# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_Gd_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1574217'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H76 Gd2 N2 O18'
_chemical_formula_weight         1499.79

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'
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'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9275(4)
_cell_length_b                   12.2795(4)
_cell_length_c                   13.7315(5)
_cell_angle_alpha                64.929(4)
_cell_angle_beta                 78.551(3)
_cell_angle_gamma                75.154(3)
_cell_volume                     1604.71(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    16566
_cell_measurement_theta_min      2.9308
_cell_measurement_theta_max      33.1226

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_F_000             758
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    2.121
_shelx_estimated_absorpt_T_min   0.588
_shelx_estimated_absorpt_T_max   0.800
_exptl_absorpt_correction_T_min  0.78422
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15105
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.935
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5631
_reflns_number_gt                5138
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0297P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5631
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0481
_refine_ls_wR_factor_gt          0.0475
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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_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
Gd1 Gd 0.63075(2) 0.06995(2) 0.39212(2) 0.01717(5) Uani 1 1 d . . . . .
O1 O 0.80742(15) 0.14421(15) 0.29568(13) 0.0264(4) Uani 1 1 d . . . . .
O2 O 0.43753(14) 0.11837(13) 0.48822(12) 0.0184(3) Uani 1 1 d . . . . .
O3 O 0.19543(14) 0.11583(14) 0.54514(12) 0.0227(4) Uani 1 1 d . . . . .
O4 O 0.50969(15) 0.20676(14) 0.25291(12) 0.0227(4) Uani 1 1 d . . . . .
O5 O 0.65480(16) -0.01877(15) 0.26935(12) 0.0240(4) Uani 1 1 d . . . . .
O6 O 0.71043(16) 0.05239(15) 0.55706(12) 0.0268(4) Uani 1 1 d . . . . .
H6S H 0.6934 0.1186 0.5657 0.032 Uiso 1 1 calc R U . . .
N1 N 0.62995(18) 0.27554(17) 0.38918(14) 0.0203(4) Uani 1 1 d . . . . .
C1 C 0.8394(2) 0.2380(2) 0.30254(18) 0.0249(6) Uani 1 1 d . . . . .
C2 C 0.9583(2) 0.2700(2) 0.2604(2) 0.0333(6) Uani 1 1 d . . . . .
H2 H 1.0174 0.2271 0.2218 0.040 Uiso 1 1 calc R U . . .
C3 C 0.9906(3) 0.3632(3) 0.2744(2) 0.0403(7) Uani 1 1 d . . . . .
H3 H 1.0720 0.3837 0.2455 0.048 Uiso 1 1 calc R U . . .
C4 C 0.9067(3) 0.4273(3) 0.3298(2) 0.0383(7) Uani 1 1 d . . . . .
H4 H 0.9309 0.4902 0.3403 0.046 Uiso 1 1 calc R U . . .
C5 C 0.7879(3) 0.3996(2) 0.3697(2) 0.0305(6) Uani 1 1 d . . . . .
H5 H 0.7300 0.4433 0.4082 0.037 Uiso 1 1 calc R U . . .
C6 C 0.7517(2) 0.3084(2) 0.35412(19) 0.0243(6) Uani 1 1 d . . . . .
C7 C 0.5335(2) 0.3548(2) 0.40170(19) 0.0241(5) Uani 1 1 d . . . . .
H7 H 0.5489 0.4337 0.3854 0.029 Uiso 1 1 calc R U . . .
C8 C 0.4028(2) 0.3380(2) 0.43807(19) 0.0226(5) Uani 1 1 d . . . . .
C9 C 0.3612(2) 0.2262(2) 0.47734(17) 0.0191(5) Uani 1 1 d . . . . .
C10 C 0.2299(2) 0.2280(2) 0.50818(18) 0.0209(5) Uani 1 1 d . . . . .
C11 C 0.1440(2) 0.3346(2) 0.5008(2) 0.0309(6) Uani 1 1 d . . . . .
H11 H 0.0561 0.3329 0.5225 0.037 Uiso 1 1 calc R U . . .
C12 C 0.1862(3) 0.4439(3) 0.4619(2) 0.0382(7) Uani 1 1 d . . . . .
H12 H 0.1274 0.5177 0.4562 0.046 Uiso 1 1 calc R U . . .
C13 C 0.3127(3) 0.4453(2) 0.4317(2) 0.0318(6) Uani 1 1 d . . . . .
H13 H 0.3408 0.5207 0.4056 0.038 Uiso 1 1 calc R U . . .
C14 C 0.0632(2) 0.1147(2) 0.5482(2) 0.0320(6) Uani 1 1 d . . . . .
H14A H 0.0136 0.1394 0.6058 0.048 Uiso 1 1 calc R U . . .
H14B H 0.0539 0.0318 0.5623 0.048 Uiso 1 1 calc R U . . .
H14C H 0.0321 0.1719 0.4786 0.048 Uiso 1 1 calc R U . . .
C15 C 0.6888(2) -0.0703(2) 0.11818(18) 0.0217(5) Uani 1 1 d . . . . .
C16 C 0.7512(3) -0.1867(2) 0.1784(2) 0.0373(7) Uani 1 1 d . . . . .
H16 H 0.7626 -0.2076 0.2515 0.045 Uiso 1 1 calc R U . . .
C17 C 0.7972(3) -0.2728(3) 0.1334(2) 0.0449(8) Uani 1 1 d . . . . .
H17 H 0.8392 -0.3525 0.1762 0.054 Uiso 1 1 calc R U . . .
C18 C 0.7832(3) -0.2449(3) 0.0283(2) 0.0370(7) Uani 1 1 d . . . . .
H18 H 0.8144 -0.3047 -0.0019 0.044 Uiso 1 1 calc R U . . .
C19 C 0.7238(3) -0.1300(3) -0.0325(2) 0.0391(7) Uani 1 1 d . . . . .
H19 H 0.7147 -0.1094 -0.1059 0.047 Uiso 1 1 calc R U . . .
C20 C 0.6768(3) -0.0433(3) 0.0115(2) 0.0334(6) Uani 1 1 d . . . . .
H20 H 0.6355 0.0363 -0.0322 0.040 Uiso 1 1 calc R U . . .
