# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
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data_ho3_new_sq
_database_code_depnum_ccdc_archive 'CCDC 1915657'
_audit_update_record             
;
2019-08-22 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H74 Cl2 Ho3 N9 O18'
_chemical_formula_weight         1594.82

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'
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'
Cl Cl 0.1484 0.1585 '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           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 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, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   17.5514(4)
_cell_length_b                   17.5514(4)
_cell_length_c                   13.1932(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3519.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9632
_cell_measurement_theta_min      2.11
_cell_measurement_theta_max      30.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_F_000             1572
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.477
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12975
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.093
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5390
_reflns_number_gt                4588
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  CIFTAB
_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)+(0.0423P)²+4.0302P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5390
_refine_ls_number_parameters     258
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0912
_refine_ls_wR_factor_gt          0.0873
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.005 765 447 '16(C2 H3 N), 6(H2O)'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
 After refinement of the main molecule, residual electron density was tentatively 
 assigned as partially occupied acetonitrile and water molecules. In the final model, 
 these were accounted for using PLATON/SQUEEZE (Spek, 2015). The calculated electron 
 count of 223.5 electrons per formula unit corresponds approximately to 8 x CH3CN and 
 6 x H2O molecules (calc 224 e-).
;


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 0.62209(2) 0.42840(2) 0.33397(2) 0.01480(8) Uani 1 1 d . . . . .
Cl1 Cl 0.666667 0.333333 0.03546(14) 0.0236(4) Uani 1 3 d S T P . .
O1 O 0.6169(2) 0.4545(2) 0.1511(2) 0.0227(7) Uani 1 1 d D . . . .
H1 H 0.634(3) 0.422(3) 0.117(4) 0.034 Uiso 1 1 d D U . . .
O2 O 0.5355(2) 0.28976(19) 0.2725(2) 0.0168(7) Uani 1 1 d . . . . .
O5 O 0.5192(2) 0.3965(2) 0.4665(2) 0.0196(7) Uani 1 1 d D . . . .
H2 H 0.520(4) 0.368(3) 0.522(2) 0.029 Uiso 1 1 d D U . . .
O6 O 0.666667 0.333333 0.4061(4) 0.0138(11) Uani 1 3 d DS T P . .
H6 H 0.666667 0.333333 0.4735(9) 0.021 Uiso 1 3 d DS U P . .
O8 O 0.7030(2) 0.5037(2) 0.4834(2) 0.0192(7) Uani 1 1 d . . . . .
O10 O 0.6523(2) 0.5697(2) 0.3192(2) 0.0203(7) Uani 1 1 d . . . . .
N3 N 0.8038(3) 0.4875(3) 0.6449(3) 0.0200(8) Uani 1 1 d . . . . .
N4 N 0.4725(2) 0.4069(3) 0.2701(3) 0.0183(8) Uani 1 1 d . . . . .
N7 N 0.7975(3) 0.6114(3) 0.5908(3) 0.0233(9) Uani 1 1 d . . . . .
H7 H 0.830745 0.668374 0.600567 0.028 Uiso 1 1 calc R U . . .
C2 C 0.4662(3) 0.2706(3) 0.2035(3) 0.0209(10) Uani 1 1 d . . . . .
H2A H 0.426443 0.206188 0.199152 0.025 Uiso 1 1 calc R U . . .
H2B H 0.490665 0.292619 0.135187 0.025 Uiso 1 1 calc R U . . .
C3 C 0.4344(3) 0.4310(3) 0.3556(3) 0.0228(10) Uani 1 1 d . . . . .
H3A H 0.373493 0.415822 0.338256 0.027 Uiso 1 1 calc R U . . .
H3B H 0.469127 0.495364 0.366496 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4147(3) 0.3147(3) 0.2399(4) 0.0219(10) Uani 1 1 d . . . . .
H4A H 0.375304 0.312440 0.184843 0.026 Uiso 1 1 calc R U . . .
H4B H 0.377564 0.281425 0.298304 0.026 Uiso 1 1 calc R U . . .
C5 C 0.4331(3) 0.3847(3) 0.4521(3) 0.0225(10) Uani 1 1 d . . . . .
H5A H 0.417218 0.409863 0.510038 0.027 Uiso 1 1 calc R U . . .
H5B H 0.389089 0.321298 0.447152 0.027 Uiso 1 1 calc R U . . .
C9 C 0.7892(3) 0.4481(4) 0.8206(4) 0.0284(12) Uani 1 1 d . . . . .
H9 H 0.787673 0.409290 0.871700 0.034 Uiso 1 1 calc R U . . .
C11 C 0.7796(4) 0.5188(4) 0.8448(4) 0.0317(12) Uani 1 1 d . . . . .
H11 H 0.771417 0.529813 0.913337 0.038 Uiso 1 1 calc R U . . .
C13 C 0.8011(3) 0.4346(3) 0.7193(3) 0.0222(10) Uani 1 1 d . . . . .
H13 H 0.807659 0.385537 0.702339 0.027 Uiso 1 1 calc R U . . .
C17 C 0.7688(3) 0.6539(3) 0.4321(4) 0.0255(11) Uani 1 1 d . . . . .
H17 H 0.816172 0.711163 0.446760 0.031 Uiso 1 1 calc R U . . .
C18 C 0.7933(3) 0.5555(3) 0.6694(3) 0.0227(10) Uani 1 1 d . . . . .
C20 C 0.7820(3) 0.5740(4) 0.7684(4) 0.0282(12) Uani 1 1 d . . . . .
H20 H 0.775893 0.623645 0.783615 0.034 Uiso 1 1 calc R U . . .
C23 C 0.5465(3) 0.4600(4) 0.1032(3) 0.0257(11) Uani 1 1 d . . . . .
H23A H 0.509773 0.406245 0.062967 0.031 Uiso 1 1 calc R U . . .
H23B H 0.570533 0.511350 0.057012 0.031 Uiso 1 1 calc R U . . .
C24 C 0.7186(3) 0.6426(3) 0.3474(4) 0.0219(10) Uani 1 1 d . . . . .
C25 C 0.7533(3) 0.5839(3) 0.4987(4) 0.0219(10) Uani 1 1 d . . . . .
C28 C 0.7390(4) 0.7209(3) 0.2802(4) 0.0356(13) Uani 1 1 d . . . . .
H28A H 0.762808 0.714991 0.215383 0.053 Uiso 1 1 calc R U . . .
H28B H 0.782393 0.775267 0.313842 0.053 Uiso 1 1 calc R U . . .
H28C H 0.684971 0.722980 0.268089 0.053 Uiso 1 1 calc R U . . .
C29 C 0.4912(3) 0.4698(3) 0.1857(3) 0.0225(10) Uani 1 1 d . . . . .
H29A H 0.522902 0.530650 0.212529 0.027 Uiso 1 1 calc R U . . .
H29B H 0.435008 0.459591 0.156149 0.027 Uiso 1 1 calc R U . . .
Cl2 Cl 0.8612(7) 0.7930(5) 0.6476(8) 0.095(3) Uani 0.3333 1 d . U P A 1
O3 O 0.8228(13) 0.8347(13) 0.6260(17) 0.093(6) Uani 0.3333 1 d . U P B 2
H3C H 0.878602 0.859705 0.627682 0.140 Uiso 0.3333 1 d R U P B 2
H3D H 0.809472 0.854805 0.677422 0.140 Uiso 0.3333 1 d R U P B 2
O4 O 0.8341(12) 0.8027(14) 0.7001(18) 0.082(6) Uani 0.3333 1 d . U P C 3
H4C H 0.868325 0.821865 0.649253 0.122 Uiso 0.3333 1 d R U P C 3
H4D H 0.861404 0.840146 0.746643 0.122 Uiso 0.3333 1 d R U P C 3


