# 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).
# 
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# 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 
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data_lixl-Dy6-NO3
_database_code_depnum_ccdc_archive 'CCDC 1419275'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;
_audit_creation_date             2015-05-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        lixl-Dy6-NO3
_chemical_formula_moiety         'C44 H54 Dy6 N14 O38, 10(O), 2(N O3)'
_chemical_formula_sum            'C44 H54 Dy6 N16 O54'
_chemical_formula_weight         2646.03
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7890(11)
_cell_length_b                   12.7071(13)
_cell_length_c                   16.9727(18)
_cell_angle_alpha                100.954(2)
_cell_angle_beta                 100.243(2)
_cell_angle_gamma                109.293(2)
_cell_volume                     2082.3(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5464
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.09
_cell_measurement_theta_min      2.43
_shelx_estimated_absorpt_T_max   0.613
_shelx_estimated_absorpt_T_min   0.293
_exptl_absorpt_coefficient_mu    5.427
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   (sadabs;bruker,2000)
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11482
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.762
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5452
_reflns_number_total             6956
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.984
_refine_diff_density_min         -1.509
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         6956
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0457
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0765P)²+8.7372P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1393
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H7-O7
 0.9 with sigma of 0.02
 H7-Dy3
 2.9 with sigma of 0.02
 H7-Dy2
 2.9 with sigma of 0.02
 H3-Dy2
 2.9 with sigma of 0.02
 H3-O3
 0.9 with sigma of 0.02
 O14-O15 \\sim O15-O16
 with sigma of 0.01
 O15-N6 \\sim O16-N6 \\sim O14-N6
 with sigma of 0.01
 O22-O20 \\sim O20-O21
 with sigma of 0.02
 O20-O21 \\sim O20-O22 \\sim O22-O21
 with sigma of 0.01
3. Rigid bond restraints
 O14, O15, O16, N6
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O20, O21, O22, N8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
O20 \\sim O21 \\sim O22 \\sim N8: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O14 \\sim O15 \\sim O16 \\sim N6: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5.a Rotating group:
 O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.29408(5) 0.24385(4) 0.28488(3) 0.02978(15) Uani 1 1 d . . . . .
Dy2 Dy 0.38581(5) 0.01547(4) 0.19676(3) 0.02663(15) Uani 1 1 d D . . . .
Dy3 Dy 0.41015(5) 0.24449(4) 0.10424(3) 0.02579(15) Uani 1 1 d D . . . .
O1 O 0.1821(9) 0.1736(7) 0.3914(5) 0.046(2) Uani 1 1 d . . . . .
O2 O 0.3214(8) 0.0786(6) 0.3142(4) 0.0347(18) Uani 1 1 d . . . . .
O3 O 0.4446(7) 0.0744(6) 0.0851(4) 0.0260(15) Uani 1 1 d D . . . .
H3 H 0.498(17) 0.052(14) 0.057(8) 0.15(9) Uiso 1 1 d D . . . .
O4 O 0.3203(8) 0.3511(6) 0.1855(4) 0.0339(17) Uani 1 1 d . . . . .
O5 O 0.2688(9) 0.4334(7) 0.3236(4) 0.0415(19) Uani 1 1 d . . . . .
O6 O 0.4787(8) 0.2333(6) 0.2408(4) 0.0287(16) Uani 1 1 d . . . . .
H6 H 0.563(13) 0.281(10) 0.275(7) 0.04(3) Uiso 1 1 d . . . . .
O7 O 0.2507(6) 0.1164(6) 0.1606(4) 0.0253(14) Uani 1 1 d D . . . .
H7 H 0.1665(15) 0.082(3) 0.129(3) 0.02(3) Uiso 1 1 d D . . . .
O8 O 0.4643(9) 0.3437(8) 0.4090(5) 0.053(2) Uani 1 1 d . . . . .
H8A H 0.5134 0.3037 0.4192 0.079 Uiso 1 1 d GR . . . .
H8B H 0.4285 0.3550 0.4500 0.079 Uiso 1 1 d GR . . . .
O9 O 0.0594(8) 0.2028(8) 0.2336(5) 0.049(2) Uani 1 1 d . . . . .
H9A H 0.0489 0.2485 0.2037 0.073 Uiso 1 1 d GR . . . .
H9B H 0.0232 0.2128 0.2744 0.073 Uiso 1 1 d GR . . . .
O10 O 0.6247(8) 0.0795(8) 0.2600(6) 0.055(2) Uani 1 1 d . . . . .
H10A H 0.6605 0.1551 0.2839 0.082 Uiso 1 1 d GR . . . .
H10B H 0.6690 0.0652 0.2226 0.082 Uiso 1 1 d GR . . . .
O11 O 0.2019(9) -0.1225(8) 0.0671(5) 0.053(2) Uani 1 1 d . . . . .
O12 O 0.1563(9) -0.1357(8) 0.1814(6) 0.052(2) Uani 1 1 d . . . . .
O13 O 0.0137(11) -0.2497(10) 0.0677(7) 0.079(3) Uani 1 1 d . . . . .
O14 O 0.2084(9) 0.1378(8) -0.0079(5) 0.057(2) Uani 1 1 d D U . . .
O15 O 0.0286(18) 0.0658(19) 0.0304(10) 0.224(12) Uani 1 1 d D U . A -1
O16 O 0.0306(18) 0.021(2) -0.0971(9) 0.241(13) Uani 1 1 d D U . . .
O17 O 0.6640(8) 0.2964(7) 0.1329(5) 0.0417(19) Uani 1 1 d . . . . .
O18 O 0.6003(9) 0.4391(7) 0.1362(5) 0.045(2) Uani 1 1 d . . . . .
O19 O 0.8090(9) 0.4622(10) 0.1373(7) 0.073(3) Uani 1 1 d . . . . .
N1 N 0.4242(10) -0.1072(8) 0.2947(5) 0.036(2) Uani 1 1 d . . . . .
N2 N 0.4528(9) -0.1491(8) 0.1392(5) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.4754(9) 0.2418(7) -0.0322(5) 0.029(2) Uani 1 1 d . . . . .
N4 N 0.3406(9) 0.3762(7) 0.0222(5) 0.0280(19) Uani 1 1 d . . . . .
N5 N 0.1175(11) -0.1731(9) 0.1040(7) 0.046(3) Uani 1 1 d . . . . .
N6 N 0.0904(11) 0.0713(16) -0.0236(8) 0.121(6) Uani 1 1 d D U . . .
N7 N 0.6963(10) 0.4006(9) 0.1355(6) 0.042(2) Uani 1 1 d . . . . .
C1 C 0.0820(15) 0.2058(14) 0.4218(9) 0.064(4) Uani 1 1 d . . . . .
H1A H 0.1230 0.2590 0.4761 0.097 Uiso 1 1 calc GR . . . .
H1B H 0.0116 0.1381 0.4251 0.097 Uiso 1 1 calc GR . . . .
H1C H 0.0436 0.2421 0.3849 0.097 Uiso 1 1 calc GR . . . .
C2 C 0.2219(11) 0.0957(9) 0.4261(7) 0.034(2) Uani 1 1 d . . . . .
C3 C 0.1969(13) 0.0699(12) 0.4977(8) 0.047(3) Uani 1 1 d . . . . .
H3A H 0.1488 0.1047 0.5266 0.056 Uiso 1 1 calc R . . . .
C4 C 0.2437(15) -0.0087(12) 0.5276(8) 0.056(4) Uani 1 1 d . . . . .
H4 H 0.2304 -0.0235 0.5777 0.067 Uiso 1 1 calc R . . . .
C5 C 0.3090(15) -0.0642(13) 0.4834(8) 0.059(4) Uani 1 1 d . . . . .
H5 H 0.3376 -0.1179 0.5034 0.071 Uiso 1 1 calc R . . . .
C6 C 0.3345(12) -0.0412(10) 0.4065(7) 0.037(3) Uani 1 1 d . . . . .
C7 C 0.2933(11) 0.0427(9) 0.3795(6) 0.028(2) Uani 1 1 d . . . . .
C8 C 0.4006(12) -0.1065(10) 0.3673(7) 0.040(3) Uani 1 1 d . . . . .
H8 H 0.4298 -0.1532 0.3958 0.048 Uiso 1 1 calc R . . . .
C9 C 0.4893(10) -0.1804(9) 0.2706(6) 0.026(2) Uani 1 1 d . . . . .
