# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ic18499
_database_code_depnum_ccdc_archive 'CCDC 1834300'
loop_
_audit_author_name
_audit_author_address
'Gene-Hsiang Lee'
;National Taiwan university
Taiwan
;
_audit_update_record             
;
2018-04-03 deposited with the CCDC.	2020-03-27 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         ?
_chemical_formula_sum            'C25 H27 N3 O6'
_chemical_formula_weight         465.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   11.8148(3)
_cell_length_b                   9.6634(2)
_cell_length_c                   20.8234(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.5727(10)
_cell_angle_gamma                90
_cell_volume                     2350.87(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    7578
_cell_measurement_theta_min      3.78
_cell_measurement_theta_max      70.03

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    0.784
_shelx_estimated_absorpt_T_min   0.885
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6024
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11420
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         4.294
_diffrn_reflns_theta_max         69.990
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4394
_reflns_number_gt                3715
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_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)+(0.0421P)²+0.8741P] 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         4394
_refine_ls_number_parameters     323
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.041
_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
O1 O 0.90794(11) 0.32296(16) 0.18259(8) 0.0605(4) Uani 1 1 d . . . . .
O2 O 1.01279(10) 0.47810(15) 0.23607(7) 0.0548(3) Uani 1 1 d . . . . .
O3 O 0.38437(11) 1.29265(13) 0.13625(5) 0.0447(3) Uani 1 1 d . . . . .
O4 O 0.28129(8) 1.25132(11) 0.03742(5) 0.0327(2) Uani 1 1 d . . . . .
O5 O 0.65644(10) 1.05387(14) 0.19150(6) 0.0455(3) Uani 1 1 d . . . . .
O6 O 0.69557(9) 0.95053(14) 0.10131(6) 0.0429(3) Uani 1 1 d D . . . .
N1 N 0.42102(10) 0.71878(16) 0.19791(7) 0.0375(3) Uani 1 1 d . . . . .
H1 H 0.4161(16) 0.659(2) 0.2286(10) 0.046(5) Uiso 1 1 d . . . . .
N2 N 0.49303(12) 0.73913(16) 0.03439(6) 0.0401(3) Uani 1 1 d . . . . .
N3 N 0.92035(11) 0.43497(16) 0.20979(7) 0.0405(3) Uani 1 1 d . . . . .
C1 C 0.31733(12) 0.78203(17) 0.17476(6) 0.0307(3) Uani 1 1 d . . . . .
C2 C 0.21536(13) 0.71256(18) 0.18087(7) 0.0363(3) Uani 1 1 d . . . . .
H2A H 0.2183 0.6267 0.2033 0.044 Uiso 1 1 calc R U . . .
C3 C 0.11119(13) 0.7671(2) 0.15483(8) 0.0426(4) Uani 1 1 d . . . . .
H3 H 0.0427 0.7194 0.1596 0.051 Uiso 1 1 calc R U . . .
C4 C 0.10607(13) 0.8911(2) 0.12182(10) 0.0506(5) Uani 1 1 d . . . . .
H4 H 0.0342 0.9281 0.1030 0.061 Uiso 1 1 calc R U . . .
C5 C 0.20599(13) 0.9613(2) 0.11620(8) 0.0417(4) Uani 1 1 d . . . . .
H5 H 0.2017 1.0471 0.0937 0.050 Uiso 1 1 calc R U . . .
C6 C 0.31271(11) 0.90951(17) 0.14265(6) 0.0293(3) Uani 1 1 d . . . . .
C7 C 0.42195(11) 0.98875(16) 0.13865(6) 0.0274(3) Uani 1 1 d . . . . .
H7 H 0.4372 1.0485 0.1782 0.033 Uiso 1 1 calc R U . . .
C8 C 0.52395(11) 0.88657(16) 0.14097(6) 0.0264(3) Uani 1 1 d . . . . .
C9 C 0.52886(11) 0.79187(16) 0.20228(6) 0.0301(3) Uani 1 1 d . . . . .
H9 H 0.5384 0.8516 0.2420 0.036 Uiso 1 1 calc R U . . .
C10 C 0.62927(12) 0.69160(17) 0.20704(6) 0.0303(3) Uani 1 1 d . . . . .
C11 C 0.61775(12) 0.55968(18) 0.18050(7) 0.0354(3) Uani 1 1 d . . . . .
H11 H 0.5446 0.5279 0.1609 0.042 Uiso 1 1 calc R U . . .
C12 C 0.71258(13) 0.47376(18) 0.18237(8) 0.0371(3) Uani 1 1 d . . . . .
H12 H 0.7049 0.3830 0.1647 0.045 Uiso 1 1 calc R U . . .
C13 C 0.81837(12) 0.52300(17) 0.21047(7) 0.0332(3) Uani 1 1 d . . . . .
C14 C 0.83244(12) 0.65188(17) 0.23852(7) 0.0347(3) Uani 1 1 d . . . . .
H14 H 0.9057 0.6827 0.2584 0.042 Uiso 1 1 calc R U . . .
