15) . . ?
C62 C63 C64 112.1(14) . . ?
C62 C63 H63A 109.1 . . ?
C64 C63 H63A 109.2 . . ?
C62 C63 H63B 109.2 . . ?
C64 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C67 C66 C65 113.0(12) . . ?
C67 C66 H66A 108.9 . . ?
C65 C66 H66A 109.0 . . ?
C67 C66 H66B 109.0 . . ?
C65 C66 H66B 109.0 . . ?
H66A C66 H66B 107.8 . . ?
C69 C70 C71 109.5(13) . . ?
C69 C70 H70A 109.9 . . ?
C71 C70 H70A 109.8 . . ?
C69 C70 H70B 109.7 . . ?
C71 C70 H70B 109.7 . . ?
H70A C70 H70B 108.2 . . ?
C4 C10 C9 124(2) . . ?
C4 C10 H10 118.0 . . ?
C9 C10 H10 117.8 . . ?
C4 C5 C6 117.0(18) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 H5 121.5 . . ?
C8 C6 C7 133(3) . . ?
C8 C6 C5 114.1(18) . . ?
C7 C6 C5 113(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C8 C9 C10 114(2) . . ?
C8 C9 H9 122.9 . . ?
C10 C9 H9 123.1 . . ?
C68 C67 C66 116.6(16) . . ?
C68 C67 H67A 108.2 . . ?
C66 C67 H67A 108.2 . . ?
C68 C67 H67B 108.0 . . ?
C66 C67 H67B 108.1 . . ?
H67A C67 H67B 107.3 . . ?
C77 C78 C79 109.8(18) . . ?
C77 C78 H78A 109.8 . . ?
C79 C78 H78A 109.6 . . ?
C77 C78 H78B 109.8 . . ?
C79 C78 H78B 109.7 . . ?
H78A C78 H78B 108.2 . . ?
C87 C86 C85 107.7(15) . . ?
C87 C86 H86A 110.1 . . ?
C85 C86 H86A 110.2 . . ?
C87 C86 H86B 110.2 . . ?
C85 C86 H86B 110.1 . . ?
H86A C86 H86B 108.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.4 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C91 C92 H92A 109.6 . . ?
C91 C92 H92B 109.4 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.4 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C81 C82 C83 102.3(16) . . ?
C81 C82 H82A 111.2 . . ?
C83 C82 H82A 111.3 . . ?
C81 C82 H82B 111.4 . . ?
C83 C82 H82B 111.4 . . ?
H82A C82 H82B 109.2 . . ?
C9 C8 C6 130(2) . . ?
C9 C8 Br1 123.3(18) . . ?
C6 C8 Br1 107(2) . . ?
C88 C87 C86 111.1(19) . . ?
C88 C87 H87A 109.3 . . ?
C86 C87 H87A 109.4 . . ?
C88 C87 H87B 109.4 . . ?
C86 C87 H87B 109.5 . . ?
H87A C87 H87B 108.0 . . ?
C80 C79 C78 117.0(16) . . ?
C80 C79 H79A 107.6 . . ?
C78 C79 H79A 107.8 . . ?
C80 C79 H79B 108.6 . . ?
C78 C79 H79B 108.2 . . ?
H79A C79 H79B 107.3 . . ?
C75 C76 H76A 109.4 . . ?
C75 C76 H76B 109.6 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.4 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C72 C71 C70 111(2) . . ?
C72 C71 H71A 109.4 . . ?
C70 C71 H71A 109.3 . . ?
C72 C71 H71B 109.3 . . ?
C70 C71 H71B 109.3 . . ?
H71A C71 H71B 108.0 . . ?
C18 C19 H19A 109.3 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.4 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C79 C80 H80A 109.8 . . ?
C79 C80 H80B 108.9 . . ?
H80A C80 H80B 109.4 . . ?
C79 C80 H80C 109.9 . . ?
H80A C80 H80C 109.4 . . ?
H80B C80 H80C 109.4 . . ?
C71 C72 H72A 109.6 . . ?
C71 C72 H72B 109.4 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.4 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C87 C88 H88A 109.3 . . ?
C87 C88 H88B 109.6 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.4 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C28 C27 C26 126.1(19) . . ?
C28 C27 Br3 115.0(18) . . ?
C26 C27 Br3 118.8(16) . . ?
C48 C47 C46 117.8(19) . . ?
C48 C47 Br5 125.1(16) . . ?
C46 C47 Br5 117.0(18) . . ?
C84 C83 C82 106.1(19) . . ?
C84 C83 H83A 110.5 . . ?
C82 C83 H83A 110.7 . . ?
C84 C83 H83B 110.3 . . ?
C82 C83 H83B 110.6 . . ?
H83A C83 H83B 108.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.3 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N13 C52 C51 110.0(12) . . ?
N13 C52 H52A 109.6 . . ?
C51 C52 H52A 109.6 . . ?
N13 C52 H52B 109.7 . . ?
C51 C52 H52B 109.7 . . ?
H52A C52 H52B 108.2 . . ?
C83 C84 H84A 113.4 . . ?
C83 C84 H84B 113.1 . . ?
H84A C84 H84B 105.5 . . ?
C83 C84 H84C 112.7 . . ?
H84A C84 H84C 105.7 . . ?
H84B C84 H84C 105.6 . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.6 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         1.104
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.069


# start Validation Reply Form
_vrf_PLAT234_T-Br-Me-TBASO4      
;
PROBLEM: Large Hirshfeld Difference C48      --C50              0.32 Ang.  
RESPONSE: This may be due to disorder in the model.
;
_vrf_PLAT242_T-Br-Me-TBASO4      
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C83 Check   
RESPONSE: This may be due to mismatching of U(eq) values.
;
####################################################################### 
# 
# 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_Tren-Br-Me-nco_Ligand_C
_database_code_depnum_ccdc_archive 'CCDC 1840354'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 Br3 N7 O3'
_chemical_formula_sum            'C30 H36 Br3 N7 O3'
_chemical_formula_weight         782.36

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'
Cl Cl 0.1484 0.1585 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   13.5642(8)
_cell_length_b                   29.3201(14)
_cell_length_c                   17.5854(14)
_cell_angle_alpha                90
_cell_angle_beta                 109.811(8)
_cell_angle_gamma                90
_cell_volume                     6579.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2384
_cell_measurement_theta_min      3.477
_cell_measurement_theta_max      21.158

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             3152.0
_exptl_transmission_factor_min   0.372
_exptl_transmission_factor_max   0.493
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.721
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30744
_diffrn_reflns_av_unetI/netI     0.2070
_diffrn_reflns_av_R_equivalents  0.0896
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.040
_diffrn_reflns_theta_max         28.827
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15020
_reflns_number_gt                11692
_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0800P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15020
_refine_ls_number_parameters     781
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2589
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.2393
_refine_ls_wR_factor_gt          0.1410
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_restrained_S_all      0.884
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002

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
Br5 Br 0.14385(8) 0.16836(3) 0.48017(7) 0.0762(4) Uani 1 1 d . . . . .
Br1 Br 0.10966(8) 0.45151(4) 0.99525(7) 0.0820(4) Uani 1 1 d . . . . .
Br4 Br -0.30702(9) 0.22338(4) 0.58777(7) 0.0883(4) Uani 1 1 d . . . . .