H9 H 0.5259 -0.2127 0.3089 0.031 Uiso 1 1 calc R . . . .
C10 C 0.5002(11) -0.2053(9) 0.1915(6) 0.030(2) Uani 1 1 d . . . . .
C11 C 0.5321(11) 0.1725(9) -0.0627(6) 0.028(2) Uani 1 1 d . . . . .
H11 H 0.5656 0.1356 -0.0267 0.034 Uiso 1 1 calc R . . . .
C12 C 0.4423(12) 0.2815(10) -0.1646(6) 0.039(3) Uani 1 1 d . . . . .
H12 H 0.4148 0.3229 -0.1991 0.046 Uiso 1 1 calc R . . . .
C13 C 0.4261(12) 0.2955(9) -0.0858(6) 0.032(2) Uani 1 1 d . . . . .
C14 C 0.3622(11) 0.3640(8) -0.0567(5) 0.025(2) Uani 1 1 d . . . . .
H14 H 0.3317 0.4044 -0.0909 0.031 Uiso 1 1 calc R . . . .
C15 C 0.2797(11) 0.4423(9) 0.0393(6) 0.032(2) Uani 1 1 d . . . . .
H15 H 0.2499 0.4713 -0.0036 0.038 Uiso 1 1 calc R . . . .
C16 C 0.2493(11) 0.4800(9) 0.1176(7) 0.034(2) Uani 1 1 d . . . . .
C17 C 0.1879(14) 0.5608(11) 0.1225(8) 0.051(3) Uani 1 1 d . . . . .
H17 H 0.1695 0.5888 0.0767 0.061 Uiso 1 1 calc R . . . .
C18 C 0.1542(15) 0.6001(11) 0.1934(8) 0.051(3) Uani 1 1 d . . . . .
H18 H 0.1118 0.6531 0.1948 0.061 Uiso 1 1 calc R . . . .
C19 C 0.1820(14) 0.5625(11) 0.2613(8) 0.047(3) Uani 1 1 d . . . . .
H19 H 0.1623 0.5920 0.3099 0.056 Uiso 1 1 calc R . . . .
C20 C 0.2391(13) 0.4813(10) 0.2581(7) 0.040(3) Uani 1 1 d . . . . .
C21 C 0.2745(11) 0.4377(10) 0.1863(6) 0.033(3) Uani 1 1 d . . . . .
C22 C 0.2438(15) 0.4790(12) 0.3997(7) 0.055(3) Uani 1 1 d . . . . .
H22A H 0.1478 0.4590 0.3924 0.082 Uiso 1 1 calc GR . . . .
H22B H 0.2893 0.5617 0.4165 0.082 Uiso 1 1 calc GR . . . .
H22C H 0.2776 0.4470 0.4418 0.082 Uiso 1 1 calc GR . . . .
O25 O 0.8292(15) 0.0119(14) 0.2192(9) 0.122(5) Uani 1 1 d . . . . .
O24 O 0.7030(9) 0.0620(8) 0.0806(6) 0.056(2) Uani 1 1 d . . . . .
O20 O 0.6218(15) 0.5915(13) 0.4410(7) 0.113(5) Uani 1 1 d D U . . .
O21 O 0.5197(16) 0.6998(13) 0.4199(10) 0.147(6) Uani 1 1 d D U . . .
O22 O 0.618(2) 0.650(2) 0.3347(10) 0.215(10) Uani 1 1 d D U . . .
N8 N 0.5903(14) 0.6497(13) 0.3977(8) 0.078(4) Uani 1 1 d . U . . .
O26 O 0.075(3) 0.147(3) 0.729(2) 0.285(14) Uani 1 1 d . U . . .
O23 O 0.9368(9) 0.2738(8) 0.1111(6) 0.058(2) Uani 1 1 d . . . . .
O27 O 0.769(3) 0.304(3) 0.394(2) 0.291(15) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Dy2 3.5232(7) . ?
Dy1 Dy3 3.5123(7) . ?
Dy1 O1 2.490(7) . ?
Dy1 O2 2.345(7) . ?
Dy1 O4 2.360(6) . ?
Dy1 O5 2.491(7) . ?
Dy1 O6 2.283(7) . ?
Dy1 O7 2.268(6) . ?
Dy1 O8 2.343(8) . ?
Dy1 O9 2.369(8) . ?
Dy2 Dy3 3.5189(7) . ?
Dy2 O2 2.313(6) . ?
Dy2 O3 2.283(6) . ?
Dy2 O6 2.518(7) . ?
Dy2 O7 2.316(6) . ?
Dy2 O10 2.399(8) . ?
Dy2 O11 2.557(9) . ?
Dy2 O12 2.514(9) . ?
Dy2 N1 2.556(8) . ?
Dy2 N2 2.514(8) . ?
Dy3 O3 2.285(6) . ?
Dy3 O4 2.305(6) . ?
Dy3 O6 2.350(7) . ?
Dy3 O7 2.419(6) . ?
Dy3 O14 2.407(9) . ?
Dy3 O17 2.526(8) . ?
Dy3 O18 2.522(8) . ?
Dy3 N3 2.535(8) . ?
Dy3 N4 2.577(8) . ?
O1 C1 1.418(13) . ?
O1 C2 1.388(13) . ?
O2 C7 1.322(11) . ?
O4 C21 1.346(11) . ?
O5 C20 1.402(12) . ?
O5 C22 1.422(13) . ?
O11 N5 1.267(13) . ?
O12 N5 1.249(13) . ?
O13 N5 1.178(14) . ?
O14 N6 1.220(10) . ?
O15 N6 1.226(10) . ?
O16 N6 1.232(10) . ?
O17 N7 1.243(12) . ?
O18 N7 1.284(12) . ?
O19 N7 1.200(13) . ?
N1 C8 1.301(13) . ?
N1 C9 1.384(12) . ?
N2 C10 1.371(12) . ?
N2 C11 1.328(12) 2_655 ?
N3 C11 1.309(12) . ?
N3 C13 1.370(12) . ?
N4 C14 1.390(11) . ?
N4 C15 1.251(12) . ?
C2 C3 1.367(15) . ?
C2 C7 1.425(14) . ?
C3 C4 1.394(17) . ?
C4 C5 1.367(17) . ?
C5 C6 1.444(15) . ?
C6 C7 1.405(14) . ?
C6 C8 1.410(15) . ?
C9 C10 1.355(13) . ?
C10 C12 1.364(14) 2_655 ?
C11 N2 1.328(12) 2_655 ?
C12 C10 1.364(14) 2_655 ?
C12 C13 1.367(14) . ?
C13 C14 1.353(13) . ?
C15 C16 1.455(14) . ?
C16 C17 1.392(14) . ?
C16 C21 1.395(14) . ?
C17 C18 1.370(16) . ?
C18 C19 1.352(16) . ?
C19 C20 1.364(15) . ?
C20 C21 1.410(14) . ?
O20 N8 1.218(15) . ?
O21 N8 1.208(17) . ?
O22 N8 1.163(17) . ?

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
Dy3 Dy1 Dy2 60.022(13) . . ?
O1 Dy1 Dy2 103.66(18) . . ?
O1 Dy1 Dy3 161.1(2) . . ?
O1 Dy1 O5 92.2(2) . . ?
O2 Dy1 Dy2 40.51(15) . . ?
O2 Dy1 Dy3 100.34(15) . . ?
O2 Dy1 O1 64.8(2) . . ?
O2 Dy1 O4 140.9(2) . . ?
O2 Dy1 O5 153.2(2) . . ?
O2 Dy1 O9 109.1(3) . . ?
O4 Dy1 Dy2 100.38(16) . . ?
O4 Dy1 Dy3 40.56(16) . . ?
O4 Dy1 O1 151.9(2) . . ?
O4 Dy1 O5 65.0(2) . . ?
O4 Dy1 O9 84.1(3) . . ?
O5 Dy1 Dy2 163.93(18) . . ?
O5 Dy1 Dy3 104.73(17) . . ?
O6 Dy1 Dy2 45.46(18) . . ?
O6 Dy1 Dy3 41.42(17) . . ?
O6 Dy1 O1 134.5(2) . . ?
O6 Dy1 O2 74.1(2) . . ?
O6 Dy1 O4 73.3(2) . . ?
O6 Dy1 O5 120.2(3) . . ?
O6 Dy1 O8 80.4(3) . . ?
O6 Dy1 O9 141.2(3) . . ?
