# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_x16009
_database_code_depnum_ccdc_archive 'CCDC 1541264'
# CIF edited on-the-fly by script CIFFIX (S. Parkin, 2000-2014). 
# CIFFIX: http://xray.uky.edu/people/parkin/programs/ciffix 
_audit_update_record             
;
2017-03-30 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;

_audit_creation_method           'SHELXL-2014/7 and CIFFIX'

_shelx_SHELXL_version_number     2014/7

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H16 O5'
_chemical_formula_sum            'C16 H16 O5'
_chemical_formula_weight         288.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   9.2686(2)
_cell_length_b                   17.7615(3)
_cell_length_c                   8.3998(1)
_cell_angle_alpha                90
_cell_angle_beta                 96.374(1)
_cell_angle_gamma                90
_cell_volume                     1374.26(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90.0(2)
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      4.98
_cell_measurement_theta_max      68.32

_exptl_crystal_description       'irregular cut block'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_F_000             608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.864
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_absorpt_special_details   
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the x-ray beam cross section, absorption by the crystal 
mount etc.  These account, by and large, for much of the difference between 
estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;

_exptl_special_details           
; 
The crystal was mounted using polyisobutene oil on the tip of a fine glass 
fibre, which was fastened in a copper mounting pin with electrical solder. 
It was placed directly into the cold gas stream of a liquid-nitrogen based 
cryostat (Hope, 1994; Parkin & Hope, 1998). 
 
Diffraction data were collected with the crystal at 90K, which is standard 
practice in this laboratory for the majority of flash-cooled crystals. 
;

_diffrn_ambient_temperature      90.0(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus rotating anode'
_diffrn_measurement_device_type  'Bruker X8 Proteum diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 5.6
_diffrn_reflns_number            18486
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         4.801
_diffrn_reflns_theta_max         68.365
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997

_reflns_number_total             2504
_reflns_number_gt                2312
_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       'APEX2 (Bruker-AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker-AXS, 2006)'
_computing_data_reduction        'APEX2 (Bruker-AXS, 2006)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELX (Sheldrick, 2008) and CIFFIX (Parkin, 2013)'