C21 C 0.6360(2) 0.0189(2) 0.17046(18) 0.0213(5) Uani 1 1 d . . . . .
C22 C 0.5687(2) 0.1353(2) 0.11282(19) 0.0243(6) Uani 1 1 d . . . . .
H22 H 0.5643 0.1572 0.0383 0.029 Uiso 1 1 calc R U . . .
C23 C 0.5073(2) 0.2222(2) 0.15574(18) 0.0209(5) Uani 1 1 d . . . . .
C24 C 0.4274(2) 0.3382(2) 0.08698(19) 0.0226(5) Uani 1 1 d . . . . .
C25 C 0.4481(3) 0.3866(2) -0.02525(19) 0.0290(6) Uani 1 1 d . . . . .
H25 H 0.5153 0.3455 -0.0605 0.035 Uiso 1 1 calc R U . . .
C26 C 0.3717(3) 0.4940(2) -0.0859(2) 0.0372(7) Uani 1 1 d . . . . .
H26 H 0.3872 0.5266 -0.1625 0.045 Uiso 1 1 calc R U . . .
C27 C 0.2736(3) 0.5541(3) -0.0366(2) 0.0393(7) Uani 1 1 d . . . . .
H27 H 0.2208 0.6273 -0.0788 0.047 Uiso 1 1 calc R U . . .
C28 C 0.2522(3) 0.5074(2) 0.0749(2) 0.0361(7) Uani 1 1 d . . . . .
H28 H 0.1845 0.5485 0.1096 0.043 Uiso 1 1 calc R U . . .
C29 C 0.3300(2) 0.4002(2) 0.1361(2) 0.0296(6) Uani 1 1 d . . . . .
H29 H 0.3159 0.3693 0.2128 0.036 Uiso 1 1 calc R U . . .
C30 C 0.7331(3) -0.0476(2) 0.6581(2) 0.0346(7) Uani 1 1 d . . . . .
H30A H 0.6581 -0.0448 0.7103 0.052 Uiso 1 1 calc R U . . .
H30B H 0.8068 -0.0417 0.6850 0.052 Uiso 1 1 calc R U . . .
H30C H 0.7501 -0.1249 0.6485 0.052 Uiso 1 1 calc R U . . .
O1S O 0.98035(19) 0.03415(19) 0.18152(16) 0.0507(6) Uani 1 1 d . . . . .
H1S H 0.9280 0.0611 0.2236 0.061 Uiso 1 1 calc R U . . .
C1S C 0.9499(3) 0.1043(3) 0.0746(2) 0.0480(8) Uani 1 1 d . . . . .
H1S1 H 0.9386 0.1916 0.0593 0.072 Uiso 1 1 calc R U . . .
H1S2 H 0.8709 0.0873 0.0657 0.072 Uiso 1 1 calc R U . . .
H1S3 H 1.0190 0.0828 0.0244 0.072 Uiso 1 1 calc R U . . .
O2S O 0.66625(18) 0.23515(17) 0.63043(14) 0.0367(5) Uani 1 1 d . . . . .
H2S H 0.7280 0.2141 0.6668 0.044 Uiso 1 1 calc R U . . .
C2S C 0.5517(3) 0.2293(3) 0.6999(3) 0.0491(8) Uani 1 1 d . . . . .
H2S1 H 0.5631 0.1539 0.7653 0.074 Uiso 1 1 calc R U . . .
H2S2 H 0.4836 0.2295 0.6628 0.074 Uiso 1 1 calc R U . . .
H2S3 H 0.5290 0.3004 0.7196 0.074 Uiso 1 1 calc R U . . .
O3S O 0.1511(2) 0.8258(2) 0.2423(2) 0.0687(8) Uani 1 1 d . . . . .
H3S H 0.0970 0.8910 0.2206 0.082 Uiso 1 1 calc R U . . .
C3S C 0.1400(5) 0.7503(4) 0.1961(3) 0.0849(14) Uani 1 1 d . . . . .
H3SC H 0.1874 0.6676 0.2342 0.102 Uiso 1 1 calc R U . . .
H3SA H 0.1747 0.7814 0.1200 0.102 Uiso 1 1 calc R U . . .
H3SB H 0.0501 0.7476 0.2010 0.102 Uiso 1 1 calc R 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
Gd1 O1 2.2751(16) . ?
Gd1 O5 2.3090(15) . ?
Gd1 O4 2.3173(15) . ?
Gd1 O2 2.3385(14) . ?
Gd1 O2 2.4044(15) 2_656 ?
Gd1 O6 2.4913(15) . ?
Gd1 N1 2.5055(19) . ?
Gd1 O3 2.5135(15) 2_656 ?
Gd1 Gd1 3.8387(3) 2_656 ?
O1 C1 1.329(3) . ?
O2 C9 1.337(3) . ?
O2 Gd1 2.4044(15) 2_656 ?
O3 C10 1.376(3) . ?
O3 C14 1.441(3) . ?
O3 Gd1 2.5135(15) 2_656 ?
O4 C23 1.271(3) . ?
O5 C21 1.277(3) . ?
O6 C30 1.425(3) . ?
O6 H6S 0.8400 . ?
N1 C7 1.277(3) . ?
N1 C6 1.422(3) . ?
C1 C2 1.396(4) . ?
C1 C6 1.411(4) . ?
C2 C3 1.375(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C7 C8 1.453(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.406(3) . ?
C8 C13 1.408(3) . ?
C9 C10 1.410(3) . ?
C10 C11 1.379(3) . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.365(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.384(4) . ?
C15 C20 1.384(3) . ?
C15 C21 1.492(3) . ?
C16 C17 1.383(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.366(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.362(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(4) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.394(3) . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.494(3) . ?
C24 C29 1.380(4) . ?
C24 C25 1.391(3) . ?
C25 C26 1.383(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.371(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.381(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.391(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O1S C1S 1.408(4) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.413(3) . ?
O2S H2S 0.8400 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
O3S C3S 1.365(4) . ?
O3S H3S 0.8400 . ?
C3S H3SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 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
O1 Gd1 O5 84.39(6) . . ?
