# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_AMDy2
_database_code_depnum_ccdc_archive 'CCDC 1028120'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.044 0.000 0.500 264 22 ' '
_platon_squeeze_details          
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H20 Dy N6 O9, N O3'
_chemical_formula_sum            'C23 H20 Dy N7 O12'
_chemical_formula_weight         748.96

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.073(3)
_cell_length_b                   11.659(4)
_cell_length_c                   16.832(5)
_cell_angle_alpha                85.771(5)
_cell_angle_beta                 85.202(7)
_cell_angle_gamma                86.025(6)
_cell_volume                     1571.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2678
_cell_measurement_theta_min      7.29
_cell_measurement_theta_max      29.50

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             738.0
_exptl_absorpt_coefficient_mu    2.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_T_max  0.532
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7424
_diffrn_reflns_av_R_equivalents  0.0129
_diffrn_reflns_av_sigmaI/netI    0.0024
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         27.45
_reflns_number_total             7178
_reflns_number_gt                7171
_reflns_threshold_expression     >2sigma(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+10.2881P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7178
_refine_ls_number_parameters     368
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1113
_refine_ls_wR_factor_gt          0.1113
_refine_ls_goodness_of_fit_ref   1.551
_refine_ls_restrained_S_all      1.569
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.017

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.3186(5) 0.3267(3) 0.1654(2) 0.0246(11) Uani 1 1 d GU . .
H1A H 1.3839 0.2639 0.1469 0.029 Uiso 1 1 calc R . .
C5 C 1.3319(5) 0.4350(4) 0.1259(2) 0.0556(14) Uani 1 1 d GU . .
H5 H 1.4061 0.4446 0.0809 0.067 Uiso 1 1 calc R . .
C4 C 1.2343(6) 0.5290(3) 0.1535(3) 0.0556(14) Uani 1 1 d GU . .
N1 N 1.1234(4) 0.5147(2) 0.2207(2) 0.0228(9) Uani 1 1 d GU . .
C3 C 1.1101(4) 0.4064(3) 0.26025(19) 0.0208(10) Uani 1 1 d GU . .
C2 C 1.2077(5) 0.3124(2) 0.2326(2) 0.0439(16) Uani 1 1 d GU . .
H2A H 1.1988 0.2399 0.2591 0.053 Uiso 1 1 calc R . .
Dy1 Dy 0.89852(3) 0.66915(2) 0.254787(14) 0.01722(8) Uani 1 1 d U . .
O4 O 1.2330(9) 1.0046(6) 0.0250(4) 0.0648(17) Uani 1 1 d U . .
H4A H 1.3191 0.9993 0.0480 0.097 Uiso 1 1 calc R . .
O5 O 0.7366(6) 0.4254(4) 0.5624(3) 0.0371(10) Uani 1 1 d U . .
H2 H 0.7935 0.4301 0.5198 0.056 Uiso 1 1 calc R . .
O6 O 0.9262(5) 0.8733(4) 0.2169(3) 0.0279(8) Uani 1 1 d U . .
O7 O 0.7404(5) 0.6828(4) 0.3744(3) 0.0300(9) Uani 1 1 d U . .
O1 O 0.6195(6) 0.7522(4) 0.2287(3) 0.0320(9) Uani 1 1 d U . .
O3 O 0.7478(5) 0.5074(3) 0.2066(2) 0.0245(8) Uani 1 1 d U . .
O2 O 1.1067(5) 0.7212(3) 0.3323(2) 0.0249(8) Uani 1 1 d U . .
O11 O 0.8523(5) 0.6356(4) 0.1152(3) 0.0300(9) Uani 1 1 d U . .
O12 O 0.7185(5) 0.4939(4) 0.0787(2) 0.0274(9) Uani 1 1 d U . .
N2 N 0.9231(6) 0.4961(4) 0.3513(3) 0.0195(8) Uani 1 1 d U . .
N3 N 0.8354(6) 0.5036(4) 0.4225(3) 0.0234(9) Uani 1 1 d U . .
N4 N 1.1371(5) 0.7229(4) 0.1545(3) 0.0197(8) Uani 1 1 d U . .
N5 N 1.1396(6) 0.8354(4) 0.1285(3) 0.0198(9) Uani 1 1 d U . .
H4 H 1.2133 0.8588 0.0921 0.024 Uiso 1 1 calc R . .
N6 N 0.7670(6) 0.5437(4) 0.1341(3) 0.0203(9) Uani 1 1 d U . .
C6 C 1.0045(7) 0.4015(5) 0.3348(4) 0.0269(11) Uani 1 1 d U . .
C7 C 1.2465(7) 0.6498(5) 0.1220(3) 0.0235(11) Uani 1 1 d U . .
C8 C 1.3712(8) 0.6838(6) 0.0573(4) 0.0327(13) Uani 1 1 d U . .
H8A H 1.3337 0.6676 0.0069 0.049 Uiso 1 1 calc R . .
H8B H 1.4753 0.6411 0.0652 0.049 Uiso 1 1 calc R . .
H8C H 1.3860 0.7647 0.0576 0.049 Uiso 1 1 calc R . .
C9 C 0.9992(7) 0.2935(5) 0.3880(4) 0.0261(11) Uani 1 1 d U . .
H9A H 1.0539 0.3031 0.4353 0.039 Uiso 1 1 calc R . .
H9B H 1.0550 0.2309 0.3604 0.039 Uiso 1 1 calc R . .
H9C H 0.8854 0.2769 0.4025 0.039 Uiso 1 1 calc R . .
C10 C 1.0210(7) 0.9108(5) 0.1620(3) 0.0207(10) Uani 1 1 d U . .
C11 C 1.0144(8) 1.0337(4) 0.1305(4) 0.0252(11) Uani 1 1 d U . .
C12 C 0.8915(7) 1.1071(5) 0.1671(4) 0.0276(12) Uani 1 1 d U . .
H12 H 0.8223 1.0809 0.2107 0.033 Uiso 1 1 calc R . .
C13 C 0.8763(8) 1.2229(5) 0.1353(5) 0.0388(16) Uani 1 1 d U . .
H13 H 0.7942 1.2731 0.1579 0.047 Uiso 1 1 calc R . .
C14 C 0.9803(8) 1.2631(5) 0.0713(3) 0.0273(12) Uani 1 1 d U . .
H14 H 0.9717 1.3401 0.0525 0.033 Uiso 1 1 calc R . .
C15 C 1.0916(8) 1.1904(5) 0.0379(4) 0.0273(12) Uani 1 1 d U . .
H15 H 1.1592 1.2160 -0.0064 0.033 Uiso 1 1 calc R . .
C16 C 1.1108(12) 1.0755(8) 0.0672(6) 0.058(2) Uani 1 1 d U . .
C17 C 0.7420(7) 0.6018(5) 0.4317(3) 0.0224(10) Uani 1 1 d U . .