C15 C 0.73693(12) 0.73549(17) 0.23696(7) 0.0337(3) Uani 1 1 d . . . . .
H15 H 0.7448 0.8244 0.2566 0.040 Uiso 1 1 calc R U . . .
C16 C 0.41578(12) 1.08420(16) 0.07925(7) 0.0307(3) Uani 1 1 d . . . . .
H16A H 0.4943 1.1010 0.0698 0.037 Uiso 1 1 calc R U . . .
H16B H 0.3724 1.0369 0.0411 0.037 Uiso 1 1 calc R U . . .
C17 C 0.35952(12) 1.22181(16) 0.08875(7) 0.0313(3) Uani 1 1 d . . . . .
C18 C 0.21806(13) 1.38411(18) 0.03196(8) 0.0397(4) Uani 1 1 d . . . . .
C19 C 0.15078(19) 1.3728(2) -0.03583(10) 0.0646(6) Uani 1 1 d . . . . .
H19A H 0.2035 1.3551 -0.0671 0.097 Uiso 1 1 calc R U . . .
H19B H 0.1096 1.4596 -0.0471 0.097 Uiso 1 1 calc R U . . .
H19C H 0.0958 1.2966 -0.0372 0.097 Uiso 1 1 calc R U . . .
C20 C 0.30052(18) 1.5043(2) 0.03628(11) 0.0581(5) Uani 1 1 d . . . . .
H20A H 0.3418 1.5110 0.0806 0.087 Uiso 1 1 calc R U . . .
H20B H 0.2580 1.5901 0.0251 0.087 Uiso 1 1 calc R U . . .
H20C H 0.3553 1.4897 0.0059 0.087 Uiso 1 1 calc R U . . .
C21 C 0.13996(17) 1.3883(2) 0.08370(11) 0.0589(5) Uani 1 1 d . . . . .
H21A H 0.0902 1.3067 0.0794 0.088 Uiso 1 1 calc R U . . .
H21B H 0.0929 1.4722 0.0782 0.088 Uiso 1 1 calc R U . . .
H21C H 0.1864 1.3889 0.1268 0.088 Uiso 1 1 calc R U . . .
C22 C 0.50928(11) 0.80186(16) 0.08122(7) 0.0281(3) Uani 1 1 d . . . . .
C23 C 0.63367(11) 0.97307(16) 0.14773(7) 0.0307(3) Uani 1 1 d . . . . .
C24 C 0.8045(5) 1.0212(7) 0.0979(3) 0.0562(13) Uani 0.577(4) 1 d D U P A 1
H24A H 0.8541 0.9621 0.0750 0.067 Uiso 0.577(4) 1 calc R U P A 1
H24B H 0.8448 1.0396 0.1422 0.067 Uiso 0.577(4) 1 calc R U P A 1
C25 C 0.7800(3) 1.1555(5) 0.06182(18) 0.0572(8) Uani 0.577(4) 1 d D U P A 1
H25A H 0.8514 1.2074 0.0624 0.086 Uiso 0.577(4) 1 calc R U P A 1
H25B H 0.7261 1.2104 0.0828 0.086 Uiso 0.577(4) 1 calc R U P A 1
H25C H 0.7465 1.1362 0.0168 0.086 Uiso 0.577(4) 1 calc R U P A 1
C24' C 0.7978(8) 1.0401(11) 0.1150(4) 0.0562(13) Uani 0.423(4) 1 d D . P A 2
H24C H 0.8618 0.9885 0.1403 0.067 Uiso 0.423(4) 1 calc R U P A 2
H24D H 0.7807 1.1219 0.1405 0.067 Uiso 0.423(4) 1 calc R U P A 2
C25' C 0.8292(5) 1.0842(7) 0.0515(2) 0.0572(8) Uani 0.423(4) 1 d D . P A 2
H25D H 0.9020 1.1346 0.0588 0.086 Uiso 0.423(4) 1 calc R U P A 2
H25E H 0.7692 1.1447 0.0292 0.086 Uiso 0.423(4) 1 calc R U P A 2
H25F H 0.8370 1.0025 0.0246 0.086 Uiso 0.423(4) 1 calc R U P A 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
O1 N3 1.220(2) . ?
O2 N3 1.2197(19) . ?
O3 C17 1.2028(19) . ?
O4 C17 1.3355(17) . ?
O4 C18 1.4807(19) . ?
O5 C23 1.1998(19) . ?
O6 C23 1.3144(18) . ?
O6 C24 1.468(6) . ?
O6 C24' 1.478(8) . ?
N1 C1 1.3894(19) . ?
N1 C9 1.4477(19) . ?
N2 C22 1.140(2) . ?
N3 C13 1.4767(19) . ?
C1 C6 1.399(2) . ?
C1 C2 1.401(2) . ?
C2 C3 1.374(2) . ?
C3 C4 1.378(3) . ?
C4 C5 1.382(2) . ?
C5 C6 1.392(2) . ?
