# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_xstr0165
_database_code_depnum_ccdc_archive 'CCDC 992713'
_audit_update_record             
;
2015-01-24 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;
_audit_creation_date             2015-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_chemical_name_common            ?
_chemical_name_systematic        '[Zn(dcbpy)(DMF)]'
_chemical_formula_moiety         'C15 H13 N3 O5 Zn, C3 H7 N O'
_chemical_formula_sum            'C18 H20 N4 O6 Zn'
_chemical_formula_weight         453.75
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   9.3725(2)
_cell_length_b                   14.7643(3)
_cell_length_c                   14.7153(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.058(2)
_cell_angle_gamma                90
_cell_volume                     1998.47(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.089
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_preparation       
"Solvothermal synthesis, zinc nitrate hexahydrate, 2,2'-bipyridine-4,4'-dicarboxylic acid, DMF"
_exptl_crystal_recrystallization_method 'from reaction mixture'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.001
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14313
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        51.439
_diffrn_reflns_theta_max         51.439
_diffrn_reflns_theta_min         4.282
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1824
_reflns_number_total             2158
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00010(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2158
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0488P)²+3.1283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0950
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C16(H16)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18A(H18A,H18B,
 H18C), C18B(H18D,H18E,H18F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.01743(5) 0.10873(3) 0.22316(3) 0.0189(3) Uani 1 1 d . . . . .
O1 O 0.1515(3) 0.13661(18) 0.34495(17) 0.0239(7) Uani 1 1 d . . . . .
O2 O 0.2035(3) 0.25974(19) 0.26981(19) 0.0327(7) Uani 1 1 d . . . . .
O3 O 0.0818(3) 0.00248(17) 0.74799(18) 0.0247(7) Uani 1 1 d . . . . .
O4 O 0.1573(3) 0.02713(18) 0.8993(2) 0.0318(7) Uani 1 1 d . . . . .
O5 O 0.1860(3) 0.04976(17) 0.16786(18) 0.0245(7) Uani 1 1 d . . . . .
N1 N 0.4376(3) 0.3265(2) 0.5966(2) 0.0187(8) Uani 1 1 d . . . . .
N2 N 0.3724(3) 0.2880(2) 0.7589(2) 0.0203(8) Uani 1 1 d . . . . .
C1 C 0.2099(4) 0.2139(3) 0.3405(3) 0.0229(10) Uani 1 1 d . . . . .
C2 C 0.2939(4) 0.2513(2) 0.4309(3) 0.0209(9) Uani 1 1 d . . . . .
C3 C 0.3937(4) 0.3204(3) 0.4316(3) 0.0246(10) Uani 1 1 d . . . . .
H3 H 0.4141 0.3432 0.3751 0.030 Uiso 1 1 calc R . . . .
C4 C 0.4636(4) 0.3561(3) 0.5153(3) 0.0228(10) Uani 1 1 d . . . . .
H4 H 0.5325 0.4033 0.5151 0.027 Uiso 1 1 calc R . . . .
C5 C 0.2672(4) 0.2203(3) 0.5153(3) 0.0213(10) Uani 1 1 d . . . . .
H5 H 0.1992 0.1729 0.5170 0.026 Uiso 1 1 calc R . . . .
C6 C 0.3405(4) 0.2590(2) 0.5972(3) 0.0176(9) Uani 1 1 d . . . . .