C18 C 0.6436(7) 0.6154(5) 0.5100(3) 0.0206(10) Uani 1 1 d U . .
C19 C 0.5537(10) 0.7178(6) 0.5233(4) 0.0408(15) Uani 1 1 d U . .
H19 H 0.5506 0.7756 0.4822 0.049 Uiso 1 1 calc R . .
C20 C 0.4698(9) 0.7360(7) 0.5946(4) 0.0426(16) Uani 1 1 d U . .
H20 H 0.4160 0.8078 0.6029 0.051 Uiso 1 1 calc R . .
C21 C 0.4626(9) 0.6491(6) 0.6558(4) 0.0375(14) Uani 1 1 d U . .
H21 H 0.3977 0.6578 0.7036 0.045 Uiso 1 1 calc R . .
C22 C 0.5580(9) 0.5494(7) 0.6409(4) 0.0396(15) Uani 1 1 d U . .
H22 H 0.5625 0.4920 0.6822 0.048 Uiso 1 1 calc R . .
C23 C 0.6435(7) 0.5288(5) 0.5727(3) 0.0242(11) Uani 1 1 d U . .
O10 O 0.4398(10) 0.0374(7) 0.1910(5) 0.0745(19) Uani 1 1 d U . .
O9 O 0.5355(7) 0.1163(5) 0.0791(3) 0.0500(13) Uani 1 1 d U . .
O8 O 0.602(3) -0.0726(13) 0.1070(10) 0.254(9) Uani 1 1 d U . .
N16 N 0.526(4) 0.0210(17) 0.1271(13) 0.254(9) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C1 H1A 0.9300 . ?
C5 C4 1.3900 . ?
C5 H5 0.9300 . ?
C4 N1 1.3900 . ?
C4 C7 1.474(6) . ?
N1 C3 1.3900 . ?
N1 Dy1 2.528(3) . ?
C3 C2 1.3900 . ?
C3 C6 1.457(7) . ?
C2 H2A 0.9300 . ?
Dy1 O7 2.302(5) . ?
Dy1 O2 2.350(4) . ?
Dy1 O6 2.438(4) . ?
Dy1 O1 2.450(4) . ?
Dy1 O11 2.472(4) . ?
Dy1 N2 2.504(5) . ?
Dy1 O3 2.531(4) . ?
Dy1 N4 2.534(5) . ?
O4 C16 1.420(11) . ?
O4 H4A 0.8201 . ?
O5 C23 1.390(7) . ?
O5 H2 0.8200 . ?
O6 C10 1.225(7) . ?
O7 C17 1.299(7) . ?
O3 N6 1.263(6) . ?
O11 N6 1.318(6) . ?
O12 N6 1.237(6) . ?
N2 C6 1.280(7) . ?
N2 N3 1.345(6) . ?
N3 C17 1.337(7) . ?
N4 C7 1.299(7) . ?
N4 N5 1.353(6) . ?
N5 C10 1.368(7) . ?
N5 H4 0.8600 . ?
C6 C9 1.491(8) . ?
C7 C8 1.472(9) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.489(7) . ?
C11 C16 1.348(11) . ?
C11 C12 1.399(9) . ?
C12 C13 1.416(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.313(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.396(11) . ?
C15 H15 0.9300 . ?
C17 C18 1.494(8) . ?
C18 C19 1.376(9) . ?
C18 C23 1.406(8) . ?
C19 C20 1.352(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.392(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.376(11) . ?
C21 H21 0.9300 . ?
C22 C23 1.317(9) . ?
C22 H22 0.9300 . ?
O10 N16 1.251(19) . ?
O9 N16 1.328(18) . ?
O8 N16 1.27(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
C5 C1 C2 120.0 . . ?
C5 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C1 C5 C4 120.0 . . ?
C1 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C4 N1 120.0 . . ?
C5 C4 C7 125.6(3) . . ?
N1 C4 C7 114.1(3) . . ?
C3 N1 C4 120.0 . . ?
C3 N1 Dy1 117.50(18) . . ?
C4 N1 Dy1 121.02(18) . . ?
N1 C3 C2 120.0 . . ?
N1 C3 C6 116.2(3) . . ?
C2 C3 C6 123.4(3) . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
O7 Dy1 O2 81.56(15) . . ?
O7 Dy1 O6 99.71(15) . . ?
O2 Dy1 O6 75.74(14) . . ?
O7 Dy1 O1 70.97(15) . . ?
O2 Dy1 O1 133.83(15) . . ?
O6 Dy1 O1 73.34(15) . . ?
O7 Dy1 O11 137.31(15) . . ?
O2 Dy1 O11 140.86(14) . . ?
O6 Dy1 O11 90.03(15) . . ?
O1 Dy1 O11 72.40(14) . . ?
O7 Dy1 N2 64.74(15) . . ?
O2 Dy1 N2 78.92(14) . . ?
O6 Dy1 N2 152.05(15) . . ?
O1 Dy1 N2 118.40(15) . . ?
O11 Dy1 N2 117.33(15) . . ?
O7 Dy1 N1 126.80(14) . . ?
O2 Dy1 N1 80.37(13) . . ?
O6 Dy1 N1 123.09(13) . . ?
O1 Dy1 N1 145.71(14) . . ?
O11 Dy1 N1 77.43(14) . . ?
N2 Dy1 N1 62.84(14) . . ?
O7 Dy1 O3 96.24(14) . . ?
O2 Dy1 O3 146.94(14) . . ?
O6 Dy1 O3 136.53(14) . . ?
O1 Dy1 O3 74.23(15) . . ?
O11 Dy1 O3 52.69(14) . . ?
N2 Dy1 O3 70.57(14) . . ?
N1 Dy1 O3 74.69(13) . . ?
O7 Dy1 N4 153.39(15) . . ?
O2 Dy1 N4 75.16(14) . . ?
O6 Dy1 N4 62.37(14) . . ?
O1 Dy1 N4 117.34(15) . . ?
O11 Dy1 N4 66.00(14) . . ?
N2 Dy1 N4 121.64(14) . . ?
N1 Dy1 N4 61.83(13) . . ?
O3 Dy1 N4 110.29(14) . . ?
C16 O4 H4A 109.3 . . ?
C23 O5 H2 109.5 . . ?
C10 O6 Dy1 124.5(4) . . ?
C17 O7 Dy1 123.0(4) . . ?
N6 O3 Dy1 93.7(3) . . ?
N6 O11 Dy1 94.9(3) . . ?
C6 N2 N3 119.8(5) . . ?
C6 N2 Dy1 124.0(4) . . ?
N3 N2 Dy1 116.1(3) . . ?
C17 N3 N2 115.6(5) . . ?
C7 N4 N5 118.6(5) . . ?
C7 N4 Dy1 124.9(4) . . ?
N5 N4 Dy1 116.3(3) . . ?
N4 N5 C10 117.8(4) . . ?
