# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_0644_010115_mh_dibrpd1_0m
_audit_block_doi                 10.5517/cc1j2j9f
_database_code_depnum_ccdc_archive 'CCDC 1402604'
_audit_update_record             
;
2015-05-23 deposited with the CCDC.
2017-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H24 Br2 N2 O8'
_chemical_formula_sum            'C34 H24 Br2 N2 O8'
_chemical_formula_weight         748.37

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_HALL  '-P 1 '

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

_cell_length_a                   4.8146(7)
_cell_length_b                   9.1602(14)
_cell_length_c                   17.672(3)
_cell_angle_alpha                76.925(5)
_cell_angle_beta                 84.870(5)
_cell_angle_gamma                75.057(5)
_cell_volume                     733.11(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4884
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      30.09

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      1.694
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             376
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5386
_exptl_absorpt_correction_T_max  0.7654
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10852
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2566
_reflns_number_gt                2065
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0710P)²+0.8752P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    CONSTR
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2566
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1463
_refine_ls_wR_factor_gt          0.1260
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.1459(10) 0.6841(5) 0.3028(3) 0.0552(11) Uani 1 1 d . . .
C2 C -0.1313(10) 0.7484(5) 0.3720(2) 0.0509(11) Uani 1 1 d . . .
C3 C 0.0040(8) 0.8675(5) 0.3681(2) 0.0409(9) Uani 1 1 d . B .
C4 C 0.1394(10) 0.9211(5) 0.2976(2) 0.0505(11) Uani 1 1 d . . .
C5 C 0.1501(10) 0.8512(5) 0.2296(2) 0.0504(10) Uani 1 1 d . . .
C6 C -0.0082(10) 0.6724(5) 0.1675(2) 0.0516(11) Uani 1 1 d . . .
H6A H 0.0297 0.7445 0.1207 0.062 Uiso 1 1 calc R . .
H6B H -0.1982 0.6569 0.1642 0.062 Uiso 1 1 calc R . .
C7 C 0.2147(11) 0.5185(6) 0.1723(3) 0.0635(13) Uani 1 1 d . . .
H7A H 0.4061 0.5347 0.1722 0.076 Uiso 1 1 calc R . .
H7B H 0.1843 0.4481 0.2205 0.076 Uiso 1 1 calc R . .
C8 C 0.1924(12) 0.4489(6) 0.1053(3) 0.0683(14) Uani 1 1 d . . .
H8A H 0.0072 0.4244 0.1073 0.082 Uiso 1 1 calc R . .
H8B H 0.2111 0.5209 0.0567 0.082 Uiso 1 1 calc R . .
C9 C 0.4558(11) 0.2421(6) 0.0502(3) 0.0627(13) Uani 1 1 d . . .
C10 C 0.6979(13) 0.1056(7) 0.0578(4) 0.0841(18) Uani 1 1 d . . .
H10A H 0.7921 0.0915 0.1055 0.126 Uiso 1 1 calc R . .
H10B H 0.8318 0.1196 0.0147 0.126 Uiso 1 1 calc R . .
H10C H 0.6286 0.0161 0.0581 0.126 Uiso 1 1 calc R . .
C11 C -0.2566(12) 0.6912(6) 0.4400(3) 0.0662(14) Uani 1 1 d . B .
H11 H -0.3476 0.6122 0.4423 0.079 Uiso 1 1 calc R . .
C12 C -0.2532(10) 0.7475(5) 0.5070(2) 0.0530(11) Uani 1 1 d . . .
C13 C -0.1337(9) 0.8714(5) 0.5065(2) 0.0425(9) Uani 1 1 d . B .
C14 C 0.0007(8) 0.9322(5) 0.4345(2) 0.0399(9) Uani 1 1 d . . .
C15 C -0.1363(10) 0.9425(5) 0.5728(2) 0.0495(10) Uani 1 1 d . . .
C16 C -0.2686(17) 0.8976(8) 0.6438(3) 0.102(3) Uani 1 1 d . B .
H16 H -0.3604 0.8179 0.6493 0.122 Uiso 1 1 calc R A 2
C17 C -0.2739(16) 0.9626(8) 0.7069(3) 0.095(2) Uani 1 1 d . . .
