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

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

data_T-Ph-NCO-Ligand
_database_code_depnum_ccdc_archive 'CCDC 1576489'
_audit_update_record             
;
2017-09-25 deposited with the CCDC.
2018-05-29 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 H33 N7 O3'
_chemical_formula_sum            'C27 H33 N7 O3'
_chemical_formula_weight         503.60

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'
P P 0.1023 0.0942 '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                   9.4626(10)
_cell_length_b                   12.2484(14)
_cell_length_c                   12.7852(13)
_cell_angle_alpha                84.367(9)
_cell_angle_beta                 71.200(9)
_cell_angle_gamma                74.329(10)
_cell_volume                     1350.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1323
_cell_measurement_theta_min      3.2450
_cell_measurement_theta_max      21.2030

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_F_000             536.0
_exptl_transmission_factor_min   0.976
_exptl_transmission_factor_max   0.983
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.084
_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            8182
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.251
_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             4757
_reflns_number_gt                2399
_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)+(0.0800P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4757
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.2272
_refine_ls_wR_factor_gt          0.1809
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001

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
O1 O 0.0703(3) 0.4523(2) 1.10478(18) 0.0614(7) Uani 1 1 d . . . . .
O2 O 0.2830(3) 0.5026(2) 0.54268(19) 0.0702(8) Uani 1 1 d . . . . .
N1 N 0.3799(3) 0.6709(2) 0.8224(2) 0.0535(8) Uani 1 1 d . . . . .
O3 O 0.5492(3) 0.3707(2) 0.8260(2) 0.0699(8) Uani 1 1 d . . . . .
N4 N 0.1896(4) 0.5870(3) 0.7084(2) 0.0646(9) Uani 1 1 d . . . . .
H4N H 0.1372 0.5829 0.7769 0.078 Uiso 1 1 calc R U . . .
N2 N 0.2645(3) 0.5116(3) 0.9760(2) 0.0593(9) Uani 1 1 d . . . . .
H2N H 0.3504 0.4907 0.9241 0.071 Uiso 1 1 calc R U . . .
C3 C 0.1908(4) 0.4319(3) 1.0257(3) 0.0522(10) Uani 1 1 d . . . . .
N6 N 0.6510(3) 0.4893(3) 0.6924(2) 0.0631(9) Uani 1 1 d . . . . .
H6N H 0.6863 0.5003 0.6224 0.076 Uiso 1 1 calc R U . . .
N5 N 0.1029(3) 0.4380(3) 0.6827(2) 0.0665(9) Uani 1 1 d . . . . .
H5N H 0.0493 0.4485 0.7511 0.080 Uiso 1 1 calc R U . . .
C12 C 0.1972(4) 0.5097(3) 0.6378(3) 0.0568(10) Uani 1 1 d . . . . .
N3 N 0.2605(4) 0.3272(3) 0.9822(3) 0.0676(10) Uani 1 1 d . . . . .
H3N H 0.3417 0.3216 0.9257 0.081 Uiso 1 1 calc R U . . .
N7 N 0.5908(4) 0.3387(3) 0.6448(3) 0.0687(10) Uani 1 1 d . . . . .
H7N H 0.6126 0.3681 0.5795 0.082 Uiso 1 1 calc R U . . .
C21 C 0.5955(4) 0.3984(3) 0.7276(3) 0.0559(10) Uani 1 1 d . . . . .
C5 C 0.1595(5) 0.1998(4) 1.1290(3) 0.0693(11) Uani 1 1 d . . . . .
H5 H 0.1485 0.2506 1.1824 0.083 Uiso 1 1 calc R U . . .
C13 C 0.0834(4) 0.3498(3) 0.6308(3) 0.0593(10) Uani 1 1 d . . . . .
C1 C 0.3309(4) 0.6898(3) 0.9408(3) 0.0605(10) Uani 1 1 d . . . . .
H1A H 0.2903 0.7705 0.9546 0.073 Uiso 1 1 calc R U . . .
H1B H 0.4195 0.6636 0.9675 0.073 Uiso 1 1 calc R U . . .
C19 C 0.5374(4) 0.6814(3) 0.7673(3) 0.0645(11) Uani 1 1 d . . . . .
H19A H 0.5582 0.7372 0.8052 0.077 Uiso 1 1 calc R U . . .
H19B H 0.5466 0.7080 0.6919 0.077 Uiso 1 1 calc R U . . .
C2 C 0.2090(4) 0.6291(3) 1.0038(3) 0.0614(11) Uani 1 1 d . . . . .
H2A H 0.1862 0.6375 1.0826 0.074 Uiso 1 1 calc R U . . .
H2B H 0.1148 0.6617 0.9848 0.074 Uiso 1 1 calc R U . . .
C4 C 0.2142(4) 0.2268(3) 1.0194(3) 0.0607(10) Uani 1 1 d . . . . .
C10 C 0.2701(5) 0.7380(3) 0.7684(3) 0.0640(11) Uani 1 1 d . . . . .
H10A H 0.2966 0.8092 0.7427 0.077 Uiso 1 1 calc R U . . .
H10B H 0.1677 0.7552 0.8217 0.077 Uiso 1 1 calc R U . . .
C20 C 0.6550(4) 0.5702(3) 0.7658(3) 0.0632(11) Uani 1 1 d . . . . .
H20A H 0.7571 0.5837 0.7428 0.076 Uiso 1 1 calc R U . . .
H20B H 0.6360 0.5384 0.8401 0.076 Uiso 1 1 calc R U . . .
C11 C 0.2680(5) 0.6773(3) 0.6716(3) 0.0653(11) Uani 1 1 d . . . . .
H11A H 0.2160 0.7313 0.6266 0.078 Uiso 1 1 calc R U . . .
H11B H 0.3731 0.6457 0.6261 0.078 Uiso 1 1 calc R U . . .
C22 C 0.5537(5) 0.2340(4) 0.6560(3) 0.0653(11) Uani 1 1 d . . . . .
C18 C 0.0993(5) 0.3519(4) 0.5202(3) 0.0803(13) Uani 1 1 d . . . . .
H18 H 0.1269 0.4127 0.4764 0.096 Uiso 1 1 calc R U . . .
C23 C 0.4716(5) 0.2141(4) 0.5907(4) 0.0771(13) Uani 1 1 d . . . . .
H23 H 0.4392 0.2706 0.5432 0.092 Uiso 1 1 calc R U . . .
C14 C 0.0382(5) 0.2617(4) 0.6936(4) 0.0822(14) Uani 1 1 d . . . . .
H14 H 0.0250 0.2595 0.7690 0.099 Uiso 1 1 calc R U . . .
C27 C 0.5990(5) 0.1490(4) 0.7267(4) 0.0871(14) Uani 1 1 d . . . . .
H27 H 0.6525 0.1619 0.7719 0.104 Uiso 1 1 calc R U . . .
C6 C 0.1205(5) 0.0981(4) 1.1613(4) 0.0869(14) Uani 1 1 d . . . . .
H6 H 0.0830 0.0811 1.2361 0.104 Uiso 1 1 calc R U . . .
C26 C 0.5658(7) 0.0450(4) 0.7310(5) 0.1112(19) Uani 1 1 d . . . . .
H26 H 0.5981 -0.0122 0.7779 0.133 Uiso 1 1 calc R U . . .
C7 C 0.1363(7) 0.0232(5) 1.0849(6) 0.1137(19) Uani 1 1 d . . . . .
H7 H 0.1099 -0.0452 1.1068 0.136 Uiso 1 1 calc R U . . .
C24 C 0.4381(6) 0.1106(5) 0.5962(5) 0.0992(16) Uani 1 1 d . . . . .
H24 H 0.3831 0.0980 0.5519 0.119 Uiso 1 1 calc R U . . .
C25 C 0.4836(8) 0.0272(5) 0.6645(6) 0.114(2) Uani 1 1 d . . . . .
H25 H 0.4599 -0.0421 0.6671 0.137 Uiso 1 1 calc R U . . .
C9 C 0.2283(6) 0.1503(4) 0.9423(4) 0.0905(15) Uani 1 1 d . . . . .
H9 H 0.2630 0.1678 0.8675 0.109 Uiso 1 1 calc R U . . .
C15 C 0.0119(7) 0.1761(5) 0.6469(5) 0.1078(19) Uani 1 1 d . . . . .
H15 H -0.0201 0.1171 0.6914 0.129 Uiso 1 1 calc R U . . .
C17 C 0.0745(6) 0.2645(5) 0.4731(4) 0.1057(18) Uani 1 1 d . . . . .
H17 H 0.0873 0.2663 0.3978 0.127 Uiso 1 1 calc R U . . .
C8 C 0.1919(7) 0.0488(5) 0.9746(5) 0.119(2) Uani 1 1 d . . . . .
H8 H 0.2047 -0.0029 0.9216 0.143 Uiso 1 1 calc R U . . .
C16 C 0.0317(7) 0.1759(5) 0.5366(5) 0.118(2) Uani 1 1 d . . . . .
H16 H 0.0162 0.1165 0.5053 0.141 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
O1 C3 1.240(4) . ?
O2 C12 1.221(4) . ?
N1 C1 1.455(4) . ?
N1 C10 1.457(5) . ?
N1 C19 1.464(4) . ?
O3 C21 1.238(4) . ?
N4 C12 1.344(4) . ?
N4 C11 1.454(4) . ?
N2 C3 1.343(4) . ?
N2 C2 1.430(4) . ?
C3 N3 1.355(4) . ?
N6 C21 1.336(4) . ?
N6 C20 1.446(4) . ?
N5 C12 1.375(4) . ?
N5 C13 1.404(4) . ?
N3 C4 1.405(4) . ?
N7 C21 1.362(4) . ?
N7 C22 1.401(5) . ?
C5 C4 1.370(5) . ?
C5 C6 1.381(5) . ?
C13 C14 1.360(5) . ?
C13 C18 1.371(5) . ?
C1 C2 1.510(4) . ?
C19 C20 1.505(5) . ?
C4 C9 1.376(5) . ?
C10 C11 1.513(5) . ?
C22 C27 1.380(6) . ?
C22 C23 1.386(6) . ?
C18 C17 1.384(6) . ?
C23 C24 1.377(6) . ?
C14 C15 1.370(6) . ?
C27 C26 1.384(6) . ?
C6 C7 1.351(7) . ?
C26 C25 1.390(8) . ?
C7 C8 1.375(7) . ?
C24 C25 1.350(8) . ?
C9 C8 1.369(6) . ?
C15 C16 1.361(7) . ?
C17 C16 1.362(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C10 113.3(3) . . ?
C1 N1 C19 112.5(3) . . ?
C10 N1 C19 112.7(3) . . ?
C12 N4 C11 121.4(3) . . ?
C3 N2 C2 124.1(3) . . ?
O1 C3 N2 122.9(4) . . ?
O1 C3 N3 123.1(3) . . ?
N2 C3 N3 114.0(3) . . ?
C21 N6 C20 123.5(3) . . ?
C12 N5 C13 128.0(3) . . ?
O2 C12 N4 122.6(3) . . ?
O2 C12 N5 123.2(3) . . ?
N4 C12 N5 114.2(3) . . ?
C3 N3 C4 126.9(3) . . ?
C21 N7 C22 126.2(3) . . ?
O3 C21 N6 124.0(4) . . ?
O3 C21 N7 122.2(4) . . ?
N6 C21 N7 113.8(3) . . ?
C4 C5 C6 120.8(4) . . ?
C14 C13 C18 118.4(4) . . ?
C14 C13 N5 118.8(4) . . ?
C18 C13 N5 122.6(4) . . ?
N1 C1 C2 112.1(3) . . ?
N1 C19 C20 111.9(3) . . ?
N2 C2 C1 109.0(3) . . ?
C5 C4 C9 118.3(4) . . ?
C5 C4 N3 123.0(4) . . ?
C9 C4 N3 118.6(4) . . ?
N1 C10 C11 112.4(3) . . ?
N6 C20 C19 112.5(3) . . ?
N4 C11 C10 111.4(3) . . ?
C27 C22 C23 118.8(4) . . ?
C27 C22 N7 123.0(4) . . ?
C23 C22 N7 118.2(4) . . ?
C13 C18 C17 120.7(4) . . ?
C24 C23 C22 120.0(5) . . ?
C13 C14 C15 120.7(4) . . ?
C22 C27 C26 120.8(5) . . ?
C7 C6 C5 120.4(5) . . ?
C27 C26 C25 119.2(6) . . ?
C6 C7 C8 119.5(5) . . ?
C25 C24 C23 121.2(6) . . ?
C24 C25 C26 120.0(6) . . ?
C8 C9 C4 120.8(5) . . ?
C16 C15 C14 121.3(5) . . ?
C16 C17 C18 120.3(5) . . ?
C9 C8 C7 120.3(5) . . ?
C15 C16 C17 118.6(5) . . ?

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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-Ph-NCO-TBAH2PO4
_database_code_depnum_ccdc_archive 'CCDC 1576491'
_audit_update_record             
;
2017-09-25 deposited with the CCDC.
2018-05-29 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 H33 N7 O3, C16 H36 N, H2 O4 P'
_chemical_formula_sum            'C43 H71 N8 O7 P'
_chemical_formula_weight         843.05


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'
P P 0.1023 0.0942 '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                   15.4695(14)
_cell_length_b                   25.496(2)
_cell_length_c                   12.3469(17)
_cell_angle_alpha                90
_cell_angle_beta                 94.928(10)
_cell_angle_gamma                90
_cell_volume                     4851.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2108
_cell_measurement_theta_min      3.3870
_cell_measurement_theta_max      19.9150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_F_000             1824.0
_exptl_transmission_factor_min   0.968
_exptl_transmission_factor_max   0.977
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.110
_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            20006
_diffrn_reflns_av_unetI/netI     0.1483
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.089
_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             8535
_reflns_number_gt                3362
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0500P)²+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         8535
_refine_ls_number_parameters     538
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2010
_refine_ls_R_factor_gt           0.0862
_refine_ls_wR_factor_ref         0.2330
_refine_ls_wR_factor_gt          0.1711
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.010
_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
P1 P 0.61496(8) 0.50027(6) 0.93197(12) 0.0524(4) Uani 1 1 d . . . . .
O5 O 0.61543(19) 0.50887(16) 1.0582(3) 0.0599(10) Uani 1 1 d . . . . .
H5O H 0.5681 0.5006 1.0782 0.090 Uiso 1 1 calc R U . . .
O4 O 0.69456(19) 0.52686(13) 0.8976(3) 0.0600(10) Uani 1 1 d . . . . .
O6 O 0.6214(2) 0.43976(13) 0.9141(3) 0.0643(11) Uani 1 1 d . . . . .
O7 O 0.5300(2) 0.51702(14) 0.8733(3) 0.0676(11) Uani 1 1 d . . . . .
H7O H 0.5262 0.5491 0.8748 0.101 Uiso 1 1 calc R U . . .
O2 O 0.0884(2) 0.40336(14) -0.1616(3) 0.0671(11) Uani 1 1 d . . . . .
N1 N 0.1355(3) 0.41998(17) 0.2055(4) 0.0549(12) Uani 1 1 d . . . . .
O3 O 0.3967(3) 0.34659(17) 0.3981(4) 0.0812(13) Uani 1 1 d . . . . .
N8 N 0.5750(3) 0.63714(15) 0.2756(4) 0.0526(11) Uani 1 1 d . . . . .
O1 O 0.2209(2) 0.59486(15) 0.0559(4) 0.0856(14) Uani 1 1 d . . . . .
N5 N 0.1934(3) 0.46648(18) -0.1486(4) 0.0641(13) Uani 1 1 d . . . . .
H5N H 0.2389 0.4771 -0.1099 0.077 Uiso 1 1 calc R U . . .
N7 N 0.4618(3) 0.39028(18) 0.2648(4) 0.0656(13) Uani 1 1 d . . . . .
H7N H 0.4568 0.4178 0.2244 0.079 Uiso 1 1 calc R U . . .
N3 N 0.0843(3) 0.61307(19) 0.0969(4) 0.0679(14) Uani 1 1 d . . . . .
H3N H 0.0365 0.6000 0.1156 0.081 Uiso 1 1 calc R U . . .
N2 N 0.1453(3) 0.53111(18) 0.1321(4) 0.0658(13) Uani 1 1 d . . . . .
H2N H 0.1913 0.5120 0.1366 0.079 Uiso 1 1 calc R U . . .
N4 N 0.1892(3) 0.40444(18) -0.0154(4) 0.0662(13) Uani 1 1 d . . . . .
H4N H 0.2390 0.4161 0.0103 0.079 Uiso 1 1 calc R U . . .
N6 N 0.3239(3) 0.4112(2) 0.2996(4) 0.0785(15) Uani 1 1 d . . . . .
H6N H 0.3243 0.4326 0.2458 0.094 Uiso 1 1 calc R U . . .
C12 C 0.1529(3) 0.4235(2) -0.1100(5) 0.0560(14) Uani 1 1 d . . . . .
C28 C 0.4991(3) 0.6580(2) 0.3339(4) 0.0587(15) Uani 1 1 d . . . . .
H28A H 0.5092 0.6489 0.4102 0.070 Uiso 1 1 calc R U . . .
H28B H 0.4997 0.6960 0.3292 0.070 Uiso 1 1 calc R U . . .
C36 C 0.6550(3) 0.66378(19) 0.3311(5) 0.0609(15) Uani 1 1 d . . . . .
H36A H 0.6578 0.6559 0.4082 0.073 Uiso 1 1 calc R U . . .
H36B H 0.6480 0.7014 0.3231 0.073 Uiso 1 1 calc R U . . .
C32 C 0.5639(4) 0.6491(2) 0.1551(4) 0.0620(15) Uani 1 1 d . . . . .
H32A H 0.5109 0.6325 0.1243 0.074 Uiso 1 1 calc R U . . .
H32B H 0.6118 0.6333 0.1209 0.074 Uiso 1 1 calc R U . . .
C40 C 0.5824(3) 0.57810(18) 0.2823(5) 0.0600(15) Uani 1 1 d . . . . .
H40A H 0.6280 0.5671 0.2381 0.072 Uiso 1 1 calc R U . . .
H40B H 0.5285 0.5631 0.2502 0.072 Uiso 1 1 calc R U . . .
C3 C 0.1532(4) 0.5797(2) 0.0937(5) 0.0666(17) Uani 1 1 d . . . . .
C19 C 0.1698(3) 0.3860(2) 0.2941(5) 0.0746(18) Uani 1 1 d . . . . .
H19A H 0.1857 0.3526 0.2640 0.090 Uiso 1 1 calc R U . . .
H19B H 0.1243 0.3795 0.3418 0.090 Uiso 1 1 calc R U . . .
C13 C 0.1700(3) 0.4956(2) -0.2437(5) 0.0601(15) Uani 1 1 d . . . . .
C33 C 0.5602(5) 0.7068(2) 0.1266(5) 0.090(2) Uani 1 1 d . . . . .
H33A H 0.6126 0.7239 0.1577 0.107 Uiso 1 1 calc R U . . .
H33B H 0.5112 0.7228 0.1581 0.107 Uiso 1 1 calc R U . . .
C20 C 0.2483(4) 0.4084(3) 0.3612(5) 0.086(2) Uani 1 1 d . . . . .
H20A H 0.2345 0.4433 0.3860 0.103 Uiso 1 1 calc R U . . .
H20B H 0.2616 0.3866 0.4249 0.103 Uiso 1 1 calc R U . . .
C11 C 0.1463(4) 0.3647(2) 0.0438(5) 0.0719(17) Uani 1 1 d . . . . .
H11A H 0.1895 0.3432 0.0843 0.086 Uiso 1 1 calc R U . . .
H11B H 0.1127 0.3422 -0.0073 0.086 Uiso 1 1 calc R U . . .
C10 C 0.0864(3) 0.3888(2) 0.1220(5) 0.0652(16) Uani 1 1 d . . . . .
H10A H 0.0440 0.4110 0.0818 0.078 Uiso 1 1 calc R U . . .
H10B H 0.0555 0.3611 0.1563 0.078 Uiso 1 1 calc R U . . .
C21 C 0.3934(4) 0.3805(3) 0.3260(5) 0.0678(16) Uani 1 1 d . . . . .
C27 C 0.5666(4) 0.3238(2) 0.3359(6) 0.0764(18) Uani 1 1 d . . . . .
H27 H 0.5341 0.3170 0.3943 0.092 Uiso 1 1 calc R U . . .
C22 C 0.5389(4) 0.3613(2) 0.2594(5) 0.0626(16) Uani 1 1 d . . . . .
C18 C 0.1258(3) 0.4735(3) -0.3350(5) 0.0699(17) Uani 1 1 d . . . . .
H18 H 0.1086 0.4385 -0.3347 0.084 Uiso 1 1 calc R U . . .
C29 C 0.4097(3) 0.6394(2) 0.2940(5) 0.0756(18) Uani 1 1 d . . . . .
H29A H 0.4074 0.6015 0.2976 0.091 Uiso 1 1 calc R U . . .
H29B H 0.3968 0.6498 0.2188 0.091 Uiso 1 1 calc R U . . .
C4 C 0.0850(4) 0.6664(3) 0.0723(6) 0.0708(18) Uani 1 1 d . . . . .
C1 C 0.0850(4) 0.4627(2) 0.2443(5) 0.0712(17) Uani 1 1 d . . . . .
H1A H 0.1154 0.4765 0.3102 0.085 Uiso 1 1 calc R U . . .
H1B H 0.0300 0.4487 0.2636 0.085 Uiso 1 1 calc R U . . .
C41 C 0.6011(4) 0.5549(2) 0.3945(5) 0.0748(18) Uani 1 1 d . . . . .
H41A H 0.6572 0.5670 0.4261 0.090 Uiso 1 1 calc R U . . .
H41B H 0.5574 0.5662 0.4412 0.090 Uiso 1 1 calc R U . . .
C17 C 0.1077(4) 0.5037(3) -0.4254(6) 0.085(2) Uani 1 1 d . . . . .
H17 H 0.0788 0.4887 -0.4869 0.103 Uiso 1 1 calc R U . . .
C30 C 0.3429(4) 0.6626(2) 0.3627(6) 0.0790(19) Uani 1 1 d . . . . .
H30A H 0.3571 0.6526 0.4379 0.095 Uiso 1 1 calc R U . . .
H30B H 0.3458 0.7006 0.3586 0.095 Uiso 1 1 calc R U . . .
C37 C 0.7414(4) 0.6481(2) 0.2885(6) 0.084(2) Uani 1 1 d . . . . .
H37A H 0.7390 0.6544 0.2108 0.101 Uiso 1 1 calc R U . . .
H37B H 0.7518 0.6110 0.3011 0.101 Uiso 1 1 calc R U . . .
C9 C 0.0456(4) 0.7005(3) 0.1378(6) 0.092(2) Uani 1 1 d . . . . .
H9 H 0.0205 0.6876 0.1983 0.110 Uiso 1 1 calc R U . . .
C34 C 0.5512(5) 0.7154(3) 0.0042(5) 0.097(2) Uani 1 1 d . . . . .
H34A H 0.4982 0.6984 -0.0253 0.117 Uiso 1 1 calc R U . . .
H34B H 0.5445 0.7527 -0.0094 0.117 Uiso 1 1 calc R U . . .
C23 C 0.5887(4) 0.3711(2) 0.1731(6) 0.0796(19) Uani 1 1 d . . . . .
H23 H 0.5709 0.3963 0.1216 0.096 Uiso 1 1 calc R U . . .
C14 C 0.1927(4) 0.5473(3) -0.2462(6) 0.096(2) Uani 1 1 d . . . . .
H14 H 0.2206 0.5626 -0.1844 0.115 Uiso 1 1 calc R U . . .
C16 C 0.1308(5) 0.5551(4) -0.4281(7) 0.115(3) Uani 1 1 d . . . . .
H16 H 0.1167 0.5751 -0.4901 0.138 Uiso 1 1 calc R U . . .
C26 C 0.6425(5) 0.2968(3) 0.3251(7) 0.092(2) Uani 1 1 d . . . . .
H26 H 0.6614 0.2720 0.3771 0.111 Uiso 1 1 calc R U . . .
C2 C 0.0667(4) 0.5069(2) 0.1672(6) 0.082(2) Uani 1 1 d . . . . .
H2C H 0.0315 0.4942 0.1038 0.098 Uiso 1 1 calc R U . . .
H2D H 0.0333 0.5334 0.2016 0.098 Uiso 1 1 calc R U . . .
C24 C 0.6639(4) 0.3438(3) 0.1638(7) 0.095(2) Uani 1 1 d . . . . .
H24 H 0.6967 0.3513 0.1061 0.114 Uiso 1 1 calc R U . . .
C42 C 0.6011(4) 0.4957(2) 0.3869(6) 0.093(2) Uani 1 1 d . . . . .
H42A H 0.5433 0.4840 0.3610 0.111 Uiso 1 1 calc R U . . .
H42B H 0.6403 0.4851 0.3337 0.111 Uiso 1 1 calc R U . . .
C25 C 0.6920(5) 0.3062(3) 0.2357(8) 0.096(2) Uani 1 1 d . . . . .
H25 H 0.7422 0.2872 0.2268 0.115 Uiso 1 1 calc R U . . .
C5 C 0.1198(4) 0.6857(3) -0.0182(8) 0.112(3) Uani 1 1 d . . . . .
H5 H 0.1463 0.6633 -0.0647 0.134 Uiso 1 1 calc R U . . .
C43 C 0.6277(5) 0.4690(3) 0.4927(7) 0.131(3) Uani 1 1 d . . . . .
H43A H 0.6873 0.4769 0.5145 0.196 Uiso 1 1 calc R U . . .
H43B H 0.6208 0.4318 0.4841 0.196 Uiso 1 1 calc R U . . .
H43C H 0.5919 0.4812 0.5473 0.196 Uiso 1 1 calc R U . . .
C31 C 0.2511(4) 0.6451(3) 0.3277(7) 0.121(3) Uani 1 1 d . . . . .
H31A H 0.2356 0.6564 0.2544 0.182 Uiso 1 1 calc R U . . .
H31B H 0.2119 0.6603 0.3750 0.182 Uiso 1 1 calc R U . . .
H31C H 0.2478 0.6076 0.3314 0.182 Uiso 1 1 calc R U . . .
C15 C 0.1752(5) 0.5773(3) -0.3381(8) 0.121(3) Uani 1 1 d . . . . .
H15 H 0.1931 0.6121 -0.3395 0.146 Uiso 1 1 calc R U . . .
C38 C 0.8171(5) 0.6808(3) 0.3478(9) 0.150(4) Uani 1 1 d . U . . .
H38A H 0.8072 0.6836 0.4241 0.180 Uiso 1 1 calc R U . . .
H38B H 0.8710 0.6618 0.3431 0.180 Uiso 1 1 calc R U . . .
C8 C 0.0422(6) 0.7531(3) 0.1167(9) 0.129(3) Uani 1 1 d . . . . .
H8 H 0.0148 0.7752 0.1629 0.155 Uiso 1 1 calc R U . . .
C7 C 0.0774(7) 0.7735(4) 0.0310(12) 0.159(5) Uani 1 1 d . . . . .
H7 H 0.0768 0.8095 0.0189 0.190 Uiso 1 1 calc R U . . .
C6 C 0.1147(6) 0.7397(4) -0.0396(10) 0.150(4) Uani 1 1 d . . . . .
H6 H 0.1367 0.7529 -0.1018 0.180 Uiso 1 1 calc R U . . .
C35 C 0.6232(5) 0.6961(3) -0.0562(6) 0.123(3) Uani 1 1 d . . . . .
H35A H 0.6770 0.7103 -0.0243 0.184 Uiso 1 1 calc R U . . .
H35B H 0.6142 0.7071 -0.1307 0.184 Uiso 1 1 calc R U . . .
H35C H 0.6253 0.6585 -0.0529 0.184 Uiso 1 1 calc R U . . .
C39 C 0.8262(7) 0.7278(4) 0.3095(13) 0.256(8) Uani 1 1 d . U . . .
H39A H 0.8348 0.7258 0.2335 0.384 Uiso 1 1 calc R U . . .
H39B H 0.8755 0.7444 0.3477 0.384 Uiso 1 1 calc R U . . .
H39C H 0.7750 0.7480 0.3190 0.384 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
P1 O4 1.498(3) . ?
P1 O7 1.506(3) . ?
P1 O6 1.563(3) . ?
P1 O5 1.574(3) . ?
O2 C12 1.248(6) . ?
N1 C1 1.447(6) . ?
N1 C19 1.458(6) . ?
N1 C10 1.462(6) . ?
O3 C21 1.238(7) . ?
N8 C32 1.514(6) . ?
N8 C40 1.511(6) . ?
N8 C36 1.522(6) . ?
N8 C28 1.525(6) . ?
O1 C3 1.244(6) . ?
N5 C12 1.367(6) . ?
N5 C13 1.409(7) . ?
N7 C21 1.374(7) . ?
N7 C22 1.409(7) . ?
N3 C3 1.367(6) . ?
N3 C4 1.393(7) . ?
N2 C3 1.337(7) . ?
N2 C2 1.462(6) . ?
N4 C12 1.343(7) . ?
N4 C11 1.444(6) . ?
N6 C21 1.349(7) . ?
N6 C20 1.451(7) . ?
C28 C29 1.504(7) . ?
C36 C37 1.532(7) . ?
C32 C33 1.513(7) . ?
C40 C41 1.512(7) . ?
C19 C20 1.522(7) . ?
C13 C14 1.367(7) . ?
C13 C18 1.387(7) . ?
C33 C34 1.521(8) . ?
C11 C10 1.524(7) . ?
C27 C26 1.378(8) . ?
C27 C22 1.385(8) . ?
C22 C23 1.390(8) . ?
C18 C17 1.364(8) . ?
C29 C30 1.512(7) . ?
C4 C5 1.372(9) . ?
C4 C9 1.367(8) . ?
C1 C2 1.487(7) . ?
C41 C42 1.511(7) . ?
C17 C16 1.359(9) . ?
C30 C31 1.515(8) . ?
C37 C38 1.568(9) . ?
C9 C8 1.367(9) . ?
C34 C35 1.477(8) . ?
C23 C24 1.369(8) . ?
C14 C15 1.376(9) . ?
C16 C15 1.376(10) . ?
C26 C25 1.417(9) . ?
C24 C25 1.352(9) . ?
C42 C43 1.500(9) . ?
C5 C6 1.402(9) . ?
C38 C39 1.300(12) . ?
C8 C7 1.336(12) . ?
C7 C6 1.386(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
O4 P1 O7 116.1(2) . . ?
O4 P1 O6 110.06(19) . . ?
O7 P1 O6 106.0(2) . . ?
O4 P1 O5 106.46(19) . . ?
O7 P1 O5 111.5(2) . . ?
O6 P1 O5 106.4(2) . . ?
C1 N1 C19 111.8(5) . . ?
C1 N1 C10 112.4(4) . . ?
C19 N1 C10 109.9(4) . . ?
C32 N8 C40 104.9(4) . . ?
C32 N8 C36 111.8(4) . . ?
C40 N8 C36 111.4(4) . . ?
C32 N8 C28 111.5(4) . . ?
C40 N8 C28 112.3(4) . . ?
C36 N8 C28 105.1(4) . . ?
C12 N5 C13 128.3(5) . . ?
C21 N7 C22 128.7(5) . . ?
C3 N3 C4 125.5(5) . . ?
C3 N2 C2 126.9(5) . . ?
C12 N4 C11 121.2(5) . . ?
C21 N6 C20 120.4(5) . . ?
O2 C12 N4 123.5(5) . . ?
O2 C12 N5 121.5(6) . . ?
N4 C12 N5 115.0(5) . . ?
C29 C28 N8 117.3(4) . . ?
N8 C36 C37 115.3(4) . . ?
N8 C32 C33 115.0(4) . . ?
N8 C40 C41 116.6(5) . . ?
O1 C3 N2 121.8(5) . . ?
O1 C3 N3 120.1(6) . . ?
N2 C3 N3 118.1(5) . . ?
N1 C19 C20 114.0(5) . . ?
C14 C13 C18 118.8(6) . . ?
C14 C13 N5 118.6(6) . . ?
C18 C13 N5 122.5(6) . . ?
C32 C33 C34 111.6(5) . . ?
N6 C20 C19 112.0(5) . . ?
N4 C11 C10 111.6(5) . . ?
N1 C10 C11 111.1(4) . . ?
O3 C21 N6 124.3(6) . . ?
O3 C21 N7 122.4(6) . . ?
N6 C21 N7 113.4(6) . . ?
C26 C27 C22 119.7(7) . . ?
C27 C22 C23 119.1(6) . . ?
C27 C22 N7 122.9(6) . . ?
C23 C22 N7 118.0(6) . . ?
C17 C18 C13 119.2(6) . . ?
C28 C29 C30 110.3(5) . . ?
C5 C4 C9 118.6(7) . . ?
C5 C4 N3 122.6(7) . . ?
C9 C4 N3 118.7(7) . . ?
N1 C1 C2 115.9(5) . . ?
C42 C41 C40 109.5(5) . . ?
C16 C17 C18 121.9(7) . . ?
C31 C30 C29 113.2(5) . . ?
C36 C37 C38 109.8(5) . . ?
C8 C9 C4 121.6(8) . . ?
C35 C34 C33 116.5(6) . . ?
C24 C23 C22 120.3(7) . . ?
C13 C14 C15 121.5(7) . . ?
C17 C16 C15 119.3(7) . . ?
C27 C26 C25 120.8(7) . . ?
N2 C2 C1 113.1(5) . . ?
C25 C24 C23 122.2(7) . . ?
C43 C42 C41 113.6(6) . . ?
C24 C25 C26 117.8(7) . . ?
C4 C5 C6 119.1(9) . . ?
C14 C15 C16 119.1(7) . . ?
C39 C38 C37 114.9(11) . . ?
C7 C8 C9 121.4(10) . . ?
C8 C7 C6 118.5(9) . . ?
C7 C6 C5 120.8(10) . . ?

