# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2017

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

data_20160613ngdnai_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1558696'
_audit_update_record             
;
2017-10-18 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C88 H86 N2 O8'
_chemical_formula_weight         1299.59

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'

_symmetry_cell_setting           Triclinic'
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.742(5)
_cell_length_b                   12.270(5)
_cell_length_c                   13.311(5)
_cell_angle_alpha                67.566(10)
_cell_angle_beta                 84.865(11)
_cell_angle_gamma                77.303(12)
_cell_volume                     1729.1(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2715
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      26.98

_exptl_crystal_description       BLOCK
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9786
_exptl_absorpt_correction_T_max  0.9832
_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_reflns_number            11312
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0972
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         25.01
_reflns_number_total             6022
_reflns_number_gt                3038
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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)+(0.0000P)²+25.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6022
_refine_ls_number_parameters     445
_refine_ls_number_restraints     278
_refine_ls_R_factor_all          0.3528
_refine_ls_R_factor_gt           0.2481
_refine_ls_wR_factor_ref         0.4987
_refine_ls_wR_factor_gt          0.4416
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.227
_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
C2 C -0.121(3) 1.437(3) 0.1258(19) 0.268(19) Uani 1 1 d DU . .
H2A H -0.2053 1.4466 0.1228 0.322 Uiso 1 1 calc R . .
H2B H -0.0886 1.3667 0.1087 0.322 Uiso 1 1 calc R . .
C3 C -0.098(2) 1.3960(17) 0.2442(15) 0.143(8) Uani 1 1 d DU . .
H3A H -0.1508 1.4563 0.2657 0.171 Uiso 1 1 calc R . .
H3B H -0.0208 1.4114 0.2456 0.171 Uiso 1 1 calc R . .
C4 C -0.0982(13) 1.2807(12) 0.3427(11) 0.083(4) Uani 1 1 d DU . .
H4A H -0.1316 1.3051 0.4021 0.100 Uiso 1 1 calc R . .
H4B H -0.1532 1.2408 0.3272 0.100 Uiso 1 1 calc R . .
C5 C 0.0841(13) 1.2072(14) 0.4526(11) 0.068(4) Uani 1 1 d U . .
C44 C 0.1792(13) 1.1182(13) 0.4964(10) 0.064(3) Uani 1 1 d U . .
C6 C 0.2593(14) 1.1305(14) 0.5633(11) 0.072(4) Uani 1 1 d U . .
H6 H 0.2451 1.1999 0.5791 0.086 Uiso 1 1 calc R . .
C7 C 0.3514(14) 1.0487(13) 0.6031(11) 0.071(4) Uani 1 1 d U . .
H7 H 0.3983 1.0607 0.6492 0.085 Uiso 1 1 calc R . .
C8 C 0.3839(13) 0.9453(14) 0.5813(11) 0.070(4) Uani 1 1 d U . .
H8 H 0.4524 0.8900 0.6089 0.084 Uiso 1 1 calc R . .
C9 C 0.3056(13) 0.9262(13) 0.5124(10) 0.060(3) Uani 1 1 d U . .
C10 C 0.2149(13) 1.0072(13) 0.4746(10) 0.060(3) Uani 1 1 d U . .
C11 C 0.1284(14) 1.0016(13) 0.3982(10) 0.065(3) Uani 1 1 d U . .
C12 C 0.0346(15) 1.0829(14) 0.3580(12) 0.073(4) Uani 1 1 d U . .
C13 C 0.1710(14) 0.8930(13) 0.3747(11) 0.069(4) Uani 1 1 d U . .
H13 H 0.1264 0.8815 0.3267 0.082 Uiso 1 1 calc R . .
C14 C 0.2598(14) 0.8137(13) 0.4109(11) 0.068(4) Uani 1 1 d U . .
H14 H 0.2744 0.7484 0.3890 0.081 Uiso 1 1 calc R . .
C15 C 0.3422(13) 0.8162(13) 0.4851(10) 0.065(3) Uani 1 1 d U . .
C16 C 0.4365(13) 0.7297(13) 0.5239(11) 0.065(4) Uani 1 1 d U . .
C17 C 0.4772(13) 0.6636(13) 0.6372(11) 0.064(3) Uani 1 1 d U . .
H17 H 0.4284 0.6805 0.6906 0.077 Uiso 1 1 calc R . .
C18 C 0.5689(13) 0.5881(13) 0.6695(11) 0.063(3) Uani 1 1 d U . .
C19 C 0.6579(13) 0.5553(13) 0.5929(11) 0.064(3) Uani 1 1 d U . .
C20 C 0.6166(14) 0.6145(13) 0.4825(11) 0.068(4) Uani 1 1 d U . .
H20 H 0.6633 0.5923 0.4304 0.082 Uiso 1 1 calc R . .
C21 C 0.5245(14) 0.6929(13) 0.4480(11) 0.068(4) Uani 1 1 d U . .
H21 H 0.5109 0.7286 0.3736 0.082 Uiso 1 1 calc R . .
C22 C 0.7508(13) 0.4767(13) 0.6449(11) 0.066(4) Uani 1 1 d U . .
C23 C 0.8650(12) 0.4218(12) 0.6136(11) 0.062(3) Uani 1 1 d U . .
H23 H 0.8832 0.4467 0.5399 0.074 Uiso 1 1 calc R . .
C24 C 0.9392(13) 0.3452(13) 0.6770(12) 0.065(4) Uani 1 1 d U . .
H24 H 1.0060 0.3140 0.6459 0.078 Uiso 1 1 calc R . .
C25 C 0.9335(13) 0.2964(13) 0.7999(12) 0.066(4) Uani 1 1 d U . .
C26 C 0.8179(11) 0.3608(12) 0.8285(11) 0.058(3) Uani 1 1 d U . .
H26 H 0.7995 0.3386 0.9021 0.069 Uiso 1 1 calc R . .
C27 C 0.7435(12) 0.4416(13) 0.7635(11) 0.059(3) Uani 1 1 d U . .
C28 C 0.6244(12) 0.5112(14) 0.7837(12) 0.071(4) Uani 1 1 d U . .
C29 C 0.6418(12) 0.6007(13) 0.8386(11) 0.070(4) Uani 1 1 d U . .
H29A H 0.5660 0.6467 0.8483 0.084 Uiso 1 1 calc R . .
H29B H 0.6755 0.5540 0.9100 0.084 Uiso 1 1 calc R . .
C30 C 0.7213(13) 0.6891(14) 0.7718(12) 0.078(4) Uani 1 1 d U . .
H30A H 0.6931 0.7290 0.6977 0.093 Uiso 1 1 calc R . .
H30B H 0.7998 0.6439 0.7698 0.093 Uiso 1 1 calc R . .
C31 C 0.7251(14) 0.7849(14) 0.8189(12) 0.075(4) Uani 1 1 d U . .
H31A H 0.7337 0.7451 0.8971 0.090 Uiso 1 1 calc R . .
H31B H 0.7943 0.8180 0.7908 0.090 Uiso 1 1 calc R . .
C32 C 0.6299(15) 0.8794(15) 0.7980(13) 0.087(5) Uani 1 1 d U . .
H32A H 0.6247 0.9250 0.7212 0.130 Uiso 1 1 calc R . .
H32B H 0.6389 0.9304 0.8351 0.130 Uiso 1 1 calc R . .
H32C H 0.5600 0.8483 0.8231 0.130 Uiso 1 1 calc R . .
C33 C 0.5442(12) 0.4302(13) 0.8605(11) 0.071(4) Uani 1 1 d U . .
H33A H 0.5829 0.3852 0.9300 0.085 Uiso 1 1 calc R . .
H33B H 0.4731 0.4811 0.8730 0.085 Uiso 1 1 calc R . .
C34 C 0.5117(13) 0.3415(13) 0.8182(11) 0.071(4) Uani 1 1 d U . .
H34A H 0.4664 0.3861 0.7523 0.085 Uiso 1 1 calc R . .
H34B H 0.5825 0.2946 0.8000 0.085 Uiso 1 1 calc R . .
C35 C 0.4419(14) 0.2572(15) 0.9008(13) 0.084(4) Uani 1 1 d U . .
H35A H 0.3727 0.3046 0.9208 0.101 Uiso 1 1 calc R . .
H35B H 0.4884 0.2110 0.9657 0.101 Uiso 1 1 calc R . .
C36 C 0.4041(16) 0.1688(16) 0.8581(15) 0.103(5) Uani 1 1 d U . .
H36A H 0.4696 0.1341 0.8238 0.155 Uiso 1 1 calc R . .
H36B H 0.3424 0.2117 0.8063 0.155 Uiso 1 1 calc R . .
H36C H 0.3770 0.1060 0.9178 0.155 Uiso 1 1 calc R . .
C37 C 1.0078(12) 0.2102(13) 0.8665(10) 0.063(3) Uani 1 1 d DU . .
C38 C 1.0812(12) 0.1137(13) 0.8405(12) 0.065(4) Uani 1 1 d U . .
H38 H 1.0771 0.1168 0.7700 0.079 Uiso 1 1 calc R . .
C39 C 1.1530(12) 0.0222(14) 0.9066(11) 0.066(4) Uani 1 1 d DU . .
C40 C 1.1707(14) 0.0108(15) 1.0154(12) 0.076(4) Uani 1 1 d DU . .
C41 C 1.0967(12) 0.1079(13) 1.0399(12) 0.067(4) Uani 1 1 d U . .
H41 H 1.0998 0.1051 1.1105 0.081 Uiso 1 1 calc R . .
C42 C 1.0287(13) 0.1957(14) 0.9762(10) 0.071(4) Uani 1 1 d DU . .
H42 H 0.9893 0.2551 1.0011 0.085 Uiso 1 1 calc R . .
C43 C 1.2180(14) -0.0717(14) 0.8760(15) 0.083(5) Uani 1 1 d DU . .
H43 H 1.2054 -0.0630 0.8051 0.100 Uiso 1 1 calc R . .
N1 N 0.0052(11) 1.1890(11) 0.3855(9) 0.078(3) Uani 1 1 d DU . .
O1 O -0.0417(13) 1.0792(14) 0.2969(9) 0.141(7) Uani 1 1 d . . .
O2 O 0.0535(10) 1.3030(14) 0.4679(10) 0.125(5) Uani 1 1 d . . .
O3 O 1.2913(11) -0.1667(13) 0.9289(9) 0.106(5) Uani 1 1 d D . .
O4 O 1.2412(12) -0.0763(14) 1.0844(10) 0.118(5) Uani 1 1 d . . .
H4 H 1.2758 -0.1224 1.0554 0.177 Uiso 1 1 calc R . .
C1 C -0.094(4) 1.541(3) 0.0249(17) 0.32(2) Uani 1 1 d DU . .
H1A H -0.1481 1.5578 -0.0315 0.482 Uiso 1 1 calc R . .
H1B H -0.0159 1.5193 0.0006 0.482 Uiso 1 1 calc R . .
H1C H -0.1007 1.6114 0.0422 0.482 Uiso 1 1 calc R . .


