# 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_pena47
_database_code_depnum_ccdc_archive 'CCDC 1039917'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H46 Gd2 N8 O14'
_chemical_formula_weight         1153.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   12.3327(2)
_cell_length_b                   14.0747(3)
_cell_length_c                   12.6772(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.2590(10)
_cell_angle_gamma                90.00
_cell_volume                     2199.97(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    30960
_cell_measurement_theta_min      6.99
_cell_measurement_theta_max      71.87

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    19.917
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.045
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37020
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         6.99
_diffrn_reflns_theta_max         64.96
_reflns_number_total             3711
_reflns_number_gt                3444
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0404P)²+4.4714P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3711
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.918703(19) 0.110592(17) 0.029085(16) 0.01620(11) Uani 1 1 d . . .
N1 N 0.8902(3) 0.1282(3) -0.1691(3) 0.0206(8) Uani 1 1 d . . .
O1 O 1.0620(2) 0.0509(2) -0.0705(2) 0.0187(6) Uani 1 1 d . . .
O2 O 0.7463(2) 0.0744(3) -0.0093(2) 0.0271(7) Uani 1 1 d . . .
C1 C 1.0788(4) 0.0892(3) -0.1656(3) 0.0181(9) Uani 1 1 d . . .
C2 C 1.1813(4) 0.0887(4) -0.2107(4) 0.0270(11) Uani 1 1 d . . .
C3 C 1.1962(5) 0.1264(4) -0.3099(4) 0.0314(12) Uani 1 1 d . . .
C4 C 1.1105(5) 0.1657(4) -0.3663(4) 0.0331(12) Uani 1 1 d . . .
C5 C 1.0081(4) 0.1677(4) -0.3236(4) 0.0288(11) Uani 1 1 d . . .
C6 C 0.9907(4) 0.1286(3) -0.2225(3) 0.0207(10) Uani 1 1 d . . .
C7 C 0.8004(4) 0.1366(3) -0.2211(4) 0.0230(10) Uani 1 1 d . . .
C8 C 0.6936(4) 0.1353(3) -0.1785(4) 0.0240(10) Uani 1 1 d . . .
C9 C 0.6063(4) 0.1609(4) -0.2470(4) 0.0327(12) Uani 1 1 d . . .
C10 C 0.5014(4) 0.1610(4) -0.2148(5) 0.0396(13) Uani 1 1 d . . .
C11 C 0.4795(5) 0.1352(5) -0.1106(5) 0.0400(13) Uani 1 1 d . . .
C12 C 0.5610(5) 0.1079(4) -0.0436(4) 0.0315(12) Uani 1 1 d . . .
C13 C 0.6709(4) 0.1058(3) -0.0739(4) 0.0231(10) Uani 1 1 d . . .
N2 N 0.9413(4) 0.3156(3) 0.0001(3) 0.0282(9) Uani 1 1 d . . .
O3 O 1.0218(3) 0.2591(2) 0.0012(3) 0.0322(8) Uani 1 1 d . . .
O4 O 0.8489(3) 0.2771(2) 0.0096(3) 0.0321(8) Uani 1 1 d . . .
O5 O 0.9516(4) 0.4006(3) -0.0097(4) 0.0502(12) Uani 1 1 d . . .
O6 O 1.0677(3) 0.1061(2) 0.1580(3) 0.0295(8) Uani 1 1 d . . .
N3 N 1.2348(4) 0.1046(3) 0.2333(4) 0.0315(10) Uani 1 1 d . . .
C14 C 1.1677(5) 0.1079(3) 0.1501(4) 0.0292(12) Uani 1 1 d . . .
C15 C 1.3522(5) 0.1069(4) 0.2222(6) 0.0485(17) Uani 1 1 d . . .
H15A H 1.3819 0.1628 0.2586 0.073 Uiso 1 1 calc R . .
H15B H 1.3697 0.1099 0.1472 0.073 Uiso 1 1 calc R . .
H15C H 1.3841 0.0493 0.2534 0.073 Uiso 1 1 calc R . .
C16 C 1.1915(6) 0.0975(4) 0.3393(4) 0.0453(16) Uani 1 1 d . . .
H16A H 1.2497 0.0793 0.3892 0.068 Uiso 1 1 calc R . .
