# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2020

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

data_tll1701
_database_code_depnum_ccdc_archive 'CCDC 1891386'
loop_
_audit_author_name
_audit_author_address
'Robert McDonald'
;Department of Chemistry, University of Alberta
Canada
;
_audit_update_record             
;
2019-01-16 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'{1-(Cyclohexyloxy)-1,3,3a,9a-tetrahydrofuro[3,4-b][1,4]benzodioxin-1-  yl}methanol'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H26 O5'
_chemical_formula_sum            'C19 H26 O5'
_chemical_formula_weight         334.40

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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   5.3125(2)
_cell_length_b                   12.3867(5)
_cell_length_c                   13.7161(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.529(3)
_cell_angle_gamma                90
_cell_volume                     902.54(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3968
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      68.16

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_F_000             360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.595
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.035
_exptl_absorpt_coefficient_mu    0.719
_shelx_estimated_absorpt_T_min   0.674
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS 2016/2 (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5417
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.810
_diffrn_reflns_theta_max         68.451
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             3190
_reflns_number_gt                2371
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.902
_reflns_Friedel_fraction_max     0.958
_reflns_Friedel_fraction_full    0.961

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXD (Schneider & Sheldrick, 2002)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1292P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 678 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.0(4)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         3190
_refine_ls_number_parameters     218
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0828
_refine_ls_wR_factor_ref         0.2221
_refine_ls_wR_factor_gt          0.2137
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O -0.2665(8) 0.0698(4) 0.2292(3) 0.0291(11) Uani 1 1 d . . . . .
O2 O -0.1909(9) 0.2280(4) 0.4231(3) 0.0338(11) Uani 1 1 d . . . . .
O3 O 0.2065(7) 0.0117(4) 0.4057(3) 0.0288(11) Uani 1 1 d . . . . .
O4 O 0.1429(7) 0.0008(4) 0.2154(3) 0.0298(11) Uani 1 1 d . . . . .
O5 O -0.4057(8) -0.1192(4) 0.3362(4) 0.0348(12) Uani 1 1 d . . . . .
H5O H -0.5180 -0.0759 0.3174 0.052 Uiso 1 1 calc R U . . .
C1 C -0.1989(14) 0.1792(6) 0.2559(5) 0.0348(16) Uani 1 1 d . . . . .
H1A H -0.3520 0.2235 0.2654 0.042 Uiso 1 1 calc R U . . .
H1B H -0.0964 0.2129 0.2042 0.042 Uiso 1 1 calc R U . . .
C2 C -0.0483(13) 0.1715(6) 0.3505(5) 0.0289(14) Uani 1 1 d . . . . .
H2 H 0.1223 0.2045 0.3430 0.035 Uiso 1 1 calc R U . . .