Br2 Br 0.49081(9) 0.33056(4) 0.63040(9) 0.0975(4) Uani 1 1 d . . . . .
Br6 Br 0.05751(9) 0.13288(4) 0.20781(8) 0.1012(5) Uani 1 1 d . . . . .
Br3 Br 0.59338(10) 0.37264(4) 0.91262(9) 0.1176(5) Uani 1 1 d . . . . .
O1 O 0.1725(4) 0.62592(18) 0.7611(4) 0.0562(17) Uani 1 1 d . . . . .
O4 O -0.2469(4) 0.41812(17) 0.4020(3) 0.0510(15) Uani 1 1 d . . . . .
O5 O 0.1197(4) 0.40481(18) 0.4860(3) 0.0535(16) Uani 1 1 d . . . . .
O2 O 0.5989(4) 0.56515(19) 0.6214(4) 0.0604(17) Uani 1 1 d . . . . .
O6 O 0.1700(4) 0.3682(2) 0.2315(4) 0.071(2) Uani 1 1 d . . . . .
N2 N 0.3347(4) 0.6510(2) 0.7724(4) 0.0468(18) Uani 1 1 d . . . . .
H2N H 0.4008 0.6475 0.7973 0.056 Uiso 1 1 calc R U . . .
N1 N 0.4773(4) 0.6975(2) 0.7097(4) 0.0432(17) Uani 1 1 d . . . . .
N8 N 0.0477(4) 0.4948(2) 0.3390(4) 0.0430(17) Uani 1 1 d . . . . .
O3 O 0.5350(4) 0.6088(2) 0.8647(4) 0.0659(19) Uani 1 1 d . . . . .
N10 N -0.0993(5) 0.3781(2) 0.4698(4) 0.055(2) Uani 1 1 d . . . . .
H10N H -0.0323 0.3771 0.4824 0.067 Uiso 1 1 calc R U . . .
C7 C 0.1765(6) 0.4930(3) 0.9459(5) 0.050(2) Uani 1 1 d . . . . .
N3 N 0.3167(5) 0.5868(2) 0.8373(5) 0.059(2) Uani 1 1 d . . . . .
H3N H 0.3828 0.5833 0.8470 0.071 Uiso 1 1 calc R U . . .
N6 N 0.6565(5) 0.6450(3) 0.8245(4) 0.059(2) Uani 1 1 d . . . . .
H6N H 0.7070 0.6414 0.8059 0.070 Uiso 1 1 calc R U . . .
N9 N -0.0874(4) 0.4443(2) 0.4066(4) 0.0437(17) Uani 1 1 d . . . . .
H9N H -0.0207 0.4416 0.4298 0.052 Uiso 1 1 calc R U . . .
C3 C 0.2680(6) 0.6219(3) 0.7880(5) 0.048(2) Uani 1 1 d . . . . .
N5 N 0.4459(5) 0.5357(2) 0.6304(4) 0.054(2) Uani 1 1 d . . . . .
H5N H 0.3873 0.5439 0.6350 0.065 Uiso 1 1 calc R U . . .
C34 C -0.1474(5) 0.3426(3) 0.4982(5) 0.045(2) Uani 1 1 d . . . . .
N11 N 0.2388(5) 0.4450(2) 0.4479(4) 0.054(2) Uani 1 1 d . . . . .
H11N H 0.2900 0.4431 0.4297 0.064 Uiso 1 1 calc R U . . .
C8 C 0.2468(6) 0.4776(3) 0.9100(5) 0.052(2) Uani 1 1 d . . . . .
N13 N 0.0377(5) 0.4124(2) 0.2393(5) 0.057(2) Uani 1 1 d . . . . .
H13N H -0.0214 0.4130 0.2474 0.068 Uiso 1 1 calc R U . . .
N14 N 0.0212(5) 0.3363(2) 0.2436(5) 0.065(2) Uani 1 1 d . . . . .
H14N H -0.0349 0.3434 0.2533 0.078 Uiso 1 1 calc R U . . .
C33 C -0.1504(6) 0.4140(2) 0.4240(5) 0.041(2) Uani 1 1 d . . . . .
C43 C 0.1951(6) 0.4062(3) 0.4614(5) 0.045(2) Uani 1 1 d . . . . .
N4 N 0.4631(5) 0.6110(2) 0.6148(5) 0.058(2) Uani 1 1 d . . . . .
H4N H 0.4001 0.6128 0.6156 0.069 Uiso 1 1 calc R U . . .
C37 C -0.2392(6) 0.2717(3) 0.5519(5) 0.053(2) Uani 1 1 d . . . . .
C14 C 0.4633(6) 0.4888(3) 0.6326(5) 0.047(2) Uani 1 1 d . . . . .
N12 N 0.2383(5) 0.3674(2) 0.4424(5) 0.059(2) Uani 1 1 d . . . . .
H12N H 0.2855 0.3715 0.4205 0.071 Uiso 1 1 calc R U . . .
C4 C 0.2657(6) 0.5557(3) 0.8736(5) 0.050(2) Uani 1 1 d . . . . .
C38 C -0.1679(6) 0.2604(3) 0.5139(5) 0.055(2) Uani 1 1 d . . . . .
N7 N 0.6524(5) 0.5678(3) 0.8244(5) 0.062(2) Uani 1 1 d . . . . .
H7N H 0.6970 0.5708 0.7998 0.075 Uiso 1 1 calc R U . . .
C32 C -0.1267(5) 0.4808(3) 0.3510(5) 0.044(2) Uani 1 1 d . . . . .
H32B H -0.1840 0.4958 0.3623 0.053 Uiso 1 1 calc R U . . .
H32A H -0.1531 0.4690 0.2962 0.053 Uiso 1 1 calc R U . . .
C51 C 0.0287(6) 0.4940(3) 0.2527(5) 0.045(2) Uani 1 1 d . . . . .
H51B H 0.0526 0.5225 0.2369 0.055 Uiso 1 1 calc R U . . .
H51A H -0.0460 0.4915 0.2241 0.055 Uiso 1 1 calc R U . . .
C41 C 0.1485(6) 0.5153(3) 0.3860(5) 0.048(2) Uani 1 1 d . . . . .
H41A H 0.1366 0.5464 0.3998 0.058 Uiso 1 1 calc R U . . .
H41B H 0.1928 0.5166 0.3528 0.058 Uiso 1 1 calc R U . . .
C53 C 0.0818(6) 0.3718(3) 0.2373(6) 0.055(2) Uani 1 1 d . . . . .
C5 C 0.1969(6) 0.5700(3) 0.9111(5) 0.057(2) Uani 1 1 d . . . . .
H5 H 0.1804 0.6007 0.9118 0.068 Uiso 1 1 calc R U . . .
C60 C -0.0280(6) 0.2608(3) 0.2601(5) 0.052(2) Uani 1 1 d . . . . .
H60 H -0.0759 0.2735 0.2814 0.062 Uiso 1 1 calc R U . . .
C1 C 0.3898(5) 0.7204(3) 0.7250(5) 0.051(2) Uani 1 1 d . . . . .
H1A H 0.3656 0.7456 0.6875 0.061 Uiso 1 1 calc R U . . .
H1B H 0.4137 0.7328 0.7794 0.061 Uiso 1 1 calc R U . . .
