# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_xb9262_0m
_database_code_depnum_ccdc_archive 'CCDC 1469449'
_audit_update_record             
;
2017-08-04 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H36 Dy2 N10 O12'
_chemical_formula_sum            'C32 H36 Dy2 N10 O12'
_chemical_formula_weight         1077.71

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   11.392(2)
_cell_length_b                   14.396(2)
_cell_length_c                   11.488(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.493(3)
_cell_angle_gamma                90
_cell_volume                     1839.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1432
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      20.96

_exptl_crystal_description       needle-like
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.946
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    4.107
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6156
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
'SADABS 2015/2 (Bruker,2015) was used for absorption correction. R(int) was 0.0777 before and 0.0560 after correction. The Ratio of minimum to maximum transmission is 0.8260. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9355
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.283
_diffrn_reflns_theta_max         25.497
_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             3418
_reflns_number_gt                2904
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0786P)²+13.3401P] 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         3418
_refine_ls_number_parameters     255
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.1806
_refine_ls_wR_factor_gt          0.1724
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.159
_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
O4 O 0.4826(8) 0.5833(6) 0.5529(7) 0.034(2) Uani 1 1 d . . . . .
Dy1 Dy 0.53797(5) 0.42244(4) 0.65467(5) 0.0252(2) Uani 1 1 d . . . . .
C1 C 0.4915(18) 0.7242(13) 0.6621(17) 0.077(6) Uani 1 1 d . . . . .
H1A H 0.5131 0.7539 0.5949 0.115 Uiso 1 1 calc R U . . .
H1B H 0.5436 0.7456 0.7343 0.115 Uiso 1 1 calc R U . . .
H1C H 0.4097 0.7392 0.6636 0.115 Uiso 1 1 calc R U . . .
N4 N 0.3877(13) 0.3763(9) 0.9944(9) 0.049(3) Uani 1 1 d . . . . .
H4A H 0.3240 0.4135 0.9758 0.073 Uiso 1 1 d R U . . .
H4B H 0.4297 0.3903 1.0669 0.073 Uiso 1 1 d R U . . .
O1 O 0.3338(8) 0.4093(7) 0.5796(8) 0.038(2) Uani 1 1 d . . . . .
O2 O 0.5265(9) 0.5752(6) 0.7464(8) 0.038(2) Uani 1 1 d . . . . .
C6 C 0.5039(12) 0.6221(9) 0.6522(11) 0.031(3) Uani 1 1 d . . . . .
O7 O 0.5155(9) 0.2544(7) 0.6570(10) 0.051(3) Uani 1 1 d . . . . .
N5 N -0.0773(12) 0.4076(9) 0.5983(15) 0.054(4) Uani 1 1 d . . . . .
O5 O 0.7183(8) 0.4965(6) 0.6310(8) 0.034(2) Uani 1 1 d . . . . .
H5A H 0.7009 0.5366 0.5627 0.051 Uiso 1 1 d R U . . .
H5B H 0.7753 0.4501 0.6196 0.051 Uiso 1 1 d R U . . .
N1 N 0.4171(10) 0.3956(8) 0.8012(10) 0.036(3) Uani 1 1 d . . . . .
N2 N 0.6511(10) 0.4046(8) 0.8659(10) 0.036(3) Uani 1 1 d . . . . .
C12 C 0.6519(16) 0.3865(13) 1.0742(12) 0.055(4) Uani 1 1 d . . . . .
H12 H 0.6085 0.3771 1.1331 0.065 Uiso 1 1 calc R U . . .
C13 C 0.7728(18) 0.3914(14) 1.1027(17) 0.070(5) Uani 1 1 d . . . . .
H13 H 0.8141 0.3849 1.1815 0.084 Uiso 1 1 calc R U . . .
C14 C 0.2618(12) 0.3956(10) 0.6515(12) 0.036(3) Uani 1 1 d . . . . .
N3 N 0.2906(10) 0.3870(9) 0.7633(10) 0.039(3) Uani 1 1 d . . . . .
C16 C 0.5923(14) 0.3959(10) 0.9540(14) 0.043(4) Uani 1 1 d . . . . .