H16B H 1.1340 0.0494 0.3399 0.068 Uiso 1 1 calc R . .
H16C H 1.1616 0.1591 0.3600 0.068 Uiso 1 1 calc R . .
N4 N 0.7554(4) 0.1197(3) 0.3443(3) 0.0325(11) Uani 1 1 d . . .
O7 O 0.8436(3) 0.1434(3) 0.1935(2) 0.0328(8) Uani 1 1 d . . .
C17 C 0.8423(5) 0.1306(4) 0.2891(4) 0.0372(13) Uani 1 1 d . . .
C18 C 0.7597(7) 0.1029(6) 0.4577(5) 0.072(3) Uani 1 1 d . . .
H18A H 0.7181 0.1522 0.4934 0.108 Uiso 1 1 calc R . .
H18B H 0.8353 0.1047 0.4831 0.108 Uiso 1 1 calc R . .
H18C H 0.7285 0.0404 0.4729 0.108 Uiso 1 1 calc R . .
C19 C 0.6477(5) 0.1207(5) 0.2938(6) 0.0517(18) Uani 1 1 d . . .
H19A H 0.6066 0.0651 0.3167 0.078 Uiso 1 1 calc R . .
H19B H 0.6549 0.1190 0.2170 0.078 Uiso 1 1 calc R . .
H19C H 0.6094 0.1787 0.3139 0.078 Uiso 1 1 calc R . .
H2 H 1.233(5) 0.066(4) -0.170(5) 0.042(17) Uiso 1 1 d . . .
H3 H 1.255(5) 0.128(4) -0.334(5) 0.033(16) Uiso 1 1 d . . .
H4 H 1.118(4) 0.195(4) -0.428(4) 0.026(13) Uiso 1 1 d . . .
H5 H 0.942(4) 0.198(4) -0.357(4) 0.033(14) Uiso 1 1 d . . .
H7 H 0.799(4) 0.145(4) -0.289(4) 0.021(13) Uiso 1 1 d . . .
H9 H 0.623(5) 0.184(4) -0.316(5) 0.045(17) Uiso 1 1 d . . .
H10 H 0.434(5) 0.174(4) -0.259(4) 0.042(16) Uiso 1 1 d . . .
H11 H 0.401(5) 0.133(4) -0.085(4) 0.027(14) Uiso 1 1 d . . .
H13 H 0.549(6) 0.089(4) 0.023(6) 0.052(19) Uiso 1 1 d . . .
H14 H 1.199(4) 0.119(3) 0.071(4) 0.020(13) Uiso 1 1 d . . .
H17 H 0.919(5) 0.128(4) 0.341(4) 0.032(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O2 2.229(3) . ?
Gd1 O1 2.344(3) 3_755 ?
Gd1 O7 2.346(3) . ?
Gd1 O1 2.349(3) . ?
Gd1 O6 2.434(3) . ?
Gd1 O3 2.476(3) . ?
Gd1 O4 2.507(3) . ?
Gd1 N1 2.541(4) . ?
Gd1 N2 2.923(4) . ?
Gd1 Gd1 3.7843(5) 3_755 ?
N1 C7 1.282(6) . ?
N1 C6 1.425(6) . ?
O1 C1 1.341(5) . ?
O1 Gd1 2.344(3) 3_755 ?
O2 C13 1.303(6) . ?
C1 C2 1.399(6) . ?
C1 C6 1.406(7) . ?
C2 C3 1.381(7) . ?
C2 H2 0.87(6) . ?
C3 C4 1.378(8) . ?
C3 H3 0.80(6) . ?
C4 C5 1.385(7) . ?
C4 H4 0.88(5) . ?
C5 C6 1.415(6) . ?
C5 H5 1.00(5) . ?
C7 C8 1.435(7) . ?
C7 H7 0.86(5) . ?
C8 C9 1.415(7) . ?
C8 C13 1.423(7) . ?
C9 C10 1.365(8) . ?
C9 H9 0.96(6) . ?
C10 C11 1.402(8) . ?
C10 H10 1.01(6) . ?
C11 C12 1.358(8) . ?
C11 H11 1.03(5) . ?
C12 C13 1.418(7) . ?
C12 H13 0.90(7) . ?
N2 O5 1.210(5) . ?
N2 O4 1.270(5) . ?
N2 O3 1.271(5) . ?