O1 Gd1 O4 90.38(6) . . ?
O5 Gd1 O4 73.13(5) . . ?
O1 Gd1 O2 142.91(6) . . ?
O5 Gd1 O2 124.47(6) . . ?
O4 Gd1 O2 78.60(5) . . ?
O1 Gd1 O2 141.56(5) . 2_656 ?
O5 Gd1 O2 81.35(5) . 2_656 ?
O4 Gd1 O2 118.77(5) . 2_656 ?
O2 Gd1 O2 71.94(6) . 2_656 ?
O1 Gd1 O6 87.81(6) . . ?
O5 Gd1 O6 144.38(5) . . ?
O4 Gd1 O6 141.75(5) . . ?
O2 Gd1 O6 80.11(5) . . ?
O2 Gd1 O6 83.53(5) 2_656 . ?
O1 Gd1 N1 67.95(6) . . ?
O5 Gd1 N1 137.95(6) . . ?
O4 Gd1 N1 75.94(6) . . ?
O2 Gd1 N1 75.01(6) . . ?
O2 Gd1 N1 139.41(5) 2_656 . ?
O6 Gd1 N1 68.03(6) . . ?
O1 Gd1 O3 77.83(5) . 2_656 ?
O5 Gd1 O3 75.13(5) . 2_656 ?
O4 Gd1 O3 147.03(5) . 2_656 ?
O2 Gd1 O3 128.12(5) . 2_656 ?
O2 Gd1 O3 64.06(5) 2_656 2_656 ?
O6 Gd1 O3 69.26(5) . 2_656 ?
N1 Gd1 O3 125.23(6) . 2_656 ?
O1 Gd1 Gd1 167.57(4) . 2_656 ?
O5 Gd1 Gd1 104.52(4) . 2_656 ?
O4 Gd1 Gd1 100.43(4) . 2_656 ?
O2 Gd1 Gd1 36.55(4) . 2_656 ?
O2 Gd1 Gd1 35.39(3) 2_656 2_656 ?
O6 Gd1 Gd1 79.91(4) . 2_656 ?
N1 Gd1 Gd1 108.55(4) . 2_656 ?
O3 Gd1 Gd1 95.86(4) 2_656 2_656 ?
C1 O1 Gd1 121.60(14) . . ?
C9 O2 Gd1 131.09(14) . . ?
C9 O2 Gd1 120.38(13) . 2_656 ?
Gd1 O2 Gd1 108.06(6) . 2_656 ?
C10 O3 C14 117.67(18) . . ?
C10 O3 Gd1 116.56(13) . 2_656 ?
C14 O3 Gd1 125.73(14) . 2_656 ?
C23 O4 Gd1 135.08(15) . . ?
C21 O5 Gd1 135.81(15) . . ?
C30 O6 Gd1 132.14(15) . . ?
C30 O6 H6S 109.5 . . ?
Gd1 O6 H6S 113.4 . . ?
C7 N1 C6 119.5(2) . . ?
C7 N1 Gd1 127.53(16) . . ?
C6 N1 Gd1 112.33(15) . . ?
O1 C1 C2 122.2(2) . . ?
O1 C1 C6 119.8(2) . . ?
C2 C1 C6 118.0(2) . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 N1 124.8(2) . . ?
C1 C6 N1 115.0(2) . . ?
N1 C7 C8 127.4(2) . . ?
N1 C7 H7 116.3 . . ?
C8 C7 H7 116.3 . . ?
C9 C8 C13 119.0(2) . . ?
C9 C8 C7 125.7(2) . . ?
C13 C8 C7 115.3(2) . . ?
O2 C9 C8 124.6(2) . . ?
O2 C9 C10 117.8(2) . . ?
C8 C9 C10 117.6(2) . . ?
O3 C10 C11 123.3(2) . . ?
O3 C10 C9 114.70(19) . . ?
C11 C10 C9 122.0(2) . . ?
C10 C11 C12 119.8(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.7(2) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C8 121.9(2) . . ?
C12 C13 H13 119.1 . . ?
C8 C13 H13 119.1 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 117.6(2) . . ?
C16 C15 C21 119.3(2) . . ?
C20 C15 C21 123.1(2) . . ?
C17 C16 C15 120.7(2) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C18 C17 C16 120.9(3) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 119.1(3) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 120.7(3) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C15 121.1(3) . . ?
C19 C20 H20 119.5 . . ?
C15 C20 H20 119.5 . . ?
O5 C21 C22 123.3(2) . . ?
O5 C21 C15 116.1(2) . . ?
C22 C21 C15 120.5(2) . . ?
C23 C22 C21 125.3(2) . . ?
C23 C22 H22 117.4 . . ?
C21 C22 H22 117.4 . . ?
O4 C23 C22 123.9(2) . . ?
O4 C23 C24 116.8(2) . . ?
C22 C23 C24 119.3(2) . . ?
C29 C24 C25 118.6(2) . . ?
C29 C24 C23 119.1(2) . . ?
C25 C24 C23 122.3(2) . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 120.7(3) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 119.5(3) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 C29 119.9(3) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C24 C29 C28 120.8(2) . . ?
C24 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
O6 C30 H30A 109.5 . . ?
O6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C3S O3S H3S 109.5 . . ?
O3S C3S H3SC 109.5 . . ?
O3S C3S H3SA 109.5 . . ?
H3SC C3S H3SA 109.5 . . ?
O3S C3S H3SB 109.5 . . ?
H3SC C3S H3SB 109.5 . . ?
H3SA C3S H3SB 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
Gd1 O1 C1 C2 167.81(17) . . . . ?
Gd1 O1 C1 C6 -12.0(3) . . . . ?
O1 C1 C2 C3 -176.3(2) . . . . ?
C6 C1 C2 C3 3.5(4) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C3 C4 C5 C6 -0.3(4) . . . . ?
C4 C5 C6 C1 3.7(4) . . . . ?
C4 C5 C6 N1 -177.9(2) . . . . ?
O1 C1 C6 C5 174.6(2) . . . . ?
C2 C1 C6 C5 -5.2(3) . . . . ?
O1 C1 C6 N1 -3.9(3) . . . . ?