O6 O 0.6887(10) 0.3014(8) 0.6421(11) 0.057(3) Uani 1 1 d . . . . .
C18 C -0.1046(14) 0.3693(12) 0.4901(17) 0.054(4) Uani 1 1 d . . . . .
H18 H -0.1859 0.3641 0.4551 0.065 Uiso 1 1 calc R U . . .
C20 C 0.1298(12) 0.3843(11) 0.5920(15) 0.044(4) Uani 1 1 d . . . . .
C21 C 0.6195(13) 0.2406(9) 0.6486(13) 0.043(4) Uani 1 1 d D . . . .
C23 C 0.8336(17) 0.4059(15) 1.0148(18) 0.077(6) Uani 1 1 d . . . . .
H23 H 0.8870 0.3713 1.0331 0.092 Uiso 1 1 d R U . . .
C28 C 0.0423(13) 0.4142(10) 0.6486(14) 0.045(4) Uani 1 1 d . . . . .
H28 H 0.0655 0.4400 0.7243 0.054 Uiso 1 1 calc R U . . .
C25 C 0.0961(14) 0.3472(12) 0.4772(13) 0.051(4) Uani 1 1 d . . . . .
H25 H 0.1539 0.3293 0.4355 0.061 Uiso 1 1 calc R U . . .
C26 C 0.7701(15) 0.4095(13) 0.8957(16) 0.062(5) Uani 1 1 d . . . . .
H26 H 0.8129 0.4155 0.8357 0.074 Uiso 1 1 calc R U . . .
C27 C -0.0267(14) 0.3374(11) 0.4261(17) 0.054(4) Uani 1 1 d . . . . .
H27 H -0.0532 0.3101 0.3517 0.065 Uiso 1 1 calc R U . . .
C24 C 0.6542(16) 0.1425(9) 0.6339(18) 0.065(5) Uani 1 1 d D . . . .
H24A H 0.6977 0.1387 0.5712 0.097 Uiso 1 1 calc R U . . .
H24B H 0.5832 0.1048 0.6139 0.097 Uiso 1 1 calc R U . . .
H24C H 0.7042 0.1207 0.7070 0.097 Uiso 1 1 calc R U . . .
C29 C 0.4562(13) 0.3891(10) 0.9153(11) 0.036(3) Uani 1 1 d . . . . .


_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
O4 C6 1.246(14) . ?
O4 Dy1 2.346(8) 3_666 ?
O4 Dy1 2.610(9) . ?
Dy1 O1 2.306(9) . ?
Dy1 O4 2.346(8) 3_666 ?
Dy1 O5 2.382(8) . ?
Dy1 N1 2.425(11) . ?
Dy1 O7 2.433(10) . ?
Dy1 O2 2.454(9) . ?
Dy1 O6 2.473(11) . ?
Dy1 N2 2.503(11) . ?
Dy1 C21 2.784(12) . ?
Dy1 C6 2.900(14) . ?
C1 C6 1.48(2) . ?
N4 C29 1.333(17) . ?
O1 C14 1.299(16) . ?
O2 C6 1.254(15) . ?
O7 C21 1.225(17) . ?
N5 C18 1.33(2) . ?
N5 C28 1.363(18) . ?
N1 C29 1.293(17) . ?
N1 N3 1.417(15) . ?
N2 C26 1.326(19) . ?
N2 C16 1.335(19) . ?
C12 C13 1.35(2) . ?
C12 C16 1.41(2) . ?
C13 C23 1.36(3) . ?
C14 N3 1.262(17) . ?
C14 C20 1.520(19) . ?
C16 C29 1.52(2) . ?
O6 C21 1.191(17) . ?
C18 C27 1.35(2) . ?
C20 C28 1.37(2) . ?
C20 C25 1.40(2) . ?
C21 C24 1.486(5) . ?
C23 C26 1.40(2) . ?
C25 C27 1.40(2) . ?

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
C6 O4 Dy1 154.6(9) . 3_666 ?
C6 O4 Dy1 90.4(8) . . ?
Dy1 O4 Dy1 112.7(3) 3_666 . ?
O1 Dy1 O4 75.3(3) . 3_666 ?