O6 C14 1.239(7) . ?
N3 C14 1.327(7) . ?
N3 C15 1.458(8) . ?
N3 C16 1.461(7) . ?
C14 H14 1.09(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N4 C17 1.302(7) . ?
N4 C18 1.456(7) . ?
N4 C19 1.462(8) . ?
O7 C17 1.225(6) . ?
C17 H17 1.14(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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 Gd1 O1 85.35(12) . 3_755 ?
O2 Gd1 O7 81.10(12) . . ?
O1 Gd1 O7 91.85(11) 3_755 . ?
O2 Gd1 O1 121.74(11) . . ?
O1 Gd1 O1 72.52(11) 3_755 . ?
O7 Gd1 O1 149.81(12) . . ?
O2 Gd1 O6 147.45(12) . . ?
O1 Gd1 O6 75.68(11) 3_755 . ?
O7 Gd1 O6 73.47(13) . . ?
O1 Gd1 O6 77.62(11) . . ?
O2 Gd1 O3 130.68(12) . . ?
O1 Gd1 O3 143.21(11) 3_755 . ?
O7 Gd1 O3 100.06(12) . . ?
O1 Gd1 O3 80.24(11) . . ?
O6 Gd1 O3 74.67(11) . . ?
O2 Gd1 O4 82.44(12) . . ?
O1 Gd1 O4 164.08(10) 3_755 . ?
O7 Gd1 O4 76.22(12) . . ?
O1 Gd1 O4 122.82(10) . . ?
O6 Gd1 O4 110.07(11) . . ?
O3 Gd1 O4 51.16(11) . . ?
O2 Gd1 N1 72.31(12) . . ?
O1 Gd1 N1 109.09(11) 3_755 . ?
O7 Gd1 N1 144.15(13) . . ?
O1 Gd1 N1 65.99(11) . . ?
O6 Gd1 N1 138.83(12) . . ?
O3 Gd1 N1 80.61(12) . . ?
O4 Gd1 N1 76.81(11) . . ?
O2 Gd1 N2 106.94(12) . . ?
O1 Gd1 N2 167.43(11) 3_755 . ?
O7 Gd1 N2 87.58(12) . . ?
O1 Gd1 N2 102.15(11) . . ?
O6 Gd1 N2 92.16(11) . . ?
O3 Gd1 N2 25.56(11) . . ?
O4 Gd1 N2 25.61(11) . . ?
N1 Gd1 N2 77.94(11) . . ?
O2 Gd1 Gd1 106.04(9) . 3_755 ?
O1 Gd1 Gd1 36.30(7) 3_755 3_755 ?
O7 Gd1 Gd1 123.82(9) . 3_755 ?
O1 Gd1 Gd1 36.21(7) . 3_755 ?
O6 Gd1 Gd1 73.36(8) . 3_755 ?
O3 Gd1 Gd1 113.01(8) . 3_755 ?
O4 Gd1 Gd1 158.76(7) . 3_755 ?
N1 Gd1 Gd1 87.14(9) . 3_755 ?
N2 Gd1 Gd1 137.33(8) . 3_755 ?
C7 N1 C6 120.3(4) . . ?
C7 N1 Gd1 128.1(3) . . ?
C6 N1 Gd1 111.5(3) . . ?
C1 O1 Gd1 125.0(3) . 3_755 ?
C1 O1 Gd1 118.2(3) . . ?
Gd1 O1 Gd1 107.48(11) 3_755 . ?
C13 O2 Gd1 136.4(3) . . ?
O1 C1 C2 121.6(4) . . ?
O1 C1 C6 119.1(4) . . ?
C2 C1 C6 119.2(4) . . ?
C3 C2 C1 120.6(5) . . ?
C3 C2 H2 125(4) . . ?
C1 C2 H2 115(4) . . ?
C4 C3 C2 120.8(5) . . ?
C4 C3 H3 119(4) . . ?
C2 C3 H3 120(4) . . ?
C3 C4 C5 120.0(5) . . ?
C3 C4 H4 123(3) . . ?
C5 C4 H4 117(3) . . ?
C4 C5 C6 120.3(5) . . ?
C4 C5 H5 125(3) . . ?
C6 C5 H5 114(3) . . ?
C1 C6 C5 119.1(4) . . ?
C1 C6 N1 115.2(4) . . ?
