# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_Dy3
_database_code_depnum_ccdc_archive 'CCDC 1983277'
loop_
_audit_author_name
_audit_author_address
'Yang Liu'
;SunYatSenUniversity
China
;
_audit_update_record             
;
2020-02-11 deposited with the CCDC.	2020-07-06 downloaded from the CCDC.
;
_audit_creation_date             2020-02-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C85 H78 Cl6 Dy3 N12 O9, 2(C0.5 F1.5 O1.5 S0.5)'
_chemical_formula_sum            'C86 H78 Cl6 Dy3 F3 N12 O12 S'
_chemical_formula_weight         2260.86
_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 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.9365(5)
_cell_length_b                   15.9365(5)
_cell_length_c                   34.8754(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7670.7(5)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9224
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.527
_cell_measurement_theta_min      2.556
_shelx_estimated_absorpt_T_max   0.838
_shelx_estimated_absorpt_T_min   0.784
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_T_max  0.0949
_exptl_absorpt_correction_T_min  0.0669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0873 before and 0.0434 after correction. The Ratio of minimum to maximum transmission is 0.7050. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3351
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.076
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            22955
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         3.009
_diffrn_ambient_temperature      119.86
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'I\mS microfocus'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3863
_reflns_number_total             3918
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.177
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.269(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3918
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0247
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0514P)²+13.8985P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0754
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.731(14)
 0.269(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: S1(0.16667) F1(0.5) O3(0.5) C16(0.16667)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15)
;
_atom_sites_solution_hydrogens   geom
_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
Dy1 Dy 1.17489(2) 1.000000 1.000000 0.02429(10) Uani 1 2 d S T P . .
Cl1 Cl 1.16420(10) 0.77756(10) 1.19875(4) 0.0385(3) Uani 1 1 d . . . . .
O1 O 1.000000 0.9200(3) 1.000000 0.0262(9) Uani 1 2 d S T P . .
O2 O 1.1421(3) 0.9801(3) 1.06204(10) 0.0384(8) Uani 1 1 d . . . . .
N1 N 1.2729(3) 0.9208(3) 1.02936(11) 0.0249(8) Uani 1 1 d . . . . .
N2 N 1.1248(3) 0.8332(3) 0.97613(14) 0.0322(10) Uani 1 1 d . . . . .
C1 C 1.000000 1.000000 1.000000 0.028(2) Uani 1 6 d S T P . .
C2 C 1.1488(4) 0.9374(4) 1.09342(14) 0.0310(10) Uani 1 1 d . . . . .
C3 C 1.0781(4) 0.9075(5) 1.12267(15) 0.0394(13) Uani 1 1 d . . . . .
H3 H 1.025961 0.920054 1.120258 0.047 Uiso 1 1 calc R . . . .
C4 C 1.0844(4) 0.8602(4) 1.15464(15) 0.0376(12) Uani 1 1 d . . . . .
H4 H 1.036655 0.840853 1.174149 0.045 Uiso 1 1 calc R . . . .
C5 C 1.1573(4) 0.8411(4) 1.15871(14) 0.0339(11) Uani 1 1 d . . . . .
C6 C 1.2309(4) 0.8720(4) 1.13065(14) 0.0313(10) Uani 1 1 d . . . . .
H6 H 1.283167 0.859939 1.133806 0.038 Uiso 1 1 calc R . . . .
C7 C 1.2258(3) 0.9198(3) 1.09879(12) 0.0274(9) Uani 1 1 d . . . . .
C8 C 1.3062(4) 0.9553(4) 1.06903(13) 0.0297(10) Uani 1 1 d . . . . .
H8A H 1.341574 1.027053 1.068997 0.036 Uiso 1 1 calc R . . . .
H8B H 1.352480 0.934202 1.076814 0.036 Uiso 1 1 calc R . . . .
C9 C 1.3581(4) 0.9475(4) 1.00495(13) 0.0262(9) Uani 1 1 d . . . . .
H9A H 1.336957 0.908854 0.981046 0.031 Uiso 1 1 calc R . . . .
H9B H 1.402861 0.931411 1.018514 0.031 Uiso 1 1 calc R . . . .
C10 C 1.2099(4) 0.8130(4) 1.02945(14) 0.0325(11) Uani 1 1 d . . . . .
H10A H 1.163706 0.793539 1.051114 0.039 Uiso 1 1 calc R . . . .
H10B H 1.250683 0.783069 1.033394 0.039 Uiso 1 1 calc R . . . .
C11 C 1.1540(4) 0.7756(4) 0.99247(15) 0.0308(11) Uani 1 1 d . . . . .
