# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_Tb-160K
_database_code_depnum_ccdc_archive 'CCDC 1537481'
_audit_update_record             
;
2017-03-12 deposited with the CCDC.
2017-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H56 N7 O15 Tb'
_chemical_formula_weight         841.67

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   10.5797(14)
_cell_length_b                   11.7633(15)
_cell_length_c                   30.267(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3766.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      3.20
_cell_measurement_theta_max      27.52

_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             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.30
_exptl_absorpt_coefficient_mu    1.947
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52046
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.918
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3700
_reflns_number_gt                3425
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+29.8055P] 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         3700
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.1115
_refine_ls_goodness_of_fit_ref   1.361
_refine_ls_restrained_S_all      1.361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.2500 0.7500 0.65026(2) 0.02617(13) Uani 1 2 d S T P . .
O1 O 0.4732(4) 0.7502(5) 0.62929(14) 0.0396(10) Uani 1 1 d . . . . .
O2 O 0.4161(4) 0.8833(4) 0.67331(16) 0.0381(12) Uani 1 1 d . . . . .
O3 O 0.6083(4) 0.8815(5) 0.64827(18) 0.0491(14) Uani 1 1 d . . . . .
O4 O 0.2559(6) 0.8716(4) 0.58479(15) 0.0471(12) Uani 1 1 d . . . . .
O5 O 0.1717(4) 0.9511(4) 0.64132(15) 0.0344(11) Uani 1 1 d . . . . .
O6 O 0.1931(5) 1.0470(4) 0.58054(18) 0.0494(14) Uani 1 1 d . . . . .
O7 O 0.3176(4) 0.6814(4) 0.72158(15) 0.0364(11) Uani 1 1 d . . . . .
O8 O 0.2500 0.7500 0.7838(2) 0.074(3) Uani 1 2 d S T P . .
N1 N 0.5031(5) 0.8400(5) 0.65004(18) 0.0316(12) Uani 1 1 d . . . . .
N2 N 0.2067(5) 0.9591(5) 0.60148(19) 0.0308(12) Uani 1 1 d . . . . .
N3 N 0.2500 0.7500 0.7440(2) 0.0381(19) Uani 1 2 d S T P . .
N4 N 0.2500 0.2500 0.7175(2) 0.0273(15) Uani 1 2 d S T P . .
N5 N 0.7500 0.7500 0.5290(2) 0.0263(14) Uani 1 2 d S T P . .
C1 C 0.2395(7) 0.3571(5) 0.7454(2) 0.0292(13) Uani 1 1 d . . . . .
H1A H 0.3192 0.3660 0.7622 0.035 Uiso 1 1 calc R U . . .
H1B H 0.2326 0.4230 0.7252 0.035 Uiso 1 1 calc R U . . .
C2 C 0.1314(7) 0.3622(6) 0.7774(2) 0.0383(17) Uani 1 1 d . . . . .
H2A H 0.1469 0.3088 0.8021 0.046 Uiso 1 1 calc R U . . .
H2B H 0.0523 0.3391 0.7624 0.046 Uiso 1 1 calc R U . . .
C3 C 0.1175(8) 0.4820(7) 0.7953(3) 0.049(2) Uani 1 1 d . . . . .
H3A H 0.0468 0.4846 0.8162 0.073 Uiso 1 1 calc R U . . .
H3B H 0.1956 0.5043 0.8104 0.073 Uiso 1 1 calc R U . . .
H3C H 0.1012 0.5345 0.7708 0.073 Uiso 1 1 calc R U . . .
C4 C 0.3676(6) 0.2676(4) 0.6889(2) 0.0267(14) Uani 1 1 d . . . . .
H4A H 0.3542 0.3350 0.6699 0.032 Uiso 1 1 calc R U . . .
H4B H 0.4403 0.2841 0.7085 0.032 Uiso 1 1 calc R U . . .
C5 C 0.4013(8) 0.1665(6) 0.6597(3) 0.053(2) Uani 1 1 d . . . . .
H5A H 0.4147 0.0982 0.6782 0.063 Uiso 1 1 calc R U . . .
H5B H 0.3308 0.1507 0.6391 0.063 Uiso 1 1 calc R U . . .
C6 C 0.5201(9) 0.1920(7) 0.6338(3) 0.059(2) Uani 1 1 d . . . . .