C2 C1 C6 N1 176.3(2) . . . . ?
C7 N1 C6 C5 25.6(3) . . . . ?
Gd1 N1 C6 C5 -163.03(19) . . . . ?
C7 N1 C6 C1 -156.0(2) . . . . ?
Gd1 N1 C6 C1 15.4(2) . . . . ?
C6 N1 C7 C8 -179.1(2) . . . . ?
Gd1 N1 C7 C8 11.0(3) . . . . ?
N1 C7 C8 C9 7.2(4) . . . . ?
N1 C7 C8 C13 -172.4(2) . . . . ?
Gd1 O2 C9 C8 -29.4(3) . . . . ?
Gd1 O2 C9 C8 159.46(17) 2_656 . . . ?
Gd1 O2 C9 C10 151.13(15) . . . . ?
Gd1 O2 C9 C10 -20.0(2) 2_656 . . . ?
C13 C8 C9 O2 -179.3(2) . . . . ?
C7 C8 C9 O2 1.1(4) . . . . ?
C13 C8 C9 C10 0.2(3) . . . . ?
C7 C8 C9 C10 -179.5(2) . . . . ?
C14 O3 C10 C11 17.3(3) . . . . ?
Gd1 O3 C10 C11 -160.54(19) 2_656 . . . ?
C14 O3 C10 C9 -162.3(2) . . . . ?
Gd1 O3 C10 C9 19.8(2) 2_656 . . . ?
O2 C9 C10 O3 -1.0(3) . . . . ?
C8 C9 C10 O3 179.57(18) . . . . ?
O2 C9 C10 C11 179.4(2) . . . . ?
C8 C9 C10 C11 -0.1(3) . . . . ?
O3 C10 C11 C12 -179.4(2) . . . . ?
C9 C10 C11 C12 0.2(4) . . . . ?
C10 C11 C12 C13 -0.4(4) . . . . ?
C11 C12 C13 C8 0.5(4) . . . . ?
C9 C8 C13 C12 -0.4(4) . . . . ?
C7 C8 C13 C12 179.3(2) . . . . ?
C20 C15 C16 C17 -1.2(4) . . . . ?
C21 C15 C16 C17 177.7(3) . . . . ?
C15 C16 C17 C18 0.6(5) . . . . ?
C16 C17 C18 C19 0.5(5) . . . . ?
C17 C18 C19 C20 -0.9(5) . . . . ?
C18 C19 C20 C15 0.2(4) . . . . ?
C16 C15 C20 C19 0.9(4) . . . . ?
C21 C15 C20 C19 -178.0(2) . . . . ?
Gd1 O5 C21 C22 -12.1(4) . . . . ?
Gd1 O5 C21 C15 168.92(15) . . . . ?
C16 C15 C21 O5 1.3(3) . . . . ?
C20 C15 C21 O5 -179.8(2) . . . . ?
C16 C15 C21 C22 -177.6(2) . . . . ?
C20 C15 C21 C22 1.2(4) . . . . ?
O5 C21 C22 C23 -4.0(4) . . . . ?
C15 C21 C22 C23 174.9(2) . . . . ?
Gd1 O4 C23 C22 14.4(4) . . . . ?
Gd1 O4 C23 C24 -168.98(15) . . . . ?
C21 C22 C23 O4 2.8(4) . . . . ?
C21 C22 C23 C24 -173.7(2) . . . . ?
O4 C23 C24 C29 -22.0(3) . . . . ?
C22 C23 C24 C29 154.7(2) . . . . ?
O4 C23 C24 C25 157.6(2) . . . . ?
C22 C23 C24 C25 -25.6(3) . . . . ?
C29 C24 C25 C26 -0.6(4) . . . . ?
C23 C24 C25 C26 179.8(2) . . . . ?
C24 C25 C26 C27 -0.6(4) . . . . ?
C25 C26 C27 C28 0.8(4) . . . . ?
C26 C27 C28 C29 0.0(4) . . . . ?
C25 C24 C29 C28 1.4(4) . . . . ?
C23 C24 C29 C28 -178.9(2) . . . . ?
C27 C28 C29 C24 -1.2(4) . . . . ?

_refine_diff_density_max         0.638
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_Dy_DMF
_database_code_depnum_ccdc_archive 'CCDC 1574219'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H58 Dy2 N4 O12'
_chemical_formula_weight         1400.14

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   11.2623(2)
_cell_length_b                   15.7686(3)
_cell_length_c                   15.5235(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.256(2)
_cell_angle_gamma                90
_cell_volume                     2740.41(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    13167
_cell_measurement_theta_min      2.9329
_cell_measurement_theta_max      33.1937

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_F_000             1396
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.280
_exptl_absorpt_coefficient_mu    2.776
_shelx_estimated_absorpt_T_min   0.435
_shelx_estimated_absorpt_T_max   0.510
_exptl_absorpt_correction_T_min  0.74282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15850
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.939
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4832
_reflns_number_gt                4121
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0317P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4832
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0525
_refine_ls_wR_factor_gt          0.0514
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.003
_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_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 0.52223(2) 0.11200(2) 0.54261(2) 0.01770(6) Uani 1 1 d . . . . .
O5 O 0.60951(16) 0.06413(12) 0.67425(12) 0.0224(4) Uani 1 1 d . . . . .
C28 C 0.8590(3) -0.07132(19) 0.8357(2) 0.0287(7) Uani 1 1 d . . . . .
H28 H 0.9424 -0.0631 0.8344 0.034 Uiso 1 1 calc R U . . .
O3 O 0.34430(17) 0.17551(12) 0.45908(13) 0.0262(5) Uani 1 1 d . . . . .
O1 O 0.62393(15) -0.01188(12) 0.51384(11) 0.0190(4) Uani 1 1 d . . . . .
O6 O 0.55849(19) 0.13609(13) 0.39550(13) 0.0277(5) Uani 1 1 d . . . . .
O4 O 0.38130(17) 0.12159(12) 0.64046(12) 0.0230(4) Uani 1 1 d . . . . .
C30 C 0.7795(3) 0.1476(3) 0.2468(2) 0.0420(9) Uani 1 1 d . . . . .
