# 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_xb8432_0m
_audit_block_doi                 10.5517/cc1jq2gs
_database_code_depnum_ccdc_archive 'CCDC 1421395'
_audit_update_record             
;
2015-10-13 deposited with the CCDC.
2015-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62 H62 Dy2 N8 O22'
_chemical_formula_weight         1596.20

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   p21/c

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

_cell_length_a                   13.432(2)
_cell_length_b                   10.503(2)
_cell_length_c                   24.428(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.478(4)
_cell_angle_gamma                90.00
_cell_volume                     3408.9(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3524
_cell_measurement_theta_min      1.96
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7973
_exptl_absorpt_correction_T_max  0.9019
_exptl_absorpt_process_details   SADABS

_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  'Bruker APEX SMART II'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16331
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_sigmaI/netI    0.1524
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5965
_reflns_number_gt                4465
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0350P)²+0.0560P] 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_number_reflns         5965
_refine_ls_number_parameters     391
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1904
_refine_ls_R_factor_gt           0.1549
_refine_ls_wR_factor_ref         0.2222
_refine_ls_wR_factor_gt          0.2116
_refine_ls_goodness_of_fit_ref   1.577
_refine_ls_restrained_S_all      1.574
_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
C23 C 0.5302(13) 0.0184(16) 0.3745(6) 0.085(8) Uani 1 1 d G . .
C22 C 0.5961(11) -0.084(2) 0.3749(7) 0.112(10) Uani 1 1 d G . .
H22 H 0.6463 -0.0823 0.3525 0.134 Uiso 1 1 calc R . .
C21 C 0.5869(11) -0.1880(16) 0.4088(8) 0.127(12) Uani 1 1 d G . .
H21 H 0.6310 -0.2563 0.4091 0.153 Uiso 1 1 calc R . .
C20 C 0.5118(12) -0.1901(13) 0.4423(7) 0.089(8) Uani 1 1 d G . .
H20 H 0.5057 -0.2599 0.4650 0.106 Uiso 1 1 calc R . .
C18 C 0.4459(9) -0.0880(15) 0.4419(6) 0.063(6) Uani 1 1 d G . .
C19 C 0.4551(10) 0.0163(12) 0.4080(7) 0.064(6) Uani 1 1 d G . .
C4 C 0.0242(11) 0.1695(15) 0.2809(7) 0.095(8) Uani 1 1 d G . .
H4 H 0.0765 0.2284 0.2857 0.114 Uiso 1 1 calc R . .
C5 C -0.0037(15) 0.1121(19) 0.2297(6) 0.140(14) Uani 1 1 d G . .
H5 H 0.0298 0.1326 0.2002 0.169 Uiso 1 1 calc R . .
C6 C -0.0818(15) 0.0241(18) 0.2226(5) 0.127(13) Uani 1 1 d G . .
H6 H -0.1005 -0.0143 0.1883 0.152 Uiso 1 1 calc R . .
C7 C -0.1319(12) -0.0066(15) 0.2667(8) 0.111(10) Uani 1 1 d G . .
H7 H -0.1842 -0.0655 0.2619 0.134 Uiso 1 1 calc R . .
C8 C -0.1040(12) 0.0507(15) 0.3179(6) 0.084(8) Uani 1 1 d G . .
H8 H -0.1375 0.0302 0.3474 0.101 Uiso 1 1 calc R . .
C3 C -0.0259(12) 0.1388(14) 0.3250(5) 0.068(6) Uani 1 1 d G . .
C26 C -0.2532(14) 0.4438(18) 0.2558(7) 0.144(13) Uani 1 1 d G . .
H26 H -0.2565 0.3762 0.2310 0.173 Uiso 1 1 calc R . .
C27 C -0.2961(13) 0.560(2) 0.2387(5) 0.131(13) Uani 1 1 d G . .
H27 H -0.3280 0.5707 0.2026 0.157 Uiso 1 1 calc R . .
C28 C -0.2912(12) 0.6615(17) 0.2758(7) 0.134(12) Uani 1 1 d G . .
H28 H -0.3198 0.7394 0.2644 0.161 Uiso 1 1 calc R . .
C31 C -0.2434(12) 0.6461(14) 0.3298(7) 0.095(8) Uani 1 1 d G . .
H31 H -0.2401 0.7137 0.3546 0.114 Uiso 1 1 calc R . .
C29 C -0.2005(10) 0.5295(16) 0.3469(5) 0.070(6) Uani 1 1 d G . .
C30 C -0.2054(13) 0.4284(13) 0.3098(8) 0.096(8) Uani 1 1 d G . .