_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
C2 C3 1.490(11) . ?
C2 C1 1.524(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.518(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N1 1.449(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C44 1.37(2) . ?
C5 O2 1.240(18) . ?
C5 N1 1.448(18) . ?
C44 C6 1.420(19) . ?
C44 C10 1.464(18) . ?
C6 C7 1.30(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.375(18) . ?
C7 H7 0.9300 . ?
C8 C9 1.466(18) . ?
C8 H8 0.9300 . ?
C9 C10 1.275(18) . ?
C9 C15 1.494(18) . ?
C10 C11 1.530(19) . ?
C11 C12 1.31(2) . ?
C11 C13 1.456(18) . ?
C12 O1 1.282(19) . ?
C12 N1 1.446(18) . ?
C13 C14 1.246(19) . ?
C13 H13 0.9300 . ?
C14 C15 1.456(19) . ?
C14 H14 0.9300 . ?
C15 C16 1.336(19) . ?
C16 C17 1.478(19) . ?
C16 C21 1.500(18) . ?
C17 C18 1.242(18) . ?
C17 H17 0.9300 . ?
C18 C19 1.493(17) . ?
C18 C28 1.56(2) . ?
C19 C22 1.328(19) . ?
C19 C20 1.443(19) . ?
C20 C21 1.265(19) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.464(18) . ?
C22 C27 1.469(18) . ?
C23 C24 1.232(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.513(19) . ?
C24 H24 0.9300 . ?
C25 C37 1.297(18) . ?
C25 C26 1.509(18) . ?
C26 C27 1.262(18) . ?
C26 H26 0.9300 . ?
C27 C28 1.530(19) . ?
C28 C33 1.544(17) . ?
C28 C29 1.587(16) . ?
C29 C30 1.548(18) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.539(17) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.38(2) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.528(16) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.515(18) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 C36 1.56(2) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C42 1.440(10) . ?
C37 C38 1.440(18) . ?
C38 C39 1.306(19) . ?
C38 H38 0.9300 . ?
C39 C40 1.430(10) . ?
C39 C43 1.41(2) . ?
C40 O4 1.292(19) . ?
C40 C41 1.44(2) . ?
C41 C42 1.250(18) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 O3 1.280(10) . ?
C43 H43 0.9300 . ?
O4 H4 0.8200 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 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
C3 C2 C1 134.6(16) . . ?
C3 C2 H2A 103.5 . . ?
C1 C2 H2A 103.5 . . ?
C3 C2 H2B 103.5 . . ?
C1 C2 H2B 103.5 . . ?
H2A C2 H2B 105.3 . . ?
C2 C3 C4 136(2) . . ?
C2 C3 H3A 103.2 . . ?
C4 C3 H3A 103.2 . . ?
C2 C3 H3B 103.2 . . ?
C4 C3 H3B 103.2 . . ?
H3A C3 H3B 105.1 . . ?
N1 C4 C3 124.1(15) . . ?
N1 C4 H4A 106.3 . . ?
C3 C4 H4A 106.3 . . ?
N1 C4 H4B 106.3 . . ?
C3 C4 H4B 106.3 . . ?
H4A C4 H4B 106.4 . . ?
C44 C5 O2 126.7(15) . . ?
C44 C5 N1 118.9(13) . . ?
O2 C5 N1 114.3(15) . . ?
C5 C44 C6 121.5(13) . . ?
C5 C44 C10 125.4(13) . . ?
C6 C44 C10 112.9(14) . . ?
C7 C6 C44 122.5(14) . . ?
C7 C6 H6 118.8 . . ?
C44 C6 H6 118.8 . . ?
C6 C7 C8 123.8(14) . . ?
C6 C7 H7 118.1 . . ?
C8 C7 H7 118.1 . . ?
C7 C8 C9 117.0(15) . . ?
C7 C8 H8 121.5 . . ?
C9 C8 H8 121.5 . . ?
C10 C9 C8 118.4(12) . . ?
C10 C9 C15 124.2(13) . . ?
C8 C9 C15 117.3(14) . . ?
C9 C10 C44 125.5(13) . . ?
C9 C10 C11 124.0(12) . . ?
C44 C10 C11 110.5(13) . . ?
C12 C11 C13 126.1(14) . . ?
C12 C11 C10 125.6(13) . . ?
C13 C11 C10 108.3(14) . . ?
O1 C12 C11 127.2(16) . . ?
O1 C12 N1 112.7(16) . . ?
C11 C12 N1 120.1(14) . . ?
C14 C13 C11 128.1(14) . . ?
C14 C13 H13 115.9 . . ?
C11 C13 H13 115.9 . . ?
C13 C14 C15 124.5(14) . . ?
C13 C14 H14 117.7 . . ?
C15 C14 H14 117.7 . . ?
C16 C15 C14 123.8(13) . . ?
C16 C15 C9 125.4(12) . . ?
C14 C15 C9 110.9(14) . . ?
C15 C16 C17 129.7(13) . . ?
C15 C16 C21 120.5(13) . . ?
C17 C16 C21 109.7(14) . . ?
C18 C17 C16 127.7(13) . . ?
C18 C17 H17 116.1 . . ?
C16 C17 H17 116.1 . . ?
C17 C18 C19 122.2(14) . . ?
C17 C18 C28 134.2(13) . . ?
C19 C18 C28 103.6(13) . . ?
C22 C19 C20 137.4(13) . . ?
C22 C19 C18 111.9(12) . . ?
C20 C19 C18 110.6(14) . . ?
C21 C20 C19 127.8(14) . . ?
C21 C20 H20 116.1 . . ?
C19 C20 H20 116.1 . . ?
C20 C21 C16 121.7(14) . . ?
C20 C21 H21 119.1 . . ?
C16 C21 H21 119.1 . . ?
C19 C22 C23 136.0(13) . . ?
C19 C22 C27 113.7(12) . . ?
C23 C22 C27 110.2(14) . . ?
C24 C23 C22 125.4(13) . . ?
C24 C23 H23 117.3 . . ?
C22 C23 H23 117.3 . . ?
C23 C24 C25 127.2(13) . . ?
C23 C24 H24 116.4 . . ?
C25 C24 H24 116.4 . . ?
C37 C25 C24 127.1(12) . . ?
C37 C25 C26 127.1(12) . . ?
C24 C25 C26 105.6(13) . . ?
C27 C26 C25 127.2(12) . . ?
C27 C26 H26 116.4 . . ?
C25 C26 H26 116.4 . . ?
C26 C27 C22 123.8(12) . . ?
C26 C27 C28 131.2(12) . . ?
C22 C27 C28 104.5(13) . . ?
C33 C28 C29 106.6(10) . . ?
C33 C28 C27 113.8(12) . . ?
C29 C28 C27 109.6(11) . . ?
C33 C28 C18 112.4(11) . . ?
C29 C28 C18 108.1(12) . . ?
C27 C28 C18 106.3(11) . . ?
C30 C29 C28 113.5(10) . . ?
C30 C29 H29A 108.9 . . ?
C28 C29 H29A 108.9 . . ?
C30 C29 H29B 108.9 . . ?
C28 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C29 C30 C31 112.7(11) . . ?
C29 C30 H30A 109.1 . . ?
C31 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
C31 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C32 C31 C30 116.5(14) . . ?
C32 C31 H31A 108.2 . . ?
C30 C31 H31A 108.2 . . ?
C32 C31 H31B 108.2 . . ?
C30 C31 H31B 108.2 . . ?
H31A C31 H31B 107.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C28 114.4(10) . . ?
C34 C33 H33A 108.7 . . ?
C28 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C28 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C35 C34 C33 112.1(11) . . ?
C35 C34 H34A 109.2 . . ?
C33 C34 H34A 109.2 . . ?
C35 C34 H34B 109.2 . . ?
C33 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C34 C35 C36 113.1(12) . . ?
C34 C35 H35A 109.0 . . ?
C36 C35 H35A 109.0 . . ?