H30A H 0.8066 0.0903 0.2635 0.063 Uiso 1 1 calc R U . . .
H30B H 0.8462 0.1875 0.2583 0.063 Uiso 1 1 calc R U . . .
H30C H 0.7507 0.1486 0.1850 0.063 Uiso 1 1 calc R U . . .
N1 N 0.7360(2) 0.15655(15) 0.54231(14) 0.0212(5) Uani 1 1 d . . . . .
C32 C 0.6442(3) 0.12053(18) 0.35533(18) 0.0249(7) Uani 1 1 d . . . . .
H32 H 0.6850 0.0683 0.3668 0.030 Uiso 1 1 calc R U . . .
N2 N 0.6833(2) 0.17220(17) 0.29684(15) 0.0321(6) Uani 1 1 d . . . . .
C23 C 0.5708(2) 0.02861(17) 0.73892(18) 0.0210(6) Uani 1 1 d . . . . .
C15 C 0.2491(3) 0.10486(17) 0.74597(19) 0.0216(6) Uani 1 1 d . . . . .
C29 C 0.7779(3) -0.01852(19) 0.78833(19) 0.0254(7) Uani 1 1 d . . . . .
H29 H 0.8060 0.0251 0.7536 0.030 Uiso 1 1 calc R U . . .
O2 O 0.54483(17) 0.25158(13) 0.55734(13) 0.0280(5) Uani 1 1 d . . . . .
C8 C 0.7472(3) 0.24568(18) 0.52920(18) 0.0233(6) Uani 1 1 d . . . . .
C22 C 0.4554(2) 0.04209(18) 0.76318(18) 0.0224(6) Uani 1 1 d . . . . .
H22 H 0.4357 0.0174 0.8156 0.027 Uiso 1 1 calc R U . . .
C24 C 0.6554(3) -0.02889(18) 0.79123(18) 0.0214(6) Uani 1 1 d . . . . .
C17 C 0.0586(3) 0.1766(2) 0.7270(2) 0.0328(7) Uani 1 1 d . . . . .
H17 H 0.0052 0.2142 0.6945 0.039 Uiso 1 1 calc R U . . .
C20 C 0.2148(3) 0.0687(2) 0.8213(2) 0.0290(7) Uani 1 1 d . . . . .
H20 H 0.2681 0.0316 0.8547 0.035 Uiso 1 1 calc R U . . .
C4 C 0.9625(3) -0.1022(2) 0.6008(2) 0.0355(8) Uani 1 1 d . . . . .
H4 H 1.0400 -0.1239 0.6188 0.043 Uiso 1 1 calc R U . . .
C9 C 0.8489(3) 0.2874(2) 0.5078(2) 0.0302(7) Uani 1 1 d . . . . .
H9 H 0.9204 0.2564 0.5039 0.036 Uiso 1 1 calc R U . . .
C16 C 0.1687(3) 0.1586(2) 0.69887(19) 0.0269(7) Uani 1 1 d . . . . .
H16 H 0.1893 0.1833 0.6467 0.032 Uiso 1 1 calc R U . . .
C27 C 0.8180(3) -0.1362(2) 0.8852(2) 0.0350(8) Uani 1 1 d . . . . .
H27 H 0.8734 -0.1715 0.9190 0.042 Uiso 1 1 calc R U . . .
C11 C 0.7417(3) 0.4187(2) 0.4960(2) 0.0309(7) Uani 1 1 d . . . . .
H11 H 0.7399 0.4779 0.4842 0.037 Uiso 1 1 calc R U . . .
C5 C 0.9450(3) -0.0169(2) 0.5902(2) 0.0320(7) Uani 1 1 d . . . . .
H5 H 1.0112 0.0202 0.6021 0.038 Uiso 1 1 calc R U . . .
C21 C 0.3686(2) 0.08987(17) 0.71408(18) 0.0198(6) Uani 1 1 d . . . . .
C10 C 0.8464(3) 0.3737(2) 0.4922(2) 0.0352(8) Uani 1 1 d . . . . .
H10 H 0.9166 0.4020 0.4788 0.042 Uiso 1 1 calc R U . . .
C7 C 0.8297(3) 0.10935(18) 0.55422(19) 0.0246(7) Uani 1 1 d . . . . .
H7 H 0.9048 0.1374 0.5581 0.030 Uiso 1 1 calc R U . . .
C33 C 0.3449(3) 0.2507(2) 0.4069(2) 0.0389(8) Uani 1 1 d . . . . .
H33A H 0.3255 0.2357 0.3457 0.058 Uiso 1 1 calc R U . . .
H33B H 0.4243 0.2768 0.4153 0.058 Uiso 1 1 calc R U . . .
H33C H 0.2854 0.2908 0.4242 0.058 Uiso 1 1 calc R U . . .
C1 C 0.7343(2) -0.03730(18) 0.54361(17) 0.0201(6) Uani 1 1 d . . . . .
C19 C 0.1043(3) 0.0858(2) 0.8481(2) 0.0334(8) Uani 1 1 d . . . . .
H19 H 0.0819 0.0598 0.8991 0.040 Uiso 1 1 calc R U . . .
C31 C 0.6284(4) 0.2541(2) 0.2792(2) 0.0484(10) Uani 1 1 d . . . . .
H31A H 0.5661 0.2493 0.2302 0.073 Uiso 1 1 calc R U . . .
H31B H 0.6891 0.2948 0.2650 0.073 Uiso 1 1 calc R U . . .
H31C H 0.5928 0.2737 0.3305 0.073 Uiso 1 1 calc R U . . .
C12 C 0.6399(3) 0.37836(18) 0.51691(19) 0.0277(7) Uani 1 1 d . . . . .
H12 H 0.5686 0.4101 0.5187 0.033 Uiso 1 1 calc R U . . .
C25 C 0.6158(3) -0.09594(19) 0.8394(2) 0.0290(7) Uani 1 1 d . . . . .
H25 H 0.5325 -0.1047 0.8406 0.035 Uiso 1 1 calc R U . . .
C6 C 0.8324(2) 0.01758(18) 0.56227(18) 0.0233(6) Uani 1 1 d . . . . .