C7 C 0.3141(4) 0.2320(2) 0.6897(2) 0.0175(9) Uani 1 1 d . . . . .
C8 C 0.2377(4) 0.1543(2) 0.7053(3) 0.0200(9) Uani 1 1 d . . . . .
H8 H 0.1977 0.1156 0.6553 0.024 Uiso 1 1 calc R . . . .
C9 C 0.2206(4) 0.1339(2) 0.7948(3) 0.0204(10) Uani 1 1 d . . . . .
C10 C 0.2798(4) 0.1934(3) 0.8656(3) 0.0248(10) Uani 1 1 d . . . . .
H10 H 0.2690 0.1821 0.9275 0.030 Uiso 1 1 calc R . . . .
C11 C 0.3539(4) 0.2685(3) 0.8450(3) 0.0242(10) Uani 1 1 d . . . . .
H11 H 0.3939 0.3085 0.8939 0.029 Uiso 1 1 calc R . . . .
C12 C 0.1475(4) 0.0479(3) 0.8177(3) 0.0219(10) Uani 1 1 d . . . . .
C13 C 0.3011(6) 0.0896(3) 0.1688(4) 0.0399(13) Uani 1 1 d . . . . .
C15 C 0.4125(6) -0.0360(3) 0.1084(4) 0.0624(17) Uani 1 1 d . . . . .
H15A H 0.4074 -0.0802 0.1574 0.094 Uiso 1 1 calc GR . . A .
H15B H 0.4999 -0.0472 0.0827 0.094 Uiso 1 1 calc GR . . A .
H15C H 0.3262 -0.0419 0.0593 0.094 Uiso 1 1 calc GR . . A .
C14 C 0.5538(7) 0.1056(4) 0.1550(7) 0.121(4) Uani 1 1 d . . . . .
H14A H 0.5350 0.1699 0.1642 0.182 Uiso 1 1 calc GR . . B .
H14B H 0.5929 0.0982 0.0982 0.182 Uiso 1 1 calc GR . . B .
H14C H 0.6244 0.0829 0.2079 0.182 Uiso 1 1 calc GR . . B .
N3 N 0.4185(4) 0.0548(3) 0.1467(3) 0.0482(11) Uani 1 1 d . . . C 2
O6 O 0.0578(5) 0.8163(5) 0.4394(3) 0.132(3) Uani 1 1 d . . . . .
N4 N 0.2451(8) 0.9097(3) 0.4314(3) 0.0802(19) Uani 1 1 d . . . . .
C16 C 0.1526(7) 0.8462(7) 0.4035(4) 0.095(3) Uani 1 1 d . . . . .
H16 H 0.1606 0.8190 0.3461 0.114 Uiso 1 1 calc R . . . .
C17 C 0.3572(8) 0.9378(5) 0.3780(6) 0.100(3) Uani 1 1 d . . . . .
H17A H 0.4533 0.9184 0.4109 0.150 Uiso 1 1 calc GR . . . .
H17B H 0.3558 1.0039 0.3714 0.150 Uiso 1 1 calc GR . . . .
H17C H 0.3364 0.9097 0.3166 0.150 Uiso 1 1 calc GR . . . .
C18A C 0.124(2) 0.9601(9) 0.4873(10) 0.059(7) Uani 0.366(15) 1 d . . P D 1
H18A H 0.0980 1.0198 0.4599 0.089 Uiso 0.366(15) 1 calc GR . P D 1
H18B H 0.1679 0.9673 0.5529 0.089 Uiso 0.366(15) 1 calc GR . P D 1
H18C H 0.0368 0.9225 0.4813 0.089 Uiso 0.366(15) 1 calc GR . P D 1
C18B C 0.2887(18) 0.9519(8) 0.5211(7) 0.108(6) Uani 0.634(15) 1 d . . P D 2
H18D H 0.2025 0.9633 0.5480 0.161 Uiso 0.634(15) 1 calc GR . P D 2
H18E H 0.3379 1.0093 0.5141 0.161 Uiso 0.634(15) 1 calc GR . P D 2
H18F H 0.3552 0.9115 0.5619 0.161 Uiso 0.634(15) 1 calc GR . P D 2
H13 H 0.316(5) 0.149(3) 0.187(3) 0.043(14) Uiso 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
Zn1 O1 2.024(2) . ?
Zn1 O3 1.973(3) 3_556 ?
Zn1 O5 2.100(3) . ?
Zn1 N1 2.099(3) 4_565 ?
Zn1 N2 2.173(3) 4_565 ?
O1 C1 1.272(5) . ?
O2 C1 1.233(5) . ?
O3 Zn1 1.973(3) 3_556 ?
O3 C12 1.281(5) . ?
O4 C12 1.225(5) . ?
O5 C13 1.226(5) . ?
N1 Zn1 2.099(3) 4_666 ?
N1 C4 1.339(5) . ?
N1 C6 1.351(5) . ?
N2 Zn1 2.173(3) 4_666 ?
N2 C7 1.344(5) . ?
N2 C11 1.343(5) . ?
C1 C2 1.514(5) . ?
C2 C3 1.383(5) . ?
C2 C5 1.391(5) . ?
C3 C4 1.384(5) . ?
C5 C6 1.391(5) . ?
C6 C7 1.483(5) . ?
C7 C8 1.395(5) . ?
C8 C9 1.390(5) . ?
C9 C10 1.394(5) . ?
C9 C12 1.512(5) . ?
C10 C11 1.373(5) . ?
C13 N3 1.310(6) . ?
C15 N3 1.452(6) . ?
C14 N3 1.458(6) . ?
O6 C16 1.202(7) . ?
N4 C16 1.290(9) . ?
N4 C17 1.486(9) . ?
N4 C18A 1.694(16) . ?
N4 C18B 1.445(11) . ?