C13 C 0.5086(6) 0.5705(3) 0.6221(5) 0.050(2) Uani 1 1 d . . . . .
C48 C 0.2449(6) 0.2422(3) 0.4304(6) 0.057(2) Uani 1 1 d . . . . .
C11 C 0.4624(6) 0.6941(3) 0.6233(5) 0.053(2) Uani 1 1 d . . . . .
H11B H 0.4907 0.7211 0.6064 0.064 Uiso 1 1 calc R U . . .
H11A H 0.3881 0.6927 0.5925 0.064 Uiso 1 1 calc R U . . .
C18 C 0.4097(6) 0.4145(3) 0.6654(6) 0.062(3) Uani 1 1 d . . . . .
C10 C 0.2901(6) 0.5099(3) 0.8728(5) 0.053(2) Uani 1 1 d . . . . .
H10 H 0.3361 0.5006 0.8469 0.063 Uiso 1 1 calc R U . . .
C12 C 0.5159(6) 0.6524(3) 0.6057(5) 0.057(2) Uani 1 1 d . . . . .
H12B H 0.5171 0.6542 0.5510 0.068 Uiso 1 1 calc R U . . .
H12A H 0.5878 0.6516 0.6423 0.068 Uiso 1 1 calc R U . . .
C44 C 0.2153(6) 0.3226(3) 0.4541(6) 0.055(2) Uani 1 1 d . . . . .
C52 C 0.0834(6) 0.4553(3) 0.2287(6) 0.057(2) Uani 1 1 d . . . . .
H52B H 0.0778 0.4588 0.1725 0.069 Uiso 1 1 calc R U . . .
H52A H 0.1571 0.4557 0.2614 0.069 Uiso 1 1 calc R U . . .
C36 C -0.2634(6) 0.3157(3) 0.5649(5) 0.060(3) Uani 1 1 d . . . . .
H36 H -0.3105 0.3217 0.5917 0.071 Uiso 1 1 calc R U . . .
C35 C -0.2168(6) 0.3511(3) 0.5378(5) 0.052(2) Uani 1 1 d . . . . .
H35 H -0.2327 0.3811 0.5465 0.062 Uiso 1 1 calc R U . . .
C2 C 0.3006(6) 0.6880(3) 0.7156(5) 0.052(2) Uani 1 1 d . . . . .
H2A H 0.2432 0.7041 0.7249 0.063 Uiso 1 1 calc R U . . .
H2B H 0.2756 0.6760 0.6610 0.063 Uiso 1 1 calc R U . . .
C6 C 0.1529(6) 0.5383(3) 0.9475(5) 0.058(2) Uani 1 1 d . . . . .
H6 H 0.1069 0.5477 0.9734 0.070 Uiso 1 1 calc R U . . .
C40 C -0.1242(6) 0.2976(3) 0.4863(5) 0.050(2) Uani 1 1 d . . . . .
H40 H -0.0776 0.2919 0.4590 0.060 Uiso 1 1 calc R U . . .
C23 C 0.6098(7) 0.6075(3) 0.8401(5) 0.056(2) Uani 1 1 d . . . . .
C21 C 0.5795(6) 0.7166(3) 0.7594(6) 0.058(3) Uani 1 1 d . . . . .
H21B H 0.5702 0.7483 0.7715 0.069 Uiso 1 1 calc R U . . .
H21A H 0.6271 0.7157 0.7289 0.069 Uiso 1 1 calc R U . . .
C58 C -0.0248(6) 0.2137(3) 0.2534(5) 0.054(2) Uani 1 1 d . . . . .
C16 C 0.5387(7) 0.4206(3) 0.6002(6) 0.070(3) Uani 1 1 d . . . . .
H16 H 0.5843 0.4066 0.5780 0.084 Uiso 1 1 calc R U . . .
C54 C 0.0376(6) 0.2896(3) 0.2363(5) 0.052(2) Uani 1 1 d . . . . .
C24 C 0.6331(6) 0.5229(3) 0.8432(6) 0.059(3) Uani 1 1 d . . . . .
C42 C 0.2047(6) 0.4897(3) 0.4622(5) 0.050(2) Uani 1 1 d . . . . .
H42B H 0.2652 0.5072 0.4940 0.060 Uiso 1 1 calc R U . . .
H42A H 0.1585 0.4866 0.4936 0.060 Uiso 1 1 calc R U . . .
C20 C 0.4053(6) 0.4618(3) 0.6659(5) 0.056(2) Uani 1 1 d . . . . .
H20 H 0.3614 0.4759 0.6896 0.067 Uiso 1 1 calc R U . . .
C47 C 0.1770(7) 0.2298(3) 0.4693(6) 0.060(3) Uani 1 1 d . . . . .
C30 C 0.6824(7) 0.4881(4) 0.8169(6) 0.069(3) Uani 1 1 d . . . . .
H30 H 0.7221 0.4954 0.7846 0.083 Uiso 1 1 calc R U . . .
C50 C 0.2602(6) 0.2882(3) 0.4227(6) 0.062(3) Uani 1 1 d . . . . .
H50 H 0.3038 0.2968 0.3942 0.074 Uiso 1 1 calc R U . . .
C22 C 0.6270(6) 0.6908(3) 0.8372(5) 0.059(3) Uani 1 1 d . . . . .
H22B H 0.6885 0.7070 0.8712 0.071 Uiso 1 1 calc R U . . .
H22A H 0.5770 0.6897 0.8656 0.071 Uiso 1 1 calc R U . . .
C31 C -0.0396(6) 0.5147(3) 0.3589(5) 0.055(2) Uani 1 1 d . . . . .
H31A H -0.0676 0.5403 0.3234 0.066 Uiso 1 1 calc R U . . .
H31B H -0.0136 0.5261 0.4139 0.066 Uiso 1 1 calc R U . . .
C25 C 0.5728(6) 0.5126(4) 0.8915(6) 0.064(3) Uani 1 1 d . . . . .
H25 H 0.5409 0.5355 0.9115 0.077 Uiso 1 1 calc R U . . .
C15 C 0.5310(6) 0.4674(3) 0.6000(5) 0.059(3) Uani 1 1 d . . . . .
H15 H 0.5716 0.4849 0.5778 0.071 Uiso 1 1 calc R U . . .
C59 C -0.0990(7) 0.1854(3) 0.2791(6) 0.088(3) Uani 1 1 d . . . . .
H59A H -0.1323 0.1636 0.2376 0.132 Uiso 1 1 calc R U . . .
H59C H -0.1512 0.2047 0.2879 0.132 Uiso 1 1 calc R U . . .
H59B H -0.0614 0.1697 0.3282 0.132 Uiso 1 1 calc R U . . .
C57 C 0.0473(8) 0.1973(3) 0.2222(6) 0.066(3) Uani 1 1 d . . . . .
C17 C 0.4793(7) 0.3946(3) 0.6330(6) 0.068(3) Uani 1 1 d . . . . .
C9 C 0.2748(7) 0.4283(3) 0.9088(6) 0.071(3) Uani 1 1 d . . . . .
H9B H 0.2138 0.4114 0.8778 0.106 Uiso 1 1 calc R U . . .
H9A H 0.3003 0.4168 0.9631 0.106 Uiso 1 1 calc R U . . .