_refine_diff_density_max         0.396
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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-Ph-ncs-TBAOCOCH3
_database_code_depnum_ccdc_archive 'CCDC 1589920'
_audit_update_record             
;
2017-12-08 deposited with the CCDC.
2018-05-29 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 H33 N7 S3, C16 H36 N, C2 H3 O2'
_chemical_formula_sum            'C45 H72 N8 O2 S3'
_chemical_formula_weight         853.29

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'

_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                   12.4753(15)
_cell_length_b                   12.4982(9)
_cell_length_c                   16.6285(16)
_cell_angle_alpha                102.863(7)
_cell_angle_beta                 96.291(9)
_cell_angle_gamma                97.109(8)
_cell_volume                     2482.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3460
_cell_measurement_theta_min      3.3620
_cell_measurement_theta_max      21.8840

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_F_000             924.0
_exptl_transmission_factor_min   0.949
_exptl_transmission_factor_max   0.966
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    0.192
_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            16084
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.118
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             8626
_reflns_number_gt                4090
_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)+(0.0482P)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         8626
_refine_ls_number_parameters     528
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.0815
_refine_ls_wR_factor_ref         0.2219
_refine_ls_wR_factor_gt          0.1752
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_restrained_S_all      0.966
_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
S1 S 0.33891(13) -0.02445(11) 0.13069(9) 0.0857(5) Uani 1 1 d . . . . .
S3 S 0.84050(13) 0.45429(12) 0.07012(10) 0.0878(5) Uani 1 1 d . . . . .
S2 S 0.85441(15) 0.16967(13) 0.46007(10) 0.0994(6) Uani 1 1 d . . . . .
N1 N 0.7209(3) 0.1262(3) 0.1776(2) 0.0590(10) Uani 1 1 d . . . . .
O2 O 0.5066(3) 0.3487(3) 0.3767(2) 0.0834(10) Uani 1 1 d . . . . .
O1 O 0.5756(3) 0.3738(3) 0.2653(3) 0.0936(12) Uani 1 1 d . . . . .
N3 N 0.3729(3) 0.1444(3) 0.2657(3) 0.0708(11) Uani 1 1 d . . . . .
H3N H 0.4143 0.2039 0.2942 0.085 Uiso 1 1 calc R U . . .
N8 N 0.1364(3) 0.6857(3) 0.2317(2) 0.0647(10) Uani 1 1 d . . . . .
N2 N 0.4879(3) 0.1574(3) 0.1712(2) 0.0670(11) Uani 1 1 d . . . . .
H2N H 0.5128 0.2216 0.2036 0.080 Uiso 1 1 calc R U . . .
N5 N 0.7178(4) 0.3205(3) 0.4577(3) 0.0757(12) Uani 1 1 d . . . . .
H5N H 0.6505 0.3250 0.4431 0.091 Uiso 1 1 calc R U . . .
N6 N 0.7825(3) 0.3675(3) 0.1940(3) 0.0785(12) Uani 1 1 d . . . . .
H6N H 0.7466 0.3724 0.2356 0.094 Uiso 1 1 calc R U . . .
N7 N 0.6716(4) 0.4812(3) 0.1557(3) 0.0778(12) Uani 1 1 d . . . . .
H7N H 0.6336 0.4555 0.1893 0.093 Uiso 1 1 calc R U . . .
N4 N 0.6791(4) 0.1655(3) 0.3549(3) 0.0792(12) Uani 1 1 d . . . . .
H4N H 0.6237 0.1952 0.3407 0.095 Uiso 1 1 calc R U . . .
C1 C 0.6311(4) 0.0558(4) 0.1177(3) 0.0652(13) Uani 1 1 d . . . . .
H1A H 0.6020 -0.0053 0.1400 0.078 Uiso 1 1 calc R U . . .
H1B H 0.6583 0.0249 0.0664 0.078 Uiso 1 1 calc R U . . .
C2 C 0.5407(4) 0.1214(4) 0.0990(3) 0.0712(14) Uani 1 1 d . . . . .
H2A H 0.5711 0.1857 0.0808 0.085 Uiso 1 1 calc R U . . .
H2B H 0.4871 0.0755 0.0540 0.085 Uiso 1 1 calc R U . . .
C3 C 0.4023(4) 0.0974(4) 0.1907(3) 0.0660(13) Uani 1 1 d . . . . .
C21 C 0.7479(4) 0.2213(4) 0.4225(3) 0.0692(13) Uani 1 1 d . . . . .
C10 C 0.8039(4) 0.1753(4) 0.1367(3) 0.0744(14) Uani 1 1 d . . . . .
H10A H 0.7709 0.1807 0.0825 0.089 Uiso 1 1 calc R U . . .
H10B H 0.8588 0.1269 0.1281 0.089 Uiso 1 1 calc R U . . .
C44 C 0.5341(4) 0.4080(4) 0.3296(4) 0.0721(14) Uani 1 1 d . . . . .
C22 C 0.7760(5) 0.4165(4) 0.5134(3) 0.0705(14) Uani 1 1 d . . . . .
C12 C 0.7629(4) 0.4339(4) 0.1419(3) 0.0678(13) Uani 1 1 d . . . . .
C19 C 0.7651(4) 0.0693(4) 0.2389(3) 0.0732(14) Uani 1 1 d . . . . .
H19A H 0.8355 0.1103 0.2667 0.088 Uiso 1 1 calc R U . . .
H19B H 0.7764 -0.0041 0.2103 0.088 Uiso 1 1 calc R U . . .
C13 C 0.6292(5) 0.5658(4) 0.1237(3) 0.0677(13) Uani 1 1 d . . . . .
C4 C 0.2829(4) 0.1073(4) 0.3021(4) 0.0706(14) Uani 1 1 d . . . . .
C23 C 0.8857(5) 0.4349(5) 0.5412(3) 0.0799(15) Uani 1 1 d . . . . .
H23 H 0.9269 0.3783 0.5263 0.096 Uiso 1 1 calc R U . . .
C20 C 0.6907(5) 0.0584(4) 0.3036(3) 0.0845(17) Uani 1 1 d . . . . .
H20A H 0.6193 0.0202 0.2758 0.101 Uiso 1 1 calc R U . . .
H20B H 0.7198 0.0137 0.3390 0.101 Uiso 1 1 calc R U . . .
C11 C 0.8586(4) 0.2893(4) 0.1858(4) 0.0869(17) Uani 1 1 d . . . . .
H11A H 0.8899 0.2848 0.2407 0.104 Uiso 1 1 calc R U . . .
H11B H 0.9175 0.3152 0.1580 0.104 Uiso 1 1 calc R U . . .
C28 C 0.1490(5) 0.5641(5) 0.2328(4) 0.0940(18) Uani 1 1 d . . . . .
H28A H 0.1745 0.5630 0.2898 0.113 Uiso 1 1 calc R U . . .
H28B H 0.0768 0.5203 0.2181 0.113 Uiso 1 1 calc R U . . .
C32 C 0.0715(6) 0.7291(5) 0.2988(4) 0.102(2) Uani 1 1 d . . . . .
H32A H 0.1085 0.7210 0.3511 0.122 Uiso 1 1 calc R U . . .
H32B H 0.0737 0.8080 0.3032 0.122 Uiso 1 1 calc R U . . .
C25 C 0.8756(8) 0.6210(6) 0.6137(4) 0.113(2) Uani 1 1 d . . . . .
H25 H 0.9091 0.6897 0.6469 0.135 Uiso 1 1 calc R U . . .
C5 C 0.3023(6) 0.0936(5) 0.3821(4) 0.0942(18) Uani 1 1 d . . . . .
H5 H 0.3734 0.1039 0.4092 0.113 Uiso 1 1 calc R U . . .
C24 C 0.9361(6) 0.5369(5) 0.5913(4) 0.0963(19) Uani 1 1 d . . . . .
H24 H 1.0107 0.5483 0.6098 0.116 Uiso 1 1 calc R U . . .
C29 C 0.2197(6) 0.5078(4) 0.1804(4) 0.0954(18) Uani 1 1 d . . . . .
H29A H 0.2946 0.5402 0.2031 0.114 Uiso 1 1 calc R U . . .
H29B H 0.2054 0.5223 0.1256 0.114 Uiso 1 1 calc R U . . .
C14 C 0.6933(5) 0.6569(4) 0.1126(4) 0.100(2) Uani 1 1 d . . . . .
H14 H 0.7689 0.6630 0.1220 0.119 Uiso 1 1 calc R U . . .
C27 C 0.7166(6) 0.5019(5) 0.5381(4) 0.0962(19) Uani 1 1 d . . . . .
H27 H 0.6416 0.4911 0.5217 0.115 Uiso 1 1 calc R U . . .
C33 C -0.0425(5) 0.6799(7) 0.2913(4) 0.116(2) Uani 1 1 d . . . . .
H33A H -0.0460 0.6036 0.2959 0.139 Uiso 1 1 calc R U . . .
H33B H -0.0792 0.6791 0.2366 0.139 Uiso 1 1 calc R U . . .
C18 C 0.5191(6) 0.5585(5) 0.1087(4) 0.0954(18) Uani 1 1 d . . . . .
H18 H 0.4749 0.4964 0.1154 0.114 Uiso 1 1 calc R U . . .
C9 C 0.1783(5) 0.0905(4) 0.2624(4) 0.0943(18) Uani 1 1 d . . . . .
H9 H 0.1647 0.0992 0.2083 0.113 Uiso 1 1 calc R U . . .
C37 C 0.0493(6) 0.7903(5) 0.1348(4) 0.101(2) Uani 1 1 d . . . . .
H37A H -0.0037 0.8094 0.1721 0.122 Uiso 1 1 calc R U . . .
H37B H 0.1115 0.8491 0.1509 0.122 Uiso 1 1 calc R U . . .
C40 C 0.2489(5) 0.7546(5) 0.2511(4) 0.100(2) Uani 1 1 d . . . . .
H40A H 0.2888 0.7257 0.2062 0.121 Uiso 1 1 calc R U . . .
H40B H 0.2391 0.8292 0.2472 0.121 Uiso 1 1 calc R U . . .
C45 C 0.5186(6) 0.5289(4) 0.3502(4) 0.113(2) Uani 1 1 d . . . . .
H45A H 0.4536 0.5377 0.3173 0.169 Uiso 1 1 calc R U . . .
H45B H 0.5804 0.5735 0.3382 0.169 Uiso 1 1 calc R U . . .
H45C H 0.5120 0.5521 0.4083 0.169 Uiso 1 1 calc R U . . .
C16 C 0.5371(7) 0.7333(6) 0.0742(4) 0.103(2) Uani 1 1 d . . . . .
H16 H 0.5060 0.7908 0.0586 0.124 Uiso 1 1 calc R U . . .
C17 C 0.4715(6) 0.6432(6) 0.0835(4) 0.110(2) Uani 1 1 d . . . . .
H17 H 0.3960 0.6378 0.0731 0.131 Uiso 1 1 calc R U . . .
C36 C 0.0854(5) 0.6858(5) 0.1465(4) 0.103(2) Uani 1 1 d . . . . .
H36A H 0.1373 0.6665 0.1083 0.123 Uiso 1 1 calc R U . . .
H36B H 0.0226 0.6275 0.1304 0.123 Uiso 1 1 calc R U . . .
C26 C 0.7691(8) 0.6032(6) 0.5873(4) 0.116(2) Uani 1 1 d . . . . .
H26 H 0.7286 0.6604 0.6022 0.139 Uiso 1 1 calc R U . . .
C8 C 0.0905(6) 0.0598(5) 0.3039(7) 0.129(3) Uani 1 1 d . . . . .
H8 H 0.0191 0.0473 0.2772 0.155 Uiso 1 1 calc R U . . .
C41 C 0.3195(5) 0.7657(5) 0.3273(4) 0.104(2) Uani 1 1 d . . . . .
H41A H 0.3246 0.6915 0.3346 0.125 Uiso 1 1 calc R U . . .
H41B H 0.2840 0.8025 0.3725 0.125 Uiso 1 1 calc R U . . .
C7 C 0.1119(9) 0.0489(7) 0.3833(8) 0.142(4) Uani 1 1 d . . . . .
H7 H 0.0542 0.0303 0.4112 0.171 Uiso 1 1 calc R U . . .
C42 C 0.4300(6) 0.8246(6) 0.3377(5) 0.131(3) Uani 1 1 d . . . . .
H42A H 0.4665 0.7828 0.2954 0.158 Uiso 1 1 calc R U . . .
H42B H 0.4239 0.8951 0.3236 0.158 Uiso 1 1 calc R U . . .
C15 C 0.6446(7) 0.7408(5) 0.0872(5) 0.119(2) Uani 1 1 d . . . . .
H15 H 0.6881 0.8026 0.0792 0.143 Uiso 1 1 calc R U . . .
C31 C 0.2789(6) 0.3238(6) 0.1266(5) 0.138(3) Uani 1 1 d . . . . .
H31A H 0.2771 0.3378 0.0721 0.207 Uiso 1 1 calc R U . . .
H31B H 0.2558 0.2461 0.1216 0.207 Uiso 1 1 calc R U . . .
H31C H 0.3519 0.3450 0.1558 0.207 Uiso 1 1 calc R U . . .
C34 C -0.0993(6) 0.7394(8) 0.3542(5) 0.157(3) Uani 1 1 d D . . . .
H34A H -0.0550 0.7476 0.4075 0.189 Uiso 1 1 calc R U . . .
H34B H -0.0988 0.8135 0.3452 0.189 Uiso 1 1 calc R U . . .
C6 C 0.2145(9) 0.0643(6) 0.4223(6) 0.137(3) Uani 1 1 d . . . . .
H6 H 0.2273 0.0555 0.4764 0.164 Uiso 1 1 calc R U . . .
C30 C 0.2093(6) 0.3850(6) 0.1703(5) 0.129(3) Uani 1 1 d . . . . .
H30A H 0.2162 0.3717 0.2259 0.155 Uiso 1 1 calc R U . . .
H30B H 0.1354 0.3536 0.1440 0.155 Uiso 1 1 calc R U . . .
C38 C 0.0004(7) 0.7862(7) 0.0492(5) 0.136(3) Uani 1 1 d . . . . .
H38A H 0.0565 0.7743 0.0136 0.163 Uiso 1 1 calc R U . . .
H38B H -0.0557 0.7214 0.0314 0.163 Uiso 1 1 calc R U . . .
C43 C 0.5012(7) 0.8484(7) 0.4127(6) 0.164(4) Uani 1 1 d . . . . .
H43A H 0.4662 0.8855 0.4572 0.246 Uiso 1 1 calc R U . . .
H43B H 0.5662 0.8955 0.4084 0.246 Uiso 1 1 calc R U . . .
H43C H 0.5201 0.7804 0.4239 0.246 Uiso 1 1 calc R U . . .
C39 C -0.0473(8) 0.8802(7) 0.0339(6) 0.180(4) Uani 1 1 d . . . . .
H39A H -0.0951 0.9009 0.0742 0.270 Uiso 1 1 calc R U . . .
H39B H -0.0881 0.8609 -0.0211 0.270 Uiso 1 1 calc R U . . .
H39C H 0.0095 0.9413 0.0382 0.270 Uiso 1 1 calc R U . . .
C35 C -0.2171(7) 0.6972(11) 0.3643(7) 0.256(7) Uani 1 1 d D . . . .
H35A H -0.2649 0.6942 0.3143 0.384 Uiso 1 1 calc R U . . .
H35B H -0.2389 0.7468 0.4104 0.384 Uiso 1 1 calc R U . . .
H35C H -0.2209 0.6243 0.3745 0.384 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
S1 C3 1.671(5) . ?
S3 C12 1.660(5) . ?
S2 C21 1.668(5) . ?
N1 C10 1.447(6) . ?
N1 C1 1.464(5) . ?
N1 C19 1.465(6) . ?
O2 C44 1.239(6) . ?
O1 C44 1.251(6) . ?
N3 C3 1.364(6) . ?
N3 C4 1.410(6) . ?
N3 H3N 0.8600 . ?
N8 C36 1.489(7) . ?
N8 C32 1.495(6) . ?
N8 C40 1.514(7) . ?
N8 C28 1.550(6) . ?
N2 C3 1.340(6) . ?
N2 C2 1.444(6) . ?
N2 H2N 0.8600 . ?
N5 C21 1.365(6) . ?
N5 C22 1.403(6) . ?
N5 H5N 0.8600 . ?
N6 C12 1.350(6) . ?
N6 C11 1.440(6) . ?
N6 H6N 0.8600 . ?
N7 C12 1.365(6) . ?
N7 C13 1.418(6) . ?
N7 H7N 0.8600 . ?
N4 C21 1.332(6) . ?
N4 C20 1.451(6) . ?
N4 H4N 0.8600 . ?
C1 C2 1.517(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C10 C11 1.510(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C44 C45 1.514(7) . ?
C22 C23 1.369(7) . ?
C22 C27 1.387(7) . ?
C19 C20 1.514(7) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C13 C18 1.357(7) . ?
C13 C14 1.368(7) . ?
C4 C9 1.366(8) . ?
C4 C5 1.378(8) . ?
C23 C24 1.389(7) . ?
C23 H23 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C28 C29 1.444(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C32 C33 1.459(8) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C25 C26 1.329(10) . ?
C25 C24 1.378(9) . ?
C25 H25 0.9300 . ?
C5 C6 1.396(9) . ?
C5 H5 0.9300 . ?
C24 H24 0.9300 . ?
C29 C30 1.494(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C14 C15 1.395(8) . ?
C14 H14 0.9300 . ?
C27 C26 1.384(9) . ?
C27 H27 0.9300 . ?
C33 C34 1.447(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C18 C17 1.395(8) . ?
C18 H18 0.9300 . ?
C9 C8 1.414(10) . ?
C9 H9 0.9300 . ?
C37 C38 1.474(9) . ?
C37 C36 1.478(8) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C40 C41 1.432(8) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C16 C15 1.323(9) . ?
C16 C17 1.356(9) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C26 H26 0.9300 . ?
C8 C7 1.358(12) . ?
C8 H8 0.9300 . ?
C41 C42 1.454(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C7 C6 1.341(12) . ?
C7 H7 0.9300 . ?
C42 C43 1.400(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C15 H15 0.9300 . ?
C31 C30 1.386(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C34 C35 1.5386(11) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C6 H6 0.9300 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C38 C39 1.439(9) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 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 112.0(4) . . ?
C10 N1 C19 113.1(4) . . ?
C1 N1 C19 112.5(4) . . ?
C3 N3 C4 127.9(4) . . ?
C3 N3 H3N 116.0 . . ?
C4 N3 H3N 116.0 . . ?
C36 N8 C32 113.8(5) . . ?
C36 N8 C40 109.9(4) . . ?
C32 N8 C40 108.4(4) . . ?
C36 N8 C28 107.7(4) . . ?
C32 N8 C28 108.5(4) . . ?
C40 N8 C28 108.4(4) . . ?
C3 N2 C2 124.1(4) . . ?
C3 N2 H2N 117.9 . . ?
C2 N2 H2N 117.9 . . ?
C21 N5 C22 132.0(5) . . ?
C21 N5 H5N 114.0 . . ?
C22 N5 H5N 114.0 . . ?
C12 N6 C11 125.6(5) . . ?
C12 N6 H6N 117.2 . . ?
C11 N6 H6N 117.2 . . ?
C12 N7 C13 130.4(4) . . ?
C12 N7 H7N 114.8 . . ?
C13 N7 H7N 114.8 . . ?
C21 N4 C20 125.0(5) . . ?
C21 N4 H4N 117.5 . . ?
C20 N4 H4N 117.5 . . ?
N1 C1 C2 111.2(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 . . ?
N2 C2 C1 111.7(4) . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 N3 113.3(4) . . ?
N2 C3 S1 123.7(4) . . ?
N3 C3 S1 122.9(4) . . ?
N4 C21 N5 112.3(5) . . ?
N4 C21 S2 122.3(4) . . ?
N5 C21 S2 125.3(4) . . ?
N1 C10 C11 113.1(4) . . ?
N1 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
O2 C44 O1 123.5(5) . . ?
O2 C44 C45 119.2(5) . . ?
O1 C44 C45 117.3(5) . . ?
C23 C22 C27 118.1(6) . . ?
C23 C22 N5 125.9(5) . . ?
C27 C22 N5 115.9(5) . . ?
N6 C12 N7 111.5(4) . . ?
N6 C12 S3 123.8(4) . . ?
N7 C12 S3 124.7(4) . . ?
N1 C19 C20 112.5(4) . . ?
N1 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N1 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C18 C13 C14 119.0(5) . . ?
C18 C13 N7 117.5(5) . . ?
C14 C13 N7 123.3(5) . . ?
C9 C4 C5 119.7(6) . . ?
C9 C4 N3 122.1(6) . . ?
C5 C4 N3 118.0(5) . . ?
C22 C23 C24 120.8(6) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
N4 C20 C19 112.2(4) . . ?
N4 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
N4 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
N6 C11 C10 111.5(4) . . ?
N6 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N6 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C29 C28 N8 119.2(5) . . ?
C29 C28 H28A 107.5 . . ?
N8 C28 H28A 107.5 . . ?
C29 C28 H28B 107.5 . . ?
N8 C28 H28B 107.5 . . ?
H28A C28 H28B 107.0 . . ?
C33 C32 N8 118.6(5) . . ?
C33 C32 H32A 107.6 . . ?
N8 C32 H32A 107.7 . . ?
C33 C32 H32B 107.7 . . ?
N8 C32 H32B 107.7 . . ?
H32A C32 H32B 107.1 . . ?
C26 C25 C24 119.4(7) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C4 C5 C6 119.6(7) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C25 C24 C23 120.0(7) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C28 C29 C30 116.1(6) . . ?
C28 C29 H29A 108.3 . . ?
C30 C29 H29A 108.3 . . ?
C28 C29 H29B 108.3 . . ?
C30 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C13 C14 C15 119.6(6) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C26 C27 C22 120.0(7) . . ?
C26 C27 H27 120.0 . . ?
C22 C27 H27 120.0 . . ?
C32 C33 C34 112.7(6) . . ?
C32 C33 H33A 109.1 . . ?
C34 C33 H33A 109.1 . . ?
C32 C33 H33B 109.0 . . ?
C34 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C13 C18 C17 120.7(6) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C4 C9 C8 119.8(7) . . ?
C4 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C38 C37 C36 114.6(6) . . ?
C38 C37 H37A 108.6 . . ?
C36 C37 H37A 108.6 . . ?
C38 C37 H37B 108.6 . . ?
C36 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C41 C40 N8 122.5(6) . . ?
C41 C40 H40A 106.7 . . ?
N8 C40 H40A 106.7 . . ?
C41 C40 H40B 106.7 . . ?
N8 C40 H40B 106.7 . . ?
H40A C40 H40B 106.6 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C15 C16 C17 121.0(7) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C16 C17 C18 119.0(7) . . ?
C16 C17 H17 120.5 . . ?
C18 C17 H17 120.5 . . ?
C37 C36 N8 116.9(5) . . ?
C37 C36 H36A 108.1 . . ?
N8 C36 H36A 108.1 . . ?
C37 C36 H36B 108.1 . . ?
N8 C36 H36B 108.1 . . ?
H36A C36 H36B 107.3 . . ?
C25 C26 C27 121.8(7) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C7 C8 C9 119.2(8) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C40 C41 C42 119.0(7) . . ?
C40 C41 H41A 107.6 . . ?
C42 C41 H41A 107.6 . . ?
C40 C41 H41B 107.6 . . ?
C42 C41 H41B 107.6 . . ?
H41A C41 H41B 107.0 . . ?
C6 C7 C8 121.2(10) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C43 C42 C41 122.9(8) . . ?
C43 C42 H42A 106.6 . . ?
C41 C42 H42A 106.6 . . ?
C43 C42 H42B 106.6 . . ?
C41 C42 H42B 106.6 . . ?
H42A C42 H42B 106.6 . . ?
C16 C15 C14 120.6(7) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
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 . . ?
C35 C34 C33 122.3(8) . . ?
C35 C34 H34A 106.7 . . ?
C33 C34 H34A 106.7 . . ?
C35 C34 H34B 106.8 . . ?
C33 C34 H34B 106.8 . . ?
H34A C34 H34B 106.6 . . ?
C7 C6 C5 120.4(9) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C31 C30 C29 120.9(7) . . ?
C31 C30 H30A 107.1 . . ?
C29 C30 H30A 107.1 . . ?
C31 C30 H30B 107.1 . . ?
C29 C30 H30B 107.1 . . ?
H30A C30 H30B 106.8 . . ?
C39 C38 C37 118.4(8) . . ?
C39 C38 H38A 107.7 . . ?
C37 C38 H38A 107.7 . . ?
C39 C38 H38B 107.7 . . ?
C37 C38 H38B 107.7 . . ?
H38A C38 H38B 107.1 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 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 . . ?
C34 C35 H35A 109.4 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

