# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1843779'
_audit_update_record             
;
2018-06-09 deposited with the CCDC.
2018-07-16 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            'C32 H46 Gd2 N4 O16'
_chemical_formula_weight         1057.23

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'
Gd Gd -0.1653 3.9035 '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                   11.4479(7)
_cell_length_b                   13.9987(9)
_cell_length_c                   13.0690(8)
_cell_angle_alpha                90
_cell_angle_beta                 108.991(2)
_cell_angle_gamma                90
_cell_volume                     1980.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5138
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      23.57

_exptl_crystal_description       cuboid
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_F_000             1044
_exptl_transmission_factor_min   0.550
_exptl_transmission_factor_max   0.613
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    3.393
_shelx_estimated_absorpt_T_min   0.550
_shelx_estimated_absorpt_T_max   0.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_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            24420
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.059
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4312
_reflns_number_gt                3187
_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)+(0.0500P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         4312
_refine_ls_number_parameters     257
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0770
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_restrained_S_all      0.937
_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
C1 C 0.6727(4) 0.9450(3) 0.9312(3) 0.0419(10) Uani 1 1 d . . . . .
C2 C 0.6718(4) 1.0006(4) 1.0215(4) 0.0468(11) Uani 1 1 d . . . . .
C3 C 0.7009(5) 0.9618(4) 1.1228(4) 0.0580(14) Uani 1 1 d . . . . .
H3 H 0.6955 0.9991 1.1799 0.070 Uiso 1 1 calc R U . . .
C4 C 0.7387(5) 0.8671(4) 1.1411(4) 0.0654(15) Uani 1 1 d . . . . .
H4 H 0.7615 0.8421 1.2107 0.078 Uiso 1 1 calc R U . . .
C5 C 0.7421(5) 0.8110(4) 1.0567(4) 0.0616(14) Uani 1 1 d . . . . .
H5 H 0.7686 0.7479 1.0688 0.074 Uiso 1 1 calc R U . . .
C6 C 0.7049(4) 0.8494(3) 0.9498(3) 0.0470(11) Uani 1 1 d . . . . .
C7 C 0.6922(4) 0.7822(3) 0.8641(3) 0.0472(11) Uani 1 1 d . . . . .
H7 H 0.7201 0.7203 0.8836 0.057 Uiso 1 1 calc R U . . .
C8 C 0.5889(4) 0.7336(3) 0.5897(4) 0.0459(11) Uani 1 1 d . . . . .
C9 C 0.5750(5) 0.6480(3) 0.5210(4) 0.0601(14) Uani 1 1 d . . . . .
H9A H 0.4893 0.6308 0.4926 0.090 Uiso 1 1 calc R U . . .
H9B H 0.6209 0.5961 0.5635 0.090 Uiso 1 1 calc R U . . .
H9C H 0.6057 0.6612 0.4624 0.090 Uiso 1 1 calc R U . . .
C10 C 0.6342(5) 1.1549(4) 1.0842(4) 0.0590(13) Uani 1 1 d . . . . .
H10A H 0.7142 1.1568 1.1403 0.071 Uiso 1 1 calc R U . . .
H10B H 0.5737 1.1314 1.1156 0.071 Uiso 1 1 calc R U . . .
C11 C 0.5992(7) 1.2519(4) 1.0383(5) 0.0864(19) Uani 1 1 d . . . . .
H11A H 0.6603 1.2748 1.0085 0.130 Uiso 1 1 calc R U . . .
H11B H 0.5944 1.2944 1.0944 0.130 Uiso 1 1 calc R U . . .
H11C H 0.5204 1.2491 0.9823 0.130 Uiso 1 1 calc R U . . .
C12 C 0.5234(7) 1.1835(4) 0.7371(4) 0.0795(18) Uani 1 1 d . . . . .
H12A H 0.4361 1.1937 0.7194 0.119 Uiso 1 1 calc R U . . .
H12B H 0.5639 1.2437 0.7383 0.119 Uiso 1 1 calc R U . . .
H12C H 0.5549 1.1539 0.8069 0.119 Uiso 1 1 calc R U . . .