N4 N5 H4 121.1 . . ?
C10 N5 H4 121.1 . . ?
O12 N6 O3 123.6(5) . . ?
O12 N6 O11 117.6(5) . . ?
O3 N6 O11 118.7(4) . . ?
N2 C6 C3 115.3(5) . . ?
N2 C6 C9 123.8(6) . . ?
C3 C6 C9 120.9(5) . . ?
N4 C7 C8 122.9(5) . . ?
N4 C7 C4 115.0(5) . . ?
C8 C7 C4 122.1(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O6 C10 N5 117.9(5) . . ?
O6 C10 C11 123.4(5) . . ?
N5 C10 C11 118.7(5) . . ?
C16 C11 C12 119.1(6) . . ?
C16 C11 C10 124.4(6) . . ?
C12 C11 C10 116.4(6) . . ?
C11 C12 C13 117.4(6) . . ?
C11 C12 H12 121.3 . . ?
C13 C12 H12 121.3 . . ?
C14 C13 C12 121.7(6) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C15 C14 C13 118.7(6) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 121.6(7) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C11 C16 C15 121.5(8) . . ?
C11 C16 O4 122.1(8) . . ?
C15 C16 O4 116.4(8) . . ?
O7 C17 N3 120.5(5) . . ?
O7 C17 C18 121.7(5) . . ?
N3 C17 C18 117.8(5) . . ?
C19 C18 C23 117.9(6) . . ?
C19 C18 C17 119.4(5) . . ?
C23 C18 C17 122.6(5) . . ?
C20 C19 C18 121.5(7) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 121.0(7) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C22 C21 C20 115.4(7) . . ?
C22 C21 H21 122.3 . . ?
C20 C21 H21 122.3 . . ?
C23 C22 C21 125.2(7) . . ?
C23 C22 H22 117.4 . . ?
C21 C22 H22 117.4 . . ?
C22 C23 O5 121.7(6) . . ?
C22 C23 C18 118.7(6) . . ?
O5 C23 C18 119.6(5) . . ?
O10 N16 O8 127.0(18) . . ?
O10 N16 O9 112.3(15) . . ?
O8 N16 O9 120.7(17) . . ?

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
C2 C1 C5 C4 0.0 . . . . ?
C1 C5 C4 N1 0.0 . . . . ?
C1 C5 C4 C7 174.1(5) . . . . ?
C5 C4 N1 C3 0.0 . . . . ?
C7 C4 N1 C3 -174.7(4) . . . . ?
C5 C4 N1 Dy1 -165.8(2) . . . . ?
C7 C4 N1 Dy1 19.5(4) . . . . ?
C4 N1 C3 C2 0.0 . . . . ?
Dy1 N1 C3 C2 166.2(2) . . . . ?
C4 N1 C3 C6 173.6(4) . . . . ?
Dy1 N1 C3 C6 -20.2(4) . . . . ?
N1 C3 C2 C1 0.0 . . . . ?
C6 C3 C2 C1 -173.1(4) . . . . ?
C5 C1 C2 C3 0.0 . . . . ?
C3 N1 Dy1 O7 28.2(3) . . . . ?
C4 N1 Dy1 O7 -165.7(2) . . . . ?
C3 N1 Dy1 O2 99.9(2) . . . . ?
C4 N1 Dy1 O2 -94.0(2) . . . . ?
C3 N1 Dy1 O6 165.8(2) . . . . ?
C4 N1 Dy1 O6 -28.1(3) . . . . ?
C3 N1 Dy1 O1 -83.8(3) . . . . ?
C4 N1 Dy1 O1 82.3(3) . . . . ?
C3 N1 Dy1 O11 -112.5(2) . . . . ?
C4 N1 Dy1 O11 53.6(2) . . . . ?
C3 N1 Dy1 N2 17.5(2) . . . . ?
C4 N1 Dy1 N2 -176.4(2) . . . . ?
C3 N1 Dy1 O3 -58.2(2) . . . . ?
C4 N1 Dy1 O3 107.9(2) . . . . ?
C3 N1 Dy1 N4 178.2(3) . . . . ?
C4 N1 Dy1 N4 -15.7(2) . . . . ?
O7 Dy1 O6 C10 169.2(4) . . . . ?
O2 Dy1 O6 C10 90.5(4) . . . . ?
O1 Dy1 O6 C10 -124.2(5) . . . . ?
O11 Dy1 O6 C10 -52.6(4) . . . . ?
N2 Dy1 O6 C10 116.1(5) . . . . ?
N1 Dy1 O6 C10 22.4(5) . . . . ?
O3 Dy1 O6 C10 -80.9(5) . . . . ?
N4 Dy1 O6 C10 10.0(4) . . . . ?
O2 Dy1 O7 C17 -80.0(4) . . . . ?
O6 Dy1 O7 C17 -153.8(4) . . . . ?
O1 Dy1 O7 C17 137.7(5) . . . . ?
O11 Dy1 O7 C17 105.4(4) . . . . ?
N2 Dy1 O7 C17 1.7(4) . . . . ?
N1 Dy1 O7 C17 -8.8(5) . . . . ?
O3 Dy1 O7 C17 66.8(4) . . . . ?
N4 Dy1 O7 C17 -109.0(5) . . . . ?
O7 Dy1 O3 N6 146.3(3) . . . . ?
O2 Dy1 O3 N6 -129.6(3) . . . . ?
O6 Dy1 O3 N6 35.1(4) . . . . ?
O1 Dy1 O3 N6 78.1(3) . . . . ?
O11 Dy1 O3 N6 -1.5(3) . . . . ?
N2 Dy1 O3 N6 -153.3(3) . . . . ?
N1 Dy1 O3 N6 -87.2(3) . . . . ?
N4 Dy1 O3 N6 -35.7(3) . . . . ?
O7 Dy1 O11 N6 -49.9(4) . . . . ?
O2 Dy1 O11 N6 138.6(3) . . . . ?
O6 Dy1 O11 N6 -154.4(3) . . . . ?
O1 Dy1 O11 N6 -81.9(3) . . . . ?
N2 Dy1 O11 N6 31.6(3) . . . . ?
N1 Dy1 O11 N6 81.6(3) . . . . ?
O3 Dy1 O11 N6 1.4(3) . . . . ?
N4 Dy1 O11 N6 146.2(3) . . . . ?
O7 Dy1 N2 C6 173.9(5) . . . . ?
O2 Dy1 N2 C6 -100.3(5) . . . . ?
O6 Dy1 N2 C6 -125.5(5) . . . . ?
O1 Dy1 N2 C6 125.6(4) . . . . ?
O11 Dy1 N2 C6 41.8(5) . . . . ?
N1 Dy1 N2 C6 -15.5(4) . . . . ?
O3 Dy1 N2 C6 66.8(4) . . . . ?
N4 Dy1 N2 C6 -35.6(5) . . . . ?
