# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_1
_database_code_depnum_ccdc_archive 'CCDC 2015334'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-24T10:08:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H22 N4 O2'
_chemical_formula_sum            'C26 H22 N4 O2'
_chemical_formula_weight         422.47

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   13.1438(2)
_cell_length_b                   4.63066(7)
_cell_length_c                   35.1361(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.9688(17)
_cell_angle_gamma                90
_cell_volume                     2106.25(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    4494
_cell_measurement_theta_min      5.1140
_cell_measurement_theta_max      75.9840

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.053
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             888

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.38280
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_number            8324
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         5.112
_diffrn_reflns_theta_max         67.973
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             1927
_reflns_number_gt                1742
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SIR-2014 (Burla et al., 2015)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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+0.5985P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1927
_refine_ls_number_parameters     181
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1318
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.036


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'

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 0.37422(7) 0.57144(19) 0.11547(3) 0.0577(3) Uani 1 1 d . . . . .
N1 N 0.45002(8) 0.1497(2) 0.13781(3) 0.0534(3) Uani 1 1 d . . . . .
H1 H 0.445971 -0.035588 0.136904 0.064 Uiso 1 1 calc R U . . .
N2 N 0.29766(8) 0.1452(2) 0.09537(3) 0.0497(3) Uani 1 1 d . . . . .
H2 H 0.300808 -0.03909 0.098429 0.06 Uiso 1 1 calc R U . . .
C1 C 0.53591(9) 0.2779(3) 0.16197(4) 0.0473(3) Uani 1 1 d . . . . .
C2 C 0.63468(11) 0.2056(4) 0.15755(4) 0.0611(4) Uani 1 1 d . . . . .
H2A H 0.645216 0.073726 0.138659 0.073 Uiso 1 1 calc R U . . .
C3 C 0.71884(11) 0.3301(4) 0.18137(5) 0.0731(5) Uani 1 1 d . . . . .
H3 H 0.785519 0.280408 0.178332 0.088 Uiso 1 1 calc R U . . .
C4 C 0.70444(12) 0.5245(4) 0.20918(5) 0.0729(5) Uani 1 1 d . . . . .
H4 H 0.760944 0.607768 0.224956 0.087 Uiso 1 1 calc R U . . .
C5 C 0.60659(14) 0.5955(4) 0.21361(5) 0.0767(5) Uani 1 1 d . . . . .
H5 H 0.596535 0.728304 0.23246 0.092 Uiso 1 1 calc R U . . .
C6 C 0.52188(12) 0.4721(4) 0.19035(5) 0.0638(4) Uani 1 1 d . . . . .
H6 H 0.455465 0.520271 0.193884 0.077 Uiso 1 1 calc R U . . .
C7 C 0.37392(8) 0.3063(3) 0.11605(3) 0.0432(3) Uani 1 1 d . . . . .
C8 C 0.21304(9) 0.2585(2) 0.06906(3) 0.0424(3) Uani 1 1 d . . . . .
C11 C 0.04471(8) 0.4510(3) 0.01463(3) 0.0445(3) Uani 1 1 d D . . . .
C9 C 0.1131(3) 0.2169(8) 0.07450(12) 0.0456(8) Uani 0.51 1 d . . P A 1
H9 H 0.101073 0.126371 0.096925 0.055 Uiso 0.51 1 calc R U P A 1
C10 C 0.0300(5) 0.3067(10) 0.04737(13) 0.0460(10) Uani 0.51 1 d D . P A 1
H10 H -0.036833 0.268642 0.051373 0.055 Uiso 0.51 1 calc R U P A 1
C12 C 0.14651(16) 0.4775(7) 0.00780(9) 0.0487(6) Uani 0.51 1 d D . P A 1
H12 H 0.158111 0.55865 -0.01528 0.058 Uiso 0.51 1 calc R U P A 1
C13 C 0.2310(2) 0.3843(7) 0.03500(10) 0.0499(6) Uani 0.51 1 d . . P A 1
H13 H 0.298 0.406496 0.030292 0.06 Uiso 0.51 1 calc R U P A 1
C9' C 0.1197(4) 0.1155(9) 0.06478(13) 0.0497(9) Uani 0.49 1 d . . P A 2
H9' H 0.1127 -0.048303 0.07942 0.06 Uiso 0.49 1 calc R U P A 2
C10' C 0.0361(5) 0.2178(11) 0.03843(14) 0.0474(10) Uani 0.49 1 d . . P A 2
H10' H -0.027574 0.126473 0.03678 0.057 Uiso 0.49 1 calc R U P A 2
C12' C 0.13485(19) 0.6101(6) 0.02261(8) 0.0416(5) Uani 0.49 1 d . . P A 2
H12' H 0.138544 0.787907 0.010626 0.05 Uiso 0.49 1 calc R U P A 2
C13' C 0.2193(2) 0.5104(7) 0.04795(8) 0.0424(6) Uani 0.49 1 d . . P A 2
H13' H 0.281084 0.612443 0.051008 0.051 Uiso 0.49 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.2282(16) . ?
N1 H1 0.86 . ?
N1 C1 1.4198(15) . ?
N1 C7 1.3584(15) . ?
N2 H2 0.86 . ?
N2 C7 1.3554(14) . ?
N2 C8 1.4181(14) . ?
C1 C2 1.3752(19) . ?
C1 C6 1.379(2) . ?
C2 H2A 0.93 . ?
C2 C3 1.391(2) . ?
C3 H3 0.93 . ?
C3 C4 1.366(3) . ?
C4 H4 0.93 . ?
C4 C5 1.362(2) . ?
C5 H5 0.93 . ?
C5 C6 1.385(2) . ?
C6 H6 0.93 . ?
C8 C9 1.373(5) . ?
C8 C13 1.387(3) . ?
C8 C9' 1.379(5) . ?
C8 C13' 1.392(3) . ?
C11 C11 1.492(2) 5_565 ?
C11 C10 1.373(5) . ?
C11 C12 1.405(2) . ?
C11 C10' 1.382(5) . ?
C11 C12' 1.382(3) . ?
C9 H9 0.93 . ?
C9 C10 1.384(7) . ?
C10 H10 0.93 . ?
C12 H12 0.93 . ?
C12 C13 1.402(4) . ?
C13 H13 0.93 . ?
C9' H9' 0.93 . ?
C9' C10' 1.392(7) . ?
C10' H10' 0.93 . ?
C12' H12' 0.93 . ?
C12' C13' 1.376(4) . ?
C13' H13' 0.93 . ?

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 H1 118.5 . . ?
C7 N1 H1 118.5 . . ?
C7 N1 C1 123.04(10) . . ?
C7 N2 H2 117.6 . . ?
C7 N2 C8 124.71(10) . . ?
C8 N2 H2 117.6 . . ?
C2 C1 N1 119.96(13) . . ?
C2 C1 C6 119.17(13) . . ?
C6 C1 N1 120.87(12) . . ?
C1 C2 H2A 120 . . ?
C1 C2 C3 119.94(15) . . ?
C3 C2 H2A 120 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.61(15) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.3 . . ?
C5 C4 C3 119.42(14) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.76(16) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 120.09(14) . . ?
C1 C6 H6 120 . . ?
C5 C6 H6 120 . . ?
O1 C7 N1 122.60(10) . . ?
O1 C7 N2 123.07(10) . . ?
N2 C7 N1 114.34(11) . . ?
C9 C8 N2 121.2(2) . . ?
C9 C8 C13 119.2(2) . . ?
C13 C8 N2 119.12(15) . . ?
C9' C8 N2 118.4(2) . . ?
C9' C8 C13' 118.5(2) . . ?
C13' C8 N2 123.07(14) . . ?
C10 C11 C11 121.1(3) . 5_565 ?
C10 C11 C12 117.5(3) . . ?
C12 C11 C11 121.03(16) . 5_565 ?
C10' C11 C11 121.1(3) . 5_565 ?
C12' C11 C11 121.53(16) . 5_565 ?
C12' C11 C10' 116.8(3) . . ?
C8 C9 H9 119.3 . . ?
C8 C9 C10 121.5(4) . . ?
C10 C9 H9 119.3 . . ?
C11 C10 C9 121.0(5) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C11 C12 H12 119.3 . . ?
C13 C12 C11 121.5(2) . . ?
C13 C12 H12 119.3 . . ?
C8 C13 C12 119.0(2) . . ?
C8 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C8 C9' H9' 120.2 . . ?
C8 C9' C10' 119.6(4) . . ?
C10' C9' H9' 120.2 . . ?
C11 C10' C9' 122.0(5) . . ?
C11 C10' H10' 119 . . ?
C9' C10' H10' 119 . . ?
C11 C12' H12' 119.4 . . ?
C13' C12' C11 121.3(2) . . ?
C13' C12' H12' 119.4 . . ?
C8 C13' H13' 119.7 . . ?
C12' C13' C8 120.7(2) . . ?
C12' C13' H13' 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -179.65(13) . . . . ?
N1 C1 C6 C5 -179.86(14) . . . . ?
N2 C8 C9 C10 -174.7(3) . . . . ?
N2 C8 C13 C12 175.5(2) . . . . ?
N2 C8 C9' C10' -178.4(3) . . . . ?
N2 C8 C13' C12' 179.6(2) . . . . ?
C1 N1 C7 O1 0.54(19) . . . . ?
C1 N1 C7 N2 -179.00(12) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C1 C6 C5 1.0(2) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C4 C5 C6 C1 -0.9(3) . . . . ?
C6 C1 C2 C3 -0.5(2) . . . . ?
C7 N1 C1 C2 -124.51(15) . . . . ?
C7 N1 C1 C6 56.37(18) . . . . ?
C7 N2 C8 C9 -119.3(2) . . . . ?
C7 N2 C8 C13 68.3(2) . . . . ?
C7 N2 C8 C9' -148.0(2) . . . . ?
C7 N2 C8 C13' 30.7(2) . . . . ?
C8 N2 C7 O1 3.95(19) . . . . ?
C8 N2 C7 N1 -176.51(12) . . . . ?
C8 C9 C10 C11 -2.5(6) . . . . ?
C8 C9' C10' C11 3.6(6) . . . . ?
C11 C11 C10 C9 -179.8(3) 5_565 . . . ?
C11 C11 C12 C13 -179.6(2) 5_565 . . . ?
C11 C11 C10' C9' 177.3(3) 5_565 . . . ?
C11 C11 C12' C13' -176.1(2) 5_565 . . . ?
C11 C12 C13 C8 1.2(5) . . . . ?
C11 C12' C13' C8 -6.0(4) . . . . ?
C9 C8 C13 C12 2.9(4) . . . . ?
C10 C11 C12 C13 -5.8(4) . . . . ?
C12 C11 C10 C9 6.4(5) . . . . ?
C13 C8 C9 C10 -2.3(5) . . . . ?
C9' C8 C13' C12' -1.7(4) . . . . ?
C10' C11 C12' C13' 12.1(4) . . . . ?
C12' C11 C10' C9' -10.9(5) . . . . ?
C13' C8 C9' C10' 2.9(5) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
####################################################################### 
# 
# 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_1-((TBA)AcO)2-H2O
_database_code_depnum_ccdc_archive 'CCDC 2015335'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-17T19:16:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2014/7

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         
'C26 H22 N4 O2, 2(C16 H36 N), 2(C2 H3 O2), H2 O'
_chemical_formula_sum            'C62 H102 N6 O7'
_chemical_formula_weight         1043.49
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

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

_cell_length_a                   10.0943(7)
_cell_length_b                   16.7406(10)
_cell_length_c                   18.7190(12)
_cell_angle_alpha                90
_cell_angle_beta                 91.772(6)
_cell_angle_gamma                90
_cell_volume                     3161.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    2465
_cell_measurement_theta_min      4.7190
_cell_measurement_theta_max      22.4710

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.793
_exptl_crystal_size_mid          0.471
_exptl_crystal_size_min          0.203
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_F_000             1144

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.50098
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_number            13957
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.329
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.842
_reflns_Friedel_fraction_full    0.697
_reflns_Friedel_fraction_max     0.679
_reflns_Friedel_coverage         0.635
_reflns_number_total             10473
_reflns_number_gt                6486
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
'CrysAlisPro 1.171.37.35 (Agilent Technologies, 2014)'
_computing_cell_refinement       
'CrysAlisPro 1.171.37.35 (Agilent Technologies, 2014)'
_computing_data_reduction        
'CrysAlisPro 1.171.37.35 (Agilent Technologies, 2014)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1070P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10473
_refine_ls_number_parameters     689
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.1991
_refine_ls_wR_factor_gt          0.1625
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 1991 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(8)
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.045


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 1.0120(4) 0.5891(2) 0.2372(2) 0.0798(11) Uani 1 1 d . . . . .
H1N H 0.9625 0.5981 0.1999 0.096 Uiso 1 1 calc R U . . .
N2 N 0.8278(5) 0.6221(3) 0.2958(2) 0.0800(11) Uani 1 1 d . . . . .
H2N H 0.7976 0.632 0.2532 0.096 Uiso 1 1 calc R U . . .
N3 N 0.1536(4) 0.6220(2) 0.66994(19) 0.0702(10) Uani 1 1 d . . . . .
H3N H 0.1847 0.637 0.7111 0.084 Uiso 1 1 calc R U . . .
N4 N -0.0231(4) 0.5868(2) 0.73488(19) 0.0689(9) Uani 1 1 d . . . . .
H4N H 0.0298 0.5982 0.7703 0.083 Uiso 1 1 calc R U . . .
O1 O 1.0190(4) 0.5992(3) 0.3578(2) 0.1065(14) Uani 1 1 d . . . . .
O2 O -0.0375(4) 0.5790(2) 0.61320(17) 0.0814(9) Uani 1 1 d . . . . .
C1 C 1.1420(6) 0.5623(3) 0.2257(3) 0.0794(14) Uani 1 1 d . . . . .
C2 C 1.1897(6) 0.5717(4) 0.1578(3) 0.0896(15) Uani 1 1 d . . . . .
H2 H 1.1357 0.5946 0.1222 0.107 Uiso 1 1 calc R U . . .
C3 C 1.3144(7) 0.5479(4) 0.1420(4) 0.107(2) Uani 1 1 d . . . . .
H3 H 1.3452 0.5548 0.0961 0.129 Uiso 1 1 calc R U . . .
C4 C 1.3947(8) 0.5134(6) 0.1944(5) 0.125(3) Uani 1 1 d . . . . .
H4 H 1.4809 0.4983 0.1845 0.15 Uiso 1 1 calc R U . . .
C5 C 1.3470(8) 0.5019(5) 0.2600(5) 0.119(2) Uani 1 1 d . . . . .
H5 H 1.3997 0.4769 0.295 0.143 Uiso 1 1 calc R U . . .
C6 C 1.2213(7) 0.5267(4) 0.2760(4) 0.1004(18) Uani 1 1 d . . . . .
H6 H 1.1905 0.5189 0.3218 0.121 Uiso 1 1 calc R U . . .
C7 C 0.9573(6) 0.6022(3) 0.3020(3) 0.0793(14) Uani 1 1 d . . . . .
C8 C 0.7371(6) 0.6286(3) 0.3507(3) 0.0747(13) Uani 1 1 d . . . . .
C9 C 0.6052(6) 0.6367(3) 0.3308(3) 0.0836(15) Uani 1 1 d . . . . .
H9 H 0.5809 0.6397 0.2825 0.1 Uiso 1 1 calc R U . . .
C10 C 0.5088(6) 0.6405(3) 0.3811(2) 0.0810(14) Uani 1 1 d . . . . .
H10 H 0.4207 0.6454 0.3657 0.097 Uiso 1 1 calc R U . . .
C11 C 0.5380(6) 0.6373(3) 0.4539(2) 0.0712(12) Uani 1 1 d . . . . .
C12 C 0.6709(6) 0.6292(3) 0.4728(3) 0.0839(15) Uani 1 1 d . . . . .
H12 H 0.695 0.6262 0.5211 0.101 Uiso 1 1 calc R U . . .
C13 C 0.7702(6) 0.6253(3) 0.4232(3) 0.0873(15) Uani 1 1 d . . . . .
H13 H 0.8584 0.6205 0.4385 0.105 Uiso 1 1 calc R U . . .
C14 C 0.4336(5) 0.6379(3) 0.5076(2) 0.0693(12) Uani 1 1 d . . . . .
C15 C 0.3082(6) 0.6083(3) 0.4929(2) 0.0780(13) Uani 1 1 d . . . . .
H15 H 0.2874 0.5911 0.4467 0.094 Uiso 1 1 calc R U . . .
C16 C 0.2122(5) 0.6030(3) 0.5435(2) 0.0757(12) Uani 1 1 d . . . . .
H16 H 0.129 0.5825 0.5311 0.091 Uiso 1 1 calc R U . . .
C17 C 0.2396(5) 0.6284(3) 0.6132(2) 0.0659(11) Uani 1 1 d . . . . .
C18 C 0.3637(5) 0.6599(3) 0.6285(2) 0.0746(13) Uani 1 1 d . . . . .
H18 H 0.3841 0.6782 0.6745 0.089 Uiso 1 1 calc R U . . .
C19 C 0.4585(6) 0.6647(3) 0.5766(3) 0.0811(14) Uani 1 1 d . . . . .
H19 H 0.541 0.6866 0.5885 0.097 Uiso 1 1 calc R U . . .
C20 C 0.0263(5) 0.5947(2) 0.6679(2) 0.0636(11) Uani 1 1 d . . . . .
C21 C -0.1500(5) 0.5621(2) 0.7516(3) 0.0657(12) Uani 1 1 d . . . . .
C22 C -0.2603(6) 0.5650(3) 0.7056(3) 0.0810(14) Uani 1 1 d . . . . .
H22 H -0.2514 0.5816 0.6586 0.097 Uiso 1 1 calc R U . . .
C23 C -0.3836(6) 0.5432(3) 0.7295(4) 0.0945(18) Uani 1 1 d . . . . .
H23 H -0.4566 0.5454 0.6981 0.113 Uiso 1 1 calc R U . . .
C24 C -0.4004(7) 0.5186(4) 0.7977(4) 0.1029(19) Uani 1 1 d . . . . .
H24 H -0.484 0.5044 0.813 0.123 Uiso 1 1 calc R U . . .
C25 C -0.2917(7) 0.5149(4) 0.8440(4) 0.1030(18) Uani 1 1 d . . . . .
H25 H -0.3018 0.4977 0.8907 0.124 Uiso 1 1 calc R U . . .
C26 C -0.1682(6) 0.5364(3) 0.8214(3) 0.0834(15) Uani 1 1 d . . . . .
H26 H -0.0958 0.5338 0.8532 0.1 Uiso 1 1 calc R U . . .
N1A N 0.1187(4) 0.8375(2) 0.3901(2) 0.0693(10) Uani 1 1 d . . . . .
C1A C 0.1729(6) 0.7806(3) 0.3355(3) 0.0797(14) Uani 1 1 d . . . . .
H1AA H 0.1017 0.7457 0.319 0.096 Uiso 1 1 calc R U . . .
H1AB H 0.2399 0.7475 0.3591 0.096 Uiso 1 1 calc R U . . .
C2A C 0.2331(7) 0.8189(4) 0.2711(3) 0.1035(19) Uani 1 1 d . . . . .
H2AA H 0.1655 0.8489 0.2447 0.124 Uiso 1 1 calc R U . . .
H2AB H 0.3019 0.856 0.2868 0.124 Uiso 1 1 calc R U . . .
C3A C 0.2903(11) 0.7584(5) 0.2239(5) 0.145(3) Uani 1 1 d . U . . .
H3AA H 0.3572 0.7295 0.2518 0.174 Uiso 1 1 calc R U . . .
H3AB H 0.2206 0.7205 0.2115 0.174 Uiso 1 1 calc R U . . .
C4A C 0.3498(13) 0.7826(6) 0.1583(5) 0.181(5) Uani 1 1 d . . . . .
H4AA H 0.2823 0.7872 0.1212 0.272 Uiso 1 1 calc R U . . .
H4AB H 0.4138 0.7434 0.1448 0.272 Uiso 1 1 calc R U . . .
H4AC H 0.3928 0.8333 0.1651 0.272 Uiso 1 1 calc R U . . .
C5A C 0.0073(5) 0.8872(3) 0.3575(3) 0.0775(14) Uani 1 1 d . . . . .
H5AA H -0.0208 0.925 0.3932 0.093 Uiso 1 1 calc R U . . .
H5AB H 0.0423 0.9177 0.3183 0.093 Uiso 1 1 calc R U . . .
C6A C -0.1131(5) 0.8425(3) 0.3299(3) 0.0854(15) Uani 1 1 d . . . . .
H6AA H -0.1426 0.8061 0.3665 0.102 Uiso 1 1 calc R U . . .
H6AB H -0.0902 0.8112 0.2885 0.102 Uiso 1 1 calc R U . . .
C7A C -0.2238(6) 0.8994(4) 0.3096(4) 0.1034(19) Uani 1 1 d . . . . .
H7AA H -0.194 0.9354 0.2728 0.124 Uiso 1 1 calc R U . . .
H7AB H -0.2452 0.9313 0.3509 0.124 Uiso 1 1 calc R U . . .
C8A C -0.3479(7) 0.8563(5) 0.2824(5) 0.132(3) Uani 1 1 d . . . . .
H8AA H -0.3285 0.827 0.2399 0.198 Uiso 1 1 calc R U . . .
H8AB H -0.4165 0.8946 0.2718 0.198 Uiso 1 1 calc R U . . .
H8AC H -0.377 0.8199 0.3184 0.198 Uiso 1 1 calc R U . . .
C9A C 0.0702(5) 0.7876(3) 0.4513(3) 0.0768(13) Uani 1 1 d . . . . .
H9AA H 0.0135 0.7457 0.4316 0.092 Uiso 1 1 calc R U . . .
H9AB H 0.1461 0.7619 0.4745 0.092 Uiso 1 1 calc R U . . .
C10A C -0.0043(7) 0.8311(4) 0.5067(3) 0.0969(17) Uani 1 1 d . . . . .
H10A H -0.0826 0.8558 0.485 0.116 Uiso 1 1 calc R U . . .
H10B H 0.0509 0.873 0.5276 0.116 Uiso 1 1 calc R U . . .
C11A C -0.0447(8) 0.7730(5) 0.5646(3) 0.116(2) Uani 1 1 d . . . . .
H11A H -0.0915 0.7284 0.5423 0.139 Uiso 1 1 calc R U . . .
H11B H 0.0346 0.7521 0.5885 0.139 Uiso 1 1 calc R U . . .
C12A C -0.1309(9) 0.8095(7) 0.6191(4) 0.150(3) Uani 1 1 d . . . . .
H12A H -0.0846 0.8529 0.6423 0.226 Uiso 1 1 calc R U . . .
H12B H -0.1528 0.77 0.6539 0.226 Uiso 1 1 calc R U . . .
H12C H -0.2107 0.8292 0.5961 0.226 Uiso 1 1 calc R U . . .
C13A C 0.2257(5) 0.8954(3) 0.4163(3) 0.0748(13) Uani 1 1 d . . . . .
H13A H 0.2493 0.9291 0.3766 0.09 Uiso 1 1 calc R U . . .
H13B H 0.1881 0.9297 0.4522 0.09 Uiso 1 1 calc R U . . .
C14A C 0.3507(5) 0.8589(3) 0.4476(3) 0.0855(15) Uani 1 1 d . . . . .
H14A H 0.3305 0.8308 0.4913 0.103 Uiso 1 1 calc R U . . .
H14B H 0.3847 0.8202 0.4142 0.103 Uiso 1 1 calc R U . . .
C15A C 0.4546(6) 0.9205(4) 0.4637(4) 0.105(2) Uani 1 1 d . . . . .
H15A H 0.4182 0.961 0.4944 0.125 Uiso 1 1 calc R U . . .
H15B H 0.4785 0.9462 0.4194 0.125 Uiso 1 1 calc R U . . .
C16A C 0.5779(7) 0.8862(5) 0.4995(5) 0.129(3) Uani 1 1 d . . . . .
H16A H 0.5564 0.8646 0.5452 0.193 Uiso 1 1 calc R U . . .
H16B H 0.643 0.9276 0.5059 0.193 Uiso 1 1 calc R U . . .
H16C H 0.6127 0.8446 0.4701 0.193 Uiso 1 1 calc R U . . .
N1B N -0.0705(4) 0.3541(2) 0.1215(2) 0.0698(10) Uani 1 1 d . . . . .
C1B C -0.1926(5) 0.3140(3) 0.0882(3) 0.0783(13) Uani 1 1 d . . . . .
H1BA H -0.1651 0.282 0.048 0.094 Uiso 1 1 calc R U . . .
H1BB H -0.2285 0.2778 0.1231 0.094 Uiso 1 1 calc R U . . .
C2B C -0.3014(6) 0.3688(4) 0.0625(4) 0.0956(17) Uani 1 1 d . . . . .
H2BA H -0.3285 0.4022 0.1018 0.115 Uiso 1 1 calc R U . . .
H2BB H -0.2683 0.4035 0.0255 0.115 Uiso 1 1 calc R U . . .
C3B C -0.4182(6) 0.3234(5) 0.0335(4) 0.115(2) Uani 1 1 d . . . . .
H3BA H -0.4527 0.2903 0.0712 0.138 Uiso 1 1 calc R U . . .
H3BB H -0.3897 0.2883 -0.0043 0.138 Uiso 1 1 calc R U . . .
C4B C -0.5279(8) 0.3770(7) 0.0043(6) 0.157(3) Uani 1 1 d . . . . .
H4BA H -0.5766 0.3985 0.0432 0.235 Uiso 1 1 calc R U . . .
H4BB H -0.5866 0.3466 -0.0265 0.235 Uiso 1 1 calc R U . . .
H4BC H -0.4902 0.42 -0.0223 0.235 Uiso 1 1 calc R U . . .
C5B C -0.1081(6) 0.4024(3) 0.1857(3) 0.0841(15) Uani 1 1 d . . . . .
H5BA H -0.0273 0.4229 0.2084 0.101 Uiso 1 1 calc R U . . .
H5BB H -0.1596 0.448 0.169 0.101 Uiso 1 1 calc R U . . .
C6B C -0.1845(8) 0.3605(4) 0.2409(4) 0.115(2) Uani 1 1 d . . . . .
H6BA H -0.1305 0.3183 0.2623 0.138 Uiso 1 1 calc R U . . .
H6BB H -0.2626 0.3361 0.2187 0.138 Uiso 1 1 calc R U . . .
C7B C -0.2261(10) 0.4180(5) 0.2985(4) 0.137(3) Uani 1 1 d . . . . .
H7BA H -0.1467 0.4354 0.3245 0.165 Uiso 1 1 calc R U . . .
H7BB H -0.2643 0.4646 0.2751 0.165 Uiso 1 1 calc R U . . .
C8B C -0.3169(10) 0.3906(7) 0.3489(6) 0.158(3) Uani 1 1 d . . . . .
H8BA H -0.3979 0.3749 0.3246 0.237 Uiso 1 1 calc R U . . .
H8BB H -0.3348 0.4327 0.3821 0.237 Uiso 1 1 calc R U . . .
H8BC H -0.2798 0.3456 0.3742 0.237 Uiso 1 1 calc R U . . .
C9B C 0.0281(5) 0.2888(3) 0.1421(3) 0.0771(13) Uani 1 1 d . . . . .
H9BA H 0.0443 0.2568 0.1 0.092 Uiso 1 1 calc R U . . .
H9BB H -0.0119 0.2542 0.177 0.092 Uiso 1 1 calc R U . . .
C10B C 0.1610(6) 0.3182(3) 0.1729(3) 0.0861(15) Uani 1 1 d . . . . .
H10C H 0.195 0.3598 0.1424 0.103 Uiso 1 1 calc R U . . .
H10D H 0.1485 0.341 0.2198 0.103 Uiso 1 1 calc R U . . .
C11B C 0.2597(7) 0.2518(4) 0.1788(5) 0.116(2) Uani 1 1 d . . . . .
H11C H 0.2206 0.2082 0.2049 0.14 Uiso 1 1 calc R U . . .
H11D H 0.277 0.2326 0.1311 0.14 Uiso 1 1 calc R U . . .
C12B C 0.3884(7) 0.2734(5) 0.2148(4) 0.123(2) Uani 1 1 d . . . . .
H12D H 0.4332 0.3122 0.1865 0.184 Uiso 1 1 calc R U . . .
H12E H 0.4425 0.2264 0.22 0.184 Uiso 1 1 calc R U . . .
H12F H 0.3725 0.2954 0.2611 0.184 Uiso 1 1 calc R U . . .
C13B C -0.0101(6) 0.4122(3) 0.0690(3) 0.0876(16) Uani 1 1 d . . . . .
H13C H -0.0748 0.4533 0.0571 0.105 Uiso 1 1 calc R U . . .
H13D H 0.0657 0.4381 0.0923 0.105 Uiso 1 1 calc R U . . .
C14B C 0.0341(9) 0.3738(5) 0.0006(4) 0.125(2) Uani 1 1 d . . . . .
H14C H 0.0929 0.3297 0.013 0.15 Uiso 1 1 calc R U . . .
H14D H -0.0431 0.3515 -0.0243 0.15 Uiso 1 1 calc R U . . .
C15B C 0.0983(11) 0.4238(7) -0.0459(5) 0.162(4) Uani 1 1 d . . . . .
H15C H 0.1798 0.4423 -0.0226 0.195 Uiso 1 1 calc R U . . .
H15D H 0.0428 0.4702 -0.0552 0.195 Uiso 1 1 calc R U . . .
C16B C 0.1316(13) 0.3855(8) -0.1175(5) 0.189(5) Uani 1 1 d . . . . .
H16D H 0.2089 0.3525 -0.1112 0.284 Uiso 1 1 calc R U . . .
H16E H 0.1486 0.4266 -0.1517 0.284 Uiso 1 1 calc R U . . .
H16F H 0.0583 0.3534 -0.1343 0.284 Uiso 1 1 calc R U . . .
O1A O 0.8734(5) 0.6027(3) 0.1023(2) 0.1172(15) Uani 1 1 d . . . . .
O2A O 0.7020(5) 0.6016(5) 0.1621(3) 0.170(2) Uani 1 1 d . U . . .
C17A C 0.7566(7) 0.6143(4) 0.1066(3) 0.0985(18) Uani 1 1 d . . . . .
C18A C 0.6704(8) 0.6328(7) 0.0424(4) 0.149(3) Uani 1 1 d . . . . .
H18A H 0.6915 0.5972 0.0042 0.224 Uiso 1 1 calc R U . . .
H18B H 0.6852 0.687 0.0278 0.224 Uiso 1 1 calc R U . . .
H18C H 0.5791 0.6261 0.054 0.224 Uiso 1 1 calc R U . . .
O1B O 0.1290(4) 0.6001(3) 0.86316(19) 0.1035(12) Uani 1 1 d . . . . .
O2B O 0.2877(4) 0.6465(4) 0.8007(2) 0.1207(16) Uani 1 1 d . . . . .
C17B C 0.2471(5) 0.6163(3) 0.8553(3) 0.0760(13) Uani 1 1 d . . . . .
C18B C 0.3427(6) 0.6029(5) 0.9174(3) 0.1040(19) Uani 1 1 d . . . . .
H18D H 0.3527 0.5466 0.9258 0.156 Uiso 1 1 calc R U . . .
H18E H 0.3092 0.6279 0.9593 0.156 Uiso 1 1 calc R U . . .
H18F H 0.4271 0.6257 0.9069 0.156 Uiso 1 1 calc R U . . .
O3 O 1.0342(6) 0.6631(3) -0.0040(3) 0.1320(17) Uani 1 1 d G . . . .
H3A H 0.9669 0.6438 0.0161 0.198 Uiso 1 1 d G U . . .
H3B H 1.0604 0.6306 -0.0355 0.198 Uiso 1 1 d G U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.366(6) . ?
N1 C1 1.409(7) . ?
N1 H1N 0.86 . ?
N2 C7 1.350(7) . ?
N2 C8 1.401(6) . ?
N2 H2N 0.86 . ?
N3 C20 1.363(6) . ?
N3 C17 1.397(6) . ?
N3 H3N 0.86 . ?
N4 C20 1.370(5) . ?
N4 C21 1.390(6) . ?
N4 H4N 0.86 . ?
O1 C7 1.201(6) . ?
O2 C20 1.221(5) . ?
C1 C6 1.355(9) . ?
C1 C2 1.383(8) . ?
C2 C3 1.361(9) . ?
C2 H2 0.93 . ?
C3 C4 1.380(11) . ?
C3 H3 0.93 . ?
C4 C5 1.346(11) . ?
C4 H4 0.93 . ?
C5 C6 1.377(10) . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
C8 C9 1.379(7) . ?
C8 C13 1.390(7) . ?
C9 C10 1.377(7) . ?
C9 H9 0.93 . ?
C10 C11 1.387(7) . ?
C10 H10 0.93 . ?
C11 C12 1.383(8) . ?
C11 C14 1.478(7) . ?
C12 C13 1.388(7) . ?
C12 H12 0.93 . ?
C13 H13 0.93 . ?
C14 C15 1.379(7) . ?
C14 C19 1.385(6) . ?
C15 C16 1.378(7) . ?
C15 H15 0.93 . ?
C16 C17 1.392(6) . ?
C16 H16 0.93 . ?
C17 C18 1.381(7) . ?
C18 C19 1.387(7) . ?
C18 H18 0.93 . ?
C19 H19 0.93 . ?
C21 C22 1.388(7) . ?
C21 C26 1.392(7) . ?
C22 C23 1.384(8) . ?
C22 H22 0.93 . ?
C23 C24 1.358(9) . ?
C23 H23 0.93 . ?
C24 C25 1.378(9) . ?
C24 H24 0.93 . ?
C25 C26 1.377(8) . ?
C25 H25 0.93 . ?
C26 H26 0.93 . ?
N1A C1A 1.511(6) . ?
N1A C9A 1.512(6) . ?
N1A C5A 1.512(6) . ?
N1A C13A 1.522(6) . ?
C1A C2A 1.510(8) . ?
C1A H1AA 0.97 . ?
C1A H1AB 0.97 . ?
C2A C3A 1.474(9) . ?
C2A H2AA 0.97 . ?
C2A H2AB 0.97 . ?
C3A C4A 1.441(11) . ?
C3A H3AA 0.97 . ?
C3A H3AB 0.97 . ?
C4A H4AA 0.96 . ?
C4A H4AB 0.96 . ?
C4A H4AC 0.96 . ?
C5A C6A 1.504(7) . ?
C5A H5AA 0.97 . ?
C5A H5AB 0.97 . ?
C6A C7A 1.508(8) . ?
C6A H6AA 0.97 . ?
C6A H6AB 0.97 . ?
C7A C8A 1.520(10) . ?
C7A H7AA 0.97 . ?
C7A H7AB 0.97 . ?
C8A H8AA 0.96 . ?
C8A H8AB 0.96 . ?
C8A H8AC 0.96 . ?
C9A C10A 1.491(8) . ?
C9A H9AA 0.97 . ?
C9A H9AB 0.97 . ?
C10A C11A 1.522(9) . ?
C10A H10A 0.97 . ?
C10A H10B 0.97 . ?
C11A C12A 1.492(10) . ?
C11A H11A 0.97 . ?
C11A H11B 0.97 . ?
C12A H12A 0.96 . ?
C12A H12B 0.96 . ?
C12A H12C 0.96 . ?
C13A C14A 1.504(7) . ?
C13A H13A 0.97 . ?
C13A H13B 0.97 . ?
C14A C15A 1.495(8) . ?
C14A H14A 0.97 . ?
C14A H14B 0.97 . ?
C15A C16A 1.508(9) . ?
C15A H15A 0.97 . ?
C15A H15B 0.97 . ?
C16A H16A 0.96 . ?
C16A H16B 0.96 . ?
C16A H16C 0.96 . ?
N1B C5B 1.507(6) . ?
N1B C1B 1.520(6) . ?
N1B C9B 1.520(6) . ?
N1B C13B 1.523(7) . ?
C1B C2B 1.499(8) . ?
C1B H1BA 0.97 . ?
C1B H1BB 0.97 . ?
C2B C3B 1.491(8) . ?
C2B H2BA 0.97 . ?
C2B H2BB 0.97 . ?
C3B C4B 1.515(11) . ?
C3B H3BA 0.97 . ?
C3B H3BB 0.97 . ?
C4B H4BA 0.96 . ?
C4B H4BB 0.96 . ?
C4B H4BC 0.96 . ?
C5B C6B 1.485(8) . ?
C5B H5BA 0.97 . ?
C5B H5BB 0.97 . ?
C6B C7B 1.514(9) . ?
C6B H6BA 0.97 . ?
C6B H6BB 0.97 . ?
C7B C8B 1.411(11) . ?
C7B H7BA 0.97 . ?
C7B H7BB 0.97 . ?
C8B H8BA 0.96 . ?
C8B H8BB 0.96 . ?
C8B H8BC 0.96 . ?
C9B C10B 1.526(7) . ?
C9B H9BA 0.97 . ?
C9B H9BB 0.97 . ?
C10B C11B 1.493(9) . ?
C10B H10C 0.97 . ?
C10B H10D 0.97 . ?
C11B C12B 1.490(10) . ?
C11B H11C 0.97 . ?
C11B H11D 0.97 . ?
C12B H12D 0.96 . ?
C12B H12E 0.96 . ?
C12B H12F 0.96 . ?
C13B C14B 1.513(10) . ?
C13B H13C 0.97 . ?
C13B H13D 0.97 . ?
C14B C15B 1.383(11) . ?
C14B H14C 0.97 . ?
C14B H14D 0.97 . ?
C15B C16B 1.533(13) . ?
C15B H15C 0.97 . ?
C15B H15D 0.97 . ?
C16B H16D 0.96 . ?
C16B H16E 0.96 . ?
C16B H16F 0.96 . ?
O1A C17A 1.199(7) . ?
O2A C17A 1.209(7) . ?
C17A C18A 1.495(9) . ?
C18A H18A 0.96 . ?
C18A H18B 0.96 . ?
C18A H18C 0.96 . ?
O1B C17B 1.236(6) . ?
O2B C17B 1.221(6) . ?
C17B C18B 1.505(7) . ?
C18B H18D 0.96 . ?
C18B H18E 0.96 . ?
C18B H18F 0.96 . ?
O3 H3A 0.85 . ?
O3 H3B 0.85 . ?

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
C7 N1 C1 126.2(5) . . ?
C7 N1 H1N 116.9 . . ?
C1 N1 H1N 116.9 . . ?
C7 N2 C8 127.5(5) . . ?
C7 N2 H2N 116.3 . . ?
C8 N2 H2N 116.3 . . ?
C20 N3 C17 127.7(4) . . ?
C20 N3 H3N 116.1 . . ?
C17 N3 H3N 116.1 . . ?
C20 N4 C21 126.8(4) . . ?
C20 N4 H4N 116.6 . . ?
C21 N4 H4N 116.6 . . ?
C6 C1 C2 118.3(6) . . ?
C6 C1 N1 124.6(5) . . ?
C2 C1 N1 117.2(5) . . ?
C3 C2 C1 121.1(6) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 119.7(7) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.3(7) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.8(8) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 120.7(7) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
O1 C7 N2 124.0(5) . . ?
O1 C7 N1 123.6(6) . . ?
N2 C7 N1 112.4(5) . . ?
C9 C8 C13 117.9(5) . . ?
C9 C8 N2 117.2(4) . . ?
C13 C8 N2 124.8(5) . . ?
C10 C9 C8 121.2(5) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 122.5(5) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C12 C11 C10 115.5(5) . . ?
C12 C11 C14 122.3(4) . . ?
C10 C11 C14 122.2(5) . . ?
C11 C12 C13 123.3(5) . . ?
C11 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C12 C13 C8 119.6(5) . . ?
C12 C13 H13 120.2 . . ?
C8 C13 H13 120.2 . . ?
C15 C14 C19 116.2(4) . . ?
C15 C14 C11 122.2(4) . . ?
C19 C14 C11 121.6(5) . . ?
C14 C15 C16 123.2(4) . . ?
C14 C15 H15 118.4 . . ?
C16 C15 H15 118.4 . . ?
C15 C16 C17 120.0(5) . . ?
C15 C16 H16 120 . . ?
C17 C16 H16 120 . . ?
C18 C17 C16 117.7(4) . . ?
C18 C17 N3 116.9(4) . . ?
C16 C17 N3 125.4(5) . . ?
C17 C18 C19 121.2(4) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C14 C19 C18 121.7(5) . . ?
C14 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
O2 C20 N3 124.6(4) . . ?
O2 C20 N4 123.3(4) . . ?
N3 C20 N4 112.1(4) . . ?
C22 C21 N4 125.2(5) . . ?
C22 C21 C26 117.7(5) . . ?
N4 C21 C26 116.9(4) . . ?
C23 C22 C21 120.2(5) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 121.6(6) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 118.9(6) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C26 C25 C24 120.4(6) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 121.1(6) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C1A N1A C9A 107.3(3) . . ?
C1A N1A C5A 110.8(4) . . ?
C9A N1A C5A 110.8(4) . . ?
C1A N1A C13A 110.6(4) . . ?
C9A N1A C13A 110.6(4) . . ?
C5A N1A C13A 106.9(3) . . ?
N1A C1A C2A 115.8(4) . . ?
N1A C1A H1AA 108.3 . . ?
C2A C1A H1AA 108.3 . . ?
N1A C1A H1AB 108.3 . . ?
C2A C1A H1AB 108.3 . . ?
H1AA C1A H1AB 107.4 . . ?
C3A C2A C1A 111.2(5) . . ?
C3A C2A H2AA 109.4 . . ?
C1A C2A H2AA 109.4 . . ?
C3A C2A H2AB 109.4 . . ?
C1A C2A H2AB 109.4 . . ?
H2AA C2A H2AB 108 . . ?
C4A C3A C2A 120.0(7) . . ?
C4A C3A H3AA 107.3 . . ?
C2A C3A H3AA 107.3 . . ?
C4A C3A H3AB 107.3 . . ?
C2A C3A H3AB 107.3 . . ?
H3AA C3A H3AB 106.9 . . ?
C3A C4A H4AA 109.5 . . ?
C3A C4A H4AB 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
C3A C4A H4AC 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
C6A C5A N1A 116.6(4) . . ?
C6A C5A H5AA 108.1 . . ?
N1A C5A H5AA 108.1 . . ?
C6A C5A H5AB 108.1 . . ?
N1A C5A H5AB 108.1 . . ?
H5AA C5A H5AB 107.3 . . ?
C5A C6A C7A 111.0(4) . . ?
C5A C6A H6AA 109.4 . . ?
C7A C6A H6AA 109.4 . . ?
C5A C6A H6AB 109.4 . . ?
C7A C6A H6AB 109.4 . . ?
H6AA C6A H6AB 108 . . ?
C6A C7A C8A 112.4(5) . . ?
C6A C7A H7AA 109.1 . . ?
C8A C7A H7AA 109.1 . . ?
C6A C7A H7AB 109.1 . . ?
C8A C7A H7AB 109.1 . . ?
H7AA C7A H7AB 107.9 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C10A C9A N1A 116.1(4) . . ?
C10A C9A H9AA 108.3 . . ?
N1A C9A H9AA 108.3 . . ?
C10A C9A H9AB 108.3 . . ?
N1A C9A H9AB 108.3 . . ?
H9AA C9A H9AB 107.4 . . ?
C9A C10A C11A 109.6(5) . . ?
C9A C10A H10A 109.8 . . ?
C11A C10A H10A 109.8 . . ?
C9A C10A H10B 109.8 . . ?
C11A C10A H10B 109.8 . . ?
H10A C10A H10B 108.2 . . ?
C12A C11A C10A 113.5(7) . . ?
C12A C11A H11A 108.9 . . ?
C10A C11A H11A 108.9 . . ?
C12A C11A H11B 108.9 . . ?
C10A C11A H11B 108.9 . . ?
H11A C11A H11B 107.7 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C14A C13A N1A 116.4(4) . . ?
C14A C13A H13A 108.2 . . ?
N1A C13A H13A 108.2 . . ?
C14A C13A H13B 108.2 . . ?
N1A C13A H13B 108.2 . . ?
H13A C13A H13B 107.3 . . ?
C15A C14A C13A 111.9(4) . . ?
C15A C14A H14A 109.2 . . ?
C13A C14A H14A 109.2 . . ?
C15A C14A H14B 109.2 . . ?
C13A C14A H14B 109.2 . . ?
H14A C14A H14B 107.9 . . ?
C14A C15A C16A 113.0(5) . . ?
C14A C15A H15A 109 . . ?
C16A C15A H15A 109 . . ?
C14A C15A H15B 109 . . ?
C16A C15A H15B 109 . . ?
H15A C15A H15B 107.8 . . ?
C15A C16A H16A 109.5 . . ?
C15A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C5B N1B C1B 110.1(4) . . ?
C5B N1B C9B 111.2(4) . . ?
C1B N1B C9B 107.6(3) . . ?
C5B N1B C13B 106.7(4) . . ?
C1B N1B C13B 110.7(4) . . ?
C9B N1B C13B 110.5(4) . . ?
C2B C1B N1B 115.9(4) . . ?
C2B C1B H1BA 108.3 . . ?
N1B C1B H1BA 108.3 . . ?
C2B C1B H1BB 108.3 . . ?
N1B C1B H1BB 108.3 . . ?
H1BA C1B H1BB 107.4 . . ?
C3B C2B C1B 111.6(5) . . ?
C3B C2B H2BA 109.3 . . ?
C1B C2B H2BA 109.3 . . ?
C3B C2B H2BB 109.3 . . ?
C1B C2B H2BB 109.3 . . ?
H2BA C2B H2BB 108 . . ?
C2B C3B C4B 113.0(7) . . ?
C2B C3B H3BA 109 . . ?
C4B C3B H3BA 109 . . ?
C2B C3B H3BB 109 . . ?
C4B C3B H3BB 109 . . ?
H3BA C3B H3BB 107.8 . . ?
C3B C4B H4BA 109.5 . . ?
C3B C4B H4BB 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
C3B C4B H4BC 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
C6B C5B N1B 116.8(4) . . ?
C6B C5B H5BA 108.1 . . ?
N1B C5B H5BA 108.1 . . ?
C6B C5B H5BB 108.1 . . ?
N1B C5B H5BB 108.1 . . ?
H5BA C5B H5BB 107.3 . . ?
C5B C6B C7B 110.9(6) . . ?
C5B C6B H6BA 109.5 . . ?
C7B C6B H6BA 109.5 . . ?
C5B C6B H6BB 109.5 . . ?
C7B C6B H6BB 109.5 . . ?
H6BA C6B H6BB 108 . . ?
C8B C7B C6B 118.0(7) . . ?
C8B C7B H7BA 107.8 . . ?
C6B C7B H7BA 107.8 . . ?
C8B C7B H7BB 107.8 . . ?
C6B C7B H7BB 107.8 . . ?
H7BA C7B H7BB 107.1 . . ?
C7B C8B H8BA 109.5 . . ?
C7B C8B H8BB 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
C7B C8B H8BC 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
N1B C9B C10B 115.2(4) . . ?
N1B C9B H9BA 108.5 . . ?
C10B C9B H9BA 108.5 . . ?
N1B C9B H9BB 108.5 . . ?
C10B C9B H9BB 108.5 . . ?
H9BA C9B H9BB 107.5 . . ?
C11B C10B C9B 111.4(5) . . ?
C11B C10B H10C 109.3 . . ?
C9B C10B H10C 109.3 . . ?
C11B C10B H10D 109.3 . . ?
C9B C10B H10D 109.3 . . ?
H10C C10B H10D 108 . . ?
C12B C11B C10B 115.1(6) . . ?
C12B C11B H11C 108.5 . . ?
C10B C11B H11C 108.5 . . ?
C12B C11B H11D 108.5 . . ?
C10B C11B H11D 108.5 . . ?
H11C C11B H11D 107.5 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C14B C13B N1B 114.1(5) . . ?
C14B C13B H13C 108.7 . . ?
N1B C13B H13C 108.7 . . ?
C14B C13B H13D 108.7 . . ?
N1B C13B H13D 108.7 . . ?
H13C C13B H13D 107.6 . . ?
C15B C14B C13B 115.5(8) . . ?
C15B C14B H14C 108.4 . . ?
C13B C14B H14C 108.4 . . ?
C15B C14B H14D 108.4 . . ?
C13B C14B H14D 108.4 . . ?
H14C C14B H14D 107.5 . . ?
C14B C15B C16B 114.6(10) . . ?
C14B C15B H15C 108.6 . . ?
C16B C15B H15C 108.6 . . ?
C14B C15B H15D 108.6 . . ?
C16B C15B H15D 108.6 . . ?
H15C C15B H15D 107.6 . . ?
C15B C16B H16D 109.5 . . ?
C15B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C15B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
O1A C17A O2A 120.2(6) . . ?
O1A C17A C18A 121.9(6) . . ?
O2A C17A C18A 117.2(6) . . ?
C17A C18A H18A 109.5 . . ?
C17A C18A H18B 109.5 . . ?
H18A C18A H18B 109.5 . . ?
C17A C18A H18C 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
O2B C17B O1B 122.7(5) . . ?
O2B C17B C18B 119.0(5) . . ?
O1B C17B C18B 118.2(5) . . ?
C17B C18B H18D 109.5 . . ?
C17B C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
C17B C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
H3A O3 H3B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 C1 C6 17.3(8) . . . . ?
C7 N1 C1 C2 -164.2(5) . . . . ?
C6 C1 C2 C3 -1.8(8) . . . . ?
N1 C1 C2 C3 179.7(5) . . . . ?
C1 C2 C3 C4 0.3(9) . . . . ?
C2 C3 C4 C5 1.8(11) . . . . ?
C3 C4 C5 C6 -2.4(12) . . . . ?
C2 C1 C6 C5 1.2(9) . . . . ?
N1 C1 C6 C5 179.6(6) . . . . ?
C4 C5 C6 C1 0.9(11) . . . . ?
C8 N2 C7 O1 -12.5(9) . . . . ?
C8 N2 C7 N1 170.3(4) . . . . ?
C1 N1 C7 O1 7.3(8) . . . . ?
C1 N1 C7 N2 -175.5(4) . . . . ?
C7 N2 C8 C9 -169.4(5) . . . . ?
C7 N2 C8 C13 8.8(8) . . . . ?
C13 C8 C9 C10 -0.8(8) . . . . ?
N2 C8 C9 C10 177.6(5) . . . . ?
C8 C9 C10 C11 0.7(8) . . . . ?
C9 C10 C11 C12 -0.7(8) . . . . ?
C9 C10 C11 C14 -177.3(5) . . . . ?
C10 C11 C12 C13 0.7(8) . . . . ?
C14 C11 C12 C13 177.4(5) . . . . ?
C11 C12 C13 C8 -0.8(9) . . . . ?
C9 C8 C13 C12 0.8(8) . . . . ?
N2 C8 C13 C12 -177.4(5) . . . . ?
C12 C11 C14 C15 -148.2(5) . . . . ?
C10 C11 C14 C15 28.2(7) . . . . ?
C12 C11 C14 C19 28.6(7) . . . . ?
C10 C11 C14 C19 -155.0(5) . . . . ?
C19 C14 C15 C16 -1.7(7) . . . . ?
C11 C14 C15 C16 175.3(5) . . . . ?
C14 C15 C16 C17 0.2(8) . . . . ?
C15 C16 C17 C18 1.2(7) . . . . ?
C15 C16 C17 N3 -176.1(4) . . . . ?
C20 N3 C17 C18 178.5(4) . . . . ?
C20 N3 C17 C16 -4.2(7) . . . . ?
C16 C17 C18 C19 -1.1(7) . . . . ?
N3 C17 C18 C19 176.5(4) . . . . ?
C15 C14 C19 C18 1.8(8) . . . . ?
C11 C14 C19 C18 -175.2(4) . . . . ?
C17 C18 C19 C14 -0.5(8) . . . . ?
C17 N3 C20 O2 -8.0(7) . . . . ?
C17 N3 C20 N4 172.1(4) . . . . ?
C21 N4 C20 O2 -1.4(7) . . . . ?
C21 N4 C20 N3 178.6(4) . . . . ?
C20 N4 C21 C22 -21.4(7) . . . . ?
C20 N4 C21 C26 162.1(4) . . . . ?
N4 C21 C22 C23 -176.2(4) . . . . ?
C26 C21 C22 C23 0.3(7) . . . . ?
C21 C22 C23 C24 0.0(8) . . . . ?
C22 C23 C24 C25 -0.4(9) . . . . ?
C23 C24 C25 C26 0.5(10) . . . . ?
C24 C25 C26 C21 -0.2(9) . . . . ?
C22 C21 C26 C25 -0.2(7) . . . . ?
N4 C21 C26 C25 176.6(5) . . . . ?
C9A N1A C1A C2A -177.1(5) . . . . ?
C5A N1A C1A C2A 61.8(6) . . . . ?
C13A N1A C1A C2A -56.5(6) . . . . ?
N1A C1A C2A C3A 176.4(6) . . . . ?
C1A C2A C3A C4A 178.4(9) . . . . ?
C1A N1A C5A C6A 61.5(6) . . . . ?
C9A N1A C5A C6A -57.3(6) . . . . ?
C13A N1A C5A C6A -177.9(5) . . . . ?
N1A C5A C6A C7A 171.2(5) . . . . ?
C5A C6A C7A C8A -179.2(6) . . . . ?
C1A N1A C9A C10A -171.9(5) . . . . ?
C5A N1A C9A C10A -50.9(6) . . . . ?
C13A N1A C9A C10A 67.4(6) . . . . ?
N1A C9A C10A C11A -179.4(5) . . . . ?
C9A C10A C11A C12A -174.5(7) . . . . ?
C1A N1A C13A C14A -56.2(6) . . . . ?
C9A N1A C13A C14A 62.4(6) . . . . ?
C5A N1A C13A C14A -176.9(5) . . . . ?
N1A C13A C14A C15A 173.3(5) . . . . ?
C13A C14A C15A C16A 176.3(6) . . . . ?
C5B N1B C1B C2B 60.0(6) . . . . ?
C9B N1B C1B C2B -178.7(5) . . . . ?
C13B N1B C1B C2B -57.8(6) . . . . ?
N1B C1B C2B C3B -177.7(5) . . . . ?
C1B C2B C3B C4B -177.7(7) . . . . ?
C1B N1B C5B C6B 52.5(7) . . . . ?
C9B N1B C5B C6B -66.7(7) . . . . ?
C13B N1B C5B C6B 172.7(6) . . . . ?
N1B C5B C6B C7B -174.7(6) . . . . ?
C5B C6B C7B C8B 170.2(9) . . . . ?
C5B N1B C9B C10B -62.5(6) . . . . ?
C1B N1B C9B C10B 176.8(4) . . . . ?
C13B N1B C9B C10B 55.8(6) . . . . ?
N1B C9B C10B C11B -169.4(5) . . . . ?
C9B C10B C11B C12B -174.5(6) . . . . ?
C5B N1B C13B C14B 179.9(6) . . . . ?
C1B N1B C13B C14B -60.3(7) . . . . ?
C9B N1B C13B C14B 58.8(7) . . . . ?
N1B C13B C14B C15B -175.4(7) . . . . ?
C13B C14B C15B C16B -175.1(9) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylformamide'
####################################################################### 
# 
# 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_1-((TBA)Br)2
_database_code_depnum_ccdc_archive 'CCDC 2015336'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T12:44:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H22 N4 O2, 2(C16 H36 N), 2(Br), H2 O'
_chemical_formula_sum            'C58 H96 Br2 N6 O3'
_chemical_formula_weight         1085.22

