# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_testm1
_database_code_depnum_ccdc_archive 'CCDC 1839028'
_audit_update_record             
;
2018-04-23 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_audit_creation_date             2018-04-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            'Agnestin B'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H12 O6, H2 O'
_chemical_formula_sum            'C15 H14 O7'
_chemical_formula_weight         306.26
_chemical_absolute_configuration unk
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   7.1336(12)
_cell_length_b                   7.3556(13)
_cell_length_c                   13.246(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.455(4)
_cell_angle_gamma                90
_cell_volume                     678.7(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.91
_cell_measurement_theta_min      6.35
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11998
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        66.072
_diffrn_reflns_theta_max         66.072
_diffrn_reflns_theta_min         6.354
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker Pt135 CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'Bruker Mircostar Rotating anode'
_diffrn_measurement_device_type  'Rotating anode'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus rotating anode'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.678
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                2099
_reflns_number_total             2118
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex suite'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2118
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0926P)²+0.4044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1338
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 C13(H13), C14(H14)
2.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
2.d Aromatic/amide H refined with riding coordinates:
 C4(H4A), C3(H3), C2(H2)
2.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
2.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
O3 O 0.7317(3) 0.7267(4) 0.53680(19) 0.0170(6) Uani 1 1 d . . . . .
O5 O 0.9127(4) 0.6448(4) 0.85320(19) 0.0207(6) Uani 1 1 d . . . . .
O1 O 0.7957(4) 0.1202(4) 0.4124(2) 0.0219(7) Uani 1 1 d . . . . .
H1 H 0.787708 0.096632 0.471838 0.033 Uiso 1 1 calc GR . . . .
O4 O 0.5622(4) 0.5049(4) 0.9045(2) 0.0229(6) Uani 1 1 d . . . . .
H4 H 0.491137 0.574581 0.926856 0.034 Uiso 1 1 calc GR . . . .
O2 O 0.7318(4) 0.1807(4) 0.5955(2) 0.0218(7) Uani 1 1 d . . . . .
O6 O 1.0367(4) 0.3650(5) 0.8556(2) 0.0314(8) Uani 1 1 d . . . . .
O7 O 0.3046(4) 0.7340(5) 0.9544(2) 0.0278(7) Uani 1 1 d . . . . .
H7A H 0.339829 0.816453 0.999447 0.042 Uiso 1 1 d G . . . .
H7B H 0.183070 0.723889 0.941978 0.042 Uiso 1 1 d G . . . .
C1 C 0.7863(5) 0.3028(6) 0.3979(3) 0.0175(9) Uani 1 1 d . . . . .
C8 C 0.7160(5) 0.4830(6) 0.6536(3) 0.0161(8) Uani 1 1 d . . . . .
C6 C 0.7567(5) 0.4194(6) 0.4787(3) 0.0159(8) Uani 1 1 d . . . . .
C13 C 0.5866(5) 0.5672(6) 0.8072(3) 0.0179(8) Uani 1 1 d . . . . .
H13 H 0.463245 0.591446 0.760006 0.021 Uiso 1 1 calc R . . . .
C7 C 0.7339(5) 0.3462(6) 0.5778(3) 0.0154(8) Uani 1 1 d . . . . .
C4 C 0.7660(5) 0.6806(6) 0.3657(3) 0.0189(9) Uani 1 1 d . . . . .
H4A H 0.759185 0.805604 0.354927 0.023 Uiso 1 1 calc R . . . .
C9 C 0.7200(5) 0.6617(6) 0.6309(3) 0.0154(8) Uani 1 1 d . . . . .
C3 C 0.7914(5) 0.5609(6) 0.2883(3) 0.0203(9) Uani 1 1 d . . . . .
H3 H 0.801252 0.607394 0.224298 0.024 Uiso 1 1 calc R . . . .
C11 C 0.7229(5) 0.7312(6) 0.8157(3) 0.0175(8) Uani 1 1 d . . . . .
C14 C 0.7046(5) 0.4280(6) 0.7627(3) 0.0173(8) Uani 1 1 d . . . . .