H9C H 0.3281 0.4252 0.8846 0.106 Uiso 1 1 calc R U . . .
C39 C -0.1395(7) 0.2127(3) 0.5008(7) 0.087(3) Uani 1 1 d . . . . .
H39C H -0.1149 0.1970 0.5517 0.131 Uiso 1 1 calc R U . . .
H39A H -0.0852 0.2130 0.4772 0.131 Uiso 1 1 calc R U . . .
H39B H -0.2000 0.1973 0.4652 0.131 Uiso 1 1 calc R U . . .
C45 C 0.1533(6) 0.3083(3) 0.4982(6) 0.063(3) Uani 1 1 d . . . . .
H45 H 0.1245 0.3298 0.5235 0.075 Uiso 1 1 calc R U . . .
C28 C 0.6753(7) 0.4435(4) 0.8368(7) 0.074(3) Uani 1 1 d . . . . .
C55 C 0.1103(7) 0.2706(3) 0.2072(6) 0.071(3) Uani 1 1 d . . . . .
H55 H 0.1565 0.2893 0.1927 0.085 Uiso 1 1 calc R U . . .
C49 C 0.3004(8) 0.2070(3) 0.3963(7) 0.088(3) Uani 1 1 d . . . . .
H49C H 0.3329 0.2218 0.3622 0.131 Uiso 1 1 calc R U . . .
H49B H 0.2505 0.1850 0.3653 0.131 Uiso 1 1 calc R U . . .
H49A H 0.3530 0.1919 0.4399 0.131 Uiso 1 1 calc R U . . .
C46 C 0.1340(6) 0.2623(3) 0.5050(6) 0.062(3) Uani 1 1 d . . . . .
H46 H 0.0913 0.2533 0.5340 0.074 Uiso 1 1 calc R U . . .
C27 C 0.6108(8) 0.4334(4) 0.8818(7) 0.077(3) Uani 1 1 d . . . . .
C56 C 0.1147(8) 0.2243(4) 0.1996(7) 0.084(3) Uani 1 1 d . . . . .
H56 H 0.1632 0.2114 0.1793 0.101 Uiso 1 1 calc R U . . .
C19 C 0.3424(7) 0.3874(3) 0.7005(6) 0.084(3) Uani 1 1 d . . . . .
H19B H 0.2922 0.3703 0.6584 0.125 Uiso 1 1 calc R U . . .
H19A H 0.3064 0.4076 0.7250 0.125 Uiso 1 1 calc R U . . .
H19C H 0.3854 0.3668 0.7406 0.125 Uiso 1 1 calc R U . . .
C26 C 0.5621(7) 0.4670(4) 0.9088(6) 0.078(3) Uani 1 1 d . . . . .
H26 H 0.5207 0.4593 0.9396 0.093 Uiso 1 1 calc R U . . .
C29 C 0.7324(9) 0.4066(4) 0.8086(8) 0.117(5) Uani 1 1 d . . . . .
H29C H 0.7569 0.4186 0.7674 0.175 Uiso 1 1 calc R U . . .
H29B H 0.6856 0.3816 0.7871 0.175 Uiso 1 1 calc R U . . .
H29A H 0.7910 0.3962 0.8535 0.175 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br5 C47 1.882(9) . ?
Br1 C7 1.896(8) . ?
Br4 C37 1.909(8) . ?
Br2 C17 1.885(9) . ?
Br6 C57 1.916(9) . ?
Br3 C27 1.899(10) . ?
O1 C3 1.224(8) . ?
O4 C33 1.238(8) . ?
O5 C43 1.239(8) . ?
O2 C13 1.240(8) . ?
O6 C53 1.240(8) . ?
N2 C3 1.340(9) . ?
N2 C2 1.439(9) . ?
N1 C1 1.467(9) . ?
N1 C11 1.467(9) . ?
N1 C21 1.477(9) . ?
N8 C51 1.450(9) . ?
N8 C31 1.465(9) . ?
N8 C41 1.466(8) . ?
O3 C23 1.232(9) . ?
N10 C33 1.363(9) . ?
N10 C34 1.407(9) . ?
C7 C6 1.368(11) . ?
C7 C8 1.384(10) . ?
N3 C3 1.363(10) . ?
N3 C4 1.422(9) . ?
N6 C23 1.342(10) . ?
N6 C22 1.441(10) . ?
N9 C33 1.339(9) . ?
N9 C32 1.427(9) . ?
N5 C13 1.368(10) . ?
N5 C14 1.393(10) . ?
C34 C35 1.370(10) . ?
C34 C40 1.389(11) . ?
N11 C43 1.341(9) . ?
N11 C42 1.439(9) . ?
C8 C10 1.389(11) . ?
C8 C9 1.496(11) . ?
N13 C53 1.339(10) . ?
N13 C52 1.442(9) . ?
N14 C53 1.353(10) . ?
N14 C54 1.400(10) . ?
C43 N12 1.371(9) . ?
N4 C13 1.326(10) . ?
N4 C12 1.444(9) . ?
C37 C36 1.369(11) . ?
C37 C38 1.390(11) . ?
C14 C20 1.378(11) . ?
C14 C15 1.386(10) . ?
N12 C44 1.383(10) . ?
C4 C5 1.378(11) . ?
C4 C10 1.383(11) . ?
C38 C40 1.403(11) . ?
C38 C39 1.491(12) . ?
N7 C23 1.369(10) . ?
N7 C24 1.404(10) . ?
C32 C31 1.513(9) . ?
C51 C52 1.493(10) . ?
C41 C42 1.499(10) . ?
C5 C6 1.373(11) . ?
C60 C58 1.388(11) . ?
C60 C54 1.391(11) . ?
C1 C2 1.503(10) . ?
C48 C47 1.370(11) . ?
C48 C50 1.378(11) . ?
C48 C49 1.514(11) . ?
C11 C12 1.506(10) . ?
C18 C17 1.387(12) . ?
C18 C20 1.390(12) . ?
C18 C19 1.491(11) . ?
C44 C50 1.387(11) . ?
C44 C45 1.388(11) . ?
C36 C35 1.382(11) . ?
C21 C22 1.505(11) . ?
C58 C57 1.362(11) . ?
C58 C59 1.487(12) . ?
C16 C17 1.371(12) . ?
C16 C15 1.377(12) . ?
C54 C55 1.373(11) . ?
C24 C30 1.383(12) . ?
C24 C25 1.398(12) . ?
C47 C46 1.375(12) . ?
C30 C28 1.366(13) . ?
C25 C26 1.390(13) . ?
C57 C56 1.368(13) . ?
C45 C46 1.387(12) . ?
C28 C27 1.397(14) . ?
C28 C29 1.508(13) . ?
C55 C56 1.367(12) . ?
C27 C26 1.359(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
C3 N2 C2 122.8(7) . . ?
C1 N1 C11 112.7(6) . . ?
C1 N1 C21 111.8(6) . . ?
C11 N1 C21 114.3(6) . . ?
C51 N8 C31 112.6(6) . . ?
C51 N8 C41 113.4(6) . . ?
C31 N8 C41 112.1(6) . . ?
C33 N10 C34 125.2(6) . . ?
C6 C7 C8 121.9(8) . . ?
C6 C7 Br1 117.5(6) . . ?
C8 C7 Br1 120.6(7) . . ?
C3 N3 C4 124.4(7) . . ?