H6A H 0.5411 0.1267 0.6150 0.088 Uiso 1 1 calc R U . . .
H6B H 0.5062 0.2591 0.6152 0.088 Uiso 1 1 calc R U . . .
H6C H 0.5899 0.2067 0.6542 0.088 Uiso 1 1 calc R U . . .
C7 C 0.6427(6) 0.7861(5) 0.49923(19) 0.0254(13) Uani 1 1 d . . . . .
H7A H 0.6242 0.7229 0.4786 0.031 Uiso 1 1 calc R U . . .
H7B H 0.6715 0.8516 0.4813 0.031 Uiso 1 1 calc R U . . .
C8 C 0.5205(6) 0.8191(6) 0.5224(2) 0.0326(15) Uani 1 1 d . . . . .
H8A H 0.4899 0.7542 0.5403 0.039 Uiso 1 1 calc R U . . .
H8B H 0.5367 0.8836 0.5426 0.039 Uiso 1 1 calc R U . . .
C9 C 0.4200(7) 0.8524(6) 0.4891(2) 0.0395(17) Uani 1 1 d . . . . .
H9A H 0.3422 0.8733 0.5047 0.059 Uiso 1 1 calc R U . . .
H9B H 0.4498 0.9173 0.4717 0.059 Uiso 1 1 calc R U . . .
H9C H 0.4031 0.7881 0.4694 0.059 Uiso 1 1 calc R U . . .
C10 C 0.7910(6) 0.8466(5) 0.55930(19) 0.0263(14) Uani 1 1 d . . . . .
H10A H 0.7155 0.8744 0.5753 0.032 Uiso 1 1 calc R U . . .
H10B H 0.8500 0.8152 0.5816 0.032 Uiso 1 1 calc R U . . .
C11 C 0.8538(7) 0.9466(6) 0.5375(2) 0.0360(16) Uani 1 1 d . . . . .
H11A H 0.8004 0.9750 0.5130 0.043 Uiso 1 1 calc R U . . .
H11B H 0.9365 0.9234 0.5251 0.043 Uiso 1 1 calc R U . . .
C12 C 0.8725(8) 1.0391(7) 0.5714(3) 0.051(2) Uani 1 1 d . . . . .
H12A H 0.9134 1.1047 0.5575 0.077 Uiso 1 1 calc R U . . .
H12B H 0.7903 1.0620 0.5833 0.077 Uiso 1 1 calc R U . . .
H12C H 0.9260 1.0105 0.5954 0.077 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
Tb1 O7 2.413(4) . ?
Tb1 O7 2.413(4) 2_565 ?
Tb1 O1 2.445(4) 2_565 ?
Tb1 O1 2.445(4) . ?
Tb1 O4 2.445(4) 2_565 ?
Tb1 O4 2.445(4) . ?
Tb1 O2 2.456(5) . ?
Tb1 O2 2.456(5) 2_565 ?
Tb1 O5 2.521(4) . ?
Tb1 O5 2.521(4) 2_565 ?
Tb1 N3 2.836(7) . ?
Tb1 N1 2.879(5) . ?
O1 N1 1.269(8) . ?
O2 N1 1.266(7) . ?
O3 N1 1.217(7) . ?
O4 N2 1.259(7) . ?
O5 N2 1.265(7) . ?
O6 N2 1.221(7) . ?
O7 N3 1.274(6) . ?
O8 N3 1.207(10) . ?
N3 O7 1.274(6) 2_565 ?
N4 C1 1.520(7) . ?
N4 C1 1.520(7) 2 ?
N4 C4 1.529(7) 2 ?
N4 C4 1.529(7) . ?
N5 C7 1.510(7) 2_665 ?
N5 C7 1.510(7) . ?
N5 C10 1.522(7) . ?
N5 C10 1.522(7) 2_665 ?
C1 C2 1.501(9) . ?
C2 C3 1.516(10) . ?
C4 C5 1.525(9) . ?
C5 C6 1.511(11) . ?
C7 C8 1.522(8) . ?
C8 C9 1.518(9) . ?
C10 C11 1.504(9) . ?
C11 C12 1.509(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
O7 Tb1 O7 53.1(2) . 2_565 ?
O7 Tb1 O1 121.22(15) . 2_565 ?