_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 O2 2.230(3) 3_665 ?
Ho1 O10 2.271(3) . ?
Ho1 O2 2.278(3) . ?
Ho1 O6 2.3681(19) . ?
Ho1 O5 2.371(3) . ?
Ho1 O8 2.402(3) . ?
Ho1 O1 2.465(3) . ?
Ho1 N4 2.599(4) . ?
O1 C23 1.435(6) . ?
O1 H1 0.891(10) . ?
O2 C2 1.418(5) . ?
O5 C5 1.432(5) . ?
O5 H2 0.888(10) . ?
O6 H6 0.888(10) . ?
O8 C25 1.249(5) . ?
O10 C24 1.281(6) . ?
N3 C18 1.335(6) . ?
N3 C13 1.336(6) . ?
N4 C4 1.471(6) . ?
N4 C3 1.478(6) . ?
N4 C29 1.485(6) . ?
N7 C25 1.392(6) . ?
N7 C18 1.404(6) . ?
N7 H7 0.8800 . ?
C2 C4 1.531(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C5 1.503(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C9 C11 1.371(8) . ?
C9 C13 1.391(6) . ?
C9 H9 0.9500 . ?
C11 C20 1.384(7) . ?
C11 H11 0.9500 . ?
C13 H13 0.9500 . ?
C17 C24 1.376(7) . ?
C17 C25 1.422(7) . ?
C17 H17 0.9500 . ?
C18 C20 1.385(6) . ?
C20 H20 0.9500 . ?
C23 C29 1.524(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C28 1.520(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
O3 H3C 0.8498 . ?
O3 H3D 0.8499 . ?
O4 H4C 0.8501 . ?
O4 H4D 0.8501 . ?

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
O2 Ho1 O10 90.97(11) 3_665 . ?
O2 Ho1 O2 102.61(15) 3_665 . ?
O10 Ho1 O2 143.39(11) . . ?
O2 Ho1 O6 71.53(10) 3_665 . ?
O10 Ho1 O6 145.62(10) . . ?
O2 Ho1 O6 70.71(10) . . ?
O2 Ho1 O5 153.73(11) 3_665 . ?
O10 Ho1 O5 93.16(11) . . ?
O2 Ho1 O5 89.29(11) . . ?
O6 Ho1 O5 91.03(11) . . ?
O2 Ho1 O8 84.08(11) 3_665 . ?
O10 Ho1 O8 73.68(11) . . ?
O2 Ho1 O8 140.77(11) . . ?
O6 Ho1 O8 75.21(11) . . ?
O5 Ho1 O8 72.29(11) . . ?
O2 Ho1 O1 73.80(11) 3_665 . ?
O10 Ho1 O1 73.95(11) . . ?
O2 Ho1 O1 77.48(11) . . ?
O6 Ho1 O1 125.44(13) . . ?
O5 Ho1 O1 132.16(11) . . ?
O8 Ho1 O1 140.11(11) . . ?
O2 Ho1 N4 139.06(11) 3_665 . ?
O10 Ho1 N4 78.34(12) . . ?
O2 Ho1 N4 69.09(11) . . ?
O6 Ho1 N4 133.91(9) . . ?
O5 Ho1 N4 67.05(11) . . ?
O8 Ho1 N4 128.51(11) . . ?
O1 Ho1 N4 65.26(11) . . ?
C23 O1 Ho1 123.8(3) . . ?
C23 O1 H1 113(4) . . ?
Ho1 O1 H1 109(4) . . ?
C2 O2 Ho1 126.1(3) . 2_655 ?
C2 O2 Ho1 121.1(3) . . ?
Ho1 O2 Ho1 112.83(12) 2_655 . ?
C5 O5 Ho1 124.1(2) . . ?
C5 O5 H2 110(4) . . ?
Ho1 O5 H2 121(3) . . ?
Ho1 O6 Ho1 104.93(12) 3_665 2_655 ?
Ho1 O6 Ho1 104.92(12) 3_665 . ?
Ho1 O6 Ho1 104.92(12) 2_655 . ?
Ho1 O6 H6 113.71(10) 3_665 . ?
Ho1 O6 H6 113.71(10) 2_655 . ?
Ho1 O6 H6 113.71(10) . . ?
C25 O8 Ho1 130.0(3) . . ?
C24 O10 Ho1 131.7(3) . . ?
C18 N3 C13 118.1(4) . . ?
C4 N4 C3 111.1(4) . . ?
C4 N4 C29 112.9(4) . . ?
C3 N4 C29 108.8(4) . . ?
C4 N4 Ho1 109.8(3) . . ?
C3 N4 Ho1 106.3(3) . . ?
C29 N4 Ho1 107.7(3) . . ?
C25 N7 C18 125.3(4) . . ?
C25 N7 H7 117.4 . . ?
C18 N7 H7 117.4 . . ?
O2 C2 C4 109.4(4) . . ?
O2 C2 H2A 109.8 . . ?
C4 C2 H2A 109.8 . . ?
O2 C2 H2B 109.8 . . ?
C4 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N4 C3 C5 112.2(4) . . ?
N4 C3 H3A 109.2 . . ?
C5 C3 H3A 109.2 . . ?
N4 C3 H3B 109.2 . . ?
C5 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N4 C4 C2 112.6(4) . . ?
N4 C4 H4A 109.1 . . ?
C2 C4 H4A 109.1 . . ?
N4 C4 H4B 109.1 . . ?
C2 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
O5 C5 C3 107.8(4) . . ?
O5 C5 H5A 110.2 . . ?
C3 C5 H5A 110.2 . . ?
O5 C5 H5B 110.2 . . ?
C3 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
C11 C9 C13 118.4(5) . . ?
C11 C9 H9 120.8 . . ?
C13 C9 H9 120.8 . . ?
C9 C11 C20 119.3(5) . . ?
C9 C11 H11 120.4 . . ?
C20 C11 H11 120.4 . . ?
N3 C13 C9 122.9(5) . . ?
N3 C13 H13 118.6 . . ?
C9 C13 H13 118.6 . . ?
C24 C17 C25 123.1(5) . . ?
C24 C17 H17 118.5 . . ?
C25 C17 H17 118.5 . . ?
N3 C18 C20 122.7(5) . . ?
N3 C18 N7 117.6(4) . . ?
C20 C18 N7 119.7(4) . . ?
C11 C20 C18 118.7(5) . . ?
C11 C20 H20 120.7 . . ?
C18 C20 H20 120.7 . . ?
O1 C23 C29 108.2(4) . . ?
O1 C23 H23A 110.1 . . ?
C29 C23 H23A 110.1 . . ?
O1 C23 H23B 110.1 . . ?
C29 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
O10 C24 C17 125.2(4) . . ?
O10 C24 C28 114.8(4) . . ?
C17 C24 C28 119.9(5) . . ?
O8 C25 N7 119.3(4) . . ?
O8 C25 C17 126.6(4) . . ?
N7 C25 C17 114.0(4) . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N4 C29 C23 111.6(4) . . ?
N4 C29 H29A 109.3 . . ?
C23 C29 H29A 109.3 . . ?
N4 C29 H29B 109.3 . . ?
C23 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
H3C O3 H3D 104.5 . . ?
H4C O4 H4D 104.5 . . ?