C13 C 1.0013(5) 0.9767(5) 0.7424(6) 0.084(2) Uani 1 1 d . . . . .
H13A H 1.0346 0.9770 0.8199 0.126 Uiso 1 1 calc R U . . .
H13B H 1.0255 1.0341 0.7145 0.126 Uiso 1 1 calc R U . . .
H13C H 1.0322 0.9223 0.7146 0.126 Uiso 1 1 calc R U . . .
C14 C 0.8629(5) 0.9717(4) 0.7081(4) 0.0519(13) Uani 1 1 d . . . . .
C15 C 0.1998(5) 0.9688(4) 0.5513(5) 0.0706(17) Uani 1 1 d . . . . .
H15A H 0.1749 0.9467 0.6106 0.106 Uiso 1 1 calc R U . . .
H15B H 0.1593 0.9316 0.4880 0.106 Uiso 1 1 calc R U . . .
H15C H 0.1774 1.0348 0.5373 0.106 Uiso 1 1 calc R U . . .
C16 C 0.3360(5) 0.9586(3) 0.5793(4) 0.0446(11) Uani 1 1 d . . . . .
Gd1 Gd 0.60408(2) 0.95876(2) 0.66027(2) 0.03874(10) Uani 1 1 d . . . . .
H2A H 0.650(5) 0.6685(18) 0.720(4) 0.08(2) Uiso 1 1 d D . . . .
H4A H 0.517(4) 1.149(3) 0.6015(17) 0.034(12) Uiso 1 1 d D . . . .
N1 N 0.6452(3) 0.8005(3) 0.7619(3) 0.0446(9) Uani 1 1 d . . . . .
N2 N 0.6346(4) 0.7211(3) 0.6950(3) 0.0500(10) Uani 1 1 d D . . . .
O1 O 0.6431(3) 0.9838(2) 0.8363(2) 0.0516(8) Uani 1 1 d . . . . .
O2 O 0.5585(3) 0.8150(2) 0.5506(2) 0.0500(8) Uani 1 1 d . . . . .
O3 O 0.6387(3) 1.0941(2) 0.9981(2) 0.0551(9) Uani 1 1 d . . . . .
O4 O 0.5456(4) 1.1238(2) 0.6587(2) 0.0622(10) Uani 1 1 d D . . . .
O5 O 0.8086(3) 0.8955(2) 0.6731(3) 0.0594(9) Uani 1 1 d . . . . .
O6 O 0.8022(3) 1.0459(2) 0.7129(3) 0.0544(9) Uani 1 1 d . . . . .
O7 O 0.3971(3) 0.9277(3) 0.6698(3) 0.0574(9) Uani 1 1 d . . . . .
O8 O 0.3882(3) 0.9820(2) 0.5115(2) 0.0455(7) 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
C1 O1 1.294(5) . ?
C1 C6 1.389(6) . ?
C1 C2 1.416(6) . ?
C2 C3 1.368(7) . ?
C2 O3 1.369(6) . ?
C3 C4 1.391(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.426(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.432(6) . ?
C7 N1 1.293(5) . ?
C7 H7 0.9300 . ?
C8 O2 1.250(5) . ?
C8 N2 1.315(6) . ?
C8 C9 1.475(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.425(6) . ?
C10 C11 1.486(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O4 1.408(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.501(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 O5 1.244(6) . ?
C14 O6 1.262(6) . ?
C15 C16 1.488(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O7 1.240(6) . ?
C16 O8 1.262(5) . ?
Gd1 O1 2.224(3) . ?
Gd1 O4 2.404(3) . ?
Gd1 O8 2.422(3) 3_676 ?
Gd1 O2 2.427(3) . ?
Gd1 O7 2.452(4) . ?
Gd1 O5 2.458(3) . ?
Gd1 O6 2.468(3) . ?
Gd1 N1 2.547(4) . ?
Gd1 O8 2.621(3) . ?
N1 N2 1.396(5) . ?
N2 H2A 0.802(10) . ?
O4 H4A 0.794(10) . ?
O8 Gd1 2.422(3) 3_676 ?

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 C1 C6 122.9(4) . . ?
O1 C1 C2 119.8(4) . . ?