C3 C -0.0281(10) 0.0499(5) 0.3692(4) 0.0220(12) Uani 1 1 d . . . . .
H3 H -0.1633 0.0283 0.4155 0.026 Uiso 1 1 calc R U . . .
C4 C -0.0844(9) -0.0002(5) 0.2713(4) 0.0211(13) Uani 1 1 d . . . . .
C5 C -0.1958(11) -0.1122(6) 0.2729(5) 0.0285(14) Uani 1 1 d . . . . .
H5A H -0.2495 -0.1325 0.2061 0.034 Uiso 1 1 calc R U . . .
H5B H -0.0653 -0.1642 0.2946 0.034 Uiso 1 1 calc R U . . .
C6 C -0.0605(15) 0.2487(6) 0.5139(5) 0.0382(17) Uani 1 1 d . . . . .
H6A H -0.1393 0.3112 0.5467 0.046 Uiso 1 1 calc R U . . .
H6B H 0.1168 0.2677 0.5002 0.046 Uiso 1 1 calc R U . . .
C7 C -0.0665(12) 0.1521(5) 0.5814(5) 0.0264(14) Uani 1 1 d . . . . .
C8 C -0.2482(13) 0.1508(6) 0.6540(5) 0.0343(17) Uani 1 1 d . . . . .
H8 H -0.3592 0.2105 0.6601 0.041 Uiso 1 1 calc R U . . .
C9 C -0.2701(13) 0.0653(7) 0.7169(5) 0.0378(16) Uani 1 1 d . . . . .
H9 H -0.3955 0.0659 0.7659 0.045 Uiso 1 1 calc R U . . .
C10 C -0.1091(15) -0.0218(7) 0.7088(5) 0.0390(17) Uani 1 1 d . . . . .
H10 H -0.1240 -0.0817 0.7516 0.047 Uiso 1 1 calc R U . . .
C11 C 0.0748(13) -0.0211(6) 0.6374(5) 0.0342(16) Uani 1 1 d . . . . .
H11 H 0.1867 -0.0807 0.6326 0.041 Uiso 1 1 calc R U . . .
C12 C 0.0988(10) 0.0635(6) 0.5734(4) 0.0239(13) Uani 1 1 d . . . . .
C13 C 0.2953(11) 0.0587(6) 0.4954(4) 0.0297(15) Uani 1 1 d . . . . .
H13A H 0.3558 0.1328 0.4822 0.036 Uiso 1 1 calc R U . . .
H13B H 0.4403 0.0161 0.5199 0.036 Uiso 1 1 calc R U . . .
C14 C 0.1208(12) -0.0218(7) 0.1135(5) 0.0338(16) Uani 1 1 d . . . . .
H14 H -0.0617 -0.0218 0.0949 0.041 Uiso 1 1 calc R U . . .
C15 C 0.2527(15) 0.0667(8) 0.0568(6) 0.047(2) Uani 1 1 d . . . . .
H15A H 0.4294 0.0723 0.0797 0.057 Uiso 1 1 calc R U . . .
H15B H 0.1689 0.1366 0.0698 0.057 Uiso 1 1 calc R U . . .
C16 C 0.2488(18) 0.0449(10) -0.0528(7) 0.063(3) Uani 1 1 d . . . . .
H16A H 0.3471 0.1014 -0.0865 0.076 Uiso 1 1 calc R U . . .
H16B H 0.0733 0.0482 -0.0775 0.076 Uiso 1 1 calc R U . . .
C17 C 0.3602(18) -0.0659(10) -0.0752(7) 0.063(3) Uani 1 1 d . . . . .
H17A H 0.3426 -0.0809 -0.1458 0.076 Uiso 1 1 calc R U . . .
H17B H 0.5420 -0.0659 -0.0586 0.076 Uiso 1 1 calc R U . . .
C18 C 0.2290(16) -0.1541(9) -0.0178(6) 0.054(2) Uani 1 1 d . . . . .
H18A H 0.0526 -0.1605 -0.0410 0.065 Uiso 1 1 calc R U . . .
H18B H 0.3139 -0.2239 -0.0300 0.065 Uiso 1 1 calc R U . . .
C19 C 0.2310(15) -0.1315(8) 0.0893(6) 0.047(2) Uani 1 1 d . . . . .
H19A H 0.4065 -0.1349 0.1140 0.056 Uiso 1 1 calc R U . . .
H19B H 0.1332 -0.1881 0.1230 0.056 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 1.418(7) . ?
O1 C1 1.449(9) . ?
O2 C2 1.439(8) . ?
O2 C6 1.442(9) . ?
O3 C3 1.420(6) . ?
O3 C13 1.437(7) . ?
O4 C14 1.429(8) . ?
O4 C4 1.437(6) . ?
O5 C5 1.422(7) . ?
C1 C2 1.521(9) . ?
C2 C3 1.531(9) . ?
C3 C4 1.507(8) . ?
C4 C5 1.509(9) . ?
C6 C7 1.513(10) . ?
C7 C8 1.393(9) . ?
C7 C12 1.410(9) . ?
C8 C9 1.373(11) . ?
C9 C10 1.382(12) . ?
C10 C11 1.390(10) . ?
C11 C12 1.374(10) . ?
C12 C13 1.503(8) . ?
C14 C19 1.517(12) . ?
C14 C15 1.519(10) . ?
C15 C16 1.527(11) . ?
C16 C17 1.528(16) . ?
C17 C18 1.519(14) . ?
C18 C19 1.496(11) . ?