O1 Dy1 O5 145.0(3) . . ?
O4 Dy1 O5 78.4(3) 3_666 . ?
O1 Dy1 N1 64.5(3) . . ?
O4 Dy1 N1 138.8(4) 3_666 . ?
O5 Dy1 N1 141.6(3) . . ?
O1 Dy1 O7 79.8(3) . . ?
O4 Dy1 O7 89.3(3) 3_666 . ?
O5 Dy1 O7 122.8(3) . . ?
N1 Dy1 O7 75.9(4) . . ?
O1 Dy1 O2 95.2(3) . . ?
O4 Dy1 O2 117.7(3) 3_666 . ?
O5 Dy1 O2 77.0(3) . . ?
N1 Dy1 O2 75.8(4) . . ?
O7 Dy1 O2 150.5(3) . . ?
O1 Dy1 O6 125.2(4) . . ?
O4 Dy1 O6 80.4(4) 3_666 . ?
O5 Dy1 O6 71.5(3) . . ?
N1 Dy1 O6 115.7(4) . . ?
O7 Dy1 O6 51.4(3) . . ?
O2 Dy1 O6 139.4(4) . . ?
O1 Dy1 N2 128.4(4) . . ?
O4 Dy1 N2 154.0(4) 3_666 . ?
O5 Dy1 N2 83.1(3) . . ?
N1 Dy1 N2 64.0(4) . . ?
O7 Dy1 N2 85.5(4) . . ?
O2 Dy1 N2 74.9(3) . . ?
O6 Dy1 N2 76.5(4) . . ?
O1 Dy1 O4 77.2(3) . . ?
O4 Dy1 O4 67.3(3) 3_666 . ?
O5 Dy1 O4 71.5(3) . . ?
N1 Dy1 O4 109.5(3) . . ?
O7 Dy1 O4 150.6(3) . . ?
O2 Dy1 O4 50.7(3) . . ?
O6 Dy1 O4 134.7(3) . . ?
N2 Dy1 O4 123.3(3) . . ?
O1 Dy1 C21 103.2(4) . . ?
O4 Dy1 C21 84.4(4) 3_666 . ?
O5 Dy1 C21 96.8(4) . . ?
N1 Dy1 C21 96.3(4) . . ?
O7 Dy1 C21 26.1(4) . . ?
O2 Dy1 C21 154.5(4) . . ?
O6 Dy1 C21 25.3(4) . . ?
N2 Dy1 C21 79.8(4) . . ?
O4 Dy1 C21 150.8(4) . . ?
O1 Dy1 C6 87.5(4) . . ?
O4 Dy1 C6 92.4(3) 3_666 . ?
O5 Dy1 C6 70.8(3) . . ?
N1 Dy1 C6 94.0(4) . . ?
O7 Dy1 C6 166.3(4) . . ?
O2 Dy1 C6 25.4(3) . . ?
O6 Dy1 C6 142.3(4) . . ?
N2 Dy1 C6 98.7(4) . . ?
O4 Dy1 C6 25.4(3) . . ?
C21 Dy1 C6 167.6(4) . . ?
C14 O1 Dy1 119.9(8) . . ?
C6 O2 Dy1 97.6(8) . . ?
O4 C6 O2 120.8(13) . . ?
O4 C6 C1 120.8(14) . . ?
O2 C6 C1 118.2(13) . . ?
O4 C6 Dy1 64.1(7) . . ?
O2 C6 Dy1 57.0(7) . . ?
C1 C6 Dy1 175.0(11) . . ?
C21 O7 Dy1 93.1(8) . . ?
C18 N5 C28 115.7(14) . . ?
C29 N1 N3 114.2(11) . . ?
C29 N1 Dy1 126.3(9) . . ?
N3 N1 Dy1 119.5(8) . . ?
C26 N2 C16 117.5(13) . . ?
C26 N2 Dy1 121.9(11) . . ?
C16 N2 Dy1 120.4(10) . . ?
C13 C12 C16 119.0(16) . . ?
C23 C13 C12 119.1(17) . . ?
N3 C14 O1 127.0(13) . . ?
N3 C14 C20 117.5(13) . . ?
O1 C14 C20 115.5(12) . . ?