H14 H 0.661316 0.302556 0.767784 0.021 Uiso 1 1 calc R . . . .
C5 C 0.7515(5) 0.6051(6) 0.4594(3) 0.0164(8) Uani 1 1 d . . . . .
C2 C 0.8025(5) 0.3737(6) 0.3039(3) 0.0195(9) Uani 1 1 d . . . . .
H2 H 0.820691 0.296795 0.251110 0.023 Uiso 1 1 calc R . . . .
C10 C 0.7165(5) 0.8095(6) 0.7081(3) 0.0168(8) Uani 1 1 d . . . . .
H10A H 0.600584 0.881164 0.686479 0.020 Uiso 1 1 calc R . . . .
H10B H 0.825726 0.889237 0.710707 0.020 Uiso 1 1 calc R . . . .
C15 C 0.9029(5) 0.4649(6) 0.8284(3) 0.0221(9) Uani 1 1 d . . . . .
C12 C 0.7026(5) 0.8777(6) 0.8925(3) 0.0220(9) Uani 1 1 d . . . . .
H12A H 0.719007 0.825362 0.960279 0.033 Uiso 1 1 calc GR . . . .
H12B H 0.577356 0.931485 0.873218 0.033 Uiso 1 1 calc GR . . . .
H12C H 0.798534 0.969389 0.892956 0.033 Uiso 1 1 calc GR . . . .


_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
O3 C9 1.354(4) . ?
O3 C5 1.390(4) . ?
O5 C11 1.481(4) . ?
O5 C15 1.362(5) . ?
O1 H1 0.8200 . ?
O1 C1 1.357(5) . ?
O4 H4 0.8200 . ?
O4 C13 1.414(4) . ?
O2 C7 1.241(5) . ?
O6 C15 1.197(5) . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8498 . ?
C1 C6 1.422(5) . ?
C1 C2 1.378(5) . ?
C8 C7 1.447(5) . ?
C8 C9 1.350(6) . ?
C8 C14 1.520(5) . ?
C6 C7 1.459(5) . ?
C6 C5 1.389(6) . ?
C13 H13 0.9800 . ?
C13 C11 1.538(6) . ?
C13 C14 1.523(6) . ?
C4 H4A 0.9300 . ?
C4 C3 1.393(6) . ?
C4 C5 1.384(5) . ?
C9 C10 1.496(5) . ?
C3 H3 0.9300 . ?
C3 C2 1.393(6) . ?
C11 C10 1.529(5) . ?
C11 C12 1.511(6) . ?
C14 H14 0.9800 . ?
C14 C15 1.517(5) . ?
C2 H2 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 O3 C5 119.2(3) . . ?
C15 O5 C11 109.9(3) . . ?
C1 O1 H1 109.5 . . ?
C13 O4 H4 109.5 . . ?
H7A O7 H7B 109.5 . . ?
O1 C1 C6 120.1(3) . . ?
O1 C1 C2 119.4(4) . . ?
C2 C1 C6 120.5(4) . . ?
C7 C8 C14 120.4(4) . . ?
C9 C8 C7 120.9(3) . . ?
C9 C8 C14 118.6(3) . . ?
C1 C6 C7 121.2(4) . . ?
C5 C6 C1 117.2(4) . . ?
C5 C6 C7 121.7(3) . . ?
O4 C13 H13 111.8 . . ?
O4 C13 C11 112.8(3) . . ?
O4 C13 C14 108.8(3) . . ?
C11 C13 H13 111.8 . . ?
C14 C13 H13 111.8 . . ?
C14 C13 C11 99.3(3) . . ?
O2 C7 C8 123.0(3) . . ?
O2 C7 C6 122.7(4) . . ?
C8 C7 C6 114.3(4) . . ?
C3 C4 H4A 121.5 . . ?
C5 C4 H4A 121.5 . . ?
C5 C4 C3 117.0(4) . . ?
O3 C9 C10 112.7(3) . . ?
C8 C9 O3 123.8(3) . . ?
C8 C9 C10 123.5(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 C4 121.8(4) . . ?
