# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_h008
_database_code_depnum_ccdc_archive 'CCDC 1578212'
_audit_update_record             
;
2017-10-05 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H30 Er O9 S3'
_chemical_formula_weight         797.98

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.1961(18)
_cell_length_b                   15.1961(18)
_cell_length_c                   23.961(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4791.8(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2331
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      22.43

_exptl_crystal_description       'prism frag'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             2388
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.148
_exptl_absorpt_coefficient_mu    2.874
_shelx_estimated_absorpt_T_min   0.504
_shelx_estimated_absorpt_T_max   0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\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            9413
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.299
_diffrn_reflns_theta_max         26.858
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2289
_reflns_number_gt                2030
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²+73.2726P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2289
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1254
_refine_ls_wR_factor_gt          0.1182
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.002
_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
Er1 Er 0.6667 0.3333 0.51298(2) 0.02548(17) Uani 1 3 d S T P . .
O1 O 0.5510(3) 0.3277(3) 0.57821(17) 0.0316(9) Uani 1 1 d . . . . .
O2 O 0.4775(3) 0.1757(3) 0.53860(15) 0.0314(9) Uani 1 1 d . . . . .
C1 C 0.4816(4) 0.2339(4) 0.5760(2) 0.0250(11) Uani 1 1 d . . . . .
C2 C 0.4045(4) 0.1975(4) 0.6230(2) 0.0203(10) Uani 1 1 d . . . . .
C3 C 0.4304(4) 0.1777(4) 0.6759(2) 0.0200(10) Uani 1 1 d . . . . .
C4 C 0.5277(4) 0.1867(4) 0.6870(2) 0.0270(11) Uani 1 1 d . . . . .
H4 H 0.5769 0.2072 0.6581 0.032 Uiso 1 1 calc R U . . .
C5 C 0.5495(5) 0.1656(5) 0.7391(2) 0.0311(12) Uani 1 1 d . . . . .
H5 H 0.6142 0.1727 0.7460 0.037 Uiso 1 1 calc R U . . .
C6 C 0.4773(4) 0.1336(5) 0.7827(2) 0.0294(12) Uani 1 1 d . . . . .
H6 H 0.4936 0.1190 0.8185 0.035 Uiso 1 1 calc R U . . .
C7 C 0.3847(4) 0.1237(4) 0.7734(2) 0.0228(10) Uani 1 1 d . . . . .
H7 H 0.3368 0.1015 0.8030 0.027 Uiso 1 1 calc R U . . .
C8 C 0.3573(4) 0.1459(4) 0.72031(19) 0.0193(9) Uani 1 1 d . . . . .
O3 O 0.5660(3) 0.3544(3) 0.44937(16) 0.0303(9) Uani 1 1 d . . . . .
S1 S 0.49679(14) 0.40043(13) 0.45512(7) 0.0393(4) Uani 1 1 d . . . . .
C9 C 0.5542(9) 0.5165(7) 0.4163(5) 0.080(3) Uani 1 1 d . . . . .
H9A H 0.6156 0.5672 0.4355 0.120 Uiso 1 1 calc R U . . .
H9B H 0.5062 0.5415 0.4130 0.120 Uiso 1 1 calc R U . . .
H9C H 0.5721 0.5042 0.3789 0.120 Uiso 1 1 calc R U . . .
C10 C 0.3943(6) 0.3290(7) 0.4089(3) 0.0528(19) Uani 1 1 d . . . . .
H10A H 0.4194 0.3411 0.3704 0.079 Uiso 1 1 calc R U . . .
H10B H 0.3432 0.3499 0.4131 0.079 Uiso 1 1 calc R U . . .
H10C H 0.3637 0.2565 0.4176 0.079 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
Er1 O3 2.293(4) 2_655 ?
Er1 O3 2.293(4) 3_665 ?
Er1 O3 2.293(4) . ?
Er1 O1 2.322(4) . ?