C14 N3 N1 109.1(11) . . ?
N2 C16 C12 122.5(15) . . ?
N2 C16 C29 115.6(13) . . ?
C12 C16 C29 121.7(14) . . ?
C21 O6 Dy1 92.1(8) . . ?
N5 C18 C27 126.9(15) . . ?
C28 C20 C25 119.1(14) . . ?
C28 C20 C14 120.2(14) . . ?
C25 C20 C14 120.6(14) . . ?
O6 C21 O7 123.4(12) . . ?
O6 C21 C24 119.6(14) . . ?
O7 C21 C24 116.7(14) . . ?
O6 C21 Dy1 62.6(7) . . ?
O7 C21 Dy1 60.8(7) . . ?
C24 C21 Dy1 174.3(11) . . ?
C13 C23 C26 119.5(18) . . ?
N5 C28 C20 122.7(15) . . ?
C20 C25 C27 118.7(16) . . ?
N2 C26 C23 122.2(18) . . ?
C18 C27 C25 116.8(17) . . ?
N1 C29 N4 125.2(14) . . ?
N1 C29 C16 113.4(12) . . ?
N4 C29 C16 121.3(13) . . ?

_refine_diff_density_max         1.186
_refine_diff_density_min         -2.489
_refine_diff_density_rms         0.183

_shelxl_version_number           2014/6



####################################################################### 
# 
# 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_exp_0803_2-1
_database_code_depnum_ccdc_archive 'CCDC 1523394'
_audit_update_record             
;
2017-08-21 deposited with the CCDC.
2017-08-23 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         'C32 H36 Dy2 N10 O12, 4(H2 O)'
_chemical_formula_sum            'C32 H44 Dy2 N10 O16'
_chemical_formula_weight         1149.77

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'
Dy Dy -0.1892 4.4098 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   17.6569(7)
_cell_length_b                   13.0716(5)
_cell_length_c                   18.0859(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.960(4)
_cell_angle_gamma                90
_cell_volume                     4134.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4230
_cell_measurement_theta_min      3.8410
_cell_measurement_theta_max      28.8310

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_F_000             2264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    3.668
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82314
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
'SADABS 2015/2 (Bruker,2015) was used for absorption correction. R(int) was  0.07741 before and 0.05435 after correction. The Ratio of minimum to maximum transmission is 0.8231. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11114
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.318
_diffrn_reflns_theta_max         29.323
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4803
_reflns_number_gt                3688
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0840P)²+1.2560P] 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         4803
_refine_ls_number_parameters     261
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1290
_refine_ls_wR_factor_gt          0.1129
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.946
_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 0.18874(2) 0.83873(2) 0.56712(2) 0.02625(12) Uani 1 1 d . . . . .
O6 O 0.2633(3) 0.8418(3) 0.4683(2) 0.0314(10) Uani 1 1 d . . . . .
O5 O 0.3183(2) 0.8284(3) 0.6188(2) 0.0339(10) Uani 1 1 d . . . . .
H5A H 0.3450 0.7878 0.5923 0.051 Uiso 1 1 d R U . . .
H5B H 0.3227 0.8029 0.6650 0.051 Uiso 1 1 d R U . . .
O1 O 0.0934(2) 0.7738(3) 0.4755(2) 0.0331(10) Uani 1 1 d . . . . .
O2 O 0.0841(3) 0.8700(5) 0.6389(3) 0.0550(14) Uani 1 1 d . . . . .
O3 O 0.1972(3) 0.8662(4) 0.7021(3) 0.0518(13) Uani 1 1 d . . . . .
C1 C -0.1070(5) 0.8217(9) 0.2710(5) 0.062(3) Uani 1 1 d . . . . .
H1 H -0.1381 0.8669 0.2409 0.074 Uiso 1 1 calc R U . . .
N4 N 0.0786(4) 1.1332(5) 0.4546(3) 0.0440(14) Uani 1 1 d . . . . .
H4A H 0.0959 1.1389 0.4109 0.053 Uiso 1 1 d R U . . .
H4B H 0.0307 1.1107 0.4472 0.053 Uiso 1 1 d R U . . .
