# 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_p131202h
_database_code_depnum_ccdc_archive 'CCDC 1008252'
_audit_update_record             
;
2015-02-04 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_audit_creation_date             2014-06-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C18 H13 Dy N4 O9'
_chemical_formula_sum            'C18 H13 Dy N4 O9'
_chemical_formula_weight         591.82
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1O1N1DY1
_chemical_oxdiff_usercomment     DYLS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_H-M_alt        'P 65'
_space_group_name_Hall           'P 65'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'x-y, x, z+5/6'
3 '-y, x-y, z+2/3'
4 '-x, -y, z+1/2'
5 '-x+y, -x, z+1/3'
6 'y, -x+y, z+1/6'

_cell_length_a                   11.1993(9)
_cell_length_b                   11.1993(9)
_cell_length_c                   26.5836(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2887.5(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    3023
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      28.1630
_cell_measurement_theta_min      3.6320
_exptl_absorpt_coefficient_mu    3.945
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            5649
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.64
_diffrn_ambient_temperature      128(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   34.00   59.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   41.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   77.0000  150.0000 89
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0703118000
_diffrn_orient_matrix_UB_12      0.0245644000
_diffrn_orient_matrix_UB_13      0.0057828000
_diffrn_orient_matrix_UB_21      -0.0125871000
_diffrn_orient_matrix_UB_22      -0.0687615000
_diffrn_orient_matrix_UB_23      0.0000594000
_diffrn_orient_matrix_UB_31      0.0153921000
_diffrn_orient_matrix_UB_32      0.0051526000
_diffrn_orient_matrix_UB_33      -0.0260384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2104
_reflns_number_total             2241
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(15)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2241
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0282
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0130P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0550
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C9(H9), C15(H15), N2(H2), C17(H17), C13(H13), C11(H11),
 C5(H5), C16(H16), C3(H3), C10(H10), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Dy1 Dy 0.97387(4) 0.14509(4) 0.06279(3) 0.01115(10) Uani 1 1 d . . . .
O2 O 0.7126(6) -0.1512(6) -0.0319(2) 0.0176(14) Uani 1 1 d . . . .
C4 C 0.4845(10) -0.3132(10) 0.1241(4) 0.028(2) Uani 1 1 d . . . .
H4 H 0.4645 -0.2988 0.1567 0.034 Uiso 1 1 calc . . R .
O5 O 1.1829(6) 0.2170(6) 0.0980(2) 0.0167(15) Uani 1 1 d . . . .
O6 O 1.2931(6) 0.1856(6) 0.1619(2) 0.0187(15) Uani 1 1 d . . . .
O7 O 0.8676(6) 0.2865(6) 0.0447(2) 0.0216(15) Uani 1 1 d . . . .
O3 O 0.9116(6) -0.0676(6) 0.1048(2) 0.0184(15) Uani 1 1 d . . . .
C8 C 0.8555(9) -0.2507(8) 0.1621(3) 0.0138(19) Uani 1 1 d . . . .
O1 O 0.7623(6) 0.0018(6) 0.0284(2) 0.0164(15) Uani 1 1 d . . . .
O8 O 1.0554(6) 0.3872(6) 0.0881(2) 0.0184(14) Uani 1 1 d . . . .
O9 O 0.9400(7) 0.4937(6) 0.0732(3) 0.0368(19) Uani 1 1 d . . . .
C7 C 0.8499(8) -0.2846(8) 0.2127(3) 0.019(2) Uani 1 1 d . . . .
H7 H 0.8955 -0.2145 0.2362 0.023 Uiso 1 1 calc . . R .
O4 O 1.0172(6) -0.0184(6) 0.1792(2) 0.0194(15) Uani 1 1 d . . . .
C9 C 0.7871(9) -0.3558(9) 0.1282(3) 0.022(2) Uani 1 1 d . . . .
H9 H 0.7858 -0.3367 0.0942 0.026 Uiso 1 1 calc . . R .