C2 C3 H3 119.1 . . ?
O5 C11 C13 101.9(3) . . ?
O5 C11 C10 108.4(3) . . ?
O5 C11 C12 107.1(3) . . ?
C10 C11 C13 109.6(3) . . ?
C12 C11 C13 117.3(3) . . ?
C12 C11 C10 111.8(3) . . ?
C8 C14 C13 109.7(3) . . ?
C8 C14 H14 113.5 . . ?
C13 C14 H14 113.5 . . ?
C15 C14 C8 105.3(3) . . ?
C15 C14 C13 100.5(3) . . ?
C15 C14 H14 113.5 . . ?
C6 C5 O3 120.0(3) . . ?
C4 C5 O3 116.3(4) . . ?
C4 C5 C6 123.8(4) . . ?
C1 C2 C3 119.7(4) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C9 C10 C11 111.2(3) . . ?
C9 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
O5 C15 C14 107.8(3) . . ?
O6 C15 O5 121.9(4) . . ?
O6 C15 C14 130.4(4) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_Agnestin_A
_database_code_depnum_ccdc_archive 'CCDC 1839029'
_audit_update_record             
;
2018-04-23 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_audit_creation_date             2013-09-11
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_chemical_formula_moiety         '2(C15 H12 O6), H2 O'
_chemical_formula_sum            'C30 H26 O13'
_chemical_formula_weight         594.51
_chemical_absolute_configuration abs
_chemical_melting_point          ?
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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        P
_space_group_name_Hall           P
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a                   7.4082(14)
_cell_length_b                   7.9771(15)
_cell_length_c                   43.956(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2597.6(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      65.91
_cell_measurement_theta_min      5.63
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1332 before and 0.0681 after correction.
The Ratio of minimum to maximum transmission is 0.5873.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear whitish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whitish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            32711
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        68.500
_diffrn_reflns_theta_max         66.403
_diffrn_reflns_theta_min         4.023
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker Proteum CCD'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Bruker Proteum CCD'
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Bruker Mircostar Rotating anode'
_diffrn_measurement_device_type  'Rotating anode'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus rotating anode'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.689
_reflns_Friedel_fraction_full    0.915
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                4432
_reflns_number_total             4450
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 
;
 Flack x determined using 1808 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         4450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0287
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0449P)²+0.6535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0775
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O13(H13A,H13B)
2.b Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C24(H24), C25(H25)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C4(H4), C2(H2A), C3(H3), C27(H27), C18(H18), C19(H19), C17(H17)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C)
2.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O6(H6), O5(H5), O11(H11), O8(H8), O12O(H12O)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
O3 O 0.52225(19) 0.66250(17) 0.20674(3) 0.0175(3) Uani 1 1 d . . . . .
O1 O 0.30685(19) 0.38750(18) 0.13725(3) 0.0164(3) Uani 1 1 d . . . . .
O2 O 0.5980(2) 0.90035(18) 0.16787(3) 0.0211(3) Uani 1 1 d . . . . .
H2 H 0.5955 0.8519 0.1848 0.025 Uiso 1 1 calc R U . . .
O6 O 0.22977(19) 0.10820(18) 0.24955(3) 0.0187(3) Uani 1 1 d . . . . .
H6 H 0.2962 0.1278 0.2646 0.022 Uiso 1 1 calc R U . . .
O5 O 0.06671(19) 0.45592(19) 0.22638(3) 0.0210(3) Uani 1 1 d . . . . .
H5 H -0.0095 0.4983 0.2383 0.025 Uiso 1 1 calc R U . . .
O4 O 0.2549(2) 0.4954(2) 0.26557(3) 0.0231(3) Uani 1 1 d . . . . .
C6 C 0.4504(3) 0.6418(3) 0.15432(4) 0.0147(4) Uani 1 1 d . . . . .
C12 C 0.2225(3) 0.1671(3) 0.16890(4) 0.0171(4) Uani 1 1 d . . . . .
H12 H 0.1674 0.1176 0.1516 0.021 Uiso 1 1 calc R U . . .