C5 C6 N1 125.7(4) . . ?
N1 C7 C8 126.5(4) . . ?
N1 C7 H7 121(3) . . ?
C8 C7 H7 112(3) . . ?
C9 C8 C13 119.0(5) . . ?
C9 C8 C7 117.2(4) . . ?
C13 C8 C7 123.8(4) . . ?
C10 C9 C8 122.0(5) . . ?
C10 C9 H9 120(4) . . ?
C8 C9 H9 118(4) . . ?
C9 C10 C11 119.1(5) . . ?
C9 C10 H10 127(3) . . ?
C11 C10 H10 114(3) . . ?
C12 C11 C10 120.5(5) . . ?
C12 C11 H11 119(3) . . ?
C10 C11 H11 121(3) . . ?
C11 C12 C13 122.4(5) . . ?
C11 C12 H13 123(4) . . ?
C13 C12 H13 115(4) . . ?
O2 C13 C12 120.7(5) . . ?
O2 C13 C8 122.1(4) . . ?
C12 C13 C8 117.1(5) . . ?
O5 N2 O4 121.9(4) . . ?
O5 N2 O3 122.4(5) . . ?
O4 N2 O3 115.7(4) . . ?
O5 N2 Gd1 178.6(4) . . ?
O4 N2 Gd1 58.6(2) . . ?
O3 N2 Gd1 57.1(2) . . ?
N2 O3 Gd1 97.3(3) . . ?
N2 O4 Gd1 95.8(3) . . ?
C14 O6 Gd1 133.1(3) . . ?
C14 N3 C15 121.8(5) . . ?
C14 N3 C16 119.9(5) . . ?
C15 N3 C16 118.3(5) . . ?
O6 C14 N3 122.6(5) . . ?
O6 C14 H14 117(3) . . ?
N3 C14 H14 120(3) . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 N4 C18 122.6(6) . . ?
C17 N4 C19 120.9(5) . . ?
C18 N4 C19 116.5(5) . . ?
C17 O7 Gd1 149.7(4) . . ?
O7 C17 N4 125.4(6) . . ?
O7 C17 H17 123(3) . . ?
N4 C17 H17 112(3) . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 H19A 109.5 . . ?
N4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        64.96
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039918'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-04-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H46 Dy2 N8 O14'
_chemical_formula_weight         1163.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   12.3132(2)
_cell_length_b                   14.0547(2)
_cell_length_c                   12.6042(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4120(10)
_cell_angle_gamma                90.00
_cell_volume                     2180.60(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    25741
_cell_measurement_theta_min      7.03
_cell_measurement_theta_max      71.87

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1148
_exptl_absorpt_coefficient_mu    18.755
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26874
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         7.20
_diffrn_reflns_theta_max         64.98
_reflns_number_total             3687
_reflns_number_gt                3516
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0574P)²+1.2674P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3687
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.919721(17) 0.109603(15) 0.028238(17) 0.01778(12) Uani 1 1 d . . .
N1 N 0.8915(3) 0.1283(2) -0.1697(3) 0.0204(7) Uani 1 1 d . . .
O1 O 1.0626(2) 0.05079(18) -0.0692(2) 0.0193(5) Uani 1 1 d . . .
O2 O 0.7490(2) 0.0738(2) -0.0089(2) 0.0295(7) Uani 1 1 d . . .
C1 C 1.0798(3) 0.0881(3) -0.1645(3) 0.0207(8) Uani 1 1 d . . .
C2 C 1.1828(4) 0.0883(3) -0.2095(4) 0.0267(9) Uani 1 1 d . . .
C3 C 1.1987(4) 0.1265(3) -0.3080(4) 0.0329(11) Uani 1 1 d . . .
C4 C 1.1130(4) 0.1662(3) -0.3655(4) 0.0338(11) Uani 1 1 d . . .
C5 C 1.0098(4) 0.1675(3) -0.3236(3) 0.0301(9) Uani 1 1 d . . .
C6 C 0.9927(4) 0.1291(3) -0.2229(4) 0.0222(9) Uani 1 1 d . . .
C7 C 0.8018(4) 0.1375(3) -0.2216(3) 0.0247(9) Uani 1 1 d . . .
C8 C 0.6948(3) 0.1360(3) -0.1781(4) 0.0244(9) Uani 1 1 d . . .