C34 C35 H35B 109.0 . . ?
C36 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C25 C37 C42 125.7(13) . . ?
C25 C37 C38 124.3(12) . . ?
C42 C37 C38 110.1(13) . . ?
C39 C38 C37 126.2(13) . . ?
C39 C38 H38 116.9 . . ?
C37 C38 H38 116.9 . . ?
C38 C39 C40 121.9(14) . . ?
C38 C39 C43 122.6(13) . . ?
C40 C39 C43 115.5(15) . . ?
O4 C40 C39 125.1(15) . . ?
O4 C40 C41 123.8(14) . . ?
C39 C40 C41 111.1(14) . . ?
C42 C41 C40 126.7(14) . . ?
C42 C41 H41 116.7 . . ?
C40 C41 H41 116.7 . . ?
C41 C42 C37 123.9(14) . . ?
C41 C42 H42 118.1 . . ?
C37 C42 H42 118.1 . . ?
O3 C43 C39 131.1(17) . . ?
O3 C43 H43 114.4 . . ?
C39 C43 H43 114.4 . . ?
C4 N1 C5 119.1(12) . . ?
C4 N1 C12 121.5(13) . . ?
C5 N1 C12 119.2(13) . . ?
C40 O4 H4 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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
C1 C2 C3 C4 -163(4) . . . . ?
C2 C3 C4 N1 96(4) . . . . ?
O2 C5 C44 C6 -3(2) . . . . ?
N1 C5 C44 C6 -179.6(11) . . . . ?
O2 C5 C44 C10 -178.4(12) . . . . ?
N1 C5 C44 C10 5.2(18) . . . . ?
C5 C44 C6 C7 -178.1(13) . . . . ?
C10 C44 C6 C7 -2.4(18) . . . . ?
C44 C6 C7 C8 3(2) . . . . ?
C6 C7 C8 C9 -3(2) . . . . ?
C7 C8 C9 C10 2.0(17) . . . . ?
C7 C8 C9 C15 177.9(11) . . . . ?
C8 C9 C10 C44 -1.8(18) . . . . ?
C15 C9 C10 C44 -177.4(11) . . . . ?
C8 C9 C10 C11 177.4(10) . . . . ?
C15 C9 C10 C11 1.9(19) . . . . ?
C5 C44 C10 C9 177.4(12) . . . . ?
C6 C44 C10 C9 1.9(17) . . . . ?
C5 C44 C10 C11 -1.9(16) . . . . ?
C6 C44 C10 C11 -177.5(10) . . . . ?
C9 C10 C11 C12 180.0(13) . . . . ?
C44 C10 C11 C12 -0.7(17) . . . . ?
C9 C10 C11 C13 -2.3(16) . . . . ?
C44 C10 C11 C13 177.0(10) . . . . ?
C13 C11 C12 O1 5(2) . . . . ?
C10 C11 C12 O1 -177.5(12) . . . . ?
C13 C11 C12 N1 -177.6(11) . . . . ?
C10 C11 C12 N1 -0.3(19) . . . . ?
C12 C11 C13 C14 179.8(15) . . . . ?
C10 C11 C13 C14 2.1(19) . . . . ?
C11 C13 C14 C15 -1(2) . . . . ?
C13 C14 C15 C16 179.4(14) . . . . ?
C13 C14 C15 C9 0.3(18) . . . . ?
C10 C9 C15 C16 -179.7(13) . . . . ?
C8 C9 C15 C16 4.7(18) . . . . ?
C10 C9 C15 C14 -0.7(17) . . . . ?
C8 C9 C15 C14 -176.3(10) . . . . ?
C14 C15 C16 C17 -129.6(14) . . . . ?
C9 C15 C16 C17 49(2) . . . . ?
C14 C15 C16 C21 55.1(17) . . . . ?
C9 C15 C16 C21 -126.1(13) . . . . ?
C15 C16 C17 C18 -175.9(14) . . . . ?
C21 C16 C17 C18 -0.1(18) . . . . ?
C16 C17 C18 C19 2(2) . . . . ?
C16 C17 C18 C28 179.9(12) . . . . ?
C17 C18 C19 C22 177.4(13) . . . . ?
C28 C18 C19 C22 -0.7(14) . . . . ?
C17 C18 C19 C20 -5.1(17) . . . . ?
C28 C18 C19 C20 176.8(10) . . . . ?
C22 C19 C20 C21 -176.8(16) . . . . ?
C18 C19 C20 C21 6.6(19) . . . . ?
C19 C20 C21 C16 -5(2) . . . . ?
C15 C16 C21 C20 177.3(13) . . . . ?
C17 C16 C21 C20 1.2(17) . . . . ?
C20 C19 C22 C23 9(3) . . . . ?
C18 C19 C22 C23 -174.0(13) . . . . ?
C20 C19 C22 C27 -176.6(14) . . . . ?
C18 C19 C22 C27 0.0(15) . . . . ?
C19 C22 C23 C24 -177.3(15) . . . . ?
C27 C22 C23 C24 8.6(18) . . . . ?
C22 C23 C24 C25 -4(2) . . . . ?
C23 C24 C25 C37 175.0(14) . . . . ?
C23 C24 C25 C26 0.2(18) . . . . ?
C37 C25 C26 C27 -177.0(13) . . . . ?
C24 C25 C26 C27 -2.2(17) . . . . ?
C25 C26 C27 C22 8(2) . . . . ?
C25 C26 C27 C28 179.4(11) . . . . ?
C19 C22 C27 C26 174.0(12) . . . . ?
C23 C22 C27 C26 -10.4(17) . . . . ?
C19 C22 C27 C28 0.8(14) . . . . ?
C23 C22 C27 C28 176.3(10) . . . . ?
C26 C27 C28 C33 -49.5(18) . . . . ?
C22 C27 C28 C33 123.0(11) . . . . ?
C26 C27 C28 C29 69.7(18) . . . . ?
C22 C27 C28 C29 -117.8(11) . . . . ?
C26 C27 C28 C18 -173.7(13) . . . . ?
C22 C27 C28 C18 -1.2(12) . . . . ?
C17 C18 C28 C33 58(2) . . . . ?
C19 C18 C28 C33 -123.9(11) . . . . ?
C17 C18 C28 C29 -59.0(19) . . . . ?
C19 C18 C28 C29 118.8(11) . . . . ?
C17 C18 C28 C27 -176.6(14) . . . . ?
C19 C18 C28 C27 1.2(12) . . . . ?
C33 C28 C29 C30 179.8(13) . . . . ?
C27 C28 C29 C30 56.2(17) . . . . ?
C18 C28 C29 C30 -59.2(16) . . . . ?
C28 C29 C30 C31 173.0(13) . . . . ?
C29 C30 C31 C32 -77.7(18) . . . . ?
C29 C28 C33 C34 176.9(13) . . . . ?
C27 C28 C33 C34 -62.2(17) . . . . ?
C18 C28 C33 C34 58.6(17) . . . . ?
C28 C33 C34 C35 175.0(14) . . . . ?
C33 C34 C35 C36 178.1(14) . . . . ?
C24 C25 C37 C42 153.8(12) . . . . ?
C26 C25 C37 C42 -33(2) . . . . ?
C24 C25 C37 C38 -27(2) . . . . ?
C26 C25 C37 C38 147.0(12) . . . . ?
C25 C37 C38 C39 -176.6(13) . . . . ?
C42 C37 C38 C39 3.0(18) . . . . ?
C37 C38 C39 C40 -3(2) . . . . ?
C37 C38 C39 C43 177.0(13) . . . . ?
C38 C39 C40 O4 -179.1(13) . . . . ?
C43 C39 C40 O4 1(2) . . . . ?
C38 C39 C40 C41 2.5(18) . . . . ?
C43 C39 C40 C41 -177.4(12) . . . . ?
O4 C40 C41 C42 178.4(14) . . . . ?
C39 C40 C41 C42 -3(2) . . . . ?
C40 C41 C42 C37 4(2) . . . . ?
C25 C37 C42 C41 176.1(14) . . . . ?
C38 C37 C42 C41 -3.4(18) . . . . ?
C38 C39 C43 O3 179.9(15) . . . . ?
C40 C39 C43 O3 0(2) . . . . ?
C3 C4 N1 C5 79(2) . . . . ?
C3 C4 N1 C12 -97.2(19) . . . . ?
C44 C5 N1 C4 177.4(11) . . . . ?
O2 C5 N1 C4 0.6(16) . . . . ?
C44 C5 N1 C12 -6.0(16) . . . . ?
O2 C5 N1 C12 177.2(11) . . . . ?
O1 C12 N1 C4 -2.3(16) . . . . ?
C11 C12 N1 C4 -179.8(12) . . . . ?
O1 C12 N1 C5 -178.8(10) . . . . ?
C11 C12 N1 C5 3.6(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.152
####################################################################### 
# 
# 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_20160613ngd_wu_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1558697'
_audit_update_record             
;
2017-06-27 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H29 Br O2'
_chemical_formula_weight         477.42

