# 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_amgacldy
_database_code_depnum_ccdc_archive 'CCDC 920636'
_audit_update_record             
;
2013-01-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'amer_Dy6.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H90 Dy6 N12 O36, 6(C2 H3 N)'
_chemical_formula_sum            'C54 H108 Dy6 N18 O36'
_chemical_formula_weight         2560.58

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           trigonal
_symmetry_space_group_name_H-M   'R -3:H'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.5124(14)
_cell_length_b                   17.5124(14)
_cell_length_c                   24.2551(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6442.1(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14552
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      28.08

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3726
_exptl_absorpt_coefficient_mu    5.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_process_details   'TWINABS 1.05 (Bruker AXS Inc., 2006)'

_exptl_special_details           
;
The crystal used was a twin, and the data were integrated and corrected
for absorption taking this twinning into account.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33133
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         26.73
_reflns_number_total             3048
_reflns_number_gt                3003
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2003)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_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.
The O(3)-H(3) bond length was restrained. All other H-atoms were placed
in calculated positions (for the MeCN molecule the torsion angle of the
methyl group was refined).
;

_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)+(0.0212P)²+14.6837P] 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         3048
_refine_ls_number_parameters     176
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0451
_refine_ls_wR_factor_gt          0.0449
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.167
_refine_ls_shift/su_max          0.002
_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
Dy1 Dy 0.664113(7) 0.544864(7) 0.333992(5) 0.01432(5) Uani 1 1 d . . .
N1 N 0.65016(13) 0.58609(13) 0.43439(9) 0.0175(4) Uani 1 1 d . . .
C1 C 0.74198(16) 0.64245(16) 0.45425(10) 0.0194(5) Uani 1 1 d . . .
H1A H 0.7416 0.6527 0.4944 0.023 Uiso 1 1 calc R . .
H1B H 0.7691 0.7003 0.4354 0.023 Uiso 1 1 calc R . .
C2 C 0.79577(17) 0.59805(17) 0.44272(11) 0.0206(5) Uani 1 1 d . . .
H2A H 0.8590 0.6406 0.4490 0.025 Uiso 1 1 calc R . .
H2B H 0.7778 0.5480 0.4684 0.025 Uiso 1 1 calc R . .
O1 O 0.78332(11) 0.56687(11) 0.38765(7) 0.0183(3) Uani 1 1 d . . .
C3 C 0.60228(17) 0.50303(16) 0.46670(11) 0.0217(5) Uani 1 1 d . . .
H3A H 0.5413 0.4903 0.4736 0.026 Uiso 1 1 calc R . .
H3B H 0.6317 0.5113 0.5028 0.026 Uiso 1 1 calc R . .
C4 C 0.59894(17) 0.42437(17) 0.43744(11) 0.0202(5) Uani 1 1 d . . .
H4A H 0.6578 0.4294 0.4387 0.024 Uiso 1 1 calc R . .
H4B H 0.5565 0.3692 0.4564 0.024 Uiso 1 1 calc R . .
O2 O 0.57288(11) 0.42176(11) 0.38202(7) 0.0170(3) Uani 1 1 d . . .
C5 C 0.60323(17) 0.63698(17) 0.43655(11) 0.0222(5) Uani 1 1 d . . .
H5A H 0.6436 0.6983 0.4244 0.027 Uiso 1 1 calc R . .
H5B H 0.5856 0.6390 0.4751 0.027 Uiso 1 1 calc R . .
C6 C 0.52240(17) 0.59657(17) 0.40035(11) 0.0231(5) Uani 1 1 d . . .
H6A H 0.4808 0.5353 0.4133 0.028 Uiso 1 1 calc R . .
C7 C 0.47528(19) 0.64931(19) 0.39981(13) 0.0296(6) Uani 1 1 d . . .
H7A H 0.4232 0.6200 0.3760 0.044 Uiso 1 1 calc R . .
H7B H 0.5152 0.7087 0.3857 0.044 Uiso 1 1 calc R . .
H7C H 0.4570 0.6534 0.4374 0.044 Uiso 1 1 calc R . .
O3 O 0.55429(12) 0.59291(13) 0.34609(8) 0.0226(4) Uani 1 1 d D . .
H3 H 0.520(2) 0.574(2) 0.3238(13) 0.027 Uiso 1 1 d D . .
N2 N 0.72740(14) 0.71895(14) 0.28535(9) 0.0219(4) Uani 1 1 d . . .
O4 O 0.75069(12) 0.70870(12) 0.33350(8) 0.0232(4) Uani 1 1 d . . .
O5 O 0.68518(12) 0.65007(11) 0.25624(8) 0.0222(4) Uani 1 1 d . . .