O7 Dy1 Dy2 40.27(16) . . ?
O7 Dy1 Dy3 43.12(16) . . ?
O7 Dy1 O1 118.5(3) . . ?
O7 Dy1 O2 73.5(2) . . ?
O7 Dy1 O4 72.9(2) . . ?
O7 Dy1 O5 132.5(2) . . ?
O7 Dy1 O6 63.5(2) . . ?
O7 Dy1 O8 141.5(3) . . ?
O7 Dy1 O9 80.0(3) . . ?
O8 Dy1 Dy2 104.3(2) . . ?
O8 Dy1 Dy3 114.5(2) . . ?
O8 Dy1 O1 77.2(3) . . ?
O8 Dy1 O2 84.6(3) . . ?
O8 Dy1 O4 110.6(3) . . ?
O8 Dy1 O5 76.5(3) . . ?
O8 Dy1 O9 137.8(3) . . ?
O9 Dy1 Dy2 111.8(2) . . ?
O9 Dy1 Dy3 102.3(2) . . ?
O9 Dy1 O1 73.7(3) . . ?
O9 Dy1 O5 74.8(3) . . ?
Dy3 Dy2 Dy1 59.835(14) . . ?
O2 Dy2 Dy1 41.19(16) . . ?
O2 Dy2 Dy3 100.83(16) . . ?
O2 Dy2 O6 70.4(2) . . ?
O2 Dy2 O7 73.2(2) . . ?
O2 Dy2 O10 97.7(3) . . ?
O2 Dy2 O11 118.9(3) . . ?
O2 Dy2 O12 75.2(3) . . ?
O2 Dy2 N1 73.3(3) . . ?
O2 Dy2 N2 136.7(2) . . ?
O3 Dy2 Dy1 99.46(16) . . ?
O3 Dy2 Dy3 39.63(16) . . ?
O3 Dy2 O2 140.4(2) . . ?
O3 Dy2 O6 73.7(2) . . ?
O3 Dy2 O7 74.4(2) . . ?
O3 Dy2 O10 87.0(3) . . ?
O3 Dy2 O11 72.9(3) . . ?
O3 Dy2 O12 121.0(3) . . ?
O3 Dy2 N1 143.3(3) . . ?
O3 Dy2 N2 82.6(2) . . ?
O6 Dy2 Dy1 40.26(15) . . ?
O6 Dy2 Dy3 41.85(15) . . ?
O6 Dy2 O11 128.7(3) . . ?
O6 Dy2 N1 123.2(3) . . ?
O7 Dy2 Dy1 39.27(16) . . ?
O7 Dy2 Dy3 43.13(16) . . ?
O7 Dy2 O6 59.2(2) . . ?
O7 Dy2 O10 131.5(3) . . ?
O7 Dy2 O11 74.9(3) . . ?
O7 Dy2 O12 80.8(2) . . ?
O7 Dy2 N1 142.0(3) . . ?
O7 Dy2 N2 142.6(2) . . ?
O10 Dy2 Dy1 104.4(2) . . ?
O10 Dy2 Dy3 95.9(2) . . ?
O10 Dy2 O6 72.7(3) . . ?
O10 Dy2 O11 141.4(3) . . ?
O10 Dy2 O12 144.3(3) . . ?
O10 Dy2 N1 70.8(3) . . ?
O10 Dy2 N2 74.8(3) . . ?
O11 Dy2 Dy1 111.0(2) . . ?
O11 Dy2 Dy3 89.1(2) . . ?
O12 Dy2 Dy1 93.0(2) . . ?
O12 Dy2 Dy3 119.74(19) . . ?
O12 Dy2 O6 132.8(2) . . ?
O12 Dy2 O11 49.1(3) . . ?
O12 Dy2 N1 73.7(3) . . ?
N1 Dy2 Dy1 113.9(2) . . ?
N1 Dy2 Dy3 164.1(2) . . ?
N1 Dy2 O11 106.7(3) . . ?
N2 Dy2 Dy1 177.80(18) . . ?
N2 Dy2 Dy3 122.18(18) . . ?
N2 Dy2 O6 140.4(3) . . ?
N2 Dy2 O11 70.3(3) . . ?
N2 Dy2 O12 86.6(3) . . ?
N2 Dy2 N1 63.9(3) . . ?
Dy1 Dy3 Dy2 60.143(13) . . ?
O3 Dy3 Dy1 99.72(16) . . ?
O3 Dy3 Dy2 39.58(16) . . ?
O3 Dy3 O4 141.0(2) . . ?
O3 Dy3 O6 77.0(2) . . ?
O3 Dy3 O7 72.4(2) . . ?
O3 Dy3 O14 84.9(3) . . ?
O3 Dy3 O17 73.1(2) . . ?
O3 Dy3 O18 123.0(3) . . ?
O3 Dy3 N3 81.7(2) . . ?
O3 Dy3 N4 141.4(2) . . ?
O4 Dy3 Dy1 41.75(16) . . ?
O4 Dy3 Dy2 101.68(16) . . ?
O4 Dy3 O6 73.1(2) . . ?
O4 Dy3 O7 71.2(2) . . ?
O4 Dy3 O14 97.9(3) . . ?
O4 Dy3 O17 120.9(3) . . ?
O4 Dy3 O18 82.2(3) . . ?
O4 Dy3 N3 136.2(2) . . ?
O4 Dy3 N4 72.3(2) . . ?
O6 Dy3 Dy1 40.00(16) . . ?
O6 Dy3 Dy2 45.63(18) . . ?
O6 Dy3 O7 60.3(2) . . ?
O6 Dy3 O14 133.7(3) . . ?
O6 Dy3 O17 74.8(2) . . ?
O6 Dy3 O18 90.7(3) . . ?
O6 Dy3 N3 144.2(2) . . ?
O6 Dy3 N4 141.6(2) . . ?
O7 Dy3 Dy1 39.85(15) . . ?
O7 Dy3 Dy2 40.88(15) . . ?
O7 Dy3 O17 127.9(2) . . ?
O7 Dy3 O18 144.9(2) . . ?
O7 Dy3 N3 137.9(3) . . ?
O7 Dy3 N4 121.4(2) . . ?
O14 Dy3 Dy1 104.5(2) . . ?
O14 Dy3 Dy2 95.50(19) . . ?
O14 Dy3 O7 73.7(2) . . ?
O14 Dy3 O17 139.2(3) . . ?
O14 Dy3 O18 134.0(3) . . ?
O14 Dy3 N3 71.4(3) . . ?
O14 Dy3 N4 67.9(3) . . ?
O17 Dy3 Dy1 112.75(18) . . ?
O17 Dy3 Dy2 89.05(16) . . ?
O17 Dy3 N3 71.6(3) . . ?
O17 Dy3 N4 109.9(3) . . ?
O18 Dy3 Dy1 105.27(19) . . ?
O18 Dy3 Dy2 129.80(18) . . ?
O18 Dy3 O17 50.1(3) . . ?
O18 Dy3 N3 77.2(3) . . ?
O18 Dy3 N4 68.5(3) . . ?
N3 Dy3 Dy1 175.60(19) . . ?
N3 Dy3 Dy2 121.22(18) . . ?
N3 Dy3 N4 64.3(2) . . ?
N4 Dy3 Dy1 112.95(17) . . ?
N4 Dy3 Dy2 160.68(19) . . ?
C1 O1 Dy1 127.0(7) . . ?
C2 O1 Dy1 117.4(6) . . ?
C2 O1 C1 115.6(9) . . ?
Dy2 O2 Dy1 98.3(2) . . ?
C7 O2 Dy1 123.4(6) . . ?
C7 O2 Dy2 138.1(6) . . ?
Dy2 O3 Dy3 100.8(3) . . ?
Dy3 O4 Dy1 97.7(2) . . ?
C21 O4 Dy1 121.5(6) . . ?
C21 O4 Dy3 140.5(6) . . ?
C20 O5 Dy1 116.3(6) . . ?
C20 O5 C22 116.5(9) . . ?
C22 O5 Dy1 124.7(7) . . ?
Dy1 O6 Dy2 94.3(3) . . ?
Dy1 O6 Dy3 98.6(3) . . ?
Dy3 O6 Dy2 92.5(3) . . ?
Dy1 O7 Dy2 100.5(2) . . ?
Dy1 O7 Dy3 97.0(2) . . ?
Dy2 O7 Dy3 96.0(2) . . ?