C23 N6 C22 123.8(7) . . ?
C33 N9 C32 122.3(6) . . ?
O1 C3 N2 124.0(8) . . ?
O1 C3 N3 122.7(7) . . ?
N2 C3 N3 113.4(7) . . ?
C13 N5 C14 129.3(7) . . ?
C35 C34 C40 118.7(8) . . ?
C35 C34 N10 121.7(8) . . ?
C40 C34 N10 119.6(7) . . ?
C43 N11 C42 123.6(7) . . ?
C7 C8 C10 117.3(8) . . ?
C7 C8 C9 122.6(8) . . ?
C10 C8 C9 120.1(8) . . ?
C53 N13 C52 123.9(7) . . ?
C53 N14 C54 128.7(7) . . ?
O4 C33 N9 123.6(7) . . ?
O4 C33 N10 122.2(7) . . ?
N9 C33 N10 114.2(7) . . ?
O5 C43 N11 123.8(8) . . ?
O5 C43 N12 121.9(8) . . ?
N11 C43 N12 114.2(7) . . ?
C13 N4 C12 122.1(7) . . ?
C36 C37 C38 123.3(8) . . ?
C36 C37 Br4 118.4(7) . . ?
C38 C37 Br4 118.3(7) . . ?
C20 C14 C15 118.1(8) . . ?
C20 C14 N5 117.5(7) . . ?
C15 C14 N5 124.3(8) . . ?
C43 N12 C44 128.0(7) . . ?
C5 C4 C10 120.3(8) . . ?
C5 C4 N3 122.1(8) . . ?
C10 C4 N3 117.6(8) . . ?
C37 C38 C40 115.2(8) . . ?
C37 C38 C39 123.8(8) . . ?
C40 C38 C39 121.0(8) . . ?
C23 N7 C24 128.7(8) . . ?
N9 C32 C31 109.2(6) . . ?
N8 C51 C52 112.3(7) . . ?
N8 C41 C42 113.1(6) . . ?
O6 C53 N13 122.0(8) . . ?
O6 C53 N14 124.8(8) . . ?
N13 C53 N14 113.2(7) . . ?
C6 C5 C4 119.2(8) . . ?
C58 C60 C54 122.5(8) . . ?
N1 C1 C2 111.1(6) . . ?
O2 C13 N4 122.8(8) . . ?
O2 C13 N5 124.0(8) . . ?
N4 C13 N5 113.2(7) . . ?
C47 C48 C50 117.2(9) . . ?
C47 C48 C49 121.8(9) . . ?
C50 C48 C49 121.1(8) . . ?
N1 C11 C12 111.1(7) . . ?
C17 C18 C20 117.3(8) . . ?
C17 C18 C19 122.9(9) . . ?
C20 C18 C19 119.7(9) . . ?
C4 C10 C8 121.0(8) . . ?
N4 C12 C11 111.5(6) . . ?
N12 C44 C50 118.7(8) . . ?
N12 C44 C45 125.5(8) . . ?
C50 C44 C45 115.8(8) . . ?
N13 C52 C51 110.5(6) . . ?
C37 C36 C35 119.1(8) . . ?
C34 C35 C36 120.8(8) . . ?
N2 C2 C1 110.0(6) . . ?
C7 C6 C5 120.3(8) . . ?
C34 C40 C38 122.8(8) . . ?
O3 C23 N6 123.3(9) . . ?
O3 C23 N7 123.5(9) . . ?
N6 C23 N7 113.2(8) . . ?
N1 C21 C22 112.0(7) . . ?
C57 C58 C60 115.7(9) . . ?
C57 C58 C59 125.3(9) . . ?
C60 C58 C59 119.0(8) . . ?
C17 C16 C15 120.0(9) . . ?
C55 C54 C60 118.6(8) . . ?
C55 C54 N14 125.9(8) . . ?
C60 C54 N14 115.4(7) . . ?
C30 C24 C25 119.6(9) . . ?
C30 C24 N7 117.6(9) . . ?
C25 C24 N7 122.7(9) . . ?
N11 C42 C41 113.4(7) . . ?
C14 C20 C18 122.6(8) . . ?
C48 C47 C46 120.4(9) . . ?
C48 C47 Br5 121.9(7) . . ?
C46 C47 Br5 117.6(7) . . ?
C28 C30 C24 122.5(10) . . ?
C48 C50 C44 124.9(9) . . ?
N6 C22 C21 112.6(8) . . ?
N8 C31 C32 112.8(6) . . ?
C26 C25 C24 117.8(10) . . ?
C16 C15 C14 120.7(9) . . ?
C58 C57 C56 123.7(9) . . ?
C58 C57 Br6 119.7(8) . . ?
C56 C57 Br6 116.6(8) . . ?
C16 C17 C18 121.2(9) . . ?
C16 C17 Br2 118.6(7) . . ?
C18 C17 Br2 120.1(7) . . ?
C46 C45 C44 120.6(9) . . ?
C30 C28 C27 117.4(10) . . ?
C30 C28 C29 120.9(11) . . ?
C27 C28 C29 121.6(11) . . ?
C56 C55 C54 120.0(9) . . ?
C47 C46 C45 120.9(9) . . ?
C26 C27 C28 121.1(10) . . ?
C26 C27 Br3 117.3(10) . . ?
C28 C27 Br3 121.5(9) . . ?
C55 C56 C57 119.4(9) . . ?
C27 C26 C25 121.5(10) . . ?

_refine_diff_density_max         0.718
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_Tren-Cl-Me-nco_TBACl
_database_code_depnum_ccdc_archive 'CCDC 1840355'
_audit_update_record             
;
2018-05-30 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H35 Cl3 N7 O3, C16 H36 N, Cl'
_chemical_formula_sum            'C46 H71 Cl4 N8 O3'
_chemical_formula_weight         925.91

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   16.6856(13)
_cell_length_b                   21.5029(18)
_cell_length_c                   14.7395(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5288.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2590
_cell_measurement_theta_min      3.727
_cell_measurement_theta_max      19.880

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_F_000             1980.0
_exptl_transmission_factor_min   0.929
_exptl_transmission_factor_max   0.953
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.268
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16340
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.961
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_point_group_measured_fraction_full 0.817
_reflns_number_total             8911
_reflns_number_gt                6419
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.570
_reflns_Friedel_fraction_max     0.619
_reflns_Friedel_fraction_full    0.619

_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       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_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)+(0.0400P)²+4.6652P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 852 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8911
_refine_ls_number_parameters     554
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1871
_refine_ls_R_factor_gt           0.0956
_refine_ls_wR_factor_ref         0.2218
_refine_ls_wR_factor_gt          0.1837
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.003

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
C24 C 0.4792(6) 0.7598(9) 0.3714(11) 0.129(6) Uani 1 1 d G . . . .
C25 C 0.4943(7) 0.7128(7) 0.3090(16) 0.197(11) Uani 1 1 d G . . . .
H25 H 0.4954 0.6715 0.3278 0.236 Uiso 1 1 calc R U . . .
C26 C 0.5077(7) 0.7275(11) 0.2184(14) 0.27(2) Uani 1 1 d G . . . .
C27 C 0.5060(8) 0.7892(13) 0.1903(10) 0.31(3) Uani 1 1 d G . . . .