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 C1 107.6(5) . . ?
C2 O2 C6 115.6(5) . . ?
C3 O3 C13 116.6(5) . . ?
C14 O4 C4 117.3(4) . . ?
O1 C1 C2 106.5(5) . . ?
O2 C2 C1 106.5(6) . . ?
O2 C2 C3 113.6(5) . . ?
C1 C2 C3 103.9(5) . . ?
O3 C3 C4 110.1(5) . . ?
O3 C3 C2 116.5(5) . . ?
C4 C3 C2 104.1(5) . . ?
O1 C4 O4 110.6(5) . . ?
O1 C4 C3 103.9(5) . . ?
O4 C4 C3 108.1(4) . . ?
O1 C4 C5 107.6(5) . . ?
O4 C4 C5 110.3(5) . . ?
C3 C4 C5 116.1(5) . . ?
O5 C5 C4 112.0(5) . . ?
O2 C6 C7 112.0(6) . . ?
C8 C7 C12 118.9(6) . . ?
C8 C7 C6 117.7(6) . . ?
C12 C7 C6 123.5(6) . . ?
C9 C8 C7 121.4(7) . . ?
C8 C9 C10 119.7(6) . . ?
C9 C10 C11 119.5(7) . . ?
C12 C11 C10 121.6(7) . . ?
C11 C12 C7 118.9(6) . . ?
C11 C12 C13 119.6(6) . . ?
C7 C12 C13 121.5(6) . . ?
O3 C13 C12 113.6(5) . . ?
O4 C14 C19 111.1(6) . . ?
O4 C14 C15 109.0(6) . . ?
C19 C14 C15 110.7(6) . . ?
C14 C15 C16 112.0(8) . . ?
C15 C16 C17 110.8(9) . . ?
C18 C17 C16 111.2(7) . . ?
C19 C18 C17 112.0(8) . . ?
C18 C19 C14 112.5(8) . . ?

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
C4 O1 C1 C2 -25.7(7) . . . . ?
C6 O2 C2 C1 -168.5(6) . . . . ?
C6 O2 C2 C3 77.8(7) . . . . ?
O1 C1 C2 O2 -117.1(6) . . . . ?
O1 C1 C2 C3 3.0(7) . . . . ?
C13 O3 C3 C4 175.4(5) . . . . ?
C13 O3 C3 C2 57.2(7) . . . . ?
O2 C2 C3 O3 -104.5(6) . . . . ?
C1 C2 C3 O3 140.3(5) . . . . ?
O2 C2 C3 C4 134.1(5) . . . . ?
C1 C2 C3 C4 18.8(6) . . . . ?
C1 O1 C4 O4 -77.9(6) . . . . ?
C1 O1 C4 C3 37.9(6) . . . . ?
C1 O1 C4 C5 161.5(5) . . . . ?
C14 O4 C4 O1 -54.0(7) . . . . ?
C14 O4 C4 C3 -167.1(6) . . . . ?
C14 O4 C4 C5 64.9(7) . . . . ?
O3 C3 C4 O1 -160.3(5) . . . . ?
C2 C3 C4 O1 -34.7(6) . . . . ?
O3 C3 C4 O4 -42.8(7) . . . . ?
C2 C3 C4 O4 82.8(6) . . . . ?
O3 C3 C4 C5 81.8(6) . . . . ?
C2 C3 C4 C5 -152.6(5) . . . . ?
O1 C4 C5 O5 -65.7(7) . . . . ?
O4 C4 C5 O5 173.6(5) . . . . ?
C3 C4 C5 O5 50.2(7) . . . . ?
C2 O2 C6 C7 -82.5(7) . . . . ?
O2 C6 C7 C8 -97.8(7) . . . . ?
O2 C6 C7 C12 81.4(8) . . . . ?
C12 C7 C8 C9 -0.6(10) . . . . ?
C6 C7 C8 C9 178.6(7) . . . . ?
C7 C8 C9 C10 0.2(11) . . . . ?
C8 C9 C10 C11 0.6(11) . . . . ?
C9 C10 C11 C12 -0.9(11) . . . . ?
C10 C11 C12 C7 0.5(10) . . . . ?
C10 C11 C12 C13 -178.0(7) . . . . ?
C8 C7 C12 C11 0.2(9) . . . . ?
C6 C7 C12 C11 -178.9(6) . . . . ?
C8 C7 C12 C13 178.7(6) . . . . ?
C6 C7 C12 C13 -0.4(9) . . . . ?
C3 O3 C13 C12 47.4(8) . . . . ?
C11 C12 C13 O3 90.5(7) . . . . ?
C7 C12 C13 O3 -87.9(8) . . . . ?
C4 O4 C14 C19 -109.1(7) . . . . ?
C4 O4 C14 C15 128.6(6) . . . . ?
O4 C14 C15 C16 177.0(7) . . . . ?
C19 C14 C15 C16 54.5(9) . . . . ?
C14 C15 C16 C17 -55.0(10) . . . . ?
C15 C16 C17 C18 54.3(10) . . . . ?
C16 C17 C18 C19 -54.5(11) . . . . ?
C17 C18 C19 C14 54.7(9) . . . . ?
O4 C14 C19 C18 -175.6(6) . . . . ?
C15 C14 C19 C18 -54.3(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5O O3 0.84 2.20 2.796(6) 128.4 1_455