H17 H -0.3693 0.9273 0.7528 0.114 Uiso 1 1 calc R B .
N1 N -0.0019(8) 0.7387(4) 0.23581(19) 0.0478(8) Uani 1 1 d . . .
O1 O -0.2824(10) 0.5896(5) 0.3036(2) 0.0861(13) Uani 1 1 d . . .
O2 O 0.2855(8) 0.8892(4) 0.17007(19) 0.0731(11) Uani 1 1 d . . .
O3 O 0.4215(8) 0.3099(4) 0.1105(2) 0.0684(10) Uani 1 1 d . . .
O4 O 0.3013(12) 0.2873(6) -0.0026(3) 0.125(2) Uani 1 1 d . . .
Br1 Br -0.43596(15) 0.63473(7) 0.59247(3) 0.0681(3) Uani 0.8537(19) 1 d P B 1
Br1' Br -0.4996(10) 0.7365(5) 0.6653(2) 0.0747(16) Uani 0.1463(19) 1 d P B 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.211(5) . ?
C1 N1 1.376(6) . ?
C1 C2 1.487(5) . ?
C2 C11 1.353(6) . ?
C2 C3 1.395(6) . ?
C3 C4 1.401(6) . ?
C3 C14 1.425(5) . ?
C4 C17 1.368(7) 2_576 ?
C4 C5 1.476(5) . ?
C5 O2 1.217(5) . ?
C5 N1 1.390(6) . ?
C6 N1 1.474(5) . ?
C6 C7 1.526(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.490(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 O3 1.445(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 O4 1.178(6) . ?
C9 O3 1.327(5) . ?
C9 C10 1.463(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.396(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.397(6) . ?
C12 Br1 1.910(4) . ?
C13 C14 1.437(6) . ?
C13 C15 1.461(5) . ?
C14 C15 1.437(6) 2_576 ?
C15 C16 1.382(7) . ?
C15 C14 1.437(6) 2_576 ?
C16 C17 1.372(7) . ?
C16 Br1' 2.019(6) . ?
C16 H16 0.9300 . ?
C17 C4 1.368(7) 2_576 ?
C17 H17 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 N1 120.3(4) . . ?
O1 C1 C2 122.3(4) . . ?
N1 C1 C2 117.4(4) . . ?
C11 C2 C3 119.4(4) . . ?
C11 C2 C1 119.0(4) . . ?
C3 C2 C1 121.6(4) . . ?
C2 C3 C4 118.0(4) . . ?
C2 C3 C14 120.2(4) . . ?
C4 C3 C14 121.8(4) . . ?
C17 C4 C3 118.6(4) 2_576 . ?
C17 C4 C5 119.6(4) 2_576 . ?
C3 C4 C5 121.8(4) . . ?
O2 C5 N1 120.6(4) . . ?
O2 C5 C4 122.1(4) . . ?
N1 C5 C4 117.3(4) . . ?
N1 C6 C7 111.4(4) . . ?
N1 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
N1 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 110.5(4) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
O3 C8 C7 107.5(4) . . ?
O3 C8 H8A 110.2 . . ?
C7 C8 H8A 110.2 . . ?
O3 C8 H8B 110.2 . . ?
C7 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
O4 C9 O3 122.5(5) . . ?
O4 C9 C10 124.4(5) . . ?
O3 C9 C10 113.1(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C2 C11 C12 121.9(4) . . ?
C2 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C13 121.8(4) . . ?
C11 C12 Br1 110.4(3) . . ?
C13 C12 Br1 127.8(3) . . ?
C12 C13 C14 116.4(4) . . ?
C12 C13 C15 125.1(4) . . ?
C14 C13 C15 118.4(3) . . ?
C3 C14 C15 118.2(4) . 2_576 ?
C3 C14 C13 120.2(3) . . ?
C15 C14 C13 121.6(3) 2_576 . ?
C16 C15 C14 116.6(4) . 2_576 ?
C16 C15 C13 123.5(4) . . ?
C14 C15 C13 119.9(4) 2_576 . ?
C17 C16 C15 124.5(5) . . ?
C17 C16 Br1' 111.6(4) . . ?
C15 C16 Br1' 123.8(4) . . ?
C17 C16 H16 117.7 . . ?