Er1 O1 2.322(4) 2_655 ?
Er1 O1 2.322(4) 3_665 ?
Er1 O2 2.737(4) 2_655 ?
Er1 O2 2.737(4) 3_665 ?
Er1 O2 2.737(4) . ?
Er1 C1 2.867(5) . ?
Er1 C1 2.867(5) 2_655 ?
Er1 C1 2.867(5) 3_665 ?
O1 C1 1.281(7) . ?
O2 C1 1.239(7) . ?
C1 C2 1.517(7) . ?
C2 C8 1.397(7) 13_556 ?
C2 C3 1.402(7) . ?
C3 C8 1.436(7) . ?
C3 C4 1.441(7) . ?
C4 C5 1.369(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.413(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.356(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.430(7) . ?
C7 H7 0.9500 . ?
C8 C2 1.397(7) 13_556 ?
O3 S1 1.532(4) . ?
S1 C10 1.772(7) . ?
S1 C9 1.789(9) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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
O3 Er1 O3 80.64(15) 2_655 3_665 ?
O3 Er1 O3 80.64(15) 2_655 . ?
O3 Er1 O3 80.64(15) 3_665 . ?
O3 Er1 O1 128.31(15) 2_655 . ?
O3 Er1 O1 144.66(15) 3_665 . ?
O3 Er1 O1 84.64(14) . . ?
O3 Er1 O1 84.64(14) 2_655 2_655 ?
O3 Er1 O1 128.31(14) 3_665 2_655 ?
O3 Er1 O1 144.66(15) . 2_655 ?
O1 Er1 O1 79.65(15) . 2_655 ?
O3 Er1 O1 144.66(15) 2_655 3_665 ?
O3 Er1 O1 84.64(15) 3_665 3_665 ?
O3 Er1 O1 128.31(15) . 3_665 ?
O1 Er1 O1 79.65(15) . 3_665 ?
O1 Er1 O1 79.65(15) 2_655 3_665 ?
O3 Er1 O2 77.84(14) 2_655 2_655 ?
O3 Er1 O2 77.33(13) 3_665 2_655 ?
O3 Er1 O2 151.30(13) . 2_655 ?
O1 Er1 O2 123.75(13) . 2_655 ?
O1 Er1 O2 51.12(13) 2_655 2_655 ?
O1 Er1 O2 67.63(13) 3_665 2_655 ?
O3 Er1 O2 151.30(13) 2_655 3_665 ?
O3 Er1 O2 77.83(14) 3_665 3_665 ?
O3 Er1 O2 77.33(13) . 3_665 ?
O1 Er1 O2 67.62(13) . 3_665 ?
O1 Er1 O2 123.74(13) 2_655 3_665 ?
O1 Er1 O2 51.12(13) 3_665 3_665 ?
O2 Er1 O2 115.12(6) 2_655 3_665 ?
O3 Er1 O2 77.33(13) 2_655 . ?
O3 Er1 O2 151.30(13) 3_665 . ?
O3 Er1 O2 77.84(14) . . ?
O1 Er1 O2 51.12(13) . . ?
O1 Er1 O2 67.62(13) 2_655 . ?
O1 Er1 O2 123.74(13) 3_665 . ?
O2 Er1 O2 115.12(6) 2_655 . ?
O2 Er1 O2 115.12(6) 3_665 . ?
O3 Er1 C1 102.72(15) 2_655 . ?
O3 Er1 C1 162.44(15) 3_665 . ?
O3 Er1 C1 82.91(15) . . ?
O1 Er1 C1 25.97(15) . . ?
O1 Er1 C1 69.24(15) 2_655 . ?
O1 Er1 C1 100.94(15) 3_665 . ?
O2 Er1 C1 120.21(13) 2_655 . ?
O2 Er1 C1 92.62(14) 3_665 . ?
O2 Er1 C1 25.41(14) . . ?