_refine_special_details          
; 
Refinement progress was checked using Platon (Spek, 2009) and by 
an R-tensor (Parkin, 2000). The final model was further checked 
with the IUCr utility checkCIF. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0559P)²+0.4786P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2504
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.13097(9) 0.27241(5) 0.29643(10) 0.0184(2) Uani 1 1 d . . . . .
O2 O 0.60825(9) 0.44085(5) 0.53336(11) 0.0208(2) Uani 1 1 d . . . . .
O3 O 0.75655(10) 0.34173(5) 0.59738(11) 0.0234(2) Uani 1 1 d . . . . .
O4 O 0.97052(9) 0.43698(5) 0.71391(11) 0.0214(2) Uani 1 1 d . . . . .
O5 O 1.39230(9) 0.61044(5) 1.05647(11) 0.0210(2) Uani 1 1 d . . . . .
C1 C 0.49016(13) 0.39431(7) 0.47813(15) 0.0174(3) Uani 1 1 d . . . . .
C2 C 0.47136(13) 0.37326(7) 0.31919(15) 0.0189(3) Uani 1 1 d . . . . .
H2A H 0.5414 0.3866 0.2497 0.023 Uiso 1 1 calc R U . . .
C3 C 0.34956(13) 0.33251(7) 0.26203(14) 0.0178(3) Uani 1 1 d . . . . .
H3A H 0.3358 0.3176 0.1528 0.021 Uiso 1 1 calc R U . . .
C4 C 0.24673(13) 0.31323(7) 0.36455(14) 0.0153(3) Uani 1 1 d . . . . .
C5 C 0.26568(13) 0.33608(7) 0.52408(14) 0.0182(3) Uani 1 1 d . . . . .
H5A H 0.1951 0.3239 0.5937 0.022 Uiso 1 1 calc R U . . .
C6 C 0.38895(14) 0.37682(7) 0.58045(15) 0.0192(3) Uani 1 1 d . . . . .
H6A H 0.4033 0.3925 0.6892 0.023 Uiso 1 1 calc R U . . .
C7 C 0.02308(13) 0.24959(7) 0.39657(16) 0.0203(3) Uani 1 1 d . . . . .
H7A H -0.0505 0.2188 0.3342 0.030 Uiso 1 1 calc R U . . .
H7B H -0.0230 0.2943 0.4370 0.030 Uiso 1 1 calc R U . . .
H7C H 0.0691 0.2201 0.4870 0.030 Uiso 1 1 calc R U . . .
C8 C 0.73450(13) 0.40787(7) 0.59069(14) 0.0165(3) Uani 1 1 d . . . . .
C9 C 0.84028(13) 0.46985(7) 0.64345(15) 0.0175(3) Uani 1 1 d . . . . .
H9A H 0.8595 0.5008 0.5501 0.021 Uiso 1 1 calc R U . . .
H9B H 0.7990 0.5029 0.7219 0.021 Uiso 1 1 calc R U . . .
C10 C 1.06929(13) 0.48523(7) 0.79497(14) 0.0168(3) Uani 1 1 d . . . . .
C11 C 1.18673(13) 0.45102(7) 0.88521(15) 0.0180(3) Uani 1 1 d . . . . .
H11A H 1.1943 0.3977 0.8880 0.022 Uiso 1 1 calc R U . . .
C12 C 1.29181(13) 0.49436(7) 0.97037(14) 0.0179(3) Uani 1 1 d . . . . .
H12A H 1.3719 0.4707 1.0311 0.021 Uiso 1 1 calc R U . . .
C13 C 1.28145(13) 0.57288(7) 0.96807(14) 0.0166(3) Uani 1 1 d . . . . .
C14 C 1.16538(13) 0.60696(7) 0.87806(15) 0.0183(3) Uani 1 1 d . . . . .
H14A H 1.1579 0.6603 0.8753 0.022 Uiso 1 1 calc R U . . .
C15 C 1.05929(13) 0.56301(7) 0.79126(15) 0.0194(3) Uani 1 1 d . . . . .
H15A H 0.9799 0.5866 0.7294 0.023 Uiso 1 1 calc R U . . .
C16 C 1.38667(14) 0.69087(7) 1.05428(16) 0.0229(3) Uani 1 1 d . . . . .
H16A H 1.4735 0.7111 1.1169 0.034 Uiso 1 1 calc R U . . .
H16B H 1.3000 0.7079 1.1009 0.034 Uiso 1 1 calc R U . . .
H16C H 1.3827 0.7087 0.9435 0.034 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C4 1.3668(14) . ?
O1 C7 1.4347(14) . ?
O2 C8 1.3488(15) . ?
O2 C1 1.4084(14) . ?
O3 C8 1.1926(15) . ?
O4 C10 1.3776(14) . ?
O4 C9 1.4105(14) . ?
O5 C13 1.3721(15) . ?
O5 C16 1.4295(15) . ?
C1 C6 1.3763(18) . ?
C1 C2 1.3788(18) . ?