C15 C16 H16 117.7 . . ?
Br1' C16 H16 6.9 . . ?
C4 C17 C16 120.2(5) 2_576 . ?
C4 C17 H17 119.9 2_576 . ?
C16 C17 H17 119.9 . . ?
C1 N1 C5 123.6(3) . . ?
C1 N1 C6 117.8(3) . . ?
C5 N1 C6 118.6(3) . . ?
C9 O3 C8 115.8(4) . . ?

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
O1 C1 C2 C11 5.1(8) . . . . ?
N1 C1 C2 C11 -176.3(5) . . . . ?
O1 C1 C2 C3 -173.9(5) . . . . ?
N1 C1 C2 C3 4.8(7) . . . . ?
C11 C2 C3 C4 178.1(5) . . . . ?
C1 C2 C3 C4 -3.0(7) . . . . ?
C11 C2 C3 C14 -2.3(7) . . . . ?
C1 C2 C3 C14 176.6(4) . . . . ?
C2 C3 C4 C17 -179.7(5) . . . 2_576 ?
C14 C3 C4 C17 0.7(8) . . . 2_576 ?
C2 C3 C4 C5 -2.2(7) . . . . ?
C14 C3 C4 C5 178.2(4) . . . . ?
C17 C4 C5 O2 3.1(8) 2_576 . . . ?
C3 C4 C5 O2 -174.4(5) . . . . ?
C17 C4 C5 N1 -176.9(5) 2_576 . . . ?
C3 C4 C5 N1 5.6(7) . . . . ?
N1 C6 C7 C8 176.5(4) . . . . ?
C6 C7 C8 O3 176.0(4) . . . . ?
C3 C2 C11 C12 -0.4(8) . . . . ?
C1 C2 C11 C12 -179.3(5) . . . . ?
C2 C11 C12 C13 3.5(9) . . . . ?
C2 C11 C12 Br1 -177.7(5) . . . . ?
C11 C12 C13 C14 -3.5(7) . . . . ?
Br1 C12 C13 C14 177.8(3) . . . . ?
C11 C12 C13 C15 176.3(5) . . . . ?
Br1 C12 C13 C15 -2.3(7) . . . . ?
C2 C3 C14 C15 -178.4(4) . . . 2_576 ?
C4 C3 C14 C15 1.2(6) . . . 2_576 ?
C2 C3 C14 C13 2.1(6) . . . . ?
C4 C3 C14 C13 -178.3(4) . . . . ?
C12 C13 C14 C3 0.8(6) . . . . ?
C15 C13 C14 C3 -179.1(4) . . . . ?
C12 C13 C14 C15 -178.7(4) . . . 2_576 ?
C15 C13 C14 C15 1.4(7) . . . 2_576 ?
C12 C13 C15 C16 -2.4(8) . . . . ?
C14 C13 C15 C16 177.5(6) . . . . ?
C12 C13 C15 C14 178.7(4) . . . 2_576 ?
C14 C13 C15 C14 -1.4(7) . . . 2_576 ?
C14 C15 C16 C17 -1.1(11) 2_576 . . . ?
C13 C15 C16 C17 180.0(7) . . . . ?
C14 C15 C16 Br1' 174.9(5) 2_576 . . . ?
C13 C15 C16 Br1' -4.0(10) . . . . ?
C15 C16 C17 C4 -0.8(13) . . . 2_576 ?
Br1' C16 C17 C4 -177.3(6) . . . 2_576 ?
O1 C1 N1 C5 177.5(5) . . . . ?
C2 C1 N1 C5 -1.1(7) . . . . ?
O1 C1 N1 C6 -3.1(7) . . . . ?
C2 C1 N1 C6 178.3(4) . . . . ?
O2 C5 N1 C1 176.2(5) . . . . ?
C4 C5 N1 C1 -3.8(7) . . . . ?
O2 C5 N1 C6 -3.2(7) . . . . ?
C4 C5 N1 C6 176.8(4) . . . . ?
C7 C6 N1 C1 -81.6(5) . . . . ?
C7 C6 N1 C5 97.8(5) . . . . ?
O4 C9 O3 C8 -3.6(8) . . . . ?
C10 C9 O3 C8 177.8(5) . . . . ?