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   16.5304(6)
_cell_length_b                   18.1277(4)
_cell_length_c                   19.8203(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.4926(14)
_cell_angle_gamma                90
_cell_volume                     5933.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    170.00(10)
_cell_measurement_reflns_used    9855
_cell_measurement_theta_min      0.41
_cell_measurement_theta_max      27.48

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.136
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_F_000             2320

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.6092
_exptl_absorpt_correction_T_max  0.7456

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      170.00(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD with APEXII detector'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.1185
_diffrn_reflns_number            28501
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.668
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_reflns_Friedel_coverage         0
_reflns_number_total             10211
_reflns_number_gt                4085
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0877P)²+16.9879P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10211
_refine_ls_number_parameters     803
_refine_ls_number_restraints     255
_refine_ls_R_factor_all          0.2217
_refine_ls_R_factor_gt           0.0892
_refine_ls_wR_factor_ref         0.2792
_refine_ls_wR_factor_gt          0.2057
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.066


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.17003(6) 0.87092(5) 0.71393(6) 0.0882(4) Uani 1 1 d . . . . .
Br2 Br 0.82400(6) 0.62450(5) 0.30046(7) 0.1110(5) Uani 1 1 d . . . . .
O1 O 0.6287(4) 0.8446(4) 0.2495(3) 0.0887(19) Uani 1 1 d . . . . .
O2 O 0.3649(3) 0.6545(3) 0.7746(3) 0.0764(17) Uani 1 1 d . . . . .
N1 N 0.7420(5) 0.7804(4) 0.2231(4) 0.094(3) Uani 1 1 d . . . . .
H1 H 0.774887 0.745482 0.238538 0.113 Uiso 1 1 calc R U . . .
N2 N 0.6729(4) 0.7465(4) 0.3142(5) 0.090(3) Uani 1 1 d . . . . .
H2 H 0.707028 0.709269 0.313957 0.108 Uiso 1 1 calc R U . . .
N3 N 0.3212(4) 0.7511(4) 0.7095(4) 0.075(2) Uani 1 1 d . . . . .
H3 H 0.288043 0.789129 0.709522 0.09 Uiso 1 1 calc R U . . .
N4 N 0.2478(4) 0.7165(4) 0.7984(4) 0.077(2) Uani 1 1 d . . . . .
H4 H 0.214465 0.750151 0.781325 0.092 Uiso 1 1 calc R U . . .
C1 C 0.7632(6) 0.8128(6) 0.1638(6) 0.092(3) Uani 1 1 d . U . . .
C2 C 0.8289(6) 0.7832(6) 0.1308(6) 0.105(3) Uani 1 1 d . U . . .
H2A H 0.857483 0.742527 0.150435 0.126 Uiso 1 1 calc R U . . .
C3 C 0.8527(8) 0.8114(7) 0.0711(7) 0.119(4) Uani 1 1 d . U . . .
H3A H 0.897781 0.790279 0.050048 0.143 Uiso 1 1 calc R U . . .
C4 C 0.8126(8) 0.8702(7) 0.0408(7) 0.119(4) Uani 1 1 d . U . . .
H4A H 0.827533 0.888419 -0.001788 0.143 Uiso 1 1 calc R U . . .
C5 C 0.7481(7) 0.9024(6) 0.0755(7) 0.120(4) Uani 1 1 d . . . . .
H5 H 0.721221 0.944467 0.056654 0.144 Uiso 1 1 calc R U . . .
C6 C 0.7238(7) 0.8743(7) 0.1355(7) 0.111(4) Uani 1 1 d . . . . .
H6 H 0.68027 0.896514 0.157748 0.133 Uiso 1 1 calc R U . . .
C7 C 0.6771(6) 0.7946(6) 0.2615(6) 0.087(3) Uani 1 1 d . . . . .
C8 C 0.6218(5) 0.7485(4) 0.3685(5) 0.073(3) Uani 1 1 d . . . . .
C9 C 0.6418(5) 0.7060(5) 0.4248(6) 0.083(3) Uani 1 1 d . . . . .
H9 H 0.690099 0.67753 0.425707 0.1 Uiso 1 1 calc R U . . .
C10 C 0.5936(5) 0.7043(4) 0.4793(5) 0.074(3) Uani 1 1 d . . . . .
H10 H 0.608204 0.673136 0.516446 0.089 Uiso 1 1 calc R U . . .
C11 C 0.5236(5) 0.7470(4) 0.4816(5) 0.067(2) Uani 1 1 d . . . . .
C12 C 0.5049(5) 0.7897(5) 0.4264(5) 0.074(2) Uani 1 1 d . . . . .
H12 H 0.458195 0.820123 0.427256 0.088 Uiso 1 1 calc R U . . .
C13 C 0.5508(5) 0.7911(5) 0.3685(5) 0.079(3) Uani 1 1 d . . . . .
H13 H 0.534303 0.820061 0.330427 0.094 Uiso 1 1 calc R U . . .
C14 C 0.4727(5) 0.7464(4) 0.5412(5) 0.064(2) Uani 1 1 d . . . . .
C15 C 0.4996(5) 0.7206(4) 0.6044(5) 0.070(3) Uani 1 1 d . . . . .
H15 H 0.553329 0.702065 0.609232 0.084 Uiso 1 1 calc R U . . .
C16 C 0.4524(5) 0.7202(4) 0.6610(5) 0.064(2) Uani 1 1 d . . . . .
H16 H 0.473972 0.70186 0.702863 0.077 Uiso 1 1 calc R U . . .
C17 C 0.3739(5) 0.7467(4) 0.6558(5) 0.062(2) Uani 1 1 d . . . . .
C18 C 0.3447(5) 0.7717(4) 0.5937(5) 0.072(2) Uani 1 1 d . . . . .
H18 H 0.290384 0.788698 0.588765 0.086 Uiso 1 1 calc R U . . .
C19 C 0.3931(5) 0.7723(4) 0.5384(4) 0.072(2) Uani 1 1 d . . . . .
H19 H 0.371269 0.791216 0.496764 0.086 Uiso 1 1 calc R U . . .
C20 C 0.3163(5) 0.7026(4) 0.7614(5) 0.067(2) Uani 1 1 d . . . . .
C21 C 0.2250(6) 0.6840(4) 0.8589(5) 0.073(2) Uani 1 1 d . . . . .
C22 C 0.2704(6) 0.6294(4) 0.8923(5) 0.078(3) Uani 1 1 d . . . . .
H22 H 0.318995 0.611675 0.874078 0.093 Uiso 1 1 calc R U . . .
C23 C 0.2443(7) 0.6018(5) 0.9515(6) 0.093(3) Uani 1 1 d . . . . .
H23 H 0.274154 0.563549 0.973852 0.111 Uiso 1 1 calc R U . . .
C24 C 0.1749(8) 0.6285(6) 0.9795(5) 0.094(3) Uani 1 1 d . . . . .
H24 H 0.158239 0.609923 1.021479 0.112 Uiso 1 1 calc R U . . .
C25 C 0.1297(7) 0.6829(6) 0.9456(6) 0.093(3) Uani 1 1 d . . . . .
H25 H 0.081674 0.700952 0.964414 0.112 Uiso 1 1 calc R U . . .
C26 C 0.1540(6) 0.7106(5) 0.8854(5) 0.084(3) Uani 1 1 d . . . . .
H26 H 0.122815 0.747372 0.862057 0.101 Uiso 1 1 calc R U . . .
N1A N 0.4862(4) 0.4527(3) 0.7433(3) 0.073(2) Uani 1 1 d D . . . .
C1A C 0.5294(5) 0.3953(5) 0.7031(5) 0.092(3) Uani 1 1 d D U . . .
H1A1 H 0.548864 0.356021 0.734482 0.111 Uiso 1 1 calc R U . . .
H1A2 H 0.489509 0.372603 0.670671 0.111 Uiso 1 1 calc R U . . .
C2A C 0.5999(7) 0.4218(6) 0.6645(6) 0.141(4) Uani 1 1 d D U . . .
H2A1 H 0.643945 0.439274 0.695972 0.17 Uiso 1 1 calc R U . . .
H2A2 H 0.583161 0.463065 0.634289 0.17 Uiso 1 1 calc R U . . .
C3A C 0.6291(6) 0.3564(6) 0.6230(6) 0.123(4) Uani 1 1 d D . . . .
H3A1 H 0.636368 0.312917 0.652832 0.147 Uiso 1 1 calc R U . . .
H3A2 H 0.587143 0.34408 0.587587 0.147 Uiso 1 1 calc R U . . .
C4A C 0.7072(7) 0.3725(6) 0.5904(7) 0.159(6) Uani 1 1 d D . . . .
H4A1 H 0.698171 0.410297 0.555465 0.239 Uiso 1 1 calc R U . . .
H4A2 H 0.727423 0.327385 0.569749 0.239 Uiso 1 1 calc R U . . .
H4A3 H 0.747089 0.390452 0.624533 0.239 Uiso 1 1 calc R U . . .
C5A C 0.5472(6) 0.4934(4) 0.7902(5) 0.086(3) Uani 1 1 d D . . . .
H5A1 H 0.581435 0.525093 0.762402 0.103 Uiso 1 1 calc R U . . .
H5A2 H 0.517086 0.526199 0.820217 0.103 Uiso 1 1 calc R U . . .
C6A C 0.6019(7) 0.4439(6) 0.8336(6) 0.130(4) Uani 1 1 d D U . . .
H6A1 H 0.635376 0.412969 0.804521 0.156 Uiso 1 1 calc R U . . .
H6A2 H 0.568837 0.410898 0.861085 0.156 Uiso 1 1 calc R U . . .
C7A C 0.6566(8) 0.4918(8) 0.8798(7) 0.192(8) Uani 1 1 d D . . . .
H7A1 H 0.704315 0.463289 0.896961 0.23 Uiso 1 1 calc R U . . .
H7A2 H 0.675812 0.535429 0.855075 0.23 Uiso 1 1 calc R U . . .
C8A C 0.6064(9) 0.5151(8) 0.9368(6) 0.204(7) Uani 1 1 d D U . . .
H8A1 H 0.569869 0.554956 0.921668 0.306 Uiso 1 1 calc R U . . .
H8A2 H 0.641826 0.532673 0.974369 0.306 Uiso 1 1 calc R U . . .
H8A3 H 0.574544 0.473081 0.951782 0.306 Uiso 1 1 calc R U . . .
C9A C 0.4264(6) 0.4078(4) 0.7825(5) 0.090(3) Uani 1 1 d D . . . .
H9A1 H 0.387466 0.383915 0.750052 0.108 Uiso 1 1 calc R U . . .
H9A2 H 0.456333 0.368182 0.807323 0.108 Uiso 1 1 calc R U . . .
C10A C 0.3801(6) 0.4517(6) 0.8319(5) 0.123(4) Uani 1 1 d D . . . .
H10A H 0.361651 0.49789 0.809337 0.148 Uiso 1 1 calc R U . . .
H10B H 0.417741 0.465752 0.869915 0.148 Uiso 1 1 calc R U . . .
C11A C 0.3076(7) 0.4148(7) 0.8605(6) 0.171(6) Uani 1 1 d D . . . .
H11A H 0.273895 0.452017 0.882595 0.205 Uiso 1 1 calc R U . . .
H11B H 0.274373 0.391552 0.823553 0.205 Uiso 1 1 calc R U . . .
C12A C 0.3347(8) 0.3575(7) 0.9107(7) 0.148(5) Uani 1 1 d D U . . .
H12A H 0.362479 0.317639 0.887555 0.222 Uiso 1 1 calc R U . . .
H12B H 0.28754 0.337433 0.932718 0.222 Uiso 1 1 calc R U . . .
H12C H 0.371913 0.379728 0.944755 0.222 Uiso 1 1 calc R U . . .
C13A C 0.4437(5) 0.5104(4) 0.7011(4) 0.082(3) Uani 1 1 d D . . . .
H13A H 0.484948 0.537795 0.676314 0.098 Uiso 1 1 calc R U . . .
H13B H 0.418314 0.545844 0.731686 0.098 Uiso 1 1 calc R U . . .
C14A C 0.3797(5) 0.4836(4) 0.6506(4) 0.094(3) Uani 1 1 d D . . . .
H14A H 0.406478 0.457004 0.614056 0.113 Uiso 1 1 calc R U . A 1
H14B H 0.344648 0.44779 0.673202 0.113 Uiso 1 1 calc R U . A 1
C15A C 0.3267(10) 0.5435(7) 0.6191(9) 0.090(6) Uani 0.51 1 d D U P B 1
H15A H 0.304308 0.573547 0.655619 0.108 Uiso 0.51 1 calc R U P B 1
H15B H 0.360632 0.576278 0.592127 0.108 Uiso 0.51 1 calc R U P B 1
C16A C 0.2577(13) 0.5149(14) 0.5745(13) 0.193(13) Uani 0.51 1 d D U P B 1
H16A H 0.276837 0.505275 0.529178 0.289 Uiso 0.51 1 calc R U P B 1
H16B H 0.214276 0.551712 0.571611 0.289 Uiso 0.51 1 calc R U P B 1
H16C H 0.237063 0.469051 0.593488 0.289 Uiso 0.51 1 calc R U P B 1
C15X C 0.3719(11) 0.5382(10) 0.5924(7) 0.111(8) Uani 0.49 1 d D U P B 2
H15C H 0.321742 0.527161 0.565128 0.133 Uiso 0.49 1 calc R U P B 2
H15D H 0.366667 0.588535 0.610974 0.133 Uiso 0.49 1 calc R U P B 2
C16X C 0.4420(14) 0.5366(12) 0.5473(9) 0.136(9) Uani 0.49 1 d D U P B 2
H16D H 0.426085 0.559235 0.503789 0.204 Uiso 0.49 1 calc R U P B 2
H16E H 0.458474 0.485403 0.54005 0.204 Uiso 0.49 1 calc R U P B 2
H16F H 0.487323 0.564209 0.56842 0.204 Uiso 0.49 1 calc R U P B 2
N1B N -0.0022(3) 0.5529(2) 0.7484(3) 0.0543(16) Uani 1 1 d D . . . .
C1B C 0.0606(7) 0.5263(8) 0.7996(6) 0.074(5) Uani 0.52 1 d D U P C 1
H1B1 H 0.084352 0.569537 0.823673 0.088 Uiso 0.52 1 calc R U P C 1
H1B2 H 0.104568 0.501892 0.775593 0.088 Uiso 0.52 1 calc R U P C 1
C2B C 0.0298(9) 0.4733(9) 0.8510(9) 0.084(6) Uani 0.52 1 d D U P C 1
H2B1 H -0.003695 0.435283 0.827345 0.101 Uiso 0.52 1 calc R U P C 1
H2B2 H -0.005483 0.500499 0.881553 0.101 Uiso 0.52 1 calc R U P C 1
C3B C 0.0960(9) 0.4357(12) 0.8928(12) 0.058(7) Uani 0.52 1 d D U P C 1
H3B1 H 0.129833 0.473417 0.916521 0.07 Uiso 0.52 1 calc R U P C 1
H3B2 H 0.130971 0.407666 0.862619 0.07 Uiso 0.52 1 calc R U P C 1
C4B C 0.0620(13) 0.3838(11) 0.9440(9) 0.118(8) Uani 0.52 1 d D U P C 1
H4B1 H 0.013689 0.405771 0.962663 0.177 Uiso 0.52 1 calc R U P C 1
H4B2 H 0.102812 0.374983 0.980452 0.177 Uiso 0.52 1 calc R U P C 1
H4B3 H 0.047535 0.336863 0.922034 0.177 Uiso 0.52 1 calc R U P C 1
C1Y C 0.0196(8) 0.4892(5) 0.7958(6) 0.037(4) Uani 0.48 1 d D . P C 2
H1Y1 H -0.031374 0.466936 0.810525 0.045 Uiso 0.48 1 calc R U P C 2
H1Y2 H 0.047888 0.451241 0.769785 0.045 Uiso 0.48 1 calc R U P C 2
C2Y C 0.0720(8) 0.5070(7) 0.8585(6) 0.051(4) Uani 0.48 1 d D . P C 2
H2Y1 H 0.125602 0.524061 0.844419 0.061 Uiso 0.48 1 calc R U P C 2
H2Y2 H 0.046758 0.548049 0.882893 0.061 Uiso 0.48 1 calc R U P C 2
C3Y C 0.0840(12) 0.4425(16) 0.9061(17) 0.109(16) Uani 0.48 1 d D U P C 2
H3Y1 H 0.107124 0.400584 0.881356 0.13 Uiso 0.48 1 calc R U P C 2
H3Y2 H 0.123412 0.456482 0.942937 0.13 Uiso 0.48 1 calc R U P C 2
C4Y C 0.0061(13) 0.4181(13) 0.9364(11) 0.111(8) Uani 0.48 1 d D U P C 2
H4Y1 H -0.017216 0.376952 0.910076 0.167 Uiso 0.48 1 calc R U P C 2
H4Y2 H -0.032255 0.45934 0.935689 0.167 Uiso 0.48 1 calc R U P C 2
H4Y3 H 0.01727 0.402209 0.98316 0.167 Uiso 0.48 1 calc R U P C 2
C5B C -0.0628(7) 0.5261(7) 0.6953(6) 0.045(3) Uani 0.52 1 d D . P C 1
H5B1 H -0.085879 0.56917 0.670445 0.054 Uiso 0.52 1 calc R U P C 1
H5B2 H -0.107658 0.501111 0.71768 0.054 Uiso 0.52 1 calc R U P C 1
C6B C -0.0272(9) 0.4735(8) 0.6454(9) 0.069(6) Uani 0.52 1 d D . P C 1
H6B1 H 0.005336 0.435298 0.66987 0.083 Uiso 0.52 1 calc R U P C 1
H6B2 H 0.008909 0.500654 0.615498 0.083 Uiso 0.52 1 calc R U P C 1
C7B C -0.0951(13) 0.4372(14) 0.6035(12) 0.097(9) Uani 0.52 1 d D U P C 1
H7B1 H -0.13047 0.408893 0.633058 0.117 Uiso 0.52 1 calc R U P C 1
H7B2 H -0.128279 0.475259 0.579511 0.117 Uiso 0.52 1 calc R U P C 1
C8B C -0.0580(16) 0.3864(11) 0.5532(11) 0.118(8) Uani 0.52 1 d D U P C 1
H8B1 H -0.100964 0.358657 0.528795 0.177 Uiso 0.52 1 calc R U P C 1
H8B2 H -0.021159 0.351872 0.577068 0.177 Uiso 0.52 1 calc R U P C 1
H8B3 H -0.027825 0.41545 0.521083 0.177 Uiso 0.52 1 calc R U P C 1
C5Y C -0.0147(10) 0.4875(6) 0.7020(6) 0.062(5) Uani 0.48 1 d D U P C 2
H5Y1 H 0.038951 0.469241 0.689066 0.075 Uiso 0.48 1 calc R U P C 2
H5Y2 H -0.040834 0.447491 0.727198 0.075 Uiso 0.48 1 calc R U P C 2
C6Y C -0.0652(12) 0.5033(8) 0.6390(7) 0.074(6) Uani 0.48 1 d D . P C 2
H6Y1 H -0.041107 0.54555 0.6154 0.089 Uiso 0.48 1 calc R U P C 2
H6Y2 H -0.120041 0.518155 0.651856 0.089 Uiso 0.48 1 calc R U P C 2
C7Y C -0.0730(10) 0.4387(12) 0.5902(10) 0.064(7) Uani 0.48 1 d D U P C 2
H7Y1 H -0.0938 0.39565 0.614788 0.077 Uiso 0.48 1 calc R U P C 2
H7Y2 H -0.113878 0.451517 0.554099 0.077 Uiso 0.48 1 calc R U P C 2
C8Y C 0.0039(13) 0.4162(16) 0.5575(13) 0.126(10) Uani 0.48 1 d D . P C 2
H8Y1 H 0.023284 0.45712 0.530241 0.188 Uiso 0.48 1 calc R U P C 2
H8Y2 H -0.006731 0.373183 0.528537 0.188 Uiso 0.48 1 calc R U P C 2
H8Y3 H 0.045267 0.403631 0.592606 0.188 Uiso 0.48 1 calc R U P C 2
C9B C -0.0369(8) 0.6162(6) 0.7885(7) 0.058(4) Uani 0.55 1 d D . P C 1
H9B1 H 0.006472 0.635197 0.819897 0.07 Uiso 0.55 1 calc R U P C 1
H9B2 H -0.051776 0.656505 0.756624 0.07 Uiso 0.55 1 calc R U P C 1
C10B C -0.1097(10) 0.5987(9) 0.8289(9) 0.069(5) Uani 0.55 1 d D . P C 1
H10C H -0.100449 0.551683 0.853434 0.082 Uiso 0.55 1 calc R U P C 1
H10D H -0.157771 0.592457 0.797889 0.082 Uiso 0.55 1 calc R U P C 1
C11B C -0.1259(11) 0.6593(10) 0.8790(10) 0.076(6) Uani 0.55 1 d D U P C 1
H11C H -0.07717 0.665702 0.909287 0.092 Uiso 0.55 1 calc R U P C 1
H11D H -0.134871 0.706074 0.854045 0.092 Uiso 0.55 1 calc R U P C 1
C12B C -0.1978(12) 0.6452(13) 0.9217(11) 0.126(9) Uani 0.55 1 d D . P C 1
H12D H -0.24714 0.642492 0.892503 0.189 Uiso 0.55 1 calc R U P C 1
H12E H -0.202832 0.685482 0.954197 0.189 Uiso 0.55 1 calc R U P C 1
H12F H -0.190149 0.598475 0.945987 0.189 Uiso 0.55 1 calc R U P C 1
C9Y C -0.0824(11) 0.5726(8) 0.7782(9) 0.067(6) Uani 0.45 1 d D . P C 2
H9Y1 H -0.121515 0.5867 0.741142 0.081 Uiso 0.45 1 calc R U P C 2
H9Y2 H -0.104132 0.52844 0.800634 0.081 Uiso 0.45 1 calc R U P C 2
C10Y C -0.0755(14) 0.6350(12) 0.8287(13) 0.091(9) Uani 0.45 1 d D . P C 2
H10E H -0.06899 0.682412 0.804748 0.109 Uiso 0.45 1 calc R U P C 2
H10F H -0.027315 0.62743 0.859368 0.109 Uiso 0.45 1 calc R U P C 2
C11Y C -0.1511(13) 0.6371(12) 0.8690(11) 0.064(7) Uani 0.45 1 d D U P C 2
H11E H -0.156993 0.589874 0.893355 0.076 Uiso 0.45 1 calc R U P C 2
H11F H -0.199234 0.643652 0.838075 0.076 Uiso 0.45 1 calc R U P C 2
C12Y C -0.1458(16) 0.7001(12) 0.9190(12) 0.104(8) Uani 0.45 1 d D . P C 2
H12G H -0.138607 0.746649 0.894837 0.157 Uiso 0.45 1 calc R U P C 2
H12H H -0.099635 0.692233 0.950912 0.157 Uiso 0.45 1 calc R U P C 2
H12I H -0.195804 0.702333 0.943804 0.157 Uiso 0.45 1 calc R U P C 2
C13B C 0.0757(6) 0.5823(7) 0.7208(6) 0.074(4) Uani 0.63 1 d D . P C 1
H13C H 0.108974 0.604707 0.758172 0.089 Uiso 0.63 1 calc R U P C 1
H13D H 0.106829 0.540683 0.702563 0.089 Uiso 0.63 1 calc R U P C 1
C14B C 0.0612(9) 0.6388(7) 0.6662(8) 0.078(5) Uani 0.63 1 d D . P C 1
H14C H 0.042234 0.685272 0.686471 0.094 Uiso 0.63 1 calc R U P C 1
H14D H 0.018025 0.620995 0.63397 0.094 Uiso 0.63 1 calc R U P C 1
C15B C 0.1381(15) 0.6541(14) 0.6279(14) 0.125(9) Uani 0.63 1 d D U P C 1
H15E H 0.183647 0.667507 0.659693 0.15 Uiso 0.63 1 calc R U P C 1
H15F H 0.153681 0.610295 0.601687 0.15 Uiso 0.63 1 calc R U P C 1
C16B C 0.1162(16) 0.7181(13) 0.5814(12) 0.219(12) Uani 0.63 1 d D U P C 1
H16G H 0.107129 0.699815 0.535132 0.329 Uiso 0.63 1 calc R U P C 1
H16H H 0.16053 0.754027 0.582688 0.329 Uiso 0.63 1 calc R U P C 1
H16I H 0.066731 0.741815 0.596201 0.329 Uiso 0.63 1 calc R U P C 1
C13Y C 0.0256(11) 0.6198(7) 0.7101(10) 0.050(5) Uani 0.37 1 d D U P C 2
H13E H 0.035278 0.660625 0.742634 0.06 Uiso 0.37 1 calc R U P C 2
H13F H -0.018649 0.635214 0.677975 0.06 Uiso 0.37 1 calc R U P C 2
C14Y C 0.1016(13) 0.6086(10) 0.6713(12) 0.064(7) Uani 0.37 1 d D U P C 2
H14E H 0.093437 0.567183 0.639151 0.077 Uiso 0.37 1 calc R U P C 2
H14F H 0.147345 0.595754 0.703075 0.077 Uiso 0.37 1 calc R U P C 2
C15Y C 0.1219(19) 0.6781(13) 0.6330(17) 0.085(11) Uani 0.37 1 d D U P C 2
H15G H 0.072248 0.698007 0.609952 0.103 Uiso 0.37 1 calc R U P C 2
H15H H 0.143617 0.71592 0.664926 0.103 Uiso 0.37 1 calc R U P C 2
C16Y C 0.184(2) 0.661(2) 0.5813(19) 0.22(2) Uani 0.37 1 d D U P C 2
H16J H 0.160971 0.670521 0.535867 0.336 Uiso 0.37 1 calc R U P C 2
H16K H 0.199687 0.608642 0.584976 0.336 Uiso 0.37 1 calc R U P C 2
H16L H 0.23209 0.691748 0.589738 0.336 Uiso 0.37 1 calc R U P C 2
O3 O -0.0007(5) 0.7889(4) 0.7639(4) 0.133(3) Uani 1 1 d D U . . .
H31 H 0.040(4) 0.815(6) 0.756(6) 0.2 Uiso 1 1 d D U . . .
H32 H -0.035(5) 0.790(8) 0.731(4) 0.2 Uiso 1 1 d D U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.226(12) . ?
O2 C20 1.206(8) . ?
N1 C7 1.367(11) . ?
N1 C1 1.373(13) . ?
N1 H1 0.88 . ?
N2 C7 1.363(13) . ?
N2 C8 1.397(11) . ?
N2 H2 0.88 . ?
N3 C20 1.359(10) . ?
N3 C17 1.407(10) . ?
N3 H3 0.88 . ?
N4 C20 1.398(10) . ?
N4 C21 1.403(10) . ?
N4 H4 0.88 . ?
C1 C6 1.396(15) . ?
C1 C2 1.400(13) . ?
C2 C3 1.363(14) . ?
C2 H2A 0.95 . ?
C3 C4 1.379(15) . ?
C3 H3A 0.95 . ?
C4 C5 1.418(16) . ?
C4 H4A 0.95 . ?
C5 C6 1.371(15) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C8 C9 1.385(12) . ?
C8 C13 1.405(11) . ?
C9 C10 1.371(12) . ?
C9 H9 0.95 . ?
C10 C11 1.396(10) . ?
C10 H10 0.95 . ?
C11 C12 1.363(11) . ?
C11 C14 1.480(12) . ?
C12 C13 1.403(11) . ?
C12 H12 0.95 . ?
C13 H13 0.95 . ?
C14 C15 1.392(11) . ?
C14 C19 1.395(10) . ?
C15 C16 1.394(11) . ?
C15 H15 0.95 . ?
C16 C17 1.383(10) . ?
C16 H16 0.95 . ?
C17 C18 1.378(11) . ?
C18 C19 1.386(11) . ?
C18 H18 0.95 . ?
C19 H19 0.95 . ?
C21 C26 1.393(12) . ?
C21 C22 1.392(11) . ?
C22 C23 1.363(13) . ?
C22 H22 0.95 . ?
C23 C24 1.383(14) . ?
C23 H23 0.95 . ?
C24 C25 1.391(13) . ?
C24 H24 0.95 . ?
C25 C26 1.372(12) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
N1A C13A 1.495(6) . ?
N1A C1A 1.510(10) . ?
N1A C5A 1.531(10) . ?
N1A C9A 1.521(9) . ?
C1A C2A 1.501(7) . ?
C1A H1A1 0.99 . ?
C1A H1A2 0.99 . ?
C2A C3A 1.532(7) . ?
C2A H2A1 0.99 . ?
C2A H2A2 0.99 . ?
C3A C4A 1.498(5) . ?
C3A H3A1 0.99 . ?
C3A H3A2 0.99 . ?
C4A H4A1 0.98 . ?
C4A H4A2 0.98 . ?
C4A H4A3 0.98 . ?
C5A C6A 1.515(7) . ?
C5A H5A1 0.99 . ?
C5A H5A2 0.99 . ?
C6A C7A 1.530(7) . ?
C6A H6A1 0.99 . ?
C6A H6A2 0.99 . ?
C7A C8A 1.491(8) . ?
C7A H7A1 0.99 . ?
C7A H7A2 0.99 . ?
C8A H8A1 0.98 . ?
C8A H8A2 0.98 . ?
C8A H8A3 0.98 . ?
C9A C10A 1.497(7) . ?
C9A H9A1 0.99 . ?
C9A H9A2 0.99 . ?
C10A C11A 1.504(7) . ?
C10A H10A 0.99 . ?
C10A H10B 0.99 . ?
C11A C12A 1.494(5) . ?
C11A H11A 0.99 . ?
C11A H11B 0.99 . ?
C12A H12A 0.98 . ?
C12A H12B 0.98 . ?
C12A H12C 0.98 . ?
C13A C14A 1.506(5) . ?
C13A H13A 0.99 . ?
C13A H13B 0.99 . ?
C14A C15A 1.512(5) . ?
C14A C15X 1.521(8) . ?
C14A H14A 0.99 . ?
C14A H14B 0.99 . ?
C15A C16A 1.505(8) . ?
C15A H15A 0.99 . ?
C15A H15B 0.99 . ?
C16A H16A 0.98 . ?
C16A H16B 0.98 . ?
C16A H16C 0.98 . ?
C15X C16X 1.493(8) . ?
C15X H15C 0.99 . ?
C15X H15D 0.99 . ?
C16X H16D 0.98 . ?
C16X H16E 0.98 . ?
C16X H16F 0.98 . ?
N1B C1B 1.500(7) . ?
N1B C5B 1.502(7) . ?
N1B C5Y 1.510(7) . ?
N1B C13Y 1.511(8) . ?
N1B C9Y 1.518(18) . ?
N1B C13B 1.517(7) . ?
N1B C9B 1.522(7) . ?
N1B C1Y 1.523(7) . ?
C1B C2B 1.504(5) . ?
C1B C13B 1.890(15) . ?
C1B H1B1 0.99 . ?
C1B H1B2 0.99 . ?
C2B C3B 1.506(8) . ?
C2B H2B1 0.99 . ?
C2B H2B2 0.99 . ?
C3B C4B 1.510(8) . ?
C3B H3B1 0.99 . ?
C3B H3B2 0.99 . ?
C4B H4B1 0.98 . ?
C4B H4B2 0.98 . ?
C4B H4B3 0.98 . ?
C1Y C2Y 1.516(8) . ?
C1Y C5Y 1.921(15) . ?
C1Y H1Y1 0.99 . ?
C1Y H1Y2 0.99 . ?
C2Y C3Y 1.511(8) . ?
C2Y H2Y1 0.99 . ?
C2Y H2Y2 0.99 . ?
C3Y C4Y 1.510(8) . ?
C3Y H3Y1 0.99 . ?
C3Y H3Y2 0.99 . ?
C4Y H4Y1 0.98 . ?
C4Y H4Y2 0.98 . ?
C4Y H4Y3 0.98 . ?
C5B C6B 1.513(8) . ?
C5B H5B1 0.99 . ?
C5B H5B2 0.99 . ?
C6B C7B 1.517(8) . ?
C6B H6B1 0.99 . ?
C6B H6B2 0.99 . ?
C7B C8B 1.506(8) . ?
C7B H7B1 0.99 . ?
C7B H7B2 0.99 . ?
C8B H8B1 0.98 . ?
C8B H8B2 0.98 . ?
C8B H8B3 0.98 . ?
C5Y C6Y 1.500(8) . ?
C5Y H5Y1 0.99 . ?
C5Y H5Y2 0.99 . ?
C6Y C7Y 1.520(8) . ?
C6Y H6Y1 0.99 . ?
C6Y H6Y2 0.99 . ?
C7Y C8Y 1.508(8) . ?
C7Y H7Y1 0.99 . ?
C7Y H7Y2 0.99 . ?
C8Y H8Y1 0.98 . ?
C8Y H8Y2 0.98 . ?
C8Y H8Y3 0.98 . ?
C9B C10B 1.509(8) . ?
C9B H9B1 0.99 . ?
C9B H9B2 0.99 . ?
C10B C11B 1.512(8) . ?
C10B H10C 0.99 . ?
C10B H10D 0.99 . ?
C11B C12B 1.510(8) . ?
C11B H11C 0.99 . ?
C11B H11D 0.99 . ?
C12B H12D 0.98 . ?
C12B H12E 0.98 . ?
C12B H12F 0.98 . ?
C9Y C10Y 1.512(8) . ?
C9Y H9Y1 0.99 . ?
C9Y H9Y2 0.99 . ?
C10Y C11Y 1.513(8) . ?
C10Y H10E 0.99 . ?
C10Y H10F 0.99 . ?
C11Y C12Y 1.513(8) . ?
C11Y H11E 0.99 . ?
C11Y H11F 0.99 . ?
C12Y H12G 0.98 . ?
C12Y H12H 0.98 . ?
C12Y H12I 0.98 . ?
C13B C14B 1.502(8) . ?
C13B H13C 0.99 . ?
C13B H13D 0.99 . ?
C14B C15B 1.53(2) . ?
C14B H14C 0.99 . ?
C14B H14D 0.99 . ?
C15B C16B 1.516(8) . ?
C15B H15E 0.99 . ?
C15B H15F 0.99 . ?
C16B H16G 0.98 . ?
C16B H16H 0.98 . ?
C16B H16I 0.98 . ?
C13Y C14Y 1.515(8) . ?
C13Y H13E 0.99 . ?
C13Y H13F 0.99 . ?
C14Y C15Y 1.516(8) . ?
C14Y H14E 0.99 . ?
C14Y H14F 0.99 . ?
C15Y C16Y 1.516(8) . ?
C15Y H15G 0.99 . ?
C15Y H15H 0.99 . ?
C16Y H16J 0.98 . ?
C16Y H16K 0.98 . ?
C16Y H16L 0.98 . ?
O3 H31 0.841(5) . ?
O3 H32 0.841(5) . ?

