# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_T-p-Cl-Ligand
_database_code_depnum_ccdc_archive 'CCDC 1832718'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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         'C27 H30 Cl3 N7 O3'
_chemical_formula_sum            'C27 H30 Cl3 N7 O3'
_chemical_formula_weight         606.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   9.4221(10)
_cell_length_b                   12.9875(12)
_cell_length_c                   13.6802(13)
_cell_angle_alpha                83.836(8)
_cell_angle_beta                 70.603(9)
_cell_angle_gamma                70.406(9)
_cell_volume                     1487.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2384
_cell_measurement_theta_min      3.3170
_cell_measurement_theta_max      26.1520

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             632.0
_exptl_transmission_factor_min   0.897
_exptl_transmission_factor_max   0.920
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    0.349
_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            5638
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0103
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.157
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4968
_reflns_number_gt                3513
_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)+(0.0609P)²+0.4067P] 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         4968
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1265
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.005
_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
Cl3 Cl 0.97072(16) 1.01890(9) 0.88437(8) 0.1096(4) Uani 1 1 d . . . . .
Cl1 Cl 0.89329(16) 0.39078(11) 1.03932(8) 0.1187(5) Uani 1 1 d . . . . .
Cl2 Cl 0.51400(19) 0.81347(11) 1.05694(9) 0.1372(5) Uani 1 1 d . . . . .
O2 O 0.4355(2) 0.68146(14) 0.62232(14) 0.0552(5) Uani 1 1 d . . . . .
O1 O 0.9221(2) 0.39791(14) 0.54070(14) 0.0543(5) Uani 1 1 d . . . . .
O3 O 0.7133(2) 0.95277(14) 0.49207(15) 0.0593(5) Uani 1 1 d . . . . .
N1 N 0.6239(2) 0.67818(16) 0.34533(15) 0.0428(5) Uani 1 1 d . . . . .
N4 N 0.3467(3) 0.81481(17) 0.51533(16) 0.0505(6) Uani 1 1 d . . . . .
H4N H 0.3181 0.8840 0.5040 0.061 Uiso 1 1 calc R U . . .
N6 N 0.8168(3) 0.78784(17) 0.41357(17) 0.0542(6) Uani 1 1 d . . . . .
H6N H 0.8718 0.7203 0.4157 0.065 Uiso 1 1 calc R U . . .
N2 N 0.7266(3) 0.52421(17) 0.49021(16) 0.0512(6) Uani 1 1 d . . . . .
H2N H 0.6361 0.5745 0.5110 0.061 Uiso 1 1 calc R U . . .
N5 N 0.3981(3) 0.85990(18) 0.65352(17) 0.0552(6) Uani 1 1 d . . . . .
H5N H 0.3803 0.9245 0.6276 0.066 Uiso 1 1 calc R U . . .
N7 N 0.8883(3) 0.81194(17) 0.55078(17) 0.0551(6) Uani 1 1 d . . . . .
H7N H 0.9403 0.7433 0.5428 0.066 Uiso 1 1 calc R U . . .
N3 N 0.7197(3) 0.52246(19) 0.65713(18) 0.0581(6) Uani 1 1 d . . . . .
H3N H 0.6348 0.5774 0.6641 0.070 Uiso 1 1 calc R U . . .
C12 C 0.3959(3) 0.7790(2) 0.5975(2) 0.0452(6) Uani 1 1 d . . . . .
C3 C 0.7981(3) 0.4768(2) 0.5605(2) 0.0458(6) Uani 1 1 d . . . . .
C21 C 0.8013(3) 0.8571(2) 0.4852(2) 0.0459(6) Uani 1 1 d . . . . .
C22 C 0.9022(3) 0.8653(2) 0.6300(2) 0.0461(6) Uani 1 1 d . . . . .
C4 C 0.7660(3) 0.4874(2) 0.7458(2) 0.0492(6) Uani 1 1 d . . . . .
C13 C 0.4269(3) 0.8465(2) 0.7492(2) 0.0499(7) Uani 1 1 d . . . . .
C11 C 0.3391(3) 0.7433(2) 0.4442(2) 0.0517(7) Uani 1 1 d . . . . .
H11A H 0.2351 0.7702 0.4351 0.062 Uiso 1 1 calc R U . . .
H11B H 0.3525 0.6708 0.4740 0.062 Uiso 1 1 calc R U . . .
C19 C 0.7413(3) 0.7276(2) 0.2801(2) 0.0521(7) Uani 1 1 d . . . . .
H19A H 0.7180 0.7519 0.2159 0.062 Uiso 1 1 calc R U . . .
H19B H 0.8457 0.6729 0.2629 0.062 Uiso 1 1 calc R U . . .
C10 C 0.4641(3) 0.7359(2) 0.3399(2) 0.0507(7) Uani 1 1 d . . . . .
H10A H 0.4427 0.6980 0.2918 0.061 Uiso 1 1 calc R U . . .
H10B H 0.4588 0.8090 0.3136 0.061 Uiso 1 1 calc R U . . .
C1 C 0.6710(3) 0.5601(2) 0.3282(2) 0.0513(7) Uani 1 1 d . . . . .
H1A H 0.7161 0.5448 0.2544 0.062 Uiso 1 1 calc R U . . .
H1B H 0.5778 0.5365 0.3545 0.062 Uiso 1 1 calc R U . . .
C5 C 0.8146(3) 0.3789(2) 0.7728(2) 0.0570(7) Uani 1 1 d . . . . .
H5 H 0.8206 0.3254 0.7302 0.068 Uiso 1 1 calc R U . . .
C2 C 0.7916(3) 0.4962(2) 0.3814(2) 0.0532(7) Uani 1 1 d . . . . .
H2A H 0.8155 0.4184 0.3727 0.064 Uiso 1 1 calc R U . . .
H2B H 0.8893 0.5139 0.3508 0.064 Uiso 1 1 calc R U . . .
C27 C 0.8859(4) 0.9756(2) 0.6285(2) 0.0594(8) Uani 1 1 d . . . . .
H27 H 0.8612 1.0186 0.5738 0.071 Uiso 1 1 calc R U . . .
C20 C 0.7434(4) 0.8235(2) 0.3326(2) 0.0561(7) Uani 1 1 d . . . . .
H20A H 0.8015 0.8650 0.2815 0.067 Uiso 1 1 calc R U . . .
H20B H 0.6354 0.8712 0.3623 0.067 Uiso 1 1 calc R U . . .
C23 C 0.9432(4) 0.8031(2) 0.7106(2) 0.0601(8) Uani 1 1 d . . . . .
H23 H 0.9563 0.7288 0.7126 0.072 Uiso 1 1 calc R U . . .
C6 C 0.8546(3) 0.3489(3) 0.8632(2) 0.0637(8) Uani 1 1 d . . . . .
H6 H 0.8890 0.2756 0.8807 0.076 Uiso 1 1 calc R U . . .
C24 C 0.9650(4) 0.8497(3) 0.7885(2) 0.0690(9) Uani 1 1 d . . . . .
H24 H 0.9931 0.8069 0.8423 0.083 Uiso 1 1 calc R U . . .
C26 C 0.9058(4) 1.0223(3) 0.7066(2) 0.0688(9) Uani 1 1 d . . . . .
H26 H 0.8925 1.0966 0.7050 0.083 Uiso 1 1 calc R U . . .
C9 C 0.7564(4) 0.5660(3) 0.8109(2) 0.0642(8) Uani 1 1 d . . . . .
H9 H 0.7238 0.6394 0.7933 0.077 Uiso 1 1 calc R U . . .
C18 C 0.3779(4) 0.7719(3) 0.8223(2) 0.0654(8) Uani 1 1 d . . . . .
H18 H 0.3268 0.7282 0.8078 0.078 Uiso 1 1 calc R U . . .
C14 C 0.5006(4) 0.9116(3) 0.7729(2) 0.0651(8) Uani 1 1 d . . . . .
H14 H 0.5341 0.9614 0.7243 0.078 Uiso 1 1 calc R U . . .
C25 C 0.9448(4) 0.9599(3) 0.7860(2) 0.0671(8) Uani 1 1 d . . . . .
C7 C 0.8429(4) 0.4287(3) 0.9263(2) 0.0709(9) Uani 1 1 d . . . . .
C8 C 0.7940(4) 0.5371(3) 0.9008(3) 0.0778(10) Uani 1 1 d . . . . .
H8 H 0.7865 0.5905 0.9441 0.093 Uiso 1 1 calc R U . . .
C17 C 0.4050(4) 0.7630(3) 0.9158(2) 0.0786(10) Uani 1 1 d . . . . .
H17 H 0.3735 0.7125 0.9643 0.094 Uiso 1 1 calc R U . . .
C15 C 0.5254(4) 0.9037(3) 0.8682(3) 0.0782(10) Uani 1 1 d . . . . .
H15 H 0.5731 0.9488 0.8844 0.094 Uiso 1 1 calc R U . . .
C16 C 0.4783(5) 0.8284(3) 0.9379(3) 0.0803(10) Uani 1 1 d . . . . .


_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 C25 1.739(3) . ?
Cl1 C7 1.739(3) . ?
Cl2 C16 1.748(3) . ?
O2 C12 1.238(3) . ?
O1 C3 1.239(3) . ?
O3 C21 1.234(3) . ?
N1 C19 1.460(3) . ?
N1 C10 1.463(3) . ?
N1 C1 1.468(3) . ?
N4 C12 1.336(3) . ?
N4 C11 1.449(3) . ?
N4 H4N 0.8600 . ?
N6 C21 1.340(3) . ?
N6 C20 1.451(3) . ?
N6 H6N 0.8600 . ?
N2 C3 1.336(3) . ?
N2 C2 1.444(3) . ?
N2 H2N 0.8600 . ?
N5 C12 1.374(3) . ?
N5 C13 1.404(3) . ?
N5 H5N 0.8600 . ?
N7 C21 1.369(3) . ?
N7 C22 1.410(3) . ?
N7 H7N 0.8600 . ?
N3 C3 1.367(3) . ?
N3 C4 1.403(3) . ?
N3 H3N 0.8600 . ?
C22 C23 1.378(4) . ?
C22 C27 1.387(4) . ?
C4 C5 1.378(4) . ?
C4 C9 1.386(4) . ?
C13 C14 1.380(4) . ?
C13 C18 1.392(4) . ?
C11 C10 1.506(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C19 C20 1.512(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C1 C2 1.516(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C5 C6 1.390(4) . ?
C5 H5 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C27 C26 1.376(4) . ?
C27 H27 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C23 C24 1.383(4) . ?
C23 H23 0.9300 . ?
C6 C7 1.372(4) . ?
C6 H6 0.9300 . ?
C24 C25 1.377(4) . ?
C24 H24 0.9300 . ?
C26 C25 1.360(4) . ?
C26 H26 0.9300 . ?
C9 C8 1.372(4) . ?
C9 H9 0.9300 . ?
C18 C17 1.371(4) . ?
C18 H18 0.9300 . ?
C14 C15 1.386(4) . ?
C14 H14 0.9300 . ?
C7 C8 1.372(5) . ?
C8 H8 0.9300 . ?
C17 C16 1.370(5) . ?
C17 H17 0.9300 . ?
C15 C16 1.369(5) . ?
C15 H15 0.9300 . ?

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
C19 N1 C10 112.6(2) . . ?
C19 N1 C1 113.2(2) . . ?
C10 N1 C1 112.3(2) . . ?
C12 N4 C11 123.5(2) . . ?
C12 N4 H4N 118.2 . . ?
C11 N4 H4N 118.2 . . ?
C21 N6 C20 122.0(2) . . ?
C21 N6 H6N 119.0 . . ?
C20 N6 H6N 119.0 . . ?
C3 N2 C2 124.1(2) . . ?
C3 N2 H2N 118.0 . . ?
C2 N2 H2N 118.0 . . ?
C12 N5 C13 125.9(2) . . ?
C12 N5 H5N 117.1 . . ?
C13 N5 H5N 117.1 . . ?
C21 N7 C22 127.4(2) . . ?
C21 N7 H7N 116.3 . . ?
C22 N7 H7N 116.3 . . ?
C3 N3 C4 125.6(2) . . ?
C3 N3 H3N 117.2 . . ?
C4 N3 H3N 117.2 . . ?
O2 C12 N4 123.4(2) . . ?
O2 C12 N5 122.3(2) . . ?
N4 C12 N5 114.3(2) . . ?
O1 C3 N2 123.3(2) . . ?
O1 C3 N3 123.1(2) . . ?
N2 C3 N3 113.5(2) . . ?
O3 C21 N6 122.4(2) . . ?
O3 C21 N7 123.3(2) . . ?
N6 C21 N7 114.4(2) . . ?
C23 C22 C27 118.1(3) . . ?
C23 C22 N7 118.1(2) . . ?
C27 C22 N7 123.7(2) . . ?
C5 C4 C9 118.8(3) . . ?
C5 C4 N3 122.8(2) . . ?
C9 C4 N3 118.3(2) . . ?
C14 C13 C18 119.1(3) . . ?
C14 C13 N5 119.2(3) . . ?
C18 C13 N5 121.7(3) . . ?
N4 C11 C10 112.5(2) . . ?
N4 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
N4 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N1 C19 C20 112.2(2) . . ?
N1 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
N1 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
N1 C10 C11 112.0(2) . . ?
N1 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
N1 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N1 C1 C2 111.6(2) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
N2 C2 C1 108.8(2) . . ?
N2 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
N2 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C26 C27 C22 121.0(3) . . ?
C26 C27 H27 119.5 . . ?
C22 C27 H27 119.5 . . ?
N6 C20 C19 111.4(2) . . ?
N6 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
N6 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C22 C23 C24 120.9(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C7 C6 C5 119.3(3) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C25 C24 C23 119.7(3) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C25 C26 C27 120.1(3) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C8 C9 C4 121.0(3) . . ?
C8 C9 H9 119.5 . . ?
C4 C9 H9 119.5 . . ?
C17 C18 C13 120.0(3) . . ?
C17 C18 H18 120.0 . . ?
C13 C18 H18 120.0 . . ?
C13 C14 C15 120.9(3) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C26 C25 C24 120.2(3) . . ?
C26 C25 Cl3 120.0(3) . . ?
C24 C25 Cl3 119.8(2) . . ?
C8 C7 C6 121.0(3) . . ?
C8 C7 Cl1 119.9(3) . . ?
C6 C7 Cl1 119.1(3) . . ?
C9 C8 C7 119.4(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C16 C17 C18 120.1(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C15 C14 118.8(3) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C15 C16 C17 121.2(3) . . ?
C15 C16 Cl2 119.8(3) . . ?
C17 C16 Cl2 119.0(3) . . ?

_refine_diff_density_max         0.503
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.042

####################################################################### 
# 
# 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-p-I-Ligand
_database_code_depnum_ccdc_archive 'CCDC 1832720'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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         'C27 H30 I3 N7 O3'
_chemical_formula_sum            'C27 H30 I3 N7 O3'
_chemical_formula_weight         881.28

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'
I I -0.4742 1.8119 '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                   9.618(5)
_cell_length_b                   13.244(6)
_cell_length_c                   13.946(7)
_cell_angle_alpha                84.13(3)
_cell_angle_beta                 72.77(3)
_cell_angle_gamma                69.73(3)
_cell_volume                     1591.7(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4724
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      23.70

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_F_000             848.0
_exptl_transmission_factor_min   0.428
_exptl_transmission_factor_max   0.567
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    2.985
_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                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16333
_diffrn_reflns_av_unetI/netI     0.1335
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.529
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5591
_reflns_number_gt                4066
_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)+(0.0400P)²+4.0000P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5591
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.2280
_refine_ls_wR_factor_gt          0.1979
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
I3 I 1.34227(7) 1.01161(5) 0.11443(5) 0.0796(3) Uani 1 1 d . . . . .
I2 I 1.09391(9) 0.80929(8) -0.04049(6) 0.1154(4) Uani 1 1 d . . . . .
I1 I 1.44188(10) 0.36405(11) -0.01921(8) 0.1437(5) Uani 1 1 d . . . . .
N1 N 0.4759(6) 0.6817(5) 0.6462(4) 0.0477(13) Uani 1 1 d . . . . .
C3 C 0.8469(8) 0.4789(5) 0.4436(6) 0.0536(18) Uani 1 1 d . . . . .
C9 C 1.0550(9) 0.5588(7) 0.2096(7) 0.063(2) Uani 1 1 d . . . . .
H9 H 1.0114 0.6312 0.2273 0.076 Uiso 1 1 calc R U . . .
C5 C 1.0560(10) 0.3794(7) 0.2416(8) 0.070(2) Uani 1 1 d . . . . .
H5 H 1.0143 0.3296 0.2797 0.084 Uiso 1 1 calc R U . . .
C4 C 0.9927(8) 0.4849(6) 0.2675(6) 0.0568(19) Uani 1 1 d . . . . .
C7 C 1.2435(9) 0.4185(8) 0.1011(7) 0.070(2) Uani 1 1 d . . . . .
C2 C 0.6710(9) 0.5019(6) 0.6159(6) 0.060(2) Uani 1 1 d . . . . .
H2A H 0.7378 0.5194 0.6469 0.072 Uiso 1 1 calc R U . . .
H2B H 0.6858 0.4257 0.6255 0.072 Uiso 1 1 calc R U . . .
C6 C 1.1821(10) 0.3459(8) 0.1590(8) 0.075(3) Uani 1 1 d . . . . .
H6 H 1.2260 0.2732 0.1424 0.090 Uiso 1 1 calc R U . . .
C1 C 0.5058(9) 0.5664(6) 0.6639(6) 0.0558(18) Uani 1 1 d . . . . .
H1A H 0.4393 0.5435 0.6371 0.067 Uiso 1 1 calc R U . . .
H1B H 0.4811 0.5529 0.7356 0.067 Uiso 1 1 calc R U . . .
C8 C 1.1815(11) 0.5264(9) 0.1255(7) 0.078(3) Uani 1 1 d . . . . .
H8 H 1.2231 0.5760 0.0869 0.094 Uiso 1 1 calc R U . . .
N3 N 0.8639(7) 0.5233(5) 0.3501(5) 0.0633(18) Uani 1 1 d . . . . .
H3N H 0.7898 0.5792 0.3412 0.076 Uiso 1 1 calc R U . . .
N2 N 0.7106(7) 0.5264(5) 0.5089(5) 0.0589(17) Uani 1 1 d . . . . .
H2N H 0.6414 0.5747 0.4863 0.071 Uiso 1 1 calc R U . . .
O1 O 0.9485(6) 0.4002(4) 0.4666(5) 0.0648(15) Uani 1 1 d . . . . .
C12 C 0.4893(8) 0.7830(5) 0.4018(5) 0.0454(16) Uani 1 1 d . . . . .
C13 C 0.6660(8) 0.8473(6) 0.2620(6) 0.0547(19) Uani 1 1 d . . . . .
C11 C 0.2905(8) 0.7479(6) 0.5464(6) 0.0514(17) Uani 1 1 d . . . . .
H11A H 0.3329 0.6764 0.5174 0.062 Uiso 1 1 calc R U . . .
H11B H 0.1805 0.7741 0.5531 0.062 Uiso 1 1 calc R U . . .
C14 C 0.6985(9) 0.7708(7) 0.1910(6) 0.061(2) Uani 1 1 d . . . . .
H14 H 0.6401 0.7255 0.2014 0.073 Uiso 1 1 calc R U . . .
C15 C 0.8192(9) 0.7619(8) 0.1036(6) 0.069(2) Uani 1 1 d . . . . .
H15 H 0.8424 0.7102 0.0557 0.082 Uiso 1 1 calc R U . . .
C16 C 0.9054(9) 0.8312(8) 0.0885(7) 0.067(2) Uani 1 1 d . . . . .
C18 C 0.7556(10) 0.9129(7) 0.2440(7) 0.067(2) Uani 1 1 d . . . . .
H18 H 0.7342 0.9646 0.2916 0.080 Uiso 1 1 calc R U . . .
C17 C 0.8727(11) 0.9047(8) 0.1603(8) 0.081(3) Uani 1 1 d . . . . .
H17 H 0.9317 0.9494 0.1514 0.098 Uiso 1 1 calc R U . . .
N4 N 0.3619(6) 0.8184(5) 0.4787(5) 0.0501(14) Uani 1 1 d . . . . .
H4N H 0.3200 0.8867 0.4885 0.060 Uiso 1 1 calc R U . . .
N5 N 0.5426(7) 0.8613(5) 0.3502(5) 0.0547(15) Uani 1 1 d . . . . .
H5N H 0.4965 0.9256 0.3737 0.066 Uiso 1 1 calc R U . . .
O2 O 0.5528(6) 0.6863(4) 0.3794(4) 0.0560(13) Uani 1 1 d . . . . .
C10 C 0.3151(8) 0.7409(6) 0.6502(6) 0.0529(18) Uani 1 1 d . . . . .
H10A H 0.2868 0.8129 0.6756 0.064 Uiso 1 1 calc R U . . .
H10B H 0.2492 0.7051 0.6958 0.064 Uiso 1 1 calc R U . . .
C25 C 1.2036(8) 0.9467(6) 0.2327(6) 0.0543(18) Uani 1 1 d . . . . .
C21 C 0.7800(8) 0.8568(6) 0.5217(6) 0.0469(16) Uani 1 1 d . . . . .
C22 C 1.0155(8) 0.8607(6) 0.3855(5) 0.0479(16) Uani 1 1 d . . . . .
C27 C 0.9929(9) 0.9694(6) 0.3806(6) 0.058(2) Uani 1 1 d . . . . .
H27 H 0.9133 1.0150 0.4290 0.070 Uiso 1 1 calc R U . . .
C19 C 0.5320(9) 0.7282(7) 0.7128(6) 0.0574(19) Uani 1 1 d . . . . .
H19A H 0.6191 0.6733 0.7293 0.069 Uiso 1 1 calc R U . . .
H19B H 0.4508 0.7518 0.7748 0.069 Uiso 1 1 calc R U . . .
C24 C 1.2297(9) 0.8376(6) 0.2364(6) 0.064(2) Uani 1 1 d . . . . .
H24 H 1.3101 0.7925 0.1880 0.077 Uiso 1 1 calc R U . . .
C23 C 1.1354(9) 0.7953(6) 0.3128(6) 0.0577(19) Uani 1 1 d . . . . .
H23 H 1.1535 0.7216 0.3149 0.069 Uiso 1 1 calc R U . . .
C26 C 1.0868(9) 1.0119(6) 0.3044(6) 0.062(2) Uani 1 1 d . . . . .
H26 H 1.0699 1.0855 0.3025 0.075 Uiso 1 1 calc R U . . .
C20 C 0.5811(9) 0.8237(6) 0.6632(7) 0.062(2) Uani 1 1 d . . . . .
H20A H 0.5037 0.8702 0.6321 0.074 Uiso 1 1 calc R U . . .
H20B H 0.5882 0.8651 0.7139 0.074 Uiso 1 1 calc R U . . .
N6 N 0.7293(7) 0.7875(5) 0.5876(5) 0.0589(16) Uani 1 1 d . . . . .
H6N H 0.7853 0.7207 0.5852 0.071 Uiso 1 1 calc R U . . .
N7 N 0.9279(7) 0.8109(5) 0.4609(5) 0.0563(16) Uani 1 1 d . . . . .
H7N H 0.9719 0.7435 0.4705 0.068 Uiso 1 1 calc R U . . .
O3 O 0.7038(6) 0.9509(4) 0.5166(4) 0.0600(14) Uani 1 1 d . . . . .


_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
I3 C25 2.107(8) . ?
I2 C16 2.102(9) . ?
I1 C7 2.092(9) . ?
N1 C10 1.458(9) . ?
N1 C1 1.461(9) . ?
N1 C19 1.475(10) . ?
C3 O1 1.247(8) . ?
C3 N2 1.335(10) . ?
C3 N3 1.362(10) . ?
C9 C4 1.387(12) . ?
C9 C8 1.391(12) . ?
C5 C4 1.355(11) . ?
C5 C6 1.378(13) . ?
C4 N3 1.400(10) . ?
C7 C6 1.370(14) . ?
C7 C8 1.379(13) . ?
C2 N2 1.459(10) . ?
C2 C1 1.500(11) . ?
C12 O2 1.241(8) . ?
C12 N4 1.340(9) . ?
C12 N5 1.361(10) . ?
C13 C14 1.381(11) . ?
C13 C18 1.381(12) . ?
C13 N5 1.409(10) . ?
C11 N4 1.454(9) . ?
C11 C10 1.523(11) . ?
C14 C15 1.394(12) . ?
C15 C16 1.398(14) . ?
C16 C17 1.360(14) . ?
C18 C17 1.344(13) . ?
C25 C26 1.359(11) . ?
C25 C24 1.376(11) . ?
C21 O3 1.215(9) . ?
C21 N6 1.340(10) . ?
C21 N7 1.380(9) . ?
C22 C27 1.377(11) . ?
C22 C23 1.380(10) . ?
C22 N7 1.403(9) . ?
C27 C26 1.387(11) . ?
C19 C20 1.531(12) . ?
C24 C23 1.388(12) . ?
C20 N6 1.453(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
C10 N1 C1 112.9(6) . . ?
C10 N1 C19 112.5(6) . . ?
C1 N1 C19 111.5(6) . . ?
O1 C3 N2 122.6(8) . . ?
O1 C3 N3 123.4(7) . . ?
N2 C3 N3 114.0(6) . . ?
C4 C9 C8 121.1(8) . . ?
C4 C5 C6 120.1(9) . . ?
C5 C4 C9 119.5(8) . . ?
C5 C4 N3 122.4(8) . . ?
C9 C4 N3 118.1(7) . . ?
C6 C7 C8 120.5(8) . . ?
C6 C7 I1 119.7(7) . . ?
C8 C7 I1 119.7(8) . . ?
N2 C2 C1 109.3(6) . . ?
C7 C6 C5 120.7(8) . . ?
N1 C1 C2 111.8(6) . . ?
C7 C8 C9 118.1(9) . . ?
C3 N3 C4 125.0(6) . . ?
C3 N2 C2 124.5(6) . . ?
O2 C12 N4 122.3(7) . . ?
O2 C12 N5 122.7(7) . . ?
N4 C12 N5 114.9(6) . . ?
C14 C13 C18 118.5(8) . . ?
C14 C13 N5 121.8(8) . . ?
C18 C13 N5 119.7(8) . . ?
N4 C11 C10 112.8(6) . . ?
C13 C14 C15 119.7(9) . . ?
C14 C15 C16 119.6(9) . . ?
C17 C16 C15 119.6(8) . . ?
C17 C16 I2 121.9(8) . . ?
C15 C16 I2 118.2(7) . . ?
C17 C18 C13 122.3(10) . . ?
C18 C17 C16 120.3(10) . . ?
C12 N4 C11 123.8(6) . . ?
C12 N5 C13 126.4(6) . . ?
N1 C10 C11 110.8(6) . . ?
C26 C25 C24 119.7(8) . . ?
C26 C25 I3 120.5(6) . . ?
C24 C25 I3 119.8(6) . . ?
O3 C21 N6 123.3(7) . . ?
O3 C21 N7 123.3(7) . . ?
N6 C21 N7 113.3(6) . . ?
C27 C22 C23 117.8(7) . . ?
C27 C22 N7 124.7(6) . . ?
C23 C22 N7 117.4(7) . . ?
C22 C27 C26 121.1(7) . . ?
N1 C19 C20 111.4(6) . . ?
C25 C24 C23 119.7(7) . . ?
C22 C23 C24 121.2(7) . . ?
C25 C26 C27 120.4(7) . . ?
N6 C20 C19 111.1(6) . . ?
C21 N6 C20 121.0(6) . . ?
C21 N7 C22 127.9(6) . . ?

_refine_diff_density_max         1.787
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.120

####################################################################### 
# 
# 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-p-I-TEACO3
_database_code_depnum_ccdc_archive 'CCDC 1832726'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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(C27 H30 I3 N7 O3), C O3, 2(O)'
_chemical_formula_sum            'C55 H60 I6 N14 O11'
_chemical_formula_weight         1854.57

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'
I I -0.4742 1.8119 '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                   17.7358(5)
_cell_length_b                   20.8986(9)
_cell_length_c                   23.8529(9)
_cell_angle_alpha                90
_cell_angle_beta                 99.333(3)
_cell_angle_gamma                90
_cell_volume                     8724.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4108
_cell_measurement_theta_min      3.5890
_cell_measurement_theta_max      21.4090

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_F_000             3576.0
_exptl_transmission_factor_min   0.472
_exptl_transmission_factor_max   0.602
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    2.186
_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            17797
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.036
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7674
_reflns_number_gt                3938
_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)+(0.1000P)²+1.3612P] 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         7674
_refine_ls_number_parameters     389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.2093
_refine_ls_wR_factor_gt          0.1853
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
C28 C 0.0000 0.4492(6) 0.2500 0.071(2) Uani 1 2 d S T P . .
O5 O 0.0559(3) 0.4782(3) 0.2766(3) 0.122(2) Uani 1 1 d . . . . .
I3 I 1.12551(3) 0.03043(3) 0.26527(3) 0.1149(3) Uani 1 1 d . . . . .
I2 I 1.36140(4) 0.70736(4) 0.43227(4) 0.1529(4) Uani 1 1 d . . . . .
I1 I 0.61559(4) 0.53107(5) -0.04422(3) 0.1500(4) Uani 1 1 d . . . . .
C25 C 1.1001(4) 0.1228(4) 0.2928(4) 0.089(2) Uani 1 1 d . . . . .
N7 N 1.0470(3) 0.3054(3) 0.3414(2) 0.0875(17) Uani 1 1 d . . . . .
H7N H 1.0450 0.3330 0.3145 0.105 Uiso 1 1 calc R U . . .
O1 O 0.6987(3) 0.3891(3) 0.2333(2) 0.0985(16) Uani 1 1 d . . . . .
N3 N 0.7923(3) 0.4300(3) 0.1877(2) 0.0884(17) Uani 1 1 d . . . . .
H3N H 0.8410 0.4354 0.1918 0.106 Uiso 1 1 calc R U . . .
N1 N 0.8606(3) 0.4440(3) 0.3914(2) 0.0812(16) Uani 1 1 d . . . . .
N4 N 0.9177(3) 0.5568(3) 0.3297(2) 0.0930(18) Uani 1 1 d . . . . .
H4N H 0.9268 0.5346 0.3012 0.112 Uiso 1 1 calc R U . . .
O3 O 1.0286(4) 0.2943(3) 0.4334(2) 0.1172(19) Uani 1 1 d . . . . .
N5 N 1.0409(4) 0.5894(3) 0.3385(2) 0.0948(19) Uani 1 1 d . . . . .
H5N H 1.0420 0.5648 0.3097 0.114 Uiso 1 1 calc R U . . .
N6 N 1.0168(3) 0.3921(4) 0.3922(3) 0.0905(17) Uani 1 1 d . . . . .
H6N H 1.0228 0.4151 0.3633 0.109 Uiso 1 1 calc R U . . .
O2 O 0.9599(3) 0.6333(3) 0.3934(3) 0.123(2) Uani 1 1 d . . . . .
C23 C 1.0986(5) 0.2347(5) 0.2806(4) 0.107(3) Uani 1 1 d . . . . .
H23 H 1.1100 0.2703 0.2601 0.128 Uiso 1 1 calc R U . . .
C9 C 0.6704(4) 0.4532(5) 0.1248(3) 0.102(3) Uani 1 1 d . . . . .
H9 H 0.6428 0.4388 0.1523 0.123 Uiso 1 1 calc R U . . .
C3 C 0.7657(5) 0.4016(4) 0.2324(3) 0.082(2) Uani 1 1 d . . . . .
C4 C 0.7503(4) 0.4513(4) 0.1360(3) 0.0779(19) Uani 1 1 d . . . . .
C2 C 0.8066(4) 0.3578(4) 0.3270(3) 0.095(2) Uani 1 1 d . . . . .
H2A H 0.8498 0.3316 0.3434 0.114 Uiso 1 1 calc R U . . .
H2B H 0.7623 0.3301 0.3189 0.114 Uiso 1 1 calc R U . . .
C22 C 1.0657(4) 0.2430(4) 0.3276(3) 0.0752(19) Uani 1 1 d . . . . .
C5 C 0.7874(4) 0.4745(4) 0.0955(3) 0.097(3) Uani 1 1 d . . . . .
H5 H 0.8406 0.4742 0.1024 0.117 Uiso 1 1 calc R U . . .
C21 C 1.0316(4) 0.3279(4) 0.3912(3) 0.084(2) Uani 1 1 d . . . . .
C20 C 0.9913(4) 0.4225(4) 0.4401(3) 0.094(2) Uani 1 1 d . . . . .
H20B H 1.0024 0.4679 0.4396 0.113 Uiso 1 1 calc R U . . .
H20A H 1.0193 0.4048 0.4750 0.113 Uiso 1 1 calc R U . . .
C10 C 0.8470(4) 0.5129(4) 0.4016(3) 0.091(2) Uani 1 1 d . . . . .
H10A H 0.8875 0.5290 0.4303 0.109 Uiso 1 1 calc R U . . .
H10B H 0.7990 0.5176 0.4158 0.109 Uiso 1 1 calc R U . . .
C1 C 0.7922(4) 0.4079(4) 0.3700(3) 0.088(2) Uani 1 1 d . . . . .
H1A H 0.7528 0.4371 0.3524 0.106 Uiso 1 1 calc R U . . .
H1B H 0.7737 0.3871 0.4015 0.106 Uiso 1 1 calc R U . . .
C24 C 1.1154(5) 0.1752(5) 0.2630(4) 0.109(3) Uani 1 1 d . . . . .
H24 H 1.1374 0.1705 0.2304 0.130 Uiso 1 1 calc R U . . .
C12 C 0.9725(5) 0.5948(4) 0.3572(3) 0.091(2) Uani 1 1 d . . . . .
C13 C 1.1110(5) 0.6202(4) 0.3618(3) 0.091(2) Uani 1 1 d . . . . .
C16 C 1.2524(5) 0.6701(5) 0.4019(5) 0.119(3) Uani 1 1 d . . . . .
C19 C 0.9075(4) 0.4132(4) 0.4395(3) 0.087(2) Uani 1 1 d . . . . .
H19A H 0.8963 0.3677 0.4384 0.104 Uiso 1 1 calc R U . . .
H19B H 0.8940 0.4303 0.4743 0.104 Uiso 1 1 calc R U . . .
C11 C 0.8440(5) 0.5525(4) 0.3470(3) 0.101(2) Uani 1 1 d . . . . .
H11B H 0.8082 0.5329 0.3168 0.121 Uiso 1 1 calc R U . . .
H11A H 0.8257 0.5952 0.3534 0.121 Uiso 1 1 calc R U . . .
C27 C 1.0493(5) 0.1900(5) 0.3591(4) 0.103(2) Uani 1 1 d . . . . .
H27 H 1.0278 0.1947 0.3919 0.124 Uiso 1 1 calc R U . . .
C18 C 1.1731(5) 0.6068(5) 0.3333(4) 0.107(3) Uani 1 1 d . . . . .
H18 H 1.1669 0.5814 0.3008 0.128 Uiso 1 1 calc R U . . .
C6 C 0.7525(4) 0.4981(5) 0.0457(3) 0.104(3) Uani 1 1 d . . . . .
H6 H 0.7805 0.5152 0.0195 0.125 Uiso 1 1 calc R U . . .
C26 C 1.0656(5) 0.1315(5) 0.3400(4) 0.108(3) Uani 1 1 d . . . . .
H26 H 1.0531 0.0956 0.3597 0.129 Uiso 1 1 calc R U . . .
C14 C 1.1208(5) 0.6590(5) 0.4083(3) 0.115(3) Uani 1 1 d . . . . .
H14 H 1.0796 0.6681 0.4267 0.138 Uiso 1 1 calc R U . . .
C15 C 1.1907(5) 0.6847(5) 0.4280(4) 0.117(3) Uani 1 1 d . . . . .
H15 H 1.1968 0.7121 0.4591 0.141 Uiso 1 1 calc R U . . .
C17 C 1.2421(5) 0.6323(5) 0.3549(4) 0.122(3) Uani 1 1 d . . . . .
H17 H 1.2837 0.6236 0.3370 0.146 Uiso 1 1 calc R U . . .
C8 C 0.6328(4) 0.4752(5) 0.0751(3) 0.100(3) Uani 1 1 d . . . . .
H8 H 0.5796 0.4761 0.0684 0.120 Uiso 1 1 calc R U . . .
C7 C 0.6732(4) 0.4963(5) 0.0343(3) 0.101(2) Uani 1 1 d . . . . .
O4 O 0.0000 0.3891(5) 0.2500 0.158(5) Uani 1 2 d S T P . .
N2 N 0.8221(3) 0.3850(3) 0.2746(2) 0.0851(17) Uani 1 1 d . . . . .
H2N H 0.8687 0.3908 0.2701 0.102 Uiso 1 1 calc R U . . .
O6 O 0.9584(5) 0.7506(5) 0.4525(4) 0.265(3) Uani 1 1 d . . . . .