O7 Dy1 N2 N3 -1.9(3) . . . . ?
O2 Dy1 N2 N3 84.0(4) . . . . ?
O6 Dy1 N2 N3 58.7(5) . . . . ?
O1 Dy1 N2 N3 -50.2(4) . . . . ?
O11 Dy1 N2 N3 -134.0(3) . . . . ?
N1 Dy1 N2 N3 168.7(4) . . . . ?
O3 Dy1 N2 N3 -108.9(4) . . . . ?
N4 Dy1 N2 N3 148.7(3) . . . . ?
C6 N2 N3 C17 -174.0(5) . . . . ?
Dy1 N2 N3 C17 1.9(6) . . . . ?
O7 Dy1 N4 C7 127.9(5) . . . . ?
O2 Dy1 N4 C7 98.1(4) . . . . ?
O6 Dy1 N4 C7 179.5(5) . . . . ?
O1 Dy1 N4 C7 -129.9(4) . . . . ?
O11 Dy1 N4 C7 -76.9(4) . . . . ?
N2 Dy1 N4 C7 31.5(5) . . . . ?
N1 Dy1 N4 C7 11.2(4) . . . . ?
O3 Dy1 N4 C7 -47.6(5) . . . . ?
O7 Dy1 N4 N5 -58.2(5) . . . . ?
O2 Dy1 N4 N5 -87.9(4) . . . . ?
O6 Dy1 N4 N5 -6.5(3) . . . . ?
O1 Dy1 N4 N5 44.1(4) . . . . ?
O11 Dy1 N4 N5 97.0(4) . . . . ?
N2 Dy1 N4 N5 -154.5(3) . . . . ?
N1 Dy1 N4 N5 -174.8(4) . . . . ?
O3 Dy1 N4 N5 126.3(3) . . . . ?
C7 N4 N5 C10 178.5(5) . . . . ?
Dy1 N4 N5 C10 4.1(6) . . . . ?
Dy1 O3 N6 O12 178.2(4) . . . . ?
Dy1 O3 N6 O11 2.5(5) . . . . ?
Dy1 O11 N6 O12 -178.5(4) . . . . ?
Dy1 O11 N6 O3 -2.6(5) . . . . ?
N3 N2 C6 C3 -173.3(4) . . . . ?
Dy1 N2 C6 C3 11.1(7) . . . . ?
N3 N2 C6 C9 4.6(8) . . . . ?
Dy1 N2 C6 C9 -171.0(4) . . . . ?
N1 C3 C6 N2 6.6(6) . . . . ?
C2 C3 C6 N2 179.9(4) . . . . ?
N1 C3 C6 C9 -171.5(4) . . . . ?
C2 C3 C6 C9 1.9(7) . . . . ?
N5 N4 C7 C8 -1.1(8) . . . . ?
Dy1 N4 C7 C8 172.7(4) . . . . ?
N5 N4 C7 C4 -179.6(4) . . . . ?
Dy1 N4 C7 C4 -5.8(7) . . . . ?
C5 C4 C7 N4 176.8(4) . . . . ?
N1 C4 C7 N4 -8.8(6) . . . . ?
C5 C4 C7 C8 -1.8(7) . . . . ?
N1 C4 C7 C8 172.6(4) . . . . ?
Dy1 O6 C10 N5 -12.0(7) . . . . ?
Dy1 O6 C10 C11 168.6(4) . . . . ?
N4 N5 C10 O6 4.5(7) . . . . ?
N4 N5 C10 C11 -176.0(4) . . . . ?
O6 C10 C11 C16 -175.9(7) . . . . ?
N5 C10 C11 C16 4.6(9) . . . . ?
O6 C10 C11 C12 -0.3(8) . . . . ?
N5 C10 C11 C12 -179.7(5) . . . . ?
C16 C11 C12 C13 -0.4(9) . . . . ?
C10 C11 C12 C13 -176.4(5) . . . . ?
C11 C12 C13 C14 -1.1(10) . . . . ?
C12 C13 C14 C15 2.6(10) . . . . ?
C13 C14 C15 C16 -2.4(10) . . . . ?
C12 C11 C16 C15 0.6(12) . . . . ?
C10 C11 C16 C15 176.2(6) . . . . ?
C12 C11 C16 O4 -177.2(7) . . . . ?
C10 C11 C16 O4 -1.6(13) . . . . ?
C14 C15 C16 C11 0.9(13) . . . . ?
C14 C15 C16 O4 178.8(7) . . . . ?
Dy1 O7 C17 N3 -1.5(7) . . . . ?
Dy1 O7 C17 C18 177.2(4) . . . . ?
N2 N3 C17 O7 -0.5(8) . . . . ?
N2 N3 C17 C18 -179.2(5) . . . . ?
O7 C17 C18 C19 -2.4(9) . . . . ?
N3 C17 C18 C19 176.3(6) . . . . ?
O7 C17 C18 C23 179.9(5) . . . . ?
N3 C17 C18 C23 -1.3(8) . . . . ?
C23 C18 C19 C20 1.1(10) . . . . ?
C17 C18 C19 C20 -176.6(6) . . . . ?
C18 C19 C20 C21 -4.1(12) . . . . ?
C19 C20 C21 C22 5.7(11) . . . . ?
C20 C21 C22 C23 -4.8(11) . . . . ?
C21 C22 C23 O5 -179.8(6) . . . . ?
C21 C22 C23 C18 2.1(11) . . . . ?
C19 C18 C23 C22 -0.1(9) . . . . ?
C17 C18 C23 C22 177.6(6) . . . . ?
C19 C18 C23 O5 -178.2(6) . . . . ?
C17 C18 C23 O5 -0.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.944
_refine_diff_density_min         -3.177
_refine_diff_density_rms         0.175
####################################################################### 
# 
# 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_AMDy1
_database_code_depnum_ccdc_archive 'CCDC 1028133'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-01-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H27 Dy N6 O10, 2(N O3), H2 O'
_chemical_formula_sum            'C23 H29 Dy N8 O17'
_chemical_formula_weight         852.04

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   10.1352(7)
_cell_length_b                   15.3564(13)
_cell_length_c                   10.6736(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.060(3)
_cell_angle_gamma                90.00
_cell_volume                     1570.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9927
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      26.72

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             850.0
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_T_max  0.501
_exptl_absorpt_process_details   multi-scan

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22518
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         26.80
_reflns_number_total             6724
_reflns_number_gt                5064
_reflns_threshold_expression     >2sigma(I)

_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-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(7)
_refine_ls_number_reflns         6724
_refine_ls_number_parameters     252
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0411
_refine_ls_wR_factor_gt          0.0406
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_restrained_S_all      1.326
_refine_ls_shift/su_max          0.007
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy01 Dy 0.672316(12) 0.10023(3) 0.376488(11) 0.02724(5) Uani 1 1 d . . .
