# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

####################################################################### 
# 
# 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_k182
_database_code_depnum_ccdc_archive 'CCDC 1561880'
_audit_update_record             
;
2017-07-12 deposited with the CCDC.
2017-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
;
7,16-[2,2'-(hexano-2,4-diyne-1,6-dioxy)-dibenzoylo]-5,14-dihydrodibenzo[b,i][1,4,8,11]tetraazacyclotetradecine
;
_chemical_melting_point          ?
_chemical_formula_sum            'C38 H26 N4 O4'
_chemical_formula_weight         602.63

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

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

_cell_length_a                   21.1618(16)
_cell_length_b                   11.9414(11)
_cell_length_c                   23.2097(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5865.1(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    291
_cell_measurement_reflns_used    7864
_cell_measurement_theta_min      1.7189
_cell_measurement_theta_max      35.9327

_exptl_crystal_description       Prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             2512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_diffrn_ambient_temperature      291
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 8.2356
_diffrn_source                   'Seifert Mo tube'
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       ω
_diffrn_reflns_number            66233
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_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         1.755
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.026
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5176
_reflns_number_gt                2230
_reflns_threshold_expression     'I > 2σ(I)'

_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_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.5783P] 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         5176
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0619
_refine_ls_wR_factor_gt          0.0583
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
N1 N 0.57827(7) 0.23287(18) 0.31538(7) 0.0615(5) Uani 1 1 d . . . . .
H1N H 0.571879 0.203654 0.282014 0.074 Uiso 1 1 calc R U . . .
N2 N 0.58081(7) 0.34752(15) 0.21768(7) 0.0592(5) Uani 1 1 d . . . . .
N3 N 0.57815(7) 0.03989(15) 0.25205(7) 0.0617(5) Uani 1 1 d . . . . .
N4 N 0.57143(7) 0.15389(18) 0.15440(7) 0.0635(5) Uani 1 1 d . . . . .
H4N H 0.574141 0.181943 0.188435 0.076 Uiso 1 1 calc R U . . .
O1 O 0.55451(7) 0.36967(13) 0.01982(6) 0.0820(5) Uani 1 1 d . . . . .
O2 O 0.71203(8) 0.40338(16) 0.09718(8) 0.0992(6) Uani 1 1 d . . . . .
O3 O 0.60707(7) 0.02859(14) 0.45356(6) 0.1000(6) Uani 1 1 d . . . . .
O4 O 0.72086(6) -0.03726(15) 0.33120(7) 0.0865(5) Uani 1 1 d . . . . .
C1 C 0.59141(9) 0.1643(2) 0.35822(9) 0.0649(7) Uani 1 1 d . . . . .
H1 H 0.595554 0.195402 0.394754 0.078 Uiso 1 1 calc R U . . .
C2 C 0.57390(8) 0.3493(2) 0.31987(9) 0.0559(6) Uani 1 1 d . . . . .
C3 C 0.56652(9) 0.4046(2) 0.37195(9) 0.0675(7) Uani 1 1 d . . . . .
H3 H 0.563330 0.363494 0.405853 0.081 Uiso 1 1 calc R U . . .
C4 C 0.56389(10) 0.5186(3) 0.37405(10) 0.0769(7) Uani 1 1 d . . . . .
H4 H 0.559433 0.554516 0.409364 0.092 Uiso 1 1 calc R U . . .
C5 C 0.56777(9) 0.5811(2) 0.32416(10) 0.0729(7) Uani 1 1 d . . . . .
H5 H 0.566874 0.658894 0.325624 0.087 Uiso 1 1 calc R U . . .
C6 C 0.57305(9) 0.5259(2) 0.27175(9) 0.0659(6) Uani 1 1 d . . . . .
H6 H 0.574347 0.567444 0.237888 0.079 Uiso 1 1 calc R U . . .
C7 C 0.57638(8) 0.4114(2) 0.26884(9) 0.0545(6) Uani 1 1 d . . . . .
C8 C 0.59002(8) 0.39569(19) 0.16746(9) 0.0609(6) Uani 1 1 d . . . . .
H8 H 0.600437 0.471331 0.166626 0.073 Uiso 1 1 calc R U . . .
C9 C 0.58482(9) 0.3380(2) 0.11517(8) 0.0588(6) Uani 1 1 d . . . . .
C10 C 0.58702(10) 0.4008(2) 0.06127(9) 0.0670(7) Uani 1 1 d . . . . .
C11 C 0.62837(12) 0.5000(2) 0.05451(9) 0.0680(7) Uani 1 1 d . . . . .
C12 C 0.60520(12) 0.5928(3) 0.02623(9) 0.0817(8) Uani 1 1 d . . . . .
H12 H 0.563024 0.594273 0.015008 0.098 Uiso 1 1 calc R U . . .