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'
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

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

_cell_length_a                   8.7300(7)
_cell_length_b                   10.4348(8)
_cell_length_c                   13.1284(13)
_cell_angle_alpha                99.414(3)
_cell_angle_beta                 97.111(3)
_cell_angle_gamma                97.020(2)
_cell_volume                     1158.30(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4533
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_T_max  0.6933
_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_reflns_number            8517
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4068
_reflns_number_gt                3421
_reflns_threshold_expression     >2sigma(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 > 2sigma(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)+(0.0529P)²+1.4229P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4068
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1198
_refine_ls_wR_factor_gt          0.1143
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
Br1 Br -0.21476(4) 0.01214(3) 0.02131(3) 0.04463(16) Uani 1 1 d . . .
C1 C -0.0028(4) 0.2491(3) 0.1244(3) 0.0325(8) Uani 1 1 d . . .
H1 H -0.0018 0.2672 0.0574 0.039 Uiso 1 1 calc R . .
C2 C -0.0879(4) 0.1347(3) 0.1414(3) 0.0364(9) Uani 1 1 d . . .
C3 C -0.0896(4) 0.1056(3) 0.2406(3) 0.0399(9) Uani 1 1 d . . .
H3 H -0.1455 0.0274 0.2495 0.048 Uiso 1 1 calc R . .
C4 C -0.0080(4) 0.1932(3) 0.3265(3) 0.0373(9) Uani 1 1 d . . .
H4 H -0.0098 0.1751 0.3934 0.045 Uiso 1 1 calc R . .
C5 C 0.0763(4) 0.3079(3) 0.3112(3) 0.0292(8) Uani 1 1 d . . .
C6 C 0.0802(4) 0.3348(3) 0.2106(3) 0.0267(7) Uani 1 1 d . . .
C7 C 0.1715(4) 0.4173(3) 0.3861(3) 0.0282(7) Uani 1 1 d . . .
C8 C 0.1972(4) 0.4426(4) 0.4942(3) 0.0335(8) Uani 1 1 d . . .
H8 H 0.1527 0.3832 0.5317 0.040 Uiso 1 1 calc R . .
C9 C 0.2903(4) 0.5577(4) 0.5456(3) 0.0336(8) Uani 1 1 d . . .
H9 H 0.3077 0.5745 0.6181 0.040 Uiso 1 1 calc R . .
C10 C 0.3586(4) 0.6491(3) 0.4922(3) 0.0275(7) Uani 1 1 d . . .
C11 C 0.3322(4) 0.6214(3) 0.3826(3) 0.0272(7) Uani 1 1 d . . .
H11 H 0.3784 0.6797 0.3450 0.033 Uiso 1 1 calc R . .
C12 C 0.2376(4) 0.5077(3) 0.3302(3) 0.0261(7) Uani 1 1 d . . .
C13 C 0.1836(4) 0.4646(3) 0.2132(3) 0.0268(7) Uani 1 1 d . . .
C14 C 0.0889(4) 0.5644(3) 0.1691(3) 0.0292(8) Uani 1 1 d . . .
H14A H 0.1604 0.6425 0.1669 0.035 Uiso 1 1 calc R . .
H14B H 0.0425 0.5267 0.0978 0.035 Uiso 1 1 calc R . .
C15 C -0.0402(4) 0.6053(3) 0.2303(3) 0.0294(7) Uani 1 1 d . . .
H15A H -0.1062 0.5271 0.2386 0.035 Uiso 1 1 calc R . .
H15B H 0.0067 0.6518 0.2994 0.035 Uiso 1 1 calc R . .
C16 C -0.1406(4) 0.6922(4) 0.1787(3) 0.0384(9) Uani 1 1 d . . .
H16A H -0.1924 0.6442 0.1112 0.046 Uiso 1 1 calc R . .
H16B H -0.0742 0.7684 0.1671 0.046 Uiso 1 1 calc R . .
C17 C -0.2630(5) 0.7378(4) 0.2440(3) 0.0440(10) Uani 1 1 d . . .
H17A H -0.3290 0.6627 0.2559 0.066 Uiso 1 1 calc R . .
H17B H -0.3249 0.7907 0.2076 0.066 Uiso 1 1 calc R . .
H17C H -0.2122 0.7886 0.3098 0.066 Uiso 1 1 calc R . .
C18 C 0.3214(4) 0.4462(3) 0.1513(3) 0.0294(7) Uani 1 1 d . . .
H18A H 0.2806 0.4237 0.0775 0.035 Uiso 1 1 calc R . .
H18B H 0.3899 0.5293 0.1626 0.035 Uiso 1 1 calc R . .
C19 C 0.4171(4) 0.3415(4) 0.1798(3) 0.0368(9) Uani 1 1 d . . .
H19A H 0.3539 0.2561 0.1571 0.044 Uiso 1 1 calc R . .
H19B H 0.4431 0.3552 0.2552 0.044 Uiso 1 1 calc R . .
C20 C 0.5678(4) 0.3411(4) 0.1318(3) 0.0437(10) Uani 1 1 d . . .
H20A H 0.6296 0.4274 0.1532 0.052 Uiso 1 1 calc R . .
H20B H 0.6272 0.2786 0.1596 0.052 Uiso 1 1 calc R . .
C21 C 0.5436(5) 0.3071(5) 0.0150(3) 0.0538(12) Uani 1 1 d . . .
H21A H 0.4819 0.2221 -0.0071 0.081 Uiso 1 1 calc R . .
H21B H 0.6429 0.3060 -0.0091 0.081 Uiso 1 1 calc R . .
H21C H 0.4904 0.3714 -0.0135 0.081 Uiso 1 1 calc R . .
C22 C 0.4570(4) 0.7738(3) 0.5502(3) 0.0272(7) Uani 1 1 d . . .
C23 C 0.4235(4) 0.8335(3) 0.6466(3) 0.0356(8) Uani 1 1 d . . .
H23 H 0.3377 0.7962 0.6726 0.043 Uiso 1 1 calc R . .
C24 C 0.5133(5) 0.9462(4) 0.7048(3) 0.0386(9) Uani 1 1 d . . .
H24 H 0.4878 0.9835 0.7687 0.046 Uiso 1 1 calc R . .
C25 C 0.6408(4) 1.0026(3) 0.6674(3) 0.0354(8) Uani 1 1 d . . .
C26 C 0.6749(4) 0.9474(3) 0.5695(3) 0.0332(8) Uani 1 1 d . . .
C27 C 0.5805(4) 0.8322(3) 0.5124(3) 0.0316(8) Uani 1 1 d . . .
H27 H 0.6032 0.7956 0.4475 0.038 Uiso 1 1 calc R . .
C28 C 0.8052(4) 1.0063(4) 0.5268(3) 0.0423(9) Uani 1 1 d . . .
H28 H 0.8203 0.9679 0.4604 0.051 Uiso 1 1 calc R . .
O1 O 0.8979(3) 1.1037(3) 0.5717(2) 0.0503(7) Uani 1 1 d . . .
O2 O 0.7299(4) 1.1110(3) 0.7262(2) 0.0496(7) Uani 1 1 d . . .
H2 H 0.8049 1.1319 0.6974 0.074 Uiso 1 1 calc R . .