N3 N 0.1160(3) 0.9675(4) 0.4905(3) 0.0299(11) Uani 1 1 d . . . . .
N2 N 0.0584(3) 0.9364(5) 0.4343(3) 0.0362(12) Uani 1 1 d . . . . .
C6 C 0.0512(3) 0.8378(5) 0.4315(3) 0.0321(14) Uani 1 1 d . . . . .
C8 C 0.1825(2) 1.1032(3) 0.5529(2) 0.0333(14) Uani 1 1 d G . . . .
N5 N 0.2246(2) 1.0274(2) 0.5938(2) 0.0380(13) Uani 1 1 d G . . . .
C12 C 0.2815(3) 1.0540(3) 0.6516(3) 0.060(2) Uani 1 1 d G . . . .
H12 H 0.3097 1.0032 0.6790 0.071 Uiso 1 1 calc R U . . .
C11 C 0.2963(3) 1.1564(3) 0.6685(3) 0.070(3) Uani 1 1 d G . . . .
H11 H 0.3344 1.1742 0.7071 0.084 Uiso 1 1 calc R U . . .
C10 C 0.2542(3) 1.2323(2) 0.6275(3) 0.063(2) Uani 1 1 d G . . . .
H10 H 0.2641 1.3008 0.6388 0.076 Uiso 1 1 calc R U . . .
C9 C 0.1973(3) 1.2057(2) 0.5697(3) 0.051(2) Uani 1 1 d G . . . .
H9 H 0.1691 1.2564 0.5423 0.062 Uiso 1 1 calc R U . . .
C2 C -0.0731(5) 0.6591(7) 0.3026(5) 0.059(2) Uani 1 1 d . . . . .
H2 H -0.0793 0.5890 0.2952 0.071 Uiso 1 1 calc R U . . .
C5 C -0.0548(4) 0.8617(7) 0.3267(4) 0.0501(19) Uani 1 1 d . . . . .
H5 H -0.0507 0.9322 0.3333 0.060 Uiso 1 1 calc R U . . .
C7 C 0.1231(3) 1.0657(5) 0.4968(3) 0.0320(13) Uani 1 1 d . . . . .
C4 C -0.0088(3) 0.7972(6) 0.3723(3) 0.0397(16) Uani 1 1 d . . . . .
C3 C -0.0190(4) 0.6940(7) 0.3612(4) 0.0501(18) Uani 1 1 d . . . . .
H3 H 0.0098 0.6476 0.3924 0.060 Uiso 1 1 calc R U . . .
C13 C 0.1273(5) 0.8757(7) 0.7008(4) 0.0463(18) Uani 1 1 d . . . . .
N1 N -0.1158(3) 0.7227(7) 0.2574(3) 0.059(2) Uani 1 1 d . . . . .
C14 C 0.0971(6) 0.8897(10) 0.7659(5) 0.091(4) Uani 1 1 d . . . . .
H14A H 0.0632 0.9312 0.7587 0.137 Uiso 1 1 d R U . . .
H14B H 0.1358 0.9126 0.8049 0.137 Uiso 1 1 d R U . . .
H14C H 0.0760 0.8263 0.7804 0.137 Uiso 1 1 d R U . . .
C15 C 0.2954(4) 0.8820(6) 0.4166(4) 0.0426(16) Uani 1 1 d . . . A 2
C16 C 0.2858(9) 0.9926(7) 0.4021(8) 0.113(5) Uani 1 1 d . . . A 2
H16A H 0.2524 1.0029 0.3561 0.170 Uiso 1 1 calc R U . A 2
H16B H 0.3346 1.0229 0.3985 0.170 Uiso 1 1 calc R U . A 2
H16C H 0.2640 1.0241 0.4422 0.170 Uiso 1 1 calc R U . A 2
O17 O 0.3344(4) 0.8278(4) 0.3780(3) 0.0531(15) Uani 1 1 d . . . A 2
O9 O 0.4653(10) 0.1398(10) 0.5356(7) 0.210(7) Uani 1 1 d . . . B 2
H9A H 0.5019 0.1825 0.5393 0.314 Uiso 1 1 d R U . B 2
H9B H 0.4816 0.0828 0.5538 0.314 Uiso 1 1 d R U . B 2
O10 O 0.5264(6) 0.1204(12) 0.6826(6) 0.190(6) Uani 1 1 d . . . C -1
H10A H 0.5411 0.1533 0.6594 0.285 Uiso 1 1 d R U . C -1
H10B H 0.5564 0.1002 0.7206 0.285 Uiso 1 1 d R U . C -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 2.350(4) . ?