C11 C 0.2209(3) 0.0851(2) 0.19525(4) 0.0156(4) Uani 1 1 d . . . . .
C7 C 0.4549(3) 0.5773(2) 0.18532(4) 0.0140(4) Uani 1 1 d . . . . .
C8 C 0.3776(3) 0.4156(2) 0.18999(4) 0.0143(4) Uani 1 1 d . . . . .
C13 C 0.3061(3) 0.3298(3) 0.16611(4) 0.0152(4) Uani 1 1 d . . . . .
C1 C 0.3764(3) 0.5438(3) 0.13116(4) 0.0154(4) Uani 1 1 d . . . . .
C5 C 0.5205(3) 0.8011(3) 0.14668(4) 0.0169(4) Uani 1 1 d . . . . .
C9 C 0.3634(3) 0.3442(2) 0.22181(4) 0.0135(4) Uani 1 1 d . . . . .
H9 H 0.4833 0.3608 0.2318 0.016 Uiso 1 1 calc R U . . .
C4 C 0.5130(3) 0.8564(3) 0.11671(5) 0.0197(4) Uani 1 1 d . . . . .
H4 H 0.5582 0.9641 0.1115 0.024 Uiso 1 1 calc R U . . .
C10 C 0.3230(3) 0.1521(2) 0.22228(4) 0.0149(4) Uani 1 1 d . . . . .
H10 H 0.4421 0.0931 0.2228 0.018 Uiso 1 1 calc R U . . .
C2 C 0.3708(3) 0.5962(3) 0.10106(4) 0.0183(4) Uani 1 1 d . . . . .
H2A H 0.3220 0.5267 0.0856 0.022 Uiso 1 1 calc R U . . .
C3 C 0.4391(3) 0.7534(3) 0.09452(4) 0.0190(4) Uani 1 1 d . . . . .
H3 H 0.4353 0.7923 0.0741 0.023 Uiso 1 1 calc R U . . .
C14 C 0.2243(3) 0.4406(2) 0.24066(4) 0.0154(4) Uani 1 1 d . . . . .
C15 C 0.1378(3) -0.0848(3) 0.19835(5) 0.0199(4) Uani 1 1 d . . . . .
H15A H 0.0210 -0.0750 0.2087 0.030 Uiso 1 1 calc R U . . .
H15B H 0.2178 -0.1572 0.2103 0.030 Uiso 1 1 calc R U . . .
H15C H 0.1199 -0.1337 0.1781 0.030 Uiso 1 1 calc R U . . .
O7 O 0.95288(19) 0.74527(18) 0.12282(3) 0.0167(3) Uani 1 1 d . . . . .
O11 O 0.7439(2) 1.04630(18) 0.03036(3) 0.0226(3) Uani 1 1 d . . . . .
H11 H 0.6469 1.0826 0.0230 0.027 Uiso 1 1 calc R U . . .
O8 O 0.6747(2) 0.23127(19) 0.09018(3) 0.0247(4) Uani 1 1 d . . . . .
H8 H 0.6832 0.2791 0.0732 0.030 Uiso 1 1 calc R U . . .
O12O O 1.1046(2) 1.00429(17) 0.01031(3) 0.0196(3) Uani 1 1 d . . . . .
H12O H 1.1231 0.9367 -0.0040 0.024 Uiso 1 1 calc R U . . .
O9 O 0.7675(2) 0.46431(18) 0.05126(3) 0.0224(3) Uani 1 1 d . . . . .
O10 O 0.6099(2) 0.79954(18) 0.02257(3) 0.0211(3) Uani 1 1 d . . . . .
C22 C 0.8255(3) 0.5500(3) 0.07306(4) 0.0163(4) Uani 1 1 d . . . . .
C16 C 0.8886(3) 0.5863(2) 0.12814(4) 0.0161(4) Uani 1 1 d . . . . .
C27 C 1.0265(3) 0.9723(3) 0.09171(4) 0.0180(4) Uani 1 1 d . . . . .