C6 C1 C2 117.2(4) . . ?
C3 C2 O3 123.9(4) . . ?
C3 C2 C1 121.5(5) . . ?
O3 C2 C1 114.6(4) . . ?
C2 C3 C4 120.6(5) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.9(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 119.8(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 120.8(4) . . ?
C1 C6 C7 122.8(4) . . ?
C5 C6 C7 116.2(4) . . ?
N1 C7 C6 125.5(4) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
O2 C8 N2 120.9(4) . . ?
O2 C8 C9 122.1(4) . . ?
N2 C8 C9 117.1(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 107.5(4) . . ?
O3 C10 H10A 110.2 . . ?
C11 C10 H10A 110.2 . . ?
O3 C10 H10B 110.2 . . ?
C11 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C12 H12A 109.5 . . ?
O4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 O6 120.4(5) . . ?
O5 C14 C13 120.1(5) . . ?
O6 C14 C13 119.4(5) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 O8 120.7(5) . . ?
O7 C16 C15 119.3(5) . . ?
O8 C16 C15 120.0(4) . . ?
O1 Gd1 O4 79.57(11) . . ?
O1 Gd1 O8 148.15(12) . 3_676 ?
O4 Gd1 O8 75.97(11) . 3_676 ?
O1 Gd1 O2 132.36(11) . . ?
O4 Gd1 O2 141.85(10) . . ?
O8 Gd1 O2 78.57(10) 3_676 . ?
O1 Gd1 O7 81.23(12) . . ?
O4 Gd1 O7 84.24(14) . . ?
O8 Gd1 O7 115.82(11) 3_676 . ?
O2 Gd1 O7 81.80(12) . . ?
O1 Gd1 O5 96.89(12) . . ?
O4 Gd1 O5 127.13(14) . . ?
O8 Gd1 O5 82.23(11) 3_676 . ?
O2 Gd1 O5 76.01(12) . . ?
O7 Gd1 O5 147.97(13) . . ?
O1 Gd1 O6 77.11(13) . . ?
O4 Gd1 O6 75.85(13) . . ?
O8 Gd1 O6 77.37(11) 3_676 . ?
O2 Gd1 O6 125.15(12) . . ?
O7 Gd1 O6 152.80(12) . . ?
O5 Gd1 O6 52.42(12) . . ?
O1 Gd1 N1 69.92(11) . . ?
O4 Gd1 N1 147.58(11) . . ?
O8 Gd1 N1 136.45(11) 3_676 . ?
O2 Gd1 N1 63.53(11) . . ?
O7 Gd1 N1 80.60(12) . . ?
O5 Gd1 N1 68.96(12) . . ?
O6 Gd1 N1 106.72(12) . . ?
O1 Gd1 O8 124.84(11) . . ?
O4 Gd1 O8 71.42(11) . . ?
O8 Gd1 O8 65.18(12) 3_676 . ?
O2 Gd1 O8 72.28(10) . . ?
O7 Gd1 O8 50.65(10) . . ?
O5 Gd1 O8 138.00(11) . . ?
O6 Gd1 O8 134.81(11) . . ?
N1 Gd1 O8 117.68(11) . . ?
C7 N1 N2 114.3(4) . . ?
C7 N1 Gd1 130.9(3) . . ?
N2 N1 Gd1 113.8(3) . . ?
C8 N2 N1 118.2(4) . . ?
C8 N2 H2A 121(4) . . ?
N1 N2 H2A 121(4) . . ?
C1 O1 Gd1 145.8(3) . . ?
C8 O2 Gd1 122.4(3) . . ?
C2 O3 C10 118.2(4) . . ?
C12 O4 Gd1 132.9(3) . . ?
C12 O4 H4A 108(3) . . ?
Gd1 O4 H4A 117(3) . . ?
C14 O5 Gd1 93.8(3) . . ?
C14 O6 Gd1 92.9(3) . . ?
C16 O7 Gd1 98.3(3) . . ?
C16 O8 Gd1 155.2(3) . 3_676 ?
C16 O8 Gd1 89.7(3) . . ?
Gd1 O8 Gd1 114.82(12) 3_676 . ?