Dy1 O5 2.352(4) . ?
Dy1 O6 2.363(4) . ?
Dy1 N3 2.431(5) . ?
Dy1 O2 2.434(5) . ?
Dy1 O3 2.452(5) . ?
Dy1 O17 2.450(5) 7_566 ?
Dy1 N5 2.575(3) . ?
Dy1 O6 2.617(4) 7_566 ?
Dy1 C13 2.825(7) . ?
Dy1 C15 2.909(8) 7_566 ?
O6 C15 1.271(8) . ?
O6 Dy1 2.617(4) 7_566 ?
O5 H5A 0.8920 . ?
O5 H5B 0.8919 . ?
O1 C6 1.313(7) . ?
O2 C13 1.266(9) . ?
O3 C13 1.239(9) . ?
C1 N1 1.322(12) . ?
C1 C5 1.372(11) . ?
C1 H1 0.9300 . ?
N4 C7 1.346(8) . ?
N4 H4A 0.8895 . ?
N4 H4B 0.8889 . ?
N3 C7 1.294(8) . ?
N3 N2 1.396(7) . ?
N2 C6 1.295(8) . ?
C6 C4 1.495(9) . ?
C8 N5 1.3900 . ?
C8 C9 1.3900 . ?
C8 C7 1.440(7) . ?
N5 C12 1.3900 . ?
C12 C11 1.3900 . ?
C12 H12 0.9300 . ?
C11 C10 1.3900 . ?
C11 H11 0.9300 . ?
C10 C9 1.3900 . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C2 N1 1.325(12) . ?
C2 C3 1.402(11) . ?
C2 H2 0.9300 . ?
C5 C4 1.366(11) . ?
C5 H5 0.9300 . ?
C4 C3 1.371(11) . ?
C3 H3 0.9300 . ?
C13 C14 1.371(11) . ?
C14 H14A 0.8047 . ?
C14 H14B 0.9597 . ?
C14 H14C 0.9601 . ?
C15 O17 1.264(8) . ?
C15 C16 1.476(11) . ?
C15 Dy1 2.909(8) 7_566 ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O17 Dy1 2.450(5) 7_566 ?
O9 H9A 0.8491 . ?
O9 H9B 0.8493 . ?
O10 H10A 0.6758 . ?
O10 H10B 0.8510 . ?

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 O5 145.22(14) . . ?
O1 Dy1 O6 83.81(15) . . ?
O5 Dy1 O6 71.86(16) . . ?
O1 Dy1 N3 65.02(15) . . ?
O5 Dy1 N3 132.40(16) . . ?
O6 Dy1 N3 82.08(16) . . ?
O1 Dy1 O2 85.09(17) . . ?
O5 Dy1 O2 124.45(17) . . ?
O6 Dy1 O2 160.70(17) . . ?
N3 Dy1 O2 78.93(18) . . ?
O1 Dy1 O3 133.96(17) . . ?
O5 Dy1 O3 71.97(17) . . ?
O6 Dy1 O3 141.93(17) . . ?
N3 Dy1 O3 114.91(18) . . ?
O2 Dy1 O3 52.48(18) . . ?
O1 Dy1 O17 79.73(18) . 7_566 ?
O5 Dy1 O17 89.75(19) . 7_566 ?
O6 Dy1 O17 117.62(15) . 7_566 ?
N3 Dy1 O17 137.9(2) . 7_566 ?
O2 Dy1 O17 75.61(19) . 7_566 ?
O3 Dy1 O17 73.58(19) . 7_566 ?
O1 Dy1 N5 127.68(13) . . ?
O5 Dy1 N5 77.30(13) . . ?
O6 Dy1 N5 88.70(14) . . ?
N3 Dy1 N5 62.66(14) . . ?