C2 C3 1.3815(18) . ?
C2 H2A 0.9500 . ?
C3 C4 1.3963(17) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3925(17) . ?
C5 C6 1.3904(17) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.5077(16) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.3846(18) . ?
C10 C11 1.3948(17) . ?
C11 C12 1.3777(17) . ?
C11 H11A 0.9500 . ?
C12 C13 1.3978(18) . ?
C12 H12A 0.9500 . ?
C13 C14 1.3838(17) . ?
C14 C15 1.3960(17) . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 O1 C7 118.05(9) . . ?
C8 O2 C1 118.31(9) . . ?
C10 O4 C9 116.15(9) . . ?
C13 O5 C16 117.06(9) . . ?
C6 C1 C2 121.46(11) . . ?
C6 C1 O2 119.04(11) . . ?
C2 C1 O2 119.22(11) . . ?
C1 C2 C3 119.29(11) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C2 C3 C4 120.10(11) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
O1 C4 C5 124.53(10) . . ?
O1 C4 C3 115.46(10) . . ?
C5 C4 C3 120.02(11) . . ?
C6 C5 C4 119.37(11) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C1 C6 C5 119.74(11) . . ?
C1 C6 H6A 120.1 . . ?
C5 C6 H6A 120.1 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 O2 125.59(11) . . ?
O3 C8 C9 127.07(11) . . ?
O2 C8 C9 107.33(10) . . ?
O4 C9 C8 108.63(10) . . ?
O4 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
O4 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
O4 C10 C15 124.78(11) . . ?
O4 C10 C11 115.68(11) . . ?
C15 C10 C11 119.54(11) . . ?
C12 C11 C10 120.19(11) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 120.45(11) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
O5 C13 C14 124.96(11) . . ?
O5 C13 C12 115.56(11) . . ?
C14 C13 C12 119.48(11) . . ?
C13 C14 C15 120.03(11) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C10 C15 C14 120.31(11) . . ?
C10 C15 H15A 119.8 . . ?
C14 C15 H15A 119.8 . . ?
O5 C16 H16A 109.5 . . ?
O5 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O5 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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
C8 O2 C1 C6 95.46(13) . . . . ?
C8 O2 C1 C2 -90.58(13) . . . . ?
C6 C1 C2 C3 -1.21(18) . . . . ?
O2 C1 C2 C3 -175.02(10) . . . . ?
C1 C2 C3 C4 0.22(18) . . . . ?
C7 O1 C4 C5 -1.77(17) . . . . ?
C7 O1 C4 C3 178.76(10) . . . . ?
C2 C3 C4 O1 -179.5(1) . . . . ?
C2 C3 C4 C5 1.00(18) . . . . ?
O1 C4 C5 C6 179.31(11) . . . . ?
C3 C4 C5 C6 -1.24(18) . . . . ?
C2 C1 C6 C5 0.97(18) . . . . ?
O2 C1 C6 C5 174.79(10) . . . . ?
C4 C5 C6 C1 0.27(18) . . . . ?
C1 O2 C8 O3 0.99(17) . . . . ?
C1 O2 C8 C9 -179.09(10) . . . . ?
C10 O4 C9 C8 -168.50(9) . . . . ?
O3 C8 C9 O4 -3.94(17) . . . . ?
O2 C8 C9 O4 176.13(9) . . . . ?
C9 O4 C10 C15 -10.15(16) . . . . ?
C9 O4 C10 C11 170.22(10) . . . . ?
O4 C10 C11 C12 179.81(10) . . . . ?
C15 C10 C11 C12 0.17(17) . . . . ?
C10 C11 C12 C13 0.40(17) . . . . ?
C16 O5 C13 C14 -0.17(16) . . . . ?
C16 O5 C13 C12 178.8(1) . . . . ?
C11 C12 C13 O5 -179.72(10) . . . . ?
C11 C12 C13 C14 -0.68(17) . . . . ?
O5 C13 C14 C15 179.34(11) . . . . ?
C12 C13 C14 C15 0.40(17) . . . . ?
O4 C10 C15 C14 179.94(11) . . . . ?
C11 C10 C15 C14 -0.45(18) . . . . ?
C13 C14 C15 C10 0.16(18) . . . . ?