H27 H 1.0300 1.0414 0.1093 0.022 Uiso 1 1 calc R U . . .
C23 C 0.9027(3) 0.7143(2) 0.06926(4) 0.0152(4) Uani 1 1 d . . . . .
C28 C 0.9581(3) 0.8035(3) 0.09392(4) 0.0157(4) Uani 1 1 d . . . . .
C18 C 0.8278(3) 0.3729(3) 0.16428(5) 0.0190(4) Uani 1 1 d . . . . .
H18 H 0.8326 0.3318 0.1846 0.023 Uiso 1 1 calc R U . . .
C21 C 0.8209(3) 0.4888(2) 0.10433(4) 0.0161(4) Uani 1 1 d . . . . .
C19 C 0.7535(3) 0.2721(3) 0.14166(5) 0.0198(4) Uani 1 1 d . . . . .
H19 H 0.7060 0.1649 0.1466 0.024 Uiso 1 1 calc R U . . .
C24 C 0.9204(3) 0.7973(3) 0.03822(4) 0.0169(4) Uani 1 1 d . . . . .
H24 H 0.9432 0.7067 0.0230 0.020 Uiso 1 1 calc R U . . .
C25 C 1.0857(3) 0.9138(2) 0.03814(4) 0.0164(4) Uani 1 1 d . . . . .
H25 H 1.1948 0.8410 0.0402 0.020 Uiso 1 1 calc R U . . .
C26 C 1.0850(3) 1.0318(3) 0.06513(5) 0.0189(4) Uani 1 1 d . . . . .
C20 C 0.7494(3) 0.3291(3) 0.11184(4) 0.0178(4) Uani 1 1 d . . . . .
C17 C 0.8947(3) 0.5312(3) 0.15810(4) 0.0178(4) Uani 1 1 d . . . . .
H17 H 0.9431 0.5997 0.1738 0.021 Uiso 1 1 calc R U . . .
C29 C 0.7434(3) 0.8819(3) 0.02963(4) 0.0167(4) Uani 1 1 d . . . . .
C30 C 1.1594(4) 1.2051(3) 0.06247(5) 0.0281(5) Uani 1 1 d . . . . .
H30A H 1.1484 1.2625 0.0821 0.042 Uiso 1 1 calc R U . . .
H30B H 1.0918 1.2672 0.0470 0.042 Uiso 1 1 calc R U . . .
H30C H 1.2869 1.1994 0.0566 0.042 Uiso 1 1 calc R U . . .
O13 O 0.4629(2) 0.1864(2) 0.00814(4) 0.0290(4) Uani 1 1 d G . . . .
H13A H 0.3692 0.1408 -0.0004 0.043 Uiso 1 1 d G U . . .
H13B H 0.4801 0.2860 0.0006 0.043 Uiso 1 1 d G 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
O3 C7 1.264(2) . ?
O1 C13 1.349(2) . ?
O1 C1 1.376(2) . ?
O2 H2 0.8400 . ?
O2 C5 1.351(3) . ?
O6 H6 0.8400 . ?
O6 C10 1.427(2) . ?
O5 H5 0.8400 . ?
O5 C14 1.331(3) . ?
O4 C14 1.201(2) . ?
C6 C7 1.457(3) . ?
C6 C1 1.395(3) . ?
C6 C5 1.413(3) . ?
C12 H12 0.9500 . ?
C12 C11 1.330(3) . ?
C12 C13 1.444(3) . ?
C11 C10 1.507(3) . ?
C11 C15 1.495(3) . ?
C7 C8 1.426(3) . ?
C8 C13 1.360(3) . ?
C8 C9 1.514(3) . ?
C1 C2 1.388(3) . ?
C5 C4 1.390(3) . ?
C9 H9 1.0000 . ?
C9 C10 1.561(2) . ?
C9 C14 1.529(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.388(3) . ?
C10 H10 1.0000 . ?
C2 H2A 0.9500 . ?
C2 C3 1.382(3) . ?
C3 H3 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O7 C16 1.375(2) . ?
O7 C28 1.353(2) . ?
O11 H11 0.8400 . ?