O2 Dy1 N5 85.66(19) . . ?
O3 Dy1 N5 72.14(17) . . ?
O17 Dy1 N5 145.61(16) 7_566 . ?
O1 Dy1 O6 74.11(14) . 7_566 ?
O5 Dy1 O6 73.48(14) . 7_566 ?
O6 Dy1 O6 66.25(15) . 7_566 ?
N3 Dy1 O6 130.40(15) . 7_566 ?
O2 Dy1 O6 125.22(18) . 7_566 ?
O3 Dy1 O6 113.48(16) . 7_566 ?
O17 Dy1 O6 51.37(16) 7_566 7_566 ?
N5 Dy1 O6 146.13(14) . 7_566 ?
O1 Dy1 C13 110.0(2) . . ?
O5 Dy1 C13 97.90(19) . . ?
O6 Dy1 C13 164.8(2) . . ?
N3 Dy1 C13 97.73(19) . . ?
O2 Dy1 C13 26.55(19) . . ?
O3 Dy1 C13 25.9(2) . . ?
O17 Dy1 C13 72.5(2) 7_566 . ?
N5 Dy1 C13 77.8(2) . . ?
O6 Dy1 C13 122.62(19) 7_566 . ?
O1 Dy1 C15 76.28(19) . 7_566 ?
O5 Dy1 C15 80.10(18) . 7_566 ?
O6 Dy1 C15 92.15(17) . 7_566 ?
N3 Dy1 C15 141.2(2) . 7_566 ?
O2 Dy1 C15 100.5(2) . 7_566 ?
O3 Dy1 C15 93.04(19) . 7_566 ?
O17 Dy1 C15 25.49(18) 7_566 7_566 ?
N5 Dy1 C15 155.92(17) . 7_566 ?
O6 Dy1 C15 25.90(16) 7_566 7_566 ?
C13 Dy1 C15 97.2(2) . 7_566 ?
C15 O6 Dy1 156.2(4) . . ?
C15 O6 Dy1 90.0(4) . 7_566 ?
Dy1 O6 Dy1 113.74(15) . 7_566 ?
Dy1 O5 H5A 112.2 . . ?
Dy1 O5 H5B 110.4 . . ?
H5A O5 H5B 107.2 . . ?
C6 O1 Dy1 119.3(4) . . ?
C13 O2 Dy1 94.2(4) . . ?
C13 O3 Dy1 94.1(4) . . ?
N1 C1 C5 124.0(8) . . ?
N1 C1 H1 118.0 . . ?
C5 C1 H1 118.0 . . ?
C7 N4 H4A 108.3 . . ?
C7 N4 H4B 109.7 . . ?
H4A N4 H4B 109.3 . . ?
C7 N3 N2 113.9(5) . . ?
C7 N3 Dy1 126.9(4) . . ?
N2 N3 Dy1 119.2(4) . . ?
C6 N2 N3 112.1(5) . . ?
O1 C6 N2 124.4(6) . . ?
O1 C6 C4 119.6(6) . . ?
N2 C6 C4 115.9(6) . . ?
N5 C8 C9 120.0 . . ?
N5 C8 C7 114.6(3) . . ?
C9 C8 C7 125.4(3) . . ?
C8 N5 C12 120.0 . . ?
C8 N5 Dy1 118.93(18) . . ?
C12 N5 Dy1 120.92(18) . . ?
C11 C12 N5 120.0 . . ?
C11 C12 H12 120.0 . . ?
N5 C12 H12 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C9 C10 C11 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
N1 C2 C3 122.1(8) . . ?
N1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C1 C5 C4 119.4(9) . . ?
C1 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
N3 C7 N4 124.0(6) . . ?
N3 C7 C8 116.9(5) . . ?
N4 C7 C8 119.1(6) . . ?
C5 C4 C3 117.6(7) . . ?
C5 C4 C6 121.1(7) . . ?
C3 C4 C6 121.3(7) . . ?
C4 C3 C2 119.6(8) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
O3 C13 O2 119.2(6) . . ?
O3 C13 C14 120.1(8) . . ?
O2 C13 C14 120.7(8) . . ?