O2 O 0.59213(19) 0.1058(4) 0.56040(18) 0.0408(7) Uani 1 1 d . . .
H2A H 0.6488 0.0783 0.6248 0.061 Uiso 1 1 d R . .
H2B H 0.5119 0.0823 0.5400 0.061 Uiso 1 1 d R . .
N3 N 0.9615(5) 0.1387(4) 0.6280(5) 0.0358(13) Uani 1 1 d . . .
H3 H 1.0367 0.1629 0.6781 0.043 Uiso 1 1 calc R . .
O7 O 0.8366(4) 0.0183(3) 0.5495(4) 0.0341(10) Uani 1 1 d . . .
O1 O 0.7391(3) -0.0238(2) 0.2751(3) 0.0463(7) Uani 1 1 d . . .
H1A H 0.8061 -0.0099 0.2475 0.070 Uiso 1 1 d R . .
H1B H 0.6698 -0.0406 0.2099 0.070 Uiso 1 1 d R . .
N1 N 0.6354(3) 0.2631(2) 0.3939(2) 0.0282(7) Uani 1 1 d . . .
N4 N 0.4254(4) 0.1606(3) 0.2859(3) 0.0315(9) Uani 1 1 d . . .
C11 C 0.2594(5) -0.0538(4) 0.1981(4) 0.0347(13) Uani 1 1 d . . .
O3 O 0.6160(3) 0.1400(2) 0.1504(2) 0.0535(10) Uani 1 1 d . . .
H3A H 0.5279 0.1394 0.1133 0.080 Uiso 1 1 d R . .
H3B H 0.6533 0.1039 0.1117 0.080 Uiso 1 1 d R . .
N5 N 0.3248(2) 0.0984(5) 0.2347(2) 0.0365(6) Uani 1 1 d . . .
H5 H 0.2395 0.1127 0.1937 0.044 Uiso 1 1 calc R . .
N2 N 0.8553(4) 0.1876(4) 0.5489(4) 0.0311(12) Uani 1 1 d . . .
O6 O 0.4883(3) -0.0030(2) 0.3118(3) 0.0419(7) Uani 1 1 d . . .
O9 O 0.3978(3) 0.5838(5) 0.1387(3) 0.0779(18) Uani 1 1 d . . .
O10 O 0.2035(2) 0.5728(3) -0.0184(2) 0.0659(17) Uani 1 1 d . . .
C8 C 0.3945(4) 0.2414(3) 0.2711(4) 0.0341(10) Uani 1 1 d . . .
O8 O 0.2199(3) 0.5441(3) 0.1838(3) 0.0790(13) Uani 1 1 d . . .
C4 C 0.7416(3) 0.3156(3) 0.4611(3) 0.0302(9) Uani 1 1 d . . .
C10 C 0.3636(4) 0.0149(4) 0.2506(4) 0.0353(11) Uani 1 1 d . . .
N6 N 0.2743(3) 0.5669(3) 0.1024(3) 0.0457(11) Uani 1 1 d . . .
C1 C 0.4948(4) 0.3905(3) 0.3266(4) 0.0442(11) Uani 1 1 d . . .
H1 H 0.4084 0.4149 0.2813 0.053 Uiso 1 1 calc R . .
C2 C 0.6063(5) 0.4434(4) 0.3889(5) 0.0504(12) Uani 1 1 d . . .
H2 H 0.5982 0.5037 0.3830 0.060 Uiso 1 1 calc R . .
C17 C 0.9472(6) 0.0523(5) 0.6265(5) 0.0313(14) Uani 1 1 d . . .
C3 C 0.7304(4) 0.4046(3) 0.4604(4) 0.0385(10) Uani 1 1 d . . .
H3C H 0.8062 0.4385 0.5081 0.046 Uiso 1 1 calc R . .
C5 C 0.5110(3) 0.3019(3) 0.3313(3) 0.0316(9) Uani 1 1 d . . .
C6 C 0.8700(3) 0.2694(3) 0.5427(3) 0.0298(9) Uani 1 1 d . . .
C7 C 1.0004(4) 0.3200(3) 0.6076(4) 0.0473(11) Uani 1 1 d . . .
H7A H 0.9957 0.3456 0.6880 0.071 Uiso 1 1 calc R . .
H7B H 1.0098 0.3651 0.5488 0.071 Uiso 1 1 calc R . .
H7C H 1.0795 0.2817 0.6276 0.071 Uiso 1 1 calc R . .
O4 O 0.0754(3) 0.0466(2) 0.0920(3) 0.0527(8) Uani 1 1 d . . .
H4 H -0.0091 0.0492 0.0778 0.079 Uiso 1 1 calc R . .
C23 C 1.0362(4) -0.0908(3) 0.7176(4) 0.0366(10) Uani 1 1 d . . .
H23 H 0.9518 -0.1138 0.6639 0.044 Uiso 1 1 calc R . .
C19 C 1.0578(4) -0.0025(3) 0.7163(3) 0.0350(10) Uani 1 1 d . . .
C16 C 0.1190(4) -0.0363(3) 0.1200(4) 0.0428(11) Uani 1 1 d . . .
C12 C 0.3011(4) -0.1385(4) 0.2218(4) 0.0470(12) Uani 1 1 d . . .
H12 H 0.3931 -0.1500 0.2728 0.056 Uiso 1 1 calc R . .
C14 C 0.0762(5) -0.1894(4) 0.0978(4) 0.0613(15) Uani 1 1 d . . .
H14 H 0.0149 -0.2352 0.0639 0.074 Uiso 1 1 calc R . .
C15 C 0.0293(4) -0.1060(4) 0.0717(4) 0.0540(13) Uani 1 1 d . . .
H15 H -0.0633 -0.0956 0.0213 0.065 Uiso 1 1 calc R . .
C13 C 0.2127(5) -0.2077(4) 0.1734(4) 0.0590(13) Uani 1 1 d . . .
H13 H 0.2436 -0.2649 0.1909 0.071 Uiso 1 1 calc R . .
C20 C 1.1859(5) 0.0322(4) 0.7974(5) 0.0431(13) Uani 1 1 d . . .
C24 C 1.1362(4) -0.1463(3) 0.7962(4) 0.0473(11) Uani 1 1 d . . .
H24 H 1.1191 -0.2058 0.7969 0.057 Uiso 1 1 calc R . .
C21 C 1.2874(4) -0.0240(4) 0.8755(4) 0.0505(13) Uani 1 1 d . . .
H21 H 1.3727 -0.0018 0.9290 0.061 Uiso 1 1 calc R . .
O5 O 1.2071(3) 0.1185(3) 0.7934(4) 0.0751(16) Uani 1 1 d . . .
H5A H 1.2878 0.1301 0.8380 0.113 Uiso 1 1 calc R . .
C22 C 1.2623(4) -0.1120(4) 0.8740(4) 0.0506(13) Uani 1 1 d . . .
H22 H 1.3311 -0.1489 0.9261 0.061 Uiso 1 1 calc R . .