C13 C 0.64344(18) 0.6835(3) 0.01424(10) 0.1010(9) Uani 1 1 d . . . . .
H13 H 0.627105 0.747026 -0.003525 0.121 Uiso 1 1 calc R U . . .
C14 C 0.70595(17) 0.6778(3) 0.02911(12) 0.1098(10) Uani 1 1 d . . . . .
H14 H 0.732437 0.737553 0.020415 0.132 Uiso 1 1 calc R U . . .
C15 C 0.73021(13) 0.5862(3) 0.05641(12) 0.1021(9) Uani 1 1 d . . . . .
H15 H 0.772937 0.583755 0.065709 0.123 Uiso 1 1 calc R U . . .
C16 C 0.69191(13) 0.4983(3) 0.07009(10) 0.0803(7) Uani 1 1 d . . . . .
C17 C 0.77231(11) 0.4045(2) 0.12404(11) 0.0999(9) Uani 1 1 d . . . . .
H17A H 0.777969 0.472849 0.146063 0.120 Uiso 1 1 calc R U . . .
H17B H 0.805575 0.399816 0.095394 0.120 Uiso 1 1 calc R U . . .
C18 C 0.77382(12) 0.3068(3) 0.16203(13) 0.0930(9) Uani 1 1 d . . . . .
C19 C 0.77309(12) 0.2279(3) 0.19272(13) 0.0911(9) Uani 1 1 d . . . . .
C20 C 0.77269(12) 0.1362(3) 0.22740(13) 0.0910(9) Uani 1 1 d . . . . .
C21 C 0.77201(12) 0.0573(3) 0.25787(12) 0.0917(9) Uani 1 1 d . . . . .
C22 C 0.77334(11) -0.0416(2) 0.29499(11) 0.0977(9) Uani 1 1 d . . . . .
H22A H 0.772053 -0.109108 0.271772 0.117 Uiso 1 1 calc R U . . .
H22B H 0.811867 -0.042420 0.317623 0.117 Uiso 1 1 calc R U . . .
C23 C 0.70816(11) -0.1273(3) 0.36580(10) 0.0695(7) Uani 1 1 d . . . . .
C24 C 0.74348(11) -0.2239(3) 0.36678(11) 0.0847(8) Uani 1 1 d . . . . .
H24 H 0.778924 -0.230484 0.343337 0.102 Uiso 1 1 calc R U . . .
C25 C 0.72649(13) -0.3102(2) 0.40219(12) 0.0916(8) Uani 1 1 d . . . . .
H25 H 0.750392 -0.375534 0.402807 0.110 Uiso 1 1 calc R U . . .
C26 C 0.67449(14) -0.3007(2) 0.43668(10) 0.0890(8) Uani 1 1 d . . . . .
H26 H 0.662398 -0.360161 0.460078 0.107 Uiso 1 1 calc R U . . .
C27 C 0.64015(11) -0.2034(3) 0.43677(9) 0.0790(7) Uani 1 1 d . . . . .
H27 H 0.605794 -0.196679 0.461512 0.095 Uiso 1 1 calc R U . . .
C28 C 0.65532(10) -0.1155(2) 0.40113(9) 0.0641(7) Uani 1 1 d . . . . .
C29 C 0.61916(10) -0.0098(2) 0.40566(10) 0.0710(7) Uani 1 1 d . . . . .
C30 C 0.59952(9) 0.0501(2) 0.35327(9) 0.0610(6) Uani 1 1 d . . . . .
C31 C 0.59380(8) -0.00814(19) 0.30106(9) 0.0613(6) Uani 1 1 d . . . . .
H31 H 0.601482 -0.084824 0.301069 0.074 Uiso 1 1 calc R U . . .
C32 C 0.56898(8) -0.0240(2) 0.20157(9) 0.0574(6) Uani 1 1 d . . . . .
C33 C 0.56250(9) -0.1381(2) 0.19918(10) 0.0738(7) Uani 1 1 d . . . . .
H33 H 0.565192 -0.179626 0.232993 0.089 Uiso 1 1 calc R U . . .
C34 C 0.55205(10) -0.1929(2) 0.14747(12) 0.0841(8) Uani 1 1 d . . . . .
H34 H 0.548509 -0.270525 0.146347 0.101 Uiso 1 1 calc R U . . .
C35 C 0.54698(10) -0.1308(3) 0.09782(11) 0.0837(8) Uani 1 1 d . . . . .
H35 H 0.538967 -0.166784 0.063037 0.100 Uiso 1 1 calc R U . . .
C36 C 0.55351(9) -0.0174(2) 0.09884(10) 0.0747(7) Uani 1 1 d . . . . .
H36 H 0.550467 0.023315 0.064794 0.090 Uiso 1 1 calc R U . . .