O6 O 0.74595(15) 0.79198(13) 0.26828(9) 0.0338(5) Uani 1 1 d . . .
N21 N 0.4522(2) 0.6109(2) 0.24488(18) 0.0655(10) Uani 1 1 d . . .
C21 C 0.4928(2) 0.6856(2) 0.24386(16) 0.0436(8) Uani 1 1 d . . .
C22 C 0.5464(3) 0.7797(2) 0.2450(2) 0.0571(11) Uani 1 1 d . . .
H22A H 0.5245 0.8035 0.2735 0.086 Uiso 1 1 calc R . .
H22B H 0.5438 0.8037 0.2090 0.086 Uiso 1 1 calc R . .
H22C H 0.6076 0.7962 0.2532 0.086 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 2.2478(17) 17 ?
Dy1 O2 2.2611(17) . ?
Dy1 O1 2.2851(17) 18_545 ?
Dy1 O1 2.3229(17) . ?
Dy1 O3 2.4720(18) . ?
Dy1 O4 2.4862(18) . ?
Dy1 O5 2.5313(18) . ?
Dy1 N1 2.586(2) . ?
Dy1 Dy1 3.7271(3) 17 ?
N1 C1 1.485(3) . ?
N1 C5 1.485(3) . ?
N1 C3 1.488(3) . ?
C1 C2 1.518(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.418(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O1 Dy1 2.2850(17) 17 ?
C3 C4 1.524(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O2 1.413(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O2 Dy1 2.2478(17) 18_545 ?
C5 C6 1.508(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O3 1.444(3) . ?
C6 C7 1.515(4) . ?
C6 H6A 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
O3 H3 0.75(3) . ?
N2 O6 1.224(3) . ?
N2 O5 1.268(3) . ?
N2 O4 1.279(3) . ?
N21 C21 1.133(5) . ?
C21 C22 1.432(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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 O2 107.46(9) 17 . ?
O2 Dy1 O1 89.23(6) 17 18_545 ?
O2 Dy1 O1 70.30(6) . 18_545 ?
O2 Dy1 O1 69.84(6) 17 . ?
O2 Dy1 O1 91.00(6) . . ?
O1 Dy1 O1 146.69(8) 18_545 . ?
O2 Dy1 O3 154.41(6) 17 . ?
O2 Dy1 O3 87.95(6) . . ?
O1 Dy1 O3 76.63(6) 18_545 . ?
O1 Dy1 O3 131.65(6) . . ?
O2 Dy1 O4 99.68(6) 17 . ?
O2 Dy1 O4 146.64(6) . . ?
O1 Dy1 O4 130.05(6) 18_545 . ?
O1 Dy1 O4 80.35(6) . . ?
O3 Dy1 O4 74.76(6) . . ?
O2 Dy1 O5 84.70(6) 17 . ?
O2 Dy1 O5 148.66(6) . . ?
O1 Dy1 O5 81.39(6) 18_545 . ?
O1 Dy1 O5 120.32(6) . . ?
O3 Dy1 O5 72.29(6) . . ?
O4 Dy1 O5 51.22(6) . . ?
O2 Dy1 N1 137.89(6) 17 . ?
O2 Dy1 N1 70.17(6) . . ?
O1 Dy1 N1 125.58(6) 18_545 . ?
O1 Dy1 N1 68.20(6) . . ?
O3 Dy1 N1 66.11(6) . . ?
O4 Dy1 N1 76.73(6) . . ?
O5 Dy1 N1 119.87(6) . . ?
C1 N1 C5 109.27(19) . . ?
C1 N1 C3 111.9(2) . . ?
C5 N1 C3 110.96(19) . . ?
C1 N1 Dy1 105.61(14) . . ?
C5 N1 Dy1 111.02(15) . . ?
C3 N1 Dy1 107.99(14) . . ?
N1 C1 C2 110.1(2) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
O1 C2 C1 110.8(2) . . ?
O1 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O1 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 O1 Dy1 128.59(14) . 17 ?
C2 O1 Dy1 122.97(14) . . ?
Dy1 O1 Dy1 107.96(7) 17 . ?
N1 C3 C4 112.7(2) . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
O2 C4 C3 109.8(2) . . ?
O2 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
O2 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 O2 Dy1 134.63(15) . 18_545 ?
C4 O2 Dy1 113.36(14) . . ?
Dy1 O2 Dy1 111.50(7) 18_545 . ?
N1 C5 C6 111.7(2) . . ?
N1 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N1 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
O3 C6 C5 105.0(2) . . ?
O3 C6 C7 111.1(2) . . ?
C5 C6 C7 112.9(2) . . ?
O3 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
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 . . ?
C6 O3 Dy1 120.49(15) . . ?
C6 O3 H3 116(3) . . ?
Dy1 O3 H3 111(3) . . ?
O6 N2 O5 122.0(2) . . ?
O6 N2 O4 121.3(2) . . ?
O5 N2 O4 116.8(2) . . ?
N2 O4 Dy1 96.49(13) . . ?
N2 O5 Dy1 94.64(14) . . ?
N21 C21 C22 177.2(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 N21 0.75(3) 2.50(3) 3.145(5) 145(3) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.110
####################################################################### 
# 
# 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_aml11dy4s
_database_code_depnum_ccdc_archive 'CCDC 920637'
_audit_update_record             
;
2013-01-18 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
#TrackingRef 'amer_Dy6.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C42 H96 Dy6 N18 O30), 2(C4 H8 O)'
_chemical_formula_sum            'C50 H112 Dy6 N18 O32'
_chemical_formula_weight         2452.58