_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
Br1 C2 1.977(4) . ?
C1 C6 1.383(5) . ?
C1 C2 1.391(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(6) . ?
C3 C4 1.385(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(5) . ?
C5 C7 1.469(5) . ?
C6 C13 1.526(4) . ?
C7 C8 1.385(5) . ?
C7 C12 1.400(5) . ?
C8 C9 1.385(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.393(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.404(5) . ?
C10 C22 1.501(5) . ?
C11 C12 1.384(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.525(5) . ?
C13 C18 1.546(5) . ?
C13 C14 1.547(5) . ?
C14 C15 1.526(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.516(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.523(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.521(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.527(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.498(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C27 1.361(5) . ?
C22 C23 1.398(5) . ?
C23 C24 1.383(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.377(5) . ?
C24 H24 0.9300 . ?
C25 O2 1.353(4) . ?
C25 C26 1.402(5) . ?
C26 C27 1.413(5) . ?
C26 C28 1.444(5) . ?
C27 H27 0.9300 . ?
C28 O1 1.233(4) . ?
C28 H28 0.9300 . ?
O2 H2 0.8200 . ?

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
C6 C1 C2 117.7(4) . . ?
C6 C1 H1 121.2 . . ?
C2 C1 H1 121.2 . . ?
C3 C2 C1 121.9(3) . . ?
C3 C2 Br1 118.8(3) . . ?
C1 C2 Br1 119.3(3) . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 120.6(3) . . ?
C4 C5 C7 130.9(3) . . ?
C6 C5 C7 108.4(3) . . ?
C1 C6 C5 120.9(3) . . ?
C1 C6 C13 128.1(3) . . ?
C5 C6 C13 111.1(3) . . ?
C8 C7 C12 120.2(3) . . ?
C8 C7 C5 131.4(3) . . ?
C12 C7 C5 108.4(3) . . ?
C9 C8 C7 118.9(3) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 122.2(3) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
C9 C10 C11 118.1(3) . . ?
C9 C10 C22 120.9(3) . . ?
C11 C10 C22 121.0(3) . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C7 120.2(3) . . ?
C11 C12 C13 128.7(3) . . ?
C7 C12 C13 111.0(3) . . ?
C12 C13 C6 101.0(3) . . ?
C12 C13 C18 112.3(3) . . ?
C6 C13 C18 112.1(3) . . ?
C12 C13 C14 111.2(3) . . ?
C6 C13 C14 111.3(3) . . ?
C18 C13 C14 108.8(3) . . ?
C15 C14 C13 115.1(3) . . ?
C15 C14 H14A 108.5 . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C16 C15 C14 113.5(3) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 C17 112.5(3) . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C17 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
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 C13 114.8(3) . . ?
C19 C18 H18A 108.6 . . ?
C13 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
C13 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C18 C19 C20 113.8(3) . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C20 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 C19 114.3(3) . . ?
C21 C20 H20A 108.7 . . ?
C19 C20 H20A 108.7 . . ?
C21 C20 H20B 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
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 . . ?
C27 C22 C23 117.8(3) . . ?
C27 C22 C10 122.1(3) . . ?
C23 C22 C10 120.1(3) . . ?
C24 C23 C22 122.4(3) . . ?
C24 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
O2 C25 C24 118.9(3) . . ?
O2 C25 C26 121.5(3) . . ?
C24 C25 C26 119.6(3) . . ?
C25 C26 C27 119.3(3) . . ?
C25 C26 C28 120.9(3) . . ?
C27 C26 C28 119.8(3) . . ?
C22 C27 C26 121.4(3) . . ?
C22 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
O1 C28 C26 124.9(4) . . ?
O1 C28 H28 117.6 . . ?
C26 C28 H28 117.6 . . ?
C25 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
C6 C1 C2 C3 -0.6(5) . . . . ?
C6 C1 C2 Br1 177.7(2) . . . . ?
C1 C2 C3 C4 1.6(6) . . . . ?
Br1 C2 C3 C4 -176.7(3) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C3 C4 C5 C6 -0.4(5) . . . . ?
C3 C4 C5 C7 179.6(3) . . . . ?
C2 C1 C6 C5 -0.9(5) . . . . ?
C2 C1 C6 C13 179.0(3) . . . . ?
C4 C5 C6 C1 1.5(5) . . . . ?
C7 C5 C6 C1 -178.6(3) . . . . ?
C4 C5 C6 C13 -178.5(3) . . . . ?
C7 C5 C6 C13 1.5(4) . . . . ?
C4 C5 C7 C8 -4.8(6) . . . . ?
C6 C5 C7 C8 175.2(3) . . . . ?
C4 C5 C7 C12 177.7(3) . . . . ?
C6 C5 C7 C12 -2.3(4) . . . . ?
C12 C7 C8 C9 -0.6(5) . . . . ?
C5 C7 C8 C9 -177.9(3) . . . . ?
C7 C8 C9 C10 0.2(5) . . . . ?
C8 C9 C10 C11 -0.6(5) . . . . ?
C8 C9 C10 C22 179.1(3) . . . . ?
C9 C10 C11 C12 1.5(5) . . . . ?
C22 C10 C11 C12 -178.2(3) . . . . ?
C10 C11 C12 C7 -2.0(5) . . . . ?
C10 C11 C12 C13 174.6(3) . . . . ?
C8 C7 C12 C11 1.6(5) . . . . ?
C5 C7 C12 C11 179.4(3) . . . . ?
C8 C7 C12 C13 -175.6(3) . . . . ?
C5 C7 C12 C13 2.2(4) . . . . ?
C11 C12 C13 C6 -178.1(3) . . . . ?
C7 C12 C13 C6 -1.3(3) . . . . ?
C11 C12 C13 C18 62.2(4) . . . . ?
C7 C12 C13 C18 -120.9(3) . . . . ?
C11 C12 C13 C14 -60.0(4) . . . . ?
C7 C12 C13 C14 116.9(3) . . . . ?
C1 C6 C13 C12 179.9(3) . . . . ?
C5 C6 C13 C12 -0.2(3) . . . . ?
C1 C6 C13 C18 -60.3(4) . . . . ?
C5 C6 C13 C18 119.6(3) . . . . ?
C1 C6 C13 C14 61.7(4) . . . . ?
C5 C6 C13 C14 -118.3(3) . . . . ?
C12 C13 C14 C15 -48.9(4) . . . . ?
C6 C13 C14 C15 62.9(4) . . . . ?
C18 C13 C14 C15 -173.2(3) . . . . ?
C13 C14 C15 C16 -174.2(3) . . . . ?
C14 C15 C16 C17 -176.9(3) . . . . ?
C12 C13 C18 C19 61.5(4) . . . . ?
C6 C13 C18 C19 -51.4(4) . . . . ?
C14 C13 C18 C19 -174.9(3) . . . . ?
C13 C18 C19 C20 -170.1(3) . . . . ?
C18 C19 C20 C21 -64.5(5) . . . . ?
C9 C10 C22 C27 147.6(3) . . . . ?
C11 C10 C22 C27 -32.7(5) . . . . ?
C9 C10 C22 C23 -32.1(5) . . . . ?
C11 C10 C22 C23 147.6(3) . . . . ?
C27 C22 C23 C24 -1.8(5) . . . . ?
C10 C22 C23 C24 177.9(3) . . . . ?
C22 C23 C24 C25 0.0(6) . . . . ?
C23 C24 C25 O2 -178.4(3) . . . . ?
C23 C24 C25 C26 1.9(5) . . . . ?
O2 C25 C26 C27 178.4(3) . . . . ?
C24 C25 C26 C27 -2.0(5) . . . . ?
O2 C25 C26 C28 -1.3(5) . . . . ?
C24 C25 C26 C28 178.3(3) . . . . ?
C23 C22 C27 C26 1.8(5) . . . . ?
C10 C22 C27 C26 -178.0(3) . . . . ?
C25 C26 C27 C22 0.1(5) . . . . ?
C28 C26 C27 C22 179.8(3) . . . . ?
C25 C26 C28 O1 2.5(6) . . . . ?
C27 C26 C28 O1 -177.2(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_20160607ngdshu_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1558698'
_audit_update_record             
;
2017-06-27 deposited with the CCDC.
2017-10-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H53 N O2'
_chemical_formula_weight         675.91

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'

_symmetry_cell_setting           Triclinic'
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.417(3)
_cell_length_b                   14.259(4)
_cell_length_c                   14.489(4)
_cell_angle_alpha                100.327(4)
_cell_angle_beta                 110.851(4)
_cell_angle_gamma                112.865(4)
_cell_volume                     1888.0(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4008
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.39