O7 Tb1 O1 86.91(16) 2_565 2_565 ?
O7 Tb1 O1 86.91(16) . . ?
O7 Tb1 O1 121.22(15) 2_565 . ?
O1 Tb1 O1 149.9(2) 2_565 . ?
O7 Tb1 O4 122.47(16) . 2_565 ?
O7 Tb1 O4 155.94(19) 2_565 2_565 ?
O1 Tb1 O4 76.38(19) 2_565 2_565 ?
O1 Tb1 O4 79.32(19) . 2_565 ?
O7 Tb1 O4 155.94(19) . . ?
O7 Tb1 O4 122.48(16) 2_565 . ?
O1 Tb1 O4 79.32(19) 2_565 . ?
O1 Tb1 O4 76.38(19) . . ?
O4 Tb1 O4 71.7(2) 2_565 . ?
O7 Tb1 O2 75.35(17) . . ?
O7 Tb1 O2 75.20(16) 2_565 . ?
O1 Tb1 O2 139.92(18) 2_565 . ?
O1 Tb1 O2 51.85(16) . . ?
O4 Tb1 O2 128.46(19) 2_565 . ?
O4 Tb1 O2 80.70(19) . . ?
O7 Tb1 O2 75.20(16) . 2_565 ?
O7 Tb1 O2 75.35(17) 2_565 2_565 ?
O1 Tb1 O2 51.85(16) 2_565 2_565 ?
O1 Tb1 O2 139.92(18) . 2_565 ?
O4 Tb1 O2 80.70(19) 2_565 2_565 ?
O4 Tb1 O2 128.46(19) . 2_565 ?
O2 Tb1 O2 147.0(2) . 2_565 ?
O7 Tb1 O5 120.47(16) . . ?
O7 Tb1 O5 71.63(15) 2_565 . ?
O1 Tb1 O5 69.87(18) 2_565 . ?
O1 Tb1 O5 106.76(18) . . ?
O4 Tb1 O5 116.99(15) 2_565 . ?
O4 Tb1 O5 51.11(15) . . ?
O2 Tb1 O5 70.51(16) . . ?
O2 Tb1 O5 113.24(15) 2_565 . ?
O7 Tb1 O5 71.63(15) . 2_565 ?
O7 Tb1 O5 120.47(16) 2_565 2_565 ?
O1 Tb1 O5 106.77(18) 2_565 2_565 ?
O1 Tb1 O5 69.87(18) . 2_565 ?
O4 Tb1 O5 51.11(15) 2_565 2_565 ?
O4 Tb1 O5 117.00(15) . 2_565 ?
O2 Tb1 O5 113.24(15) . 2_565 ?
O2 Tb1 O5 70.51(16) 2_565 2_565 ?
O5 Tb1 O5 167.7(2) . 2_565 ?
O7 Tb1 N3 26.54(12) . . ?
O7 Tb1 N3 26.54(12) 2_565 . ?
O1 Tb1 N3 105.04(10) 2_565 . ?
O1 Tb1 N3 105.05(10) . . ?
O4 Tb1 N3 144.14(12) 2_565 . ?
O4 Tb1 N3 144.14(12) . . ?
O2 Tb1 N3 73.50(12) . . ?
O2 Tb1 N3 73.50(12) 2_565 . ?
O5 Tb1 N3 96.16(10) . . ?
O5 Tb1 N3 96.16(10) 2_565 . ?
O7 Tb1 N1 81.33(15) . . ?
O7 Tb1 N1 98.91(16) 2_565 . ?
O1 Tb1 N1 153.86(16) 2_565 . ?
O1 Tb1 N1 25.98(16) . . ?
O4 Tb1 N1 103.71(19) 2_565 . ?
O4 Tb1 N1 76.06(18) . . ?
O2 Tb1 N1 25.92(15) . . ?
O2 Tb1 N1 154.25(15) 2_565 . ?
O5 Tb1 N1 87.70(16) . . ?
O5 Tb1 N1 92.27(16) 2_565 . ?
N3 Tb1 N1 90.14(11) . . ?
N1 O1 Tb1 96.5(3) . . ?
N1 O2 Tb1 96.1(4) . . ?
N2 O4 Tb1 98.2(3) . . ?
N2 O5 Tb1 94.3(3) . . ?
N3 O7 Tb1 95.6(4) . . ?