_refine_diff_density_max         0.357
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.088


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethyl Acetate and Hexanes'
####################################################################### 
# 
# 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_tll1601
_database_code_depnum_ccdc_archive 'CCDC 1986079'
loop_
_audit_author_name
_audit_author_address
'Robert McDonald'
;Department of Chemistry, University of Alberta
Canada
;
_audit_update_record             
;
2020-02-24 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'{1-(4-Methylphenyl)sulfanyl-1,3,3a,5,10,11a-hexahydrofuro[3,4-c][2,5]benzo-dioxocin-1-yl}methyl benzoate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H26 O5 S'
_chemical_formula_sum            'C27 H26 O5 S'
_chemical_formula_weight         462.54

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   10.125(3)
_cell_length_b                   13.806(4)
_cell_length_c                   16.436(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2297.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6325
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      19.50

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.121
_exptl_absorpt_coefficient_mu    0.178
_shelx_estimated_absorpt_T_min   0.949
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7128
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'SADABS 2016/2 (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17017
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.926
_diffrn_reflns_theta_max         25.745
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4347
_reflns_number_gt                2964
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXD (Schneider & Sheldrick, 2002)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0921P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.029(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1048 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.02(5)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         4347
_refine_ls_number_parameters     319
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1536
_refine_ls_wR_factor_gt          0.1336
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.999
_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
S S 0.47750(11) -0.11950(11) 0.02309(7) 0.0691(4) Uani 1 1 d . . . . .
O1 O 0.2164(3) -0.0785(3) 0.04379(19) 0.0691(9) Uani 1 1 d . . . . .
O2 O 0.1655(3) 0.0762(3) -0.10812(19) 0.0714(10) Uani 1 1 d . . . . .
O3 O 0.4749(3) 0.0716(3) -0.02359(17) 0.0664(9) Uani 1 1 d . . . . .
O4A O 0.2571(5) 0.0395(6) 0.1756(3) 0.0712(19) Uani 0.65 1 d D . P A 1