C12 C 1.1296(5) 0.6851(4) 0.97749(17) 0.0438(15) Uani 1 1 d . . . . .
H12 H 1.151278 0.645965 0.989599 0.053 Uiso 1 1 calc R . . . .
C13 C 1.0738(5) 0.6536(4) 0.94491(17) 0.0441(14) Uani 1 1 d . . . . .
H13 H 1.057725 0.592780 0.933980 0.053 Uiso 1 1 calc R . . . .
C14 C 1.0420(4) 0.7089(4) 0.92852(17) 0.0384(12) Uani 1 1 d . . . . .
H14 H 1.001653 0.686620 0.906479 0.046 Uiso 1 1 calc R . . . .
C15 C 1.0692(4) 0.7995(4) 0.94436(16) 0.0391(12) Uani 1 1 d . . . . .
H15 H 1.047710 0.838918 0.932319 0.047 Uiso 1 1 calc R . . . .
S1 S 1.333333 0.666667 1.05146(13) 0.0274(8) Uani 0.5 3 d S T P A 1
F1 F 1.2898(6) 0.7124(6) 1.1181(3) 0.059(2) Uani 0.5 1 d . . . A 1
O3 O 1.2306(6) 0.6158(6) 1.0419(3) 0.044(2) Uani 0.5 1 d . . . A 1
C16 C 1.333333 0.666667 1.0958(5) 0.0319(16) Uani 0.5 3 d S TU P A 1


_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
Dy1 O1 2.4166(4) . ?
Dy1 O1 2.4166(3) 2_765 ?
Dy1 O2 2.211(3) . ?
Dy1 O2 2.211(3) 4_677 ?
Dy1 N1 2.655(4) 4_677 ?
Dy1 N1 2.655(4) . ?
Dy1 N2 2.504(5) 4_677 ?
Dy1 N2 2.504(5) . ?
Dy1 C1 2.7871(3) . ?
Cl1 C5 1.759(6) . ?
O1 C1 1.274(5) . ?
O2 C2 1.321(6) . ?
N1 C8 1.485(6) . ?
N1 C9 1.475(6) . ?
N1 C10 1.495(7) . ?
N2 C11 1.346(7) . ?
N2 C15 1.351(7) . ?
C2 C3 1.415(7) . ?
C2 C7 1.402(7) . ?
C3 C4 1.377(9) . ?
C4 C5 1.349(9) . ?
C5 C6 1.413(7) . ?
C6 C7 1.372(7) . ?
C7 C8 1.521(6) . ?
C9 C9 1.490(10) 4_677 ?
C10 C11 1.511(7) . ?
C11 C12 1.394(8) . ?
C12 C13 1.374(8) . ?
C13 C14 1.343(9) . ?
C14 C15 1.398(7) . ?
S1 O3 1.456(8) . ?
S1 O3 1.456(8) 2_755 ?
S1 O3 1.456(8) 3_775 ?
S1 C16 1.545(19) . ?
F1 C16 1.458(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O1 54.3(2) . 2_765 ?
O1 Dy1 N1 157.31(8) . 4_677 ?
O1 Dy1 N1 123.13(15) 2_765 4_677 ?
O1 Dy1 N1 123.13(15) . . ?
O1 Dy1 N1 157.31(8) 2_765 . ?
O1 Dy1 N2 76.62(15) . . ?
O1 Dy1 N2 127.44(15) . 4_677 ?
O1 Dy1 N2 127.44(16) 2_765 . ?
O1 Dy1 N2 76.62(16) 2_765 4_677 ?
O1 Dy1 C1 27.17(12) 2_765 . ?
O1 Dy1 C1 27.17(12) . . ?
O2 Dy1 O1 78.29(10) . . ?
O2 Dy1 O1 78.29(10) 4_677 2_765 ?
O2 Dy1 O1 84.85(11) 4_677 . ?
O2 Dy1 O1 84.85(11) . 2_765 ?
O2 Dy1 O2 161.1(2) . 4_677 ?
O2 Dy1 N1 124.35(13) 4_677 . ?
O2 Dy1 N1 124.35(13) . 4_677 ?
O2 Dy1 N1 72.99(13) . . ?
O2 Dy1 N1 72.99(13) 4_677 4_677 ?
O2 Dy1 N2 104.26(16) . . ?
O2 Dy1 N2 79.83(16) 4_677 . ?
O2 Dy1 N2 79.83(16) . 4_677 ?
O2 Dy1 N2 104.26(16) 4_677 4_677 ?