C6 C7 1.5136(19) . ?
C7 C16 1.5360(19) . ?
C7 C8 1.5532(18) . ?
C8 C22 1.4779(19) . ?
C8 C23 1.5313(19) . ?
C8 C9 1.5648(19) . ?
C9 C10 1.5235(19) . ?
C10 C11 1.388(2) . ?
C10 C15 1.396(2) . ?
C11 C12 1.390(2) . ?
C12 C13 1.383(2) . ?
C13 C14 1.375(2) . ?
C14 C15 1.384(2) . ?
C16 C17 1.513(2) . ?
C18 C20 1.510(3) . ?
C18 C19 1.517(2) . ?
C18 C21 1.520(3) . ?
C24 C25 1.506(7) . ?
C24' C25' 1.488(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
C17 O4 C18 121.84(12) . . ?
C23 O6 C24 123.1(3) . . ?
C23 O6 C24' 106.8(3) . . ?
C1 N1 C9 121.96(13) . . ?
O2 N3 O1 123.29(14) . . ?
O2 N3 C13 118.44(15) . . ?
O1 N3 C13 118.27(14) . . ?
N1 C1 C6 121.52(13) . . ?
N1 C1 C2 118.90(14) . . ?
C6 C1 C2 119.50(13) . . ?
C3 C2 C1 120.79(16) . . ?
C2 C3 C4 120.05(15) . . ?
C3 C4 C5 119.64(15) . . ?
C4 C5 C6 121.67(16) . . ?
C5 C6 C1 118.32(14) . . ?
C5 C6 C7 121.73(14) . . ?
C1 C6 C7 119.93(12) . . ?
C6 C7 C16 114.18(11) . . ?
C6 C7 C8 109.92(12) . . ?
C16 C7 C8 110.50(11) . . ?
C22 C8 C23 111.79(11) . . ?
C22 C8 C7 109.44(11) . . ?
C23 C8 C7 107.34(12) . . ?
C22 C8 C9 110.39(12) . . ?
C23 C8 C9 108.44(11) . . ?
C7 C8 C9 109.35(10) . . ?
N1 C9 C10 111.30(13) . . ?
N1 C9 C8 107.99(11) . . ?
C10 C9 C8 111.02(11) . . ?
C11 C10 C15 119.04(14) . . ?
C11 C10 C9 121.94(13) . . ?
C15 C10 C9 118.98(14) . . ?
C10 C11 C12 120.43(14) . . ?
C13 C12 C11 118.69(15) . . ?
C14 C13 C12 122.39(14) . . ?
C14 C13 N3 118.60(13) . . ?
C12 C13 N3 119.01(15) . . ?
C13 C14 C15 118.18(14) . . ?
C14 C15 C10 121.22(15) . . ?
C17 C16 C7 113.06(11) . . ?
O3 C17 O4 126.27(15) . . ?
O3 C17 C16 123.35(13) . . ?
O4 C17 C16 110.38(12) . . ?
O4 C18 C20 110.38(13) . . ?
O4 C18 C19 101.39(14) . . ?
C20 C18 C19 110.77(17) . . ?
O4 C18 C21 108.76(14) . . ?
C20 C18 C21 113.05(17) . . ?
C19 C18 C21 111.85(16) . . ?
N2 C22 C8 176.82(15) . . ?
O5 C23 O6 125.46(14) . . ?
O5 C23 C8 121.07(13) . . ?
O6 C23 C8 113.46(12) . . ?
O6 C24 C25 108.7(5) . . ?
O6 C24' C25' 107.5(6) . . ?

_refine_diff_density_max         0.248
_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_ic18555
_database_code_depnum_ccdc_archive 'CCDC 1834305'
loop_
_audit_author_name
_audit_author_address
'Gene-Hsiang Lee'
;National Taiwan university
Taiwan
;
_audit_update_record             
;
2018-04-03 deposited with the CCDC.	2020-03-27 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         ?
_chemical_formula_sum            'C25 H27 N3 O6'
_chemical_formula_weight         465.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.4969(2)
_cell_length_b                   12.7230(3)
_cell_length_c                   20.1047(5)
_cell_angle_alpha                89.5889(12)
_cell_angle_beta                 87.0347(11)
_cell_angle_gamma                88.2917(12)
_cell_volume                     2424.86(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      4.10
_cell_measurement_theta_max      70.11

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.086
_exptl_absorpt_coefficient_mu    0.760
_shelx_estimated_absorpt_T_min   0.907
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6439
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15799
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.475
_diffrn_reflns_theta_max         69.998
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             9164
_reflns_number_gt                7652
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_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)+(0.0517P)²+1.0398P] 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         9164
_refine_ls_number_parameters     644
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1267
_refine_ls_wR_factor_gt          0.1169
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.037
_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
O1 O 0.85473(15) 0.25938(15) 0.10163(7) 0.0686(4) Uani 1 1 d . . . . .
O2 O 0.63543(13) 0.22358(11) 0.14101(6) 0.0507(3) Uani 1 1 d . . . . .