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
_geom_hbond_publ_flag
O1 H1 Cl1 0.891(10) 2.187(11) 3.077(3) 176(5) . yes
O5 H2 N3 0.888(10) 1.834(14) 2.714(5) 171(5) 2_655 yes
N7 H7 Cl2^a 0.88 2.07 2.900(8) 156.8 . yes

_refine_diff_density_max         0.868
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.144



####################################################################### 
# 
# 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_dy6_new
_database_code_depnum_ccdc_archive 'CCDC 1915659'
_audit_update_record             
;
2019-08-22 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H106 Dy6 N12 O44'
_chemical_formula_weight         2458.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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'

_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                   15.6400(9)
_cell_length_b                   15.6400(9)
_cell_length_c                   25.8676(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5479.7(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9812
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      30.10

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.235
_exptl_crystal_F_000             3570
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    6.165
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_T_max  0.540
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5092
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.177
_diffrn_reflns_theta_max         27.500
_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             2797
_reflns_number_gt                2371
_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 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0166P)²+9.3457P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2797
_refine_ls_number_parameters     184
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0552
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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
Dy1 Dy 0.46445(2) 0.07168(2) 0.32793(2) 0.01474(7) Uani 1 1 d . . . . .
O2 O 0.3559(2) -0.0309(2) 0.40292(11) 0.0306(8) Uani 1 1 d . . . . .
O3 O 0.6115(2) 0.1367(2) 0.28809(10) 0.0212(6) Uani 1 1 d . . . . .
O1 O 0.4034(2) 0.1579(2) 0.28513(10) 0.0192(6) Uani 1 1 d . . . . .
O5 O 0.2782(2) -0.0275(2) 0.33574(11) 0.0282(7) Uani 1 1 d . . . . .
N3 N 0.4393(3) 0.0248(3) 0.22776(13) 0.0211(8) Uani 1 1 d . . . . .
O4 O 0.4414(2) -0.0911(2) 0.32006(13) 0.0303(7) Uani 1 1 d D . . . .
H8 H 0.496(2) -0.093(4) 0.3149(19) 0.036 Uiso 1 1 d D U . . .
N5 N 0.2750(3) -0.0516(3) 0.38291(14) 0.0221(8) Uani 1 1 d . . . . .
O6 O 0.1984(2) -0.0894(3) 0.40727(13) 0.0378(9) Uani 1 1 d . . . . .
C8 C 0.4060(3) 0.0901(3) 0.20385(16) 0.0239(10) Uani 1 1 d . . . . .
H8A H 0.464433 0.152708 0.192905 0.029 Uiso 1 1 calc R U . . .
H8B H 0.366164 0.057491 0.172685 0.029 Uiso 1 1 calc R U . . .
C9 C 0.6175(3) 0.1474(4) 0.23253(17) 0.0314(11) Uani 1 1 d . . . . .
H9A H 0.683596 0.161986 0.220558 0.038 Uiso 1 1 calc R U . . .
H9B H 0.607971 0.203038 0.222336 0.038 Uiso 1 1 calc R U . . .
C10 C 0.5382(3) 0.0522(3) 0.20740(16) 0.0261(10) Uani 1 1 d . . . . .
H10A H 0.539234 0.061326 0.169487 0.031 Uiso 1 1 calc R U . . .
H10B H 0.552271 -0.001789 0.214425 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3812(4) -0.1599(4) 0.2359(2) 0.0363(12) Uani 1 1 d . . . . .
H11A H 0.334271 -0.222898 0.218959 0.044 Uiso 1 1 calc R U . . .
H11B H 0.448768 -0.145210 0.226939 0.044 Uiso 1 1 calc R U . . .
C12 C 0.3657(3) -0.0789(3) 0.21396(18) 0.0281(10) Uani 1 1 d . . . . .
H12A H 0.363998 -0.084549 0.175810 0.034 Uiso 1 1 calc R U . . .
H12B H 0.299855 -0.091598 0.225201 0.034 Uiso 1 1 calc R U . . .
C13 C 0.3686(4) -0.1733(3) 0.2924(2) 0.0377(12) Uani 1 1 d . . . . .
H13A H 0.302519 -0.184356 0.301979 0.045 Uiso 1 1 calc R U . . .
H13B H 0.371619 -0.232798 0.302410 0.045 Uiso 1 1 calc R U . . .
C1 C 0.3460(3) 0.1119(3) 0.24059(16) 0.0236(10) Uani 1 1 d . . . . .
H1A H 0.325864 0.156203 0.223990 0.028 Uiso 1 1 calc R U . . .
H1B H 0.285581 0.049993 0.250396 0.028 Uiso 1 1 calc R U . . .
O7 O 0.4498(5) -0.2866(7) 0.4162(3) 0.0484(18) Uani 0.6 1 d G . P A 2
H7A H 0.410649 -0.324227 0.391898 0.073 Uiso 0.6 1 d G U P A 2
H7B H 0.496252 -0.235989 0.399981 0.073 Uiso 0.6 1 d G U P A 2
O8 O 0.4191(14) -0.2449(11) 0.4248(6) 0.049(4) Uani 0.4 1 d G . P B 1
H8C H 0.371063 -0.305653 0.427295 0.073 Uiso 0.4 1 d G U P B 1
H8D H 0.419479 -0.230095 0.392340 0.073 Uiso 0.4 1 d G U P B 1
O9 O 0.3742(19) -0.2463(16) 0.4344(9) 0.063(6) Uani 0.3333 1 d G . P C 3
H9C H 0.389644 -0.187221 0.424207 0.094 Uiso 0.3333 1 d G U P C 3
H9D H 0.378779 -0.241970 0.467887 0.094 Uiso 0.3333 1 d G U P C 3