C15 C 1.4627(9) 0.1433(9) 0.0968(3) 0.019(2) Uani 1 1 d . . . .
H15 H 1.4684 0.1280 0.1308 0.023 Uiso 1 1 calc . . R .
N2 N 0.7809(7) -0.4149(7) 0.2285(3) 0.0269(18) Uani 1 1 d . . . .
H2 H 0.7768 -0.4332 0.2601 0.032 Uiso 1 1 calc . . R .
C17 C 1.5349(10) 0.1472(9) 0.0126(4) 0.027(2) Uani 1 1 d . . . .
H17 H 1.5897 0.1344 -0.0106 0.032 Uiso 1 1 calc . . R .
N3 N 1.4453(7) 0.1849(8) -0.0031(3) 0.0196(18) Uani 1 1 d . . . .
C13 C 1.3637(9) 0.2045(9) 0.0291(3) 0.018(2) Uani 1 1 d . . . .
H13 H 1.3037 0.2328 0.0172 0.022 Uiso 1 1 calc . . R .
C18 C 1.2735(9) 0.1951(8) 0.1165(3) 0.015(2) Uani 1 1 d . . . .
C11 C 0.7179(10) -0.5177(10) 0.1949(3) 0.029(2) Uani 1 1 d . . . .
H11 H 0.6722 -0.6086 0.2060 0.035 Uiso 1 1 calc . . R .
C2 C 0.6037(9) -0.2317(9) 0.0458(3) 0.018(2) Uani 1 1 d . . . .
C6 C 0.6994(9) -0.1189(9) 0.0121(3) 0.015(2) Uani 1 1 d . . . U
C14 C 1.3698(9) 0.1821(9) 0.0804(3) 0.014(2) Uani 1 1 d . . . .
C5 C 0.4221(10) -0.4448(10) 0.1035(4) 0.031(3) Uani 1 1 d . . . .
H5 H 0.3576 -0.5172 0.1231 0.037 Uiso 1 1 calc . . R .
C12 C 0.9324(9) -0.1017(9) 0.1473(4) 0.018(2) Uani 1 1 d . . . .
C16 C 1.5465(8) 0.1273(8) 0.0632(4) 0.021(2) Uani 1 1 d . . . .
H16 H 1.6103 0.1032 0.0744 0.025 Uiso 1 1 calc . . R .
N4 N 0.9536(8) 0.3929(8) 0.0687(3) 0.0267(19) Uani 1 1 d . . . .
N1 N 0.4480(8) -0.4746(7) 0.0580(3) 0.037(2) Uani 1 1 d . . . .
C3 C 0.5767(9) -0.2047(10) 0.0948(3) 0.024(2) Uani 1 1 d . . . .
H3 H 0.6204 -0.1151 0.1072 0.028 Uiso 1 1 calc . . R .
C10 C 0.7200(10) -0.4907(9) 0.1452(4) 0.027(2) Uani 1 1 d . . . U
H10 H 0.6762 -0.5629 0.1224 0.032 Uiso 1 1 calc . . R .
C1 C 0.5391(9) -0.3654(9) 0.0313(3) 0.026(2) Uani 1 1 d . . . .
H1 H 0.5604 -0.3834 -0.0006 0.031 Uiso 1 1 calc . . R .


_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 O2 2.344(6) 6_665 ?
Dy1 O5 2.262(6) . ?
Dy1 O6 2.395(6) 2_544 ?
Dy1 O7 2.458(6) . ?
Dy1 O3 2.398(6) . ?
Dy1 O1 2.285(6) . ?
Dy1 O8 2.483(6) . ?
Dy1 O4 2.303(6) 2_544 ?
Dy1 N4 2.900(8) . ?
O2 Dy1 2.344(6) 2_544 ?
O2 C6 1.255(9) . ?
C4 C5 1.389(13) . ?
C4 C3 1.376(12) . ?
O5 C18 1.257(10) . ?