O3 O 0.86971(13) 0.08200(11) 0.21797(7) 0.0511(3) Uani 1 1 d . . . . .
O4 O 1.09609(15) 0.09344(14) 0.18189(9) 0.0759(5) Uani 1 1 d D . . . .
O5 O 1.06040(16) -0.23806(11) 0.47644(7) 0.0567(3) Uani 1 1 d . U . . .
O6 O 1.25890(16) -0.16525(12) 0.48944(8) 0.0629(4) Uani 1 1 d . . . . .
N1 N 0.9689(2) 0.29379(13) 0.37060(8) 0.0588(5) Uani 1 1 d . . . . .
H1 H 0.959(2) 0.2855(19) 0.4127(13) 0.064(7) Uiso 1 1 d . . . . .
N2 N 1.27470(17) 0.25907(14) 0.26390(10) 0.0596(4) Uani 1 1 d . . . . .
N3 N 1.14106(16) -0.16500(12) 0.46761(7) 0.0439(3) Uani 1 1 d . U . . .
C1 C 0.96326(19) 0.39448(14) 0.34493(9) 0.0446(4) Uani 1 1 d . . . . .
C2 C 0.9782(2) 0.48019(16) 0.38696(11) 0.0552(5) Uani 1 1 d . . . . .
H2 H 0.9840 0.4688 0.4335 0.066 Uiso 1 1 calc R U . . .
C3 C 0.9847(2) 0.58031(16) 0.36183(13) 0.0619(6) Uani 1 1 d . . . . .
H3 H 0.9956 0.6376 0.3910 0.074 Uiso 1 1 calc R U . . .
C4 C 0.9756(2) 0.59873(16) 0.29440(13) 0.0604(5) Uani 1 1 d . . . . .
H4A H 0.9815 0.6681 0.2769 0.073 Uiso 1 1 calc R U . . .
C5 C 0.95778(19) 0.51454(15) 0.25271(10) 0.0506(4) Uani 1 1 d . . . . .
H5A H 0.9499 0.5271 0.2064 0.061 Uiso 1 1 calc R U . . .
C6 C 0.95113(17) 0.41224(14) 0.27678(9) 0.0408(4) Uani 1 1 d . . . . .
C7 C 0.93451(17) 0.32189(14) 0.22965(8) 0.0396(4) Uani 1 1 d . . . . .
H7 H 0.9887 0.3390 0.1872 0.048 Uiso 1 1 calc R U . . .
C8 C 1.00589(16) 0.22056(13) 0.25930(8) 0.0378(3) Uani 1 1 d . . . . .
C9 C 0.94152(18) 0.20220(13) 0.33158(8) 0.0402(4) Uani 1 1 d . . . . .
H9 H 0.8371 0.1963 0.3294 0.048 Uiso 1 1 calc R U . . .
C10 C 0.77974(17) 0.30960(15) 0.21265(8) 0.0433(4) Uani 1 1 d . . . . .
H10A H 0.7323 0.2655 0.2473 0.052 Uiso 1 1 calc R U . . .
H10B H 0.7316 0.3797 0.2135 0.052 Uiso 1 1 calc R U . . .
C11 C 0.76369(18) 0.26058(16) 0.14553(8) 0.0459(4) Uani 1 1 d . . . . .
C12 C 0.5910(2) 0.17635(19) 0.07866(10) 0.0592(5) Uani 1 1 d . . . . .
C13 C 0.4411(3) 0.1467(3) 0.09711(13) 0.0885(9) Uani 1 1 d . . . . .
H13A H 0.4407 0.0953 0.1336 0.133 Uiso 1 1 calc R U . . .
H13B H 0.3994 0.1161 0.0584 0.133 Uiso 1 1 calc R U . . .
H13C H 0.3858 0.2097 0.1113 0.133 Uiso 1 1 calc R U . . .
C14 C 0.5924(3) 0.2588(2) 0.02428(11) 0.0800(8) Uani 1 1 d . . . . .
H14A H 0.5362 0.3207 0.0395 0.120 Uiso 1 1 calc R U . . .
H14B H 0.5523 0.2302 -0.0155 0.120 Uiso 1 1 calc R U . . .
H14C H 0.6898 0.2790 0.0135 0.120 Uiso 1 1 calc R U . . .
C15 C 0.6839(4) 0.0812(3) 0.06143(17) 0.1063(12) Uani 1 1 d . . . . .
H15A H 0.7787 0.1038 0.0473 0.159 Uiso 1 1 calc R U . . .
H15B H 0.6440 0.0427 0.0252 0.159 Uiso 1 1 calc R U . . .
H15C H 0.6895 0.0353 0.1006 0.159 Uiso 1 1 calc R U . . .
C16 C 0.98173(18) 0.12327(15) 0.21791(8) 0.0430(4) Uani 1 1 d . . . . .