O5A O 0.3697(4) 0.1765(4) 0.1596(3) 0.0715(14) Uani 0.65 1 d D . P A 1
O4B O 0.2844(14) 0.0780(9) 0.1663(11) 0.087(7) Uiso 0.35 1 d D . P A 2
O5B O 0.1212(10) -0.0042(7) 0.2205(6) 0.074(3) Uiso 0.35 1 d D . P A 2
C1 C 0.1857(4) -0.0763(4) -0.0421(3) 0.0727(14) Uani 1 1 d . . . . .
H1A H 0.0895 -0.0685 -0.0503 0.087 Uiso 1 1 calc R U . . .
H1B H 0.2139 -0.1375 -0.0684 0.087 Uiso 1 1 calc R U . . .
C2 C 0.2598(5) 0.0092(4) -0.0788(3) 0.0658(13) Uani 1 1 d . . . . .
H2 H 0.3188 -0.0130 -0.1239 0.079 Uiso 1 1 calc R U . . .
C3 C 0.3422(4) 0.0473(4) -0.0069(2) 0.0619(12) Uani 1 1 d . . . . .
H3 H 0.2966 0.1044 0.0179 0.074 Uiso 1 1 calc R U . . .
C4 C 0.3413(4) -0.0362(4) 0.0533(3) 0.0612(12) Uani 1 1 d . . . . .
C5 C 0.3633(4) -0.0097(4) 0.1413(3) 0.0668(13) Uani 1 1 d D . . . .
H5A H 0.3796 -0.0696 0.1729 0.080 Uiso 1 1 calc R U . A 1
H5B H 0.4432 0.0313 0.1455 0.080 Uiso 1 1 calc R U . A 1
C6 C 0.4285(4) -0.2279(4) 0.0727(2) 0.0606(12) Uani 1 1 d . . . . .
C7 C 0.3453(4) -0.2925(4) 0.0346(3) 0.0681(14) Uani 1 1 d . . . . .
H7 H 0.3091 -0.2767 -0.0171 0.082 Uiso 1 1 calc R U . . .
C8 C 0.3136(4) -0.3804(5) 0.0706(3) 0.0713(14) Uani 1 1 d . . . . .
H8 H 0.2557 -0.4240 0.0437 0.086 Uiso 1 1 calc R U . . .
C9 C 0.3660(5) -0.4047(4) 0.1454(3) 0.0761(16) Uani 1 1 d . . . . .
C10 C 0.4483(6) -0.3405(5) 0.1824(3) 0.0827(17) Uani 1 1 d . . . . .
H10 H 0.4859 -0.3569 0.2336 0.099 Uiso 1 1 calc R U . . .
C11 C 0.4789(5) -0.2512(4) 0.1475(3) 0.0742(14) Uani 1 1 d . . . . .
H11 H 0.5345 -0.2068 0.1754 0.089 Uiso 1 1 calc R U . . .
C12 C 0.3362(8) -0.5024(5) 0.1836(4) 0.103(2) Uani 1 1 d . . . . .
H12A H 0.3341 -0.4958 0.2430 0.124 Uiso 1 1 calc R U . . .
H12B H 0.4051 -0.5488 0.1683 0.124 Uiso 1 1 calc R U . . .
H12C H 0.2503 -0.5257 0.1643 0.124 Uiso 1 1 calc R U . . .
C13 C 0.2196(5) 0.1514(4) -0.1591(3) 0.0765(15) Uani 1 1 d . . . . .
H13A H 0.1480 0.1779 -0.1936 0.092 Uiso 1 1 calc R U . . .
H13B H 0.2862 0.1222 -0.1958 0.092 Uiso 1 1 calc R U . . .
C14 C 0.2828(5) 0.2331(4) -0.1139(3) 0.0669(13) Uani 1 1 d . . . . .
C15 C 0.2121(5) 0.3187(4) -0.1036(3) 0.0744(15) Uani 1 1 d . . . . .
H15 H 0.1242 0.3222 -0.1235 0.089 Uiso 1 1 calc R U . . .
C16 C 0.2656(5) 0.3981(4) -0.0657(3) 0.0791(15) Uani 1 1 d . . . . .
H16 H 0.2159 0.4562 -0.0604 0.095 Uiso 1 1 calc R U . . .
C17 C 0.3930(5) 0.3925(5) -0.0351(3) 0.0779(15) Uani 1 1 d . . . . .
H17 H 0.4311 0.4470 -0.0087 0.093 Uiso 1 1 calc R U . . .
C18 C 0.4637(5) 0.3091(4) -0.0428(3) 0.0720(14) Uani 1 1 d . . . . .
H18 H 0.5501 0.3057 -0.0203 0.086 Uiso 1 1 calc R U . . .
C19 C 0.4122(4) 0.2285(4) -0.0829(3) 0.0668(14) Uani 1 1 d . . . . .
C20 C 0.4944(4) 0.1390(4) -0.0895(3) 0.0707(14) Uani 1 1 d . . . . .
H20A H 0.4733 0.1061 -0.1414 0.085 Uiso 1 1 calc R U . . .