C3 C 0.8661(3) -0.1568(2) 0.5849(2) 0.0311(7) Uani 1 1 d . . . . .
H3 H 0.8766 -0.2161 0.5930 0.037 Uiso 1 1 calc R U . . .
C18 C 0.0265(3) 0.1404(2) 0.8015(2) 0.0325(8) Uani 1 1 d . . . . .
H18 H -0.0488 0.1530 0.8207 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6400(3) 0.29144(19) 0.53551(18) 0.0242(6) Uani 1 1 d . . . . .
C26 C 0.6961(3) -0.1496(2) 0.8854(2) 0.0360(8) Uani 1 1 d . . . . .
H26 H 0.6682 -0.1956 0.9172 0.043 Uiso 1 1 calc R U . . .
C2 C 0.7554(3) -0.12437(18) 0.55735(18) 0.0236(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.225(2) . ?
Dy1 O5 2.2966(19) . ?
Dy1 O4 2.3184(18) . ?
Dy1 O1 2.3320(18) . ?
Dy1 O1 2.3781(18) 3_656 ?
Dy1 O6 2.3936(19) . ?
Dy1 O3 2.4766(19) . ?
Dy1 N1 2.508(2) . ?
Dy1 Dy1 3.7858(3) 3_656 ?
O5 C23 1.268(3) . ?
C28 C29 1.387(4) . ?
C28 C27 1.388(4) . ?
C28 H28 0.9500 . ?
O3 C2 1.383(3) 3_656 ?
O3 C33 1.435(3) . ?
O1 C1 1.340(3) . ?
O1 Dy1 2.3782(18) 3_656 ?
O6 C32 1.229(4) . ?
O4 C21 1.270(3) . ?
C30 N2 1.453(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
N1 C7 1.288(4) . ?
N1 C8 1.428(4) . ?
C32 N2 1.330(4) . ?
C32 H32 0.9500 . ?
N2 C31 1.445(4) . ?
C23 C22 1.408(4) . ?
C23 C24 1.490(4) . ?
C15 C16 1.389(4) . ?
C15 C20 1.393(4) . ?
C15 C21 1.503(4) . ?
C29 C24 1.395(4) . ?
C29 H29 0.9500 . ?
O2 C13 1.319(3) . ?
C8 C9 1.392(4) . ?
C8 C13 1.419(4) . ?
C22 C21 1.393(4) . ?
C22 H22 0.9500 . ?
C24 C25 1.396(4) . ?
C17 C18 1.374(4) . ?
C17 C16 1.387(4) . ?
C17 H17 0.9500 . ?
C20 C19 1.381(4) . ?
C20 H20 0.9500 . ?
C4 C5 1.366(4) . ?
C4 C3 1.386(5) . ?
C4 H4 0.9500 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9500 . ?
C16 H16 0.9500 . ?
C27 C26 1.389(5) . ?
C27 H27 0.9500 . ?
C11 C12 1.381(4) . ?
C11 C10 1.384(5) . ?
C11 H11 0.9500 . ?
C5 C6 1.404(4) . ?
C5 H5 0.9500 . ?
C10 H10 0.9500 . ?
C7 C6 1.452(4) . ?
C7 H7 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C1 C2 1.406(4) . ?
C1 C6 1.409(4) . ?
C19 C18 1.376(5) . ?
C19 H19 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C12 C13 1.401(4) . ?
C12 H12 0.9500 . ?
C25 C26 1.380(4) . ?
C25 H25 0.9500 . ?
C3 C2 1.372(4) . ?
C3 H3 0.9500 . ?
C18 H18 0.9500 . ?
C26 H26 0.9500 . ?
C2 O3 1.383(3) 3_656 ?

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 O5 101.57(7) . . ?
O2 Dy1 O4 86.96(7) . . ?
O5 Dy1 O4 72.28(7) . . ?
O2 Dy1 O1 142.69(6) . . ?
O5 Dy1 O1 73.95(6) . . ?
O4 Dy1 O1 124.45(6) . . ?
O2 Dy1 O1 139.60(7) . 3_656 ?
O5 Dy1 O1 108.76(6) . 3_656 ?
O4 Dy1 O1 77.81(6) . 3_656 ?
O1 Dy1 O1 73.03(7) . 3_656 ?
O2 Dy1 O6 84.93(7) . . ?
O5 Dy1 O6 143.14(7) . . ?
O4 Dy1 O6 144.58(7) . . ?
O1 Dy1 O6 79.16(7) . . ?
O1 Dy1 O6 86.39(6) 3_656 . ?
O2 Dy1 O3 74.38(7) . . ?
O5 Dy1 O3 147.38(7) . . ?
O4 Dy1 O3 75.17(7) . . ?
O1 Dy1 O3 128.66(6) . . ?
O1 Dy1 O3 65.64(6) 3_656 . ?
O6 Dy1 O3 69.44(7) . . ?
O2 Dy1 N1 67.92(7) . . ?
O5 Dy1 N1 77.05(7) . . ?
O4 Dy1 N1 135.13(7) . . ?
O1 Dy1 N1 75.09(7) . . ?
O1 Dy1 N1 144.21(7) 3_656 . ?
O6 Dy1 N1 71.95(7) . . ?
O3 Dy1 N1 127.43(7) . . ?
O2 Dy1 Dy1 165.54(5) . 3_656 ?
O5 Dy1 Dy1 91.82(5) . 3_656 ?
O4 Dy1 Dy1 102.46(5) . 3_656 ?
O1 Dy1 Dy1 36.93(4) . 3_656 ?
O1 Dy1 Dy1 36.10(4) 3_656 3_656 ?
O6 Dy1 Dy1 81.06(5) . 3_656 ?
O3 Dy1 Dy1 97.22(5) . 3_656 ?
N1 Dy1 Dy1 110.55(5) . 3_656 ?
C23 O5 Dy1 134.37(17) . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C2 O3 C33 115.5(2) 3_656 . ?
C2 O3 Dy1 117.05(16) 3_656 . ?
C33 O3 Dy1 125.15(18) . . ?
C1 O1 Dy1 129.89(17) . . ?
C1 O1 Dy1 120.50(17) . 3_656 ?