C37 C 0.56468(8) 0.0376(2) 0.15042(10) 0.0569(6) Uani 1 1 d . . . . .
C38 C 0.57400(9) 0.2241(2) 0.11097(9) 0.0620(6) Uani 1 1 d . . . . .
H38 H 0.568045 0.194746 0.074253 0.074 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
N1 C1 1.318(2) . ?
N1 C2 1.398(2) . ?
N2 C8 1.314(2) . ?
N2 C7 1.414(2) . ?
N3 C31 1.316(2) . ?
N3 C32 1.411(2) . ?
N4 C38 1.312(2) . ?
N4 C37 1.398(2) . ?
O1 C10 1.240(2) . ?
O2 C16 1.365(3) . ?
O2 C17 1.420(2) . ?
O3 C29 1.230(2) . ?
O4 C23 1.369(3) . ?
O4 C22 1.394(2) . ?
C1 C30 1.378(3) . ?
C2 C3 1.386(2) . ?
C2 C7 1.398(3) . ?
C3 C4 1.363(3) . ?
C4 C5 1.380(3) . ?
C5 C6 1.388(2) . ?
C6 C7 1.371(3) . ?
C8 C9 1.400(2) . ?
C9 C38 1.382(3) . ?
C9 C10 1.459(3) . ?
C10 C11 1.481(3) . ?
C11 C12 1.378(3) . ?
C11 C16 1.392(3) . ?
C12 C13 1.381(3) . ?
C13 C14 1.369(3) . ?
C14 C15 1.364(3) . ?
C15 C16 1.364(3) . ?
C17 C18 1.464(3) . ?
C18 C19 1.181(4) . ?
C19 C20 1.359(4) . ?
C20 C21 1.178(4) . ?
C21 C22 1.462(3) . ?
C23 C24 1.375(3) . ?
C23 C28 1.394(3) . ?
C24 C25 1.366(3) . ?
C25 C26 1.365(3) . ?
C26 C27 1.370(3) . ?
C27 C28 1.374(3) . ?
C28 C29 1.479(3) . ?
C29 C30 1.471(3) . ?
C30 C31 1.403(3) . ?
C32 C33 1.371(3) . ?
C32 C37 1.400(3) . ?
C33 C34 1.385(3) . ?
C34 C35 1.374(3) . ?
C35 C36 1.362(3) . ?
C36 C37 1.386(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
C1 N1 C2 125.2(2) . . ?
C8 N2 C7 121.2(2) . . ?
C31 N3 C32 121.1(2) . . ?
C38 N4 C37 126.0(2) . . ?
C16 O2 C17 118.3(2) . . ?
C23 O4 C22 118.8(2) . . ?
N1 C1 C30 125.3(2) . . ?
C3 C2 N1 123.1(2) . . ?
C3 C2 C7 119.4(2) . . ?
N1 C2 C7 117.5(2) . . ?
C4 C3 C2 120.7(2) . . ?
C3 C4 C5 120.5(2) . . ?
C4 C5 C6 118.9(2) . . ?
C7 C6 C5 121.4(2) . . ?
C6 C7 C2 119.0(2) . . ?
C6 C7 N2 125.6(2) . . ?
C2 C7 N2 115.3(2) . . ?
N2 C8 C9 122.8(2) . . ?
C38 C9 C8 123.9(2) . . ?
C38 C9 C10 116.8(2) . . ?
C8 C9 C10 119.2(2) . . ?
O1 C10 C9 119.6(2) . . ?
O1 C10 C11 119.0(2) . . ?
C9 C10 C11 121.4(2) . . ?
C12 C11 C16 118.6(3) . . ?
C12 C11 C10 118.9(2) . . ?
C16 C11 C10 122.1(3) . . ?
C11 C12 C13 121.2(3) . . ?
C14 C13 C12 118.4(3) . . ?
C15 C14 C13 121.4(3) . . ?
C16 C15 C14 120.1(3) . . ?
C15 C16 O2 124.2(3) . . ?
C15 C16 C11 120.2(3) . . ?
O2 C16 C11 115.6(3) . . ?
O2 C17 C18 106.0(2) . . ?
C19 C18 C17 178.0(3) . . ?
C18 C19 C20 179.2(4) . . ?
C21 C20 C19 179.3(4) . . ?
C20 C21 C22 178.0(3) . . ?
O4 C22 C21 108.1(2) . . ?
O4 C23 C24 124.2(2) . . ?
O4 C23 C28 115.1(3) . . ?
C24 C23 C28 120.7(3) . . ?
C25 C24 C23 120.0(3) . . ?
C26 C25 C24 120.1(3) . . ?
C25 C26 C27 119.9(3) . . ?
C26 C27 C28 121.5(2) . . ?
C27 C28 C23 117.7(2) . . ?
C27 C28 C29 119.2(2) . . ?
C23 C28 C29 122.9(3) . . ?