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 Zn1 O5 92.41(10) . . ?
O1 Zn1 N1 138.41(11) . 4_565 ?
O1 Zn1 N2 87.36(11) . 4_565 ?
O3 Zn1 O1 102.53(11) 3_556 . ?
O3 Zn1 O5 99.14(10) 3_556 . ?
O3 Zn1 N1 117.87(11) 3_556 4_565 ?
O3 Zn1 N2 100.92(11) 3_556 4_565 ?
O5 Zn1 N2 159.50(11) . 4_565 ?
N1 Zn1 O5 90.66(11) 4_565 . ?
N1 Zn1 N2 76.25(12) 4_565 4_565 ?
C1 O1 Zn1 109.7(2) . . ?
C12 O3 Zn1 115.9(2) . 3_556 ?
C13 O5 Zn1 121.5(3) . . ?
C4 N1 Zn1 123.3(3) . 4_666 ?
C4 N1 C6 119.0(3) . . ?
C6 N1 Zn1 117.1(2) . 4_666 ?
C7 N2 Zn1 115.5(2) . 4_666 ?
C11 N2 Zn1 125.3(2) . 4_666 ?
C11 N2 C7 118.5(3) . . ?
O1 C1 C2 116.0(4) . . ?
O2 C1 O1 125.8(4) . . ?
O2 C1 C2 118.2(4) . . ?
C3 C2 C1 120.9(4) . . ?
C3 C2 C5 118.2(4) . . ?
C5 C2 C1 120.8(3) . . ?
C2 C3 C4 119.5(4) . . ?
N1 C4 C3 122.3(4) . . ?
C6 C5 C2 119.7(4) . . ?
N1 C6 C5 121.2(3) . . ?
N1 C6 C7 115.8(3) . . ?
C5 C6 C7 122.9(3) . . ?
N2 C7 C6 114.5(3) . . ?
N2 C7 C8 121.9(3) . . ?
C8 C7 C6 123.6(3) . . ?
C9 C8 C7 119.3(4) . . ?
C8 C9 C10 118.1(4) . . ?
C8 C9 C12 122.2(4) . . ?
C10 C9 C12 119.7(4) . . ?
C11 C10 C9 119.3(4) . . ?
N2 C11 C10 122.9(4) . . ?
O3 C12 C9 115.5(4) . . ?
O4 C12 O3 126.0(4) . . ?
O4 C12 C9 118.5(4) . . ?
O5 C13 N3 126.0(4) . . ?
C13 N3 C15 119.1(4) . . ?
C13 N3 C14 122.5(4) . . ?
C15 N3 C14 118.4(4) . . ?
C16 N4 C17 122.3(5) . . ?
C16 N4 C18A 90.2(8) . . ?
C16 N4 C18B 131.2(8) . . ?
C17 N4 C18A 137.7(7) . . ?
C18B N4 C17 105.0(8) . . ?
O6 C16 N4 129.4(7) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_original_sample_id MJ.3B
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_xstr0263
_database_code_depnum_ccdc_archive 'CCDC 1026241'
_audit_update_record             
;
2014-10-21 deposited with the CCDC.
2015-02-17 downloaded from the CCDC.
;
_audit_creation_date             2014-10-20
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        Dy(DCBPY)(DMF)2(NO2)(H2O)
_chemical_formula_moiety         'C18 H20 Dy N5 O9'
_chemical_formula_sum            'C18 H20 Dy N5 O9'
_chemical_formula_weight         612.89
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H20 N20 O16 Dy2'
_chemical_oxdiff_usercomment     3dy_3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2414(5)
_cell_length_b                   10.3040(5)
_cell_length_c                   12.8291(6)
_cell_angle_alpha                76.388(4)
_cell_angle_beta                 69.431(4)
_cell_angle_gamma                86.377(4)
_cell_volume                     1111.37(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    149.90(15)
_cell_measurement_theta_max      74.2680
_cell_measurement_theta_min      4.3960
_exptl_absorpt_coefficient_mu    18.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'pinkish colourless'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             602
_exptl_crystal_preparation       
"solvoethermal synthesis. Dysprosium nitrate pentahydrate , 2,2'-bipyridine-4,4'-dicarboxylic acid, DMF"
_exptl_crystal_recrystallization_method 'From reaction mixture'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16503
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.895
_diffrn_reflns_theta_min         4.416
_diffrn_ambient_temperature      149.90(15)
_diffrn_detector_area_resol_mean 5.2031
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.8812
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000    0.0000 37