_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 O3 2.247(3) . ?
Dy1 O3 2.256(3) 17 ?
Dy1 O1 2.274(3) 18_545 ?
Dy1 O1 2.290(3) . ?
Dy1 O4 2.394(3) . ?
Dy1 O5 2.532(3) . ?
Dy1 O2 2.548(3) . ?
Dy1 N3 2.668(3) . ?
O2 N5 1.251(4) . ?
O3 C9 1.444(5) . ?
O1 C1 1.416(5) . ?
O5 N5 1.271(4) . ?
N3 C10 1.480(5) . ?
N3 C12 1.488(6) . ?
N3 C8 1.492(5) . ?
O4 C13 1.414(5) . ?
N5 O6 1.215(4) . ?
C8 C1 1.491(6) . ?
C9 C10 1.527(6) . ?
C11 C13 1.475(7) . ?
C11 C12 1.514(6) . ?

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 Dy1 O3 106.58(15) . 17 ?
O3 Dy1 O1 69.60(10) . 18_545 ?
O3 Dy1 O1 87.27(10) 17 18_545 ?
O3 Dy1 O1 98.40(10) . . ?
O3 Dy1 O1 69.16(10) 17 . ?
O1 Dy1 O1 149.74(13) 18_545 . ?
O3 Dy1 O4 91.02(11) . . ?
O3 Dy1 O4 149.01(11) 17 . ?
O1 Dy1 O4 75.00(11) 18_545 . ?
O1 Dy1 O4 134.36(10) . . ?
O3 Dy1 O5 156.57(10) . . ?
O3 Dy1 O5 90.98(10) 17 . ?
O1 Dy1 O5 127.96(10) 18_545 . ?
O1 Dy1 O5 73.05(10) . . ?
O4 Dy1 O5 80.78(11) . . ?
O3 Dy1 O2 147.43(10) . . ?
O3 Dy1 O2 79.55(11) 17 . ?
O1 Dy1 O2 78.97(10) 18_545 . ?
O1 Dy1 O2 113.34(10) . . ?
O4 Dy1 O2 72.32(11) . . ?
O5 Dy1 O2 49.74(9) . . ?
O3 Dy1 N3 69.87(10) . . ?
O3 Dy1 N3 137.04(11) 17 . ?
O1 Dy1 N3 126.72(10) 18_545 . ?
O1 Dy1 N3 69.18(10) . . ?
O4 Dy1 N3 72.66(11) . . ?
O5 Dy1 N3 86.71(10) . . ?
O2 Dy1 N3 127.29(10) . . ?
N5 O2 Dy1 96.7(2) . . ?
C9 O3 Dy1 120.1(2) . . ?
C9 O3 Dy1 125.1(3) . 18_545 ?
Dy1 O3 Dy1 111.68(11) . 18_545 ?
C1 O1 Dy1 130.7(2) . 17 ?
C1 O1 Dy1 116.1(2) . . ?
Dy1 O1 Dy1 109.48(10) 17 . ?
N5 O5 Dy1 97.0(2) . . ?
C10 N3 C12 110.9(3) . . ?
C10 N3 C8 109.0(3) . . ?
C12 N3 C8 107.6(3) . . ?
C10 N3 Dy1 106.1(2) . . ?
C12 N3 Dy1 117.4(3) . . ?
C8 N3 Dy1 105.6(2) . . ?
C13 O4 Dy1 129.4(3) . . ?
O6 N5 O2 122.4(4) . . ?
O6 N5 O5 121.7(4) . . ?
O2 N5 O5 115.8(3) . . ?
C1 C8 N3 111.6(3) . . ?
O3 C9 C10 109.7(4) . . ?
N3 C10 C9 110.7(4) . . ?
C13 C11 C12 115.1(4) . . ?
N3 C12 C11 117.5(4) . . ?
O4 C13 C11 112.5(4) . . ?
O1 C1 C8 108.8(4) . . ?