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
C7 N1 C1 129.2(10) . . ?
C7 N1 H1 115.4 . . ?
C1 N1 H1 115.4 . . ?
C7 N2 C8 128.7(8) . . ?
C7 N2 H2 115.6 . . ?
C8 N2 H2 115.6 . . ?
C20 N3 C17 126.5(7) . . ?
C20 N3 H3 116.7 . . ?
C17 N3 H3 116.7 . . ?
C20 N4 C21 128.8(7) . . ?
C20 N4 H4 115.6 . . ?
C21 N4 H4 115.6 . . ?
N1 C1 C6 123.7(10) . . ?
N1 C1 C2 117.9(12) . . ?
C6 C1 C2 118.4(12) . . ?
C3 C2 C1 121.5(12) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
C2 C3 C4 121.0(13) . . ?
C2 C3 H3A 119.5 . . ?
C4 C3 H3A 119.5 . . ?
C3 C4 C5 117.8(13) . . ?
C3 C4 H4A 121.1 . . ?
C5 C4 H4A 121.1 . . ?
C6 C5 C4 121.4(13) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 119.8(12) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
O1 C7 N2 124.6(9) . . ?
O1 C7 N1 123.5(12) . . ?
N2 C7 N1 111.9(10) . . ?
C9 C8 N2 118.4(8) . . ?
C9 C8 C13 118.4(9) . . ?
N2 C8 C13 123.2(10) . . ?
C10 C9 C8 121.5(8) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C10 C11 121.6(9) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 H10 119.2 . . ?
C12 C11 C10 116.7(8) . . ?
C12 C11 C14 121.9(7) . . ?
C10 C11 C14 121.5(9) . . ?
C11 C12 C13 123.7(8) . . ?
C11 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C8 118.2(9) . . ?
C12 C13 H13 120.9 . . ?
C8 C13 H13 120.9 . . ?
C15 C14 C19 114.4(8) . . ?
C15 C14 C11 123.4(7) . . ?
C19 C14 C11 122.2(8) . . ?
C14 C15 C16 123.8(8) . . ?
C14 C15 H15 118.1 . . ?
C16 C15 H15 118.1 . . ?
C17 C16 C15 119.7(8) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C18 C17 C16 118.1(8) . . ?
C18 C17 N3 116.9(7) . . ?
C16 C17 N3 125.0(8) . . ?
C17 C18 C19 121.1(8) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C14 122.8(8) . . ?
C18 C19 H19 118.6 . . ?
C14 C19 H19 118.6 . . ?
O2 C20 N3 124.8(9) . . ?
O2 C20 N4 124.3(9) . . ?
N3 C20 N4 110.8(7) . . ?
C26 C21 C22 120.9(9) . . ?
C26 C21 N4 116.1(8) . . ?
C22 C21 N4 123.0(9) . . ?
C23 C22 C21 119.0(10) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 121.1(10) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 119.4(10) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 120.6(11) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C21 119.0(9) . . ?
C25 C26 H26 120.5 . . ?
C21 C26 H26 120.5 . . ?
C13A N1A C1A 114.1(7) . . ?
C13A N1A C5A 106.5(6) . . ?
C1A N1A C5A 109.8(7) . . ?
C13A N1A C9A 111.2(6) . . ?
C1A N1A C9A 103.5(6) . . ?
C5A N1A C9A 111.9(7) . . ?
C2A C1A N1A 116.4(7) . . ?
C2A C1A H1A1 108.2 . . ?
N1A C1A H1A1 108.2 . . ?
C2A C1A H1A2 108.2 . . ?
N1A C1A H1A2 108.2 . . ?
H1A1 C1A H1A2 107.3 . . ?
C1A C2A C3A 107.2(8) . . ?
C1A C2A H2A1 110.3 . . ?
C3A C2A H2A1 110.3 . . ?
C1A C2A H2A2 110.3 . . ?
C3A C2A H2A2 110.3 . . ?
H2A1 C2A H2A2 108.5 . . ?
C4A C3A C2A 112.2(9) . . ?
C4A C3A H3A1 109.2 . . ?
C2A C3A H3A1 109.2 . . ?
C4A C3A H3A2 109.2 . . ?
C2A C3A H3A2 109.2 . . ?
H3A1 C3A H3A2 107.9 . . ?
C3A C4A H4A1 109.5 . . ?
C3A C4A H4A2 109.5 . . ?
H4A1 C4A H4A2 109.5 . . ?
C3A C4A H4A3 109.5 . . ?
H4A1 C4A H4A3 109.5 . . ?
H4A2 C4A H4A3 109.5 . . ?
C6A C5A N1A 114.8(7) . . ?
C6A C5A H5A1 108.6 . . ?
N1A C5A H5A1 108.6 . . ?
C6A C5A H5A2 108.6 . . ?
N1A C5A H5A2 108.6 . . ?
H5A1 C5A H5A2 107.5 . . ?
C5A C6A C7A 109.0(9) . . ?
C5A C6A H6A1 109.9 . . ?
C7A C6A H6A1 109.9 . . ?
C5A C6A H6A2 109.9 . . ?
C7A C6A H6A2 109.9 . . ?
H6A1 C6A H6A2 108.3 . . ?
C8A C7A C6A 106.3(9) . . ?
C8A C7A H7A1 110.5 . . ?
C6A C7A H7A1 110.5 . . ?
C8A C7A H7A2 110.5 . . ?
C6A C7A H7A2 110.5 . . ?
H7A1 C7A H7A2 108.7 . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C10A C9A N1A 114.3(6) . . ?
C10A C9A H9A1 108.7 . . ?
N1A C9A H9A1 108.7 . . ?
C10A C9A H9A2 108.7 . . ?
N1A C9A H9A2 108.7 . . ?
H9A1 C9A H9A2 107.6 . . ?
C9A C10A C11A 116.6(8) . . ?
C9A C10A H10A 108.2 . . ?
C11A C10A H10A 108.2 . . ?
C9A C10A H10B 108.2 . . ?
C11A C10A H10B 108.2 . . ?
H10A C10A H10B 107.3 . . ?
C12A C11A C10A 109.9(10) . . ?
C12A C11A H11A 109.7 . . ?
C10A C11A H11A 109.7 . . ?
C12A C11A H11B 109.7 . . ?
C10A C11A H11B 109.7 . . ?
H11A C11A H11B 108.2 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N1A C13A C14A 116.5(6) . . ?
N1A C13A H13A 108.2 . . ?
C14A C13A H13A 108.2 . . ?
N1A C13A H13B 108.2 . . ?
C14A C13A H13B 108.2 . . ?
H13A C13A H13B 107.3 . . ?
C15A C14A C13A 114.8(8) . . ?
C13A C14A C15X 109.1(8) . . ?
C15A C14A H14A 108.6 . . ?
C13A C14A H14A 108.6 . . ?
C15A C14A H14B 108.6 . . ?
C13A C14A H14B 108.6 . . ?
H14A C14A H14B 107.5 . . ?
C16A C15A C14A 113.9(10) . . ?
C16A C15A H15A 108.8 . . ?
C14A C15A H15A 108.8 . . ?
C16A C15A H15B 108.8 . . ?
C14A C15A H15B 108.8 . . ?
H15A C15A H15B 107.7 . . ?
C15A C16A H16A 109.5 . . ?
C15A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C16X C15X C14A 113.6(10) . . ?
C16X C15X H15C 108.9 . . ?
C14A C15X H15C 108.9 . . ?
C16X C15X H15D 108.9 . . ?
C14A C15X H15D 108.9 . . ?
H15C C15X H15D 107.7 . . ?
C15X C16X H16D 109.5 . . ?
C15X C16X H16E 109.5 . . ?
H16D C16X H16E 109.5 . . ?
C15X C16X H16F 109.5 . . ?
H16D C16X H16F 109.5 . . ?
H16E C16X H16F 109.5 . . ?
C1B N1B C5B 142.3(9) . . ?
C5Y N1B C13Y 111.2(10) . . ?
C5Y N1B C9Y 108.8(10) . . ?
C13Y N1B C9Y 107.3(9) . . ?
C1B N1B C13B 77.5(7) . . ?
C5B N1B C13B 114.4(8) . . ?
C1B N1B C9B 98.9(9) . . ?
C5B N1B C9B 110.8(9) . . ?
C13B N1B C9B 105.6(8) . . ?
C5Y N1B C1Y 78.6(7) . . ?
C13Y N1B C1Y 148.1(10) . . ?
C9Y N1B C1Y 97.2(9) . . ?
N1B C1B C2B 114.8(10) . . ?
N1B C1B C13B 51.6(5) . . ?
C2B C1B C13B 164.5(12) . . ?
N1B C1B H1B1 108.6 . . ?
C2B C1B H1B1 108.6 . . ?
C13B C1B H1B1 84.7 . . ?
N1B C1B H1B2 108.6 . . ?
C2B C1B H1B2 108.6 . . ?
C13B C1B H1B2 73.5 . . ?
H1B1 C1B H1B2 107.5 . . ?
C1B C2B C3B 113.7(9) . . ?
C1B C2B H2B1 108.8 . . ?
C3B C2B H2B1 108.8 . . ?
C1B C2B H2B2 108.8 . . ?
C3B C2B H2B2 108.8 . . ?
H2B1 C2B H2B2 107.7 . . ?
C2B C3B C4B 111.7(10) . . ?
C2B C3B H3B1 109.3 . . ?
C4B C3B H3B1 109.3 . . ?
C2B C3B H3B2 109.3 . . ?
C4B C3B H3B2 109.3 . . ?
H3B1 C3B H3B2 107.9 . . ?
C3B C4B H4B1 109.5 . . ?
C3B C4B H4B2 109.5 . . ?
H4B1 C4B H4B2 109.5 . . ?
C3B C4B H4B3 109.5 . . ?
H4B1 C4B H4B3 109.5 . . ?
H4B2 C4B H4B3 109.5 . . ?
C2Y C1Y N1B 117.1(9) . . ?
C2Y C1Y C5Y 158.4(11) . . ?
N1B C1Y C5Y 50.4(4) . . ?
C2Y C1Y H1Y1 108 . . ?
N1B C1Y H1Y1 108 . . ?
C5Y C1Y H1Y1 93.4 . . ?
C2Y C1Y H1Y2 108 . . ?
N1B C1Y H1Y2 108 . . ?
C5Y C1Y H1Y2 67 . . ?
H1Y1 C1Y H1Y2 107.3 . . ?
C3Y C2Y C1Y 113.7(17) . . ?
C3Y C2Y H2Y1 108.8 . . ?
C1Y C2Y H2Y1 108.8 . . ?
C3Y C2Y H2Y2 108.8 . . ?
C1Y C2Y H2Y2 108.8 . . ?
H2Y1 C2Y H2Y2 107.7 . . ?
C4Y C3Y C2Y 112.6(11) . . ?
C4Y C3Y H3Y1 109.1 . . ?
C2Y C3Y H3Y1 109.1 . . ?
C4Y C3Y H3Y2 109.1 . . ?
C2Y C3Y H3Y2 109.1 . . ?
H3Y1 C3Y H3Y2 107.8 . . ?
C3Y C4Y H4Y1 109.5 . . ?
C3Y C4Y H4Y2 109.5 . . ?
H4Y1 C4Y H4Y2 109.5 . . ?
C3Y C4Y H4Y3 109.5 . . ?
H4Y1 C4Y H4Y3 109.5 . . ?
H4Y2 C4Y H4Y3 109.5 . . ?
N1B C5B C6B 113.3(10) . . ?
N1B C5B H5B1 108.9 . . ?
C6B C5B H5B1 108.9 . . ?
N1B C5B H5B2 108.9 . . ?
C6B C5B H5B2 108.9 . . ?
H5B1 C5B H5B2 107.7 . . ?
C5B C6B C7B 109.4(10) . . ?
C5B C6B H6B1 109.8 . . ?
C7B C6B H6B1 109.8 . . ?
C5B C6B H6B2 109.8 . . ?
C7B C6B H6B2 109.8 . . ?
H6B1 C6B H6B2 108.2 . . ?
C8B C7B C6B 108.4(17) . . ?
C8B C7B H7B1 110 . . ?
C6B C7B H7B1 110 . . ?
C8B C7B H7B2 110 . . ?
C6B C7B H7B2 110 . . ?
H7B1 C7B H7B2 108.4 . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C6Y C5Y N1B 114.4(8) . . ?
C6Y C5Y C1Y 159.0(13) . . ?
N1B C5Y C1Y 51.0(4) . . ?
C6Y C5Y H5Y1 108.7 . . ?
N1B C5Y H5Y1 108.7 . . ?
C1Y C5Y H5Y1 91.5 . . ?
C6Y C5Y H5Y2 108.7 . . ?
N1B C5Y H5Y2 108.7 . . ?
C1Y C5Y H5Y2 69 . . ?
H5Y1 C5Y H5Y2 107.6 . . ?
C5Y C6Y C7Y 114.3(11) . . ?
C5Y C6Y H6Y1 108.7 . . ?
C7Y C6Y H6Y1 108.7 . . ?
C5Y C6Y H6Y2 108.7 . . ?
C7Y C6Y H6Y2 108.7 . . ?
H6Y1 C6Y H6Y2 107.6 . . ?
C8Y C7Y C6Y 115.6(17) . . ?
C8Y C7Y H7Y1 108.4 . . ?
C6Y C7Y H7Y1 108.4 . . ?
C8Y C7Y H7Y2 108.4 . . ?
C6Y C7Y H7Y2 108.4 . . ?
H7Y1 C7Y H7Y2 107.4 . . ?
C7Y C8Y H8Y1 109.5 . . ?
C7Y C8Y H8Y2 109.5 . . ?
H8Y1 C8Y H8Y2 109.5 . . ?
C7Y C8Y H8Y3 109.5 . . ?
H8Y1 C8Y H8Y3 109.5 . . ?
H8Y2 C8Y H8Y3 109.5 . . ?
C10B C9B N1B 116.5(10) . . ?
C10B C9B H9B1 108.2 . . ?
N1B C9B H9B1 108.2 . . ?
C10B C9B H9B2 108.2 . . ?
N1B C9B H9B2 108.2 . . ?
H9B1 C9B H9B2 107.3 . . ?
C9B C10B C11B 111.4(12) . . ?
C9B C10B H10C 109.4 . . ?
C11B C10B H10C 109.4 . . ?
C9B C10B H10D 109.4 . . ?
C11B C10B H10D 109.4 . . ?
H10C C10B H10D 108 . . ?
C12B C11B C10B 114.3(15) . . ?
C12B C11B H11C 108.7 . . ?
C10B C11B H11C 108.7 . . ?
C12B C11B H11D 108.7 . . ?
C10B C11B H11D 108.7 . . ?
H11C C11B H11D 107.6 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C10Y C9Y N1B 112.9(14) . . ?
C10Y C9Y H9Y1 109 . . ?
N1B C9Y H9Y1 109 . . ?
C10Y C9Y H9Y2 109 . . ?
N1B C9Y H9Y2 109 . . ?
H9Y1 C9Y H9Y2 107.8 . . ?
C9Y C10Y C11Y 109.1(16) . . ?
C9Y C10Y H10E 109.9 . . ?
C11Y C10Y H10E 109.9 . . ?
C9Y C10Y H10F 109.9 . . ?
C11Y C10Y H10F 109.9 . . ?
H10E C10Y H10F 108.3 . . ?
C10Y C11Y C12Y 109.9(17) . . ?
C10Y C11Y H11E 109.7 . . ?
C12Y C11Y H11E 109.7 . . ?
C10Y C11Y H11F 109.7 . . ?
C12Y C11Y H11F 109.7 . . ?
H11E C11Y H11F 108.2 . . ?
C11Y C12Y H12G 109.5 . . ?
C11Y C12Y H12H 109.5 . . ?
H12G C12Y H12H 109.5 . . ?
C11Y C12Y H12I 109.5 . . ?
H12G C12Y H12I 109.5 . . ?
H12H C12Y H12I 109.5 . . ?
C14B C13B N1B 112.8(9) . . ?
C14B C13B C1B 160.0(11) . . ?
N1B C13B C1B 50.8(4) . . ?
C14B C13B H13C 109 . . ?
N1B C13B H13C 109 . . ?
C1B C13B H13C 72 . . ?
C14B C13B H13D 109 . . ?
N1B C13B H13D 109 . . ?
C1B C13B H13D 88.9 . . ?
H13C C13B H13D 107.8 . . ?
C13B C14B C15B 111.6(13) . . ?
C13B C14B H14C 109.3 . . ?
C15B C14B H14C 109.3 . . ?
C13B C14B H14D 109.3 . . ?
C15B C14B H14D 109.3 . . ?
H14C C14B H14D 108 . . ?
C16B C15B C14B 104.9(15) . . ?
C16B C15B H15E 110.8 . . ?
C14B C15B H15E 110.8 . . ?
C16B C15B H15F 110.8 . . ?
C14B C15B H15F 110.8 . . ?
H15E C15B H15F 108.8 . . ?
C15B C16B H16G 109.5 . . ?
C15B C16B H16H 109.5 . . ?
H16G C16B H16H 109.5 . . ?
C15B C16B H16I 109.5 . . ?
H16G C16B H16I 109.5 . . ?
H16H C16B H16I 109.5 . . ?
N1B C13Y C14Y 115.1(11) . . ?
N1B C13Y H13E 108.5 . . ?
C14Y C13Y H13E 108.5 . . ?
N1B C13Y H13F 108.5 . . ?
C14Y C13Y H13F 108.5 . . ?
H13E C13Y H13F 107.5 . . ?
C13Y C14Y C15Y 110.4(11) . . ?
C13Y C14Y H14E 109.6 . . ?
C15Y C14Y H14E 109.6 . . ?
C13Y C14Y H14F 109.6 . . ?
C15Y C14Y H14F 109.6 . . ?
H14E C14Y H14F 108.1 . . ?
C16Y C15Y C14Y 109.7(12) . . ?
C16Y C15Y H15G 109.7 . . ?
C14Y C15Y H15G 109.7 . . ?
C16Y C15Y H15H 109.7 . . ?
C14Y C15Y H15H 109.7 . . ?
H15G C15Y H15H 108.2 . . ?
C15Y C16Y H16J 109.5 . . ?
C15Y C16Y H16K 109.5 . . ?
H16J C16Y H16K 109.5 . . ?
C15Y C16Y H16L 109.5 . . ?
H16J C16Y H16L 109.5 . . ?
H16K C16Y H16L 109.5 . . ?
H31 O3 H32 110.1(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 C1 C6 7.3(16) . . . . ?
C7 N1 C1 C2 -173.9(9) . . . . ?
N1 C1 C2 C3 178.8(9) . . . . ?
C6 C1 C2 C3 -2.4(15) . . . . ?
C1 C2 C3 C4 -0.3(17) . . . . ?
C2 C3 C4 C5 3.0(16) . . . . ?
C3 C4 C5 C6 -3.0(16) . . . . ?
C4 C5 C6 C1 0.4(16) . . . . ?
N1 C1 C6 C5 -179.0(9) . . . . ?
C2 C1 C6 C5 2.3(15) . . . . ?
C8 N2 C7 O1 -8.5(16) . . . . ?
C8 N2 C7 N1 171.6(8) . . . . ?
C1 N1 C7 O1 -5.0(15) . . . . ?
C1 N1 C7 N2 174.9(8) . . . . ?
C7 N2 C8 C9 -163.1(9) . . . . ?
C7 N2 C8 C13 17.3(14) . . . . ?
N2 C8 C9 C10 -178.7(8) . . . . ?
C13 C8 C9 C10 0.9(13) . . . . ?
C8 C9 C10 C11 -2.3(13) . . . . ?
C9 C10 C11 C12 1.1(12) . . . . ?
C9 C10 C11 C14 -178.5(8) . . . . ?
C10 C11 C12 C13 1.4(13) . . . . ?
C14 C11 C12 C13 -179.0(8) . . . . ?
C11 C12 C13 C8 -2.7(13) . . . . ?
C9 C8 C13 C12 1.5(12) . . . . ?
N2 C8 C13 C12 -178.9(8) . . . . ?
C12 C11 C14 C15 -161.9(8) . . . . ?
C10 C11 C14 C15 17.6(12) . . . . ?
C12 C11 C14 C19 17.7(12) . . . . ?
C10 C11 C14 C19 -162.7(8) . . . . ?
C19 C14 C15 C16 -0.2(11) . . . . ?
C11 C14 C15 C16 179.5(7) . . . . ?
C14 C15 C16 C17 0.0(12) . . . . ?
C15 C16 C17 C18 1.1(11) . . . . ?
C15 C16 C17 N3 -178.2(7) . . . . ?
C20 N3 C17 C18 145.2(8) . . . . ?
C20 N3 C17 C16 -35.5(12) . . . . ?
C16 C17 C18 C19 -1.9(12) . . . . ?
N3 C17 C18 C19 177.4(7) . . . . ?
C17 C18 C19 C14 1.8(13) . . . . ?
C15 C14 C19 C18 -0.7(12) . . . . ?
C11 C14 C19 C18 179.7(8) . . . . ?
C17 N3 C20 O2 11.9(14) . . . . ?
C17 N3 C20 N4 -169.0(7) . . . . ?
C21 N4 C20 O2 5.9(14) . . . . ?
C21 N4 C20 N3 -173.3(7) . . . . ?
C20 N4 C21 C26 178.1(8) . . . . ?
C20 N4 C21 C22 -0.5(13) . . . . ?
C26 C21 C22 C23 0.4(13) . . . . ?
N4 C21 C22 C23 178.9(8) . . . . ?
C21 C22 C23 C24 -1.8(14) . . . . ?
C22 C23 C24 C25 2.0(15) . . . . ?
C23 C24 C25 C26 -0.8(14) . . . . ?
C24 C25 C26 C21 -0.6(14) . . . . ?
C22 C21 C26 C25 0.8(13) . . . . ?
N4 C21 C26 C25 -177.8(8) . . . . ?
C13A N1A C1A C2A 65.9(11) . . . . ?
C5A N1A C1A C2A -53.5(12) . . . . ?
C9A N1A C1A C2A -173.2(10) . . . . ?
N1A C1A C2A C3A -175.0(9) . . . . ?
C1A C2A C3A C4A -171.2(11) . . . . ?
C13A N1A C5A C6A -175.1(9) . . . . ?
C1A N1A C5A C6A -51.1(11) . . . . ?
C9A N1A C5A C6A 63.2(10) . . . . ?
N1A C5A C6A C7A -177.4(9) . . . . ?
C5A C6A C7A C8A 79.3(13) . . . . ?
C13A N1A C9A C10A -62.3(10) . . . . ?
C1A N1A C9A C10A 174.9(9) . . . . ?
C5A N1A C9A C10A 56.7(11) . . . . ?
N1A C9A C10A C11A 166.6(9) . . . . ?
C9A C10A C11A C12A 73.8(15) . . . . ?
C1A N1A C13A C14A 59.1(10) . . . . ?
C5A N1A C13A C14A -179.7(8) . . . . ?
C9A N1A C13A C14A -57.5(10) . . . . ?
N1A C13A C14A C15A 168.1(11) . . . . ?
N1A C13A C14A C15X -153.3(10) . . . . ?
C13A C14A C15A C16A -173.9(17) . . . . ?
C13A C14A C15X C16X 71.9(19) . . . . ?
C5B N1B C1B C2B -57(2) . . . . ?
C13B N1B C1B C2B -171.3(16) . . . . ?
C9B N1B C1B C2B 84.6(14) . . . . ?
C5B N1B C1B C13B 113.9(13) . . . . ?
C9B N1B C1B C13B -104.1(8) . . . . ?
N1B C1B C2B C3B 168.3(17) . . . . ?
C13B C1B C2B C3B 142(4) . . . . ?
C1B C2B C3B C4B 179.4(18) . . . . ?
C5Y N1B C1Y C2Y 158.8(13) . . . . ?
C13Y N1B C1Y C2Y 47(2) . . . . ?
C9Y N1B C1Y C2Y -93.4(13) . . . . ?
C13Y N1B C1Y C5Y -111.9(19) . . . . ?
C9Y N1B C1Y C5Y 107.8(10) . . . . ?
N1B C1Y C2Y C3Y 174.4(13) . . . . ?
C5Y C1Y C2Y C3Y -136(2) . . . . ?
C1Y C2Y C3Y C4Y -65(3) . . . . ?
C1B N1B C5B C6B -51.4(18) . . . . ?
C13B N1B C5B C6B 50.0(14) . . . . ?
C9B N1B C5B C6B 169.2(11) . . . . ?
N1B C5B C6B C7B 168.2(16) . . . . ?
C5B C6B C7B C8B 178.8(18) . . . . ?
C13Y N1B C5Y C6Y -49.6(18) . . . . ?
C9Y N1B C5Y C6Y 68.3(17) . . . . ?
C1Y N1B C5Y C6Y 162.1(16) . . . . ?
C13Y N1B C5Y C1Y 148.3(11) . . . . ?
C9Y N1B C5Y C1Y -93.8(10) . . . . ?
N1B C5Y C6Y C7Y 176.1(15) . . . . ?
C1Y C5Y C6Y C7Y -142(3) . . . . ?
C5Y C6Y C7Y C8Y -67(3) . . . . ?
C1B N1B C9B C10B -93.1(15) . . . . ?
C5B N1B C9B C10B 63.1(15) . . . . ?
C13B N1B C9B C10B -172.6(13) . . . . ?
N1B C9B C10B C11B 166.2(15) . . . . ?
C9B C10B C11B C12B -179.6(17) . . . . ?
C5Y N1B C9Y C10Y 176.7(16) . . . . ?
C13Y N1B C9Y C10Y -63(2) . . . . ?
C1Y N1B C9Y C10Y 96.3(17) . . . . ?
N1B C9Y C10Y C11Y -164.9(18) . . . . ?
C9Y C10Y C11Y C12Y -179(2) . . . . ?
C1B N1B C13B C14B -166.6(14) . . . . ?
C5B N1B C13B C14B 51.3(14) . . . . ?
C9B N1B C13B C14B -70.7(13) . . . . ?
C5B N1B C13B C1B -142.1(9) . . . . ?
C9B N1B C13B C1B 95.9(10) . . . . ?
N1B C1B C13B C14B 39(3) . . . . ?
C2B C1B C13B C14B 70(7) . . . . ?
C2B C1B C13B N1B 31(5) . . . . ?
N1B C13B C14B C15B -166.6(16) . . . . ?
C1B C13B C14B C15B 162(3) . . . . ?
C13B C14B C15B C16B -173.2(18) . . . . ?
C5Y N1B C13Y C14Y -56(2) . . . . ?
C9Y N1B C13Y C14Y -174.8(18) . . . . ?
C1Y N1B C13Y C14Y 47(3) . . . . ?
N1B C13Y C14Y C15Y 178(2) . . . . ?
C13Y C14Y C15Y C16Y -166(3) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
####################################################################### 
# 
# 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_1-((TBA)I)2-DMSO
_database_code_depnum_ccdc_archive 'CCDC 2015337'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T15:21:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H22 N4 O2, 2(C16 H36 N), C2 H6 O S, 2(I)'
_chemical_formula_sum            'C60 H100 I2 N6 O3 S'
_chemical_formula_weight         1239.31

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_Int_Tables_number      1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   9.8525(2)
_cell_length_b                   9.8769(2)
_cell_length_c                   17.3039(4)
_cell_angle_alpha                85.666(2)
_cell_angle_beta                 86.551(2)
_cell_angle_gamma                76.335(2)
_cell_volume                     1629.98(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    14119
_cell_measurement_theta_min      4.6090
_cell_measurement_theta_max      76.2150

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_F_000             648

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    8.207
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.38152
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_number            15717
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.617
_diffrn_reflns_theta_max         67.989
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.672
_diffrn_reflns_point_group_measured_fraction_max 0.671
_reflns_Friedel_fraction_full    0.346
_reflns_Friedel_fraction_max     0.346
_reflns_Friedel_coverage         0.347
_reflns_number_total             7966
_reflns_number_gt                7908
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          'Refined as a 2-component inversion twin.,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)+(0.0425P)²+0.0695P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7966
_refine_ls_number_parameters     660
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0691
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.274(4)
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.051


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
I1 I 0.52050(2) -0.03400(2) 0.80027(2) 0.08311(10) Uani 1 1 d . . . . .
I2 I 1.42338(2) 0.43544(2) 0.21392(2) 0.07748(9) Uani 1 1 d . . . . .
S1 S -0.34204(17) 0.6250(2) 1.00799(13) 0.1118(5) Uani 1 1 d . . . . .
O3 O -0.4150(5) 0.5491(7) 0.9601(3) 0.1258(16) Uani 1 1 d . . . . .
C1C C -0.2069(11) 0.6757(11) 0.9452(6) 0.141(3) Uani 1 1 d . . . . .
H1CA H -0.161801 0.599482 0.914471 0.211 Uiso 1 1 calc GR . . . .
H1CB H -0.139322 0.699698 0.9761 0.211 Uiso 1 1 calc GR . . . .
H1CC H -0.247792 0.754971 0.911701 0.211 Uiso 1 1 calc GR . . . .
C2C C -0.2332(12) 0.4954(14) 1.0667(6) 0.157(4) Uani 1 1 d . . . . .
H2CA H -0.289185 0.442371 1.097549 0.236 Uiso 1 1 calc GR . . . .
H2CB H -0.184182 0.538811 1.100199 0.236 Uiso 1 1 calc GR . . . .
H2CC H -0.167009 0.434435 1.034448 0.236 Uiso 1 1 calc GR . . . .
O2 O 0.8939(3) 0.7353(4) 0.1759(2) 0.0860(9) Uani 1 1 d . . . . .
O1 O 0.2628(5) 0.0877(5) 0.5268(2) 0.0997(11) Uani 1 1 d . . . . .
N1 N 0.2700(4) 0.0043(4) 0.6542(2) 0.0795(9) Uani 1 1 d . . . . .
H1 H 0.319823 -0.003485 0.694201 0.095 Uiso 1 1 calc R . . . .
N2 N 0.4447(4) 0.0970(4) 0.6016(2) 0.0711(8) Uani 1 1 d . . . . .
H2 H 0.478358 0.069696 0.646386 0.085 Uiso 1 1 calc R . . . .
N3 N 1.0472(4) 0.5708(4) 0.2474(2) 0.0734(8) Uani 1 1 d . . . . .
H3 H 1.135131 0.539028 0.253809 0.088 Uiso 1 1 calc R . . . .
N4 N 1.1279(4) 0.6845(4) 0.1431(2) 0.0773(9) Uani 1 1 d . . . . .
H4 H 1.205898 0.630828 0.156969 0.093 Uiso 1 1 calc R . . . .
C1 C 0.1484(5) -0.0469(5) 0.6651(3) 0.0772(11) Uani 1 1 d . . . . .
C2 C 0.1173(7) -0.0940(7) 0.7389(4) 0.0948(16) Uani 1 1 d . . . . .
H2A H 0.176105 -0.091382 0.778607 0.114 Uiso 1 1 calc R . . . .
C3 C -0.0027(8) -0.1461(8) 0.7552(5) 0.118(2) Uani 1 1 d . . . . .
H3A H -0.022811 -0.17775 0.805549 0.142 Uiso 1 1 calc R . . . .
C4 C -0.0889(7) -0.1506(8) 0.6985(7) 0.132(3) Uani 1 1 d . . . . .
H4A H -0.169277 -0.183794 0.709399 0.159 Uiso 1 1 calc R . . . .
C5 C -0.0559(6) -0.1055(8) 0.6246(6) 0.116(2) Uani 1 1 d . . . . .
H5 H -0.113948 -0.110959 0.585111 0.139 Uiso 1 1 calc R . . . .
C6 C 0.0590(6) -0.0529(7) 0.6069(4) 0.0985(15) Uani 1 1 d . . . . .
H6 H 0.077424 -0.021269 0.556254 0.118 Uiso 1 1 calc R . . . .
C7 C 0.3195(5) 0.0651(4) 0.5879(3) 0.0726(10) Uani 1 1 d . . . . .
C8 C 0.5233(4) 0.1694(4) 0.5503(2) 0.0632(8) Uani 1 1 d . . . . .
C9 C 0.4740(4) 0.2442(5) 0.4826(2) 0.0706(9) Uani 1 1 d . . . . .
H9 H 0.383566 0.248155 0.468353 0.085 Uiso 1 1 calc R . . . .
C10 C 0.5599(5) 0.3139(5) 0.4358(2) 0.0700(9) Uani 1 1 d . . . . .
H10 H 0.525664 0.362524 0.390211 0.084 Uiso 1 1 calc R . . . .
C11 C 0.6968(4) 0.3123(4) 0.4557(2) 0.0613(8) Uani 1 1 d . . . . .
C12 C 0.7422(5) 0.2372(4) 0.5249(2) 0.0688(8) Uani 1 1 d . . . . .
H12 H 0.831741 0.234167 0.540303 0.083 Uiso 1 1 calc R . . . .
C13 C 0.6582(5) 0.1674(4) 0.5711(2) 0.0705(9) Uani 1 1 d . . . . .
H13 H 0.692126 0.118328 0.616606 0.085 Uiso 1 1 calc R . . . .
C14 C 0.7870(4) 0.3830(4) 0.4038(2) 0.0639(8) Uani 1 1 d . . . . .
C15 C 0.7323(5) 0.4716(5) 0.3416(3) 0.0736(10) Uani 1 1 d . . . . .
H15 H 0.636979 0.487982 0.334183 0.088 Uiso 1 1 calc R . . . .
C16 C 0.8140(5) 0.5375(5) 0.2895(3) 0.0719(10) Uani 1 1 d . . . . .
H16 H 0.772992 0.595933 0.248419 0.086 Uiso 1 1 calc R . . . .
C17 C 0.9560(4) 0.5153(4) 0.2995(2) 0.0654(8) Uani 1 1 d . . . . .
C18 C 1.0127(5) 0.4276(6) 0.3617(3) 0.0800(11) Uani 1 1 d . . . . .
H18 H 1.107886 0.411839 0.36941 0.096 Uiso 1 1 calc R . . . .
C19 C 0.9300(5) 0.3631(5) 0.4127(2) 0.0762(10) Uani 1 1 d . . . . .
H19 H 0.97106 0.305063 0.453956 0.091 Uiso 1 1 calc R . . . .
C20 C 1.0119(4) 0.6690(4) 0.1879(2) 0.0667(8) Uani 1 1 d . . . . .
C21 C 1.1363(4) 0.7759(4) 0.0779(2) 0.0633(8) Uani 1 1 d . . . . .
C22 C 1.0240(5) 0.8742(6) 0.0486(3) 0.0819(12) Uani 1 1 d . . . . .
H22 H 0.934484 0.881354 0.070737 0.098 Uiso 1 1 calc R . . . .
C23 C 1.0476(6) 0.9620(7) -0.0147(3) 0.0997(16) Uani 1 1 d . . . . .
H23 H 0.97324 1.030491 -0.033738 0.12 Uiso 1 1 calc R . . . .
C24 C 1.1794(7) 0.9497(7) -0.0500(3) 0.0901(14) Uani 1 1 d . . . . .
H24 H 1.193132 1.007083 -0.093479 0.108 Uiso 1 1 calc R . . . .
C25 C 1.2878(5) 0.8532(6) -0.0203(3) 0.0812(11) Uani 1 1 d . . . . .
H25 H 1.377105 0.845864 -0.042875 0.097 Uiso 1 1 calc R . . . .
C26 C 1.2678(5) 0.7653(5) 0.0432(3) 0.0719(10) Uani 1 1 d . . . . .
H26 H 1.343376 0.698734 0.062519 0.086 Uiso 1 1 calc R . . . .
N1A N 0.4230(4) 0.9620(4) 0.2584(2) 0.0663(7) Uani 1 1 d . . . . .
C1A C 0.3946(5) 0.8235(4) 0.2926(3) 0.0731(9) Uani 1 1 d . . . . .
H1AA H 0.338166 0.791704 0.256937 0.088 Uiso 1 1 calc R . . . .
H1AB H 0.483267 0.755185 0.295033 0.088 Uiso 1 1 calc R . . . .
C2A C 0.3223(6) 0.8249(5) 0.3719(3) 0.0789(11) Uani 1 1 d . . . . .
H2AA H 0.377705 0.854665 0.408924 0.095 Uiso 1 1 calc R . . . .
H2AB H 0.23179 0.890222 0.370589 0.095 Uiso 1 1 calc R . . . .
C3A C 0.3039(9) 0.6807(7) 0.3965(4) 0.1063(19) Uani 1 1 d D . . . .
H3AA H 0.249275 0.65254 0.358478 0.128 Uiso 1 1 calc R . . . .
H3AB H 0.395231 0.616593 0.39581 0.128 Uiso 1 1 calc R . . . .
C4A C 0.2341(8) 0.6659(9) 0.4753(4) 0.1107(19) Uani 1 1 d D . . . .
H4AA H 0.134532 0.694073 0.471358 0.166 Uiso 1 1 calc GR . . . .
H4AB H 0.263613 0.723929 0.50988 0.166 Uiso 1 1 calc GR . . . .
H4AC H 0.259732 0.570275 0.495079 0.166 Uiso 1 1 calc GR . . . .
C5A C 0.2887(5) 1.0765(4) 0.2559(3) 0.0712(9) Uani 1 1 d . . . . .
H5AA H 0.251975 1.090435 0.308674 0.085 Uiso 1 1 calc R . . . .
H5AB H 0.312337 1.162599 0.23541 0.085 Uiso 1 1 calc R . . . .
C6A C 0.1740(5) 1.0519(6) 0.2087(3) 0.0843(12) Uani 1 1 d . . . . .
H6AA H 0.153643 0.962372 0.225145 0.101 Uiso 1 1 calc R . . . .
H6AB H 0.203561 1.050511 0.154255 0.101 Uiso 1 1 calc R . . . .
C7A C 0.0442(6) 1.1680(7) 0.2204(4) 0.1013(16) Uani 1 1 d . . . . .
H7AA H 0.017654 1.168917 0.275286 0.122 Uiso 1 1 calc R . . . .
H7AB H 0.067248 1.256565 0.20467 0.122 Uiso 1 1 calc R . . . .
C8A C -0.0798(8) 1.1565(9) 0.1764(5) 0.123(2) Uani 1 1 d . . . . .
H8AA H -0.066923 1.185986 0.122856 0.184 Uiso 1 1 calc GR . . . .
H8AB H -0.163312 1.214894 0.198092 0.184 Uiso 1 1 calc GR . . . .
H8AC H -0.088168 1.061308 0.18022 0.184 Uiso 1 1 calc GR . . . .
C9A C 0.4878(5) 0.9344(5) 0.1770(3) 0.0730(9) Uani 1 1 d . . . . .
H9AA H 0.567717 0.855445 0.180825 0.088 Uiso 1 1 calc R . . . .
H9AB H 0.419918 0.908269 0.146308 0.088 Uiso 1 1 calc R . . . .
C10A C 0.5350(6) 1.0560(5) 0.1343(3) 0.0808(11) Uani 1 1 d . . . . .
H10A H 0.457197 1.13731 0.132617 0.097 Uiso 1 1 calc R . . . .
H10B H 0.608547 1.078264 0.16224 0.097 Uiso 1 1 calc R . . . .
C11A C 0.5884(7) 1.0231(7) 0.0524(3) 0.0933(14) Uani 1 1 d . . . . .
H11A H 0.662932 0.939018 0.0545 0.112 Uiso 1 1 calc R . . . .
H11B H 0.513267 1.004115 0.024369 0.112 Uiso 1 1 calc R . . . .
C12A C 0.6421(7) 1.1381(8) 0.0085(4) 0.1057(18) Uani 1 1 d . . . . .
H12A H 0.679299 1.108528 -0.041597 0.158 Uiso 1 1 calc GR . . . .
H12B H 0.714356 1.159896 0.036746 0.158 Uiso 1 1 calc GR . . . .
H12C H 0.566954 1.219588 0.00234 0.158 Uiso 1 1 calc GR . . . .
C13A C 0.5204(5) 1.0125(4) 0.3078(2) 0.0680(9) Uani 1 1 d . . . . .
H13A H 0.4754 1.027438 0.358833 0.082 Uiso 1 1 calc R . . . .
H13B H 0.531522 1.102373 0.285258 0.082 Uiso 1 1 calc R . . . .
C14A C 0.6645(5) 0.9187(5) 0.3179(3) 0.0735(10) Uani 1 1 d . . . . .
H14A H 0.656334 0.830472 0.344161 0.088 Uiso 1 1 calc R . . . .
H14B H 0.710593 0.899676 0.267395 0.088 Uiso 1 1 calc R . . . .
C15A C 0.7504(5) 0.9873(6) 0.3644(3) 0.0815(11) Uani 1 1 d . . . . .
H15A H 0.703336 1.006291 0.414638 0.098 Uiso 1 1 calc R . . . .
H15B H 0.756968 1.075879 0.33806 0.098 Uiso 1 1 calc R . . . .
C16A C 0.8972(6) 0.8981(8) 0.3763(4) 0.1075(18) Uani 1 1 d . . . . .
H16A H 0.945415 0.881246 0.326865 0.161 Uiso 1 1 calc GR . . . .
H16B H 0.891485 0.810633 0.403028 0.161 Uiso 1 1 calc GR . . . .
H16C H 0.947212 0.946034 0.406649 0.161 Uiso 1 1 calc GR . . . .
N1B N 0.4409(3) 0.4635(4) 0.7506(2) 0.0640(7) Uani 1 1 d . . . . .
C1B C 0.3741(5) 0.5010(5) 0.8295(3) 0.0734(10) Uani 1 1 d D . . . .
H1BA H 0.4411 0.532158 0.858453 0.088 Uiso 1 1 calc R . . . .
H1BB H 0.29485 0.579782 0.821989 0.088 Uiso 1 1 calc R . . . .
C2B C 0.3240(6) 0.3880(6) 0.8789(3) 0.0850(12) Uani 1 1 d D . . . .
H2BA H 0.255004 0.356847 0.851492 0.102 Uiso 1 1 calc R . . . .
H2BB H 0.402082 0.308767 0.887994 0.102 Uiso 1 1 calc R . . . .
C3B C 0.2607(8) 0.4401(8) 0.9552(4) 0.112(2) Uani 1 1 d D . . . .
H3BA H 0.185624 0.521977 0.945335 0.134 Uiso 1 1 calc R . . . .
H3BB H 0.331154 0.468867 0.982571 0.134 Uiso 1 1 calc R . . . .
C4B C 0.2031(10) 0.3342(11) 1.0071(4) 0.135(3) Uani 1 1 d D . . . .
H4BA H 0.180247 0.266996 0.975923 0.202 Uiso 1 1 calc GR . . . .
H4BB H 0.120548 0.381057 1.035237 0.202 Uiso 1 1 calc GR . . . .
H4BC H 0.272152 0.287399 1.043043 0.202 Uiso 1 1 calc GR . . . .
C5B C 0.3478(5) 0.4016(5) 0.7041(3) 0.0679(9) Uani 1 1 d . . . . .
H5BA H 0.33814 0.314236 0.73083 0.082 Uiso 1 1 calc R . . . .
H5BB H 0.395571 0.379339 0.654326 0.082 Uiso 1 1 calc R . . . .
C6B C 0.2017(5) 0.4901(5) 0.6888(3) 0.0744(10) Uani 1 1 d . . . . .
H6BA H 0.150877 0.513129 0.737671 0.089 Uiso 1 1 calc R . . . .
H6BB H 0.208127 0.576485 0.65981 0.089 Uiso 1 1 calc R . . . .
C7B C 0.1255(6) 0.4087(6) 0.6431(3) 0.0844(12) Uani 1 1 d . . . . .
H7BA H 0.118344 0.323581 0.673229 0.101 Uiso 1 1 calc R . . . .
H7BB H 0.179882 0.382395 0.595687 0.101 Uiso 1 1 calc R . . . .
C8B C -0.0198(6) 0.4901(8) 0.6225(4) 0.1067(18) Uani 1 1 d . . . . .
H8BA H -0.013442 0.573711 0.591926 0.16 Uiso 1 1 calc GR . . . .
H8BB H -0.07512 0.514163 0.669251 0.16 Uiso 1 1 calc GR . . . .
H8BC H -0.062916 0.433852 0.593443 0.16 Uiso 1 1 calc GR . . . .
C9B C 0.4697(4) 0.5961(4) 0.7102(3) 0.0708(9) Uani 1 1 d . . . . .
H9BA H 0.380943 0.662524 0.702732 0.085 Uiso 1 1 calc R . . . .
H9BB H 0.522294 0.635953 0.74431 0.085 Uiso 1 1 calc R . . . .
C10B C 0.5488(5) 0.5795(5) 0.6326(3) 0.0783(10) Uani 1 1 d . . . . .
H10C H 0.498287 0.53877 0.597768 0.094 Uiso 1 1 calc R . . . .
H10D H 0.640004 0.517092 0.639278 0.094 Uiso 1 1 calc R . . . .
C11B C 0.5663(7) 0.7200(6) 0.5977(3) 0.0977(16) Uani 1 1 d D . . . .
H11C H 0.474299 0.780032 0.589638 0.117 Uiso 1 1 calc R . . . .
H11D H 0.611023 0.762256 0.634752 0.117 Uiso 1 1 calc R . . . .
C12B C 0.6504(8) 0.7151(8) 0.5220(4) 0.1114(19) Uani 1 1 d D . . . .
H12D H 0.607728 0.672745 0.484854 0.167 Uiso 1 1 calc GR . . . .
H12E H 0.743796 0.661225 0.529887 0.167 Uiso 1 1 calc GR . . . .
H12F H 0.65331 0.808309 0.502993 0.167 Uiso 1 1 calc GR . . . .
C13B C 0.5747(4) 0.3502(5) 0.7581(3) 0.0711(9) Uani 1 1 d D . . . .
H13C H 0.550999 0.26829 0.784767 0.085 Uiso 1 1 calc R . . . .
H13D H 0.610164 0.325161 0.706372 0.085 Uiso 1 1 calc R . . . .
C14B C 0.6910(5) 0.3838(6) 0.7999(3) 0.0822(11) Uani 1 1 d D . . . .
H14C H 0.662684 0.397259 0.853994 0.099 Uiso 1 1 calc R . . . .
H14D H 0.712689 0.469155 0.776797 0.099 Uiso 1 1 calc R . . . .
C15B C 0.8206(6) 0.2618(7) 0.7938(4) 0.0952(14) Uani 1 1 d . . . . .
H15C H 0.796539 0.176029 0.814516 0.114 Uiso 1 1 calc R . . . .
H15D H 0.849928 0.251043 0.739599 0.114 Uiso 1 1 calc R . . . .
C16B C 0.9391(7) 0.2861(9) 0.8374(5) 0.118(2) Uani 1 1 d . . . . .
H16D H 0.958538 0.374237 0.819435 0.177 Uiso 1 1 calc GR . . . .
H16E H 1.0208 0.212725 0.828697 0.177 Uiso 1 1 calc GR . . . .
H16F H 0.913742 0.286836 0.891787 0.177 Uiso 1 1 calc GR . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O3 1.478(5) . ?
S1 C1C 1.806(10) . ?
S1 C2C 1.763(11) . ?
C1C H1CA 0.96 . ?
C1C H1CB 0.96 . ?
C1C H1CC 0.96 . ?
C2C H2CA 0.96 . ?
C2C H2CB 0.96 . ?
C2C H2CC 0.96 . ?
O2 C20 1.214(5) . ?
O1 C7 1.205(6) . ?
N1 H1 0.86 . ?
N1 C1 1.404(6) . ?
N1 C7 1.372(6) . ?
N2 H2 0.86 . ?
N2 C7 1.382(7) . ?
N2 C8 1.408(5) . ?
N3 H3 0.86 . ?
N3 C17 1.407(5) . ?
N3 C20 1.361(6) . ?
N4 H4 0.86 . ?
N4 C20 1.374(5) . ?
N4 C21 1.401(6) . ?
C1 C2 1.369(8) . ?
C1 C6 1.391(9) . ?
C2 H2A 0.93 . ?
C2 C3 1.402(9) . ?
C3 H3A 0.93 . ?
C3 C4 1.345(13) . ?
C4 H4A 0.93 . ?
C4 C5 1.368(13) . ?
C5 H5 0.93 . ?
C5 C6 1.363(9) . ?
C6 H6 0.93 . ?
C8 C9 1.386(6) . ?
C8 C13 1.393(7) . ?
C9 H9 0.93 . ?
C9 C10 1.398(6) . ?
C10 H10 0.93 . ?
C10 C11 1.409(7) . ?
C11 C12 1.399(6) . ?
C11 C14 1.479(5) . ?
C12 H12 0.93 . ?
C12 C13 1.380(6) . ?
C13 H13 0.93 . ?
C14 C15 1.385(6) . ?
C14 C19 1.391(6) . ?
C15 H15 0.93 . ?
C15 C16 1.398(6) . ?
C16 H16 0.93 . ?
C16 C17 1.384(6) . ?
C17 C18 1.388(6) . ?
C18 H18 0.93 . ?
C18 C19 1.387(7) . ?
C19 H19 0.93 . ?
C21 C22 1.382(7) . ?
C21 C26 1.380(6) . ?
C22 H22 0.93 . ?
C22 C23 1.387(7) . ?
C23 H23 0.93 . ?
C23 C24 1.384(8) . ?
C24 H24 0.93 . ?
C24 C25 1.350(9) . ?
C25 H25 0.93 . ?
C25 C26 1.382(7) . ?
C26 H26 0.93 . ?
N1A C1A 1.529(6) . ?
N1A C5A 1.524(6) . ?
N1A C9A 1.529(5) . ?
N1A C13A 1.512(6) . ?
C1A H1AA 0.97 . ?
C1A H1AB 0.97 . ?
C1A C2A 1.508(7) . ?
C2A H2AA 0.97 . ?
C2A H2AB 0.97 . ?
C2A C3A 1.504(8) . ?
C3A H3AA 0.97 . ?
C3A H3AB 0.97 . ?
C3A C4A 1.503(7) . ?
C4A H4AA 0.96 . ?
C4A H4AB 0.96 . ?
C4A H4AC 0.96 . ?
C5A H5AA 0.97 . ?
C5A H5AB 0.97 . ?
C5A C6A 1.507(6) . ?
C6A H6AA 0.97 . ?
C6A H6AB 0.97 . ?
C6A C7A 1.517(8) . ?
C7A H7AA 0.97 . ?
C7A H7AB 0.97 . ?
C7A C8A 1.509(9) . ?
C8A H8AA 0.96 . ?
C8A H8AB 0.96 . ?
C8A H8AC 0.96 . ?
C9A H9AA 0.97 . ?
C9A H9AB 0.97 . ?
C9A C10A 1.514(7) . ?
C10A H10A 0.97 . ?
C10A H10B 0.97 . ?
C10A C11A 1.512(6) . ?
C11A H11A 0.97 . ?
C11A H11B 0.97 . ?
C11A C12A 1.502(9) . ?
C12A H12A 0.96 . ?
C12A H12B 0.96 . ?
C12A H12C 0.96 . ?
C13A H13A 0.97 . ?
C13A H13B 0.97 . ?
C13A C14A 1.513(6) . ?
C14A H14A 0.97 . ?
C14A H14B 0.97 . ?
C14A C15A 1.503(7) . ?
C15A H15A 0.97 . ?
C15A H15B 0.97 . ?
C15A C16A 1.522(8) . ?
C16A H16A 0.96 . ?
C16A H16B 0.96 . ?
C16A H16C 0.96 . ?
N1B C1B 1.513(5) . ?
N1B C5B 1.514(5) . ?
N1B C9B 1.515(5) . ?
N1B C13B 1.519(5) . ?
C1B H1BA 0.97 . ?
C1B H1BB 0.97 . ?
C1B C2B 1.512(6) . ?
C2B H2BA 0.97 . ?
C2B H2BB 0.97 . ?
C2B C3B 1.499(7) . ?
C3B H3BA 0.97 . ?
C3B H3BB 0.97 . ?
C3B C4B 1.517(8) . ?
C4B H4BA 0.96 . ?
C4B H4BB 0.96 . ?
C4B H4BC 0.96 . ?
C5B H5BA 0.97 . ?
C5B H5BB 0.97 . ?
C5B C6B 1.524(6) . ?
C6B H6BA 0.97 . ?
C6B H6BB 0.97 . ?
C6B C7B 1.513(7) . ?
C7B H7BA 0.97 . ?
C7B H7BB 0.97 . ?
C7B C8B 1.516(8) . ?
C8B H8BA 0.96 . ?
C8B H8BB 0.96 . ?
C8B H8BC 0.96 . ?
C9B H9BA 0.97 . ?
C9B H9BB 0.97 . ?
C9B C10B 1.512(6) . ?
C10B H10C 0.97 . ?
C10B H10D 0.97 . ?
C10B C11B 1.514(7) . ?
C11B H11C 0.97 . ?
C11B H11D 0.97 . ?
C11B C12B 1.505(7) . ?
C12B H12D 0.96 . ?
C12B H12E 0.96 . ?
C12B H12F 0.96 . ?
C13B H13C 0.97 . ?
C13B H13D 0.97 . ?
C13B C14B 1.504(6) . ?
C14B H14C 0.97 . ?
C14B H14D 0.97 . ?
C14B C15B 1.539(7) . ?
C15B H15C 0.97 . ?
C15B H15D 0.97 . ?
C15B C16B 1.502(9) . ?
C16B H16D 0.96 . ?
C16B H16E 0.96 . ?
C16B H16F 0.96 . ?