H20B H 0.5887 0.1578 -0.0912 0.085 Uiso 1 1 calc R U . . .
C21A C 0.2756(6) 0.1312(6) 0.1803(4) 0.0525(19) Uani 0.65 1 d D . P A 1
C22A C 0.1650(8) 0.1801(8) 0.2313(4) 0.064(3) Uani 0.65 1 d . . P A 1
C23A C 0.1827(10) 0.2736(9) 0.2578(7) 0.073(4) Uani 0.65 1 d . . P A 1
H23A H 0.2603 0.3087 0.2441 0.088 Uiso 0.65 1 calc R U P A 1
C24A C 0.0847(13) 0.3157(9) 0.3051(6) 0.088(3) Uani 0.65 1 d . . P A 1
H24A H 0.0988 0.3784 0.3271 0.105 Uiso 0.65 1 calc R U P A 1
C25A C -0.0308(10) 0.2694(9) 0.3207(6) 0.075(3) Uani 0.65 1 d . . P A 1
H25A H -0.0990 0.3005 0.3507 0.090 Uiso 0.65 1 calc R U P A 1
C26A C -0.0464(8) 0.1785(10) 0.2927(6) 0.086(3) Uani 0.65 1 d . . P A 1
H26A H -0.1263 0.1455 0.3049 0.103 Uiso 0.65 1 calc R U P A 1
C27A C 0.0509(10) 0.1296(8) 0.2459(4) 0.072(2) Uani 0.65 1 d . . P A 1
H27A H 0.0377 0.0658 0.2259 0.086 Uiso 0.65 1 calc R U P A 1
C21B C 0.1710(12) 0.0716(9) 0.2071(8) 0.059(3) Uiso 0.35 1 d D . P A 2
C22B C 0.117(2) 0.1657(11) 0.2437(10) 0.063(3) Uiso 0.35 1 d G U P A 2
C23B C 0.1868(14) 0.2522(16) 0.2467(10) 0.063(3) Uiso 0.35 1 d G U P A 2
H23B H 0.2711 0.2569 0.2217 0.075 Uiso 0.35 1 calc R U P A 2
C24B C 0.1334(17) 0.3320(10) 0.2865(9) 0.063(3) Uiso 0.35 1 d G U P A 2
H24B H 0.1812 0.3912 0.2886 0.075 Uiso 0.35 1 calc R U P A 2
C25B C 0.0101(17) 0.3252(9) 0.3232(7) 0.063(3) Uiso 0.35 1 d G U P A 2
H25B H -0.0264 0.3797 0.3504 0.075 Uiso 0.35 1 calc R U P A 2
C26B C -0.0598(12) 0.2387(13) 0.3201(10) 0.063(3) Uiso 0.35 1 d G U P A 2
H26B H -0.1441 0.2340 0.3452 0.075 Uiso 0.35 1 calc R U P A 2
C27B C -0.0064(19) 0.1589(8) 0.2804(11) 0.063(3) Uiso 0.35 1 d G U P A 2
H27B H -0.0542 0.0997 0.2783 0.075 Uiso 0.35 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S C6 1.775(5) . ?
S C4 1.863(5) . ?
O1 C4 1.401(5) . ?
O1 C1 1.447(6) . ?
O2 C2 1.415(6) . ?
O2 C13 1.443(6) . ?
O3 C3 1.412(5) . ?
O3 C20 1.441(5) . ?
O4A C21A 1.283(11) . ?
O4A C5 1.391(6) . ?
O5A C21A 1.189(8) . ?
O4B C21B 1.334(12) . ?
O4B C5 1.507(11) . ?
O5B C21B 1.181(12) . ?
C1 C2 1.522(8) . ?
C2 C3 1.540(6) . ?
C3 C4 1.519(7) . ?
C4 C5 1.509(6) . ?
C6 C11 1.369(7) . ?
C6 C7 1.377(7) . ?
C7 C8 1.388(8) . ?
C8 C9 1.380(7) . ?
C9 C10 1.360(8) . ?
C9 C12 1.518(8) . ?
C10 C11 1.395(8) . ?
C13 C14 1.495(7) . ?
C14 C15 1.391(7) . ?
C14 C19 1.407(7) . ?
C15 C16 1.373(8) . ?
C16 C17 1.387(8) . ?
C17 C18 1.362(8) . ?
C18 C19 1.394(8) . ?
C19 C20 1.494(7) . ?
C21A C22A 1.553(10) . ?
C22A C27A 1.370(12) . ?
C22A C23A 1.375(14) . ?
C23A C24A 1.388(15) . ?
C24A C25A 1.357(16) . ?
C25A C26A 1.346(16) . ?
C26A C27A 1.421(11) . ?
C21B C22B 1.532(16) . ?
C22B C23B 1.3900 . ?
C22B C27B 1.3900 . ?
C23B C24B 1.3900 . ?
C24B C25B 1.3900 . ?
C25B C26B 1.3900 . ?
C26B C27B 1.3900 . ?