H30 H -0.1768 0.3505 0.3213 0.115 Uiso 1 1 calc R . .
Dy1 Dy 0.05485(7) 0.35218(8) 0.47630(4) 0.0439(3) Uani 1 1 d . . .
O1 O -0.0260(9) 0.1672(11) 0.4225(5) 0.054(3) Uani 1 1 d . . .
O2 O 0.0724(10) 0.2924(13) 0.3817(5) 0.061(4) Uani 1 1 d . . .
C2 C 0.0113(15) 0.2035(18) 0.3800(9) 0.052(5) Uani 1 1 d . . .
O3 O 0.1765(9) 0.1899(12) 0.4845(5) 0.056(4) Uani 1 1 d . . .
N1 N 0.0249(11) 0.1704(14) 0.5419(6) 0.052(4) Uani 1 1 d . . .
N3 N 0.2316(11) -0.0120(15) 0.5068(7) 0.061(5) Uani 1 1 d . . .
H3 H 0.2258 -0.0813 0.5248 0.074 Uiso 1 1 calc R . .
N2 N 0.0917(11) 0.0707(15) 0.5388(6) 0.059(4) Uani 1 1 d . . .
H10A H 0.0842 -0.0008 0.5548 0.071 Uiso 1 1 calc R . .
C25 C 0.1668(14) 0.089(2) 0.5105(8) 0.051(5) Uani 1 1 d . . .
O4 O -0.0614(9) 0.4186(11) 0.5330(5) 0.056(3) Uani 1 1 d . . .
C11 C -0.1204(11) 0.3764(16) 0.5612(6) 0.035(4) Uani 1 1 d U . .
C13 C -0.0364(13) 0.160(2) 0.5767(7) 0.056(5) Uani 1 1 d U . .
H13 H -0.0314 0.0858 0.5979 0.067 Uiso 1 1 calc R . .
C12 C -0.1106(14) 0.2468(18) 0.5864(7) 0.049(5) Uani 1 1 d . . .
O6 O -0.2158(11) 0.5567(13) 0.5466(6) 0.074(4) Uani 1 1 d U . .
C16 C -0.2734(14) 0.392(2) 0.6071(9) 0.071(7) Uani 1 1 d . . .
H16 H -0.3258 0.4426 0.6159 0.085 Uiso 1 1 calc R . .
C10 C -0.2116(13) 0.4401(19) 0.5701(8) 0.056(5) Uani 1 1 d . . .
C15 C -0.2591(19) 0.273(2) 0.6309(8) 0.079(7) Uani 1 1 d . . .
H15 H -0.3033 0.2404 0.6534 0.094 Uiso 1 1 calc R . .
O5 O 0.5362(14) 0.120(2) 0.3408(9) 0.132(7) Uani 1 1 d . . .
C24 C 0.601(2) 0.125(4) 0.2994(14) 0.196(18) Uani 1 1 d . . .
H24A H 0.6692 0.1356 0.3168 0.294 Uiso 1 1 calc R . .
H24B H 0.5819 0.1965 0.2754 0.294 Uiso 1 1 calc R . .
H24C H 0.5946 0.0481 0.2782 0.294 Uiso 1 1 calc R . .
C14 C -0.1802(17) 0.206(2) 0.6205(8) 0.075(7) Uani 1 1 d . . .
H14 H -0.1701 0.1259 0.6369 0.090 Uiso 1 1 calc R . .
C9 C -0.3139(18) 0.610(3) 0.5382(11) 0.121(9) Uani 1 1 d U . .
H9A H -0.3626 0.5435 0.5292 0.181 Uiso 1 1 calc R . .
H9B H -0.3192 0.6702 0.5084 0.181 Uiso 1 1 calc R . .
H9C H -0.3262 0.6523 0.5714 0.181 Uiso 1 1 calc R . .
O11 O 0.3971(13) 0.1199(15) 0.4058(7) 0.098(5) Uani 1 1 d . . .
H11 H 0.3562 0.1119 0.4274 0.147 Uiso 1 1 calc R . .
C32 C -0.1452(14) 0.522(2) 0.4076(9) 0.054(5) Uani 1 1 d . . .
O7 O -0.0931(10) 0.4204(13) 0.4161(5) 0.067(4) Uani 1 1 d . . .
O8 O -0.1540(9) 0.6045(11) 0.4396(5) 0.055(4) Uani 1 1 d . . .
O9 O 0.2432(11) 0.7750(13) 0.5757(7) 0.115(6) Uani 1 1 d D . .
O10 O 0.449(4) 0.592(3) 0.6070(14) 0.59(3) Uani 1 1 d DU . .