O3 C29 C30 120.4(2) . . ?
O3 C29 C28 119.4(2) . . ?
C30 C29 C28 120.2(2) . . ?
C1 C30 C31 123.5(2) . . ?
C1 C30 C29 116.6(2) . . ?
C31 C30 C29 119.8(2) . . ?
N3 C31 C30 123.5(2) . . ?
C33 C32 C37 118.8(2) . . ?
C33 C32 N3 125.8(2) . . ?
C37 C32 N3 115.4(2) . . ?
C32 C33 C34 121.4(2) . . ?
C35 C34 C33 119.0(3) . . ?
C36 C35 C34 120.9(3) . . ?
C35 C36 C37 120.3(2) . . ?
C36 C37 N4 123.0(2) . . ?
C36 C37 C32 119.6(2) . . ?
N4 C37 C32 117.3(2) . . ?
N4 C38 C9 125.5(2) . . ?

_refine_diff_density_max         0.180
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.036



####################################################################### 
# 
# 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_KPIR
_database_code_depnum_ccdc_archive 'CCDC 1573504'
_audit_update_record             
;
2017-09-09 deposited with the CCDC.
2017-09-27 downloaded from the CCDC.
;

_chemical_name_systematic        
;
{7,16-bis[2-(prop-2-yn-1-yloxy)benzoyl]-5,14-dihydrodibenzo[b,i][1,4,8,11]tetraazacyclotetradecinato(2-)k⁴N} zinc(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H32 N4 O5 S Zn, 3(C2 H6 O S)'
_chemical_formula_sum            'C46 H50 N4 O8 S4 Zn'
_chemical_formula_weight         980.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.2639(12)
_cell_length_b                   15.6341(17)
_cell_length_c                   13.7495(15)
_cell_angle_alpha                90
_cell_angle_beta                 110.204(2)
_cell_angle_gamma                90
_cell_volume                     2272.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    9475
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.6

_exptl_crystal_description       Prism
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37356
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.578
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8035
_reflns_number_gt                7890
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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.
;

_refine_special_details          
'Refined as a 2-component inversion twin.,2-component inversion twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0426P)²+0.7690P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.201(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8035
_refine_ls_number_parameters     587
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0708
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Zn1 Zn 0.25533(3) 0.73708(2) 1.01180(2) 0.01070(10) Uani 1 1 d . . . A 1
S1 S 0.28280(8) 0.54953(5) 0.95933(6) 0.01692(18) Uani 1 1 d . . . A 1
O1 O -0.2544(2) 0.81465(18) 0.88759(17) 0.0211(5) Uani 1 1 d . . . A 1
O2 O -0.1810(2) 0.61829(15) 0.74852(17) 0.0155(5) Uani 1 1 d . . . A 1
O3 O 0.7679(2) 0.76440(17) 1.11226(18) 0.0205(5) Uani 1 1 d . . . A 1
O4 O 0.6871(2) 0.94051(14) 1.25505(16) 0.0151(5) Uani 1 1 d . . . A 1
O5 O 0.2731(2) 0.60645(15) 1.04720(18) 0.0175(5) Uani 1 1 d . . . A 1
N1 N 0.1128(3) 0.77297(17) 1.0603(2) 0.0122(6) Uani 1 1 d . . . A 1
N2 N 0.1435(2) 0.7404(2) 0.86093(17) 0.0112(5) Uani 1 1 d . . . A 1
N3 N 0.3931(2) 0.75653(17) 0.94992(19) 0.0120(5) Uani 1 1 d . . . A 1
N4 N 0.3624(2) 0.78877(17) 1.14860(19) 0.0115(5) Uani 1 1 d . . . A 1