_refine_diff_density_max         0.723
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_exp_T-Ph-ncs-TBACl
_database_code_depnum_ccdc_archive 'CCDC 1576492'
_audit_update_record             
;
2017-09-25 deposited with the CCDC.
2018-05-29 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 H33 N7 S3, C16 H36 N, Cl'
_chemical_formula_sum            'C43 H69 Cl N8 S3'
_chemical_formula_weight         829.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.3430(9)
_cell_length_b                   22.987(4)
_cell_length_c                   20.053(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.231(10)
_cell_angle_gamma                90
_cell_volume                     4691.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1183
_cell_measurement_theta_min      3.5000
_cell_measurement_theta_max      18.1570

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_F_000             1792.0
_exptl_transmission_factor_min   0.918
_exptl_transmission_factor_max   0.943
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.23
_exptl_absorpt_coefficient_mu    0.253
_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 and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17433
_diffrn_reflns_av_unetI/netI     0.3083
_diffrn_reflns_av_R_equivalents  0.1314
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.991
_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             8245
_reflns_number_gt                6156
_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)+(0.0100P)²+2.0010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00068(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8245
_refine_ls_number_parameters     557
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.3175
_refine_ls_R_factor_gt           0.0986
_refine_ls_wR_factor_ref         0.2023
_refine_ls_wR_factor_gt          0.1306
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.997
_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
C42A C 0.7001(14) 0.7563(6) 0.3530(10) 0.080(7) Uani 0.5 1 d D . P A 1
H42A H 0.7779 0.7379 0.3785 0.096 Uiso 0.5 1 calc R U P A 1
H42B H 0.6896 0.7436 0.3063 0.096 Uiso 0.5 1 calc R U P A 1
C1A C -0.0130(15) 0.6113(9) 0.3450(9) 0.106(7) Uani 0.5 1 d D U P B 1
H1A1 H 0.0145 0.5889 0.3860 0.127 Uiso 0.5 1 calc R U P B 1
H1A2 H -0.0426 0.6490 0.3578 0.127 Uiso 0.5 1 calc R U P B 1
C10A C -0.2197(17) 0.5678(9) 0.3452(9) 0.104(7) Uani 0.5 1 d D . P B 1
H10A H -0.2994 0.5540 0.3165 0.125 Uiso 0.5 1 calc R U P B 1
H10B H -0.2411 0.6029 0.3677 0.125 Uiso 0.5 1 calc R U P B 1
C19A C -0.1907(19) 0.6199(7) 0.2499(8) 0.107(8) Uani 0.5 1 d D U P B 1
H19A H -0.1254 0.6412 0.2305 0.128 Uiso 0.5 1 calc R U P B 1
H19B H -0.2395 0.6481 0.2715 0.128 Uiso 0.5 1 calc R U P B 1
C39A C 0.067(2) 0.7852(17) 0.3989(18) 0.115(11) Uani 0.5 1 d D . P C 1
H39A H 0.0660 0.7450 0.3857 0.173 Uiso 0.5 1 calc R U P C 1
H39B H -0.0106 0.8041 0.3748 0.173 Uiso 0.5 1 calc R U P C 1
H39C H 0.0673 0.7879 0.4467 0.173 Uiso 0.5 1 calc R U P C 1
C43A C 0.7138(17) 0.8213(6) 0.3571(11) 0.082(7) Uani 0.5 1 d D U P A 1
H43F H 0.6376 0.8390 0.3305 0.124 Uiso 0.5 1 calc R U P A 1
H43E H 0.7908 0.8329 0.3399 0.124 Uiso 0.5 1 calc R U P A 1
H43D H 0.7216 0.8335 0.4034 0.124 Uiso 0.5 1 calc R U P A 1
C42B C 0.695(2) 0.7798(12) 0.3798(8) 0.26(2) Uani 0.5 1 d D . P A 2
H42C H 0.6912 0.8134 0.4086 0.309 Uiso 0.5 1 calc R U P A 2
H42D H 0.7776 0.7596 0.3953 0.309 Uiso 0.5 1 calc R U P A 2
C1B C -0.0425(11) 0.6311(6) 0.2832(8) 0.058(4) Uani 0.5 1 d D U P B 2
H1B1 H -0.0683 0.6669 0.3030 0.069 Uiso 0.5 1 calc R U P B 2
H1B2 H -0.0591 0.6356 0.2343 0.069 Uiso 0.5 1 calc R U P B 2
C10B C -0.1107(17) 0.5778(7) 0.3758(6) 0.068(6) Uani 0.5 1 d D . P B 2
H10D H -0.1546 0.6110 0.3917 0.081 Uiso 0.5 1 calc R U P B 2
H10C H -0.0187 0.5796 0.3968 0.081 Uiso 0.5 1 calc R U P B 2
C19B C -0.2594(11) 0.5902(8) 0.2697(6) 0.059(5) Uani 0.5 1 d D U P B 2
H19C H -0.2907 0.6262 0.2863 0.071 Uiso 0.5 1 calc R U P B 2
H19D H -0.3114 0.5588 0.2836 0.071 Uiso 0.5 1 calc R U P B 2
C39B C 0.100(4) 0.7795(13) 0.3385(15) 0.159(15) Uani 0.5 1 d D . P C 2
H39D H 0.1491 0.7457 0.3305 0.239 Uiso 0.5 1 calc R U P C 2
H39E H 0.0820 0.8026 0.2980 0.239 Uiso 0.5 1 calc R U P C 2
H39F H 0.0181 0.7677 0.3510 0.239 Uiso 0.5 1 calc R U P C 2
C43B C 0.686(2) 0.7984(14) 0.3075(8) 0.142(10) Uani 0.5 1 d D U P A 2
H43A H 0.6978 0.7652 0.2801 0.213 Uiso 0.5 1 calc R U P A 2
H43B H 0.7538 0.8265 0.3044 0.213 Uiso 0.5 1 calc R U P A 2
H43C H 0.6018 0.8155 0.2916 0.213 Uiso 0.5 1 calc R U P A 2
Cl1 Cl 0.99822(16) 0.43997(10) 0.22395(10) 0.0653(7) Uani 1 1 d . . . . .
S3 S -0.3338(2) 0.57396(11) 0.03795(11) 0.0819(8) Uani 1 1 d . . . . .
S1 S 0.39639(19) 0.59733(12) 0.30158(12) 0.0860(9) Uani 1 1 d . . . . .
S2 S -0.1500(2) 0.40661(12) 0.47363(12) 0.0871(9) Uani 1 1 d . . . . .
N5 N -0.0326(6) 0.3828(4) 0.3672(3) 0.076(2) Uani 1 1 d . . . . .
H5N H -0.0274 0.3949 0.3272 0.091 Uiso 1 1 calc R U . . .
N2 N 0.1450(6) 0.5658(3) 0.2816(3) 0.072(2) Uani 1 1 d . . . . .
H2N H 0.0854 0.5402 0.2683 0.087 Uiso 1 1 calc R U . . .
N8 N 0.4638(6) 0.7272(4) 0.4849(4) 0.076(2) Uani 1 1 d . . . . .
N1 N -0.1213(6) 0.5817(3) 0.3025(3) 0.0576(19) Uani 1 1 d D U . . .
N3 N 0.2822(6) 0.5008(3) 0.2465(3) 0.071(2) Uani 1 1 d . . . . .
H3N H 0.2107 0.4819 0.2329 0.085 Uiso 1 1 calc R U . . .
N7 N -0.1812(6) 0.4828(4) 0.0828(4) 0.078(2) Uani 1 1 d . . . . .
H7N H -0.1353 0.4661 0.1175 0.093 Uiso 1 1 calc R U . . .
N4 N -0.1079(6) 0.4731(4) 0.3732(3) 0.069(2) Uani 1 1 d . . . . .
H4N H -0.0774 0.4778 0.3363 0.083 Uiso 1 1 calc R U . . .
N6 N -0.2237(6) 0.5446(3) 0.1631(4) 0.074(2) Uani 1 1 d . . . . .
H6N H -0.1713 0.5226 0.1901 0.089 Uiso 1 1 calc R U . . .
C3 C 0.2698(8) 0.5532(4) 0.2758(4) 0.063(3) Uani 1 1 d . . . . .
C4 C 0.4001(8) 0.4738(4) 0.2358(5) 0.073(3) Uani 1 1 d . . . . .
C12 C -0.0929(8) 0.4211(5) 0.4027(4) 0.068(3) Uani 1 1 d . . . . .
C11 C -0.1712(8) 0.5217(5) 0.3983(4) 0.079(3) Uani 1 1 d D . . . .
H11A H -0.1100 0.5397 0.4347 0.094 Uiso 1 1 calc R U . B 1
H11B H -0.2454 0.5076 0.4172 0.094 Uiso 1 1 calc R U . B 1
C2 C 0.1056(7) 0.6197(4) 0.3085(4) 0.082(3) Uani 1 1 d D U . . .
H2A H 0.0826 0.6474 0.2719 0.098 Uiso 1 1 calc R U . B 1
H2B H 0.1789 0.6355 0.3403 0.098 Uiso 1 1 calc R U . B 1
C21 C -0.2426(8) 0.5316(5) 0.0964(5) 0.069(3) Uani 1 1 d . . . . .
C26 C -0.0607(11) 0.4057(5) -0.0545(7) 0.098(4) Uani 1 1 d . . . . .
H22 H 0.0185 0.3924 -0.0646 0.117 Uiso 1 1 calc R U . . .
C13 C 0.0239(8) 0.3271(5) 0.3819(5) 0.066(3) Uani 1 1 d . . . . .
C18 C 0.0957(8) 0.3055(5) 0.3365(4) 0.079(3) Uani 1 1 d . . . . .
H16 H 0.1034 0.3277 0.2985 0.095 Uiso 1 1 calc R U . . .
C20 C -0.2840(7) 0.5923(4) 0.1928(4) 0.078(3) Uani 1 1 d D . . . .
H20A H -0.3606 0.5782 0.2096 0.094 Uiso 1 1 calc R U . B 1
H20B H -0.3131 0.6213 0.1583 0.094 Uiso 1 1 calc R U . B 1
C29 C 0.6034(8) 0.6382(4) 0.5297(4) 0.087(3) Uani 1 1 d . . . . .
H33A H 0.6782 0.6534 0.5122 0.104 Uiso 1 1 calc R U . . .
H33B H 0.6107 0.6507 0.5764 0.104 Uiso 1 1 calc R U . . .
C22 C -0.1803(9) 0.4547(4) 0.0209(5) 0.068(3) Uani 1 1 d . . . . .
C31 C 0.7247(8) 0.5466(4) 0.5697(4) 0.112(4) Uani 1 1 d . . . . .
H31A H 0.8014 0.5567 0.5514 0.169 Uiso 1 1 calc R U . . .
H31C H 0.7148 0.5051 0.5694 0.169 Uiso 1 1 calc R U . . .
H31B H 0.7339 0.5607 0.6153 0.169 Uiso 1 1 calc R U . . .
C23 C -0.2951(8) 0.4441(4) -0.0235(4) 0.076(3) Uani 1 1 d . . . . .
H25 H -0.3748 0.4566 -0.0132 0.091 Uiso 1 1 calc R U . . .
C28 C 0.4777(7) 0.6619(4) 0.4883(4) 0.076(3) Uani 1 1 d . . . . .
H32A H 0.4702 0.6473 0.4424 0.091 Uiso 1 1 calc R U . . .
H32B H 0.4043 0.6463 0.5067 0.091 Uiso 1 1 calc R U . . .
C15 C 0.0743(9) 0.2412(5) 0.4464(5) 0.094(3) Uani 1 1 d . . . . .
H13 H 0.0657 0.2187 0.4840 0.113 Uiso 1 1 calc R U . . .
C9 C 0.4929(9) 0.4555(4) 0.2895(4) 0.085(3) Uani 1 1 d . . . . .
H4 H 0.4810 0.4622 0.3338 0.102 Uiso 1 1 calc R U . . .
C17 C 0.1565(9) 0.2527(5) 0.3447(5) 0.089(3) Uani 1 1 d . . . . .
H15 H 0.2042 0.2391 0.3128 0.107 Uiso 1 1 calc R U . . .
C5 C 0.4168(9) 0.4623(4) 0.1715(5) 0.085(3) Uani 1 1 d . . . . .
H8 H 0.3526 0.4733 0.1351 0.101 Uiso 1 1 calc R U . . .
C6 C 0.5284(11) 0.4346(5) 0.1600(5) 0.101(4) Uani 1 1 d . . . . .
H7 H 0.5400 0.4281 0.1157 0.121 Uiso 1 1 calc R U . . .
C34 C 0.3988(9) 0.7605(5) 0.6643(5) 0.112(4) Uani 1 1 d . . . . .
H34A H 0.4836 0.7465 0.6872 0.134 Uiso 1 1 calc R U . . .
H34B H 0.4045 0.8024 0.6602 0.134 Uiso 1 1 calc R U . . .
C36 C 0.3297(7) 0.7376(4) 0.4415(4) 0.079(3) Uani 1 1 d . . . . .
H36A H 0.2638 0.7180 0.4623 0.094 Uiso 1 1 calc R U . . .
H36B H 0.3284 0.7201 0.3974 0.094 Uiso 1 1 calc R U . . .
C30 C 0.6048(8) 0.5738(5) 0.5269(4) 0.093(3) Uani 1 1 d . . . . .
H30A H 0.6006 0.5618 0.4802 0.111 Uiso 1 1 calc R U . . .
H30B H 0.5269 0.5591 0.5420 0.111 Uiso 1 1 calc R U . . .
C32 C 0.4718(8) 0.7538(4) 0.5545(5) 0.094(3) Uani 1 1 d . . . . .
H40A H 0.5576 0.7451 0.5809 0.113 Uiso 1 1 calc R U . . .
H40B H 0.4654 0.7957 0.5494 0.113 Uiso 1 1 calc R U . . .
C14 C 0.0144(8) 0.2944(5) 0.4384(5) 0.087(3) Uani 1 1 d . . . . .
H12 H -0.0322 0.3084 0.4707 0.105 Uiso 1 1 calc R U . . .
C16 C 0.1465(10) 0.2201(5) 0.4007(6) 0.099(4) Uani 1 1 d . . . . .
H14 H 0.1882 0.1842 0.4076 0.119 Uiso 1 1 calc R U . . .
C24 C -0.2924(11) 0.4145(5) -0.0839(5) 0.101(4) Uani 1 1 d . . . . .
H24 H -0.3702 0.4073 -0.1140 0.122 Uiso 1 1 calc R U . . .
C8 C 0.6052(10) 0.4268(5) 0.2771(6) 0.111(4) Uani 1 1 d . . . . .
H5 H 0.6688 0.4147 0.3132 0.133 Uiso 1 1 calc R U . . .
C27 C -0.0632(9) 0.4353(4) 0.0052(5) 0.090(3) Uani 1 1 d . . . . .
H44 H 0.0149 0.4422 0.0351 0.108 Uiso 1 1 calc R U . . .
C35 C 0.2982(10) 0.7464(5) 0.7061(5) 0.135(5) Uani 1 1 d . . . . .
H35A H 0.2136 0.7593 0.6832 0.203 Uiso 1 1 calc R U . . .
H35B H 0.3197 0.7657 0.7491 0.203 Uiso 1 1 calc R U . . .
H35C H 0.2963 0.7051 0.7130 0.203 Uiso 1 1 calc R U . . .
C25 C -0.1761(14) 0.3961(5) -0.0990(5) 0.104(4) Uani 1 1 d . . . . .
H23 H -0.1745 0.3770 -0.1396 0.125 Uiso 1 1 calc R U . . .
C7 C 0.6221(10) 0.4165(5) 0.2122(8) 0.110(5) Uani 1 1 d . . . . .
H46 H 0.6966 0.3972 0.2037 0.132 Uiso 1 1 calc R U . . .
C40 C 0.5717(8) 0.7562(4) 0.4540(5) 0.097(3) Uani 1 1 d . . . . .
H28A H 0.5592 0.7980 0.4556 0.116 Uiso 1 1 calc R U . . .
H28B H 0.6553 0.7474 0.4826 0.116 Uiso 1 1 calc R U . . .
C33 C 0.3693(9) 0.7340(5) 0.5937(5) 0.112(4) Uani 1 1 d . . . . .
H33C H 0.3699 0.6919 0.5969 0.134 Uiso 1 1 calc R U . . .
H33D H 0.2830 0.7462 0.5708 0.134 Uiso 1 1 calc R U . . .
C37 C 0.2917(10) 0.8025(5) 0.4315(5) 0.131(5) Uani 1 1 d . . . . .
H37A H 0.2861 0.8198 0.4751 0.158 Uiso 1 1 calc R U . . .
H37B H 0.3592 0.8229 0.4129 0.158 Uiso 1 1 calc R U . . .
C41 C 0.5814(9) 0.7400(5) 0.3824(5) 0.137(5) Uani 1 1 d D . . . .
H41A H 0.5724 0.6980 0.3788 0.164 Uiso 1 1 calc R U . A 1
H41B H 0.5055 0.7565 0.3532 0.164 Uiso 1 1 calc R U . A 1
C38 C 0.1641(16) 0.8089(7) 0.3854(14) 0.191(8) Uani 1 1 d D . . . .
H38A H 0.1453 0.8502 0.3808 0.229 Uiso 1 1 calc R U . C 1
H38B H 0.1757 0.7950 0.3411 0.229 Uiso 1 1 calc R U . C 1