N5 N 0.3046(12) 0.0006(16) 0.4744(7) 0.063(5) Uani 1 1 d . . .
C34 C 0.3665(12) -0.0916(15) 0.4746(8) 0.064(6) Uani 1 1 d U . .
H34 H 0.3595 -0.1626 0.4965 0.077 Uiso 1 1 calc R . .
H1W H 0.2756 0.8443 0.5702 0.096 Uiso 1 1 d RD . .
H2W H 0.2741 0.7067 0.5687 0.096 Uiso 1 1 d RD . .
H3W H 0.4367 0.6530 0.5849 0.096 Uiso 1 1 d RD . .
H4W H 0.4825 0.6068 0.6393 0.096 Uiso 1 1 d RD . .


_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
C23 O5 1.35(2) . ?
C23 C22 1.3900 . ?
C23 C19 1.3900 . ?
C22 C21 1.3900 . ?
C21 C20 1.3900 . ?
C20 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 C34 1.425(19) . ?
C19 O11 1.335(16) . ?
C4 C5 1.3900 . ?
C4 C3 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C8 C3 1.3900 . ?
C3 C2 1.52(2) . ?
C26 C27 1.3900 . ?
C26 C30 1.3900 . ?
C27 C28 1.3900 . ?
C28 C31 1.3900 . ?
C31 C29 1.3900 . ?
C29 C30 1.3900 . ?
C29 C32 1.56(2) . ?
Dy1 O8 2.322(12) 3_566 ?
Dy1 O4 2.341(12) . ?
Dy1 O3 2.349(12) . ?
Dy1 O7 2.401(14) . ?
Dy1 O4 2.421(11) 3_566 ?
Dy1 O2 2.439(12) . ?
Dy1 O6 2.502(14) 3_566 ?
Dy1 O1 2.503(12) . ?
Dy1 N1 2.563(15) . ?
Dy1 Dy1 3.6957(18) 3_566 ?
O1 C2 1.276(19) . ?
O2 C2 1.24(2) . ?
O3 C25 1.25(2) . ?
N1 C13 1.27(2) . ?
N1 N2 1.389(18) . ?
N3 N5 1.355(18) . ?
N3 C25 1.382(19) . ?
N2 C25 1.32(2) . ?
O4 C11 1.208(17) . ?
O4 Dy1 2.421(11) 3_566 ?
C11 C10 1.44(2) . ?
C11 C12 1.49(2) . ?
C13 C12 1.40(2) . ?
C12 C14 1.41(2) . ?
O6 C10 1.35(2) . ?
O6 C9 1.42(2) . ?
O6 Dy1 2.502(14) 3_566 ?
C16 C15 1.38(3) . ?
C16 C10 1.41(3) . ?
C15 C14 1.33(3) . ?
O5 C24 1.43(3) . ?
C32 O8 1.19(2) . ?
C32 O7 1.27(2) . ?
O8 Dy1 2.322(12) 3_566 ?
N5 C34 1.276(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 C23 C22 121.0(16) . . ?
O5 C23 C19 119.0(16) . . ?
C22 C23 C19 120.0 . . ?
C23 C22 C21 120.0 . . ?
C22 C21 C20 120.0 . . ?
C18 C20 C21 120.0 . . ?
C19 C18 C20 120.0 . . ?
C19 C18 C34 119.7(13) . . ?
C20 C18 C34 120.3(13) . . ?
O11 C19 C18 124.3(14) . . ?
O11 C19 C23 115.7(14) . . ?
C18 C19 C23 120.0 . . ?
C5 C4 C3 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C7 C8 C3 120.0 . . ?
C8 C3 C4 120.0 . . ?
C8 C3 C2 123.4(14) . . ?
C4 C3 C2 116.6(14) . . ?
C27 C26 C30 120.0 . . ?
C26 C27 C28 120.0 . . ?
C31 C28 C27 120.0 . . ?
C29 C31 C28 120.0 . . ?
C30 C29 C31 120.0 . . ?
C30 C29 C32 123.2(14) . . ?
C31 C29 C32 116.8(14) . . ?
C29 C30 C26 120.0 . . ?
O8 Dy1 O4 76.3(4) 3_566 . ?
O8 Dy1 O3 76.5(4) 3_566 . ?
O4 Dy1 O3 133.0(4) . . ?
O8 Dy1 O7 143.0(4) 3_566 . ?
O4 Dy1 O7 73.1(4) . . ?
O3 Dy1 O7 140.5(4) . . ?
O8 Dy1 O4 82.2(4) 3_566 3_566 ?
O4 Dy1 O4 78.2(4) . 3_566 ?