#__ type_ start__ end____ width___ exp.time_
  2 omega  -59.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000   60.0000 86

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00   27.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   61.0000 -180.0000 91

#__ type_ start__ end____ width___ exp.time_
  4 omega  -84.00   -4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000 -120.0000 80

#__ type_ start__ end____ width___ exp.time_
  5 omega   15.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000   30.0000 100

#__ type_ start__ end____ width___ exp.time_
  6 omega   23.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   38.0000 -180.0000 90

#__ type_ start__ end____ width___ exp.time_
  7 omega   14.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  -90.0000 100

#__ type_ start__ end____ width___ exp.time_
  8 omega   14.00   52.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  150.0000 38

#__ type_ start__ end____ width___ exp.time_
  9 omega   74.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   18.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000   90.0000 51

#__ type_ start__ end____ width___ exp.time_
 11 omega   55.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 12 omega   16.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000 -150.0000 61

#__ type_ start__ end____ width___ exp.time_
 13 omega   15.00   58.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0390   77.0000  -30.0000 43

#__ type_ start__ end____ width___ exp.time_
 14 omega   83.00  109.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -94.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   78.00  178.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000 -180.0000 100

#__ type_ start__ end____ width___ exp.time_
 16 omega   81.00  175.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
 17 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
 18 omega  138.00  176.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000    0.0000 38

#__ type_ start__ end____ width___ exp.time_
 19 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 20 omega   82.00  173.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  150.0000 91

#__ type_ start__ end____ width___ exp.time_
 21 omega   77.00  103.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 22 omega   44.00  121.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940 -125.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
 23 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  120.0000 27

#__ type_ start__ end____ width___ exp.time_
 24 omega   77.00  165.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
 25 omega  123.00  168.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   90.0000 45

#__ type_ start__ end____ width___ exp.time_
 26 omega   81.00  140.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -120.0000 59

#__ type_ start__ end____ width___ exp.time_
 27 omega   82.00  134.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000   30.0000 52

#__ type_ start__ end____ width___ exp.time_
 28 omega   33.00   60.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -94.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega   82.00  156.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  120.0000 74

#__ type_ start__ end____ width___ exp.time_
 30 omega   81.00  137.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  -60.0000 56

#__ type_ start__ end____ width___ exp.time_
 31 omega   79.00  105.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 32 omega   81.00  107.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 33 omega   81.00  107.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 34 omega  125.00  152.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 35 omega   77.00  104.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 36 omega   78.00  105.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
 37 omega   77.00  103.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 38 omega   81.00  107.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 39 omega   84.00  111.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   61.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 40 omega   79.00  176.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000 -120.0000 97

#__ type_ start__ end____ width___ exp.time_
 41 omega   36.00  136.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -77.0000  -30.0000 100