C9 C 0.6077(4) 0.1618(3) -0.2464(4) 0.0332(10) Uani 1 1 d . . .
C10 C 0.5022(4) 0.1623(4) -0.2132(4) 0.0391(11) Uani 1 1 d . . .
C11 C 0.4812(4) 0.1353(4) -0.1099(5) 0.0399(12) Uani 1 1 d . . .
C12 C 0.5632(4) 0.1078(3) -0.0419(5) 0.0313(12) Uani 1 1 d . . .
C13 C 0.6733(4) 0.1055(2) -0.0730(4) 0.0232(10) Uani 1 1 d . . .
N2 N 0.9412(3) 0.3132(2) -0.0001(3) 0.0290(8) Uani 1 1 d . . .
O3 O 1.0224(2) 0.2566(2) 0.0022(3) 0.0320(7) Uani 1 1 d . . .
O4 O 0.8492(2) 0.2743(2) 0.0088(2) 0.0321(7) Uani 1 1 d . . .
O5 O 0.9516(4) 0.3987(2) -0.0097(4) 0.0490(11) Uani 1 1 d . . .
O6 O 1.0671(3) 0.10564(18) 0.1578(3) 0.0289(7) Uani 1 1 d . . .
N3 N 1.2345(3) 0.1043(2) 0.2326(3) 0.0302(9) Uani 1 1 d . . .
C14 C 1.1676(5) 0.1073(3) 0.1486(5) 0.0301(12) Uani 1 1 d . . .
C15 C 1.3526(4) 0.1062(3) 0.2205(6) 0.0447(15) Uani 1 1 d . . .
H15A H 1.3833 0.1603 0.2601 0.067 Uiso 1 1 calc R . .
H15B H 1.3692 0.1127 0.1452 0.067 Uiso 1 1 calc R . .
H15C H 1.3842 0.0469 0.2482 0.067 Uiso 1 1 calc R . .
C16 C 1.1929(5) 0.0965(4) 0.3387(4) 0.0458(14) Uani 1 1 d . . .
H16A H 1.2452 0.0619 0.3840 0.069 Uiso 1 1 calc R . .
H16B H 1.1237 0.0620 0.3360 0.069 Uiso 1 1 calc R . .
H16C H 1.1815 0.1603 0.3678 0.069 Uiso 1 1 calc R . .
N4 N 0.7573(3) 0.1198(3) 0.3436(3) 0.0331(9) Uani 1 1 d . . .
O7 O 0.8450(3) 0.1427(2) 0.1913(3) 0.0351(7) Uani 1 1 d . . .
C17 C 0.8439(5) 0.1302(4) 0.2872(5) 0.0406(12) Uani 1 1 d . . .
C18 C 0.7624(7) 0.1037(5) 0.4574(5) 0.077(3) Uani 1 1 d . . .
H18A H 0.7247 0.1554 0.4935 0.115 Uiso 1 1 calc R . .
H18B H 0.8385 0.1018 0.4820 0.115 Uiso 1 1 calc R . .
H18C H 0.7273 0.0430 0.4736 0.115 Uiso 1 1 calc R . .
C19 C 0.6490(5) 0.1216(4) 0.2933(6) 0.0529(16) Uani 1 1 d . . .
H19A H 0.6069 0.0670 0.3177 0.079 Uiso 1 1 calc R . .
H19B H 0.6556 0.1184 0.2160 0.079 Uiso 1 1 calc R . .
H19C H 0.6119 0.1807 0.3123 0.079 Uiso 1 1 calc R . .
H2 H 1.243(5) 0.053(4) -0.174(4) 0.058(17) Uiso 1 1 d . . .
H3 H 1.264(5) 0.126(3) -0.335(4) 0.034(14) Uiso 1 1 d . . .
H4 H 1.120(4) 0.191(4) -0.422(4) 0.048(16) Uiso 1 1 d . . .
H5 H 0.950(4) 0.204(3) -0.362(4) 0.040(13) Uiso 1 1 d . . .
H7 H 0.805(4) 0.147(4) -0.293(4) 0.034(13) Uiso 1 1 d . . .
H9 H 0.621(4) 0.182(4) -0.314(4) 0.039(14) Uiso 1 1 d . . .