_refine_diff_density_max         0.211
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_x17027
_database_code_depnum_ccdc_archive 'CCDC 1541265'
# CIF edited on-the-fly by script CIFFIX (S. Parkin, 2000-2016). 
# CIFFIX: http://xray.uky.edu/people/parkin/programs/ciffix 
_audit_update_record             
;
2017-03-30 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6

_shelx_SHELXL_version_number     2016/6

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H16 O5'
_chemical_formula_sum            'C16 H16 O5'
_chemical_formula_weight         288.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   5.8859(5)
_cell_length_b                   12.7775(10)
_cell_length_c                   19.1219(14)
_cell_angle_alpha                87.423(4)
_cell_angle_beta                 89.813(5)
_cell_angle_gamma                77.523(5)
_cell_volume                     1402.69(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    90.0(2)
_cell_measurement_reflns_used    4563
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      68.21

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.847
_shelx_estimated_absorpt_T_min   0.849
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008b)'
_exptl_absorpt_special_details   
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the x-ray beam cross section, absorption by the crystal 
mount etc.  These account, by and large, for much of the difference between 
estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;

_exptl_special_details           
; 
The crystal was mounted using polyisobutene oil on the tip of a fine glass 
fibre, which was fastened in a copper mounting pin with electrical solder. 
It was placed directly into the cold gas stream of a liquid-nitrogen based 
cryostat (Hope, 1994; Parkin & Hope, 1998). 
 