O11 C29 1.312(3) . ?
O8 H8 0.8400 . ?
O8 C20 1.349(3) . ?
O12O H12O 0.8400 . ?
O12O C25 1.427(2) . ?
O9 C22 1.253(2) . ?
O10 C29 1.227(3) . ?
C22 C23 1.440(3) . ?
C22 C21 1.459(3) . ?
C16 C21 1.397(3) . ?
C16 C17 1.390(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.442(3) . ?
C27 C26 1.334(3) . ?
C23 C28 1.360(3) . ?
C23 C24 1.523(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(3) . ?
C18 C17 1.384(3) . ?
C21 C20 1.419(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.388(3) . ?
C24 H24 1.0000 . ?
C24 C25 1.537(3) . ?
C24 C29 1.522(3) . ?
C25 H25 1.0000 . ?
C25 C26 1.515(3) . ?
C26 C30 1.493(3) . ?
C17 H17 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O13 H13A 0.8697 . ?
O13 H13B 0.8700 . ?

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
C13 O1 C1 119.57(15) . . ?
C5 O2 H2 109.5 . . ?
C10 O6 H6 109.5 . . ?
C14 O5 H5 109.5 . . ?
C1 C6 C7 119.58(17) . . ?
C1 C6 C5 118.31(17) . . ?
C5 C6 C7 122.11(18) . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C13 121.33(18) . . ?
C13 C12 H12 119.3 . . ?
C12 C11 C10 120.53(17) . . ?
C12 C11 C15 121.93(18) . . ?
C15 C11 C10 117.16(17) . . ?
O3 C7 C6 121.06(17) . . ?
O3 C7 C8 122.52(17) . . ?
C8 C7 C6 116.42(17) . . ?
C7 C8 C9 120.09(16) . . ?
C13 C8 C7 119.99(17) . . ?
C13 C8 C9 119.78(17) . . ?
O1 C13 C12 112.84(17) . . ?
O1 C13 C8 123.54(18) . . ?
C8 C13 C12 123.61(17) . . ?
O1 C1 C6 120.85(17) . . ?
O1 C1 C2 116.56(17) . . ?
C2 C1 C6 122.59(19) . . ?
O2 C5 C6 121.28(18) . . ?
O2 C5 C4 118.95(18) . . ?
C4 C5 C6 119.75(19) . . ?
C8 C9 H9 107.1 . . ?
C8 C9 C10 113.26(16) . . ?
C8 C9 C14 111.01(15) . . ?
C10 C9 H9 107.1 . . ?
C14 C9 H9 107.1 . . ?
C14 C9 C10 110.93(15) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 C5 119.56(19) . . ?
C3 C4 H4 120.2 . . ?
O6 C10 C11 109.43(15) . . ?
O6 C10 C9 110.17(15) . . ?
O6 C10 H10 107.0 . . ?
C11 C10 C9 115.72(16) . . ?
C11 C10 H10 107.0 . . ?
C9 C10 H10 107.0 . . ?
C1 C2 H2A 121.3 . . ?
C3 C2 C1 117.41(19) . . ?
C3 C2 H2A 121.3 . . ?
C4 C3 H3 118.8 . . ?
C2 C3 C4 122.37(18) . . ?
C2 C3 H3 118.8 . . ?
O5 C14 C9 112.42(16) . . ?
O4 C14 O5 124.18(18) . . ?
O4 C14 C9 123.40(18) . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C28 O7 C16 119.07(15) . . ?
C29 O11 H11 109.5 . . ?
C20 O8 H8 109.5 . . ?
C25 O12O H12O 109.5 . . ?
O9 C22 C23 122.96(18) . . ?
O9 C22 C21 122.01(18) . . ?
C23 C22 C21 115.02(17) . . ?
O7 C16 C21 120.73(17) . . ?
O7 C16 C17 116.20(18) . . ?
C17 C16 C21 123.06(19) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C26 C27 C28 120.40(18) . . ?
C22 C23 C24 122.27(17) . . ?
C28 C23 C22 120.25(18) . . ?