H10 H 0.439(4) 0.176(3) -0.261(4) 0.031(12) Uiso 1 1 d . . .
H11 H 0.404(5) 0.136(4) -0.076(5) 0.054(16) Uiso 1 1 d . . .
H13 H 0.548(4) 0.084(3) 0.026(4) 0.026(12) Uiso 1 1 d . . .
H14 H 1.203(4) 0.116(3) 0.076(4) 0.024(13) Uiso 1 1 d . . .
H17 H 0.918(5) 0.129(4) 0.343(5) 0.056(17) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.200(3) . ?
Dy1 O7 2.319(3) . ?
Dy1 O1 2.322(3) 3_755 ?
Dy1 O1 2.323(2) . ?
Dy1 O6 2.411(3) . ?
Dy1 O3 2.448(3) . ?
Dy1 O4 2.482(3) . ?
Dy1 N1 2.525(4) . ?
Dy1 N2 2.897(3) . ?
Dy1 Dy1 3.7384(4) 3_755 ?
N1 C7 1.276(5) . ?
N1 C6 1.430(6) . ?
O1 C1 1.332(5) . ?
O1 Dy1 2.322(3) 3_755 ?
O2 C13 1.298(5) . ?
C1 C2 1.402(6) . ?
C1 C6 1.409(6) . ?
C2 C3 1.371(7) . ?
C2 H2 1.00(6) . ?
C3 C4 1.382(7) . ?
C3 H3 0.88(6) . ?
C4 C5 1.388(6) . ?
C4 H4 0.80(6) . ?
C5 C6 1.400(6) . ?
C5 H5 1.01(5) . ?
C7 C8 1.440(6) . ?
C7 H7 0.91(5) . ?
C8 C9 1.406(6) . ?
C8 C13 1.422(7) . ?
C9 C10 1.374(7) . ?
C9 H9 0.91(5) . ?
C10 C11 1.387(8) . ?
C10 H10 0.99(5) . ?
C11 C12 1.364(8) . ?
C11 H11 1.05(6) . ?
C12 C13 1.421(7) . ?
C12 H13 0.94(5) . ?
N2 O5 1.214(4) . ?
N2 O4 1.266(4) . ?
N2 O3 1.278(4) . ?
O6 C14 1.246(7) . ?
N3 C14 1.326(7) . ?
N3 C16 1.448(7) . ?
N3 C15 1.465(7) . ?
C14 H14 1.03(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N4 C17 1.305(7) . ?
N4 C18 1.452(8) . ?
N4 C19 1.463(8) . ?
O7 C17 1.222(7) . ?
C17 H17 1.14(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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 O7 80.59(12) . . ?
O2 Dy1 O1 84.76(10) . 3_755 ?
O7 Dy1 O1 91.96(10) . 3_755 ?
O2 Dy1 O1 122.56(10) . . ?
O7 Dy1 O1 149.56(11) . . ?
O1 Dy1 O1 72.80(10) 3_755 . ?
O2 Dy1 O6 146.87(11) . . ?
O7 Dy1 O6 73.31(12) . . ?
O1 Dy1 O6 76.24(9) 3_755 . ?
O1 Dy1 O6 77.45(10) . . ?
O2 Dy1 O3 131.17(10) . . ?
O7 Dy1 O3 99.63(11) . . ?
O1 Dy1 O3 143.45(9) 3_755 . ?
O1 Dy1 O3 80.15(9) . . ?
O6 Dy1 O3 74.22(10) . . ?
O2 Dy1 O4 82.09(11) . . ?
O7 Dy1 O4 75.83(11) . . ?
O1 Dy1 O4 163.33(9) 3_755 . ?
O1 Dy1 O4 123.18(9) . . ?
O6 Dy1 O4 110.12(10) . . ?
O3 Dy1 O4 51.72(9) . . ?
O2 Dy1 N1 72.91(11) . . ?
O7 Dy1 N1 143.80(12) . . ?
O1 Dy1 N1 109.32(10) 3_755 . ?
O1 Dy1 N1 66.54(10) . . ?
O6 Dy1 N1 139.00(11) . . ?
O3 Dy1 N1 80.71(11) . . ?
O4 Dy1 N1 76.47(10) . . ?
O2 Dy1 N2 106.83(11) . . ?
O7 Dy1 N2 87.18(11) . . ?