O3 N1 O2 122.0(6) . . ?
O3 N1 O1 122.7(6) . . ?
O2 N1 O1 115.4(5) . . ?
O3 N1 Tb1 176.9(4) . . ?
O2 N1 Tb1 58.0(3) . . ?
O1 N1 Tb1 57.5(3) . . ?
O6 N2 O4 122.2(6) . . ?
O6 N2 O5 121.5(6) . . ?
O4 N2 O5 116.3(5) . . ?
O6 N2 Tb1 177.7(5) . . ?
O4 N2 Tb1 56.4(3) . . ?
O5 N2 Tb1 59.9(3) . . ?
O8 N3 O7 122.2(3) . 2_565 ?
O8 N3 O7 122.2(3) . . ?
O7 N3 O7 115.7(7) 2_565 . ?
O8 N3 Tb1 180.0 . . ?
O7 N3 Tb1 57.8(3) 2_565 . ?
O7 N3 Tb1 57.8(3) . . ?
C1 N4 C1 112.5(6) . 2 ?
C1 N4 C4 111.5(3) . 2 ?
C1 N4 C4 105.1(3) 2 2 ?
C1 N4 C4 105.1(3) . . ?
C1 N4 C4 111.5(3) 2 . ?
C4 N4 C4 111.2(6) 2 . ?
C7 N5 C7 106.7(6) 2_665 . ?
C7 N5 C10 110.8(3) 2_665 . ?
C7 N5 C10 111.3(3) . . ?
C7 N5 C10 111.3(3) 2_665 2_665 ?
C7 N5 C10 110.8(3) . 2_665 ?
C10 N5 C10 106.0(6) . 2_665 ?
C2 C1 N4 116.6(5) . . ?
C1 C2 C3 110.0(6) . . ?
C5 C4 N4 114.4(5) . . ?
C6 C5 C4 109.9(6) . . ?
N5 C7 C8 115.7(5) . . ?
C9 C8 C7 110.8(5) . . ?
C11 C10 N5 116.4(5) . . ?
C10 C11 C12 108.9(6) . . ?

_refine_diff_density_max         0.606
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.094

####################################################################### 
# 
# 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_Dy-100K
_database_code_depnum_ccdc_archive 'CCDC 1537482'
_audit_update_record             
;
2017-03-12 deposited with the CCDC.
2017-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H56 Dy N7 O15'
_chemical_formula_weight         845.25

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   10.5239(8)
_cell_length_b                   11.7488(9)
_cell_length_c                   30.109(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3722.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9646
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      30.16

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             1740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    2.078
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54797
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.930
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3660
_reflns_number_gt                3335
_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+25.0105P] 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         3660
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_restrained_S_all      1.256
_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 0.7500 0.7500 0.65081(2) 0.01716(9) Uani 1 2 d S T P . .
O1 O 0.9735(3) 0.7488(4) 0.62964(10) 0.0254(7) Uani 1 1 d . . . . .
O2 O 0.9156(3) 0.8832(3) 0.67388(12) 0.0237(8) Uani 1 1 d . . . . .
O3 O 1.1093(3) 0.8809(3) 0.64841(13) 0.0316(9) Uani 1 1 d . . . . .
O4 O 0.7582(4) 0.8709(3) 0.58552(11) 0.0298(8) Uani 1 1 d . . . . .
O5 O 0.6712(3) 0.9512(3) 0.64219(11) 0.0218(7) Uani 1 1 d . . . . .
O6 O 0.6937(4) 1.0467(3) 0.58078(13) 0.0327(9) Uani 1 1 d . . . . .
O7 O 0.8182(3) 0.6814(3) 0.72203(11) 0.0243(8) Uani 1 1 d . . . . .
O8 O 0.7500 0.7500 0.78493(16) 0.0503(17) Uani 1 2 d S T P . .
N1 N 1.0034(4) 0.8393(3) 0.65030(13) 0.0207(9) Uani 1 1 d . . . . .
N2 N 0.7072(4) 0.9590(3) 0.60217(14) 0.0211(9) Uani 1 1 d . . . . .
N3 N 0.7500 0.7500 0.74478(18) 0.0263(13) Uani 1 2 d S T P . .
N4 N 0.7500 0.2500 0.71765(17) 0.0182(11) Uani 1 2 d S T P . .