O6 Dy1 2.395(6) 6_665 ?
O6 C18 1.241(9) . ?
O7 N4 1.267(9) . ?
O3 C12 1.250(11) . ?
C8 C7 1.391(11) . ?
C8 C9 1.373(11) . ?
C8 C12 1.498(11) . ?
O1 C6 1.248(10) . ?
O8 N4 1.283(9) . ?
O9 N4 1.218(9) . ?
C7 N2 1.332(10) . ?
O4 Dy1 2.303(6) 6_665 ?
O4 C12 1.267(10) . ?
C9 C10 1.384(11) . ?
C15 C14 1.384(12) . ?
C15 C16 1.369(11) . ?
N2 C11 1.344(11) . ?
C17 N3 1.336(11) . ?
C17 C16 1.380(13) . ?
N3 C13 1.348(11) . ?
C13 C14 1.395(11) . ?
C18 C14 1.502(11) . ?
C11 C10 1.353(12) . ?
C2 C6 1.481(11) . ?
C2 C3 1.404(11) . ?
C2 C1 1.353(12) . ?
C5 N1 1.325(12) . ?
N1 C1 1.338(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
O2 Dy1 O6 142.68(19) 6_665 2_544 ?
O2 Dy1 O7 73.49(19) 6_665 . ?
O2 Dy1 O3 72.94(19) 6_665 . ?
O2 Dy1 O8 73.17(19) 6_665 . ?
O2 Dy1 N4 70.5(2) 6_665 . ?
O5 Dy1 O2 99.6(2) . 6_665 ?
O5 Dy1 O6 83.5(2) . 2_544 ?
O5 Dy1 O7 126.9(2) . . ?
O5 Dy1 O3 84.0(2) . . ?
O5 Dy1 O1 160.1(2) . . ?
O5 Dy1 O8 75.5(2) . . ?
O5 Dy1 O4 83.3(2) . 2_544 ?
O5 Dy1 N4 101.5(2) . . ?
O6 Dy1 O7 75.13(19) 2_544 . ?
O6 Dy1 O3 143.9(2) 2_544 . ?
O6 Dy1 O8 71.71(19) 2_544 . ?
O6 Dy1 N4 72.5(2) 2_544 . ?
O7 Dy1 O8 51.80(17) . . ?
O7 Dy1 N4 25.7(2) . . ?
O3 Dy1 O7 137.5(2) . . ?
O3 Dy1 O8 136.40(19) . . ?
O3 Dy1 N4 143.4(2) . . ?
O1 Dy1 O2 84.8(2) . 6_665 ?
O1 Dy1 O6 104.8(2) . 2_544 ?
O1 Dy1 O7 73.0(2) . . ?
O1 Dy1 O3 78.7(2) . . ?
O1 Dy1 O8 124.2(2) . . ?
O1 Dy1 O4 81.9(2) . 2_544 ?
O1 Dy1 N4 98.3(2) . . ?
O8 Dy1 N4 26.13(18) . . ?
O4 Dy1 O2 143.7(2) 2_544 6_665 ?
O4 Dy1 O6 73.6(2) 2_544 2_544 ?
O4 Dy1 O7 132.80(19) 2_544 . ?
O4 Dy1 O3 71.41(17) 2_544 . ?
O4 Dy1 O8 140.9(2) 2_544 . ?
O4 Dy1 N4 144.9(2) 2_544 . ?
C6 O2 Dy1 134.4(6) . 2_544 ?
C3 C4 C5 118.2(9) . . ?
C18 O5 Dy1 152.2(6) . . ?
C18 O6 Dy1 126.1(6) . 6_665 ?
N4 O7 Dy1 97.0(5) . . ?
C12 O3 Dy1 135.9(6) . . ?
C7 C8 C12 118.8(8) . . ?
C9 C8 C7 118.1(8) . . ?
C9 C8 C12 123.1(8) . . ?
C6 O1 Dy1 136.4(6) . . ?