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           trigonal
_symmetry_space_group_name_H-M   'R -3:H'
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   15.7780(10)
_cell_length_b                   15.7780(10)
_cell_length_c                   26.4045(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5692.6(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      25.97

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3570
_exptl_absorpt_coefficient_mu    5.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_process_details   
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(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  'Stoe IPDS'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15286
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         26.05
_reflns_number_total             2499
_reflns_number_gt                2174
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_cell_refinement       'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_data_reduction        'IPDS 2.92 (Stoe & Cie GmbH, 1999)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_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.
N-H bond lengths were restrained, all other H-atoms placed in calculated
positions.
The lattice THF molecules were badly disordered over sites of threefold
symmetry and were treated using the SQUEEZE option in PLATON (see below).
;

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 0.000 0.000 0.000 18 4 ' '
2 0.000 0.000 0.238 135 47 'THF (= 40 e)'
3 0.000 0.000 0.762 135 47 'THF (= 40 e)'
4 0.333 0.667 0.904 131 47 'THF (= 40 e)'
5 0.333 0.667 0.429 131 47 'THF (= 40 e)'
6 0.333 0.667 0.667 18 4 ' '
7 0.667 0.333 0.571 131 47 'THF (= 40 e)'
8 0.667 0.333 0.096 131 47 'THF (= 40 e)'
9 0.666 0.333 0.333 18 4 ' '
_platon_squeeze_details          
;
;