_refine_diff_density_max         0.867
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1843780'
_audit_update_record             
;
2018-06-09 deposited with the CCDC.
2018-07-16 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            'C32 H46 Dy2 N4 O16'
_chemical_formula_weight         1067.73

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                   11.4531(5)
_cell_length_b                   13.9589(6)
_cell_length_c                   13.0023(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.982(2)
_cell_angle_gamma                90
_cell_volume                     1965.67(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6225
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      23.66

_exptl_crystal_description       cuboid
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   0.513
_exptl_transmission_factor_max   0.578
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    3.846
_shelx_estimated_absorpt_T_min   0.513
_shelx_estimated_absorpt_T_max   0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_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            28225
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.062
_diffrn_reflns_theta_max         26.866
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4220
_reflns_number_gt                3299
_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)+(0.0500P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_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         4220
_refine_ls_number_parameters     257
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_restrained_S_all      0.952
_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
C1 C 0.1730(4) 0.0541(3) 0.4306(4) 0.0393(10) Uani 1 1 d . . . . .
C2 C 0.1716(4) -0.0020(3) 0.5221(4) 0.0417(10) Uani 1 1 d . . . . .
C3 C 0.2011(5) 0.0375(3) 0.6239(4) 0.0541(13) Uani 1 1 d . . . . .
H3 H 0.1955 0.0005 0.6816 0.065 Uiso 1 1 calc R U . . .
C4 C 0.2392(5) 0.1320(4) 0.6419(4) 0.0635(14) Uani 1 1 d . . . . .
H4 H 0.2612 0.1574 0.7117 0.076 Uiso 1 1 calc R U . . .
C5 C 0.2445(5) 0.1880(4) 0.5572(4) 0.0572(13) Uani 1 1 d . . . . .
H5 H 0.2735 0.2505 0.5701 0.069 Uiso 1 1 calc R U . . .
C6 C 0.2060(4) 0.1510(3) 0.4504(4) 0.0454(11) Uani 1 1 d . . . . .
C7 C 0.1939(4) 0.2177(3) 0.3644(4) 0.0457(11) Uani 1 1 d . . . . .
H7 H 0.2224 0.2796 0.3838 0.055 Uiso 1 1 calc R U . . .
C8 C 0.0885(4) 0.2651(3) 0.0893(4) 0.0432(10) Uani 1 1 d . . . . .
C9 C 0.0735(5) 0.3510(3) 0.0188(4) 0.0561(13) Uani 1 1 d . . . . .
H9A H 0.1147 0.3407 -0.0338 0.084 Uiso 1 1 calc R U . . .
H9B H 0.1089 0.4057 0.0627 0.084 Uiso 1 1 calc R U . . .
H9C H -0.0127 0.3623 -0.0180 0.084 Uiso 1 1 calc R U . . .
C10 C 0.1325(5) -0.1567(4) 0.5844(4) 0.0564(13) Uani 1 1 d . . . . .
H10A H 0.0725 -0.1332 0.6165 0.068 Uiso 1 1 calc R U . . .
H10B H 0.2126 -0.1594 0.6405 0.068 Uiso 1 1 calc R U . . .
C11 C 0.0961(6) -0.2532(4) 0.5364(5) 0.0786(18) Uani 1 1 d . . . . .
H11A H 0.0173 -0.2493 0.4803 0.118 Uiso 1 1 calc R U . . .
H11B H 0.0909 -0.2966 0.5920 0.118 Uiso 1 1 calc R U . . .
H11C H 0.1568 -0.2760 0.5058 0.118 Uiso 1 1 calc R U . . .
C12 C 0.0216(7) -0.1813(4) 0.2371(5) 0.0771(18) Uani 1 1 d . . . . .
H12A H 0.0645 -0.1576 0.3087 0.116 Uiso 1 1 calc R U . . .
H12B H 0.0487 -0.2454 0.2302 0.116 Uiso 1 1 calc R U . . .
H12C H -0.0656 -0.1815 0.2254 0.116 Uiso 1 1 calc R U . . .
C13 C 0.4996(5) 0.0226(5) 0.2404(7) 0.084(2) Uani 1 1 d . . . . .