C1 C -0.0055(3) 0.78073(19) 1.0011(2) 0.0118(6) Uani 1 1 d . . . A 1
H1 H -0.064600 0.796402 1.033303 0.014 Uiso 1 1 calc R U . A 1
C2 C 0.0214(3) 0.7531(2) 0.8278(2) 0.0119(6) Uani 1 1 d . . . A 1
H2 H -0.021521 0.752725 0.754910 0.014 Uiso 1 1 calc R U . A 1
C3 C -0.0530(3) 0.7675(2) 0.8917(2) 0.0123(6) Uani 1 1 d . . . A 1
C4 C -0.1890(3) 0.7817(2) 0.8411(2) 0.0126(6) Uani 1 1 d . . . A 1
C5 C -0.2546(3) 0.7610(2) 0.7280(2) 0.0118(6) Uani 1 1 d . . . A 1
C6 C -0.3307(3) 0.8248(2) 0.6663(2) 0.0126(6) Uani 1 1 d . . . A 1
H6 H -0.338393 0.877975 0.697003 0.015 Uiso 1 1 calc R U . A 1
C7 C -0.3953(3) 0.8126(2) 0.5618(2) 0.0153(7) Uani 1 1 d . . . A 1
H7 H -0.444919 0.857299 0.520691 0.018 Uiso 1 1 calc R U . A 1
C8 C -0.3866(3) 0.7338(3) 0.5176(2) 0.0160(6) Uani 1 1 d . . . A 1
H8 H -0.430517 0.724855 0.445784 0.019 Uiso 1 1 calc R U . A 1
C9 C -0.3144(3) 0.6682(2) 0.5773(2) 0.0145(6) Uani 1 1 d . . . A 1
H9 H -0.309269 0.614589 0.546433 0.017 Uiso 1 1 calc R U . A 1
C10 C -0.2496(3) 0.6812(2) 0.6825(2) 0.0128(6) Uani 1 1 d . . . A 1
C11 C -0.1754(3) 0.5359(2) 0.7034(3) 0.0160(7) Uani 1 1 d . . . A 1
H11A H -0.262197 0.517603 0.661444 0.019 Uiso 1 1 calc R U . A 1
H11B H -0.140520 0.493475 0.759477 0.019 Uiso 1 1 calc R U . A 1
C12 C -0.0971(3) 0.5371(2) 0.6375(2) 0.0163(7) Uani 1 1 d . . . A 1
C13 C -0.0375(3) 0.5400(2) 0.5810(3) 0.0199(7) Uani 1 1 d . . . A 1
H13 H 0.010047 0.542240 0.535901 0.024 Uiso 1 1 calc R U . A 1
C14 C 0.2146(3) 0.7376(2) 0.7930(2) 0.0113(5) Uani 1 1 d . . . A 1
C15 C 0.1630(3) 0.7236(2) 0.6868(2) 0.0133(6) Uani 1 1 d . . . A 1
H15 H 0.074497 0.714644 0.655334 0.016 Uiso 1 1 calc R U . A 1
C16 C 0.2391(3) 0.7226(2) 0.6259(2) 0.0144(6) Uani 1 1 d . . . A 1
H16 H 0.202759 0.712902 0.553416 0.017 Uiso 1 1 calc R U . A 1
C17 C 0.3689(3) 0.7357(2) 0.6717(2) 0.0141(6) Uani 1 1 d . . . A 1
H17 H 0.420678 0.736019 0.629844 0.017 Uiso 1 1 calc R U . A 1
C18 C 0.4232(3) 0.7484(2) 0.7774(2) 0.0136(6) Uani 1 1 d . . . A 1
H18 H 0.511841 0.757372 0.807572 0.016 Uiso 1 1 calc R U . A 1
C19 C 0.3480(3) 0.7481(2) 0.8408(2) 0.0109(6) Uani 1 1 d . . . A 1
C21 C 0.5126(3) 0.7666(2) 1.0054(2) 0.0122(6) Uani 1 1 d . . . A 1
H21 H 0.571911 0.765189 0.970337 0.015 Uiso 1 1 calc R U . A 1
C22 C 0.4867(3) 0.7931(2) 1.1795(2) 0.0106(6) Uani 1 1 d . . . A 1
H22 H 0.530481 0.806346 1.250305 0.013 Uiso 1 1 calc R U . A 1
C23 C 0.5605(3) 0.7796(2) 1.1155(2) 0.0119(6) Uani 1 1 d . . . A 1
C24 C 0.6981(3) 0.7815(2) 1.1621(2) 0.0124(6) Uani 1 1 d . . . A 1
C25 C 0.7615(3) 0.7987(2) 1.2765(2) 0.0113(6) Uani 1 1 d . . . A 1
C26 C 0.8364(3) 0.7341(2) 1.3372(2) 0.0133(6) Uani 1 1 d . . . A 1
H26 H 0.843246 0.680981 1.306115 0.016 Uiso 1 1 calc R U . A 1
C27 C 0.9011(3) 0.7461(2) 1.4423(2) 0.0155(6) Uani 1 1 d . . . A 1
H27 H 0.950897 0.701367 1.483211 0.019 Uiso 1 1 calc R U . A 1
C28 C 0.8919(3) 0.8243(2) 1.4866(2) 0.0147(6) Uani 1 1 d . . . A 1
H28 H 0.935179 0.832641 1.558678 0.018 Uiso 1 1 calc R U . A 1
C29 C 0.8201(3) 0.8909(2) 1.4274(2) 0.0143(6) Uani 1 1 d . . . A 1
H29 H 0.814976 0.944346 1.458617 0.017 Uiso 1 1 calc R U . A 1
C30 C 0.7563(3) 0.8780(2) 1.3222(2) 0.0119(6) Uani 1 1 d . . . A 1