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
O3 S1 C1C 106.2(4) . . ?
O3 S1 C2C 105.6(5) . . ?
C2C S1 C1C 97.9(5) . . ?
S1 C1C H1CA 109.5 . . ?
S1 C1C H1CB 109.5 . . ?
S1 C1C H1CC 109.5 . . ?
H1CA C1C H1CB 109.5 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?
S1 C2C H2CA 109.5 . . ?
S1 C2C H2CB 109.5 . . ?
S1 C2C H2CC 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
C1 N1 H1 115.9 . . ?
C7 N1 H1 115.9 . . ?
C7 N1 C1 128.1(5) . . ?
C7 N2 H2 116.5 . . ?
C7 N2 C8 127.0(4) . . ?
C8 N2 H2 116.5 . . ?
C17 N3 H3 116.3 . . ?
C20 N3 H3 116.3 . . ?
C20 N3 C17 127.4(4) . . ?
C20 N4 H4 115.6 . . ?
C20 N4 C21 128.8(4) . . ?
C21 N4 H4 115.6 . . ?
C2 C1 N1 116.6(5) . . ?
C2 C1 C6 118.5(5) . . ?
C6 C1 N1 125.0(5) . . ?
C1 C2 H2A 119.8 . . ?
C1 C2 C3 120.4(7) . . ?
C3 C2 H2A 119.8 . . ?
C2 C3 H3A 119.7 . . ?
C4 C3 C2 120.6(8) . . ?
C4 C3 H3A 119.7 . . ?
C3 C4 H4A 120.7 . . ?
C3 C4 C5 118.6(6) . . ?
C5 C4 H4A 120.7 . . ?
C4 C5 H5 118.8 . . ?
C6 C5 C4 122.3(8) . . ?
C6 C5 H5 118.8 . . ?
C1 C6 H6 120.2 . . ?
C5 C6 C1 119.5(7) . . ?
C5 C6 H6 120.2 . . ?
O1 C7 N1 125.5(5) . . ?
O1 C7 N2 124.9(4) . . ?
N1 C7 N2 109.5(4) . . ?
C9 C8 N2 124.5(4) . . ?
C9 C8 C13 118.8(4) . . ?
C13 C8 N2 116.7(4) . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.1(4) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.1 . . ?
C9 C10 C11 121.8(4) . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C14 120.7(4) . . ?
C12 C11 C10 116.3(4) . . ?
C12 C11 C14 123.0(4) . . ?
C11 C12 H12 119 . . ?
C13 C12 C11 122.1(4) . . ?
C13 C12 H12 119 . . ?
C8 C13 H13 119.6 . . ?
C12 C13 C8 120.8(4) . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C11 120.8(4) . . ?
C15 C14 C19 116.2(4) . . ?
C19 C14 C11 123.0(4) . . ?
C14 C15 H15 118.5 . . ?
C14 C15 C16 123.0(4) . . ?
C16 C15 H15 118.5 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.7(4) . . ?
C17 C16 H16 120.2 . . ?
C16 C17 N3 123.4(4) . . ?
C16 C17 C18 118.2(4) . . ?
C18 C17 N3 118.3(4) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.2(4) . . ?
C19 C18 H18 119.4 . . ?
C14 C19 H19 119.2 . . ?
C18 C19 C14 121.7(4) . . ?
C18 C19 H19 119.2 . . ?
O2 C20 N3 124.9(4) . . ?
O2 C20 N4 124.0(4) . . ?
N3 C20 N4 111.1(4) . . ?
C22 C21 N4 124.5(4) . . ?
C26 C21 N4 115.9(4) . . ?
C26 C21 C22 119.6(4) . . ?
C21 C22 H22 120.6 . . ?
C21 C22 C23 118.7(4) . . ?
C23 C22 H22 120.6 . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.4(5) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 120.5 . . ?
C25 C24 C23 119.0(5) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 H25 119.5 . . ?
C24 C25 C26 120.9(4) . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C25 120.4(5) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C5A N1A C1A 111.2(3) . . ?
C5A N1A C9A 111.2(4) . . ?
C9A N1A C1A 106.0(3) . . ?
C13A N1A C1A 111.2(3) . . ?
C13A N1A C5A 106.2(3) . . ?
C13A N1A C9A 111.1(3) . . ?
N1A C1A H1AA 108.2 . . ?
N1A C1A H1AB 108.2 . . ?
H1AA C1A H1AB 107.3 . . ?
C2A C1A N1A 116.5(4) . . ?
C2A C1A H1AA 108.2 . . ?
C2A C1A H1AB 108.2 . . ?
C1A C2A H2AA 109.8 . . ?
C1A C2A H2AB 109.8 . . ?
H2AA C2A H2AB 108.2 . . ?
C3A C2A C1A 109.4(4) . . ?
C3A C2A H2AA 109.8 . . ?
C3A C2A H2AB 109.8 . . ?
C2A C3A H3AA 108.5 . . ?
C2A C3A H3AB 108.5 . . ?
H3AA C3A H3AB 107.5 . . ?
C4A C3A C2A 115.3(6) . . ?
C4A C3A H3AA 108.4 . . ?
C4A C3A H3AB 108.4 . . ?
C3A C4A H4AA 109.5 . . ?
C3A C4A H4AB 109.5 . . ?
C3A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
N1A C5A H5AA 108.1 . . ?
N1A C5A H5AB 108.1 . . ?
H5AA C5A H5AB 107.3 . . ?
C6A C5A N1A 116.6(3) . . ?
C6A C5A H5AA 108.1 . . ?
C6A C5A H5AB 108.1 . . ?
C5A C6A H6AA 109.9 . . ?
C5A C6A H6AB 109.9 . . ?
C5A C6A C7A 109.0(4) . . ?
H6AA C6A H6AB 108.3 . . ?
C7A C6A H6AA 109.9 . . ?
C7A C6A H6AB 109.9 . . ?
C6A C7A H7AA 108.6 . . ?
C6A C7A H7AB 108.6 . . ?
H7AA C7A H7AB 107.6 . . ?
C8A C7A C6A 114.7(6) . . ?
C8A C7A H7AA 108.6 . . ?
C8A C7A H7AB 108.6 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
N1A C9A H9AA 108.5 . . ?
N1A C9A H9AB 108.5 . . ?
H9AA C9A H9AB 107.5 . . ?
C10A C9A N1A 115.1(3) . . ?
C10A C9A H9AA 108.5 . . ?
C10A C9A H9AB 108.5 . . ?
C9A C10A H10A 109.3 . . ?
C9A C10A H10B 109.3 . . ?
H10A C10A H10B 108 . . ?
C11A C10A C9A 111.5(4) . . ?
C11A C10A H10A 109.3 . . ?
C11A C10A H10B 109.3 . . ?
C10A C11A H11A 108.8 . . ?
C10A C11A H11B 108.8 . . ?
H11A C11A H11B 107.7 . . ?
C12A C11A C10A 113.7(5) . . ?
C12A C11A H11A 108.8 . . ?
C12A C11A H11B 108.8 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N1A C13A H13A 108.1 . . ?
N1A C13A H13B 108.1 . . ?
N1A C13A C14A 116.9(3) . . ?
H13A C13A H13B 107.3 . . ?
C14A C13A H13A 108.1 . . ?
C14A C13A H13B 108.1 . . ?
C13A C14A H14A 109.6 . . ?
C13A C14A H14B 109.6 . . ?
H14A C14A H14B 108.1 . . ?
C15A C14A C13A 110.2(4) . . ?
C15A C14A H14A 109.6 . . ?
C15A C14A H14B 109.6 . . ?
C14A C15A H15A 109 . . ?
C14A C15A H15B 109 . . ?
C14A C15A C16A 112.8(5) . . ?
H15A C15A H15B 107.8 . . ?
C16A C15A H15A 109 . . ?
C16A C15A H15B 109 . . ?
C15A C16A H16A 109.5 . . ?
C15A C16A H16B 109.5 . . ?
C15A C16A H16C 109.5 . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C1B N1B C5B 111.4(3) . . ?
C1B N1B C9B 106.9(3) . . ?
C1B N1B C13B 111.0(3) . . ?
C5B N1B C9B 111.6(3) . . ?
C5B N1B C13B 104.8(3) . . ?
C9B N1B C13B 111.2(3) . . ?
N1B C1B H1BA 108 . . ?
N1B C1B H1BB 108 . . ?
H1BA C1B H1BB 107.3 . . ?
C2B C1B N1B 117.1(4) . . ?
C2B C1B H1BA 108 . . ?
C2B C1B H1BB 108 . . ?
C1B C2B H2BA 109.4 . . ?
C1B C2B H2BB 109.4 . . ?
H2BA C2B H2BB 108 . . ?
C3B C2B C1B 111.1(5) . . ?
C3B C2B H2BA 109.4 . . ?
C3B C2B H2BB 109.4 . . ?
C2B C3B H3BA 108.7 . . ?
C2B C3B H3BB 108.7 . . ?
C2B C3B C4B 114.4(6) . . ?
H3BA C3B H3BB 107.6 . . ?
C4B C3B H3BA 108.7 . . ?
C4B C3B H3BB 108.7 . . ?
C3B C4B H4BA 109.5 . . ?
C3B C4B H4BB 109.5 . . ?
C3B C4B H4BC 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
N1B C5B H5BA 108 . . ?
N1B C5B H5BB 108 . . ?
N1B C5B C6B 117.3(3) . . ?
H5BA C5B H5BB 107.2 . . ?
C6B C5B H5BA 108 . . ?
C6B C5B H5BB 108 . . ?
C5B C6B H6BA 109.9 . . ?
C5B C6B H6BB 109.9 . . ?
H6BA C6B H6BB 108.3 . . ?
C7B C6B C5B 108.9(4) . . ?
C7B C6B H6BA 109.9 . . ?
C7B C6B H6BB 109.9 . . ?
C6B C7B H7BA 109 . . ?
C6B C7B H7BB 109 . . ?
C6B C7B C8B 113.0(5) . . ?
H7BA C7B H7BB 107.8 . . ?
C8B C7B H7BA 109 . . ?
C8B C7B H7BB 109 . . ?
C7B C8B H8BA 109.5 . . ?
C7B C8B H8BB 109.5 . . ?
C7B C8B H8BC 109.5 . . ?
H8BA C8B H8BB 109.5 . . ?
H8BA C8B H8BC 109.5 . . ?
H8BB C8B H8BC 109.5 . . ?
N1B C9B H9BA 108.3 . . ?
N1B C9B H9BB 108.3 . . ?
H9BA C9B H9BB 107.4 . . ?
C10B C9B N1B 115.8(3) . . ?
C10B C9B H9BA 108.3 . . ?
C10B C9B H9BB 108.3 . . ?
C9B C10B H10C 109.6 . . ?
C9B C10B H10D 109.6 . . ?
C9B C10B C11B 110.2(4) . . ?
H10C C10B H10D 108.1 . . ?
C11B C10B H10C 109.6 . . ?
C11B C10B H10D 109.6 . . ?
C10B C11B H11C 108.6 . . ?
C10B C11B H11D 108.6 . . ?
H11C C11B H11D 107.5 . . ?
C12B C11B C10B 114.8(5) . . ?
C12B C11B H11C 108.6 . . ?
C12B C11B H11D 108.6 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12E 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
N1B C13B H13C 108 . . ?
N1B C13B H13D 108 . . ?
H13C C13B H13D 107.3 . . ?
C14B C13B N1B 117.2(4) . . ?
C14B C13B H13C 108 . . ?
C14B C13B H13D 108 . . ?
C13B C14B H14C 110 . . ?
C13B C14B H14D 110 . . ?
C13B C14B C15B 108.6(4) . . ?
H14C C14B H14D 108.3 . . ?
C15B C14B H14C 110 . . ?
C15B C14B H14D 110 . . ?
C14B C15B H15C 109.4 . . ?
C14B C15B H15D 109.4 . . ?
H15C C15B H15D 108 . . ?
C16B C15B C14B 111.3(6) . . ?
C16B C15B H15C 109.4 . . ?
C16B C15B H15D 109.4 . . ?
C15B C16B H16D 109.5 . . ?
C15B C16B H16E 109.5 . . ?
C15B C16B H16F 109.5 . . ?
H16D C16B H16E 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 179.6(6) . . . . ?
N1 C1 C6 C5 179.7(5) . . . . ?
N2 C8 C9 C10 179.4(4) . . . . ?
N2 C8 C13 C12 -179.0(4) . . . . ?
N3 C17 C18 C19 -176.3(5) . . . . ?
N4 C21 C22 C23 177.5(5) . . . . ?
N4 C21 C26 C25 -178.3(4) . . . . ?
C1 N1 C7 O1 1.8(8) . . . . ?
C1 N1 C7 N2 -178.3(4) . . . . ?
C1 C2 C3 C4 0.0(11) . . . . ?
C2 C1 C6 C5 -0.3(8) . . . . ?
C2 C3 C4 C5 1.0(12) . . . . ?
C3 C4 C5 C6 -1.7(12) . . . . ?
C4 C5 C6 C1 1.4(11) . . . . ?
C6 C1 C2 C3 -0.4(9) . . . . ?
C7 N1 C1 C2 -175.5(5) . . . . ?
C7 N1 C1 C6 4.5(8) . . . . ?
C7 N2 C8 C9 13.2(6) . . . . ?
C7 N2 C8 C13 -168.6(4) . . . . ?
C8 N2 C7 O1 5.0(7) . . . . ?
C8 N2 C7 N1 -174.9(4) . . . . ?
C8 C9 C10 C11 -0.9(6) . . . . ?
C9 C8 C13 C12 -0.7(6) . . . . ?
C9 C10 C11 C12 0.1(6) . . . . ?
C9 C10 C11 C14 177.9(4) . . . . ?
C10 C11 C12 C13 0.4(6) . . . . ?
C10 C11 C14 C15 11.1(6) . . . . ?
C10 C11 C14 C19 -167.4(4) . . . . ?
C11 C12 C13 C8 -0.1(6) . . . . ?
C11 C14 C15 C16 -178.0(4) . . . . ?
C11 C14 C19 C18 178.1(4) . . . . ?
C12 C11 C14 C15 -171.2(4) . . . . ?
C12 C11 C14 C19 10.3(6) . . . . ?
C13 C8 C9 C10 1.2(6) . . . . ?
C14 C11 C12 C13 -177.4(4) . . . . ?
C14 C15 C16 C17 -0.3(8) . . . . ?
C15 C14 C19 C18 -0.5(7) . . . . ?
C15 C16 C17 N3 176.2(4) . . . . ?
C15 C16 C17 C18 -0.2(7) . . . . ?
C16 C17 C18 C19 0.3(7) . . . . ?
C17 N3 C20 O2 8.3(7) . . . . ?
C17 N3 C20 N4 -172.0(4) . . . . ?
C17 C18 C19 C14 0.1(8) . . . . ?
C19 C14 C15 C16 0.6(7) . . . . ?
C20 N3 C17 C16 11.0(7) . . . . ?
C20 N3 C17 C18 -172.6(4) . . . . ?
C20 N4 C21 C22 2.9(8) . . . . ?
C20 N4 C21 C26 -178.3(4) . . . . ?
C21 N4 C20 O2 0.9(8) . . . . ?
C21 N4 C20 N3 -178.8(4) . . . . ?
C21 C22 C23 C24 2.1(10) . . . . ?
C22 C21 C26 C25 0.6(7) . . . . ?
C22 C23 C24 C25 -2.3(11) . . . . ?
C23 C24 C25 C26 1.6(10) . . . . ?
C24 C25 C26 C21 -0.7(8) . . . . ?
C26 C21 C22 C23 -1.2(8) . . . . ?
N1A C1A C2A C3A -179.6(5) . . . . ?
N1A C5A C6A C7A 173.7(5) . . . . ?
N1A C9A C10A C11A -176.1(5) . . . . ?
N1A C13A C14A C15A 176.8(4) . . . . ?
C1A N1A C5A C6A -59.7(5) . . . . ?
C1A N1A C9A C10A -175.5(4) . . . . ?
C1A N1A C13A C14A 60.6(5) . . . . ?
C1A C2A C3A C4A 179.4(6) . . . . ?
C5A N1A C1A C2A -55.6(5) . . . . ?
C5A N1A C9A C10A 63.5(5) . . . . ?
C5A N1A C13A C14A -178.3(4) . . . . ?
C5A C6A C7A C8A -179.9(6) . . . . ?
C9A N1A C1A C2A -176.6(4) . . . . ?
C9A N1A C5A C6A 58.2(5) . . . . ?
C9A N1A C13A C14A -57.2(5) . . . . ?
C9A C10A C11A C12A -177.6(5) . . . . ?
C13A N1A C1A C2A 62.5(5) . . . . ?
C13A N1A C5A C6A 179.2(4) . . . . ?
C13A N1A C9A C10A -54.6(5) . . . . ?
C13A C14A C15A C16A -179.8(5) . . . . ?
N1B C1B C2B C3B 179.9(5) . . . . ?
N1B C5B C6B C7B -179.0(4) . . . . ?
N1B C9B C10B C11B 178.2(4) . . . . ?
N1B C13B C14B C15B -174.3(4) . . . . ?
C1B N1B C5B C6B 57.9(5) . . . . ?
C1B N1B C9B C10B 174.7(4) . . . . ?
C1B N1B C13B C14B -61.7(5) . . . . ?
C1B C2B C3B C4B 178.0(7) . . . . ?
C5B N1B C1B C2B 52.8(5) . . . . ?
C5B N1B C9B C10B -63.2(5) . . . . ?
C5B N1B C13B C14B 177.9(4) . . . . ?
C5B C6B C7B C8B -178.0(5) . . . . ?
C9B N1B C1B C2B 175.0(4) . . . . ?
C9B N1B C5B C6B -61.5(5) . . . . ?
C9B N1B C13B C14B 57.2(5) . . . . ?
C9B C10B C11B C12B 177.0(5) . . . . ?
C13B N1B C1B C2B -63.6(5) . . . . ?
C13B N1B C5B C6B 178.0(4) . . . . ?
C13B N1B C9B C10B 53.4(5) . . . . ?
C13B C14B C15B C16B -177.6(5) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
####################################################################### 
# 
# 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_1-((TBA)NO3)2
_database_code_depnum_ccdc_archive 'CCDC 2015339'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T17:08:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H22 N4 O2, 2(C16 H36 N), 2(N O3)'
_chemical_formula_sum            'C58 H94 N8 O8'
_chemical_formula_weight         1031.41

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   15.0086(13)
_cell_length_b                   9.8413(5)
_cell_length_c                   20.6682(16)
_cell_angle_alpha                90
_cell_angle_beta                 99.841(8)
_cell_angle_gamma                90
_cell_volume                     3007.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    2738
_cell_measurement_theta_min      4.4930
_cell_measurement_theta_max      27.0640

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.744
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.206
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             1124

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_T_max  0.979

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_number            15814
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.216
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             5886
_reflns_number_gt                3210
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1382P)²+0.6040P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5886
_refine_ls_number_parameters     338
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.2708
_refine_ls_wR_factor_gt          0.2218
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.042


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.66329(19) 0.7906(3) 0.04043(12) 0.1012(9) Uani 1 1 d . . . . .
N1 N 0.63620(19) 0.7749(3) 0.14591(13) 0.0760(8) Uani 1 1 d . . . . .
H1 H 0.654201 0.734365 0.182682 0.091 Uiso 1 1 calc R . . . .
N2 N 0.75434(18) 0.6607(3) 0.11617(12) 0.0690(7) Uani 1 1 d . . . . .
H2 H 0.759855 0.630619 0.155728 0.083 Uiso 1 1 calc R . . . .
C1 C 0.5617(2) 0.8640(3) 0.14344(17) 0.0678(8) Uani 1 1 d . . . . .
C2 C 0.5403(2) 0.9065(3) 0.20291(19) 0.0808(10) Uani 1 1 d . . . . .
H2A H 0.573582 0.874228 0.242006 0.097 Uiso 1 1 calc R . . . .
C3 C 0.4699(3) 0.9966(4) 0.2045(2) 0.0896(11) Uani 1 1 d . . . . .
H3 H 0.455757 1.024145 0.244611 0.108 Uiso 1 1 calc R . . . .
C4 C 0.4212(3) 1.0450(4) 0.1473(3) 0.0941(12) Uani 1 1 d . . . . .
H4 H 0.37485 1.107199 0.148435 0.113 Uiso 1 1 calc R . . . .
C5 C 0.4406(2) 1.0023(4) 0.0890(2) 0.0929(12) Uani 1 1 d . . . . .
H5 H 0.406927 1.035547 0.050226 0.111 Uiso 1 1 calc R . . . .
C6 C 0.5094(2) 0.9104(4) 0.08576(19) 0.0848(10) Uani 1 1 d . . . . .
H6 H 0.520579 0.879924 0.045301 0.102 Uiso 1 1 calc R . . . .
C7 C 0.6826(2) 0.7463(3) 0.09621(16) 0.0712(9) Uani 1 1 d . . . . .
C8 C 0.8197(2) 0.6164(3) 0.07981(14) 0.0588(7) Uani 1 1 d . . . . .
C9 C 0.8766(2) 0.5121(3) 0.10550(15) 0.0711(9) Uani 1 1 d . . . . .
H9 H 0.867818 0.47102 0.144441 0.085 Uiso 1 1 calc R . . . .
C10 C 0.9461(2) 0.4674(3) 0.07497(14) 0.0668(8) Uani 1 1 d . . . . .
H10 H 0.982961 0.397291 0.09422 0.08 Uiso 1 1 calc R . . . .
C11 C 0.9629(2) 0.5233(3) 0.01649(13) 0.0541(7) Uani 1 1 d . . . . .
C12 C 0.9032(2) 0.6256(3) -0.00954(15) 0.0688(8) Uani 1 1 d . . . . .
H12 H 0.910608 0.665032 -0.049169 0.083 Uiso 1 1 calc R . . . .
C13 C 0.8333(2) 0.6716(3) 0.02074(16) 0.0698(9) Uani 1 1 d . . . . .
H13 H 0.795291 0.740117 0.001187 0.084 Uiso 1 1 calc R . . . .
O2 O 0.7389(2) 0.7828(3) 0.28499(16) 0.1114(10) Uani 1 1 d . . . . .
O3 O 0.8406(3) 0.6710(3) 0.34763(15) 0.1361(13) Uani 1 1 d . . . . .
O4 O 0.7831(2) 0.5936(2) 0.25507(12) 0.1014(9) Uani 1 1 d . . . . .
N3 N 0.7882(2) 0.6829(3) 0.29700(15) 0.0735(8) Uani 1 1 d . . . . .
N4 N 0.78456(16) 0.2257(2) 0.34025(12) 0.0601(7) Uani 1 1 d . . . . .
C14 C 0.7251(2) 0.2722(3) 0.27750(16) 0.0701(9) Uani 1 1 d . . . . .
H14A H 0.663506 0.278679 0.285651 0.084 Uiso 1 1 calc R . . . .
H14B H 0.743928 0.363011 0.267493 0.084 Uiso 1 1 calc R . . . .
C15 C 0.7248(3) 0.1850(4) 0.21767(18) 0.0923(11) Uani 1 1 d . . . . .
H15A H 0.705889 0.093346 0.226148 0.111 Uiso 1 1 calc R . . . .
H15B H 0.785101 0.180737 0.206831 0.111 Uiso 1 1 calc R . . . .
C16 C 0.6594(3) 0.2470(6) 0.1607(2) 0.1299(18) Uani 1 1 d D . . . .
H16A H 0.598184 0.225866 0.166718 0.156 Uiso 1 1 calc R . . . .
H16B H 0.666037 0.345001 0.162928 0.156 Uiso 1 1 calc R . . . .
C17 C 0.6708(5) 0.2011(8) 0.0932(2) 0.178(3) Uani 1 1 d D . . . .
H17A H 0.619334 0.229216 0.061878 0.266 Uiso 1 1 calc GR . . . .
H17B H 0.675788 0.103901 0.092574 0.266 Uiso 1 1 calc GR . . . .
H17C H 0.724582 0.240989 0.082093 0.266 Uiso 1 1 calc GR . . . .
C18 C 0.7494(2) 0.0944(3) 0.36572(17) 0.0715(9) Uani 1 1 d D . . . .
H18A H 0.753257 0.023079 0.333947 0.086 Uiso 1 1 calc R . . . .
H18B H 0.788938 0.069387 0.406115 0.086 Uiso 1 1 calc R . . . .
C19 C 0.6535(2) 0.0996(4) 0.3789(2) 0.0933(12) Uani 1 1 d D . . . .
H19A H 0.612072 0.115 0.33811 0.112 Uiso 1 1 calc R . . . .
H19B H 0.647199 0.173981 0.408532 0.112 Uiso 1 1 calc R . . . .
C20 C 0.6309(3) -0.0344(5) 0.4094(3) 0.1207(16) Uani 1 1 d D . . . .
H20A H 0.641578 -0.108468 0.38065 0.145 Uiso 1 1 calc R . . . .
H20B H 0.671142 -0.046752 0.450941 0.145 Uiso 1 1 calc R . . . .
C21 C 0.5346(3) -0.0414(8) 0.4207(4) 0.186(3) Uani 1 1 d D . . . .
H21A H 0.494393 -0.038809 0.37931 0.279 Uiso 1 1 calc GR . . . .
H21B H 0.52247 0.03452 0.447064 0.279 Uiso 1 1 calc GR . . . .
H21C H 0.52553 -0.124451 0.443124 0.279 Uiso 1 1 calc GR . . . .
C22 C 0.8802(2) 0.1975(3) 0.32871(17) 0.0688(9) Uani 1 1 d . . . . .
H22A H 0.916471 0.168246 0.36973 0.083 Uiso 1 1 calc R . . . .
H22B H 0.878384 0.123382 0.297607 0.083 Uiso 1 1 calc R . . . .
C23 C 0.9255(2) 0.3182(4) 0.3030(2) 0.0852(10) Uani 1 1 d D . . . .
H23A H 0.889151 0.348571 0.26221 0.102 Uiso 1 1 calc R . . . .
H23B H 0.928717 0.392056 0.334408 0.102 Uiso 1 1 calc R . . . .
C24 C 1.0192(2) 0.2853(4) 0.2913(3) 0.1164(16) Uani 1 1 d D . . . .
H24A H 1.055206 0.25486 0.332174 0.14 Uiso 1 1 calc R . . . .
H24B H 1.015646 0.210946 0.260124 0.14 Uiso 1 1 calc R . . . .
C25 C 1.0659(3) 0.4034(4) 0.2655(2) 0.1068(14) Uani 1 1 d D . . . .
H25A H 1.041686 0.416727 0.21983 0.16 Uiso 1 1 calc GR . . . .
H25B H 1.12954 0.385027 0.270409 0.16 Uiso 1 1 calc GR . . . .
H25C H 1.056404 0.483843 0.289634 0.16 Uiso 1 1 calc GR . . . .
C26 C 0.7844(2) 0.3401(3) 0.38960(16) 0.0699(9) Uani 1 1 d D . . . .
H26A H 0.803981 0.422631 0.370503 0.084 Uiso 1 1 calc R . . . .
H26B H 0.722653 0.35441 0.396147 0.084 Uiso 1 1 calc R . . . .
C27 C 0.8429(3) 0.3197(4) 0.45610(17) 0.0866(11) Uani 1 1 d D . . . .
H27A H 0.820328 0.243716 0.478447 0.104 Uiso 1 1 calc R . . . .
H27B H 0.904474 0.29968 0.450774 0.104 Uiso 1 1 calc R . . . .
C28 C 0.8410(3) 0.4469(4) 0.4960(2) 0.1130(15) Uani 1 1 d D . . . .
H28A H 0.779348 0.463425 0.502409 0.136 Uiso 1 1 calc R . . . .
H28B H 0.859349 0.522966 0.471557 0.136 Uiso 1 1 calc R . . . .
C29 C 0.9012(5) 0.4411(7) 0.5621(3) 0.166(2) Uani 1 1 d D . . . .
H29A H 0.963251 0.437118 0.55627 0.249 Uiso 1 1 calc GR . . . .
H29B H 0.886937 0.361665 0.585283 0.249 Uiso 1 1 calc GR . . . .
H29C H 0.891854 0.520776 0.586866 0.249 Uiso 1 1 calc GR . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.220(4) . ?
N1 H1 0.86 . ?
N1 C1 1.416(4) . ?
N1 C7 1.365(4) . ?
N2 H2 0.86 . ?
N2 C7 1.374(4) . ?
N2 C8 1.403(4) . ?
C1 C2 1.387(5) . ?
C1 C6 1.387(5) . ?
C2 H2A 0.93 . ?
C2 C3 1.384(5) . ?
C3 H3 0.93 . ?
C3 C4 1.365(6) . ?
C4 H4 0.93 . ?
C4 C5 1.356(6) . ?
C5 H5 0.93 . ?
C5 C6 1.383(5) . ?
C6 H6 0.93 . ?
C8 C9 1.381(4) . ?
C8 C13 1.383(4) . ?
C9 H9 0.93 . ?
C9 C10 1.380(4) . ?
C10 H10 0.93 . ?
C10 C11 1.390(4) . ?
C11 C11 1.475(6) 3_765 ?
C11 C12 1.394(4) . ?
C12 H12 0.93 . ?
C12 C13 1.386(4) . ?
C13 H13 0.93 . ?
O2 N3 1.230(4) . ?
O3 N3 1.202(4) . ?
O4 N3 1.228(3) . ?
N4 C14 1.514(4) . ?
N4 C18 1.523(4) . ?
N4 C22 1.520(4) . ?
N4 C26 1.519(4) . ?
C14 H14A 0.97 . ?
C14 H14B 0.97 . ?
C14 C15 1.505(5) . ?
C15 H15A 0.97 . ?
C15 H15B 0.97 . ?
C15 C16 1.525(6) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C16 C17 1.504(3) . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
C18 C19 1.509(4) . ?
C19 H19A 0.97 . ?
C19 H19B 0.97 . ?
C19 C20 1.525(5) . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C20 C21 1.505(2) . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 C23 1.509(5) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C23 C24 1.5024(19) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 C25 1.502(3) . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C26 C27 1.512(4) . ?
C27 H27A 0.97 . ?
C27 H27B 0.97 . ?
C27 C28 1.502(5) . ?
C28 H28A 0.97 . ?
C28 H28B 0.97 . ?
C28 C29 1.504(5) . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?

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 H1 116.5 . . ?
C7 N1 H1 116.5 . . ?
C7 N1 C1 127.0(3) . . ?
C7 N2 H2 116.1 . . ?
C7 N2 C8 127.8(3) . . ?
C8 N2 H2 116.1 . . ?
C2 C1 N1 117.1(3) . . ?
C2 C1 C6 118.7(3) . . ?
C6 C1 N1 124.2(3) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 C1 120.5(4) . . ?
C3 C2 H2A 119.8 . . ?
C2 C3 H3 120 . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3 120 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.4(4) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 H6 120.3 . . ?
C5 C6 C1 119.4(4) . . ?
C5 C6 H6 120.3 . . ?
O1 C7 N1 124.6(3) . . ?
O1 C7 N2 123.4(3) . . ?
N1 C7 N2 112.0(3) . . ?
C9 C8 N2 117.9(3) . . ?
C9 C8 C13 117.1(3) . . ?
C13 C8 N2 125.0(3) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 C8 121.8(3) . . ?
C10 C9 H9 119.1 . . ?
C9 C10 H10 118.8 . . ?
C9 C10 C11 122.3(3) . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C11 122.9(3) . 3_765 ?
C10 C11 C12 114.9(3) . . ?
C12 C11 C11 122.2(3) . 3_765 ?
C11 C12 H12 118.4 . . ?
C13 C12 C11 123.2(3) . . ?
C13 C12 H12 118.4 . . ?
C8 C13 C12 120.5(3) . . ?
C8 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
O3 N3 O2 122.3(3) . . ?
O3 N3 O4 119.8(3) . . ?
O4 N3 O2 117.8(3) . . ?
C14 N4 C18 111.3(2) . . ?
C14 N4 C22 110.8(2) . . ?
C14 N4 C26 106.4(2) . . ?
C22 N4 C18 107.0(2) . . ?
C26 N4 C18 110.9(2) . . ?
C26 N4 C22 110.5(2) . . ?
N4 C14 H14A 108.1 . . ?
N4 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
C15 C14 N4 116.8(3) . . ?
C15 C14 H14A 108.1 . . ?
C15 C14 H14B 108.1 . . ?
C14 C15 H15A 110 . . ?
C14 C15 H15B 110 . . ?
C14 C15 C16 108.5(3) . . ?
H15A C15 H15B 108.4 . . ?
C16 C15 H15A 110 . . ?
C16 C15 H15B 110 . . ?
C15 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C17 C16 C15 115.8(5) . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 108.4 . . ?
N4 C18 H18B 108.4 . . ?
H18A C18 H18B 107.5 . . ?
C19 C18 N4 115.5(2) . . ?
C19 C18 H18A 108.4 . . ?
C19 C18 H18B 108.4 . . ?
C18 C19 H19A 109.8 . . ?
C18 C19 H19B 109.8 . . ?
C18 C19 C20 109.4(3) . . ?
H19A C19 H19B 108.2 . . ?
C20 C19 H19A 109.8 . . ?
C20 C19 H19B 109.8 . . ?
C19 C20 H20A 109 . . ?
C19 C20 H20B 109 . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 C19 113.1(4) . . ?
C21 C20 H20A 109 . . ?
C21 C20 H20B 109 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 108.8 . . ?
N4 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 N4 114.0(2) . . ?
C23 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
C22 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 C22 112.2(3) . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C23 C24 H24A 108.9 . . ?
C23 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 C23 113.4(3) . . ?
C25 C24 H24A 108.9 . . ?
C25 C24 H24B 108.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 H26A 108.2 . . ?
N4 C26 H26B 108.2 . . ?
H26A C26 H26B 107.3 . . ?
C27 C26 N4 116.4(2) . . ?
C27 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
C26 C27 H27A 109.9 . . ?
C26 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C28 C27 C26 109.1(3) . . ?
C28 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
C27 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C27 C28 C29 113.7(4) . . ?
H28A C28 H28B 107.7 . . ?
C29 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 178.2(3) . . . . ?
N1 C1 C6 C5 -177.0(3) . . . . ?
N2 C8 C9 C10 -176.2(3) . . . . ?
N2 C8 C13 C12 176.3(3) . . . . ?
C1 N1 C7 O1 -3.3(6) . . . . ?
C1 N1 C7 N2 176.9(3) . . . . ?
C1 C2 C3 C4 -0.4(5) . . . . ?
C2 C1 C6 C5 3.1(5) . . . . ?
C2 C3 C4 C5 1.5(6) . . . . ?
C3 C4 C5 C6 -0.3(6) . . . . ?
C4 C5 C6 C1 -2.1(6) . . . . ?
C6 C1 C2 C3 -1.9(5) . . . . ?
C7 N1 C1 C2 -163.0(3) . . . . ?
C7 N1 C1 C6 17.2(5) . . . . ?
C7 N2 C8 C9 -169.0(3) . . . . ?
C7 N2 C8 C13 12.9(5) . . . . ?
C8 N2 C7 O1 4.3(5) . . . . ?
C8 N2 C7 N1 -175.9(3) . . . . ?
C8 C9 C10 C11 -0.4(5) . . . . ?
C9 C8 C13 C12 -1.9(5) . . . . ?
C9 C10 C11 C11 179.7(3) . . . 3_765 ?
C9 C10 C11 C12 -1.3(4) . . . . ?
C10 C11 C12 C13 1.4(5) . . . . ?
C11 C11 C12 C13 -179.6(3) 3_765 . . . ?
C11 C12 C13 C8 0.1(5) . . . . ?
C13 C8 C9 C10 2.0(5) . . . . ?
N4 C14 C15 C16 178.6(3) . . . . ?
N4 C18 C19 C20 -175.3(3) . . . . ?
N4 C22 C23 C24 -179.1(4) . . . . ?
N4 C26 C27 C28 175.0(3) . . . . ?
C14 N4 C18 C19 -57.4(4) . . . . ?
C14 N4 C22 C23 58.4(4) . . . . ?
C14 N4 C26 C27 -177.6(3) . . . . ?
C14 C15 C16 C17 161.7(5) . . . . ?
C18 N4 C14 C15 -67.6(4) . . . . ?
C18 N4 C22 C23 179.9(3) . . . . ?
C18 N4 C26 C27 61.2(4) . . . . ?
C18 C19 C20 C21 -176.8(4) . . . . ?
C22 N4 C14 C15 51.3(4) . . . . ?
C22 N4 C18 C19 -178.5(3) . . . . ?
C22 N4 C26 C27 -57.3(4) . . . . ?
C22 C23 C24 C25 179.8(4) . . . . ?
C26 N4 C14 C15 171.4(3) . . . . ?
C26 N4 C18 C19 60.9(4) . . . . ?
C26 N4 C22 C23 -59.3(4) . . . . ?
C26 C27 C28 C29 -176.7(4) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
####################################################################### 
# 
# 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_2-((TBA)AcO)2
_database_code_depnum_ccdc_archive 'CCDC 2015341'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-20T09:19:56-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H20 N6 O6, 2(C2 H3 O2), 2(C16 H36 N)'
_chemical_formula_sum            'C62 H98 N8 O10'
_chemical_formula_weight         1115.48

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   12.1290(3)
_cell_length_b                   14.2416(3)
_cell_length_c                   38.0026(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.258(2)
_cell_angle_gamma                90
_cell_volume                     6564.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    4374
_cell_measurement_theta_min      3.2070
_cell_measurement_theta_max      72.7370

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.488
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.105
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             2424

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.07208
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_number            15369
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         4.789
_diffrn_reflns_theta_max         67.992
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             5956
_reflns_number_gt                3994
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5956
_refine_ls_number_parameters     366
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0893
_refine_ls_wR_factor_ref         0.3548
_refine_ls_wR_factor_gt          0.3183
_refine_ls_goodness_of_fit_ref   1.309
_refine_ls_restrained_S_all      1.312
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.040


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'

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 0.7626(2) 0.7114(2) 0.62746(6) 0.1245(9) Uani 1 1 d . . . . .
O3 O 1.1583(3) 0.6992(6) 0.47763(10) 0.285(4) Uani 1 1 d . . . . .
N1 N 0.9273(2) 0.7876(2) 0.62113(7) 0.1090(8) Uani 1 1 d . . . . .
H1 H 0.971838 0.826056 0.631312 0.131 Uiso 1 1 calc R . . . .
N2 N 0.8192(2) 0.81882(19) 0.66831(6) 0.1023(7) Uani 1 1 d . . . . .
H2 H 0.872589 0.855696 0.673969 0.123 Uiso 1 1 calc R . . . .
N3 N 1.0842(3) 0.6554(6) 0.49106(11) 0.194(3) Uani 1 1 d . . . . .
C1 C 0.9601(2) 0.7515(3) 0.58872(8) 0.1090(10) Uani 1 1 d . . . . .
C2 C 0.9143(3) 0.6756(4) 0.57224(10) 0.1269(13) Uani 1 1 d . . . . .
H2A H 0.854674 0.645454 0.582611 0.152 Uiso 1 1 calc R . . . .
C3 C 0.9544(3) 0.6422(4) 0.54038(10) 0.1439(17) Uani 1 1 d . . . . .
H3 H 0.923616 0.589174 0.52997 0.173 Uiso 1 1 calc R . . . .
C4 C 1.0396(3) 0.6884(5) 0.52460(10) 0.1443(18) Uani 1 1 d . . . . .
C5 C 1.0867(3) 0.7661(5) 0.54005(12) 0.149(2) Uani 1 1 d . . . . .
H5 H 1.143467 0.797666 0.52873 0.179 Uiso 1 1 calc R . . . .
C6 C 1.0495(3) 0.7975(4) 0.57261(10) 0.1276(13) Uani 1 1 d . . . . .
H6 H 1.08327 0.848323 0.583595 0.153 Uiso 1 1 calc R . . . .
C7 C 0.8303(3) 0.7677(3) 0.63850(8) 0.1020(8) Uani 1 1 d . . . . .
C8 C 0.7271(3) 0.8164(2) 0.69082(7) 0.0944(7) Uani 1 1 d . . . . .
C9 C 0.6606(3) 0.7383(2) 0.69490(7) 0.0934(7) Uani 1 1 d . . . . .
H9 H 0.674913 0.684291 0.681922 0.112 Uiso 1 1 calc R . . . .
C10 C 0.5726(2) 0.73955(19) 0.71819(7) 0.0897(7) Uani 1 1 d . . . . .
H10 H 0.529758 0.685861 0.720811 0.108 Uiso 1 1 calc R . . . .
C11 C 0.5473(2) 0.8187(2) 0.73752(7) 0.0898(7) Uani 1 1 d . . . . .
C12 C 0.6143(3) 0.8967(2) 0.73344(8) 0.1041(9) Uani 1 1 d . . . . .
H12 H 0.599349 0.950998 0.746163 0.125 Uiso 1 1 calc R . . . .
C13 C 0.7036(3) 0.8951(2) 0.71059(8) 0.1047(9) Uani 1 1 d . . . . .
H13 H 0.74825 0.947888 0.708621 0.126 Uiso 1 1 calc R . . . .
O4 O 1.0963(4) 0.8943(4) 0.64502(11) 0.1928(19) Uani 1 1 d . . . . .
O5 O 0.9842(3) 0.9511(2) 0.68453(10) 0.1552(11) Uani 1 1 d . . . . .
C14 C 1.1748(6) 0.9703(5) 0.6948(2) 0.217(4) Uani 1 1 d . . . . .
H14A H 1.203103 1.027923 0.685291 0.326 Uiso 1 1 calc GR . . . .
H14B H 1.232268 0.923973 0.695209 0.326 Uiso 1 1 calc GR . . . .
H14C H 1.149051 0.981029 0.718308 0.326 Uiso 1 1 calc GR . . . .
C15 C 1.0790(4) 0.9353(3) 0.67175(15) 0.1343(14) Uani 1 1 d . . . . .
N4 N 0.3636(2) 0.67427(19) 0.62091(9) 0.1090(8) Uani 1 1 d . . . . .
C16 C 0.3537(3) 0.7788(2) 0.61322(9) 0.1033(9) Uani 1 1 d . . . . .
H16A H 0.373014 0.789174 0.588794 0.124 Uiso 1 1 calc R . . . .
H16B H 0.277069 0.796854 0.615981 0.124 Uiso 1 1 calc R . . . .
C17 C 0.4231(3) 0.8424(2) 0.63565(11) 0.1153(10) Uani 1 1 d . . . . .
H17A H 0.500105 0.825125 0.633415 0.138 Uiso 1 1 calc R . . . .
H17B H 0.402405 0.835356 0.660134 0.138 Uiso 1 1 calc R . . . .
C18 C 0.4076(4) 0.9436(3) 0.62446(11) 0.1244(11) Uani 1 1 d . . . . .
H18A H 0.329672 0.958972 0.62486 0.149 Uiso 1 1 calc R . . . .
H18B H 0.433399 0.951269 0.600512 0.149 Uiso 1 1 calc R . . . .
C19 C 0.4704(4) 1.0115(3) 0.64867(14) 0.1534(17) Uani 1 1 d . . . . .
H19A H 0.461342 1.074566 0.640246 0.23 Uiso 1 1 calc GR . . . .
H19B H 0.547336 0.995508 0.648775 0.23 Uiso 1 1 calc GR . . . .
H19C H 0.441965 1.006809 0.672135 0.23 Uiso 1 1 calc GR . . . .
C20 C 0.4795(3) 0.6392(3) 0.61279(15) 0.1372(15) Uani 1 1 d . . . . .
H20A H 0.531537 0.674759 0.626937 0.165 Uiso 1 1 calc R . . . .
H20B H 0.484748 0.574053 0.620098 0.165 Uiso 1 1 calc R . . . .
C21 C 0.5140(4) 0.6456(5) 0.57509(17) 0.175(2) Uani 1 1 d . . . . .
H21A H 0.529599 0.710599 0.56929 0.21 Uiso 1 1 calc R . . . .
H21B H 0.454007 0.624509 0.560083 0.21 Uiso 1 1 calc R . . . .
C22 C 0.6147(5) 0.5868(6) 0.5682(2) 0.227(4) Uani 1 1 d D . . . .
H22A H 0.601065 0.523054 0.576073 0.272 Uiso 1 1 calc R . . . .
H22B H 0.676106 0.611442 0.581779 0.272 Uiso 1 1 calc R . . . .
C23 C 0.6459(7) 0.5850(8) 0.5295(2) 0.322(8) Uani 1 1 d D . . . .
H23A H 0.581108 0.594325 0.515333 0.483 Uiso 1 1 calc GR . . . .
H23B H 0.678402 0.525429 0.52389 0.483 Uiso 1 1 calc GR . . . .
H23C H 0.697972 0.634209 0.524836 0.483 Uiso 1 1 calc GR . . . .
C24 C 0.2804(3) 0.6248(3) 0.59733(11) 0.1158(10) Uani 1 1 d . . . . .
H24A H 0.20739 0.646882 0.603499 0.139 Uiso 1 1 calc R . . . .
H24B H 0.29411 0.643797 0.573234 0.139 Uiso 1 1 calc R . . . .
C25 C 0.2798(3) 0.5198(3) 0.59863(16) 0.1481(17) Uani 1 1 d . . . . .
H25A H 0.252415 0.498095 0.621161 0.178 Uiso 1 1 calc R . . . .
H25B H 0.353653 0.495335 0.595339 0.178 Uiso 1 1 calc R . . . .
C26 C 0.2025(4) 0.4865(3) 0.56835(19) 0.168(2) Uani 1 1 d D . . . .
H26A H 0.12763 0.505608 0.573602 0.202 Uiso 1 1 calc R . . . .
H26B H 0.224219 0.517479 0.546722 0.202 Uiso 1 1 calc R . . . .
C27 C 0.2049(6) 0.3830(3) 0.5628(2) 0.217(4) Uani 1 1 d D . . . .
H27A H 0.152121 0.366253 0.544974 0.326 Uiso 1 1 calc GR . . . .
H27B H 0.186682 0.351784 0.584401 0.326 Uiso 1 1 calc GR . . . .
H27C H 0.27724 0.364334 0.555476 0.326 Uiso 1 1 calc GR . . . .
C28 C 0.3448(3) 0.6537(2) 0.65939(11) 0.1187(11) Uani 1 1 d . . . . .
H28A H 0.356881 0.587193 0.663412 0.142 Uiso 1 1 calc R . . . .
H28B H 0.39922 0.687754 0.673131 0.142 Uiso 1 1 calc R . . . .
C29 C 0.2320(3) 0.6790(3) 0.67259(11) 0.1277(12) Uani 1 1 d . . . . .
H29A H 0.178111 0.634385 0.663775 0.153 Uiso 1 1 calc R . . . .
H29B H 0.211663 0.741046 0.664303 0.153 Uiso 1 1 calc R . . . .
C30 C 0.2336(4) 0.6773(3) 0.71227(14) 0.1490(16) Uani 1 1 d D . . . .
H30A H 0.28186 0.726584 0.720921 0.179 Uiso 1 1 calc R . . . .
H30B H 0.262596 0.617595 0.720342 0.179 Uiso 1 1 calc R . . . .
C31 C 0.1189(6) 0.6915(5) 0.72696(18) 0.196(3) Uani 1 1 d D . . . .
H31A H 0.066883 0.655932 0.713301 0.294 Uiso 1 1 calc GR . . . .
H31B H 0.100048 0.756909 0.725906 0.294 Uiso 1 1 calc GR . . . .
H31C H 0.117194 0.670654 0.750969 0.294 Uiso 1 1 calc GR . . . .
O2 O 1.0433(5) 0.5882(6) 0.47766(12) 0.253(4) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.221(4) . ?
O3 N3 1.208(8) . ?
N1 H1 0.86 . ?
N1 C1 1.395(5) . ?
N1 C7 1.381(4) . ?
N2 H2 0.86 . ?
N2 C7 1.354(4) . ?
N2 C8 1.411(4) . ?
N3 C4 1.465(6) . ?
N3 O2 1.191(9) . ?
C1 C2 1.367(6) . ?
C1 C6 1.408(5) . ?
C2 H2A 0.93 . ?
C2 C3 1.391(5) . ?
C3 H3 0.93 . ?
C3 C4 1.366(7) . ?
C4 C5 1.375(8) . ?
C5 H5 0.93 . ?
C5 C6 1.393(6) . ?
C6 H6 0.93 . ?
C8 C9 1.384(4) . ?
C8 C13 1.379(4) . ?
C9 H9 0.93 . ?
C9 C10 1.390(4) . ?
C10 H10 0.93 . ?
C10 C11 1.381(4) . ?
C11 C11 1.491(5) 2_656 ?
C11 C12 1.386(4) . ?
C12 H12 0.93 . ?
C12 C13 1.392(4) . ?
C13 H13 0.93 . ?
O4 C15 1.192(6) . ?
O5 C15 1.270(6) . ?
C14 H14A 0.96 . ?
C14 H14B 0.96 . ?
C14 H14C 0.96 . ?
C14 C15 1.536(7) . ?
N4 C16 1.521(4) . ?
N4 C20 1.525(5) . ?
N4 C24 1.519(4) . ?
N4 C28 1.510(5) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C16 C17 1.500(5) . ?
C17 H17A 0.97 . ?
C17 H17B 0.97 . ?
C17 C18 1.514(5) . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
C18 C19 1.535(6) . ?
C19 H19A 0.96 . ?
C19 H19B 0.96 . ?
C19 H19C 0.96 . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C20 C21 1.497(8) . ?
C21 H21A 0.97 . ?
C21 H21B 0.97 . ?
C21 C22 1.506(8) . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 C23 1.520(8) . ?
C23 H23A 0.96 . ?
C23 H23B 0.96 . ?
C23 H23C 0.96 . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 C25 1.496(6) . ?
C25 H25A 0.97 . ?
C25 H25B 0.97 . ?
C25 C26 1.554(7) . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C26 C27 1.489(4) . ?
C27 H27A 0.96 . ?
C27 H27B 0.96 . ?
C27 H27C 0.96 . ?
C28 H28A 0.97 . ?
C28 H28B 0.97 . ?
C28 C29 1.503(6) . ?
C29 H29A 0.97 . ?
C29 H29B 0.97 . ?
C29 C30 1.508(6) . ?
C30 H30A 0.97 . ?
C30 H30B 0.97 . ?
C30 C31 1.514(6) . ?
C31 H31A 0.96 . ?
C31 H31B 0.96 . ?
C31 H31C 0.96 . ?