O1 Dy1 N2 168.04(10) 3_755 . ?
O1 Dy1 N2 102.33(10) . . ?
O6 Dy1 N2 92.12(9) . . ?
O3 Dy1 N2 25.96(10) . . ?
O4 Dy1 N2 25.77(9) . . ?
N1 Dy1 N2 77.64(10) . . ?
O2 Dy1 Dy1 106.13(8) . 3_755 ?
O7 Dy1 Dy1 123.85(9) . 3_755 ?
O1 Dy1 Dy1 36.41(6) 3_755 3_755 ?
O1 Dy1 Dy1 36.39(6) . 3_755 ?
O6 Dy1 Dy1 73.58(7) . 3_755 ?
O3 Dy1 Dy1 113.11(7) . 3_755 ?
O4 Dy1 Dy1 159.23(7) . 3_755 ?
N1 Dy1 Dy1 87.60(8) . 3_755 ?
N2 Dy1 Dy1 137.75(8) . 3_755 ?
C7 N1 C6 120.9(4) . . ?
C7 N1 Dy1 127.8(3) . . ?
C6 N1 Dy1 111.3(3) . . ?
C1 O1 Dy1 124.5(2) . 3_755 ?
C1 O1 Dy1 118.4(2) . . ?
Dy1 O1 Dy1 107.20(10) 3_755 . ?
C13 O2 Dy1 136.1(3) . . ?
O1 C1 C2 122.0(4) . . ?
O1 C1 C6 119.8(4) . . ?
C2 C1 C6 118.2(4) . . ?
C3 C2 C1 121.2(4) . . ?
C3 C2 H2 119(3) . . ?
C1 C2 H2 119(3) . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 H3 120(4) . . ?
C4 C3 H3 119(4) . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 123(4) . . ?
C5 C4 H4 117(4) . . ?
C4 C5 C6 119.9(4) . . ?
C4 C5 H5 120(3) . . ?
C6 C5 H5 120(3) . . ?
C5 C6 C1 120.1(4) . . ?
C5 C6 N1 125.5(4) . . ?
C1 C6 N1 114.4(4) . . ?
N1 C7 C8 126.3(4) . . ?
N1 C7 H7 117(3) . . ?
C8 C7 H7 116(3) . . ?
C9 C8 C13 119.4(4) . . ?
C9 C8 C7 117.0(4) . . ?
C13 C8 C7 123.5(4) . . ?
C10 C9 C8 121.8(5) . . ?
C10 C9 H9 119(3) . . ?
C8 C9 H9 119(3) . . ?
C9 C10 C11 118.9(4) . . ?
C9 C10 H10 123(3) . . ?
C11 C10 H10 118(3) . . ?
C12 C11 C10 121.0(5) . . ?
C12 C11 H11 114(3) . . ?
C10 C11 H11 125(3) . . ?
C11 C12 C13 122.0(5) . . ?
C11 C12 H13 121(3) . . ?
C13 C12 H13 117(3) . . ?
O2 C13 C12 120.7(5) . . ?
O2 C13 C8 122.5(4) . . ?
C12 C13 C8 116.8(4) . . ?
O5 N2 O4 122.3(4) . . ?
O5 N2 O3 122.3(4) . . ?
O4 N2 O3 115.4(3) . . ?
O5 N2 Dy1 178.4(3) . . ?
O4 N2 Dy1 58.45(18) . . ?
O3 N2 Dy1 56.98(18) . . ?
N2 O3 Dy1 97.1(2) . . ?
N2 O4 Dy1 95.8(2) . . ?
C14 O6 Dy1 132.0(4) . . ?
C14 N3 C16 120.8(5) . . ?
C14 N3 C15 121.0(5) . . ?
C16 N3 C15 118.2(5) . . ?
O6 C14 N3 121.6(5) . . ?
O6 C14 H14 122(3) . . ?
N3 C14 H14 117(3) . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 N4 C18 122.7(6) . . ?
C17 N4 C19 120.7(5) . . ?
C18 N4 C19 116.6(5) . . ?
C17 O7 Dy1 149.5(4) . . ?
O7 C17 N4 125.8(6) . . ?
O7 C17 H17 126(3) . . ?
N4 C17 H17 108(3) . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 H19A 109.5 . . ?
N4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        64.98
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.442
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.138