N5 N 1.2500 0.7500 0.52893(17) 0.0199(11) Uani 1 2 d S T P . .
C1 C 0.7411(5) 0.3574(4) 0.74581(14) 0.0195(9) Uani 1 1 d . . . . .
H1A H 0.8214 0.3655 0.7626 0.023 Uiso 1 1 calc R U . . .
H1B H 0.7346 0.4236 0.7256 0.023 Uiso 1 1 calc R U . . .
C2 C 0.6323(5) 0.3628(4) 0.77826(17) 0.0257(11) Uani 1 1 d . . . . .
H2A H 0.6486 0.3106 0.8034 0.031 Uiso 1 1 calc R U . . .
H2B H 0.5528 0.3387 0.7634 0.031 Uiso 1 1 calc R U . . .
C3 C 0.6182(5) 0.4839(5) 0.79535(19) 0.0321(13) Uani 1 1 d . . . . .
H3A H 0.5474 0.4875 0.8165 0.048 Uiso 1 1 calc R U . . .
H3B H 0.6968 0.5072 0.8102 0.048 Uiso 1 1 calc R U . . .
H3C H 0.6013 0.5352 0.7704 0.048 Uiso 1 1 calc R U . . .
C4 C 0.8686(5) 0.2653(4) 0.68892(16) 0.0204(10) Uani 1 1 d . . . . .
H4A H 0.8559 0.3325 0.6695 0.025 Uiso 1 1 calc R U . . .
H4B H 0.9415 0.2820 0.7086 0.025 Uiso 1 1 calc R U . . .
C5 C 0.9026(6) 0.1644(5) 0.6600(2) 0.0371(15) Uani 1 1 d . . . . .
H5A H 0.9176 0.0968 0.6789 0.045 Uiso 1 1 calc R U . . .
H5B H 0.8311 0.1471 0.6397 0.045 Uiso 1 1 calc R U . . .
C6 C 1.0202(6) 0.1896(5) 0.63317(19) 0.0387(15) Uani 1 1 d . . . . .
H6A H 1.0411 0.1237 0.6146 0.058 Uiso 1 1 calc R U . . .
H6B H 1.0048 0.2559 0.6142 0.058 Uiso 1 1 calc R U . . .
H6C H 1.0912 0.2057 0.6533 0.058 Uiso 1 1 calc R U . . .
C7 C 1.1417(4) 0.7863(4) 0.49884(15) 0.0176(10) Uani 1 1 d . . . . .
H7A H 1.1230 0.7233 0.4780 0.021 Uiso 1 1 calc R U . . .
H7B H 1.1703 0.8522 0.4809 0.021 Uiso 1 1 calc R U . . .
C8 C 1.0194(5) 0.8188(4) 0.52267(16) 0.0238(11) Uani 1 1 d . . . . .
H8A H 1.0359 0.8828 0.5433 0.029 Uiso 1 1 calc R U . . .
H8B H 0.9884 0.7533 0.5403 0.029 Uiso 1 1 calc R U . . .
C9 C 0.9188(5) 0.8536(5) 0.48892(17) 0.0285(12) Uani 1 1 d . . . . .
H9A H 0.8404 0.8743 0.5045 0.043 Uiso 1 1 calc R U . . .
H9B H 0.9494 0.9189 0.4718 0.043 Uiso 1 1 calc R U . . .
H9C H 0.9019 0.7898 0.4688 0.043 Uiso 1 1 calc R U . . .
C10 C 1.2921(5) 0.8464(4) 0.55937(15) 0.0201(10) Uani 1 1 d . . . . .
H10A H 1.2165 0.8748 0.5755 0.024 Uiso 1 1 calc R U . . .
H10B H 1.3513 0.8147 0.5817 0.024 Uiso 1 1 calc R U . . .
C11 C 1.3560(5) 0.9462(4) 0.53716(17) 0.0254(11) Uani 1 1 d . . . . .
H11A H 1.3026 0.9743 0.5124 0.030 Uiso 1 1 calc R U . . .
H11B H 1.4391 0.9224 0.5249 0.030 Uiso 1 1 calc R U . . .
C12 C 1.3750(6) 1.0400(5) 0.57113(19) 0.0356(14) Uani 1 1 d . . . . .
H12A H 1.4165 1.1052 0.5570 0.053 Uiso 1 1 calc R U . . .