C7 C8 O3 C9 -172.4(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C7 H7B Br1' 0.97 2.63 3.405(7) 137.1 2_566
C11 H11 Br1 0.93 2.92 3.827(4) 164.7 2_466
C16 H16 Br1' 0.93 1.10 2.019(6) 167.3 .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.129
####################################################################### 
# 
# 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_2d
_audit_block_doi                 10.5517/cc1j2jbg
_database_code_depnum_ccdc_archive 'CCDC 1402605'
_audit_update_record             
;
2016-07-23 deposited with the CCDC.
2017-01-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H54 N2 O4, 4(C7 H8)'
_chemical_formula_sum            'C104 H86 N2 O4'
_chemical_formula_weight         1427.74

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4627(5)
_cell_length_b                   11.8704(5)
_cell_length_c                   15.6450(6)
_cell_angle_alpha                76.067(2)
_cell_angle_beta                 89.834(2)
_cell_angle_gamma                72.7700(10)
_cell_volume                     1968.03(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4049
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      23.53

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      1.205
_exptl_crystal_density_method    NONE
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_F_000             756
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.072
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9891
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_reflns_number            31608
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.379
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             7652
_reflns_number_gt                3794
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0985P)²+0.2570P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7652
_refine_ls_number_parameters     472
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.2099
_refine_ls_wR_factor_gt          0.1717
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9158(3) 0.1783(3) 0.24456(16) 0.0401(7) Uani 1 1 d . . . . .
C2 C 0.8948(3) 0.0680(3) 0.24706(18) 0.0471(7) Uani 1 1 d . . . . .
C3 C 0.7948(3) 0.0286(3) 0.2977(2) 0.0627(9) Uani 1 1 d . . . . .
H3 H 0.7455 0.0976 0.3193 0.075 Uiso 1 1 calc R U . . .
C4 C 0.8493(5) -0.0765(4) 0.3775(3) 0.1058(15) Uani 1 1 d . . . . .
H4A H 0.9024 -0.0541 0.4132 0.159 Uiso 1 1 calc R U . . .
H4B H 0.7847 -0.0953 0.4116 0.159 Uiso 1 1 calc R U . . .
H4C H 0.8953 -0.1466 0.3583 0.159 Uiso 1 1 calc R U . . .
C5 C 0.7104(4) -0.0033(5) 0.2398(3) 0.1165(17) Uani 1 1 d . . . . .
H5A H 0.6485 -0.0276 0.2743 0.175 Uiso 1 1 calc R U . . .
H5B H 0.6722 0.0666 0.1923 0.175 Uiso 1 1 calc R U . . .
H5C H 0.7568 -0.0690 0.2161 0.175 Uiso 1 1 calc R U . . .
C6 C 0.9719(3) -0.0086(3) 0.2015(2) 0.0616(9) Uani 1 1 d . . . . .
H6 H 0.9597 -0.0826 0.2013 0.074 Uiso 1 1 calc R U . . .
C7 C 1.0643(3) 0.0229(3) 0.1574(2) 0.0655(10) Uani 1 1 d . . . . .
H7 H 1.1144 -0.0295 0.1273 0.079 Uiso 1 1 calc R U . . .
C8 C 1.0844(3) 0.1313(3) 0.1568(2) 0.0591(9) Uani 1 1 d . . . . .
H8 H 1.1488 0.1511 0.1271 0.071 Uiso 1 1 calc R U . . .
C9 C 1.0094(3) 0.2126(3) 0.20029(18) 0.0473(8) Uani 1 1 d . . . . .
C10 C 1.0336(3) 0.3309(3) 0.1990(2) 0.0578(9) Uani 1 1 d . . . . .
H10 H 0.9658 0.3795 0.2257 0.069 Uiso 1 1 calc R U . . .
C11 C 1.1524(4) 0.3096(4) 0.2538(3) 0.0888(13) Uani 1 1 d . . . . .
H11A H 1.1653 0.3865 0.2517 0.133 Uiso 1 1 calc R U . . .
H11B H 1.1462 0.2694 0.3139 0.133 Uiso 1 1 calc R U . . .
H11C H 1.2200 0.2597 0.2301 0.133 Uiso 1 1 calc R U . . .