_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
C28 O4 1.256(13) . ?
C28 O5 1.245(7) . ?
C28 O5 1.245(7) 2 ?
I3 C25 2.110(8) . ?
I2 C16 2.101(9) . ?
I1 C7 2.111(8) . ?
C25 C24 1.358(12) . ?
C25 C26 1.379(11) . ?
N7 C21 1.346(9) . ?
N7 C22 1.398(9) . ?
O1 C3 1.220(8) . ?
N3 C3 1.369(9) . ?
N3 C4 1.407(9) . ?
N1 C1 1.449(8) . ?
N1 C10 1.486(10) . ?
N1 C19 1.453(8) . ?
N4 C12 1.341(9) . ?
N4 C11 1.436(10) . ?
O3 C21 1.235(9) . ?
N5 C12 1.363(9) . ?
N5 C13 1.430(9) . ?
N6 C21 1.367(10) . ?
N6 C20 1.444(9) . ?
O2 C12 1.228(9) . ?
C23 C22 1.356(10) . ?
C23 C24 1.361(12) . ?
C9 C8 1.344(10) . ?
C9 C4 1.399(10) . ?
C3 N2 1.343(8) . ?
C4 C5 1.344(10) . ?
C2 N2 1.440(9) . ?
C2 C1 1.517(11) . ?
C22 C27 1.395(11) . ?
C5 C6 1.342(11) . ?
C20 C19 1.497(10) . ?
C10 C11 1.536(11) . ?
C13 C14 1.363(11) . ?
C13 C18 1.413(11) . ?
C16 C17 1.360(12) . ?
C16 C15 1.376(13) . ?
C27 C26 1.351(11) . ?
C18 C17 1.358(12) . ?
C6 C7 1.389(10) . ?
C14 C15 1.363(11) . ?
C8 C7 1.372(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
O4 C28 O5 119.1(6) . . ?
O4 C28 O5 119.1(6) . 2 ?
O5 C28 O5 121.7(11) . 2 ?
C24 C25 C26 118.3(8) . . ?
C24 C25 I3 120.3(7) . . ?
C26 C25 I3 121.4(7) . . ?
C21 N7 C22 128.6(7) . . ?
C3 N3 C4 128.4(6) . . ?
C1 N1 C10 114.3(6) . . ?
C1 N1 C19 112.8(6) . . ?
C10 N1 C19 112.8(6) . . ?
C12 N4 C11 121.3(7) . . ?
C12 N5 C13 126.8(7) . . ?
C21 N6 C20 122.1(7) . . ?
C22 C23 C24 121.1(9) . . ?
C8 C9 C4 121.4(7) . . ?
O1 C3 N2 122.8(7) . . ?
O1 C3 N3 124.4(6) . . ?
N2 C3 N3 112.7(7) . . ?
C5 C4 N3 119.6(6) . . ?
C5 C4 C9 116.9(7) . . ?
N3 C4 C9 123.5(6) . . ?
N2 C2 C1 113.0(7) . . ?
C23 C22 N7 117.6(8) . . ?
C23 C22 C27 120.0(8) . . ?
N7 C22 C27 122.4(7) . . ?
C4 C5 C6 124.0(7) . . ?
O3 C21 N7 124.2(8) . . ?
O3 C21 N6 120.6(8) . . ?
N7 C21 N6 115.2(8) . . ?
N6 C20 C19 111.9(6) . . ?
N1 C10 C11 111.6(6) . . ?
N1 C1 C2 111.9(6) . . ?
C25 C24 C23 120.2(8) . . ?
O2 C12 N4 122.1(7) . . ?
O2 C12 N5 123.9(8) . . ?
N4 C12 N5 113.9(8) . . ?
C14 C13 C18 120.3(7) . . ?
C14 C13 N5 124.9(7) . . ?
C18 C13 N5 114.8(7) . . ?
C17 C16 C15 119.4(8) . . ?
C17 C16 I2 119.5(8) . . ?
C15 C16 I2 121.1(8) . . ?
N1 C19 C20 113.0(6) . . ?
N4 C11 C10 111.7(6) . . ?
C26 C27 C22 117.5(8) . . ?
C17 C18 C13 117.6(8) . . ?
C5 C6 C7 118.1(7) . . ?
C25 C26 C27 122.9(9) . . ?
C13 C14 C15 120.2(8) . . ?
C16 C15 C14 120.2(9) . . ?
C16 C17 C18 122.3(9) . . ?
C9 C8 C7 119.6(7) . . ?
C6 C7 C8 119.9(7) . . ?
C6 C7 I1 119.5(6) . . ?
C8 C7 I1 120.4(6) . . ?
C3 N2 C2 121.9(6) . . ?

_refine_diff_density_max         0.945
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.084


# 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 0.053 0.250 0.697 1260 157 ' '
2 -0.008 0.750 0.258 1260 157 ' '
_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_T-p-Br-Ligand
_database_code_depnum_ccdc_archive 'CCDC 1832719'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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         'C27 H30 Br3 N7 O3'
_chemical_formula_sum            'C27 H30 Br3 N7 O3'
_chemical_formula_weight         740.28

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

_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                   9.464(2)
_cell_length_b                   13.104(3)
_cell_length_c                   13.846(3)
_cell_angle_alpha                83.330(14)
_cell_angle_beta                 70.953(14)
_cell_angle_gamma                70.070(14)
_cell_volume                     1525.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2095
_cell_measurement_theta_min      3.425
_cell_measurement_theta_max      20.258

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             740.0
_exptl_transmission_factor_min   0.382
_exptl_transmission_factor_max   0.486
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    4.006
_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                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12314
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.653
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4883
_reflns_number_gt                2281
_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)+(0.1000P)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         4883
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1570
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.2228
_refine_ls_wR_factor_gt          0.1690
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.005
_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
Br2 Br 0.15030(13) 0.48361(8) 0.38580(8) 0.0960(5) Uani 1 1 d . . . . .
Br3 Br 0.06416(15) 1.11712(12) 0.53412(10) 0.1317(7) Uani 1 1 d . . . . .
Br1 Br 0.41855(15) 0.68978(11) 0.55263(9) 0.1285(6) Uani 1 1 d . . . . .
N1 N 1.0275(7) 0.8202(4) -0.1507(5) 0.0458(16) Uani 1 1 d . . . . .
C3 C 1.0087(9) 0.7188(6) 0.0990(6) 0.0454(19) Uani 1 1 d . . . . .
C12 C 0.7139(10) 0.6433(6) -0.0159(6) 0.053(2) Uani 1 1 d . . . . .
C21 C 0.6472(9) 1.0214(6) 0.0596(7) 0.051(2) Uani 1 1 d . . . . .
C14 C 0.4937(9) 0.5263(6) 0.1247(6) 0.057(2) Uani 1 1 d . . . . .
H14 H 0.5724 0.4823 0.0723 0.068 Uiso 1 1 calc R U . . .
C22 C 0.4974(9) 1.0127(6) 0.2413(6) 0.052(2) Uani 1 1 d . . . . .
C11 C 0.9206(9) 0.6785(6) -0.1681(6) 0.060(2) Uani 1 1 d . . . . .
H11A H 0.9119 0.6394 -0.2201 0.072 Uiso 1 1 calc R U . . .
H11B H 1.0000 0.6296 -0.1394 0.072 Uiso 1 1 calc R U . . .
C13 C 0.4739(9) 0.6363(6) 0.1244(6) 0.050(2) Uani 1 1 d . . . . .
C27 C 0.4253(10) 1.1215(7) 0.2674(7) 0.063(2) Uani 1 1 d . . . . .
H27 H 0.4626 1.1741 0.2266 0.076 Uiso 1 1 calc R U . . .
C23 C 0.4392(10) 0.9367(7) 0.3028(7) 0.063(2) Uani 1 1 d . . . . .
H23 H 0.4866 0.8638 0.2849 0.076 Uiso 1 1 calc R U . . .
C4 C 0.8280(9) 0.6533(6) 0.2461(6) 0.048(2) Uani 1 1 d . . . . .
C15 C 0.3975(10) 0.4823(7) 0.2020(7) 0.070(3) Uani 1 1 d . . . . .
H15 H 0.4126 0.4084 0.2019 0.083 Uiso 1 1 calc R U . . .
C1 C 1.1909(8) 0.7621(6) -0.1558(6) 0.054(2) Uani 1 1 d . . . . .
H1A H 1.2586 0.7999 -0.2021 0.064 Uiso 1 1 calc R U . . .
H1B H 1.2216 0.6899 -0.1825 0.064 Uiso 1 1 calc R U . . .
C10 C 0.9727(10) 0.7737(6) -0.2167(6) 0.057(2) Uani 1 1 d . . . . .
H10A H 1.0573 0.7505 -0.2801 0.068 Uiso 1 1 calc R U . . .
H10B H 0.8851 0.8292 -0.2331 0.068 Uiso 1 1 calc R U . . .
C25 C 0.2402(10) 1.0752(8) 0.4162(7) 0.071(3) Uani 1 1 d . . . . .
C18 C 0.3530(9) 0.7001(6) 0.2017(6) 0.061(2) Uani 1 1 d . . . . .
H18 H 0.3362 0.7742 0.2024 0.073 Uiso 1 1 calc R U . . .
C20 C 0.8258(9) 1.0024(6) -0.1169(6) 0.054(2) Uani 1 1 d . . . . .
H20A H 0.8122 1.0793 -0.1259 0.065 Uiso 1 1 calc R U . . .
H20B H 0.7572 0.9860 -0.1475 0.065 Uiso 1 1 calc R U . . .
C24 C 0.3127(11) 0.9658(8) 0.3903(7) 0.079(3) Uani 1 1 d . . . . .
H24 H 0.2760 0.9132 0.4315 0.095 Uiso 1 1 calc R U . . .
C16 C 0.2807(10) 0.5454(7) 0.2787(6) 0.060(2) Uani 1 1 d . . . . .
C26 C 0.2949(10) 1.1515(7) 0.3566(7) 0.068(3) Uani 1 1 d . . . . .
H26 H 0.2460 1.2243 0.3745 0.081 Uiso 1 1 calc R U . . .
C17 C 0.2563(10) 0.6533(7) 0.2786(6) 0.066(2) Uani 1 1 d . . . . .
H17 H 0.1744 0.6966 0.3301 0.080 Uiso 1 1 calc R U . . .
C2 C 1.2135(9) 0.7534(6) -0.0509(6) 0.053(2) Uani 1 1 d . . . . .
H2A H 1.3255 0.7257 -0.0585 0.063 Uiso 1 1 calc R U . . .
H2B H 1.1717 0.8252 -0.0213 0.063 Uiso 1 1 calc R U . . .
C19 C 0.9964(9) 0.9368(6) -0.1686(6) 0.055(2) Uani 1 1 d . . . . .
H19A H 1.0219 0.9509 -0.2416 0.066 Uiso 1 1 calc R U . . .
H19B H 1.0647 0.9602 -0.1434 0.066 Uiso 1 1 calc R U . . .
C9 C 0.8000(10) 0.7282(7) 0.3173(6) 0.061(2) Uani 1 1 d . . . . .
H9 H 0.8623 0.7731 0.3033 0.074 Uiso 1 1 calc R U . . .
C5 C 0.7330(11) 0.5880(7) 0.2674(7) 0.067(2) Uani 1 1 d . . . . .
H5 H 0.7494 0.5378 0.2193 0.081 Uiso 1 1 calc R U . . .
C8 C 0.6806(11) 0.7386(8) 0.4100(7) 0.077(3) Uani 1 1 d . . . . .
H8 H 0.6635 0.7894 0.4577 0.092 Uiso 1 1 calc R U . . .
C7 C 0.5866(11) 0.6718(8) 0.4306(7) 0.077(3) Uani 1 1 d . . . . .
C6 C 0.6149(11) 0.5967(8) 0.3588(8) 0.076(3) Uani 1 1 d . . . . .
H6 H 0.5534 0.5515 0.3724 0.092 Uiso 1 1 calc R U . . .
N2 N 1.1363(7) 0.6830(4) 0.0179(5) 0.0509(17) Uani 1 1 d . . . . .
H1N H 1.1746 0.6144 0.0061 0.061 Uiso 1 1 calc R U . . .
N6 N 0.7845(7) 0.9753(5) -0.0089(5) 0.0556(17) Uani 1 1 d . . . . .
H5N H 0.8547 0.9254 0.0121 0.067 Uiso 1 1 calc R U . . .
N7 N 0.6294(7) 0.9776(5) 0.1554(5) 0.0591(18) Uani 1 1 d . . . . .
H6N H 0.7069 0.9232 0.1637 0.071 Uiso 1 1 calc R U . . .
N4 N 0.7679(7) 0.7119(5) -0.0870(5) 0.0558(18) Uani 1 1 d . . . . .
H3N H 0.7099 0.7789 -0.0848 0.067 Uiso 1 1 calc R U . . .
N3 N 0.9504(7) 0.6398(4) 0.1530(5) 0.0561(18) Uani 1 1 d . . . . .
H2N H 0.9929 0.5757 0.1275 0.067 Uiso 1 1 calc R U . . .
N5 N 0.5642(7) 0.6887(4) 0.0465(5) 0.0579(18) Uani 1 1 d . . . . .
H4N H 0.5198 0.7567 0.0375 0.069 Uiso 1 1 calc R U . . .
O2 O 0.7955(6) 0.5475(4) -0.0112(4) 0.0620(16) Uani 1 1 d . . . . .
O1 O 0.9429(6) 0.8163(4) 0.1227(4) 0.0565(14) Uani 1 1 d . . . . .
O3 O 0.5422(6) 1.1018(4) 0.0379(4) 0.0586(15) Uani 1 1 d . . . . .


_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
Br2 C16 1.893(8) . ?
Br3 C25 1.885(9) . ?
Br1 C7 1.877(9) . ?
N1 C1 1.454(9) . ?
N1 C10 1.460(9) . ?
N1 C19 1.461(9) . ?
C3 O1 1.245(8) . ?
C3 N2 1.337(9) . ?
C3 N3 1.370(8) . ?
C12 O2 1.237(8) . ?
C12 N4 1.348(9) . ?
C12 N5 1.361(9) . ?
C21 O3 1.263(8) . ?
C21 N6 1.322(9) . ?
C21 N7 1.364(9) . ?
C14 C15 1.374(10) . ?
C14 C13 1.388(9) . ?
C22 C23 1.375(10) . ?
C22 C27 1.387(10) . ?
C22 N7 1.397(9) . ?
C11 N4 1.471(9) . ?
C11 C10 1.503(10) . ?
C13 C18 1.382(10) . ?
C13 N5 1.411(9) . ?
C27 C26 1.411(11) . ?
C23 C24 1.377(11) . ?
C4 C9 1.372(10) . ?
C4 C5 1.386(10) . ?
C4 N3 1.404(9) . ?
C15 C16 1.359(11) . ?
C1 C2 1.521(10) . ?
C25 C26 1.353(11) . ?
C25 C24 1.394(12) . ?
C18 C17 1.393(10) . ?
C20 N6 1.451(9) . ?
C20 C19 1.517(10) . ?
C16 C17 1.353(10) . ?
C2 N2 1.446(8) . ?
C9 C8 1.390(11) . ?
C5 C6 1.374(12) . ?
C8 C7 1.394(12) . ?
C7 C6 1.379(12) . ?

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 C10 112.8(6) . . ?
C1 N1 C19 112.9(5) . . ?
C10 N1 C19 111.3(6) . . ?
O1 C3 N2 123.6(6) . . ?
O1 C3 N3 121.6(7) . . ?
N2 C3 N3 114.8(6) . . ?
O2 C12 N4 121.3(7) . . ?
O2 C12 N5 124.6(7) . . ?
N4 C12 N5 114.1(7) . . ?
O3 C21 N6 122.1(8) . . ?
O3 C21 N7 122.8(7) . . ?
N6 C21 N7 115.1(7) . . ?
C15 C14 C13 120.2(7) . . ?
C23 C22 C27 119.1(8) . . ?
C23 C22 N7 118.9(7) . . ?
C27 C22 N7 122.0(7) . . ?
N4 C11 C10 112.2(6) . . ?
C18 C13 C14 118.5(7) . . ?
C18 C13 N5 117.5(7) . . ?
C14 C13 N5 123.9(7) . . ?
C22 C27 C26 119.3(8) . . ?
C22 C23 C24 121.6(8) . . ?
C9 C4 C5 118.7(8) . . ?
C9 C4 N3 122.4(7) . . ?
C5 C4 N3 118.9(8) . . ?
C16 C15 C14 120.9(7) . . ?
N1 C1 C2 111.2(6) . . ?
N1 C10 C11 112.5(7) . . ?
C26 C25 C24 120.3(8) . . ?
C26 C25 Br3 119.9(7) . . ?
C24 C25 Br3 119.8(7) . . ?
C13 C18 C17 120.0(7) . . ?
N6 C20 C19 109.0(6) . . ?
C23 C24 C25 119.1(8) . . ?
C17 C16 C15 120.0(7) . . ?
C17 C16 Br2 119.5(6) . . ?
C15 C16 Br2 120.5(6) . . ?
C25 C26 C27 120.5(8) . . ?
C16 C17 C18 120.4(7) . . ?
N2 C2 C1 112.7(6) . . ?
N1 C19 C20 112.5(6) . . ?
C4 C9 C8 121.5(8) . . ?
C6 C5 C4 120.6(9) . . ?
C9 C8 C7 119.2(9) . . ?
C6 C7 C8 119.2(9) . . ?
C6 C7 Br1 121.2(8) . . ?
C8 C7 Br1 119.6(8) . . ?
C5 C6 C7 120.8(9) . . ?
C3 N2 C2 123.6(6) . . ?
C21 N6 C20 125.0(7) . . ?
C21 N7 C22 126.3(6) . . ?
C12 N4 C11 123.6(6) . . ?
C3 N3 C4 126.4(6) . . ?
C12 N5 C13 127.1(6) . . ?

_refine_diff_density_max         0.658
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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-p-Cl-TBASO4
_database_code_depnum_ccdc_archive 'CCDC 1832722'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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(C27 H30 Cl3 N7 O3), 2(C16 H36 N), O4 S, O'
_chemical_formula_sum            'C86 H132 Cl6 N16 O11 S'
_chemical_formula_weight         1810.84

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'
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/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   17.9510(8)
_cell_length_b                   21.3843(9)
_cell_length_c                   26.2654(9)
_cell_angle_alpha                90
_cell_angle_beta                 97.717(4)
_cell_angle_gamma                90
_cell_volume                     9991.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5526
_cell_measurement_theta_min      3.4100
_cell_measurement_theta_max      20.7350

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_F_000             3864.0
_exptl_transmission_factor_min   0.929
_exptl_transmission_factor_max   0.950
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.254
_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            41701
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.979
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17572
_reflns_number_gt                7559
_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+8.4557P] 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         17572
_refine_ls_number_parameters     1089
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.2433
_refine_ls_wR_factor_gt          0.1770
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.005
_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
S1 S 0.45591(6) 0.46286(6) 0.24978(4) 0.0547(3) Uani 1 1 d . . . . .
Cl4 Cl 0.31304(12) 0.08645(8) 0.22711(6) 0.1211(7) Uani 1 1 d . . . . .
Cl6 Cl 0.82467(11) 0.57300(10) 0.46477(7) 0.1302(7) Uani 1 1 d . . . . .
Cl5 Cl 0.14138(10) 0.70519(10) 0.08160(8) 0.1364(7) Uani 1 1 d . . . . .
Cl2 Cl 0.05830(13) 0.52986(10) 0.05456(8) 0.1535(9) Uani 1 1 d . . . . .
Cl3 Cl 0.54565(17) 0.08494(14) 0.22364(13) 0.2159(14) Uani 1 1 d . . . . .
O2 O 0.15719(18) 0.39095(18) 0.28856(13) 0.0823(11) Uani 1 1 d . . . . .
O3 O 0.5121(2) 0.28944(18) 0.41767(13) 0.0859(11) Uani 1 1 d . . . . .
O7 O 0.51034(19) 0.45230(18) 0.29589(13) 0.0856(11) Uani 1 1 d . . . . .
O9 O 0.39991(19) 0.41313(18) 0.24506(15) 0.0950(12) Uani 1 1 d . . . . .
N10 N 0.3926(2) 0.33477(19) 0.15260(14) 0.0689(11) Uani 1 1 d . . . . .
H10N H 0.3996 0.3623 0.1766 0.083 Uiso 1 1 calc R U . . .
Cl1 Cl 0.78275(16) 0.71127(15) 0.3652(2) 0.299(2) Uani 1 1 d . . . . .
O4 O 0.3873(3) 0.32337(18) 0.06610(13) 0.0987(13) Uani 1 1 d . . . . .
O8 O 0.4957(2) 0.46114(19) 0.20440(13) 0.0939(12) Uani 1 1 d . . . . .
N6 N 0.4942(2) 0.3916(2) 0.39614(16) 0.0739(12) Uani 1 1 d . . . . .
H6N H 0.4965 0.4195 0.3729 0.089 Uiso 1 1 calc R U . . .
N1 N 0.3424(2) 0.4309(2) 0.41733(14) 0.0699(11) Uani 1 1 d . . . . .
O5 O 0.5152(2) 0.63961(19) 0.09698(16) 0.1011(13) Uani 1 1 d . . . . .
O10 O 0.4213(3) 0.52387(18) 0.25253(14) 0.1063(13) Uani 1 1 d . . . . .
N16 N 0.6131(2) 0.20651(18) 0.54587(15) 0.0682(11) Uani 1 1 d . . . . .
N5 N 0.2420(2) 0.4279(2) 0.23811(15) 0.0702(12) Uani 1 1 d . . . . .
H5N H 0.2895 0.4325 0.2375 0.084 Uiso 1 1 calc R U . . .
O1 O 0.4416(2) 0.61002(19) 0.42243(15) 0.0985(13) Uani 1 1 d . . . . .
N15 N 0.9647(2) 0.3520(2) 0.36464(16) 0.0684(11) Uani 1 1 d . . . . .
N4 N 0.2813(2) 0.3802(2) 0.31379(15) 0.0751(12) Uani 1 1 d . . . . .
H4N H 0.3256 0.3854 0.3055 0.090 Uiso 1 1 calc R U . . .
N11 N 0.5612(2) 0.5645(2) 0.15367(16) 0.0766(12) Uani 1 1 d . . . . .
H11N H 0.5561 0.5458 0.1820 0.092 Uiso 1 1 calc R U . . .
N9 N 0.4373(2) 0.4110(2) 0.10497(15) 0.0774(12) Uani 1 1 d . . . . .
H9N H 0.4420 0.4330 0.1326 0.093 Uiso 1 1 calc R U . . .
N7 N 0.5122(2) 0.3201(2) 0.33426(17) 0.0775(12) Uani 1 1 d . . . . .
H7N H 0.5091 0.3525 0.3147 0.093 Uiso 1 1 calc R U . . .
O6 O 0.7624(2) 0.4098(2) 0.23994(17) 0.1085(14) Uani 1 1 d . . . . .
N8 N 0.5970(2) 0.4496(2) 0.09849(16) 0.0721(12) Uani 1 1 d . . . . .
N12 N 0.4398(3) 0.5968(2) 0.15114(18) 0.0908(14) Uani 1 1 d . . . . .
H12N H 0.4409 0.5737 0.1780 0.109 Uiso 1 1 calc R U . . .
C31 C 0.3707(2) 0.2754(2) 0.16717(17) 0.0577(12) Uani 1 1 d . . . . .
N14 N 0.6680(2) 0.4482(2) 0.28084(18) 0.0843(13) Uani 1 1 d . . . . .
H14N H 0.6199 0.4508 0.2789 0.101 Uiso 1 1 calc R U . . .
N2 N 0.3759(3) 0.5486(2) 0.36229(17) 0.0805(13) Uani 1 1 d . . . . .
H2N H 0.3746 0.5307 0.3329 0.097 Uiso 1 1 calc R U . . .
N13 N 0.6411(3) 0.3996(2) 0.20353(18) 0.0838(13) Uani 1 1 d . . . . .
H13N H 0.5949 0.4063 0.2072 0.101 Uiso 1 1 calc R U . . .
N3 N 0.4881(3) 0.5884(2) 0.34776(19) 0.0896(14) Uani 1 1 d . . . . .
H3N H 0.4773 0.5694 0.3189 0.107 Uiso 1 1 calc R U . . .
C21 C 0.5065(3) 0.3313(3) 0.3854(2) 0.0689(14) Uani 1 1 d . . . . .
C12 C 0.2217(3) 0.3995(2) 0.2808(2) 0.0663(13) Uani 1 1 d . . . . .
C30 C 0.4044(3) 0.3543(3) 0.1047(2) 0.0688(14) Uani 1 1 d . . . . .
C36 C 0.3641(3) 0.2237(3) 0.13551(19) 0.0739(15) Uani 1 1 d . . . . .
H36 H 0.3720 0.2276 0.1014 0.089 Uiso 1 1 calc R U . . .
C13 C 0.1953(3) 0.4504(2) 0.19569(19) 0.0643(13) Uani 1 1 d . . . . .
C18 C 0.1187(3) 0.4609(2) 0.1945(2) 0.0754(15) Uani 1 1 d . . . . .
H18 H 0.0954 0.4516 0.2231 0.090 Uiso 1 1 calc R U . . .
C22 C 0.5222(3) 0.2633(3) 0.3101(2) 0.0738(14) Uani 1 1 d . . . . .
C32 C 0.3581(3) 0.2672(3) 0.21786(18) 0.0683(13) Uani 1 1 d . . . . .
H32 H 0.3626 0.3013 0.2400 0.082 Uiso 1 1 calc R U . . .
C49 C 0.7091(3) 0.4748(3) 0.3237(2) 0.0727(15) Uani 1 1 d . . . . .
C67 C 1.0101(3) 0.3087(2) 0.4030(2) 0.0733(14) Uani 1 1 d . . . . .
H67A H 0.9981 0.2659 0.3928 0.088 Uiso 1 1 calc R U . . .
H67B H 1.0630 0.3151 0.4007 0.088 Uiso 1 1 calc R U . . .
C40 C 0.3701(3) 0.6238(3) 0.1334(2) 0.0778(15) Uani 1 1 d . . . . .
C19 C 0.3963(3) 0.3957(3) 0.45313(18) 0.0783(15) Uani 1 1 d . . . . .
H19A H 0.3873 0.3513 0.4478 0.094 Uiso 1 1 calc R U . . .
H19B H 0.3885 0.4055 0.4881 0.094 Uiso 1 1 calc R U . . .
C3 C 0.4355(4) 0.5840(3) 0.3802(2) 0.0759(15) Uani 1 1 d . . . . .
C35 C 0.3459(3) 0.1661(3) 0.1541(2) 0.0831(16) Uani 1 1 d . . . . .
H35 H 0.3412 0.1316 0.1324 0.100 Uiso 1 1 calc R U . . .
C48 C 0.6955(3) 0.4182(3) 0.2411(2) 0.0785(15) Uani 1 1 d . . . . .
C33 C 0.3394(3) 0.2103(3) 0.2358(2) 0.0773(15) Uani 1 1 d . . . . .
H33 H 0.3298 0.2060 0.2696 0.093 Uiso 1 1 calc R U . . .
C10 C 0.2714(3) 0.3978(3) 0.4054(2) 0.0836(17) Uani 1 1 d . . . . .
H10A H 0.2315 0.4278 0.3954 0.100 Uiso 1 1 calc R U . . .
H10B H 0.2599 0.3762 0.4359 0.100 Uiso 1 1 calc R U . . .
C34 C 0.3347(3) 0.1596(3) 0.2039(2) 0.0759(15) Uani 1 1 d . . . . .
C83 C 0.6299(3) 0.2683(2) 0.5218(2) 0.0771(15) Uani 1 1 d . . . . .
H83A H 0.6065 0.2680 0.4863 0.092 Uiso 1 1 calc R U . . .
H83B H 0.6061 0.3012 0.5393 0.092 Uiso 1 1 calc R U . . .
C71 C 0.6446(3) 0.2029(2) 0.60199(18) 0.0764(15) Uani 1 1 d . . . . .
H71A H 0.6333 0.1618 0.6145 0.092 Uiso 1 1 calc R U . . .
H71B H 0.6989 0.2063 0.6047 0.092 Uiso 1 1 calc R U . . .
C50 C 0.7786(3) 0.5029(3) 0.3232(2) 0.0797(16) Uani 1 1 d . . . . .
H50 H 0.8017 0.5019 0.2936 0.096 Uiso 1 1 calc R U . . .
C55 C 0.9889(3) 0.3399(3) 0.31286(19) 0.0733(14) Uani 1 1 d . . . . .
H55A H 0.9776 0.2968 0.3035 0.088 Uiso 1 1 calc R U . . .
H55B H 1.0430 0.3451 0.3157 0.088 Uiso 1 1 calc R U . . .
C39 C 0.5063(3) 0.6020(3) 0.1317(2) 0.0781(15) Uani 1 1 d . . . . .
C54 C 0.6771(3) 0.4770(3) 0.3689(2) 0.0816(16) Uani 1 1 d . . . . .
H54 H 0.6311 0.4575 0.3703 0.098 Uiso 1 1 calc R U . . .
C27 C 0.5060(3) 0.2071(3) 0.3305(2) 0.0909(17) Uani 1 1 d . . . . .
H27 H 0.4898 0.2055 0.3626 0.109 Uiso 1 1 calc R U . . .
C1 C 0.3327(3) 0.4945(3) 0.4356(2) 0.0854(17) Uani 1 1 d . . . . .
H1A H 0.3784 0.5077 0.4568 0.102 Uiso 1 1 calc R U . . .
H1B H 0.2923 0.4951 0.4567 0.102 Uiso 1 1 calc R U . . .
C17 C 0.0775(3) 0.4850(3) 0.1512(3) 0.0900(17) Uani 1 1 d . . . . .
H17 H 0.0262 0.4916 0.1506 0.108 Uiso 1 1 calc R U . . .
C20 C 0.4770(3) 0.4101(3) 0.4465(2) 0.0823(16) Uani 1 1 d . . . . .
H20A H 0.4858 0.4547 0.4510 0.099 Uiso 1 1 calc R U . . .
H20B H 0.5104 0.3884 0.4727 0.099 Uiso 1 1 calc R U . . .
C37 C 0.6152(3) 0.5128(3) 0.0838(2) 0.0849(17) Uani 1 1 d . . . . .
H37A H 0.5742 0.5294 0.0598 0.102 Uiso 1 1 calc R U . . .
H37B H 0.6598 0.5118 0.0667 0.102 Uiso 1 1 calc R U . . .
C14 C 0.2278(3) 0.4649(3) 0.1525(2) 0.0802(16) Uani 1 1 d . . . . .
H14 H 0.2790 0.4582 0.1525 0.096 Uiso 1 1 calc R U . . .
C63 C 0.9790(3) 0.4200(2) 0.3802(2) 0.0799(15) Uani 1 1 d . . . . .
H63A H 0.9527 0.4465 0.3537 0.096 Uiso 1 1 calc R U . . .
H63B H 0.9575 0.4276 0.4116 0.096 Uiso 1 1 calc R U . . .
C79 C 0.6476(3) 0.1524(2) 0.5197(2) 0.0808(16) Uani 1 1 d . . . . .
H79A H 0.7018 0.1560 0.5272 0.097 Uiso 1 1 calc R U . . .
H79B H 0.6334 0.1139 0.5356 0.097 Uiso 1 1 calc R U . . .
C75 C 0.5283(3) 0.2021(3) 0.5387(2) 0.0833(16) Uani 1 1 d . . . . .
H75A H 0.5088 0.2386 0.5543 0.100 Uiso 1 1 calc R U . . .
H75B H 0.5106 0.2038 0.5021 0.100 Uiso 1 1 calc R U . . .
C2 C 0.3145(3) 0.5400(3) 0.3910(2) 0.0902(18) Uani 1 1 d . . . . .
H2A H 0.2715 0.5245 0.3683 0.108 Uiso 1 1 calc R U . . .
H2B H 0.3009 0.5801 0.4043 0.108 Uiso 1 1 calc R U . . .
C72 C 0.6175(3) 0.2507(3) 0.63735(19) 0.0884(17) Uani 1 1 d . . . . .
H72A H 0.6346 0.2920 0.6287 0.106 Uiso 1 1 calc R U . . .
H72B H 0.5630 0.2511 0.6329 0.106 Uiso 1 1 calc R U . . .
C38 C 0.6289(3) 0.5550(3) 0.1305(2) 0.0851(17) Uani 1 1 d . . . . .
H38A H 0.6672 0.5366 0.1556 0.102 Uiso 1 1 calc R U . . .
H38B H 0.6474 0.5951 0.1204 0.102 Uiso 1 1 calc R U . . .
C51 C 0.8135(3) 0.5323(3) 0.3666(3) 0.0877(17) Uani 1 1 d . . . . .
H51 H 0.8602 0.5509 0.3660 0.105 Uiso 1 1 calc R U . . .
C59 C 0.8806(3) 0.3406(3) 0.3631(2) 0.0910(18) Uani 1 1 d . . . . .
H59A H 0.8677 0.3459 0.3976 0.109 Uiso 1 1 calc R U . . .
H59B H 0.8537 0.3723 0.3416 0.109 Uiso 1 1 calc R U . . .
C29 C 0.4648(3) 0.4354(3) 0.0595(2) 0.0869(17) Uani 1 1 d . . . . .
H29A H 0.4593 0.4805 0.0587 0.104 Uiso 1 1 calc R U . . .
H29B H 0.4348 0.4186 0.0291 0.104 Uiso 1 1 calc R U . . .
C43 C 0.2295(4) 0.6723(3) 0.1010(3) 0.0964(19) Uani 1 1 d . . . . .
C16 C 0.1109(4) 0.4994(3) 0.1092(3) 0.0939(19) Uani 1 1 d . . . . .
C68 C 0.9981(3) 0.3163(3) 0.4584(2) 0.0892(17) Uani 1 1 d . . . . .
H68A H 0.9464 0.3058 0.4619 0.107 Uiso 1 1 calc R U . . .
H68B H 1.0063 0.3597 0.4684 0.107 Uiso 1 1 calc R U . . .
C52 C 0.7805(3) 0.5345(3) 0.4109(2) 0.0851(16) Uani 1 1 d . . . . .
C28 C 0.5465(4) 0.4187(3) 0.0583(2) 0.0933(19) Uani 1 1 d . . . . .
H28A H 0.5524 0.3738 0.0622 0.112 Uiso 1 1 calc R U . . .
H28B H 0.5604 0.4302 0.0252 0.112 Uiso 1 1 calc R U . . .
C84 C 0.7104(4) 0.2846(3) 0.5227(2) 0.0972(18) Uani 1 1 d . . . . .
H84A H 0.7366 0.2508 0.5081 0.117 Uiso 1 1 calc R U . . .
H84B H 0.7336 0.2911 0.5578 0.117 Uiso 1 1 calc R U . . .
C15 C 0.1858(4) 0.4892(3) 0.1093(2) 0.0935(18) Uani 1 1 d . . . . .
H15 H 0.2085 0.4985 0.0804 0.112 Uiso 1 1 calc R U . . .
C11 C 0.2738(3) 0.3511(3) 0.3627(2) 0.0860(17) Uani 1 1 d . . . . .
H11A H 0.3158 0.3229 0.3719 0.103 Uiso 1 1 calc R U . . .
H11B H 0.2281 0.3264 0.3591 0.103 Uiso 1 1 calc R U . . .
C4 C 0.5563(4) 0.6188(3) 0.3543(3) 0.0940(18) Uani 1 1 d . . . . .
C41 C 0.3126(4) 0.6155(3) 0.1612(2) 0.0841(16) Uani 1 1 d . . . . .
H41 H 0.3209 0.5934 0.1919 0.101 Uiso 1 1 calc R U . . .
C53 C 0.7122(3) 0.5073(3) 0.4116(2) 0.0928(18) Uani 1 1 d . . . . .
H53 H 0.6890 0.5094 0.4411 0.111 Uiso 1 1 calc R U . . .
C42 C 0.2426(4) 0.6389(3) 0.1450(3) 0.0937(19) Uani 1 1 d . . . . .
H42 H 0.2037 0.6318 0.1643 0.112 Uiso 1 1 calc R U . . .
C64 C 1.0608(3) 0.4391(3) 0.3888(2) 0.0881(17) Uani 1 1 d . . . . .
H64A H 1.0844 0.4263 0.3594 0.106 Uiso 1 1 calc R U . . .
H64B H 1.0858 0.4173 0.4187 0.106 Uiso 1 1 calc R U . . .
C73 C 0.6465(3) 0.2361(3) 0.6919(2) 0.0975(19) Uani 1 1 d . . . . .
H73A H 0.7009 0.2341 0.6957 0.117 Uiso 1 1 calc R U . . .
H73B H 0.6281 0.1953 0.7004 0.117 Uiso 1 1 calc R U . . .
C46 C 0.6661(4) 0.4135(3) 0.1152(3) 0.100(2) Uani 1 1 d . . . . .
H46A H 0.7067 0.4423 0.1263 0.120 Uiso 1 1 calc R U . . .
H46B H 0.6796 0.3902 0.0861 0.120 Uiso 1 1 calc R U . . .
C23 C 0.5448(3) 0.2643(4) 0.2624(3) 0.0965(19) Uani 1 1 d . . . . .
H23 H 0.5556 0.3024 0.2480 0.116 Uiso 1 1 calc R U . . .
C56 C 0.9526(3) 0.3818(3) 0.2699(2) 0.0933(18) Uani 1 1 d . . . . .
H56A H 0.8995 0.3857 0.2726 0.112 Uiso 1 1 calc R U . . .
H56B H 0.9748 0.4232 0.2740 0.112 Uiso 1 1 calc R U . . .
C47 C 0.6577(4) 0.3691(3) 0.1577(2) 0.0977(19) Uani 1 1 d . . . . .
H47A H 0.6177 0.3398 0.1463 0.117 Uiso 1 1 calc R U . . .
H47B H 0.7039 0.3455 0.1656 0.117 Uiso 1 1 calc R U . . .
C69 C 1.0504(4) 0.2752(3) 0.4942(2) 0.104(2) Uani 1 1 d . . . . .
H69A H 1.0426 0.2319 0.4838 0.125 Uiso 1 1 calc R U . . .
H69B H 1.1020 0.2860 0.4908 0.125 Uiso 1 1 calc R U . . .
C60 C 0.8535(3) 0.2779(3) 0.3437(2) 0.099(2) Uani 1 1 d . . . . .
H60A H 0.8785 0.2451 0.3651 0.119 Uiso 1 1 calc R U . . .
H60B H 0.8640 0.2718 0.3088 0.119 Uiso 1 1 calc R U . . .
C76 C 0.4950(3) 0.1447(3) 0.5603(2) 0.0986(19) Uani 1 1 d . . . . .
H76A H 0.5129 0.1415 0.5968 0.118 Uiso 1 1 calc R U . . .
H76B H 0.5111 0.1076 0.5435 0.118 Uiso 1 1 calc R U . . .
C85 C 0.7157(4) 0.3457(3) 0.4907(3) 0.107(2) Uani 1 1 d . . . . .
H85A H 0.6986 0.3373 0.4547 0.129 Uiso 1 1 calc R U . . .
H85B H 0.6834 0.3775 0.5023 0.129 Uiso 1 1 calc R U . . .
C45 C 0.3560(4) 0.6564(4) 0.0879(3) 0.130(3) Uani 1 1 d . . . . .
H45 H 0.3943 0.6618 0.0677 0.156 Uiso 1 1 calc R U . . .
C9 C 0.5964(4) 0.6187(3) 0.3129(3) 0.118(2) Uani 1 1 d . . . . .
H9 H 0.5761 0.5994 0.2825 0.141 Uiso 1 1 calc R U . . .
C26 C 0.5136(4) 0.1523(3) 0.3036(3) 0.115(2) Uani 1 1 d . . . . .
H26 H 0.5034 0.1140 0.3180 0.138 Uiso 1 1 calc R U . . .
C5 C 0.5858(5) 0.6488(3) 0.3989(3) 0.115(2) Uani 1 1 d . . . . .
H5 H 0.5588 0.6498 0.4267 0.138 Uiso 1 1 calc R U . . .
C25 C 0.5360(4) 0.1544(5) 0.2563(4) 0.128(3) Uani 1 1 d . . . . .
C70 C 1.0389(4) 0.2815(3) 0.5495(2) 0.129(3) Uani 1 1 d . . . . .
H70A H 1.0465 0.3242 0.5601 0.194 Uiso 1 1 calc R U . . .
H70B H 1.0742 0.2553 0.5703 0.194 Uiso 1 1 calc R U . . .
H70C H 0.9887 0.2690 0.5534 0.194 Uiso 1 1 calc R U . . .
C80 C 0.6281(4) 0.1454(3) 0.4628(2) 0.107(2) Uani 1 1 d . . . . .
H80A H 0.6388 0.1838 0.4456 0.128 Uiso 1 1 calc R U . . .
H80B H 0.5750 0.1359 0.4541 0.128 Uiso 1 1 calc R U . . .
C24 C 0.5520(4) 0.2100(5) 0.2353(3) 0.124(3) Uani 1 1 d . . . . .
H24 H 0.5676 0.2113 0.2029 0.149 Uiso 1 1 calc R U . . .
C6 C 0.6560(7) 0.6777(5) 0.4025(5) 0.166(5) Uani 1 1 d . . . . .
H6 H 0.6766 0.6974 0.4327 0.199 Uiso 1 1 calc R U . . .
C44 C 0.2854(4) 0.6813(4) 0.0720(3) 0.132(3) Uani 1 1 d . . . . .
H44 H 0.2765 0.7041 0.0416 0.159 Uiso 1 1 calc R U . . .
C65 C 1.0715(4) 0.5092(3) 0.3967(3) 0.131(3) Uani 1 1 d . . . . .
H65A H 1.1251 0.5177 0.4018 0.157 Uiso 1 1 calc R U . . .
H65B H 1.0506 0.5300 0.3651 0.157 Uiso 1 1 calc R U . . .
C57 C 0.9618(4) 0.3574(4) 0.2175(2) 0.118(2) Uani 1 1 d . . . . .
H57A H 0.9503 0.3907 0.1926 0.142 Uiso 1 1 calc R U . . .
H57B H 1.0138 0.3453 0.2172 0.142 Uiso 1 1 calc R U . . .
C86 C 0.7940(4) 0.3687(4) 0.4966(3) 0.137(3) Uani 1 1 d . . . . .
H86A H 0.8094 0.3802 0.5317 0.205 Uiso 1 1 calc R U . . .
H86B H 0.7971 0.4045 0.4749 0.205 Uiso 1 1 calc R U . . .
H86C H 0.8263 0.3363 0.4869 0.205 Uiso 1 1 calc R U . . .
C74 C 0.6235(4) 0.2836(3) 0.7294(2) 0.132(3) Uani 1 1 d . . . . .
H74A H 0.6449 0.3235 0.7230 0.198 Uiso 1 1 calc R U . . .
H74B H 0.6413 0.2705 0.7638 0.198 Uiso 1 1 calc R U . . .
H74C H 0.5697 0.2869 0.7251 0.198 Uiso 1 1 calc R U . . .
C81 C 0.6772(5) 0.0901(3) 0.4453(3) 0.139(3) Uani 1 1 d . . . . .
H81A H 0.7299 0.1016 0.4518 0.167 Uiso 1 1 calc R U . . .
H81B H 0.6701 0.0532 0.4656 0.167 Uiso 1 1 calc R U . . .
C77 C 0.4093(4) 0.1485(4) 0.5522(3) 0.136(3) Uani 1 1 d . . . . .
H77A H 0.3937 0.1850 0.5699 0.163 Uiso 1 1 calc R U . . .
H77B H 0.3921 0.1538 0.5158 0.163 Uiso 1 1 calc R U . . .
C61 C 0.7670(4) 0.2755(4) 0.3455(4) 0.156(3) Uani 1 1 d . . . . .
H61A H 0.7572 0.2806 0.3807 0.187 Uiso 1 1 calc R U . . .
H61B H 0.7428 0.3096 0.3253 0.187 Uiso 1 1 calc R U . . .
C58 C 0.9130(5) 0.3033(4) 0.2021(3) 0.149(3) Uani 1 1 d . . . . .
H58A H 0.9243 0.2700 0.2264 0.224 Uiso 1 1 calc R U . . .
H58B H 0.9216 0.2894 0.1686 0.224 Uiso 1 1 calc R U . . .
H58C H 0.8613 0.3153 0.2011 0.224 Uiso 1 1 calc R U . . .
C66 C 1.0406(5) 0.5366(4) 0.4367(4) 0.169(4) Uani 1 1 d . . . . .
H66A H 0.9868 0.5337 0.4301 0.254 Uiso 1 1 calc R U . . .
H66B H 1.0552 0.5798 0.4395 0.254 Uiso 1 1 calc R U . . .
H66C H 1.0584 0.5153 0.4681 0.254 Uiso 1 1 calc R U . . .
C82 C 0.6581(5) 0.0754(4) 0.3918(4) 0.173(4) Uani 1 1 d . . . . .
H82A H 0.6054 0.0661 0.3849 0.259 Uiso 1 1 calc R U . . .
H82B H 0.6866 0.0398 0.3835 0.259 Uiso 1 1 calc R U . . .
H82C H 0.6694 0.1105 0.3715 0.259 Uiso 1 1 calc R U . . .
C78 C 0.3725(5) 0.0916(5) 0.5712(4) 0.188(4) Uani 1 1 d . . . . .
H78A H 0.3938 0.0547 0.5581 0.281 Uiso 1 1 calc R U . . .
H78B H 0.3195 0.0928 0.5595 0.281 Uiso 1 1 calc R U . . .
H78C H 0.3808 0.0908 0.6080 0.281 Uiso 1 1 calc R U . . .
C62 C 0.7369(5) 0.2183(5) 0.3261(5) 0.240(6) Uani 1 1 d . . . . .
H62A H 0.7427 0.2149 0.2904 0.360 Uiso 1 1 calc R U . . .
H62B H 0.6844 0.2165 0.3298 0.360 Uiso 1 1 calc R U . . .
H62C H 0.7629 0.1844 0.3448 0.360 Uiso 1 1 calc R U . . .
C8 C 0.6666(5) 0.6470(4) 0.3161(5) 0.156(4) Uani 1 1 d . . . . .
H8 H 0.6942 0.6459 0.2886 0.187 Uiso 1 1 calc R U . . .
C7 C 0.6938(6) 0.6765(5) 0.3608(7) 0.169(6) Uani 1 1 d . . . . .
O11 O 0.3684(2) 0.3122(2) 0.95932(14) 0.1061(13) Uani 1 1 d . . . . .