Diffraction data were collected with the crystal at 90K, which is standard 
practice in this laboratory for the majority of flash-cooled crystals. 
;

_diffrn_ambient_temperature      90.0(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus rotating anode'
_diffrn_measurement_device_type  'Bruker X8 Proteum diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 5.6
_diffrn_reflns_number            24835
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.313
_diffrn_reflns_theta_max         68.429
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.985

_reflns_number_total             24835
_reflns_number_gt                18988
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
_reflns_special_details          
; 
_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       'APEX2 (Bruker-AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker-AXS, 2006)'
_computing_data_reduction        'APEX2 (Bruker-AXS, 2006)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015b)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  
'SHELX (Sheldrick, 2008) and CIFFIX (Parkin, 2013)'

_refine_special_details          'Refined as a 2-component twin., Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1138P)²+0.4394P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick, 2015b)'
_refine_ls_extinction_coef       0.0022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         24835
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.2283
_refine_ls_wR_factor_gt          0.2084
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1A O 0.2150(5) 0.7404(2) 0.66458(14) 0.0344(7) Uani 1 1 d . . . . .
O2A O 0.5866(5) 0.6609(2) 0.59717(13) 0.0326(7) Uani 1 1 d . . . . .
O3A O 0.8031(5) 0.8072(2) 0.54137(14) 0.0372(7) Uani 1 1 d . . . . .
O4A O 1.0074(5) 0.6864(2) 0.46903(13) 0.0340(7) Uani 1 1 d . . . . .
O5A O 1.4437(5) 0.9738(2) 0.32655(13) 0.0362(7) Uani 1 1 d . . . . .
C1A C 0.2642(7) 0.6317(3) 0.66171(19) 0.0283(9) Uani 1 1 d . . . . .
C2A C 0.1354(7) 0.5634(3) 0.69255(19) 0.0329(10) Uani 1 1 d . . . . .
H2A H 0.001042 0.592094 0.718930 0.039 Uiso 1 1 calc R U . . .
C3A C 0.2010(8) 0.4540(4) 0.6852(2) 0.0367(10) Uani 1 1 d . . . . .
H3A H 0.111535 0.408013 0.706740 0.044 Uiso 1 1 calc R U . . .
C4A C 0.3939(7) 0.4109(3) 0.6471(2) 0.0355(10) Uani 1 1 d . . . . .
H4A H 0.436750 0.335648 0.641815 0.043 Uiso 1 1 calc R U . . .
C5A C 0.5273(7) 0.4788(3) 0.61603(19) 0.0329(9) Uani 1 1 d . . . . .
H5A H 0.661433 0.449542 0.589734 0.039 Uiso 1 1 calc R U . . .
C6A C 0.4641(7) 0.5876(3) 0.62362(19) 0.0298(9) Uani 1 1 d . . . . .
C7A C 0.0054(7) 0.7876(3) 0.7004(2) 0.0386(10) Uani 1 1 d . . . . .
H7A1 H -0.126753 0.764443 0.679765 0.058 Uiso 1 1 calc R U . . .
H7A2 H -0.019943 0.865988 0.695715 0.058 Uiso 1 1 calc R U . . .
H7A3 H 0.020077 0.764612 0.750035 0.058 Uiso 1 1 calc R U . . .
C8A C 0.7595(7) 0.6234(3) 0.54677(19) 0.0316(9) Uani 1 1 d . . . . .
H8A1 H 0.690836 0.592660 0.507437 0.038 Uiso 1 1 calc R U . . .
H8A2 H 0.885506 0.567166 0.568256 0.038 Uiso 1 1 calc R U . . .
C9A C 0.8535(7) 0.7184(3) 0.52109(19) 0.0309(9) Uani 1 1 d . . . . .
C10A C 1.1132(7) 0.7663(3) 0.43614(19) 0.0313(9) Uani 1 1 d . . . . .
C11A C 1.2588(7) 0.8144(3) 0.47255(19) 0.0340(9) Uani 1 1 d . . . . .
H11A H 1.282684 0.799088 0.521377 0.041 Uiso 1 1 calc R U . . .
C12A C 1.3713(7) 0.8858(3) 0.43763(19) 0.0328(9) Uani 1 1 d . . . . .
H12A H 1.471825 0.920224 0.462506 0.039 Uiso 1 1 calc R U . . .
C13A C 1.3366(7) 0.9069(3) 0.36606(19) 0.0309(9) Uani 1 1 d . . . . .