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 S C4 101.0(2) . . ?
C4 O1 C1 107.1(3) . . ?
C2 O2 C13 114.4(4) . . ?
C3 O3 C20 115.5(3) . . ?
C21A O4A C5 113.2(5) . . ?
C21B O4B C5 122.7(11) . . ?
O1 C1 C2 107.2(4) . . ?
O2 C2 C1 108.0(4) . . ?
O2 C2 C3 113.8(5) . . ?
C1 C2 C3 103.2(4) . . ?
O3 C3 C4 108.3(4) . . ?
O3 C3 C2 116.6(4) . . ?
C4 C3 C2 103.7(4) . . ?
O1 C4 C5 109.9(3) . . ?
O1 C4 C3 104.4(3) . . ?
C5 C4 C3 116.1(5) . . ?
O1 C4 S 112.4(4) . . ?
C5 C4 S 107.2(3) . . ?
C3 C4 S 106.9(3) . . ?
O4A C5 C4 113.1(4) . . ?
O4B C5 C4 112.1(8) . . ?
C11 C6 C7 118.9(5) . . ?
C11 C6 S 120.4(4) . . ?
C7 C6 S 120.5(3) . . ?
C6 C7 C8 120.9(4) . . ?
C9 C8 C7 120.2(5) . . ?
C10 C9 C8 118.4(6) . . ?
C10 C9 C12 121.0(6) . . ?
C8 C9 C12 120.5(6) . . ?
C9 C10 C11 121.8(5) . . ?
C6 C11 C10 119.6(6) . . ?
O2 C13 C14 114.6(4) . . ?
C15 C14 C19 118.3(5) . . ?
C15 C14 C13 118.7(4) . . ?
C19 C14 C13 123.0(5) . . ?
C16 C15 C14 122.0(5) . . ?
C15 C16 C17 119.1(6) . . ?
C18 C17 C16 120.2(6) . . ?
C17 C18 C19 121.4(5) . . ?
C18 C19 C14 118.9(5) . . ?
C18 C19 C20 119.1(4) . . ?
C14 C19 C20 122.0(5) . . ?
O3 C20 C19 113.7(3) . . ?
O5A C21A O4A 128.2(7) . . ?
O5A C21A C22A 120.3(8) . . ?
O4A C21A C22A 110.9(6) . . ?
C27A C22A C23A 122.2(8) . . ?
C27A C22A C21A 118.8(9) . . ?
C23A C22A C21A 119.0(10) . . ?
C22A C23A C24A 118.5(11) . . ?
C25A C24A C23A 121.7(11) . . ?
C26A C25A C24A 118.4(9) . . ?
C25A C26A C27A 123.1(9) . . ?
C22A C27A C26A 116.0(10) . . ?
O5B C21B O4B 121.3(12) . . ?
O5B C21B C22B 121.7(13) . . ?
O4B C21B C22B 116.7(13) . . ?
C23B C22B C27B 120.0 . . ?
C23B C22B C21B 124.1(17) . . ?
C27B C22B C21B 115.7(17) . . ?
C22B C23B C24B 120.0 . . ?
C25B C24B C23B 120.0 . . ?
C26B C25B C24B 120.0 . . ?
C25B C26B C27B 120.0 . . ?
C26B C27B C22B 120.0 . . ?