O3 Er1 C1 82.91(15) 2_655 2_655 ?
O3 Er1 C1 102.72(15) 3_665 2_655 ?
O3 Er1 C1 162.44(15) . 2_655 ?
O1 Er1 C1 100.94(15) . 2_655 ?
O1 Er1 C1 25.98(15) 2_655 2_655 ?
O1 Er1 C1 69.24(14) 3_665 2_655 ?
O2 Er1 C1 25.41(14) 2_655 2_655 ?
O2 Er1 C1 120.21(13) 3_665 2_655 ?
O2 Er1 C1 92.62(14) . 2_655 ?
C1 Er1 C1 94.81(14) . 2_655 ?
O3 Er1 C1 162.44(15) 2_655 3_665 ?
O3 Er1 C1 82.91(15) 3_665 3_665 ?
O3 Er1 C1 102.72(15) . 3_665 ?
O1 Er1 C1 69.24(15) . 3_665 ?
O1 Er1 C1 100.94(15) 2_655 3_665 ?
O1 Er1 C1 25.98(15) 3_665 3_665 ?
O2 Er1 C1 92.62(14) 2_655 3_665 ?
O2 Er1 C1 25.41(14) 3_665 3_665 ?
O2 Er1 C1 120.21(13) . 3_665 ?
C1 Er1 C1 94.81(14) . 3_665 ?
C1 Er1 C1 94.81(14) 2_655 3_665 ?
C1 O1 Er1 101.5(3) . . ?
C1 O2 Er1 83.2(3) . . ?
O2 C1 O1 123.0(5) . . ?
O2 C1 C2 121.6(5) . . ?
O1 C1 C2 115.5(5) . . ?
O2 C1 Er1 71.4(3) . . ?
O1 C1 Er1 52.5(3) . . ?
C2 C1 Er1 163.5(4) . . ?
C8 C2 C3 121.2(5) 13_556 . ?
C8 C2 C1 118.8(4) 13_556 . ?
C3 C2 C1 120.0(5) . . ?
C2 C3 C8 119.3(5) . . ?
C2 C3 C4 122.1(5) . . ?
C8 C3 C4 118.6(5) . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.2(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 120.1(5) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 121.8(5) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C2 C8 C7 122.3(5) 13_556 . ?
C2 C8 C3 119.5(4) 13_556 . ?
C7 C8 C3 118.2(5) . . ?
S1 O3 Er1 131.5(2) . . ?
O3 S1 C10 104.9(3) . . ?
O3 S1 C9 107.2(4) . . ?
C10 S1 C9 97.1(5) . . ?
S1 C9 H9A 109.5 . . ?
S1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
S1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
S1 C10 H10A 109.5 . . ?
S1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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
Er1 O2 C1 O1 10.6(5) . . . . ?
Er1 O2 C1 C2 -168.6(5) . . . . ?
Er1 O1 C1 O2 -12.6(6) . . . . ?
Er1 O1 C1 C2 166.6(4) . . . . ?
O2 C1 C2 C8 -79.6(7) . . . 13_556 ?
O1 C1 C2 C8 101.1(6) . . . 13_556 ?
Er1 C1 C2 C8 141.3(11) . . . 13_556 ?
O2 C1 C2 C3 102.3(6) . . . . ?
O1 C1 C2 C3 -77.0(6) . . . . ?
Er1 C1 C2 C3 -36.7(15) . . . . ?
C8 C2 C3 C8 0.3(8) 13_556 . . . ?
C1 C2 C3 C8 178.4(5) . . . . ?
C8 C2 C3 C4 179.4(5) 13_556 . . . ?
C1 C2 C3 C4 -2.6(8) . . . . ?
C2 C3 C4 C5 -179.4(5) . . . . ?
C8 C3 C4 C5 -0.3(8) . . . . ?
C3 C4 C5 C6 0.8(9) . . . . ?
C4 C5 C6 C7 -0.4(9) . . . . ?