C12 C 1.0378(4) 0.4035(4) 0.1057(2) 0.0851(12) Uani 1 1 d . . . . .
H12A H 1.0533 0.4781 0.1074 0.128 Uiso 1 1 calc R U . . .
H12B H 1.1019 0.3567 0.0773 0.128 Uiso 1 1 calc R U . . .
H12C H 0.9607 0.4216 0.0732 0.128 Uiso 1 1 calc R U . . .
C13 C 0.7222(3) 0.3324(3) 0.25029(17) 0.0412(7) Uani 1 1 d . . . . .
C14 C 0.6359(2) 0.4011(3) 0.30399(15) 0.0371(7) Uani 1 1 d . . . . .
C15 C 0.6726(2) 0.3930(2) 0.39201(15) 0.0341(6) Uani 1 1 d . . . . .
C16 C 0.7927(2) 0.3260(2) 0.42834(16) 0.0359(6) Uani 1 1 d . . . . .
C17 C 0.8783(3) 0.2513(3) 0.37825(17) 0.0427(7) Uani 1 1 d . . . . .
C18 C 0.5871(2) 0.4481(2) 0.44516(15) 0.0326(6) Uani 1 1 d . . . . .
C19 C 0.4642(2) 0.5108(2) 0.40983(16) 0.0344(6) Uani 1 1 d . . . . .
C20 C 0.4309(2) 0.5282(2) 0.31937(15) 0.0348(6) Uani 1 1 d . . . . .
C21 C 0.5193(2) 0.4683(3) 0.26940(16) 0.0386(7) Uani 1 1 d . . . . .
H21 H 0.4978 0.4744 0.2108 0.046 Uiso 1 1 calc R U . . .
C22 C 0.3766(2) 0.5595(2) 0.46610(15) 0.0326(6) Uani 1 1 d . . . . .
C23 C 0.2518(2) 0.6125(2) 0.43489(15) 0.0345(6) Uani 1 1 d . . . . .
C24 C 0.1708(2) 0.6751(3) 0.48807(16) 0.0377(7) Uani 1 1 d . . . . .
H24 H 0.0906 0.7182 0.4658 0.045 Uiso 1 1 calc R U . . .
C25 C 0.2158(2) 0.6125(2) 0.34644(16) 0.0359(6) Uani 1 1 d . . . . .
C26 C 0.3047(2) 0.5939(2) 0.28610(16) 0.0365(6) Uani 1 1 d . . . . .
C27 C 0.2662(3) 0.6439(3) 0.19194(16) 0.0386(7) Uani 1 1 d . . . . .
C28 C 0.3470(3) 0.6753(3) 0.12971(17) 0.0481(8) Uani 1 1 d . . . . .
H28 H 0.4287 0.6597 0.1480 0.058 Uiso 1 1 calc R U . . .
C29 C 0.3081(3) 0.7287(3) 0.04247(18) 0.0591(9) Uani 1 1 d . . . . .
H29 H 0.3634 0.7478 0.0022 0.071 Uiso 1 1 calc R U . . .
C30 C 0.1873(3) 0.7540(3) 0.01441(19) 0.0635(10) Uani 1 1 d . . . . .
H30 H 0.1617 0.7869 -0.0451 0.076 Uiso 1 1 calc R U . . .
C31 C 0.1049(3) 0.7305(3) 0.07449(18) 0.0533(8) Uani 1 1 d . . . . .
H31 H 0.0229 0.7511 0.0553 0.064 Uiso 1 1 calc R U . . .
C32 C 0.1410(3) 0.6765(2) 0.16392(16) 0.0400(7) Uani 1 1 d . . . . .
C33 C 0.0539(3) 0.6530(2) 0.22844(17) 0.0396(7) Uani 1 1 d . . . . .
C34 C 0.0897(2) 0.6257(2) 0.31922(16) 0.0367(7) Uani 1 1 d . . . . .
C35 C 0.0081(3) 0.5945(3) 0.38039(18) 0.0451(7) Uani 1 1 d . . . . .
H35 H 0.0325 0.5726 0.4403 0.054 Uiso 1 1 calc R U . . .
C36 C -0.1061(3) 0.5949(3) 0.3553(2) 0.0533(8) Uani 1 1 d . . . . .