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
C4 O1 C1 C2 -27.4(5) . . . . ?
C13 O2 C2 C1 -168.0(4) . . . . ?
C13 O2 C2 C3 78.1(5) . . . . ?
O1 C1 C2 O2 -116.1(4) . . . . ?
O1 C1 C2 C3 4.7(5) . . . . ?
C20 O3 C3 C4 170.3(4) . . . . ?
C20 O3 C3 C2 54.0(6) . . . . ?
O2 C2 C3 O3 -107.0(5) . . . . ?
C1 C2 C3 O3 136.2(5) . . . . ?
O2 C2 C3 C4 134.1(4) . . . . ?
C1 C2 C3 C4 17.3(5) . . . . ?
C1 O1 C4 C5 163.8(5) . . . . ?
C1 O1 C4 C3 38.7(5) . . . . ?
C1 O1 C4 S -76.9(4) . . . . ?
O3 C3 C4 O1 -158.9(4) . . . . ?
C2 C3 C4 O1 -34.5(5) . . . . ?
O3 C3 C4 C5 79.9(5) . . . . ?
C2 C3 C4 C5 -155.6(4) . . . . ?
O3 C3 C4 S -39.6(4) . . . . ?
C2 C3 C4 S 84.9(4) . . . . ?
C6 S C4 O1 -46.5(3) . . . . ?
C6 S C4 C5 74.5(4) . . . . ?
C6 S C4 C3 -160.5(3) . . . . ?
C21A O4A C5 C4 -101.2(6) . . . . ?
C21B O4B C5 C4 100.0(17) . . . . ?
O1 C4 C5 O4A -47.6(7) . . . . ?
C3 C4 C5 O4A 70.6(6) . . . . ?
S C4 C5 O4A -170.1(5) . . . . ?
O1 C4 C5 O4B -73.9(7) . . . . ?
C3 C4 C5 O4B 44.3(7) . . . . ?
S C4 C5 O4B 163.6(6) . . . . ?
C4 S C6 C11 -95.8(4) . . . . ?
C4 S C6 C7 88.0(4) . . . . ?
C11 C6 C7 C8 -0.7(7) . . . . ?
S C6 C7 C8 175.6(4) . . . . ?
C6 C7 C8 C9 -0.4(7) . . . . ?
C7 C8 C9 C10 0.2(7) . . . . ?
C7 C8 C9 C12 -177.5(5) . . . . ?
C8 C9 C10 C11 1.0(8) . . . . ?
C12 C9 C10 C11 178.7(5) . . . . ?
C7 C6 C11 C10 1.8(7) . . . . ?
S C6 C11 C10 -174.5(4) . . . . ?
C9 C10 C11 C6 -2.0(8) . . . . ?
C2 O2 C13 C14 -80.5(5) . . . . ?
O2 C13 C14 C15 -100.5(5) . . . . ?
O2 C13 C14 C19 81.3(6) . . . . ?
C19 C14 C15 C16 1.0(7) . . . . ?
C13 C14 C15 C16 -177.3(5) . . . . ?
C14 C15 C16 C17 -1.3(8) . . . . ?
C15 C16 C17 C18 0.0(8) . . . . ?
C16 C17 C18 C19 1.6(8) . . . . ?
C17 C18 C19 C14 -1.9(7) . . . . ?
C17 C18 C19 C20 179.9(4) . . . . ?
C15 C14 C19 C18 0.5(7) . . . . ?
C13 C14 C19 C18 178.8(4) . . . . ?
C15 C14 C19 C20 178.7(4) . . . . ?
C13 C14 C19 C20 -3.1(7) . . . . ?
C3 O3 C20 C19 51.0(6) . . . . ?
C18 C19 C20 O3 91.0(5) . . . . ?
C14 C19 C20 O3 -87.1(5) . . . . ?
C5 O4A C21A O5A -0.1(10) . . . . ?
C5 O4A C21A C22A -170.8(5) . . . . ?
O5A C21A C22A C27A 172.2(6) . . . . ?
O4A C21A C22A C27A -16.2(8) . . . . ?
O5A C21A C22A C23A -5.5(9) . . . . ?
O4A C21A C22A C23A 166.1(7) . . . . ?
C27A C22A C23A C24A 4.0(12) . . . . ?
C21A C22A C23A C24A -178.4(7) . . . . ?
C22A C23A C24A C25A -4.6(12) . . . . ?
C23A C24A C25A C26A 3.5(12) . . . . ?
C24A C25A C26A C27A -1.6(13) . . . . ?
C23A C22A C27A C26A -2.2(11) . . . . ?
C21A C22A C27A C26A -179.8(7) . . . . ?
C25A C26A C27A C22A 1.0(12) . . . . ?
C5 O4B C21B O5B -6(3) . . . . ?
C5 O4B C21B C22B 167.6(14) . . . . ?
O5B C21B C22B C23B 164.0(12) . . . . ?
O4B C21B C22B C23B -9.5(19) . . . . ?
O5B C21B C22B C27B -11.5(19) . . . . ?
O4B C21B C22B C27B 175.1(13) . . . . ?
C27B C22B C23B C24B 0.0 . . . . ?
C21B C22B C23B C24B -175.2(14) . . . . ?
C22B C23B C24B C25B 0.0 . . . . ?
C23B C24B C25B C26B 0.0 . . . . ?
C24B C25B C26B C27B 0.0 . . . . ?
C25B C26B C27B C22B 0.0 . . . . ?
C23B C22B C27B C26B 0.0 . . . . ?
C21B C22B C27B C26B 175.6(13) . . . . ?

_refine_diff_density_max         0.351
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.065


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: ethyl acetate'