_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)+(0.0401P)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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2499
_refine_ls_number_parameters     152
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0576
_refine_ls_wR_factor_gt          0.0557
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.061579(12) 0.262337(13) 0.005584(6) 0.02263(9) Uani 1 1 d . . .
N1 N 0.0817(2) 0.3067(3) 0.10489(13) 0.0302(7) Uani 1 1 d . . .
C1 C 0.1534(3) 0.2795(4) 0.12363(16) 0.0352(9) Uani 1 1 d . . .
H1A H 0.1460 0.2693 0.1607 0.042 Uiso 1 1 calc R . .
H1B H 0.2206 0.3337 0.1168 0.042 Uiso 1 1 calc R . .
C2 C 0.1392(4) 0.1873(3) 0.09836(15) 0.0337(9) Uani 1 1 d . . .
H2A H 0.1903 0.1728 0.1101 0.040 Uiso 1 1 calc R . .
H2B H 0.0745 0.1314 0.1077 0.040 Uiso 1 1 calc R . .
O1 O 0.1450(2) 0.1996(2) 0.04519(10) 0.0279(6) Uani 1 1 d . . .
C3 C -0.0147(3) 0.2415(3) 0.12805(15) 0.0354(9) Uani 1 1 d . . .
H3A H -0.0225 0.2726 0.1589 0.042 Uiso 1 1 calc R . .
H3B H -0.0186 0.1792 0.1381 0.042 Uiso 1 1 calc R . .
C4 C -0.0956(3) 0.2209(3) 0.09123(16) 0.0326(9) Uani 1 1 d . . .
H4A H -0.1598 0.1773 0.1073 0.039 Uiso 1 1 calc R . .
H4B H -0.0932 0.2829 0.0820 0.039 Uiso 1 1 calc R . .
O2 O -0.08561(18) 0.1763(2) 0.04759(10) 0.0261(6) Uani 1 1 d . . .
C5 C 0.1105(4) 0.4078(3) 0.12112(19) 0.0415(11) Uani 1 1 d . . .
H5A H 0.1168 0.4108 0.1585 0.050 Uiso 1 1 calc R . .
H5B H 0.0563 0.4197 0.1125 0.050 Uiso 1 1 calc R . .
C6 C 0.2040(4) 0.4912(4) 0.0993(2) 0.0488(12) Uani 1 1 d . . .
H6A H 0.2577 0.4770 0.1052 0.059 Uiso 1 1 calc R . .
H6B H 0.2203 0.5516 0.1182 0.059 Uiso 1 1 calc R . .
C7 C 0.2014(4) 0.5111(3) 0.0431(2) 0.0450(12) Uani 1 1 d . . .
H7A H 0.1418 0.5147 0.0356 0.054 Uiso 1 1 calc R . .
H7B H 0.2589 0.5751 0.0344 0.054 Uiso 1 1 calc R . .
N2 N 0.2017(3) 0.4344(3) 0.01155(16) 0.0364(8) Uani 1 1 d D . .
H21 H 0.262(3) 0.439(4) 0.016(2) 0.044 Uiso 1 1 d D . .
H22 H 0.210(4) 0.462(4) -0.0194(15) 0.044 Uiso 1 1 d D . .
N3 N 0.0013(3) 0.3876(3) -0.05036(15) 0.0362(8) Uani 1 1 d . . .
O4 O 0.0587(2) 0.3637(2) -0.07054(12) 0.0398(7) Uani 1 1 d . . .
O5 O -0.0192(2) 0.3658(2) -0.00369(12) 0.0371(7) Uani 1 1 d . . .
O6 O -0.0355(4) 0.4264(4) -0.07471(17) 0.0679(12) 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
Dy1 O1 2.260(3) . ?
Dy1 O1 2.278(3) 12 ?
Dy1 O2 2.293(3) 11 ?
Dy1 O2 2.305(3) . ?
Dy1 N2 2.507(4) . ?
Dy1 O5 2.535(3) . ?
Dy1 O4 2.583(3) . ?
Dy1 N1 2.692(3) . ?
Dy1 Dy1 3.7606(3) 11 ?
N1 C3 1.477(5) . ?
N1 C1 1.482(5) . ?
N1 C5 1.487(6) . ?
C1 C2 1.512(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O1 1.414(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O1 Dy1 2.278(3) 11 ?