N5 O11 Dy2 97.3(7) . . ?
N5 O12 Dy2 99.9(7) . . ?
N6 O14 Dy3 142.8(8) . . ?
N7 O17 Dy3 97.3(6) . . ?
N7 O18 Dy3 96.3(6) . . ?
C8 N1 Dy2 130.1(7) . . ?
C8 N1 C9 113.8(8) . . ?
C9 N1 Dy2 115.9(6) . . ?
C10 N2 Dy2 119.9(6) . . ?
C11 N2 Dy2 123.0(6) 2_655 . ?
C11 N2 C10 116.1(8) 2_655 . ?
C11 N3 Dy3 122.8(6) . . ?
C11 N3 C13 115.9(8) . . ?
C13 N3 Dy3 119.9(6) . . ?
C14 N4 Dy3 115.3(5) . . ?
C15 N4 Dy3 130.0(6) . . ?
C15 N4 C14 114.3(8) . . ?
O12 N5 O11 113.7(11) . . ?
O13 N5 O11 122.1(12) . . ?
O13 N5 O12 124.1(11) . . ?
O14 N6 O15 120.8(9) . . ?
O14 N6 O16 117.8(15) . . ?
O15 N6 O16 120.8(10) . . ?
O17 N7 O18 115.4(10) . . ?
O19 N7 O17 123.1(11) . . ?
O19 N7 O18 121.5(11) . . ?
O1 C2 C7 113.4(9) . . ?
C3 C2 O1 124.9(10) . . ?
C3 C2 C7 121.7(10) . . ?
C2 C3 C4 119.9(10) . . ?
C5 C4 C3 120.2(11) . . ?
C4 C5 C6 121.4(12) . . ?
C7 C6 C5 117.7(10) . . ?
C7 C6 C8 127.3(9) . . ?
C8 C6 C5 115.0(10) . . ?
O2 C7 C2 117.7(9) . . ?
O2 C7 C6 123.3(8) . . ?
C6 C7 C2 118.9(8) . . ?
N1 C8 C6 125.8(10) . . ?
C10 C9 N1 120.5(8) . . ?
C9 C10 N2 117.2(9) . . ?
C9 C10 C12 121.9(9) . 2_655 ?
C12 C10 N2 120.9(9) 2_655 . ?
N3 C11 N2 127.2(8) . 2_655 ?
C10 C12 C13 118.3(9) 2_655 . ?
C12 C13 N3 121.4(9) . . ?
C14 C13 N3 117.1(9) . . ?
C14 C13 C12 121.5(9) . . ?
C13 C14 N4 122.3(8) . . ?
N4 C15 C16 128.5(9) . . ?
C17 C16 C15 117.3(9) . . ?
C17 C16 C21 118.7(10) . . ?
C21 C16 C15 124.0(9) . . ?
C18 C17 C16 121.3(11) . . ?
C19 C18 C17 120.6(11) . . ?
C18 C19 C20 119.7(10) . . ?
O5 C20 C21 113.6(9) . . ?
C19 C20 O5 124.8(10) . . ?
C19 C20 C21 121.6(10) . . ?
O4 C21 C16 123.6(9) . . ?
O4 C21 C20 118.1(9) . . ?
C16 C21 C20 118.1(9) . . ?
O21 N8 O20 117.0(13) . . ?
O22 N8 O20 121.4(14) . . ?
O22 N8 O21 121.3(12) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_r150126c
_database_code_depnum_ccdc_archive 'CCDC 1419276'
_audit_update_record             
;
2015-08-18 deposited with the CCDC.
2015-10-20 downloaded from the CCDC.
;
_audit_creation_date             2015-07-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C24 H25 Dy3 N10 O9 S4, 0.5(C2 N), 2.75(C2 H3 N), 0.5(C H4 O), O'
_chemical_formula_sum            'C31 H35.25 Dy3 N13.25 O10.50 S4'
_chemical_formula_weight         1377.21
_chemical_melting_point          ?
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   40.411(8)
_cell_length_b                   11.713(2)
_cell_length_c                   30.558(6)
_cell_angle_alpha                90
_cell_angle_beta                 129.65(3)
_cell_angle_gamma                90
_cell_volume                     11137(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    10603
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.9223
_cell_measurement_theta_min      1.3483
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.189
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4914
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            33379
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.309
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
scan:
	Number of images: 90
	           Slice: -120.0000 - 60.0000
	     Image width: 2.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 60.2424
	          2theta: -30.0069
scan:
	Number of images: 70
	           Slice: -120.0000 - 20.0000
	     Image width: 2.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 60.2424
	          2theta: -30.0069
scan:
	Number of images: 60
	           Slice: -120.0000 - 0.0000
	     Image width: 2.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 60.2424
	          2theta: -30.0069
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             13682
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0211
_diffrn_orient_matrix_UB_12      -0.0095
_diffrn_orient_matrix_UB_13      0.0223
_diffrn_orient_matrix_UB_21      0.0095
_diffrn_orient_matrix_UB_22      -0.0810
_diffrn_orient_matrix_UB_23      -0.0253
_diffrn_orient_matrix_UB_31      0.0066
_diffrn_orient_matrix_UB_32      -0.0118
_diffrn_orient_matrix_UB_33      0.0403
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8342
_reflns_number_total             10824
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         10824
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0741
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0693P)²+255.4697P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1806
_refine_ls_wR_factor_ref         0.1933
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 S4A-N8
 2.8 with sigma of 0.02
 S4A-C22 = S4-C22
 1.78 with sigma of 0.02
 S4-N8
 2.8 with sigma of 0.02
 S4A-N8 = S1A-N10
 2.78 with sigma of 0.01
 S1A-C24
 1.7 with sigma of 0.05
 N10-S1A
 2.85 with sigma of 0.005
 O7-H7
 0.9 with sigma of 0.02
 H7-Dy1
 2.9 with sigma of 0.02
 H7-Dy3
 2.9 with sigma of 0.02
 H3-Dy2
 2.9 with sigma of 0.02
3. Rigid bond restraints
 S1, S1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1, S1A, S1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
S1 \\sim S1A \\sim S1B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(S4) \\sim Ueq, Uanis(S4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O13) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(S1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(S4A)=1-FVAR(1)
 Sof(S4)=FVAR(1)
 Fixed Sof: C28(0.75) N12(0.75) C29(0.75) H29A(0.75) H29B(0.75) H29C(0.75)
 O10(0.5) H10(0.5) O13(0.25) S1(0.32377) S1A(0.34623) S1B(0.33) O11(0.25)
 O12(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
6.a Rotating group:
 O9(H9A,H9B), O8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C8(H8), C3(H3A), C19(H19), C20(H20), C4(H4), C17(H17), C5(H5),
 C14(H14), C12(H12), C13(H13), N5(H5A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C10(H10A,H10B,
 H10C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C)
6.d Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy2 Dy 0.11911(2) 0.87219(4) 0.32377(2) 0.03042(16) Uani 1 1 d D . . . .
Dy3 Dy 0.04635(2) 0.87919(5) 0.17485(2) 0.03147(16) Uani 1 1 d D . . . .
Dy1 Dy 0.15796(2) 0.88576(5) 0.24779(2) 0.03590(17) Uani 1 1 d D . . . .
C7 C 0.2277(4) 0.8721(10) 0.3884(5) 0.037(3) Uani 1 1 d . . . . .
C16 C 0.0900(4) 0.8970(10) 0.1066(5) 0.038(3) Uani 1 1 d . . . . .
S2 S 0.1111(2) 0.4633(4) 0.3810(2) 0.109(2) Uani 1 1 d . . . . .
N1 N 0.1770(3) 0.8760(8) 0.4317(4) 0.038(2) Uani 1 1 d . . . . .
N6 N -0.0004(3) 0.8677(9) 0.0670(4) 0.040(2) Uani 1 1 d . . . . .
S3 S -0.0152(2) 1.2905(4) 0.1272(2) 0.127(3) Uani 1 1 d . . . . .
O6 O 0.1111(2) 0.7740(6) 0.2469(3) 0.0322(18) Uani 1 1 d . . . . .
C11 C 0.1295(4) 0.9148(10) 0.1187(6) 0.043(3) Uani 1 1 d . . . . .
O7 O 0.1085(2) 0.9817(7) 0.2507(3) 0.0324(17) Uani 1 1 d D . . . .
N7 N 0.0250(4) 1.0760(9) 0.1512(4) 0.044(3) Uani 1 1 d . . . . .