H13A H 0.5312 0.0771 0.2129 0.126 Uiso 1 1 calc R U . . .
H13B H 0.5224 -0.0350 0.2114 0.126 Uiso 1 1 calc R U . . .
H13C H 0.5335 0.0216 0.3183 0.126 Uiso 1 1 calc R U . . .
C14 C 0.3617(5) 0.0291(4) 0.2069(4) 0.0494(12) Uani 1 1 d . . . . .
C15 C -0.2991(5) 0.0329(4) 0.0512(5) 0.0683(17) Uani 1 1 d . . . . .
H15A H -0.3224 0.0530 0.1123 0.102 Uiso 1 1 calc R U . . .
H15B H -0.3232 -0.0326 0.0341 0.102 Uiso 1 1 calc R U . . .
H15C H -0.3394 0.0726 -0.0104 0.102 Uiso 1 1 calc R U . . .
C16 C -0.1628(4) 0.0415(3) 0.0782(4) 0.0424(11) Uani 1 1 d . . . . .
Dy1 Dy 0.10519(2) 0.04156(2) 0.16099(2) 0.03631(9) Uani 1 1 d . . . . .
H2A H 0.147(4) 0.3315(14) 0.218(4) 0.045(13) Uiso 1 1 d D . . . .
H4A H 0.014(3) -0.142(2) 0.0999(14) 0.015(9) Uiso 1 1 d D . . . .
N1 N 0.1468(3) 0.1993(2) 0.2622(3) 0.0429(9) Uani 1 1 d . . . . .
N2 N 0.1349(4) 0.2778(3) 0.1939(3) 0.0457(9) Uani 1 1 d D . . . .
O1 O 0.1426(3) 0.0163(2) 0.3352(3) 0.0520(8) Uani 1 1 d . . . . .
O2 O 0.0583(3) 0.18331(19) 0.0499(2) 0.0463(8) Uani 1 1 d . . . . .
O3 O 0.1371(3) -0.0951(2) 0.4978(3) 0.0517(8) Uani 1 1 d . . . . .
O4 O 0.0468(4) -0.1218(2) 0.1592(3) 0.0581(9) Uani 1 1 d D . . . .
O5 O 0.3073(3) 0.1049(2) 0.1727(3) 0.0551(9) Uani 1 1 d . . . . .
O6 O 0.3018(3) -0.0455(2) 0.2142(3) 0.0520(9) Uani 1 1 d . . . . .
O7 O -0.1001(3) 0.0723(3) 0.1687(3) 0.0536(8) Uani 1 1 d . . . . .
O8 O 0.1123(3) -0.0172(2) -0.0090(3) 0.0443(7) 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
C1 O1 1.287(5) . ?
C1 C6 1.405(6) . ?
C1 C2 1.428(6) . ?
C2 O3 1.365(6) . ?
C2 C3 1.372(7) . ?
C3 C4 1.384(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.427(6) . ?
C7 N1 1.288(5) . ?
C7 H7 0.9300 . ?
C8 O2 1.253(5) . ?
C8 N2 1.301(6) . ?
C8 C9 1.485(6) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.431(5) . ?
C10 C11 1.486(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O4 1.411(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.498(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 O5 1.234(5) . ?
C14 O6 1.268(6) . ?
C15 C16 1.488(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O7 1.239(6) . ?
C16 O8 1.265(6) 3 ?
Dy1 O1 2.193(3) . ?
Dy1 O4 2.374(3) . ?
Dy1 O8 2.384(3) . ?
Dy1 O2 2.405(3) . ?
Dy1 O7 2.423(3) . ?
Dy1 O5 2.436(3) . ?
Dy1 O6 2.452(3) . ?
Dy1 N1 2.530(3) . ?
Dy1 O8 2.650(3) 3 ?
N1 N2 1.389(5) . ?
N2 H2A 0.804(10) . ?
O4 H4A 0.793(10) . ?
O8 C16 1.265(6) 3 ?
O8 Dy1 2.650(3) 3 ?

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 C1 C6 122.9(4) . . ?
O1 C1 C2 120.3(4) . . ?
C6 C1 C2 116.8(4) . . ?