C3 C4 1.506(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O2 1.400(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O2 Dy1 2.293(3) 12 ?
C5 C6 1.516(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.523(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N2 1.469(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N2 H21 0.93(3) . ?
N2 H22 0.90(3) . ?
N3 O6 1.217(5) . ?
N3 O4 1.260(5) . ?
N3 O5 1.277(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O1 108.94(15) . 12 ?
O1 Dy1 O2 69.43(9) . 11 ?
O1 Dy1 O2 87.30(10) 12 11 ?
O1 Dy1 O2 98.94(10) . . ?
O1 Dy1 O2 68.91(9) 12 . ?
O2 Dy1 O2 148.98(13) 11 . ?
O1 Dy1 N2 93.09(12) . . ?
O1 Dy1 N2 146.38(12) 12 . ?
O2 Dy1 N2 76.81(11) 11 . ?
O2 Dy1 N2 133.70(11) . . ?
O1 Dy1 O5 156.47(10) . . ?
O1 Dy1 O5 90.40(10) 12 . ?
O2 Dy1 O5 126.47(10) 11 . ?
O2 Dy1 O5 75.10(10) . . ?
N2 Dy1 O5 76.33(11) . . ?
O1 Dy1 O4 145.63(10) . . ?
O1 Dy1 O4 77.82(10) 12 . ?
O2 Dy1 O4 77.50(9) 11 . ?
O2 Dy1 O4 114.50(10) . . ?
N2 Dy1 O4 69.96(12) . . ?
O5 Dy1 O4 49.94(10) . . ?
O1 Dy1 N1 69.18(10) . . ?
O1 Dy1 N1 136.63(10) 12 . ?
O2 Dy1 N1 127.34(10) 11 . ?
O2 Dy1 N1 68.75(10) . . ?
N2 Dy1 N1 74.42(12) . . ?
O5 Dy1 N1 87.62(10) . . ?
O4 Dy1 N1 129.30(11) . . ?
C3 N1 C1 109.2(4) . . ?
C3 N1 C5 106.5(3) . . ?
C1 N1 C5 110.3(3) . . ?
C3 N1 Dy1 106.0(2) . . ?
C1 N1 Dy1 104.9(2) . . ?
C5 N1 Dy1 119.5(3) . . ?
N1 C1 C2 111.3(3) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
O1 C2 C1 109.7(3) . . ?
O1 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O1 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 O1 Dy1 120.5(2) . . ?
C2 O1 Dy1 125.6(2) . 11 ?
Dy1 O1 Dy1 111.91(11) . 11 ?
N1 C3 C4 110.5(4) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O2 C4 C3 110.0(3) . . ?
O2 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
O2 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 O2 Dy1 131.0(2) . 12 ?
C4 O2 Dy1 115.7(2) . . ?
Dy1 O2 Dy1 109.73(11) 12 . ?
N1 C5 C6 117.7(4) . . ?
N1 C5 H5A 107.9 . . ?
C6 C5 H5A 107.9 . . ?
N1 C5 H5B 107.9 . . ?
C6 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
C5 C6 C7 115.7(4) . . ?
C5 C6 H6A 108.3 . . ?
C7 C6 H6A 108.3 . . ?
C5 C6 H6B 108.3 . . ?
C7 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
N2 C7 C6 111.8(4) . . ?
N2 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C7 N2 Dy1 124.3(3) . . ?
C7 N2 H21 106(3) . . ?
Dy1 N2 H21 114(3) . . ?
C7 N2 H22 100(4) . . ?
Dy1 N2 H22 107(4) . . ?
H21 N2 H22 101(5) . . ?
O6 N3 O4 121.5(4) . . ?
O6 N3 O5 121.7(4) . . ?
O4 N3 O5 116.8(3) . . ?
N3 O4 Dy1 95.4(2) . . ?
N3 O5 Dy1 97.2(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H21 O5 0.93(3) 2.22(4) 3.062(5) 151(5) 11

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.113