_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
C42A C43A 1.5000(11) . ?
C42A C41 1.5003(10) . ?
C1A N1 1.451(14) . ?
C1A C2 1.547(14) . ?
C10A N1 1.476(14) . ?
C10A C11 1.522(14) . ?
C19A N1 1.460(14) . ?
C19A C20 1.500(14) . ?
C39A C38 1.218(16) . ?
C42B C43B 1.4999(10) . ?
C42B C41 1.5001(10) . ?
C1B N1 1.490(12) . ?
C1B C2 1.549(12) . ?
C10B N1 1.458(13) . ?
C10B C11 1.536(15) . ?
C19B N1 1.476(11) . ?
C19B C20 1.519(12) . ?
C39B C38 1.250(17) . ?
S3 C21 1.678(9) . ?
S1 C3 1.664(8) . ?
S2 C12 1.668(9) . ?
N5 C12 1.352(10) . ?
N5 C13 1.417(10) . ?
N2 C3 1.348(8) . ?
N2 C2 1.438(9) . ?
N8 C28 1.507(10) . ?
N8 C32 1.512(9) . ?
N8 C36 1.520(8) . ?
N8 C40 1.524(9) . ?
N3 C3 1.356(9) . ?
N3 C4 1.418(9) . ?
N7 C21 1.341(10) . ?
N7 C22 1.401(10) . ?
N4 C12 1.330(10) . ?
N4 C11 1.431(10) . ?
N6 C21 1.351(9) . ?
N6 C20 1.441(9) . ?
C4 C5 1.357(10) . ?
C4 C9 1.376(10) . ?
C26 C25 1.375(11) . ?
C26 C27 1.381(11) . ?
C13 C18 1.367(10) . ?
C13 C14 1.377(11) . ?
C18 C17 1.363(11) . ?
C29 C30 1.481(11) . ?
C29 C28 1.515(10) . ?
C22 C23 1.373(9) . ?
C22 C27 1.378(10) . ?
C31 C30 1.512(9) . ?
C23 C24 1.394(11) . ?
C15 C14 1.368(12) . ?
C15 C16 1.370(11) . ?
C9 C8 1.397(11) . ?
C17 C16 1.370(12) . ?
C5 C6 1.373(10) . ?
C6 C7 1.359(12) . ?
C34 C35 1.483(10) . ?
C34 C33 1.521(10) . ?
C36 C37 1.546(12) . ?
C32 C33 1.498(10) . ?
C24 C25 1.358(11) . ?
C8 C7 1.364(12) . ?
C40 C41 1.504(11) . ?
C37 C38 1.478(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C43A C42A C41 107.7(11) . . ?
N1 C1A C2 112.1(11) . . ?
N1 C10A C11 112.4(10) . . ?
N1 C19A C20 117.7(12) . . ?
C43B C42B C41 107.1(15) . . ?
N1 C1B C2 109.9(9) . . ?
N1 C10B C11 112.6(10) . . ?
N1 C19B C20 115.6(9) . . ?
C12 N5 C13 133.7(9) . . ?
C3 N2 C2 123.8(7) . . ?
C28 N8 C32 111.9(7) . . ?
C28 N8 C36 104.6(7) . . ?
C32 N8 C36 111.0(7) . . ?
C28 N8 C40 112.5(7) . . ?
C32 N8 C40 105.9(7) . . ?
C36 N8 C40 111.0(7) . . ?
C1A N1 C19A 111.7(12) . . ?
C10B N1 C19B 110.6(10) . . ?
C1A N1 C10A 107.6(12) . . ?
C19A N1 C10A 104.4(11) . . ?
C10B N1 C1B 111.2(9) . . ?
C19B N1 C1B 108.3(10) . . ?
C3 N3 C4 127.2(7) . . ?
C21 N7 C22 130.1(8) . . ?
C12 N4 C11 124.7(8) . . ?
C21 N6 C20 125.5(8) . . ?
N2 C3 N3 113.2(7) . . ?
N2 C3 S1 123.7(7) . . ?
N3 C3 S1 123.1(7) . . ?
C5 C4 C9 119.7(9) . . ?
C5 C4 N3 119.2(8) . . ?
C9 C4 N3 121.0(9) . . ?
N4 C12 N5 112.3(8) . . ?
N4 C12 S2 121.9(8) . . ?
N5 C12 S2 125.8(8) . . ?
N4 C11 C10A 114.3(10) . . ?
N4 C11 C10B 108.5(10) . . ?
N2 C2 C1B 110.6(9) . . ?
N2 C2 C1A 111.8(10) . . ?
N7 C21 N6 113.3(8) . . ?
N7 C21 S3 124.9(7) . . ?
N6 C21 S3 121.8(8) . . ?
C25 C26 C27 119.6(10) . . ?
C18 C13 C14 118.5(10) . . ?
C18 C13 N5 116.3(10) . . ?
C14 C13 N5 125.2(10) . . ?
C17 C18 C13 122.4(10) . . ?
N6 C20 C19A 111.7(10) . . ?
N6 C20 C19B 112.9(9) . . ?
C30 C29 C28 110.7(8) . . ?
C23 C22 C27 119.3(9) . . ?
C23 C22 N7 121.0(9) . . ?
C27 C22 N7 119.7(8) . . ?
C22 C23 C24 120.1(9) . . ?
N8 C28 C29 116.7(7) . . ?
C14 C15 C16 121.8(11) . . ?
C4 C9 C8 119.4(9) . . ?
C18 C17 C16 119.2(10) . . ?
C4 C5 C6 120.2(9) . . ?
C7 C6 C5 121.3(10) . . ?
C35 C34 C33 113.2(9) . . ?
N8 C36 C37 114.3(8) . . ?
C29 C30 C31 113.9(8) . . ?
C33 C32 N8 115.7(8) . . ?
C15 C14 C13 119.2(10) . . ?
C17 C16 C15 118.9(11) . . ?
C25 C24 C23 120.0(10) . . ?
C7 C8 C9 120.3(10) . . ?
C22 C27 C26 120.6(9) . . ?
C24 C25 C26 120.5(11) . . ?
C6 C7 C8 119.1(11) . . ?
C41 C40 N8 117.2(8) . . ?
C32 C33 C34 108.9(8) . . ?
C38 C37 C36 110.8(10) . . ?
C42B C41 C40 93.9(10) . . ?
C42A C41 C40 120.7(11) . . ?
C39A C38 C37 120(3) . . ?
C39B C38 C37 136(3) . . ?

_refine_diff_density_max         0.282
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.052

####################################################################### 
# 
# 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-Ph-ncs-TBACO3
_database_code_depnum_ccdc_archive 'CCDC 1576493'
_audit_update_record             
;
2017-09-25 deposited with the CCDC.
2018-05-29 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 H33 N7 S3), 2(C16 H36 N), C O3'
_chemical_formula_sum            'C87 H138 N16 O3 S6'
_chemical_formula_weight         1648.49

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'

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

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

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

_cell_length_a                   30.643(4)
_cell_length_b                   13.4778(16)
_cell_length_c                   23.218(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9589(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2033
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      12.41

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_F_000             3568.0
_exptl_transmission_factor_min   0.947
_exptl_transmission_factor_max   0.963
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.196
_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            68006
_diffrn_reflns_av_unetI/netI     0.1916
_diffrn_reflns_av_R_equivalents  0.1516
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.329
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.942
_reflns_number_total             15901
_reflns_number_gt                5463
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_max     0.926
_reflns_Friedel_fraction_full    0.926

_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)+(0.0600P)²+0.0482P] 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 1682 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.29(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15901
_refine_ls_number_parameters     1044
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2414
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.1985
_refine_ls_wR_factor_gt          0.1383
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_restrained_S_all      0.933
_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
O1A O 0.1456(8) 0.4445(19) 0.9683(10) 0.107(8) Uani 0.4 1 d . . P A 1
O2A O 0.1263(12) 0.571(3) 0.9125(13) 0.079(9) Uani 0.3 1 d . . P A 1
O3A O 0.0933(10) 0.433(3) 0.8967(13) 0.090(10) Uani 0.3 1 d . . P A 1
O1B O 0.1075(4) 0.5026(11) 0.8624(6) 0.076(4) Uani 0.6 1 d . . P A 2
O2B O 0.1216(5) 0.3822(11) 0.9232(5) 0.094(4) Uani 0.7 1 d . . P A 2
O3B O 0.1524(6) 0.5232(18) 0.9339(8) 0.119(5) Uani 0.7 1 d . . P A 2
S3 S 0.04656(11) 0.1828(3) 1.08113(15) 0.1035(12) Uani 1 1 d . . . . .
S2 S -0.04669(11) 0.6492(3) 0.87645(17) 0.1098(12) Uani 1 1 d . . . . .
S6 S 0.19682(12) 0.7733(3) 0.74957(16) 0.1135(13) Uani 1 1 d . . . . .
S5 S 0.17718(14) 0.7498(3) 1.10764(17) 0.1236(14) Uani 1 1 d . . . . .
N5 N 0.0380(3) 0.6422(9) 0.9049(4) 0.087(3) Uani 1 1 d . . . . .
H5N H 0.0590 0.6032 0.9146 0.105 Uiso 1 1 calc R U . . .
N2 N 0.0810(3) 0.2604(7) 0.8359(4) 0.080(3) Uani 1 1 d . . . . .
H2N H 0.0902 0.3025 0.8609 0.096 Uiso 1 1 calc R U . . .
N7 N 0.1154(4) 0.2541(7) 1.0236(4) 0.083(3) Uani 1 1 d . . . . .
H7N H 0.1248 0.2903 0.9957 0.100 Uiso 1 1 calc R U . . .
N1 N -0.0048(3) 0.2970(8) 0.8910(5) 0.083(3) Uani 1 1 d . . . . .
N3 N 0.1208(3) 0.3521(8) 0.7721(4) 0.089(3) Uani 1 1 d . . . . .
H3N H 0.1221 0.3938 0.8001 0.107 Uiso 1 1 calc R U . . .
N6 N 0.0504(4) 0.3140(8) 0.9961(4) 0.088(3) Uani 1 1 d . . . . .
H6N H 0.0655 0.3511 0.9735 0.106 Uiso 1 1 calc R U . . .
N4 N 0.0120(3) 0.5085(9) 0.8595(5) 0.091(3) Uani 1 1 d . . . . .
H4N H 0.0382 0.4873 0.8641 0.109 Uiso 1 1 calc R U . . .
C13 C 0.0444(4) 0.7442(12) 0.9177(7) 0.079(4) Uani 1 1 d . . . . .
C15 C 0.0426(6) 0.9173(12) 0.9025(7) 0.107(5) Uani 1 1 d . . . . .
H15 H 0.0327 0.9712 0.8812 0.128 Uiso 1 1 calc R U . . .
C12 C 0.0031(4) 0.5978(11) 0.8793(5) 0.077(3) Uani 1 1 d . . . . .
C14 C 0.0291(4) 0.8240(13) 0.8881(5) 0.083(4) Uani 1 1 d . . . . .
H14 H 0.0094 0.8150 0.8580 0.100 Uiso 1 1 calc R U . . .
C10 C -0.0370(4) 0.3660(11) 0.8704(6) 0.101(4) Uani 1 1 d . . . . .
H10A H -0.0503 0.3990 0.9031 0.122 Uiso 1 1 calc R U . . .
H10B H -0.0598 0.3297 0.8504 0.122 Uiso 1 1 calc R U . . .
C11 C -0.0184(5) 0.4426(11) 0.8307(6) 0.117(5) Uani 1 1 d . . . . .
H11A H -0.0035 0.4095 0.7992 0.140 Uiso 1 1 calc R U . . .
H11B H -0.0420 0.4815 0.8145 0.140 Uiso 1 1 calc R U . . .
C17 C 0.0848(5) 0.8533(16) 0.9782(7) 0.108(5) Uani 1 1 d . . . . .
H17 H 0.1038 0.8624 1.0089 0.130 Uiso 1 1 calc R U . . .
C18 C 0.0716(5) 0.7609(13) 0.9643(7) 0.106(5) Uani 1 1 d . . . . .
H18 H 0.0810 0.7075 0.9864 0.127 Uiso 1 1 calc R U . . .
C4 C 0.1450(4) 0.3775(14) 0.7232(6) 0.086(4) Uani 1 1 d . . . . .
C1 C 0.0048(5) 0.2190(11) 0.8503(6) 0.097(4) Uani 1 1 d . . . . .
H1A H -0.0005 0.2428 0.8116 0.117 Uiso 1 1 calc R U . . .
H1B H -0.0144 0.1631 0.8574 0.117 Uiso 1 1 calc R U . . .
C5 C 0.1485(6) 0.4739(13) 0.7095(8) 0.125(5) Uani 1 1 d . . . . .
H5 H 0.1341 0.5211 0.7317 0.150 Uiso 1 1 calc R U . . .
C2 C 0.0518(6) 0.1851(10) 0.8552(5) 0.106(5) Uani 1 1 d . . . . .
H2C H 0.0582 0.1689 0.8950 0.127 Uiso 1 1 calc R U . . .
H2D H 0.0559 0.1257 0.8323 0.127 Uiso 1 1 calc R U . . .
C3 C 0.0953(4) 0.2708(11) 0.7817(6) 0.085(4) Uani 1 1 d . . . . .
C7 C 0.1955(6) 0.433(2) 0.6317(7) 0.140(6) Uani 1 1 d . . . . .
H7 H 0.2130 0.4509 0.6006 0.168 Uiso 1 1 calc R U . . .
C6 C 0.1736(7) 0.5042(13) 0.6621(11) 0.148(6) Uani 1 1 d . . . . .
H6 H 0.1753 0.5708 0.6517 0.177 Uiso 1 1 calc R U . . .
C9 C 0.1668(6) 0.3098(12) 0.6919(8) 0.134(6) Uani 1 1 d . . . . .
H9 H 0.1647 0.2430 0.7014 0.161 Uiso 1 1 calc R U . . .
C22 C 0.1476(5) 0.2047(13) 1.0560(5) 0.084(4) Uani 1 1 d . . . . .
C21 C 0.0717(5) 0.2517(10) 1.0307(5) 0.078(3) Uani 1 1 d . . . . .
C24 C 0.1787(9) 0.0628(13) 1.1018(8) 0.134(6) Uani 1 1 d . . . . .
H24 H 0.1776 -0.0043 1.1111 0.160 Uiso 1 1 calc R U . . .
C20 C 0.0037(5) 0.3229(9) 0.9943(5) 0.091(4) Uani 1 1 d . . . . .
H20A H -0.0040 0.3917 0.9877 0.109 Uiso 1 1 calc R U . . .
H20B H -0.0082 0.3035 1.0313 0.109 Uiso 1 1 calc R U . . .
C19 C -0.0164(4) 0.2599(9) 0.9479(6) 0.094(4) Uani 1 1 d . . . . .
H19A H -0.0064 0.1920 0.9520 0.113 Uiso 1 1 calc R U . . .
H19B H -0.0479 0.2602 0.9522 0.113 Uiso 1 1 calc R U . . .
C27 C 0.1826(6) 0.2593(11) 1.0747(6) 0.097(4) Uani 1 1 d . . . . .
H27 H 0.1843 0.3267 1.0663 0.116 Uiso 1 1 calc R U . . .
C23 C 0.1451(5) 0.1043(15) 1.0696(6) 0.111(4) Uani 1 1 d . . . . .
H23 H 0.1216 0.0660 1.0575 0.134 Uiso 1 1 calc R U . . .
C26 C 0.2159(6) 0.2136(19) 1.1067(10) 0.153(8) Uani 1 1 d . . . . .
H26 H 0.2400 0.2503 1.1186 0.183 Uiso 1 1 calc R U . . .
S1 S 0.08223(16) 0.1884(3) 0.73041(15) 0.1385(17) Uani 1 1 d . . . . .
N10 N 0.2100(4) 0.2903(13) 0.9182(5) 0.112(4) Uani 1 1 d . . . . .
H10N H 0.1883 0.3286 0.9109 0.134 Uiso 1 1 calc R U . . .
N8 N 0.2564(3) 0.6450(10) 0.9324(6) 0.099(3) Uani 1 1 d . . . . .
N9 N 0.2380(4) 0.4265(12) 0.9611(5) 0.109(4) Uani 1 1 d . . . . .
H9N H 0.2122 0.4501 0.9568 0.131 Uiso 1 1 calc R U . . .
C30 C 0.2448(6) 0.3329(15) 0.9418(7) 0.106(5) Uani 1 1 d . . . . .
C31 C 0.2046(5) 0.1895(15) 0.9036(9) 0.093(4) Uani 1 1 d . . . . .
C36 C 0.1868(4) 0.1667(18) 0.8508(8) 0.126(7) Uani 1 1 d . . . . .
H36 H 0.1810 0.2158 0.8237 0.151 Uiso 1 1 calc R U . . .
S4 S 0.29498(13) 0.2835(3) 0.9453(2) 0.1352(15) Uani 1 1 d . . . . .
C28 C 0.2878(4) 0.5667(14) 0.9472(7) 0.128(5) Uani 1 1 d . . . . .
H28A H 0.3134 0.5970 0.9643 0.154 Uiso 1 1 calc R U . . .
H28B H 0.2969 0.5334 0.9122 0.154 Uiso 1 1 calc R U . . .
C48 C 0.1739(5) 0.6966(10) 0.7973(5) 0.078(3) Uani 1 1 d . . . . .
C53 C 0.0259(5) 0.7359(14) 0.7325(6) 0.105(4) Uani 1 1 d . . . . .
H53 H 0.0016 0.7002 0.7206 0.127 Uiso 1 1 calc R U . . .
C52 C 0.0270(6) 0.8375(14) 0.7252(6) 0.112(5) Uani 1 1 d . . . . .
H52 H 0.0041 0.8700 0.7068 0.134 Uiso 1 1 calc R U . . .
C47 C 0.2443(5) 0.6261(12) 0.8289(6) 0.118(5) Uani 1 1 d . . . . .
H47A H 0.2551 0.6492 0.7920 0.141 Uiso 1 1 calc R U . . .
H47B H 0.2524 0.5568 0.8330 0.141 Uiso 1 1 calc R U . . .
C51 C 0.0620(6) 0.8900(11) 0.7453(6) 0.099(4) Uani 1 1 d . . . . .
H51 H 0.0621 0.9587 0.7418 0.119 Uiso 1 1 calc R U . . .
C54 C 0.0607(5) 0.6872(9) 0.7573(5) 0.088(4) Uani 1 1 d . . . . .
H54 H 0.0600 0.6186 0.7614 0.106 Uiso 1 1 calc R U . . .
C50 C 0.0972(5) 0.8430(12) 0.7707(5) 0.090(4) Uani 1 1 d . . . . .
H50 H 0.1210 0.8794 0.7841 0.108 Uiso 1 1 calc R U . . .
C49 C 0.0964(5) 0.7395(11) 0.7759(5) 0.074(3) Uani 1 1 d . . . . .
C46 C 0.2650(5) 0.6847(12) 0.8757(8) 0.124(5) Uani 1 1 d . . . . .
H46A H 0.2963 0.6864 0.8695 0.149 Uiso 1 1 calc R U . . .
H46B H 0.2543 0.7523 0.8740 0.149 Uiso 1 1 calc R U . . .
N14 N 0.1302(3) 0.6889(7) 0.8060(4) 0.078(3) Uani 1 1 d . . . . .
H14N H 0.1220 0.6488 0.8327 0.093 Uiso 1 1 calc R U . . .
N13 N 0.1973(4) 0.6348(8) 0.8303(4) 0.089(3) Uani 1 1 d . . . . .
H13N H 0.1834 0.5975 0.8540 0.106 Uiso 1 1 calc R U . . .
C37 C 0.2536(6) 0.7238(14) 0.9779(8) 0.135(6) Uani 1 1 d . . . . .
H37A H 0.2631 0.6968 1.0145 0.162 Uiso 1 1 calc R U . . .
H37B H 0.2729 0.7783 0.9680 0.162 Uiso 1 1 calc R U . . .
C38 C 0.2084(7) 0.7611(12) 0.9832(7) 0.131(6) Uani 1 1 d . . . . .
H38A H 0.2082 0.8161 1.0101 0.157 Uiso 1 1 calc R U . . .
H38B H 0.1992 0.7864 0.9460 0.157 Uiso 1 1 calc R U . . .
C39 C 0.1631(6) 0.6761(13) 1.0528(7) 0.096(4) Uani 1 1 d . . . . .
N11 N 0.1784(4) 0.6904(9) 1.0016(7) 0.104(3) Uani 1 1 d . . . . .
H11N H 0.1687 0.6509 0.9754 0.125 Uiso 1 1 calc R U . . .
N12 N 0.1352(4) 0.5984(9) 1.0583(5) 0.087(3) Uani 1 1 d . . . . .
H12N H 0.1370 0.5559 1.0307 0.105 Uiso 1 1 calc R U . . .
C45 C 0.0860(6) 0.6430(11) 1.1355(7) 0.104(4) Uani 1 1 d . . . . .
H45 H 0.0955 0.7085 1.1345 0.125 Uiso 1 1 calc R U . . .
C40 C 0.1043(5) 0.5740(15) 1.0998(6) 0.089(4) Uani 1 1 d . . . . .
C43 C 0.0397(5) 0.5199(18) 1.1755(6) 0.121(5) Uani 1 1 d . . . . .
H43 H 0.0175 0.5029 1.2009 0.145 Uiso 1 1 calc R U . . .
C42 C 0.0588(7) 0.4491(11) 1.1409(8) 0.114(5) Uani 1 1 d . . . . .
H42 H 0.0497 0.3834 1.1430 0.137 Uiso 1 1 calc R U . . .
C41 C 0.0912(6) 0.4761(13) 1.1035(7) 0.100(4) Uani 1 1 d . . . . .
H41 H 0.1044 0.4284 1.0804 0.120 Uiso 1 1 calc R U . . .
C44 C 0.0541(7) 0.6157(16) 1.1719(7) 0.125(5) Uani 1 1 d . . . . .
H44 H 0.0415 0.6635 1.1955 0.150 Uiso 1 1 calc R U . . .
N15 N 0.9489(3) 0.9084(8) 0.0573(4) 0.082(3) Uani 1 1 d . . . . .
C64 C 0.9947(3) 0.9271(8) 0.0769(5) 0.078(3) Uani 1 1 d . . . . .
H64A H 1.0022 0.9950 0.0671 0.094 Uiso 1 1 calc R U . . .
H64B H 1.0140 0.8840 0.0552 0.094 Uiso 1 1 calc R U . . .
C66 C 1.0511(4) 0.9311(9) 0.1538(6) 0.093(4) Uani 1 1 d . . . . .
H66A H 1.0691 0.8880 0.1304 0.112 Uiso 1 1 calc R U . . .
H66B H 1.0582 0.9991 0.1439 0.112 Uiso 1 1 calc R U . . .
C65 C 1.0039(4) 0.9122(9) 0.1397(5) 0.090(4) Uani 1 1 d . . . . .
H65A H 0.9964 0.8447 0.1503 0.108 Uiso 1 1 calc R U . . .
H65B H 0.9857 0.9567 0.1621 0.108 Uiso 1 1 calc R U . . .
C67 C 1.0616(5) 0.9141(10) 0.2161(6) 0.131(5) Uani 1 1 d . . . . .
H67A H 1.0443 0.9576 0.2395 0.197 Uiso 1 1 calc R U . . .
H67B H 1.0920 0.9274 0.2226 0.197 Uiso 1 1 calc R U . . .
H67C H 1.0553 0.8465 0.2260 0.197 Uiso 1 1 calc R U . . .
C60 C 0.9166(4) 0.9790(11) 0.0853(5) 0.091(4) Uani 1 1 d . . . . .
H60A H 0.8875 0.9598 0.0732 0.109 Uiso 1 1 calc R U . . .
H60B H 0.9181 0.9694 0.1266 0.109 Uiso 1 1 calc R U . . .
C62 C 0.8844(5) 1.1491(14) 0.0978(7) 0.131(5) Uani 1 1 d . . . . .
H62A H 0.8575 1.1284 0.0793 0.158 Uiso 1 1 calc R U . . .
H62B H 0.8817 1.1346 0.1386 0.158 Uiso 1 1 calc R U . . .
C61 C 0.9219(4) 1.0869(11) 0.0734(6) 0.109(4) Uani 1 1 d . . . . .
H61A H 0.9235 1.0971 0.0321 0.130 Uiso 1 1 calc R U . . .
H61B H 0.9492 1.1095 0.0901 0.130 Uiso 1 1 calc R U . . .
C63 C 0.8887(7) 1.2532(15) 0.0911(10) 0.200(10) Uani 1 1 d . . . . .
H63A H 0.9159 1.2745 0.1074 0.300 Uiso 1 1 calc R U . . .
H63B H 0.8651 1.2860 0.1104 0.300 Uiso 1 1 calc R U . . .
H63C H 0.8881 1.2696 0.0508 0.300 Uiso 1 1 calc R U . . .
C68 C 0.9337(4) 0.8082(11) 0.0728(6) 0.095(4) Uani 1 1 d . . . . .
H68A H 0.9042 0.8001 0.0583 0.114 Uiso 1 1 calc R U . . .
H68B H 0.9323 0.8039 0.1145 0.114 Uiso 1 1 calc R U . . .
C70 C 0.9392(7) 0.6260(17) 0.0800(11) 0.216(12) Uani 1 1 d . . . . .
H70A H 0.9436 0.6255 0.1214 0.259 Uiso 1 1 calc R U . . .
H70B H 0.9082 0.6224 0.0720 0.259 Uiso 1 1 calc R U . . .
C69 C 0.9605(6) 0.7247(14) 0.0513(7) 0.134(6) Uani 1 1 d . . . . .
H69A H 0.9907 0.7323 0.0631 0.161 Uiso 1 1 calc R U . . .
H69B H 0.9594 0.7211 0.0096 0.161 Uiso 1 1 calc R U . . .
C56 C 0.9490(4) 0.9201(10) -0.0090(5) 0.097(4) Uani 1 1 d . . . . .
H56A H 0.9597 0.9860 -0.0182 0.117 Uiso 1 1 calc R U . . .
H56B H 0.9696 0.8727 -0.0250 0.117 Uiso 1 1 calc R U . . .
N16 N 0.1819(3) 0.5133(7) 0.2765(4) 0.074(3) Uani 1 1 d . . . . .
C86 C 0.1678(6) 0.4900(14) 0.4420(6) 0.153(7) Uani 1 1 d . . . . .
H86A H 0.1678 0.4181 0.4420 0.183 Uiso 1 1 calc R U . . .
H86B H 0.1971 0.5120 0.4511 0.183 Uiso 1 1 calc R U . . .
C85 C 0.1551(4) 0.5283(10) 0.3801(5) 0.102(4) Uani 1 1 d . . . . .
H85A H 0.1283 0.4971 0.3674 0.123 Uiso 1 1 calc R U . . .
H85B H 0.1507 0.5996 0.3808 0.123 Uiso 1 1 calc R U . . .
C84 C 0.1919(4) 0.5022(9) 0.3400(5) 0.082(4) Uani 1 1 d . . . . .
H84A H 0.2004 0.4340 0.3473 0.098 Uiso 1 1 calc R U . . .
H84B H 0.2167 0.5439 0.3493 0.098 Uiso 1 1 calc R U . . .
C80 C 0.1456(4) 0.4425(9) 0.2574(5) 0.079(3) Uani 1 1 d . . . . .
H80A H 0.1192 0.4596 0.2782 0.095 Uiso 1 1 calc R U . . .
H80B H 0.1400 0.4539 0.2168 0.095 Uiso 1 1 calc R U . . .
C82 C 0.1205(5) 0.2731(13) 0.2352(7) 0.130(5) Uani 1 1 d . . . . .
H82A H 0.1216 0.2890 0.1945 0.156 Uiso 1 1 calc R U . . .
H82B H 0.0919 0.2922 0.2494 0.156 Uiso 1 1 calc R U . . .
C72 C 0.1661(4) 0.6183(9) 0.2639(5) 0.084(4) Uani 1 1 d . . . . .
H72A H 0.1574 0.6213 0.2238 0.101 Uiso 1 1 calc R U . . .
H72B H 0.1402 0.6303 0.2869 0.101 Uiso 1 1 calc R U . . .
C76 C 0.2239(4) 0.4924(9) 0.2446(5) 0.083(3) Uani 1 1 d . . . . .
H76A H 0.2353 0.4291 0.2575 0.100 Uiso 1 1 calc R U . . .
H76B H 0.2450 0.5430 0.2547 0.100 Uiso 1 1 calc R U . . .
C55 C 0.1252(5) 0.4742(11) 0.9141(5) 0.046(3) Uani 1 1 d . . . . .
C29 C 0.2697(6) 0.4913(13) 0.9882(7) 0.138(6) Uani 1 1 d . . . . .
H29A H 0.2935 0.4516 1.0033 0.166 Uiso 1 1 calc R U . . .
H29B H 0.2560 0.5252 1.0203 0.166 Uiso 1 1 calc R U . . .
C33 C 0.2042(7) 0.0260(18) 0.9308(9) 0.134(7) Uani 1 1 d . . . . .
H33 H 0.2106 -0.0220 0.9583 0.160 Uiso 1 1 calc R U . . .
C32 C 0.2135(5) 0.1194(17) 0.9436(7) 0.113(5) Uani 1 1 d . . . . .
H32 H 0.2257 0.1362 0.9789 0.136 Uiso 1 1 calc R U . . .
C34 C 0.1857(6) -0.0057(15) 0.8799(13) 0.148(8) Uani 1 1 d . . . . .
H34 H 0.1792 -0.0722 0.8736 0.177 Uiso 1 1 calc R U . . .
C59 C 0.9064(8) 1.0279(16) -0.1168(8) 0.197(10) Uani 1 1 d . . . . .
H59A H 0.8924 1.0346 -0.1536 0.295 Uiso 1 1 calc R U . . .
H59B H 0.9354 1.0549 -0.1188 0.295 Uiso 1 1 calc R U . . .
H59C H 0.8899 1.0631 -0.0882 0.295 Uiso 1 1 calc R U . . .
C58 C 0.9087(5) 0.9280(17) -0.1020(7) 0.162(8) Uani 1 1 d . . . . .
H58A H 0.9360 0.9014 -0.1163 0.194 Uiso 1 1 calc R U . . .
H58B H 0.8853 0.8932 -0.1215 0.194 Uiso 1 1 calc R U . . .
C57 C 0.9056(4) 0.9058(14) -0.0385(6) 0.136(6) Uani 1 1 d . . . . .
H57A H 0.8960 0.8378 -0.0331 0.164 Uiso 1 1 calc R U . . .
H57B H 0.8841 0.9492 -0.0210 0.164 Uiso 1 1 calc R U . . .
C73 C 0.1976(4) 0.7003(10) 0.2750(6) 0.096(4) Uani 1 1 d . . . . .
H73A H 0.2212 0.6968 0.2473 0.115 Uiso 1 1 calc R U . . .
H73B H 0.2099 0.6930 0.3132 0.115 Uiso 1 1 calc R U . . .
C74 C 0.1748(5) 0.8009(11) 0.2701(6) 0.124(5) Uani 1 1 d . . . . .
H74A H 0.1604 0.8051 0.2330 0.148 Uiso 1 1 calc R U . . .
H74B H 0.1525 0.8054 0.2996 0.148 Uiso 1 1 calc R U . . .
C78 C 0.2647(6) 0.4755(13) 0.1503(6) 0.142(6) Uani 1 1 d . . . . .
H78A H 0.2801 0.4228 0.1702 0.171 Uiso 1 1 calc R U . . .
H78B H 0.2607 0.4548 0.1106 0.171 Uiso 1 1 calc R U . . .
C77 C 0.2195(5) 0.4897(10) 0.1786(5) 0.111(4) Uani 1 1 d . . . . .
H77A H 0.2065 0.5512 0.1652 0.133 Uiso 1 1 calc R U . . .
H77B H 0.2004 0.4356 0.1675 0.133 Uiso 1 1 calc R U . . .
C16 C 0.0706(5) 0.9333(15) 0.9480(8) 0.117(6) Uani 1 1 d . . . . .
H16 H 0.0795 0.9971 0.9578 0.140 Uiso 1 1 calc R U . . .
C75 C 0.2052(6) 0.8864(12) 0.2763(8) 0.160(7) Uani 1 1 d . . . . .
H75A H 0.2140 0.8924 0.3158 0.239 Uiso 1 1 calc R U . . .
H75B H 0.1907 0.9462 0.2645 0.239 Uiso 1 1 calc R U . . .
H75C H 0.2304 0.8759 0.2525 0.239 Uiso 1 1 calc R U . . .
C79 C 0.2913(6) 0.5634(15) 0.1511(9) 0.176(8) Uani 1 1 d . . . . .
H79A H 0.2729 0.6210 0.1487 0.264 Uiso 1 1 calc R U . . .
H79B H 0.3110 0.5625 0.1189 0.264 Uiso 1 1 calc R U . . .
H79C H 0.3077 0.5656 0.1863 0.264 Uiso 1 1 calc R U . . .
C81 C 0.1544(4) 0.3330(10) 0.2660(6) 0.096(4) Uani 1 1 d . . . . .
H81A H 0.1831 0.3165 0.2512 0.115 Uiso 1 1 calc R U . . .
H81B H 0.1539 0.3174 0.3068 0.115 Uiso 1 1 calc R U . . .
C87 C 0.1411(7) 0.522(2) 0.4821(10) 0.259(13) Uani 1 1 d . . . . .
H87A H 0.1353 0.5908 0.4764 0.388 Uiso 1 1 calc R U . . .
H87B H 0.1541 0.5118 0.5193 0.388 Uiso 1 1 calc R U . . .
H87C H 0.1142 0.4850 0.4800 0.388 Uiso 1 1 calc R U . . .
C83 C 0.1257(6) 0.1633(13) 0.2423(8) 0.174(8) Uani 1 1 d . . . . .
H83A H 0.1525 0.1424 0.2246 0.261 Uiso 1 1 calc R U . . .
H83B H 0.1016 0.1299 0.2242 0.261 Uiso 1 1 calc R U . . .
H83C H 0.1263 0.1470 0.2825 0.261 Uiso 1 1 calc R U . . .
C71 C 0.9607(8) 0.5498(19) 0.0548(9) 0.229(11) Uani 1 1 d . . . . .
H71A H 0.9491 0.5388 0.0169 0.343 Uiso 1 1 calc R U . . .
H71B H 0.9570 0.4909 0.0776 0.343 Uiso 1 1 calc R U . . .
H71C H 0.9912 0.5656 0.0521 0.343 Uiso 1 1 calc R U . . .
C25 C 0.2130(7) 0.118(2) 1.1200(9) 0.158(8) Uani 1 1 d . . . . .
H25 H 0.2348 0.0886 1.1421 0.189 Uiso 1 1 calc R U . . .
C8 C 0.1918(7) 0.3380(17) 0.6468(9) 0.164(8) Uani 1 1 d . . . . .
H8 H 0.2067 0.2900 0.6258 0.197 Uiso 1 1 calc R U . . .
C35 C 0.1774(5) 0.064(2) 0.8394(10) 0.141(7) Uani 1 1 d . . . . .
H35 H 0.1657 0.0456 0.8041 0.170 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
O1A C55 1.46(3) . ?
O2A C55 1.30(3) . ?
O3A C55 1.19(3) . ?
O1B C55 1.371(19) . ?
O2B C55 1.263(17) . ?
O3B C55 1.160(19) . ?
S3 C21 1.680(13) . ?
S2 C12 1.678(13) . ?
S6 C48 1.670(12) . ?
S5 C39 1.672(16) . ?
N5 C12 1.361(14) . ?
N5 C13 1.420(15) . ?
N2 C3 1.339(13) . ?
N2 C2 1.427(14) . ?
N7 C21 1.352(14) . ?
N7 C22 1.409(16) . ?
N1 C10 1.439(14) . ?
N1 C1 1.443(14) . ?
N1 C19 1.457(14) . ?
N3 C3 1.364(15) . ?
N3 C4 1.399(14) . ?
N6 C21 1.333(14) . ?
N6 C20 1.435(13) . ?
N4 C12 1.317(14) . ?
N4 C11 1.451(14) . ?
C13 C14 1.358(16) . ?
C13 C18 1.386(18) . ?
C15 C14 1.366(16) . ?
C15 C16 1.377(18) . ?
C10 C11 1.497(16) . ?
C17 C18 1.348(17) . ?
C17 C16 1.357(18) . ?
C4 C5 1.342(16) . ?
C4 C9 1.343(17) . ?
C1 C2 1.513(17) . ?
C5 C6 1.40(2) . ?
C3 S1 1.676(13) . ?
C7 C8 1.33(2) . ?
C7 C6 1.37(2) . ?
C9 C8 1.35(2) . ?
C22 C27 1.370(17) . ?
C22 C23 1.393(18) . ?
C24 C25 1.36(2) . ?
C24 C23 1.39(2) . ?
C20 C19 1.503(15) . ?
C27 C26 1.40(2) . ?
C26 C25 1.33(2) . ?
N10 C30 1.328(18) . ?
N10 C31 1.409(17) . ?
N8 C46 1.444(16) . ?
N8 C28 1.467(16) . ?
N8 C37 1.501(18) . ?
N9 C30 1.355(16) . ?
N9 C29 1.449(17) . ?
C30 S4 1.678(16) . ?
C31 C32 1.352(18) . ?
C31 C36 1.377(19) . ?
C36 C35 1.44(2) . ?
C28 C29 1.497(18) . ?
C48 N13 1.339(13) . ?
C48 N14 1.359(13) . ?
C53 C54 1.378(17) . ?
C53 C52 1.380(16) . ?
C52 C51 1.366(18) . ?
C47 N13 1.445(14) . ?
C47 C46 1.486(19) . ?
C51 C50 1.385(16) . ?
C54 C49 1.371(15) . ?
C50 C49 1.401(15) . ?
C49 N14 1.424(14) . ?
C37 C38 1.478(19) . ?
C38 N11 1.393(17) . ?
C39 N11 1.293(16) . ?
C39 N12 1.359(17) . ?
N12 C40 1.390(16) . ?
C45 C44 1.343(19) . ?
C45 C40 1.366(17) . ?
C40 C41 1.382(17) . ?
C43 C44 1.367(19) . ?
C43 C42 1.377(19) . ?
C42 C41 1.369(18) . ?
N15 C68 1.473(14) . ?
N15 C64 1.497(12) . ?
N15 C60 1.520(14) . ?
N15 C56 1.546(13) . ?
C64 C65 1.499(13) . ?
C66 C67 1.500(16) . ?
C66 C65 1.504(14) . ?
C60 C61 1.489(16) . ?
C62 C63 1.417(19) . ?
C62 C61 1.530(17) . ?
C68 C69 1.483(18) . ?
C70 C71 1.35(2) . ?
C70 C69 1.62(3) . ?
C56 C57 1.508(15) . ?
N16 C76 1.510(12) . ?
N16 C84 1.513(12) . ?
N16 C72 1.524(13) . ?
N16 C80 1.532(12) . ?
C86 C87 1.31(2) . ?
C86 C85 1.575(17) . ?
C85 C84 1.503(14) . ?
C80 C81 1.515(14) . ?
C82 C81 1.497(16) . ?
C82 C83 1.498(17) . ?
C72 C73 1.489(15) . ?
C76 C77 1.538(15) . ?
C33 C32 1.324(19) . ?
C33 C34 1.38(2) . ?
C34 C35 1.35(2) . ?
C59 C58 1.39(2) . ?
C58 C57 1.507(18) . ?
C73 C74 1.529(16) . ?
C74 C75 1.488(17) . ?
C78 C79 1.438(19) . ?
C78 C77 1.547(17) . ?