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 H1 116.8 . . ?
C7 N1 H1 116.8 . . ?
C7 N1 C1 126.4(3) . . ?
C7 N2 H2 117.4 . . ?
C7 N2 C8 125.2(3) . . ?
C8 N2 H2 117.4 . . ?
O3 N3 C4 118.7(7) . . ?
O2 N3 O3 122.9(6) . . ?
O2 N3 C4 118.3(6) . . ?
N1 C1 C6 115.9(4) . . ?
C2 C1 N1 125.4(3) . . ?
C2 C1 C6 118.8(4) . . ?
C1 C2 H2A 119.1 . . ?
C1 C2 C3 121.8(4) . . ?
C3 C2 H2A 119.1 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(5) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 N3 120.8(6) . . ?
C3 C4 C5 120.9(4) . . ?
C5 C4 N3 118.3(5) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.1(4) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 120.3 . . ?
C5 C6 C1 119.3(5) . . ?
C5 C6 H6 120.3 . . ?
O1 C7 N1 122.9(3) . . ?
O1 C7 N2 124.9(3) . . ?
N2 C7 N1 112.2(3) . . ?
C9 C8 N2 123.5(3) . . ?
C13 C8 N2 118.5(3) . . ?
C13 C8 C9 118.1(3) . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.7(3) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.5(2) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C11 120.80(19) . 2_656 ?
C10 C11 C12 117.6(3) . . ?
C12 C11 C11 121.60(18) . 2_656 ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 121.0(3) . . ?
C13 C12 H12 119.5 . . ?
C8 C13 C12 121.1(3) . . ?
C8 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
O4 C15 O5 125.2(5) . . ?
O4 C15 C14 120.7(6) . . ?
O5 C15 C14 114.1(6) . . ?
C16 N4 C20 110.7(3) . . ?
C24 N4 C16 106.8(3) . . ?
C24 N4 C20 109.8(3) . . ?
C28 N4 C16 111.3(3) . . ?
C28 N4 C20 106.0(3) . . ?
C28 N4 C24 112.2(3) . . ?
N4 C16 H16A 108.3 . . ?
N4 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C17 C16 N4 116.0(3) . . ?
C17 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C16 C17 H17A 109.6 . . ?
C16 C17 H17B 109.6 . . ?
C16 C17 C18 110.3(3) . . ?
H17A C17 H17B 108.1 . . ?
C18 C17 H17A 109.6 . . ?
C18 C17 H17B 109.6 . . ?
C17 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C17 C18 C19 111.7(4) . . ?
H18A C18 H18B 107.9 . . ?
C19 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 H20A 108.3 . . ?
N4 C20 H20B 108.3 . . ?
H20A C20 H20B 107.4 . . ?
C21 C20 N4 115.8(4) . . ?
C21 C20 H20A 108.3 . . ?
C21 C20 H20B 108.3 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C20 C21 C22 111.3(6) . . ?
H21A C21 H21B 108 . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C21 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
C21 C22 C23 112.5(7) . . ?
H22A C22 H22B 107.8 . . ?
C23 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 H24A 108.1 . . ?
N4 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
C25 C24 N4 116.6(3) . . ?
C25 C24 H24A 108.1 . . ?
C25 C24 H24B 108.1 . . ?
C24 C25 H25A 110.4 . . ?
C24 C25 H25B 110.4 . . ?
C24 C25 C26 106.5(4) . . ?
H25A C25 H25B 108.6 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
C25 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 C25 113.2(5) . . ?
C27 C26 H26A 108.9 . . ?
C27 C26 H26B 108.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 H28A 108.6 . . ?
N4 C28 H28B 108.6 . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 N4 114.7(3) . . ?
C29 C28 H28A 108.6 . . ?
C29 C28 H28B 108.6 . . ?
C28 C29 H29A 109.9 . . ?
C28 C29 H29B 109.9 . . ?
C28 C29 C30 108.8(4) . . ?
H29A C29 H29B 108.3 . . ?
C30 C29 H29A 109.9 . . ?
C30 C29 H29B 109.9 . . ?
C29 C30 H30A 109.4 . . ?
C29 C30 H30B 109.4 . . ?
C29 C30 C31 111.0(5) . . ?
H30A C30 H30B 108 . . ?
C31 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 N3 C4 C3 178.7(6) . . . . ?
O3 N3 C4 C5 -2.3(8) . . . . ?
N1 C1 C2 C3 -177.9(4) . . . . ?
N1 C1 C6 C5 -179.5(3) . . . . ?
N2 C8 C9 C10 178.4(3) . . . . ?
N2 C8 C13 C12 -179.6(3) . . . . ?
N3 C4 C5 C6 -177.5(4) . . . . ?
C1 N1 C7 O1 3.1(6) . . . . ?
C1 N1 C7 N2 -175.8(3) . . . . ?
C1 C2 C3 C4 -2.1(7) . . . . ?
C2 C1 C6 C5 1.7(6) . . . . ?
C2 C3 C4 N3 180.0(4) . . . . ?
C2 C3 C4 C5 0.9(7) . . . . ?
C3 C4 C5 C6 1.5(8) . . . . ?
C4 C5 C6 C1 -2.8(7) . . . . ?
C6 C1 C2 C3 0.8(6) . . . . ?
C7 N1 C1 C2 -15.1(6) . . . . ?
C7 N1 C1 C6 166.1(3) . . . . ?
C7 N2 C8 C9 29.0(5) . . . . ?
C7 N2 C8 C13 -152.9(3) . . . . ?
C8 N2 C7 O1 -1.3(6) . . . . ?
C8 N2 C7 N1 177.5(3) . . . . ?
C8 C9 C10 C11 1.1(5) . . . . ?
C9 C8 C13 C12 -1.4(5) . . . . ?
C9 C10 C11 C11 -179.8(3) . . . 2_656 ?
C9 C10 C11 C12 -1.3(5) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C11 C11 C12 C13 178.6(3) 2_656 . . . ?
C11 C12 C13 C8 1.2(6) . . . . ?
C13 C8 C9 C10 0.2(5) . . . . ?
N4 C16 C17 C18 178.4(3) . . . . ?
N4 C20 C21 C22 -164.7(4) . . . . ?
N4 C24 C25 C26 -171.1(4) . . . . ?
N4 C28 C29 C30 -166.3(3) . . . . ?
C16 N4 C20 C21 -63.5(5) . . . . ?
C16 N4 C24 C25 176.4(4) . . . . ?
C16 N4 C28 C29 62.2(4) . . . . ?
C16 C17 C18 C19 175.6(4) . . . . ?
C20 N4 C16 C17 -64.8(4) . . . . ?
C20 N4 C24 C25 56.2(5) . . . . ?
C20 N4 C28 C29 -177.3(3) . . . . ?
C20 C21 C22 C23 175.0(6) . . . . ?
C24 N4 C16 C17 175.7(3) . . . . ?
C24 N4 C20 C21 54.2(5) . . . . ?
C24 N4 C28 C29 -57.4(4) . . . . ?
C24 C25 C26 C27 172.0(6) . . . . ?
C28 N4 C16 C17 52.9(4) . . . . ?
C28 N4 C20 C21 175.6(4) . . . . ?
C28 N4 C24 C25 -61.4(4) . . . . ?
C28 C29 C30 C31 -173.6(4) . . . . ?
O2 N3 C4 C3 1.1(9) . . . . ?
O2 N3 C4 C5 -179.9(6) . . . . ?


_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.042 0.250 7.1 4.4 ?
2 0.000 0.042 0.750 7.1 4.4 ?
3 0.500 0.458 0.250 7.1 4.4 ?
4 0.500 0.542 0.750 7.1 4.4 ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2015340'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T18:07:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H20 N6 O6'
_chemical_formula_sum            'C26 H20 N6 O6'
_chemical_formula_weight         512.48

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   25.2125(6)
_cell_length_b                   8.18205(12)
_cell_length_c                   47.2764(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.9897(17)
_cell_angle_gamma                90
_cell_volume                     9746.8(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    6865
_cell_measurement_theta_min      3.7270
_cell_measurement_theta_max      75.7320

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.199
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_F_000             3192

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.90179
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_number            17506
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         3.508
_diffrn_reflns_theta_max         67.991
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.968
_reflns_Friedel_coverage         0
_reflns_number_total             8582
_reflns_number_gt                7302
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0844P)²+19.3521P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8582
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0839
_refine_ls_wR_factor_ref         0.2327
_refine_ls_wR_factor_gt          0.2263
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.043


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'

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 0.52794(12) 0.7911(3) 0.53482(5) 0.0878(8) Uani 1 1 d . . . . .
O2A O 0.63994(11) 0.6782(3) 0.78164(6) 0.0872(8) Uani 1 1 d . . . . .
O3A O 0.4855(2) 0.8505(5) 0.38981(9) 0.1559(18) Uani 1 1 d . . . . .
O4A O 0.5394(2) 0.6667(7) 0.37748(9) 0.171(2) Uani 1 1 d . . . . .
O5A O 0.6372(2) 0.8366(6) 0.93818(8) 0.1515(16) Uani 1 1 d . . . . .
O6A O 0.68773(18) 0.6450(5) 0.92693(8) 0.1363(14) Uani 1 1 d . . . . .
N1A N 0.56296(11) 0.5844(4) 0.50856(6) 0.0707(7) Uani 1 1 d . . . . .
H1A H 0.580342 0.494325 0.510284 0.085 Uiso 1 1 calc R U . . .
N2A N 0.56877(12) 0.5724(4) 0.55637(6) 0.0720(7) Uani 1 1 d . . . . .
H2A H 0.581821 0.477929 0.552694 0.086 Uiso 1 1 calc R U . . .
N3A N 0.59404(11) 0.8847(3) 0.75937(6) 0.0710(7) Uani 1 1 d . . . . .
H3A H 0.58151 0.980807 0.762259 0.085 Uiso 1 1 calc R U . . .
N4A N 0.60616(11) 0.8913(3) 0.80691(6) 0.0687(7) Uani 1 1 d . . . . .
H4A H 0.589549 0.982508 0.804753 0.082 Uiso 1 1 calc R U . . .
N5A N 0.5175(2) 0.7451(6) 0.39553(9) 0.1127(14) Uani 1 1 d . . . . .
N6A N 0.65805(18) 0.7540(5) 0.92048(9) 0.0994(11) Uani 1 1 d . . . . .
C1A C 0.55067(12) 0.6337(4) 0.48092(7) 0.0654(8) Uani 1 1 d . . . . .
C2A C 0.52066(16) 0.7702(5) 0.47365(9) 0.0811(10) Uani 1 1 d . . . . .
H2AA H 0.50791 0.837315 0.48776 0.097 Uiso 1 1 calc R U . . .
C3A C 0.50965(18) 0.8067(5) 0.44573(9) 0.0880(11) Uani 1 1 d . . . . .
H3AA H 0.488977 0.897241 0.44087 0.106 Uiso 1 1 calc R U . . .
C4A C 0.52943(17) 0.7084(5) 0.42502(9) 0.0836(11) Uani 1 1 d . . . . .
C5A C 0.55951(16) 0.5733(6) 0.43172(8) 0.0872(11) Uani 1 1 d . . . . .
H5A H 0.57269 0.507906 0.417491 0.105 Uiso 1 1 calc R U . . .
C6A C 0.56993(15) 0.5358(5) 0.45965(8) 0.0778(10) Uani 1 1 d . . . . .
H6A H 0.590078 0.443891 0.464346 0.093 Uiso 1 1 calc R U . . .
C7A C 0.55099(13) 0.6608(4) 0.53354(7) 0.0666(8) Uani 1 1 d . . . . .
C8A C 0.56858(13) 0.6152(4) 0.58501(7) 0.0657(8) Uani 1 1 d . . . . .
C9A C 0.59988(15) 0.5248(4) 0.60364(7) 0.0764(10) Uani 1 1 d . . . . .
H9A H 0.619498 0.43817 0.596748 0.092 Uiso 1 1 calc R U . . .
C10A C 0.60299(15) 0.5589(4) 0.63208(7) 0.0735(9) Uani 1 1 d . . . . .
H10A H 0.624617 0.495168 0.64399 0.088 Uiso 1 1 calc R U . . .
C11A C 0.57418(12) 0.6879(4) 0.64347(7) 0.0594(7) Uani 1 1 d . . . . .
C12A C 0.54188(15) 0.7743(5) 0.62453(8) 0.0783(10) Uani 1 1 d . . . . .
H12A H 0.521332 0.858809 0.631423 0.094 Uiso 1 1 calc R U . . .
C13A C 0.53869(16) 0.7410(5) 0.59590(8) 0.0826(11) Uani 1 1 d . . . . .
H13A H 0.516546 0.802861 0.583953 0.099 Uiso 1 1 calc R U . . .
C14A C 0.57880(11) 0.7310(4) 0.67381(7) 0.0577(7) Uani 1 1 d . . . . .
C15A C 0.62093(14) 0.6773(5) 0.69152(8) 0.0734(9) Uani 1 1 d . . . . .
H15A H 0.646172 0.608466 0.683979 0.088 Uiso 1 1 calc R U . . .
C16A C 0.62673(14) 0.7212(5) 0.71944(8) 0.0763(10) Uani 1 1 d . . . . .
H16A H 0.655098 0.680868 0.730435 0.092 Uiso 1 1 calc R U . . .
C17A C 0.59006(12) 0.8266(4) 0.73139(7) 0.0617(7) Uani 1 1 d . . . . .
C18A C 0.54842(14) 0.8801(5) 0.71433(8) 0.0755(10) Uani 1 1 d . . . . .
H18A H 0.523421 0.949761 0.721859 0.091 Uiso 1 1 calc R U . . .
C19A C 0.54257(14) 0.8334(5) 0.68636(7) 0.0722(9) Uani 1 1 d . . . . .
H19A H 0.513566 0.871676 0.67562 0.087 Uiso 1 1 calc R U . . .
C20A C 0.61539(13) 0.8063(4) 0.78230(8) 0.0664(8) Uani 1 1 d . . . . .
C21A C 0.62010(12) 0.8493(4) 0.83471(7) 0.0629(8) Uani 1 1 d . . . . .
C22A C 0.64895(15) 0.7100(4) 0.84252(8) 0.0773(10) Uani 1 1 d . . . . .
H22A H 0.660431 0.638597 0.828706 0.093 Uiso 1 1 calc R U . . .
C23A C 0.66041(16) 0.6783(5) 0.87064(9) 0.0816(10) Uani 1 1 d . . . . .
H23A H 0.679163 0.584601 0.875887 0.098 Uiso 1 1 calc R U . . .
C24A C 0.64414(15) 0.7850(5) 0.89085(8) 0.0745(9) Uani 1 1 d . . . . .
C25A C 0.61583(16) 0.9231(5) 0.88376(8) 0.0830(10) Uani 1 1 d . . . . .
H25A H 0.604778 0.994012 0.897764 0.1 Uiso 1 1 calc R U . . .
C26A C 0.60403(15) 0.9555(5) 0.85580(8) 0.0770(9) Uani 1 1 d . . . . .
H26A H 0.585077 1.049327 0.850853 0.092 Uiso 1 1 calc R U . . .
O1B O 0.70351(12) 1.2800(3) 0.87566(5) 0.0852(8) Uani 1 1 d . . . . .
O2B O 0.65682(15) 1.3064(5) 0.73124(7) 0.1181(11) Uani 1 1 d . . . . .
O3B O 0.70434(17) 1.1019(5) 0.72006(7) 0.1322(14) Uani 1 1 d . . . . .
N1B N 0.73999(11) 1.0683(3) 0.85131(5) 0.0653(7) Uani 1 1 d . . . . .
H1B H 0.75815 0.980059 0.8537 0.078 Uiso 1 1 calc R U . . .
N2B N 0.74769(11) 1.0741(3) 0.89930(5) 0.0691(7) Uani 1 1 d . . . . .
H2B H 0.762058 0.980112 0.896789 0.083 Uiso 1 1 calc R U . . .
N3B N 0.68580(15) 1.1928(5) 0.73744(7) 0.0882(9) Uani 1 1 d . . . . .
C1B C 0.72601(12) 1.1086(4) 0.82352(7) 0.0598(7) Uani 1 1 d . . . . .
C2B C 0.73894(13) 0.9965(4) 0.80269(7) 0.0694(8) Uani 1 1 d . . . . .
H2BA H 0.756319 0.900232 0.807891 0.083 Uiso 1 1 calc R U . . .
C3B C 0.72657(14) 1.0251(5) 0.77476(7) 0.0747(9) Uani 1 1 d . . . . .
H3B H 0.735747 0.949712 0.761042 0.09 Uiso 1 1 calc R U . . .
C4B C 0.70065(13) 1.1654(5) 0.76724(7) 0.0684(8) Uani 1 1 d . . . . .
C5B C 0.68716(16) 1.2797(5) 0.78692(8) 0.0787(10) Uani 1 1 d . . . . .
H5B H 0.669576 1.374967 0.781347 0.094 Uiso 1 1 calc R U . . .
C6B C 0.69999(16) 1.2517(4) 0.81503(8) 0.0778(10) Uani 1 1 d . . . . .
H6B H 0.691203 1.328983 0.828509 0.093 Uiso 1 1 calc R U . . .
C7B C 0.72825(14) 1.1525(4) 0.87545(7) 0.0645(8) Uani 1 1 d . . . . .
C8B C 0.74670(13) 1.1302(4) 0.92726(7) 0.0606(7) Uani 1 1 d . . . . .
C9B C 0.78248(16) 1.0640(5) 0.94670(7) 0.0831(11) Uani 1 1 d . . . . .
H9B H 0.806452 0.985898 0.94073 0.1 Uiso 1 1 calc R U . . .
C10B C 0.78379(16) 1.1097(5) 0.97456(8) 0.0843(11) Uani 1 1 d . . . . .
H10B H 0.808658 1.061685 0.986955 0.101 Uiso 1 1 calc R U . . .
C11B C 0.74920(12) 1.2253(4) 0.98491(6) 0.0567(7) Uani 1 1 d . . . . .
C12B C 0.71328(15) 1.2891(5) 0.96516(7) 0.0784(10) Uani 1 1 d . . . . .
H12B H 0.689098 1.366433 0.971158 0.094 Uiso 1 1 calc R U . . .
C13B C 0.71130(16) 1.2444(5) 0.93703(8) 0.0834(11) Uani 1 1 d . . . . .
H13B H 0.686171 1.291033 0.924627 0.1 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7A 1.217(4) . ?
O2A C20A 1.218(4) . ?
O3A N5A 1.207(6) . ?
O4A N5A 1.215(6) . ?
O5A N6A 1.210(5) . ?
O6A N6A 1.197(5) . ?
N1A C7A 1.379(4) . ?
N1A C1A 1.392(4) . ?
N1A H1A 0.86 . ?
N2A C7A 1.362(4) . ?
N2A C8A 1.399(4) . ?
N2A H2A 0.86 . ?
N3A C20A 1.355(4) . ?
N3A C17A 1.406(4) . ?
N3A H3A 0.86 . ?
N4A C20A 1.382(4) . ?
N4A C21A 1.392(4) . ?
N4A H4A 0.86 . ?
N5A C4A 1.447(5) . ?
N6A C24A 1.454(5) . ?
C1A C2A 1.385(5) . ?
C1A C6A 1.387(5) . ?
C2A C3A 1.372(5) . ?
C2A H2AA 0.93 . ?
C3A C4A 1.374(6) . ?
C3A H3AA 0.93 . ?
C4A C5A 1.371(6) . ?
C5A C6A 1.372(5) . ?
C5A H5A 0.93 . ?
C6A H6A 0.93 . ?
C8A C9A 1.377(5) . ?
C8A C13A 1.386(5) . ?
C9A C10A 1.373(5) . ?
C9A H9A 0.93 . ?
C10A C11A 1.399(4) . ?
C10A H10A 0.93 . ?
C11A C12A 1.383(5) . ?
C11A C14A 1.478(4) . ?
C12A C13A 1.380(5) . ?
C12A H12A 0.93 . ?
C13A H13A 0.93 . ?
C14A C19A 1.388(4) . ?
C14A C15A 1.400(4) . ?
C15A C16A 1.371(5) . ?
C15A H15A 0.93 . ?
C16A C17A 1.398(4) . ?
C16A H16A 0.93 . ?
C17A C18A 1.373(5) . ?
C18A C19A 1.379(5) . ?
C18A H18A 0.93 . ?
C19A H19A 0.93 . ?
C21A C26A 1.393(5) . ?
C21A C22A 1.395(5) . ?
C22A C23A 1.375(5) . ?
C22A H22A 0.93 . ?
C23A C24A 1.368(5) . ?
C23A H23A 0.93 . ?
C24A C25A 1.373(5) . ?
C25A C26A 1.371(5) . ?
C25A H25A 0.93 . ?
C26A H26A 0.93 . ?
O1B C7B 1.216(4) . ?
O2B N3B 1.212(5) . ?
O3B N3B 1.214(5) . ?
N1B C7B 1.374(4) . ?
N1B C1B 1.388(4) . ?
N1B H1B 0.86 . ?
N2B C7B 1.372(4) . ?
N2B C8B 1.400(4) . ?
N2B H2B 0.86 . ?
N3B C4B 1.462(5) . ?
C1B C2B 1.393(4) . ?
C1B C6B 1.394(5) . ?
C2B C3B 1.367(5) . ?
C2B H2BA 0.93 . ?
C3B C4B 1.362(5) . ?
C3B H3B 0.93 . ?
C4B C5B 1.371(5) . ?
C5B C6B 1.376(5) . ?
C5B H5B 0.93 . ?
C6B H6B 0.93 . ?
C8B C9B 1.376(5) . ?
C8B C13B 1.383(5) . ?
C9B C10B 1.369(5) . ?
C9B H9B 0.93 . ?
C10B C11B 1.387(4) . ?
C10B H10B 0.93 . ?
C11B C12B 1.380(5) . ?
C11B C11B 1.482(6) 7_677 ?
C12B C13B 1.379(5) . ?
C12B H12B 0.93 . ?
C13B H13B 0.93 . ?

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
C7A N1A C1A 128.6(3) . . ?
C7A N1A H1A 115.7 . . ?
C1A N1A H1A 115.7 . . ?
C7A N2A C8A 128.4(3) . . ?
C7A N2A H2A 115.8 . . ?
C8A N2A H2A 115.8 . . ?
C20A N3A C17A 127.3(3) . . ?
C20A N3A H3A 116.4 . . ?
C17A N3A H3A 116.4 . . ?
C20A N4A C21A 128.8(3) . . ?
C20A N4A H4A 115.6 . . ?
C21A N4A H4A 115.6 . . ?
O3A N5A O4A 122.5(5) . . ?
O3A N5A C4A 118.6(5) . . ?
O4A N5A C4A 118.9(5) . . ?
O6A N6A O5A 121.5(5) . . ?
O6A N6A C24A 120.2(4) . . ?
O5A N6A C24A 118.2(4) . . ?
C2A C1A C6A 119.2(3) . . ?
C2A C1A N1A 124.6(3) . . ?
C6A C1A N1A 116.2(3) . . ?
C3A C2A C1A 120.3(4) . . ?
C3A C2A H2AA 119.8 . . ?
C1A C2A H2AA 119.8 . . ?
C2A C3A C4A 119.4(4) . . ?
C2A C3A H3AA 120.3 . . ?
C4A C3A H3AA 120.3 . . ?
C5A C4A C3A 121.2(4) . . ?
C5A C4A N5A 118.9(4) . . ?
C3A C4A N5A 119.8(4) . . ?
C4A C5A C6A 119.2(4) . . ?
C4A C5A H5A 120.4 . . ?
C6A C5A H5A 120.4 . . ?
C5A C6A C1A 120.6(4) . . ?
C5A C6A H6A 119.7 . . ?
C1A C6A H6A 119.7 . . ?
O1A C7A N2A 124.8(3) . . ?
O1A C7A N1A 124.0(3) . . ?
N2A C7A N1A 111.2(3) . . ?
C9A C8A C13A 117.9(3) . . ?
C9A C8A N2A 117.6(3) . . ?
C13A C8A N2A 124.5(3) . . ?
C10A C9A C8A 122.0(3) . . ?
C10A C9A H9A 119 . . ?
C8A C9A H9A 119 . . ?
C9A C10A C11A 121.1(3) . . ?
C9A C10A H10A 119.4 . . ?
C11A C10A H10A 119.4 . . ?
C12A C11A C10A 116.0(3) . . ?
C12A C11A C14A 122.1(3) . . ?
C10A C11A C14A 121.9(3) . . ?
C13A C12A C11A 123.2(3) . . ?
C13A C12A H12A 118.4 . . ?
C11A C12A H12A 118.4 . . ?
C12A C13A C8A 119.8(3) . . ?
C12A C13A H13A 120.1 . . ?
C8A C13A H13A 120.1 . . ?
C19A C14A C15A 115.5(3) . . ?
C19A C14A C11A 121.9(3) . . ?
C15A C14A C11A 122.5(3) . . ?
C16A C15A C14A 123.1(3) . . ?
C16A C15A H15A 118.4 . . ?
C14A C15A H15A 118.4 . . ?
C15A C16A C17A 120.1(3) . . ?
C15A C16A H16A 120 . . ?
C17A C16A H16A 120 . . ?
C18A C17A C16A 117.5(3) . . ?
C18A C17A N3A 118.2(3) . . ?
C16A C17A N3A 124.2(3) . . ?
C17A C18A C19A 121.9(3) . . ?
C17A C18A H18A 119 . . ?
C19A C18A H18A 119 . . ?
C18A C19A C14A 121.8(3) . . ?
C18A C19A H19A 119.1 . . ?
C14A C19A H19A 119.1 . . ?
O2A C20A N3A 125.1(3) . . ?
O2A C20A N4A 123.7(3) . . ?
N3A C20A N4A 111.2(3) . . ?
N4A C21A C26A 116.9(3) . . ?
N4A C21A C22A 124.3(3) . . ?
C26A C21A C22A 118.8(3) . . ?
C23A C22A C21A 120.0(4) . . ?
C23A C22A H22A 120 . . ?
C21A C22A H22A 120 . . ?
C24A C23A C22A 119.8(4) . . ?
C24A C23A H23A 120.1 . . ?
C22A C23A H23A 120.1 . . ?
C23A C24A C25A 121.4(4) . . ?
C23A C24A N6A 119.6(4) . . ?
C25A C24A N6A 119.0(4) . . ?
C26A C25A C24A 119.2(4) . . ?
C26A C25A H25A 120.4 . . ?
C24A C25A H25A 120.4 . . ?
C25A C26A C21A 120.7(4) . . ?
C25A C26A H26A 119.6 . . ?
C21A C26A H26A 119.6 . . ?
C7B N1B C1B 127.7(3) . . ?
C7B N1B H1B 116.1 . . ?
C1B N1B H1B 116.1 . . ?
C7B N2B C8B 127.2(3) . . ?
C7B N2B H2B 116.4 . . ?
C8B N2B H2B 116.4 . . ?
O2B N3B O3B 123.3(4) . . ?
O2B N3B C4B 118.9(4) . . ?
O3B N3B C4B 117.8(4) . . ?
N1B C1B C2B 117.0(3) . . ?
N1B C1B C6B 125.0(3) . . ?
C2B C1B C6B 118.0(3) . . ?
C3B C2B C1B 121.3(3) . . ?
C3B C2B H2BA 119.4 . . ?
C1B C2B H2BA 119.4 . . ?
C4B C3B C2B 119.2(3) . . ?
C4B C3B H3B 120.4 . . ?
C2B C3B H3B 120.4 . . ?
C3B C4B C5B 121.8(3) . . ?
C3B C4B N3B 119.0(4) . . ?
C5B C4B N3B 119.2(4) . . ?
C4B C5B C6B 119.1(3) . . ?
C4B C5B H5B 120.5 . . ?
C6B C5B H5B 120.5 . . ?
C5B C6B C1B 120.7(3) . . ?
C5B C6B H6B 119.7 . . ?
C1B C6B H6B 119.7 . . ?
O1B C7B N2B 124.3(3) . . ?
O1B C7B N1B 124.2(3) . . ?
N2B C7B N1B 111.5(3) . . ?
C9B C8B C13B 117.3(3) . . ?
C9B C8B N2B 118.0(3) . . ?
C13B C8B N2B 124.7(3) . . ?
C10B C9B C8B 121.9(3) . . ?
C10B C9B H9B 119 . . ?
C8B C9B H9B 119 . . ?
C9B C10B C11B 122.1(3) . . ?
C9B C10B H10B 119 . . ?
C11B C10B H10B 119 . . ?
C12B C11B C10B 115.1(3) . . ?
C12B C11B C11B 122.9(3) . 7_677 ?
C10B C11B C11B 121.9(4) . 7_677 ?
C13B C12B C11B 123.6(3) . . ?
C13B C12B H12B 118.2 . . ?
C11B C12B H12B 118.2 . . ?
C12B C13B C8B 119.9(3) . . ?
C12B C13B H13B 120 . . ?
C8B C13B H13B 120 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7A N1A C1A C2A -3.5(6) . . . . ?
C7A N1A C1A C6A 177.2(3) . . . . ?
C6A C1A C2A C3A 0.8(6) . . . . ?
N1A C1A C2A C3A -178.5(4) . . . . ?
C1A C2A C3A C4A -1.1(6) . . . . ?
C2A C3A C4A C5A 0.7(7) . . . . ?
C2A C3A C4A N5A 179.3(4) . . . . ?
O3A N5A C4A C5A 170.3(5) . . . . ?
O4A N5A C4A C5A -8.4(7) . . . . ?
O3A N5A C4A C3A -8.3(7) . . . . ?
O4A N5A C4A C3A 173.0(5) . . . . ?
C3A C4A C5A C6A 0.1(6) . . . . ?
N5A C4A C5A C6A -178.5(4) . . . . ?
C4A C5A C6A C1A -0.5(6) . . . . ?
C2A C1A C6A C5A 0.1(6) . . . . ?
N1A C1A C6A C5A 179.4(3) . . . . ?
C8A N2A C7A O1A -5.6(6) . . . . ?
C8A N2A C7A N1A 173.8(3) . . . . ?
C1A N1A C7A O1A -2.1(6) . . . . ?
C1A N1A C7A N2A 178.5(3) . . . . ?
C7A N2A C8A C9A -164.6(4) . . . . ?
C7A N2A C8A C13A 16.0(6) . . . . ?
C13A C8A C9A C10A -1.6(6) . . . . ?
N2A C8A C9A C10A 179.0(4) . . . . ?
C8A C9A C10A C11A 0.1(6) . . . . ?
C9A C10A C11A C12A 1.6(5) . . . . ?
C9A C10A C11A C14A -177.3(3) . . . . ?
C10A C11A C12A C13A -1.9(6) . . . . ?
C14A C11A C12A C13A 177.0(4) . . . . ?
C11A C12A C13A C8A 0.4(7) . . . . ?
C9A C8A C13A C12A 1.4(6) . . . . ?
N2A C8A C13A C12A -179.3(4) . . . . ?
C12A C11A C14A C19A 15.4(5) . . . . ?
C10A C11A C14A C19A -165.8(3) . . . . ?
C12A C11A C14A C15A -161.9(4) . . . . ?
C10A C11A C14A C15A 16.9(5) . . . . ?
C19A C14A C15A C16A 0.1(6) . . . . ?
C11A C14A C15A C16A 177.5(3) . . . . ?
C14A C15A C16A C17A -1.1(6) . . . . ?
C15A C16A C17A C18A 1.2(6) . . . . ?
C15A C16A C17A N3A -176.8(4) . . . . ?
C20A N3A C17A C18A 150.3(4) . . . . ?
C20A N3A C17A C16A -31.7(6) . . . . ?
C16A C17A C18A C19A -0.4(6) . . . . ?
N3A C17A C18A C19A 177.8(3) . . . . ?
C17A C18A C19A C14A -0.6(6) . . . . ?
C15A C14A C19A C18A 0.8(5) . . . . ?
C11A C14A C19A C18A -176.7(3) . . . . ?
C17A N3A C20A O2A 8.4(6) . . . . ?
C17A N3A C20A N4A -172.1(3) . . . . ?
C21A N4A C20A O2A -2.6(6) . . . . ?
C21A N4A C20A N3A 177.9(3) . . . . ?
C20A N4A C21A C26A -177.7(3) . . . . ?
C20A N4A C21A C22A 2.7(6) . . . . ?
N4A C21A C22A C23A -179.4(3) . . . . ?
C26A C21A C22A C23A 0.9(5) . . . . ?
C21A C22A C23A C24A -1.0(6) . . . . ?
C22A C23A C24A C25A 0.8(6) . . . . ?
C22A C23A C24A N6A -177.7(4) . . . . ?
O6A N6A C24A C23A 7.2(6) . . . . ?
O5A N6A C24A C23A -169.9(5) . . . . ?
O6A N6A C24A C25A -171.4(4) . . . . ?
O5A N6A C24A C25A 11.5(6) . . . . ?
C23A C24A C25A C26A -0.6(6) . . . . ?
N6A C24A C25A C26A 178.0(4) . . . . ?
C24A C25A C26A C21A 0.5(6) . . . . ?
N4A C21A C26A C25A 179.7(3) . . . . ?
C22A C21A C26A C25A -0.6(6) . . . . ?
C7B N1B C1B C2B -174.9(3) . . . . ?
C7B N1B C1B C6B 4.8(6) . . . . ?
N1B C1B C2B C3B 179.7(3) . . . . ?
C6B C1B C2B C3B 0.0(5) . . . . ?
C1B C2B C3B C4B -0.6(6) . . . . ?
C2B C3B C4B C5B 0.8(6) . . . . ?
C2B C3B C4B N3B -177.8(3) . . . . ?
O2B N3B C4B C3B 170.4(4) . . . . ?
O3B N3B C4B C3B -11.3(6) . . . . ?
O2B N3B C4B C5B -8.2(6) . . . . ?
O3B N3B C4B C5B 170.1(4) . . . . ?
C3B C4B C5B C6B -0.2(6) . . . . ?
N3B C4B C5B C6B 178.4(4) . . . . ?
C4B C5B C6B C1B -0.5(6) . . . . ?
N1B C1B C6B C5B -179.1(3) . . . . ?
C2B C1B C6B C5B 0.6(6) . . . . ?
C8B N2B C7B O1B -5.5(6) . . . . ?
C8B N2B C7B N1B 174.8(3) . . . . ?
C1B N1B C7B O1B -0.9(6) . . . . ?
C1B N1B C7B N2B 178.7(3) . . . . ?
C7B N2B C8B C9B -158.8(4) . . . . ?
C7B N2B C8B C13B 23.1(6) . . . . ?
C13B C8B C9B C10B -0.8(6) . . . . ?
N2B C8B C9B C10B -179.0(4) . . . . ?
C8B C9B C10B C11B 0.0(7) . . . . ?
C9B C10B C11B C12B 0.6(6) . . . . ?
C9B C10B C11B C11B -179.9(4) . . . 7_677 ?
C10B C11B C12B C13B -0.5(6) . . . . ?
C11B C11B C12B C13B -180.0(4) 7_677 . . . ?
C11B C12B C13B C8B -0.2(7) . . . . ?
C9B C8B C13B C12B 0.8(6) . . . . ?
N2B C8B C13B C12B 178.9(4) . . . . ?

# SQUEEZE RESULTS (Version = 110917)
# 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 0.275 0.250 -0.025 1471 509 ' '
2 0.714 -0.250 0.036 1471 509 ' '
_platon_squeeze_void_probe_radius 1.20


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_1-((TBA)H2PO4)2
_database_code_depnum_ccdc_archive 'CCDC 2015338'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T14:51:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2017/1

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         
'C26 H22 N4 O2, 2(C16 H36 N), 2(H2 O4 P), 0.5(H2 O)'
_chemical_formula_sum            'C58 H99 N6 O10.50 P2'
_chemical_formula_weight         1110.37

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 2/a'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_Int_Tables_number      15

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

_cell_length_a                   18.2621(5)
_cell_length_b                   14.8485(4)
_cell_length_c                   24.8790(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.576(3)
_cell_angle_gamma                90
_cell_volume                     6746.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    8523
_cell_measurement_theta_min      2.9850
_cell_measurement_theta_max      76.5166

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.147
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_F_000             2412

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.74599
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_number            23142
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.466
_diffrn_reflns_theta_max         67.996
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.975
_reflns_Friedel_coverage         0
_reflns_number_total             6002
_reflns_number_gt                4908
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
'CrysAlisPro 1.171.36.20 (Agilent Technologies,2012)'
_computing_cell_refinement       
'CrysAlisPro 1.171.36.20 (Agilent Technologies,2012)'
_computing_data_reduction        
'CrysAlisPro 1.171.36.20 (Agilent Technologies,2012)'
_computing_structure_solution    'SIR-2004 (Burla et al., 2005)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6002
_refine_ls_number_parameters     407
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.1039
_refine_ls_wR_factor_ref         0.3711
_refine_ls_wR_factor_gt          0.3457
_refine_ls_goodness_of_fit_ref   1.590
_refine_ls_restrained_S_all      1.600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.060


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.65173(11) 0.37802(13) 0.14217(9) 0.0800(6) Uani 1 1 d . . . . .
H1 H 0.645986 0.415782 0.116265 0.096 Uiso 1 1 calc R U . . .
N2 N 0.59878(13) 0.28084(13) 0.08252(10) 0.0842(6) Uani 1 1 d . . . . .
H2 H 0.598484 0.32697 0.061618 0.101 Uiso 1 1 calc R U . . .
O1 O 0.62561(13) 0.23352(14) 0.16762(10) 0.1016(7) Uani 1 1 d . . . . .
C1 C 0.68593(12) 0.41077(17) 0.18839(10) 0.0762(6) Uani 1 1 d . . . . .
C2 C 0.70725(13) 0.50069(18) 0.18781(12) 0.0825(7) Uani 1 1 d . . . . .
H2A H 0.698547 0.535318 0.157262 0.099 Uiso 1 1 calc R U . . .
C3 C 0.74123(16) 0.5393(2) 0.23208(14) 0.0941(8) Uani 1 1 d . . . . .
H3 H 0.753236 0.600111 0.231543 0.113 Uiso 1 1 calc R U . . .
C4 C 0.75760(19) 0.4881(3) 0.27734(14) 0.1009(9) Uani 1 1 d . . . . .
H4 H 0.780778 0.513826 0.30703 0.121 Uiso 1 1 calc R U . . .
C5 C 0.7390(2) 0.3995(3) 0.27727(12) 0.1035(9) Uani 1 1 d . . . . .
H5 H 0.751074 0.364379 0.307012 0.124 Uiso 1 1 calc R U . . .
C6 C 0.70254(16) 0.3598(2) 0.23416(12) 0.0912(7) Uani 1 1 d . . . . .
H6 H 0.68919 0.299409 0.235728 0.109 Uiso 1 1 calc R U . . .
C7 C 0.62604(12) 0.29227(16) 0.13311(12) 0.0791(6) Uani 1 1 d . . . . .
C8 C 0.57095(13) 0.19931(16) 0.06162(12) 0.0792(6) Uani 1 1 d . . . . .
C9 C 0.51424(18) 0.20401(17) 0.02514(13) 0.0945(8) Uani 1 1 d . . . . .
H9 H 0.493967 0.25967 0.016473 0.113 Uiso 1 1 calc R U . . .
C10 C 0.48668(19) 0.12625(18) 0.00093(14) 0.0963(8) Uani 1 1 d . . . . .
H10 H 0.448288 0.131132 -0.023743 0.116 Uiso 1 1 calc R U . . .
C11 C 0.51509(13) 0.04168(15) 0.01271(11) 0.0761(6) Uani 1 1 d . . . . .
C12 C 0.57255(15) 0.03920(17) 0.04919(15) 0.0907(8) Uani 1 1 d . . . . .
H12 H 0.593495 -0.016114 0.057773 0.109 Uiso 1 1 calc R U . . .
C13 C 0.60020(15) 0.11649(18) 0.07353(15) 0.0934(8) Uani 1 1 d . . . . .
H13 H 0.638796 0.112028 0.098056 0.112 Uiso 1 1 calc R U . . .
N3 N 0.46779(14) 0.5947(2) 0.18429(14) 0.1079(9) Uani 1 1 d . . . . .
C14 C 0.47314(16) 0.5050(3) 0.15477(14) 0.1006(9) Uani 1 1 d . . . . .
H14A H 0.474621 0.517114 0.116491 0.121 Uiso 1 1 calc R U . . .
H14B H 0.519248 0.476832 0.164744 0.121 Uiso 1 1 calc R U . . .
C15 C 0.41226(19) 0.4382(3) 0.16487(15) 0.1073(10) Uani 1 1 d . . . . .
H15A H 0.405525 0.431031 0.20326 0.129 Uiso 1 1 calc R U . . .
H15B H 0.366828 0.46064 0.149421 0.129 Uiso 1 1 calc R U . . .
C16 C 0.4305(3) 0.3490(3) 0.1403(2) 0.1262(13) Uani 1 1 d . . . . .
H16A H 0.474422 0.325572 0.157593 0.151 Uiso 1 1 calc R U . . .
H16B H 0.441192 0.357824 0.102575 0.151 Uiso 1 1 calc R U . . .
C17 C 0.3703(5) 0.2806(5) 0.1452(3) 0.178(3) Uani 1 1 d . . . . .
H17A H 0.353233 0.279456 0.181587 0.267 Uiso 1 1 calc R U . . .
H17B H 0.388632 0.222207 0.135719 0.267 Uiso 1 1 calc R U . . .
H17C H 0.330589 0.296482 0.121495 0.267 Uiso 1 1 calc R U . . .
C18 C 0.39917(18) 0.6448(3) 0.1710(2) 0.1265(15) Uani 1 1 d D . . . .
H18A H 0.357872 0.60553 0.177978 0.152 Uiso 1 1 calc R U . . .
H18B H 0.39552 0.695747 0.195195 0.152 Uiso 1 1 calc R U . . .
C19 C 0.3925(2) 0.6784(4) 0.1151(2) 0.1356(16) Uani 1 1 d D . . . .
H19A H 0.39779 0.628836 0.090045 0.163 Uiso 1 1 calc R U . . .
H19B H 0.430847 0.721947 0.108144 0.163 Uiso 1 1 calc R U . . .
C20 C 0.3190(3) 0.7215(5) 0.1078(3) 0.168(2) Uani 1 1 d D . . . .
H20A H 0.281814 0.675124 0.110477 0.202 Uiso 1 1 calc R U . . .
H20B H 0.311533 0.763422 0.137146 0.202 Uiso 1 1 calc R U . . .
C21 C 0.3077(4) 0.7708(7) 0.0560(4) 0.230(5) Uani 1 1 d D . . . .
H21A H 0.294054 0.728778 0.028295 0.346 Uiso 1 1 calc R U . . .
H21B H 0.352306 0.800574 0.046224 0.346 Uiso 1 1 calc R U . . .
H21C H 0.26954 0.814602 0.060099 0.346 Uiso 1 1 calc R U . . .
C22 C 0.53575(18) 0.6497(3) 0.1705(2) 0.1190(12) Uani 1 1 d . . . . .
H22A H 0.536938 0.656877 0.131804 0.143 Uiso 1 1 calc R U . . .
H22B H 0.578482 0.614652 0.180843 0.143 Uiso 1 1 calc R U . . .
C23 C 0.5432(3) 0.7424(4) 0.1958(3) 0.1462(18) Uani 1 1 d D . . . .
H23A H 0.536106 0.737578 0.23426 0.175 Uiso 1 1 calc R U . . .
H23B H 0.505293 0.781508 0.18135 0.175 Uiso 1 1 calc R U . . .
C24 C 0.6174(5) 0.7841(7) 0.1853(4) 0.233(5) Uani 1 1 d D U . . .
H24A H 0.61984 0.843316 0.201671 0.28 Uiso 1 1 calc R U . . .
H24B H 0.655464 0.747018 0.201445 0.28 Uiso 1 1 calc R U . . .
C25 C 0.6297(9) 0.7918(10) 0.1265(5) 0.286(6) Uani 1 1 d D U . . .
H25A H 0.64428 0.73432 0.112514 0.428 Uiso 1 1 calc R U . . .
H25B H 0.667454 0.835241 0.119979 0.428 Uiso 1 1 calc R U . . .
H25C H 0.585161 0.8107 0.109006 0.428 Uiso 1 1 calc R U . . .
C26 C 0.4647(2) 0.5802(3) 0.24462(17) 0.1259(14) Uani 1 1 d D . . . .
H26A H 0.461855 0.638654 0.261901 0.151 Uiso 1 1 calc R U . . .
H26B H 0.419888 0.548091 0.252687 0.151 Uiso 1 1 calc R U . . .
C27 C 0.5274(2) 0.5297(4) 0.26901(19) 0.1442(18) Uani 1 1 d D U . . .
H27A H 0.528931 0.469029 0.254561 0.173 Uiso 1 1 calc R U . . .
H27B H 0.573128 0.559442 0.260532 0.173 Uiso 1 1 calc R U . . .
C28 C 0.5179(4) 0.5264(5) 0.3278(2) 0.162(2) Uani 1 1 d D . . . .
H28A H 0.471974 0.496391 0.335488 0.195 Uiso 1 1 calc R U . . .
H28B H 0.514439 0.587511 0.34131 0.195 Uiso 1 1 calc R U . . .
C29 C 0.5779(4) 0.4792(8) 0.3575(3) 0.208(4) Uani 1 1 d D U . . .
H29A H 0.600204 0.519857 0.382722 0.312 Uiso 1 1 calc R U . . .
H29B H 0.613912 0.458758 0.332429 0.312 Uiso 1 1 calc R U . . .
H29C H 0.55809 0.428421 0.376333 0.312 Uiso 1 1 calc R U . . .
P1 P 0.63517(16) 0.50766(10) 0.01340(7) 0.1063(6) Uani 0.55 1 d . . P A 1
O2 O 0.5860(4) 0.5925(3) 0.0202(3) 0.1295(19) Uani 0.55 1 d . . P A 1
H2B H 0.548691 0.586882 0.001877 0.194 Uiso 0.55 1 calc R U P A 1
O3 O 0.6700(5) 0.5226(5) -0.0428(2) 0.1306(18) Uani 0.55 1 d . . P A 1
H3A H 0.714691 0.51977 -0.040038 0.196 Uiso 0.55 1 calc R U P A 1
O4 O 0.5903(4) 0.4256(4) 0.0122(3) 0.1277(18) Uani 0.55 1 d . . P A 1
O5 O 0.6913(5) 0.5068(4) 0.0564(2) 0.1219(17) Uani 0.55 1 d . . P A 1
P1' P 0.58481(15) 0.51308(14) 0.02170(8) 0.0955(6) Uani 0.45 1 d D . P B 2
O2' O 0.5342(4) 0.5936(4) 0.0304(3) 0.125(2) Uani 0.45 1 d D . P B 2
H2' H 0.517149 0.610022 0.001395 0.187 Uiso 0.45 1 calc R U P B 2
O3' O 0.6184(7) 0.5259(9) -0.0355(3) 0.160(4) Uani 0.45 1 d . U P B 2
H3' H 0.657636 0.499087 -0.03703 0.241 Uiso 0.45 1 calc R U P B 2
O4' O 0.5428(4) 0.4278(3) 0.0196(3) 0.1043(15) Uani 0.45 1 d D . P B 2
O5' O 0.6419(4) 0.5177(5) 0.0637(2) 0.1074(16) Uani 0.45 1 d D . P B 2
O1W O 0.7337(7) 0.5917(4) -0.0649(5) 0.134(4) Uani 0.25 1 d D . P C 4
H1WA H 0.763(6) 0.554(8) -0.054(7) 0.202 Uiso 0.25 1 d D U P D 4
H1WB H 0.743(11) 0.611(12) -0.095(3) 0.202 Uiso 0.25 1 d D U P E 4