N4 O8 Dy1 95.4(5) . . ?
N2 C7 C8 121.7(8) . . ?
C12 O4 Dy1 163.5(6) . 6_665 ?
C8 C9 C10 119.1(8) . . ?
C16 C15 C14 120.6(8) . . ?
C7 N2 C11 119.9(8) . . ?
N3 C17 C16 120.2(8) . . ?
C17 N3 C13 122.0(8) . . ?
N3 C13 C14 119.6(8) . . ?
O5 C18 C14 117.2(8) . . ?
O6 C18 O5 126.3(8) . . ?
O6 C18 C14 116.5(8) . . ?
N2 C11 C10 120.9(9) . . ?
C3 C2 C6 121.3(8) . . ?
C1 C2 C6 122.1(8) . . ?
C1 C2 C3 116.7(8) . . ?
O2 C6 C2 117.2(8) . . ?
O1 C6 O2 123.4(8) . . ?
O1 C6 C2 119.4(7) . . ?
C15 C14 C13 118.4(8) . . ?
C15 C14 C18 121.3(8) . . ?
C13 C14 C18 120.3(8) . . ?
N1 C5 C4 124.7(9) . . ?
O3 C12 C8 119.1(8) . . ?
O3 C12 O4 124.4(8) . . ?
O4 C12 C8 116.5(8) . . ?
C15 C16 C17 119.2(9) . . ?
O7 N4 Dy1 57.3(4) . . ?
O7 N4 O8 115.6(7) . . ?
O8 N4 Dy1 58.5(4) . . ?
O9 N4 Dy1 176.5(7) . . ?
O9 N4 O7 122.2(8) . . ?
O9 N4 O8 122.1(8) . . ?
C5 N1 C1 114.6(8) . . ?
C4 C3 C2 118.8(9) . . ?
C11 C10 C9 120.2(9) . . ?
N1 C1 C2 127.0(9) . . ?

####################################################################### 
# 
# 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_p131202g
_database_code_depnum_ccdc_archive 'CCDC 1008253'
_audit_update_record             
;
2015-02-04 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_audit_creation_date             2014-06-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C18 H13 Dy N4 O9'
_chemical_formula_sum            'C18 H13 Dy N4 O9'
_chemical_formula_weight         591.82
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1H1O1N1DY1
_chemical_oxdiff_usercomment     DYLS
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_H-M_alt        'P 61'
_space_group_name_Hall           'P 61'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'x-y, x, z+1/6'
3 '-y, x-y, z+1/3'
4 '-x, -y, z+1/2'
5 '-x+y, -x, z+2/3'
6 'y, -x+y, z+5/6'

_cell_length_a                   11.2159(8)
_cell_length_b                   11.2159(8)
_cell_length_c                   26.5973(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2897.6(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    2490
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      28.7700
_cell_measurement_theta_min      3.6350
_exptl_absorpt_coefficient_mu    3.931
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40912
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.035
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            5641
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.63
_diffrn_ambient_temperature      128(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   35.00   61.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  178.0000   30.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   40.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8185   77.0000  120.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0385597000
_diffrn_orient_matrix_UB_12      0.0721290000
_diffrn_orient_matrix_UB_13      0.0040814000
_diffrn_orient_matrix_UB_21      0.0620771000
_diffrn_orient_matrix_UB_22      -0.0014568000
_diffrn_orient_matrix_UB_23      -0.0033126000
_diffrn_orient_matrix_UB_31      -0.0018517000
_diffrn_orient_matrix_UB_32      0.0113385000
_diffrn_orient_matrix_UB_33      -0.0261137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2135
_reflns_number_total             2249
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(18)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         2249
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0369P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0770
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C8) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C16(H16), C8(H8), C3(H3), C15(H15), C17(H17), C5(H5), C13(H13),
 C9(H9), C2(H2), C11(H11), C7(H7), C1(H1a)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Dy1 Dy 0.97373(4) 0.82860(4) 0.37322(3) 0.00969(13) Uani 1 1 d . . . .