_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 O10 1.451(4) . ?
S1 O9 1.457(4) . ?
S1 O7 1.468(3) . ?
S1 O8 1.470(3) . ?
Cl4 C34 1.741(5) . ?
Cl6 C52 1.734(6) . ?
Cl5 C43 1.743(7) . ?
Cl2 C16 1.734(6) . ?
Cl3 C25 1.737(8) . ?
O2 C12 1.216(5) . ?
O3 C21 1.228(6) . ?
N10 C30 1.368(6) . ?
N10 C31 1.398(6) . ?
N10 H10N 0.8600 . ?
Cl1 C7 1.750(11) . ?
O4 C30 1.216(6) . ?
N6 C21 1.344(6) . ?
N6 C20 1.453(6) . ?
N6 H6N 0.8600 . ?
N1 C10 1.455(6) . ?
N1 C1 1.461(6) . ?
N1 C19 1.465(6) . ?
O5 C39 1.243(6) . ?
N16 C71 1.508(6) . ?
N16 C75 1.511(6) . ?
N16 C83 1.511(6) . ?
N16 C79 1.521(6) . ?
N5 C12 1.369(6) . ?
N5 C13 1.387(6) . ?
N5 H5N 0.8600 . ?
O1 C3 1.233(6) . ?
N15 C55 1.505(6) . ?
N15 C63 1.522(6) . ?
N15 C67 1.522(6) . ?
N15 C59 1.526(6) . ?
N4 C12 1.347(6) . ?
N4 C11 1.451(6) . ?
N4 H4N 0.8600 . ?
N11 C39 1.340(6) . ?
N11 C38 1.445(6) . ?
N11 H11N 0.8600 . ?
N9 C30 1.347(6) . ?
N9 C29 1.451(6) . ?
N9 H9N 0.8600 . ?
N7 C21 1.380(6) . ?
N7 C22 1.393(7) . ?
N7 H7N 0.8600 . ?
O6 C48 1.220(6) . ?
N8 C37 1.454(6) . ?
N8 C28 1.454(7) . ?
N8 C46 1.477(7) . ?
N12 C39 1.363(7) . ?
N12 C40 1.401(6) . ?
N12 H12N 0.8600 . ?
C31 C36 1.379(6) . ?
C31 C32 1.391(6) . ?
N14 C48 1.372(7) . ?
N14 C49 1.382(6) . ?
N14 H14N 0.8600 . ?
N2 C3 1.344(7) . ?
N2 C2 1.428(6) . ?
N2 H2N 0.8600 . ?
N13 C48 1.351(7) . ?
N13 C47 1.435(6) . ?
N13 H13N 0.8600 . ?
N3 C3 1.357(7) . ?
N3 C4 1.375(7) . ?
N3 H3N 0.8600 . ?
C36 C35 1.380(7) . ?
C36 H36 0.9300 . ?
C13 C14 1.381(6) . ?
C13 C18 1.389(7) . ?
C18 C17 1.371(7) . ?
C18 H18 0.9300 . ?
C22 C27 1.365(7) . ?
C22 C23 1.366(7) . ?
C32 C33 1.364(7) . ?
C32 H32 0.9300 . ?
C49 C50 1.386(7) . ?
C49 C54 1.389(7) . ?
C67 C68 1.508(7) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C40 C41 1.352(7) . ?
C40 C45 1.378(8) . ?
C19 C20 1.513(7) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C35 C34 1.357(7) . ?
C35 H35 0.9300 . ?
C33 C34 1.365(7) . ?
C33 H33 0.9300 . ?
C10 C11 1.505(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C83 C84 1.484(7) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C71 C72 1.505(7) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C50 C51 1.376(7) . ?
C50 H50 0.9300 . ?
C55 C56 1.517(7) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C54 C53 1.372(7) . ?
C54 H54 0.9300 . ?
C27 C26 1.383(8) . ?
C27 H27 0.9300 . ?
C1 C2 1.524(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C17 C16 1.361(8) . ?
C17 H17 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C37 C38 1.516(7) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9300 . ?
C63 C64 1.511(7) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C79 C80 1.496(7) . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C75 C76 1.509(7) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C72 C73 1.491(7) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C51 C52 1.375(7) . ?
C51 H51 0.9300 . ?
C59 C60 1.493(8) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C29 C28 1.512(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C43 C42 1.351(8) . ?
C43 C44 1.353(9) . ?
C16 C15 1.363(8) . ?
C68 C69 1.517(8) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C52 C53 1.360(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C84 C85 1.564(8) . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C15 H15 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C4 C5 1.377(9) . ?
C4 C9 1.383(9) . ?
C41 C42 1.367(8) . ?
C41 H41 0.9300 . ?
C53 H53 0.9300 . ?
C42 H42 0.9300 . ?
C64 C65 1.523(8) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C73 C74 1.509(8) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C46 C47 1.488(7) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C23 C24 1.378(9) . ?
C23 H23 0.9300 . ?
C56 C57 1.500(7) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C69 C70 1.501(8) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C60 C61 1.559(8) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C76 C77 1.528(9) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C85 C86 1.477(8) . ?
C85 H85A 0.9700 . ?
C85 H85B 0.9700 . ?
C45 C44 1.387(9) . ?
C45 H45 0.9300 . ?
C9 C8 1.390(10) . ?
C9 H9 0.9300 . ?
C26 C25 1.356(10) . ?
C26 H26 0.9300 . ?
C5 C6 1.395(12) . ?
C5 H5 0.9300 . ?
C25 C24 1.357(11) . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C80 C81 1.580(9) . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C24 H24 0.9300 . ?
C6 C7 1.364(15) . ?
C6 H6 0.9300 . ?
C44 H44 0.9300 . ?
C65 C66 1.382(9) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C57 C58 1.475(9) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C86 H86A 0.9600 . ?
C86 H86B 0.9600 . ?
C86 H86C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C81 C82 1.434(10) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C77 C78 1.502(10) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C61 C62 1.406(12) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C82 H82A 0.9600 . ?
C82 H82B 0.9600 . ?
C82 H82C 0.9600 . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C8 C7 1.365(15) . ?
C8 H8 0.9300 . ?

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 O9 111.4(2) . . ?
O10 S1 O7 109.8(2) . . ?
O9 S1 O7 109.5(2) . . ?
O10 S1 O8 108.7(2) . . ?
O9 S1 O8 108.5(2) . . ?
O7 S1 O8 108.9(2) . . ?
C30 N10 C31 127.8(4) . . ?
C30 N10 H10N 116.1 . . ?
C31 N10 H10N 116.1 . . ?
C21 N6 C20 121.0(5) . . ?
C21 N6 H6N 119.5 . . ?
C20 N6 H6N 119.5 . . ?
C10 N1 C1 112.6(4) . . ?
C10 N1 C19 111.9(4) . . ?
C1 N1 C19 111.4(4) . . ?
C71 N16 C75 111.0(4) . . ?
C71 N16 C83 112.5(4) . . ?
C75 N16 C83 104.9(4) . . ?
C71 N16 C79 106.3(4) . . ?
C75 N16 C79 111.1(4) . . ?
C83 N16 C79 111.1(4) . . ?
C12 N5 C13 127.8(4) . . ?
C12 N5 H5N 116.1 . . ?
C13 N5 H5N 116.1 . . ?
C55 N15 C63 110.4(4) . . ?
C55 N15 C67 107.5(4) . . ?
C63 N15 C67 110.3(4) . . ?
C55 N15 C59 110.7(4) . . ?
C63 N15 C59 106.9(4) . . ?
C67 N15 C59 111.0(4) . . ?
C12 N4 C11 122.6(4) . . ?
C12 N4 H4N 118.7 . . ?
C11 N4 H4N 118.7 . . ?
C39 N11 C38 120.9(5) . . ?
C39 N11 H11N 119.5 . . ?
C38 N11 H11N 119.5 . . ?
C30 N9 C29 121.2(4) . . ?
C30 N9 H9N 119.4 . . ?
C29 N9 H9N 119.4 . . ?
C21 N7 C22 128.7(5) . . ?
C21 N7 H7N 115.6 . . ?
C22 N7 H7N 115.6 . . ?
C37 N8 C28 111.8(4) . . ?
C37 N8 C46 110.8(4) . . ?
C28 N8 C46 113.2(5) . . ?
C39 N12 C40 129.0(5) . . ?
C39 N12 H12N 115.5 . . ?
C40 N12 H12N 115.5 . . ?
C36 C31 C32 117.6(5) . . ?
C36 C31 N10 124.6(4) . . ?
C32 C31 N10 117.7(4) . . ?
C48 N14 C49 127.1(5) . . ?
C48 N14 H14N 116.4 . . ?
C49 N14 H14N 116.4 . . ?
C3 N2 C2 121.5(5) . . ?
C3 N2 H2N 119.2 . . ?
C2 N2 H2N 119.2 . . ?
C48 N13 C47 122.3(5) . . ?
C48 N13 H13N 118.8 . . ?
C47 N13 H13N 118.8 . . ?
C3 N3 C4 129.5(6) . . ?
C3 N3 H3N 115.2 . . ?
C4 N3 H3N 115.2 . . ?
O3 C21 N6 123.6(5) . . ?
O3 C21 N7 122.4(5) . . ?
N6 C21 N7 114.0(5) . . ?
O2 C12 N4 122.7(5) . . ?
O2 C12 N5 124.6(5) . . ?
N4 C12 N5 112.7(4) . . ?
O4 C30 N9 123.6(5) . . ?
O4 C30 N10 123.3(5) . . ?
N9 C30 N10 113.1(5) . . ?
C31 C36 C35 120.5(5) . . ?
C31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C14 C13 N5 117.5(5) . . ?
C14 C13 C18 118.1(5) . . ?
N5 C13 C18 124.4(5) . . ?
C17 C18 C13 120.2(5) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
C27 C22 C23 118.6(6) . . ?
C27 C22 N7 122.8(5) . . ?
C23 C22 N7 118.5(6) . . ?
C33 C32 C31 121.5(5) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
N14 C49 C50 123.7(5) . . ?
N14 C49 C54 118.2(5) . . ?
C50 C49 C54 118.0(5) . . ?
C68 C67 N15 116.1(4) . . ?
C68 C67 H67A 108.3 . . ?
N15 C67 H67A 108.3 . . ?
C68 C67 H67B 108.3 . . ?
N15 C67 H67B 108.3 . . ?
H67A C67 H67B 107.4 . . ?
C41 C40 C45 118.1(6) . . ?
C41 C40 N12 118.6(5) . . ?
C45 C40 N12 123.3(5) . . ?
N1 C19 C20 112.4(4) . . ?
N1 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N1 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
O1 C3 N2 122.6(6) . . ?
O1 C3 N3 123.3(6) . . ?
N2 C3 N3 114.1(5) . . ?
C34 C35 C36 120.3(5) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
O6 C48 N13 123.8(6) . . ?
O6 C48 N14 123.0(6) . . ?
N13 C48 N14 113.2(5) . . ?
C32 C33 C34 119.6(5) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
N1 C10 C11 111.8(4) . . ?
N1 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
N1 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C35 C34 C33 120.4(5) . . ?
C35 C34 Cl4 119.8(5) . . ?
C33 C34 Cl4 119.8(4) . . ?
C84 C83 N16 116.6(5) . . ?
C84 C83 H83A 108.1 . . ?
N16 C83 H83A 108.1 . . ?
C84 C83 H83B 108.1 . . ?
N16 C83 H83B 108.1 . . ?
H83A C83 H83B 107.3 . . ?
C72 C71 N16 117.3(4) . . ?
C72 C71 H71A 108.0 . . ?
N16 C71 H71A 108.0 . . ?
C72 C71 H71B 108.0 . . ?
N16 C71 H71B 108.0 . . ?
H71A C71 H71B 107.2 . . ?
C51 C50 C49 120.1(5) . . ?
C51 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
N15 C55 C56 115.1(4) . . ?
N15 C55 H55A 108.5 . . ?
C56 C55 H55A 108.5 . . ?
N15 C55 H55B 108.5 . . ?
C56 C55 H55B 108.5 . . ?
H55A C55 H55B 107.5 . . ?
O5 C39 N11 122.9(5) . . ?
O5 C39 N12 122.2(5) . . ?
N11 C39 N12 114.9(5) . . ?
C53 C54 C49 121.1(5) . . ?
C53 C54 H54 119.4 . . ?
C49 C54 H54 119.4 . . ?
C22 C27 C26 120.3(6) . . ?
C22 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
N1 C1 C2 111.3(4) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C16 C17 C18 120.7(6) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
N6 C20 C19 111.9(4) . . ?
N6 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
N6 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
N8 C37 C38 110.9(4) . . ?
N8 C37 H37A 109.5 . . ?
C38 C37 H37A 109.5 . . ?
N8 C37 H37B 109.5 . . ?
C38 C37 H37B 109.5 . . ?
H37A C37 H37B 108.0 . . ?
C15 C14 C13 121.2(6) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C64 C63 N15 115.0(4) . . ?
C64 C63 H63A 108.5 . . ?
N15 C63 H63A 108.5 . . ?
C64 C63 H63B 108.5 . . ?
N15 C63 H63B 108.5 . . ?
H63A C63 H63B 107.5 . . ?
C80 C79 N16 118.2(5) . . ?
C80 C79 H79A 107.8 . . ?
N16 C79 H79A 107.8 . . ?
C80 C79 H79B 107.8 . . ?
N16 C79 H79B 107.8 . . ?
H79A C79 H79B 107.1 . . ?
C76 C75 N16 116.5(5) . . ?
C76 C75 H75A 108.2 . . ?
N16 C75 H75A 108.2 . . ?
C76 C75 H75B 108.2 . . ?
N16 C75 H75B 108.2 . . ?
H75A C75 H75B 107.3 . . ?
N2 C2 C1 112.8(4) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C73 C72 C71 110.5(5) . . ?
C73 C72 H72A 109.5 . . ?
C71 C72 H72A 109.5 . . ?
C73 C72 H72B 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 108.1 . . ?
N11 C38 C37 111.7(4) . . ?
N11 C38 H38A 109.3 . . ?
C37 C38 H38A 109.3 . . ?
N11 C38 H38B 109.3 . . ?
C37 C38 H38B 109.3 . . ?
H38A C38 H38B 107.9 . . ?
C52 C51 C50 121.1(5) . . ?
C52 C51 H51 119.5 . . ?
C50 C51 H51 119.5 . . ?
C60 C59 N15 115.4(5) . . ?
C60 C59 H59A 108.4 . . ?
N15 C59 H59A 108.4 . . ?
C60 C59 H59B 108.4 . . ?
N15 C59 H59B 108.4 . . ?
H59A C59 H59B 107.5 . . ?
N9 C29 C28 111.7(5) . . ?
N9 C29 H29A 109.3 . . ?
C28 C29 H29A 109.3 . . ?
N9 C29 H29B 109.3 . . ?
C28 C29 H29B 109.3 . . ?
H29A C29 H29B 107.9 . . ?
C42 C43 C44 120.0(7) . . ?
C42 C43 Cl5 120.7(6) . . ?
C44 C43 Cl5 119.3(6) . . ?
C17 C16 C15 120.2(6) . . ?
C17 C16 Cl2 120.4(6) . . ?
C15 C16 Cl2 119.3(6) . . ?
C67 C68 C69 112.2(5) . . ?
C67 C68 H68A 109.2 . . ?
C69 C68 H68A 109.2 . . ?
C67 C68 H68B 109.2 . . ?
C69 C68 H68B 109.2 . . ?
H68A C68 H68B 107.9 . . ?
C53 C52 C51 119.2(6) . . ?
C53 C52 Cl6 120.5(5) . . ?
C51 C52 Cl6 120.3(5) . . ?
N8 C28 C29 113.0(5) . . ?
N8 C28 H28A 109.0 . . ?
C29 C28 H28A 109.0 . . ?
N8 C28 H28B 109.0 . . ?
C29 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
C83 C84 C85 108.5(5) . . ?
C83 C84 H84A 110.0 . . ?
C85 C84 H84A 110.0 . . ?
C83 C84 H84B 110.0 . . ?
C85 C84 H84B 110.0 . . ?
H84A C84 H84B 108.4 . . ?
C16 C15 C14 119.6(6) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
N4 C11 C10 112.9(5) . . ?
N4 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
N4 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N3 C4 C5 124.1(7) . . ?
N3 C4 C9 116.7(7) . . ?
C5 C4 C9 119.2(7) . . ?
C40 C41 C42 121.3(6) . . ?
C40 C41 H41 119.3 . . ?
C42 C41 H41 119.3 . . ?
C52 C53 C54 120.5(6) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C43 C42 C41 120.5(6) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C63 C64 C65 112.9(5) . . ?
C63 C64 H64A 109.0 . . ?
C65 C64 H64A 109.0 . . ?
C63 C64 H64B 109.0 . . ?
C65 C64 H64B 109.0 . . ?
H64A C64 H64B 107.8 . . ?
C72 C73 C74 113.3(5) . . ?
C72 C73 H73A 108.9 . . ?
C74 C73 H73A 108.9 . . ?
C72 C73 H73B 108.9 . . ?
C74 C73 H73B 108.9 . . ?
H73A C73 H73B 107.7 . . ?
N8 C46 C47 113.0(5) . . ?
N8 C46 H46A 109.0 . . ?
C47 C46 H46A 109.0 . . ?
N8 C46 H46B 109.0 . . ?
C47 C46 H46B 109.0 . . ?
H46A C46 H46B 107.8 . . ?
C22 C23 C24 121.4(7) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
C57 C56 C55 112.8(5) . . ?
C57 C56 H56A 109.0 . . ?
C55 C56 H56A 109.0 . . ?
C57 C56 H56B 109.0 . . ?
C55 C56 H56B 109.0 . . ?
H56A C56 H56B 107.8 . . ?
N13 C47 C46 113.2(5) . . ?
N13 C47 H47A 108.9 . . ?
C46 C47 H47A 108.9 . . ?
N13 C47 H47B 108.9 . . ?
C46 C47 H47B 108.9 . . ?
H47A C47 H47B 107.8 . . ?
C70 C69 C68 113.1(6) . . ?
C70 C69 H69A 109.0 . . ?
C68 C69 H69A 109.0 . . ?
C70 C69 H69B 109.0 . . ?
C68 C69 H69B 109.0 . . ?
H69A C69 H69B 107.8 . . ?
C59 C60 C61 107.4(6) . . ?
C59 C60 H60A 110.2 . . ?
C61 C60 H60A 110.2 . . ?
C59 C60 H60B 110.2 . . ?
C61 C60 H60B 110.2 . . ?
H60A C60 H60B 108.5 . . ?
C75 C76 C77 110.3(6) . . ?
C75 C76 H76A 109.6 . . ?
C77 C76 H76A 109.6 . . ?
C75 C76 H76B 109.6 . . ?
C77 C76 H76B 109.6 . . ?
H76A C76 H76B 108.1 . . ?
C86 C85 C84 110.4(6) . . ?
C86 C85 H85A 109.6 . . ?
C84 C85 H85A 109.6 . . ?
C86 C85 H85B 109.6 . . ?
C84 C85 H85B 109.6 . . ?
H85A C85 H85B 108.1 . . ?
C40 C45 C44 120.6(6) . . ?
C40 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C4 C9 C8 121.0(9) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C25 C26 C27 120.0(8) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C4 C5 C6 120.3(9) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C26 C25 C24 120.5(8) . . ?
C26 C25 Cl3 119.0(9) . . ?
C24 C25 Cl3 120.4(9) . . ?
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 . . ?
C79 C80 C81 107.5(6) . . ?
C79 C80 H80A 110.2 . . ?
C81 C80 H80A 110.2 . . ?
C79 C80 H80B 110.2 . . ?
C81 C80 H80B 110.2 . . ?
H80A C80 H80B 108.5 . . ?
C25 C24 C23 119.1(8) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C7 C6 C5 118.7(12) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C43 C44 C45 119.5(7) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
C66 C65 C64 117.7(7) . . ?
C66 C65 H65A 107.9 . . ?
C64 C65 H65A 107.9 . . ?
C66 C65 H65B 107.9 . . ?
C64 C65 H65B 107.9 . . ?
H65A C65 H65B 107.2 . . ?
C58 C57 C56 113.1(6) . . ?
C58 C57 H57A 109.0 . . ?
C56 C57 H57A 109.0 . . ?
C58 C57 H57B 109.0 . . ?
C56 C57 H57B 109.0 . . ?
H57A C57 H57B 107.8 . . ?
C85 C86 H86A 109.5 . . ?
C85 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C85 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 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 . . ?
C82 C81 C80 112.2(7) . . ?
C82 C81 H81A 109.2 . . ?
C80 C81 H81A 109.2 . . ?
C82 C81 H81B 109.2 . . ?
C80 C81 H81B 109.2 . . ?
H81A C81 H81B 107.9 . . ?
C78 C77 C76 112.9(7) . . ?
C78 C77 H77A 109.0 . . ?
C76 C77 H77A 109.0 . . ?
C78 C77 H77B 109.0 . . ?
C76 C77 H77B 109.0 . . ?
H77A C77 H77B 107.8 . . ?
C62 C61 C60 110.7(8) . . ?
C62 C61 H61A 109.5 . . ?
C60 C61 H61A 109.5 . . ?
C62 C61 H61B 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 108.1 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C7 C8 C9 118.1(11) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C6 C7 C8 122.6(12) . . ?
C6 C7 Cl1 119.2(13) . . ?
C8 C7 Cl1 118.1(13) . . ?

_refine_diff_density_max         0.698
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.044

####################################################################### 
# 
# 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-p-I-TBAF
_database_code_depnum_ccdc_archive 'CCDC 1832725'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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         'C27 H30 I3 N7 O3, C16 H36 N, F'
_chemical_formula_sum            'C43 H66 F I3 N8 O3'
_chemical_formula_weight         1142.74

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'
I I -0.4742 1.8119 '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                   9.2062(17)
_cell_length_b                   23.534(4)
_cell_length_c                   25.684(5)
_cell_angle_alpha                113.443(6)
_cell_angle_beta                 90.877(7)
_cell_angle_gamma                94.305(6)
_cell_volume                     5084.8(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7872
_cell_measurement_theta_min      3.2760
_cell_measurement_theta_max      22.5812