O3 C13 Dy1 60.0(4) . . ?
O2 C13 Dy1 59.2(4) . . ?
C14 C13 Dy1 177.8(8) . . ?
C2 N1 C1 117.2(7) . . ?
C13 C14 H14A 108.6 . . ?
C13 C14 H14B 110.6 . . ?
H14A C14 H14B 110.3 . . ?
C13 C14 H14C 109.3 . . ?
H14A C14 H14C 108.6 . . ?
H14B C14 H14C 109.5 . . ?
O6 C15 O17 120.5(7) . . ?
O6 C15 C16 118.9(7) . . ?
O17 C15 C16 120.6(7) . . ?
O6 C15 Dy1 64.1(4) . 7_566 ?
O17 C15 Dy1 56.5(4) . 7_566 ?
C16 C15 Dy1 175.5(7) . 7_566 ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 O17 Dy1 98.0(4) . 7_566 ?
H9A O9 H9B 109.4 . . ?
H10A O10 H10B 116.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N3 N2 C6 -177.6(6) . . . . ?
Dy1 N3 N2 C6 0.6(7) . . . . ?
Dy1 O1 C6 N2 0.5(8) . . . . ?
Dy1 O1 C6 C4 179.1(4) . . . . ?
N3 N2 C6 O1 -0.7(9) . . . . ?
N3 N2 C6 C4 -179.4(5) . . . . ?
C9 C8 N5 C12 0.0 . . . . ?
C7 C8 N5 C12 -177.4(5) . . . . ?
C9 C8 N5 Dy1 175.6(3) . . . . ?
C7 C8 N5 Dy1 -1.8(4) . . . . ?
C8 N5 C12 C11 0.0 . . . . ?
Dy1 N5 C12 C11 -175.5(3) . . . . ?
N5 C12 C11 C10 0.0 . . . . ?
C12 C11 C10 C9 0.0 . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
N5 C8 C9 C10 0.0 . . . . ?
C7 C8 C9 C10 177.1(5) . . . . ?
N1 C1 C5 C4 -0.6(14) . . . . ?
N2 N3 C7 N4 1.2(9) . . . . ?
Dy1 N3 C7 N4 -176.9(5) . . . . ?
N2 N3 C7 C8 -178.9(5) . . . . ?
Dy1 N3 C7 C8 3.0(8) . . . . ?
N5 C8 C7 N3 -0.5(7) . . . . ?
C9 C8 C7 N3 -177.8(4) . . . . ?
N5 C8 C7 N4 179.4(5) . . . . ?
C9 C8 C7 N4 2.1(8) . . . . ?
C1 C5 C4 C3 -2.0(12) . . . . ?
C1 C5 C4 C6 177.3(7) . . . . ?
O1 C6 C4 C5 178.6(6) . . . . ?
N2 C6 C4 C5 -2.7(10) . . . . ?
O1 C6 C4 C3 -2.2(10) . . . . ?
N2 C6 C4 C3 176.5(7) . . . . ?
C5 C4 C3 C2 2.6(12) . . . . ?
C6 C4 C3 C2 -176.7(7) . . . . ?
N1 C2 C3 C4 -0.7(13) . . . . ?
Dy1 O3 C13 O2 -1.0(9) . . . . ?
Dy1 O3 C13 C14 177.5(9) . . . . ?
Dy1 O2 C13 O3 1.0(9) . . . . ?
Dy1 O2 C13 C14 -177.5(9) . . . . ?
C3 C2 N1 C1 -1.9(13) . . . . ?
C5 C1 N1 C2 2.5(13) . . . . ?
Dy1 O6 C15 O17 180.0(7) . . . . ?
Dy1 O6 C15 O17 -3.2(8) 7_566 . . . ?
Dy1 O6 C15 C16 -0.6(18) . . . . ?
Dy1 O6 C15 C16 176.3(10) 7_566 . . . ?
Dy1 O6 C15 Dy1 -176.8(12) . . . 7_566 ?
O6 C15 O17 Dy1 3.4(8) . . . 7_566 ?
C16 C15 O17 Dy1 -176.0(10) . . . 7_566 ?

_refine_diff_density_max         1.059
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.144