Dy1 O1 Dy1 106.97(7) . 3_656 ?
C32 O6 Dy1 132.62(19) . . ?
C21 O4 Dy1 135.73(18) . . ?
N2 C30 H30A 109.5 . . ?
N2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C7 N1 C8 120.4(2) . . ?
C7 N1 Dy1 127.56(19) . . ?
C8 N1 Dy1 112.06(17) . . ?
O6 C32 N2 124.1(3) . . ?
O6 C32 H32 117.9 . . ?
N2 C32 H32 117.9 . . ?
C32 N2 C31 120.6(3) . . ?
C32 N2 C30 121.6(3) . . ?
C31 N2 C30 117.8(3) . . ?
O5 C23 C22 123.5(3) . . ?
O5 C23 C24 116.5(2) . . ?
C22 C23 C24 120.0(3) . . ?
C16 C15 C20 117.9(3) . . ?
C16 C15 C21 118.6(3) . . ?
C20 C15 C21 123.5(3) . . ?
C28 C29 C24 120.6(3) . . ?
C28 C29 H29 119.7 . . ?
C24 C29 H29 119.7 . . ?
C13 O2 Dy1 122.16(17) . . ?
C9 C8 C13 120.3(3) . . ?
C9 C8 N1 125.9(3) . . ?
C13 C8 N1 113.7(2) . . ?
C21 C22 C23 123.2(3) . . ?
C21 C22 H22 118.4 . . ?
C23 C22 H22 118.4 . . ?
C29 C24 C25 118.7(3) . . ?
C29 C24 C23 119.1(3) . . ?
C25 C24 C23 122.0(3) . . ?
C18 C17 C16 120.4(3) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C19 C20 C15 120.9(3) . . ?
C19 C20 H20 119.5 . . ?
C15 C20 H20 119.5 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C10 C9 C8 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C17 C16 C15 120.9(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C4 C5 C6 122.2(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
O4 C21 C22 124.4(3) . . ?
O4 C21 C15 115.3(2) . . ?
C22 C21 C15 120.3(3) . . ?
C9 C10 C11 119.9(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
N1 C7 C6 126.6(3) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
O3 C33 H33A 109.5 . . ?
O3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O1 C1 C2 118.6(2) . . ?
O1 C1 C6 124.4(3) . . ?
C2 C1 C6 117.0(3) . . ?
C18 C19 C20 120.5(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
N2 C31 H31A 109.5 . . ?
N2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C11 C12 C13 121.2(3) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C26 C25 C24 120.8(3) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C5 C6 C1 119.1(3) . . ?
C5 C6 C7 115.0(3) . . ?
C1 C6 C7 125.9(3) . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C17 C18 C19 119.5(3) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
O2 C13 C12 122.5(3) . . ?
O2 C13 C8 119.8(3) . . ?
C12 C13 C8 117.7(3) . . ?
C25 C26 C27 119.8(3) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C3 C2 O3 122.2(3) . 3_656 ?
C3 C2 C1 122.9(3) . . ?
O3 C2 C1 114.9(2) 3_656 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C33 H33B O2 0.98 2.49 3.062(4) 116.8 .
C31 H31A O2 0.98 2.67 3.471(4) 139.4 4_565

_refine_diff_density_max         1.024
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.076

####################################################################### 
# 
# 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_Dy_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1574218'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H76 Dy2 N2 O18'
_chemical_formula_weight         1510.28

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8879(2)
_cell_length_b                   12.2929(2)
_cell_length_c                   13.6009(3)
_cell_angle_alpha                65.334(2)
_cell_angle_beta                 78.453(2)
_cell_angle_gamma                74.994(2)
_cell_volume                     1589.06(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    17836
_cell_measurement_theta_min      2.9306
_cell_measurement_theta_max      33.2039

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_F_000             762
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.406
_shelx_estimated_absorpt_T_min   0.504
_shelx_estimated_absorpt_T_max   0.729
_exptl_absorpt_correction_T_min  0.74362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14994
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.930
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5579
_reflns_number_gt                5256
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0262P)²+0.4046P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5579
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0421
_refine_ls_wR_factor_gt          0.0418
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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_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 0.63050(2) 0.06908(2) 0.39287(2) 0.01379(4) Uani 1 1 d . . . . .
O1 O 0.80569(13) 0.13989(13) 0.29455(11) 0.0219(3) Uani 1 1 d . . . . .
O2 O 0.43771(12) 0.11605(12) 0.48878(10) 0.0151(3) Uani 1 1 d . . . . .
O3 O 0.19494(13) 0.11330(13) 0.54632(11) 0.0184(3) Uani 1 1 d . . . . .
O4 O 0.51059(13) 0.20468(13) 0.25467(11) 0.0193(3) Uani 1 1 d . . . . .
O5 O 0.65422(14) -0.02047(13) 0.27161(11) 0.0196(3) Uani 1 1 d . . . . .
O6 O 0.70959(14) 0.05362(13) 0.55626(11) 0.0214(3) Uani 1 1 d . . . . .
H6S H 0.6926 0.1200 0.5648 0.026 Uiso 1 1 calc R U . . .
N1 N 0.63027(16) 0.27232(15) 0.38952(13) 0.0163(4) Uani 1 1 d . . . . .
C1 C 0.8396(2) 0.23270(19) 0.30132(16) 0.0208(5) Uani 1 1 d . . . . .
C2 C 0.9598(2) 0.2629(2) 0.25815(18) 0.0279(5) Uani 1 1 d . . . . .
H2 H 1.0183 0.2187 0.2194 0.033 Uiso 1 1 calc R U . . .
C3 C 0.9942(2) 0.3560(2) 0.2712(2) 0.0337(6) Uani 1 1 d . . . . .
H3 H 1.0761 0.3754 0.2414 0.040 Uiso 1 1 calc R U . . .
C4 C 0.9104(2) 0.4214(2) 0.3274(2) 0.0325(6) Uani 1 1 d . . . . .
H4 H 0.9358 0.4839 0.3378 0.039 Uiso 1 1 calc R U . . .
C5 C 0.7901(2) 0.3957(2) 0.36813(18) 0.0264(5) Uani 1 1 d . . . . .