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9804
_exptl_absorpt_correction_T_max  0.9846
_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_reflns_number            8467
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.01
_reflns_number_total             6447
_reflns_number_gt                5055
_reflns_threshold_expression     >2sigma(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 > 2sigma(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)+(0.0843P)²+1.1742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6447
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1611
_refine_ls_wR_factor_gt          0.1435
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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 -0.1925(2) -0.09609(18) -0.02637(17) 0.0259(5) Uani 1 1 d . . .
C2 C -0.1273(2) -0.12537(19) 0.05558(17) 0.0288(5) Uani 1 1 d . . .
H2 H -0.1488 -0.1978 0.0430 0.035 Uiso 1 1 calc R . .
C3 C -0.0309(2) -0.04660(18) 0.15530(17) 0.0274(5) Uani 1 1 d . . .
H3 H 0.0126 -0.0673 0.2092 0.033 Uiso 1 1 calc R . .
C4 C 0.0046(2) 0.06365(19) 0.17929(16) 0.0252(5) Uani 1 1 d . . .
C5 C -0.0637(2) 0.09107(19) 0.09666(17) 0.0266(5) Uani 1 1 d . . .
H5 H -0.0433 0.1633 0.1095 0.032 Uiso 1 1 calc R . .
C6 C -0.1623(2) 0.01211(19) -0.00542(17) 0.0266(5) Uani 1 1 d . . .
C7 C -0.2271(3) 0.0466(2) -0.08941(18) 0.0335(5) Uani 1 1 d . . .
H7 H -0.1996 0.1206 -0.0721 0.040 Uiso 1 1 calc R . .
C8 C 0.1120(2) 0.14732(18) 0.28696(16) 0.0238(5) Uani 1 1 d . . .
C9 C 0.0965(2) 0.23642(19) 0.32734(17) 0.0266(5) Uani 1 1 d . . .
H9 H 0.0177 0.2420 0.2860 0.032 Uiso 1 1 calc R . .
C10 C 0.1957(2) 0.31611(18) 0.42719(16) 0.0248(5) Uani 1 1 d . . .
H10 H 0.1842 0.3748 0.4528 0.030 Uiso 1 1 calc R . .
C11 C 0.3132(2) 0.30703(17) 0.48874(16) 0.0222(4) Uani 1 1 d . . .
C12 C 0.3311(2) 0.21901(17) 0.44930(16) 0.0216(4) Uani 1 1 d . . .
C13 C 0.2315(2) 0.14003(18) 0.35000(16) 0.0238(5) Uani 1 1 d . . .
H13 H 0.2435 0.0815 0.3246 0.029 Uiso 1 1 calc R . .
C14 C 0.4724(2) 0.23087(17) 0.52817(16) 0.0214(4) Uani 1 1 d . . .
C15 C 0.5275(2) 0.33519(17) 0.61907(16) 0.0209(4) Uani 1 1 d . . .
C16 C 0.4342(2) 0.37838(17) 0.59468(16) 0.0212(4) Uani 1 1 d . . .
C17 C 0.4654(2) 0.47451(17) 0.66608(16) 0.0238(5) Uani 1 1 d . . .
H17 H 0.4017 0.5017 0.6503 0.029 Uiso 1 1 calc R . .
C18 C 0.5919(2) 0.52946(17) 0.76073(16) 0.0243(5) Uani 1 1 d . . .
H18 H 0.6154 0.5952 0.8081 0.029 Uiso 1 1 calc R . .
C19 C 0.6842(2) 0.48607(17) 0.78500(16) 0.0217(4) Uani 1 1 d . . .
C20 C 0.6524(2) 0.38846(17) 0.71502(16) 0.0215(4) Uani 1 1 d . . .
H20 H 0.7141 0.3596 0.7325 0.026 Uiso 1 1 calc R . .
C21 C 0.4523(2) 0.13226(18) 0.56385(16) 0.0236(5) Uani 1 1 d . . .
H21A H 0.4193 0.0692 0.5032 0.028 Uiso 1 1 calc R . .
H21B H 0.5456 0.1484 0.6168 0.028 Uiso 1 1 calc R . .
C22 C 0.3484(2) 0.10089(18) 0.60971(17) 0.0253(5) Uani 1 1 d . . .
H22A H 0.2509 0.0697 0.5534 0.030 Uiso 1 1 calc R . .
H22B H 0.3695 0.1662 0.6620 0.030 Uiso 1 1 calc R . .
C23 C 0.3579(3) 0.0183(2) 0.66194(19) 0.0313(5) Uani 1 1 d . . .
H23A H 0.3474 -0.0433 0.6118 0.038 Uiso 1 1 calc R . .
H23B H 0.4525 0.0524 0.7228 0.038 Uiso 1 1 calc R . .
C24 C 0.2441(3) -0.0237(2) 0.6982(2) 0.0409(6) Uani 1 1 d . . .
H24A H 0.2554 0.0366 0.7493 0.061 Uiso 1 1 calc R . .
H24B H 0.2550 -0.0753 0.7300 0.061 Uiso 1 1 calc R . .
H24C H 0.1501 -0.0589 0.6381 0.061 Uiso 1 1 calc R . .
C25 C 0.5789(2) 0.24689(18) 0.48206(17) 0.0252(5) Uani 1 1 d . . .
H25A H 0.6702 0.2630 0.5379 0.030 Uiso 1 1 calc R . .
H25B H 0.5425 0.1782 0.4266 0.030 Uiso 1 1 calc R . .
C26 C 0.6065(3) 0.33706(19) 0.43594(18) 0.0294(5) Uani 1 1 d . . .
H26A H 0.6095 0.3987 0.4800 0.035 Uiso 1 1 calc R . .
H26B H 0.5273 0.3097 0.3653 0.035 Uiso 1 1 calc R . .
C27 C 0.7483(3) 0.3763(2) 0.4293(2) 0.0450(7) Uani 1 1 d . . .
H27A H 0.7567 0.4299 0.3956 0.054 Uiso 1 1 calc R . .
H27B H 0.8278 0.4130 0.5010 0.054 Uiso 1 1 calc R . .
C28 C 0.7620(4) 0.2882(3) 0.3700(3) 0.0572(9) Uani 1 1 d . . .
H28A H 0.7701 0.2414 0.4090 0.086 Uiso 1 1 calc R . .
H28B H 0.8464 0.3203 0.3611 0.086 Uiso 1 1 calc R . .
H28C H 0.6785 0.2462 0.3016 0.086 Uiso 1 1 calc R . .
C29 C 0.9518(2) 0.57875(17) 0.89266(16) 0.0215(4) Uani 1 1 d . . .
C30 C 0.9947(2) 0.56552(18) 0.81460(17) 0.0258(5) Uani 1 1 d . . .
H30 H 0.9273 0.5261 0.7433 0.031 Uiso 1 1 calc R . .
C31 C 1.1401(2) 0.61267(18) 0.84652(17) 0.0270(5) Uani 1 1 d . . .
H31 H 1.1695 0.6041 0.7949 0.032 Uiso 1 1 calc R . .
C32 C 1.2464(2) 0.67308(17) 0.95316(17) 0.0238(5) Uani 1 1 d . . .