C9 C 0.2489(5) 0.2744(5) 0.1991(6) 0.061(2) Uani 1 1 d . . .
H9A H 0.2097 0.2422 0.1183 0.091 Uiso 1 1 calc R . .
H9B H 0.2529 0.3351 0.1790 0.091 Uiso 1 1 calc R . .
H9C H 0.1916 0.2668 0.2544 0.091 Uiso 1 1 calc R . .
O11 O 0.8791(2) 0.1378(2) 0.3158(2) 0.0422(8) Uani 1 1 d . . .
N10 N 1.0059(4) 0.1178(5) 0.3566(4) 0.057(2) Uani 1 1 d . . .
O13 O 0.6069(3) 0.7157(3) 0.0357(3) 0.0762(11) Uani 1 1 d . . .
O17 O 0.6550(4) 0.7993(3) 0.2088(3) 0.0790(12) Uani 1 1 d . . .
N9 N 0.6214(4) 0.7905(3) 0.0867(4) 0.0557(11) Uani 1 1 d . . .
O19 O 1.0408(6) 0.0426(4) 0.3717(6) 0.099(2) Uani 1 1 d . . .
O18 O 0.6044(5) 0.8544(4) 0.0162(4) 0.1078(15) Uani 1 1 d . . .
O15 O 0.3684(3) 0.1919(4) 0.5723(4) 0.0948(17) Uani 1 1 d G . .
H15A H 0.3636 0.1935 0.6503 0.142 Uiso 1 1 d G . .
H15B H 0.2877 0.1820 0.5173 0.142 Uiso 1 1 d G . .
O20 O 1.0927(4) 0.1774(4) 0.3818(5) 0.0998(19) 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
Dy01 O2 2.3587(19) . ?
Dy01 O6 2.373(3) . ?
Dy01 O3 2.372(2) . ?
Dy01 O1 2.396(3) . ?
Dy01 O7 2.400(4) . ?
Dy01 O11 2.456(2) . ?
Dy01 N2 2.529(5) . ?
Dy01 N4 2.545(4) . ?
Dy01 N1 2.544(3) . ?
O2 H2A 0.8504 . ?
O2 H2B 0.8504 . ?
N3 C17 1.334(5) . ?
N3 N2 1.358(6) . ?
N3 H3 0.8600 . ?
O7 C17 1.266(7) . ?
O1 H1A 0.8511 . ?
O1 H1B 0.8511 . ?
N1 C4 1.349(5) . ?
N1 C5 1.357(4) . ?
N4 C8 1.277(6) . ?
N4 N5 1.374(6) . ?
C11 C12 1.366(8) . ?
C11 C16 1.420(6) . ?
C11 C10 1.469(7) . ?
O3 H3A 0.8500 . ?
O3 H3B 0.8499 . ?
N5 C10 1.335(8) . ?
N5 H5 0.8600 . ?
N2 C6 1.269(7) . ?
O6 C10 1.249(5) . ?
O9 N6 1.211(4) . ?
O10 N6 1.258(4) . ?
C8 C5 1.474(6) . ?
C8 C9 1.511(6) . ?
O8 N6 1.222(4) . ?
C4 C3 1.370(6) . ?
C4 C6 1.489(5) . ?
C1 C2 1.374(6) . ?
C1 C5 1.371(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(6) . ?
C2 H2 0.9300 . ?
C17 C19 1.477(7) . ?
C3 H3C 0.9300 . ?
C6 C7 1.494(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
O4 C16 1.349(6) . ?
O4 H4 0.8200 . ?
C23 C24 1.379(5) . ?
C23 C19 1.375(6) . ?
C23 H23 0.9300 . ?
C19 C20 1.409(6) . ?
C16 C15 1.389(6) . ?
C12 C13 1.378(6) . ?
C12 H12 0.9300 . ?
C14 C15 1.364(8) . ?
C14 C13 1.383(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C13 H13 0.9300 . ?
C20 O5 1.347(7) . ?
C20 C21 1.392(6) . ?
C24 C22 1.381(6) . ?
C24 H24 0.9300 . ?
C21 C22 1.375(7) . ?
C21 H21 0.9300 . ?
O5 H5A 0.8200 . ?
C22 H22 0.9300 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
O11 N10 1.253(4) . ?
N10 O19 1.203(9) . ?
N10 O20 1.237(8) . ?
O13 N9 1.259(6) . ?
O17 N9 1.243(5) . ?
N9 O18 1.214(6) . ?
O15 H15A 0.8500 . ?
O15 H15B 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy01 O6 79.34(12) . . ?
O2 Dy01 O3 143.50(10) . . ?
O6 Dy01 O3 88.32(10) . . ?
O2 Dy01 O1 129.06(16) . . ?
O6 Dy01 O1 69.41(10) . . ?
O3 Dy01 O1 75.78(10) . . ?
O2 Dy01 O7 73.73(13) . . ?
O6 Dy01 O7 98.95(12) . . ?
O3 Dy01 O7 142.57(11) . . ?
O1 Dy01 O7 72.73(12) . . ?
O2 Dy01 O11 140.05(9) . . ?
O6 Dy01 O11 137.54(10) . . ?
O3 Dy01 O11 67.26(8) . . ?
O1 Dy01 O11 71.11(10) . . ?
O7 Dy01 O11 83.62(11) . . ?
O2 Dy01 N2 75.23(13) . . ?
O6 Dy01 N2 152.42(12) . . ?
O3 Dy01 N2 118.65(14) . . ?
O1 Dy01 N2 120.16(12) . . ?
O7 Dy01 N2 63.81(9) . . ?
O11 Dy01 N2 65.24(11) . . ?
O2 Dy01 N4 74.89(10) . . ?
O6 Dy01 N4 63.31(13) . . ?
O3 Dy01 N4 68.89(10) . . ?
O1 Dy01 N4 120.41(11) . . ?
O7 Dy01 N4 146.35(12) . . ?
O11 Dy01 N4 129.21(10) . . ?
N2 Dy01 N4 118.65(14) . . ?
O2 Dy01 N1 78.73(15) . . ?
O6 Dy01 N1 123.91(10) . . ?
O3 Dy01 N1 80.16(10) . . ?
O1 Dy01 N1 152.21(9) . . ?
O7 Dy01 N1 122.73(11) . . ?
O11 Dy01 N1 86.94(9) . . ?
N2 Dy01 N1 61.03(13) . . ?
N4 Dy01 N1 61.32(10) . . ?
Dy01 O2 H2A 109.3 . . ?
Dy01 O2 H2B 109.4 . . ?
H2A O2 H2B 109.5 . . ?
C17 N3 N2 118.8(6) . . ?
C17 N3 H3 120.6 . . ?
N2 N3 H3 120.6 . . ?
C17 O7 Dy01 121.9(4) . . ?
Dy01 O1 H1A 109.3 . . ?