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
C12 N5 C13 128.6(12) . . ?
C3 N2 C2 125.1(11) . . ?
C21 N7 C22 128.2(11) . . ?
C10 N1 C1 113.3(11) . . ?
C10 N1 C19 110.8(11) . . ?
C1 N1 C19 113.2(11) . . ?
C3 N3 C4 129.3(11) . . ?
C21 N6 C20 123.9(11) . . ?
C12 N4 C11 126.0(12) . . ?
C14 C13 C18 118.3(14) . . ?
C14 C13 N5 127.8(15) . . ?
C18 C13 N5 113.8(15) . . ?
C14 C15 C16 121.4(15) . . ?
N4 C12 N5 113.1(12) . . ?
N4 C12 S2 123.5(12) . . ?
N5 C12 S2 123.4(12) . . ?
C13 C14 C15 120.1(14) . . ?
N1 C10 C11 112.8(11) . . ?
N4 C11 C10 112.5(10) . . ?
C18 C17 C16 121.0(16) . . ?
C17 C18 C13 121.1(15) . . ?
C5 C4 C9 119.3(14) . . ?
C5 C4 N3 118.1(16) . . ?
C9 C4 N3 122.5(16) . . ?
N1 C1 C2 111.5(11) . . ?
C4 C5 C6 120.7(16) . . ?
N2 C2 C1 111.0(10) . . ?
N2 C3 N3 115.1(11) . . ?
N2 C3 S1 121.3(12) . . ?
N3 C3 S1 123.5(10) . . ?
C8 C7 C6 119.8(18) . . ?
C7 C6 C5 118.0(16) . . ?
C4 C9 C8 120.7(16) . . ?
C27 C22 C23 119.5(15) . . ?
C27 C22 N7 117.7(16) . . ?
C23 C22 N7 122.8(16) . . ?
N6 C21 N7 113.3(11) . . ?
N6 C21 S3 123.0(11) . . ?
N7 C21 S3 123.5(11) . . ?
C25 C24 C23 121.4(19) . . ?
N6 C20 C19 112.5(10) . . ?
N1 C19 C20 110.9(10) . . ?
C22 C27 C26 120.0(16) . . ?
C24 C23 C22 118.2(16) . . ?
C25 C26 C27 120(2) . . ?
C30 N10 C31 127.6(15) . . ?
C46 N8 C28 111.2(12) . . ?
C46 N8 C37 112.9(13) . . ?
C28 N8 C37 112.4(13) . . ?
C30 N9 C29 127.0(15) . . ?
N10 C30 N9 114.6(15) . . ?
N10 C30 S4 125.7(14) . . ?
N9 C30 S4 119.5(16) . . ?
C32 C31 C36 122.3(17) . . ?
C32 C31 N10 119.1(19) . . ?
C36 C31 N10 118(2) . . ?
C31 C36 C35 117.3(17) . . ?
N8 C28 C29 113.3(12) . . ?
N13 C48 N14 113.3(11) . . ?
N13 C48 S6 122.6(11) . . ?
N14 C48 S6 124.1(11) . . ?
C54 C53 C52 120.4(13) . . ?
C51 C52 C53 119.3(15) . . ?
N13 C47 C46 111.5(12) . . ?
C52 C51 C50 121.5(14) . . ?
C49 C54 C53 120.2(13) . . ?
C51 C50 C49 118.5(13) . . ?
C54 C49 C50 120.0(13) . . ?
C54 C49 N14 119.3(13) . . ?
C50 C49 N14 120.4(13) . . ?
N8 C46 C47 113.0(12) . . ?
C48 N14 C49 127.4(10) . . ?
C48 N13 C47 124.9(11) . . ?
C38 C37 N8 110.6(13) . . ?
N11 C38 C37 114.4(14) . . ?
N11 C39 N12 115.4(14) . . ?
N11 C39 S5 121.3(15) . . ?
N12 C39 S5 123.3(14) . . ?
C39 N11 C38 128.6(15) . . ?
C39 N12 C40 132.5(13) . . ?
C44 C45 C40 119.6(16) . . ?
C45 C40 C41 119.5(15) . . ?
C45 C40 N12 122.7(18) . . ?
C41 C40 N12 117.8(16) . . ?
C44 C43 C42 118.8(16) . . ?
C41 C42 C43 119.5(15) . . ?
C42 C41 C40 120.3(15) . . ?
C45 C44 C43 122.2(16) . . ?
C68 N15 C64 112.2(9) . . ?
C68 N15 C60 105.2(10) . . ?
C64 N15 C60 112.0(9) . . ?
C68 N15 C56 109.8(10) . . ?
C64 N15 C56 106.4(8) . . ?
C60 N15 C56 111.3(9) . . ?
N15 C64 C65 116.7(9) . . ?
C67 C66 C65 113.0(11) . . ?
C64 C65 C66 111.7(9) . . ?
C61 C60 N15 117.5(10) . . ?
C63 C62 C61 115.6(15) . . ?
C60 C61 C62 112.6(13) . . ?
N15 C68 C69 115.9(12) . . ?
C71 C70 C69 104(2) . . ?
C68 C69 C70 105.1(15) . . ?
C57 C56 N15 115.8(10) . . ?
C76 N16 C84 106.8(8) . . ?
C76 N16 C72 110.5(8) . . ?
C84 N16 C72 110.0(8) . . ?
C76 N16 C80 111.1(9) . . ?
C84 N16 C80 111.6(8) . . ?
C72 N16 C80 106.9(9) . . ?
C87 C86 C85 112.9(16) . . ?
C84 C85 C86 107.7(11) . . ?
C85 C84 N16 115.4(9) . . ?
C81 C80 N16 116.1(10) . . ?
C81 C82 C83 114.0(14) . . ?
C73 C72 N16 116.7(10) . . ?
N16 C76 C77 114.8(9) . . ?
O3B C55 O2B 124(2) . . ?
O3A C55 O2A 118(3) . . ?
O3B C55 O1B 118.3(19) . . ?
O2B C55 O1B 112.7(16) . . ?
O3A C55 O1A 121(2) . . ?
O2A C55 O1A 107(2) . . ?
N9 C29 C28 112.4(12) . . ?
C32 C33 C34 125(2) . . ?
C33 C32 C31 117.9(19) . . ?
C35 C34 C33 117(2) . . ?
C59 C58 C57 115.5(18) . . ?
C58 C57 C56 111.3(12) . . ?
C72 C73 C74 110.5(12) . . ?
C75 C74 C73 113.3(13) . . ?
C79 C78 C77 113.6(15) . . ?
C76 C77 C78 110.3(11) . . ?
C17 C16 C15 118.1(16) . . ?
C82 C81 C80 109.8(11) . . ?
C26 C25 C24 121(2) . . ?
C7 C8 C9 121.4(17) . . ?
C34 C35 C36 120.2(19) . . ?

_refine_diff_density_max         0.252
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.032

####################################################################### 
# 
# 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-Ph-NCS-Ligand
_database_code_depnum_ccdc_archive 'CCDC 1589919'
_audit_update_record             
;
2017-12-08 deposited with the CCDC.
2018-05-29 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 H32 N7 S3, C27 H33 N7 S3'
_chemical_formula_sum            'C54 H65 N14 S6'
_chemical_formula_weight         1102.56

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

_cell_length_a                   25.9879(8)
_cell_length_b                   9.8507(3)
_cell_length_c                   26.8930(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6884.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4946
_cell_measurement_theta_min      3.4390
_cell_measurement_theta_max      24.8450

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_F_000             2332.0
_exptl_transmission_factor_min   0.933
_exptl_transmission_factor_max   0.955
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    0.240
_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            18835
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.005
_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 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.907
_reflns_number_total             10986
_reflns_number_gt                7701
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_max     0.811
_reflns_Friedel_fraction_full    0.811

_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+0.6495P] 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 2525 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10986
_refine_ls_number_parameters     631
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.2072
_refine_ls_wR_factor_gt          0.1910
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