C33 C 1.2002(2) 0.68545(17) 1.02907(16) 0.0227(5) Uani 1 1 d . . .
H33 H 1.2676 0.7243 1.1004 0.027 Uiso 1 1 calc R . .
C34 C 1.0540(2) 0.64038(16) 0.99948(15) 0.0204(4) Uani 1 1 d . . .
C35 C 0.9744(2) 0.64498(17) 1.05720(16) 0.0212(4) Uani 1 1 d . . .
C36 C 0.8278(2) 0.58549(17) 0.98278(16) 0.0215(4) Uani 1 1 d . . .
C37 C 0.7228(2) 0.57562(17) 1.01343(17) 0.0236(5) Uani 1 1 d . . .
H37 H 0.6257 0.5364 0.9640 0.028 Uiso 1 1 calc R . .
C38 C 0.7669(2) 0.62581(18) 1.11956(17) 0.0244(5) Uani 1 1 d . . .
H38 H 0.6973 0.6189 1.1410 0.029 Uiso 1 1 calc R . .
C39 C 0.9124(2) 0.68682(18) 1.19644(16) 0.0237(5) Uani 1 1 d . . .
C40 C 1.0156(2) 0.69542(17) 1.16394(16) 0.0225(4) Uani 1 1 d . . .
H40 H 1.1127 0.7350 1.2135 0.027 Uiso 1 1 calc R . .
C41 C 0.9518(3) 0.73480(19) 1.31387(17) 0.0284(5) Uani 1 1 d . . .
C42 C 1.1082(3) 0.8248(2) 1.38048(18) 0.0349(6) Uani 1 1 d . . .
H42A H 1.1701 0.7950 1.3788 0.052 Uiso 1 1 calc R . .
H42B H 1.1275 0.8544 1.4525 0.052 Uiso 1 1 calc R . .
H42C H 1.1257 0.8819 1.3522 0.052 Uiso 1 1 calc R . .
C43 C 0.8576(3) 0.7826(2) 1.32771(19) 0.0377(6) Uani 1 1 d . . .
H43A H 0.8698 0.8401 1.3000 0.057 Uiso 1 1 calc R . .
H43B H 0.8852 0.8116 1.4018 0.057 Uiso 1 1 calc R . .
H43C H 0.7585 0.7261 1.2900 0.057 Uiso 1 1 calc R . .
C44 C 0.9276(3) 0.6408(2) 1.3562(2) 0.0431(7) Uani 1 1 d . . .
H44A H 0.8291 0.5837 1.3148 0.065 Uiso 1 1 calc R . .
H44B H 0.9492 0.6679 1.4291 0.065 Uiso 1 1 calc R . .
H44C H 0.9895 0.6123 1.3509 0.065 Uiso 1 1 calc R . .
C45 C 1.4062(2) 0.72879(19) 0.98253(18) 0.0289(5) Uani 1 1 d . . .
C46 C 1.4371(3) 0.6666(2) 0.90522(19) 0.0335(5) Uani 1 1 d . . .
H46A H 1.5392 0.6994 0.9308 0.050 Uiso 1 1 calc R . .
H46B H 1.3927 0.6697 0.8366 0.050 Uiso 1 1 calc R . .
H46C H 1.3987 0.5916 0.8996 0.050 Uiso 1 1 calc R . .
C47 C 1.4521(3) 0.8450(2) 0.9820(2) 0.0425(6) Uani 1 1 d . . .
H47A H 1.4365 0.8851 1.0329 0.064 Uiso 1 1 calc R . .
H47B H 1.3961 0.8412 0.9125 0.064 Uiso 1 1 calc R . .
H47C H 1.5523 0.8815 1.0004 0.064 Uiso 1 1 calc R . .
C48 C 1.4971(2) 0.7350(2) 1.09328(19) 0.0370(6) Uani 1 1 d . . .
H48A H 1.4636 0.6628 1.0953 0.055 Uiso 1 1 calc R . .
H48B H 1.4886 0.7802 1.1454 0.055 Uiso 1 1 calc R . .
H48C H 1.5962 0.7660 1.1084 0.055 Uiso 1 1 calc R . .
N1 N 0.81432(18) 0.54382(14) 0.88213(13) 0.0226(4) Uani 1 1 d . . .
O1 O -0.28435(17) -0.17447(13) -0.12444(12) 0.0329(4) Uani 1 1 d . . .
H1 H -0.3163 -0.1475 -0.1656 0.049 Uiso 1 1 calc R . .
O2 O -0.31496(18) -0.01525(15) -0.18099(13) 0.0398(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.352(3) . ?
C1 C2 1.389(3) . ?
C1 C6 1.391(3) . ?
C2 C3 1.373(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.402(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(3) . ?
C4 C8 1.481(3) . ?
C5 C6 1.398(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.458(3) . ?
C7 O2 1.221(3) . ?
C7 H7 0.9300 . ?
C8 C13 1.402(3) . ?
C8 C9 1.403(3) . ?
C9 C10 1.382(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.404(3) . ?
C11 C16 1.462(3) . ?
C12 C13 1.375(3) . ?
C12 C14 1.531(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.524(3) . ?
C14 C21 1.546(3) . ?
C14 C25 1.547(3) . ?
C15 C20 1.383(3) . ?
C15 C16 1.399(3) . ?
C16 C17 1.388(3) . ?
C17 C18 1.380(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.392(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.392(3) . ?
C19 N1 1.418(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.518(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.527(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.522(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.530(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.538(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.485(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 N1 1.389(3) . ?
C29 C30 1.394(3) . ?
C29 C34 1.400(3) . ?
C30 C31 1.377(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.406(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.392(3) . ?
C32 C45 1.530(3) . ?
C33 C34 1.393(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.448(3) . ?
C35 C40 1.397(3) . ?
C35 C36 1.403(3) . ?
C36 C37 1.387(3) . ?
C36 N1 1.401(3) . ?
C37 C38 1.380(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.403(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.388(3) . ?
C39 C41 1.537(3) . ?
C40 H40 0.9300 . ?
C41 C42 1.522(3) . ?
C41 C43 1.529(3) . ?
C41 C44 1.541(3) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C46 1.527(3) . ?
C45 C48 1.533(3) . ?
C45 C47 1.534(3) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
O1 H1 0.8200 . ?