H36 H -0.1584 0.5738 0.3975 0.064 Uiso 1 1 calc R U . . .
C37 C -0.1431(3) 0.6272(3) 0.2665(2) 0.0584(9) Uani 1 1 d . . . . .
H37 H -0.2214 0.6299 0.2487 0.070 Uiso 1 1 calc R U . . .
C38 C -0.0647(3) 0.6550(3) 0.20477(19) 0.0524(8) Uani 1 1 d . . . . .
H38 H -0.0907 0.6759 0.1452 0.063 Uiso 1 1 calc R U . . .
C40 C 0.5056(9) 0.8198(6) 0.4828(4) 0.198(5) Uani 1 1 d G . . . .
C41 C 0.3849(10) 0.8889(6) 0.4855(5) 0.256(8) Uani 1 1 d G . . . .
H41 H 0.3589 0.9126 0.5367 0.307 Uiso 1 1 calc R U . . .
C42 C 0.3030(5) 0.9227(5) 0.4118(8) 0.322(11) Uani 1 1 d G . . . .
H42 H 0.2223 0.9689 0.4136 0.386 Uiso 1 1 calc R U . . .
C43 C 0.3418(9) 0.8873(7) 0.3354(6) 0.230(6) Uani 1 1 d G . . . .
H43 H 0.2871 0.9098 0.2861 0.276 Uiso 1 1 calc R U . . .
C44 C 0.4625(11) 0.8182(6) 0.3327(4) 0.188(4) Uani 1 1 d G . . . .
H44 H 0.4885 0.7945 0.2815 0.226 Uiso 1 1 calc R U . . .
C45 C 0.5444(5) 0.7844(4) 0.4064(7) 0.140(2) Uani 1 1 d G . . . .
H45 H 0.6251 0.7382 0.4046 0.168 Uiso 1 1 calc R U . . .
C50 C 0.3798(5) 0.3031(7) 0.0334(4) 0.295(9) Uani 1 1 d DG . . . .
C51 C 0.3354(4) 0.2886(8) -0.0446(3) 0.218(6) Uani 1 1 d G . . . .
H51 H 0.3127 0.3542 -0.0941 0.262 Uiso 1 1 calc R U . . .
C52 C 0.3248(5) 0.1763(10) -0.0484(5) 0.365(13) Uani 1 1 d G . . . .
H52 H 0.2950 0.1667 -0.1006 0.438 Uiso 1 1 calc R U . . .
C53 C 0.3586(6) 0.0784(8) 0.0257(7) 0.308(9) Uani 1 1 d G . . . .
H53 H 0.3515 0.0032 0.0231 0.369 Uiso 1 1 calc R U . . .
C54 C 0.4031(5) 0.0928(7) 0.1036(5) 0.388(13) Uani 1 1 d G . . . .
H54 H 0.4257 0.0272 0.1532 0.465 Uiso 1 1 calc R U . . .
C55 C 0.4137(5) 0.2051(9) 0.1075(3) 0.269(10) Uani 1 1 d G . . . .
H55 H 0.4435 0.2147 0.1596 0.322 Uiso 1 1 calc R U . . .
C46 C 0.5790(13) 0.7930(10) 0.5584(6) 0.333(9) Uani 1 1 d . . . . .
H46A H 0.6601 0.7454 0.5504 0.499 Uiso 1 1 calc R U . . .
H46B H 0.5820 0.8673 0.5711 0.499 Uiso 1 1 calc R U . . .
H46C H 0.5463 0.7476 0.6066 0.499 Uiso 1 1 calc R U . . .
N1 N 0.8364(2) 0.2587(2) 0.29219(13) 0.0385(6) Uani 1 1 d . . . . .
O1 O 0.69633(19) 0.3356(2) 0.17455(12) 0.0623(7) Uani 1 1 d . . . . .
O2 O 0.97940(19) 0.1849(2) 0.40821(13) 0.0651(7) Uani 1 1 d . . . . .
C56 C 0.3773(9) 0.4058(10) 0.0371(10) 0.251(6) Uani 1 1 d D . . . .
H56A H 0.4105 0.4025 0.0942 0.376 Uiso 1 1 calc R U . . .