#__ type_ start__ end____ width___ exp.time_
 42 omega   78.00  163.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940   77.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
 43 omega   37.00  135.00   1.0000    1.4200
omega____ theta____ kappa____ phi______ frames
    -      107.1940  -77.0000 -180.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1389665000
_diffrn_orient_matrix_UB_12      0.0987776000
_diffrn_orient_matrix_UB_13      -0.0548622000
_diffrn_orient_matrix_UB_21      -0.0623812000
_diffrn_orient_matrix_UB_22      0.0643304000
_diffrn_orient_matrix_UB_23      -0.0965586000
_diffrn_orient_matrix_UB_31      -0.0922766000
_diffrn_orient_matrix_UB_32      0.0988915000
_diffrn_orient_matrix_UB_33      0.0708545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4086
_reflns_number_total             4464
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max         2.707
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0577
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0938P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1526
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C7(H7), C15(H15), C17(H17), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC), C1E(H1EA,H1EB,
 H1EC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.45968(3) 0.25111(3) -0.00233(2) 0.02040(15) Uani 1 1 d . . . . .
O5 O 0.5397(5) 0.1356(5) -0.1454(4) 0.0282(9) Uani 1 1 d . . . . .
O3 O 0.5885(5) 0.5512(4) 0.1141(3) 0.0245(9) Uani 1 1 d . . . . .
O1 O 0.3371(6) 0.0580(5) 0.1244(4) 0.0345(11) Uani 1 1 d . . . . .
O4 O 0.6988(5) 0.3511(5) -0.1257(5) 0.0381(11) Uani 1 1 d . . . . .
N4 N 0.1003(8) -0.1460(7) 0.5426(5) 0.0465(17) Uani 1 1 d . . . . .
N3 N 0.3732(7) 0.3570(6) 0.5355(4) 0.0303(12) Uani 1 1 d . . . . .
C1 C 0.5075(7) 0.4476(6) 0.1684(5) 0.0249(12) Uani 1 1 d . . . . .
C3 C 0.0667(7) -0.0410(7) 0.4730(5) 0.0284(13) Uani 1 1 d . . . . .
C4 C 0.1509(7) -0.0047(6) 0.3559(5) 0.0232(12) Uani 1 1 d . . . . .
H4 H 0.1263 0.0731 0.3091 0.028 Uiso 1 1 calc R U . . .
N1 N 0.9398(7) 0.4394(7) -0.2075(6) 0.0462(17) Uani 1 1 d . . . . .
C5 C 0.4707(6) 0.4606(6) 0.4696(5) 0.0217(12) Uani 1 1 d . . . . .
C6 C 0.2198(11) -0.2196(10) 0.4971(7) 0.059(3) Uani 1 1 d . . . . .
H6 H 0.2459 -0.2939 0.5465 0.070 Uiso 1 1 calc R U . . .
O9 O 0.6376(7) 0.1435(6) 0.0759(6) 0.0584(18) Uani 1 1 d . . . . .
C8 C 0.5145(6) 0.4933(6) 0.3511(5) 0.0215(12) Uani 1 1 d . . . . .
H8 H 0.5803 0.5686 0.3072 0.026 Uiso 1 1 calc R U . . .
C7 C 0.8162(8) 0.3948(7) -0.1191(7) 0.0353(16) Uani 1 1 d . . . . .
H7 H 0.8166 0.3960 -0.0454 0.042 Uiso 1 1 calc R U . . .
N2 N 0.7640(8) 0.0203(6) 0.1847(6) 0.0394(14) Uani 1 1 d . . . . .
C12 C 0.4607(7) 0.4145(6) 0.2979(5) 0.0240(12) Uani 1 1 d . . . . .
C13 C 0.3632(7) -0.0519(6) 0.1836(5) 0.0215(12) Uani 1 1 d . . . . .