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.375(3) . ?
N1 C1 1.391(3) . ?
N1 H1 0.86 . ?
N2 C7 1.359(4) . ?
N2 C8 1.410(3) . ?
N2 H2 0.86 . ?
O1 C7 1.224(3) . ?
C1 C2 1.391(4) . ?
C1 C6 1.398(4) . ?
C2 C3 1.383(4) . ?
C2 H2A 0.93 . ?
C3 C4 1.389(5) . ?
C3 H3 0.93 . ?
C4 C5 1.358(5) . ?
C4 H4 0.93 . ?
C5 C6 1.388(5) . ?
C5 H5 0.93 . ?
C6 H6 0.93 . ?
C8 C9 1.372(4) . ?
C8 C13 1.372(4) . ?
C9 C10 1.394(4) . ?
C9 H9 0.93 . ?
C10 C11 1.389(4) . ?
C10 H10 0.93 . ?
C11 C12 1.381(4) . ?
C11 C11 1.493(5) 5_655 ?
C12 C13 1.390(4) . ?
C12 H12 0.93 . ?
C13 H13 0.93 . ?
N3 C18 1.491(5) . ?
N3 C26 1.518(5) . ?
N3 C22 1.527(5) . ?
N3 C14 1.525(5) . ?
C14 C15 1.513(5) . ?
C14 H14A 0.97 . ?
C14 H14B 0.97 . ?
C15 C16 1.497(6) . ?
C15 H15A 0.97 . ?
C15 H15B 0.97 . ?
C16 C17 1.503(9) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 C19 1.481(6) . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
C19 C20 1.497(7) . ?
C19 H19A 0.97 . ?
C19 H19B 0.97 . ?
C20 C21 1.495(5) . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 C23 1.519(7) . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C23 C24 1.514(7) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C24 C25 1.488(5) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 C27 1.493(4) . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C27 C28 1.476(7) . ?
C27 H27A 0.97 . ?
C27 H27B 0.97 . ?
C28 C29 1.489(5) . ?
C28 H28A 0.97 . ?
C28 H28B 0.97 . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?
P1 O4 1.468(7) . ?
P1 O5 1.474(6) . ?
P1 O3 1.557(7) . ?
P1 O2 1.558(7) . ?
O2 H2B 0.82 . ?
O3 H3A 0.82 . ?
P1' O5' 1.470(6) . ?
P1' O4' 1.480(5) . ?
P1' O2' 1.528(4) . ?
P1' O3' 1.567(8) . ?
O2' H2' 0.82 . ?
O3' H3' 0.82 . ?
O1W H1WA 0.820(3) . ?
O1W H1WB 0.820(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
C7 N1 C1 127.5(2) . . ?
C7 N1 H1 116.2 . . ?
C1 N1 H1 116.2 . . ?
C7 N2 C8 125.2(2) . . ?
C7 N2 H2 117.4 . . ?
C8 N2 H2 117.4 . . ?
N1 C1 C2 116.8(2) . . ?
N1 C1 C6 125.2(2) . . ?
C2 C1 C6 118.0(3) . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 118.5(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 122.0(3) . . ?
C4 C5 H5 119 . . ?
C6 C5 H5 119 . . ?
C5 C6 C1 119.8(3) . . ?
C5 C6 H6 120.1 . . ?
C1 C6 H6 120.1 . . ?
O1 C7 N2 123.8(2) . . ?
O1 C7 N1 123.3(3) . . ?
N2 C7 N1 112.9(2) . . ?
C9 C8 C13 118.6(2) . . ?
C9 C8 N2 117.8(2) . . ?
C13 C8 N2 123.5(2) . . ?
C8 C9 C10 120.7(2) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 121.7(3) . . ?
C11 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
C12 C11 C10 116.3(2) . . ?
C12 C11 C11 122.1(3) . 5_655 ?
C10 C11 C11 121.6(3) . 5_655 ?
C11 C12 C13 122.3(2) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C8 C13 C12 120.5(3) . . ?
C8 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C18 N3 C26 104.5(3) . . ?
C18 N3 C22 111.5(3) . . ?
C26 N3 C22 109.6(3) . . ?
C18 N3 C14 112.7(3) . . ?
C26 N3 C14 110.8(3) . . ?
C22 N3 C14 107.6(3) . . ?
C15 C14 N3 116.2(3) . . ?
C15 C14 H14A 108.2 . . ?
N3 C14 H14A 108.2 . . ?
C15 C14 H14B 108.2 . . ?
N3 C14 H14B 108.2 . . ?
H14A C14 H14B 107.4 . . ?
C16 C15 C14 110.2(3) . . ?
C16 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
C14 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C15 C16 C17 113.5(4) . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N3 115.9(3) . . ?
C19 C18 H18A 108.3 . . ?
N3 C18 H18A 108.3 . . ?
C19 C18 H18B 108.3 . . ?
N3 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
C18 C19 C20 108.9(4) . . ?
C18 C19 H19A 109.9 . . ?
C20 C19 H19A 109.9 . . ?
C18 C19 H19B 109.9 . . ?
C20 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C21 C20 C19 115.5(5) . . ?
C21 C20 H20A 108.4 . . ?
C19 C20 H20A 108.4 . . ?
C21 C20 H20B 108.4 . . ?
C19 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 C23 117.5(3) . . ?
N3 C22 H22A 107.9 . . ?
C23 C22 H22A 107.9 . . ?
N3 C22 H22B 107.9 . . ?
C23 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C22 C23 C24 112.1(5) . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23B 109.2 . . ?
C24 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 110.1(9) . . ?
C25 C24 H24A 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C25 C24 H24B 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 N3 115.9(3) . . ?
C27 C26 H26A 108.3 . . ?
N3 C26 H26A 108.3 . . ?
C27 C26 H26B 108.3 . . ?
N3 C26 H26B 108.3 . . ?
H26A C26 H26B 107.4 . . ?
C28 C27 C26 108.8(4) . . ?
C28 C27 H27A 109.9 . . ?
C26 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
C26 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C27 C28 C29 114.4(5) . . ?
C27 C28 H28A 108.7 . . ?
C29 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
C29 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O4 P1 O5 113.1(3) . . ?
O4 P1 O3 109.4(4) . . ?
O5 P1 O3 111.4(4) . . ?
O4 P1 O2 110.6(5) . . ?
O5 P1 O2 109.0(4) . . ?
O3 P1 O2 102.9(4) . . ?
P1 O2 H2B 109.5 . . ?
P1 O3 H3A 109.5 . . ?
O5' P1' O4' 115.4(4) . . ?
O5' P1' O2' 106.8(5) . . ?
O4' P1' O2' 111.1(4) . . ?
O5' P1' O3' 111.0(5) . . ?
O4' P1' O3' 106.2(5) . . ?
O2' P1' O3' 106.1(6) . . ?
P1' O2' H2' 109.5 . . ?
P1' O3' H3' 109.5 . . ?
H1WA O1W H1WB 113(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N1 C1 C2 179.9(2) . . . . ?
C7 N1 C1 C6 2.2(4) . . . . ?
N1 C1 C2 C3 179.6(2) . . . . ?
C6 C1 C2 C3 -2.5(4) . . . . ?
C1 C2 C3 C4 2.7(5) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C3 C4 C5 C6 -1.9(6) . . . . ?
C4 C5 C6 C1 2.0(5) . . . . ?
N1 C1 C6 C5 177.9(3) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
C8 N2 C7 O1 -4.4(4) . . . . ?
C8 N2 C7 N1 177.9(2) . . . . ?
C1 N1 C7 O1 5.5(4) . . . . ?
C1 N1 C7 N2 -176.8(2) . . . . ?
C7 N2 C8 C9 146.7(3) . . . . ?
C7 N2 C8 C13 -37.1(4) . . . . ?
C13 C8 C9 C10 0.3(5) . . . . ?
N2 C8 C9 C10 176.8(3) . . . . ?
C8 C9 C10 C11 0.2(6) . . . . ?
C9 C10 C11 C12 -0.7(5) . . . . ?
C9 C10 C11 C11 179.2(3) . . . 5_655 ?
C10 C11 C12 C13 0.8(5) . . . . ?
C11 C11 C12 C13 -179.1(3) 5_655 . . . ?
C9 C8 C13 C12 -0.2(5) . . . . ?
N2 C8 C13 C12 -176.4(3) . . . . ?
C11 C12 C13 C8 -0.4(5) . . . . ?
C18 N3 C14 C15 -59.1(5) . . . . ?
C26 N3 C14 C15 57.6(4) . . . . ?
C22 N3 C14 C15 177.5(3) . . . . ?
N3 C14 C15 C16 -171.3(4) . . . . ?
C14 C15 C16 C17 -175.9(5) . . . . ?
C26 N3 C18 C19 172.4(4) . . . . ?
C22 N3 C18 C19 54.0(5) . . . . ?
C14 N3 C18 C19 -67.2(5) . . . . ?
N3 C18 C19 C20 176.5(4) . . . . ?
C18 C19 C20 C21 171.5(7) . . . . ?
C18 N3 C22 C23 56.3(6) . . . . ?
C26 N3 C22 C23 -58.9(5) . . . . ?
C14 N3 C22 C23 -179.5(4) . . . . ?
N3 C22 C23 C24 171.9(7) . . . . ?
C22 C23 C24 C25 58.6(12) . . . . ?
C18 N3 C26 C27 179.2(4) . . . . ?
C22 N3 C26 C27 -61.1(5) . . . . ?
C14 N3 C26 C27 57.5(5) . . . . ?
N3 C26 C27 C28 176.7(5) . . . . ?
C26 C27 C28 C29 -178.8(7) . . . . ?

# SQUEEZE RESULTS (Version =  71116)
# 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 0.250 0.133 1.000 173 43 ' '
2 0.750 -0.133 1.000 173 43 ' '
3 0.250 0.367 0.500 173 43 ' '
4 0.750 0.633 0.500 173 43 ' '
_platon_squeeze_void_probe_radius 1.20


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_3-((TBA)Br)2
_database_code_depnum_ccdc_archive 'CCDC 2015345'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-19T12:45:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C34 H26 N4 O2, 2(C16 H36 N), 2(Br)'
_chemical_formula_sum            'C66 H98 Br2 N6 O2'
_chemical_formula_weight         1167.32

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_Int_Tables_number      13

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

_cell_length_a                   21.451(2)
_cell_length_b                   8.7308(7)
_cell_length_c                   17.3855(11)
_cell_angle_alpha                90
_cell_angle_beta                 92.489(7)
_cell_angle_gamma                90
_cell_volume                     3252.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    2669
_cell_measurement_theta_min      4.3600
_cell_measurement_theta_max      25.4040


#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.810
_exptl_crystal_size_mid          0.546
_exptl_crystal_size_min          0.347
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_F_000             1244

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_T_max  0.698

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_number            13652
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.303
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             6364
_reflns_number_gt                4311
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0755P)²+0.8676P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6364
_refine_ls_number_parameters     347
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1471
_refine_ls_wR_factor_gt          0.1254
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.049


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.24415(10) 0.1162(3) 0.35262(13) 0.0706(6) Uani 1 1 d . . . . .
N1 N 0.22408(11) 0.0081(3) 0.46879(14) 0.0572(6) Uani 1 1 d . . . . .
H1 H 0.240207 -0.048713 0.504829 0.069 Uiso 1 1 calc R . . . .
N2 N 0.31650(11) -0.0360(3) 0.41383(13) 0.0548(6) Uani 1 1 d . . . . .
H2 H 0.321947 -0.096307 0.452666 0.066 Uiso 1 1 calc R . . . .
C1 C 0.16413(14) 0.0624(4) 0.47940(18) 0.0574(8) Uani 1 1 d . . . . .
C2 C 0.12598(17) 0.1093(5) 0.4194(2) 0.0775(10) Uani 1 1 d . . . . .
H2A H 0.140162 0.107141 0.369617 0.093 Uiso 1 1 calc R . . . .
C3 C 0.0655(2) 0.1609(7) 0.4322(3) 0.1109(17) Uani 1 1 d . . . . .
H3 H 0.040134 0.193543 0.390678 0.133 Uiso 1 1 calc R . . . .
C4 C 0.0436(2) 0.1639(7) 0.5033(3) 0.1185(18) Uani 1 1 d . . . . .
H4 H 0.003196 0.197909 0.51025 0.142 Uiso 1 1 calc R . . . .
C5 C 0.08079(18) 0.1166(5) 0.5671(2) 0.0844(11) Uani 1 1 d . . . . .
C6 C 0.0590(2) 0.1180(6) 0.6433(3) 0.1058(15) Uani 1 1 d . . . . .
H6 H 0.01859 0.15096 0.651129 0.127 Uiso 1 1 calc R . . . .
C7 C 0.0950(2) 0.0733(6) 0.7040(3) 0.0982(14) Uani 1 1 d . . . . .
H7 H 0.079273 0.074756 0.753024 0.118 Uiso 1 1 calc R . . . .
C8 C 0.15574(19) 0.0247(5) 0.6938(2) 0.0768(10) Uani 1 1 d . . . . .
H8 H 0.180752 -0.005032 0.73617 0.092 Uiso 1 1 calc R . . . .
C9 C 0.17897(16) 0.0204(4) 0.62208(18) 0.0622(8) Uani 1 1 d . . . . .
H9 H 0.219658 -0.013165 0.616364 0.075 Uiso 1 1 calc R . . . .
C10 C 0.14286(15) 0.0655(4) 0.55666(19) 0.0599(8) Uani 1 1 d . . . . .
C11 C 0.26041(14) 0.0353(3) 0.40695(17) 0.0511(7) Uani 1 1 d . . . . .
C12 C 0.36677(13) -0.0233(3) 0.36512(16) 0.0481(7) Uani 1 1 d . . . . .
C13 C 0.42516(15) -0.0641(4) 0.39561(17) 0.0607(8) Uani 1 1 d . . . . .
H13 H 0.42939 -0.094752 0.446803 0.073 Uiso 1 1 calc R . . . .
C14 C 0.47707(15) -0.0602(4) 0.35179(17) 0.0601(8) Uani 1 1 d . . . . .
H14 H 0.515759 -0.087377 0.373862 0.072 Uiso 1 1 calc R . . . .
C15 C 0.47228(14) -0.0156(3) 0.27410(16) 0.0516(7) Uani 1 1 d . . . . .
C16 C 0.41382(14) 0.0252(3) 0.24461(16) 0.0522(7) Uani 1 1 d . . . . .
H16 H 0.409385 0.055757 0.193422 0.063 Uiso 1 1 calc R . . . .
C17 C 0.36153(14) 0.0220(3) 0.28864(16) 0.0498(7) Uani 1 1 d . . . . .
H17 H 0.322867 0.050349 0.266891 0.06 Uiso 1 1 calc R . . . .
N3 N 0.27112(12) 0.5362(3) 0.26943(15) 0.0595(7) Uani 1 1 d . . . . .
C18 C 0.24356(17) 0.6060(4) 0.3403(2) 0.0704(9) Uani 1 1 d . . . . .
H18A H 0.210133 0.674855 0.323691 0.084 Uiso 1 1 calc R . . . .
H18B H 0.275521 0.666833 0.367016 0.084 Uiso 1 1 calc R . . . .
C19 C 0.2179(2) 0.4909(5) 0.3971(2) 0.0891(12) Uani 1 1 d . . . . .
H19A H 0.190004 0.420545 0.369444 0.107 Uiso 1 1 calc R . . . .
H19B H 0.252171 0.431751 0.420031 0.107 Uiso 1 1 calc R . . . .
C20 C 0.1830(2) 0.5684(6) 0.4603(2) 0.1004(14) Uani 1 1 d D . . . .
H20A H 0.173386 0.49233 0.498658 0.121 Uiso 1 1 calc R . . . .
H20B H 0.210273 0.643946 0.485126 0.121 Uiso 1 1 calc R . . . .
C21 C 0.1235(2) 0.6461(8) 0.4335(4) 0.138(2) Uani 1 1 d D . . . .
H21A H 0.131944 0.71688 0.393011 0.208 Uiso 1 1 calc GR . . . .
H21B H 0.106434 0.70043 0.47575 0.208 Uiso 1 1 calc GR . . . .
H21C H 0.094091 0.570647 0.414661 0.208 Uiso 1 1 calc GR . . . .
C22 C 0.22440(15) 0.4330(4) 0.22698(19) 0.0635(8) Uani 1 1 d . . . . .
H22A H 0.214467 0.34861 0.260627 0.076 Uiso 1 1 calc R . . . .
H22B H 0.244049 0.390027 0.182638 0.076 Uiso 1 1 calc R . . . .
C23 C 0.16395(18) 0.5093(5) 0.1996(3) 0.0864(11) Uani 1 1 d . . . . .
H23A H 0.146954 0.566166 0.241835 0.104 Uiso 1 1 calc R . . . .
H23B H 0.172288 0.581323 0.158829 0.104 Uiso 1 1 calc R . . . .
C24 C 0.1166(2) 0.3926(6) 0.1702(4) 0.1194(17) Uani 1 1 d D . . . .
H24A H 0.108169 0.321369 0.211274 0.143 Uiso 1 1 calc R . . . .
H24B H 0.134062 0.33491 0.128575 0.143 Uiso 1 1 calc R . . . .
C25 C 0.0561(3) 0.4660(9) 0.1416(6) 0.207(4) Uani 1 1 d D . . . .
H25A H 0.063973 0.533806 0.099657 0.31 Uiso 1 1 calc GR . . . .
H25B H 0.038547 0.522978 0.182668 0.31 Uiso 1 1 calc GR . . . .
H25C H 0.027268 0.387838 0.124342 0.31 Uiso 1 1 calc GR . . . .
C26 C 0.28907(17) 0.6683(4) 0.2188(2) 0.0684(9) Uani 1 1 d D . . . .
H26A H 0.251767 0.72601 0.204164 0.082 Uiso 1 1 calc R . . . .
H26B H 0.316796 0.735924 0.248402 0.082 Uiso 1 1 calc R . . . .
C27 C 0.3207(2) 0.6208(4) 0.1468(2) 0.0971(13) Uani 1 1 d D . . . .
H27A H 0.293194 0.552458 0.117252 0.117 Uiso 1 1 calc R . . . .
H27B H 0.358334 0.564456 0.161229 0.117 Uiso 1 1 calc R . . . .
C28 C 0.3375(3) 0.7542(4) 0.0967(3) 0.1138(17) Uani 1 1 d D . . . .
H28A H 0.29956 0.809052 0.081544 0.137 Uiso 1 1 calc R . . . .
H28B H 0.363965 0.823667 0.12684 0.137 Uiso 1 1 calc R . . . .
C29 C 0.3704(2) 0.7103(5) 0.0251(2) 0.0975(13) Uani 1 1 d D . . . .
H29A H 0.365841 0.790978 -0.012194 0.146 Uiso 1 1 calc GR . . . .
H29B H 0.352561 0.617706 0.00416 0.146 Uiso 1 1 calc GR . . . .
H29C H 0.413949 0.694277 0.03788 0.146 Uiso 1 1 calc GR . . . .
C30 C 0.32707(15) 0.4367(4) 0.2904(2) 0.0631(8) Uani 1 1 d . . . . .
H30A H 0.313711 0.35526 0.323834 0.076 Uiso 1 1 calc R . . . .
H30B H 0.340978 0.389283 0.243662 0.076 Uiso 1 1 calc R . . . .
C31 C 0.38193(17) 0.5164(4) 0.3295(2) 0.0795(10) Uani 1 1 d . . . . .
H31A H 0.37066 0.552775 0.379766 0.095 Uiso 1 1 calc R . . . .
H31B H 0.393862 0.604005 0.299189 0.095 Uiso 1 1 calc R . . . .
C32 C 0.43653(18) 0.4049(5) 0.3384(3) 0.0902(12) Uani 1 1 d . . . . .
H32A H 0.424424 0.318366 0.369371 0.108 Uiso 1 1 calc R . . . .
H32B H 0.446651 0.366574 0.28806 0.108 Uiso 1 1 calc R . . . .
C33 C 0.4936(2) 0.4802(7) 0.3759(4) 0.131(2) Uani 1 1 d . . . . .
H33A H 0.504819 0.568157 0.346399 0.197 Uiso 1 1 calc GR . . . .
H33B H 0.527665 0.408618 0.377935 0.197 Uiso 1 1 calc GR . . . .
H33C H 0.484699 0.511442 0.427202 0.197 Uiso 1 1 calc GR . . . .
Br1 Br 0.32397(2) -0.21890(4) 0.57867(2) 0.07113(17) Uani 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.218(3) . ?
N1 H1 0.86 . ?
N1 C1 1.390(4) . ?
N1 C11 1.376(4) . ?
N2 H2 0.86 . ?
N2 C11 1.356(4) . ?
N2 C12 1.404(4) . ?
C1 C2 1.361(5) . ?
C1 C10 1.437(4) . ?
C2 H2A 0.93 . ?
C2 C3 1.399(5) . ?
C3 H3 0.93 . ?
C3 C4 1.342(7) . ?
C4 H4 0.93 . ?
C4 C5 1.400(6) . ?
C5 C6 1.423(6) . ?
C5 C10 1.423(5) . ?
C6 H6 0.93 . ?
C6 C7 1.337(6) . ?
C7 H7 0.93 . ?
C7 C8 1.390(6) . ?
C8 H8 0.93 . ?
C8 C9 1.363(5) . ?
C9 H9 0.93 . ?
C9 C10 1.404(5) . ?
C12 C13 1.385(4) . ?
C12 C17 1.387(4) . ?
C13 H13 0.93 . ?
C13 C14 1.377(4) . ?
C14 H14 0.93 . ?
C14 C15 1.405(4) . ?
C15 C15 1.484(6) 2_655 ?
C15 C16 1.381(4) . ?
C16 H16 0.93 . ?
C16 C17 1.385(4) . ?
C17 H17 0.93 . ?
N3 C18 1.517(4) . ?
N3 C22 1.516(4) . ?
N3 C26 1.511(4) . ?
N3 C30 1.513(4) . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
C18 C19 1.528(5) . ?
C19 H19A 0.97 . ?
C19 H19B 0.97 . ?
C19 C20 1.516(5) . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C20 C21 1.501(5) . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 C23 1.516(5) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C23 C24 1.512(6) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 C25 1.513(4) . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C26 C27 1.507(5) . ?
C27 H27A 0.97 . ?
C27 H27B 0.97 . ?
C27 C28 1.5070(10) . ?
C28 H28A 0.97 . ?
C28 H28B 0.97 . ?
C28 C29 1.507(3) . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?
C30 H30A 0.97 . ?
C30 H30B 0.97 . ?
C30 C31 1.504(5) . ?
C31 H31A 0.97 . ?
C31 H31B 0.97 . ?
C31 C32 1.525(5) . ?
C32 H32A 0.97 . ?
C32 H32B 0.97 . ?
C32 C33 1.513(6) . ?
C33 H33A 0.96 . ?
C33 H33B 0.96 . ?
C33 H33C 0.96 . ?

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 H1 116.4 . . ?
C11 N1 H1 116.4 . . ?
C11 N1 C1 127.1(3) . . ?
C11 N2 H2 116.1 . . ?
C11 N2 C12 127.8(2) . . ?
C12 N2 H2 116.1 . . ?
N1 C1 C10 117.6(3) . . ?
C2 C1 N1 122.0(3) . . ?
C2 C1 C10 120.4(3) . . ?
C1 C2 H2A 119.8 . . ?
C1 C2 C3 120.4(4) . . ?
C3 C2 H2A 119.8 . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 121.0(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 122.5(4) . . ?
C4 C5 C10 119.6(4) . . ?
C6 C5 C10 117.9(4) . . ?
C5 C6 H6 119 . . ?
C7 C6 C5 122.1(4) . . ?
C7 C6 H6 119 . . ?
C6 C7 H7 120 . . ?
C6 C7 C8 120.0(4) . . ?
C8 C7 H7 120 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.5(4) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 119.3 . . ?
C8 C9 C10 121.5(3) . . ?
C10 C9 H9 119.3 . . ?
C5 C10 C1 117.5(3) . . ?
C9 C10 C1 124.4(3) . . ?
C9 C10 C5 118.1(3) . . ?
O1 C11 N1 123.6(3) . . ?
O1 C11 N2 123.9(3) . . ?
N2 C11 N1 112.5(3) . . ?
C13 C12 N2 117.0(2) . . ?
C13 C12 C17 118.3(3) . . ?
C17 C12 N2 124.6(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 C12 121.4(3) . . ?
C14 C13 H13 119.3 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.8(3) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C15 121.1(3) . 2_655 ?
C16 C15 C14 117.1(3) . . ?
C16 C15 C15 121.8(3) . 2_655 ?
C15 C16 H16 118.9 . . ?
C15 C16 C17 122.3(3) . . ?
C17 C16 H16 118.9 . . ?
C12 C17 H17 119.9 . . ?
C16 C17 C12 120.1(3) . . ?
C16 C17 H17 119.9 . . ?
C22 N3 C18 111.2(2) . . ?
C26 N3 C18 106.5(2) . . ?
C26 N3 C22 110.5(2) . . ?
C26 N3 C30 111.0(2) . . ?
C30 N3 C18 111.6(3) . . ?
C30 N3 C22 106.1(2) . . ?
N3 C18 H18A 108.5 . . ?
N3 C18 H18B 108.5 . . ?
N3 C18 C19 115.1(3) . . ?
H18A C18 H18B 107.5 . . ?
C19 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C18 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 C18 112.2(4) . . ?
C20 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C19 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C21 C20 C19 114.6(4) . . ?
C21 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 108.4 . . ?
N3 C22 H22B 108.4 . . ?
N3 C22 C23 115.4(3) . . ?
H22A C22 H22B 107.5 . . ?
C23 C22 H22A 108.4 . . ?
C23 C22 H22B 108.4 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108 . . ?
C24 C23 C22 111.2(3) . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C23 C24 H24A 109.1 . . ?
C23 C24 H24B 109.1 . . ?
C23 C24 C25 112.3(4) . . ?
H24A C24 H24B 107.9 . . ?
C25 C24 H24A 109.1 . . ?
C25 C24 H24B 109.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 H26A 108.7 . . ?
N3 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 N3 114.2(3) . . ?
C27 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
C26 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
C26 C27 C28 113.3(3) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C27 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 C27 114.4(3) . . ?
C29 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N3 C30 H30A 108.3 . . ?
N3 C30 H30B 108.3 . . ?
H30A C30 H30B 107.4 . . ?
C31 C30 N3 116.1(3) . . ?
C31 C30 H30A 108.3 . . ?
C31 C30 H30B 108.3 . . ?
C30 C31 H31A 109.8 . . ?
C30 C31 H31B 109.8 . . ?
C30 C31 C32 109.5(3) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
C31 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?
C33 C32 C31 111.7(4) . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 178.9(4) . . . . ?
N1 C1 C10 C5 -178.1(3) . . . . ?
N1 C1 C10 C9 1.4(5) . . . . ?
N2 C12 C13 C14 178.0(3) . . . . ?
N2 C12 C17 C16 -177.5(3) . . . . ?
C1 N1 C11 O1 1.6(5) . . . . ?
C1 N1 C11 N2 -179.3(3) . . . . ?
C1 C2 C3 C4 -0.6(8) . . . . ?
C2 C1 C10 C5 1.0(5) . . . . ?
C2 C1 C10 C9 -179.5(3) . . . . ?
C2 C3 C4 C5 0.5(9) . . . . ?
C3 C4 C5 C6 -179.9(6) . . . . ?
C3 C4 C5 C10 0.4(8) . . . . ?
C4 C5 C6 C7 -179.6(5) . . . . ?
C4 C5 C10 C1 -1.1(6) . . . . ?
C4 C5 C10 C9 179.3(4) . . . . ?
C5 C6 C7 C8 0.5(8) . . . . ?
C6 C5 C10 C1 179.2(4) . . . . ?
C6 C5 C10 C9 -0.4(6) . . . . ?
C6 C7 C8 C9 -0.8(7) . . . . ?
C7 C8 C9 C10 0.5(6) . . . . ?
C8 C9 C10 C1 -179.4(3) . . . . ?
C8 C9 C10 C5 0.1(5) . . . . ?
C10 C1 C2 C3 -0.1(6) . . . . ?
C10 C5 C6 C7 0.0(7) . . . . ?
C11 N1 C1 C2 21.7(5) . . . . ?
C11 N1 C1 C10 -159.3(3) . . . . ?
C11 N2 C12 C13 159.1(3) . . . . ?
C11 N2 C12 C17 -23.1(5) . . . . ?
C12 N2 C11 O1 4.9(5) . . . . ?
C12 N2 C11 N1 -174.2(3) . . . . ?
C12 C13 C14 C15 -0.5(5) . . . . ?
C13 C12 C17 C16 0.3(4) . . . . ?
C13 C14 C15 C15 -178.1(3) . . . 2_655 ?
C13 C14 C15 C16 0.7(5) . . . . ?
C14 C15 C16 C17 -0.4(4) . . . . ?
C15 C15 C16 C17 178.4(2) 2_655 . . . ?
C15 C16 C17 C12 -0.1(4) . . . . ?
C17 C12 C13 C14 0.0(5) . . . . ?
N3 C18 C19 C20 -171.8(3) . . . . ?
N3 C22 C23 C24 -170.5(4) . . . . ?
N3 C26 C27 C28 179.3(4) . . . . ?
N3 C30 C31 C32 -173.7(3) . . . . ?
C18 N3 C22 C23 58.9(4) . . . . ?
C18 N3 C26 C27 177.0(3) . . . . ?
C18 N3 C30 C31 -62.1(4) . . . . ?
C18 C19 C20 C21 66.9(6) . . . . ?
C22 N3 C18 C19 55.4(4) . . . . ?
C22 N3 C26 C27 -62.1(4) . . . . ?
C22 N3 C30 C31 176.7(3) . . . . ?
C22 C23 C24 C25 -179.3(5) . . . . ?
C26 N3 C18 C19 175.9(3) . . . . ?
C26 N3 C22 C23 -59.2(4) . . . . ?
C26 N3 C30 C31 56.6(4) . . . . ?
C26 C27 C28 C29 178.7(5) . . . . ?
C30 N3 C18 C19 -62.8(4) . . . . ?
C30 N3 C22 C23 -179.6(3) . . . . ?
C30 N3 C26 C27 55.2(4) . . . . ?
C30 C31 C32 C33 178.7(4) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylformamide'
####################################################################### 
# 
# 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_3-((TBA)AcO)2
_database_code_depnum_ccdc_archive 'CCDC 2015344'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-19T13:02:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C34 H26 N4 O2, 2(C16 H36 N), 2(C2 H3 O2)'
_chemical_formula_sum            'C70 H104 N6 O6'
_chemical_formula_weight         1125.59

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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

_cell_length_a                   10.0860(14)
_cell_length_b                   17.874(3)
_cell_length_c                   19.228(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.871(15)
_cell_angle_gamma                90
_cell_volume                     3415.0(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    2353
_cell_measurement_theta_min      4.5930
_cell_measurement_theta_max      24.3420

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.713
_exptl_crystal_size_mid          0.369
_exptl_crystal_size_min          0.305
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_F_000             1228

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.72835
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_number            19409
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.362
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             6697
_reflns_number_gt                3064
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1542P)²+0.1348P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6697
_refine_ls_number_parameters     395
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1640
_refine_ls_R_factor_gt           0.0814
_refine_ls_wR_factor_ref         0.2996
_refine_ls_wR_factor_gt          0.2284
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.038


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.4144(2) 0.43102(17) 0.39688(13) 0.1031(8) Uani 1 1 d . . . . .
N1 N 0.3655(3) 0.41996(15) 0.27701(15) 0.0806(8) Uani 1 1 d . . . . .
H1 H 0.398538 0.4306 0.239842 0.097 Uiso 1 1 calc R . . . .
N2 N 0.5801(3) 0.44119(14) 0.33091(14) 0.0753(7) Uani 1 1 d . . . . .
H2 H 0.59428 0.436889 0.288252 0.09 Uiso 1 1 calc R . . . .
C1 C 0.2317(3) 0.39429(17) 0.2652(2) 0.0785(9) Uani 1 1 d . . . . .
C2 C 0.1772(4) 0.36088(19) 0.3174(2) 0.0896(10) Uani 1 1 d . . . . .
H2A H 0.227141 0.356047 0.362586 0.108 Uiso 1 1 calc R . . . .
C3 C 0.0418(4) 0.3332(2) 0.3018(3) 0.1065(13) Uani 1 1 d . U . . .
H3 H 0.004138 0.310974 0.337543 0.128 Uiso 1 1 calc R . . . .
C4 C -0.0321(4) 0.3387(3) 0.2365(3) 0.1119(14) Uani 1 1 d . U . . .
H4 H -0.119506 0.320127 0.228084 0.134 Uiso 1 1 calc R . . . .
C5 C 0.0206(4) 0.3719(2) 0.1816(3) 0.1014(12) Uani 1 1 d . . . . .
C6 C -0.0546(5) 0.3772(3) 0.1136(4) 0.1279(17) Uani 1 1 d . . . . .
H6 H -0.141466 0.3579 0.104807 0.154 Uiso 1 1 calc R . . . .
C7 C -0.0051(7) 0.4091(3) 0.0611(4) 0.147(2) Uani 1 1 d . . . . .
H7 H -0.057475 0.412035 0.016428 0.176 Uiso 1 1 calc R . . . .
C8 C 0.1280(6) 0.4390(3) 0.0731(3) 0.1300(16) Uani 1 1 d . . . . .
H8 H 0.162814 0.460619 0.036127 0.156 Uiso 1 1 calc R . . . .
C9 C 0.2045(4) 0.4357(2) 0.1392(2) 0.1024(12) Uani 1 1 d . . . . .
H9 H 0.290514 0.456266 0.146946 0.123 Uiso 1 1 calc R . . . .
C10 C 0.1546(4) 0.40174(19) 0.1956(2) 0.0881(10) Uani 1 1 d . . . . .
C11 C 0.4499(3) 0.43021(18) 0.34006(19) 0.0750(9) Uani 1 1 d . . . . .
C12 C 0.6931(3) 0.45842(16) 0.38125(16) 0.0674(8) Uani 1 1 d . . . . .
C13 C 0.8174(3) 0.45538(18) 0.36000(17) 0.0785(9) Uani 1 1 d . . . . .
H13 H 0.821572 0.441947 0.313692 0.094 Uiso 1 1 calc R . . . .
C14 C 0.9356(3) 0.47168(18) 0.40545(17) 0.0758(9) Uani 1 1 d . . . . .
H14 H 1.016849 0.469121 0.388886 0.091 Uiso 1 1 calc R . . . .
C15 C 0.9358(3) 0.49183(15) 0.47542(15) 0.0640(7) Uani 1 1 d . . . . .
C16 C 0.8100(3) 0.49684(17) 0.49557(16) 0.0736(8) Uani 1 1 d . . . . .
H16 H 0.805673 0.512307 0.541302 0.088 Uiso 1 1 calc R . . . .
C17 C 0.6910(3) 0.47991(18) 0.45087(17) 0.0767(9) Uani 1 1 d . . . . .
H17 H 0.60956 0.482863 0.467235 0.092 Uiso 1 1 calc R . . . .
O2 O 0.5347(4) 0.4642(2) 0.17816(19) 0.1479(13) Uani 1 1 d . . . . .
O3 O 0.6069(4) 0.3554(2) 0.1735(3) 0.192(2) Uani 1 1 d . . . . .
C34 C 0.5727(6) 0.4259(4) 0.0693(2) 0.175(3) Uani 1 1 d . . . . .
H34A H 0.489629 0.448986 0.048114 0.262 Uiso 1 1 calc GR . . . .
H34B H 0.58246 0.378884 0.046495 0.262 Uiso 1 1 calc GR . . . .
H34C H 0.646516 0.458035 0.063999 0.262 Uiso 1 1 calc GR . . . .
C35 C 0.5719(4) 0.4128(2) 0.1462(2) 0.0888(10) Uani 1 1 d . . . . .
N3 N 0.5664(3) 0.67245(14) 0.26819(16) 0.0835(8) Uani 1 1 d . . . . .
C18 C 0.6622(3) 0.61764(18) 0.2433(2) 0.0885(10) Uani 1 1 d D . . . .
H18A H 0.700729 0.586788 0.283181 0.106 Uiso 1 1 calc R . . . .
H18B H 0.610315 0.584932 0.208612 0.106 Uiso 1 1 calc R . . . .
C19 C 0.7758(4) 0.6498(2) 0.2114(2) 0.1041(12) Uani 1 1 d D . . . .
H19A H 0.827748 0.683924 0.244709 0.125 Uiso 1 1 calc R . . . .
H19B H 0.739697 0.67774 0.1692 0.125 Uiso 1 1 calc R . . . .
C20 C 0.8679(5) 0.5869(3) 0.1927(3) 0.1382(18) Uani 1 1 d D . . . .
H20A H 0.906943 0.560866 0.235572 0.166 Uiso 1 1 calc R . . . .
H20B H 0.813863 0.551196 0.162041 0.166 Uiso 1 1 calc R . . . .
C21 C 0.9795(6) 0.6147(3) 0.1566(3) 0.171(2) Uani 1 1 d D . . . .
H21A H 0.942177 0.632911 0.110364 0.256 Uiso 1 1 calc GR . . . .
H21B H 1.040751 0.574506 0.152465 0.256 Uiso 1 1 calc GR . . . .
H21C H 1.026701 0.65451 0.183816 0.256 Uiso 1 1 calc GR . . . .
C22 C 0.4608(3) 0.62549(18) 0.2956(2) 0.0938(11) Uani 1 1 d . . . . .
H22A H 0.422094 0.591051 0.258632 0.113 Uiso 1 1 calc R . . . .
H22B H 0.505359 0.595797 0.334989 0.113 Uiso 1 1 calc R . . . .
C23 C 0.3474(4) 0.6686(2) 0.3194(3) 0.1119(14) Uani 1 1 d D . . . .
H23A H 0.384627 0.704876 0.354972 0.134 Uiso 1 1 calc R . . . .
H23B H 0.297333 0.695579 0.279643 0.134 Uiso 1 1 calc R . . . .
C24 C 0.2537(4) 0.6171(2) 0.3495(3) 0.1230(16) Uani 1 1 d D . . . .
H24A H 0.304383 0.590774 0.389578 0.148 Uiso 1 1 calc R . . . .
H24B H 0.219139 0.580063 0.314131 0.148 Uiso 1 1 calc R . . . .
C25 C 0.1361(5) 0.6566(3) 0.3731(3) 0.1399(18) Uani 1 1 d . . . . .
H25A H 0.083188 0.681262 0.333364 0.21 Uiso 1 1 calc GR . . . .
H25B H 0.169146 0.692906 0.408599 0.21 Uiso 1 1 calc GR . . . .
H25C H 0.081296 0.620643 0.39211 0.21 Uiso 1 1 calc GR . . . .
C26 C 0.6400(4) 0.72199(19) 0.3257(2) 0.0959(11) Uani 1 1 d . . . . .
H26A H 0.57568 0.756461 0.340332 0.115 Uiso 1 1 calc R . . . .
H26B H 0.705368 0.75149 0.306127 0.115 Uiso 1 1 calc R . . . .
C27 C 0.7122(5) 0.6816(3) 0.3906(3) 0.1245(15) Uani 1 1 d D . . . .
H27A H 0.648073 0.653072 0.412059 0.149 Uiso 1 1 calc R . . . .
H27B H 0.77786 0.64718 0.377279 0.149 Uiso 1 1 calc R . . . .
C28 C 0.7816(7) 0.7382(4) 0.4424(4) 0.167(2) Uani 1 1 d D . . . .
H28A H 0.715303 0.77409 0.452517 0.2 Uiso 0.65 1 calc R . P A 1
H28B H 0.84692 0.765174 0.420402 0.2 Uiso 0.65 1 calc R . P A 1
H28C H 0.868185 0.718181 0.464123 0.2 Uiso 0.35 1 calc R . P B 2
H28D H 0.798204 0.783005 0.416735 0.2 Uiso 0.35 1 calc R . P B 2
C29 C 0.8525(14) 0.7055(7) 0.5112(5) 0.206(5) Uani 0.65 1 d D . P C 1
H29A H 0.800051 0.714753 0.547525 0.309 Uiso 0.65 1 calc GR . P C 1
H29B H 0.939384 0.728298 0.523942 0.309 Uiso 0.65 1 calc GR . P C 1
H29C H 0.863041 0.652495 0.505877 0.309 Uiso 0.65 1 calc GR . P C 1
C29' C 0.7044(19) 0.7595(11) 0.4995(8) 0.195(9) Uani 0.35 1 d D . P C 2
H29D H 0.688717 0.715699 0.525882 0.292 Uiso 0.35 1 calc GR . P C 2
H29E H 0.619779 0.781153 0.478743 0.292 Uiso 0.35 1 calc GR . P C 2
H29F H 0.755385 0.795177 0.530514 0.292 Uiso 0.35 1 calc GR . P C 2
C30 C 0.5026(4) 0.7239(2) 0.2098(2) 0.0994(12) Uani 1 1 d . . . . .
H30A H 0.572896 0.753425 0.194498 0.119 Uiso 1 1 calc R . . . .
H30B H 0.443281 0.758166 0.228833 0.119 Uiso 1 1 calc R . . . .
C31 C 0.4225(6) 0.6850(3) 0.1458(3) 0.151(2) Uani 1 1 d . . . . .
H31A H 0.350097 0.656215 0.160002 0.181 Uiso 1 1 calc R . . . .
H31B H 0.480498 0.65089 0.125787 0.181 Uiso 1 1 calc R . . . .
C32 C 0.3642(9) 0.7428(5) 0.0906(5) 0.206(3) Uani 1 1 d D U . . .
H32A H 0.422895 0.786069 0.093505 0.247 Uiso 0.52 1 calc R . P D 1
H32B H 0.356754 0.721519 0.0437 0.247 Uiso 0.52 1 calc R . P D 1
H32C H 0.359444 0.790581 0.113962 0.247 Uiso 0.48 1 calc R . P E 2
H32D H 0.425557 0.748478 0.057265 0.247 Uiso 0.48 1 calc R . P E 2
C33 C 0.2268(16) 0.7658(9) 0.1043(12) 0.217(7) Uani 0.52 1 d D U P F 1
H33A H 0.16984 0.722579 0.102176 0.325 Uiso 0.52 1 calc GR . P F 1
H33B H 0.188004 0.801324 0.069153 0.325 Uiso 0.52 1 calc GR . P F 1
H33C H 0.235368 0.788222 0.150224 0.325 Uiso 0.52 1 calc GR . P F 1
C33' C 0.2267(14) 0.7243(12) 0.0503(9) 0.210(7) Uani 0.48 1 d D U P F 2
H33D H 0.235349 0.690585 0.012403 0.316 Uiso 0.48 1 calc GR . P F 2
H33E H 0.183068 0.769362 0.031254 0.316 Uiso 0.48 1 calc GR . P F 2
H33F H 0.17399 0.701056 0.081365 0.316 Uiso 0.48 1 calc GR . P F 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.207(4) . ?
N1 H1 0.86 . ?
N1 C1 1.406(4) . ?
N1 C11 1.369(4) . ?
N2 H2 0.86 . ?
N2 C11 1.368(4) . ?
N2 C12 1.398(4) . ?
C1 C2 1.363(5) . ?
C1 C10 1.434(5) . ?
C2 H2A 0.93 . ?
C2 C3 1.435(5) . ?
C3 H3 0.93 . ?
C3 C4 1.349(6) . ?
C4 H4 0.93 . ?
C4 C5 1.393(6) . ?
C5 C6 1.399(7) . ?
C5 C10 1.434(5) . ?
C6 H6 0.93 . ?
C6 C7 1.328(7) . ?
C7 H7 0.93 . ?
C7 C8 1.426(8) . ?
C8 H8 0.93 . ?
C8 C9 1.370(6) . ?
C9 H9 0.93 . ?
C9 C10 1.409(5) . ?
C12 C13 1.385(4) . ?
C12 C17 1.396(4) . ?
C13 H13 0.93 . ?
C13 C14 1.383(4) . ?
C14 H14 0.93 . ?
C14 C15 1.392(4) . ?
C15 C15 1.495(6) 3_766 ?
C15 C16 1.392(4) . ?
C16 H16 0.93 . ?
C16 C17 1.385(4) . ?
C17 H17 0.93 . ?
O2 C35 1.200(5) . ?
O3 C35 1.179(5) . ?
C34 H34A 0.96 . ?
C34 H34B 0.96 . ?
C34 H34C 0.96 . ?
C34 C35 1.498(6) . ?
N3 C18 1.511(4) . ?
N3 C22 1.519(4) . ?
N3 C26 1.509(4) . ?
N3 C30 1.507(4) . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
C18 C19 1.503(4) . ?
C19 H19A 0.97 . ?
C19 H19B 0.97 . ?
C19 C20 1.540(5) . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C20 C21 1.505(5) . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 C23 1.514(5) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C23 C24 1.504(4) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 C25 1.515(5) . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C26 C27 1.514(6) . ?
C27 H27A 0.97 . ?
C27 H27B 0.97 . ?
C27 C28 1.505(6) . ?
C28 H28A 0.97 . ?
C28 H28B 0.97 . ?
C28 H28C 0.97 . ?
C28 H28D 0.97 . ?
C28 C29 1.510(5) . ?
C28 C29' 1.500(9) . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?
C29' H29D 0.96 . ?
C29' H29E 0.96 . ?
C29' H29F 0.96 . ?
C30 H30A 0.97 . ?
C30 H30B 0.97 . ?
C30 C31 1.519(6) . ?
C31 H31A 0.97 . ?
C31 H31B 0.97 . ?
C31 C32 1.524(8) . ?
C32 H32A 0.97 . ?
C32 H32B 0.97 . ?
C32 H32C 0.97 . ?
C32 H32D 0.97 . ?
C32 C33 1.511(6) . ?
C32 C33' 1.505(8) . ?
C33 H33A 0.96 . ?
C33 H33B 0.96 . ?
C33 H33C 0.96 . ?
C33' H33D 0.96 . ?
C33' H33E 0.96 . ?
C33' H33F 0.96 . ?