O4 O 1.0020(6) 0.7615(7) 0.5054(3) 0.0170(17) Uani 1 1 d . . . .
O6 O 0.9653(7) 0.7841(7) 0.2416(3) 0.0134(16) Uani 1 1 d . . . .
O5 O 1.1074(7) 0.8140(7) 0.3057(3) 0.0181(17) Uani 1 1 d . . . .
O8 O 1.0549(7) 0.6682(7) 0.3985(3) 0.0200(17) Uani 1 1 d . . . .
O3 O 0.8470(8) 0.7117(7) 0.4450(3) 0.0192(17) Uani 1 1 d . . . .
N1 N 0.7814(9) 1.1968(9) 0.5395(4) 0.027(2) Uani 1 1 d . . . .
H1 H 0.7804 1.2144 0.5709 0.033 Uiso 1 1 calc . . R .
O2 O 1.0178(7) 1.0364(7) 0.4894(3) 0.0169(17) Uani 1 1 d . . . U
O1 O 0.9129(7) 0.9798(7) 0.4149(3) 0.0180(17) Uani 1 1 d . . . .
O7 O 0.8668(7) 0.5812(7) 0.3553(3) 0.0210(18) Uani 1 1 d . . . .
C14 C 1.1855(10) 0.8168(10) 0.2245(4) 0.009(2) Uani 1 1 d . . . U
N4 N 0.9539(9) 0.5613(9) 0.3794(4) 0.020(2) Uani 1 1 d . . . .
C16 C 1.4197(10) 0.8739(10) 0.2065(4) 0.020(2) Uani 1 1 d . . . .
H16 H 1.5080 0.8997 0.2176 0.024 Uiso 1 1 calc . . R .
C10 C 0.7688(10) 0.6040(11) 0.5231(4) 0.017(3) Uani 1 1 d . . . U
O9 O 0.9394(8) 0.4463(7) 0.3837(3) 0.032(2) Uani 1 1 d . . . .
N3 N 1.2601(9) 0.8138(8) 0.1402(3) 0.020(2) Uani 1 1 d . . . .
C8 C 0.6870(11) 0.4850(11) 0.6014(4) 0.020(3) Uani 1 1 d . . . U
H8 H 0.7019 0.4649 0.6339 0.024 Uiso 1 1 calc . . R .
C3 C 0.7874(11) 1.1421(10) 0.4385(4) 0.020(2) Uani 1 1 d . . . U
H3 H 0.7871 1.1226 0.4046 0.024 Uiso 1 1 calc . . R .
C15 C 1.3187(10) 0.8568(10) 0.2399(4) 0.019(3) Uani 1 1 d . . . U
H15 H 1.3403 0.8726 0.2739 0.022 Uiso 1 1 calc . . R .
C17 C 1.3867(12) 0.8518(11) 0.1568(4) 0.024(3) Uani 1 1 d . . . .
H17 H 1.4542 0.8635 0.1338 0.029 Uiso 1 1 calc . . R .
C4 C 0.8559(10) 1.1050(11) 0.4733(4) 0.017(2) Uani 1 1 d . . . .
N2 N 0.5256(9) 0.4473(9) 0.5352(4) 0.034(2) Uani 1 1 d . . . .
C5 C 0.8487(10) 1.1345(10) 0.5235(4) 0.016(2) Uani 1 1 d . . . .
H5 H 0.8933 1.1094 0.5471 0.019 Uiso 1 1 calc . . R .
C18 C 1.0790(10) 0.8037(10) 0.2610(4) 0.016(2) Uani 1 1 d . . . .
C12 C 0.8811(10) 0.7007(9) 0.4890(4) 0.012(2) Uani 1 1 d . . . .
C6 C 0.9339(9) 1.0336(9) 0.4581(4) 0.010(2) Uani 1 1 d . . . .