C29 C 0.4910(8) 0.8362(9) 0.2527(14) 0.29(2) Uani 1 1 d G . . . .
C30 C 0.4776(7) 0.8215(8) 0.3433(13) 0.186(10) Uani 1 1 d G . . . .
H30 H 0.4675 0.8529 0.3851 0.223 Uiso 1 1 calc R U . . .
Cl4 Cl 0.50284(17) 0.86282(14) 0.6077(7) 0.0907(9) Uani 1 1 d . . . . .
Cl2 Cl 0.0624(2) 1.01609(19) 0.6823(7) 0.1330(14) Uani 1 1 d . . . . .
Cl1 Cl 0.8912(4) 1.0323(3) 0.8394(8) 0.234(3) Uani 1 1 d . . . . .
N1 N 0.4797(6) 0.7168(4) 0.7913(9) 0.084(3) Uani 1 1 d . . . . .
N5 N 0.3337(5) 0.9080(4) 0.6992(9) 0.078(2) Uani 1 1 d . . . . .
H5N H 0.3797 0.9035 0.6737 0.094 Uiso 1 1 calc R U . . .
C13 C 0.3206(7) 0.8713(5) 0.7722(10) 0.072(3) Uani 1 1 d . . . . .
N8 N 0.2222(5) 0.6049(5) 0.3996(9) 0.106(4) Uani 1 1 d D . . . .
O2 O 0.2654(5) 0.8789(4) 0.8257(9) 0.110(3) Uani 1 1 d . . . . .
C14 C 0.2837(7) 0.9519(5) 0.6591(10) 0.073(3) Uani 1 1 d . . . . .
C20 C 0.2070(7) 0.9622(5) 0.6872(10) 0.078(3) Uani 1 1 d . . . . .
H20 H 0.1862 0.9403 0.7363 0.094 Uiso 1 1 calc R U . . .
N7 N 0.4670(7) 0.7524(7) 0.4661(10) 0.113(4) Uani 1 1 d . . . . .
H7N H 0.4665 0.7856 0.4985 0.135 Uiso 1 1 calc R U . . .
N3 N 0.6616(7) 0.8945(6) 0.7326(10) 0.109(3) Uani 1 1 d . . . . .
H3N H 0.6290 0.8897 0.6880 0.131 Uiso 1 1 calc R U . . .
N6 N 0.4558(6) 0.7028(5) 0.5992(11) 0.106(3) Uani 1 1 d . . . . .
H6N H 0.4633 0.7392 0.6216 0.128 Uiso 1 1 calc R U . . .
N4 N 0.3762(5) 0.8245(5) 0.7836(9) 0.093(3) Uani 1 1 d . . . . .
H4N H 0.4146 0.8215 0.7448 0.111 Uiso 1 1 calc R U . . .
C3 C 0.6744(8) 0.8453(7) 0.7902(13) 0.097(4) Uani 1 1 d . . . . .
C19 C 0.1601(7) 1.0061(6) 0.6416(11) 0.085(3) Uani 1 1 d . . . . .
N2 N 0.6217(6) 0.7967(5) 0.7731(10) 0.110(4) Uani 1 1 d . . . . .
H2N H 0.5891 0.7999 0.7281 0.132 Uiso 1 1 calc R U . . .
C4 C 0.6988(9) 0.9512(7) 0.7432(11) 0.097(4) Uani 1 1 d . . . . .
O1 O 0.7241(6) 0.8430(4) 0.8474(11) 0.142(5) Uani 1 1 d . . . . .
O3 O 0.4451(6) 0.6483(5) 0.4692(10) 0.141(4) Uani 1 1 d . . . . .
C11 C 0.4164(13) 0.7294(9) 0.8509(15) 0.209(12) Uani 1 1 d . . . . .
H11A H 0.3780 0.6962 0.8411 0.251 Uiso 1 1 calc R U . . .
H11B H 0.4382 0.7228 0.9111 0.251 Uiso 1 1 calc R U . . .
C9 C 0.7980(9) 1.0215(9) 0.7909(14) 0.129(5) Uani 1 1 d . . . . .
C23 C 0.4557(9) 0.6962(9) 0.5113(15) 0.114(5) Uani 1 1 d . . . . .
C15 C 0.3118(8) 0.9852(6) 0.5863(12) 0.109(4) Uani 1 1 d . . . . .
H15 H 0.3636 0.9778 0.5655 0.131 Uiso 1 1 calc R U . . .
C17 C 0.1868(9) 1.0400(6) 0.5688(13) 0.103(4) Uani 1 1 d . . . . .
C21 C 0.4728(18) 0.6574(7) 0.7471(14) 0.231(14) Uani 1 1 d . . . . .
H21A H 0.5260 0.6392 0.7472 0.278 Uiso 1 1 calc R U . . .
H21B H 0.4400 0.6316 0.7862 0.278 Uiso 1 1 calc R U . . .
C10 C 0.7724(9) 0.9634(7) 0.7812(13) 0.118(5) Uani 1 1 d . . . . .
H10 H 0.8046 0.9306 0.8003 0.142 Uiso 1 1 calc R U . . .
C22 C 0.4434(11) 0.6504(8) 0.6610(15) 0.154(7) Uani 1 1 d . . . . .
H22B H 0.3862 0.6426 0.6653 0.185 Uiso 1 1 calc R U . . .
H22A H 0.4678 0.6138 0.6344 0.185 Uiso 1 1 calc R U . . .
C2 C 0.6193(10) 0.7408(6) 0.8281(15) 0.149(7) Uani 1 1 d . . . . .
H2B H 0.6549 0.7105 0.8007 0.179 Uiso 1 1 calc R U . . .
H2A H 0.6410 0.7509 0.8874 0.179 Uiso 1 1 calc R U . . .
C16 C 0.2645(10) 1.0301(7) 0.5421(13) 0.130(5) Uani 1 1 d . . . . .
H16 H 0.2860 1.0531 0.4945 0.155 Uiso 1 1 calc R U . . .
C12 C 0.3734(8) 0.7805(8) 0.8569(11) 0.122(5) Uani 1 1 d . . . . .
H12B H 0.3897 0.8020 0.9117 0.146 Uiso 1 1 calc R U . . .
H12A H 0.3179 0.7682 0.8650 0.146 Uiso 1 1 calc R U . . .
C18 C 0.1342(9) 1.0852(8) 0.5177(13) 0.160(7) Uani 1 1 d . . . . .
H18C H 0.0929 1.1004 0.5573 0.240 Uiso 1 1 calc R U . . .
H18A H 0.1101 1.0644 0.4669 0.240 Uiso 1 1 calc R U . . .
H18B H 0.1660 1.1194 0.4965 0.240 Uiso 1 1 calc R U . . .
C32 C 0.2989(13) 0.5284(12) 0.4262(15) 0.39(3) Uani 1 1 d D U . . .
H32A H 0.2519 0.5037 0.4120 0.472 Uiso 1 1 calc R U . . .
H32B H 0.3257 0.5393 0.3701 0.472 Uiso 1 1 calc R U . . .
C44 C 0.2264(12) 0.7004(9) 0.4891(15) 0.196(10) Uani 1 1 d D . . . .
H44A H 0.2677 0.7110 0.4456 0.235 Uiso 1 1 calc R U . . .