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 H1 115.8 . . ?
C11 N1 H1 115.8 . . ?
C11 N1 C1 128.4(3) . . ?
C11 N2 H2 115.5 . . ?
C11 N2 C12 129.0(3) . . ?
C12 N2 H2 115.5 . . ?
N1 C1 C10 118.2(3) . . ?
C2 C1 N1 121.4(4) . . ?
C2 C1 C10 120.4(3) . . ?
C1 C2 H2A 120.5 . . ?
C1 C2 C3 119.1(4) . . ?
C3 C2 H2A 120.5 . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.6(4) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 120.9(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 121.4(5) . . ?
C4 C5 C10 119.1(4) . . ?
C6 C5 C10 119.5(5) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 C5 121.7(6) . . ?
C7 C6 H6 119.2 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.2(6) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 120 . . ?
C9 C8 C7 119.9(5) . . ?
C9 C8 H8 120 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.9(5) . . ?
C10 C9 H9 119.6 . . ?
C1 C10 C5 118.9(4) . . ?
C9 C10 C1 123.3(4) . . ?
C9 C10 C5 117.7(4) . . ?
O1 C11 N1 124.5(3) . . ?
O1 C11 N2 123.7(3) . . ?
N2 C11 N1 111.7(3) . . ?
C13 C12 N2 117.3(3) . . ?
C13 C12 C17 117.2(3) . . ?
C17 C12 N2 125.4(3) . . ?
C12 C13 H13 119 . . ?
C14 C13 C12 122.1(3) . . ?
C14 C13 H13 119 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.6(3) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C15 121.3(3) . 3_766 ?
C16 C15 C14 115.8(3) . . ?
C16 C15 C15 122.9(3) . 3_766 ?
C15 C16 H16 118.4 . . ?
C17 C16 C15 123.2(3) . . ?
C17 C16 H16 118.4 . . ?
C12 C17 H17 120 . . ?
C16 C17 C12 120.1(3) . . ?
C16 C17 H17 120 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
O2 C35 C34 116.2(5) . . ?
O3 C35 O2 122.3(5) . . ?
O3 C35 C34 121.5(5) . . ?
C18 N3 C22 106.0(2) . . ?
C26 N3 C18 110.6(3) . . ?
C26 N3 C22 110.8(3) . . ?
C30 N3 C18 112.0(3) . . ?
C30 N3 C22 111.1(3) . . ?
C30 N3 C26 106.4(3) . . ?
N3 C18 H18A 108 . . ?
N3 C18 H18B 108 . . ?
H18A C18 H18B 107.3 . . ?
C19 C18 N3 117.1(3) . . ?
C19 C18 H18A 108 . . ?
C19 C18 H18B 108 . . ?
C18 C19 H19A 109.6 . . ?
C18 C19 H19B 109.6 . . ?
C18 C19 C20 110.4(3) . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 C19 113.3(4) . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 108.3 . . ?
N3 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N3 115.8(3) . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108 . . ?
C24 C23 C22 111.2(3) . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C23 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
C23 C24 C25 113.9(3) . . ?
H24A C24 H24B 107.7 . . ?
C25 C24 H24A 108.8 . . ?
C25 C24 H24B 108.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C26 H26A 108.4 . . ?
N3 C26 H26B 108.4 . . ?
N3 C26 C27 115.5(3) . . ?
H26A C26 H26B 107.5 . . ?
C27 C26 H26A 108.4 . . ?
C27 C26 H26B 108.4 . . ?
C26 C27 H27A 109.9 . . ?
C26 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C28 C27 C26 109.1(4) . . ?
C28 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
C27 C28 H28A 108.6 . . ?
C27 C28 H28B 108.6 . . ?
C27 C28 H28C 108.6 . . ?
C27 C28 H28D 108.6 . . ?
C27 C28 C29 114.6(7) . . ?
H28A C28 H28B 107.6 . . ?
H28C C28 H28D 107.6 . . ?
C29 C28 H28A 108.6 . . ?
C29 C28 H28B 108.6 . . ?
C29' C28 C27 114.5(9) . . ?
C29' C28 H28C 108.6 . . ?
C29' C28 H28D 108.6 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C29' H29D 109.5 . . ?
C28 C29' H29E 109.5 . . ?
C28 C29' H29F 109.5 . . ?
H29D C29' H29E 109.5 . . ?
H29D C29' H29F 109.5 . . ?
H29E C29' H29F 109.5 . . ?
N3 C30 H30A 108.5 . . ?
N3 C30 H30B 108.5 . . ?
N3 C30 C31 115.1(3) . . ?
H30A C30 H30B 107.5 . . ?
C31 C30 H30A 108.5 . . ?
C31 C30 H30B 108.5 . . ?
C30 C31 H31A 109.7 . . ?
C30 C31 H31B 109.7 . . ?
C30 C31 C32 110.0(5) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C31 C32 H32A 110 . . ?
C31 C32 H32B 110 . . ?
C31 C32 H32C 108.5 . . ?
C31 C32 H32D 108.5 . . ?
H32A C32 H32B 108.3 . . ?
H32C C32 H32D 107.5 . . ?
C33 C32 C31 108.6(10) . . ?
C33 C32 H32A 110 . . ?
C33 C32 H32B 110 . . ?
C33' C32 C31 114.9(9) . . ?
C33' C32 H32C 108.5 . . ?
C33' C32 H32D 108.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33' H33D 109.5 . . ?
C32 C33' H33E 109.5 . . ?
C32 C33' H33F 109.5 . . ?
H33D C33' H33E 109.5 . . ?
H33D C33' H33F 109.5 . . ?
H33E C33' H33F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -177.7(3) . . . . ?
N1 C1 C10 C5 176.4(3) . . . . ?
N1 C1 C10 C9 -2.3(5) . . . . ?
N2 C12 C13 C14 179.7(3) . . . . ?
N2 C12 C17 C16 -178.9(3) . . . . ?
C1 N1 C11 O1 -13.8(5) . . . . ?
C1 N1 C11 N2 167.6(3) . . . . ?
C1 C2 C3 C4 0.8(5) . . . . ?
C2 C1 C10 C5 -1.4(5) . . . . ?
C2 C1 C10 C9 179.9(3) . . . . ?
C2 C3 C4 C5 -0.2(6) . . . . ?
C3 C4 C5 C6 179.3(4) . . . . ?
C3 C4 C5 C10 -1.2(6) . . . . ?
C4 C5 C6 C7 179.7(5) . . . . ?
C4 C5 C10 C1 2.0(5) . . . . ?
C4 C5 C10 C9 -179.3(4) . . . . ?
C5 C6 C7 C8 0.2(8) . . . . ?
C6 C5 C10 C1 -178.5(3) . . . . ?
C6 C5 C10 C9 0.3(5) . . . . ?
C6 C7 C8 C9 -1.0(8) . . . . ?
C7 C8 C9 C10 1.4(7) . . . . ?
C8 C9 C10 C1 177.7(3) . . . . ?
C8 C9 C10 C5 -1.0(5) . . . . ?
C10 C1 C2 C3 0.1(5) . . . . ?
C10 C5 C6 C7 0.1(7) . . . . ?
C11 N1 C1 C2 -14.1(5) . . . . ?
C11 N1 C1 C10 168.1(3) . . . . ?
C11 N2 C12 C13 170.3(3) . . . . ?
C11 N2 C12 C17 -11.0(5) . . . . ?
C12 N2 C11 O1 -3.3(5) . . . . ?
C12 N2 C11 N1 175.3(3) . . . . ?
C12 C13 C14 C15 0.3(5) . . . . ?
C13 C12 C17 C16 -0.2(4) . . . . ?
C13 C14 C15 C15 179.0(3) . . . 3_766 ?
C13 C14 C15 C16 -2.1(4) . . . . ?
C14 C15 C16 C17 2.8(4) . . . . ?
C15 C15 C16 C17 -178.3(3) 3_766 . . . ?
C15 C16 C17 C12 -1.7(5) . . . . ?
C17 C12 C13 C14 0.9(5) . . . . ?
N3 C18 C19 C20 176.9(4) . . . . ?
N3 C22 C23 C24 -176.5(4) . . . . ?
N3 C26 C27 C28 179.3(4) . . . . ?
N3 C30 C31 C32 -179.6(5) . . . . ?
C18 N3 C22 C23 -176.3(4) . . . . ?
C18 N3 C26 C27 -58.3(4) . . . . ?
C18 N3 C30 C31 59.1(4) . . . . ?
C18 C19 C20 C21 176.6(5) . . . . ?
C22 N3 C18 C19 178.4(3) . . . . ?
C22 N3 C26 C27 59.0(4) . . . . ?
C22 N3 C30 C31 -59.3(5) . . . . ?
C22 C23 C24 C25 -178.8(4) . . . . ?
C26 N3 C18 C19 -61.4(4) . . . . ?
C26 N3 C22 C23 63.7(4) . . . . ?
C26 N3 C30 C31 180.0(4) . . . . ?
C26 C27 C28 C29 177.3(8) . . . . ?
C26 C27 C28 C29' 97.3(10) . . . . ?
C30 N3 C18 C19 57.1(4) . . . . ?
C30 N3 C22 C23 -54.3(4) . . . . ?
C30 N3 C26 C27 179.8(3) . . . . ?
C30 C31 C32 C33 -90.1(11) . . . . ?
C30 C31 C32 C33' -143.9(12) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
####################################################################### 
# 
# 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_2-((TBA)Br)2
_database_code_depnum_ccdc_archive 'CCDC 2015342'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T17:25:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C26 H20 N6 O6, 2(C16 H36 N), 2(Br)'
_chemical_formula_sum            'C58 H92 Br2 N8 O6'
_chemical_formula_weight         1157.21

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9775(4)
_cell_length_b                   10.0854(5)
_cell_length_c                   20.0463(10)
_cell_angle_alpha                101.107(4)
_cell_angle_beta                 96.410(4)
_cell_angle_gamma                93.701(4)
_cell_volume                     1566.61(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    3486
_cell_measurement_theta_min      4.6490
_cell_measurement_theta_max      25.5380

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.839
_exptl_crystal_size_mid          0.564
_exptl_crystal_size_min          0.136
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             614

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.61579
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_number            14947
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.272
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             6138
_reflns_number_gt                4615
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+0.4474P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6138
_refine_ls_number_parameters     338
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.042


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.01446(4) 1.23667(3) 0.17534(2) 0.06409(12) Uani 1 1 d . . . . .
O1 O 0.1567(3) 0.83383(19) 0.28214(10) 0.0736(6) Uani 1 1 d . . . . .
O2 O 0.1893(4) 1.2159(3) 0.61039(13) 0.1054(9) Uani 1 1 d . . . . .
O3 O 0.1481(3) 1.4087(3) 0.58430(13) 0.1004(8) Uani 1 1 d . . . . .
N1 N 0.0993(3) 1.0552(2) 0.28887(11) 0.0564(6) Uani 1 1 d . . . . .
H1 H 0.073765 1.112707 0.263633 0.068 Uiso 1 1 calc R . . . .
N2 N 0.0842(3) 0.91374(19) 0.18500(11) 0.0506(5) Uani 1 1 d . . . . .
H2 H 0.073373 0.987812 0.170317 0.061 Uiso 1 1 calc R . . . .
N3 N 0.1622(3) 1.2876(4) 0.56842(15) 0.0789(8) Uani 1 1 d . . . . .
C1 C 0.1181(3) 1.1053(2) 0.35858(13) 0.0508(6) Uani 1 1 d . . . . .
C2 C 0.0973(3) 1.2426(3) 0.37949(14) 0.0570(7) Uani 1 1 d . . . . .
H2A H 0.073544 1.294995 0.346759 0.068 Uiso 1 1 calc R . . . .
C3 C 0.1116(4) 1.3013(3) 0.44775(15) 0.0638(7) Uani 1 1 d . . . . .
H3 H 0.096161 1.392732 0.461297 0.077 Uiso 1 1 calc R . . . .
C4 C 0.1487(3) 1.2244(3) 0.49564(14) 0.0608(7) Uani 1 1 d . . . . .
C5 C 0.1713(4) 1.0893(3) 0.47677(15) 0.0688(8) Uani 1 1 d . . . . .
H5 H 0.196773 1.038489 0.510062 0.083 Uiso 1 1 calc R . . . .
C6 C 0.1561(4) 1.0293(3) 0.40842(15) 0.0664(8) Uani 1 1 d . . . . .
H6 H 0.171316 0.937633 0.395508 0.08 Uiso 1 1 calc R . . . .
C7 C 0.1158(3) 0.9257(2) 0.25396(14) 0.0511(6) Uani 1 1 d . . . . .
C8 C 0.0672(3) 0.7933(2) 0.13493(13) 0.0447(5) Uani 1 1 d . . . . .
C9 C 0.0767(4) 0.8038(2) 0.06789(14) 0.0610(7) Uani 1 1 d . . . . .
H9 H 0.100484 0.888715 0.057776 0.073 Uiso 1 1 calc R . . . .
C10 C 0.0517(4) 0.6905(3) 0.01532(14) 0.0628(7) Uani 1 1 d . . . . .
H10 H 0.059145 0.700781 -0.029397 0.075 Uiso 1 1 calc R . . . .
C11 C 0.0154(3) 0.5612(2) 0.02802(12) 0.0444(5) Uani 1 1 d . . . . .
C12 C 0.0083(3) 0.5531(2) 0.09627(12) 0.0454(6) Uani 1 1 d . . . . .
H12 H -0.01429 0.468437 0.106838 0.054 Uiso 1 1 calc R . . . .
C13 C 0.0334(3) 0.6657(2) 0.14874(13) 0.0466(6) Uani 1 1 d . . . . .
H13 H 0.027673 0.655903 0.193633 0.056 Uiso 1 1 calc R . . . .
N4 N 0.4989(2) 0.4896(2) 0.23018(11) 0.0538(5) Uani 1 1 d . . . . .
C14 C 0.6088(3) 0.6135(3) 0.22357(16) 0.0613(7) Uani 1 1 d . . . . .
H14A H 0.698039 0.583536 0.1966 0.074 Uiso 1 1 calc R . . . .
H14B H 0.662299 0.657935 0.268912 0.074 Uiso 1 1 calc R . . . .
C15 C 0.5176(4) 0.7170(3) 0.19106(18) 0.0695(8) Uani 1 1 d . . . . .
H15A H 0.45896 0.673099 0.146479 0.083 Uiso 1 1 calc R . . . .
H15B H 0.433863 0.753325 0.219446 0.083 Uiso 1 1 calc R . . . .
C16 C 0.6410(4) 0.8316(3) 0.1830(2) 0.0854(10) Uani 1 1 d . . . . .
H16A H 0.701802 0.87315 0.227524 0.102 Uiso 1 1 calc R . . . .
H16B H 0.723202 0.794759 0.153894 0.102 Uiso 1 1 calc R . . . .
C17 C 0.5558(5) 0.9386(4) 0.1525(2) 0.0963(11) Uani 1 1 d . . . . .
H17A H 0.494651 0.898049 0.108496 0.144 Uiso 1 1 calc GR . . . .
H17B H 0.639638 1.007181 0.147208 0.144 Uiso 1 1 calc GR . . . .
H17C H 0.478535 0.978866 0.182233 0.144 Uiso 1 1 calc GR . . . .
C18 C 0.3578(3) 0.5313(3) 0.27291(15) 0.0573(7) Uani 1 1 d . . . . .
H18A H 0.288527 0.588953 0.250036 0.069 Uiso 1 1 calc R . . . .
H18B H 0.286542 0.450541 0.274351 0.069 Uiso 1 1 calc R . . . .
C19 C 0.4158(4) 0.6052(3) 0.34526(16) 0.0700(8) Uani 1 1 d . . . . .
H19A H 0.472585 0.692785 0.344529 0.084 Uiso 1 1 calc R . . . .
H19B H 0.496786 0.553762 0.366854 0.084 Uiso 1 1 calc R . . . .
C20 C 0.2703(4) 0.6256(3) 0.38688(17) 0.0719(8) Uani 1 1 d . . . . .
H20A H 0.210788 0.538154 0.385838 0.086 Uiso 1 1 calc R . . . .
H20B H 0.191674 0.679942 0.366107 0.086 Uiso 1 1 calc R . . . .
C21 C 0.3266(5) 0.6948(5) 0.4607(2) 0.1084(13) Uani 1 1 d . . . . .
H21A H 0.386727 0.781092 0.46211 0.163 Uiso 1 1 calc GR . . . .
H21B H 0.399544 0.639136 0.482327 0.163 Uiso 1 1 calc GR . . . .
H21C H 0.229154 0.708139 0.484529 0.163 Uiso 1 1 calc GR . . . .
C22 C 0.6141(3) 0.4008(3) 0.26449(15) 0.0604(7) Uani 1 1 d . . . . .
H22A H 0.692994 0.366856 0.23316 0.073 Uiso 1 1 calc R . . . .
H22B H 0.679852 0.457354 0.304724 0.073 Uiso 1 1 calc R . . . .
C23 C 0.5276(4) 0.2816(3) 0.28607(18) 0.0739(9) Uani 1 1 d . . . . .
H23A H 0.46559 0.221113 0.246185 0.089 Uiso 1 1 calc R . . . .
H23B H 0.447475 0.313166 0.317294 0.089 Uiso 1 1 calc R . . . .
C24 C 0.6576(4) 0.2057(4) 0.32101(19) 0.0869(10) Uani 1 1 d D . . . .
H24A H 0.731513 0.168862 0.288127 0.104 Uiso 1 1 calc R . . . .
H24B H 0.72662 0.269563 0.357736 0.104 Uiso 1 1 calc R . . . .
C25 C 0.5828(6) 0.0919(4) 0.3502(2) 0.1109(13) Uani 1 1 d D . . . .
H25A H 0.505616 0.032657 0.315251 0.166 Uiso 1 1 calc GR . . . .
H25B H 0.523141 0.128713 0.387604 0.166 Uiso 1 1 calc GR . . . .
H25C H 0.671751 0.041875 0.366318 0.166 Uiso 1 1 calc GR . . . .
C26 C 0.4148(3) 0.4129(3) 0.16042(15) 0.0603(7) Uani 1 1 d . . . . .
H26A H 0.351748 0.331692 0.166776 0.072 Uiso 1 1 calc R . . . .
H26B H 0.333741 0.468967 0.142508 0.072 Uiso 1 1 calc R . . . .
C27 C 0.5319(4) 0.3714(4) 0.10702(18) 0.0920(12) Uani 1 1 d . . . . .
H27A H 0.608292 0.309624 0.122735 0.11 Uiso 1 1 calc R . . . .
H27B H 0.59955 0.451117 0.10158 0.11 Uiso 1 1 calc R . . . .
C28 C 0.4336(5) 0.3023(4) 0.0374(2) 0.0992(12) Uani 1 1 d D . . . .
H28A H 0.346332 0.35875 0.024735 0.119 Uiso 1 1 calc R . . . .
H28B H 0.510306 0.293923 0.002816 0.119 Uiso 1 1 calc R . . . .
C29 C 0.3532(7) 0.1643(5) 0.0387(3) 0.1412(19) Uani 1 1 d D . . . .
H29A H 0.300209 0.122067 -0.006451 0.212 Uiso 1 1 calc GR . . . .
H29B H 0.269514 0.172887 0.06981 0.212 Uiso 1 1 calc GR . . . .
H29C H 0.438345 0.109521 0.053546 0.212 Uiso 1 1 calc GR . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7 1.218(3) . ?
O2 N3 1.221(4) . ?
O3 N3 1.217(4) . ?
N1 H1 0.86 . ?
N1 C1 1.379(3) . ?
N1 C7 1.379(3) . ?
N2 H2 0.86 . ?
N2 C7 1.358(3) . ?
N2 C8 1.407(3) . ?
N3 C4 1.464(4) . ?
C1 C2 1.393(3) . ?
C1 C6 1.392(4) . ?
C2 H2A 0.93 . ?
C2 C3 1.371(4) . ?
C3 H3 0.93 . ?
C3 C4 1.365(4) . ?
C4 C5 1.371(4) . ?
C5 H5 0.93 . ?
C5 C6 1.376(4) . ?
C6 H6 0.93 . ?
C8 C9 1.379(4) . ?
C8 C13 1.383(3) . ?
C9 H9 0.93 . ?
C9 C10 1.384(4) . ?
C10 H10 0.93 . ?
C10 C11 1.395(3) . ?
C11 C11 1.487(4) 2_565 ?
C11 C12 1.393(3) . ?
C12 H12 0.93 . ?
C12 C13 1.378(3) . ?
C13 H13 0.93 . ?
N4 C14 1.515(3) . ?
N4 C18 1.522(3) . ?
N4 C22 1.524(3) . ?
N4 C26 1.520(3) . ?
C14 H14A 0.97 . ?
C14 H14B 0.97 . ?
C14 C15 1.516(4) . ?
C15 H15A 0.97 . ?
C15 H15B 0.97 . ?
C15 C16 1.515(4) . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C16 C17 1.502(5) . ?
C17 H17A 0.96 . ?
C17 H17B 0.96 . ?
C17 H17C 0.96 . ?
C18 H18A 0.97 . ?
C18 H18B 0.97 . ?
C18 C19 1.504(4) . ?
C19 H19A 0.97 . ?
C19 H19B 0.97 . ?
C19 C20 1.505(4) . ?
C20 H20A 0.97 . ?
C20 H20B 0.97 . ?
C20 C21 1.514(5) . ?
C21 H21A 0.96 . ?
C21 H21B 0.96 . ?
C21 H21C 0.96 . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 C23 1.506(4) . ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C23 C24 1.516(4) . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 C25 1.504(5) . ?
C25 H25A 0.96 . ?
C25 H25B 0.96 . ?
C25 H25C 0.96 . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C26 C27 1.515(4) . ?
C27 H27A 0.97 . ?
C27 H27B 0.97 . ?
C27 C28 1.535(5) . ?
C28 H28A 0.97 . ?
C28 H28B 0.97 . ?
C28 C29 1.501(5) . ?
C29 H29A 0.96 . ?
C29 H29B 0.96 . ?
C29 H29C 0.96 . ?

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 H1 115.5 . . ?
C1 N1 C7 129.1(2) . . ?
C7 N1 H1 115.5 . . ?
C7 N2 H2 116.5 . . ?
C7 N2 C8 127.1(2) . . ?
C8 N2 H2 116.5 . . ?
O2 N3 C4 118.1(3) . . ?
O3 N3 O2 123.1(3) . . ?
O3 N3 C4 118.8(3) . . ?
N1 C1 C2 116.5(2) . . ?
N1 C1 C6 124.8(2) . . ?
C6 C1 C2 118.6(3) . . ?
C1 C2 H2A 119.6 . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2A 119.6 . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 N3 119.1(3) . . ?
C3 C4 C5 121.2(3) . . ?
C5 C4 N3 119.7(3) . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.8(3) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
O1 C7 N1 123.5(2) . . ?
O1 C7 N2 124.3(2) . . ?
N2 C7 N1 112.2(2) . . ?
C9 C8 N2 118.0(2) . . ?
C9 C8 C13 118.3(2) . . ?
C13 C8 N2 123.7(2) . . ?
C8 C9 H9 119.4 . . ?
C8 C9 C10 121.3(2) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 119.3 . . ?
C9 C10 C11 121.4(3) . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C11 122.0(3) . 2_565 ?
C12 C11 C10 116.2(2) . . ?
C12 C11 C11 121.8(3) . 2_565 ?
C11 C12 H12 118.7 . . ?
C13 C12 C11 122.6(2) . . ?
C13 C12 H12 118.7 . . ?
C8 C13 H13 119.8 . . ?
C12 C13 C8 120.3(2) . . ?
C12 C13 H13 119.8 . . ?
C14 N4 C18 110.39(19) . . ?
C14 N4 C22 106.86(19) . . ?
C14 N4 C26 111.1(2) . . ?
C18 N4 C22 110.8(2) . . ?
C26 N4 C18 107.03(18) . . ?
C26 N4 C22 110.78(19) . . ?
N4 C14 H14A 108.4 . . ?
N4 C14 H14B 108.4 . . ?
N4 C14 C15 115.5(2) . . ?
H14A C14 H14B 107.5 . . ?
C15 C14 H14A 108.4 . . ?
C15 C14 H14B 108.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108 . . ?
C16 C15 C14 110.9(2) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C15 C16 H16A 109 . . ?
C15 C16 H16B 109 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 C15 112.9(3) . . ?
C17 C16 H16A 109 . . ?
C17 C16 H16B 109 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 108.5 . . ?
N4 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C19 C18 N4 115.2(2) . . ?
C19 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C18 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
C18 C19 C20 111.9(2) . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C19 C20 H20A 109 . . ?
C19 C20 H20B 109 . . ?
C19 C20 C21 112.8(3) . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 H20A 109 . . ?
C21 C20 H20B 109 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 108.2 . . ?
N4 C22 H22B 108.2 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N4 116.2(2) . . ?
C23 C22 H22A 108.2 . . ?
C23 C22 H22B 108.2 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
C22 C23 C24 110.1(3) . . ?
H23A C23 H23B 108.2 . . ?
C24 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C23 C24 H24A 108.7 . . ?
C23 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C25 C24 C23 114.2(3) . . ?
C25 C24 H24A 108.7 . . ?
C25 C24 H24B 108.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N4 C26 H26A 108.2 . . ?
N4 C26 H26B 108.2 . . ?
H26A C26 H26B 107.4 . . ?
C27 C26 N4 116.2(2) . . ?
C27 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
C26 C27 H27A 109.2 . . ?
C26 C27 H27B 109.2 . . ?
C26 C27 C28 112.0(3) . . ?
H27A C27 H27B 107.9 . . ?
C28 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
C27 C28 H28A 109.2 . . ?
C27 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 C27 112.2(4) . . ?
C29 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 N3 C4 C3 177.4(3) . . . . ?
O2 N3 C4 C5 -1.8(4) . . . . ?
O3 N3 C4 C3 -3.6(4) . . . . ?
O3 N3 C4 C5 177.2(3) . . . . ?
N1 C1 C2 C3 179.2(2) . . . . ?
N1 C1 C6 C5 -179.7(3) . . . . ?
N2 C8 C9 C10 -176.3(3) . . . . ?
N2 C8 C13 C12 176.0(2) . . . . ?
N3 C4 C5 C6 179.0(3) . . . . ?
C1 N1 C7 O1 -2.4(5) . . . . ?
C1 N1 C7 N2 178.7(2) . . . . ?
C1 C2 C3 C4 0.8(4) . . . . ?
C2 C1 C6 C5 0.5(4) . . . . ?
C2 C3 C4 N3 -179.4(3) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C4 C5 C6 C1 0.0(5) . . . . ?
C6 C1 C2 C3 -0.9(4) . . . . ?
C7 N1 C1 C2 178.6(3) . . . . ?
C7 N1 C1 C6 -1.2(4) . . . . ?
C7 N2 C8 C9 -164.3(3) . . . . ?
C7 N2 C8 C13 18.9(4) . . . . ?
C8 N2 C7 O1 10.3(4) . . . . ?
C8 N2 C7 N1 -170.7(2) . . . . ?
C8 C9 C10 C11 0.1(5) . . . . ?
C9 C8 C13 C12 -0.8(4) . . . . ?
C9 C10 C11 C11 178.7(3) . . . 2_565 ?
C9 C10 C11 C12 -0.8(4) . . . . ?
C10 C11 C12 C13 0.7(4) . . . . ?
C11 C11 C12 C13 -178.8(3) 2_565 . . . ?
C11 C12 C13 C8 0.1(4) . . . . ?
C13 C8 C9 C10 0.7(4) . . . . ?
N4 C14 C15 C16 -176.4(3) . . . . ?
N4 C18 C19 C20 -172.0(2) . . . . ?
N4 C22 C23 C24 -178.4(3) . . . . ?
N4 C26 C27 C28 -176.6(3) . . . . ?
C14 N4 C18 C19 -61.0(3) . . . . ?
C14 N4 C22 C23 171.1(2) . . . . ?
C14 N4 C26 C27 54.5(3) . . . . ?
C14 C15 C16 C17 -178.6(3) . . . . ?
C18 N4 C14 C15 -58.8(3) . . . . ?
C18 N4 C22 C23 50.8(3) . . . . ?
C18 N4 C26 C27 175.1(3) . . . . ?
C18 C19 C20 C21 177.7(3) . . . . ?
C22 N4 C14 C15 -179.4(2) . . . . ?
C22 N4 C18 C19 57.2(3) . . . . ?
C22 N4 C26 C27 -64.1(3) . . . . ?
C22 C23 C24 C25 174.8(3) . . . . ?
C26 N4 C14 C15 59.7(3) . . . . ?
C26 N4 C18 C19 178.0(2) . . . . ?
C26 N4 C22 C23 -67.8(3) . . . . ?
C26 C27 C28 C29 -70.1(5) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dimethyl sulfoxide'
####################################################################### 
# 
# 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_(2)2-(TBA)2HPO4
_database_code_depnum_ccdc_archive 'CCDC 2015343'
loop_
_audit_author_name
_audit_author_address
'Mario Cetina'
;Department of Applied Chemistry, Facutly of Textile Technology, University of Zagreb
Croatia
;
_audit_update_record             
;
2020-07-09 deposited with the CCDC.	2020-08-18 downloaded from the CCDC.
;

_audit_creation_date             2020-04-18T18:56:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_shelx_SHELXL_version_number     2018/3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         '2(C26 H20 N6 O6), 2(C16 H36 N), H O4 P'
_chemical_formula_sum            'C84 H113 N14 O16 P'
_chemical_formula_weight         1605.85

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.8036(8)
_cell_length_b                   18.2461(10)
_cell_length_c                   18.3745(9)
_cell_angle_alpha                81.787(4)
_cell_angle_beta                 83.628(4)
_cell_angle_gamma                70.879(5)
_cell_volume                     4317.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(1)
_cell_measurement_reflns_used    6008
_cell_measurement_theta_min      4.4380
_cell_measurement_theta_max      29.5660

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.656
_exptl_crystal_size_mid          0.364
_exptl_crystal_size_min          0.240
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             1716

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.77868
_exptl_absorpt_correction_T_max  1.00000

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_ambient_temperature      295(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_number            39563
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         4.211
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_Friedel_coverage         0
_reflns_number_total             16919
_reflns_number_gt                8741
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2006)'
_computing_publication_material  
'OLEX2 (Dolomanov et al., 2009) & WinGX (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1755P)²+0.9712P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         16919
_refine_ls_number_parameters     1071
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.1649
_refine_ls_R_factor_gt           0.0915
_refine_ls_wR_factor_ref         0.3163
_refine_ls_wR_factor_gt          0.2562
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.052
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.060

# start Validation Reply Form
_vrf_PLAT910_2~2~-TBA~2~HPO~4~   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         75 Note  
RESPONSE: Reflections were not omitted from the final least-squares refinement.
The unit cell is a bit large, but due to very weakly diffracting crystal
detector distance was set to lower limit.
;
# end Validation Reply Form