C31 C 0.6799(3) 1.0229(2) 1.2990(2) 0.0162(7) Uani 1 1 d . . . A 1
H31A H 0.643801 1.064672 1.242303 0.019 Uiso 1 1 calc R U . A 1
H31B H 0.766317 1.042219 1.340398 0.019 Uiso 1 1 calc R U . A 1
C32 C 0.6018(3) 1.0216(2) 1.3654(3) 0.0166(7) Uani 1 1 d . . . A 1
C33 C 0.5415(3) 1.0187(2) 1.4213(3) 0.0192(7) Uani 1 1 d . . . A 1
H33 H 0.493346 1.016396 1.465884 0.023 Uiso 1 1 calc R U . A 1
C34 C 0.2918(3) 0.8048(2) 1.2138(2) 0.0112(6) Uani 1 1 d . . . A 1
C35 C 0.3417(3) 0.8285(2) 1.3174(2) 0.0129(6) Uani 1 1 d . . . A 1
H35 H 0.430097 0.838290 1.348068 0.015 Uiso 1 1 calc R U . A 1
C36 C 0.2650(3) 0.8383(2) 1.3770(2) 0.0131(6) Uani 1 1 d . . . A 1
H36 H 0.300930 0.854360 1.447765 0.016 Uiso 1 1 calc R U . A 1
C37 C 0.1349(3) 0.8244(2) 1.3322(2) 0.0138(6) Uani 1 1 d . . . A 1
H37 H 0.082527 0.829845 1.373242 0.017 Uiso 1 1 calc R U . A 1
C38 C 0.0816(3) 0.8028(2) 1.2283(2) 0.0129(6) Uani 1 1 d . . . A 1
H38 H -0.007090 0.794006 1.198245 0.015 Uiso 1 1 calc R U . A 1
C39 C 0.1584(3) 0.7938(2) 1.1675(2) 0.0113(6) Uani 1 1 d . . . A 1
C41 C 0.3855(4) 0.4645(2) 1.0208(3) 0.0235(8) Uani 1 1 d . . . A 1
H41A H 0.471938 0.486338 1.052071 0.035 Uiso 1 1 calc R U . A 1
H41B H 0.383476 0.420524 0.969410 0.035 Uiso 1 1 calc R U . A 1
H41C H 0.357864 0.439566 1.074816 0.035 Uiso 1 1 calc R U . A 1
C42 C 0.1371(4) 0.4919(3) 0.9150(4) 0.0355(10) Uani 1 1 d . . . A 1
H42A H 0.126910 0.459807 0.972866 0.053 Uiso 1 1 calc R U . A 1
H42B H 0.137714 0.452094 0.860159 0.053 Uiso 1 1 calc R U . A 1
H42C H 0.066721 0.532183 0.887769 0.053 Uiso 1 1 calc R U . A 1
S2 S 0.07829(8) 0.57716(6) 0.30148(7) 0.02050(19) Uani 1 1 d . . . B 1
O6 O 0.0773(3) 0.56963(19) 0.4097(2) 0.0325(6) Uani 1 1 d . . . B 1
C43 C 0.2404(4) 0.5914(3) 0.3122(3) 0.0263(8) Uani 1 1 d . . . B 1
H43A H 0.270726 0.646870 0.344390 0.039 Uiso 1 1 calc R U . B 1
H43B H 0.246982 0.589563 0.242973 0.039 Uiso 1 1 calc R U . B 1
H43C H 0.291892 0.545593 0.354954 0.039 Uiso 1 1 calc R U . B 1
C44 C 0.0603(4) 0.4697(3) 0.2506(3) 0.0293(9) Uani 1 1 d . . . B 1
H44A H 0.118953 0.431524 0.301294 0.044 Uiso 1 1 calc R U . B 1
H44B H 0.078954 0.468844 0.186051 0.044 Uiso 1 1 calc R U . B 1
H44C H -0.026740 0.450346 0.236779 0.044 Uiso 1 1 calc R U . B 1
S3 S 0.41502(8) -0.02202(5) 0.69023(7) 0.01863(18) Uani 1 1 d . . . C 1
O7 O 0.4241(3) -0.0136(2) 0.5845(2) 0.0331(7) Uani 1 1 d . . . C 1
C45 C 0.4248(4) 0.0843(3) 0.7409(3) 0.0295(9) Uani 1 1 d . . . C 1
H45A H 0.512144 0.104858 0.760697 0.044 Uiso 1 1 calc R U . C 1
H45B H 0.398542 0.084127 0.801791 0.044 Uiso 1 1 calc R U . C 1
H45C H 0.369009 0.122150 0.687783 0.044 Uiso 1 1 calc R U . C 1
C46 C 0.2518(4) -0.0402(3) 0.6712(3) 0.0269(8) Uani 1 1 d . . . C 1
H46A H 0.200349 0.004877 0.626957 0.040 Uiso 1 1 calc R U . C 1
H46B H 0.239523 -0.039654 0.738420 0.040 Uiso 1 1 calc R U . C 1
H46C H 0.226025 -0.095948 0.637947 0.040 Uiso 1 1 calc R U . C 1
S4A S 0.75719(10) 0.49556(8) 0.99867(9) 0.0241(4) Uani 0.819(4) 1 d . . P D 1
O8 O 0.7127(4) 0.4966(3) 1.0908(3) 0.0621(12) Uani 1 1 d . . . D 1
C47 C 0.8421(4) 0.5932(3) 1.0060(3) 0.0268(8) Uani 1 1 d . . . D 1
H47A H 0.791236 0.641053 1.015767 0.040 Uiso 1 1 calc R U . D 1
H47B H 0.859668 0.601438 0.941587 0.040 Uiso 1 1 calc R U . D 1