C13 C 1.1606(12) 0.7973(11) 0.1733(4) 0.019(2) Uani 1 1 d . . . .
H13 H 1.0734 0.7723 0.1612 0.023 Uiso 1 1 calc . . R .
C9 C 0.7953(11) 0.5780(10) 0.5720(4) 0.019(2) Uani 1 1 d . . . .
H9 H 0.8846 0.6227 0.5846 0.023 Uiso 1 1 calc . . R .
C2 C 0.7194(12) 1.2088(12) 0.4558(5) 0.029(3) Uani 1 1 d . . . .
H2 H 0.6766 1.2380 0.4330 0.035 Uiso 1 1 calc . . R .
C11 C 0.6352(11) 0.5377(11) 0.5084(4) 0.022(3) Uani 1 1 d . . . .
H11 H 0.6175 0.5570 0.4761 0.027 Uiso 1 1 calc . . R .
C7 C 0.5555(12) 0.4225(12) 0.5811(5) 0.031(3) Uani 1 1 d . . . .
H7 H 0.4833 0.3590 0.6010 0.037 Uiso 1 1 calc . . R .
C1 C 0.7146(12) 1.2320(12) 0.5054(4) 0.027(3) Uani 1 1 d . . . .
H1A H 0.6645 1.2728 0.5163 0.032 Uiso 1 1 calc . . R .


_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 O4 2.295(7) 6_564 ?
Dy1 O6 2.252(7) 2_655 ?
Dy1 O5 2.397(7) . ?
Dy1 O8 2.481(7) . ?
Dy1 O3 2.350(7) . ?
Dy1 O2 2.310(7) 6_564 ?
Dy1 O1 2.393(7) . ?
Dy1 O7 2.458(7) . ?
Dy1 N4 2.898(9) . ?
O4 Dy1 2.295(7) 2_655 ?
O4 C12 1.252(11) . ?
O6 Dy1 2.252(6) 6_564 ?
O6 C18 1.288(12) . ?
O5 C18 1.223(12) . ?
O8 N4 1.273(10) . ?
O3 C12 1.256(11) . ?
N1 C5 1.329(13) . ?
N1 C1 1.355(14) . ?
O2 Dy1 2.310(7) 2_655 ?
O2 C6 1.246(11) . ?
O1 C6 1.263(12) . ?
O7 N4 1.278(11) . ?
C14 C15 1.390(14) . ?
C14 C18 1.487(13) . ?
C14 C13 1.387(14) . ?
N4 O9 1.222(10) . ?
C16 C15 1.375(14) . ?
C16 C17 1.362(16) . ?
C10 C12 1.489(13) . ?
C10 C9 1.398(14) . ?
C10 C11 1.355(14) . ?
N3 C17 1.338(14) . ?
N3 C13 1.359(13) . ?
C8 C9 1.380(14) . ?
C8 C7 1.387(16) . ?
C3 C4 1.391(14) . ?
C3 C2 1.387(14) . ?
C4 C5 1.388(14) . ?
C4 C6 1.507(13) . ?
N2 C11 1.343(13) . ?
N2 C7 1.331(15) . ?
C2 C1 1.350(15) . ?

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
O4 Dy1 O5 104.8(2) 6_564 . ?
O4 Dy1 O8 123.9(2) 6_564 . ?
O4 Dy1 O3 84.3(3) 6_564 . ?
O4 Dy1 O2 82.2(2) 6_564 6_564 ?
O4 Dy1 O1 79.0(2) 6_564 . ?
O4 Dy1 O7 72.7(2) 6_564 . ?
O4 Dy1 N4 98.2(2) 6_564 . ?
O6 Dy1 O4 160.1(2) 2_655 6_564 ?
O6 Dy1 O5 83.6(2) 2_655 . ?
O6 Dy1 O8 75.7(2) 2_655 . ?
O6 Dy1 O3 100.0(3) 2_655 . ?