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
_geom_hbond_publ_flag
O4 H8 O5 0.885(10) 2.05(2) 2.866(5) 154(5) 18_545 yes

_refine_diff_density_max         1.379
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_Tb3_new_sq
_database_code_depnum_ccdc_archive 'CCDC 1915658'
_audit_update_record             
;
2019-08-22 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H74 Cl2 N9 O18 Tb3'
_chemical_formula_weight         1576.79

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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 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, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   17.5762(6)
_cell_length_b                   17.5762(6)
_cell_length_c                   13.1892(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3528.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9898
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      30.11

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.111
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.339
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18823
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.089
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5398
_reflns_number_gt                5126
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  CIFTAB
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0394P)²+0.2824P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5398
_refine_ls_number_parameters     262
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0916
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.077 756 411 '14(C2 H3 N), 12(H2 O)'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
 After refinement of the main molecule, residual electron density was tentatively 
 assigned as partially occupied acetonitrile and water molecules. In the final model, 
 these were accounted for using PLATON/SQUEEZE (Spek, 2015). The calculated electron 
 count of 205.5 electrons per formula unit corresponds approximately to 7 x CH3CN and 
 6 x H2O molecules (calc 202 e-).
;

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
Tb1 Tb 0.19303(2) -0.37770(2) 0.83479(2) 0.01691(8) Uani 1 1 d . . . . .
Cl1 Cl 0.333333 -0.333333 0.53653(16) 0.0260(5) Uani 1 3 d S T P . .
Cl2 Cl 0.0664(7) -0.1401(9) 1.1477(9) 0.103(4) Uani 0.3333 1 d . . P A 1
O1 O 0.2443(2) -0.4668(3) 0.7733(2) 0.0184(8) Uani 1 1 d . . . . .
O2 O 0.1621(3) -0.3834(3) 0.6499(3) 0.0248(9) Uani 1 1 d D . . . .
H2 H 0.201(3) -0.347(3) 0.607(3) 0.037 Uiso 1 1 d D U . . .
O3 O 0.1207(3) -0.4828(3) 0.9678(3) 0.0220(9) Uani 1 1 d D . . . .
H3 H 0.139(4) -0.476(3) 1.0312(16) 0.033 Uiso 1 1 d D U . . .
O4 O 0.0826(2) -0.3453(3) 0.8201(3) 0.0209(8) Uani 1 1 d . . . . .
O5 O 0.1986(3) -0.2966(3) 0.9844(3) 0.0205(8) Uani 1 1 d . . . . .
O6 O 0.333333 -0.333333 0.9090(5) 0.0172(13) Uani 1 3 d DS T P . .
H6 H 0.333333 -0.333333 0.9849(9) 0.026 Uiso 1 3 d DS U P . .
N1 N 0.0645(3) -0.5277(3) 0.7700(3) 0.0206(10) Uani 1 1 d . . . . .
N2 N 0.1864(3) -0.2004(4) 1.0929(3) 0.0237(11) Uani 1 1 d D . . . .
H2N H 0.147(3) -0.185(4) 1.112(2) 0.036 Uiso 1 1 d D U . . .
N3 N 0.3161(3) -0.1955(3) 1.1452(3) 0.0198(10) Uani 1 1 d . . . . .
C1 C 0.0992(4) -0.5850(4) 0.7385(4) 0.0249(13) Uani 1 1 d . . . . .
H1A H 0.062835 -0.623186 0.682267 0.030 Uiso 1 1 calc R U . . .
H1B H 0.094404 -0.623399 0.795988 0.030 Uiso 1 1 calc R U . . .
C2 C 0.1941(4) -0.5339(4) 0.7044(4) 0.0207(12) Uani 1 1 d . . . . .
H2A H 0.218092 -0.574044 0.698805 0.025 Uiso 1 1 calc R U . . .
H2B H 0.197302 -0.508195 0.636603 0.025 Uiso 1 1 calc R U . . .
C3 C 0.0208(4) -0.5089(4) 0.6847(4) 0.0238(13) Uani 1 1 d . . . . .
H3A H -0.008227 -0.477045 0.711000 0.029 Uiso 1 1 calc R U . . .
H3B H -0.025102 -0.565047 0.655111 0.029 Uiso 1 1 calc R U . . .
C4 C 0.0856(4) -0.4547(4) 0.6034(4) 0.0241(12) Uani 1 1 d D . . . .
H4A H 0.102685 -0.491733 0.563969 0.029 Uiso 1 1 calc R U . . .
H4B H 0.058429 -0.431199 0.556414 0.029 Uiso 1 1 calc R U . . .
C5 C 0.0034(4) -0.5656(4) 0.8544(4) 0.0257(13) Uani 1 1 d . . . . .
H5A H -0.042314 -0.626193 0.836437 0.031 Uiso 1 1 calc R U . . .
H5B H -0.026174 -0.530854 0.865350 0.031 Uiso 1 1 calc R U . . .
C6 C 0.0479(4) -0.5679(4) 0.9530(4) 0.0233(12) Uani 1 1 d D . . . .
H6A H 0.006419 -0.584251 1.010475 0.028 Uiso 1 1 calc R U . . .
H6B H 0.067652 -0.611550 0.948003 0.028 Uiso 1 1 calc R U . . .
C7 C 0.0189(5) -0.2578(5) 0.7810(5) 0.0380(16) Uani 1 1 d . . . . .
H7A H 0.030742 -0.198429 0.797179 0.057 Uiso 1 1 calc R U . . .
H7B H -0.043258 -0.300043 0.793316 0.057 Uiso 1 1 calc R U . . .
H7C H 0.032791 -0.260369 0.709562 0.057 Uiso 1 1 calc R U . . .
C8 C 0.0758(4) -0.2805(4) 0.8480(4) 0.0239(13) Uani 1 1 d . . . . .
C9 C 0.1163(4) -0.2286(4) 0.9335(5) 0.0284(13) Uani 1 1 d . . . . .
H9 H 0.108532 -0.179832 0.946663 0.034 Uiso 1 1 calc R U . . .
C10 C 0.1684(4) -0.2458(4) 1.0010(5) 0.0266(13) Uani 1 1 d D . . . .
C11 C 0.2375(4) -0.2061(4) 1.1690(4) 0.0249(13) Uani 1 1 d D . . . .
C12 C 0.2087(5) -0.2172(5) 1.2696(4) 0.0331(15) Uani 1 1 d . . . . .
H12 H 0.153385 -0.222794 1.285280 0.040 Uiso 1 1 calc R U . . .
C13 C 0.2610(5) -0.2199(4) 1.3463(4) 0.0303(14) Uani 1 1 d . . . . .
H13 H 0.242224 -0.227717 1.414980 0.036 Uiso 1 1 calc R U . . .
C14 C 0.3403(5) -0.2109(4) 1.3206(5) 0.0319(15) Uani 1 1 d . . . . .
H14 H 0.377947 -0.212401 1.371296 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3657(4) -0.1995(4) 1.2182(5) 0.0254(13) Uani 1 1 d . . . . .
H15 H 0.420431 -0.194384 1.200655 0.030 Uiso 1 1 calc R U . . .
O8 O -0.0070(16) -0.1739(15) 1.134(2) 0.092(7) Uani 0.3333 1 d . U P B 2
H8A H -0.002337 -0.160912 1.198579 0.138 Uiso 0.3333 1 d R U P B 2
H8B H -0.046033 -0.160255 1.111905 0.138 Uiso 0.3333 1 d R U P B 2
O9 O 0.0355(19) -0.1671(15) 1.205(2) 0.095(9) Uani 0.3333 1 d . U P C 3
H9A H 0.042233 -0.205087 1.241258 0.142 Uiso 0.3333 1 d R U P C 3
H9B H 0.086639 -0.118605 1.209691 0.142 Uiso 0.3333 1 d R U P C 3