O3 Dy1 O4 134.0(4) . 3_566 ?
O7 Dy1 O4 71.6(4) . 3_566 ?
O8 Dy1 O2 139.9(4) 3_566 . ?
O4 Dy1 O2 143.4(4) . . ?
O3 Dy1 O2 74.4(4) . . ?
O7 Dy1 O2 71.5(4) . . ?
O4 Dy1 O2 99.1(4) 3_566 . ?
O8 Dy1 O6 73.8(5) 3_566 3_566 ?
O4 Dy1 O6 133.8(4) . 3_566 ?
O3 Dy1 O6 71.6(4) . 3_566 ?
O7 Dy1 O6 114.4(5) . 3_566 ?
O4 Dy1 O6 63.5(4) 3_566 3_566 ?
O2 Dy1 O6 71.3(5) . 3_566 ?
O8 Dy1 O1 139.9(4) 3_566 . ?
O4 Dy1 O1 105.4(4) . . ?
O3 Dy1 O1 74.0(4) . . ?
O7 Dy1 O1 69.8(4) . . ?
O4 Dy1 O1 137.9(4) 3_566 . ?
O2 Dy1 O1 53.0(4) . . ?
O6 Dy1 O1 120.2(4) 3_566 . ?
O8 Dy1 N1 73.5(4) 3_566 . ?
O4 Dy1 N1 70.8(4) . . ?
O3 Dy1 N1 65.0(4) . . ?
O7 Dy1 N1 114.4(5) . . ?
O4 Dy1 N1 144.2(4) 3_566 . ?
O2 Dy1 N1 116.5(4) . . ?
O6 Dy1 N1 130.2(5) 3_566 . ?
O1 Dy1 N1 69.7(4) . . ?
O8 Dy1 Dy1 76.2(3) 3_566 3_566 ?
O4 Dy1 Dy1 39.9(3) . 3_566 ?
O3 Dy1 Dy1 152.6(3) . 3_566 ?
O7 Dy1 Dy1 67.0(3) . 3_566 ?
O4 Dy1 Dy1 38.3(3) 3_566 3_566 ?
O2 Dy1 Dy1 127.7(3) . 3_566 ?
O6 Dy1 Dy1 98.4(3) 3_566 3_566 ?
O1 Dy1 Dy1 130.9(3) . 3_566 ?
N1 Dy1 Dy1 108.9(3) . 3_566 ?
C2 O1 Dy1 90.1(12) . . ?
C2 O2 Dy1 94.0(12) . . ?
O2 C2 O1 122(2) . . ?
O2 C2 C3 119.7(17) . . ?
O1 C2 C3 117.8(18) . . ?
C25 O3 Dy1 122.3(11) . . ?
C13 N1 N2 117.2(16) . . ?
C13 N1 Dy1 131.3(14) . . ?
N2 N1 Dy1 111.4(10) . . ?
N5 N3 C25 118.7(17) . . ?
C25 N2 N1 118.1(16) . . ?
O3 C25 N2 122.2(16) . . ?
O3 C25 N3 120.1(18) . . ?
N2 C25 N3 117.5(19) . . ?
C11 O4 Dy1 141.1(11) . . ?
C11 O4 Dy1 117.0(11) . 3_566 ?
Dy1 O4 Dy1 101.8(4) . 3_566 ?
O4 C11 C10 124.0(17) . . ?
O4 C11 C12 123.0(15) . . ?
C10 C11 C12 112.8(15) . . ?
N1 C13 C12 127(2) . . ?
C13 C12 C14 116.7(19) . . ?
C13 C12 C11 123.3(17) . . ?
C14 C12 C11 119.9(16) . . ?
C10 O6 C9 113.5(18) . . ?
C10 O6 Dy1 117.4(12) . 3_566 ?
C9 O6 Dy1 129.2(14) . 3_566 ?
C15 C16 C10 122.3(19) . . ?
O6 C10 C16 127.3(16) . . ?
O6 C10 C11 109.9(16) . . ?
C16 C10 C11 121.8(18) . . ?
C14 C15 C16 118(2) . . ?
C23 O5 C24 124(2) . . ?
C15 C14 C12 125(2) . . ?
O8 C32 O7 127.6(19) . . ?
O8 C32 C29 120.5(18) . . ?
O7 C32 C29 111.9(18) . . ?
C32 O7 Dy1 137.3(13) . . ?
C32 O8 Dy1 128.8(13) . 3_566 ?
C34 N5 N3 116.7(16) . . ?
N5 C34 C18 121.2(17) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.325
_refine_diff_density_min         -2.542
_refine_diff_density_rms         0.169