N2 N 0.1624(3) 0.8743(9) 0.4622(4) 0.042(2) Uani 1 1 d . . . . .
H2 H 0.1807 0.8747 0.4987 0.050 Uiso 1 1 calc R . . . .
N9 N 0.1214(3) 0.6756(8) 0.3490(4) 0.036(2) Uani 1 1 d . . . . .
C6 C 0.2437(4) 0.8812(11) 0.4446(5) 0.044(3) Uani 1 1 d . . . . .
O3 O 0.0473(2) 0.8654(7) 0.2500(3) 0.0353(18) Uani 1 1 d . . . . .
C23 C 0.1180(5) 0.5872(12) 0.3614(5) 0.055(4) Uani 1 1 d . . . . .
C21 C 0.0099(6) 1.1640(16) 0.1428(6) 0.070(5) Uani 1 1 d . . . . .
N3 N 0.0913(3) 0.8826(8) 0.3770(4) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.2185(4) 0.8834(11) 0.4629(5) 0.042(3) Uani 1 1 d . . . . .
H8 H 0.2338 0.8912 0.5018 0.050 Uiso 1 1 calc R . . . .
C15 C 0.0522(4) 0.8763(12) 0.0519(5) 0.046(3) Uani 1 1 d . . . . .
C3 C 0.2996(4) 0.8682(13) 0.4195(6) 0.054(4) Uani 1 1 d . . . . .
H3A H 0.3181 0.8622 0.4113 0.064 Uiso 1 1 calc R . . . .
C2 C 0.2562(4) 0.8642(11) 0.3767(5) 0.047(3) Uani 1 1 d . . . . .
C19 C -0.1052(4) 0.8629(11) 0.0333(5) 0.044(3) Uani 1 1 d . . . . .
H19 H -0.1245 0.8579 -0.0061 0.053 Uiso 1 1 calc R . . . .
N8 N 0.1885(4) 1.0716(7) 0.2752(5) 0.055(3) Uani 1 1 d D . . . .
O4 O 0.0917(3) 0.8974(7) 0.1534(3) 0.0381(19) Uani 1 1 d . . . . .
C9 C 0.1189(4) 0.8720(10) 0.4348(5) 0.037(3) Uani 1 1 d . . . . .
O5 O 0.1639(3) 0.9424(8) 0.1746(4) 0.049(2) Uani 1 1 d . . . . .
C20 C -0.0503(4) 0.8860(10) 0.1467(5) 0.036(3) Uani 1 1 d . . . . .
H20 H -0.0310 0.8974 0.1858 0.044 Uiso 1 1 calc R . . . .
C4 C 0.3163(4) 0.8814(13) 0.4758(6) 0.058(4) Uani 1 1 d . . . . .
H4 H 0.3458 0.8867 0.5050 0.069 Uiso 1 1 calc R . . . .
C17 C 0.0104(4) 0.8644(12) 0.0345(5) 0.047(3) Uani 1 1 d . . . . .
H17 H -0.0119 0.8531 -0.0042 0.057 Uiso 1 1 calc R . . . .
C5 C 0.2887(4) 0.8863(12) 0.4873(6) 0.048(3) Uani 1 1 d . . . . .
H5 H 0.3002 0.8934 0.5249 0.058 Uiso 1 1 calc R . . . .
C1 C 0.2642(5) 0.8093(14) 0.3069(7) 0.064(4) Uani 1 1 d . . . . .
H1A H 0.2473 0.7919 0.2673 0.097 Uiso 1 1 calc GR . . . .
H1B H 0.2805 0.7432 0.3290 0.097 Uiso 1 1 calc GR . . . .
H1C H 0.2834 0.8711 0.3167 0.097 Uiso 1 1 calc GR . . . .
C14 C 0.0555(5) 0.8714(14) 0.0082(6) 0.058(4) Uani 1 1 d . . . . .
H14 H 0.0312 0.8552 -0.0289 0.069 Uiso 1 1 calc R . . . .
C18 C -0.0614(4) 0.8621(10) 0.0642(5) 0.038(3) Uani 1 1 d . . . . .
N10 N 0.1661(4) 0.7100(10) 0.2164(5) 0.052(3) Uani 1 1 d D . . . .
C12 C 0.1310(5) 0.9119(12) 0.0750(6) 0.055(4) Uani 1 1 d . . . . .
H12 H 0.1569 0.9245 0.0825 0.066 Uiso 1 1 calc R . . . .
N11 N 0.0000 0.6700(13) 0.2500 0.049(4) Uani 1 2 d S T P . .
C26 C 0.0000 0.5702(19) 0.2500 0.055(5) Uani 1 2 d S T P . .
N13 N 0.2806(4) 0.5728(12) 0.4124(5) 0.066(4) Uani 1 1 d . . . . .
C31 C 0.1991(5) 0.5594(16) 0.3413(8) 0.080(5) Uani 1 1 d . . . . .
H31A H 0.1887 0.5847 0.3046 0.121 Uiso 1 1 calc GR . . . .
H31B H 0.1878 0.6079 0.3543 0.121 Uiso 1 1 calc GR . . . .
H31C H 0.1899 0.4822 0.3386 0.121 Uiso 1 1 calc GR . . . .
C13 C 0.0938(5) 0.8902(14) 0.0195(6) 0.063(4) Uani 1 1 d . . . . .
H13 H 0.0949 0.8884 -0.0099 0.075 Uiso 1 1 calc R . . . .
C28 C 0.0958(8) 0.428(2) 0.2406(9) 0.071(6) Uani 0.75 1 d . . . . .
N12 N 0.0915(5) 0.5254(15) 0.2173(9) 0.099(9) Uani 0.75 1 d . . . . .
C32 C 0.1107(7) 1.2184(17) 0.1177(9) 0.089(6) Uani 1 1 d . . . . .
C30 C 0.2442(4) 0.5642(11) 0.3800(6) 0.044(3) Uani 1 1 d . . . . .
O2 O 0.1844(2) 0.8675(7) 0.3430(3) 0.0368(18) Uani 1 1 d . . . . .
O1 O 0.2354(3) 0.8426(8) 0.3189(4) 0.048(2) Uani 1 1 d . . . . .
S4A S 0.2097(4) 1.3028(6) 0.2914(6) 0.089(4) Uani 0.60(2) 1 d D U . A 2
C22 C 0.2035(8) 1.1540(14) 0.2904(10) 0.120(9) Uani 1 1 d D . . . .
O9 O 0.1254(3) 1.0702(7) 0.3511(4) 0.048(2) Uani 1 1 d . . . . .
H9A H 0.1079 1.1076 0.3571 0.071 Uiso 1 1 d GR . . . .
H9B H 0.1458 1.1232 0.3574 0.071 Uiso 1 1 d GR . . . .
C27 C 0.0000 0.448(2) 0.2500 0.118(12) Uani 1 2 d S T P . .
N4 N -0.0330(3) 0.8750(8) 0.1217(4) 0.035(2) Uani 1 1 d . . . . .
N5 N -0.0440(3) 0.8540(10) 0.0376(4) 0.046(3) Uani 1 1 d . . . . .
H5A H -0.0606 0.8401 0.0017 0.055 Uiso 1 1 calc R . . . .
O8 O 0.0271(3) 0.6822(7) 0.1535(3) 0.046(2) Uani 1 1 d . . . . .
H8A H 0.0352 0.6538 0.1354 0.069 Uiso 1 1 d GR . . . .
H8B H -0.0007 0.6745 0.1322 0.069 Uiso 1 1 d GR . . . .
N14 N 0.1078(8) 1.2159(16) 0.0813(6) 0.130(9) Uani 1 1 d . . . . .
C33 C 0.1010(12) 1.221(4) 0.1471(16) 0.22(2) Uani 1 1 d . . . . .
H33A H 0.0720 1.2478 0.1254 0.336 Uiso 1 1 calc GR . . . .
H33B H 0.1199 1.2722 0.1784 0.336 Uiso 1 1 calc GR . . . .
H33C H 0.1033 1.1461 0.1614 0.336 Uiso 1 1 calc GR . . . .
C10 C 0.2024(5) 0.9868(13) 0.1866(7) 0.062(4) Uani 1 1 d . . . . .
H10A H 0.2237 1.0015 0.2266 0.093 Uiso 1 1 calc GR . . . .