H56B H 0.4252 0.4371 -0.0076 0.376 Uiso 1 1 calc R U . . .
H56C H 0.2942 0.4581 0.0275 0.376 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C9 1.384(4) . ?
C1 C2 1.392(4) . ?
C1 N1 1.455(3) . ?
C2 C6 1.396(4) . ?
C2 C3 1.515(4) . ?
C3 C5 1.513(5) . ?
C3 C4 1.516(5) . ?
C3 H3 0.9800 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.358(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.371(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.398(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.504(4) . ?
C10 C12 1.514(5) . ?
C10 C11 1.534(5) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O1 1.211(3) . ?
C13 N1 1.400(3) . ?
C13 C14 1.482(4) . ?
C14 C21 1.372(4) . ?
C14 C15 1.414(3) . ?
C15 C18 1.399(3) . ?
C15 C16 1.410(4) . ?
C16 C24 1.370(3) 2_666 ?
C16 C17 1.476(4) . ?
C17 O2 1.212(3) . ?
C17 N1 1.405(3) . ?
C18 C22 1.425(3) 2_666 ?
C18 C19 1.425(3) . ?
C19 C20 1.417(3) . ?
C19 C22 1.419(3) . ?
C20 C21 1.407(4) . ?
C20 C26 1.454(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.415(3) . ?
C22 C18 1.425(3) 2_666 ?
C23 C24 1.411(4) . ?
C23 C25 1.445(3) . ?
C24 C16 1.370(3) 2_666 ?
C24 H24 0.9300 . ?
C25 C26 1.392(4) . ?
C25 C34 1.460(4) . ?
C26 C27 1.464(3) . ?
C27 C28 1.403(4) . ?
C27 C32 1.412(4) . ?
C28 C29 1.372(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.375(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.370(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.398(4) . ?
C31 H31 0.9300 . ?
C32 C33 1.456(4) . ?
C33 C38 1.401(4) . ?
C33 C34 1.412(3) . ?
C34 C35 1.399(4) . ?
C35 C36 1.367(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.381(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.366(4) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C40 C46 1.369(8) . ?
C40 C41 1.3900 . ?
C40 C45 1.3900 . ?
C41 C42 1.3900 . ?
C41 H41 0.9300 . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 C44 1.3900 . ?
C43 H43 0.9300 . ?
C44 C45 1.3900 . ?
C44 H44 0.9300 . ?
C45 H45 0.9300 . ?
C50 C56 1.226(8) . ?
C50 C51 1.3900 . ?
C50 C55 1.3900 . ?
C51 C52 1.3900 . ?
C51 H51 0.9300 . ?
C52 C53 1.3900 . ?
C52 H52 0.9300 . ?
C53 C54 1.3900 . ?
C53 H53 0.9300 . ?
C54 C55 1.3900 . ?
C54 H54 0.9300 . ?
C55 H55 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 C1 C2 122.7(3) . . ?
C9 C1 N1 119.5(3) . . ?
C2 C1 N1 117.7(2) . . ?
C1 C2 C6 117.2(3) . . ?
C1 C2 C3 122.8(3) . . ?
C6 C2 C3 120.0(3) . . ?
C5 C3 C2 112.1(3) . . ?
C5 C3 C4 111.0(4) . . ?
C2 C3 C4 110.7(3) . . ?
C5 C3 H3 107.6 . . ?
C2 C3 H3 107.6 . . ?
C4 C3 H3 107.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C2 121.3(3) . . ?
C7 C6 H6 119.4 . . ?
C2 C6 H6 119.4 . . ?
C6 C7 C8 120.5(3) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C7 C8 C9 121.0(3) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C1 C9 C8 117.3(3) . . ?
C1 C9 C10 122.8(3) . . ?
C8 C9 C10 119.9(3) . . ?
C9 C10 C12 111.8(3) . . ?
C9 C10 C11 111.4(3) . . ?
C12 C10 C11 110.1(3) . . ?
C9 C10 H10 107.8 . . ?
C12 C10 H10 107.8 . . ?
C11 C10 H10 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 N1 120.3(2) . . ?
O1 C13 C14 123.0(3) . . ?
N1 C13 C14 116.7(2) . . ?
C21 C14 C15 120.2(2) . . ?