C28 C23 C24 117.45(17) . . ?
O7 C28 C27 113.18(16) . . ?
O7 C28 C23 124.07(18) . . ?
C23 C28 C27 122.74(17) . . ?
C19 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C17 C18 C19 121.91(19) . . ?
C16 C21 C22 120.72(18) . . ?
C16 C21 C20 117.39(17) . . ?
C20 C21 C22 121.89(17) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.63(19) . . ?
C20 C19 H19 120.2 . . ?
C23 C24 H24 107.5 . . ?
C23 C24 C25 109.48(16) . . ?
C25 C24 H24 107.5 . . ?
C29 C24 C23 109.95(16) . . ?
C29 C24 H24 107.5 . . ?
C29 C24 C25 114.66(16) . . ?
O12O C25 C24 112.72(16) . . ?
O12O C25 H25 107.0 . . ?
O12O C25 C26 110.95(15) . . ?
C24 C25 H25 107.0 . . ?
C26 C25 C24 111.80(16) . . ?
C26 C25 H25 107.0 . . ?
C27 C26 C25 117.77(18) . . ?
C27 C26 C30 121.23(19) . . ?
C30 C26 C25 120.87(17) . . ?
O8 C20 C21 120.53(17) . . ?
O8 C20 C19 119.11(18) . . ?
C19 C20 C21 120.36(18) . . ?
C16 C17 H17 121.2 . . ?
C18 C17 C16 117.59(19) . . ?
C18 C17 H17 121.2 . . ?
O11 C29 C24 115.79(18) . . ?
O10 C29 O11 122.9(2) . . ?
O10 C29 C24 121.28(18) . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H13A O13 H13B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 C7 C8 C13 179.67(18) . . . . ?
O3 C7 C8 C9 3.9(3) . . . . ?
O1 C1 C2 C3 179.62(17) . . . . ?
O2 C5 C4 C3 177.88(18) . . . . ?
C6 C7 C8 C13 0.4(3) . . . . ?
C6 C7 C8 C9 -175.37(16) . . . . ?
C6 C1 C2 C3 -1.3(3) . . . . ?
C6 C5 C4 C3 -0.9(3) . . . . ?
C12 C11 C10 O6 147.78(18) . . . . ?
C12 C11 C10 C9 22.6(3) . . . . ?
C11 C12 C13 O1 175.12(18) . . . . ?
C11 C12 C13 C8 -4.5(3) . . . . ?
C7 C6 C1 O1 0.3(3) . . . . ?
C7 C6 C1 C2 -178.81(18) . . . . ?
C7 C6 C5 O2 1.1(3) . . . . ?
C7 C6 C5 C4 179.93(18) . . . . ?
C7 C8 C13 O1 1.6(3) . . . . ?
C7 C8 C13 C12 -178.83(17) . . . . ?
C7 C8 C9 C10 -165.20(16) . . . . ?
C7 C8 C9 C14 69.2(2) . . . . ?
C8 C9 C10 O6 -152.66(16) . . . . ?
C8 C9 C10 C11 -27.9(2) . . . . ?
C8 C9 C14 O5 50.8(2) . . . . ?
C8 C9 C14 O4 -129.4(2) . . . . ?
C13 O1 C1 C6 1.7(3) . . . . ?
C13 O1 C1 C2 -179.20(17) . . . . ?
C13 C12 C11 C10 -6.2(3) . . . . ?
C13 C12 C11 C15 -178.88(18) . . . . ?
C13 C8 C9 C10 19.0(2) . . . . ?
C13 C8 C9 C14 -106.5(2) . . . . ?
C1 O1 C13 C12 177.71(16) . . . . ?
C1 O1 C13 C8 -2.7(3) . . . . ?
C1 C6 C7 O3 179.47(18) . . . . ?
C1 C6 C7 C8 -1.3(3) . . . . ?
C1 C6 C5 O2 -178.35(17) . . . . ?
C1 C6 C5 C4 0.4(3) . . . . ?
C1 C2 C3 C4 0.8(3) . . . . ?