C17 C 1.0906(5) 0.0063(3) 0.1357(2) 0.0632(11) Uani 0.668(6) 1 d D . P A 1
H17A H 1.1531 0.0169 0.0954 0.076 Uiso 0.668(6) 1 calc R U P A 1
H17B H 0.9932 -0.0047 0.1223 0.076 Uiso 0.668(6) 1 calc R U P A 1
C18 C 1.1439(8) -0.0839(4) 0.1785(3) 0.1030(19) Uani 0.668(6) 1 d D . P A 1
H18A H 1.1458 -0.1493 0.1529 0.155 Uiso 0.668(6) 1 calc R U P A 1
H18B H 1.2394 -0.0696 0.1916 0.155 Uiso 0.668(6) 1 calc R U P A 1
H18C H 1.0811 -0.0909 0.2183 0.155 Uiso 0.668(6) 1 calc R U P A 1
C17' C 1.0787(10) -0.0238(6) 0.1648(5) 0.0632(11) Uani 0.332(6) 1 d D . P A 2
H17C H 1.0377 -0.0610 0.2042 0.076 Uiso 0.332(6) 1 calc R U P A 2
H17D H 1.0129 -0.0291 0.1284 0.076 Uiso 0.332(6) 1 calc R U P A 2
C18' C 1.2116(12) -0.0728(8) 0.1446(8) 0.1030(19) Uani 0.332(6) 1 d D . P A 2
H18D H 1.1978 -0.1467 0.1340 0.155 Uiso 0.332(6) 1 calc R U P A 2
H18E H 1.2516 -0.0366 0.1051 0.155 Uiso 0.332(6) 1 calc R U P A 2
H18F H 1.2763 -0.0685 0.1808 0.155 Uiso 0.332(6) 1 calc R U P A 2
C19 C 1.15839(18) 0.24028(14) 0.26165(9) 0.0425(4) Uani 1 1 d . . . . .
C20 C 0.99900(17) 0.10394(13) 0.36498(8) 0.0373(3) Uani 1 1 d . . . . .
C21 C 0.91849(16) 0.01435(14) 0.36820(9) 0.0410(4) Uani 1 1 d . . . . .
H21 H 0.8310 0.0143 0.3474 0.049 Uiso 1 1 calc R U . . .
C22 C 0.96452(17) -0.07462(14) 0.40140(9) 0.0426(4) Uani 1 1 d . . . . .
H22 H 0.9090 -0.1355 0.4043 0.051 Uiso 1 1 calc R U . . .
C23 C 1.09290(16) -0.07285(13) 0.43014(8) 0.0369(3) Uani 1 1 d . . . . .
C24 C 1.17710(18) 0.01314(15) 0.42618(9) 0.0459(4) Uani 1 1 d . . . . .
H24 H 1.2666 0.0114 0.4452 0.055 Uiso 1 1 calc R U . . .
C25 C 1.12870(19) 0.10229(15) 0.39383(9) 0.0471(4) Uani 1 1 d . . . . .
H25 H 1.1847 0.1630 0.3913 0.056 Uiso 1 1 calc R U . . .
O7 O 0.62827(14) 0.78825(13) 0.10670(6) 0.0597(4) Uani 1 1 d . . . . .
O8 O 0.85215(12) 0.73683(11) 0.12618(6) 0.0494(3) Uani 1 1 d . . . . .
O9 O 0.62088(14) 0.59225(11) 0.20951(7) 0.0551(3) Uani 1 1 d . . . . .
O10 O 0.39590(17) 0.64303(15) 0.18745(9) 0.0502(4) Uani 0.777(2) 1 d . . P B 1
O10' O 0.3953(6) 0.5935(5) 0.2220(3) 0.0502(4) Uani 0.223(2) 1 d D . P B 2
O11 O 0.38054(19) 0.26092(11) 0.46262(9) 0.0694(4) Uani 1 1 d . . . . .
O12 O 0.21813(19) 0.36568(14) 0.50219(10) 0.0820(5) Uani 1 1 d . . . . .
N4 N 0.6072(2) 0.78193(13) 0.37971(9) 0.0602(5) Uani 1 1 d . . . . .
H4 H 0.622(3) 0.7653(19) 0.4200(13) 0.067(7) Uiso 1 1 d . . . . .
N5 N 0.24583(16) 0.77851(14) 0.31316(9) 0.0556(4) Uani 1 1 d . . . . .
N6 N 0.32505(18) 0.34851(12) 0.46816(8) 0.0509(4) Uani 1 1 d . . . . .
C26 C 0.58201(17) 0.88623(13) 0.36406(8) 0.0389(4) Uani 1 1 d . . . . .
C27 C 0.57775(18) 0.96232(16) 0.41389(9) 0.0462(4) Uani 1 1 d . . . . .
H27 H 0.5923 0.9418 0.4586 0.055 Uiso 1 1 calc R U . . .
C28 C 0.55269(18) 1.06656(16) 0.39887(10) 0.0501(5) Uani 1 1 d . . . . .
H28 H 0.5514 1.1177 0.4331 0.060 Uiso 1 1 calc R U . . .