C21 C14 C13 119.9(2) . . ?
C15 C14 C13 119.8(2) . . ?
C18 C15 C16 119.4(2) . . ?
C18 C15 C14 119.5(2) . . ?
C16 C15 C14 121.1(2) . . ?
C24 C16 C15 120.5(2) 2_666 . ?
C24 C16 C17 119.3(2) 2_666 . ?
C15 C16 C17 120.1(2) . . ?
O2 C17 N1 120.1(2) . . ?
O2 C17 C16 123.3(2) . . ?
N1 C17 C16 116.5(2) . . ?
C15 C18 C22 119.8(2) . 2_666 ?
C15 C18 C19 119.4(2) . . ?
C22 C18 C19 120.7(2) 2_666 . ?
C20 C19 C22 120.5(2) . . ?
C20 C19 C18 120.6(2) . . ?
C22 C19 C18 118.8(2) . . ?
C21 C20 C19 117.4(2) . . ?
C21 C20 C26 123.6(2) . . ?
C19 C20 C26 118.7(2) . . ?
C14 C21 C20 122.4(2) . . ?
C14 C21 H21 118.8 . . ?
C20 C21 H21 118.8 . . ?
C23 C22 C19 119.9(2) . . ?
C23 C22 C18 119.7(2) . 2_666 ?
C19 C22 C18 120.3(2) . 2_666 ?
C24 C23 C22 118.0(2) . . ?
C24 C23 C25 122.8(2) . . ?
C22 C23 C25 118.8(2) . . ?
C16 C24 C23 121.6(2) 2_666 . ?
C16 C24 H24 119.2 2_666 . ?
C23 C24 H24 119.2 . . ?
C26 C25 C23 119.3(2) . . ?
C26 C25 C34 118.6(2) . . ?
C23 C25 C34 122.1(2) . . ?
C25 C26 C20 118.7(2) . . ?
C25 C26 C27 118.1(2) . . ?
C20 C26 C27 123.2(2) . . ?
C28 C27 C32 118.2(2) . . ?
C28 C27 C26 121.9(2) . . ?
C32 C27 C26 119.3(2) . . ?
C29 C28 C27 121.4(3) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C31 C30 C29 119.8(3) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 121.7(3) . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C31 C32 C27 118.6(3) . . ?
C31 C32 C33 122.1(3) . . ?
C27 C32 C33 119.4(2) . . ?
C38 C33 C34 118.0(3) . . ?
C38 C33 C32 123.0(2) . . ?
C34 C33 C32 119.0(2) . . ?
C35 C34 C33 118.2(2) . . ?
C35 C34 C25 121.7(2) . . ?
C33 C34 C25 119.4(2) . . ?
C36 C35 C34 122.4(3) . . ?
C36 C35 H35 118.8 . . ?
C34 C35 H35 118.8 . . ?
C35 C36 C37 119.2(3) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C38 C37 C36 120.1(3) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C37 C38 C33 122.0(3) . . ?
C37 C38 H38 119.0 . . ?
C33 C38 H38 119.0 . . ?
C46 C40 C41 115.3(11) . . ?
C46 C40 C45 124.7(11) . . ?
C41 C40 C45 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C44 C43 C42 120.0 . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C45 C44 C43 120.0 . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C45 C40 120.0 . . ?
C44 C45 H45 120.0 . . ?
C40 C45 H45 120.0 . . ?
C56 C50 C51 118.3(8) . . ?
C56 C50 C55 121.4(8) . . ?
C51 C50 C55 120.0 . . ?
C50 C51 C52 120.0 . . ?
C50 C51 H51 120.0 . . ?
C52 C51 H51 120.0 . . ?
C51 C52 C53 120.0 . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C55 120.0 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C54 C55 C50 120.0 . . ?
C54 C55 H55 120.0 . . ?
C50 C55 H55 120.0 . . ?
C40 C46 H46A 109.5 . . ?
C40 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C40 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C13 N1 C17 125.3(2) . . ?
C13 N1 C1 117.4(2) . . ?
C17 N1 C1 117.2(2) . . ?
C50 C56 H56A 109.5 . . ?
C50 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C50 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

_refine_diff_density_max         0.563
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.042

_shelxl_version_number           2014-3