C5 C6 C7 C8 -0.6(9) . . . . ?
C6 C7 C8 C2 179.9(5) . . . 13_556 ?
C6 C7 C8 C3 1.1(8) . . . . ?
C2 C3 C8 C2 -0.3(8) . . . 13_556 ?
C4 C3 C8 C2 -179.4(5) . . . 13_556 ?
C2 C3 C8 C7 178.5(5) . . . . ?
C4 C3 C8 C7 -0.6(7) . . . . ?
Er1 O3 S1 C10 -146.4(4) . . . . ?
Er1 O3 S1 C9 111.1(5) . . . . ?

_refine_diff_density_max         1.926
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.176

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_h009
_database_code_depnum_ccdc_archive 'CCDC 1578213'
_audit_update_record             
;
2017-10-05 deposited with the CCDC.
2017-11-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H30 Ho O9 S3'
_chemical_formula_weight         795.65

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.229(2)
_cell_length_b                   15.229(2)
_cell_length_c                   23.906(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4801.3(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1832
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      22.24

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             2382
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.148
_exptl_absorpt_coefficient_mu    2.718
_shelx_estimated_absorpt_T_min   0.521
_shelx_estimated_absorpt_T_max   0.689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\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            11460
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.300
_diffrn_reflns_theta_max         28.272
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2660
_reflns_number_gt                2222
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0829P)²+35.0531P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2660
_refine_ls_number_parameters     132
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1423
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_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
Ho1 Ho 0.6667 0.3333 0.51310(2) 0.02746(17) Uani 1 3 d S T P . .
O1 O 0.5514(3) 0.3286(3) 0.57914(16) 0.0334(8) Uani 1 1 d . . . . .
O2 O 0.4785(3) 0.1774(3) 0.53853(15) 0.0330(8) Uani 1 1 d . . . . .
C1 C 0.4819(4) 0.2347(4) 0.5763(2) 0.0264(10) Uani 1 1 d . . . . .
C2 C 0.4045(4) 0.1980(3) 0.62323(19) 0.0223(9) Uani 1 1 d . . . . .
C3 C 0.4302(4) 0.1781(4) 0.67631(19) 0.0217(9) Uani 1 1 d . . . . .
C4 C 0.5272(4) 0.1873(4) 0.6876(2) 0.0297(11) Uani 1 1 d . . . . .
H4 H 0.5768 0.2087 0.6589 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5482(4) 0.1652(5) 0.7398(2) 0.0334(12) Uani 1 1 d . . . . .
H5 H 0.6126 0.1716 0.7468 0.040 Uiso 1 1 calc R U . . .
C6 C 0.4766(4) 0.1335(4) 0.7830(2) 0.0325(11) Uani 1 1 d . . . . .
H6 H 0.4930 0.1190 0.8189 0.039 Uiso 1 1 calc R U . . .
C7 C 0.3834(4) 0.1232(4) 0.77381(19) 0.0249(10) Uani 1 1 d . . . . .
H7 H 0.3354 0.1008 0.8034 0.030 Uiso 1 1 calc R U . . .
C8 C 0.3567(4) 0.1455(3) 0.72052(19) 0.0213(9) Uani 1 1 d . . . . .
O3 O 0.5659(3) 0.3550(3) 0.44885(16) 0.0335(8) Uani 1 1 d . . . . .
S1 S 0.49697(13) 0.40118(12) 0.45503(7) 0.0429(4) Uani 1 1 d . . . . .
C9 C 0.5543(9) 0.5169(7) 0.4168(5) 0.090(3) Uani 1 1 d . . . . .
H9A H 0.5962 0.5732 0.4420 0.135 Uiso 1 1 calc R U . . .
H9B H 0.5014 0.5274 0.4003 0.135 Uiso 1 1 calc R U . . .
H9C H 0.5968 0.5137 0.3870 0.135 Uiso 1 1 calc R U . . .