C29 C 0.52939(19) 1.09729(15) 0.33434(11) 0.0522(5) Uani 1 1 d . . . . .
H29 H 0.5106 1.1692 0.3240 0.063 Uiso 1 1 calc R U . . .
C30 C 0.53379(18) 1.02183(14) 0.28469(9) 0.0452(4) Uani 1 1 d . . . . .
H30 H 0.5172 1.0428 0.2403 0.054 Uiso 1 1 calc R U . . .
C31 C 0.56169(15) 0.91689(13) 0.29838(8) 0.0358(3) Uani 1 1 d . . . . .
C32 C 0.56990(16) 0.83498(13) 0.24434(8) 0.0369(3) Uani 1 1 d . . . . .
H32 H 0.5079 0.8600 0.2084 0.044 Uiso 1 1 calc R U . . .
C33 C 0.50739(16) 0.73113(13) 0.27443(8) 0.0388(4) Uani 1 1 d . . . . .
C34 C 0.59263(18) 0.69476(14) 0.33536(9) 0.0428(4) Uani 1 1 d . . . . .
H34 H 0.6891 0.6711 0.3184 0.051 Uiso 1 1 calc R U . . .
C35 C 0.72048(17) 0.82037(15) 0.21331(8) 0.0404(4) Uani 1 1 d . . . . .
H35A H 0.7676 0.8887 0.2134 0.048 Uiso 1 1 calc R U . . .
H35B H 0.7742 0.7708 0.2413 0.048 Uiso 1 1 calc R U . . .
C36 C 0.72497(18) 0.77932(15) 0.14299(8) 0.0443(4) Uani 1 1 d . . . . .
C37 C 0.8868(2) 0.69950(19) 0.05763(9) 0.0586(5) Uani 1 1 d . . . . .
C38 C 0.8834(3) 0.7927(2) 0.01039(11) 0.0844(9) Uani 1 1 d . . . . .
H38A H 0.7879 0.8242 0.0114 0.127 Uiso 1 1 calc R U . . .
H38B H 0.9106 0.7692 -0.0349 0.127 Uiso 1 1 calc R U . . .
H38C H 0.9496 0.8450 0.0241 0.127 Uiso 1 1 calc R U . . .
C39 C 1.0364(2) 0.6557(2) 0.06233(12) 0.0701(6) Uani 1 1 d . . . . .
H39A H 1.0958 0.7101 0.0793 0.105 Uiso 1 1 calc R U . . .
H39B H 1.0736 0.6337 0.0181 0.105 Uiso 1 1 calc R U . . .
H39C H 1.0364 0.5951 0.0927 0.105 Uiso 1 1 calc R U . . .
C40 C 0.7894(3) 0.6130(3) 0.04029(14) 0.0873(9) Uani 1 1 d . . . . .
H40A H 0.7861 0.5605 0.0762 0.131 Uiso 1 1 calc R U . . .
H40B H 0.8245 0.5795 -0.0013 0.131 Uiso 1 1 calc R U . . .
H40C H 0.6944 0.6429 0.0348 0.131 Uiso 1 1 calc R U . . .
C41 C 0.51567(19) 0.64327(15) 0.22256(10) 0.0495(4) Uani 1 1 d . . . . .
C42 C 0.3910(3) 0.5639(2) 0.13407(14) 0.0609(7) Uani 0.777(2) 1 d . . P B 1
H42A H 0.3255 0.5887 0.1001 0.073 Uiso 0.777(2) 1 calc R U P B 1
H42B H 0.4859 0.5530 0.1120 0.073 Uiso 0.777(2) 1 calc R U P B 1
C43 C 0.3431(5) 0.4662(3) 0.1636(3) 0.0911(12) Uani 0.777(2) 1 d . . P B 1
H43A H 0.3392 0.4129 0.1288 0.137 Uiso 0.777(2) 1 calc R U P B 1
H43B H 0.4087 0.4420 0.1969 0.137 Uiso 0.777(2) 1 calc R U P B 1
H43C H 0.2488 0.4776 0.1851 0.137 Uiso 0.777(2) 1 calc R U P B 1
C42' C 0.4084(11) 0.5002(8) 0.1805(5) 0.0609(7) Uani 0.223(2) 1 d D . P B 2
H42C H 0.4290 0.4382 0.2088 0.073 Uiso 0.223(2) 1 calc R U P B 2
H42D H 0.4889 0.5078 0.1477 0.073 Uiso 0.223(2) 1 calc R U P B 2
C43' C 0.2801(15) 0.4821(15) 0.1449(10) 0.0911(12) Uani 0.223(2) 1 d D . P B 2
H43D H 0.2939 0.4187 0.1177 0.137 Uiso 0.223(2) 1 calc R U P B 2
H43E H 0.2004 0.4730 0.1772 0.137 Uiso 0.223(2) 1 calc R U P B 2
H43F H 0.2603 0.5426 0.1161 0.137 Uiso 0.223(2) 1 calc R U P B 2
C44 C 0.35884(17) 0.75622(14) 0.29581(9) 0.0417(4) Uani 1 1 d . . . . .