O6 Dy1 O2 83.0(3) 2_655 6_564 ?
O6 Dy1 O1 83.6(3) 2_655 . ?
O6 Dy1 O7 127.2(2) 2_655 . ?
O6 Dy1 N4 101.5(2) 2_655 . ?
O5 Dy1 O8 71.6(2) . . ?
O5 Dy1 O7 75.3(2) . . ?
O5 Dy1 N4 72.5(2) . . ?
O8 Dy1 N4 25.9(2) . . ?
O3 Dy1 O5 142.7(2) . . ?
O3 Dy1 O8 73.4(2) . . ?
O3 Dy1 O1 73.2(2) . . ?
O3 Dy1 O7 73.2(2) . . ?
O3 Dy1 N4 70.4(2) . . ?
O2 Dy1 O5 73.5(2) 6_564 . ?
O2 Dy1 O8 140.6(2) 6_564 . ?
O2 Dy1 O3 143.8(3) 6_564 . ?
O2 Dy1 O1 71.3(2) 6_564 . ?
O2 Dy1 O7 132.9(2) 6_564 . ?
O2 Dy1 N4 144.9(3) 6_564 . ?
O1 Dy1 O5 143.6(2) . . ?
O1 Dy1 O8 136.6(2) . . ?
O1 Dy1 O7 137.7(2) . . ?
O1 Dy1 N4 143.6(2) . . ?
O7 Dy1 O8 51.9(2) . . ?
O7 Dy1 N4 26.0(2) . . ?
C12 O4 Dy1 135.2(6) . 2_655 ?
C18 O6 Dy1 153.7(7) . 6_564 ?
C18 O5 Dy1 126.4(6) . . ?
N4 O8 Dy1 95.7(5) . . ?
C12 O3 Dy1 133.0(7) . . ?
C5 N1 C1 118.8(10) . . ?
C6 O2 Dy1 162.7(6) . 2_655 ?
C6 O1 Dy1 135.1(6) . . ?
N4 O7 Dy1 96.6(5) . . ?
C15 C14 C18 121.4(9) . . ?
C13 C14 C15 116.1(10) . . ?
C13 C14 C18 122.4(10) . . ?
O8 N4 Dy1 58.4(5) . . ?
O8 N4 O7 115.7(8) . . ?
O7 N4 Dy1 57.4(5) . . ?
O9 N4 Dy1 176.5(7) . . ?
O9 N4 O8 122.9(9) . . ?
O9 N4 O7 121.4(9) . . ?
C17 C16 C15 118.2(10) . . ?
C9 C10 C12 121.8(10) . . ?
C11 C10 C12 121.7(9) . . ?
C11 C10 C9 116.5(10) . . ?
C17 N3 C13 119.8(10) . . ?
C9 C8 C7 118.3(11) . . ?
C2 C3 C4 118.5(10) . . ?
C16 C15 C14 122.2(10) . . ?
N3 C17 C16 121.8(10) . . ?
C3 C4 C6 122.4(9) . . ?
C5 C4 C3 117.4(9) . . ?
C5 C4 C6 120.2(9) . . ?
C7 N2 C11 114.5(9) . . ?
N1 C5 C4 123.4(10) . . ?
O6 C18 C14 115.8(9) . . ?
O5 C18 O6 126.4(9) . . ?
O5 C18 C14 117.8(9) . . ?
O4 C12 O3 124.8(9) . . ?
O4 C12 C10 118.5(9) . . ?
O3 C12 C10 116.7(9) . . ?
O2 C6 O1 125.4(9) . . ?
O2 C6 C4 116.0(9) . . ?
O1 C6 C4 118.5(9) . . ?
N3 C13 C14 121.9(10) . . ?
C8 C9 C10 119.1(10) . . ?
C1 C2 C3 120.9(11) . . ?
N2 C11 C10 127.2(10) . . ?
N2 C7 C8 124.4(11) . . ?
C2 C1 N1 121.0(10) . . ?