C10 C 0.3942(6) 0.3297(6) 0.4093(3) 0.0554(18) Uani 1 1 d . . . . .
H10A H 0.4186 0.3412 0.3706 0.083 Uiso 1 1 calc R U . . .
H10B H 0.3434 0.3508 0.4137 0.083 Uiso 1 1 calc R U . . .
H10C H 0.3635 0.2575 0.4183 0.083 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
Ho1 O3 2.309(4) . ?
Ho1 O3 2.309(4) 3_665 ?
Ho1 O3 2.309(4) 2_655 ?
Ho1 O1 2.335(4) 2_655 ?
Ho1 O1 2.335(4) 3_665 ?
Ho1 O1 2.335(4) . ?
Ho1 O2 2.723(4) 2_655 ?
Ho1 O2 2.723(4) 3_665 ?
Ho1 O2 2.723(4) . ?
Ho1 C1 2.868(5) 2_655 ?
Ho1 C1 2.868(5) 3_665 ?
Ho1 C1 2.868(5) . ?
O1 C1 1.288(7) . ?
O2 C1 1.238(6) . ?
C1 C2 1.517(7) . ?
C2 C8 1.391(7) 13_556 ?
C2 C3 1.405(6) . ?
C3 C8 1.436(7) . ?
C3 C4 1.438(7) . ?
C4 C5 1.370(7) . ?
C5 C6 1.401(8) . ?
C6 C7 1.366(7) . ?
C7 C8 1.430(6) . ?
C8 C2 1.391(7) 13_556 ?
O3 S1 1.535(4) . ?
S1 C10 1.768(7) . ?
S1 C9 1.779(9) . ?

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
O3 Ho1 O3 80.56(15) . 3_665 ?
O3 Ho1 O3 80.56(15) . 2_655 ?
O3 Ho1 O3 80.56(15) 3_665 2_655 ?
O3 Ho1 O1 144.61(14) . 2_655 ?
O3 Ho1 O1 128.56(14) 3_665 2_655 ?
O3 Ho1 O1 84.90(14) 2_655 2_655 ?
O3 Ho1 O1 128.56(14) . 3_665 ?
O3 Ho1 O1 84.90(14) 3_665 3_665 ?
O3 Ho1 O1 144.61(14) 2_655 3_665 ?
O1 Ho1 O1 79.29(15) 2_655 3_665 ?
O3 Ho1 O1 84.91(14) . . ?
O3 Ho1 O1 144.61(14) 3_665 . ?
O3 Ho1 O1 128.56(14) 2_655 . ?
O1 Ho1 O1 79.29(15) 2_655 . ?
O1 Ho1 O1 79.29(15) 3_665 . ?
O3 Ho1 O2 151.19(12) . 2_655 ?
O3 Ho1 O2 77.34(12) 3_665 2_655 ?
O3 Ho1 O2 77.79(13) 2_655 2_655 ?
O1 Ho1 O2 51.34(12) 2_655 2_655 ?
O1 Ho1 O2 67.57(13) 3_665 2_655 ?
O1 Ho1 O2 123.59(12) . 2_655 ?
O3 Ho1 O2 77.34(12) . 3_665 ?
O3 Ho1 O2 77.80(13) 3_665 3_665 ?
O3 Ho1 O2 151.19(12) 2_655 3_665 ?
O1 Ho1 O2 123.59(12) 2_655 3_665 ?
O1 Ho1 O2 51.34(12) 3_665 3_665 ?
O1 Ho1 O2 67.57(13) . 3_665 ?
O2 Ho1 O2 115.16(5) 2_655 3_665 ?
O3 Ho1 O2 77.79(13) . . ?
O3 Ho1 O2 151.19(12) 3_665 . ?
O3 Ho1 O2 77.34(12) 2_655 . ?
O1 Ho1 O2 67.57(13) 2_655 . ?
O1 Ho1 O2 123.59(12) 3_665 . ?