H44B H 0.2519 0.6825 0.5421 0.235 Uiso 1 1 calc R U . . .
C36 C 0.1132(10) 0.5191(8) 0.4130(14) 0.155(7) Uani 1 1 d D . . . .
H36B H 0.1499 0.4850 0.4247 0.186 Uiso 1 1 calc R U . . .
H36A H 0.1068 0.5402 0.4707 0.186 Uiso 1 1 calc R U . . .
C8 C 0.7559(17) 1.0728(8) 0.7536(19) 0.192(10) Uani 1 1 d . . . . .
C43 C 0.1691(12) 0.6546(12) 0.4482(16) 0.61(6) Uani 1 1 d D . . . .
H43A H 0.1340 0.6750 0.4051 0.728 Uiso 1 1 calc R U . . .
H43B H 0.1366 0.6353 0.4950 0.728 Uiso 1 1 calc R U . . .
C45 C 0.1805(16) 0.7577(8) 0.5155(18) 0.36(3) Uani 1 1 d D . . . .
H45A H 0.1571 0.7729 0.4595 0.428 Uiso 1 1 calc R U . . .
H45B H 0.1361 0.7428 0.5519 0.428 Uiso 1 1 calc R U . . .
C39 C 0.257(2) 0.6198(12) 0.3213(12) 0.40(3) Uani 1 1 d D . . . .
H39A H 0.2543 0.5812 0.2873 0.476 Uiso 1 1 calc R U . . .
H39B H 0.3126 0.6246 0.3378 0.476 Uiso 1 1 calc R U . . .
C1 C 0.5498(12) 0.7144(10) 0.8399(19) 0.263(17) Uani 1 1 d . . . . .
H1A H 0.5342 0.7266 0.9008 0.315 Uiso 1 1 calc R U . . .
H1B H 0.5620 0.6704 0.8437 0.315 Uiso 1 1 calc R U . . .
C37 C 0.0446(11) 0.4922(8) 0.399(2) 0.222(12) Uani 1 1 d D . . . .
H37B H 0.0469 0.4867 0.3340 0.266 Uiso 1 1 calc R U . . .
H37A H 0.0090 0.5274 0.4076 0.266 Uiso 1 1 calc R U . . .
C31 C 0.2746(15) 0.5876(13) 0.4784(12) 0.45(3) Uani 1 1 d D U . . .
H31A H 0.2453 0.5795 0.5340 0.543 Uiso 1 1 calc R U . . .
H31B H 0.3185 0.6163 0.4888 0.543 Uiso 1 1 calc R U . . .
C41 C 0.3046(14) 0.6969(13) 0.1875(13) 0.33(2) Uani 1 1 d D . . . .
H41A H 0.3299 0.7326 0.2157 0.398 Uiso 1 1 calc R U . . .
H41B H 0.3458 0.6672 0.1708 0.398 Uiso 1 1 calc R U . . .
C40 C 0.2453(14) 0.6683(9) 0.2494(13) 0.224(14) Uani 1 1 d D . . . .
H40A H 0.2042 0.6516 0.2098 0.269 Uiso 1 1 calc R U . . .
H40B H 0.2206 0.7031 0.2806 0.269 Uiso 1 1 calc R U . . .
C5 C 0.6569(10) 1.0004(8) 0.7021(17) 0.175(8) Uani 1 1 d . . . . .
H5 H 0.6074 0.9917 0.6762 0.210 Uiso 1 1 calc R U . . .
C6 C 0.6864(13) 1.0652(12) 0.697(3) 0.31(2) Uani 1 1 d . . . . .
H6 H 0.6632 1.0966 0.6629 0.368 Uiso 1 1 calc R U . . .
C46 C 0.2105(16) 0.8145(10) 0.5637(17) 0.270(13) Uani 1 1 d D . . . .
H46B H 0.2608 0.8053 0.5924 0.405 Uiso 1 1 calc R U . . .
H46A H 0.1723 0.8269 0.6089 0.405 Uiso 1 1 calc R U . . .
H46C H 0.2177 0.8476 0.5208 0.405 Uiso 1 1 calc R U . . .
C34 C 0.3865(13) 0.4287(9) 0.515(2) 0.247(13) Uani 1 1 d D . . . .
H34B H 0.4393 0.4230 0.4910 0.371 Uiso 1 1 calc R U . . .
H34A H 0.3516 0.3969 0.4925 0.371 Uiso 1 1 calc R U . . .
H34C H 0.3886 0.4261 0.5805 0.371 Uiso 1 1 calc R U . . .
C33 C 0.3544(15) 0.4930(8) 0.487(2) 0.32(2) Uani 1 1 d D . . . .
H33A H 0.3376 0.5089 0.5460 0.387 Uiso 1 1 calc R U . . .
H33B H 0.4043 0.5144 0.4751 0.387 Uiso 1 1 calc R U . . .
C38 C -0.0111(12) 0.4402(9) 0.4239(18) 0.247(12) Uani 1 1 d D . . . .
H38A H -0.0655 0.4532 0.4146 0.371 Uiso 1 1 calc R U . . .
H38C H -0.0035 0.4292 0.4864 0.371 Uiso 1 1 calc R U . . .
H38B H 0.0001 0.4047 0.3864 0.371 Uiso 1 1 calc R U . . .
C42 C 0.2575(16) 0.7160(17) 0.1070(17) 0.33(2) Uani 1 1 d D . . . .
H42B H 0.2637 0.7599 0.0975 0.501 Uiso 1 1 calc R U . . .
H42C H 0.2020 0.7065 0.1169 0.501 Uiso 1 1 calc R U . . .
H42A H 0.2764 0.6939 0.0546 0.501 Uiso 1 1 calc R U . . .
C35 C 0.1607(12) 0.5636(9) 0.3561(18) 0.42(3) Uani 1 1 d D . . . .
H35B H 0.1228 0.5904 0.3251 0.506 Uiso 1 1 calc R U . . .
H35A H 0.1879 0.5395 0.3099 0.506 Uiso 1 1 calc R U . . .
C7 C 0.7969(15) 1.1370(9) 0.777(3) 0.32(2) Uani 1 1 d . . . . .
H7C H 0.7716 1.1548 0.8292 0.486 Uiso 1 1 calc R U . . .
H7A H 0.7913 1.1647 0.7262 0.486 Uiso 1 1 calc R U . . .
H7B H 0.8528 1.1304 0.7891 0.486 Uiso 1 1 calc R U . . .
Cl3B Cl 0.5277(5) 0.7002(5) 0.1356(9) 0.154(4) Uani 0.5 1 d . . P . .
C28 C 0.5260(17) 0.803(3) 0.0866(14) 0.50(4) Uani 1 1 d . . . . .
H28C H 0.4851 0.7856 0.0487 0.753 Uiso 1 1 calc R U . . .
H28B H 0.5769 0.7854 0.0713 0.753 Uiso 1 1 calc R U . . .
H28A H 0.5280 0.8475 0.0773 0.753 Uiso 1 1 calc R U . . .
Cl3A Cl 0.5137(6) 0.8812(6) 0.1934(10) 0.174(4) Uani 0.5 1 d . . P . .


_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
C24 C25 1.3900 . ?
C24 C30 1.3900 . ?
C24 N7 1.419(15) . ?
C25 C26 1.3900 . ?