_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
Tb1 O1 2.246(4) 3_655 ?
Tb1 O4 2.288(4) . ?
Tb1 O1 2.310(4) . ?
Tb1 O6 2.392(2) . ?
Tb1 O3 2.399(4) . ?
Tb1 O5 2.408(4) . ?
Tb1 O2 2.490(4) . ?
Tb1 N1 2.613(5) . ?
O1 C2 1.398(6) . ?
O2 C4 1.438(7) . ?
O3 C6 1.413(7) . ?
O4 C8 1.259(7) . ?
O5 C10 1.265(7) . ?
N1 C5 1.457(7) . ?
N1 C1 1.474(7) . ?
N1 C3 1.489(7) . ?
N2 C11 1.383(7) . ?
N2 C10 1.399(7) . ?
N3 C15 1.323(8) . ?
N3 C11 1.334(8) . ?
C1 C2 1.513(8) . ?
C3 C4 1.508(8) . ?
C5 C6 1.529(8) . ?
C7 C8 1.529(8) . ?
C8 C9 1.400(8) . ?
C9 C10 1.413(8) . ?
C11 C12 1.400(8) . ?
C12 C13 1.383(9) . ?
C13 C14 1.366(10) . ?
C14 C15 1.404(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
O1 Tb1 O4 89.80(14) 3_655 . ?
O1 Tb1 O1 103.77(19) 3_655 . ?
O4 Tb1 O1 143.72(13) . . ?
O1 Tb1 O6 72.22(12) 3_655 . ?
O4 Tb1 O6 144.89(12) . . ?
O1 Tb1 O6 71.14(12) . . ?
O1 Tb1 O3 154.15(13) 3_655 . ?
O4 Tb1 O3 93.68(14) . . ?
O1 Tb1 O3 88.33(13) . . ?
O6 Tb1 O3 90.87(14) . . ?
O1 Tb1 O5 83.73(13) 3_655 . ?
O4 Tb1 O5 73.17(14) . . ?
O1 Tb1 O5 140.82(13) . . ?
O6 Tb1 O5 75.03(14) . . ?
O3 Tb1 O5 72.87(13) . . ?
O1 Tb1 O2 73.92(13) 3_655 . ?
O4 Tb1 O2 74.42(14) . . ?
O1 Tb1 O2 77.32(13) . . ?
O6 Tb1 O2 125.64(16) . . ?
O3 Tb1 O2 131.61(13) . . ?
O5 Tb1 O2 140.35(14) . . ?
O1 Tb1 N1 138.94(14) 3_655 . ?
O4 Tb1 N1 79.09(15) . . ?
O1 Tb1 N1 68.53(14) . . ?
O6 Tb1 N1 133.83(11) . . ?
O3 Tb1 N1 66.69(14) . . ?
O5 Tb1 N1 128.63(14) . . ?
O2 Tb1 N1 65.03(14) . . ?
C2 O1 Tb1 127.5(3) . 2_545 ?
C2 O1 Tb1 120.3(3) . . ?
Tb1 O1 Tb1 112.20(15) 2_545 . ?
C4 O2 Tb1 122.9(3) . . ?
C6 O3 Tb1 124.4(3) . . ?
C8 O4 Tb1 132.6(4) . . ?
C10 O5 Tb1 130.7(4) . . ?
Tb1 O6 Tb1 104.42(15) . 3_655 ?
Tb1 O6 Tb1 104.42(15) . 2_545 ?
Tb1 O6 Tb1 104.42(15) 3_655 2_545 ?
C5 N1 C1 111.5(5) . . ?
C5 N1 C3 109.4(5) . . ?
C1 N1 C3 112.0(4) . . ?
C5 N1 Tb1 106.2(3) . . ?
C1 N1 Tb1 109.7(3) . . ?
C3 N1 Tb1 107.7(3) . . ?
C11 N2 C10 123.9(5) . . ?
C15 N3 C11 119.0(5) . . ?
N1 C1 C2 112.8(5) . . ?
O1 C2 C1 110.5(4) . . ?
N1 C3 C4 111.5(5) . . ?
O2 C4 C3 109.2(4) . . ?
N1 C5 C6 113.0(5) . . ?
O3 C6 C5 107.1(5) . . ?
O4 C8 C9 125.2(6) . . ?
O4 C8 C7 116.0(5) . . ?
C9 C8 C7 118.8(6) . . ?
C8 C9 C10 122.8(6) . . ?
O5 C10 N2 119.8(6) . . ?
O5 C10 C9 126.0(6) . . ?
N2 C10 C9 114.3(5) . . ?
N3 C11 N2 119.0(5) . . ?
N3 C11 C12 121.3(6) . . ?
N2 C11 C12 119.7(6) . . ?
C13 C12 C11 119.9(6) . . ?
C14 C13 C12 118.1(5) . . ?
C13 C14 C15 119.2(6) . . ?
N3 C15 C14 122.5(6) . . ?

_refine_diff_density_max         1.077
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.151



####################################################################### 
# 
# 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_new_sq
_database_code_depnum_ccdc_archive 'CCDC 1940155'
_audit_update_record             
;
2019-08-22 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H74 Cl2 Dy3 N9 O18'
_chemical_formula_weight         1587.53

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'
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'
Dy Dy -0.1892 4.4098 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_H-M_alt        'P -3'
_space_group_name_Hall           '-P 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, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   17.5986(3)
_cell_length_b                   17.5986(3)
_cell_length_c                   13.1888(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3537.46(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9753
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      31.12

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_F_000             1566
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    3.272
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'APEX X8'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37039
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.315
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5411
_reflns_number_gt                5125
_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.
 