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             2288.0
_exptl_transmission_factor_min   0.595
_exptl_transmission_factor_max   0.698
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    1.890
_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                   'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59081
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         0.865
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             17523
_reflns_number_gt                8399
_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)+(0.0900P)²+5.3550P] 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         17523
_refine_ls_number_parameters     1063
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0763
_refine_ls_wR_factor_ref         0.2306
_refine_ls_wR_factor_gt          0.1973
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.009
_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
I2 I 0.35491(7) 0.00560(3) 0.19386(3) 0.0961(3) Uani 1 1 d . . . . .
I6 I 0.73968(9) 0.52530(4) -0.33060(3) 0.1078(3) Uani 1 1 d . . . . .
I4 I 0.46597(12) 0.49995(4) 0.12257(5) 0.1465(5) Uani 1 1 d . . . . .
I3 I 0.95740(10) 0.08208(5) 0.46785(5) 0.1488(4) Uani 1 1 d . . . . .
I1 I 0.35389(14) 0.03353(5) 0.67191(5) 0.1584(5) Uani 1 1 d . . . . .
I5 I -0.03823(12) 0.58734(5) -0.04012(8) 0.2112(8) Uani 1 1 d . . . . .
N1 N 0.1501(7) 0.4264(3) 0.5535(3) 0.0556(17) Uani 1 1 d . . . . .
N3 N 0.1952(8) 0.2535(4) 0.6082(3) 0.074(2) Uani 1 1 d . . . . .
H3N H 0.2176 0.2489 0.5744 0.088 Uiso 1 1 calc R U . . .
C4 C 0.2296(9) 0.2062(5) 0.6248(4) 0.070(3) Uani 1 1 d . . . . .
C1 C 0.1325(12) 0.4483(5) 0.6136(4) 0.087(3) Uani 1 1 d . . . . .
H1A H 0.0825 0.4860 0.6257 0.104 Uiso 1 1 calc R U . . .
H1B H 0.2283 0.4590 0.6329 0.104 Uiso 1 1 calc R U . . .
C5 C 0.2120(10) 0.2085(5) 0.6798(4) 0.078(3) Uani 1 1 d . . . . .
H5 H 0.1755 0.2429 0.7074 0.093 Uiso 1 1 calc R U . . .
C6 C 0.2489(11) 0.1598(6) 0.6930(5) 0.091(3) Uani 1 1 d . . . . .
H6 H 0.2393 0.1622 0.7297 0.109 Uiso 1 1 calc R U . . .
C2 C 0.0485(13) 0.4022(5) 0.6320(5) 0.100(4) Uani 1 1 d . . . . .
H2A H 0.0502 0.4184 0.6731 0.120 Uiso 1 1 calc R U . . .
H2B H -0.0523 0.3960 0.6179 0.120 Uiso 1 1 calc R U . . .
C3 C 0.1299(10) 0.3068(5) 0.6391(5) 0.073(3) Uani 1 1 d . . . . .
C9 C 0.2811(13) 0.1553(5) 0.5854(5) 0.097(3) Uani 1 1 d . . . . .
H9 H 0.2921 0.1528 0.5486 0.116 Uiso 1 1 calc R U . . .
C8 C 0.3185(14) 0.1059(5) 0.5994(6) 0.108(4) Uani 1 1 d . . . . .
H8 H 0.3566 0.0717 0.5719 0.130 Uiso 1 1 calc R U . . .
C7 C 0.3002(14) 0.1072(6) 0.6517(6) 0.098(4) Uani 1 1 d . . . . .
N2 N 0.1138(9) 0.3432(4) 0.6098(3) 0.081(2) Uani 1 1 d . . . . .
H2N H 0.1443 0.3305 0.5759 0.097 Uiso 1 1 calc R U . . .
O1 O 0.0943(8) 0.3217(3) 0.6885(3) 0.095(2) Uani 1 1 d . . . . .
C12 C 0.0781(8) 0.2878(4) 0.3958(4) 0.056(2) Uani 1 1 d . . . . .
C10 C 0.0161(11) 0.4268(4) 0.5236(4) 0.079(3) Uani 1 1 d . . . . .
H10A H 0.0012 0.4695 0.5306 0.095 Uiso 1 1 calc R U . . .
H10B H -0.0642 0.4110 0.5395 0.095 Uiso 1 1 calc R U . . .
C16 C 0.2861(9) 0.0845(4) 0.2597(4) 0.071(3) Uani 1 1 d . . . . .
C11 C 0.0100(10) 0.3894(4) 0.4602(4) 0.068(2) Uani 1 1 d . . . . .
H11B H -0.0898 0.3835 0.4450 0.082 Uiso 1 1 calc R U . . .
H11A H 0.0688 0.4115 0.4420 0.082 Uiso 1 1 calc R U . . .
C15 C 0.2200(10) 0.1287(5) 0.2486(4) 0.070(2) Uani 1 1 d . . . . .
H15 H 0.2052 0.1241 0.2112 0.084 Uiso 1 1 calc R U . . .
C14 C 0.1743(10) 0.1808(4) 0.2926(4) 0.071(2) Uani 1 1 d . . . . .
H14 H 0.1308 0.2107 0.2841 0.085 Uiso 1 1 calc R U . . .
C13 C 0.1928(9) 0.1885(4) 0.3486(4) 0.058(2) Uani 1 1 d . . . . .
C17 C 0.3082(11) 0.0910(5) 0.3155(5) 0.089(3) Uani 1 1 d . . . . .
H17 H 0.3536 0.0613 0.3236 0.107 Uiso 1 1 calc R U . . .
C18 C 0.2611(12) 0.1428(5) 0.3587(4) 0.092(3) Uani 1 1 d . . . . .
H18 H 0.2757 0.1471 0.3961 0.111 Uiso 1 1 calc R U . . .
N4 N 0.0643(7) 0.3300(3) 0.4487(3) 0.0605(18) Uani 1 1 d . . . . .
H4N H 0.0888 0.3212 0.4769 0.073 Uiso 1 1 calc R U . . .
N5 N 0.1501(8) 0.2384(3) 0.3954(3) 0.0665(19) Uani 1 1 d . . . . .
H5N H 0.1713 0.2384 0.4281 0.080 Uiso 1 1 calc R U . . .
O2 O 0.0266(6) 0.2919(3) 0.3526(3) 0.0714(16) Uani 1 1 d . . . . .
C22 C 0.6305(10) 0.2457(5) 0.4979(4) 0.075(3) Uani 1 1 d . . . . .
C20 C 0.4185(10) 0.4456(5) 0.5542(4) 0.079(3) Uani 1 1 d . . . . .
H20A H 0.4939 0.4642 0.5384 0.095 Uiso 1 1 calc R U . . .
H20B H 0.4358 0.4628 0.5951 0.095 Uiso 1 1 calc R U . . .
C19 C 0.2710(10) 0.4613(4) 0.5399(5) 0.086(3) Uani 1 1 d . . . . .
H19A H 0.2630 0.5055 0.5607 0.103 Uiso 1 1 calc R U . . .
H19B H 0.2635 0.4526 0.4997 0.103 Uiso 1 1 calc R U . . .
C21 C 0.5505(11) 0.3530(5) 0.5265(4) 0.070(3) Uani 1 1 d . . . . .
C27 C 0.5769(12) 0.1851(6) 0.4853(5) 0.099(3) Uani 1 1 d . . . . .
H27 H 0.4766 0.1756 0.4838 0.119 Uiso 1 1 calc R U . . .
C23 C 0.7786(11) 0.2578(5) 0.5025(5) 0.094(3) Uani 1 1 d . . . . .
H23 H 0.8181 0.2983 0.5114 0.112 Uiso 1 1 calc R U . . .
C25 C 0.8174(12) 0.1535(6) 0.4808(5) 0.096(3) Uani 1 1 d . . . . .
C24 C 0.8704(12) 0.2126(6) 0.4945(5) 0.104(4) Uani 1 1 d . . . . .
H24 H 0.9707 0.2227 0.4986 0.125 Uiso 1 1 calc R U . . .
C26 C 0.6679(12) 0.1382(6) 0.4749(6) 0.115(4) Uani 1 1 d . . . . .
H26 H 0.6298 0.0972 0.4642 0.138 Uiso 1 1 calc R U . . .
N6 N 0.4258(8) 0.3800(4) 0.5320(3) 0.072(2) Uani 1 1 d . . . . .
H6N H 0.3455 0.3565 0.5215 0.087 Uiso 1 1 calc R U . . .
N7 N 0.5283(8) 0.2897(4) 0.5064(3) 0.077(2) Uani 1 1 d . . . . .
H7N H 0.4390 0.2746 0.4977 0.093 Uiso 1 1 calc R U . . .
O3 O 0.6718(7) 0.3826(3) 0.5354(3) 0.094(2) Uani 1 1 d . . . . .
N8 N 0.9140(6) 0.9277(3) 0.0797(3) 0.0555(17) Uani 1 1 d . . . . .
C28 C 0.9429(9) 0.9350(4) 0.1385(4) 0.069(2) Uani 1 1 d . . . . .
H28B H 0.8520 0.9400 0.1578 0.083 Uiso 1 1 calc R U . . .
H28A H 1.0074 0.9725 0.1582 0.083 Uiso 1 1 calc R U . . .
C30 C 0.8824(9) 0.7808(4) 0.1338(5) 0.068(2) Uani 1 1 d . . . . .
C29 C 1.0122(10) 0.8797(4) 0.1417(4) 0.079(3) Uani 1 1 d . . . . .
H29A H 1.1077 0.8771 0.1259 0.095 Uiso 1 1 calc R U . . .
H29B H 1.0249 0.8857 0.1812 0.095 Uiso 1 1 calc R U . . .
C36 C 0.7326(11) 0.6743(5) 0.1570(5) 0.092(3) Uani 1 1 d . . . . .
H36 H 0.7868 0.7038 0.1881 0.110 Uiso 1 1 calc R U . . .
C32 C 0.6394(14) 0.6376(5) 0.0626(5) 0.103(4) Uani 1 1 d . . . . .
H32 H 0.6325 0.6420 0.0283 0.123 Uiso 1 1 calc R U . . .
C33 C 0.5629(15) 0.5861(6) 0.0670(6) 0.122(4) Uani 1 1 d . . . . .
H33 H 0.5043 0.5578 0.0365 0.146 Uiso 1 1 calc R U . . .
C31 C 0.7235(10) 0.6816(4) 0.1064(5) 0.075(3) Uani 1 1 d . . . . .
C34 C 0.5751(13) 0.5777(5) 0.1160(6) 0.095(3) Uani 1 1 d . . . . .
C35 C 0.6579(12) 0.6210(6) 0.1610(6) 0.101(4) Uani 1 1 d . . . . .
H35 H 0.6655 0.6156 0.1949 0.121 Uiso 1 1 calc R U . . .
N9 N 0.9222(8) 0.8223(3) 0.1107(3) 0.072(2) Uani 1 1 d . . . . .
H9N H 0.8927 0.8141 0.0764 0.087 Uiso 1 1 calc R U . . .
N10 N 0.7939(8) 0.7314(4) 0.0966(3) 0.078(2) Uani 1 1 d . . . . .
H10N H 0.7795 0.7308 0.0632 0.094 Uiso 1 1 calc R U . . .
O4 O 0.9201(7) 0.7872(3) 0.1822(3) 0.0836(19) Uani 1 1 d . . . . .
C37 C 0.8054(9) 0.9693(4) 0.0771(4) 0.068(2) Uani 1 1 d . . . . .
H37A H 0.8075 0.9723 0.0406 0.081 Uiso 1 1 calc R U . . .
H37B H 0.8309 1.0105 0.1063 0.081 Uiso 1 1 calc R U . . .
C39 C 0.4815(9) 0.8550(4) 0.0364(4) 0.064(2) Uani 1 1 d . . . . .
C40 C 0.3575(9) 0.7482(4) -0.0083(4) 0.066(2) Uani 1 1 d . . . . .
C43 C 0.1331(11) 0.6568(5) -0.0291(5) 0.096(3) Uani 1 1 d . . . . .
C38 C 0.6521(9) 0.9467(5) 0.0855(4) 0.075(3) Uani 1 1 d . . . . .
H38B H 0.6440 0.9516 0.1246 0.091 Uiso 1 1 calc R U . . .
H38A H 0.5823 0.9715 0.0777 0.091 Uiso 1 1 calc R U . . .
C44 C 0.1042(11) 0.7157(5) -0.0146(5) 0.099(4) Uani 1 1 d . . . . .
H44 H 0.0077 0.7254 -0.0118 0.118 Uiso 1 1 calc R U . . .
C41 C 0.3843(11) 0.6868(5) -0.0274(5) 0.096(3) Uani 1 1 d . . . . .
H41 H 0.4796 0.6764 -0.0346 0.115 Uiso 1 1 calc R U . . .
C45 C 0.2148(10) 0.7627(4) -0.0036(4) 0.083(3) Uani 1 1 d . . . . .
H45 H 0.1930 0.8036 0.0068 0.100 Uiso 1 1 calc R U . . .
C42 C 0.2743(13) 0.6398(6) -0.0366(6) 0.121(5) Uani 1 1 d . . . . .
H42 H 0.2947 0.5986 -0.0474 0.146 Uiso 1 1 calc R U . . .
N12 N 0.4775(7) 0.7924(4) 0.0044(3) 0.070(2) Uani 1 1 d . . . . .
H12N H 0.5583 0.7787 -0.0097 0.084 Uiso 1 1 calc R U . . .
N11 N 0.6195(7) 0.8832(3) 0.0487(3) 0.0630(18) Uani 1 1 d . . . . .
H11N H 0.6906 0.8615 0.0335 0.076 Uiso 1 1 calc R U . . .
O5 O 0.3735(6) 0.8841(3) 0.0522(3) 0.0822(19) Uani 1 1 d . . . . .
C46 C 1.0472(8) 0.9370(4) 0.0533(4) 0.065(2) Uani 1 1 d . . . . .
H46B H 1.1235 0.9166 0.0636 0.078 Uiso 1 1 calc R U . . .
H46A H 1.0778 0.9812 0.0680 0.078 Uiso 1 1 calc R U . . .
C49 C 0.8169(10) 0.7117(5) -0.1541(4) 0.073(3) Uani 1 1 d . . . . .
C48 C 0.9368(10) 0.8162(4) -0.0912(5) 0.068(2) Uani 1 1 d . . . . .
C47 C 1.0301(9) 0.9120(4) -0.0111(4) 0.070(3) Uani 1 1 d . . . . .
H47B H 0.9758 0.9398 -0.0219 0.084 Uiso 1 1 calc R U . . .
H47A H 1.1256 0.9107 -0.0268 0.084 Uiso 1 1 calc R U . . .
C53 C 0.8227(9) 0.6617(5) -0.2552(4) 0.070(2) Uani 1 1 d . . . . .
H53 H 0.8436 0.6638 -0.2897 0.084 Uiso 1 1 calc R U . . .
C50 C 0.7617(13) 0.6557(5) -0.1535(5) 0.101(4) Uani 1 1 d . . . . .
H50 H 0.7423 0.6530 -0.1191 0.121 Uiso 1 1 calc R U . . .
C52 C 0.7688(10) 0.6062(5) -0.2546(5) 0.080(3) Uani 1 1 d . . . . .
C54 C 0.8465(10) 0.7142(5) -0.2059(4) 0.072(3) Uani 1 1 d . . . . .
H54 H 0.8826 0.7515 -0.2073 0.087 Uiso 1 1 calc R U . . .
C51 C 0.7352(13) 0.6039(5) -0.2032(5) 0.103(4) Uani 1 1 d . . . . .
H51 H 0.6943 0.5669 -0.2023 0.123 Uiso 1 1 calc R U . . .
N14 N 0.8449(8) 0.7627(3) -0.1014(3) 0.075(2) Uani 1 1 d . . . . .
H14N H 0.8011 0.7606 -0.0728 0.090 Uiso 1 1 calc R U . . .
N13 N 0.9552(7) 0.8510(3) -0.0342(3) 0.068(2) Uani 1 1 d . . . . .
H13N H 0.9205 0.8357 -0.0112 0.081 Uiso 1 1 calc R U . . .
O6 O 0.9947(8) 0.8303(3) -0.1268(3) 0.089(2) Uani 1 1 d . . . . .
N15 N 0.2661(8) 0.7468(4) 0.2581(3) 0.077(2) Uani 1 1 d . . . . .
C55 C 0.1817(11) 0.7977(5) 0.2985(4) 0.087(3) Uani 1 1 d . . . . .
H55A H 0.1183 0.7797 0.3188 0.104 Uiso 1 1 calc R U . . .
H55B H 0.1196 0.8119 0.2761 0.104 Uiso 1 1 calc R U . . .
C56 C 0.2715(15) 0.8544(6) 0.3422(6) 0.126(4) Uani 1 1 d D . . . .
H56A H 0.3244 0.8412 0.3677 0.151 Uiso 1 1 calc R U . . .
H56B H 0.3430 0.8696 0.3223 0.151 Uiso 1 1 calc R U . . .
C57 C 0.187(2) 0.9076(7) 0.3772(7) 0.225(12) Uani 1 1 d D . . . .
H57A H 0.1343 0.9208 0.3516 0.270 Uiso 1 1 calc R U . A 1
H57B H 0.1149 0.8922 0.3968 0.270 Uiso 1 1 calc R U . A 1
C67 C 0.3679(10) 0.7718(5) 0.2249(5) 0.092(3) Uani 1 1 d . . . . .
H67A H 0.4206 0.7379 0.2001 0.110 Uiso 1 1 calc R U . . .
H67B H 0.4390 0.8025 0.2516 0.110 Uiso 1 1 calc R U . . .
C68 C 0.2976(11) 0.8016(6) 0.1887(5) 0.097(4) Uani 1 1 d . . . . .
H68A H 0.2095 0.7762 0.1694 0.116 Uiso 1 1 calc R U . . .
H68B H 0.2697 0.8422 0.2135 0.116 Uiso 1 1 calc R U . . .
C69 C 0.3951(11) 0.8090(6) 0.1456(5) 0.125(5) Uani 1 1 d D . . . .
H69A H 0.3465 0.8314 0.1269 0.150 Uiso 1 1 calc R U . . .
H69B H 0.4083 0.7680 0.1170 0.150 Uiso 1 1 calc R U . . .
C63 C 0.1505(10) 0.6973(5) 0.2193(4) 0.077(3) Uani 1 1 d . . . . .
H63A H 0.0880 0.7166 0.2015 0.092 Uiso 1 1 calc R U . . .
H63B H 0.0903 0.6819 0.2424 0.092 Uiso 1 1 calc R U . . .
C64 C 0.2135(14) 0.6421(6) 0.1727(6) 0.123(4) Uani 1 1 d . . . . .
H64A H 0.2837 0.6247 0.1894 0.147 Uiso 1 1 calc R U . . .
H64B H 0.2626 0.6557 0.1460 0.147 Uiso 1 1 calc R U . . .
C58A C 0.273(3) 0.9636(11) 0.4206(12) 0.178(15) Uani 0.5 1 d D . P B 1
H58A H 0.2628 0.9632 0.4576 0.267 Uiso 0.5 1 calc R U P B 1
H58B H 0.2365 1.0006 0.4201 0.267 Uiso 0.5 1 calc R U P B 1
H58C H 0.3737 0.9628 0.4117 0.267 Uiso 0.5 1 calc R U P B 1
C58B C 0.131(4) 0.9282(12) 0.3330(9) 0.33(5) Uani 0.5 1 d D . P B 2
H58F H 0.2100 0.9495 0.3219 0.490 Uiso 0.5 1 calc R U P B 2
H58D H 0.0564 0.9557 0.3482 0.490 Uiso 0.5 1 calc R U P B 2
H58E H 0.0919 0.8926 0.3004 0.490 Uiso 0.5 1 calc R U P B 2
C70 C 0.5465(11) 0.8431(7) 0.1689(6) 0.143(6) Uani 1 1 d D . . . .
H70B H 0.5362 0.8796 0.2026 0.215 Uiso 1 1 calc R U . . .
H70C H 0.5915 0.8549 0.1408 0.215 Uiso 1 1 calc R U . . .
H70A H 0.6062 0.8161 0.1777 0.215 Uiso 1 1 calc R U . . .
C61 C 0.4019(16) 0.6625(8) 0.3495(7) 0.137(5) Uani 1 1 d . . . . .
H61A H 0.4615 0.6971 0.3777 0.164 Uiso 1 1 calc R U . . .
H61B H 0.3477 0.6415 0.3698 0.164 Uiso 1 1 calc R U . . .
C60 C 0.2923(13) 0.6897(7) 0.3237(6) 0.123(4) Uani 1 1 d . . . . .
H60B H 0.2212 0.6569 0.2995 0.148 Uiso 1 1 calc R U . . .
H60A H 0.2409 0.7196 0.3536 0.148 Uiso 1 1 calc R U . . .
C62 C 0.5040(17) 0.6180(8) 0.3128(7) 0.150(6) Uani 1 1 d . . . . .
H62B H 0.4486 0.5819 0.2856 0.225 Uiso 1 1 calc R U . . .
H62A H 0.5662 0.6058 0.3361 0.225 Uiso 1 1 calc R U . . .
H62C H 0.5624 0.6379 0.2931 0.225 Uiso 1 1 calc R U . . .
C59 C 0.3665(10) 0.7209(6) 0.2896(5) 0.097(4) Uani 1 1 d . . . . .
H59B H 0.4239 0.6912 0.2620 0.116 Uiso 1 1 calc R U . . .
H59A H 0.4337 0.7547 0.3149 0.116 Uiso 1 1 calc R U . . .
C65 C 0.0859(18) 0.5925(7) 0.1418(6) 0.150(6) Uani 1 1 d D . . . .
H65B H 0.0102 0.6122 0.1301 0.181 Uiso 1 1 calc R U . . .
H65A H 0.1209 0.5613 0.1077 0.181 Uiso 1 1 calc R U . . .
C66 C 0.021(3) 0.5610(8) 0.1777(7) 0.256(13) Uani 1 1 d D . . . .
H66C H 0.0972 0.5452 0.1927 0.383 Uiso 1 1 calc R U . . .
H66A H -0.0483 0.5274 0.1550 0.383 Uiso 1 1 calc R U . . .
H66B H -0.0269 0.5905 0.2085 0.383 Uiso 1 1 calc R U . . .
F1 F 0.2326(5) 0.2651(2) 0.50556(18) 0.0654(12) Uani 1 1 d . . . . .
F2 F 0.7654(4) 0.7674(2) 0.00338(19) 0.0620(12) Uani 1 1 d . . . . .
N16 N 0.3374(8) 0.7622(4) 0.7682(3) 0.087(2) Uani 1 1 d . . . . .
C75 C 0.4485(11) 0.7988(6) 0.8165(4) 0.097(3) Uani 1 1 d . . . . .
H75A H 0.5119 0.7703 0.8219 0.117 Uiso 1 1 calc R U . . .
H75B H 0.5082 0.8278 0.8059 0.117 Uiso 1 1 calc R U . . .
C76 C 0.3806(15) 0.8342(7) 0.8718(6) 0.147(6) Uani 1 1 d D . . . .
H76B H 0.3616 0.8057 0.8903 0.176 Uiso 1 1 calc R U . . .
H76A H 0.2866 0.8448 0.8626 0.176 Uiso 1 1 calc R U . . .
C77 C 0.4612(15) 0.8940(7) 0.9161(6) 0.190(8) Uani 1 1 d D . . . .
H77B H 0.4228 0.9294 0.9119 0.228 Uiso 1 1 calc R U . . .
H77A H 0.4389 0.8964 0.9536 0.228 Uiso 1 1 calc R U . . .
C78 C 0.6281(15) 0.9002(9) 0.9128(6) 0.174(7) Uani 1 1 d D . . . .
H78C H 0.6665 0.8626 0.9107 0.261 Uiso 1 1 calc R U . . .
H78A H 0.6695 0.9345 0.9461 0.261 Uiso 1 1 calc R U . . .
H78B H 0.6524 0.9074 0.8796 0.261 Uiso 1 1 calc R U . . .
C83 C 0.4297(10) 0.7272(6) 0.7180(4) 0.105(4) Uani 1 1 d . . . . .
H83B H 0.4918 0.7573 0.7094 0.126 Uiso 1 1 calc R U . . .
H83A H 0.4924 0.7021 0.7289 0.126 Uiso 1 1 calc R U . . .
C71 C 0.2416(12) 0.8040(5) 0.7546(5) 0.105(4) Uani 1 1 d . . . . .
H71B H 0.1758 0.8198 0.7852 0.126 Uiso 1 1 calc R U . . .
H71A H 0.1823 0.7785 0.7205 0.126 Uiso 1 1 calc R U . . .
C84 C 0.3397(12) 0.6859(7) 0.6653(4) 0.125(5) Uani 1 1 d D . . . .
H84A H 0.2543 0.7063 0.6621 0.150 Uiso 1 1 calc R U . . .
H84B H 0.3066 0.6474 0.6686 0.150 Uiso 1 1 calc R U . . .
C72 C 0.3146(19) 0.8592(8) 0.7453(10) 0.254(14) Uani 1 1 d D . . . .
H72B H 0.3764 0.8843 0.7788 0.305 Uiso 1 1 calc R U . . .
H72A H 0.3773 0.8437 0.7136 0.305 Uiso 1 1 calc R U . . .
C80 C 0.3173(18) 0.6712(8) 0.7994(8) 0.178(7) Uani 1 1 d D . . . .
H80A H 0.3718 0.6924 0.8355 0.213 Uiso 1 1 calc R U . . .
H80B H 0.3842 0.6502 0.7705 0.213 Uiso 1 1 calc R U . . .
C79 C 0.2392(12) 0.7168(5) 0.7837(5) 0.100(3) Uani 1 1 d . . . . .
H79B H 0.1826 0.7404 0.8154 0.120 Uiso 1 1 calc R U . . .
H79A H 0.1713 0.6935 0.7517 0.120 Uiso 1 1 calc R U . . .
C74 C 0.206(2) 0.8665(9) 0.6687(7) 0.226(10) Uani 1 1 d D . . . .
H74C H 0.2722 0.8884 0.6530 0.339 Uiso 1 1 calc R U . . .
H74B H 0.1089 0.8649 0.6541 0.339 Uiso 1 1 calc R U . . .
H74A H 0.2338 0.8250 0.6583 0.339 Uiso 1 1 calc R U . . .
C73 C 0.2133(19) 0.9005(8) 0.7339(7) 0.230(12) Uani 1 1 d D . . . .
H73A H 0.2551 0.9432 0.7469 0.277 Uiso 1 1 calc R U . . .
H73B H 0.1190 0.8991 0.7499 0.277 Uiso 1 1 calc R U . . .
C81 C 0.1967(19) 0.6243(8) 0.8034(11) 0.249(13) Uani 1 1 d D . . . .
H81A H 0.1872 0.6305 0.8429 0.299 Uiso 1 1 calc R U . . .
H81B H 0.1043 0.6310 0.7891 0.299 Uiso 1 1 calc R U . . .
C82 C 0.234(3) 0.5572(9) 0.7687(12) 0.338(18) Uani 1 1 d D . . . .
H82B H 0.3375 0.5563 0.7663 0.507 Uiso 1 1 calc R U . . .
H82C H 0.1889 0.5427 0.7311 0.507 Uiso 1 1 calc R U . . .
H82A H 0.1975 0.5308 0.7869 0.507 Uiso 1 1 calc R U . . .
C86 C 0.5678(19) 0.6415(8) 0.6143(6) 0.186(8) Uani 1 1 d D . . . .
H86B H 0.6390 0.6731 0.6388 0.280 Uiso 1 1 calc R U . . .
H86C H 0.6042 0.6229 0.5769 0.280 Uiso 1 1 calc R U . . .
H86A H 0.5488 0.6102 0.6290 0.280 Uiso 1 1 calc R U . . .
C85 C 0.4257(15) 0.6708(10) 0.6111(5) 0.272(16) Uani 1 1 d D . . . .
H85A H 0.3650 0.6423 0.5787 0.327 Uiso 1 1 calc R U . . .
H85B H 0.4490 0.7087 0.6054 0.327 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
I2 C16 2.103(9) . ?
I6 C52 2.111(10) . ?
I4 C34 2.088(11) . ?
I3 C25 2.118(11) . ?
I1 C7 2.087(11) . ?
I5 C43 2.114(10) . ?
N1 C1 1.436(11) . ?
N1 C10 1.446(11) . ?
N1 C19 1.463(11) . ?
N3 C3 1.377(12) . ?
N3 C4 1.399(11) . ?
C4 C9 1.349(13) . ?
C4 C5 1.402(12) . ?
C1 C2 1.514(13) . ?
C5 C6 1.380(14) . ?
C6 C7 1.392(15) . ?
C2 N2 1.456(12) . ?
C3 O1 1.233(11) . ?
C3 N2 1.361(11) . ?
C9 C8 1.411(15) . ?
C8 C7 1.346(15) . ?
C12 O2 1.242(9) . ?
C12 N4 1.341(10) . ?
C12 N5 1.377(10) . ?
C10 C11 1.510(12) . ?
C16 C15 1.363(13) . ?
C16 C17 1.388(13) . ?
C11 N4 1.440(10) . ?
C15 C14 1.394(12) . ?
C14 C13 1.382(12) . ?
C13 C18 1.392(12) . ?
C13 N5 1.393(11) . ?
C17 C18 1.387(13) . ?
C22 C23 1.365(13) . ?
C22 C27 1.380(13) . ?
C22 N7 1.407(12) . ?
C20 N6 1.425(11) . ?
C20 C19 1.511(12) . ?
C21 O3 1.239(10) . ?
C21 N6 1.335(11) . ?
C21 N7 1.367(12) . ?
C27 C26 1.380(15) . ?
C23 C24 1.363(14) . ?
C25 C24 1.341(15) . ?
C25 C26 1.386(15) . ?
N8 C46 1.454(10) . ?
N8 C37 1.468(10) . ?
N8 C28 1.469(10) . ?
C28 C29 1.522(12) . ?
C30 O4 1.233(10) . ?
C30 N9 1.362(11) . ?
C30 N10 1.370(11) . ?
C29 N9 1.450(11) . ?
C36 C31 1.378(13) . ?
C36 C35 1.425(14) . ?
C32 C31 1.366(14) . ?
C32 C33 1.400(15) . ?
C33 C34 1.352(16) . ?
C31 N10 1.409(11) . ?
C34 C35 1.370(16) . ?
C37 C38 1.520(11) . ?
C39 O5 1.231(9) . ?
C39 N11 1.360(10) . ?
C39 N12 1.368(11) . ?
C40 C41 1.371(12) . ?
C40 C45 1.377(12) . ?
C40 N12 1.399(10) . ?
C43 C44 1.334(14) . ?
C43 C42 1.383(14) . ?
C38 N11 1.420(11) . ?
C44 C45 1.383(13) . ?
C41 C42 1.387(14) . ?
C46 C47 1.520(12) . ?
C49 C50 1.382(13) . ?
C49 C54 1.387(12) . ?
C49 N14 1.410(11) . ?
C48 O6 1.207(10) . ?
C48 N13 1.365(11) . ?
C48 N14 1.393(11) . ?
C47 N13 1.432(10) . ?
C53 C52 1.367(13) . ?
C53 C54 1.373(12) . ?
C50 C51 1.371(14) . ?
C52 C51 1.382(14) . ?
N15 C55 1.513(12) . ?
N15 C67 1.514(11) . ?
N15 C59 1.530(11) . ?
N15 C63 1.530(12) . ?
C55 C56 1.530(15) . ?
C56 C57 1.5001(11) . ?
C57 C58B 1.5002(11) . ?
C57 C58A 1.5001(11) . ?
C67 C68 1.531(12) . ?
C68 C69 1.490(14) . ?
C69 C70 1.5395(11) . ?
C63 C64 1.534(14) . ?
C64 C65 1.550(18) . ?
C61 C62 1.503(19) . ?
C61 C60 1.510(16) . ?
C60 C59 1.491(13) . ?
C65 C66 1.5003(11) . ?
N16 C71 1.504(13) . ?
N16 C75 1.517(12) . ?
N16 C79 1.524(13) . ?
N16 C83 1.536(12) . ?
C75 C76 1.506(16) . ?
C76 C77 1.5396(11) . ?
C77 C78 1.5394(11) . ?
C83 C84 1.504(13) . ?
C71 C72 1.523(18) . ?
C84 C85 1.5396(11) . ?
C72 C73 1.5005(11) . ?
C80 C79 1.510(17) . ?
C80 C81 1.5401(11) . ?
C74 C73 1.5397(11) . ?
C81 C82 1.5396(11) . ?
C86 C85 1.5395(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
C1 N1 C10 111.3(7) . . ?
C1 N1 C19 112.0(7) . . ?
C10 N1 C19 111.1(7) . . ?
C3 N3 C4 128.1(9) . . ?
C9 C4 N3 117.6(9) . . ?
C9 C4 C5 118.7(9) . . ?
N3 C4 C5 123.7(10) . . ?
N1 C1 C2 114.5(9) . . ?
C6 C5 C4 120.2(10) . . ?
C5 C6 C7 120.7(10) . . ?
N2 C2 C1 109.8(8) . . ?
O1 C3 N2 122.8(10) . . ?
O1 C3 N3 124.6(9) . . ?
N2 C3 N3 112.5(9) . . ?
C4 C9 C8 120.5(11) . . ?
C7 C8 C9 121.3(12) . . ?
C8 C7 C6 118.6(11) . . ?
C8 C7 I1 121.0(11) . . ?
C6 C7 I1 120.4(9) . . ?
C3 N2 C2 124.5(9) . . ?
O2 C12 N4 123.6(8) . . ?
O2 C12 N5 124.2(8) . . ?
N4 C12 N5 112.1(8) . . ?
N1 C10 C11 115.4(8) . . ?
C15 C16 C17 119.9(9) . . ?
C15 C16 I2 121.4(8) . . ?
C17 C16 I2 118.7(8) . . ?
N4 C11 C10 109.2(7) . . ?
C16 C15 C14 121.0(9) . . ?
C13 C14 C15 120.8(9) . . ?
C14 C13 C18 117.0(9) . . ?
C14 C13 N5 125.2(8) . . ?
C18 C13 N5 117.7(8) . . ?
C18 C17 C16 118.5(9) . . ?
C17 C18 C13 122.8(9) . . ?
C12 N4 C11 122.6(7) . . ?
C12 N5 C13 128.2(7) . . ?
C23 C22 C27 116.8(10) . . ?
C23 C22 N7 125.9(10) . . ?
C27 C22 N7 117.3(9) . . ?
N6 C20 C19 110.8(8) . . ?
N1 C19 C20 112.8(8) . . ?
O3 C21 N6 122.8(10) . . ?
O3 C21 N7 124.6(9) . . ?
N6 C21 N7 112.5(9) . . ?
C22 C27 C26 121.8(10) . . ?
C24 C23 C22 122.3(11) . . ?
C24 C25 C26 119.9(11) . . ?
C24 C25 I3 121.4(9) . . ?
C26 C25 I3 118.7(10) . . ?
C25 C24 C23 120.6(10) . . ?
C27 C26 C25 118.6(11) . . ?
C21 N6 C20 123.7(8) . . ?
C21 N7 C22 129.3(8) . . ?
C46 N8 C37 111.5(6) . . ?
C46 N8 C28 111.8(6) . . ?
C37 N8 C28 110.7(7) . . ?
N8 C28 C29 112.4(8) . . ?
O4 C30 N9 124.2(9) . . ?
O4 C30 N10 124.4(8) . . ?
N9 C30 N10 111.4(9) . . ?
N9 C29 C28 111.0(7) . . ?
C31 C36 C35 119.3(11) . . ?
C31 C32 C33 123.1(11) . . ?
C34 C33 C32 119.4(12) . . ?
C32 C31 C36 117.7(10) . . ?
C32 C31 N10 117.4(10) . . ?
C36 C31 N10 124.9(10) . . ?
C33 C34 C35 119.3(11) . . ?
C33 C34 I4 119.9(10) . . ?
C35 C34 I4 120.8(10) . . ?
C34 C35 C36 121.2(11) . . ?
C30 N9 C29 122.7(8) . . ?
C30 N10 C31 127.9(8) . . ?
N8 C37 C38 112.3(7) . . ?
O5 C39 N11 122.2(9) . . ?
O5 C39 N12 124.9(8) . . ?
N11 C39 N12 112.9(8) . . ?
C41 C40 C45 118.4(9) . . ?
C41 C40 N12 117.7(8) . . ?
C45 C40 N12 123.8(8) . . ?
C44 C43 C42 121.3(10) . . ?
C44 C43 I5 120.1(8) . . ?
C42 C43 I5 118.6(8) . . ?
N11 C38 C37 110.4(7) . . ?
C43 C44 C45 121.3(9) . . ?
C40 C41 C42 122.3(9) . . ?
C40 C45 C44 119.3(9) . . ?
C43 C42 C41 117.0(10) . . ?
C39 N12 C40 127.7(7) . . ?
C39 N11 C38 123.1(7) . . ?
N8 C46 C47 113.2(7) . . ?
C50 C49 C54 118.5(9) . . ?
C50 C49 N14 117.9(9) . . ?
C54 C49 N14 123.6(9) . . ?
O6 C48 N13 123.9(8) . . ?
O6 C48 N14 126.1(9) . . ?
N13 C48 N14 110.0(9) . . ?
N13 C47 C46 111.1(7) . . ?
C52 C53 C54 121.3(9) . . ?
C51 C50 C49 120.8(10) . . ?
C53 C52 C51 118.8(9) . . ?
C53 C52 I6 120.7(8) . . ?
C51 C52 I6 120.5(8) . . ?
C53 C54 C49 120.1(9) . . ?
C50 C51 C52 120.4(10) . . ?
C48 N14 C49 126.3(8) . . ?
C48 N13 C47 122.6(8) . . ?
C55 N15 C67 111.0(8) . . ?
C55 N15 C59 112.0(8) . . ?
C67 N15 C59 104.4(7) . . ?
C55 N15 C63 105.3(7) . . ?
C67 N15 C63 112.0(8) . . ?
C59 N15 C63 112.3(8) . . ?
N15 C55 C56 116.7(9) . . ?
C57 C56 C55 115.9(11) . . ?
C58B C57 C56 101.4(17) . . ?
C58A C57 C56 116.8(16) . . ?
N15 C67 C68 116.6(7) . . ?
C69 C68 C67 113.4(8) . . ?
C68 C69 C70 115.4(10) . . ?
N15 C63 C64 114.0(8) . . ?
C63 C64 C65 108.2(10) . . ?
C62 C61 C60 120.7(13) . . ?
C59 C60 C61 110.6(10) . . ?
C60 C59 N15 115.7(8) . . ?
C66 C65 C64 113.2(14) . . ?
C71 N16 C75 111.9(9) . . ?
C71 N16 C79 107.8(8) . . ?
C75 N16 C79 110.5(8) . . ?
C71 N16 C83 111.5(9) . . ?
C75 N16 C83 104.4(7) . . ?
C79 N16 C83 110.8(9) . . ?
C76 C75 N16 113.4(9) . . ?
C75 C76 C77 120.2(12) . . ?
C78 C77 C76 115.9(13) . . ?
C84 C83 N16 113.3(8) . . ?
N16 C71 C72 118.1(10) . . ?
C83 C84 C85 112.3(10) . . ?
C73 C72 C71 115.7(14) . . ?
C79 C80 C81 105.6(13) . . ?
C80 C79 N16 115.3(10) . . ?
C72 C73 C74 96.3(14) . . ?
C82 C81 C80 110.4(16) . . ?
C86 C85 C84 112.3(13) . . ?