H10B H 0.1957 1.0564 0.1659 0.093 Uiso 1 1 calc GR . . . .
H10C H 0.2133 0.9317 0.1754 0.093 Uiso 1 1 calc GR . . . .
C29 C 0.1070(12) 0.301(4) 0.2682(14) 0.167(19) Uani 0.75 1 d . . . . .
H29A H 0.1091 0.2489 0.2458 0.251 Uiso 0.75 1 calc GR . . . .
H29B H 0.0847 0.2763 0.2690 0.251 Uiso 0.75 1 calc GR . . . .
H29C H 0.1339 0.3031 0.3063 0.251 Uiso 0.75 1 calc GR . . . .
O10 O -0.0529(5) 0.5891(13) 0.0867(7) 0.038(4) Uani 0.5 1 d . . . . .
H10 H -0.0659 0.5627 0.0968 0.056 Uiso 0.5 1 calc GR . . . .
O13 O 0.0000 1.148(2) 0.2500 0.142(18) Uani 0.5 2 d S TU P . .
S1 S 0.1842(5) 0.5845(11) 0.1537(5) 0.061(3) Uani 0.3238 1 d . U . B 1
S1A S 0.1421(11) 0.5342(19) 0.1372(9) 0.206(16) Uani 0.3462 1 d D U . B 3
C24 C 0.1657(8) 0.6485(18) 0.1884(9) 0.119(9) Uani 1 1 d D . . . .
S4 S 0.2386(9) 1.2686(19) 0.3312(11) 0.143(9) Uani 0.40(2) 1 d D U . A 1
S1B S 0.1622(10) 0.476(2) 0.1945(18) 0.183(13) Uani 0.33 1 d . U . B 2
O11 O 0.2389(12) 1.341(7) 0.458(2) 0.13(3) Uani 0.25 1 d . . . . .
H6 H 0.114(3) 0.696(8) 0.248(3) 0.00(2) Uiso 1 1 d . . . . .
H7 H 0.1067(8) 1.0585(17) 0.248(2) 0.12(8) Uiso 1 1 d D . . . .
H3 H 0.0310(16) 0.795(12) 0.241(4) 0.06(4) Uiso 1 1 d D . . . .
O12 O 0.1560(13) 1.190(3) 0.4731(17) 0.164(15) Uani 0.5 1 d . U . . .
C25 C -0.0686(9) 0.542(2) 0.0358(12) 0.053(7) Uani 0.5 1 d . . . . .
H25A H -0.0864 0.5972 0.0060 0.079 Uiso 0.5 1 calc GR . . . .
H25B H -0.0854 0.4759 0.0286 0.079 Uiso 0.5 1 calc GR . . . .
H25C H -0.0452 0.5209 0.0369 0.079 Uiso 0.5 1 calc GR . . . .


_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
Dy2 Dy3 3.5050(18) . ?
Dy2 Dy1 3.5401(10) . ?
Dy2 N1 2.550(9) . ?
Dy2 O6 2.444(8) . ?
Dy2 O7 2.365(7) . ?
Dy2 N9 2.411(10) . ?
Dy2 O3 2.271(8) . ?
Dy2 N3 2.501(10) . ?
Dy2 O2 2.310(8) . ?
Dy2 O9 2.422(8) . ?
Dy3 Dy1 3.5336(16) . ?
Dy3 N6 2.551(9) . ?
Dy3 O6 2.421(7) . ?
Dy3 O7 2.386(7) . ?
Dy3 N7 2.405(10) . ?
Dy3 O3 2.277(7) . ?
Dy3 O4 2.315(8) . ?
Dy3 N4 2.507(9) . ?
Dy3 O8 2.389(8) . ?
Dy1 O6 2.287(8) . ?
Dy1 O7 2.343(8) . ?
Dy1 N8 2.376(8) . ?
Dy1 O4 2.378(8) . ?
Dy1 O5 2.486(9) . ?
Dy1 N10 2.382(10) . ?
Dy1 O2 2.384(8) . ?
Dy1 O1 2.469(9) . ?
C7 C6 1.400(17) . ?
C7 C2 1.411(18) . ?
C7 O2 1.374(13) . ?
C16 C11 1.406(18) . ?
C16 C15 1.387(17) . ?
C16 O4 1.389(13) . ?
S2 C23 1.659(15) . ?
N1 N2 1.386(14) . ?
N1 C8 1.298(15) . ?
N6 C17 1.315(15) . ?
N6 N5 1.383(14) . ?
S3 C21 1.684(19) . ?
O6 H6 0.92(9) . ?
C11 O5 1.387(16) . ?
C11 C12 1.374(18) . ?
O7 H7 0.90(2) . ?
N7 C21 1.140(19) . ?
N2 H2 0.8600 . ?
N2 C9 1.383(15) . ?
N9 C23 1.142(16) . ?
C6 C8 1.442(18) . ?
C6 C5 1.410(16) . ?
O3 H3 0.98(10) . ?
N3 C9 1.366(14) . ?
N3 C20 1.320(14) 2 ?
C8 H8 0.9300 . ?
C15 C17 1.417(18) . ?
C15 C14 1.429(17) . ?
C3 H3A 0.9300 . ?
C3 C2 1.365(17) . ?
C3 C4 1.40(2) . ?
C2 O1 1.411(16) . ?
C19 H19 0.9300 . ?
C19 C9 1.396(17) 2 ?
C19 C18 1.378(17) . ?
N8 C22 1.075(15) . ?
C9 C19 1.396(17) 2 ?
O5 C10 1.448(15) . ?
C20 N3 1.320(14) 2 ?
C20 H20 0.9300 . ?
C20 N4 1.328(15) . ?
C4 H4 0.9300 . ?
C4 C5 1.37(2) . ?
C17 H17 0.9300 . ?
C5 H5 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 O1 1.476(16) . ?
C14 H14 0.9300 . ?
C14 C13 1.37(2) . ?
C18 N4 1.362(14) . ?
C18 N5 1.375(16) . ?
N10 C24 1.11(2) . ?
C12 H12 0.9300 . ?
C12 C13 1.40(2) . ?
N11 C26 1.17(2) . ?
C26 C27 1.44(3) . ?
N13 C30 1.138(17) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 C30 1.41(2) . ?
C13 H13 0.9300 . ?
C28 N12 1.30(3) . ?
C28 C29 1.62(5) . ?
C32 N14 1.04(3) . ?
C32 C33 1.19(3) . ?
S4A C22 1.758(16) . ?
C22 S4 1.762(16) . ?
O9 H9A 0.9468 . ?
O9 H9B 0.9468 . ?
N5 H5A 0.8600 . ?
O8 H8A 0.8692 . ?
O8 H8B 0.8748 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
O10 H10 0.8200 . ?
O10 C25 1.37(3) . ?
S1 C24 1.81(3) . ?
S1A C24 1.80(2) . ?
C24 S1B 2.04(3) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

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
Dy3 Dy2 Dy1 60.21(3) . . ?
N1 Dy2 Dy3 174.8(2) . . ?
N1 Dy2 Dy1 115.0(2) . . ?
O6 Dy2 Dy3 43.65(17) . . ?
O6 Dy2 Dy1 39.90(18) . . ?
O6 Dy2 N1 134.5(3) . . ?
O6 Dy2 N3 144.0(3) . . ?
O7 Dy2 Dy3 42.69(18) . . ?
O7 Dy2 Dy1 41.01(19) . . ?
O7 Dy2 N1 132.5(3) . . ?
O7 Dy2 O6 61.0(3) . . ?
O7 Dy2 N9 140.0(3) . . ?
O7 Dy2 N3 134.6(3) . . ?
O7 Dy2 O9 73.8(3) . . ?
N9 Dy2 Dy3 105.5(2) . . ?
N9 Dy2 Dy1 108.0(2) . . ?
N9 Dy2 N1 77.7(3) . . ?
N9 Dy2 O6 79.2(3) . . ?
N9 Dy2 N3 77.3(3) . . ?
N9 Dy2 O9 146.1(3) . . ?
O3 Dy2 Dy3 39.64(19) . . ?
O3 Dy2 Dy1 99.81(19) . . ?
O3 Dy2 N1 145.2(3) . . ?
O3 Dy2 O6 74.2(3) . . ?
O3 Dy2 O7 74.6(3) . . ?
O3 Dy2 N9 92.8(3) . . ?
O3 Dy2 N3 80.1(3) . . ?
O3 Dy2 O2 141.3(3) . . ?