 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.
;

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_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)+(0.0346P)²+5.7229P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5411
_refine_ls_number_parameters     258
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0693
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.072 779 461 '16(C2 H3 N), 12(H2 O)'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
 After refinement of the main molecule, residual electron density was tentatively 
 assigned as partially occupied acetonitrile and water molecules. In the final model, 
 these were accounted for using PLATON/SQUEEZE (Spek, 2015). The calculated electron 
 count of 230.5 electrons per formula unit corresponds approximately to 8 x CH3CN and 
 6 x H2O molecules (calc 224 e-).
;


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 0.19359(2) -0.37784(2) 0.83434(2) 0.01224(6) Uani 1 1 d . . . . .
Cl1 Cl 0.333333 -0.333333 0.53580(9) 0.0210(3) Uani 1 3 d S T P . .
Cl2 Cl 0.0690(4) -0.1379(5) 1.1486(6) 0.092(2) Uani 0.3333 1 d . . P A 2
O1 O 0.333333 -0.333333 0.9066(3) 0.0114(6) Uani 1 3 d DS T P . .
H1 H 0.333333 -0.333333 0.9731(8) 0.017 Uiso 1 3 d DS U P . .
O2 O 0.16235(15) -0.38359(14) 0.65012(17) 0.0201(4) Uani 1 1 d D . . . .
H2 H 0.2083(18) -0.369(2) 0.612(3) 0.030 Uiso 1 1 d D U . . .
O3 O 0.12147(14) -0.48128(14) 0.96749(16) 0.0175(4) Uani 1 1 d D . . . .
H3 H 0.145(2) -0.486(3) 1.0239(17) 0.026 Uiso 1 1 d D U . . .
O4 O 0.24475(13) -0.46480(13) 0.77306(17) 0.0155(4) Uani 1 1 d . . . . .
O5 O 0.08300(14) -0.34697(14) 0.82037(16) 0.0188(4) Uani 1 1 d . . . . .
O6 O 0.19965(14) -0.29610(14) 0.98372(16) 0.0171(4) Uani 1 1 d . . . . .
N1 N 0.06513(16) -0.52704(16) 0.76968(19) 0.0160(5) Uani 1 1 d . . . . .
N2 N 0.18707(18) -0.20168(18) 1.0921(2) 0.0222(6) Uani 1 1 d . . . . .
H2N H 0.163827 -0.168149 1.102075 0.033 Uiso 1 1 calc R U . . .
N3 N 0.31672(17) -0.19566(16) 1.1444(2) 0.0179(5) Uani 1 1 d . . . . .
C1 C 0.0865(2) -0.4538(2) 0.6031(2) 0.0221(6) Uani 1 1 d . . . . .
H1A H 0.103325 -0.490671 0.562957 0.027 Uiso 1 1 calc R U . . .
H1B H 0.059208 -0.430001 0.556803 0.027 Uiso 1 1 calc R U . . .
C2 C 0.0222(2) -0.5083(2) 0.6854(2) 0.0210(6) Uani 1 1 d . . . . .
H2A H -0.006768 -0.476447 0.711832 0.025 Uiso 1 1 calc R U . . .
H2B H -0.023733 -0.564291 0.655888 0.025 Uiso 1 1 calc R U . . .
C3 C 0.0030(2) -0.5656(2) 0.8553(2) 0.0207(6) Uani 1 1 d . . . . .
H3A H -0.042418 -0.626264 0.837499 0.025 Uiso 1 1 calc R U . . .
H3B H -0.026670 -0.531136 0.866410 0.025 Uiso 1 1 calc R U . . .
C4 C 0.0479(2) -0.5673(2) 0.9525(2) 0.0197(6) Uani 1 1 d . . . . .
H4A H 0.006770 -0.583814 1.010280 0.024 Uiso 1 1 calc R U . . .
H4B H 0.067800 -0.610803 0.947176 0.024 Uiso 1 1 calc R U . . .
C5 C 0.19467(19) -0.5335(2) 0.7042(2) 0.0186(6) Uani 1 1 d . . . . .
H5A H 0.219182 -0.573223 0.699833 0.022 Uiso 1 1 calc R U . . .
H5B H 0.197577 -0.508817 0.635921 0.022 Uiso 1 1 calc R U . . .
C6 C 0.1004(2) -0.5844(2) 0.7388(2) 0.0196(6) Uani 1 1 d . . . . .
H6A H 0.063986 -0.623164 0.683007 0.024 Uiso 1 1 calc R U . . .
H6B H 0.096044 -0.622137 0.796758 0.024 Uiso 1 1 calc R U . . .
C7 C 0.0184(2) -0.2603(3) 0.7827(3) 0.0320(8) Uani 1 1 d . . . . .
H7A H 0.048129 -0.235248 0.718255 0.048 Uiso 1 1 calc R U . . .
H7B H 0.006709 -0.218055 0.817626 0.048 Uiso 1 1 calc R U . . .
H7C H -0.037215 -0.314352 0.769577 0.048 Uiso 1 1 calc R U . . .
C8 C 0.07635(19) -0.2810(2) 0.8487(2) 0.0201(6) Uani 1 1 d . . . . .
C9 C 0.1157(2) -0.2306(2) 0.9330(3) 0.0229(7) Uani 1 1 d . . . . .
H9 H 0.106451 -0.182885 0.947211 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1695(2) -0.24636(19) 0.9999(2) 0.0180(6) Uani 1 1 d . . . . .
C11 C 0.2386(2) -0.2062(2) 1.1693(2) 0.0200(6) Uani 1 1 d . . . . .
C12 C 0.2089(2) -0.2179(2) 1.2696(3) 0.0279(7) Uani 1 1 d . . . . .
H12 H 0.153253 -0.224389 1.285212 0.033 Uiso 1 1 calc R U . . .
C13 C 0.2617(3) -0.2199(2) 1.3452(3) 0.0307(8) Uani 1 1 d . . . . .
H13 H 0.243107 -0.227158 1.413874 0.037 Uiso 1 1 calc R U . . .
C14 C 0.3420(2) -0.2113(2) 1.3205(3) 0.0269(7) Uani 1 1 d . . . . .
H14 H 0.379244 -0.213375 1.371230 0.032 Uiso 1 1 calc R U . . .
C15 C 0.3663(2) -0.1996(2) 1.2193(2) 0.0209(6) Uani 1 1 d . . . . .
H15 H 0.421193 -0.194090 1.201812 0.025 Uiso 1 1 calc R U . . .
O8 O -0.0142(7) -0.1811(8) 1.1261(11) 0.069(3) Uani 0.3333 1 d . U P B 1
H8A H -0.001670 -0.160109 1.189513 0.103 Uiso 0.3333 1 d R U P B 1
H8B H -0.049366 -0.159452 1.109838 0.103 Uiso 0.3333 1 d R U P B 1
O9 O 0.0339(10) -0.1661(9) 1.1971(16) 0.099(6) Uani 0.3333 1 d . U P C 3
H9A H 0.043552 -0.198203 1.241311 0.149 Uiso 0.3333 1 d R U P C 3
H9B H 0.087958 -0.117721 1.209744 0.149 Uiso 0.3333 1 d R U P C 3