O3 C2 C3 124.6(4) . . ?
O3 C2 C1 114.2(4) . . ?
C3 C2 C1 121.1(4) . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.1(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 120.7(4) . . ?
C1 C6 C7 122.2(4) . . ?
C5 C6 C7 116.9(4) . . ?
N1 C7 C6 125.5(4) . . ?
N1 C7 H7 117.3 . . ?
C6 C7 H7 117.3 . . ?
O2 C8 N2 121.1(4) . . ?
O2 C8 C9 121.5(4) . . ?
N2 C8 C9 117.4(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 C11 106.9(4) . . ?
O3 C10 H10A 110.3 . . ?
C11 C10 H10A 110.3 . . ?
O3 C10 H10B 110.3 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C12 H12A 109.5 . . ?
O4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 O6 120.6(5) . . ?
O5 C14 C13 121.2(5) . . ?
O6 C14 C13 118.3(5) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 O8 120.7(4) . 3 ?
O7 C16 C15 119.5(5) . . ?
O8 C16 C15 119.8(5) 3 . ?
O1 Dy1 O4 79.37(11) . . ?
O1 Dy1 O8 148.03(11) . . ?
O4 Dy1 O8 75.80(11) . . ?
O1 Dy1 O2 133.09(11) . . ?
O4 Dy1 O2 140.99(10) . . ?
O8 Dy1 O2 78.15(10) . . ?
O1 Dy1 O7 81.50(13) . . ?
O4 Dy1 O7 84.06(14) . . ?
O8 Dy1 O7 115.17(11) . . ?
O2 Dy1 O7 81.32(12) . . ?
O1 Dy1 O5 97.53(13) . . ?
O4 Dy1 O5 127.44(13) . . ?
O8 Dy1 O5 82.22(11) . . ?
O2 Dy1 O5 76.18(11) . . ?
O7 Dy1 O5 148.00(12) . . ?
O1 Dy1 O6 77.02(13) . . ?
O4 Dy1 O6 75.91(13) . . ?
O8 Dy1 O6 77.65(12) . . ?
O2 Dy1 O6 125.63(11) . . ?
O7 Dy1 O6 152.88(12) . . ?
O5 Dy1 O6 52.81(11) . . ?
O1 Dy1 N1 70.26(12) . . ?
O4 Dy1 N1 147.77(12) . . ?
O8 Dy1 N1 136.42(11) . . ?
O2 Dy1 N1 64.13(11) . . ?
O7 Dy1 N1 81.11(12) . . ?
O5 Dy1 N1 68.73(12) . . ?
O6 Dy1 N1 106.52(11) . . ?
O1 Dy1 O8 124.77(12) . 3 ?
O4 Dy1 O8 71.10(11) . 3 ?
O8 Dy1 O8 64.64(12) . 3 ?
O2 Dy1 O8 71.67(10) . 3 ?
O7 Dy1 O8 50.53(10) . 3 ?
O5 Dy1 O8 137.46(11) . 3 ?
O6 Dy1 O8 134.51(10) . 3 ?
N1 Dy1 O8 118.14(10) . 3 ?
C7 N1 N2 115.1(4) . . ?
C7 N1 Dy1 130.9(3) . . ?
N2 N1 Dy1 113.1(3) . . ?
C8 N2 N1 118.8(4) . . ?
C8 N2 H2A 119(3) . . ?
N1 N2 H2A 121(3) . . ?
C1 O1 Dy1 146.1(3) . . ?
C8 O2 Dy1 121.7(3) . . ?
C2 O3 C10 118.2(4) . . ?
C12 O4 Dy1 133.0(3) . . ?
C12 O4 H4A 110(3) . . ?
Dy1 O4 H4A 114(3) . . ?
C14 O5 Dy1 94.0(3) . . ?
C14 O6 Dy1 92.4(3) . . ?
C16 O7 Dy1 99.8(3) . . ?
C16 O8 Dy1 156.0(3) 3 . ?
C16 O8 Dy1 88.4(3) 3 3 ?
Dy1 O8 Dy1 115.36(12) . 3 ?

_refine_diff_density_max         1.070
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.112