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 0.3352(2) 0.7449(4) 0.6708(2) 0.060(2) Uani 1 1 d G . . . .
C23 C 0.3634(2) 0.7834(5) 0.7124(2) 0.079(3) Uani 1 1 d G . . . .
H23 H 0.3730 0.7188 0.7358 0.095 Uiso 1 1 calc R U . . .
C24 C 0.3772(2) 0.9185(6) 0.7190(2) 0.080(3) Uani 1 1 d G . . . .
H24 H 0.3961 0.9443 0.7468 0.096 Uiso 1 1 calc R U . . .
C25 C 0.3628(2) 1.0152(4) 0.6840(3) 0.079(3) Uani 1 1 d G . . . .
H25 H 0.3721 1.1056 0.6884 0.095 Uiso 1 1 calc R U . . .
C26 C 0.3346(3) 0.9766(5) 0.6424(3) 0.114(4) Uani 1 1 d G . . . .
H26 H 0.3250 1.0413 0.6190 0.137 Uiso 1 1 calc R U . . .
C27 C 0.3208(2) 0.8415(6) 0.6358(2) 0.097(3) Uani 1 1 d G . . . .
H27 H 0.3019 0.8157 0.6080 0.116 Uiso 1 1 calc R U . . .
C4 C 0.6799(2) 0.7982(5) 0.6424(2) 0.0579(19) Uani 1 1 d G . . . .
C9 C 0.7061(2) 0.9095(7) 0.6616(2) 0.083(3) Uani 1 1 d G . . . .
H9 H 0.7332 0.8966 0.6837 0.100 Uiso 1 1 calc R U . . .
C8 C 0.6919(4) 1.0401(5) 0.6476(3) 0.120(5) Uani 1 1 d G . . . .
H8 H 0.7094 1.1146 0.6605 0.144 Uiso 1 1 calc R U . . .
C7 C 0.6514(4) 1.0594(6) 0.6146(4) 0.139(6) Uani 1 1 d G . . . .
H7 H 0.6419 1.1467 0.6053 0.167 Uiso 1 1 calc R U . . .
C6 C 0.6252(3) 0.9480(10) 0.5954(3) 0.132(6) Uani 1 1 d G . . . .
H6 H 0.5982 0.9609 0.5733 0.159 Uiso 1 1 calc R U . . .
C5 C 0.6395(2) 0.8174(7) 0.6093(3) 0.095(3) Uani 1 1 d G . . . .
H5 H 0.6220 0.7429 0.5965 0.114 Uiso 1 1 calc R U . . .
C13 C 0.4787(3) -0.0080(8) 0.5555(2) 0.092(3) Uani 1 1 d G . . . .
C18 C 0.4439(3) 0.0964(10) 0.5646(3) 0.106(4) Uani 1 1 d G . . . .
H18 H 0.4280 0.1033 0.5954 0.128 Uiso 1 1 calc R U . . .
C17 C 0.4330(4) 0.1903(9) 0.5275(4) 0.168(7) Uani 1 1 d G . . . .
H17 H 0.4097 0.2602 0.5335 0.202 Uiso 1 1 calc R U . . .
C16 C 0.4568(4) 0.1800(10) 0.4814(4) 0.160(7) Uani 1 1 d G . . . .
H16 H 0.4495 0.2428 0.4566 0.192 Uiso 1 1 calc R U . . .
C15 C 0.4916(4) 0.0756(12) 0.4724(2) 0.128(5) Uani 1 1 d G . . . .
H15 H 0.5076 0.0687 0.4415 0.154 Uiso 1 1 calc R U . . .
C14 C 0.5025(3) -0.0184(9) 0.5094(3) 0.114(4) Uani 1 1 d G . . . .
H14 H 0.5258 -0.0882 0.5034 0.137 Uiso 1 1 calc R U . . .
S1 S 0.69515(7) 0.4128(2) 0.68865(10) 0.0679(6) Uani 1 1 d . . . . .
S6 S 0.05016(8) 0.3460(2) 0.32288(10) 0.0672(6) Uani 1 1 d . . . . .
S4 S 0.22700(9) -0.2444(2) 0.32361(10) 0.0736(6) Uani 1 1 d . . . . .
S5 S 0.41770(9) 0.3860(2) 0.36203(12) 0.0809(8) Uani 1 1 d . . . . .
S2 S 0.32759(8) 0.3473(2) 0.64267(11) 0.0736(7) Uani 1 1 d . . . . .
S3 S 0.50503(10) -0.2230(2) 0.67739(12) 0.0883(8) Uani 1 1 d . . . . .
N1 N 0.5170(2) 0.3169(6) 0.6711(2) 0.0550(16) Uani 1 1 d . . . . .
N3 N 0.6961(2) 0.6667(6) 0.6567(3) 0.0617(18) Uani 1 1 d . . . . .
H3N H 0.7283 0.6495 0.6524 0.074 Uiso 1 1 calc R U . . .
N9 N 0.2322(3) 0.0190(6) 0.3467(3) 0.0617(18) Uani 1 1 d . . . . .
H9N H 0.2410 0.0809 0.3676 0.074 Uiso 1 1 calc R U . . .
N13 N 0.3387(2) 0.5552(6) 0.3546(3) 0.0619(17) Uani 1 1 d . . . . .
H13N H 0.3274 0.6369 0.3518 0.074 Uiso 1 1 calc R U . . .
N11 N 0.1251(2) 0.5308(6) 0.3189(3) 0.0601(17) Uani 1 1 d . . . . .
H11N H 0.1355 0.6127 0.3233 0.072 Uiso 1 1 calc R U . . .
N8 N 0.2392(2) 0.2939(6) 0.3250(2) 0.0516(14) Uani 1 1 d . . . . .
N7 N 0.3204(2) 0.6071(6) 0.6634(3) 0.081(3) Uani 1 1 d . . . . .
H6N H 0.2884 0.5876 0.6676 0.097 Uiso 1 1 calc R U . . .
N14 N 0.4182(2) 0.6458(6) 0.3404(2) 0.0563(17) Uani 1 1 d . . . . .
H14N H 0.4508 0.6314 0.3404 0.068 Uiso 1 1 calc R U . . .
N10 N 0.2551(3) -0.1271(8) 0.4071(3) 0.079(2) Uani 1 1 d . . . . .
H10N H 0.2578 -0.2104 0.4163 0.095 Uiso 1 1 calc R U . . .
N2 N 0.6183(2) 0.5899(6) 0.6868(3) 0.0608(16) Uani 1 1 d . . . . .
H2N H 0.6075 0.6718 0.6828 0.073 Uiso 1 1 calc R U . . .
C30 C 0.2389(3) -0.1083(8) 0.3612(3) 0.0557(19) Uani 1 1 d . . . . .
N12 N 0.0482(2) 0.6051(6) 0.3493(3) 0.0648(19) Uani 1 1 d . . . . .
H12N H 0.0167 0.5872 0.3565 0.078 Uiso 1 1 calc R U . . .
C51 C 0.3534(3) 0.9422(9) 0.2834(3) 0.060(2) Uani 1 1 d . . . . .
H51 H 0.3270 0.9614 0.2611 0.073 Uiso 1 1 calc R U . . .
C50 C 0.3653(3) 0.8099(9) 0.2945(3) 0.0558(19) Uani 1 1 d . . . . .
H50 H 0.3479 0.7397 0.2787 0.067 Uiso 1 1 calc R U . . .
N6 N 0.4023(2) 0.5335(6) 0.6474(3) 0.0615(17) Uani 1 1 d . . . . .
H7N H 0.4112 0.6167 0.6520 0.074 Uiso 1 1 calc R U . . .
N5 N 0.4885(3) -0.1068(8) 0.5918(3) 0.082(2) Uani 1 1 d . . . . .
H5N H 0.4880 -0.1895 0.5815 0.099 Uiso 1 1 calc R U . . .
N4 N 0.5025(3) 0.0396(7) 0.6546(2) 0.0659(19) Uani 1 1 d . . . . .
H4N H 0.5030 0.1004 0.6316 0.079 Uiso 1 1 calc R U . . .
C1 C 0.5590(3) 0.4101(8) 0.6593(3) 0.059(2) Uani 1 1 d . . . . .
H1A H 0.5468 0.4747 0.6348 0.071 Uiso 1 1 calc R U . . .
H1B H 0.5866 0.3584 0.6440 0.071 Uiso 1 1 calc R U . . .
C3 C 0.6680(3) 0.5644(8) 0.6763(3) 0.0539(18) Uani 1 1 d . . . . .
C47 C 0.3007(3) 0.4509(9) 0.3631(3) 0.068(2) Uani 1 1 d . . . . .
H47A H 0.2723 0.4890 0.3820 0.082 Uiso 1 1 calc R U . . .
H47B H 0.3159 0.3790 0.3829 0.082 Uiso 1 1 calc R U . . .
C19 C 0.4687(3) 0.3878(7) 0.6837(3) 0.0518(17) Uani 1 1 d . . . . .
H19A H 0.4762 0.4637 0.7054 0.062 Uiso 1 1 calc R U . . .
H19B H 0.4460 0.3262 0.7012 0.062 Uiso 1 1 calc R U . . .
C28 C 0.2365(3) 0.1926(8) 0.2849(3) 0.062(2) Uani 1 1 d . . . . .
H28A H 0.2179 0.2314 0.2571 0.075 Uiso 1 1 calc R U . . .
H28B H 0.2712 0.1726 0.2737 0.075 Uiso 1 1 calc R U . . .
C38 C 0.1627(3) 0.4314(8) 0.2988(3) 0.060(2) Uani 1 1 d . . . . .
H38A H 0.1447 0.3665 0.2779 0.072 Uiso 1 1 calc R U . . .
H38B H 0.1875 0.4788 0.2782 0.072 Uiso 1 1 calc R U . . .
C48 C 0.3892(3) 0.5387(7) 0.3508(3) 0.0521(18) Uani 1 1 d . . . . .
C2 C 0.5818(3) 0.4908(8) 0.7041(3) 0.0562(19) Uani 1 1 d . . . . .
H2A H 0.5542 0.5360 0.7219 0.067 Uiso 1 1 calc R U . . .
H2B H 0.5986 0.4286 0.7268 0.067 Uiso 1 1 calc R U . . .
C46 C 0.2804(3) 0.3920(7) 0.3158(3) 0.0558(19) Uani 1 1 d . . . . .
H46A H 0.2674 0.4646 0.2949 0.067 Uiso 1 1 calc R U . . .
H46B H 0.3082 0.3476 0.2981 0.067 Uiso 1 1 calc R U . . .
C43 C 0.0922(4) 1.0052(10) 0.3753(5) 0.090(3) Uani 1 1 d . . . . .
H43 H 0.1018 1.0949 0.3807 0.109 Uiso 1 1 calc R U . . .
C49 C 0.4031(3) 0.7803(7) 0.3292(3) 0.0503(17) Uani 1 1 d . . . . .
C52 C 0.3799(3) 1.0451(9) 0.3050(4) 0.078(3) Uani 1 1 d . . . . .
H52 H 0.3730 1.1343 0.2959 0.093 Uiso 1 1 calc R U . . .
C31 C 0.2683(3) -0.0307(10) 0.4428(3) 0.066(2) Uani 1 1 d . . . . .
C39 C 0.0765(3) 0.5027(7) 0.3307(3) 0.056(2) Uani 1 1 d . . . . .
C37 C 0.1901(3) 0.3579(8) 0.3387(3) 0.0531(19) Uani 1 1 d . . . . .
H37A H 0.1966 0.4211 0.3656 0.064 Uiso 1 1 calc R U . . .
H37B H 0.1674 0.2879 0.3514 0.064 Uiso 1 1 calc R U . . .
C12 C 0.4984(3) -0.0895(8) 0.6399(4) 0.064(2) Uani 1 1 d . . . . .
C40 C 0.0653(3) 0.7402(7) 0.3582(3) 0.0559(19) Uani 1 1 d . . . . .
C21 C 0.3520(3) 0.5044(8) 0.6506(3) 0.060(2) Uani 1 1 d . . . . .
C53 C 0.4175(3) 1.0180(8) 0.3406(4) 0.075(3) Uani 1 1 d . . . . .
H53 H 0.4348 1.0885 0.3564 0.090 Uiso 1 1 calc R U . . .
C44 C 0.0572(4) 0.9743(10) 0.3404(4) 0.081(3) Uani 1 1 d . . . . .
H44 H 0.0419 1.0439 0.3222 0.098 Uiso 1 1 calc R U . . .
C29 C 0.2116(4) 0.0657(9) 0.2995(3) 0.073(2) Uani 1 1 d . . . . .
H29A H 0.1748 0.0798 0.3025 0.087 Uiso 1 1 calc R U . . .
H29B H 0.2174 -0.0027 0.2741 0.087 Uiso 1 1 calc R U . . .
C10 C 0.5334(4) 0.2134(8) 0.7083(3) 0.067(2) Uani 1 1 d . . . . .
H10A H 0.5699 0.1963 0.7041 0.081 Uiso 1 1 calc R U . . .
H10B H 0.5285 0.2504 0.7414 0.081 Uiso 1 1 calc R U . . .
C11 C 0.5062(4) 0.0862(11) 0.7048(4) 0.093(3) Uani 1 1 d . . . . .
H11 H 0.4927 0.0400 0.7319 0.112 Uiso 1 1 calc R U . . .
C36 C 0.3037(4) 0.0626(14) 0.4326(4) 0.103(4) Uani 1 1 d . . . . .
H36 H 0.3206 0.0599 0.4022 0.124 Uiso 1 1 calc R U . . .
C20 C 0.4423(3) 0.4387(8) 0.6372(3) 0.059(2) Uani 1 1 d . . . . .
H20A H 0.4676 0.4814 0.6159 0.071 Uiso 1 1 calc R U . . .
H20B H 0.4279 0.3620 0.6194 0.071 Uiso 1 1 calc R U . . .
C42 C 0.1144(4) 0.8998(13) 0.4037(4) 0.095(3) Uani 1 1 d . . . . .
H42 H 0.1377 0.9195 0.4289 0.114 Uiso 1 1 calc R U . . .
C54 C 0.4284(3) 0.8860(8) 0.3519(3) 0.064(2) Uani 1 1 d . . . . .
H54 H 0.4535 0.8672 0.3756 0.077 Uiso 1 1 calc R U . . .
C41 C 0.1009(3) 0.7663(10) 0.3935(4) 0.082(3) Uani 1 1 d . . . . .
H41 H 0.1163 0.6954 0.4109 0.099 Uiso 1 1 calc R U . . .
C45 C 0.0434(3) 0.8437(8) 0.3309(4) 0.071(2) Uani 1 1 d . . . . .
H45 H 0.0194 0.8242 0.3063 0.085 Uiso 1 1 calc R U . . .
C32 C 0.2452(4) -0.0338(12) 0.4888(4) 0.090(3) Uani 1 1 d . . . . .
H32 H 0.2216 -0.1028 0.4948 0.108 Uiso 1 1 calc R U . . .
C33 C 0.2538(6) 0.0533(19) 0.5253(5) 0.130(5) Uani 1 1 d . . . . .
H33 H 0.2370 0.0467 0.5557 0.156 Uiso 1 1 calc R U . . .
C35 C 0.3162(5) 0.1654(17) 0.4670(5) 0.140(6) Uani 1 1 d . . . . .
H35 H 0.3394 0.2347 0.4599 0.168 Uiso 1 1 calc R U . . .
C34 C 0.2889(9) 0.154(2) 0.5160(5) 0.186(9) Uani 1 1 d . . . . .
H34 H 0.2960 0.2167 0.5408 0.223 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
C22 C23 1.3900 . ?
C22 C27 1.3900 . ?
C22 N7 1.425(8) . ?
C23 C24 1.3900 . ?
C23 H23 0.9300 . ?
C24 C25 1.3900 . ?
C24 H24 0.9300 . ?
C25 C26 1.3900 . ?
C25 H25 0.9300 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C4 C9 1.3900 . ?
C4 C5 1.3900 . ?
C4 N3 1.415(8) . ?
C9 C8 1.3900 . ?
C9 H9 0.9300 . ?
C8 C7 1.3900 . ?
C8 H8 0.9300 . ?
C7 C6 1.3900 . ?
C7 H7 0.9300 . ?
C6 C5 1.3900 . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
C13 C18 1.3900 . ?
C13 C14 1.3900 . ?
C13 N5 1.400(10) . ?
C18 C17 1.3900 . ?
C18 H18 0.9300 . ?
C17 C16 1.3900 . ?
C17 H17 0.9300 . ?
C16 C15 1.3900 . ?
C16 H16 0.9300 . ?
C15 C14 1.3900 . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
S1 C3 1.685(8) . ?
S6 C39 1.701(8) . ?
S4 C30 1.707(8) . ?
S5 C48 1.704(7) . ?
S2 C21 1.685(8) . ?
S3 C12 1.666(9) . ?
N1 C1 1.462(9) . ?
N1 C19 1.475(9) . ?
N1 C10 1.491(10) . ?
N3 C3 1.352(9) . ?
N3 H3N 0.8600 . ?
N9 C30 1.324(10) . ?
N9 C29 1.454(10) . ?
N9 H9N 0.8600 . ?
N13 C48 1.325(9) . ?
N13 C47 1.443(9) . ?
N13 H13N 0.8600 . ?
N11 C39 1.331(9) . ?
N11 C38 1.485(9) . ?
N11 H11N 0.8600 . ?
N8 C46 1.462(9) . ?
N8 C37 1.470(9) . ?
N8 C28 1.471(10) . ?
N7 C21 1.347(10) . ?
N7 H6N 0.8600 . ?
N14 C48 1.327(9) . ?
N14 C49 1.413(9) . ?
N14 H14N 0.8600 . ?
N10 C30 1.317(10) . ?
N10 C31 1.393(12) . ?
N10 H10N 0.8600 . ?
N2 C3 1.346(9) . ?
N2 C2 1.439(9) . ?
N2 H2N 0.8600 . ?
N12 C39 1.345(10) . ?
N12 C40 1.423(9) . ?
N12 H12N 0.8600 . ?
C51 C52 1.356(12) . ?
C51 C50 1.372(11) . ?
C51 H51 0.9300 . ?
C50 C49 1.386(10) . ?
C50 H50 0.9300 . ?
N6 C21 1.343(9) . ?
N6 C20 1.423(9) . ?
N6 H7N 0.8600 . ?
N5 C12 1.332(12) . ?
N5 H5N 0.8600 . ?
N4 C12 1.335(10) . ?
N4 C11 1.430(12) . ?
N4 H4N 0.8600 . ?
C1 C2 1.560(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C47 C46 1.494(12) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C19 C20 1.510(11) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C28 C29 1.462(11) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C38 C37 1.479(11) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C43 C44 1.344(14) . ?
C43 C42 1.410(16) . ?
C43 H43 0.9300 . ?
C49 C54 1.374(10) . ?
C52 C53 1.393(12) . ?
C52 H52 0.9300 . ?
C31 C36 1.329(13) . ?
C31 C32 1.376(13) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C40 C41 1.351(12) . ?
C40 C45 1.378(12) . ?
C53 C54 1.364(11) . ?
C53 H53 0.9300 . ?
C44 C45 1.359(13) . ?
C44 H44 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C10 C11 1.443(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11 0.9300 . ?
C36 C35 1.409(19) . ?
C36 H36 0.9300 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C42 C41 1.388(14) . ?
C42 H42 0.9300 . ?
C54 H54 0.9300 . ?
C41 H41 0.9300 . ?
C45 H45 0.9300 . ?
C32 C33 1.323(17) . ?
C32 H32 0.9300 . ?
C33 C34 1.37(2) . ?
C33 H33 0.9300 . ?
C35 C34 1.50(2) . ?
C35 H35 0.9300 . ?
C34 H34 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
C23 C22 C27 120.0 . . ?
C23 C22 N7 121.0(5) . . ?
C27 C22 N7 119.0(5) . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C22 120.0 . . ?
C26 C27 H27 120.0 . . ?
C22 C27 H27 120.0 . . ?
C9 C4 C5 120.0 . . ?
C9 C4 N3 118.4(5) . . ?
C5 C4 N3 121.6(5) . . ?
C8 C9 C4 120.0 . . ?
C8 C9 H9 120.0 . . ?
C4 C9 H9 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C18 C13 C14 120.0 . . ?
C18 C13 N5 120.7(7) . . ?
C14 C13 N5 119.2(7) . . ?
C13 C18 C17 120.0 . . ?
C13 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C1 N1 C19 112.8(6) . . ?
C1 N1 C10 111.1(6) . . ?
C19 N1 C10 114.4(6) . . ?
C3 N3 C4 128.8(6) . . ?
C3 N3 H3N 115.6 . . ?
C4 N3 H3N 115.6 . . ?
C30 N9 C29 127.2(7) . . ?
C30 N9 H9N 116.4 . . ?
C29 N9 H9N 116.4 . . ?
C48 N13 C47 127.0(6) . . ?
C48 N13 H13N 116.5 . . ?
C47 N13 H13N 116.5 . . ?
C39 N11 C38 125.0(6) . . ?
C39 N11 H11N 117.5 . . ?
C38 N11 H11N 117.5 . . ?
C46 N8 C37 113.2(6) . . ?
C46 N8 C28 111.1(6) . . ?
C37 N8 C28 115.7(6) . . ?
C21 N7 C22 125.9(6) . . ?
C21 N7 H6N 117.1 . . ?
C22 N7 H6N 117.1 . . ?
C48 N14 C49 129.3(6) . . ?
C48 N14 H14N 115.4 . . ?
C49 N14 H14N 115.4 . . ?
C30 N10 C31 129.0(8) . . ?
C30 N10 H10N 115.5 . . ?
C31 N10 H10N 115.5 . . ?
C3 N2 C2 125.0(6) . . ?
C3 N2 H2N 117.5 . . ?
C2 N2 H2N 117.5 . . ?
N10 C30 N9 116.7(8) . . ?
N10 C30 S4 120.2(7) . . ?
N9 C30 S4 123.1(6) . . ?
C39 N12 C40 126.4(6) . . ?
C39 N12 H12N 116.8 . . ?
C40 N12 H12N 116.8 . . ?
C52 C51 C50 120.1(8) . . ?
C52 C51 H51 119.9 . . ?
C50 C51 H51 119.9 . . ?
C51 C50 C49 120.4(8) . . ?
C51 C50 H50 119.8 . . ?
C49 C50 H50 119.8 . . ?
C21 N6 C20 125.7(7) . . ?
C21 N6 H7N 117.1 . . ?
C20 N6 H7N 117.1 . . ?
C12 N5 C13 128.5(7) . . ?
C12 N5 H5N 115.7 . . ?
C13 N5 H5N 115.8 . . ?
C12 N4 C11 126.1(8) . . ?
C12 N4 H4N 116.9 . . ?
C11 N4 H4N 116.9 . . ?
N1 C1 C2 115.8(6) . . ?
N1 C1 H1A 108.3 . . ?
C2 C1 H1A 108.3 . . ?
N1 C1 H1B 108.3 . . ?
C2 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
N2 C3 N3 117.5(7) . . ?
N2 C3 S1 121.8(6) . . ?
N3 C3 S1 120.7(5) . . ?
N13 C47 C46 112.6(7) . . ?
N13 C47 H47A 109.1 . . ?
C46 C47 H47A 109.1 . . ?
N13 C47 H47B 109.1 . . ?
C46 C47 H47B 109.1 . . ?
H47A C47 H47B 107.8 . . ?
N1 C19 C20 110.8(6) . . ?
N1 C19 H19A 109.5 . . ?
C20 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C29 C28 N8 113.9(7) . . ?
C29 C28 H28A 108.8 . . ?
N8 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
N8 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C37 C38 N11 112.0(7) . . ?
C37 C38 H38A 109.2 . . ?
N11 C38 H38A 109.2 . . ?
C37 C38 H38B 109.2 . . ?
N11 C38 H38B 109.2 . . ?
H38A C38 H38B 107.9 . . ?
N13 C48 N14 118.8(6) . . ?
N13 C48 S5 121.7(6) . . ?
N14 C48 S5 119.5(5) . . ?
N2 C2 C1 110.2(6) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N8 C46 C47 111.8(6) . . ?
N8 C46 H46A 109.3 . . ?
C47 C46 H46A 109.3 . . ?
N8 C46 H46B 109.3 . . ?
C47 C46 H46B 109.3 . . ?
H46A C46 H46B 107.9 . . ?
C44 C43 C42 119.2(9) . . ?
C44 C43 H43 120.4 . . ?
C42 C43 H43 120.4 . . ?
C54 C49 C50 118.5(7) . . ?
C54 C49 N14 119.0(7) . . ?
C50 C49 N14 122.5(7) . . ?
C51 C52 C53 120.5(8) . . ?
C51 C52 H52 119.8 . . ?
C53 C52 H52 119.8 . . ?
C36 C31 C32 120.1(10) . . ?
C36 C31 N10 120.1(9) . . ?
C32 C31 N10 119.8(9) . . ?
N11 C39 N12 116.8(6) . . ?
N11 C39 S6 122.7(6) . . ?
N12 C39 S6 120.5(6) . . ?
N8 C37 C38 116.5(6) . . ?
N8 C37 H37A 108.2 . . ?
C38 C37 H37A 108.2 . . ?
N8 C37 H37B 108.2 . . ?
C38 C37 H37B 108.2 . . ?
H37A C37 H37B 107.3 . . ?
N5 C12 N4 115.1(8) . . ?
N5 C12 S3 120.5(7) . . ?
N4 C12 S3 124.4(8) . . ?
C41 C40 C45 121.1(8) . . ?
C41 C40 N12 120.6(8) . . ?
C45 C40 N12 118.2(8) . . ?
N6 C21 N7 116.8(7) . . ?
N6 C21 S2 123.6(6) . . ?
N7 C21 S2 119.5(6) . . ?
C54 C53 C52 118.8(8) . . ?
C54 C53 H53 120.6 . . ?
C52 C53 H53 120.6 . . ?
C43 C44 C45 121.6(10) . . ?
C43 C44 H44 119.2 . . ?
C45 C44 H44 119.2 . . ?
N9 C29 C28 109.9(7) . . ?
N9 C29 H29A 109.7 . . ?
C28 C29 H29A 109.7 . . ?
N9 C29 H29B 109.7 . . ?
C28 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C11 C10 N1 114.1(7) . . ?
C11 C10 H10A 108.7 . . ?
N1 C10 H10A 108.7 . . ?
C11 C10 H10B 108.7 . . ?
N1 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
N4 C11 C10 111.9(8) . . ?
N4 C11 H11 124.0 . . ?
C10 C11 H11 124.0 . . ?
C31 C36 C35 121.5(10) . . ?
C31 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
N6 C20 C19 113.0(7) . . ?
N6 C20 H20A 109.0 . . ?
C19 C20 H20A 109.0 . . ?
N6 C20 H20B 109.0 . . ?
C19 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C41 C42 C43 119.2(10) . . ?
C41 C42 H42 120.4 . . ?
C43 C42 H42 120.4 . . ?
C53 C54 C49 121.6(8) . . ?
C53 C54 H54 119.2 . . ?
C49 C54 H54 119.2 . . ?
C40 C41 C42 119.4(10) . . ?
C40 C41 H41 120.3 . . ?
C42 C41 H41 120.3 . . ?
C44 C45 C40 119.4(9) . . ?
C44 C45 H45 120.3 . . ?
C40 C45 H45 120.3 . . ?
C33 C32 C31 125.4(12) . . ?
C33 C32 H32 117.3 . . ?
C31 C32 H32 117.3 . . ?
C32 C33 C34 116.5(14) . . ?
C32 C33 H33 121.8 . . ?
C34 C33 H33 121.8 . . ?
C36 C35 C34 114.2(13) . . ?
C36 C35 H35 122.9 . . ?
C34 C35 H35 122.9 . . ?
C33 C34 C35 122.1(15) . . ?
C33 C34 H34 118.9 . . ?
C35 C34 H34 118.9 . . ?