C5 C6 C7 O3 0.0(3) . . . . ?
C5 C6 C7 C8 179.25(17) . . . . ?
C5 C6 C1 O1 179.76(16) . . . . ?
C5 C6 C1 C2 0.7(3) . . . . ?
C5 C4 C3 C2 0.3(3) . . . . ?
C9 C8 C13 O1 177.37(17) . . . . ?
C9 C8 C13 C12 -3.0(3) . . . . ?
C10 C9 C14 O5 -76.1(2) . . . . ?
C10 C9 C14 O4 103.7(2) . . . . ?
C14 C9 C10 O6 -27.1(2) . . . . ?
C14 C9 C10 C11 97.71(19) . . . . ?
C15 C11 C10 O6 -39.2(2) . . . . ?
C15 C11 C10 C9 -164.31(17) . . . . ?
O7 C16 C21 C22 3.2(3) . . . . ?
O7 C16 C21 C20 -177.17(16) . . . . ?
O7 C16 C17 C18 178.79(17) . . . . ?
O12O C25 C26 C27 164.55(18) . . . . ?
O12O C25 C26 C30 -19.6(3) . . . . ?
O9 C22 C23 C28 177.89(19) . . . . ?
O9 C22 C23 C24 -0.1(3) . . . . ?
O9 C22 C21 C16 179.19(19) . . . . ?
O9 C22 C21 C20 -0.4(3) . . . . ?
C22 C23 C28 O7 2.9(3) . . . . ?
C22 C23 C28 C27 -176.25(18) . . . . ?
C22 C23 C24 C25 -149.84(18) . . . . ?
C22 C23 C24 C29 83.3(2) . . . . ?
C22 C21 C20 O8 -3.2(3) . . . . ?
C22 C21 C20 C19 177.47(19) . . . . ?
C16 O7 C28 C27 179.36(16) . . . . ?
C16 O7 C28 C23 0.1(3) . . . . ?
C16 C21 C20 O8 177.16(18) . . . . ?
C16 C21 C20 C19 -2.2(3) . . . . ?
C23 C22 C21 C16 -0.2(3) . . . . ?
C23 C22 C21 C20 -179.85(17) . . . . ?
C23 C24 C25 O12O -176.36(15) . . . . ?
C23 C24 C25 C26 -50.6(2) . . . . ?
C23 C24 C29 O11 108.22(19) . . . . ?
C23 C24 C29 O10 -71.7(2) . . . . ?
C28 O7 C16 C21 -3.2(3) . . . . ?
C28 O7 C16 C17 177.08(17) . . . . ?
C28 C27 C26 C25 -3.1(3) . . . . ?
C28 C27 C26 C30 -178.89(19) . . . . ?
C28 C23 C24 C25 32.1(2) . . . . ?
C28 C23 C24 C29 -94.7(2) . . . . ?
C18 C19 C20 O8 -179.06(18) . . . . ?
C18 C19 C20 C21 0.3(3) . . . . ?
C21 C22 C23 C28 -2.7(3) . . . . ?
C21 C22 C23 C24 179.34(18) . . . . ?
C21 C16 C17 C18 -0.9(3) . . . . ?
C19 C18 C17 C16 -1.1(3) . . . . ?
C24 C23 C28 O7 -179.06(18) . . . . ?
C24 C23 C28 C27 1.8(3) . . . . ?
C24 C25 C26 C27 37.8(3) . . . . ?
C24 C25 C26 C30 -146.39(19) . . . . ?
C25 C24 C29 O11 -15.6(2) . . . . ?
C25 C24 C29 O10 164.48(17) . . . . ?
C26 C27 C28 O7 162.17(19) . . . . ?
C26 C27 C28 C23 -18.6(3) . . . . ?
C17 C16 C21 C22 -177.11(19) . . . . ?
C17 C16 C21 C20 2.5(3) . . . . ?
C17 C18 C19 C20 1.4(3) . . . . ?
C29 C24 C25 O12O -52.3(2) . . . . ?
C29 C24 C25 C26 73.5(2) . . . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-3