_refine_diff_density_max         2.054
_refine_diff_density_min         -1.989
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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-p-Cl-TBAF
_database_code_depnum_ccdc_archive 'CCDC 1832721'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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         'C27 H30 Cl3 N7 O3, C16 H36 N, F'
_chemical_formula_sum            'C43 H66 Cl3 F N8 O3'
_chemical_formula_weight         868.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   23.7562(16)
_cell_length_b                   9.1238(3)
_cell_length_c                   25.2435(16)
_cell_angle_alpha                90
_cell_angle_beta                 116.950(8)
_cell_angle_gamma                90
_cell_volume                     4877.3(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4125
_cell_measurement_theta_min      3.4290
_cell_measurement_theta_max      21.0990

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             1856.0
_exptl_transmission_factor_min   0.932
_exptl_transmission_factor_max   0.952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.236
_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            22106
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.874
_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             8573
_reflns_number_gt                4515
_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)+(0.0808P)²+2.9599P] 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         8573
_refine_ls_number_parameters     528
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.0744
_refine_ls_wR_factor_ref         0.2284
_refine_ls_wR_factor_gt          0.1854
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
Cl3 Cl 0.34592(8) 0.83434(14) 0.81599(6) 0.1009(5) Uani 1 1 d . . . . .
Cl2 Cl -0.09937(8) 0.8688(2) 0.36693(9) 0.1476(7) Uani 1 1 d . . . . .
Cl1 Cl 0.14216(12) 1.43685(18) 0.54312(11) 0.1741(10) Uani 1 1 d . . . . .
F1 F 0.26234(9) 0.6867(2) 0.49012(9) 0.0628(6) Uani 1 1 d . . . . .
O1 O 0.33381(15) 1.1078(3) 0.44230(14) 0.0822(9) Uani 1 1 d . . . . .
O3 O 0.45122(14) 0.4993(3) 0.63145(12) 0.0804(9) Uani 1 1 d . . . . .
N1 N 0.35530(13) 0.5727(3) 0.41508(13) 0.0529(7) Uani 1 1 d . . . . .
O2 O 0.12198(14) 0.5323(3) 0.30468(13) 0.0865(9) Uani 1 1 d . . . . .
N2 N 0.33331(16) 0.8596(3) 0.44290(15) 0.0673(9) Uani 1 1 d . . . . .
H2N H 0.3235 0.7825 0.4565 0.081 Uiso 1 1 calc R U . . .
N7 N 0.35583(16) 0.6193(4) 0.59971(14) 0.0690(9) Uani 1 1 d . . . . .
H7N H 0.3224 0.6413 0.5678 0.083 Uiso 1 1 calc R U . . .
N6 N 0.38301(15) 0.5163(3) 0.53339(14) 0.0644(9) Uani 1 1 d . . . . .
H6N H 0.3448 0.5364 0.5080 0.077 Uiso 1 1 calc R U . . .
N9 N 0.5000 0.1462(5) 0.7500 0.0713(13) Uani 1 2 d S T P . .
N3 N 0.28321(17) 0.9810(3) 0.48641(16) 0.0709(10) Uani 1 1 d . . . . .
H3N H 0.2799 0.8946 0.4984 0.085 Uiso 1 1 calc R U . . .
N4 N 0.22234(16) 0.5372(4) 0.37838(16) 0.0812(11) Uani 1 1 d . . . . .
H4N H 0.2459 0.5657 0.4142 0.097 Uiso 1 1 calc R U . . .
N8 N 0.0000 0.1853(5) 0.2500 0.0735(14) Uani 1 2 d S T P . .
N5 N 0.14506(16) 0.6423(4) 0.39344(16) 0.0773(10) Uani 1 1 d . . . . .
H5N H 0.1761 0.6606 0.4276 0.093 Uiso 1 1 calc R U . . .
C21 C 0.4009(2) 0.5422(4) 0.59142(17) 0.0613(10) Uani 1 1 d . . . . .
C22 C 0.3567(2) 0.6663(4) 0.65216(17) 0.0607(10) Uani 1 1 d . . . . .
C3 C 0.31786(18) 0.9923(4) 0.45610(18) 0.0611(10) Uani 1 1 d . . . . .
C19 C 0.39083(19) 0.4415(4) 0.44494(17) 0.0628(10) Uani 1 1 d . . . . .
H19B H 0.4214 0.4203 0.4304 0.075 Uiso 1 1 calc R U . . .
H19A H 0.3620 0.3591 0.4347 0.075 Uiso 1 1 calc R U . . .
C4 C 0.2522(2) 1.0934(4) 0.50047(18) 0.0645(11) Uani 1 1 d . . . . .
C12 C 0.1602(2) 0.5681(4) 0.3548(2) 0.0688(11) Uani 1 1 d . . . . .
C13 C 0.0863(2) 0.6930(4) 0.3853(2) 0.0687(11) Uani 1 1 d . . . . .
C20 C 0.42513(19) 0.4565(4) 0.51192(18) 0.0665(11) Uani 1 1 d . . . . .
H20A H 0.4402 0.3613 0.5298 0.080 Uiso 1 1 calc R U . . .
H20B H 0.4613 0.5205 0.5231 0.080 Uiso 1 1 calc R U . . .
C25 C 0.3507(3) 0.7684(5) 0.75375(19) 0.0738(12) Uani 1 1 d . . . . .
C23 C 0.4076(2) 0.6498(4) 0.70845(17) 0.0683(11) Uani 1 1 d . . . . .
H23 H 0.4445 0.6051 0.7125 0.082 Uiso 1 1 calc R U . . .
C24 C 0.4034(2) 0.6997(4) 0.75831(18) 0.0739(12) Uani 1 1 d . . . . .
H24 H 0.4373 0.6859 0.7956 0.089 Uiso 1 1 calc R U . . .
C10 C 0.3094(2) 0.5415(5) 0.35372(18) 0.0729(12) Uani 1 1 d . . . . .
H10B H 0.3298 0.4836 0.3351 0.088 Uiso 1 1 calc R U . . .
H10A H 0.2962 0.6332 0.3321 0.088 Uiso 1 1 calc R U . . .
C1 C 0.3978(2) 0.6928(4) 0.4185(2) 0.0705(11) Uani 1 1 d . . . . .
H1A H 0.4135 0.6759 0.3896 0.085 Uiso 1 1 calc R U . . .
H1B H 0.4338 0.6930 0.4576 0.085 Uiso 1 1 calc R U . . .
C2 C 0.3657(2) 0.8423(4) 0.4069(2) 0.0753(12) Uani 1 1 d . . . . .
H2A H 0.3970 0.9191 0.4163 0.090 Uiso 1 1 calc R U . . .
H2B H 0.3357 0.8508 0.3652 0.090 Uiso 1 1 calc R U . . .
C14 C 0.0318(2) 0.6813(5) 0.3320(2) 0.0787(13) Uani 1 1 d . . . . .
H14 H 0.0333 0.6378 0.2994 0.094 Uiso 1 1 calc R U . . .
C32 C 0.4866(2) 0.0465(4) 0.69773(18) 0.0801(13) Uani 1 1 d . . . . .
H32A H 0.5230 -0.0161 0.7078 0.096 Uiso 1 1 calc R U . . .
H32B H 0.4512 -0.0162 0.6917 0.096 Uiso 1 1 calc R U . . .
C11 C 0.2522(2) 0.4609(5) 0.3486(2) 0.0873(14) Uani 1 1 d . . . . .
H11B H 0.2224 0.4496 0.3070 0.105 Uiso 1 1 calc R U . . .
H11A H 0.2644 0.3638 0.3657 0.105 Uiso 1 1 calc R U . . .
C28 C 0.5559(2) 0.2471(4) 0.7620(2) 0.0786(13) Uani 1 1 d . . . . .
H28A H 0.5448 0.3090 0.7274 0.094 Uiso 1 1 calc R U . . .
H28B H 0.5624 0.3106 0.7951 0.094 Uiso 1 1 calc R U . . .
C15 C -0.0250(2) 0.7341(5) 0.3272(3) 0.0887(15) Uani 1 1 d . . . . .
H15 H -0.0616 0.7233 0.2916 0.106 Uiso 1 1 calc R U . . .
C27 C 0.3036(2) 0.7352(5) 0.64848(19) 0.0869(14) Uani 1 1 d . . . . .
H27 H 0.2693 0.7483 0.6113 0.104 Uiso 1 1 calc R U . . .
C9 C 0.2655(2) 1.2404(5) 0.5003(2) 0.0885(15) Uani 1 1 d . . . . .
H9 H 0.2979 1.2700 0.4916 0.106 Uiso 1 1 calc R U . . .
C18 C 0.0815(3) 0.7575(6) 0.4319(2) 0.1039(17) Uani 1 1 d . . . . .
H18 H 0.1173 0.7643 0.4684 0.125 Uiso 1 1 calc R U . . .
C16 C -0.0279(2) 0.8013(6) 0.3737(3) 0.0926(15) Uani 1 1 d . . . . .
C26 C 0.2997(2) 0.7856(5) 0.6985(2) 0.0911(14) Uani 1 1 d . . . . .
H26 H 0.2629 0.8306 0.6949 0.109 Uiso 1 1 calc R U . . .
C40 C -0.0060(2) 0.2863(5) 0.2946(2) 0.0815(13) Uani 1 1 d . . . . .
H40A H -0.0429 0.3476 0.2737 0.098 Uiso 1 1 calc R U . . .
H40B H 0.0306 0.3503 0.3108 0.098 Uiso 1 1 calc R U . . .
C36 C 0.05706(19) 0.0848(5) 0.2796(2) 0.0914(16) Uani 1 1 d . . . . .
H36A H 0.0506 0.0217 0.3073 0.110 Uiso 1 1 calc R U . . .
H36B H 0.0590 0.0226 0.2493 0.110 Uiso 1 1 calc R U . . .
C8 C 0.2311(3) 1.3436(5) 0.5131(3) 0.0988(17) Uani 1 1 d . . . . .
H8 H 0.2401 1.4425 0.5124 0.119 Uiso 1 1 calc R U . . .
C7 C 0.1847(3) 1.3036(6) 0.5266(2) 0.0986(16) Uani 1 1 d . . . . .
C5 C 0.2048(3) 1.0556(5) 0.5148(3) 0.1094(19) Uani 1 1 d . . . . .
H5 H 0.1956 0.9569 0.5159 0.131 Uiso 1 1 calc R U . . .
C37 C 0.1200(2) 0.1609(5) 0.3126(3) 0.108(2) Uani 1 1 d . . . . .
H37A H 0.1271 0.2250 0.2856 0.129 Uiso 1 1 calc R U . . .
H37B H 0.1195 0.2206 0.3442 0.129 Uiso 1 1 calc R U . . .
C29 C 0.6172(2) 0.1721(6) 0.7758(3) 0.1065(18) Uani 1 1 d . . . . .
H29A H 0.6124 0.1126 0.7421 0.128 Uiso 1 1 calc R U . . .
H29B H 0.6287 0.1081 0.8098 0.128 Uiso 1 1 calc R U . . .
C30 C 0.6690(3) 0.2858(7) 0.7891(3) 0.124(2) Uani 1 1 d . . . . .
H30A H 0.6551 0.3542 0.7562 0.149 Uiso 1 1 calc R U . . .
H30B H 0.6749 0.3407 0.8242 0.149 Uiso 1 1 calc R U . . .
C33 C 0.4719(3) 0.1229(6) 0.6403(2) 0.116(2) Uani 1 1 d . . . . .
H33A H 0.4369 0.1892 0.6317 0.140 Uiso 1 1 calc R U . . .
H33B H 0.5081 0.1823 0.6463 0.140 Uiso 1 1 calc R U . . .
C6 C 0.1705(3) 1.1586(6) 0.5277(3) 0.131(2) Uani 1 1 d . . . . .
H6 H 0.1384 1.1304 0.5369 0.157 Uiso 1 1 calc R U . . .
C17 C 0.0249(3) 0.8129(7) 0.4261(3) 0.1134(19) Uani 1 1 d . . . . .
H17 H 0.0230 0.8582 0.4582 0.136 Uiso 1 1 calc R U . . .
C38 C 0.1725(3) 0.0519(7) 0.3385(4) 0.157(3) Uani 1 1 d . . . . .
H38A H 0.2115 0.1070 0.3584 0.188 Uiso 1 1 calc R U . . .
H38B H 0.1670 -0.0011 0.3692 0.188 Uiso 1 1 calc R U . . .
C41 C -0.0115(3) 0.2134(7) 0.3460(3) 0.127(2) Uani 1 1 d . . . . .
H41A H 0.0285 0.1688 0.3728 0.153 Uiso 1 1 calc R U . . .
H41B H -0.0435 0.1373 0.3313 0.153 Uiso 1 1 calc R U . . .
C35 C 0.4749(4) -0.1223(8) 0.5885(3) 0.176(3) Uani 1 1 d D . . . .
H35A H 0.5127 -0.1461 0.6237 0.264 Uiso 1 1 calc R U . . .
H35B H 0.4819 -0.1360 0.5543 0.264 Uiso 1 1 calc R U . . .
H35C H 0.4412 -0.1851 0.5856 0.264 Uiso 1 1 calc R U . . .
C39 C 0.1816(3) -0.0508(10) 0.3033(4) 0.201(5) Uani 1 1 d . . . . .
H39A H 0.1504 -0.1265 0.2931 0.302 Uiso 1 1 calc R U . . .
H39B H 0.2230 -0.0929 0.3245 0.302 Uiso 1 1 calc R U . . .
H39C H 0.1780 -0.0047 0.2677 0.302 Uiso 1 1 calc R U . . .
C34 C 0.4570(5) 0.0383(8) 0.5915(3) 0.198(4) Uani 1 1 d D . . . .
H34A H 0.4113 0.0413 0.5698 0.237 Uiso 1 1 calc R U . . .
H34B H 0.4723 0.0922 0.5675 0.237 Uiso 1 1 calc R U . . .
C31 C 0.7304(3) 0.2233(9) 0.7991(3) 0.160(3) Uani 1 1 d . . . . .
H31A H 0.7464 0.1618 0.8337 0.240 Uiso 1 1 calc R U . . .
H31B H 0.7598 0.3012 0.8049 0.240 Uiso 1 1 calc R U . . .
H31C H 0.7249 0.1662 0.7652 0.240 Uiso 1 1 calc R U . . .
C42 C -0.0304(7) 0.3349(9) 0.3801(4) 0.257(7) Uani 1 1 d D . . . .
H42A H -0.0019 0.4178 0.3894 0.309 Uiso 1 1 calc R U . . .
H42B H -0.0729 0.3691 0.3550 0.309 Uiso 1 1 calc R U . . .
C43 C -0.0266(8) 0.2695(15) 0.4378(5) 0.370(9) Uani 1 1 d D . . . .
H43A H -0.0589 0.1965 0.4282 0.555 Uiso 1 1 calc R U . . .
H43B H -0.0327 0.3459 0.4609 0.555 Uiso 1 1 calc R U . . .
H43C H 0.0141 0.2255 0.4603 0.555 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 C25 1.733(4) . ?
Cl2 C16 1.740(5) . ?
Cl1 C7 1.748(5) . ?
O1 C3 1.222(4) . ?
O3 C21 1.228(4) . ?
N1 C10 1.462(5) . ?
N1 C1 1.466(5) . ?
N1 C19 1.462(4) . ?
O2 C12 1.221(5) . ?
N2 C3 1.350(5) . ?
N2 C2 1.441(5) . ?
N2 H2N 0.8600 . ?
N7 C21 1.374(5) . ?
N7 C22 1.383(5) . ?
N7 H7N 0.8600 . ?
N6 C21 1.348(5) . ?
N6 C20 1.444(5) . ?
N6 H6N 0.8600 . ?
N9 C32 1.513(5) 2_656 ?
N9 C32 1.513(5) . ?
N9 C28 1.530(5) . ?
N9 C28 1.530(5) 2_656 ?
N3 C3 1.358(5) . ?
N3 C4 1.399(5) . ?
N3 H3N 0.8600 . ?
N4 C12 1.349(5) . ?
N4 C11 1.426(6) . ?
N4 H4N 0.8600 . ?
N8 C40 1.512(5) 2 ?
N8 C40 1.512(5) . ?
N8 C36 1.522(5) 2 ?
N8 C36 1.522(5) . ?
N5 C12 1.362(5) . ?
N5 C13 1.396(5) . ?
N5 H5N 0.8600 . ?
C22 C27 1.375(6) . ?
C22 C23 1.395(5) . ?
C19 C20 1.514(5) . ?
C19 H19B 0.9700 . ?
C19 H19A 0.9700 . ?
C4 C5 1.374(6) . ?
C4 C9 1.379(6) . ?
C13 C18 1.364(6) . ?
C13 C14 1.386(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C25 C24 1.357(6) . ?
C25 C26 1.381(6) . ?
C23 C24 1.384(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C10 C11 1.500(6) . ?
C10 H10B 0.9700 . ?
C10 H10A 0.9700 . ?
C1 C2 1.526(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C14 C15 1.385(6) . ?
C14 H14 0.9300 . ?
C32 C33 1.500(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11A 0.9700 . ?
C28 C29 1.498(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C15 C16 1.354(7) . ?
C15 H15 0.9300 . ?
C27 C26 1.386(6) . ?
C27 H27 0.9300 . ?
C9 C8 1.379(6) . ?
C9 H9 0.9300 . ?
C18 C17 1.382(7) . ?
C18 H18 0.9300 . ?
C16 C17 1.351(7) . ?
C26 H26 0.9300 . ?
C40 C41 1.515(7) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C36 C37 1.511(6) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C8 C7 1.343(7) . ?
C8 H8 0.9300 . ?
C7 C6 1.368(7) . ?
C5 C6 1.375(7) . ?
C5 H5 0.9300 . ?
C37 C38 1.494(7) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C29 C30 1.527(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.478(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C33 C34 1.357(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C6 H6 0.9300 . ?
C17 H17 0.9300 . ?
C38 C39 1.375(9) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C41 C42 1.587(10) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C35 C34 1.5369(10) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C42 C43 1.5391(10) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 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
C10 N1 C1 111.8(3) . . ?
C10 N1 C19 111.4(3) . . ?
C1 N1 C19 111.1(3) . . ?
C3 N2 C2 122.4(3) . . ?
C3 N2 H2N 118.8 . . ?
C2 N2 H2N 118.8 . . ?
C21 N7 C22 129.0(3) . . ?
C21 N7 H7N 115.5 . . ?
C22 N7 H7N 115.5 . . ?
C21 N6 C20 122.9(3) . . ?
C21 N6 H6N 118.6 . . ?
C20 N6 H6N 118.5 . . ?
C32 N9 C32 106.1(4) 2_656 . ?
C32 N9 C28 111.6(3) 2_656 . ?
C32 N9 C28 110.8(3) . . ?
C32 N9 C28 110.8(3) 2_656 2_656 ?
C32 N9 C28 111.6(3) . 2_656 ?
C28 N9 C28 106.0(4) . 2_656 ?
C3 N3 C4 127.6(3) . . ?
C3 N3 H3N 116.2 . . ?
C4 N3 H3N 116.2 . . ?
C12 N4 C11 125.2(4) . . ?
C12 N4 H4N 117.4 . . ?
C11 N4 H4N 117.4 . . ?
C40 N8 C40 104.8(4) 2 . ?
C40 N8 C36 111.4(3) 2 2 ?
C40 N8 C36 111.7(3) . 2 ?
C40 N8 C36 111.7(3) 2 . ?
C40 N8 C36 111.4(3) . . ?
C36 N8 C36 106.0(4) 2 . ?
C12 N5 C13 129.1(4) . . ?
C12 N5 H5N 115.5 . . ?
C13 N5 H5N 115.5 . . ?
O3 C21 N6 123.2(4) . . ?
O3 C21 N7 125.0(4) . . ?
N6 C21 N7 111.8(3) . . ?
C27 C22 N7 117.5(4) . . ?
C27 C22 C23 117.6(4) . . ?
N7 C22 C23 124.9(4) . . ?
O1 C3 N2 123.3(4) . . ?
O1 C3 N3 124.9(4) . . ?
N2 C3 N3 111.9(4) . . ?
N1 C19 C20 113.2(3) . . ?
N1 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
N1 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
H19B C19 H19A 107.7 . . ?
C5 C4 C9 117.5(4) . . ?
C5 C4 N3 118.2(4) . . ?
C9 C4 N3 124.3(4) . . ?
O2 C12 N4 123.5(4) . . ?
O2 C12 N5 124.2(4) . . ?
N4 C12 N5 112.3(4) . . ?
C18 C13 C14 117.7(5) . . ?
C18 C13 N5 119.0(4) . . ?
C14 C13 N5 123.3(4) . . ?
N6 C20 C19 109.8(3) . . ?
N6 C20 H20A 109.7 . . ?
C19 C20 H20A 109.7 . . ?
N6 C20 H20B 109.7 . . ?
C19 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 Cl3 121.3(4) . . ?
C26 C25 Cl3 119.2(4) . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 121.3(4) . . ?
C25 C24 H24 119.4 . . ?
C23 C24 H24 119.4 . . ?
N1 C10 C11 113.5(4) . . ?
N1 C10 H10B 108.9 . . ?
C11 C10 H10B 108.9 . . ?
N1 C10 H10A 108.9 . . ?
C11 C10 H10A 108.9 . . ?
H10B C10 H10A 107.7 . . ?
N1 C1 C2 112.7(3) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N2 C2 C1 109.9(3) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 119.9 . . ?
C33 C32 N9 115.4(4) . . ?
C33 C32 H32A 108.5 . . ?
N9 C32 H32A 108.4 . . ?
C33 C32 H32B 108.4 . . ?
N9 C32 H32B 108.4 . . ?
H32A C32 H32B 107.5 . . ?
N4 C11 C10 111.3(4) . . ?
N4 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
N4 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
H11B C11 H11A 108.0 . . ?
C29 C28 N9 115.8(4) . . ?
C29 C28 H28A 108.3 . . ?
N9 C28 H28A 108.3 . . ?
C29 C28 H28B 108.3 . . ?
N9 C28 H28B 108.3 . . ?
H28A C28 H28B 107.4 . . ?
C16 C15 C14 120.8(5) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C22 C27 C26 122.0(4) . . ?
C22 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
C4 C9 C8 120.1(5) . . ?
C4 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C13 C18 C17 121.5(5) . . ?
C13 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C15 C16 C17 119.6(5) . . ?
C15 C16 Cl2 120.4(5) . . ?
C17 C16 Cl2 120.0(5) . . ?
C25 C26 C27 119.4(5) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
N8 C40 C41 116.4(4) . . ?
N8 C40 H40A 108.2 . . ?
C41 C40 H40A 108.2 . . ?
N8 C40 H40B 108.2 . . ?
C41 C40 H40B 108.2 . . ?
H40A C40 H40B 107.4 . . ?
C37 C36 N8 115.7(3) . . ?
C37 C36 H36A 108.4 . . ?
N8 C36 H36A 108.4 . . ?
C37 C36 H36B 108.4 . . ?
N8 C36 H36B 108.4 . . ?
H36A C36 H36B 107.4 . . ?
C7 C8 C9 121.1(4) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C8 C7 C6 120.3(5) . . ?
C8 C7 Cl1 120.1(4) . . ?
C6 C7 Cl1 119.6(5) . . ?
C4 C5 C6 122.3(5) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.8 . . ?
C38 C37 C36 110.9(4) . . ?
C38 C37 H37A 109.5 . . ?
C36 C37 H37A 109.4 . . ?
C38 C37 H37B 109.4 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 108.0 . . ?
C28 C29 C30 110.0(4) . . ?
C28 C29 H29A 109.7 . . ?
C30 C29 H29A 109.7 . . ?
C28 C29 H29B 109.7 . . ?
C30 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C31 C30 C29 114.2(5) . . ?
C31 C30 H30A 108.7 . . ?
C29 C30 H30A 108.7 . . ?
C31 C30 H30B 108.7 . . ?
C29 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
C34 C33 C32 117.6(5) . . ?
C34 C33 H33A 108.0 . . ?
C32 C33 H33A 107.9 . . ?
C34 C33 H33B 107.8 . . ?
C32 C33 H33B 107.9 . . ?
H33A C33 H33B 107.2 . . ?
C5 C6 C7 118.6(5) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
C16 C17 C18 120.2(6) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C39 C38 C37 121.0(7) . . ?
C39 C38 H38A 107.1 . . ?
C37 C38 H38A 107.1 . . ?
C39 C38 H38B 107.1 . . ?
C37 C38 H38B 107.1 . . ?
H38A C38 H38B 106.8 . . ?
C40 C41 C42 108.2(5) . . ?
C40 C41 H41A 110.1 . . ?
C42 C41 H41A 109.9 . . ?
C40 C41 H41B 110.1 . . ?
C42 C41 H41B 110.2 . . ?
H41A C41 H41B 108.4 . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.6 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C35 C34 C33 128.5(6) . . ?
C35 C34 H34A 105.1 . . ?
C33 C34 H34A 105.1 . . ?
C35 C34 H34B 105.3 . . ?
C33 C34 H34B 105.3 . . ?
H34A C34 H34B 105.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C43 C42 C41 109.4(8) . . ?
C43 C42 H42A 110.0 . . ?
C41 C42 H42A 109.9 . . ?
C43 C42 H42B 109.7 . . ?
C41 C42 H42B 109.6 . . ?
H42A C42 H42B 108.2 . . ?
C42 C43 H43A 109.7 . . ?
C42 C43 H43B 109.4 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.3 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

_refine_diff_density_max         0.425
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.047

####################################################################### 
# 
# 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-p-Br-TEACO3
_database_code_depnum_ccdc_archive 'CCDC 1832724'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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(C27 H30 Br3 N7 O3), 2(C8 H20 N), C O3'
_chemical_formula_sum            'C71 H100 Br6 N16 O9'
_chemical_formula_weight         1801.07

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

_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                   17.3616(9)
_cell_length_b                   20.7181(15)
_cell_length_c                   23.5639(15)
_cell_angle_alpha                90
_cell_angle_beta                 98.846(5)
_cell_angle_gamma                90
_cell_volume                     8375.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2412
_cell_measurement_theta_min      3.3590
_cell_measurement_theta_max      19.6030

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_F_000             3680.0
_exptl_transmission_factor_min   0.431
_exptl_transmission_factor_max   0.540
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    2.937
_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            19078
_diffrn_reflns_av_unetI/netI     0.2265
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.083
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             7329
_reflns_number_gt                6079
_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)+(0.0400P)²+45.6172P] 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         7329
_refine_ls_number_parameters     467
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.2997
_refine_ls_R_factor_gt           0.0921
_refine_ls_wR_factor_ref         0.2410
_refine_ls_wR_factor_gt          0.1787
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.111
_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
C34 C 0.9339(10) 0.6945(12) 0.6984(7) 0.34(2) Uani 1 1 d D U . A 1
H34A H 0.9252 0.7345 0.6770 0.405 Uiso 1 1 calc R U . A 1
H34B H 0.8854 0.6769 0.7074 0.405 Uiso 1 1 calc R U . A 1
C32 C 0.9529(10) 0.7548(9) 0.7687(11) 0.281(13) Uani 1 1 d D U . B 2
H32A H 0.9806 0.7646 0.8067 0.337 Uiso 1 1 calc R U . B 2
H32B H 0.9664 0.7896 0.7445 0.337 Uiso 1 1 calc R U . B 2
Br1 Br 0.61778(9) 0.97456(9) 0.77663(8) 0.1368(7) Uani 1 1 d . . . . .
Br2 Br 0.84802(9) 0.29073(9) 0.93056(7) 0.1370(7) Uani 1 1 d . . . . .
Br3 Br 0.11520(10) 0.45839(10) 0.46618(7) 0.1566(9) Uani 1 1 d . . . . .
O3 O 0.1928(5) 0.6130(4) 0.7324(3) 0.100(3) Uani 1 1 d . . . . .
O1 O 0.5207(5) 0.7116(4) 0.9367(4) 0.101(3) Uani 1 1 d . . . . .
O5 O 0.5546(4) 0.5295(4) 0.7804(4) 0.107(3) Uani 1 1 d . . . . .
N5 N 0.5399(7) 0.4141(5) 0.8398(4) 0.087(3) Uani 1 1 d . . . . .
H5N H 0.5445 0.4407 0.8126 0.104 Uiso 1 1 calc R U . . .
N1 N 0.3532(6) 0.5622(5) 0.8898(4) 0.073(3) Uani 1 1 d . . . . .
O2 O 0.4505(5) 0.3724(5) 0.8929(4) 0.107(3) Uani 1 1 d . . . . .
N7 N 0.2894(5) 0.5721(5) 0.6861(4) 0.083(3) Uani 1 1 d . . . . .
H7N H 0.3391 0.5670 0.6899 0.099 Uiso 1 1 calc R U . . .
N6 N 0.3195(5) 0.6225(5) 0.7717(4) 0.083(3) Uani 1 1 d . . . . .
H6N H 0.3672 0.6177 0.7668 0.099 Uiso 1 1 calc R U . . .
N2 N 0.5134(5) 0.6126(6) 0.8938(4) 0.083(3) Uani 1 1 d . . . . .
H2N H 0.5245 0.5901 0.8654 0.100 Uiso 1 1 calc R U . . .
N4 N 0.4110(7) 0.4489(5) 0.8265(4) 0.085(3) Uani 1 1 d . . . . .
H4N H 0.4216 0.4708 0.7977 0.102 Uiso 1 1 calc R U . . .
N3 N 0.5410(6) 0.7019(6) 0.8439(5) 0.092(3) Uani 1 1 d . . . . .
H3N H 0.5412 0.6746 0.8164 0.110 Uiso 1 1 calc R U . . .
O4 O 0.5000 0.6193(8) 0.7500 0.125(5) Uani 1 2 d S T P . .
C36 C 0.5000 0.5576(12) 0.7500 0.081(6) Uani 1 2 d S T P . .
C3 C 0.5233(7) 0.6782(8) 0.8943(7) 0.080(4) Uani 1 1 d . . . . .
C22 C 0.2448(7) 0.5478(6) 0.6357(5) 0.074(3) Uani 1 1 d . . . . .
C11 C 0.3330(7) 0.4546(6) 0.8428(5) 0.085(4) Uani 1 1 d . . . . .
H11A H 0.3131 0.4118 0.8490 0.102 Uiso 1 1 calc R U . . .
H11B H 0.2981 0.4745 0.8116 0.102 Uiso 1 1 calc R U . . .
C13 C 0.6065(8) 0.3810(6) 0.8620(6) 0.078(4) Uani 1 1 d . . . . .
C10 C 0.3338(7) 0.4943(7) 0.8967(5) 0.083(4) Uani 1 1 d . . . . .
H10A H 0.2829 0.4917 0.9086 0.100 Uiso 1 1 calc R U . . .
H10B H 0.3714 0.4758 0.9270 0.100 Uiso 1 1 calc R U . . .
C12 C 0.4671(11) 0.4101(7) 0.8555(6) 0.092(4) Uani 1 1 d . . . . .
C1 C 0.3987(7) 0.5912(6) 0.9406(5) 0.088(4) Uani 1 1 d . . . . .
H1A H 0.3840 0.5719 0.9748 0.106 Uiso 1 1 calc R U . . .
H1B H 0.3875 0.6370 0.9413 0.106 Uiso 1 1 calc R U . . .
C20 C 0.3014(7) 0.6508(6) 0.8242(5) 0.089(4) Uani 1 1 d . . . . .
H20A H 0.2569 0.6794 0.8152 0.106 Uiso 1 1 calc R U . . .
H20B H 0.3453 0.6765 0.8419 0.106 Uiso 1 1 calc R U . . .
C21 C 0.2603(9) 0.6034(6) 0.7297(6) 0.079(4) Uani 1 1 d . . . . .
C4 C 0.5590(8) 0.7665(9) 0.8318(6) 0.083(4) Uani 1 1 d . . . . .
C19 C 0.2830(7) 0.5995(7) 0.8668(5) 0.093(4) Uani 1 1 d . . . . .
H19A H 0.2623 0.6201 0.8982 0.111 Uiso 1 1 calc R U . . .
H19B H 0.2434 0.5704 0.8477 0.111 Uiso 1 1 calc R U . . .
C2 C 0.4846(7) 0.5815(6) 0.9405(5) 0.091(4) Uani 1 1 d . . . . .
H2A H 0.5130 0.5978 0.9763 0.110 Uiso 1 1 calc R U . . .
H2B H 0.4950 0.5356 0.9389 0.110 Uiso 1 1 calc R U . . .
C27 C 0.2856(7) 0.5269(6) 0.5928(6) 0.093(4) Uani 1 1 d . . . . .
H27 H 0.3396 0.5308 0.5980 0.112 Uiso 1 1 calc R U . . .
C18 C 0.6709(11) 0.3945(7) 0.8354(5) 0.098(4) Uani 1 1 d . . . . .
H18 H 0.6660 0.4228 0.8045 0.118 Uiso 1 1 calc R U . . .
C23 C 0.1657(8) 0.5386(6) 0.6272(6) 0.097(4) Uani 1 1 d . . . . .
H23 H 0.1368 0.5500 0.6558 0.117 Uiso 1 1 calc R U . . .
C14 C 0.6154(9) 0.3423(7) 0.9083(6) 0.092(4) Uani 1 1 d . . . . .
H14 H 0.5735 0.3344 0.9276 0.111 Uiso 1 1 calc R U . . .
C16 C 0.7494(9) 0.3275(9) 0.9016(8) 0.109(5) Uani 1 1 d . . . . .
C25 C 0.1697(9) 0.4924(7) 0.5350(5) 0.094(4) Uani 1 1 d . . . . .
C15 C 0.6875(11) 0.3143(7) 0.9271(6) 0.110(5) Uani 1 1 d . . . . .
H15 H 0.6929 0.2858 0.9580 0.132 Uiso 1 1 calc R U . . .
C5 C 0.5372(8) 0.8187(10) 0.8612(6) 0.105(5) Uani 1 1 d . . . . .
H5 H 0.5103 0.8130 0.8921 0.126 Uiso 1 1 calc R U . . .
C7 C 0.5935(9) 0.8900(9) 0.7988(9) 0.104(5) Uani 1 1 d . . . . .
C17 C 0.7410(10) 0.3665(8) 0.8546(7) 0.109(5) Uani 1 1 d . . . . .
H17 H 0.7833 0.3741 0.8356 0.131 Uiso 1 1 calc R U . . .
C24 C 0.1293(7) 0.5125(7) 0.5766(6) 0.108(5) Uani 1 1 d . . . . .
H24 H 0.0753 0.5086 0.5707 0.129 Uiso 1 1 calc R U . . .
C9 C 0.5973(8) 0.7768(8) 0.7855(6) 0.104(5) Uani 1 1 d . . . . .
H9 H 0.6121 0.7421 0.7645 0.125 Uiso 1 1 calc R U . . .
C26 C 0.2471(8) 0.5004(7) 0.5428(6) 0.108(5) Uani 1 1 d . . . . .
H26 H 0.2752 0.4879 0.5141 0.130 Uiso 1 1 calc R U . . .
C6 C 0.5558(9) 0.8799(9) 0.8445(8) 0.112(5) Uani 1 1 d . . . . .
H6 H 0.5420 0.9152 0.8651 0.134 Uiso 1 1 calc R U . . .
C8 C 0.6139(9) 0.8405(13) 0.7705(7) 0.128(6) Uani 1 1 d . . . . .
H8 H 0.6402 0.8474 0.7394 0.153 Uiso 1 1 calc R U . . .
N9 N 1.0000 0.6978(9) 0.7500 0.232(12) Uani 1 2 d DS TU P . .
N8 N 0.7500 0.7500 0.0000 0.48(2) Uani 1 2 d DS U P . .
C30 C 0.6824(9) 0.772(2) 0.0305(8) 0.50(2) Uani 1 1 d D U . . .
H30A H 0.6401 0.7415 0.0291 0.598 Uiso 1 1 calc R U . . .
H30B H 0.6630 0.8153 0.0197 0.598 Uiso 1 1 calc R U . . .
C35 C 0.9848(13) 0.6452(10) 0.6721(12) 0.306(14) Uani 1 1 d D U . . .
H35A H 1.0169 0.6675 0.6487 0.459 Uiso 1 1 calc R U . A 1
H35B H 0.9518 0.6151 0.6488 0.459 Uiso 1 1 calc R U . A 1
H35C H 1.0172 0.6225 0.7023 0.459 Uiso 1 1 calc R U . A 1
C33 C 0.8680(8) 0.7708(8) 0.7748(8) 0.208(9) Uani 1 1 d D U . . .
H33A H 0.8345 0.7602 0.7397 0.311 Uiso 1 1 calc R U . B 2
H33B H 0.8636 0.8160 0.7827 0.311 Uiso 1 1 calc R U . B 2
H33C H 0.8529 0.7461 0.8058 0.311 Uiso 1 1 calc R U . B 2
C31 C 0.7418(16) 0.7700(16) 0.0864(11) 0.46(2) Uani 1 1 d D U . . .
H31A H 0.7887 0.7918 0.0805 0.687 Uiso 1 1 calc R U . . .
H31B H 0.7534 0.7259 0.0967 0.687 Uiso 1 1 calc R U . . .
H31C H 0.7201 0.7910 0.1167 0.687 Uiso 1 1 calc R U . . .
C28 C 0.7163(14) 0.6824(5) 0.0008(14) 0.414(19) Uani 1 1 d D U . . .
H28A H 0.6654 0.6818 0.0130 0.497 Uiso 1 1 calc R U . . .
H28B H 0.7141 0.6603 -0.0357 0.497 Uiso 1 1 calc R U . . .
C29 C 0.7796(18) 0.6568(16) 0.0459(12) 0.45(2) Uani 1 1 d D U . . .
H29A H 0.7592 0.6224 0.0666 0.675 Uiso 1 1 calc R U . . .
H29B H 0.7982 0.6908 0.0721 0.675 Uiso 1 1 calc R U . . .
H29C H 0.8217 0.6407 0.0279 0.675 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
C34 N9 1.5399(10) . ?
C34 C35 1.5406(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C32 C33 1.5392(11) . ?
C32 N9 1.5395(10) . ?
C32 C32 1.97(3) 2_756 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
Br1 C7 1.893(17) . ?
Br2 C16 1.903(14) . ?
Br3 C25 1.884(12) . ?
O3 C21 1.200(13) . ?
O1 C3 1.220(14) . ?
O5 C36 1.242(11) . ?
N5 C12 1.372(16) . ?
N5 C13 1.377(13) . ?
N5 H5N 0.8600 . ?
N1 C1 1.458(12) . ?
N1 C10 1.460(13) . ?
N1 C19 1.474(13) . ?
O2 C12 1.244(14) . ?
N7 C21 1.376(14) . ?
N7 C22 1.407(13) . ?
N7 H7N 0.8600 . ?
N6 C21 1.370(13) . ?
N6 C20 1.448(12) . ?
N6 H6N 0.8600 . ?
N2 C3 1.369(15) . ?
N2 C2 1.430(13) . ?
N2 H2N 0.8600 . ?
N4 C12 1.362(14) . ?
N4 C11 1.468(13) . ?
N4 H4N 0.8600 . ?
N3 C3 1.364(15) . ?
N3 C4 1.413(15) . ?
N3 H3N 0.8600 . ?
O4 C36 1.28(2) . ?
C36 O5 1.242(11) 2_656 ?
C22 C23 1.371(14) . ?
C22 C27 1.388(14) . ?
C11 C10 1.511(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C14 1.341(15) . ?
C13 C18 1.391(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C1 C2 1.506(14) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C20 C19 1.529(14) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C4 C5 1.368(17) . ?
C4 C9 1.379(16) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C27 C26 1.378(15) . ?
C27 H27 0.9300 . ?
C18 C17 1.362(16) . ?
C18 H18 0.9300 . ?
C23 C24 1.371(15) . ?
C23 H23 0.9300 . ?
C14 C15 1.391(16) . ?
C14 H14 0.9300 . ?
C16 C15 1.337(17) . ?
C16 C17 1.360(18) . ?
C25 C26 1.338(15) . ?
C25 C24 1.356(15) . ?
C15 H15 0.9300 . ?
C5 C6 1.381(17) . ?
C5 H5 0.9300 . ?
C7 C8 1.304(19) . ?
C7 C6 1.360(18) . ?
C17 H17 0.9300 . ?
C24 H24 0.9300 . ?
C9 C8 1.41(2) . ?
C9 H9 0.9300 . ?
C26 H26 0.9300 . ?
C6 H6 0.9300 . ?
C8 H8 0.9300 . ?
N9 C32 1.5396(11) 2_756 ?
N9 C34 1.5398(11) 2_756 ?
N8 C28 1.5199(7) 7_665 ?
N8 C28 1.5199(7) . ?
N8 C30 1.5400(11) . ?
N8 C30 1.5400(11) 7_665 ?
C30 C31 1.5425(13) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C31 H31A 1.1366 . ?
C31 H31B 1.1034 . ?
C31 H31C 1.1066 . ?
C28 C29 1.5036(14) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 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
N9 C34 C35 86.8(12) . . ?
N9 C34 H34A 114.3 . . ?
C35 C34 H34A 114.2 . . ?
N9 C34 H34B 114.1 . . ?
C35 C34 H34B 114.2 . . ?
H34A C34 H34B 111.4 . . ?
C33 C32 N9 138.6(14) . . ?
C33 C32 C32 156(2) . 2_756 ?
N9 C32 C32 50.1(8) . 2_756 ?
C33 C32 H32A 102.2 . . ?
N9 C32 H32A 102.3 . . ?
C32 C32 H32A 95.4 2_756 . ?
C33 C32 H32B 102.7 . . ?
N9 C32 H32B 102.5 . . ?
C32 C32 H32B 56.2 2_756 . ?
H32A C32 H32B 104.9 . . ?
C12 N5 C13 128.5(13) . . ?
C12 N5 H5N 115.8 . . ?
C13 N5 H5N 115.7 . . ?
C1 N1 C10 114.3(9) . . ?
C1 N1 C19 113.5(10) . . ?
C10 N1 C19 110.7(10) . . ?
C21 N7 C22 125.6(10) . . ?
C21 N7 H7N 117.2 . . ?
C22 N7 H7N 117.2 . . ?
C21 N6 C20 119.8(11) . . ?
C21 N6 H6N 120.1 . . ?
C20 N6 H6N 120.1 . . ?
C3 N2 C2 119.9(12) . . ?
C3 N2 H2N 120.1 . . ?
C2 N2 H2N 120.0 . . ?
C12 N4 C11 122.3(12) . . ?
C12 N4 H4N 118.9 . . ?
C11 N4 H4N 118.8 . . ?
C3 N3 C4 127.1(12) . . ?
C3 N3 H3N 116.5 . . ?
C4 N3 H3N 116.4 . . ?
O5 C36 O5 124(2) . 2_656 ?
O5 C36 O4 118.0(11) . . ?
O5 C36 O4 118.0(11) 2_656 . ?
O1 C3 N3 123.3(15) . . ?
O1 C3 N2 123.4(15) . . ?
N3 C3 N2 113.2(14) . . ?
C23 C22 C27 117.5(12) . . ?
C23 C22 N7 125.5(12) . . ?
C27 C22 N7 116.7(12) . . ?
N4 C11 C10 111.9(9) . . ?
N4 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
N4 C11 H11B 109.2 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C14 C13 N5 126.2(14) . . ?
C14 C13 C18 119.1(13) . . ?
N5 C13 C18 114.5(14) . . ?
N1 C10 C11 113.9(10) . . ?
N1 C10 H10A 108.7 . . ?
C11 C10 H10A 108.7 . . ?
N1 C10 H10B 108.8 . . ?
C11 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
O2 C12 N4 119.9(15) . . ?
O2 C12 N5 123.5(14) . . ?
N4 C12 N5 116.6(14) . . ?
N1 C1 C2 110.8(10) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N6 C20 C19 111.9(10) . . ?
N6 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
N6 C20 H20B 109.2 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
O3 C21 N6 122.9(13) . . ?
O3 C21 N7 126.4(12) . . ?
N6 C21 N7 110.7(12) . . ?
C5 C4 C9 118.9(16) . . ?
C5 C4 N3 124.0(15) . . ?
C9 C4 N3 117.0(16) . . ?
N1 C19 C20 111.2(10) . . ?
N1 C19 H19A 109.4 . . ?
C20 C19 H19A 109.4 . . ?
N1 C19 H19B 109.4 . . ?
C20 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
N2 C2 C1 113.8(10) . . ?
N2 C2 H2A 108.8 . . ?
C1 C2 H2A 108.8 . . ?
N2 C2 H2B 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C26 C27 C22 120.9(12) . . ?
C26 C27 H27 119.6 . . ?
C22 C27 H27 119.5 . . ?
C17 C18 C13 120.3(14) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.8 . . ?
C24 C23 C22 119.9(12) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.0 . . ?
C13 C14 C15 119.6(13) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C15 C16 C17 119.7(15) . . ?
C15 C16 Br2 119.8(16) . . ?
C17 C16 Br2 120.5(16) . . ?
C26 C25 C24 118.9(12) . . ?
C26 C25 Br3 121.6(12) . . ?
C24 C25 Br3 119.4(12) . . ?
C16 C15 C14 121.1(14) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.4 . . ?
C4 C5 C6 119.1(15) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C8 C7 C6 119.1(19) . . ?
C8 C7 Br1 119.8(18) . . ?
C6 C7 Br1 121.1(18) . . ?
C16 C17 C18 120.0(15) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C25 C24 C23 121.9(12) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.0 . . ?
C4 C9 C8 119.1(15) . . ?
C4 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C25 C26 C27 120.7(13) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C7 C6 C5 122.0(16) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C7 C8 C9 121.8(18) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C32 N9 C32 79.8(16) . 2_756 ?
C34 N9 C34 175(2) 2_756 . ?
C28 N8 C28 180.0 7_665 . ?
C28 N8 C30 92.9(17) 7_665 . ?
C28 N8 C30 87.1(17) . . ?
C28 N8 C30 87.1(17) 7_665 7_665 ?
C28 N8 C30 92.9(17) . 7_665 ?
C30 N8 C30 180.0(6) . 7_665 ?
N8 C30 C31 86.0(15) . . ?
N8 C30 H30A 114.6 . . ?
C31 C30 H30A 113.8 . . ?
N8 C30 H30B 114.9 . . ?
C31 C30 H30B 113.8 . . ?
H30A C30 H30B 111.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.6 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.4 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C33 H33A 109.1 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.7 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C31 H31A 126.7 . . ?
C30 C31 H31B 123.4 . . ?
H31A C31 H31B 90.0 . . ?
C30 C31 H31C 123.7 . . ?
H31A C31 H31C 90.9 . . ?
H31B C31 H31C 92.0 . . ?
C29 C28 N8 95.3(16) . . ?
C29 C28 H28A 111.9 . . ?
N8 C28 H28A 112.6 . . ?
C29 C28 H28B 113.5 . . ?
N8 C28 H28B 112.7 . . ?
H28A C28 H28B 110.2 . . ?
C28 C29 H29A 109.9 . . ?
C28 C29 H29B 110.0 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 108.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