_refine_diff_density_max         0.423
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.071

# 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 0.618 0.500 0.001 804 98 ' '
2 0.896 0.500 0.501 804 97 ' '
_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-Ph-ncs-TBASO4
_database_code_depnum_ccdc_archive 'CCDC 1576494'
_audit_update_record             
;
2017-09-25 deposited with the CCDC.
2018-05-29 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 H33 N7 S3), 2(C16 H36 N), O4 S'
_chemical_formula_sum            'C86 H138 N16 O4 S7'
_chemical_formula_weight         1684.54

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'

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

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

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

_cell_length_a                   30.977(6)
_cell_length_b                   13.483(3)
_cell_length_c                   23.390(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9769(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6618
_cell_measurement_theta_min      3.5421
_cell_measurement_theta_max      22.0312

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_F_000             3640.0
_exptl_transmission_factor_min   0.928
_exptl_transmission_factor_max   0.954
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    0.215
_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      296(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            78900
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.315
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             17114
_reflns_number_gt                7514
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_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)+(0.1075P)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_abs_structure_details 
;
 Flack x determined using 2520 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.43(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         17114
_refine_ls_number_parameters     1062
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1776
_refine_ls_R_factor_gt           0.0662
_refine_ls_wR_factor_ref         0.2066
_refine_ls_wR_factor_gt          0.1530
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.902
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001

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
S7 S 0.37333(8) 0.97841(18) 0.14487(9) 0.0592(6) Uani 1 1 d . . . . .
N1 N 0.7563(2) 0.8484(7) 0.6279(4) 0.083(2) Uani 1 1 d . . . . .
C1 C 0.7647(3) 0.7979(10) 0.6819(5) 0.107(4) Uani 1 1 d . . . . .
H1A H 0.7956 0.7898 0.6867 0.128 Uiso 1 1 calc R U . . .
H1B H 0.7517 0.7325 0.6808 0.128 Uiso 1 1 calc R U . . .
C2 C 0.7470(3) 0.8543(10) 0.7317(5) 0.103(4) Uani 1 1 d . . . . .
H2A H 0.7579 0.8255 0.7669 0.123 Uiso 1 1 calc R U . . .
H2B H 0.7569 0.9225 0.7299 0.123 Uiso 1 1 calc R U . . .
N3 N 0.6323(3) 0.8039(6) 0.7562(3) 0.075(2) Uani 1 1 d . . . . .
H3N H 0.6250 0.8459 0.7303 0.090 Uiso 1 1 calc R U . . .
N2 N 0.6999(3) 0.8528(7) 0.7328(3) 0.084(2) Uani 1 1 d . . . . .
H2N H 0.6868 0.8941 0.7108 0.101 Uiso 1 1 calc R U . . .
C3 C 0.6755(4) 0.7935(7) 0.7646(4) 0.074(3) Uani 1 1 d . . . . .
C5 C 0.5631(4) 0.8121(8) 0.7998(5) 0.088(3) Uani 1 1 d . . . . .
H5 H 0.5639 0.8804 0.7944 0.106 Uiso 1 1 calc R U . . .
C8 C 0.5602(4) 0.6110(9) 0.8153(4) 0.096(3) Uani 1 1 d . . . . .
H8 H 0.5595 0.5426 0.8206 0.115 Uiso 1 1 calc R U . . .
C7 C 0.5249(4) 0.6684(12) 0.8318(5) 0.104(4) Uani 1 1 d . . . . .
H7 H 0.5007 0.6387 0.8480 0.125 Uiso 1 1 calc R U . . .
C6 C 0.5261(4) 0.7678(11) 0.8239(6) 0.108(4) Uani 1 1 d . . . . .
H6 H 0.5027 0.8068 0.8345 0.130 Uiso 1 1 calc R U . . .
C9 C 0.5965(4) 0.6548(8) 0.7910(4) 0.082(3) Uani 1 1 d . . . . .
H9 H 0.6198 0.6160 0.7795 0.098 Uiso 1 1 calc R U . . .
C4 C 0.5977(3) 0.7551(8) 0.7842(4) 0.068(3) Uani 1 1 d . . . . .
C10 C 0.7911(3) 0.9174(10) 0.6154(7) 0.126(5) Uani 1 1 d . . . . .
H10A H 0.8026 0.9413 0.6514 0.151 Uiso 1 1 calc R U . . .
H10B H 0.8140 0.8810 0.5965 0.151 Uiso 1 1 calc R U . . .
C11 C 0.7808(5) 1.0014(10) 0.5810(7) 0.134(5) Uani 1 1 d . . . . .
H11A H 0.7705 0.9787 0.5441 0.161 Uiso 1 1 calc R U . . .
H11B H 0.8069 1.0397 0.5746 0.161 Uiso 1 1 calc R U . . .
N5 N 0.7191(3) 1.2026(7) 0.6448(4) 0.088(3) Uani 1 1 d . . . . .
H5N H 0.6988 1.1627 0.6546 0.106 Uiso 1 1 calc R U . . .
N4 N 0.7485(3) 1.0649(8) 0.6063(4) 0.101(3) Uani 1 1 d . . . . .
H4N H 0.7235 1.0394 0.6127 0.122 Uiso 1 1 calc R U . . .
C12 C 0.7541(3) 1.1598(10) 0.6205(5) 0.091(3) Uani 1 1 d . . . . .
S2 S 0.80180(9) 1.2199(3) 0.61099(17) 0.1189(12) Uani 1 1 d . . . . .
C15 C 0.7052(5) 1.4701(10) 0.6286(7) 0.112(4) Uani 1 1 d . . . . .
H15 H 0.7100 1.5194 0.6016 0.134 Uiso 1 1 calc R U . . .
C13 C 0.7114(3) 1.3034(8) 0.6560(6) 0.080(3) Uani 1 1 d . . . . .
C18 C 0.6908(3) 1.3260(11) 0.7073(6) 0.106(4) Uani 1 1 d . . . . .
H18 H 0.6859 1.2769 0.7344 0.127 Uiso 1 1 calc R U . . .
C17 C 0.6777(4) 1.4230(13) 0.7172(7) 0.115(4) Uani 1 1 d . . . . .
H17 H 0.6635 1.4387 0.7511 0.138 Uiso 1 1 calc R U . . .
C16 C 0.6853(4) 1.4938(11) 0.6789(8) 0.116(4) Uani 1 1 d . . . . .
H16 H 0.6771 1.5590 0.6863 0.140 Uiso 1 1 calc R U . . .
C14 C 0.7183(4) 1.3741(10) 0.6171(6) 0.100(3) Uani 1 1 d . . . . .
H14 H 0.7317 1.3590 0.5827 0.120 Uiso 1 1 calc R U . . .
C27 C 0.5877(3) 1.0167(8) 0.4536(4) 0.075(3) Uani 1 1 d . . . . .
H27 H 0.6007 1.0634 0.4772 0.090 Uiso 1 1 calc R U . . .
C23 C 0.5818(4) 0.8527(8) 0.4212(5) 0.093(3) Uani 1 1 d . . . . .
H23 H 0.5899 0.7864 0.4232 0.112 Uiso 1 1 calc R U . . .
C22 C 0.6005(3) 0.9202(8) 0.4558(4) 0.064(2) Uani 1 1 d . . . . .
C26 C 0.5553(4) 1.0458(8) 0.4163(4) 0.089(3) Uani 1 1 d . . . . .
H26 H 0.5464 1.1116 0.4153 0.107 Uiso 1 1 calc R U . . .
C24 C 0.5507(4) 0.8827(11) 0.3829(5) 0.116(4) Uani 1 1 d . . . . .
H24 H 0.5392 0.8365 0.3576 0.139 Uiso 1 1 calc R U . . .
C20 C 0.7083(4) 0.7367(8) 0.5721(6) 0.107(4) Uani 1 1 d . . . . .
H20A H 0.7088 0.6846 0.5435 0.129 Uiso 1 1 calc R U . . .
H20B H 0.6989 0.7072 0.6078 0.129 Uiso 1 1 calc R U . . .
C19 C 0.7519(5) 0.7748(10) 0.5794(6) 0.124(5) Uani 1 1 d . . . . .
H19A H 0.7609 0.8066 0.5441 0.148 Uiso 1 1 calc R U . . .
H19B H 0.7713 0.7196 0.5863 0.148 Uiso 1 1 calc R U . . .
N7 N 0.6312(2) 0.8970(6) 0.4989(3) 0.068(2) Uani 1 1 d . . . . .
H7N H 0.6317 0.9380 0.5270 0.082 Uiso 1 1 calc R U . . .
N6 N 0.6772(3) 0.8111(6) 0.5551(4) 0.083(2) Uani 1 1 d . . . . .
H6N H 0.6691 0.8526 0.5809 0.099 Uiso 1 1 calc R U . . .
C21 C 0.6598(3) 0.8215(7) 0.5031(4) 0.069(2) Uani 1 1 d . . . . .
S3 S 0.67342(11) 0.7455(2) 0.44850(12) 0.1027(9) Uani 1 1 d . . . . .
C25 C 0.5365(4) 0.9773(11) 0.3809(4) 0.100(4) Uani 1 1 d . . . . .
H25 H 0.5145 0.9956 0.3561 0.120 Uiso 1 1 calc R U . . .
N8 N 0.5044(2) 0.8025(6) 0.1683(3) 0.073(2) Uani 1 1 d . . . . .
C29 C 0.5221(4) 0.9544(9) 0.2219(5) 0.104(4) Uani 1 1 d . . . . .
H29A H 0.5075 0.9247 0.2544 0.125 Uiso 1 1 calc R U . . .
H29B H 0.5463 0.9925 0.2363 0.125 Uiso 1 1 calc R U . . .
C28 C 0.5386(3) 0.8742(9) 0.1840(5) 0.097(3) Uani 1 1 d . . . . .
H28A H 0.5503 0.9035 0.1494 0.116 Uiso 1 1 calc R U . . .
H28B H 0.5618 0.8393 0.2033 0.116 Uiso 1 1 calc R U . . .
N9 N 0.4922(2) 1.0211(7) 0.1929(3) 0.083(2) Uani 1 1 d . . . . .
H9N H 0.4666 0.9990 0.1865 0.100 Uiso 1 1 calc R U . . .
N10 N 0.4667(2) 1.1535(6) 0.1471(3) 0.074(2) Uani 1 1 d . . . . .
H10N H 0.4483 1.1115 0.1339 0.089 Uiso 1 1 calc R U . . .
C30 C 0.5008(3) 1.1131(8) 0.1753(4) 0.072(3) Uani 1 1 d . . . . .
S4 S 0.54899(8) 1.1672(2) 0.18428(14) 0.0987(9) Uani 1 1 d . . . . .
C33 C 0.4553(4) 1.4239(9) 0.1597(5) 0.094(3) Uani 1 1 d . . . . .
H33 H 0.4644 1.4752 0.1833 0.113 Uiso 1 1 calc R U . . .
C31 C 0.4569(3) 1.2536(7) 0.1361(4) 0.066(2) Uani 1 1 d . . . . .
C32 C 0.4696(3) 1.3286(8) 0.1709(4) 0.073(3) Uani 1 1 d . . . . .
H32 H 0.4876 1.3162 0.2019 0.088 Uiso 1 1 calc R U . . .
C36 C 0.4299(3) 1.2717(9) 0.0888(5) 0.082(3) Uani 1 1 d . . . . .
H36 H 0.4220 1.2204 0.0644 0.099 Uiso 1 1 calc R U . . .
C34 C 0.4282(4) 1.4452(10) 0.1148(6) 0.098(3) Uani 1 1 d . . . . .
H34 H 0.4187 1.5097 0.1083 0.118 Uiso 1 1 calc R U . . .
C35 C 0.4153(3) 1.3684(11) 0.0793(6) 0.105(4) Uani 1 1 d . . . . .
H35 H 0.3968 1.3813 0.0489 0.126 Uiso 1 1 calc R U . . .
C38 C 0.4966(3) 0.8207(8) 0.0644(4) 0.088(3) Uani 1 1 d . . . . .
H38A H 0.5046 0.8896 0.0702 0.106 Uiso 1 1 calc R U . . .
H38B H 0.5089 0.7990 0.0284 0.106 Uiso 1 1 calc R U . . .
C37 C 0.5151(3) 0.7584(8) 0.1126(4) 0.082(3) Uani 1 1 d . . . . .
H37A H 0.5034 0.6918 0.1106 0.098 Uiso 1 1 calc R U . . .
H37B H 0.5462 0.7541 0.1086 0.098 Uiso 1 1 calc R U . . .
N12 N 0.3834(3) 0.7557(6) 0.0361(3) 0.076(2) Uani 1 1 d . . . . .
H12N H 0.3748 0.7891 0.0653 0.091 Uiso 1 1 calc R U . . .
N11 N 0.4496(3) 0.8122(6) 0.0619(3) 0.079(2) Uani 1 1 d . . . . .
H11N H 0.4350 0.8493 0.0848 0.095 Uiso 1 1 calc R U . . .
C39 C 0.4267(4) 0.7521(7) 0.0272(4) 0.071(3) Uani 1 1 d . . . . .
C40 C 0.3509(4) 0.7105(9) 0.0028(4) 0.083(3) Uani 1 1 d . . . . .
C44 C 0.3177(7) 0.5689(15) -0.0416(8) 0.156(6) Uani 1 1 d . . . . .
H44 H 0.3182 0.5016 -0.0502 0.187 Uiso 1 1 calc R U . . .
C42 C 0.2816(5) 0.7212(19) -0.0449(9) 0.159(7) Uani 1 1 d . . . . .
H42 H 0.2578 0.7581 -0.0564 0.191 Uiso 1 1 calc R U . . .
C41 C 0.3162(4) 0.7655(10) -0.0128(6) 0.113(4) Uani 1 1 d . . . . .
H41 H 0.3147 0.8322 -0.0026 0.135 Uiso 1 1 calc R U . . .
C45 C 0.3522(4) 0.6122(11) -0.0109(6) 0.113(4) Uani 1 1 d . . . . .
H45 H 0.3757 0.5737 0.0000 0.136 Uiso 1 1 calc R U . . .
S5 S 0.45164(9) 0.6845(2) -0.02344(13) 0.0963(9) Uani 1 1 d . . . . .
N16 N 0.4487(2) 0.5822(6) 0.5042(3) 0.066(2) Uani 1 1 d . . . . .
C71 C 0.4947(2) 0.5644(7) 0.4829(4) 0.069(2) Uani 1 1 d . . . . .
H71A H 0.5140 0.6069 0.5046 0.083 Uiso 1 1 calc R U . . .
H71B H 0.5024 0.4963 0.4917 0.083 Uiso 1 1 calc R U . . .
C79 C 0.4172(3) 0.5118(9) 0.4763(4) 0.080(3) Uani 1 1 d . . . . .
H79A H 0.3884 0.5291 0.4891 0.097 Uiso 1 1 calc R U . . .
H79B H 0.4182 0.5232 0.4353 0.097 Uiso 1 1 calc R U . . .
C80 C 0.4236(3) 0.4039(9) 0.4864(5) 0.097(3) Uani 1 1 d . . . . .
H80A H 0.4252 0.3913 0.5272 0.117 Uiso 1 1 calc R U . . .
H80B H 0.4507 0.3829 0.4693 0.117 Uiso 1 1 calc R U . . .
C81 C 0.3863(4) 0.3440(10) 0.4604(5) 0.113(4) Uani 1 1 d . . . . .
H81A H 0.3596 0.3647 0.4783 0.136 Uiso 1 1 calc R U . . .
H81B H 0.3842 0.3598 0.4200 0.136 Uiso 1 1 calc R U . . .
C82 C 0.3907(6) 0.2350(13) 0.4667(8) 0.185(8) Uani 1 1 d . . . . .
H82A H 0.4164 0.2132 0.4475 0.278 Uiso 1 1 calc R U . . .
H82B H 0.3660 0.2029 0.4501 0.278 Uiso 1 1 calc R U . . .
H82C H 0.3925 0.2184 0.5065 0.278 Uiso 1 1 calc R U . . .
C72 C 0.5032(3) 0.5815(8) 0.4207(4) 0.081(3) Uani 1 1 d . . . . .
H72A H 0.4950 0.6488 0.4109 0.097 Uiso 1 1 calc R U . . .
H72B H 0.4855 0.5366 0.3983 0.097 Uiso 1 1 calc R U . . .
C73 C 0.5502(3) 0.5655(8) 0.4060(5) 0.094(3) Uani 1 1 d . . . . .
H73A H 0.5582 0.4983 0.4163 0.113 Uiso 1 1 calc R U . . .
H73B H 0.5677 0.6105 0.4285 0.113 Uiso 1 1 calc R U . . .
C74 C 0.5600(4) 0.5817(9) 0.3428(5) 0.118(4) Uani 1 1 d . . . . .
H74A H 0.5435 0.5358 0.3203 0.177 Uiso 1 1 calc R U . . .
H74B H 0.5903 0.5712 0.3361 0.177 Uiso 1 1 calc R U . . .
H74C H 0.5525 0.6483 0.3323 0.177 Uiso 1 1 calc R U . . .
C83 C 0.4504(3) 0.5668(8) 0.5689(4) 0.082(3) Uani 1 1 d . . . . .
H83A H 0.4609 0.5002 0.5763 0.098 Uiso 1 1 calc R U . . .
H83B H 0.4712 0.6128 0.5848 0.098 Uiso 1 1 calc R U . . .
C84 C 0.4080(3) 0.5801(11) 0.6002(4) 0.115(4) Uani 1 1 d . . . . .
H84A H 0.3864 0.5373 0.5832 0.138 Uiso 1 1 calc R U . . .
H84B H 0.3984 0.6482 0.5960 0.138 Uiso 1 1 calc R U . . .
C85 C 0.4126(6) 0.5555(19) 0.6636(6) 0.196(10) Uani 1 1 d . . . . .
H85A H 0.4422 0.5693 0.6746 0.235 Uiso 1 1 calc R U . . .
H85B H 0.3944 0.6013 0.6847 0.235 Uiso 1 1 calc R U . . .
C75 C 0.4328(3) 0.6831(8) 0.4898(4) 0.081(3) Uani 1 1 d . . . . .
H75A H 0.4041 0.6907 0.5056 0.097 Uiso 1 1 calc R U . . .
H75B H 0.4304 0.6881 0.4486 0.097 Uiso 1 1 calc R U . . .
O1A O 0.3727(5) 1.0883(10) 0.1461(7) 0.105(4) Uani 0.5 1 d . . P A 1
O2A O 0.3526(5) 0.9529(11) 0.0864(5) 0.097(4) Uani 0.5 1 d . . P A 1
O3A O 0.3380(5) 0.9487(13) 0.1880(6) 0.110(5) Uani 0.5 1 d . . P A 1
O4A O 0.4112(5) 0.9357(12) 0.1533(8) 0.118(5) Uani 0.5 1 d . . P A 1
O1B O 0.3707(3) 0.8698(6) 0.1416(4) 0.037(2) Uani 0.5 1 d . . P A 2
O2B O 0.3936(3) 1.0020(7) 0.2037(4) 0.044(2) Uani 0.5 1 d . . P A 2
O3B O 0.4072(3) 1.0090(7) 0.1018(4) 0.038(2) Uani 0.5 1 d . . P A 2
O4B O 0.3338(3) 1.0255(8) 0.1372(4) 0.052(3) Uani 0.5 1 d . . P A 2
C48 C 0.4039(3) 0.7708(8) 0.2818(4) 0.078(3) Uani 1 1 d . . . . .
N13 N 0.4191(3) 0.7635(6) 0.2282(4) 0.081(2) Uani 1 1 d . . . . .
H13N H 0.4095 0.8048 0.2032 0.097 Uiso 1 1 calc R U . . .
N14 N 0.3773(3) 0.8488(7) 0.2904(3) 0.083(2) Uani 1 1 d . . . . .
H14N H 0.3747 0.8890 0.2620 0.099 Uiso 1 1 calc R U . . .
C49 C 0.3534(3) 0.8730(9) 0.3393(4) 0.079(3) Uani 1 1 d . . . . .
C54 C 0.3486(4) 0.9712(11) 0.3521(6) 0.118(4) Uani 1 1 d . . . . .
H54 H 0.3629 1.0187 0.3304 0.142 Uiso 1 1 calc R U . . .
C46 C 0.4968(4) 0.7279(8) 0.2118(5) 0.096(4) Uani 1 1 d . . . . .
H46A H 0.5030 0.7555 0.2492 0.116 Uiso 1 1 calc R U . . .
H46B H 0.5161 0.6721 0.2056 0.116 Uiso 1 1 calc R U . . .
C47 C 0.4500(4) 0.6920(9) 0.2100(5) 0.101(3) Uani 1 1 d . . . . .
H47A H 0.4431 0.6723 0.1711 0.122 Uiso 1 1 calc R U . . .
H47B H 0.4473 0.6337 0.2340 0.122 Uiso 1 1 calc R U . . .
C52 C 0.3019(5) 0.9326(17) 0.4300(6) 0.149(6) Uani 1 1 d . . . . .
H52 H 0.2846 0.9520 0.4605 0.178 Uiso 1 1 calc R U . . .
C53 C 0.3223(5) 1.0009(12) 0.3975(8) 0.143(5) Uani 1 1 d . . . . .
H53 H 0.3188 1.0680 0.4054 0.171 Uiso 1 1 calc R U . . .
S1 S 0.69695(10) 0.7142(3) 0.81235(13) 0.1063(10) Uani 1 1 d . . . . .
C62 C 0.1271(6) 0.1690(10) 0.3175(7) 0.163(6) Uani 1 1 d . . . . .
H62A H 0.1228 0.1531 0.2779 0.244 Uiso 1 1 calc R U . . .
H62B H 0.1064 0.1337 0.3403 0.244 Uiso 1 1 calc R U . . .
H62C H 0.1557 0.1502 0.3288 0.244 Uiso 1 1 calc R U . . .
C76 C 0.4602(4) 0.7681(9) 0.5107(5) 0.099(3) Uani 1 1 d . . . . .
H76A H 0.4897 0.7601 0.4974 0.119 Uiso 1 1 calc R U . . .
H76B H 0.4606 0.7691 0.5522 0.119 Uiso 1 1 calc R U . . .
C77 C 0.4412(5) 0.8666(12) 0.4876(8) 0.149(6) Uani 1 1 d . . . . .
H77A H 0.4433 0.8670 0.4462 0.178 Uiso 1 1 calc R U . . .
H77B H 0.4108 0.8700 0.4975 0.178 Uiso 1 1 calc R U . . .
C43 C 0.2852(8) 0.623(2) -0.0578(10) 0.187(10) Uani 1 1 d . . . . .
H43 H 0.2634 0.5937 -0.0792 0.225 Uiso 1 1 calc R U . . .
C50 C 0.3311(5) 0.8074(10) 0.3720(6) 0.142(5) Uani 1 1 d . . . . .
H50 H 0.3325 0.7403 0.3629 0.170 Uiso 1 1 calc R U . . .
C51 C 0.3071(6) 0.8356(15) 0.4173(7) 0.174(8) Uani 1 1 d . . . . .
H51 H 0.2939 0.7878 0.4400 0.209 Uiso 1 1 calc R U . . .
C86 C 0.4036(8) 0.4689(17) 0.6805(10) 0.228(11) Uani 1 1 d . . . . .
H86A H 0.3987 0.4269 0.6481 0.342 Uiso 1 1 calc R U . . .
H86B H 0.3781 0.4709 0.7038 0.342 Uiso 1 1 calc R U . . .
H86C H 0.4273 0.4433 0.7026 0.342 Uiso 1 1 calc R U . . .
S6 S 0.41779(15) 0.6890(3) 0.33258(13) 0.1428(16) Uani 1 1 d . . . . .
C58 C 0.2910(6) 0.5594(17) 0.4084(10) 0.206(10) Uani 1 1 d . . . . .
H58A H 0.3042 0.5567 0.3714 0.309 Uiso 1 1 calc R U . . .
H58B H 0.3128 0.5542 0.4374 0.309 Uiso 1 1 calc R U . . .
H58C H 0.2759 0.6212 0.4126 0.309 Uiso 1 1 calc R U . . .
C78 C 0.4622(6) 0.9504(13) 0.5093(7) 0.176(7) Uani 1 1 d . . . . .
H78A H 0.4578 0.9540 0.5499 0.264 Uiso 1 1 calc R U . . .
H78B H 0.4506 1.0089 0.4916 0.264 Uiso 1 1 calc R U . . .
H78C H 0.4925 0.9459 0.5014 0.264 Uiso 1 1 calc R U . . .
N15 N 0.1819(2) 0.5185(6) 0.2853(3) 0.068(2) Uani 1 1 d . . . . .
C64 C 0.1968(3) 0.7064(8) 0.2837(5) 0.090(3) Uani 1 1 d . . . . .
H64A H 0.2205 0.7034 0.3107 0.108 Uiso 1 1 calc R U . . .
H64B H 0.2087 0.6993 0.2456 0.108 Uiso 1 1 calc R U . . .
C65 C 0.1751(4) 0.8042(9) 0.2886(5) 0.109(4) Uani 1 1 d . . . . .
H65A H 0.1610 0.8083 0.3256 0.131 Uiso 1 1 calc R U . . .
H65B H 0.1529 0.8087 0.2595 0.131 Uiso 1 1 calc R U . . .
C66 C 0.2056(5) 0.8921(10) 0.2822(8) 0.164(6) Uani 1 1 d . . . . .
H66A H 0.2302 0.8829 0.3066 0.246 Uiso 1 1 calc R U . . .
H66B H 0.1909 0.9520 0.2927 0.246 Uiso 1 1 calc R U . . .
H66C H 0.2151 0.8967 0.2432 0.246 Uiso 1 1 calc R U . . .
C63 C 0.1664(3) 0.6227(7) 0.2952(4) 0.077(3) Uani 1 1 d . . . . .
H63A H 0.1410 0.6328 0.2717 0.092 Uiso 1 1 calc R U . . .
H63B H 0.1573 0.6276 0.3347 0.092 Uiso 1 1 calc R U . . .
C68 C 0.1564(3) 0.5246(9) 0.1808(4) 0.087(3) Uani 1 1 d . . . . .
H68A H 0.1497 0.5949 0.1810 0.104 Uiso 1 1 calc R U . . .
H68B H 0.1307 0.4886 0.1923 0.104 Uiso 1 1 calc R U . . .
C67 C 0.1927(3) 0.5035(8) 0.2219(4) 0.079(3) Uani 1 1 d . . . . .
H67A H 0.2168 0.5461 0.2122 0.095 Uiso 1 1 calc R U . . .
H67B H 0.2019 0.4355 0.2164 0.095 Uiso 1 1 calc R U . . .
C69 C 0.1698(5) 0.4927(11) 0.1206(5) 0.132(5) Uani 1 1 d . . . . .
H69A H 0.1965 0.5264 0.1108 0.159 Uiso 1 1 calc R U . . .
H69B H 0.1757 0.4221 0.1211 0.159 Uiso 1 1 calc R U . . .
C70 C 0.1406(6) 0.5110(19) 0.0790(7) 0.235(11) Uani 1 1 d . . . . .
H70A H 0.1256 0.4508 0.0698 0.352 Uiso 1 1 calc R U . . .
H70B H 0.1552 0.5353 0.0456 0.352 Uiso 1 1 calc R U . . .
H70C H 0.1203 0.5598 0.0921 0.352 Uiso 1 1 calc R U . . .
C55 C 0.2241(3) 0.4998(8) 0.3186(5) 0.090(3) Uani 1 1 d . . . . .
H55A H 0.2358 0.4362 0.3071 0.109 Uiso 1 1 calc R U . . .
H55B H 0.2449 0.5504 0.3081 0.109 Uiso 1 1 calc R U . . .
C56 C 0.2189(4) 0.5002(11) 0.3837(5) 0.126(4) Uani 1 1 d . . . . .
H56A H 0.1986 0.4488 0.3948 0.151 Uiso 1 1 calc R U . . .
H56B H 0.2071 0.5636 0.3957 0.151 Uiso 1 1 calc R U . . .
C60 C 0.1553(3) 0.3390(8) 0.2973(5) 0.090(3) Uani 1 1 d . . . . .
H60A H 0.1558 0.3228 0.2569 0.108 Uiso 1 1 calc R U . . .
H60B H 0.1832 0.3228 0.3134 0.108 Uiso 1 1 calc R U . . .
C59 C 0.1466(3) 0.4484(7) 0.3046(4) 0.078(3) Uani 1 1 d . . . . .
H59A H 0.1410 0.4608 0.3448 0.094 Uiso 1 1 calc R U . . .
H59B H 0.1205 0.4646 0.2838 0.094 Uiso 1 1 calc R U . . .
C61 C 0.1212(4) 0.2798(10) 0.3262(5) 0.119(4) Uani 1 1 d . . . . .
H61A H 0.0932 0.2993 0.3115 0.143 Uiso 1 1 calc R U . . .
H61B H 0.1217 0.2942 0.3668 0.143 Uiso 1 1 calc R U . . .
C57 C 0.2624(6) 0.4825(13) 0.4139(7) 0.159(6) Uani 1 1 d . . . . .
H57A H 0.2571 0.4710 0.4542 0.191 Uiso 1 1 calc R U . . .
H57B H 0.2755 0.4230 0.3983 0.191 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
S7 O4A 1.323(15) . ?
S7 O4B 1.390(10) . ?
S7 O1B 1.468(8) . ?
S7 O1A 1.482(13) . ?
S7 O3B 1.512(8) . ?
S7 O3A 1.542(13) . ?
S7 O2B 1.544(9) . ?
S7 O2A 1.549(14) . ?
N1 C10 1.455(13) . ?
N1 C1 1.458(13) . ?
N1 C19 1.512(16) . ?
C1 C2 1.497(16) . ?
C2 N2 1.458(12) . ?
N3 C3 1.358(11) . ?
N3 C4 1.419(12) . ?
N2 C3 1.329(12) . ?
C3 S1 1.684(9) . ?
C5 C4 1.369(13) . ?
C5 C6 1.408(15) . ?
C8 C9 1.393(14) . ?
C8 C7 1.395(15) . ?
C7 C6 1.353(16) . ?
C9 C4 1.362(13) . ?
C10 C11 1.425(17) . ?
C11 N4 1.444(14) . ?
N5 C12 1.353(13) . ?
N5 C13 1.405(13) . ?
N4 C12 1.333(14) . ?
C12 S2 1.700(11) . ?
C15 C16 1.365(18) . ?
C15 C14 1.382(16) . ?
C13 C14 1.335(15) . ?
C13 C18 1.392(16) . ?
C18 C17 1.389(17) . ?
C17 C16 1.331(17) . ?
C27 C22 1.362(12) . ?
C27 C26 1.386(13) . ?
C23 C22 1.349(13) . ?
C23 C24 1.378(15) . ?
C22 N7 1.419(11) . ?
C26 C25 1.369(14) . ?
C24 C25 1.350(15) . ?
C20 N6 1.447(13) . ?
C20 C19 1.457(16) . ?
N7 C21 1.353(11) . ?
N6 C21 1.338(11) . ?
C21 S3 1.691(10) . ?
N8 C46 1.449(12) . ?
N8 C37 1.469(11) . ?
N8 C28 1.479(13) . ?
C29 N9 1.458(12) . ?
C29 C28 1.490(15) . ?
N9 C30 1.334(12) . ?
N10 C30 1.359(11) . ?
N10 C31 1.407(12) . ?
C30 S4 1.675(10) . ?
C33 C34 1.376(15) . ?
C33 C32 1.383(14) . ?
C31 C32 1.355(13) . ?
C31 C36 1.408(13) . ?
C36 C35 1.398(15) . ?
C34 C35 1.386(16) . ?
C38 N11 1.464(11) . ?
C38 C37 1.517(13) . ?
N12 C39 1.359(11) . ?
N12 C40 1.410(13) . ?
N11 C39 1.348(12) . ?
C39 S5 1.683(10) . ?
C40 C41 1.356(15) . ?
C40 C45 1.364(15) . ?
C44 C43 1.30(2) . ?
C44 C45 1.414(19) . ?
C42 C43 1.36(3) . ?
C42 C41 1.44(2) . ?
N16 C75 1.485(12) . ?
N16 C79 1.509(11) . ?
N16 C83 1.528(11) . ?
N16 C71 1.530(10) . ?
C71 C72 1.496(11) . ?
C79 C80 1.488(14) . ?
C80 C81 1.535(14) . ?
C81 C82 1.483(18) . ?
C72 C73 1.511(12) . ?
C73 C74 1.525(15) . ?
C83 C84 1.512(13) . ?
C84 C85 1.528(18) . ?
C85 C86 1.26(2) . ?
C75 C76 1.507(14) . ?
C48 N13 1.343(12) . ?
C48 N14 1.351(12) . ?
C48 S6 1.676(11) . ?
N13 C47 1.423(13) . ?
N14 C49 1.402(12) . ?
C49 C50 1.357(15) . ?
C49 C54 1.366(14) . ?
C54 C53 1.396(18) . ?
C46 C47 1.531(15) . ?
C52 C51 1.35(2) . ?
C52 C53 1.350(19) . ?
C62 C61 1.518(17) . ?
C76 C77 1.552(18) . ?
C77 C78 1.399(18) . ?
C50 C51 1.350(18) . ?
C58 C57 1.37(2) . ?
N15 C63 1.503(11) . ?
N15 C59 1.515(11) . ?
N15 C67 1.533(11) . ?
N15 C55 1.542(11) . ?
C64 C65 1.485(13) . ?
C64 C63 1.493(13) . ?
C65 C66 1.524(17) . ?
C68 C67 1.506(13) . ?
C68 C69 1.530(14) . ?
C69 C70 1.350(19) . ?
C55 C56 1.530(16) . ?
C56 C57 1.541(18) . ?
C60 C61 1.485(15) . ?
C60 C59 1.508(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4B S7 O1B 113.5(5) . . ?
O4A S7 O1A 116.4(9) . . ?
O4B S7 O3B 113.6(6) . . ?
O1B S7 O3B 106.0(5) . . ?
O4A S7 O3A 114.9(10) . . ?
O1A S7 O3A 103.7(9) . . ?
O4B S7 O2B 112.2(5) . . ?
O1B S7 O2B 106.0(5) . . ?
O3B S7 O2B 104.8(5) . . ?
O4A S7 O2A 113.8(9) . . ?
O1A S7 O2A 103.5(8) . . ?
O3A S7 O2A 102.9(7) . . ?
C10 N1 C1 109.9(9) . . ?
C10 N1 C19 109.6(10) . . ?
C1 N1 C19 111.1(9) . . ?
N1 C1 C2 111.9(9) . . ?
N2 C2 C1 111.9(9) . . ?
C3 N3 C4 129.1(8) . . ?
C3 N2 C2 125.9(9) . . ?
N2 C3 N3 114.7(8) . . ?
N2 C3 S1 122.0(8) . . ?
N3 C3 S1 123.3(8) . . ?
C4 C5 C6 120.4(10) . . ?
C9 C8 C7 120.7(11) . . ?
C6 C7 C8 119.3(11) . . ?
C7 C6 C5 119.9(11) . . ?
C4 C9 C8 119.4(10) . . ?
C9 C4 C5 120.3(10) . . ?
C9 C4 N3 122.3(9) . . ?
C5 C4 N3 117.1(9) . . ?
C11 C10 N1 117.2(10) . . ?
C10 C11 N4 113.3(12) . . ?
C12 N5 C13 128.9(9) . . ?
C12 N4 C11 125.5(10) . . ?
N4 C12 N5 114.2(9) . . ?
N4 C12 S2 122.6(10) . . ?
N5 C12 S2 123.2(10) . . ?
C16 C15 C14 121.4(13) . . ?
C14 C13 C18 120.2(12) . . ?
C14 C13 N5 122.4(12) . . ?
C18 C13 N5 116.8(12) . . ?
C17 C18 C13 119.0(13) . . ?
C16 C17 C18 120.7(14) . . ?
C17 C16 C15 119.4(13) . . ?
C13 C14 C15 119.3(13) . . ?
C22 C27 C26 120.4(9) . . ?
C22 C23 C24 119.6(11) . . ?
C23 C22 C27 119.8(9) . . ?
C23 C22 N7 124.4(9) . . ?
C27 C22 N7 115.7(9) . . ?
C25 C26 C27 119.8(10) . . ?
C25 C24 C23 121.8(11) . . ?
N6 C20 C19 113.9(10) . . ?
C20 C19 N1 113.7(10) . . ?
C21 N7 C22 131.0(8) . . ?
C21 N6 C20 126.2(9) . . ?
N6 C21 N7 114.2(8) . . ?
N6 C21 S3 121.5(8) . . ?
N7 C21 S3 124.3(8) . . ?
C24 C25 C26 118.6(11) . . ?
C46 N8 C37 112.2(8) . . ?
C46 N8 C28 113.4(8) . . ?
C37 N8 C28 108.8(8) . . ?
N9 C29 C28 112.8(9) . . ?
N8 C28 C29 112.1(9) . . ?
C30 N9 C29 126.3(8) . . ?
C30 N10 C31 129.8(8) . . ?
N9 C30 N10 111.6(8) . . ?
N9 C30 S4 122.9(8) . . ?
N10 C30 S4 125.4(8) . . ?
C34 C33 C32 122.3(11) . . ?
C32 C31 N10 123.0(9) . . ?
C32 C31 C36 120.9(10) . . ?
N10 C31 C36 115.9(9) . . ?
C31 C32 C33 119.2(10) . . ?
C35 C36 C31 118.6(11) . . ?
C33 C34 C35 118.4(12) . . ?
C34 C35 C36 120.6(12) . . ?
N11 C38 C37 111.3(8) . . ?
N8 C37 C38 110.5(7) . . ?
C39 N12 C40 127.1(9) . . ?
C39 N11 C38 126.5(8) . . ?
N11 C39 N12 113.9(8) . . ?
N11 C39 S5 120.5(8) . . ?
N12 C39 S5 125.5(8) . . ?
C41 C40 C45 119.5(12) . . ?
C41 C40 N12 118.5(11) . . ?
C45 C40 N12 121.9(12) . . ?
C43 C44 C45 120(2) . . ?
C43 C42 C41 117.3(17) . . ?
C40 C41 C42 120.2(14) . . ?
C40 C45 C44 119.9(14) . . ?
C75 N16 C79 105.3(7) . . ?
C75 N16 C83 111.1(7) . . ?
C79 N16 C83 111.4(7) . . ?
C75 N16 C71 112.2(7) . . ?
C79 N16 C71 111.2(7) . . ?
C83 N16 C71 105.6(6) . . ?
C72 C71 N16 117.1(7) . . ?
C80 C79 N16 117.4(7) . . ?
C79 C80 C81 110.6(9) . . ?
C82 C81 C80 114.3(11) . . ?
C71 C72 C73 111.6(8) . . ?
C72 C73 C74 113.2(10) . . ?
C84 C83 N16 115.7(8) . . ?
C83 C84 C85 111.4(11) . . ?
C86 C85 C84 119.0(19) . . ?
N16 C75 C76 115.9(8) . . ?
N13 C48 N14 114.1(9) . . ?
N13 C48 S6 121.5(9) . . ?
N14 C48 S6 124.3(8) . . ?
C48 N13 C47 124.4(9) . . ?
C48 N14 C49 128.6(9) . . ?
C50 C49 C54 117.0(11) . . ?
C50 C49 N14 125.2(11) . . ?
C54 C49 N14 117.5(11) . . ?
C49 C54 C53 120.5(13) . . ?
N8 C46 C47 110.7(9) . . ?
N13 C47 C46 114.5(9) . . ?
C51 C52 C53 118.7(14) . . ?
C52 C53 C54 120.3(14) . . ?
C75 C76 C77 108.8(10) . . ?
C78 C77 C76 112.8(15) . . ?
C44 C43 C42 123(2) . . ?
C51 C50 C49 122.5(14) . . ?
C52 C51 C50 120.8(15) . . ?
C63 N15 C59 107.9(7) . . ?
C63 N15 C67 109.9(7) . . ?
C59 N15 C67 111.3(7) . . ?
C63 N15 C55 110.2(7) . . ?
C59 N15 C55 111.1(7) . . ?
C67 N15 C55 106.5(7) . . ?
C65 C64 C63 111.8(9) . . ?
C64 C65 C66 113.6(11) . . ?
C64 C63 N15 118.5(8) . . ?
C67 C68 C69 109.4(9) . . ?
C68 C67 N15 115.6(7) . . ?
C70 C69 C68 115.5(13) . . ?
C56 C55 N15 114.3(8) . . ?
C55 C56 C57 111.2(11) . . ?
C61 C60 C59 110.4(9) . . ?
C60 C59 N15 116.6(8) . . ?
C60 C61 C62 112.6(11) . . ?
C58 C57 C56 113.9(16) . . ?