O1 Ho1 O2 51.34(12) . . ?
O2 Ho1 O2 115.16(5) 2_655 . ?
O2 Ho1 O2 115.16(5) 3_665 . ?
O3 Ho1 C1 162.41(14) . 2_655 ?
O3 Ho1 C1 102.74(15) 3_665 2_655 ?
O3 Ho1 C1 82.94(14) 2_655 2_655 ?
O1 Ho1 C1 26.18(14) 2_655 2_655 ?
O1 Ho1 C1 69.02(14) 3_665 2_655 ?
O1 Ho1 C1 100.80(14) . 2_655 ?
O2 Ho1 C1 25.41(13) 2_655 2_655 ?
O2 Ho1 C1 120.24(12) 3_665 2_655 ?
O2 Ho1 C1 92.69(14) . 2_655 ?
O3 Ho1 C1 102.74(15) . 3_665 ?
O3 Ho1 C1 82.94(14) 3_665 3_665 ?
O3 Ho1 C1 162.41(14) 2_655 3_665 ?
O1 Ho1 C1 100.80(14) 2_655 3_665 ?
O1 Ho1 C1 26.18(14) 3_665 3_665 ?
O1 Ho1 C1 69.02(14) . 3_665 ?
O2 Ho1 C1 92.69(14) 2_655 3_665 ?
O2 Ho1 C1 25.41(13) 3_665 3_665 ?
O2 Ho1 C1 120.24(12) . 3_665 ?
C1 Ho1 C1 94.83(13) 2_655 3_665 ?
O3 Ho1 C1 82.94(14) . . ?
O3 Ho1 C1 162.41(14) 3_665 . ?
O3 Ho1 C1 102.74(15) 2_655 . ?
O1 Ho1 C1 69.02(14) 2_655 . ?
O1 Ho1 C1 100.80(14) 3_665 . ?
O1 Ho1 C1 26.17(15) . . ?
O2 Ho1 C1 120.24(12) 2_655 . ?
O2 Ho1 C1 92.69(14) 3_665 . ?
O2 Ho1 C1 25.41(13) . . ?
C1 Ho1 C1 94.83(13) 2_655 . ?
C1 Ho1 C1 94.83(13) 3_665 . ?
C1 O1 Ho1 100.7(3) . . ?
C1 O2 Ho1 83.9(3) . . ?
O2 C1 O1 122.9(5) . . ?
O2 C1 C2 121.9(5) . . ?
O1 C1 C2 115.2(4) . . ?
O2 C1 Ho1 70.7(3) . . ?
O1 C1 Ho1 53.1(3) . . ?
C2 C1 Ho1 163.8(3) . . ?
C8 C2 C3 121.5(4) 13_556 . ?
C8 C2 C1 118.6(4) 13_556 . ?
C3 C2 C1 119.9(4) . . ?
C2 C3 C8 119.1(4) . . ?
C2 C3 C4 122.2(4) . . ?
C8 C3 C4 118.8(4) . . ?
C5 C4 C3 120.1(5) . . ?
C4 C5 C6 121.3(5) . . ?
C7 C6 C5 120.4(5) . . ?
C6 C7 C8 121.3(5) . . ?
C2 C8 C7 122.3(4) 13_556 . ?
C2 C8 C3 119.5(4) 13_556 . ?
C7 C8 C3 118.2(4) . . ?
S1 O3 Ho1 131.1(2) . . ?
O3 S1 C10 104.8(3) . . ?
O3 S1 C9 107.1(4) . . ?
C10 S1 C9 97.9(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C9 H9A S1 0.98 2.96 3.540(12) 118.8 10_666
C10 H10B O2 0.98 2.60 3.451(9) 145.4 12_556

_refine_diff_density_max         2.140
_refine_diff_density_min         -1.663
_refine_diff_density_rms         0.174

_shelxl_version_number           2014-3