_refine_diff_density_max         1.229
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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-p-Br-TBAF
_database_code_depnum_ccdc_archive 'CCDC 1832723'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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         'C27 H30 Br3 N7 O3, C16 H36 N, F'
_chemical_formula_sum            'C43 H66 Br3 F N8 O3'
_chemical_formula_weight         1001.74

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                   9.124(5)
_cell_length_b                   20.617(11)
_cell_length_c                   26.103(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.927(7)
_cell_angle_gamma                90
_cell_volume                     4910(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3261
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      17.89

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_F_000             2072.0
_exptl_transmission_factor_min   0.463
_exptl_transmission_factor_max   0.547
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    2.513
_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            57289
_diffrn_reflns_av_unetI/netI     0.1273
_diffrn_reflns_av_R_equivalents  0.1319
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.259
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             8576
_reflns_number_gt                6152
_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)+(0.1000P)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         8576
_refine_ls_number_parameters     527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2043
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.2099
_refine_ls_wR_factor_gt          0.1375
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_refine_ls_shift/su_max          0.007
_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
Br2 Br 0.38014(9) 0.50653(4) 0.19230(4) 0.1071(4) Uani 1 1 d . . . . .
Br1 Br 0.92169(10) 0.43116(5) 0.43723(5) 0.1239(5) Uani 1 1 d . . . . .
Br3 Br 0.31272(14) 0.45433(5) 0.65993(4) 0.1361(5) Uani 1 1 d . . . . .
N1 N 0.0477(5) 0.0749(2) 0.39446(19) 0.0461(13) Uani 1 1 d . . . . .
C3 C 0.4653(7) 0.1567(4) 0.4049(2) 0.0573(18) Uani 1 1 d . . . . .
C1 C 0.1723(6) 0.0346(3) 0.4101(3) 0.0615(19) Uani 1 1 d . . . . .
H1A H 0.1566 -0.0091 0.3974 0.074 Uiso 1 1 calc R U . . .
H1B H 0.1765 0.0325 0.4472 0.074 Uiso 1 1 calc R U . . .
C9 C 0.7143(7) 0.2534(4) 0.4175(3) 0.085(2) Uani 1 1 d . . . . .
H9 H 0.7436 0.2105 0.4138 0.102 Uiso 1 1 calc R U . . .
C8 C 0.8192(8) 0.3022(5) 0.4232(3) 0.090(3) Uani 1 1 d . . . . .
H8 H 0.9184 0.2918 0.4229 0.108 Uiso 1 1 calc R U . . .
C6 C 0.6310(8) 0.3811(4) 0.4280(3) 0.091(3) Uani 1 1 d . . . . .
H6 H 0.6025 0.4242 0.4309 0.109 Uiso 1 1 calc R U . . .
C4 C 0.5661(7) 0.2689(4) 0.4174(3) 0.0594(19) Uani 1 1 d . . . . .
C7 C 0.7770(8) 0.3648(4) 0.4290(3) 0.077(2) Uani 1 1 d . . . . .
C5 C 0.5270(7) 0.3330(4) 0.4225(3) 0.079(2) Uani 1 1 d . . . . .
H5 H 0.4282 0.3441 0.4222 0.095 Uiso 1 1 calc R U . . .
C2 C 0.3181(6) 0.0590(4) 0.3911(3) 0.068(2) Uani 1 1 d . . . . .
H2A H 0.3973 0.0341 0.4067 0.081 Uiso 1 1 calc R U . . .
H2B H 0.3226 0.0536 0.3542 0.081 Uiso 1 1 calc R U . . .
C10 C 0.0104(7) 0.0676(3) 0.3398(3) 0.065(2) Uani 1 1 d . . . . .
H10A H -0.0465 0.0282 0.3351 0.077 Uiso 1 1 calc R U . . .
H10B H 0.1001 0.0628 0.3207 0.077 Uiso 1 1 calc R U . . .
C13 C 0.1729(7) 0.3309(4) 0.2785(3) 0.0615(19) Uani 1 1 d . . . . .
C11 C -0.0767(7) 0.1247(4) 0.3179(3) 0.070(2) Uani 1 1 d . . . . .
H11A H -0.0921 0.1187 0.2814 0.084 Uiso 1 1 calc R U . . .
H11B H -0.1720 0.1265 0.3338 0.084 Uiso 1 1 calc R U . . .
C12 C 0.0337(7) 0.2273(4) 0.2896(3) 0.0542(18) Uani 1 1 d . . . . .
C14 C 0.1623(7) 0.3352(4) 0.2258(3) 0.070(2) Uani 1 1 d . . . . .
H14 H 0.1140 0.3033 0.2069 0.084 Uiso 1 1 calc R U . . .
C16 C 0.2976(8) 0.4354(4) 0.2276(4) 0.069(2) Uani 1 1 d . . . . .
C18 C 0.2476(9) 0.3786(4) 0.3055(3) 0.086(2) Uani 1 1 d . . . . .
H18 H 0.2568 0.3763 0.3410 0.103 Uiso 1 1 calc R U . . .
C15 C 0.2251(8) 0.3884(4) 0.2013(3) 0.076(2) Uani 1 1 d . . . . .
H15 H 0.2169 0.3916 0.1658 0.091 Uiso 1 1 calc R U . . .
C17 C 0.3087(9) 0.4301(4) 0.2788(4) 0.097(3) Uani 1 1 d . . . . .
H17 H 0.3591 0.4620 0.2970 0.116 Uiso 1 1 calc R U . . .
C22 C 0.1524(7) 0.2873(4) 0.5510(3) 0.0600(19) Uani 1 1 d . . . . .
C21 C 0.0295(7) 0.1840(4) 0.5242(3) 0.0591(19) Uani 1 1 d . . . . .
C23 C 0.2157(9) 0.3423(4) 0.5321(3) 0.083(2) Uani 1 1 d . . . . .
H23 H 0.2263 0.3466 0.4969 0.100 Uiso 1 1 calc R U . . .
C27 C 0.1352(7) 0.2821(4) 0.6041(3) 0.069(2) Uani 1 1 d . . . . .
H27 H 0.0926 0.2453 0.6181 0.083 Uiso 1 1 calc R U . . .
C24 C 0.2646(9) 0.3922(4) 0.5641(4) 0.088(2) Uani 1 1 d . . . . .
H24 H 0.3087 0.4287 0.5502 0.106 Uiso 1 1 calc R U . . .
C20 C -0.0630(8) 0.0872(4) 0.4803(3) 0.069(2) Uani 1 1 d . . . . .
H20A H -0.1573 0.0869 0.4968 0.083 Uiso 1 1 calc R U . . .
H20B H 0.0027 0.0589 0.4995 0.083 Uiso 1 1 calc R U . . .
C19 C -0.0805(7) 0.0621(3) 0.4259(3) 0.063(2) Uani 1 1 d . . . . .
H19A H -0.0978 0.0157 0.4269 0.076 Uiso 1 1 calc R U . . .
H19B H -0.1657 0.0824 0.4100 0.076 Uiso 1 1 calc R U . . .
C25 C 0.2478(9) 0.3875(4) 0.6158(4) 0.084(2) Uani 1 1 d . . . . .
C26 C 0.1829(8) 0.3329(5) 0.6361(3) 0.080(2) Uani 1 1 d . . . . .
H26 H 0.1707 0.3298 0.6714 0.096 Uiso 1 1 calc R U . . .
N6 N -0.0047(5) 0.1525(3) 0.4805(2) 0.0607(15) Uani 1 1 d . . . . .
H6N H 0.0084 0.1718 0.4517 0.073 Uiso 1 1 calc R U . . .
N3 N 0.4535(5) 0.2226(3) 0.4116(2) 0.0625(15) Uani 1 1 d . . . . .
H3N H 0.3656 0.2376 0.4123 0.075 Uiso 1 1 calc R U . . .
N5 N 0.1125(5) 0.2796(3) 0.3076(2) 0.0632(16) Uani 1 1 d . . . . .
H5N H 0.1268 0.2815 0.3402 0.076 Uiso 1 1 calc R U . . .
N2 N 0.3344(5) 0.1263(3) 0.40401(19) 0.0603(15) Uani 1 1 d . . . . .
H2N H 0.2575 0.1481 0.4116 0.072 Uiso 1 1 calc R U . . .
N4 N 0.0003(5) 0.1851(3) 0.3269(2) 0.0628(16) Uani 1 1 d . . . . .
H4N H 0.0262 0.1945 0.3579 0.075 Uiso 1 1 calc R U . . .
N7 N 0.1065(6) 0.2407(3) 0.5158(2) 0.0662(16) Uani 1 1 d . . . . .
H7N H 0.1291 0.2482 0.4844 0.079 Uiso 1 1 calc R U . . .
O1 O 0.5816(4) 0.1272(2) 0.39933(18) 0.0702(14) Uani 1 1 d . . . . .
O3 O -0.0040(5) 0.2198(2) 0.2442(2) 0.0715(14) Uani 1 1 d . . . . .
O2 O -0.0060(5) 0.1646(3) 0.5671(2) 0.0842(16) Uani 1 1 d . . . . .
F1 F 0.1560(3) 0.24422(17) 0.41177(12) 0.0565(9) Uani 1 1 d . . . . .
N8 N 0.3536(6) 0.7654(3) 0.3518(2) 0.0692(17) Uani 1 1 d . . . . .
C32 C 0.2514(7) 0.8172(4) 0.3292(3) 0.073(2) Uani 1 1 d . . . . .
H32A H 0.1934 0.7977 0.3018 0.088 Uiso 1 1 calc R U . . .
H32B H 0.1844 0.8309 0.3555 0.088 Uiso 1 1 calc R U . . .
C36 C 0.4530(7) 0.7378(4) 0.3106(3) 0.073(2) Uani 1 1 d . . . . .
H36A H 0.5081 0.7733 0.2959 0.088 Uiso 1 1 calc R U . . .
H36B H 0.5227 0.7086 0.3269 0.088 Uiso 1 1 calc R U . . .
C33 C 0.3263(9) 0.8768(4) 0.3082(3) 0.094(3) Uani 1 1 d . . . . .
H33A H 0.4124 0.8636 0.2895 0.113 Uiso 1 1 calc R U . . .
H33B H 0.3585 0.9041 0.3365 0.113 Uiso 1 1 calc R U . . .
C40 C 0.2560(8) 0.7138(4) 0.3743(3) 0.091(3) Uani 1 1 d . . . . .
H40A H 0.1901 0.6984 0.3474 0.110 Uiso 1 1 calc R U . . .
H40B H 0.1963 0.7339 0.4003 0.110 Uiso 1 1 calc R U . . .
C28 C 0.4586(8) 0.7943(4) 0.3921(3) 0.091(3) Uani 1 1 d . . . . .
H28A H 0.5182 0.7594 0.4061 0.109 Uiso 1 1 calc R U . . .
H28B H 0.5240 0.8240 0.3749 0.109 Uiso 1 1 calc R U . . .
C37 C 0.3750(7) 0.7019(4) 0.2677(3) 0.087(3) Uani 1 1 d . . . . .
H37A H 0.2856 0.7247 0.2583 0.104 Uiso 1 1 calc R U . . .
H37B H 0.3486 0.6588 0.2793 0.104 Uiso 1 1 calc R U . . .
C38 C 0.4720(8) 0.6966(5) 0.2214(3) 0.115(3) Uani 1 1 d . . . . .
H38A H 0.4192 0.6717 0.1956 0.138 Uiso 1 1 calc R U . . .
H38B H 0.4851 0.7399 0.2078 0.138 Uiso 1 1 calc R U . . .
C41 C 0.3325(10) 0.6549(5) 0.3983(4) 0.125(3) Uani 1 1 d . . . . .
H41A H 0.3839 0.6677 0.4295 0.150 Uiso 1 1 calc R U . . .
H41B H 0.4037 0.6375 0.3747 0.150 Uiso 1 1 calc R U . . .
C34 C 0.2247(10) 0.9167(4) 0.2721(4) 0.104(3) Uani 1 1 d . . . . .
H34A H 0.1287 0.9205 0.2873 0.125 Uiso 1 1 calc R U . . .
H34B H 0.2643 0.9600 0.2683 0.125 Uiso 1 1 calc R U . . .
C29 C 0.3897(9) 0.8300(6) 0.4361(3) 0.132(4) Uani 1 1 d . . . . .
H29A H 0.3202 0.8614 0.4226 0.158 Uiso 1 1 calc R U . . .
H29B H 0.3361 0.7993 0.4569 0.158 Uiso 1 1 calc R U . . .
C42 C 0.2173(13) 0.6027(6) 0.4104(5) 0.183(7) Uani 1 1 d . . . . .
H42A H 0.1493 0.6196 0.4353 0.220 Uiso 1 1 calc R U . . .
H42B H 0.1622 0.5920 0.3794 0.220 Uiso 1 1 calc R U . . .
C31 C 0.6075(14) 0.9075(6) 0.4513(4) 0.166(5) Uani 1 1 d . . . . .
H31A H 0.6924 0.8836 0.4410 0.248 Uiso 1 1 calc R U . . .
H31B H 0.6345 0.9372 0.4781 0.248 Uiso 1 1 calc R U . . .
H31C H 0.5684 0.9312 0.4225 0.248 Uiso 1 1 calc R U . . .
C30 C 0.5006(12) 0.8641(8) 0.4693(4) 0.175(6) Uani 1 1 d . . . . .
H30A H 0.4454 0.8878 0.4946 0.210 Uiso 1 1 calc R U . . .
H30B H 0.5537 0.8305 0.4877 0.210 Uiso 1 1 calc R U . . .
C39 C 0.6140(8) 0.6682(5) 0.2278(3) 0.120(4) Uani 1 1 d . . . . .
H39A H 0.6723 0.6944 0.2507 0.180 Uiso 1 1 calc R U . . .
H39B H 0.6607 0.6656 0.1952 0.180 Uiso 1 1 calc R U . . .
H39C H 0.6044 0.6254 0.2419 0.180 Uiso 1 1 calc R U . . .
C43 C 0.2876(16) 0.5447(8) 0.4306(6) 0.220(6) Uani 1 1 d . . . . .
H43A H 0.3393 0.5232 0.4037 0.329 Uiso 1 1 calc R U . . .
H43B H 0.2146 0.5160 0.4439 0.329 Uiso 1 1 calc R U . . .
H43C H 0.3554 0.5565 0.4575 0.329 Uiso 1 1 calc R U . . .
C35 C 0.2092(10) 0.8856(5) 0.2202(4) 0.136(4) Uani 1 1 d . . . . .
H35A H 0.3045 0.8798 0.2058 0.203 Uiso 1 1 calc R U . . .
H35B H 0.1510 0.9129 0.1981 0.203 Uiso 1 1 calc R U . . .
H35C H 0.1623 0.8441 0.2235 0.203 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
Br2 C16 1.895(7) . ?
Br1 C7 1.911(7) . ?
Br3 C25 1.885(8) . ?
N1 C1 1.462(7) . ?
N1 C19 1.463(7) . ?
N1 C10 1.470(7) . ?
C3 O1 1.234(7) . ?
C3 N2 1.349(7) . ?
C3 N3 1.374(8) . ?
C1 C2 1.513(8) . ?
C9 C4 1.389(8) . ?
C9 C8 1.395(10) . ?
C8 C7 1.355(10) . ?
C6 C7 1.375(9) . ?
C6 C5 1.378(9) . ?
C4 C5 1.376(9) . ?
C4 N3 1.409(8) . ?
C2 N2 1.436(8) . ?
C10 C11 1.527(9) . ?
C13 C14 1.380(9) . ?
C13 C18 1.384(9) . ?
C13 N5 1.419(8) . ?
C11 N4 1.447(8) . ?
C12 O3 1.239(7) . ?
C12 N4 1.344(8) . ?
C12 N5 1.374(8) . ?
C14 C15 1.397(9) . ?
C16 C17 1.341(10) . ?
C16 C15 1.355(10) . ?
C18 C17 1.392(10) . ?
C22 C23 1.369(9) . ?
C22 N7 1.389(8) . ?
C22 C27 1.402(9) . ?
C21 O2 1.237(8) . ?
C21 N6 1.346(8) . ?
C21 N7 1.384(9) . ?
C23 C24 1.393(10) . ?
C27 C26 1.405(10) . ?
C24 C25 1.364(10) . ?
C20 N6 1.447(8) . ?
C20 C19 1.517(9) . ?
C25 C26 1.381(11) . ?
N8 C40 1.512(9) . ?
N8 C36 1.528(8) . ?
N8 C32 1.531(8) . ?
N8 C28 1.532(8) . ?
C32 C33 1.513(10) . ?
C36 C37 1.512(9) . ?
C33 C34 1.547(11) . ?
C40 C41 1.530(11) . ?
C28 C29 1.509(10) . ?
C37 C38 1.512(9) . ?
C38 C39 1.429(10) . ?
C41 C42 1.540(13) . ?
C34 C35 1.505(11) . ?
C29 C30 1.497(12) . ?
C42 C43 1.453(16) . ?
C31 C30 1.409(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
C1 N1 C19 111.5(5) . . ?
C1 N1 C10 112.3(5) . . ?
C19 N1 C10 110.5(5) . . ?
O1 C3 N2 122.1(7) . . ?
O1 C3 N3 124.9(7) . . ?
N2 C3 N3 113.0(6) . . ?
N1 C1 C2 113.8(5) . . ?
C4 C9 C8 120.0(7) . . ?
C7 C8 C9 120.2(7) . . ?
C7 C6 C5 119.4(8) . . ?
C5 C4 C9 118.3(7) . . ?
C5 C4 N3 118.1(6) . . ?
C9 C4 N3 123.6(7) . . ?
C8 C7 C6 120.5(7) . . ?
C8 C7 Br1 119.8(6) . . ?
C6 C7 Br1 119.6(7) . . ?
C4 C5 C6 121.5(7) . . ?
N2 C2 C1 109.4(5) . . ?
N1 C10 C11 113.2(6) . . ?
C14 C13 C18 119.2(7) . . ?
C14 C13 N5 124.1(7) . . ?
C18 C13 N5 116.7(7) . . ?
N4 C11 C10 110.8(5) . . ?
O3 C12 N4 123.4(7) . . ?
O3 C12 N5 124.0(7) . . ?
N4 C12 N5 112.6(7) . . ?
C13 C14 C15 119.0(7) . . ?
C17 C16 C15 118.4(8) . . ?
C17 C16 Br2 121.5(7) . . ?
C15 C16 Br2 120.0(7) . . ?
C13 C18 C17 118.9(8) . . ?
C16 C15 C14 121.9(8) . . ?
C16 C17 C18 122.5(8) . . ?
C23 C22 N7 117.3(7) . . ?
C23 C22 C27 118.3(7) . . ?
N7 C22 C27 124.4(7) . . ?
O2 C21 N6 123.4(7) . . ?
O2 C21 N7 123.9(7) . . ?
N6 C21 N7 112.6(7) . . ?
C22 C23 C24 121.9(8) . . ?
C22 C27 C26 119.6(7) . . ?
C25 C24 C23 120.0(8) . . ?
N6 C20 C19 110.7(6) . . ?
N1 C19 C20 113.0(5) . . ?
C24 C25 C26 119.6(8) . . ?
C24 C25 Br3 120.9(8) . . ?
C26 C25 Br3 119.5(8) . . ?
C25 C26 C27 120.6(8) . . ?
C21 N6 C20 122.2(6) . . ?
C3 N3 C4 128.7(6) . . ?
C12 N5 C13 127.4(6) . . ?
C3 N2 C2 122.8(6) . . ?
C12 N4 C11 123.6(6) . . ?
C21 N7 C22 128.8(6) . . ?
C40 N8 C36 111.8(6) . . ?
C40 N8 C32 106.4(5) . . ?
C36 N8 C32 110.6(5) . . ?
C40 N8 C28 112.0(6) . . ?
C36 N8 C28 104.8(5) . . ?
C32 N8 C28 111.3(6) . . ?
C33 C32 N8 115.6(6) . . ?
C37 C36 N8 115.3(5) . . ?
C32 C33 C34 112.5(7) . . ?
N8 C40 C41 116.7(7) . . ?
C29 C28 N8 116.6(6) . . ?
C36 C37 C38 110.7(6) . . ?
C39 C38 C37 118.5(8) . . ?
C40 C41 C42 109.3(8) . . ?
C35 C34 C33 111.6(8) . . ?
C30 C29 C28 112.5(7) . . ?
C43 C42 C41 110.5(10) . . ?
C31 C30 C29 124.8(11) . . ?

_refine_diff_density_max         0.623
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.057

####################################################################### 
# 
# 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-p-I-nco-TBASO4
_database_code_depnum_ccdc_archive 'CCDC 1832727'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-10-24 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(C27 H30 I3 N7 O3), 2(C16 H36 N), O4 S'
_chemical_formula_sum            'C86 H132 I6 N16 O10 S'
_chemical_formula_weight         2343.54

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   18.0490(6)
_cell_length_b                   21.7263(6)
_cell_length_c                   28.4345(10)
_cell_angle_alpha                90
_cell_angle_beta                 107.237(3)
_cell_angle_gamma                90
_cell_volume                     10649.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8425
_cell_measurement_theta_min      3.3150
_cell_measurement_theta_max      20.1360

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             4696.0
_exptl_transmission_factor_min   0.543
_exptl_transmission_factor_max   0.633
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    1.826
_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                   'micro-focus sealed X-ray tube'
_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            44541
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.866
_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 0.773
_diffrn_reflns_point_group_measured_fraction_full 0.773
_reflns_number_total             36998
_reflns_number_gt                15433
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.506
_reflns_Friedel_fraction_max     0.535
_reflns_Friedel_fraction_full    0.535

_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    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1000P)²+0.5987P] 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 4021 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         36998
_refine_ls_number_parameters     2231
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_ref         0.1893
_refine_ls_wR_factor_gt          0.1552
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_restrained_S_all      0.906
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.005