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.040

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

data_Tren-Ph-NCO-TBAF
_database_code_depnum_ccdc_archive 'CCDC 1576490'
_audit_update_record             
;
2017-09-25 deposited with the CCDC.
2018-05-29 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 H33 N7 O3, C16 H27 N, F, 3(H2 O)'
_chemical_formula_sum            'C43 H66 F N8 O6'
_chemical_formula_weight         810.02


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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.8500(10)
_cell_length_b                   13.8500(10)
_cell_length_c                   43.014(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7145.6(12)
_cell_formula_units_Z            6
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1617
_cell_measurement_theta_min      3.7240
_cell_measurement_theta_max      22.8370

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             2621.9
_exptl_transmission_factor_min   0.978
_exptl_transmission_factor_max   0.984
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    0.079
_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 and area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6282
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.941
_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             2816
_reflns_number_gt                1785
_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)+(0.1200P)²+9.9010P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2816
_refine_ls_number_parameters     214
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0821
_refine_ls_wR_factor_ref         0.2837
_refine_ls_wR_factor_gt          0.2513
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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
N3 N 0.4726(2) 0.3350(2) 0.42035(7) 0.0550(8) Uani 1 1 d . . . . .
H3N H 0.5350 0.3361 0.4185 0.066 Uiso 1 1 calc R U . . .
N1 N 0.6667 0.3333 0.51246(11) 0.0541(12) Uani 1 3 d S T P . .
O1 O 0.3575(2) 0.3489(3) 0.45588(7) 0.0772(9) Uani 1 1 d . . . . .
C4 C 0.4137(3) 0.3225(3) 0.39280(8) 0.0518(9) Uani 1 1 d . . . . .
C3 C 0.4426(3) 0.3456(3) 0.44962(9) 0.0560(9) Uani 1 1 d . . . . .
N2 N 0.5150(3) 0.3509(3) 0.47113(7) 0.0710(10) Uani 1 1 d . . . . .
H2N H 0.5733 0.3499 0.4647 0.085 Uiso 1 1 calc R U . . .
N4 N 0.0000 0.0000 0.59446(12) 0.0640(14) Uani 1 3 d DS T P . .
C9 C 0.3380(3) 0.3591(3) 0.38910(10) 0.0680(11) Uani 1 1 d . . . . .
H9 H 0.3231 0.3932 0.4056 0.082 Uiso 1 1 calc R U . . .
C5 C 0.4330(3) 0.2715(3) 0.36772(9) 0.0638(10) Uani 1 1 d . . . . .
H5 H 0.4835 0.2462 0.3698 0.077 Uiso 1 1 calc R U . . .
C11 C 0.1723(4) 0.1955(3) 0.58491(13) 0.0861(14) Uani 1 1 d . . . . .
H11A H 0.1334 0.2235 0.5724 0.103 Uiso 1 1 calc R U . . .
H11B H 0.1681 0.2136 0.6065 0.103 Uiso 1 1 calc R U . . .
C10 C 0.1175(3) 0.0708(3) 0.58118(13) 0.0836(14) Uani 1 1 d . . . . .
H10A H 0.1652 0.0467 0.5909 0.100 Uiso 1 1 calc R U . . .
H10B H 0.1145 0.0545 0.5591 0.100 Uiso 1 1 calc R U . . .
C12 C 0.2919(4) 0.2499(3) 0.57499(13) 0.0843(14) Uani 1 1 d . . . . .
H12A H 0.2953 0.2263 0.5540 0.101 Uiso 1 1 calc R U . . .
H12B H 0.3309 0.2246 0.5885 0.101 Uiso 1 1 calc R U . . .
C13 C 0.3503(4) 0.3747(4) 0.57592(14) 0.0993(16) Uani 1 1 d . . . . .
H13A H 0.3207 0.4011 0.5600 0.149 Uiso 1 1 calc R U . . .
H13B H 0.4286 0.4044 0.5725 0.149 Uiso 1 1 calc R U . . .
H13C H 0.3390 0.3985 0.5959 0.149 Uiso 1 1 calc R U . . .
C6 C 0.3788(4) 0.2577(4) 0.33989(10) 0.0773(12) Uani 1 1 d . . . . .
H6 H 0.3928 0.2234 0.3233 0.093 Uiso 1 1 calc R U . . .
C8 C 0.2845(4) 0.3452(4) 0.36100(12) 0.0849(14) Uani 1 1 d . . . . .
H8 H 0.2341 0.3705 0.3586 0.102 Uiso 1 1 calc R U . . .
C7 C 0.3046(4) 0.2945(4) 0.33658(12) 0.0874(14) Uani 1 1 d . . . . .
H7 H 0.2678 0.2851 0.3178 0.105 Uiso 1 1 calc R U . . .
C2 C 0.5033(4) 0.3579(5) 0.50398(10) 0.0922(16) Uani 1 1 d . . . . .
H2A H 0.5219 0.4336 0.5090 0.111 Uiso 1 1 calc R U . . .
H2B H 0.4257 0.3093 0.5094 0.111 Uiso 1 1 calc R U . . .
C16 C 0.0000 0.0000 0.6844(2) 0.141(5) Uani 1 3 d DS TU P . .
C1 C 0.5673(6) 0.3304(9) 0.52235(11) 0.160(4) Uani 1 1 d . . . . .
H1A H 0.5180 0.2550 0.5296 0.192 Uiso 1 1 calc R U . . .
H1B H 0.5873 0.3780 0.5405 0.192 Uiso 1 1 calc R U . . .
C14A C 0.0000 0.0000 0.63026(12) 0.127(14) Uani 0.4999 3 d DS TU P A 1
C15A C 0.058(2) -0.024(3) 0.65731(12) 0.17(2) Uani 0.1666 1 d D U P A 1
C15B C 0.030(2) -0.015(2) 0.6510(2) 0.059(9) Uani 0.1666 1 d D U P A 2
C14B C -0.0275(19) 0.020(2) 0.6267(2) 0.086(12) Uani 0.1666 1 d D U P A 2
C17 C 0.016(3) 0.0718(17) 0.7122(3) 0.170(10) Uani 0.333 1 d D . P A .
O2 O 0.1827(3) 0.1969(4) 0.49291(12) 0.1245(15) Uani 1 1 d D . . . .
F1 F 0.6667 0.3333 0.42750(8) 0.0543(9) Uani 1 3 d S T P . .
H2O H 0.233(3) 0.248(3) 0.4822(10) 0.16(3) Uiso 1 1 d D . . . .
H1O H 0.190(3) 0.1420(19) 0.4974(15) 0.17(3) Uiso 1 1 d 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
N3 C3 1.357(4) . ?
N3 C4 1.399(4) . ?
N1 C1 1.421(5) 3_665 ?
N1 C1 1.421(5) 2_655 ?
N1 C1 1.421(5) . ?
O1 C3 1.232(4) . ?
C4 C9 1.385(5) . ?
C4 C5 1.386(5) . ?
C3 N2 1.339(5) . ?
N2 C2 1.431(5) . ?
N4 C14B 1.5002(10) . ?
N4 C14B 1.5002(11) 3 ?
N4 C14B 1.5002(10) 2 ?
N4 C10 1.530(5) 3 ?
N4 C10 1.530(4) 2 ?
N4 C10 1.530(5) . ?
N4 C14A 1.5401(10) . ?
C9 C8 1.380(6) . ?
C5 C6 1.374(5) . ?
C11 C12 1.498(6) . ?
C11 C10 1.508(6) . ?
C12 C13 1.498(6) . ?
C6 C7 1.363(6) . ?
C8 C7 1.367(7) . ?
C2 C1 1.376(6) . ?
C16 C17 1.4997(11) . ?
C16 C17 1.4997(10) 3 ?
C16 C17 1.4997(11) 2 ?
C16 C15A 1.5399(11) 2 ?
C16 C15B 1.5399(11) 3 ?
C16 C15A 1.5399(11) 3 ?
C16 C15B 1.5399(11) 2 ?
C16 C15B 1.5400(10) . ?
C16 C15A 1.5400(11) . ?
C14A C15A 1.5398(11) . ?
C14A C15A 1.5399(11) 2 ?
C14A C15A 1.5399(11) 3 ?
C15A C15A 1.747(10) 2 ?
C15A C15A 1.747(10) 3 ?
C15B C15B 0.96(3) 3 ?
C15B C15B 0.96(3) 2 ?
C15B C14B 1.165(16) 3 ?
C15B C14B 1.215(19) 2 ?
C15B C14B 1.5399(10) . ?
C14B C14B 1.00(3) 2 ?
C14B C14B 1.00(3) 3 ?
C14B C15B 1.165(16) 2 ?
C14B C15B 1.215(19) 3 ?
C17 C17 1.57(3) 2 ?
C17 C17 1.57(3) 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
C3 N3 C4 127.5(3) . . ?
C1 N1 C1 111.4(3) 3_665 2_655 ?
C1 N1 C1 111.4(3) 3_665 . ?
C1 N1 C1 111.4(3) 2_655 . ?
C9 C4 C5 118.1(3) . . ?
C9 C4 N3 123.6(3) . . ?
C5 C4 N3 118.3(3) . . ?
O1 C3 N2 123.5(3) . . ?
O1 C3 N3 123.8(3) . . ?
N2 C3 N3 112.7(3) . . ?
C3 N2 C2 125.4(3) . . ?
C14B N4 C14B 38.9(12) . 3 ?
C14B N4 C14B 38.9(12) . 2 ?
C14B N4 C14B 38.9(13) 3 2 ?
C14B N4 C10 122.2(12) . 3 ?
C14B N4 C10 120.9(10) 3 3 ?
C14B N4 C10 89.3(8) 2 3 ?
C14B N4 C10 89.3(8) . 2 ?
C14B N4 C10 122.2(12) 3 2 ?
C14B N4 C10 120.9(10) 2 2 ?
C10 N4 C10 106.9(3) 3 2 ?
C14B N4 C10 120.9(11) . . ?
C14B N4 C10 89.3(8) 3 . ?
C14B N4 C10 122.2(12) 2 . ?
C10 N4 C10 106.9(3) 3 . ?
C10 N4 C10 106.9(3) 2 . ?
C10 N4 C14A 111.9(3) 3 . ?
C10 N4 C14A 111.9(3) 2 . ?
C10 N4 C14A 111.9(3) . . ?
C8 C9 C4 120.1(4) . . ?
C6 C5 C4 121.2(4) . . ?
C12 C11 C10 110.0(4) . . ?
C11 C10 N4 117.4(3) . . ?
C11 C12 C13 113.4(4) . . ?
C7 C6 C5 120.0(4) . . ?
C7 C8 C9 120.8(4) . . ?
C6 C7 C8 119.8(4) . . ?
C1 C2 N2 115.9(4) . . ?
C17 C16 C17 63.0(14) . 3 ?
C17 C16 C17 63.0(14) . 2 ?
C17 C16 C17 63.0(14) 3 2 ?
C17 C16 C15A 102.0(9) . 2 ?
C17 C16 C15A 140.8(17) 3 2 ?
C17 C16 C15A 145.5(17) 2 2 ?
C17 C16 C15B 146.1(15) . 3 ?
C17 C16 C15B 150.9(16) 3 3 ?
C17 C16 C15B 121.8(12) 2 3 ?
C17 C16 C15A 140.8(16) . 3 ?
C17 C16 C15A 145.5(17) 3 3 ?
C17 C16 C15A 102.0(9) 2 3 ?
C15A C16 C15A 69.1(5) 2 3 ?
C17 C16 C15B 121.8(12) . 2 ?
C17 C16 C15B 146.1(15) 3 2 ?
C17 C16 C15B 150.9(16) 2 2 ?
C15B C16 C15B 36.4(13) 3 2 ?
C17 C16 C15B 150.9(16) . . ?
C17 C16 C15B 121.9(11) 3 . ?
C17 C16 C15B 146.1(15) 2 . ?
C15B C16 C15B 36.4(12) 3 . ?
C15B C16 C15B 36.4(12) 2 . ?
C17 C16 C15A 145.5(17) . . ?
C17 C16 C15A 102.0(9) 3 . ?
C17 C16 C15A 140.8(16) 2 . ?
C15A C16 C15A 69.1(5) 2 . ?
C15A C16 C15A 69.1(5) 3 . ?
C2 C1 N1 124.6(5) . . ?
C15A C14A C15A 69.1(5) . 2 ?
C15A C14A C15A 69.1(5) . 3 ?
C15A C14A C15A 69.1(5) 2 3 ?
C15A C14A N4 139.1(3) . . ?
C15A C14A N4 139.1(3) 2 . ?
C15A C14A N4 139.1(3) 3 . ?
C14A C15A C16 98.2(6) . . ?
C14A C15A C15A 55.4(2) . 2 ?
C16 C15A C15A 55.4(2) . 2 ?
C14A C15A C15A 55.4(2) . 3 ?
C16 C15A C15A 55.4(2) . 3 ?
C15A C15A C15A 60.003(19) 2 3 ?
C15B C15B C15B 59.997(7) 3 2 ?
C15B C15B C14B 92.3(18) 3 3 ?
C15B C15B C14B 69(2) 2 3 ?
C15B C15B C14B 63.5(19) 3 2 ?
C15B C15B C14B 89.3(18) 2 2 ?
C14B C15B C14B 49.6(16) 3 2 ?
C15B C15B C14B 52.1(11) 3 . ?
C15B C15B C14B 49.1(10) 2 . ?
C14B C15B C14B 40.4(15) 3 . ?
C14B C15B C14B 40.4(14) 2 . ?
C15B C15B C16 71.8(6) 3 . ?
C15B C15B C16 71.8(6) 2 . ?
C14B C15B C16 140(2) 3 . ?
C14B C15B C16 135(2) 2 . ?
C14B C15B C16 111.7(9) . . ?
C14B C14B C14B 60.00(3) 2 3 ?
C14B C14B C15B 90.4(17) 2 2 ?
C14B C14B C15B 68(2) 3 2 ?
C14B C14B C15B 62.6(19) 2 3 ?
C14B C14B C15B 87.6(18) 3 3 ?
C15B C14B C15B 47.6(18) 2 3 ?
C14B C14B N4 70.6(6) 2 . ?
C14B C14B N4 70.6(6) 3 . ?
C15B C14B N4 138(2) 2 . ?
C15B C14B N4 133(2) 3 . ?
C14B C14B C15B 52.0(11) 2 . ?
C14B C14B C15B 49.1(9) 3 . ?
C15B C14B C15B 38.6(16) 2 . ?
C15B C14B C15B 38.6(15) 3 . ?
N4 C14B C15B 110.2(8) . . ?
C16 C17 C17 58.5(7) . 2 ?
C16 C17 C17 58.5(7) . 3 ?
C17 C17 C17 59.999(16) 2 3 ?

_refine_diff_density_max         0.266
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.047