C14 C 0.2716(7) -0.0853(6) 0.3096(5) 0.0246(12) Uani 1 1 d . . . . .
C15 C 0.3594(9) 0.3086(7) 0.3648(6) 0.0350(16) Uani 1 1 d . . . . .
H15 H 0.3188 0.2535 0.3313 0.042 Uiso 1 1 calc R U . . .
C17 C 0.3198(9) 0.2863(7) 0.4830(6) 0.0368(17) Uani 1 1 d . . . . .
H17 H 0.2491 0.2150 0.5292 0.044 Uiso 1 1 calc R U . . .
C18 C 0.7340(8) 0.0608(7) 0.0905(7) 0.0354(16) Uani 1 1 d . . . . .
H18 H 0.7917 0.0230 0.0279 0.042 Uiso 1 1 calc R U . . .
C19 C 0.3090(10) -0.1930(8) 0.3801(6) 0.046(2) Uani 1 1 d . . . . .
H19 H 0.3927 -0.2481 0.3509 0.055 Uiso 1 1 calc R U . . .
C20 C 0.8855(12) -0.0742(10) 0.1951(9) 0.061(3) Uani 1 1 d . . . . .
H20A H 0.8410 -0.1510 0.2585 0.092 Uiso 1 1 calc R U . . .
H20B H 0.9650 -0.0304 0.2098 0.092 Uiso 1 1 calc R U . . .
H20C H 0.9320 -0.1047 0.1239 0.092 Uiso 1 1 calc R U . . .
C1C C 1.0730(10) 0.4897(10) -0.1924(11) 0.072(3) Uani 1 1 d . . . . .
H1CA H 1.0850 0.5862 -0.2245 0.109 Uiso 1 1 calc R U . . .
H1CB H 1.1662 0.4452 -0.2317 0.109 Uiso 1 1 calc R U . . .
H1CC H 1.0576 0.4715 -0.1106 0.109 Uiso 1 1 calc R U . . .
C1D C 0.6852(17) 0.0750(16) 0.2814(10) 0.099(5) Uani 1 1 d . . . . .
H1DA H 0.6405 0.0024 0.3487 0.149 Uiso 1 1 calc R U . . .
H1DB H 0.6025 0.1325 0.2668 0.149 Uiso 1 1 calc R U . . .
H1DC H 0.7583 0.1278 0.2953 0.149 Uiso 1 1 calc R U . . .
C1E C 0.9452(13) 0.4434(15) -0.3199(9) 0.091(4) Uani 1 1 d . . . . .
H1EA H 0.8594 0.3894 -0.3165 0.136 Uiso 1 1 calc R U . . .
H1EB H 1.0435 0.4075 -0.3620 0.136 Uiso 1 1 calc R U . . .
H1EC H 0.9365 0.5359 -0.3589 0.136 Uiso 1 1 calc R U . . .
O6 O 0.2255(6) 0.2180(5) -0.0413(5) 0.0417(12) Uani 1 1 d . . . . .
O8 O 0.1872(6) 0.3025(5) 0.1027(5) 0.0409(12) Uani 1 1 d . . . . .
N5 N 0.1313(7) 0.2581(7) 0.0429(7) 0.0464(17) Uani 1 1 d . . . . .
O7 O -0.0105(7) 0.2533(8) 0.0625(9) 0.087(3) Uani 1 1 d . . . . .
O2 O 0.4620(6) 0.3668(5) 0.1274(4) 0.0371(11) Uiso 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
Dy1 O5 2.301(4) . ?
Dy1 O3 2.316(4) 2_665 ?
Dy1 O1 2.314(4) . ?
Dy1 O4 2.348(5) . ?
Dy1 O9 2.312(5) . ?
Dy1 O6 2.446(5) . ?
Dy1 O8 2.494(5) . ?
Dy1 N5 2.882(6) . ?
Dy1 O2 2.270(5) . ?
O5 C13 1.257(8) 2_655 ?
O3 Dy1 2.316(4) 2_665 ?
O3 C1 1.253(7) . ?
O1 C13 1.267(8) . ?
O4 C7 1.237(8) . ?
N4 C3 1.327(9) . ?
N4 C6 1.336(10) . ?
N3 C5 1.351(8) . ?
N3 C17 1.318(9) . ?
C1 C12 1.520(8) . ?
C1 O2 1.247(8) . ?
C3 C3 1.503(13) 2_556 ?
C3 C4 1.397(8) . ?
C4 C14 1.391(9) . ?
N1 C7 1.309(10) . ?
N1 C1C 1.456(11) . ?
N1 C1E 1.415(14) . ?
C5 C5 1.487(12) 2_666 ?
C5 C8 1.390(8) . ?
C6 C19 1.404(10) . ?
O9 C18 1.226(9) . ?
C8 C12 1.386(8) . ?
N2 C18 1.301(9) . ?
N2 C20 1.461(11) . ?
N2 C1D 1.425(12) . ?
C12 C15 1.388(9) . ?
C13 O5 1.257(8) 2_655 ?
C13 C14 1.504(8) . ?
C14 C19 1.366(10) . ?
C15 C17 1.395(9) . ?
O6 N5 1.264(9) . ?
O8 N5 1.240(9) . ?
N5 O7 1.247(8) . ?