C14A C 1.1854(7) 0.8580(3) 0.3303(2) 0.0351(10) Uani 1 1 d . . . . .
H14A H 1.159138 0.873370 0.281569 0.042 Uiso 1 1 calc R U . . .
C15A C 1.0734(7) 0.7873(3) 0.3655(2) 0.0348(10) Uani 1 1 d . . . . .
H15A H 0.970077 0.753603 0.341310 0.042 Uiso 1 1 calc R U . . .
C16A C 1.5964(7) 1.0274(3) 0.3623(2) 0.0377(10) Uani 1 1 d . . . . .
H16A H 1.506247 1.077183 0.394801 0.057 Uiso 1 1 calc R U . . .
H16B H 1.672961 1.067385 0.328046 0.057 Uiso 1 1 calc R U . . .
H16C H 1.714221 0.974248 0.388412 0.057 Uiso 1 1 calc R U . . .
O1B O -0.3053(5) 0.7696(2) -0.14894(14) 0.0335(7) Uani 1 1 d . . . . .
O2B O 0.0783(5) 0.6767(2) -0.08788(13) 0.0327(7) Uani 1 1 d . . . . .
O3B O 0.2859(5) 0.8147(2) -0.02856(13) 0.0353(7) Uani 1 1 d . . . . .
O4B O 0.5010(5) 0.6830(2) 0.04177(13) 0.0337(7) Uani 1 1 d . . . . .
O5B O 0.9295(5) 0.9583(2) 0.18099(13) 0.0343(7) Uani 1 1 d . . . . .
C1B C -0.2510(7) 0.6606(3) -0.15123(19) 0.0286(9) Uani 1 1 d . . . . .
C2B C -0.3825(7) 0.6000(3) -0.18504(19) 0.0329(10) Uani 1 1 d . . . . .
H2B H -0.521501 0.634368 -0.209044 0.039 Uiso 1 1 calc R U . . .
C3B C -0.3109(7) 0.4891(3) -0.1838(2) 0.0351(10) Uani 1 1 d . . . . .
H3B H -0.401213 0.447955 -0.207273 0.042 Uiso 1 1 calc R U . . .
C4B C -0.1093(7) 0.4377(3) -0.14879(19) 0.0345(10) Uani 1 1 d . . . . .
H4B H -0.062881 0.361658 -0.147246 0.041 Uiso 1 1 calc R U . . .
C5B C 0.0253(7) 0.4990(3) -0.11566(19) 0.0324(9) Uani 1 1 d . . . . .
H5B H 0.165396 0.464499 -0.092257 0.039 Uiso 1 1 calc R U . . .
C6B C -0.0439(7) 0.6083(3) -0.11684(19) 0.0285(9) Uani 1 1 d . . . . .
C7B C -0.5114(7) 0.8242(3) -0.1857(2) 0.0389(10) Uani 1 1 d . . . . .
H7B1 H -0.499530 0.805698 -0.235015 0.058 Uiso 1 1 calc R U . . .
H7B2 H -0.528737 0.901811 -0.182590 0.058 Uiso 1 1 calc R U . . .
H7B3 H -0.647156 0.802280 -0.164841 0.058 Uiso 1 1 calc R U . . .
C8B C 0.2545(7) 0.6307(3) -0.03862(19) 0.0313(9) Uani 1 1 d . . . . .
H8B1 H 0.381782 0.580379 -0.061489 0.038 Uiso 1 1 calc R U . . .
H8B2 H 0.190469 0.590856 -0.000490 0.038 Uiso 1 1 calc R U . . .
C9B C 0.3436(7) 0.7225(3) -0.00999(19) 0.0297(9) Uani 1 1 d . . . . .
C10B C 0.6056(7) 0.7580(3) 0.0747(2) 0.0316(9) Uani 1 1 d . . . . .
C11B C 0.7480(7) 0.8120(3) 0.0372(2) 0.0342(10) Uani 1 1 d . . . . .
H11B H 0.770501 0.802145 -0.011517 0.041 Uiso 1 1 calc R U . . .
C12B C 0.8583(7) 0.8809(3) 0.0712(2) 0.0333(9) Uani 1 1 d . . . . .
H12B H 0.955909 0.919229 0.045951 0.040 Uiso 1 1 calc R U . . .
C13B C 0.8250(7) 0.8935(3) 0.14265(19) 0.0304(9) Uani 1 1 d . . . . .
C14B C 0.6796(7) 0.8387(3) 0.17918(19) 0.0335(9) Uani 1 1 d . . . . .
H14B H 0.656684 0.847978 0.227904 0.040 Uiso 1 1 calc R U . . .
C15B C 0.5680(7) 0.7710(3) 0.1453(2) 0.0332(9) Uani 1 1 d . . . . .
H15B H 0.467119 0.733862 0.170105 0.040 Uiso 1 1 calc R U . . .
C16B C 1.0812(7) 1.0162(3) 0.1447(2) 0.0377(10) Uani 1 1 d . . . . .
H16D H 1.206314 0.965473 0.122398 0.057 Uiso 1 1 calc R U . . .
H16E H 1.148338 1.057322 0.178001 0.057 Uiso 1 1 calc R U . . .
H16F H 0.992315 1.065364 0.108775 0.057 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
O1A C1A 1.360(4) . ?
O1A C7A 1.436(4) . ?
O2A C6A 1.378(4) . ?
O2A C8A 1.421(4) . ?
O3A C9A 1.191(5) . ?
O4A C9A 1.360(4) . ?
O4A C10A 1.428(4) . ?
O5A C13A 1.368(4) . ?
O5A C16A 1.433(4) . ?
C1A C2A 1.386(5) . ?
C1A C6A 1.406(5) . ?
C2A C3A 1.382(5) . ?
C2A H2A 0.9500 . ?
C3A C4A 1.372(6) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.403(5) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.373(5) . ?
C5A H5A 0.9500 . ?
C7A H7A1 0.9800 . ?