H12B H 1.2923 1.0635 0.5830 0.053 Uiso 1 1 calc R U . . .
H12C H 1.4284 1.0118 0.5954 0.053 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
Dy1 O7 2.400(3) 2_665 ?
Dy1 O7 2.400(3) . ?
Dy1 O4 2.427(3) 2_665 ?
Dy1 O4 2.427(3) . ?
Dy1 O1 2.437(3) . ?
Dy1 O1 2.437(3) 2_665 ?
Dy1 O2 2.443(3) . ?
Dy1 O2 2.443(3) 2_665 ?
Dy1 O5 2.519(3) 2_665 ?
Dy1 O5 2.519(3) . ?
Dy1 N3 2.829(5) . ?
Dy1 N1 2.865(4) 2_665 ?
O1 N1 1.272(6) . ?
O2 N1 1.274(5) . ?
O3 N1 1.219(5) . ?
O4 N2 1.270(5) . ?
O5 N2 1.266(5) . ?
O6 N2 1.223(5) . ?
O7 N3 1.278(4) . ?
O8 N3 1.209(7) . ?
N3 O7 1.278(4) 2_665 ?
N4 C1 1.523(5) 2_655 ?
N4 C1 1.523(5) . ?
N4 C4 1.529(5) . ?
N4 C4 1.529(5) 2_655 ?
N5 C7 1.517(5) . ?
N5 C7 1.517(5) 2_765 ?
N5 C10 1.523(5) . ?
N5 C10 1.523(5) 2_765 ?
C1 C2 1.507(7) . ?
C2 C3 1.520(7) . ?
C4 C5 1.515(7) . ?
C5 C6 1.507(8) . ?
C7 C8 1.523(6) . ?
C8 C9 1.523(7) . ?
C10 C11 1.508(7) . ?
C11 C12 1.517(7) . ?

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
O7 Dy1 O7 53.44(17) 2_665 . ?
O7 Dy1 O4 155.44(13) 2_665 2_665 ?
O7 Dy1 O4 122.52(12) . 2_665 ?
O7 Dy1 O4 122.52(12) 2_665 . ?
O7 Dy1 O4 155.44(13) . . ?
O4 Dy1 O4 71.80(17) 2_665 . ?
O7 Dy1 O1 121.62(11) 2_665 . ?
O7 Dy1 O1 86.75(11) . . ?
O4 Dy1 O1 79.56(13) 2_665 . ?
O4 Dy1 O1 75.95(13) . . ?
O7 Dy1 O1 86.75(11) 2_665 2_665 ?
O7 Dy1 O1 121.61(11) . 2_665 ?
O4 Dy1 O1 75.95(13) 2_665 2_665 ?
O4 Dy1 O1 79.56(13) . 2_665 ?
O1 Dy1 O1 149.66(15) . 2_665 ?
O7 Dy1 O2 75.18(12) 2_665 . ?
O7 Dy1 O2 75.40(12) . . ?
O4 Dy1 O2 129.08(13) 2_665 . ?
O4 Dy1 O2 80.22(13) . . ?
O1 Dy1 O2 52.38(12) . . ?
O1 Dy1 O2 139.39(13) 2_665 . ?
O7 Dy1 O2 75.40(12) 2_665 2_665 ?
O7 Dy1 O2 75.18(12) . 2_665 ?
O4 Dy1 O2 80.22(13) 2_665 2_665 ?
O4 Dy1 O2 129.08(13) . 2_665 ?
O1 Dy1 O2 139.39(13) . 2_665 ?
O1 Dy1 O2 52.38(12) 2_665 2_665 ?
O2 Dy1 O2 146.97(16) . 2_665 ?
O7 Dy1 O5 120.39(11) 2_665 2_665 ?
O7 Dy1 O5 71.24(11) . 2_665 ?
O4 Dy1 O5 51.60(11) 2_665 2_665 ?
O4 Dy1 O5 117.01(11) . 2_665 ?
O1 Dy1 O5 69.49(13) . 2_665 ?
O1 Dy1 O5 107.24(13) 2_665 2_665 ?
O2 Dy1 O5 113.29(11) . 2_665 ?
O2 Dy1 O5 70.32(11) 2_665 2_665 ?
O7 Dy1 O5 71.24(11) 2_665 . ?