C26 C27 1.3900 . ?
C26 Cl3B 1.394(16) . ?
C27 C29 1.3900 . ?
C27 C28 1.59(2) . ?
C29 Cl3A 1.359(16) . ?
C29 C30 1.3900 . ?
Cl2 C19 1.751(12) . ?
Cl1 C9 1.727(17) . ?
N1 C1 1.372(19) . ?
N1 C11 1.400(18) . ?
N1 C21 1.438(17) . ?
N5 C13 1.352(13) . ?
N5 C14 1.392(12) . ?
C13 O2 1.223(12) . ?
C13 N4 1.379(13) . ?
N8 C39 1.33(3) . ?
N8 C31 1.5000(13) . ?
N8 C43 1.56(2) . ?
N8 C35 1.50(2) . ?
C14 C20 1.363(13) . ?
C14 C15 1.372(15) . ?
C20 C19 1.398(14) . ?
N7 C23 1.392(19) . ?
N3 C4 1.375(16) . ?
N3 C3 1.373(17) . ?
N6 C23 1.304(18) . ?
N6 C22 1.463(17) . ?
N4 C12 1.437(14) . ?
C3 O1 1.184(16) . ?
C3 N2 1.389(16) . ?
C19 C17 1.373(16) . ?
N2 C2 1.450(16) . ?
C4 C10 1.375(17) . ?
C4 C5 1.406(19) . ?
O3 C23 1.215(16) . ?
C11 C12 1.315(17) . ?
C9 C10 1.329(19) . ?
C9 C8 1.42(2) . ?
C15 C16 1.408(17) . ?
C17 C16 1.371(18) . ?
C17 C18 1.510(18) . ?
C21 C22 1.369(19) . ?
C2 C1 1.30(2) . ?
C32 C33 1.5002(14) . ?
C32 C31 1.5400(13) . ?
C44 C43 1.4997(13) . ?
C44 C45 1.5000(14) . ?
C36 C37 1.30(2) . ?
C36 C35 1.5001(13) . ?
C8 C6 1.43(4) . ?
C8 C7 1.58(3) . ?
C45 C46 1.4996(14) . ?
C39 C40 1.4995(13) . ?
C37 C38 1.4986(14) . ?
C41 C42 1.480(3) . ?
C41 C40 1.4799(15) . ?
C5 C6 1.48(2) . ?
C34 C33 1.5397(14) . ?

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
C25 C24 C30 120.0 . . ?
C25 C24 N7 126.5(15) . . ?
C30 C24 N7 113.4(15) . . ?
C24 C25 C26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 Cl3B 98.4(19) . . ?
C25 C26 Cl3B 141.5(19) . . ?
C26 C27 C29 120.0 . . ?
C26 C27 C28 118(3) . . ?
C29 C27 C28 122(3) . . ?
Cl3A C29 C30 145.6(17) . . ?
Cl3A C29 C27 92.3(18) . . ?
C30 C29 C27 120.0 . . ?
C29 C30 C24 120.0 . . ?
C1 N1 C11 108.8(17) . . ?
C1 N1 C21 105.8(16) . . ?
C11 N1 C21 113.3(15) . . ?
C13 N5 C14 129.6(10) . . ?
O2 C13 N5 123.8(11) . . ?
O2 C13 N4 121.7(11) . . ?
N5 C13 N4 114.5(10) . . ?
C39 N8 C31 119(2) . . ?
C39 N8 C43 118.6(18) . . ?
C31 N8 C43 98.3(14) . . ?
C39 N8 C35 93.9(18) . . ?
C31 N8 C35 125.6(16) . . ?
C43 N8 C35 102.2(12) . . ?
C20 C14 C15 118.3(11) . . ?
C20 C14 N5 122.9(11) . . ?
C15 C14 N5 118.7(11) . . ?
C14 C20 C19 119.3(11) . . ?
C23 N7 C24 126.0(15) . . ?
C4 N3 C3 122.8(13) . . ?
C23 N6 C22 122.4(14) . . ?
C13 N4 C12 123.4(10) . . ?
O1 C3 N3 125.5(15) . . ?
O1 C3 N2 122.8(16) . . ?
N3 C3 N2 111.7(14) . . ?
C17 C19 C20 123.5(12) . . ?
C17 C19 Cl2 120.4(11) . . ?
C20 C19 Cl2 116.1(10) . . ?
C3 N2 C2 122.7(13) . . ?
N3 C4 C10 128.2(13) . . ?
N3 C4 C5 113.2(15) . . ?
C10 C4 C5 118.4(14) . . ?
C12 C11 N1 128.0(13) . . ?
C10 C9 C8 122.1(17) . . ?
C10 C9 Cl1 117.4(15) . . ?
C8 C9 Cl1 120.1(16) . . ?
O3 C23 N6 126.8(19) . . ?
O3 C23 N7 120.8(17) . . ?
N6 C23 N7 112.4(15) . . ?
C14 C15 C16 121.8(13) . . ?
C16 C17 C19 116.7(13) . . ?
C16 C17 C18 120.4(15) . . ?
C19 C17 C18 122.8(14) . . ?
C22 C21 N1 123.0(16) . . ?
C9 C10 C4 120.7(16) . . ?
C21 C22 N6 116.3(15) . . ?
C1 C2 N2 117.4(14) . . ?
C17 C16 C15 120.3(15) . . ?
C11 C12 N4 118.8(13) . . ?
C33 C32 C31 106.4(18) . . ?
C43 C44 C45 108.6(18) . . ?
C37 C36 C35 131.5(19) . . ?
C9 C8 C6 122.4(19) . . ?
C9 C8 C7 112(2) . . ?
C6 C8 C7 125(2) . . ?
C44 C43 N8 105.8(15) . . ?
C46 C45 C44 128(2) . . ?
N8 C39 C40 137(3) . . ?
C2 C1 N1 132.2(18) . . ?
C36 C37 C38 147(2) . . ?
N8 C31 C32 88.4(14) . . ?
C42 C41 C40 105(2) . . ?
C41 C40 C39 130(2) . . ?
C4 C5 C6 124.3(19) . . ?
C8 C6 C5 110(3) . . ?
C32 C33 C34 146(2) . . ?
C36 C35 N8 120.0(18) . . ?

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.051


# start Validation Reply Form
_vrf_PLAT213_Tren-Cl-Me-nco_TBACl 
;
PROBLEM:  Atom C28             has ADP max/min Ratio .....        5.3 prolat
RESPONSE: This may be due to disorder of C28 atom.
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_vrf_PLAT234_Tren-Cl-Me-nco_TBACl 
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PROBLEM: Large Hirshfeld Difference N8       --C31              0.37 Ang. 
RESPONSE: This may be due to disorder in the model.
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_vrf_PLAT241_Tren-Cl-Me-nco_TBACl 
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PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        C31 Check 
RESPONSE: This may be due to mismatching of U(eq) values.
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_vrf_PLAT242_Tren-Cl-Me-nco_TBACl 
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PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         N8 Check  
RESPONSE: This may be due to mismatching of U(eq) values.
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_vrf_PLAT410_Tren-Cl-Me-nco_TBACl 
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PROBLEM: Short Intra H...H Contact  H1A      ..H11B             1.61 Ang.  
RESPONSE: This may be due to short distances between adjacent H atoms.
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