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
C22 C 0.8266(19) 0.2000(10) 0.5943(10) 0.129(8) Uani 1 1 d . . . . .
C23 C 0.8636(15) 0.2326(10) 0.6407(7) 0.117(7) Uani 1 1 d . . . . .
H23 H 0.8406 0.2331 0.6660 0.141 Uiso 1 1 calc R U . . .
C26 C 0.944(2) 0.2269(13) 0.5708(9) 0.160(11) Uani 1 1 d . . . . .
H26 H 0.9739 0.2217 0.5496 0.192 Uiso 1 1 calc R U . . .
C27 C 0.863(2) 0.1979(12) 0.5591(8) 0.155(11) Uani 1 1 d . . . . .
H27 H 0.8395 0.1795 0.5288 0.186 Uiso 1 1 calc R U . . .
I5 I 0.59898(6) 0.13098(19) 0.99044(5) 0.0983(4) Uani 1 1 d . . . . .
I4 I 1.19532(8) 0.63819(19) 1.24368(4) 0.1089(4) Uani 1 1 d . . . . .
I7 I 0.37564(7) 0.12952(19) 0.52035(5) 0.1189(4) Uani 1 1 d . . . . .
I11 I 1.14795(8) 0.77705(19) 0.12992(6) 0.1248(5) Uani 1 1 d . . . . .
I6 I 0.41711(8) 0.78713(19) 0.87051(6) 0.1229(5) Uani 1 1 d . . . . .
I12 I 0.85022(7) 0.1218(2) 0.01626(7) 0.1454(7) Uani 1 1 d . . . . .
I9 I 0.64891(7) 0.77135(19) 0.64763(7) 0.1349(6) Uani 1 1 d . . . . .
I2 I 0.32113(8) 0.1124(2) 0.26026(5) 0.1324(6) Uani 1 1 d . . . . .
I10 I 0.41780(11) 0.64156(19) -0.24970(5) 0.1461(6) Uani 1 1 d . . . . .
I8 I -0.09849(12) 0.66065(19) 0.23549(6) 0.1522(7) Uani 1 1 d . . . . .
S1 S 0.2774(2) 0.5205(2) 0.49460(14) 0.0628(9) Uani 1 1 d D . . . .
S2 S 0.78367(18) 0.5174(2) 0.01022(13) 0.0586(8) Uani 1 1 d D . . . .
I1 I 0.88064(7) -0.36099(19) 0.49517(6) 0.1250(5) Uani 1 1 d . . . . .
I3 I 1.07862(16) 0.2957(2) 0.62483(8) 0.2007(10) Uani 1 1 d . . . . .
C31 C 1.0533(8) 0.5267(7) 1.0960(6) 0.076(4) Uani 1 1 d . . . . .
C32 C 1.0193(9) 0.5401(9) 1.1319(6) 0.090(5) Uani 1 1 d . . . . .
H32 H 0.9690 0.5268 1.1286 0.108 Uiso 1 1 calc R U . . .
C33 C 1.0592(10) 0.5728(10) 1.1728(7) 0.102(6) Uani 1 1 d . . . . .
H33 H 1.0346 0.5837 1.1961 0.123 Uiso 1 1 calc R U . . .
C35 C 1.1717(10) 0.5770(9) 1.1462(7) 0.095(5) Uani 1 1 d . . . . .
H35 H 1.2235 0.5876 1.1519 0.113 Uiso 1 1 calc R U . . .
C34 C 1.1359(11) 0.5901(8) 1.1798(6) 0.090(5) Uani 1 1 d . . . . .
C30 C 1.0270(8) 0.4772(7) 1.0108(6) 0.066(4) Uani 1 1 d . . . . .
C28 C 0.9772(9) 0.4774(8) 0.8926(6) 0.084(5) Uani 1 1 d . . . . .
H28A H 1.0157 0.5091 0.9055 0.101 Uiso 1 1 calc R U . . .
H28B H 0.9904 0.4569 0.8659 0.101 Uiso 1 1 calc R U . . .
C29 C 0.9798(9) 0.4326(8) 0.9315(6) 0.089(5) Uani 1 1 d . . . . .
H29A H 0.9405 0.4017 0.9182 0.106 Uiso 1 1 calc R U . . .
H29B H 1.0298 0.4121 0.9398 0.106 Uiso 1 1 calc R U . . .
N8 N 0.9012(6) 0.5059(6) 0.8736(4) 0.070(3) Uani 1 1 d . . . . .
N12 N 0.7036(6) 0.3798(6) 0.9195(4) 0.067(3) Uani 1 1 d . . . . .
H12N H 0.7138 0.4074 0.9422 0.081 Uiso 1 1 calc R U . . .
N9 N 0.9687(6) 0.4556(7) 0.9759(4) 0.078(4) Uani 1 1 d . . . . .
H9N H 0.9232 0.4551 0.9796 0.094 Uiso 1 1 calc R U . . .
N10 N 1.0079(7) 0.4982(7) 1.0523(5) 0.092(4) Uani 1 1 d . . . . .
H10N H 0.9601 0.4928 1.0509 0.111 Uiso 1 1 calc R U . . .
N11 N 0.7473(6) 0.4539(6) 0.8768(4) 0.073(3) Uani 1 1 d . . . . .
H11N H 0.7575 0.4754 0.9034 0.088 Uiso 1 1 calc R U . . .
O4 O 1.0958(6) 0.4759(5) 1.0114(4) 0.088(3) Uani 1 1 d . . . . .
O5 O 0.7005(6) 0.3637(5) 0.8390(4) 0.080(3) Uani 1 1 d . . . . .
C39 C 0.7149(7) 0.3964(7) 0.8759(7) 0.072(4) Uani 1 1 d . . . . .
C40 C 0.6779(8) 0.3243(7) 0.9316(5) 0.063(4) Uani 1 1 d . . . . .
C45 C 0.6677(10) 0.2709(8) 0.9031(6) 0.084(4) Uani 1 1 d . . . . .
H45 H 0.6766 0.2717 0.8725 0.101 Uiso 1 1 calc R U . . .
C43 C 0.6308(7) 0.2140(7) 0.9638(6) 0.070(4) Uani 1 1 d . . . . .
C42 C 0.6390(7) 0.2661(9) 0.9917(6) 0.084(5) Uani 1 1 d . . . . .
H42 H 0.6292 0.2643 1.0220 0.101 Uiso 1 1 calc R U . . .
C38 C 0.7643(8) 0.4788(8) 0.8349(5) 0.078(4) Uani 1 1 d . . . . .
H38A H 0.7533 0.5226 0.8332 0.094 Uiso 1 1 calc R U . . .
H38B H 0.7305 0.4599 0.8055 0.094 Uiso 1 1 calc R U . . .
C44 C 0.6446(10) 0.2175(8) 0.9200(7) 0.098(5) Uani 1 1 d . . . . .
H44 H 0.6382 0.1824 0.9006 0.117 Uiso 1 1 calc R U . . .
C37 C 0.8498(8) 0.4690(7) 0.8358(5) 0.071(4) Uani 1 1 d . . . . .
H37A H 0.8633 0.4259 0.8419 0.085 Uiso 1 1 calc R U . . .
H37B H 0.8557 0.4799 0.8041 0.085 Uiso 1 1 calc R U . . .
C41 C 0.6616(8) 0.3219(7) 0.9759(5) 0.069(4) Uani 1 1 d . . . . .
H41 H 0.6655 0.3571 0.9951 0.083 Uiso 1 1 calc R U . . .
N13 N 0.8563(8) 0.6199(6) 0.9161(5) 0.086(4) Uani 1 1 d . . . . .
H13N H 0.8558 0.5991 0.9417 0.103 Uiso 1 1 calc R U . . .
C47 C 0.9221(9) 0.6155(8) 0.8975(6) 0.091(5) Uani 1 1 d . . . . .
H47A H 0.9674 0.6032 0.9239 0.109 Uiso 1 1 calc R U . . .
H47B H 0.9324 0.6555 0.8857 0.109 Uiso 1 1 calc R U . . .
C48 C 0.7957(9) 0.6558(7) 0.8940(6) 0.078(4) Uani 1 1 d . . . . .
N14 N 0.7386(7) 0.6540(6) 0.9176(4) 0.082(4) Uani 1 1 d . . . . .
H14N H 0.7469 0.6290 0.9421 0.098 Uiso 1 1 calc R U . . .
O6 O 0.7920(7) 0.6869(6) 0.8573(5) 0.103(4) Uani 1 1 d . . . . .
C49 C 0.6698(9) 0.6871(7) 0.9072(6) 0.073(4) Uani 1 1 d . . . . .
C54 C 0.6261(10) 0.6824(8) 0.9400(6) 0.086(5) Uani 1 1 d . . . . .
H54 H 0.6441 0.6597 0.9688 0.103 Uiso 1 1 calc R U . . .
C53 C 0.5548(12) 0.7126(9) 0.9287(7) 0.096(5) Uani 1 1 d . . . . .
H53 H 0.5254 0.7103 0.9505 0.115 Uiso 1 1 calc R U . . .
O15A O 0.8404(11) 0.5126(9) 0.0601(7) 0.062(5) Uani 0.5 1 d . U P . .
O13A O 0.7454(10) 0.5791(8) 0.0082(7) 0.057(4) Uani 0.5 1 d . U P . .
N25 N 0.6943(8) 0.6417(7) 0.0878(5) 0.096(4) Uani 1 1 d . . . . .
H25N H 0.6951 0.6147 0.0658 0.115 Uiso 1 1 calc R U . . .
N26 N 0.8129(8) 0.6707(6) 0.0809(5) 0.084(4) Uani 1 1 d . . . . .
H26N H 0.8019 0.6454 0.0566 0.101 Uiso 1 1 calc R U . . .
O11 O 0.7583(7) 0.7210(7) 0.1332(6) 0.122(4) Uani 1 1 d . . . . .
C94 C 0.8860(10) 0.6967(8) 0.0930(6) 0.084(4) Uani 1 1 d . . . . .
C95 C 0.9396(11) 0.6711(8) 0.0738(7) 0.098(5) Uani 1 1 d . . . . .
H95 H 0.9265 0.6360 0.0544 0.118 Uiso 1 1 calc R U . . .
C96 C 1.0116(11) 0.6955(9) 0.0823(8) 0.108(6) Uani 1 1 d . . . . .
H96 H 1.0459 0.6787 0.0670 0.129 Uiso 1 1 calc R U . . .
N3 N 0.7938(6) -0.1183(6) 0.5874(4) 0.070(3) Uani 1 1 d . . . . .
H3N H 0.7861 -0.0869 0.5682 0.084 Uiso 1 1 calc R U . . .
N2 N 0.7625(7) -0.0513(6) 0.6393(5) 0.088(4) Uani 1 1 d . . . . .
H2N H 0.7591 -0.0250 0.6161 0.105 Uiso 1 1 calc R U . . .
C4 C 0.8141(8) -0.1724(7) 0.5678(5) 0.066(4) Uani 1 1 d . . . . .
C3 C 0.7842(7) -0.1080(7) 0.6330(5) 0.058(3) Uani 1 1 d . . . . .
C2 C 0.7443(8) -0.0316(8) 0.6822(6) 0.080(4) Uani 1 1 d . . . . .
H2A H 0.7586 0.0115 0.6877 0.096 Uiso 1 1 calc R U . . .
H2B H 0.7763 -0.0546 0.7101 0.096 Uiso 1 1 calc R U . . .
C1 C 0.6624(9) -0.0383(8) 0.6813(6) 0.086(5) Uani 1 1 d . . . . .
H1A H 0.6578 -0.0290 0.7137 0.103 Uiso 1 1 calc R U . . .
H1B H 0.6463 -0.0806 0.6736 0.103 Uiso 1 1 calc R U . . .
O1 O 0.7972(5) -0.1471(5) 0.6657(3) 0.076(3) Uani 1 1 d . . . . .
N1 N 0.6104(7) 0.0029(7) 0.6445(5) 0.087(4) Uani 1 1 d . . . . .
O10 O 0.4600(5) 0.5003(5) -0.0130(4) 0.084(3) Uani 1 1 d . . . . .
N24 N 0.5591(6) 0.5154(6) -0.0455(5) 0.071(3) Uani 1 1 d . . . . .
H24N H 0.6081 0.5089 -0.0393 0.085 Uiso 1 1 calc R U . . .
N23 N 0.5824(7) 0.4788(7) 0.0335(5) 0.092(4) Uani 1 1 d . . . . .
H23N H 0.6307 0.4776 0.0349 0.111 Uiso 1 1 calc R U . . .
C84 C 0.5300(8) 0.4987(7) -0.0093(6) 0.070(4) Uani 1 1 d . . . . .
C85 C 0.5246(9) 0.5408(7) -0.0905(6) 0.070(4) Uani 1 1 d . . . . .
C90 C 0.5675(9) 0.5512(8) -0.1217(6) 0.074(4) Uani 1 1 d . . . . .
H90 H 0.6190 0.5386 -0.1116 0.089 Uiso 1 1 calc R U . . .
C86 C 0.4499(9) 0.5584(9) -0.1053(7) 0.090(5) Uani 1 1 d . . . . .
H86 H 0.4189 0.5522 -0.0847 0.108 Uiso 1 1 calc R U . . .
C76 C 0.3889(9) 0.6874(7) 0.5959(6) 0.077(4) Uani 1 1 d . . . . .
C77 C 0.4418(10) 0.6730(8) 0.5709(6) 0.079(4) Uani 1 1 d . . . . .
H77 H 0.4271 0.6476 0.5434 0.095 Uiso 1 1 calc R U . . .
C80 C 0.4870(12) 0.7486(11) 0.6522(7) 0.118(7) Uani 1 1 d . . . . .
H80 H 0.5015 0.7750 0.6792 0.141 Uiso 1 1 calc R U . . .
C81 C 0.4113(10) 0.7231(8) 0.6367(6) 0.083(4) Uani 1 1 d . . . . .
H81 H 0.3768 0.7309 0.6546 0.100 Uiso 1 1 calc R U . . .
C75 C 0.2511(10) 0.6707(7) 0.5942(6) 0.076(4) Uani 1 1 d . . . . .
C79 C 0.5382(10) 0.7338(9) 0.6268(8) 0.092(5) Uani 1 1 d . . . . .
C78 C 0.5145(11) 0.6955(9) 0.5864(9) 0.102(6) Uani 1 1 d . . . . .
H78 H 0.5495 0.6850 0.5695 0.122 Uiso 1 1 calc R U . . .
N20 N 0.1898(7) 0.6355(7) 0.5712(5) 0.091(4) Uani 1 1 d . . . . .
H20N H 0.1921 0.6116 0.5475 0.109 Uiso 1 1 calc R U . . .
N21 N 0.3137(8) 0.6598(6) 0.5789(5) 0.083(3) Uani 1 1 d . . . . .
H21N H 0.3077 0.6327 0.5560 0.099 Uiso 1 1 calc R U . . .
O9 O 0.2476(6) 0.7114(6) 0.6226(5) 0.110(4) Uani 1 1 d . . . . .
N32 N 0.2293(6) 0.9091(6) 0.5940(5) 0.075(3) Uani 1 1 d . . . . .
C165 C 0.2848(9) 0.8699(8) 0.6335(6) 0.080(4) Uani 1 1 d . . . . .
H16A H 0.2816 0.8279 0.6216 0.096 Uiso 1 1 calc R U . . .
H16B H 0.3372 0.8842 0.6373 0.096 Uiso 1 1 calc R U . . .
C161 C 0.1455(8) 0.8895(7) 0.5847(6) 0.081(4) Uani 1 1 d . . . . .
H16C H 0.1336 0.8904 0.6158 0.098 Uiso 1 1 calc R U . . .
H16D H 0.1126 0.9197 0.5633 0.098 Uiso 1 1 calc R U . . .
C108 C 0.8551(9) 0.3178(11) 0.0443(7) 0.103(6) Uani 1 1 d . . . . .
H108 H 0.8712 0.3518 0.0300 0.124 Uiso 1 1 calc R U . . .
C106 C 0.8364(10) 0.2083(11) 0.0474(9) 0.116(7) Uani 1 1 d . . . . .
C107 C 0.8626(11) 0.2576(14) 0.0289(8) 0.127(8) Uani 1 1 d . . . . .
H107 H 0.8869 0.2514 0.0047 0.152 Uiso 1 1 calc R U . . .
C103 C 0.8211(8) 0.3234(10) 0.0834(6) 0.086(5) Uani 1 1 d . . . . .
C105 C 0.8020(10) 0.2135(10) 0.0828(6) 0.094(5) Uani 1 1 d . . . . .
H105 H 0.7828 0.1788 0.0944 0.113 Uiso 1 1 calc R U . . .
C5 C 0.8327(8) -0.1713(8) 0.5254(6) 0.079(4) Uani 1 1 d . . . . .
H5 H 0.8354 -0.1333 0.5110 0.094 Uiso 1 1 calc R U . . .
C6 C 0.8482(9) -0.2246(11) 0.5014(7) 0.098(6) Uani 1 1 d . . . . .
H6 H 0.8578 -0.2224 0.4711 0.118 Uiso 1 1 calc R U . . .
C9 C 0.8134(9) -0.2315(9) 0.5919(6) 0.087(5) Uani 1 1 d . . . . .
H9 H 0.8025 -0.2335 0.6218 0.105 Uiso 1 1 calc R U . . .
C10 C 0.5322(8) -0.0251(9) 0.6262(6) 0.094(5) Uani 1 1 d . . . . .
H10A H 0.4944 0.0072 0.6133 0.113 Uiso 1 1 calc R U . . .
H10B H 0.5192 -0.0445 0.6534 0.113 Uiso 1 1 calc R U . . .
C11 C 0.5269(11) -0.0735(10) 0.5854(7) 0.108(6) Uani 1 1 d . . . . .
H11A H 0.5663 -0.1047 0.5976 0.129 Uiso 1 1 calc R U . . .
H11B H 0.4766 -0.0934 0.5771 0.129 Uiso 1 1 calc R U . . .
N4 N 0.5375(7) -0.0455(7) 0.5422(6) 0.098(4) Uani 1 1 d . . . . .
H4N H 0.5842 -0.0430 0.5405 0.118 Uiso 1 1 calc R U . . .
C18 C 0.3804(9) 0.0312(8) 0.4095(6) 0.085(5) Uani 1 1 d . . . . .
H18 H 0.3542 0.0214 0.4322 0.102 Uiso 1 1 calc R U . . .
N5 N 0.5020(7) -0.0011(8) 0.4647(7) 0.097(4) Uani 1 1 d . . . . .
H5N H 0.5512 -0.0025 0.4691 0.116 Uiso 1 1 calc R U . . .
C17 C 0.3436(10) 0.0545(10) 0.3652(8) 0.102(6) Uani 1 1 d . . . . .
H17 H 0.2906 0.0615 0.3583 0.123 Uiso 1 1 calc R U . . .
C14 C 0.4981(10) 0.0336(9) 0.3895(8) 0.097(6) Uani 1 1 d . . . . .
H14 H 0.5512 0.0260 0.3986 0.117 Uiso 1 1 calc R U . . .
C13 C 0.4588(9) 0.0227(8) 0.4197(8) 0.085(5) Uani 1 1 d . . . . .
C15 C 0.4579(12) 0.0578(10) 0.3410(9) 0.115(7) Uani 1 1 d . . . . .
H15 H 0.4859 0.0656 0.3190 0.138 Uiso 1 1 calc R U . . .
C16 C 0.3786(11) 0.0698(9) 0.3268(7) 0.104(6) Uani 1 1 d . . . . .
C12 C 0.4791(10) -0.0224(8) 0.5032(8) 0.092(5) Uani 1 1 d . . . . .
O2 O 0.4115(7) -0.0213(6) 0.5050(4) 0.105(4) Uani 1 1 d . . . . .
C98 C 0.9827(13) 0.7703(10) 0.1336(6) 0.107(6) Uani 1 1 d . . . . .
H98 H 0.9970 0.8041 0.1544 0.128 Uiso 1 1 calc R U . . .
C99 C 0.9087(12) 0.7457(10) 0.1233(7) 0.111(6) Uani 1 1 d . . . . .
H99 H 0.8736 0.7634 0.1376 0.133 Uiso 1 1 calc R U . . .
C92 C 0.6270(10) 0.6420(9) 0.1055(7) 0.109(6) Uani 1 1 d . . . . .
H92A H 0.5817 0.6288 0.0794 0.131 Uiso 1 1 calc R U . . .
H92B H 0.6177 0.6834 0.1152 0.131 Uiso 1 1 calc R U . . .
C91 C 0.6412(10) 0.5973(9) 0.1508(7) 0.102(6) Uani 1 1 d . . . . .
H91A H 0.6906 0.6068 0.1747 0.122 Uiso 1 1 calc R U . . .
H91B H 0.6007 0.6031 0.1665 0.122 Uiso 1 1 calc R U . . .
N28 N 0.8129(7) 0.3836(8) 0.0998(5) 0.090(4) Uani 1 1 d . . . . .
H28N H 0.8204 0.4123 0.0809 0.109 Uiso 1 1 calc R U . . .
C8 C 0.8293(10) -0.2845(8) 0.5696(7) 0.091(5) Uani 1 1 d . . . . .
H8 H 0.8268 -0.3225 0.5842 0.109 Uiso 1 1 calc R U . . .
C88 C 0.4663(12) 0.5962(8) -0.1818(6) 0.091(5) Uani 1 1 d . . . . .
C89 C 0.5406(10) 0.5791(8) -0.1672(6) 0.085(4) Uani 1 1 d . . . . .
H89 H 0.5729 0.5857 -0.1869 0.101 Uiso 1 1 calc R U . . .
C82 C 0.5618(9) 0.5109(10) 0.1108(7) 0.105(6) Uani 1 1 d . . . . .
H82A H 0.5308 0.5449 0.0933 0.126 Uiso 1 1 calc R U . . .
H82B H 0.5388 0.4966 0.1356 0.126 Uiso 1 1 calc R U . . .
C83 C 0.5615(11) 0.4600(9) 0.0756(7) 0.098(5) Uani 1 1 d . . . . .
H83A H 0.5973 0.4283 0.0926 0.118 Uiso 1 1 calc R U . . .
H83B H 0.5101 0.4420 0.0649 0.118 Uiso 1 1 calc R U . . .
N22 N 0.6412(6) 0.5323(6) 0.1348(4) 0.070(3) Uani 1 1 d . . . . .
C46 C 0.9066(9) 0.5679(8) 0.8549(6) 0.086(5) Uani 1 1 d . . . . .
H46A H 0.8585 0.5781 0.8299 0.104 Uiso 1 1 calc R U . . .
H46B H 0.9483 0.5695 0.8399 0.104 Uiso 1 1 calc R U . . .
C63 C 0.3587(10) 0.3260(10) 0.5350(7) 0.100(6) Uani 1 1 d . . . . .
H63 H 0.3630 0.3600 0.5161 0.121 Uiso 1 1 calc R U . . .
C58 C 0.3383(9) 0.3357(9) 0.5789(6) 0.084(5) Uani 1 1 d . . . . .
C59 C 0.3326(11) 0.2823(10) 0.6079(6) 0.102(5) Uani 1 1 d . . . . .
H59 H 0.3200 0.2856 0.6372 0.122 Uiso 1 1 calc R U . . .
C61 C 0.3646(8) 0.2190(9) 0.5478(7) 0.091(5) Uani 1 1 d . . . . .
C57 C 0.2953(10) 0.4129(10) 0.6317(8) 0.095(6) Uani 1 1 d . . . . .
C60 C 0.3466(13) 0.2260(10) 0.5898(7) 0.117(7) Uani 1 1 d . . . . .
H60 H 0.3434 0.1909 0.6079 0.141 Uiso 1 1 calc R U . . .
N16 N 0.2818(7) 0.4727(7) 0.6317(5) 0.084(4) Uani 1 1 d . . . . .
H16N H 0.2901 0.4955 0.6091 0.101 Uiso 1 1 calc R U . . .
N17 N 0.3221(7) 0.3946(6) 0.5926(5) 0.094(4) Uani 1 1 d . . . . .
H17N H 0.3297 0.4240 0.5743 0.112 Uiso 1 1 calc R U . . .
O7 O 0.2910(10) 0.3757(7) 0.6641(5) 0.136(5) Uani 1 1 d . . . . .
C56 C 0.2534(11) 0.5002(11) 0.6688(7) 0.119(7) Uani 1 1 d . . . . .
H56A H 0.2669 0.5435 0.6715 0.143 Uiso 1 1 calc R U . . .
H56B H 0.2788 0.4811 0.7003 0.143 Uiso 1 1 calc R U . . .
C74 C 0.1195(10) 0.6378(8) 0.5863(8) 0.114(6) Uani 1 1 d . . . . .
H74A H 0.0755 0.6271 0.5584 0.137 Uiso 1 1 calc R U . . .
H74B H 0.1119 0.6797 0.5958 0.137 Uiso 1 1 calc R U . . .
C73 C 0.1214(11) 0.5962(9) 0.6277(7) 0.103(6) Uani 1 1 d . . . . .
H73A H 0.1661 0.6063 0.6552 0.123 Uiso 1 1 calc R U . . .
H73B H 0.0753 0.6033 0.6379 0.123 Uiso 1 1 calc R U . . .
N15 N 0.1248(7) 0.5321(6) 0.6160(5) 0.078(3) Uani 1 1 d . . . . .
C64 C 0.0473(9) 0.5076(8) 0.5893(6) 0.087(5) Uani 1 1 d . . . . .
H64A H 0.0149 0.5412 0.5722 0.105 Uiso 1 1 calc R U . . .
H64B H 0.0234 0.4908 0.6129 0.105 Uiso 1 1 calc R U . . .
C65 C 0.0502(10) 0.4579(8) 0.5522(7) 0.095(5) Uani 1 1 d . . . . .
H65A H 0.0869 0.4262 0.5683 0.114 Uiso 1 1 calc R U . . .
H65B H -0.0005 0.4389 0.5396 0.114 Uiso 1 1 calc R U . . .
N18 N 0.0742(8) 0.4852(7) 0.5106(5) 0.089(4) Uani 1 1 d . . . . .
H18N H 0.1224 0.4850 0.5119 0.106 Uiso 1 1 calc R U . . .
C164 C 0.0325(12) 0.7999(11) 0.6071(9) 0.143(8) Uani 1 1 d . . . . .
H16E H 0.0637 0.7656 0.6227 0.215 Uiso 1 1 calc R U . . .
H16F H -0.0210 0.7916 0.6040 0.215 Uiso 1 1 calc R U . . .
H16G H 0.0488 0.8362 0.6267 0.215 Uiso 1 1 calc R U . . .
C163 C 0.0422(11) 0.8102(11) 0.5551(9) 0.128(7) Uani 1 1 d . . . . .
H16H H 0.0288 0.7730 0.5356 0.153 Uiso 1 1 calc R U . . .
H16I H 0.0083 0.8431 0.5382 0.153 Uiso 1 1 calc R U . . .
C162 C 0.1242(10) 0.8267(9) 0.5619(7) 0.100(5) Uani 1 1 d . . . . .
H16J H 0.1340 0.8257 0.5301 0.120 Uiso 1 1 calc R U . . .
H16K H 0.1573 0.7960 0.5827 0.120 Uiso 1 1 calc R U . . .
C170 C 0.3143(11) 1.0083(9) 0.6229(9) 0.144(9) Uani 1 1 d D . . . .
H17A H 0.3549 0.9805 0.6410 0.173 Uiso 1 1 calc R U . . .
H17B H 0.3248 1.0201 0.5926 0.173 Uiso 1 1 calc R U . . .
C157 C 0.2560(9) 0.9049(9) 0.5469(6) 0.098(5) Uani 1 1 d . . . . .
H15A H 0.2554 0.8621 0.5372 0.117 Uiso 1 1 calc R U . . .
H15B H 0.3090 0.9196 0.5547 0.117 Uiso 1 1 calc R U . . .
C158 C 0.2044(11) 0.9428(11) 0.5029(6) 0.137(9) Uani 1 1 d D . . . .
H15C H 0.1501 0.9382 0.5009 0.164 Uiso 1 1 calc R U . . .
H15D H 0.2178 0.9861 0.5071 0.164 Uiso 1 1 calc R U . . .
C171 C 0.3106(13) 1.0639(9) 0.6533(11) 0.235(19) Uani 1 1 d D . . . .
H17C H 0.2804 1.0530 0.6752 0.282 Uiso 1 1 calc R U . . .
H17D H 0.2817 1.0953 0.6312 0.282 Uiso 1 1 calc R U . . .
O17A O 0.2416(9) 0.5226(8) 0.5327(6) 0.057(4) Uani 0.5 1 d . . P . .
N19 N 0.0561(7) 0.5340(7) 0.4381(5) 0.081(4) Uani 1 1 d . . . . .
H19N H 0.1058 0.5315 0.4452 0.097 Uiso 1 1 calc R U . . .
C66 C 0.0225(10) 0.5099(7) 0.4718(6) 0.074(4) Uani 1 1 d . . . . .
O8 O -0.0470(6) 0.5098(5) 0.4674(4) 0.085(3) Uani 1 1 d . . . . .
C67 C 0.0167(9) 0.5621(7) 0.3935(6) 0.077(4) Uani 1 1 d . . . . .
C72 C 0.0606(12) 0.5714(10) 0.3597(8) 0.109(6) Uani 1 1 d . . . . .
H72 H 0.1116 0.5575 0.3671 0.130 Uiso 1 1 calc R U . . .
N30 N 0.6052(9) 0.3376(6) 0.6921(5) 0.086(4) Uani 1 1 d . . . . .
C137 C 0.5706(11) 0.2778(8) 0.6984(7) 0.103(5) Uani 1 1 d . . . . .
H13A H 0.5153 0.2810 0.6822 0.124 Uiso 1 1 calc R U . . .
H13B H 0.5905 0.2477 0.6799 0.124 Uiso 1 1 calc R U . . .
C130 C 0.7441(13) 0.3771(12) 0.7008(8) 0.136(8) Uani 1 1 d . . . . .
H13C H 0.7327 0.4166 0.7130 0.164 Uiso 1 1 calc R U . . .
H13D H 0.7342 0.3803 0.6655 0.164 Uiso 1 1 calc R U . . .
C129 C 0.6923(12) 0.3275(10) 0.7124(5) 0.108(6) Uani 1 1 d . . . . .
H12A H 0.7047 0.2886 0.6998 0.130 Uiso 1 1 calc R U . . .
H12B H 0.7053 0.3236 0.7479 0.130 Uiso 1 1 calc R U . . .
C134 C 0.6004(14) 0.3142(10) 0.6032(7) 0.132(7) Uani 1 1 d . . . . .
H13E H 0.5727 0.2759 0.6030 0.159 Uiso 1 1 calc R U . . .
H13F H 0.6554 0.3053 0.6154 0.159 Uiso 1 1 calc R U . . .
C127 C 0.4873(14) 0.4491(13) 0.7499(9) 0.148(9) Uani 1 1 d . . . . .
H12C H 0.5298 0.4783 0.7580 0.178 Uiso 1 1 calc R U . . .
H12D H 0.4397 0.4717 0.7353 0.178 Uiso 1 1 calc R U . . .
C126 C 0.4996(10) 0.4023(10) 0.7121(8) 0.109(6) Uani 1 1 d . . . . .
H12E H 0.4717 0.3646 0.7136 0.131 Uiso 1 1 calc R U . . .
H12F H 0.4799 0.4190 0.6791 0.131 Uiso 1 1 calc R U . . .
C125 C 0.5804(11) 0.3896(8) 0.7228(6) 0.099(6) Uani 1 1 d . . . . .
H12G H 0.6000 0.3786 0.7574 0.119 Uiso 1 1 calc R U . . .
H12H H 0.6062 0.4274 0.7184 0.119 Uiso 1 1 calc R U . . .
C135 C 0.5826(13) 0.3369(11) 0.5514(7) 0.130(8) Uani 1 1 d . . . . .
H13G H 0.5270 0.3432 0.5387 0.155 Uiso 1 1 calc R U . . .
H13H H 0.6072 0.3767 0.5521 0.155 Uiso 1 1 calc R U . . .
C133 C 0.5798(10) 0.3577(8) 0.6376(6) 0.097(5) Uani 1 1 d . . . . .
H13I H 0.5240 0.3633 0.6271 0.117 Uiso 1 1 calc R U . . .
H13J H 0.6032 0.3973 0.6352 0.117 Uiso 1 1 calc R U . . .
C52 C 0.5286(12) 0.7443(9) 0.8874(8) 0.096(5) Uani 1 1 d . . . . .
C159 C 0.2188(12) 0.9188(12) 0.4577(6) 0.201(17) Uani 1 1 d D . . . .
H15E H 0.1945 0.8789 0.4494 0.242 Uiso 1 1 calc R U . . .
H15F H 0.2741 0.9143 0.4628 0.242 Uiso 1 1 calc R U . . .
C50 C 0.6445(9) 0.7234(8) 0.8658(7) 0.087(5) Uani 1 1 d . . . . .
H50 H 0.6752 0.7291 0.8451 0.105 Uiso 1 1 calc R U . . .
C19 C 0.6073(10) 0.0640(9) 0.6632(7) 0.100(6) Uani 1 1 d . . . . .
H19A H 0.6571 0.0739 0.6865 0.120 Uiso 1 1 calc R U . . .
H19B H 0.5684 0.0654 0.6805 0.120 Uiso 1 1 calc R U . . .
C20 C 0.5884(13) 0.1102(10) 0.6234(9) 0.131(8) Uani 1 1 d . . . . .
H20C H 0.5417 0.0972 0.5984 0.158 Uiso 1 1 calc R U . . .
H20D H 0.5770 0.1489 0.6369 0.158 Uiso 1 1 calc R U . . .
C21 C 0.7062(14) 0.1619(8) 0.6161(8) 0.108(7) Uani 1 1 d . . . . .
N7 N 0.7570(15) 0.1641(9) 0.5881(6) 0.130(7) Uani 1 1 d . . . . .
H7N H 0.7452 0.1402 0.5629 0.156 Uiso 1 1 calc R U . . .
N6 N 0.6494(12) 0.1210(8) 0.5998(6) 0.119(5) Uani 1 1 d . . . . .
H6N H 0.6483 0.0998 0.5741 0.143 Uiso 1 1 calc R U . . .
O3 O 0.7089(8) 0.1944(6) 0.6525(4) 0.120(4) Uani 1 1 d . . . . .
C62 C 0.3723(11) 0.2691(10) 0.5193(8) 0.107(6) Uani 1 1 d . . . . .
H62 H 0.3862 0.2639 0.4905 0.128 Uiso 1 1 calc R U . . .
C101 C 0.7697(10) 0.4919(10) 0.1842(6) 0.099(5) Uani 1 1 d . . . . .
H10C H 0.7892 0.5338 0.1868 0.119 Uiso 1 1 calc R U . . .
H10D H 0.7944 0.4712 0.2151 0.119 Uiso 1 1 calc R U . . .
C100 C 0.6820(10) 0.4933(9) 0.1756(6) 0.097(5) Uani 1 1 d . . . . .
H10E H 0.6619 0.4517 0.1694 0.116 Uiso 1 1 calc R U . . .
H10F H 0.6717 0.5079 0.2053 0.116 Uiso 1 1 calc R U . . .
C102 C 0.7952(11) 0.4034(10) 0.1399(8) 0.099(5) Uani 1 1 d . . . . .
N27 N 0.7897(7) 0.4614(9) 0.1457(6) 0.096(4) Uani 1 1 d . . . . .
H27N H 0.7993 0.4846 0.1237 0.115 Uiso 1 1 calc R U . . .
C104 C 0.7950(9) 0.2708(8) 0.1022(6) 0.080(4) Uani 1 1 d . . . . .
H104 H 0.7729 0.2745 0.1277 0.096 Uiso 1 1 calc R U . . .
O12 O 0.7811(7) 0.3644(7) 0.1695(4) 0.110(4) Uani 1 1 d . . . . .
C93 C 0.7565(11) 0.6802(8) 0.1027(7) 0.092(5) Uani 1 1 d . . . . .
C97 C 1.0335(11) 0.7448(9) 0.1131(8) 0.099(6) Uani 1 1 d . . . . .
C87 C 0.4179(9) 0.5864(9) -0.1519(7) 0.098(5) Uani 1 1 d . . . . .
H87 H 0.3660 0.5980 -0.1625 0.117 Uiso 1 1 calc R U . . .
C138 C 0.5797(14) 0.2514(12) 0.7468(9) 0.149(9) Uani 1 1 d . . . . .
H98O H 0.6346 0.2502 0.7646 0.179 Uiso 1 1 calc R U . . .
H96O H 0.5550 0.2786 0.7647 0.179 Uiso 1 1 calc R U . . .
C7 C 0.8486(9) -0.2819(10) 0.5260(8) 0.099(6) Uani 1 1 d . . . . .
C68 C -0.0609(11) 0.5816(10) 0.3801(8) 0.109(6) Uani 1 1 d . . . . .
H68 H -0.0905 0.5764 0.4016 0.131 Uiso 1 1 calc R U . . .
C69 C -0.0919(11) 0.6079(10) 0.3363(7) 0.106(6) Uani 1 1 d . . . . .
H69 H -0.1435 0.6200 0.3276 0.127 Uiso 1 1 calc R U . . .
C71 C 0.0256(15) 0.6016(9) 0.3156(7) 0.117(7) Uani 1 1 d . . . . .
H71 H 0.0544 0.6108 0.2943 0.140 Uiso 1 1 calc R U . . .
C70 C -0.0507(14) 0.6177(8) 0.3035(8) 0.112(7) Uani 1 1 d . . . . .
C55 C 0.1646(10) 0.4938(11) 0.6579(7) 0.110(6) Uani 1 1 d . . . . .
H55A H 0.1497 0.4511 0.6507 0.132 Uiso 1 1 calc R U . . .
H55B H 0.1497 0.5061 0.6865 0.132 Uiso 1 1 calc R U . . .
C136 C 0.6060(18) 0.2985(13) 0.5182(7) 0.188(13) Uani 1 1 d . . . . .
H97O H 0.6573 0.2831 0.5338 0.282 Uiso 1 1 calc R U . . .
H95O H 0.6060 0.3218 0.4895 0.282 Uiso 1 1 calc R U . . .
H13M H 0.5706 0.2646 0.5087 0.282 Uiso 1 1 calc R U . . .
C36 C 1.1313(10) 0.5471(9) 1.1022(6) 0.092(5) Uani 1 1 d . . . . .
H36 H 1.1546 0.5407 1.0776 0.111 Uiso 1 1 calc R U . . .
C128 C 0.483(2) 0.4205(14) 0.7926(11) 0.24(2) Uani 1 1 d . . . . .
H12I H 0.4303 0.4095 0.7892 0.364 Uiso 1 1 calc R U . . .
H12J H 0.5018 0.4480 0.8199 0.364 Uiso 1 1 calc R U . . .
H12K H 0.5146 0.3840 0.7982 0.364 Uiso 1 1 calc R U . . .
N29 N 0.2829(6) 0.3846(6) 0.9905(5) 0.080(4) Uani 1 1 d . . . . .
C113 C 0.2311(9) 0.4079(9) 0.9459(8) 0.108(6) Uani 1 1 d . . . . .
H11C H 0.1838 0.4200 0.9530 0.130 Uiso 1 1 calc R U . . .
H11D H 0.2177 0.3738 0.9229 0.130 Uiso 1 1 calc R U . . .
C109 C 0.3632(7) 0.3683(8) 0.9849(7) 0.093(5) Uani 1 1 d . . . . .
H10G H 0.3854 0.4053 0.9756 0.112 Uiso 1 1 calc R U . . .
H10H H 0.3967 0.3555 1.0168 0.112 Uiso 1 1 calc R U . . .
C114 C 0.2558(11) 0.4617(11) 0.9192(8) 0.131(8) Uani 1 1 d . . . . .
H11E H 0.2691 0.4970 0.9410 0.157 Uiso 1 1 calc R U . . .
H11F H 0.3010 0.4503 0.9094 0.157 Uiso 1 1 calc R U . . .
C121 C 0.2956(11) 0.4360(8) 1.0307(9) 0.102(6) Uani 1 1 d . . . . .
H12L H 0.3229 0.4697 1.0208 0.122 Uiso 1 1 calc R U . . .
H12M H 0.2449 0.4514 1.0302 0.122 Uiso 1 1 calc R U . . .
C110 C 0.3646(12) 0.3196(11) 0.9488(9) 0.133(8) Uani 1 1 d . . . . .
H11G H 0.3294 0.3297 0.9167 0.160 Uiso 1 1 calc R U . . .
H11H H 0.3490 0.2804 0.9592 0.160 Uiso 1 1 calc R U . . .
C118 C 0.1702(10) 0.3353(9) 1.0144(9) 0.120(7) Uani 1 1 d . . . . .
H11I H 0.1740 0.3695 1.0369 0.144 Uiso 1 1 calc R U . . .
H11J H 0.1319 0.3461 0.9836 0.144 Uiso 1 1 calc R U . . .
C117 C 0.2491(9) 0.3269(8) 1.0048(8) 0.100(6) Uani 1 1 d . . . . .
H11K H 0.2856 0.3103 1.0344 0.120 Uiso 1 1 calc R U . . .
H11L H 0.2433 0.2967 0.9788 0.120 Uiso 1 1 calc R U . . .
C122 C 0.3398(11) 0.4196(11) 1.0845(10) 0.129(8) Uani 1 1 d . . . . .
H99X H 0.3905 0.4030 1.0862 0.155 Uiso 1 1 calc R U . . .
H12O H 0.3114 0.3885 1.0966 0.155 Uiso 1 1 calc R U . . .
C169 C 0.2329(9) 0.9766(8) 0.6115(7) 0.098(5) Uani 1 1 d . . . . .
H16L H 0.2163 0.9781 0.6410 0.117 Uiso 1 1 calc R U . . .
H16M H 0.1959 1.0004 0.5863 0.117 Uiso 1 1 calc R U . . .
C120 C 0.0599(9) 0.2914(11) 1.0360(8) 0.138(9) Uani 1 1 d . . . . .
H12P H 0.0537 0.3323 1.0470 0.207 Uiso 1 1 calc R U . . .
H12Q H 0.0491 0.2620 1.0583 0.207 Uiso 1 1 calc R U . . .
H12R H 0.0246 0.2852 1.0036 0.207 Uiso 1 1 calc R U . . .
C119 C 0.1440(10) 0.2827(9) 1.0343(8) 0.115(6) Uani 1 1 d . . . . .
H11M H 0.1778 0.2752 1.0673 0.138 Uiso 1 1 calc R U . . .
H99S H 0.1465 0.2470 1.0143 0.138 Uiso 1 1 calc R U . . .
C124 C 0.3946(15) 0.4553(16) 1.1688(9) 0.231(18) Uani 1 1 d D . . . .
H12S H 0.3606 0.4317 1.1822 0.346 Uiso 1 1 calc R U . . .
H12T H 0.4142 0.4899 1.1898 0.346 Uiso 1 1 calc R U . . .
H12U H 0.4370 0.4299 1.1667 0.346 Uiso 1 1 calc R U . . .
C123 C 0.3494(14) 0.4783(13) 1.1170(9) 0.163(11) Uani 1 1 d D . . . .
H12V H 0.3783 0.5098 1.1058 0.196 Uiso 1 1 calc R U . . .
H12W H 0.2993 0.4948 1.1166 0.196 Uiso 1 1 calc R U . . .
C139 C 0.550(2) 0.1930(14) 0.7471(10) 0.228(18) Uani 1 1 d . . . . .
H94O H 0.5711 0.1678 0.7261 0.273 Uiso 1 1 calc R U . . .
H92O H 0.4944 0.1959 0.7309 0.273 Uiso 1 1 calc R U . . .
C51 C 0.5703(13) 0.7521(9) 0.8553(7) 0.109(6) Uani 1 1 d . . . . .
H51 H 0.5509 0.7757 0.8270 0.130 Uiso 1 1 calc R U . . .
C115 C 0.1895(15) 0.4779(13) 0.8744(14) 0.29(3) Uani 1 1 d D . . . .
H11O H 0.1417 0.4846 0.8825 0.344 Uiso 1 1 calc R U . . .
H11P H 0.1814 0.4466 0.8490 0.344 Uiso 1 1 calc R U . . .
C111 C 0.4497(12) 0.3160(11) 0.9463(8) 0.169(12) Uani 1 1 d D . . . .
H97H H 0.4859 0.3299 0.9770 0.203 Uiso 1 1 calc R U . . .
H95H H 0.4629 0.2742 0.9399 0.203 Uiso 1 1 calc R U . . .
C112 C 0.4522(13) 0.3589(17) 0.9036(10) 0.30(3) Uani 1 1 d D . . . .
H94H H 0.4133 0.3903 0.8995 0.454 Uiso 1 1 calc R U . . .
H11R H 0.4423 0.3354 0.8738 0.454 Uiso 1 1 calc R U . . .
H11S H 0.5024 0.3778 0.9109 0.454 Uiso 1 1 calc R U . . .
C140 C 0.559(2) 0.1584(17) 0.7924(13) 0.27(2) Uani 1 1 d . . . . .
H14A H 0.5826 0.1193 0.7899 0.411 Uiso 1 1 calc R U . . .
H14B H 0.5094 0.1521 0.7973 0.411 Uiso 1 1 calc R U . . .
H14C H 0.5920 0.1810 0.8196 0.411 Uiso 1 1 calc R U . . .
N31 N 0.9699(9) 0.7776(7) 0.7666(6) 0.110(5) Uani 1 1 d . . . . .
C141 C 0.9227(10) 0.7331(10) 0.7266(6) 0.100(6) Uani 1 1 d . . . . .
H14D H 0.9481 0.7300 0.7010 0.120 Uiso 1 1 calc R U . . .
H14E H 0.8718 0.7508 0.7118 0.120 Uiso 1 1 calc R U . . .
C142 C 0.9121(14) 0.6669(11) 0.7449(8) 0.138(8) Uani 1 1 d . . . . .
H14F H 0.9621 0.6506 0.7636 0.166 Uiso 1 1 calc R U . . .
H14G H 0.8793 0.6686 0.7664 0.166 Uiso 1 1 calc R U . . .
C153 C 0.931(2) 0.7860(12) 0.8071(8) 0.167(12) Uani 1 1 d . . . . .
H15G H 0.9623 0.8142 0.8316 0.200 Uiso 1 1 calc R U . . .
H15H H 0.9305 0.7467 0.8231 0.200 Uiso 1 1 calc R U . . .
C149 C 0.9751(10) 0.8386(9) 0.7425(6) 0.099(5) Uani 1 1 d . . . . .
H14H H 0.9225 0.8516 0.7259 0.119 Uiso 1 1 calc R U . . .
H14I H 1.0000 0.8310 0.7171 0.119 Uiso 1 1 calc R U . . .
C143 C 0.8763(10) 0.6254(10) 0.7026(7) 0.131(7) Uani 1 1 d D . . . .
H98Q H 0.8363 0.6474 0.6780 0.157 Uiso 1 1 calc R U . . .
H96Q H 0.8522 0.5907 0.7138 0.157 Uiso 1 1 calc R U . . .
C151 C 1.0177(14) 0.9501(10) 0.7414(9) 0.139(8) Uani 1 1 d . . . . .
H15I H 1.0428 0.9835 0.7630 0.167 Uiso 1 1 calc R U . . .
H15J H 0.9648 0.9626 0.7249 0.167 Uiso 1 1 calc R U . . .
C150 C 1.0163(13) 0.8928(10) 0.7726(9) 0.136(8) Uani 1 1 d . . . . .
H15K H 1.0693 0.8810 0.7899 0.163 Uiso 1 1 calc R U . . .
H15L H 0.9907 0.9030 0.7972 0.163 Uiso 1 1 calc R U . . .
C154 C 0.8469(17) 0.8113(14) 0.7876(9) 0.181(13) Uani 1 1 d D . . . .
H102 H 0.8479 0.8451 0.7655 0.217 Uiso 1 1 calc R U . . .
H98X H 0.8155 0.7790 0.7678 0.217 Uiso 1 1 calc R U . . .
C146 C 1.1124(13) 0.723(2) 0.7580(15) 0.38(4) Uani 1 1 d D . . . .
H97Q H 1.0941 0.6810 0.7555 0.451 Uiso 1 1 calc R U . . .
H95Q H 1.0910 0.7397 0.7250 0.451 Uiso 1 1 calc R U . . .
C145 C 1.0595(15) 0.7529(10) 0.7840(9) 0.206(17) Uani 1 1 d . . . . .
H14L H 1.0889 0.7884 0.8001 0.247 Uiso 1 1 calc R U . . .
H14M H 1.0605 0.7242 0.8103 0.247 Uiso 1 1 calc R U . . .
C167 C 0.3354(13) 0.8381(13) 0.7213(7) 0.169(11) Uani 1 1 d D . . . .
H96S H 0.3384 0.7958 0.7112 0.203 Uiso 1 1 calc R U . . .
H16O H 0.3189 0.8371 0.7508 0.203 Uiso 1 1 calc R U . . .
C168 C 0.4184(13) 0.8649(16) 0.7358(9) 0.182(13) Uani 1 1 d . . . . .
H16P H 0.4469 0.8465 0.7158 0.273 Uiso 1 1 calc R U . . .
H16Q H 0.4440 0.8561 0.7698 0.273 Uiso 1 1 calc R U . . .
H16R H 0.4159 0.9086 0.7308 0.273 Uiso 1 1 calc R U . . .
C132 C 0.8849(14) 0.4051(18) 0.7186(10) 0.224(18) Uani 1 1 d . . . . .
H98S H 0.9191 0.3859 0.7028 0.336 Uiso 1 1 calc R U . . .
H93O H 0.9146 0.4209 0.7501 0.336 Uiso 1 1 calc R U . . .
H91O H 0.8577 0.4383 0.6985 0.336 Uiso 1 1 calc R U . . .
C152 C 1.0613(15) 0.9394(11) 0.7019(10) 0.160(9) Uani 1 1 d . . . . .
H101 H 1.0996 0.9078 0.7132 0.240 Uiso 1 1 calc R U . . .
H99W H 1.0861 0.9769 0.6970 0.240 Uiso 1 1 calc R U . . .
H15O H 1.0247 0.9269 0.6714 0.240 Uiso 1 1 calc R U . . .
C144 C 0.9382(13) 0.6019(17) 0.6796(11) 0.26(2) Uani 1 1 d D . . . .
H97S H 0.9153 0.5965 0.6448 0.383 Uiso 1 1 calc R U . . .
H14O H 0.9583 0.5632 0.6943 0.383 Uiso 1 1 calc R U . . .
H14P H 0.9797 0.6313 0.6854 0.383 Uiso 1 1 calc R U . . .
C148 C 1.175(3) 0.6508(12) 0.7776(17) 0.41(4) Uani 1 1 d D . . . .
H14Q H 1.1454 0.6569 0.8001 0.615 Uiso 1 1 calc R U . . .
H14R H 1.2223 0.6292 0.7940 0.615 Uiso 1 1 calc R U . . .
H14S H 1.1457 0.6270 0.7499 0.615 Uiso 1 1 calc R U . . .
C155 C 0.8030(19) 0.8343(12) 0.8232(11) 0.29(3) Uani 1 1 d D . . . .
H98W H 0.7475 0.8303 0.8082 0.354 Uiso 1 1 calc R U . . .
H96W H 0.8178 0.8105 0.8534 0.354 Uiso 1 1 calc R U . . .
C166 C 0.2728(9) 0.8693(11) 0.6817(7) 0.124(7) Uani 1 1 d D . . . .
H16S H 0.2239 0.8489 0.6791 0.148 Uiso 1 1 calc R U . . .
H16T H 0.2683 0.9115 0.6917 0.148 Uiso 1 1 calc R U . . .
C131 C 0.8298(14) 0.3604(17) 0.7253(11) 0.213(17) Uani 1 1 d . . . . .
H13Q H 0.8378 0.3550 0.7603 0.256 Uiso 1 1 calc R U . . .
H13R H 0.8403 0.3213 0.7122 0.256 Uiso 1 1 calc R U . . .
C147 C 1.1954(10) 0.7137(15) 0.7596(14) 0.32(3) Uani 1 1 d D . . . .
H14T H 1.2331 0.7380 0.7839 0.389 Uiso 1 1 calc R U . . .
H14U H 1.2053 0.7135 0.7278 0.389 Uiso 1 1 calc R U . . .
C160 C 0.1843(16) 0.9650(16) 0.4159(11) 0.33(3) Uani 1 1 d D . . . .
H16U H 0.1571 0.9967 0.4275 0.497 Uiso 1 1 calc R U . . .
H16V H 0.1490 0.9440 0.3886 0.497 Uiso 1 1 calc R U . . .
H16W H 0.2253 0.9830 0.4054 0.497 Uiso 1 1 calc R U . . .
C172 C 0.3865(16) 1.0936(18) 0.6851(16) 0.38(3) Uani 1 1 d D . . . .
H17E H 0.4108 1.0671 0.7122 0.573 Uiso 1 1 calc R U . . .
H17F H 0.3752 1.1326 0.6973 0.573 Uiso 1 1 calc R U . . .
H17G H 0.4209 1.0997 0.6654 0.573 Uiso 1 1 calc R U . . .
C156 C 0.825(3) 0.9024(12) 0.8341(19) 0.40(4) Uani 1 1 d D . . . .
H97W H 0.8807 0.9064 0.8442 0.601 Uiso 1 1 calc R U . . .
H95W H 0.8054 0.9168 0.8600 0.601 Uiso 1 1 calc R U . . .
H15R H 0.8034 0.9264 0.8050 0.601 Uiso 1 1 calc R U . . .
C116 C 0.2214(18) 0.5380(12) 0.8592(13) 0.27(2) Uani 1 1 d D . . . .
H96H H 0.2768 0.5388 0.8728 0.402 Uiso 1 1 calc R U . . .
H98H H 0.1994 0.5725 0.8713 0.402 Uiso 1 1 calc R U . . .
H93H H 0.2079 0.5401 0.8239 0.402 Uiso 1 1 calc R U . . .
O20A O 0.3246(10) 0.5768(7) 0.4940(6) 0.056(4) Uani 0.5 1 d . . P . .
C24 C 0.9289(18) 0.2606(12) 0.6455(9) 0.152(10) Uani 1 1 d . . . . .
H24 H 0.9504 0.2836 0.6738 0.182 Uiso 1 1 calc R U . . .
C25 C 0.9687(17) 0.2577(10) 0.6097(9) 0.143(9) Uani 1 1 d . . . . .
O17B O 0.3069(18) 0.5177(14) 0.4571(11) 0.138(10) Uani 0.5 1 d . . P . .
O18B O 0.243(2) 0.5829(17) 0.4925(12) 0.162(12) Uani 0.5 1 d . . P . .
O14B O 0.7470(19) 0.532(2) 0.0452(15) 0.189(17) Uani 0.5 1 d . . P . .
O15B O 0.7228(17) 0.492(2) -0.0300(12) 0.164(16) Uani 0.5 1 d . U P . .
O14A O 0.8237(9) 0.5138(9) -0.0288(6) 0.059(4) Uani 0.5 1 d . . P . .
O19A O 0.2183(9) 0.5142(8) 0.4460(6) 0.053(4) Uani 0.5 1 d . . P . .
O18A O 0.3326(9) 0.4674(9) 0.5024(8) 0.070(5) Uani 0.5 1 d . . P . .
O16A O 0.7231(8) 0.4689(9) 0.0022(6) 0.047(4) Uani 0.5 1 d . . P . .
O19B O 0.3338(13) 0.5090(15) 0.5420(6) 0.134(10) Uani 0.5 1 d D . P . .
O16B O 0.816(2) 0.5722(17) 0.0008(14) 0.174(15) Uani 0.5 1 d . . P . .
O20B O 0.2120(13) 0.4758(13) 0.4844(12) 0.124(10) Uani 0.5 1 d . . P . .
O13B O 0.8430(9) 0.4731(11) 0.0339(15) 0.192(19) Uani 0.5 1 d D 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
C22 C27 1.35(3) . ?
C22 N7 1.44(3) . ?
C22 C23 1.47(3) . ?
C23 C24 1.30(3) . ?
C26 C25 1.26(3) . ?
C26 C27 1.54(4) . ?
I5 C43 2.101(15) . ?
I4 C34 2.095(17) . ?
I7 C61 2.126(18) . ?
I11 C97 2.098(18) . ?
I6 C52 2.139(19) . ?
I12 C106 2.12(3) . ?
I9 C79 2.075(17) . ?
I2 C16 2.09(2) . ?
I10 C88 2.114(18) . ?
I8 C70 2.09(2) . ?
S1 O17B 1.33(3) . ?
S1 O17A 1.418(16) . ?
S1 O19B 1.4499(13) . ?
S1 O19A 1.481(16) . ?
S1 O18B 1.48(4) . ?
S1 O20B 1.49(3) . ?
S1 O20A 1.493(15) . ?
S1 O18A 1.498(18) . ?
S2 O14B 1.39(3) . ?
S2 O16B 1.39(3) . ?
S2 O15B 1.44(3) . ?
S2 O13B 1.4499(9) . ?
S2 O16A 1.486(17) . ?
S2 O15A 1.487(18) . ?
S2 O14A 1.495(15) . ?
S2 O13A 1.502(16) . ?
I1 C7 2.088(18) . ?
I3 C25 2.07(3) . ?
C31 C32 1.37(2) . ?
C31 N10 1.414(19) . ?
C31 C36 1.44(2) . ?
C32 C33 1.37(2) . ?
C33 C34 1.39(2) . ?
C35 C34 1.33(2) . ?
C35 C36 1.41(2) . ?
C30 O4 1.239(14) . ?
C30 N9 1.302(17) . ?
C30 N10 1.399(18) . ?
C28 N8 1.455(18) . ?
C28 C29 1.46(2) . ?
C29 N9 1.424(18) . ?
N8 C37 1.439(17) . ?
N8 C46 1.462(19) . ?
N12 C39 1.363(19) . ?
N12 C40 1.371(17) . ?
N11 C39 1.377(18) . ?
N11 C38 1.422(16) . ?
O5 C39 1.231(17) . ?
C40 C41 1.378(18) . ?
C40 C45 1.40(2) . ?
C45 C44 1.37(2) . ?
C43 C44 1.34(2) . ?
C43 C42 1.36(2) . ?
C42 C41 1.40(2) . ?
C38 C37 1.55(2) . ?
N13 C48 1.337(18) . ?
N13 C47 1.438(19) . ?
C47 C46 1.55(2) . ?
C48 O6 1.228(18) . ?
C48 N14 1.387(19) . ?
N14 C49 1.387(18) . ?
C49 C50 1.38(2) . ?
C49 C54 1.39(2) . ?
C54 C53 1.39(2) . ?
C53 C52 1.32(2) . ?
O15A O13B 1.15(4) . ?
O15A O14B 1.67(4) . ?
O13A O16B 1.36(4) . ?
O13A O14B 1.46(5) . ?
N25 C93 1.364(19) . ?
N25 C92 1.45(2) . ?
N26 C93 1.36(2) . ?
N26 C94 1.381(19) . ?
O11 C93 1.23(2) . ?
C94 C99 1.35(2) . ?
C94 C95 1.36(2) . ?
C95 C96 1.36(2) . ?
C96 C97 1.37(3) . ?
N3 C3 1.376(17) . ?
N3 C4 1.396(18) . ?
N2 C3 1.321(17) . ?
N2 C2 1.420(18) . ?
C4 C5 1.342(19) . ?
C4 C9 1.46(2) . ?
C3 O1 1.229(16) . ?
C2 C1 1.478(19) . ?
C1 N1 1.48(2) . ?
N1 C19 1.44(2) . ?
N1 C10 1.481(19) . ?
O10 C84 1.236(14) . ?
N24 C84 1.337(18) . ?
N24 C85 1.364(18) . ?
N23 C84 1.372(19) . ?
N23 C83 1.416(19) . ?
C85 C86 1.34(2) . ?
C85 C90 1.357(19) . ?
C90 C89 1.38(2) . ?
C86 C87 1.42(2) . ?
C76 C81 1.35(2) . ?
C76 C77 1.38(2) . ?
C76 N21 1.431(18) . ?
C77 C78 1.35(2) . ?
C80 C79 1.37(2) . ?
C80 C81 1.42(2) . ?
C75 O9 1.212(18) . ?
C75 N20 1.345(19) . ?
C75 N21 1.348(18) . ?
C79 C78 1.38(3) . ?
N20 C74 1.46(2) . ?
N32 C161 1.516(17) . ?
N32 C165 1.524(18) . ?
N32 C169 1.54(2) . ?
N32 C157 1.555(19) . ?
C165 C166 1.45(2) . ?
C161 C162 1.51(2) . ?
C108 C107 1.40(3) . ?
C108 C103 1.43(2) . ?
C106 C105 1.33(3) . ?
C106 C107 1.34(3) . ?
C103 C104 1.40(2) . ?
C103 N28 1.41(2) . ?
C105 C104 1.38(2) . ?
C5 C6 1.41(2) . ?
C6 C7 1.43(3) . ?
C9 C8 1.38(2) . ?
C10 C11 1.55(2) . ?
C11 N4 1.43(2) . ?
N4 C12 1.38(2) . ?
C18 C17 1.34(2) . ?
C18 C13 1.37(2) . ?
N5 C12 1.36(2) . ?
N5 C13 1.39(2) . ?
C17 C16 1.45(3) . ?
C14 C13 1.29(2) . ?
C14 C15 1.45(3) . ?
C15 C16 1.39(2) . ?
C12 O2 1.237(19) . ?
C98 C97 1.34(2) . ?
C98 C99 1.39(2) . ?
C92 C91 1.57(2) . ?
C91 N22 1.48(2) . ?
N28 C102 1.34(2) . ?
C8 C7 1.38(2) . ?
C88 C89 1.33(2) . ?
C88 C87 1.40(2) . ?
C82 N22 1.47(2) . ?
C82 C83 1.49(2) . ?
N22 C100 1.450(19) . ?
C63 C62 1.36(3) . ?
C63 C58 1.42(2) . ?
C58 N17 1.39(2) . ?
C58 C59 1.45(2) . ?
C59 C60 1.38(2) . ?
C61 C60 1.34(2) . ?
C61 C62 1.39(2) . ?
C57 O7 1.25(2) . ?
C57 N16 1.32(2) . ?
C57 N17 1.39(2) . ?
N16 C56 1.43(2) . ?
C56 C55 1.55(2) . ?
C74 C73 1.48(2) . ?
C73 N15 1.44(2) . ?
N15 C55 1.46(2) . ?
N15 C64 1.480(18) . ?
C64 C65 1.52(2) . ?
C65 N18 1.50(2) . ?
N18 C66 1.329(18) . ?
C164 C163 1.56(3) . ?
C163 C162 1.48(2) . ?
C170 C171 1.4997(13) . ?
C170 C169 1.57(2) . ?
C157 C158 1.56(2) . ?
C158 C159 1.4804(13) . ?
C171 C172 1.5409(15) . ?
O17A O19B 1.63(3) . ?
O17A O20B 1.66(3) . ?
O17A O18B 1.75(3) . ?
N19 C66 1.378(19) . ?
N19 C67 1.397(19) . ?
C66 O8 1.224(17) . ?
C67 C68 1.40(2) . ?
C67 C72 1.43(2) . ?
C72 C71 1.39(3) . ?
N30 C137 1.47(2) . ?
N30 C129 1.52(2) . ?
N30 C133 1.542(19) . ?
N30 C125 1.573(18) . ?
C137 C138 1.46(3) . ?
C130 C129 1.53(3) . ?
C130 C131 1.54(3) . ?
C134 C133 1.49(2) . ?
C134 C135 1.49(2) . ?
C127 C128 1.39(3) . ?
C127 C126 1.54(3) . ?
C126 C125 1.43(2) . ?
C135 C136 1.42(3) . ?
C52 C51 1.36(2) . ?
C159 C160 1.5399(13) . ?
C50 C51 1.43(2) . ?
C19 C20 1.47(3) . ?
C20 N6 1.47(3) . ?
C21 O3 1.24(2) . ?
C21 N6 1.33(2) . ?
C21 N7 1.38(3) . ?
C101 N27 1.41(2) . ?
C101 C100 1.53(2) . ?
C102 O12 1.27(2) . ?
C102 N27 1.28(2) . ?
C138 C139 1.38(3) . ?
C68 C69 1.33(2) . ?
C69 C70 1.37(3) . ?
C71 C70 1.36(3) . ?
N29 C113 1.43(2) . ?
N29 C117 1.503(19) . ?
N29 C109 1.546(17) . ?
N29 C121 1.57(2) . ?
C113 C114 1.53(2) . ?
C109 C110 1.48(2) . ?
C114 C115 1.51(3) . ?
C121 C122 1.54(3) . ?
C110 C111 1.56(3) . ?
C118 C119 1.42(2) . ?
C118 C117 1.54(2) . ?
C122 C123 1.55(3) . ?
C120 C119 1.54(2) . ?
C124 C123 1.5400(13) . ?
C139 C140 1.46(4) . ?
C115 C116 1.5399(14) . ?
C111 C112 1.5408(13) . ?
N31 C149 1.51(2) . ?
N31 C153 1.52(3) . ?
N31 C141 1.54(2) . ?
N31 C145 1.64(3) . ?
C141 C142 1.56(3) . ?
C142 C143 1.49(3) . ?
C153 C154 1.56(3) . ?
C149 C150 1.52(2) . ?
C143 C144 1.5400(14) . ?
C151 C150 1.53(3) . ?
C151 C152 1.57(3) . ?
C154 C155 1.5410(13) . ?
C146 C147 1.5001(10) . ?
C146 C145 1.51(4) . ?
C167 C166 1.5007(13) . ?
C167 C168 1.54(3) . ?
C132 C131 1.44(4) . ?
C148 C147 1.5406(13) . ?
C155 C156 1.539(2) . ?
O20A O18B 1.46(4) . ?
O20A O17B 1.63(4) . ?
C24 C25 1.41(3) . ?
O17B O19A 1.54(3) . ?
O17B O18A 1.65(3) . ?
O14B O16A 1.81(4) . ?
O15B O16A 1.05(4) . ?
O14A O16B 1.55(4) . ?
O19A O20B 1.40(3) . ?
O18A O19B 1.44(3) . ?