C7A H7A2 0.9800 . ?
C7A H7A3 0.9800 . ?
C8A C9A 1.502(5) . ?
C8A H8A1 0.9900 . ?
C8A H8A2 0.9900 . ?
C10A C11A 1.367(5) . ?
C10A C15A 1.376(5) . ?
C11A C12A 1.385(5) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.390(5) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.389(5) . ?
C14A C15A 1.380(5) . ?
C14A H14A 0.9500 . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
O1B C1B 1.363(4) . ?
O1B C7B 1.432(4) . ?
O2B C6B 1.381(4) . ?
O2B C8B 1.415(4) . ?
O3B C9B 1.191(5) . ?
O4B C9B 1.361(5) . ?
O4B C10B 1.416(4) . ?
O5B C13B 1.370(4) . ?
O5B C16B 1.436(4) . ?
C1B C2B 1.387(5) . ?
C1B C6B 1.407(5) . ?
C2B C3B 1.387(5) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.384(6) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.400(5) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.367(5) . ?
C5B H5B 0.9500 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B C9B 1.509(5) . ?
C8B H8B1 0.9900 . ?
C8B H8B2 0.9900 . ?
C10B C11B 1.376(5) . ?
C10B C15B 1.379(5) . ?
C11B C12B 1.386(5) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.391(5) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.386(5) . ?
C14B C15B 1.379(5) . ?
C14B H14B 0.9500 . ?
C15B H15B 0.9500 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1A O1A C7A 116.4(3) . . ?
C6A O2A C8A 116.4(3) . . ?
C9A O4A C10A 117.0(3) . . ?
C13A O5A C16A 117.2(3) . . ?
O1A C1A C2A 125.7(3) . . ?
O1A C1A C6A 115.5(3) . . ?
C2A C1A C6A 118.9(4) . . ?
C3A C2A C1A 120.4(4) . . ?
C3A C2A H2A 119.8 . . ?
C1A C2A H2A 119.8 . . ?
C4A C3A C2A 120.8(4) . . ?
C4A C3A H3A 119.6 . . ?
C2A C3A H3A 119.6 . . ?
C3A C4A C5A 119.5(4) . . ?
C3A C4A H4A 120.2 . . ?
C5A C4A H4A 120.2 . . ?
C6A C5A C4A 120.0(4) . . ?
C6A C5A H5A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C5A C6A O2A 124.6(3) . . ?
C5A C6A C1A 120.4(3) . . ?
O2A C6A C1A 115.0(4) . . ?
O1A C7A H7A1 109.5 . . ?
O1A C7A H7A2 109.5 . . ?
H7A1 C7A H7A2 109.5 . . ?
O1A C7A H7A3 109.5 . . ?
H7A1 C7A H7A3 109.5 . . ?
H7A2 C7A H7A3 109.5 . . ?
O2A C8A C9A 106.9(3) . . ?
O2A C8A H8A1 110.4 . . ?
C9A C8A H8A1 110.4 . . ?
O2A C8A H8A2 110.4 . . ?
C9A C8A H8A2 110.4 . . ?
H8A1 C8A H8A2 108.6 . . ?
O3A C9A O4A 124.9(4) . . ?
O3A C9A C8A 127.0(4) . . ?
O4A C9A C8A 108.1(3) . . ?
C11A C10A C15A 121.8(3) . . ?
C11A C10A O4A 121.1(3) . . ?
C15A C10A O4A 116.9(3) . . ?
C10A C11A C12A 119.4(3) . . ?
C10A C11A H11A 120.3 . . ?
C12A C11A H11A 120.3 . . ?
C11A C12A C13A 119.7(4) . . ?
C11A C12A H12A 120.1 . . ?
C13A C12A H12A 120.1 . . ?
O5A C13A C14A 115.9(3) . . ?
O5A C13A C12A 124.2(3) . . ?
C14A C13A C12A 119.8(3) . . ?
C15A C14A C13A 120.1(3) . . ?
C15A C14A H14A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C10A C15A C14A 119.1(4) . . ?
C10A C15A H15A 120.4 . . ?
C14A C15A H15A 120.4 . . ?
O5A C16A H16A 109.5 . . ?
O5A C16A H16B 109.5 . . ?
H16A C16A H16B 109.5 . . ?
O5A C16A H16C 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
C1B O1B C7B 116.5(3) . . ?
C6B O2B C8B 116.9(3) . . ?
C9B O4B C10B 116.7(3) . . ?
C13B O5B C16B 117.5(3) . . ?
O1B C1B C2B 124.9(4) . . ?
O1B C1B C6B 116.0(3) . . ?
C2B C1B C6B 119.1(4) . . ?
C3B C2B C1B 120.0(4) . . ?
C3B C2B H2B 120.0 . . ?
C1B C2B H2B 120.0 . . ?
C4B C3B C2B 120.7(4) . . ?
C4B C3B H3B 119.7 . . ?
C2B C3B H3B 119.7 . . ?
C3B C4B C5B 119.3(4) . . ?
C3B C4B H4B 120.4 . . ?
C5B C4B H4B 120.4 . . ?
C6B C5B C4B 120.3(4) . . ?
C6B C5B H5B 119.8 . . ?
C4B C5B H5B 119.8 . . ?
C5B C6B O2B 125.2(3) . . ?
C5B C6B C1B 120.5(4) . . ?
O2B C6B C1B 114.2(3) . . ?
O1B C7B H7B1 109.5 . . ?