_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 O4 2.248(2) 3_655 ?
Dy1 O5 2.275(2) . ?
Dy1 O4 2.277(2) . ?
Dy1 O1 2.3756(14) . ?
Dy1 O3 2.387(2) . ?
Dy1 O6 2.410(2) . ?
Dy1 O2 2.482(2) . ?
Dy1 N1 2.607(2) . ?
O1 H1 0.876(10) . ?
O2 C1 1.430(4) . ?
O2 H2 0.878(10) . ?
O3 C4 1.431(4) . ?
O3 H3 0.876(10) . ?
O4 C5 1.413(3) . ?
O5 C8 1.279(4) . ?
O6 C10 1.248(4) . ?
N1 C2 1.472(4) . ?
N1 C3 1.479(4) . ?
N1 C6 1.483(4) . ?
N2 C11 1.392(4) . ?
N2 C10 1.396(4) . ?
N2 H2N 0.8800 . ?
N3 C11 1.334(4) . ?
N3 C15 1.342(4) . ?
C1 C2 1.514(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.514(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.508(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.518(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.374(5) . ?
C9 C10 1.420(4) . ?
C9 H9 0.9500 . ?
C11 C12 1.399(5) . ?
C12 C13 1.375(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O8 H8A 0.8954 . ?
O8 H8B 0.8994 . ?
O9 H9A 0.8852 . ?
O9 H9B 0.9202 . ?

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
O4 Dy1 O5 90.89(7) 3_655 . ?
O4 Dy1 O4 102.95(10) 3_655 . ?
O5 Dy1 O4 143.60(7) . . ?
O4 Dy1 O1 71.34(7) 3_655 . ?
O5 Dy1 O1 145.29(6) . . ?
O4 Dy1 O1 70.85(7) . . ?
O4 Dy1 O3 153.66(8) 3_655 . ?
O5 Dy1 O3 92.84(8) . . ?
O4 Dy1 O3 89.24(8) . . ?
O1 Dy1 O3 91.39(8) . . ?
O4 Dy1 O6 83.55(8) 3_655 . ?
O5 Dy1 O6 73.23(7) . . ?
O4 Dy1 O6 140.99(7) . . ?
O1 Dy1 O6 75.27(8) . . ?
O3 Dy1 O6 72.65(7) . . ?
O4 Dy1 O2 74.19(7) 3_655 . ?
O5 Dy1 O2 74.45(8) . . ?
O4 Dy1 O2 77.24(8) . . ?
O1 Dy1 O2 125.30(9) . . ?
O3 Dy1 O2 131.81(7) . . ?
O6 Dy1 O2 140.11(7) . . ?
O4 Dy1 N1 139.10(8) 3_655 . ?
O5 Dy1 N1 78.43(8) . . ?
O4 Dy1 N1 69.03(7) . . ?
O1 Dy1 N1 134.17(6) . . ?
O3 Dy1 N1 67.04(7) . . ?
O6 Dy1 N1 128.74(7) . . ?
O2 Dy1 N1 64.90(8) . . ?
Dy1 O1 Dy1 104.98(8) 3_655 2_545 ?
Dy1 O1 Dy1 104.98(8) 3_655 . ?
Dy1 O1 Dy1 104.98(8) 2_545 . ?
Dy1 O1 H1 113.66(7) 3_655 . ?
Dy1 O1 H1 113.66(7) 2_545 . ?
Dy1 O1 H1 113.66(7) . . ?
C1 O2 Dy1 123.51(18) . . ?
C1 O2 H2 109(3) . . ?
Dy1 O2 H2 114(3) . . ?
C4 O3 Dy1 124.04(17) . . ?
C4 O3 H3 104(3) . . ?
Dy1 O3 H3 127(3) . . ?
C5 O4 Dy1 126.12(17) . 2_545 ?
C5 O4 Dy1 121.06(17) . . ?
Dy1 O4 Dy1 112.82(8) 2_545 . ?
C8 O5 Dy1 132.10(19) . . ?
C10 O6 Dy1 130.6(2) . . ?
C2 N1 C3 109.6(2) . . ?
C2 N1 C6 112.5(2) . . ?
C3 N1 C6 111.2(2) . . ?
C2 N1 Dy1 107.75(18) . . ?
C3 N1 Dy1 106.40(17) . . ?
C6 N1 Dy1 109.16(17) . . ?
C11 N2 C10 124.9(3) . . ?
C11 N2 H2N 117.5 . . ?
C10 N2 H2N 117.5 . . ?
C11 N3 C15 117.6(3) . . ?
O2 C1 C2 108.4(2) . . ?
O2 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
O2 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 112.2(2) . . ?
N1 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 C4 112.5(2) . . ?
N1 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
N1 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
O3 C4 C3 107.5(2) . . ?
O3 C4 H4A 110.2 . . ?
C3 C4 H4A 110.2 . . ?
O3 C4 H4B 110.2 . . ?
C3 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
O4 C5 C6 110.1(2) . . ?
O4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
O4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N1 C6 C5 112.9(2) . . ?
N1 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N1 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O5 C8 C9 125.2(3) . . ?
O5 C8 C7 115.3(3) . . ?
C9 C8 C7 119.4(3) . . ?
C8 C9 C10 123.1(3) . . ?
C8 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
O6 C10 N2 119.5(3) . . ?
O6 C10 C9 126.1(3) . . ?
N2 C10 C9 114.3(3) . . ?
N3 C11 N2 117.8(3) . . ?
N3 C11 C12 122.4(3) . . ?
N2 C11 C12 119.7(3) . . ?
C13 C12 C11 118.8(3) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 119.6(3) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C15 117.7(3) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
N3 C15 C14 123.8(3) . . ?
N3 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
H8A O8 H8B 97.4 . . ?
H9A O9 H9B 91.9 . . ?

_refine_diff_density_max         0.941
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.115