O3 Dy2 O9 99.4(3) . . ?
N3 Dy2 Dy3 119.4(2) . . ?
N3 Dy2 Dy1 174.6(2) . . ?
N3 Dy2 N1 65.2(3) . . ?
O2 Dy2 Dy3 101.91(19) . . ?
O2 Dy2 Dy1 41.83(19) . . ?
O2 Dy2 N1 73.5(3) . . ?
O2 Dy2 O6 70.2(3) . . ?
O2 Dy2 O7 75.1(3) . . ?
O2 Dy2 N9 95.2(3) . . ?
O2 Dy2 N3 138.6(3) . . ?
O2 Dy2 O9 94.8(3) . . ?
O9 Dy2 Dy3 104.0(2) . . ?
O9 Dy2 Dy1 100.9(2) . . ?
O9 Dy2 N1 74.3(3) . . ?
O9 Dy2 O6 134.5(3) . . ?
O9 Dy2 N3 73.9(3) . . ?
Dy2 Dy3 Dy1 60.39(4) . . ?
N6 Dy3 Dy2 173.1(2) . . ?
N6 Dy3 Dy1 114.3(2) . . ?
O6 Dy3 Dy2 44.17(18) . . ?
O6 Dy3 Dy1 39.95(19) . . ?
O6 Dy3 N6 128.9(3) . . ?
O6 Dy3 N4 140.7(3) . . ?
O7 Dy3 Dy2 42.23(18) . . ?
O7 Dy3 Dy1 41.19(19) . . ?
O7 Dy3 N6 137.3(3) . . ?
O7 Dy3 O6 61.0(3) . . ?
O7 Dy3 N7 76.3(3) . . ?
O7 Dy3 N4 139.3(3) . . ?
O7 Dy3 O8 135.1(3) . . ?
N7 Dy3 Dy2 104.8(2) . . ?
N7 Dy3 Dy1 103.7(3) . . ?
N7 Dy3 N6 80.5(3) . . ?
N7 Dy3 O6 137.2(3) . . ?
N7 Dy3 N4 76.0(3) . . ?
O3 Dy3 Dy2 39.5(2) . . ?
O3 Dy3 Dy1 99.9(2) . . ?
O3 Dy3 N6 145.2(3) . . ?
O3 Dy3 O6 74.5(3) . . ?
O3 Dy3 O7 74.1(3) . . ?
O3 Dy3 N7 98.2(3) . . ?
O3 Dy3 O4 141.6(3) . . ?
O3 Dy3 N4 81.0(3) . . ?
O3 Dy3 O8 90.0(3) . . ?
O4 Dy3 Dy2 102.13(19) . . ?
O4 Dy3 Dy1 41.83(19) . . ?
O4 Dy3 N6 72.9(3) . . ?
O4 Dy3 O6 73.3(3) . . ?
O4 Dy3 O7 72.3(3) . . ?
O4 Dy3 N7 91.3(3) . . ?
O4 Dy3 N4 137.3(3) . . ?
O4 Dy3 O8 100.9(3) . . ?
N4 Dy3 Dy2 120.5(2) . . ?
N4 Dy3 Dy1 179.1(2) . . ?
N4 Dy3 N6 64.9(3) . . ?
O8 Dy3 Dy2 100.9(2) . . ?
O8 Dy3 Dy1 104.8(2) . . ?
O8 Dy3 N6 75.7(3) . . ?
O8 Dy3 O6 74.4(3) . . ?
O8 Dy3 N7 148.4(3) . . ?
O8 Dy3 N4 75.3(3) . . ?
Dy3 Dy1 Dy2 59.41(3) . . ?
O6 Dy1 Dy2 43.27(19) . . ?
O6 Dy1 Dy3 42.82(18) . . ?
O6 Dy1 O7 63.6(3) . . ?
O6 Dy1 N8 140.2(4) . . ?
O6 Dy1 O4 74.6(3) . . ?
O6 Dy1 O5 134.1(3) . . ?
O6 Dy1 N10 80.1(3) . . ?
O6 Dy1 O2 71.7(3) . . ?
O6 Dy1 O1 117.9(3) . . ?
O7 Dy1 Dy2 41.47(18) . . ?
O7 Dy1 Dy3 42.11(18) . . ?
O7 Dy1 N8 79.1(3) . . ?
O7 Dy1 O4 72.0(3) . . ?
O7 Dy1 O5 118.7(3) . . ?
O7 Dy1 N10 140.4(3) . . ?
O7 Dy1 O2 74.1(3) . . ?
O7 Dy1 O1 134.2(3) . . ?
N8 Dy1 Dy2 99.1(3) . . ?
N8 Dy1 Dy3 114.2(3) . . ?
N8 Dy1 O4 107.8(4) . . ?
N8 Dy1 O5 75.3(4) . . ?
N8 Dy1 N10 139.4(4) . . ?
N8 Dy1 O2 85.7(4) . . ?
N8 Dy1 O1 78.2(4) . . ?
O4 Dy1 Dy2 99.80(19) . . ?
O4 Dy1 Dy3 40.49(19) . . ?
O4 Dy1 O5 64.8(3) . . ?
O4 Dy1 N10 84.2(3) . . ?
O4 Dy1 O2 140.0(3) . . ?
O4 Dy1 O1 153.4(3) . . ?
O5 Dy1 Dy2 159.9(2) . . ?
O5 Dy1 Dy3 104.8(2) . . ?
N10 Dy1 Dy2 117.3(3) . . ?
N10 Dy1 Dy3 100.2(3) . . ?
N10 Dy1 O5 75.5(4) . . ?
N10 Dy1 O2 110.2(4) . . ?
N10 Dy1 O1 75.8(3) . . ?
O2 Dy1 Dy2 40.26(19) . . ?
O2 Dy1 Dy3 99.55(19) . . ?
O2 Dy1 O5 153.6(3) . . ?
O2 Dy1 O1 65.0(3) . . ?
O1 Dy1 Dy2 104.9(2) . . ?
O1 Dy1 Dy3 160.3(2) . . ?
O1 Dy1 O5 92.9(3) . . ?
C6 C7 C2 120.2(11) . . ?
O2 C7 C6 122.4(10) . . ?
O2 C7 C2 117.3(10) . . ?
C15 C16 C11 122.5(11) . . ?
C15 C16 O4 122.1(11) . . ?
O4 C16 C11 115.4(11) . . ?
N2 N1 Dy2 115.9(7) . . ?
C8 N1 Dy2 129.8(8) . . ?
C8 N1 N2 114.2(9) . . ?
C17 N6 Dy3 130.4(8) . . ?
C17 N6 N5 113.9(10) . . ?
N5 N6 Dy3 115.5(7) . . ?
Dy2 O6 H6 119(5) . . ?
Dy3 O6 Dy2 92.2(3) . . ?
Dy3 O6 H6 126(5) . . ?
Dy1 O6 Dy2 96.8(3) . . ?
Dy1 O6 Dy3 97.2(3) . . ?
Dy1 O6 H6 119(5) . . ?
O5 C11 C16 115.7(11) . . ?
C12 C11 C16 119.2(13) . . ?
C12 C11 O5 124.9(12) . . ?
Dy2 O7 Dy3 95.1(3) . . ?
Dy2 O7 H7 126(3) . . ?
Dy3 O7 H7 116(2) . . ?
Dy1 O7 Dy2 97.5(3) . . ?
Dy1 O7 Dy3 96.7(3) . . ?
Dy1 O7 H7 119(2) . . ?
C21 N7 Dy3 166.4(13) . . ?
N1 N2 H2 119.5 . . ?
C9 N2 N1 121.0(9) . . ?
C9 N2 H2 119.5 . . ?
C23 N9 Dy2 169.9(12) . . ?
C7 C6 C8 126.1(11) . . ?
C7 C6 C5 116.8(12) . . ?
C5 C6 C8 117.0(12) . . ?
Dy2 O3 Dy3 100.8(3) . . ?
Dy2 O3 H3 121(6) . . ?
Dy3 O3 H3 102(8) . . ?
N9 C23 S2 175.8(15) . . ?
N7 C21 S3 176.6(18) . . ?
C9 N3 Dy2 120.1(8) . . ?
C20 N3 Dy2 124.9(7) 2 . ?
C20 N3 C9 114.6(10) 2 . ?
N1 C8 C6 127.8(11) . . ?
N1 C8 H8 116.1 . . ?