C45 C 0.52436(17) 0.60301(13) 0.37185(9) 0.0413(4) Uani 1 1 d . . . . .
C46 C 0.5741(2) 0.50104(15) 0.35955(10) 0.0497(4) Uani 1 1 d . . . . .
H46 H 0.6533 0.4889 0.3294 0.060 Uiso 1 1 calc R U . . .
C47 C 0.5092(2) 0.41687(14) 0.39084(10) 0.0517(4) Uani 1 1 d . . . . .
H47 H 0.5433 0.3469 0.3828 0.062 Uiso 1 1 calc R U . . .
C48 C 0.39401(18) 0.43669(13) 0.43388(9) 0.0422(4) Uani 1 1 d . . . . .
C49 C 0.34408(19) 0.53680(14) 0.44826(9) 0.0456(4) Uani 1 1 d . . . . .
H49 H 0.2654 0.5484 0.4787 0.055 Uiso 1 1 calc R U . . .
C50 C 0.41135(19) 0.62019(14) 0.41729(9) 0.0452(4) Uani 1 1 d . . . . .
H50 H 0.3797 0.6901 0.4273 0.054 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 C11 1.203(2) . ?
O2 C11 1.327(2) . ?
O2 C12 1.481(2) . ?
O3 C16 1.200(2) . ?
O4 C16 1.321(2) . ?
O4 C17 1.455(4) . ?
O4 C17' 1.548(7) . ?
O5 N3 1.228(2) . ?
O6 N3 1.223(2) . ?
N1 C1 1.378(3) . ?
N1 C9 1.447(2) . ?
N2 C19 1.140(2) . ?
N3 C23 1.464(2) . ?
C1 C6 1.397(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.369(3) . ?
C3 C4 1.381(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.387(3) . ?
C6 C7 1.512(2) . ?
C7 C10 1.539(2) . ?
C7 C8 1.567(2) . ?
C8 C19 1.480(2) . ?
C8 C16 1.526(2) . ?
C8 C9 1.566(2) . ?
C9 C20 1.516(2) . ?
C10 C11 1.507(2) . ?
C12 C15 1.509(4) . ?
C12 C14 1.509(3) . ?
C12 C13 1.510(3) . ?
C17 C18 1.520(7) . ?
C17' C18' 1.431(15) . ?
C20 C25 1.388(2) . ?
C20 C21 1.391(2) . ?
C21 C22 1.381(3) . ?
C22 C23 1.377(2) . ?
C23 C24 1.374(2) . ?
C24 C25 1.382(3) . ?
O7 C36 1.204(2) . ?
O8 C36 1.337(2) . ?
O8 C37 1.479(2) . ?
O9 C41 1.194(2) . ?
O10 C41 1.369(3) . ?
O10 C42 1.480(3) . ?
O10' C41 1.324(6) . ?
O10' C42' 1.456(8) . ?
O11 N6 1.222(2) . ?
O12 N6 1.210(2) . ?
N4 C26 1.378(2) . ?
N4 C34 1.442(2) . ?
N5 C44 1.140(2) . ?
N6 C48 1.466(2) . ?
C26 C31 1.396(2) . ?
C26 C27 1.396(2) . ?
C27 C28 1.375(3) . ?
C28 C29 1.379(3) . ?
C29 C30 1.388(3) . ?
C30 C31 1.382(2) . ?
C31 C32 1.508(2) . ?
C32 C35 1.537(2) . ?
C32 C33 1.569(2) . ?
C33 C44 1.480(2) . ?
C33 C41 1.532(2) . ?
C33 C34 1.563(2) . ?
C34 C45 1.518(2) . ?
C35 C36 1.509(2) . ?
C37 C40 1.513(4) . ?
C37 C38 1.515(3) . ?
C37 C39 1.518(3) . ?
C42 C43 1.449(5) . ?
C42' C43' 1.470(9) . ?
C45 C50 1.386(2) . ?
C45 C46 1.387(2) . ?
C46 C47 1.383(3) . ?
C47 C48 1.378(3) . ?
C48 C49 1.373(2) . ?
C49 C50 1.383(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
C11 O2 C12 121.45(14) . . ?
C16 O4 C17 119.9(2) . . ?
C16 O4 C17' 106.6(4) . . ?
C1 N1 C9 122.66(16) . . ?
O6 N3 O5 122.97(16) . . ?
O6 N3 C23 118.62(15) . . ?
O5 N3 C23 118.40(14) . . ?
N1 C1 C6 120.98(16) . . ?
N1 C1 C2 119.67(17) . . ?
C6 C1 C2 119.24(18) . . ?
C3 C2 C1 120.8(2) . . ?
C2 C3 C4 120.52(19) . . ?
C3 C4 C5 118.97(19) . . ?
C4 C5 C6 121.73(19) . . ?