Dy01 O1 H1B 109.3 . . ?
H1A O1 H1B 109.4 . . ?
C4 N1 C5 116.8(3) . . ?
C4 N1 Dy01 121.1(2) . . ?
C5 N1 Dy01 122.0(2) . . ?
C8 N4 N5 120.4(4) . . ?
C8 N4 Dy01 124.9(3) . . ?
N5 N4 Dy01 114.1(3) . . ?
C12 C11 C16 118.6(5) . . ?
C12 C11 C10 118.2(4) . . ?
C16 C11 C10 123.1(5) . . ?
Dy01 O3 H3A 109.7 . . ?
Dy01 O3 H3B 109.2 . . ?
H3A O3 H3B 109.5 . . ?
C10 N5 N4 117.8(3) . . ?
C10 N5 H5 121.1 . . ?
N4 N5 H5 121.1 . . ?
C6 N2 N3 119.8(4) . . ?
C6 N2 Dy01 123.9(3) . . ?
N3 N2 Dy01 113.8(4) . . ?
C10 O6 Dy01 124.7(3) . . ?
N4 C8 C5 115.4(4) . . ?
N4 C8 C9 123.2(5) . . ?
C5 C8 C9 121.4(5) . . ?
N1 C4 C3 122.9(3) . . ?
N1 C4 C6 114.8(4) . . ?
C3 C4 C6 122.2(4) . . ?
O6 C10 N5 119.0(4) . . ?
O6 C10 C11 121.3(5) . . ?
N5 C10 C11 119.7(4) . . ?
O9 N6 O8 119.6(3) . . ?
O9 N6 O10 119.7(3) . . ?
O8 N6 O10 120.7(3) . . ?
C2 C1 C5 120.0(4) . . ?
C2 C1 H1 120.0 . . ?
C5 C1 H1 120.0 . . ?
C3 C2 C1 118.1(5) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
O7 C17 N3 119.2(6) . . ?
O7 C17 C19 120.7(6) . . ?
N3 C17 C19 120.1(6) . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3C 120.2 . . ?
C4 C3 H3C 120.2 . . ?
N1 C5 C1 122.3(4) . . ?
N1 C5 C8 114.9(4) . . ?
C1 C5 C8 122.7(3) . . ?
N2 C6 C4 114.0(3) . . ?
N2 C6 C7 126.3(4) . . ?
C4 C6 C7 119.7(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C16 O4 H4 109.5 . . ?
C24 C23 C19 121.9(4) . . ?
C24 C23 H23 119.1 . . ?
C19 C23 H23 119.1 . . ?
C23 C19 C20 119.0(4) . . ?
C23 C19 C17 118.6(4) . . ?
C20 C19 C17 122.4(5) . . ?
O4 C16 C15 121.1(4) . . ?
O4 C16 C11 120.1(4) . . ?
C15 C16 C11 118.8(5) . . ?
C13 C12 C11 122.7(5) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C15 C14 C13 121.7(5) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C14 C15 C16 120.4(4) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C12 C13 C14 117.8(5) . . ?
C12 C13 H13 121.1 . . ?
C14 C13 H13 121.1 . . ?
O5 C20 C19 118.5(5) . . ?
O5 C20 C21 122.3(5) . . ?
C19 C20 C21 119.1(5) . . ?
C23 C24 C22 118.8(5) . . ?
C23 C24 H24 120.6 . . ?
C22 C24 H24 120.6 . . ?
C22 C21 C20 120.2(4) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C20 O5 H5A 109.5 . . ?
C21 C22 C24 121.0(4) . . ?
C21 C22 H22 119.5 . . ?
C24 C22 H22 119.5 . . ?
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 . . ?
N10 O11 Dy01 135.8(3) . . ?
O19 N10 O20 121.6(5) . . ?
O19 N10 O11 120.4(6) . . ?
O20 N10 O11 118.0(6) . . ?
O18 N9 O17 119.8(5) . . ?
O18 N9 O13 119.8(5) . . ?
O17 N9 O13 120.3(5) . . ?
H15A O15 H15B 109.5 . . ?

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
O2 Dy01 O7 C17 -94.6(4) . . . . ?
O6 Dy01 O7 C17 -170.6(4) . . . . ?
O3 Dy01 O7 C17 90.3(4) . . . . ?
O1 Dy01 O7 C17 124.3(4) . . . . ?
O11 Dy01 O7 C17 52.1(4) . . . . ?
N2 Dy01 O7 C17 -13.4(3) . . . . ?
N4 Dy01 O7 C17 -116.4(4) . . . . ?
N1 Dy01 O7 C17 -30.0(4) . . . . ?
O2 Dy01 N1 C4 94.7(2) . . . . ?
O6 Dy01 N1 C4 163.5(2) . . . . ?
O3 Dy01 N1 C4 -115.3(2) . . . . ?
O1 Dy01 N1 C4 -85.0(3) . . . . ?
O7 Dy01 N1 C4 32.6(3) . . . . ?
O11 Dy01 N1 C4 -47.8(2) . . . . ?
N2 Dy01 N1 C4 15.4(2) . . . . ?
N4 Dy01 N1 C4 173.5(3) . . . . ?
O2 Dy01 N1 C5 -88.6(2) . . . . ?
O6 Dy01 N1 C5 -19.8(3) . . . . ?
O3 Dy01 N1 C5 61.4(2) . . . . ?
O1 Dy01 N1 C5 91.7(3) . . . . ?
O7 Dy01 N1 C5 -150.7(2) . . . . ?
O11 Dy01 N1 C5 128.9(2) . . . . ?
N2 Dy01 N1 C5 -167.9(3) . . . . ?
N4 Dy01 N1 C5 -9.8(2) . . . . ?
O2 Dy01 N4 C8 95.8(3) . . . . ?
O6 Dy01 N4 C8 -178.7(4) . . . . ?
O3 Dy01 N4 C8 -79.6(3) . . . . ?
O1 Dy01 N4 C8 -137.5(3) . . . . ?
O7 Dy01 N4 C8 117.4(4) . . . . ?
O11 Dy01 N4 C8 -47.8(4) . . . . ?
N2 Dy01 N4 C8 32.4(4) . . . . ?
N1 Dy01 N4 C8 10.5(3) . . . . ?
O2 Dy01 N4 N5 -93.3(3) . . . . ?
O6 Dy01 N4 N5 -7.80(19) . . . . ?
O3 Dy01 N4 N5 91.3(2) . . . . ?
O1 Dy01 N4 N5 33.5(3) . . . . ?
O7 Dy01 N4 N5 -71.6(3) . . . . ?
O11 Dy01 N4 N5 123.2(2) . . . . ?
N2 Dy01 N4 N5 -156.6(2) . . . . ?
N1 Dy01 N4 N5 -178.5(3) . . . . ?
C8 N4 N5 C10 178.5(4) . . . . ?