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 C2 118.5(2) . . ?
O1 C1 C6 122.0(2) . . ?
C2 C1 C6 119.4(2) . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 122.8(2) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 116.8(2) . . ?
C5 C4 C8 121.6(2) . . ?
C3 C4 C8 121.58(19) . . ?
C4 C5 C6 121.3(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 120.1(2) . . ?
C1 C6 C7 121.2(2) . . ?
C5 C6 C7 118.7(2) . . ?
O2 C7 C6 124.2(2) . . ?
O2 C7 H7 117.9 . . ?
C6 C7 H7 117.9 . . ?
C13 C8 C9 118.66(19) . . ?
C13 C8 C4 120.95(19) . . ?
C9 C8 C4 120.38(19) . . ?
C10 C9 C8 121.6(2) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 118.9(2) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C12 120.37(19) . . ?
C10 C11 C16 130.88(19) . . ?
C12 C11 C16 108.73(18) . . ?
C13 C12 C11 120.24(19) . . ?
C13 C12 C14 129.05(19) . . ?
C11 C12 C14 110.65(17) . . ?
C12 C13 C8 120.3(2) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
C15 C14 C12 100.88(16) . . ?
C15 C14 C21 112.26(16) . . ?
C12 C14 C21 113.61(17) . . ?
C15 C14 C25 110.62(17) . . ?
C12 C14 C25 111.70(16) . . ?
C21 C14 C25 107.74(16) . . ?
C20 C15 C16 120.03(19) . . ?
C20 C15 C14 128.69(19) . . ?
C16 C15 C14 111.26(17) . . ?
C17 C16 C15 120.68(19) . . ?
C17 C16 C11 130.89(19) . . ?
C15 C16 C11 108.43(18) . . ?
C18 C17 C16 119.45(19) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 C19 119.73(19) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 121.29(19) . . ?
C20 C19 N1 119.57(18) . . ?
C18 C19 N1 119.14(19) . . ?
C15 C20 C19 118.79(19) . . ?
C15 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C22 C21 C14 116.24(17) . . ?
C22 C21 H21A 108.2 . . ?
C14 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
C14 C21 H21B 108.2 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 C23 112.06(18) . . ?
C21 C22 H22A 109.2 . . ?
C23 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C24 C23 C22 113.1(2) . . ?
C24 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 . . ?
C24 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C14 115.88(17) . . ?
C26 C25 H25A 108.3 . . ?
C14 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
C14 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 C27 112.52(19) . . ?
C25 C26 H26A 109.1 . . ?
C27 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
C27 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
C28 C27 C26 114.7(2) . . ?
C28 C27 H27A 108.6 . . ?
C26 C27 H27A 108.6 . . ?
C28 C27 H27B 108.6 . . ?
C26 C27 H27B 108.6 . . ?
H27A C27 H27B 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 C29 C30 129.57(19) . . ?
N1 C29 C34 109.63(17) . . ?
C30 C29 C34 120.69(19) . . ?
C31 C30 C29 117.8(2) . . ?
C31 C30 H30 121.1 . . ?
C29 C30 H30 121.1 . . ?
C30 C31 C32 123.38(19) . . ?
C30 C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C33 C32 C31 117.38(19) . . ?
C33 C32 C45 121.81(19) . . ?
C31 C32 C45 120.69(19) . . ?
C32 C33 C34 120.8(2) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C33 C34 C29 119.88(18) . . ?
C33 C34 C35 133.59(19) . . ?
C29 C34 C35 106.49(18) . . ?
C40 C35 C36 119.54(19) . . ?
C40 C35 C34 133.39(19) . . ?
C36 C35 C34 107.06(18) . . ?
C37 C36 N1 130.12(19) . . ?
C37 C36 C35 121.09(19) . . ?
N1 C36 C35 108.79(18) . . ?
C38 C37 C36 118.0(2) . . ?
C38 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
C37 C38 C39 122.8(2) . . ?
C37 C38 H38 118.6 . . ?
C39 C38 H38 118.6 . . ?
C40 C39 C38 118.24(19) . . ?
C40 C39 C41 122.27(19) . . ?
C38 C39 C41 119.35(19) . . ?
C39 C40 C35 120.4(2) . . ?
C39 C40 H40 119.8 . . ?
C35 C40 H40 119.8 . . ?
C42 C41 C43 107.8(2) . . ?
C42 C41 C39 112.06(19) . . ?
C43 C41 C39 111.92(18) . . ?
C42 C41 C44 108.9(2) . . ?
C43 C41 C44 108.6(2) . . ?
C39 C41 C44 107.48(19) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C32 112.18(19) . . ?
C46 C45 C48 106.87(19) . . ?
C32 C45 C48 110.70(19) . . ?
C46 C45 C47 109.5(2) . . ?
C32 C45 C47 108.17(19) . . ?
C48 C45 C47 109.4(2) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C29 N1 C36 108.01(17) . . ?
C29 N1 C19 125.79(17) . . ?
C36 N1 C19 125.90(17) . . ?
C1 O1 H1 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
O1 C1 C2 C3 178.41(19) . . . . ?
C6 C1 C2 C3 -1.9(3) . . . . ?
C1 C2 C3 C4 0.7(3) . . . . ?
C2 C3 C4 C5 0.5(3) . . . . ?
C2 C3 C4 C8 -178.3(2) . . . . ?
C3 C4 C5 C6 -0.4(3) . . . . ?
C8 C4 C5 C6 178.44(19) . . . . ?
O1 C1 C6 C5 -178.31(19) . . . . ?
C2 C1 C6 C5 2.0(3) . . . . ?
O1 C1 C6 C7 -1.1(3) . . . . ?
C2 C1 C6 C7 179.2(2) . . . . ?
C4 C5 C6 C1 -0.9(3) . . . . ?
C4 C5 C6 C7 -178.2(2) . . . . ?
C1 C6 C7 O2 3.3(4) . . . . ?
C5 C6 C7 O2 -179.5(2) . . . . ?
C5 C4 C8 C13 -144.8(2) . . . . ?
C3 C4 C8 C13 34.0(3) . . . . ?
C5 C4 C8 C9 34.5(3) . . . . ?
C3 C4 C8 C9 -146.7(2) . . . . ?
C13 C8 C9 C10 -0.2(3) . . . . ?
C4 C8 C9 C10 -179.5(2) . . . . ?
C8 C9 C10 C11 -0.2(3) . . . . ?
C9 C10 C11 C12 0.8(3) . . . . ?
C9 C10 C11 C16 179.0(2) . . . . ?
C10 C11 C12 C13 -1.0(3) . . . . ?
C16 C11 C12 C13 -179.56(18) . . . . ?
C10 C11 C12 C14 176.34(18) . . . . ?
C16 C11 C12 C14 -2.2(2) . . . . ?
C11 C12 C13 C8 0.6(3) . . . . ?
C14 C12 C13 C8 -176.2(2) . . . . ?
C9 C8 C13 C12 0.0(3) . . . . ?
C4 C8 C13 C12 179.24(19) . . . . ?
C13 C12 C14 C15 179.3(2) . . . . ?
C11 C12 C14 C15 2.3(2) . . . . ?
C13 C12 C14 C21 -60.3(3) . . . . ?
C11 C12 C14 C21 122.63(19) . . . . ?
C13 C12 C14 C25 61.8(3) . . . . ?
C11 C12 C14 C25 -115.24(19) . . . . ?
C12 C14 C15 C20 179.76(19) . . . . ?
C21 C14 C15 C20 58.5(3) . . . . ?
C25 C14 C15 C20 -61.9(3) . . . . ?
C12 C14 C15 C16 -1.6(2) . . . . ?
C21 C14 C15 C16 -122.88(19) . . . . ?
C25 C14 C15 C16 116.74(19) . . . . ?
C20 C15 C16 C17 -0.2(3) . . . . ?
C14 C15 C16 C17 -178.94(19) . . . . ?
C20 C15 C16 C11 179.17(18) . . . . ?
C14 C15 C16 C11 0.4(2) . . . . ?
C10 C11 C16 C17 2.0(4) . . . . ?
C12 C11 C16 C17 -179.6(2) . . . . ?
C10 C11 C16 C15 -177.2(2) . . . . ?
C12 C11 C16 C15 1.1(2) . . . . ?
C15 C16 C17 C18 1.9(3) . . . . ?
C11 C16 C17 C18 -177.3(2) . . . . ?
C16 C17 C18 C19 -2.1(3) . . . . ?
C17 C18 C19 C20 0.7(3) . . . . ?
C17 C18 C19 N1 179.50(18) . . . . ?
C16 C15 C20 C19 -1.3(3) . . . . ?
C14 C15 C20 C19 177.29(19) . . . . ?
C18 C19 C20 C15 1.0(3) . . . . ?
N1 C19 C20 C15 -177.79(18) . . . . ?
C15 C14 C21 C22 59.2(2) . . . . ?
C12 C14 C21 C22 -54.4(2) . . . . ?
C25 C14 C21 C22 -178.72(17) . . . . ?
C14 C21 C22 C23 -168.87(18) . . . . ?
C21 C22 C23 C24 -173.92(19) . . . . ?
C15 C14 C25 C26 -60.4(2) . . . . ?
C12 C14 C25 C26 51.1(2) . . . . ?
C21 C14 C25 C26 176.53(18) . . . . ?
C14 C25 C26 C27 159.3(2) . . . . ?
C25 C26 C27 C28 54.8(3) . . . . ?
N1 C29 C30 C31 177.3(2) . . . . ?
C34 C29 C30 C31 1.6(3) . . . . ?
C29 C30 C31 C32 -0.1(3) . . . . ?
C30 C31 C32 C33 -0.4(3) . . . . ?
C30 C31 C32 C45 -176.5(2) . . . . ?
C31 C32 C33 C34 -0.7(3) . . . . ?
C45 C32 C33 C34 175.41(19) . . . . ?
C32 C33 C34 C29 2.1(3) . . . . ?
C32 C33 C34 C35 -175.3(2) . . . . ?
N1 C29 C34 C33 -179.12(19) . . . . ?
C30 C29 C34 C33 -2.6(3) . . . . ?
N1 C29 C34 C35 -1.1(2) . . . . ?
C30 C29 C34 C35 175.46(19) . . . . ?
C33 C34 C35 C40 -0.9(4) . . . . ?
C29 C34 C35 C40 -178.6(2) . . . . ?
C33 C34 C35 C36 178.0(2) . . . . ?
C29 C34 C35 C36 0.3(2) . . . . ?
C40 C35 C36 C37 -0.2(3) . . . . ?
C34 C35 C36 C37 -179.22(19) . . . . ?
C40 C35 C36 N1 179.60(18) . . . . ?
C34 C35 C36 N1 0.6(2) . . . . ?
N1 C36 C37 C38 -180.0(2) . . . . ?
C35 C36 C37 C38 -0.2(3) . . . . ?
C36 C37 C38 C39 0.8(3) . . . . ?
C37 C38 C39 C40 -0.9(3) . . . . ?
C37 C38 C39 C41 -176.7(2) . . . . ?
C38 C39 C40 C35 0.5(3) . . . . ?
C41 C39 C40 C35 176.13(19) . . . . ?
C36 C35 C40 C39 0.1(3) . . . . ?
C34 C35 C40 C39 178.8(2) . . . . ?
C40 C39 C41 C42 21.6(3) . . . . ?
C38 C39 C41 C42 -162.7(2) . . . . ?
C40 C39 C41 C43 142.9(2) . . . . ?
C38 C39 C41 C43 -41.5(3) . . . . ?
C40 C39 C41 C44 -97.9(3) . . . . ?
C38 C39 C41 C44 77.7(3) . . . . ?
C33 C32 C45 C46 153.4(2) . . . . ?
C31 C32 C45 C46 -30.6(3) . . . . ?
C33 C32 C45 C48 34.2(3) . . . . ?
C31 C32 C45 C48 -149.9(2) . . . . ?
C33 C32 C45 C47 -85.7(3) . . . . ?
C31 C32 C45 C47 90.3(2) . . . . ?
C30 C29 N1 C36 -174.7(2) . . . . ?
C34 C29 N1 C36 1.4(2) . . . . ?
C30 C29 N1 C19 -0.8(3) . . . . ?
C34 C29 N1 C19 175.31(18) . . . . ?
C37 C36 N1 C29 178.5(2) . . . . ?
C35 C36 N1 C29 -1.2(2) . . . . ?
C37 C36 N1 C19 4.7(4) . . . . ?
C35 C36 N1 C19 -175.09(18) . . . . ?
C20 C19 N1 C29 55.4(3) . . . . ?
C18 C19 N1 C29 -123.4(2) . . . . ?
C20 C19 N1 C36 -131.8(2) . . . . ?
C18 C19 N1 C36 49.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.053