H47C H 0.922051 0.590583 1.064568 0.040 Uiso 1 1 calc R U . D 1
C48 C 0.6244(4) 0.5209(4) 0.8909(3) 0.0426(11) Uani 1 1 d . . . D 1
H48A H 0.649833 0.528434 0.830110 0.064 Uiso 1 1 calc R U . D 1
H48B H 0.586403 0.573944 0.904311 0.064 Uiso 1 1 calc R U . D 1
H48C H 0.562484 0.474356 0.877897 0.064 Uiso 1 1 calc R U . D 1
S4B S 0.6791(5) 0.5812(4) 0.9874(4) 0.0272(17) Uani 0.181(4) 1 d . . P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 N1 2.019(3) . ?
Zn1 N4 2.020(3) . ?
Zn1 N2 2.022(2) . ?
Zn1 N3 2.034(3) . ?
Zn1 O5 2.093(2) . ?
S1 O5 1.534(2) . ?
S1 C41 1.774(4) . ?
S1 C42 1.785(4) . ?
O1 C4 1.241(4) . ?
O2 C10 1.379(4) . ?
O2 C11 1.441(4) . ?
O3 C24 1.238(4) . ?
O4 C30 1.384(4) . ?
O4 C31 1.437(4) . ?
N1 C1 1.305(4) . ?
N1 C39 1.421(4) . ?
N2 C2 1.306(4) . ?
N2 C14 1.426(3) . ?
N3 C21 1.307(4) . ?
N3 C19 1.414(4) . ?
N4 C22 1.317(4) . ?
N4 C34 1.411(4) . ?
C1 C3 1.427(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.425(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.465(4) . ?
C4 C5 1.508(4) . ?
C5 C6 1.396(5) . ?
C5 C10 1.406(5) . ?
C6 C7 1.382(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.391(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(5) . ?
C9 H9 0.9500 . ?
C11 C12 1.466(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.190(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(4) . ?
C14 C19 1.427(4) . ?
C15 C16 1.389(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.409(4) . ?
C18 H18 0.9500 . ?
C21 C23 1.436(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.419(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.459(5) . ?
C24 C25 1.510(4) . ?
C25 C26 1.393(5) . ?
C25 C30 1.400(5) . ?
C26 C27 1.388(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.385(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.395(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(4) . ?
C29 H29 0.9500 . ?
C31 C32 1.470(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.189(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.389(4) . ?
C34 C39 1.426(4) . ?
C35 C36 1.389(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.397(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.387(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.402(4) . ?
C38 H38 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
S2 O6 1.496(3) . ?
S2 C43 1.794(4) . ?
S2 C44 1.804(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
S3 O7 1.498(3) . ?
S3 C46 1.789(4) . ?
S3 C45 1.791(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
S4A O8 1.515(4) . ?
S4A C48 1.749(5) . ?
S4A C47 1.785(4) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zn1 N4 82.45(11) . . ?
N1 Zn1 N2 92.68(10) . . ?
N4 Zn1 N2 154.89(11) . . ?
N1 Zn1 N3 154.86(11) . . ?
N4 Zn1 N3 91.90(11) . . ?
N2 Zn1 N3 82.08(10) . . ?
N1 Zn1 O5 102.57(10) . . ?
N4 Zn1 O5 101.27(10) . . ?
N2 Zn1 O5 103.83(11) . . ?
N3 Zn1 O5 102.56(10) . . ?
O5 S1 C41 105.77(15) . . ?
O5 S1 C42 104.75(17) . . ?
C41 S1 C42 99.0(2) . . ?
C10 O2 C11 116.8(2) . . ?
C30 O4 C31 116.9(2) . . ?
S1 O5 Zn1 114.20(13) . . ?
C1 N1 C39 123.4(3) . . ?
C1 N1 Zn1 125.2(2) . . ?
C39 N1 Zn1 111.2(2) . . ?
C2 N2 C14 122.5(2) . . ?
C2 N2 Zn1 124.75(19) . . ?