C5 C6 C1 118.70(17) . . ?
C5 C6 C7 120.34(16) . . ?
C1 C6 C7 120.95(16) . . ?
C6 C7 C10 111.83(14) . . ?
C6 C7 C8 108.67(13) . . ?
C10 C7 C8 114.50(14) . . ?
C19 C8 C16 110.80(14) . . ?
C19 C8 C9 109.67(14) . . ?
C16 C8 C9 108.50(14) . . ?
C19 C8 C7 107.12(13) . . ?
C16 C8 C7 111.95(13) . . ?
C9 C8 C7 108.77(13) . . ?
N1 C9 C20 109.98(14) . . ?
N1 C9 C8 107.78(14) . . ?
C20 C9 C8 113.83(13) . . ?
C11 C10 C7 113.34(14) . . ?
O1 C11 O2 125.33(17) . . ?
O1 C11 C10 123.60(17) . . ?
O2 C11 C10 111.02(14) . . ?
O2 C12 C15 109.64(17) . . ?
O2 C12 C14 109.31(19) . . ?
C15 C12 C14 113.1(2) . . ?
O2 C12 C13 102.36(17) . . ?
C15 C12 C13 111.9(3) . . ?
C14 C12 C13 110.0(2) . . ?
O3 C16 O4 125.44(17) . . ?
O3 C16 C8 122.52(15) . . ?
O4 C16 C8 112.02(15) . . ?
O4 C17 C18 100.5(4) . . ?
C18' C17' O4 111.0(8) . . ?
N2 C19 C8 177.6(2) . . ?
C25 C20 C21 119.32(16) . . ?
C25 C20 C9 121.39(15) . . ?
C21 C20 C9 119.26(15) . . ?
C22 C21 C20 120.65(15) . . ?
C23 C22 C21 118.34(15) . . ?
C24 C23 C22 122.54(16) . . ?
C24 C23 N3 118.33(15) . . ?
C22 C23 N3 119.12(15) . . ?
C23 C24 C25 118.52(16) . . ?
C24 C25 C20 120.57(16) . . ?
C36 O8 C37 120.80(14) . . ?
C41 O10 C42 116.93(18) . . ?
C41 O10' C42' 111.6(6) . . ?
C26 N4 C34 125.29(16) . . ?
O12 N6 O11 122.71(17) . . ?
O12 N6 C48 118.91(16) . . ?
O11 N6 C48 118.35(17) . . ?
N4 C26 C31 120.45(16) . . ?
N4 C26 C27 120.13(16) . . ?
C31 C26 C27 119.42(16) . . ?
C28 C27 C26 120.64(17) . . ?
C27 C28 C29 120.34(17) . . ?
C28 C29 C30 119.13(18) . . ?
C31 C30 C29 121.55(17) . . ?
C30 C31 C26 118.89(15) . . ?
C30 C31 C32 121.74(15) . . ?
C26 C31 C32 119.37(15) . . ?
C31 C32 C35 111.81(13) . . ?
C31 C32 C33 107.97(13) . . ?
C35 C32 C33 113.58(14) . . ?
C44 C33 C41 110.56(14) . . ?
C44 C33 C34 110.41(14) . . ?
C41 C33 C34 108.76(14) . . ?
C44 C33 C32 106.66(14) . . ?
C41 C33 C32 110.85(14) . . ?
C34 C33 C32 109.59(13) . . ?
N4 C34 C45 110.94(15) . . ?
N4 C34 C33 109.94(14) . . ?
C45 C34 C33 111.56(14) . . ?
C36 C35 C32 113.26(13) . . ?
O7 C36 O8 125.38(16) . . ?
O7 C36 C35 123.94(15) . . ?
O8 C36 C35 110.61(14) . . ?
O8 C37 C40 110.23(18) . . ?
O8 C37 C38 108.89(18) . . ?
C40 C37 C38 113.8(2) . . ?
O8 C37 C39 102.38(16) . . ?
C40 C37 C39 110.3(2) . . ?
C38 C37 C39 110.6(2) . . ?
O9 C41 O10' 116.7(3) . . ?
O9 C41 O10 125.32(17) . . ?
O9 C41 C33 122.96(16) . . ?
O10' C41 C33 111.1(3) . . ?
O10 C41 C33 111.01(15) . . ?
C43 C42 O10 108.5(3) . . ?
O10' C42' C43' 112.4(10) . . ?
N5 C44 C33 177.76(19) . . ?
C50 C45 C46 119.44(16) . . ?
C50 C45 C34 120.44(15) . . ?
C46 C45 C34 120.12(16) . . ?
C47 C46 C45 120.39(17) . . ?
C48 C47 C46 118.55(16) . . ?
C49 C48 C47 122.48(16) . . ?
C49 C48 N6 118.19(16) . . ?
C47 C48 N6 119.28(16) . . ?
C48 C49 C50 118.26(16) . . ?
C49 C50 C45 120.82(16) . . ?

_refine_diff_density_max         0.474
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.037