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
C27 C22 N7 119(3) . . ?
C27 C22 C23 119(3) . . ?
N7 C22 C23 121(2) . . ?
C24 C23 C22 118(2) . . ?
C25 C26 C27 119(3) . . ?
C22 C27 C26 118(2) . . ?
O17B S1 O17A 176.7(15) . . ?
O17B S1 O19B 113.6(18) . . ?
O17A S1 O19B 69.4(14) . . ?
O17B S1 O19A 66.1(14) . . ?
O17A S1 O19A 110.6(9) . . ?
O19B S1 O19A 164.6(15) . . ?
O17B S1 O18B 105.6(18) . . ?
O17A S1 O18B 74.1(15) . . ?
O19B S1 O18B 111.4(19) . . ?
O19A S1 O18B 82.7(15) . . ?
O17B S1 O20B 107.3(17) . . ?
O17A S1 O20B 69.8(12) . . ?
O19B S1 O20B 111.5(18) . . ?
O19A S1 O20B 56.4(13) . . ?
O18B S1 O20B 107.1(18) . . ?
O17B S1 O20A 70.3(14) . . ?
O17A S1 O20A 111.9(10) . . ?
O19B S1 O20A 84.6(13) . . ?
O19A S1 O20A 108.8(10) . . ?
O18B S1 O20A 58.8(15) . . ?
O20B S1 O20A 162.5(15) . . ?
O17B S1 O18A 71.1(14) . . ?
O17A S1 O18A 110.1(10) . . ?
O19B S1 O18A 58.4(14) . . ?
O19A S1 O18A 109.3(11) . . ?
O18B S1 O18A 163.8(17) . . ?
O20B S1 O18A 88.9(12) . . ?
O20A S1 O18A 106.0(9) . . ?
O14B S2 O16B 105(3) . . ?
O14B S2 O15B 104.1(18) . . ?
O16B S2 O15B 116(2) . . ?
O14B S2 O13B 105(2) . . ?
O16B S2 O13B 111.4(18) . . ?
O15B S2 O13B 114(2) . . ?
O14B S2 O16A 77.9(18) . . ?
O16B S2 O16A 155.8(16) . . ?
O15B S2 O16A 41.9(16) . . ?
O13B S2 O16A 90.5(12) . . ?
O14B S2 O15A 70.9(18) . . ?
O16B S2 O15A 91.9(17) . . ?
O15B S2 O15A 152(2) . . ?
O13B S2 O15A 46.0(17) . . ?
O16A S2 O15A 111.3(11) . . ?
O14B S2 O14A 170(2) . . ?
O16B S2 O14A 65.1(19) . . ?
O15B S2 O14A 79.2(14) . . ?
O13B S2 O14A 81.7(17) . . ?
O16A S2 O14A 110.1(9) . . ?
O15A S2 O14A 110.9(10) . . ?
O14B S2 O13A 60(2) . . ?
O16B S2 O13A 56.1(18) . . ?
O15B S2 O13A 94.2(19) . . ?
O13B S2 O13A 151.6(19) . . ?
O16A S2 O13A 108.5(10) . . ?
O15A S2 O13A 106.2(10) . . ?
O14A S2 O13A 109.7(10) . . ?
C32 C31 N10 118.6(13) . . ?
C32 C31 C36 118.9(15) . . ?
N10 C31 C36 122.3(15) . . ?
C31 C32 C33 120.2(15) . . ?
C32 C33 C34 120.8(15) . . ?
C34 C35 C36 120.1(16) . . ?
C35 C34 C33 120.9(16) . . ?
C35 C34 I4 119.7(14) . . ?
C33 C34 I4 119.4(13) . . ?
O4 C30 N9 125.5(14) . . ?
O4 C30 N10 119.7(14) . . ?
N9 C30 N10 114.6(12) . . ?
N8 C28 C29 112.3(12) . . ?
N9 C29 C28 117.1(13) . . ?
C37 N8 C28 111.6(12) . . ?
C37 N8 C46 109.9(12) . . ?
C28 N8 C46 111.8(12) . . ?
C39 N12 C40 127.8(12) . . ?
C30 N9 C29 120.6(12) . . ?
C30 N10 C31 131.4(12) . . ?
C39 N11 C38 121.8(13) . . ?
O5 C39 N12 125.0(14) . . ?
O5 C39 N11 121.4(16) . . ?
N12 C39 N11 113.6(14) . . ?
N12 C40 C41 116.2(13) . . ?
N12 C40 C45 125.5(13) . . ?
C41 C40 C45 118.3(13) . . ?
C44 C45 C40 120.1(14) . . ?
C44 C43 C42 118.3(15) . . ?
C44 C43 I5 121.9(13) . . ?
C42 C43 I5 119.8(12) . . ?
C43 C42 C41 121.7(14) . . ?
N11 C38 C37 113.2(11) . . ?
C43 C44 C45 122.3(16) . . ?
N8 C37 C38 110.7(12) . . ?
C40 C41 C42 119.3(14) . . ?
C48 N13 C47 121.0(14) . . ?
N13 C47 C46 110.6(12) . . ?
O6 C48 N13 123.4(16) . . ?
O6 C48 N14 124.3(15) . . ?
N13 C48 N14 112.3(15) . . ?
C49 N14 C48 129.0(13) . . ?
C50 C49 N14 121.9(15) . . ?
C50 C49 C54 120.1(16) . . ?
N14 C49 C54 117.9(14) . . ?
C49 C54 C53 118.7(15) . . ?
C52 C53 C54 120.8(17) . . ?
O13B O15A S2 65.3(12) . . ?
O13B O15A O14B 105(2) . . ?
S2 O15A O14B 51.8(15) . . ?
O16B O13A O14B 102(2) . . ?
O16B O13A S2 57.6(15) . . ?
O14B O13A S2 55.9(13) . . ?
C93 N25 C92 126.0(16) . . ?
C93 N26 C94 128.0(14) . . ?
C99 C94 C95 117.4(16) . . ?
C99 C94 N26 124.5(16) . . ?
C95 C94 N26 118.2(15) . . ?
C96 C95 C94 121.7(17) . . ?
C95 C96 C97 120.0(18) . . ?
C3 N3 C4 129.4(12) . . ?
C3 N2 C2 123.5(14) . . ?
C5 C4 N3 120.5(14) . . ?
C5 C4 C9 118.5(14) . . ?
N3 C4 C9 120.9(13) . . ?
O1 C3 N2 122.7(13) . . ?
O1 C3 N3 123.4(12) . . ?
N2 C3 N3 113.8(14) . . ?
N2 C2 C1 116.0(12) . . ?
C2 C1 N1 112.0(14) . . ?
C19 N1 C1 112.5(13) . . ?
C19 N1 C10 111.8(13) . . ?
C1 N1 C10 109.9(14) . . ?
C84 N24 C85 131.2(12) . . ?
C84 N23 C83 123.6(13) . . ?
O10 C84 N24 123.4(15) . . ?
O10 C84 N23 120.3(14) . . ?
N24 C84 N23 116.3(12) . . ?
C86 C85 C90 117.5(16) . . ?
C86 C85 N24 123.0(14) . . ?
C90 C85 N24 119.4(14) . . ?
C85 C90 C89 125.2(16) . . ?
C85 C86 C87 120.5(15) . . ?
C81 C76 C77 119.6(16) . . ?
C81 C76 N21 122.8(15) . . ?
C77 C76 N21 117.5(15) . . ?
C78 C77 C76 120.2(17) . . ?
C79 C80 C81 118.9(19) . . ?
C76 C81 C80 120.4(16) . . ?
O9 C75 N20 122.8(16) . . ?
O9 C75 N21 123.9(16) . . ?
N20 C75 N21 113.0(14) . . ?
C80 C79 C78 119.3(17) . . ?
C80 C79 I9 120.1(17) . . ?
C78 C79 I9 120.6(14) . . ?
C77 C78 C79 121.6(17) . . ?
C75 N20 C74 119.9(15) . . ?
C75 N21 C76 128.3(14) . . ?
C161 N32 C165 112.1(11) . . ?
C161 N32 C169 105.6(11) . . ?
C165 N32 C169 109.8(12) . . ?
C161 N32 C157 112.3(12) . . ?
C165 N32 C157 107.3(11) . . ?
C169 N32 C157 109.8(12) . . ?
C166 C165 N32 116.8(12) . . ?
C162 C161 N32 116.3(13) . . ?
C107 C108 C103 115(2) . . ?
C105 C106 C107 122(2) . . ?
C105 C106 I12 121.9(18) . . ?
C107 C106 I12 116.4(19) . . ?
C106 C107 C108 123(2) . . ?
C104 C103 N28 123.3(15) . . ?
C104 C103 C108 120.0(18) . . ?
N28 C103 C108 116.6(19) . . ?
C106 C105 C104 120(2) . . ?
C4 C5 C6 123.8(17) . . ?
C5 C6 C7 116.7(16) . . ?
C8 C9 C4 119.1(15) . . ?
N1 C10 C11 112.5(13) . . ?
N4 C11 C10 111.1(16) . . ?
C12 N4 C11 125.4(16) . . ?
C17 C18 C13 116.3(17) . . ?
C12 N5 C13 130.5(14) . . ?
C18 C17 C16 126.1(16) . . ?
C13 C14 C15 118.7(18) . . ?
C14 C13 C18 125(2) . . ?
C14 C13 N5 114.5(17) . . ?
C18 C13 N5 120.5(17) . . ?
C16 C15 C14 121.7(18) . . ?
C15 C16 C17 112.2(18) . . ?
C15 C16 I2 122.6(16) . . ?
C17 C16 I2 125.0(14) . . ?
O2 C12 N5 124.4(17) . . ?
O2 C12 N4 120(2) . . ?
N5 C12 N4 115.4(17) . . ?
C97 C98 C99 119.2(19) . . ?
C94 C99 C98 121.8(17) . . ?
N25 C92 C91 109.4(14) . . ?
N22 C91 C92 110.6(14) . . ?
C102 N28 C103 130.8(16) . . ?
C9 C8 C7 121.0(17) . . ?
C89 C88 C87 121.3(17) . . ?
C89 C88 I10 121.2(12) . . ?
C87 C88 I10 117.4(15) . . ?
C88 C89 C90 117.0(15) . . ?
N22 C82 C83 110.8(13) . . ?
N23 C83 C82 113.9(16) . . ?
C100 N22 C82 112.5(13) . . ?
C100 N22 C91 110.9(13) . . ?
C82 N22 C91 110.8(13) . . ?
N8 C46 C47 110.2(13) . . ?
C62 C63 C58 123.0(18) . . ?
N17 C58 C63 121.0(16) . . ?
N17 C58 C59 121.5(16) . . ?
C63 C58 C59 117.5(17) . . ?
C60 C59 C58 116.7(16) . . ?
C60 C61 C62 121.8(18) . . ?
C60 C61 I7 120.4(15) . . ?
C62 C61 I7 117.7(15) . . ?
O7 C57 N16 125.8(16) . . ?
O7 C57 N17 121.2(18) . . ?
N16 C57 N17 112.8(18) . . ?
C61 C60 C59 123.6(19) . . ?
C57 N16 C56 121.1(16) . . ?
C57 N17 C58 129.4(16) . . ?
N16 C56 C55 112.9(14) . . ?
N20 C74 C73 113.5(14) . . ?
N15 C73 C74 113.7(15) . . ?
C73 N15 C55 114.3(15) . . ?
C73 N15 C64 111.5(14) . . ?
C55 N15 C64 112.1(13) . . ?
N15 C64 C65 112.9(13) . . ?
N18 C65 C64 110.0(13) . . ?
C66 N18 C65 121.5(14) . . ?
C162 C163 C164 107.5(17) . . ?
C163 C162 C161 113.1(16) . . ?
C171 C170 C169 106.0(15) . . ?
N32 C157 C158 113.5(12) . . ?
C159 C158 C157 107.2(15) . . ?
C170 C171 C172 119(2) . . ?
S1 O17A O19B 56.3(8) . . ?
S1 O17A O20B 57.1(11) . . ?
O19B O17A O20B 94.9(15) . . ?
S1 O17A O18B 54.7(13) . . ?
O19B O17A O18B 91.5(16) . . ?
O20B O17A O18B 88.9(19) . . ?
C66 N19 C67 125.8(13) . . ?
O8 C66 N18 121.9(16) . . ?
O8 C66 N19 125.4(14) . . ?
N18 C66 N19 112.7(15) . . ?
N19 C67 C68 125.3(17) . . ?
N19 C67 C72 115.9(16) . . ?
C68 C67 C72 118.8(18) . . ?
C71 C72 C67 119(2) . . ?
C137 N30 C129 104.7(14) . . ?
C137 N30 C133 111.1(14) . . ?
C129 N30 C133 112.8(12) . . ?
C137 N30 C125 111.5(13) . . ?
C129 N30 C125 108.9(13) . . ?
C133 N30 C125 107.8(12) . . ?
C138 C137 N30 121.9(17) . . ?
C129 C130 C131 110(2) . . ?
N30 C129 C130 116.6(17) . . ?
C133 C134 C135 114.6(19) . . ?
C128 C127 C126 112(2) . . ?
C125 C126 C127 109.1(16) . . ?
C126 C125 N30 117.4(14) . . ?
C136 C135 C134 116.3(19) . . ?
C134 C133 N30 115.1(14) . . ?
C53 C52 C51 123(2) . . ?
C53 C52 I6 119.5(14) . . ?
C51 C52 I6 117.8(16) . . ?
C158 C159 C160 107.9(19) . . ?
C49 C50 C51 118.9(16) . . ?
N1 C19 C20 111.8(15) . . ?
N6 C20 C19 115.2(17) . . ?
O3 C21 N6 120(3) . . ?
O3 C21 N7 126(2) . . ?
N6 C21 N7 113(2) . . ?
C21 N7 C22 131(2) . . ?
C21 N6 C20 123.5(19) . . ?
C63 C62 C61 117.4(17) . . ?
N27 C101 C100 112.0(15) . . ?
N22 C100 C101 113.3(13) . . ?
O12 C102 N27 122(2) . . ?
O12 C102 N28 119.5(19) . . ?
N27 C102 N28 118(2) . . ?
C102 N27 C101 127.6(18) . . ?
C105 C104 C103 120.1(17) . . ?
O11 C93 N26 124.3(16) . . ?
O11 C93 N25 120(2) . . ?
N26 C93 N25 115.2(16) . . ?
C98 C97 C96 119.8(18) . . ?
C98 C97 I11 121.1(17) . . ?
C96 C97 I11 119.1(16) . . ?
C88 C87 C86 118.5(15) . . ?
C139 C138 C137 116(2) . . ?
C8 C7 C6 120.6(16) . . ?
C8 C7 I1 121.1(16) . . ?
C6 C7 I1 118.2(15) . . ?
C69 C68 C67 119.4(18) . . ?
C68 C69 C70 122.8(19) . . ?
C70 C71 C72 120(2) . . ?
C71 C70 C69 119.9(18) . . ?
C71 C70 I8 117.3(19) . . ?
C69 C70 I8 122.8(16) . . ?
N15 C55 C56 110.1(16) . . ?
C35 C36 C31 118.9(15) . . ?
C113 N29 C117 108.9(13) . . ?
C113 N29 C109 112.2(13) . . ?
C117 N29 C109 107.7(11) . . ?
C113 N29 C121 108.1(14) . . ?
C117 N29 C121 112.3(13) . . ?
C109 N29 C121 107.5(12) . . ?
N29 C113 C114 120.1(15) . . ?
C110 C109 N29 116.4(13) . . ?
C115 C114 C113 108.8(18) . . ?
C122 C121 N29 118.7(16) . . ?
C109 C110 C111 106.6(16) . . ?
C119 C118 C117 114.2(15) . . ?
N29 C117 C118 114.8(13) . . ?
C121 C122 C123 110(2) . . ?
N32 C169 C170 115.6(14) . . ?
C118 C119 C120 111.2(17) . . ?
C124 C123 C122 104(2) . . ?
C138 C139 C140 122(3) . . ?
C52 C51 C50 118.5(18) . . ?
C114 C115 C116 100(2) . . ?
C112 C111 C110 105.3(17) . . ?
C149 N31 C153 110.1(16) . . ?
C149 N31 C141 108.1(13) . . ?
C153 N31 C141 111.0(16) . . ?
C149 N31 C145 103.6(15) . . ?
C153 N31 C145 116.2(19) . . ?
C141 N31 C145 107.3(14) . . ?
N31 C141 C142 115.3(14) . . ?
C143 C142 C141 110.9(16) . . ?
N31 C153 C154 113.0(16) . . ?
N31 C149 C150 120.9(17) . . ?
C142 C143 C144 110.4(19) . . ?
C150 C151 C152 113.1(19) . . ?
C149 C150 C151 113(2) . . ?
C155 C154 C153 121(2) . . ?
C147 C146 C145 144(3) . . ?
C146 C145 N31 135(2) . . ?
C166 C167 C168 119(2) . . ?
C156 C155 C154 107(3) . . ?
C165 C166 C167 115.0(16) . . ?
C132 C131 C130 115(3) . . ?
C146 C147 C148 78(2) . . ?
O18B O20A S1 60.2(15) . . ?
O18B O20A O17B 93(2) . . ?
S1 O20A O17B 50.1(12) . . ?
C23 C24 C25 123(2) . . ?
C26 C25 C24 122(3) . . ?
C26 C25 I3 118(2) . . ?
C24 C25 I3 120(2) . . ?
S1 O17B O19A 61.7(14) . . ?
S1 O17B O20A 59.6(14) . . ?
O19A O17B O20A 99(2) . . ?
S1 O17B O18A 59.2(13) . . ?
O19A O17B O18A 99.2(19) . . ?
O20A O17B O18A 93.5(18) . . ?
O20A O18B S1 60.9(15) . . ?
O20A O18B O17A 97.1(19) . . ?
S1 O18B O17A 51.3(11) . . ?
S2 O14B O13A 64(2) . . ?
S2 O14B O15A 57.4(12) . . ?
O13A O14B O15A 99(2) . . ?
S2 O14B O16A 53.5(12) . . ?
O13A O14B O16A 95(2) . . ?
O15A O14B O16A 89.8(16) . . ?
O16A O15B S2 71.5(19) . . ?
S2 O14A O16B 54.0(11) . . ?
O20B O19A S1 62.1(11) . . ?
O20B O19A O17B 101.0(17) . . ?
S1 O19A O17B 52.2(13) . . ?
O19B O18A S1 59.2(9) . . ?
O19B O18A O17B 97.5(17) . . ?
S1 O18A O17B 49.7(13) . . ?
O15B O16A S2 66.6(19) . . ?
O15B O16A O14B 99(3) . . ?
S2 O16A O14B 48.6(14) . . ?
O18A O19B S1 62.5(10) . . ?
O18A O19B O17A 102.1(13) . . ?
S1 O19B O17A 54.4(8) . . ?
O13A O16B S2 66.3(14) . . ?
O13A O16B O14A 114(2) . . ?
S2 O16B O14A 60.9(16) . . ?
O19A O20B S1 61.5(14) . . ?
O19A O20B O17A 101.5(19) . . ?
S1 O20B O17A 53.1(9) . . ?
O15A O13B S2 68.7(11) . . ?

_refine_diff_density_max         1.074
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.070
# 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 -0.002 0.394 0.116 17 1 ' '
2 -0.195 -0.142 0.234 378 30 ' '
3 0.195 0.358 0.766 378 29 ' '
4 0.002 0.894 0.884 17 1 ' '
5 0.052 0.417 0.399 8 1 ' '
6 0.223 0.093 0.414 10 1 ' '
7 0.207 0.002 0.707 7 0 ' '
8 0.251 0.772 0.516 10 0 ' '
9 0.330 0.551 0.225 13 1 ' '
10 0.384 0.319 0.247 51 3 ' '
11 0.493 0.013 0.755 32 2 ' '
12 0.509 0.513 0.245 32 2 ' '
13 0.616 0.819 0.753 51 3 ' '
14 0.673 0.051 0.776 13 1 ' '
15 0.749 0.272 0.484 10 0 ' '
16 0.777 0.593 0.586 10 1 ' '
17 0.793 0.502 0.292 7 0 ' '
18 0.948 0.917 0.601 8 0 ' '
_platon_squeeze_details          
;
;