C6 C8 H8 116.1 . . ?
C16 C15 C17 127.1(11) . . ?
C16 C15 C14 116.3(12) . . ?
C17 C15 C14 116.5(12) . . ?
C2 C3 H3A 120.0 . . ?
C2 C3 C4 120.1(13) . . ?
C4 C3 H3A 120.0 . . ?
C3 C2 C7 120.7(13) . . ?
C3 C2 O1 125.5(13) . . ?
O1 C2 C7 113.5(10) . . ?
C9 C19 H19 122.2 2 . ?
C18 C19 H19 122.2 . . ?
C18 C19 C9 115.6(11) . 2 ?
C22 N8 Dy1 176.3(16) . . ?
Dy3 O4 Dy1 97.7(3) . . ?
C16 O4 Dy3 139.9(7) . . ?
C16 O4 Dy1 121.7(7) . . ?
N2 C9 C19 119.6(10) . 2 ?
N3 C9 N2 117.1(10) . . ?
N3 C9 C19 123.3(11) . 2 ?
C11 O5 Dy1 116.8(7) . . ?
C11 O5 C10 117.7(11) . . ?
C10 O5 Dy1 124.9(8) . . ?
N3 C20 H20 116.0 2 . ?
N3 C20 N4 128.1(10) 2 . ?
N4 C20 H20 116.0 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(12) . . ?
C5 C4 H4 120.4 . . ?
N6 C17 C15 127.1(11) . . ?
N6 C17 H17 116.5 . . ?
C15 C17 H17 116.5 . . ?
C6 C5 H5 118.5 . . ?
C4 C5 C6 122.9(13) . . ?
C4 C5 H5 118.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
C15 C14 H14 119.2 . . ?
C13 C14 C15 121.5(13) . . ?
C13 C14 H14 119.2 . . ?
N4 C18 C19 122.5(11) . . ?
N4 C18 N5 116.4(10) . . ?
N5 C18 C19 121.1(10) . . ?
C24 N10 Dy1 159.0(16) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.1(14) . . ?
C13 C12 H12 120.0 . . ?
N11 C26 C27 180.000(12) . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C14 C13 C12 120.4(13) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
N12 C28 C29 170(3) . . ?
N14 C32 C33 160(4) . . ?
N13 C30 C31 176.6(16) . . ?
Dy2 O2 Dy1 97.9(3) . . ?
C7 O2 Dy2 140.0(7) . . ?
C7 O2 Dy1 121.3(7) . . ?
C2 O1 Dy1 118.2(7) . . ?
C2 O1 C1 115.1(10) . . ?
C1 O1 Dy1 126.3(8) . . ?
N8 C22 S4A 159(2) . . ?
N8 C22 S4 165(3) . . ?
Dy2 O9 H9A 125.6 . . ?
Dy2 O9 H9B 125.8 . . ?
H9A O9 H9B 108.6 . . ?
C20 N4 Dy3 123.3(7) . . ?
C20 N4 C18 115.8(10) . . ?
C18 N4 Dy3 120.8(8) . . ?
N6 N5 H5A 119.1 . . ?
C18 N5 N6 121.9(9) . . ?
C18 N5 H5A 119.1 . . ?
Dy3 O8 H8A 110.8 . . ?
Dy3 O8 H8B 110.0 . . ?
H8A O8 H8B 108.4 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O5 C10 H10A 109.5 . . ?
O5 C10 H10B 109.5 . . ?
O5 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 O10 H10 109.5 . . ?
N10 C24 S1 156(2) . . ?
N10 C24 S1A 153(3) . . ?
N10 C24 S1B 123(2) . . ?
O10 C25 H25A 109.5 . . ?
O10 C25 H25B 109.5 . . ?
O10 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy2 N1 N2 C9 -0.7(13) . . . . ?
Dy2 N1 C8 C6 -6(2) . . . . ?
Dy2 N3 C9 N2 10.2(13) . . . . ?
Dy2 N3 C9 C19 -172.0(9) . . . 2 ?
Dy3 N6 C17 C15 -6(2) . . . . ?
Dy3 N6 N5 C18 8.6(15) . . . . ?
Dy1 N10 C24 S1 74(7) . . . . ?
Dy1 N10 C24 S1A -100(6) . . . . ?
Dy1 N10 C24 S1B -157(3) . . . . ?
C7 C6 C8 N1 1(2) . . . . ?
C7 C6 C5 C4 -1(2) . . . . ?
C7 C2 O1 Dy1 20.0(14) . . . . ?
C7 C2 O1 C1 -167.4(12) . . . . ?
C16 C11 O5 Dy1 22.3(13) . . . . ?
C16 C11 O5 C10 -166.2(11) . . . . ?
C16 C11 C12 C13 -1(2) . . . . ?
C16 C15 C17 N6 -2(2) . . . . ?
C16 C15 C14 C13 -2(2) . . . . ?
N1 N2 C9 N3 -6.2(16) . . . . ?
N1 N2 C9 C19 175.9(11) . . . 2 ?
C11 C16 C15 C17 -175.7(13) . . . . ?
C11 C16 C15 C14 1(2) . . . . ?
C11 C16 O4 Dy3 178.9(8) . . . . ?
C11 C16 O4 Dy1 -13.6(13) . . . . ?
C11 C12 C13 C14 0(2) . . . . ?
N2 N1 C8 C6 176.5(12) . . . . ?
C6 C7 C2 C3 -2(2) . . . . ?
C6 C7 C2 O1 173.2(11) . . . . ?
C6 C7 O2 Dy2 1.1(18) . . . . ?
C6 C7 O2 Dy1 168.8(9) . . . . ?
N3 C20 N4 Dy3 -178.4(9) 2 . . . ?
N3 C20 N4 C18 2.1(18) 2 . . . ?
C8 N1 N2 C9 177.0(11) . . . . ?
C8 C6 C5 C4 178.0(14) . . . . ?
C15 C16 C11 O5 175.6(12) . . . . ?
C15 C16 C11 C12 0.0(19) . . . . ?
C15 C16 O4 Dy3 -3.3(19) . . . . ?
C15 C16 O4 Dy1 164.3(10) . . . . ?
C15 C14 C13 C12 2(3) . . . . ?
C3 C2 O1 Dy1 -165.5(11) . . . . ?
C3 C2 O1 C1 7.1(19) . . . . ?
C3 C4 C5 C6 -1(2) . . . . ?
C2 C7 C6 C8 -176.3(13) . . . . ?
C2 C7 C6 C5 2.3(18) . . . . ?
C2 C7 O2 Dy2 179.4(8) . . . . ?
C2 C7 O2 Dy1 -12.8(14) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
C19 C18 N4 Dy3 -177.9(9) . . . . ?
C19 C18 N4 C20 1.5(17) . . . . ?
C19 C18 N5 N6 171.6(11) . . . . ?
O4 C16 C11 O5 -6.6(16) . . . . ?
O4 C16 C11 C12 177.8(11) . . . . ?
O4 C16 C15 C17 7(2) . . . . ?
O4 C16 C15 C14 -176.3(12) . . . . ?
C9 C19 C18 N4 -3.3(18) 2 . . . ?
C9 C19 C18 N5 -179.7(11) 2 . . . ?
O5 C11 C12 C13 -175.9(13) . . . . ?
C20 N3 C9 N2 -176.5(10) 2 . . . ?
C20 N3 C9 C19 1.3(17) 2 . . 2 ?
C4 C3 C2 C7 -1(2) . . . . ?
C4 C3 C2 O1 -174.8(13) . . . . ?
C17 N6 N5 C18 -176.0(12) . . . . ?
C17 C15 C14 C13 175.2(15) . . . . ?
C5 C6 C8 N1 -177.6(13) . . . . ?
C14 C15 C17 N6 -179.0(14) . . . . ?
C12 C11 O5 Dy1 -162.4(11) . . . . ?
C12 C11 O5 C10 9.1(19) . . . . ?
O2 C7 C6 C8 2(2) . . . . ?
O2 C7 C6 C5 -179.4(11) . . . . ?
O2 C7 C2 C3 179.9(12) . . . . ?
O2 C7 C2 O1 -5.2(16) . . . . ?
N4 C18 N5 N6 -5.1(17) . . . . ?
N5 N6 C17 C15 179.7(13) . . . . ?
N5 C18 N4 Dy3 -1.3(14) . . . . ?
N5 C18 N4 C20 178.2(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