C14 N2 Zn1 112.30(17) . . ?
C21 N3 C19 123.4(3) . . ?
C21 N3 Zn1 123.7(2) . . ?
C19 N3 Zn1 112.57(19) . . ?
C22 N4 C34 123.8(3) . . ?
C22 N4 Zn1 123.2(2) . . ?
C34 N4 Zn1 112.1(2) . . ?
N1 C1 C3 125.0(3) . . ?
N1 C1 H1 117.5 . . ?
C3 C1 H1 117.5 . . ?
N2 C2 C3 125.5(3) . . ?
N2 C2 H2 117.3 . . ?
C3 C2 H2 117.2 . . ?
C1 C3 C2 126.0(3) . . ?
C1 C3 C4 115.3(3) . . ?
C2 C3 C4 118.2(3) . . ?
O1 C4 C3 121.8(3) . . ?
O1 C4 C5 117.0(3) . . ?
C3 C4 C5 121.1(3) . . ?
C6 C5 C10 118.3(3) . . ?
C6 C5 C4 116.9(3) . . ?
C10 C5 C4 124.7(3) . . ?
C7 C6 C5 121.7(3) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?
C6 C7 C8 119.0(3) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C9 C8 C7 120.8(3) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
O2 C10 C9 123.6(3) . . ?
O2 C10 C5 116.0(3) . . ?
C9 C10 C5 120.3(3) . . ?
O2 C11 C12 112.3(3) . . ?
O2 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
O2 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C11 177.2(3) . . ?
C12 C13 H13 180.0 . . ?
C15 C14 N2 124.6(3) . . ?
C15 C14 C19 119.6(3) . . ?
N2 C14 C19 115.8(2) . . ?
C14 C15 C16 120.9(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 119.7(3) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 N3 125.7(3) . . ?
C18 C19 C14 118.5(3) . . ?
N3 C19 C14 115.8(2) . . ?
N3 C21 C23 124.7(3) . . ?
N3 C21 H21 117.7 . . ?
C23 C21 H21 117.7 . . ?
N4 C22 C23 125.3(3) . . ?
N4 C22 H22 117.4 . . ?
C23 C22 H22 117.4 . . ?
C22 C23 C21 126.0(3) . . ?
C22 C23 C24 119.0(3) . . ?
C21 C23 C24 115.0(3) . . ?
O3 C24 C23 122.3(3) . . ?
O3 C24 C25 116.9(3) . . ?
C23 C24 C25 120.7(3) . . ?
C26 C25 C30 118.9(3) . . ?
C26 C25 C24 117.7(3) . . ?
C30 C25 C24 123.2(3) . . ?
C27 C26 C25 121.2(3) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C28 C27 C26 119.0(3) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 121.2(3) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C30 C29 C28 119.1(3) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
O4 C30 C29 124.2(3) . . ?
O4 C30 C25 115.2(3) . . ?
C29 C30 C25 120.6(3) . . ?
O4 C31 C32 112.4(3) . . ?
O4 C31 H31A 109.1 . . ?
C32 C31 H31A 109.1 . . ?
O4 C31 H31B 109.1 . . ?
C32 C31 H31B 109.1 . . ?
H31A C31 H31B 107.9 . . ?
C33 C32 C31 177.8(4) . . ?
C32 C33 H33 180.0 . . ?
C35 C34 N4 125.5(3) . . ?
C35 C34 C39 118.8(3) . . ?
N4 C34 C39 115.7(3) . . ?
C34 C35 C36 121.3(3) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C36 C37 119.7(3) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C38 C37 C36 120.4(3) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 120.2(3) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C38 C39 N1 124.4(3) . . ?
C38 C39 C34 119.6(3) . . ?
N1 C39 C34 116.0(3) . . ?
S1 C41 H41A 109.5 . . ?
S1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
S1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
S1 C42 H42A 109.5 . . ?
S1 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
S1 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O6 S2 C43 106.56(17) . . ?
O6 S2 C44 105.90(19) . . ?
C43 S2 C44 97.02(18) . . ?
S2 C43 H43A 109.5 . . ?
S2 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
S2 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
S2 C44 H44A 109.5 . . ?
S2 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
S2 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O7 S3 C46 106.47(18) . . ?
O7 S3 C45 106.28(19) . . ?
C46 S3 C45 97.28(19) . . ?
S3 C45 H45A 109.5 . . ?
S3 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
S3 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
S3 C46 H46A 109.5 . . ?
S3 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
S3 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O8 S4A C48 105.9(2) . . ?
O8 S4A C47 105.6(2) . . ?
C48 S4A C47 98.0(2) . . ?
S4A C47 H47A 109.5 . . ?
S4A C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
S4A C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
S4A C48 H48A 109.5 . . ?
S4A C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
S4A C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

_refine_diff_density_max         0.805
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.058