O2 Dy1 C1 80.53(10) 4_677 . ?
O2 Dy1 C1 80.53(10) . . ?
N1 Dy1 N1 68.68(18) 4_677 . ?
N1 Dy1 C1 145.66(9) 4_677 . ?
N1 Dy1 C1 145.66(9) . . ?
N2 Dy1 N1 64.86(14) 4_677 4_677 ?
N2 Dy1 N1 64.85(13) . . ?
N2 Dy1 N1 94.33(14) . 4_677 ?
N2 Dy1 N1 94.33(14) 4_677 . ?
N2 Dy1 N2 155.6(2) . 4_677 ?
N2 Dy1 C1 102.22(11) . . ?
N2 Dy1 C1 102.22(11) 4_677 . ?
Dy1 O1 Dy1 174.3(2) 3_675 . ?
C1 O1 Dy1 92.83(12) . . ?
C1 O1 Dy1 92.83(12) . 3_675 ?
C2 O2 Dy1 144.1(3) . . ?
C8 N1 Dy1 111.7(3) . . ?
C8 N1 C10 109.5(4) . . ?
C9 N1 Dy1 108.4(3) . . ?
C9 N1 C8 108.9(4) . . ?
C9 N1 C10 109.0(4) . . ?
C10 N1 Dy1 109.3(3) . . ?
C11 N2 Dy1 123.2(3) . . ?
C11 N2 C15 117.2(5) . . ?
C15 N2 Dy1 119.5(4) . . ?
Dy1 C1 Dy1 120.0 2_765 . ?
Dy1 C1 Dy1 120.0 3_675 2_765 ?
Dy1 C1 Dy1 120.0 3_675 . ?
O1 C1 Dy1 60.000(1) 2_765 2_765 ?
O1 C1 Dy1 180.0 2_765 3_675 ?
O1 C1 Dy1 60.000(1) 2_765 . ?
O1 C1 Dy1 180.0 3_675 . ?
O1 C1 Dy1 60.000(4) . 3_675 ?
O1 C1 Dy1 180.0 . 2_765 ?
O1 C1 Dy1 60.000(3) 3_675 3_675 ?
O1 C1 Dy1 60.000(3) 3_675 2_765 ?
O1 C1 Dy1 60.000(4) . . ?
O1 C1 O1 120.000(2) 2_765 3_675 ?
O1 C1 O1 120.000(11) 3_675 . ?
O1 C1 O1 120.000(5) 2_765 . ?
O2 C2 C3 121.0(5) . . ?
O2 C2 C7 121.2(4) . . ?
C7 C2 C3 117.8(5) . . ?
C4 C3 C2 120.3(6) . . ?
C5 C4 C3 121.1(5) . . ?
C4 C5 Cl1 121.5(4) . . ?
C4 C5 C6 120.4(5) . . ?
C6 C5 Cl1 118.1(5) . . ?
C7 C6 C5 119.0(5) . . ?
C2 C7 C8 119.5(4) . . ?
C6 C7 C2 121.4(4) . . ?
C6 C7 C8 119.1(5) . . ?
N1 C8 C7 114.8(4) . . ?
N1 C9 C9 112.1(3) . 4_677 ?
N1 C10 C11 112.1(4) . . ?
N2 C11 C10 115.4(5) . . ?
N2 C11 C12 122.3(5) . . ?
C12 C11 C10 122.1(5) . . ?
C13 C12 C11 118.8(6) . . ?
C14 C13 C12 120.0(5) . . ?
C13 C14 C15 119.1(5) . . ?
N2 C15 C14 122.5(6) . . ?
O3 S1 O3 114.9(3) 3_775 2_755 ?
O3 S1 O3 114.9(3) . 2_755 ?
O3 S1 O3 114.9(3) 3_775 . ?
O3 S1 C16 103.2(4) 3_775 . ?
O3 S1 C16 103.2(4) . . ?
O3 S1 C16 103.2(4) 2_755 . ?
F1 C16 S1 122.4(7) . . ?
F1 C16 S1 122.4(7) 2_755 . ?
F1 C16 S1 122.4(7) 3_775 . ?
F1 C16 F1 94.0(10) . 2_755 ?
F1 C16 F1 94.0(10) . 3_775 ?
F1 C16 F1 94.0(10) 2_755 3_775 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.792 -0.629 0.167 533.6 404.3 '6 CH3CN'
2 -0.124 -0.203 0.833 533.6 404.3 ?
3 -0.070 -0.261 0.500 533.6 404.3 ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.731(14)
2 0.269(14)