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
O5 Dy1 O3 95.99(16) . 2_665 ?
O5 Dy1 O1 88.99(17) . . ?
O5 Dy1 O4 75.44(17) . . ?
O5 Dy1 O9 90.9(2) . . ?
O5 Dy1 O6 75.37(18) . . ?
O5 Dy1 O8 126.12(18) . . ?
O5 Dy1 N5 100.9(2) . . ?
O3 Dy1 O4 72.14(17) 2_665 . ?
O3 Dy1 O6 71.89(16) 2_665 . ?
O3 Dy1 O8 75.43(16) 2_665 . ?
O3 Dy1 N5 72.88(16) 2_665 . ?
O1 Dy1 O3 141.67(16) . 2_665 ?
O1 Dy1 O4 145.00(18) . . ?
O1 Dy1 O6 72.74(18) . . ?
O1 Dy1 O8 71.13(17) . . ?
O1 Dy1 N5 68.86(18) . . ?
O4 Dy1 O6 130.24(19) . . ?
O4 Dy1 O8 142.85(17) . . ?
O4 Dy1 N5 144.17(19) . . ?
O9 Dy1 O3 143.73(18) . 2_665 ?
O9 Dy1 O1 73.8(2) . . ?
O9 Dy1 O4 75.3(2) . . ?
O9 Dy1 O6 143.87(19) . . ?
O9 Dy1 O8 127.1(2) . . ?
O9 Dy1 N5 140.4(2) . . ?
O6 Dy1 O8 51.16(19) . . ?
O6 Dy1 N5 25.8(2) . . ?
O8 Dy1 N5 25.4(2) . . ?
O2 Dy1 O5 161.92(19) . . ?
O2 Dy1 O3 88.64(17) . 2_665 ?
O2 Dy1 O1 98.21(18) . . ?
O2 Dy1 O4 89.49(18) . . ?
O2 Dy1 O9 75.4(2) . . ?
O2 Dy1 O6 122.58(19) . . ?
O2 Dy1 O8 71.96(19) . . ?
O2 Dy1 N5 97.2(2) . . ?
C13 O5 Dy1 142.2(4) 2_655 . ?
C1 O3 Dy1 132.1(4) . 2_665 ?
C13 O1 Dy1 142.0(4) . . ?
C7 O4 Dy1 138.5(6) . . ?
C3 N4 C6 117.7(6) . . ?
C17 N3 C5 117.3(5) . . ?
O3 C1 C12 117.3(5) . . ?
O3 C1 O2 126.8(6) . . ?
O2 C1 C12 115.8(5) . . ?
N4 C3 C3 116.4(7) . 2_556 ?
N4 C3 C4 122.9(6) . . ?
C4 C3 C3 120.6(7) . 2_556 ?
C14 C4 C3 118.4(6) . . ?
C7 N1 C1C 120.5(8) . . ?
C7 N1 C1E 120.9(8) . . ?
C1E N1 C1C 118.6(8) . . ?
N3 C5 C5 116.6(6) . 2_666 ?
N3 C5 C8 122.4(5) . . ?
C8 C5 C5 121.1(6) . 2_666 ?
N4 C6 C19 123.6(7) . . ?
C18 O9 Dy1 157.6(6) . . ?
C5 C8 C12 119.0(5) . . ?
O4 C7 N1 123.9(8) . . ?
C18 N2 C20 122.9(7) . . ?
C18 N2 C1D 120.5(8) . . ?
C1D N2 C20 116.5(8) . . ?
C8 C12 C1 120.1(5) . . ?
C15 C12 C1 120.8(5) . . ?
C15 C12 C8 119.1(6) . . ?
O5 C13 C14 117.1(5) 2_655 . ?
O1 C13 O5 125.2(5) . 2_655 ?
O1 C13 C14 117.7(5) . . ?
C4 C14 C13 120.3(5) . . ?
C19 C14 C4 119.4(6) . . ?
C19 C14 C13 120.2(6) . . ?
C12 C15 C17 117.3(6) . . ?
N3 C17 C15 124.8(6) . . ?
O9 C18 N2 125.5(8) . . ?
C14 C19 C6 117.9(7) . . ?
N5 O6 Dy1 96.7(4) . . ?
N5 O8 Dy1 95.1(4) . . ?
O6 N5 Dy1 57.4(3) . . ?
O8 N5 Dy1 59.5(3) . . ?
O8 N5 O6 116.9(5) . . ?
O7 N5 Dy1 176.3(7) . . ?
O7 N5 O6 120.4(9) . . ?
O7 N5 O8 122.7(9) . . ?
C1 O2 Dy1 158.6(4) . . ?

_olex2_exptl_crystal_mounting_method 'Nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