Dy01 N4 N5 C10 7.1(3) . . . . ?
C17 N3 N2 C6 -175.7(5) . . . . ?
C17 N3 N2 Dy01 -13.0(7) . . . . ?
O2 Dy01 N2 C6 -106.5(4) . . . . ?
O6 Dy01 N2 C6 -129.9(3) . . . . ?
O3 Dy01 N2 C6 36.9(4) . . . . ?
O1 Dy01 N2 C6 126.6(3) . . . . ?
O7 Dy01 N2 C6 174.6(5) . . . . ?
O11 Dy01 N2 C6 79.4(4) . . . . ?
N4 Dy01 N2 C6 -43.3(4) . . . . ?
N1 Dy01 N2 C6 -21.4(3) . . . . ?
O2 Dy01 N2 N3 91.6(4) . . . . ?
O6 Dy01 N2 N3 68.2(5) . . . . ?
O3 Dy01 N2 N3 -125.0(3) . . . . ?
O1 Dy01 N2 N3 -35.3(4) . . . . ?
O7 Dy01 N2 N3 12.7(3) . . . . ?
O11 Dy01 N2 N3 -82.5(3) . . . . ?
N4 Dy01 N2 N3 154.8(3) . . . . ?
N1 Dy01 N2 N3 176.7(4) . . . . ?
O2 Dy01 O6 C10 87.7(3) . . . . ?
O3 Dy01 O6 C10 -57.8(3) . . . . ?
O1 Dy01 O6 C10 -133.2(3) . . . . ?
O7 Dy01 O6 C10 159.1(3) . . . . ?
O11 Dy01 O6 C10 -110.5(3) . . . . ?
N2 Dy01 O6 C10 110.7(4) . . . . ?
N4 Dy01 O6 C10 9.4(3) . . . . ?
N1 Dy01 O6 C10 19.2(3) . . . . ?
N5 N4 C8 C5 179.6(3) . . . . ?
Dy01 N4 C8 C5 -10.0(5) . . . . ?
N5 N4 C8 C9 0.5(6) . . . . ?
Dy01 N4 C8 C9 170.9(4) . . . . ?
C5 N1 C4 C3 -4.5(5) . . . . ?
Dy01 N1 C4 C3 172.4(3) . . . . ?
C5 N1 C4 C6 172.2(3) . . . . ?
Dy01 N1 C4 C6 -10.9(4) . . . . ?
Dy01 O6 C10 N5 -9.5(5) . . . . ?
Dy01 O6 C10 C11 171.5(3) . . . . ?
N4 N5 C10 O6 0.6(5) . . . . ?
N4 N5 C10 C11 179.7(4) . . . . ?
C12 C11 C10 O6 2.3(6) . . . . ?
C16 C11 C10 O6 -175.4(4) . . . . ?
C12 C11 C10 N5 -176.8(4) . . . . ?
C16 C11 C10 N5 5.6(6) . . . . ?
C5 C1 C2 C3 -3.2(6) . . . . ?
Dy01 O7 C17 N3 12.3(8) . . . . ?
Dy01 O7 C17 C19 -169.3(3) . . . . ?
N2 N3 C17 O7 1.6(10) . . . . ?
N2 N3 C17 C19 -176.9(3) . . . . ?
C1 C2 C3 C4 3.8(6) . . . . ?
N1 C4 C3 C2 0.1(6) . . . . ?
C6 C4 C3 C2 -176.3(3) . . . . ?
C4 N1 C5 C1 5.1(5) . . . . ?
Dy01 N1 C5 C1 -171.8(3) . . . . ?
C4 N1 C5 C8 -173.8(3) . . . . ?
Dy01 N1 C5 C8 9.3(4) . . . . ?
C2 C1 C5 N1 -1.3(6) . . . . ?
C2 C1 C5 C8 177.5(4) . . . . ?
N4 C8 C5 N1 0.2(5) . . . . ?
C9 C8 C5 N1 179.3(4) . . . . ?
N4 C8 C5 C1 -178.7(4) . . . . ?
C9 C8 C5 C1 0.4(6) . . . . ?
N3 N2 C6 C4 -175.2(4) . . . . ?
Dy01 N2 C6 C4 23.9(5) . . . . ?
N3 N2 C6 C7 5.0(7) . . . . ?
Dy01 N2 C6 C7 -155.8(3) . . . . ?
N1 C4 C6 N2 -7.6(5) . . . . ?
C3 C4 C6 N2 169.0(4) . . . . ?
N1 C4 C6 C7 172.1(3) . . . . ?
C3 C4 C6 C7 -11.2(5) . . . . ?
C24 C23 C19 C20 0.2(6) . . . . ?
C24 C23 C19 C17 178.3(4) . . . . ?
O7 C17 C19 C23 -2.1(7) . . . . ?
N3 C17 C19 C23 176.4(5) . . . . ?
O7 C17 C19 C20 176.0(5) . . . . ?
N3 C17 C19 C20 -5.6(8) . . . . ?
C12 C11 C16 O4 -178.4(4) . . . . ?
C10 C11 C16 O4 -0.8(6) . . . . ?
C12 C11 C16 C15 0.6(6) . . . . ?
C10 C11 C16 C15 178.2(4) . . . . ?
C16 C11 C12 C13 -0.1(7) . . . . ?
C10 C11 C12 C13 -177.9(4) . . . . ?
C13 C14 C15 C16 0.7(7) . . . . ?
O4 C16 C15 C14 178.1(4) . . . . ?
C11 C16 C15 C14 -0.8(6) . . . . ?
C11 C12 C13 C14 0.0(7) . . . . ?
C15 C14 C13 C12 -0.2(7) . . . . ?
C23 C19 C20 O5 178.7(5) . . . . ?
C17 C19 C20 O5 0.6(7) . . . . ?
C23 C19 C20 C21 0.6(6) . . . . ?
C17 C19 C20 C21 -177.4(4) . . . . ?
C19 C23 C24 C22 -1.1(6) . . . . ?
O5 C20 C21 C22 -178.5(5) . . . . ?
C19 C20 C21 C22 -0.5(7) . . . . ?
C20 C21 C22 C24 -0.5(7) . . . . ?
C23 C24 C22 C21 1.2(6) . . . . ?
O2 Dy01 O11 N10 58.0(6) . . . . ?
O6 Dy01 O11 N10 -93.4(5) . . . . ?
O3 Dy01 O11 N10 -153.0(5) . . . . ?
O1 Dy01 O11 N10 -71.0(5) . . . . ?
O7 Dy01 O11 N10 2.9(5) . . . . ?
N2 Dy01 O11 N10 67.0(5) . . . . ?
N4 Dy01 O11 N10 174.7(5) . . . . ?
N1 Dy01 O11 N10 126.4(5) . . . . ?
Dy01 O11 N10 O19 50.3(8) . . . . ?
Dy01 O11 N10 O20 -129.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.80
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.064