O7 Dy1 O5 120.38(11) . . ?
O4 Dy1 O5 117.01(11) 2_665 . ?
O4 Dy1 O5 51.60(11) . . ?
O1 Dy1 O5 107.24(13) . . ?
O1 Dy1 O5 69.49(13) 2_665 . ?
O2 Dy1 O5 70.32(11) . . ?
O2 Dy1 O5 113.29(11) 2_665 . ?
O5 Dy1 O5 168.16(15) 2_665 . ?
O7 Dy1 N3 26.72(8) 2_665 . ?
O7 Dy1 N3 26.72(8) . . ?
O4 Dy1 N3 144.10(8) 2_665 . ?
O4 Dy1 N3 144.10(8) . . ?
O1 Dy1 N3 105.17(7) . . ?
O1 Dy1 N3 105.17(7) 2_665 . ?
O2 Dy1 N3 73.49(8) . . ?
O2 Dy1 N3 73.48(8) 2_665 . ?
O5 Dy1 N3 95.92(7) 2_665 . ?
O5 Dy1 N3 95.92(7) . . ?
O7 Dy1 N1 81.35(11) 2_665 2_665 ?
O7 Dy1 N1 99.21(12) . 2_665 ?
O4 Dy1 N1 75.43(13) 2_665 2_665 ?
O4 Dy1 N1 104.05(13) . 2_665 ?
O1 Dy1 N1 153.45(12) . 2_665 ?
O1 Dy1 N1 26.18(12) 2_665 2_665 ?
O2 Dy1 N1 154.15(11) . 2_665 ?
O2 Dy1 N1 26.26(11) 2_665 2_665 ?
O5 Dy1 N1 87.84(11) 2_665 2_665 ?
O5 Dy1 N1 92.09(11) . 2_665 ?
N3 Dy1 N1 90.31(8) . 2_665 ?
N1 O1 Dy1 96.1(3) . . ?
N1 O2 Dy1 95.7(3) . . ?
N2 O4 Dy1 98.2(2) . . ?
N2 O5 Dy1 93.9(3) . . ?
N3 O7 Dy1 95.7(3) . . ?
O3 N1 O1 122.7(4) . . ?
O3 N1 O2 121.8(4) . . ?
O1 N1 O2 115.6(4) . . ?
O3 N1 Dy1 176.8(3) . . ?
O1 N1 Dy1 57.7(2) . . ?
O2 N1 Dy1 58.0(2) . . ?
O6 N2 O5 121.8(4) . . ?
O6 N2 O4 121.9(4) . . ?
O5 N2 O4 116.3(4) . . ?
O6 N2 Dy1 177.4(3) . . ?
O5 N2 Dy1 60.2(2) . . ?
O4 N2 Dy1 56.1(2) . . ?
O8 N3 O7 122.4(3) . . ?
O8 N3 O7 122.4(3) . 2_665 ?
O7 N3 O7 115.2(5) . 2_665 ?
O8 N3 Dy1 180.0 . . ?
O7 N3 Dy1 57.6(3) . . ?
O7 N3 Dy1 57.6(3) 2_665 . ?
C1 N4 C1 112.4(5) 2_655 . ?
C1 N4 C4 111.2(3) 2_655 . ?
C1 N4 C4 105.5(3) . . ?
C1 N4 C4 105.5(3) 2_655 2_655 ?
C1 N4 C4 111.3(3) . 2_655 ?
C4 N4 C4 111.1(5) . 2_655 ?
C7 N5 C7 106.7(5) . 2_765 ?
C7 N5 C10 111.6(3) . . ?
C7 N5 C10 110.5(3) 2_765 . ?
C7 N5 C10 110.5(3) . 2_765 ?
C7 N5 C10 111.6(3) 2_765 2_765 ?
C10 N5 C10 106.0(5) . 2_765 ?
C2 C1 N4 116.3(4) . . ?
C1 C2 C3 109.5(4) . . ?
C5 C4 N4 115.2(4) . . ?
C6 C5 C4 110.4(5) . . ?
N5 C7 C8 115.1(4) . . ?
C7 C8 C9 109.9(4) . . ?
C11 C10 N5 116.2(4) . . ?
C10 C11 C12 109.0(4) . . ?

_refine_diff_density_max         0.488
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.086