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

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 -0.5090(2) 0.60340(16) 0.3817(2) 0.0810(10) Uani 1 1 d . . . . .
O2A O 0.3159(2) 0.57116(19) 0.19370(18) 0.0752(9) Uani 1 1 d . . . . .
O3A O -1.0583(3) 0.6152(3) 0.4552(3) 0.1273(17) Uani 1 1 d . . . . .
O4A O -1.0372(3) 0.7040(3) 0.3701(3) 0.141(2) Uani 1 1 d . . . . .
O5A O 0.8593(4) 0.5711(4) 0.1069(3) 0.150(2) Uani 1 1 d . . . . .
O6A O 0.7450(4) 0.6721(3) 0.0604(3) 0.1320(17) Uani 1 1 d . . . . .
N1A N -0.5777(3) 0.50419(19) 0.4111(2) 0.0590(9) Uani 1 1 d . . . . .
H1A H -0.560637 0.454765 0.424497 0.071 Uiso 1 1 calc R . . . .
N2A N -0.4068(2) 0.47660(18) 0.38221(19) 0.0563(9) Uani 1 1 d . . . . .
H2A H -0.410087 0.429834 0.38794 0.068 Uiso 1 1 calc R . . . .
N3A N 0.3181(2) 0.4553(2) 0.25961(19) 0.0592(9) Uani 1 1 d . . . . .
H3A H 0.359522 0.410586 0.275233 0.071 Uiso 1 1 calc R . . . .
N4A N 0.4687(3) 0.4774(2) 0.22063(19) 0.0624(9) Uani 1 1 d . . . . .
H4A H 0.493899 0.430919 0.242172 0.075 Uiso 1 1 calc R . . . .
N5A N -1.0042(3) 0.6472(3) 0.4136(3) 0.0941(14) Uani 1 1 d . . . . .
N6A N 0.7711(5) 0.6077(4) 0.0969(3) 0.1052(16) Uani 1 1 d . . . . .
C1A C -0.6825(3) 0.5438(2) 0.4128(2) 0.0541(10) Uani 1 1 d . . . . .
C2A C -0.7245(3) 0.6158(3) 0.3729(3) 0.0683(12) Uani 1 1 d . . . . .
H2AA H -0.681663 0.641561 0.346042 0.082 Uiso 1 1 calc R . . . .
C3A C -0.8297(4) 0.6492(3) 0.3729(3) 0.0741(13) Uani 1 1 d . . . . .
H3AA H -0.858492 0.696344 0.344445 0.089 Uiso 1 1 calc R . . . .
C4A C -0.8915(3) 0.6115(3) 0.4160(3) 0.0690(12) Uani 1 1 d . . . . .
C5A C -0.8526(4) 0.5420(3) 0.4567(3) 0.0683(12) Uani 1 1 d . . . . .
H5A H -0.895755 0.517545 0.485048 0.082 Uiso 1 1 calc R . . . .
C6A C -0.7475(3) 0.5084(3) 0.4550(2) 0.0638(11) Uani 1 1 d . . . . .
H6A H -0.719577 0.460782 0.482922 0.077 Uiso 1 1 calc R . . . .
C7A C -0.4978(3) 0.5335(2) 0.3909(2) 0.0558(10) Uani 1 1 d . . . . .
C8A C -0.3087(3) 0.4826(2) 0.3654(2) 0.0507(9) Uani 1 1 d . . . . .
C9A C -0.2848(3) 0.5512(2) 0.3491(3) 0.0615(11) Uani 1 1 d . . . . .
H9A H -0.336834 0.598932 0.348827 0.074 Uiso 1 1 calc R . . . .
C10A C -0.1838(3) 0.5489(2) 0.3330(3) 0.0609(11) Uani 1 1 d . . . . .
H10A H -0.16931 0.595718 0.321532 0.073 Uiso 1 1 calc R . . . .
C11A C -0.1036(3) 0.4795(2) 0.3335(2) 0.0567(10) Uani 1 1 d . . . . .
C12A C -0.1294(3) 0.4123(3) 0.3497(3) 0.0689(12) Uani 1 1 d . . . . .
H12A H -0.077321 0.364555 0.349976 0.083 Uiso 1 1 calc R . . . .
C13A C -0.2286(3) 0.4128(2) 0.3654(3) 0.0678(12) Uani 1 1 d . . . . .
H13A H -0.242573 0.365777 0.376328 0.081 Uiso 1 1 calc R . . . .
C14A C 0.0058(3) 0.4763(2) 0.3144(2) 0.0570(10) Uani 1 1 d . . . . .
C15A C 0.0864(3) 0.4151(2) 0.3445(3) 0.0649(12) Uani 1 1 d . . . . .
H15A H 0.071432 0.376416 0.378013 0.078 Uiso 1 1 calc R . . . .
C16A C 0.1867(3) 0.4103(2) 0.3262(3) 0.0621(11) Uani 1 1 d . . . . .
H16A H 0.238336 0.368793 0.347977 0.074 Uiso 1 1 calc R . . . .
C17A C 0.2128(3) 0.4656(2) 0.2762(2) 0.0528(10) Uani 1 1 d . . . . .
C18A C 0.1341(3) 0.5287(3) 0.2471(3) 0.0684(12) Uani 1 1 d . . . . .
H18A H 0.149179 0.568319 0.214882 0.082 Uiso 1 1 calc R . . . .
C19A C 0.0329(3) 0.5322(3) 0.2666(3) 0.0670(12) Uani 1 1 d . . . . .
H19A H -0.019067 0.574568 0.246176 0.08 Uiso 1 1 calc R . . . .
C20A C 0.3621(3) 0.5066(3) 0.2224(2) 0.0573(10) Uani 1 1 d . . . . .
C21A C 0.5389(3) 0.5131(3) 0.1890(2) 0.0598(11) Uani 1 1 d . . . . .
C22A C 0.5139(4) 0.5897(3) 0.1540(3) 0.0768(14) Uani 1 1 d . . . . .
H22A H 0.44543 0.620593 0.151721 0.092 Uiso 1 1 calc R . . . .
C23A C 0.5905(4) 0.6188(3) 0.1231(3) 0.0827(15) Uani 1 1 d . . . . .
H23A H 0.573609 0.668961 0.098241 0.099 Uiso 1 1 calc R . . . .
C24A C 0.6909(4) 0.5755(3) 0.1283(3) 0.0775(14) Uani 1 1 d . . . . .
C25A C 0.7181(4) 0.5011(3) 0.1645(3) 0.0795(14) Uani 1 1 d . . . . .
H25A H 0.786897 0.472219 0.169232 0.095 Uiso 1 1 calc R . . . .
C26A C 0.6429(4) 0.4706(3) 0.1933(3) 0.0704(12) Uani 1 1 d . . . . .
H26A H 0.661276 0.419716 0.216555 0.085 Uiso 1 1 calc R . . . .
O1B O -0.2436(2) 0.1344(3) 0.1108(2) 0.0903(11) Uani 1 1 d . . . . .
O2B O 0.5647(2) -0.01619(17) 0.2949(2) 0.0788(10) Uani 1 1 d . . . . .
O3B O -0.7779(3) 0.1566(3) 0.0492(2) 0.1083(14) Uani 1 1 d . . . . .
O4B O -0.6610(4) 0.0603(4) 0.0083(4) 0.162(2) Uani 1 1 d . U . . .
O5B O 1.1255(3) -0.0579(2) 0.3117(3) 0.1031(13) Uani 1 1 d . . . . .
O6B O 1.0976(3) -0.1601(3) 0.2868(2) 0.1031(13) Uani 1 1 d . . . . .
N1B N -0.3955(3) 0.2040(2) 0.16550(19) 0.0654(10) Uani 1 1 d . . . . .
H1B H -0.422003 0.237813 0.196217 0.078 Uiso 1 1 calc R . . . .
N2B N -0.2465(2) 0.2088(2) 0.20075(19) 0.0611(9) Uani 1 1 d . . . . .
H2B H -0.287586 0.243581 0.226514 0.073 Uiso 1 1 calc R . . . .
N3B N 0.4756(2) 0.11070(18) 0.30968(19) 0.0549(8) Uani 1 1 d . . . . .
H3B H 0.482426 0.151073 0.324907 0.066 Uiso 1 1 calc R . . . .
N4B N 0.6457(2) 0.06546(19) 0.3254(2) 0.0586(9) Uani 1 1 d . . . . .
H4B H 0.63205 0.110738 0.339931 0.07 Uiso 1 1 calc R . . . .
N5B N -0.6885(4) 0.1177(4) 0.0406(3) 0.0930(14) Uani 1 1 d . . . . .
N6B N 1.0681(3) -0.0937(3) 0.3034(2) 0.0771(12) Uani 1 1 d . . . . .
C1B C -0.4646(3) 0.1817(3) 0.1304(2) 0.0621(11) Uani 1 1 d . . . . .
C2B C -0.5664(3) 0.2281(3) 0.1331(3) 0.0724(13) Uani 1 1 d . . . . .
H2BA H -0.585365 0.273849 0.155375 0.087 Uiso 1 1 calc R . . . .
C3B C -0.6400(4) 0.2081(3) 0.1037(3) 0.0774(14) Uani 1 1 d . . . . .
H3BA H -0.708275 0.239636 0.106279 0.093 Uiso 1 1 calc R . . . .
C4B C -0.6112(4) 0.1411(3) 0.0705(3) 0.0730(13) Uani 1 1 d . . . . .
C5B C -0.5113(4) 0.0940(4) 0.0668(3) 0.0902(16) Uani 1 1 d . . . . .
H5B H -0.492968 0.048777 0.043745 0.108 Uiso 1 1 calc R . . . .
C6B C -0.4375(4) 0.1137(3) 0.0976(3) 0.0822(15) Uani 1 1 d . . . . .
H6B H -0.369626 0.081172 0.096119 0.099 Uiso 1 1 calc R . . . .
C7B C -0.2907(3) 0.1779(3) 0.1565(2) 0.0600(11) Uani 1 1 d . . . . .
C8B C -0.1409(3) 0.1906(2) 0.2097(2) 0.0528(10) Uani 1 1 d . . . . .
C9B C -0.1159(3) 0.2296(3) 0.2605(3) 0.0682(12) Uani 1 1 d . . . . .
H9B H -0.167424 0.267125 0.284471 0.082 Uiso 1 1 calc R . . . .
C10B C -0.0137(3) 0.2128(3) 0.2756(3) 0.0699(12) Uani 1 1 d . . . . .
H10B H 0.001397 0.237167 0.312011 0.084 Uiso 1 1 calc R . . . .
C11B C 0.0658(3) 0.1612(2) 0.2384(2) 0.0531(10) Uani 1 1 d . . . . .
C12B C 0.0393(3) 0.1233(2) 0.1880(2) 0.0558(10) Uani 1 1 d . . . . .
H12B H 0.091149 0.086912 0.163081 0.067 Uiso 1 1 calc R . . . .
C13B C -0.0630(3) 0.1376(3) 0.1730(2) 0.0568(10) Uani 1 1 d . . . . .
H13B H -0.078225 0.111254 0.138234 0.068 Uiso 1 1 calc R . . . .
C14B C 0.1745(3) 0.1465(2) 0.2543(2) 0.0526(10) Uani 1 1 d . . . . .
C15B C 0.2514(3) 0.0767(2) 0.2440(2) 0.0564(10) Uani 1 1 d . . . . .
H15B H 0.234776 0.037799 0.225561 0.068 Uiso 1 1 calc R . . . .
C16B C 0.3513(3) 0.0628(2) 0.2601(2) 0.0538(10) Uani 1 1 d . . . . .
H16B H 0.401351 0.016009 0.250812 0.065 Uiso 1 1 calc R . . . .
C17B C 0.3768(3) 0.1189(2) 0.2901(2) 0.0513(9) Uani 1 1 d . . . . .
C18B C 0.3013(3) 0.1892(2) 0.2999(3) 0.0612(11) Uani 1 1 d . . . . .
H18B H 0.317458 0.228105 0.318668 0.073 Uiso 1 1 calc R . . . .
C19B C 0.2036(3) 0.2018(2) 0.2823(3) 0.0643(11) Uani 1 1 d . . . . .
H19B H 0.154405 0.249624 0.289427 0.077 Uiso 1 1 calc R . . . .
C20B C 0.5623(3) 0.0475(2) 0.3079(2) 0.0551(10) Uani 1 1 d . . . . .
C21B C 0.7486(3) 0.0209(2) 0.3228(2) 0.0539(10) Uani 1 1 d . . . . .
C22B C 0.8173(3) 0.0568(2) 0.3374(2) 0.0563(10) Uani 1 1 d . . . . .
H22B H 0.792538 0.107327 0.350782 0.068 Uiso 1 1 calc R . . . .
C23B C 0.9215(3) 0.0192(3) 0.3326(2) 0.0621(11) Uani 1 1 d . . . . .
H23B H 0.967145 0.043906 0.342159 0.074 Uiso 1 1 calc R . . . .
C24B C 0.9566(3) -0.0552(3) 0.3135(2) 0.0631(12) Uani 1 1 d . . . . .
C25B C 0.8897(4) -0.0931(3) 0.3020(3) 0.0805(14) Uani 1 1 d . . . . .
H25B H 0.914906 -0.144473 0.29109 0.097 Uiso 1 1 calc R . . . .
C26B C 0.7862(4) -0.0558(3) 0.3065(3) 0.0780(14) Uani 1 1 d . . . . .
H26B H 0.741032 -0.081721 0.298644 0.094 Uiso 1 1 calc R . . . .
N7A N 0.3990(3) 0.81363(19) 0.41150(19) 0.0588(9) Uani 1 1 d . . . . .
C27A C 0.3865(4) 0.7934(3) 0.3359(3) 0.0697(12) Uani 1 1 d . . . . .
H27A H 0.42274 0.738263 0.33399 0.084 Uiso 1 1 calc R . . . .
H27B H 0.314192 0.801183 0.332259 0.084 Uiso 1 1 calc R . . . .
C28A C 0.4230(5) 0.8375(3) 0.2689(3) 0.0963(17) Uani 1 1 d D . . . .
H28A H 0.494529 0.832444 0.272423 0.116 Uiso 1 1 calc R . . . .
H28B H 0.383416 0.892433 0.267368 0.116 Uiso 1 1 calc R . . . .
C29A C 0.4121(6) 0.8076(4) 0.1989(3) 0.124(2) Uani 1 1 d D . . . .
H29A H 0.452426 0.752784 0.200308 0.148 Uiso 1 1 calc R . . . .
H29B H 0.340666 0.811769 0.195981 0.148 Uiso 1 1 calc R . . . .
C30A C 0.4467(7) 0.8519(5) 0.1314(4) 0.158(3) Uani 1 1 d D . . . .
H30A H 0.446397 0.827199 0.088775 0.237 Uiso 1 1 calc GR . . . .
H30B H 0.515006 0.852402 0.136378 0.237 Uiso 1 1 calc GR . . . .
H30C H 0.400846 0.904588 0.126055 0.237 Uiso 1 1 calc GR . . . .
C31A C 0.3293(3) 0.7804(3) 0.4657(3) 0.0665(12) Uani 1 1 d . . . . .
H31A H 0.34617 0.725435 0.460411 0.08 Uiso 1 1 calc R . . . .
H31B H 0.344384 0.784123 0.51513 0.08 Uiso 1 1 calc R . . . .
C32A C 0.2157(4) 0.8182(3) 0.4589(3) 0.0806(15) Uani 1 1 d D . . . .
H32A H 0.198638 0.813618 0.410277 0.097 Uiso 1 1 calc R . . . .
H32B H 0.19713 0.873318 0.464376 0.097 Uiso 1 1 calc R . . . .
C33A C 0.1545(4) 0.7798(4) 0.5175(3) 0.0937(17) Uani 1 1 d D . . . .
H33A H 0.173749 0.72463 0.512081 0.112 Uiso 1 1 calc R . . . .
H33B H 0.171742 0.784555 0.565983 0.112 Uiso 1 1 calc R . . . .
C34A C 0.0398(5) 0.8165(6) 0.5116(4) 0.155(4) Uani 1 1 d . . . . .
H34A H 0.021878 0.809126 0.464757 0.233 Uiso 1 1 calc GR . . . .
H34B H 0.020699 0.871365 0.515781 0.233 Uiso 1 1 calc GR . . . .
H34C H 0.004055 0.792375 0.550425 0.233 Uiso 1 1 calc GR . . . .
C35A C 0.5061(3) 0.7706(3) 0.4373(3) 0.0720(13) Uani 1 1 d D . . . .
H35A H 0.505363 0.777293 0.488794 0.086 Uiso 1 1 calc R . . . .
H35B H 0.52031 0.715389 0.434424 0.086 Uiso 1 1 calc R . . . .
C36A C 0.5928(4) 0.7944(5) 0.3966(4) 0.121(3) Uani 1 1 d D . . . .
H36A H 0.581038 0.849197 0.400184 0.145 Uiso 1 1 calc R . . . .
H36B H 0.594974 0.787904 0.344876 0.145 Uiso 1 1 calc R . . . .
C37A C 0.6959(4) 0.7463(4) 0.4270(3) 0.106(2) Uani 1 1 d D . . . .
H37A H 0.706058 0.691412 0.425003 0.127 Uiso 1 1 calc R . . . .
H37B H 0.750361 0.759768 0.395713 0.127 Uiso 1 1 calc R . . . .
C38A C 0.7046(5) 0.7586(5) 0.5057(4) 0.139(3) Uani 1 1 d D . . . .
H38A H 0.694719 0.812738 0.50825 0.208 Uiso 1 1 calc GR . . . .
H38B H 0.771559 0.727782 0.521117 0.208 Uiso 1 1 calc GR . . . .
H38C H 0.653149 0.742888 0.53752 0.208 Uiso 1 1 calc GR . . . .
C39A C 0.3713(4) 0.9006(2) 0.4107(2) 0.0656(11) Uani 1 1 d D . . . .
H39A H 0.303428 0.925021 0.392553 0.079 Uiso 1 1 calc R . . . .
H39B H 0.419423 0.918713 0.376275 0.079 Uiso 1 1 calc R . . . .
C40A C 0.3716(4) 0.9280(3) 0.4853(3) 0.0755(13) Uani 1 1 d D . . . .
H40A H 0.325728 0.908494 0.520735 0.091 Uiso 1 1 calc R . . . .
H40B H 0.440265 0.906614 0.502578 0.091 Uiso 1 1 calc R . . . .
C41A C 0.3377(4) 1.0162(3) 0.4804(3) 0.0841(15) Uani 1 1 d . . . . .
H41A H 0.35067 1.030975 0.526203 0.101 Uiso 1 1 calc R . . . .
H41B H 0.379201 1.035514 0.44114 0.101 Uiso 1 1 calc R . . . .
C42A C 0.2274(5) 1.0546(3) 0.4665(4) 0.1031(19) Uani 1 1 d . . . . .
H42A H 0.21528 1.045134 0.418821 0.155 Uiso 1 1 calc GR . . . .
H42B H 0.20985 1.109842 0.468246 0.155 Uiso 1 1 calc GR . . . .
H42C H 0.185714 1.033752 0.503587 0.155 Uiso 1 1 calc GR . . . .
N7B N 0.0755(3) 0.7222(2) 0.0409(2) 0.0725(11) Uani 1 1 d . . . . .
C27B C 0.0282(4) 0.7201(3) -0.0287(3) 0.0765(14) Uani 1 1 d D . . . .
H27C H -0.035717 0.763076 -0.032095 0.092 Uiso 1 1 calc R . . . .
H27D H 0.07395 0.729318 -0.070418 0.092 Uiso 1 1 calc R . . . .
C28B C 0.0060(4) 0.6462(3) -0.0356(3) 0.0898(16) Uani 1 1 d D . . . .
H28C H -0.037803 0.634776 0.006526 0.108 Uiso 1 1 calc R . . . .
H28D H 0.069713 0.603002 -0.036488 0.108 Uiso 1 1 calc R . . . .
C29B C -0.0469(6) 0.6555(4) -0.1061(4) 0.118(2) Uani 1 1 d D . . . .
H29C H -0.10287 0.704523 -0.108638 0.142 Uiso 1 1 calc R . . . .
H29D H 0.001761 0.658797 -0.147738 0.142 Uiso 1 1 calc R . . . .
C30B C -0.0895(7) 0.5904(5) -0.1132(5) 0.160(3) Uani 1 1 d D . . . .
H30D H -0.119088 0.599535 -0.159816 0.239 Uiso 1 1 calc GR . . . .
H30E H -0.141257 0.588834 -0.074083 0.239 Uiso 1 1 calc GR . . . .
H30F H -0.034951 0.541417 -0.110165 0.239 Uiso 1 1 calc GR . . . .
C31B C 0.0071(4) 0.7088(3) 0.1094(3) 0.0802(15) Uani 1 1 d . . . . .
H31C H 0.001064 0.657048 0.111295 0.096 Uiso 1 1 calc R . . . .
H31D H 0.041337 0.709399 0.152563 0.096 Uiso 1 1 calc R . . . .
C32B C -0.0979(4) 0.7659(4) 0.1142(3) 0.0928(17) Uani 1 1 d D . . . .
H32C H -0.134056 0.76491 0.072135 0.111 Uiso 1 1 calc R . . . .
H32D H -0.093317 0.818032 0.112618 0.111 Uiso 1 1 calc R . . . .
C33B C -0.1578(4) 0.7469(5) 0.1851(3) 0.111(2) Uani 1 1 d D . . . .
H33C H -0.158701 0.693688 0.187901 0.133 Uiso 1 1 calc R . . . .
H33D H -0.123517 0.750831 0.227007 0.133 Uiso 1 1 calc R . . . .
C34B C -0.2675(5) 0.8022(6) 0.1886(5) 0.153(3) Uani 1 1 d D . . . .
H34D H -0.306385 0.78959 0.154797 0.229 Uiso 1 1 calc GR . . . .
H34E H -0.267255 0.854952 0.175572 0.229 Uiso 1 1 calc GR . . . .
H34F H -0.298312 0.796806 0.23775 0.229 Uiso 1 1 calc GR . . . .
C35B C 0.1784(4) 0.6592(3) 0.0479(3) 0.0879(16) Uani 1 1 d . . . . .
H35C H 0.168598 0.609058 0.047375 0.105 Uiso 1 1 calc R . . . .
H35D H 0.202868 0.659231 0.095397 0.105 Uiso 1 1 calc R . . . .
C36B C 0.2610(4) 0.6672(4) -0.0118(3) 0.0973(18) Uani 1 1 d . . . . .
H36C H 0.235128 0.672718 -0.059862 0.117 Uiso 1 1 calc R . . . .
H36D H 0.27844 0.713805 -0.007652 0.117 Uiso 1 1 calc R . . . .
C37B C 0.3553(4) 0.5972(4) -0.0046(3) 0.107(2) Uani 1 1 d D . . . .
H37C H 0.341754 0.552981 -0.020015 0.128 Uiso 1 1 calc R . . . .
H37D H 0.371242 0.584439 0.046662 0.128 Uiso 1 1 calc R . . . .
C38B C 0.4478(5) 0.6111(5) -0.0513(4) 0.128(2) Uani 1 1 d D . . . .
H38D H 0.432379 0.623663 -0.1021 0.191 Uiso 1 1 calc GR . . . .
H38E H 0.506282 0.564833 -0.045938 0.191 Uiso 1 1 calc GR . . . .
H38F H 0.462974 0.653692 -0.035025 0.191 Uiso 1 1 calc GR . . . .
C39B C 0.0877(4) 0.8027(3) 0.0358(3) 0.0896(16) Uani 1 1 d . . . . .
H39C H 0.020596 0.841589 0.030178 0.108 Uiso 1 1 calc R . . . .
H39D H 0.130626 0.809843 -0.008408 0.108 Uiso 1 1 calc R . . . .
C40B C 0.1342(6) 0.8181(5) 0.1014(4) 0.120(2) Uani 1 1 d D . . . .
H40C H 0.100123 0.801506 0.146738 0.144 Uiso 1 1 calc R . . . .
H40D H 0.206406 0.78748 0.101152 0.144 Uiso 1 1 calc R . . . .
C41B C 0.1234(11) 0.9034(5) 0.0992(8) 0.215(5) Uani 1 1 d D U . . .
H41C H 0.161676 0.906356 0.13923 0.258 Uiso 1 1 calc R . . . .
H41D H 0.051577 0.928977 0.113257 0.258 Uiso 1 1 calc R . . . .
C42B C 0.1511(14) 0.9568(10) 0.0343(9) 0.313(9) Uani 1 1 d D U . . .
H42D H 0.19986 0.925721 0.000292 0.47 Uiso 1 1 calc GR . . . .
H42E H 0.180672 0.991211 0.051893 0.47 Uiso 1 1 calc GR . . . .
H42F H 0.09026 0.986975 0.009761 0.47 Uiso 1 1 calc GR . . . .
P1 P 0.54456(7) 0.29178(5) 0.34247(5) 0.0453(3) Uani 1 1 d D . . . .
O2 O 0.5040(4) 0.34817(16) 0.40483(16) 0.1350(18) Uani 1 1 d D . . . .
H2 H 0.526624 0.325047 0.444096 0.202 Uiso 1 1 calc R . . . .
O1 O 0.5989(6) 0.21080(16) 0.3748(3) 0.098(3) Uani 0.51 1 d D . P A 1
O3 O 0.4516(5) 0.2832(6) 0.3122(5) 0.160(5) Uani 0.51 1 d D U P A 1
O4 O 0.6079(6) 0.3243(4) 0.2820(4) 0.133(4) Uani 0.51 1 d D U P A 1
O1' O 0.5458(5) 0.21057(17) 0.3738(3) 0.076(3) Uani 0.49 1 d D . P A 2
O3' O 0.4822(6) 0.3197(4) 0.2770(3) 0.112(3) Uani 0.49 1 d D U P A 2
O4' O 0.6528(4) 0.2971(5) 0.3275(6) 0.143(4) Uani 0.49 1 d D U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 C7A 1.222(5) . ?
O2A C20A 1.215(5) . ?
O3A N5A 1.229(6) . ?
O4A N5A 1.206(6) . ?
O5A N6A 1.201(6) . ?
O6A N6A 1.229(7) . ?
N1A H1A 0.86 . ?
N1A C1A 1.389(5) . ?
N1A C7A 1.370(5) . ?
N2A H2A 0.86 . ?
N2A C7A 1.353(5) . ?
N2A C8A 1.392(5) . ?
N3A H3A 0.86 . ?
N3A C17A 1.407(5) . ?
N3A C20A 1.346(5) . ?
N4A H4A 0.86 . ?
N4A C20A 1.389(5) . ?
N4A C21A 1.372(5) . ?
N5A C4A 1.480(6) . ?
N6A C24A 1.447(7) . ?
C1A C2A 1.385(6) . ?
C1A C6A 1.379(6) . ?
C2A H2AA 0.93 . ?
C2A C3A 1.378(6) . ?
C3A H3AA 0.93 . ?
C3A C4A 1.381(7) . ?
C4A C5A 1.352(6) . ?
C5A H5A 0.93 . ?
C5A C6A 1.377(6) . ?
C6A H6A 0.93 . ?
C8A C9A 1.380(5) . ?
C8A C13A 1.386(5) . ?
C9A H9A 0.93 . ?
C9A C10A 1.381(6) . ?
C10A H10A 0.93 . ?
C10A C11A 1.383(5) . ?
C11A C12A 1.370(6) . ?
C11A C14A 1.495(6) . ?
C12A H12A 0.93 . ?
C12A C13A 1.365(6) . ?
C13A H13A 0.93 . ?
C14A C15A 1.392(5) . ?
C14A C19A 1.368(6) . ?
C15A H15A 0.93 . ?
C15A C16A 1.364(6) . ?
C16A H16A 0.93 . ?
C16A C17A 1.376(6) . ?
C17A C18A 1.387(5) . ?
C18A H18A 0.93 . ?
C18A C19A 1.387(6) . ?
C19A H19A 0.93 . ?
C21A C22A 1.401(6) . ?
C21A C26A 1.395(6) . ?
C22A H22A 0.93 . ?
C22A C23A 1.368(7) . ?
C23A H23A 0.93 . ?
C23A C24A 1.358(7) . ?
C24A C25A 1.375(7) . ?
C25A H25A 0.93 . ?
C25A C26A 1.356(6) . ?
C26A H26A 0.93 . ?
O1B C7B 1.219(5) . ?
O2B C20B 1.209(5) . ?
O3B N5B 1.211(6) . ?
O4B N5B 1.208(7) . ?
O5B N6B 1.213(6) . ?
O6B N6B 1.217(6) . ?
N1B H1B 0.86 . ?
N1B C1B 1.399(6) . ?
N1B C7B 1.366(5) . ?
N2B H2B 0.86 . ?
N2B C7B 1.348(6) . ?
N2B C8B 1.408(5) . ?
N3B H3B 0.86 . ?
N3B C17B 1.404(5) . ?
N3B C20B 1.363(5) . ?
N4B H4B 0.86 . ?
N4B C20B 1.377(5) . ?
N4B C21B 1.385(5) . ?
N5B C4B 1.454(7) . ?
N6B C24B 1.470(6) . ?
C1B C2B 1.383(6) . ?
C1B C6B 1.378(7) . ?
C2B H2BA 0.93 . ?
C2B C3B 1.369(7) . ?
C3B H3BA 0.93 . ?
C3B C4B 1.367(7) . ?
C4B C5B 1.365(7) . ?
C5B H5B 0.93 . ?
C5B C6B 1.384(7) . ?
C6B H6B 0.93 . ?
C8B C9B 1.386(6) . ?
C8B C13B 1.375(6) . ?
C9B H9B 0.93 . ?
C9B C10B 1.394(6) . ?
C10B H10B 0.93 . ?
C10B C11B 1.378(6) . ?
C11B C12B 1.375(6) . ?
C11B C14B 1.489(5) . ?
C12B H12B 0.93 . ?
C12B C13B 1.402(5) . ?
C13B H13B 0.93 . ?
C14B C15B 1.386(5) . ?
C14B C19B 1.380(6) . ?
C15B H15B 0.93 . ?
C15B C16B 1.376(5) . ?
C16B H16B 0.93 . ?
C16B C17B 1.384(5) . ?
C17B C18B 1.383(5) . ?
C18B H18B 0.93 . ?
C18B C19B 1.359(6) . ?
C19B H19B 0.93 . ?
C21B C22B 1.384(6) . ?
C21B C26B 1.389(6) . ?
C22B H22B 0.93 . ?
C22B C23B 1.375(6) . ?
C23B H23B 0.93 . ?
C23B C24B 1.367(6) . ?
C24B C25B 1.371(7) . ?
C25B H25B 0.93 . ?
C25B C26B 1.365(7) . ?
C26B H26B 0.93 . ?
N7A C27A 1.529(6) . ?
N7A C31A 1.510(5) . ?
N7A C35A 1.522(5) . ?
N7A C39A 1.505(5) . ?
C27A H27A 0.97 . ?
C27A H27B 0.97 . ?
C27A C28A 1.502(7) . ?
C28A H28A 0.97 . ?
C28A H28B 0.97 . ?
C28A C29A 1.508(6) . ?
C29A H29A 0.97 . ?
C29A H29B 0.97 . ?
C29A C30A 1.502(7) . ?
C30A H30A 0.96 . ?
C30A H30B 0.96 . ?
C30A H30C 0.96 . ?
C31A H31A 0.97 . ?
C31A H31B 0.97 . ?
C31A C32A 1.503(6) . ?
C32A H32A 0.97 . ?
C32A H32B 0.97 . ?
C32A C33A 1.528(6) . ?
C33A H33A 0.97 . ?
C33A H33B 0.97 . ?
C33A C34A 1.513(8) . ?
C34A H34A 0.96 . ?
C34A H34B 0.96 . ?
C34A H34C 0.96 . ?
C35A H35A 0.97 . ?
C35A H35B 0.97 . ?
C35A C36A 1.493(6) . ?
C36A H36A 0.97 . ?
C36A H36B 0.97 . ?
C36A C37A 1.525(6) . ?
C37A H37A 0.97 . ?
C37A H37B 0.97 . ?
C37A C38A 1.518(6) . ?
C38A H38A 0.96 . ?
C38A H38B 0.96 . ?
C38A H38C 0.96 . ?
C39A H39A 0.97 . ?
C39A H39B 0.97 . ?
C39A C40A 1.524(5) . ?
C40A H40A 0.97 . ?
C40A H40B 0.97 . ?
C40A C41A 1.515(6) . ?
C41A H41A 0.97 . ?
C41A H41B 0.97 . ?
C41A C42A 1.488(7) . ?
C42A H42A 0.96 . ?
C42A H42B 0.96 . ?
C42A H42C 0.96 . ?
N7B C27B 1.510(6) . ?
N7B C31B 1.527(6) . ?
N7B C35B 1.510(6) . ?
N7B C39B 1.522(7) . ?
C27B H27C 0.97 . ?
C27B H27D 0.97 . ?
C27B C28B 1.503(6) . ?
C28B H28C 0.97 . ?
C28B H28D 0.97 . ?
C28B C29B 1.518(8) . ?
C29B H29C 0.97 . ?
C29B H29D 0.97 . ?
C29B C30B 1.515(6) . ?
C30B H30D 0.96 . ?
C30B H30E 0.96 . ?
C30B H30F 0.96 . ?
C31B H31C 0.97 . ?
C31B H31D 0.97 . ?
C31B C32B 1.485(7) . ?
C32B H32C 0.97 . ?
C32B H32D 0.97 . ?
C32B C33B 1.523(6) . ?
C33B H33C 0.97 . ?
C33B H33D 0.97 . ?
C33B C34B 1.521(7) . ?
C34B H34D 0.96 . ?
C34B H34E 0.96 . ?
C34B H34F 0.96 . ?
C35B H35C 0.97 . ?
C35B H35D 0.97 . ?
C35B C36B 1.520(7) . ?
C36B H36C 0.97 . ?
C36B H36D 0.97 . ?
C36B C37B 1.498(8) . ?
C37B H37C 0.97 . ?
C37B H37D 0.97 . ?
C37B C38B 1.529(7) . ?
C38B H38D 0.96 . ?
C38B H38E 0.96 . ?
C38B H38F 0.96 . ?
C39B H39C 0.97 . ?
C39B H39D 0.97 . ?
C39B C40B 1.527(8) . ?
C40B H40C 0.97 . ?
C40B H40D 0.97 . ?
C40B C41B 1.510(5) . ?
C41B H41C 0.97 . ?
C41B H41D 0.97 . ?
C41B C42B 1.525(6) . ?
C42B H42D 0.96 . ?
C42B H42E 0.96 . ?
C42B H42F 0.96 . ?
P1 O2 1.5819(17) . ?
P1 O1 1.490(3) . ?
P1 O3 1.514(3) . ?
P1 O4 1.512(3) . ?
P1 O1' 1.507(3) . ?
P1 O3' 1.489(3) . ?
P1 O4' 1.521(3) . ?
O2 H2 0.82 . ?

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
C1A N1A H1A 115.7 . . ?
C7A N1A H1A 115.7 . . ?
C7A N1A C1A 128.5(3) . . ?
C7A N2A H2A 115.3 . . ?
C7A N2A C8A 129.5(3) . . ?
C8A N2A H2A 115.3 . . ?
C17A N3A H3A 115.9 . . ?
C20A N3A H3A 115.9 . . ?
C20A N3A C17A 128.2(3) . . ?
C20A N4A H4A 115.7 . . ?
C21A N4A H4A 115.7 . . ?
C21A N4A C20A 128.5(4) . . ?
O3A N5A C4A 117.2(5) . . ?
O4A N5A O3A 124.3(5) . . ?
O4A N5A C4A 118.5(5) . . ?
O5A N6A O6A 122.9(6) . . ?
O5A N6A C24A 119.6(6) . . ?
O6A N6A C24A 117.6(6) . . ?
C2A C1A N1A 123.1(4) . . ?
C6A C1A N1A 118.0(4) . . ?
C6A C1A C2A 118.9(4) . . ?
C1A C2A H2AA 120 . . ?
C3A C2A C1A 120.0(4) . . ?
C3A C2A H2AA 120 . . ?
C2A C3A H3AA 120.6 . . ?
C2A C3A C4A 118.8(4) . . ?
C4A C3A H3AA 120.6 . . ?
C3A C4A N5A 118.0(5) . . ?
C5A C4A N5A 119.5(5) . . ?
C5A C4A C3A 122.3(4) . . ?
C4A C5A H5A 120.9 . . ?
C4A C5A C6A 118.3(4) . . ?
C6A C5A H5A 120.9 . . ?
C1A C6A H6A 119.2 . . ?
C5A C6A C1A 121.5(4) . . ?
C5A C6A H6A 119.2 . . ?
O1A C7A N1A 123.1(4) . . ?
O1A C7A N2A 124.6(4) . . ?
N2A C7A N1A 112.4(3) . . ?
C9A C8A N2A 125.9(3) . . ?
C9A C8A C13A 117.9(4) . . ?
C13A C8A N2A 116.2(3) . . ?
C8A C9A H9A 119.9 . . ?
C8A C9A C10A 120.1(4) . . ?
C10A C9A H9A 119.9 . . ?
C9A C10A H10A 118.9 . . ?
C9A C10A C11A 122.2(4) . . ?
C11A C10A H10A 118.9 . . ?
C10A C11A C14A 122.7(4) . . ?
C12A C11A C10A 116.5(4) . . ?
C12A C11A C14A 120.8(4) . . ?
C11A C12A H12A 118.8 . . ?
C13A C12A C11A 122.5(4) . . ?
C13A C12A H12A 118.8 . . ?
C8A C13A H13A 119.6 . . ?
C12A C13A C8A 120.8(4) . . ?
C12A C13A H13A 119.6 . . ?
C15A C14A C11A 121.1(4) . . ?
C19A C14A C11A 122.7(4) . . ?
C19A C14A C15A 116.1(4) . . ?
C14A C15A H15A 119 . . ?
C16A C15A C14A 122.0(4) . . ?
C16A C15A H15A 119 . . ?
C15A C16A H16A 119.4 . . ?
C15A C16A C17A 121.2(4) . . ?
C17A C16A H16A 119.4 . . ?
C16A C17A N3A 117.5(3) . . ?
C16A C17A C18A 118.1(4) . . ?
C18A C17A N3A 124.4(4) . . ?
C17A C18A H18A 120.3 . . ?
C19A C18A C17A 119.4(4) . . ?
C19A C18A H18A 120.3 . . ?
C14A C19A C18A 123.1(4) . . ?
C14A C19A H19A 118.5 . . ?
C18A C19A H19A 118.5 . . ?
O2A C20A N3A 125.1(4) . . ?
O2A C20A N4A 123.0(4) . . ?
N3A C20A N4A 111.9(3) . . ?
N4A C21A C22A 124.7(4) . . ?
N4A C21A C26A 117.7(4) . . ?
C26A C21A C22A 117.6(4) . . ?
C21A C22A H22A 120.2 . . ?
C23A C22A C21A 119.7(5) . . ?
C23A C22A H22A 120.2 . . ?
C22A C23A H23A 119.5 . . ?
C24A C23A C22A 120.9(5) . . ?
C24A C23A H23A 119.5 . . ?
C23A C24A N6A 120.3(5) . . ?
C23A C24A C25A 120.8(5) . . ?
C25A C24A N6A 118.9(5) . . ?
C24A C25A H25A 120.6 . . ?
C26A C25A C24A 118.9(5) . . ?
C26A C25A H25A 120.6 . . ?
C21A C26A H26A 119 . . ?
C25A C26A C21A 122.0(5) . . ?
C25A C26A H26A 119 . . ?
C1B N1B H1B 116.4 . . ?
C7B N1B H1B 116.4 . . ?
C7B N1B C1B 127.2(4) . . ?
C7B N2B H2B 116.2 . . ?
C7B N2B C8B 127.5(4) . . ?
C8B N2B H2B 116.2 . . ?
C17B N3B H3B 115.6 . . ?
C20B N3B H3B 115.6 . . ?
C20B N3B C17B 128.9(3) . . ?
C20B N4B H4B 115.4 . . ?
C20B N4B C21B 129.2(4) . . ?
C21B N4B H4B 115.4 . . ?
O3B N5B C4B 118.5(6) . . ?
O4B N5B O3B 122.7(5) . . ?
O4B N5B C4B 118.7(5) . . ?
O5B N6B O6B 123.7(5) . . ?
O5B N6B C24B 118.6(5) . . ?
O6B N6B C24B 117.7(5) . . ?
C2B C1B N1B 117.7(4) . . ?
C6B C1B N1B 123.3(4) . . ?
C6B C1B C2B 118.8(4) . . ?
C1B C2B H2BA 119.3 . . ?
C3B C2B C1B 121.5(5) . . ?
C3B C2B H2BA 119.3 . . ?
C2B C3B H3BA 120.6 . . ?
C4B C3B C2B 118.9(4) . . ?
C4B C3B H3BA 120.6 . . ?
C3B C4B N5B 119.8(5) . . ?
C5B C4B N5B 119.1(5) . . ?
C5B C4B C3B 121.1(5) . . ?
C4B C5B H5B 120 . . ?
C4B C5B C6B 119.9(5) . . ?
C6B C5B H5B 120 . . ?
C1B C6B C5B 119.9(5) . . ?
C1B C6B H6B 120.1 . . ?
C5B C6B H6B 120.1 . . ?
O1B C7B N1B 123.0(4) . . ?
O1B C7B N2B 124.4(4) . . ?
N2B C7B N1B 112.4(4) . . ?
C9B C8B N2B 115.9(4) . . ?
C13B C8B N2B 125.3(4) . . ?
C13B C8B C9B 118.8(4) . . ?
C8B C9B H9B 120 . . ?
C8B C9B C10B 120.0(4) . . ?
C10B C9B H9B 120 . . ?
C9B C10B H10B 118.9 . . ?
C11B C10B C9B 122.1(4) . . ?
C11B C10B H10B 118.9 . . ?
C10B C11B C14B 120.7(4) . . ?
C12B C11B C10B 116.8(4) . . ?
C12B C11B C14B 122.5(4) . . ?
C11B C12B H12B 118.9 . . ?
C11B C12B C13B 122.3(4) . . ?
C13B C12B H12B 118.9 . . ?
C8B C13B C12B 119.8(4) . . ?
C8B C13B H13B 120.1 . . ?
C12B C13B H13B 120.1 . . ?
C15B C14B C11B 122.7(4) . . ?
C19B C14B C11B 121.2(4) . . ?
C19B C14B C15B 116.0(4) . . ?
C14B C15B H15B 118.7 . . ?
C16B C15B C14B 122.6(4) . . ?
C16B C15B H15B 118.7 . . ?
C15B C16B H16B 120.2 . . ?
C15B C16B C17B 119.6(4) . . ?
C17B C16B H16B 120.2 . . ?
C16B C17B N3B 124.7(4) . . ?
C18B C17B N3B 116.8(3) . . ?
C18B C17B C16B 118.5(3) . . ?
C17B C18B H18B 119.7 . . ?
C19B C18B C17B 120.5(4) . . ?
C19B C18B H18B 119.7 . . ?
C14B C19B H19B 118.7 . . ?
C18B C19B C14B 122.7(4) . . ?
C18B C19B H19B 118.7 . . ?
O2B C20B N3B 124.5(4) . . ?
O2B C20B N4B 124.6(4) . . ?
N3B C20B N4B 110.8(3) . . ?
N4B C21B C26B 124.6(4) . . ?
C22B C21B N4B 116.5(4) . . ?
C22B C21B C26B 118.8(4) . . ?
C21B C22B H22B 119.4 . . ?
C23B C22B C21B 121.2(4) . . ?
C23B C22B H22B 119.4 . . ?
C22B C23B H23B 120.6 . . ?
C24B C23B C22B 118.8(4) . . ?
C24B C23B H23B 120.6 . . ?
C23B C24B N6B 118.9(5) . . ?
C23B C24B C25B 121.0(4) . . ?
C25B C24B N6B 120.1(5) . . ?
C24B C25B H25B 119.8 . . ?
C26B C25B C24B 120.4(5) . . ?
C26B C25B H25B 119.8 . . ?
C21B C26B H26B 120.1 . . ?
C25B C26B C21B 119.8(5) . . ?
C25B C26B H26B 120.1 . . ?
C31A N7A C27A 106.3(3) . . ?
C31A N7A C35A 104.1(3) . . ?
C35A N7A C27A 111.8(3) . . ?
C39A N7A C27A 110.3(3) . . ?
C39A N7A C31A 111.9(3) . . ?
C39A N7A C35A 112.1(3) . . ?
N7A C27A H27A 107.9 . . ?
N7A C27A H27B 107.9 . . ?
H27A C27A H27B 107.2 . . ?
C28A C27A N7A 117.8(4) . . ?
C28A C27A H27A 107.9 . . ?
C28A C27A H27B 107.9 . . ?
C27A C28A H28A 109.3 . . ?
C27A C28A H28B 109.3 . . ?
C27A C28A C29A 111.6(5) . . ?
H28A C28A H28B 108 . . ?
C29A C28A H28A 109.3 . . ?
C29A C28A H28B 109.3 . . ?
C28A C29A H29A 109.2 . . ?
C28A C29A H29B 109.2 . . ?
H29A C29A H29B 107.9 . . ?
C30A C29A C28A 112.2(6) . . ?
C30A C29A H29A 109.2 . . ?
C30A C29A H29B 109.2 . . ?
C29A C30A H30A 109.5 . . ?
C29A C30A H30B 109.5 . . ?
C29A C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
N7A C31A H31A 108.2 . . ?
N7A C31A H31B 108.2 . . ?
H31A C31A H31B 107.4 . . ?
C32A C31A N7A 116.4(3) . . ?
C32A C31A H31A 108.2 . . ?
C32A C31A H31B 108.2 . . ?
C31A C32A H32A 109.5 . . ?
C31A C32A H32B 109.5 . . ?
C31A C32A C33A 110.8(4) . . ?
H32A C32A H32B 108.1 . . ?
C33A C32A H32A 109.5 . . ?
C33A C32A H32B 109.5 . . ?
C32A C33A H33A 109.2 . . ?
C32A C33A H33B 109.2 . . ?
H33A C33A H33B 107.9 . . ?
C34A C33A C32A 111.9(5) . . ?
C34A C33A H33A 109.2 . . ?
C34A C33A H33B 109.2 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
N7A C35A H35A 108 . . ?
N7A C35A H35B 108 . . ?
H35A C35A H35B 107.3 . . ?
C36A C35A N7A 117.0(4) . . ?
C36A C35A H35A 108 . . ?
C36A C35A H35B 108 . . ?
C35A C36A H36A 109.2 . . ?
C35A C36A H36B 109.2 . . ?
C35A C36A C37A 111.9(5) . . ?
H36A C36A H36B 107.9 . . ?
C37A C36A H36A 109.2 . . ?
C37A C36A H36B 109.2 . . ?
C36A C37A H37A 108.9 . . ?
C36A C37A H37B 108.9 . . ?
H37A C37A H37B 107.7 . . ?
C38A C37A C36A 113.6(5) . . ?
C38A C37A H37A 108.9 . . ?
C38A C37A H37B 108.9 . . ?
C37A C38A H38A 109.5 . . ?
C37A C38A H38B 109.5 . . ?
C37A C38A H38C 109.5 . . ?
H38A C38A H38B 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
N7A C39A H39A 108.6 . . ?
N7A C39A H39B 108.6 . . ?
N7A C39A C40A 114.8(3) . . ?
H39A C39A H39B 107.5 . . ?
C40A C39A H39A 108.6 . . ?
C40A C39A H39B 108.6 . . ?
C39A C40A H40A 109.3 . . ?
C39A C40A H40B 109.3 . . ?
H40A C40A H40B 108 . . ?
C41A C40A C39A 111.4(4) . . ?
C41A C40A H40A 109.3 . . ?
C41A C40A H40B 109.3 . . ?
C40A C41A H41A 108.8 . . ?
C40A C41A H41B 108.8 . . ?
H41A C41A H41B 107.7 . . ?
C42A C41A C40A 113.9(5) . . ?
C42A C41A H41A 108.8 . . ?
C42A C41A H41B 108.8 . . ?
C41A C42A H42A 109.5 . . ?
C41A C42A H42B 109.5 . . ?
C41A C42A H42C 109.5 . . ?
H42A C42A H42B 109.5 . . ?
H42A C42A H42C 109.5 . . ?
H42B C42A H42C 109.5 . . ?
C27B N7B C31B 111.3(4) . . ?
C27B N7B C35B 111.2(4) . . ?
C27B N7B C39B 106.3(3) . . ?
C35B N7B C31B 107.2(3) . . ?
C35B N7B C39B 110.6(4) . . ?
C39B N7B C31B 110.2(4) . . ?
N7B C27B H27C 108.2 . . ?
N7B C27B H27D 108.2 . . ?
H27C C27B H27D 107.4 . . ?
C28B C27B N7B 116.3(4) . . ?
C28B C27B H27C 108.2 . . ?
C28B C27B H27D 108.2 . . ?
C27B C28B H28C 109.8 . . ?
C27B C28B H28D 109.8 . . ?
C27B C28B C29B 109.6(5) . . ?
H28C C28B H28D 108.2 . . ?
C29B C28B H28C 109.8 . . ?
C29B C28B H28D 109.8 . . ?
C28B C29B H29C 108.6 . . ?
C28B C29B H29D 108.6 . . ?
H29C C29B H29D 107.6 . . ?
C30B C29B C28B 114.7(6) . . ?
C30B C29B H29C 108.6 . . ?
C30B C29B H29D 108.6 . . ?
C29B C30B H30D 109.5 . . ?
C29B C30B H30E 109.5 . . ?
C29B C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
N7B C31B H31C 108.3 . . ?
N7B C31B H31D 108.3 . . ?
H31C C31B H31D 107.4 . . ?
C32B C31B N7B 115.9(4) . . ?
C32B C31B H31C 108.3 . . ?
C32B C31B H31D 108.3 . . ?
C31B C32B H32C 109.5 . . ?
C31B C32B H32D 109.5 . . ?
C31B C32B C33B 110.9(5) . . ?
H32C C32B H32D 108.1 . . ?
C33B C32B H32C 109.5 . . ?
C33B C32B H32D 109.5 . . ?
C32B C33B H33C 109.3 . . ?
C32B C33B H33D 109.3 . . ?
H33C C33B H33D 108 . . ?
C34B C33B C32B 111.5(5) . . ?
C34B C33B H33C 109.3 . . ?
C34B C33B H33D 109.3 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
N7B C35B H35C 108.5 . . ?
N7B C35B H35D 108.5 . . ?
N7B C35B C36B 115.2(4) . . ?
H35C C35B H35D 107.5 . . ?
C36B C35B H35C 108.5 . . ?
C36B C35B H35D 108.5 . . ?
C35B C36B H36C 109.5 . . ?
C35B C36B H36D 109.5 . . ?
H36C C36B H36D 108.1 . . ?
C37B C36B C35B 110.6(5) . . ?
C37B C36B H36C 109.5 . . ?
C37B C36B H36D 109.5 . . ?
C36B C37B H37C 109.2 . . ?
C36B C37B H37D 109.2 . . ?
C36B C37B C38B 111.9(5) . . ?
H37C C37B H37D 107.9 . . ?
C38B C37B H37C 109.2 . . ?
C38B C37B H37D 109.2 . . ?
C37B C38B H38D 109.5 . . ?
C37B C38B H38E 109.5 . . ?
C37B C38B H38F 109.5 . . ?
H38D C38B H38E 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
N7B C39B H39C 108.4 . . ?
N7B C39B H39D 108.4 . . ?
N7B C39B C40B 115.3(5) . . ?
H39C C39B H39D 107.5 . . ?
C40B C39B H39C 108.4 . . ?
C40B C39B H39D 108.4 . . ?
C39B C40B H40C 109.3 . . ?
C39B C40B H40D 109.3 . . ?
H40C C40B H40D 108 . . ?
C41B C40B C39B 111.6(7) . . ?
C41B C40B H40C 109.3 . . ?
C41B C40B H40D 109.3 . . ?
C40B C41B H41C 105.4 . . ?
C40B C41B H41D 105.4 . . ?
C40B C41B C42B 127.5(12) . . ?
H41C C41B H41D 106 . . ?
C42B C41B H41C 105.4 . . ?
C42B C41B H41D 105.4 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42E 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
O1 P1 O2 110.7(2) . . ?
O1 P1 O3 102.9(5) . . ?
O1 P1 O4 113.8(3) . . ?
O3 P1 O2 107.5(2) . . ?
O4 P1 O2 110.8(4) . . ?
O4 P1 O3 110.7(3) . . ?
O1' P1 O2 109.3(2) . . ?
O1' P1 O4' 111.5(3) . . ?
O3' P1 O2 112.1(2) . . ?
O3' P1 O1' 111.0(4) . . ?
O3' P1 O4' 113.2(3) . . ?
O4' P1 O2 99.2(5) . . ?
P1 O2 H2 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3A N5A C4A C3A -176.3(5) . . . . ?
O3A N5A C4A C5A 7.1(8) . . . . ?
O4A N5A C4A C3A 5.7(8) . . . . ?
O4A N5A C4A C5A -170.9(6) . . . . ?
O5A N6A C24A C23A 174.2(6) . . . . ?
O5A N6A C24A C25A -4.6(9) . . . . ?
O6A N6A C24A C23A -6.1(9) . . . . ?
O6A N6A C24A C25A 175.1(6) . . . . ?
N1A C1A C2A C3A 175.3(4) . . . . ?
N1A C1A C6A C5A -176.7(4) . . . . ?
N2A C8A C9A C10A -179.8(4) . . . . ?
N2A C8A C13A C12A -180.0(4) . . . . ?
N3A C17A C18A C19A 179.1(4) . . . . ?
N4A C21A C22A C23A -178.8(5) . . . . ?
N4A C21A C26A C25A -179.2(4) . . . . ?
N5A C4A C5A C6A 176.9(4) . . . . ?
N6A C24A C25A C26A -179.3(5) . . . . ?
C1A N1A C7A O1A 11.7(7) . . . . ?
C1A N1A C7A N2A -168.0(4) . . . . ?
C1A C2A C3A C4A 3.1(8) . . . . ?
C2A C1A C6A C5A 1.7(7) . . . . ?
C2A C3A C4A N5A -178.2(5) . . . . ?
C2A C3A C4A C5A -1.8(8) . . . . ?
C3A C4A C5A C6A 0.4(8) . . . . ?
C4A C5A C6A C1A -0.4(7) . . . . ?
C6A C1A C2A C3A -3.0(7) . . . . ?
C7A N1A C1A C2A 20.8(7) . . . . ?
C7A N1A C1A C6A -160.9(4) . . . . ?
C7A N2A C8A C9A -4.5(7) . . . . ?
C7A N2A C8A C13A 175.4(4) . . . . ?
C8A N2A C7A O1A 3.4(7) . . . . ?
C8A N2A C7A N1A -176.8(4) . . . . ?
C8A C9A C10A C11A -0.8(7) . . . . ?
C9A C8A C13A C12A -0.1(7) . . . . ?
C9A C10A C11A C12A 1.0(7) . . . . ?
C9A C10A C11A C14A 178.4(4) . . . . ?
C10A C11A C12A C13A -0.7(7) . . . . ?
C10A C11A C14A C15A 151.3(4) . . . . ?
C10A C11A C14A C19A -29.1(7) . . . . ?
C11A C12A C13A C8A 0.3(8) . . . . ?
C11A C14A C15A C16A 178.3(4) . . . . ?
C11A C14A C19A C18A -178.3(4) . . . . ?
C12A C11A C14A C15A -31.5(7) . . . . ?
C12A C11A C14A C19A 148.2(5) . . . . ?
C13A C8A C9A C10A 0.3(6) . . . . ?
C14A C11A C12A C13A -178.1(4) . . . . ?
C14A C15A C16A C17A -0.8(7) . . . . ?
C15A C14A C19A C18A 1.3(7) . . . . ?
C15A C16A C17A N3A -178.9(4) . . . . ?
C15A C16A C17A C18A 2.9(7) . . . . ?
C16A C17A C18A C19A -2.9(7) . . . . ?
C17A N3A C20A O2A -3.2(7) . . . . ?
C17A N3A C20A N4A 176.4(4) . . . . ?
C17A C18A C19A C14A 0.8(8) . . . . ?
C19A C14A C15A C16A -1.3(7) . . . . ?
C20A N3A C17A C16A -168.5(4) . . . . ?
C20A N3A C17A C18A 9.6(7) . . . . ?
C20A N4A C21A C22A 2.7(7) . . . . ?
C20A N4A C21A C26A -178.6(4) . . . . ?
C21A N4A C20A O2A 0.7(7) . . . . ?
C21A N4A C20A N3A -178.9(4) . . . . ?
C21A C22A C23A C24A -2.5(8) . . . . ?
C22A C21A C26A C25A -0.4(7) . . . . ?
C22A C23A C24A N6A -178.6(5) . . . . ?
C22A C23A C24A C25A 0.2(9) . . . . ?
C23A C24A C25A C26A 1.9(8) . . . . ?
C24A C25A C26A C21A -1.8(8) . . . . ?
C26A C21A C22A C23A 2.5(7) . . . . ?
O3B N5B C4B C3B -3.6(7) . . . . ?
O3B N5B C4B C5B 174.3(5) . . . . ?
O4B N5B C4B C3B 176.4(6) . . . . ?
O4B N5B C4B C5B -5.6(9) . . . . ?
O5B N6B C24B C23B -0.5(6) . . . . ?
O5B N6B C24B C25B 177.8(5) . . . . ?
O6B N6B C24B C23B 179.5(4) . . . . ?
O6B N6B C24B C25B -2.1(7) . . . . ?
N1B C1B C2B C3B -176.3(4) . . . . ?
N1B C1B C6B C5B 177.1(5) . . . . ?
N2B C8B C9B C10B 177.0(4) . . . . ?
N2B C8B C13B C12B -178.6(4) . . . . ?
N3B C17B C18B C19B -180.0(4) . . . . ?
N4B C21B C22B C23B -176.6(4) . . . . ?
N4B C21B C26B C25B 176.9(5) . . . . ?
N5B C4B C5B C6B -177.4(5) . . . . ?
N6B C24B C25B C26B -175.6(5) . . . . ?
C1B N1B C7B O1B 5.5(7) . . . . ?
C1B N1B C7B N2B -177.5(4) . . . . ?
C1B C2B C3B C4B -0.6(8) . . . . ?
C2B C1B C6B C5B 1.3(8) . . . . ?
C2B C3B C4B N5B 178.4(5) . . . . ?
C2B C3B C4B C5B 0.5(8) . . . . ?
C3B C4B C5B C6B 0.5(8) . . . . ?
C4B C5B C6B C1B -1.4(9) . . . . ?
C6B C1B C2B C3B -0.4(7) . . . . ?
C7B N1B C1B C2B -164.4(4) . . . . ?
C7B N1B C1B C6B 19.9(7) . . . . ?
C7B N2B C8B C9B -178.5(4) . . . . ?
C7B N2B C8B C13B 1.0(7) . . . . ?
C8B N2B C7B O1B -8.2(7) . . . . ?
C8B N2B C7B N1B 174.9(4) . . . . ?
C8B C9B C10B C11B 3.9(7) . . . . ?
C9B C8B C13B C12B 0.8(6) . . . . ?
C9B C10B C11B C12B -3.6(7) . . . . ?
C9B C10B C11B C14B 178.0(4) . . . . ?
C10B C11B C12B C13B 1.9(6) . . . . ?
C10B C11B C14B C15B 152.6(4) . . . . ?
C10B C11B C14B C19B -25.7(6) . . . . ?
C11B C12B C13B C8B -0.6(6) . . . . ?
C11B C14B C15B C16B -178.8(4) . . . . ?
C11B C14B C19B C18B 177.6(4) . . . . ?
C12B C11B C14B C15B -25.8(6) . . . . ?
C12B C11B C14B C19B 156.0(4) . . . . ?
C13B C8B C9B C10B -2.4(7) . . . . ?
C14B C11B C12B C13B -179.7(4) . . . . ?
C14B C15B C16B C17B 2.3(6) . . . . ?
C15B C14B C19B C18B -0.8(7) . . . . ?
C15B C16B C17B N3B 179.0(4) . . . . ?
C15B C16B C17B C18B -2.9(6) . . . . ?
C16B C17B C18B C19B 1.8(6) . . . . ?
C17B N3B C20B O2B -7.5(7) . . . . ?
C17B N3B C20B N4B 174.6(4) . . . . ?
C17B C18B C19B C14B 0.1(7) . . . . ?
C19B C14B C15B C16B -0.4(6) . . . . ?
C20B N3B C17B C16B -4.2(6) . . . . ?
C20B N3B C17B C18B 177.7(4) . . . . ?
C20B N4B C21B C22B 174.4(4) . . . . ?
C20B N4B C21B C26B -5.3(7) . . . . ?
C21B N4B C20B O2B 9.2(7) . . . . ?
C21B N4B C20B N3B -172.9(4) . . . . ?
C21B C22B C23B C24B -0.5(6) . . . . ?
C22B C21B C26B C25B -2.8(7) . . . . ?
C22B C23B C24B N6B 175.9(4) . . . . ?
C22B C23B C24B C25B -2.4(7) . . . . ?
C23B C24B C25B C26B 2.7(8) . . . . ?
C24B C25B C26B C21B 0.0(8) . . . . ?
C26B C21B C22B C23B 3.1(6) . . . . ?
N7A C27A C28A C29A 176.3(5) . . . . ?
N7A C31A C32A C33A -179.3(4) . . . . ?
N7A C35A C36A C37A -179.2(5) . . . . ?
N7A C39A C40A C41A -177.1(4) . . . . ?
C27A N7A C31A C32A -68.0(5) . . . . ?
C27A N7A C35A C36A 69.1(6) . . . . ?
C27A N7A C39A C40A 174.7(4) . . . . ?
C27A C28A C29A C30A 179.1(6) . . . . ?
C31A N7A C27A C28A 163.2(4) . . . . ?
C31A N7A C35A C36A -176.5(5) . . . . ?
C31A N7A C39A C40A 56.6(5) . . . . ?
C31A C32A C33A C34A -179.7(6) . . . . ?
C35A N7A C27A C28A -83.8(5) . . . . ?
C35A N7A C31A C32A 173.8(4) . . . . ?
C35A N7A C39A C40A -60.0(5) . . . . ?
C35A C36A C37A C38A -64.7(9) . . . . ?
C39A N7A C27A C28A 41.7(6) . . . . ?
C39A N7A C31A C32A 52.5(5) . . . . ?
C39A N7A C35A C36A -55.4(6) . . . . ?
C39A C40A C41A C42A 68.7(6) . . . . ?
N7B C27B C28B C29B 176.6(5) . . . . ?
N7B C31B C32B C33B -179.3(5) . . . . ?
N7B C35B C36B C37B -173.3(5) . . . . ?
N7B C39B C40B C41B -168.3(7) . . . . ?
C27B N7B C31B C32B -59.4(6) . . . . ?
C27B N7B C35B C36B 63.8(6) . . . . ?
C27B N7B C39B C40B 179.7(5) . . . . ?
C27B C28B C29B C30B -170.2(6) . . . . ?
C31B N7B C27B C28B -58.5(6) . . . . ?
C31B N7B C35B C36B -174.3(5) . . . . ?
C31B N7B C39B C40B 58.9(6) . . . . ?
C31B C32B C33B C34B -176.7(6) . . . . ?
C35B N7B C27B C28B 61.0(5) . . . . ?
C35B N7B C31B C32B 178.8(5) . . . . ?
C35B N7B C39B C40B -59.5(6) . . . . ?
C35B C36B C37B C38B -166.5(6) . . . . ?
C39B N7B C27B C28B -178.5(4) . . . . ?
C39B N7B C31B C32B 58.3(6) . . . . ?
C39B N7B C35B C36B -54.1(6) . . . . ?
C39B C40B C41B C42B -49.5(17) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: N,N-dimethylformamide'