O1B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
O1B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
O2B C8B C9B 106.4(3) . . ?
O2B C8B H8B1 110.4 . . ?
C9B C8B H8B1 110.4 . . ?
O2B C8B H8B2 110.4 . . ?
C9B C8B H8B2 110.4 . . ?
H8B1 C8B H8B2 108.6 . . ?
O3B C9B O4B 125.0(4) . . ?
O3B C9B C8B 126.4(4) . . ?
O4B C9B C8B 108.6(3) . . ?
C11B C10B C15B 121.8(3) . . ?
C11B C10B O4B 120.2(3) . . ?
C15B C10B O4B 117.9(3) . . ?
C10B C11B C12B 119.3(3) . . ?
C10B C11B H11B 120.4 . . ?
C12B C11B H11B 120.4 . . ?
C11B C12B C13B 119.6(3) . . ?
C11B C12B H12B 120.2 . . ?
C13B C12B H12B 120.2 . . ?
O5B C13B C14B 116.2(3) . . ?
O5B C13B C12B 123.8(3) . . ?
C14B C13B C12B 120.1(3) . . ?
C15B C14B C13B 120.5(3) . . ?
C15B C14B H14B 119.8 . . ?
C13B C14B H14B 119.8 . . ?
C14B C15B C10B 118.8(3) . . ?
C14B C15B H15B 120.6 . . ?
C10B C15B H15B 120.6 . . ?
O5B C16B H16D 109.5 . . ?
O5B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
O5B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7A O1A C1A C2A -2.8(5) . . . . ?
C7A O1A C1A C6A 177.1(3) . . . . ?
O1A C1A C2A C3A 179.1(3) . . . . ?
C6A C1A C2A C3A -0.8(6) . . . . ?
C1A C2A C3A C4A -0.2(6) . . . . ?
C2A C3A C4A C5A 0.8(6) . . . . ?
C3A C4A C5A C6A -0.2(6) . . . . ?
C4A C5A C6A O2A 177.9(3) . . . . ?
C4A C5A C6A C1A -0.8(6) . . . . ?
C8A O2A C6A C5A 13.9(5) . . . . ?
C8A O2A C6A C1A -167.3(3) . . . . ?
O1A C1A C6A C5A -178.6(3) . . . . ?
C2A C1A C6A C5A 1.3(6) . . . . ?
O1A C1A C6A O2A 2.6(5) . . . . ?
C2A C1A C6A O2A -177.5(3) . . . . ?
C6A O2A C8A C9A 175.0(3) . . . . ?
C10A O4A C9A O3A -0.7(6) . . . . ?
C10A O4A C9A C8A 178.6(3) . . . . ?
O2A C8A C9A O3A 3.6(5) . . . . ?
O2A C8A C9A O4A -175.6(3) . . . . ?
C9A O4A C10A C11A 64.9(5) . . . . ?
C9A O4A C10A C15A -119.0(4) . . . . ?
C15A C10A C11A C12A -0.5(6) . . . . ?
O4A C10A C11A C12A 175.4(3) . . . . ?
C10A C11A C12A C13A -0.6(6) . . . . ?
C16A O5A C13A C14A 178.5(4) . . . . ?
C16A O5A C13A C12A -1.7(6) . . . . ?
C11A C12A C13A O5A -178.3(4) . . . . ?
C11A C12A C13A C14A 1.4(6) . . . . ?
O5A C13A C14A C15A 178.6(4) . . . . ?
C12A C13A C14A C15A -1.2(6) . . . . ?
C11A C10A C15A C14A 0.7(6) . . . . ?
O4A C10A C15A C14A -175.3(4) . . . . ?
C13A C14A C15A C10A 0.1(6) . . . . ?
C7B O1B C1B C2B -1.4(5) . . . . ?
C7B O1B C1B C6B 177.9(3) . . . . ?
O1B C1B C2B C3B -179.8(3) . . . . ?
C6B C1B C2B C3B 0.9(5) . . . . ?
C1B C2B C3B C4B 0.3(5) . . . . ?
C2B C3B C4B C5B -1.4(6) . . . . ?
C3B C4B C5B C6B 1.2(5) . . . . ?
C4B C5B C6B O2B -177.9(3) . . . . ?
C4B C5B C6B C1B 0.0(5) . . . . ?
C8B O2B C6B C5B -17.0(5) . . . . ?
C8B O2B C6B C1B 165.0(3) . . . . ?
O1B C1B C6B C5B 179.6(3) . . . . ?
C2B C1B C6B C5B -1.1(5) . . . . ?
O1B C1B C6B O2B -2.3(4) . . . . ?
C2B C1B C6B O2B 177.1(3) . . . . ?
C6B O2B C8B C9B -174.5(3) . . . . ?
C10B O4B C9B O3B -1.2(5) . . . . ?
C10B O4B C9B C8B 179.4(3) . . . . ?
O2B C8B C9B O3B -4.1(5) . . . . ?
O2B C8B C9B O4B 175.2(3) . . . . ?
C9B O4B C10B C11B -65.0(5) . . . . ?
C9B O4B C10B C15B 117.8(4) . . . . ?
C15B C10B C11B C12B 0.4(6) . . . . ?
O4B C10B C11B C12B -176.7(4) . . . . ?
C10B C11B C12B C13B 0.6(6) . . . . ?
C16B O5B C13B C14B -179.9(4) . . . . ?
C16B O5B C13B C12B 0.2(6) . . . . ?
C11B C12B C13B O5B 178.9(4) . . . . ?
C11B C12B C13B C14B -1.0(6) . . . . ?
O5B C13B C14B C15B -179.5(4) . . . . ?
C12B C13B C14B C15B 0.4(6) . . . . ?
C13B C14B C15B C10B 0.6(6) . . . . ?
C11B C10B C15B C14B -1.0(6) . . . . ?
O4B C10B C15B C14B 176.1(4) . . . . ?

_refine_diff_density_max         0.389
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.088