H5 H 0.7324 0.4406 0.4066 0.032 Uiso 1 1 calc R U . . .
C6 C 0.7529(2) 0.30426(19) 0.35306(16) 0.0202(5) Uani 1 1 d . . . . .
C7 C 0.5336(2) 0.35154(19) 0.40323(16) 0.0202(5) Uani 1 1 d . . . . .
H7 H 0.5492 0.4300 0.3874 0.024 Uiso 1 1 calc R U . . .
C8 C 0.40240(19) 0.33493(19) 0.44033(16) 0.0187(4) Uani 1 1 d . . . . .
C9 C 0.36086(19) 0.22312(18) 0.47907(15) 0.0158(4) Uani 1 1 d . . . . .
C10 C 0.22899(19) 0.22559(18) 0.51012(16) 0.0176(4) Uani 1 1 d . . . . .
C11 C 0.1424(2) 0.3308(2) 0.50473(19) 0.0259(5) Uani 1 1 d . . . . .
H11 H 0.0542 0.3288 0.5268 0.031 Uiso 1 1 calc R U . . .
C12 C 0.1847(2) 0.4402(2) 0.4667(2) 0.0321(6) Uani 1 1 d . . . . .
H12 H 0.1255 0.5137 0.4620 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3119(2) 0.4414(2) 0.43592(19) 0.0265(5) Uani 1 1 d . . . . .
H13 H 0.3401 0.5164 0.4108 0.032 Uiso 1 1 calc R U . . .
C14 C 0.06244(19) 0.1124(2) 0.54886(19) 0.0264(5) Uani 1 1 d . . . . .
H14A H 0.0119 0.1389 0.6060 0.040 Uiso 1 1 calc R U . . .
H14B H 0.0531 0.0295 0.5640 0.040 Uiso 1 1 calc R U . . .
H14C H 0.0321 0.1681 0.4783 0.040 Uiso 1 1 calc R U . . .
C15 C 0.69066(19) -0.07329(19) 0.11907(17) 0.0189(4) Uani 1 1 d . . . . .
C16 C 0.7538(2) -0.1886(2) 0.18000(19) 0.0313(6) Uani 1 1 d . . . . .
H16 H 0.7656 -0.2081 0.2532 0.038 Uiso 1 1 calc R U . . .
C17 C 0.8001(3) -0.2762(2) 0.1355(2) 0.0372(6) Uani 1 1 d . . . . .
H17 H 0.8420 -0.3553 0.1789 0.045 Uiso 1 1 calc R U . . .
C18 C 0.7862(2) -0.2500(2) 0.0295(2) 0.0309(5) Uani 1 1 d . . . . .
H18 H 0.8181 -0.3103 -0.0007 0.037 Uiso 1 1 calc R U . . .
C19 C 0.7255(2) -0.1355(2) -0.0322(2) 0.0333(6) Uani 1 1 d . . . . .
H19 H 0.7162 -0.1162 -0.1060 0.040 Uiso 1 1 calc R U . . .
C20 C 0.6777(2) -0.0476(2) 0.01157(19) 0.0291(5) Uani 1 1 d . . . . .
H20 H 0.6356 0.0312 -0.0323 0.035 Uiso 1 1 calc R U . . .
C21 C 0.63779(19) 0.01697(19) 0.17158(16) 0.0184(4) Uani 1 1 d . . . . .
C22 C 0.5720(2) 0.1333(2) 0.11264(17) 0.0207(5) Uani 1 1 d . . . . .
H22 H 0.5695 0.1553 0.0372 0.025 Uiso 1 1 calc R U . . .
C23 C 0.50954(19) 0.21961(19) 0.15692(16) 0.0183(4) Uani 1 1 d . . . . .
C24 C 0.4297(2) 0.33629(19) 0.08739(17) 0.0196(4) Uani 1 1 d . . . . .
C25 C 0.4517(2) 0.3843(2) -0.02576(18) 0.0252(5) Uani 1 1 d . . . . .
H25 H 0.5195 0.3431 -0.0613 0.030 Uiso 1 1 calc R U . . .
C26 C 0.3754(2) 0.4916(2) -0.08672(19) 0.0319(6) Uani 1 1 d . . . . .
H26 H 0.3918 0.5243 -0.1638 0.038 Uiso 1 1 calc R U . . .
C27 C 0.2758(2) 0.5513(2) -0.0365(2) 0.0334(6) Uani 1 1 d . . . . .
H27 H 0.2227 0.6243 -0.0787 0.040 Uiso 1 1 calc R U . . .
C28 C 0.2533(2) 0.5047(2) 0.0758(2) 0.0310(5) Uani 1 1 d . . . . .
H28 H 0.1845 0.5458 0.1107 0.037 Uiso 1 1 calc R U . . .
C29 C 0.3307(2) 0.3983(2) 0.13777(18) 0.0248(5) Uani 1 1 d . . . . .
H29 H 0.3160 0.3679 0.2149 0.030 Uiso 1 1 calc R U . . .
C30 C 0.7305(2) -0.0455(2) 0.65862(18) 0.0277(5) Uani 1 1 d . . . . .
H30A H 0.6541 -0.0418 0.7102 0.042 Uiso 1 1 calc R U . . .
H30B H 0.8036 -0.0397 0.6868 0.042 Uiso 1 1 calc R U . . .
H30C H 0.7482 -0.1230 0.6490 0.042 Uiso 1 1 calc R U . . .
O1S O 0.97774(17) 0.02945(17) 0.17785(15) 0.0440(5) Uani 1 1 d . . . . .
H1S H 0.9257 0.0555 0.2214 0.053 Uiso 1 1 calc R U . . .
C1S C 0.9497(3) 0.1052(3) 0.0698(2) 0.0394(6) Uani 1 1 d . . . . .
H1S1 H 0.9364 0.1911 0.0595 0.059 Uiso 1 1 calc R U . . .
H1S2 H 0.8720 0.0894 0.0565 0.059 Uiso 1 1 calc R U . . .
H1S3 H 1.0212 0.0875 0.0186 0.059 Uiso 1 1 calc R U . . .
O2S O 0.66626(16) 0.23640(15) 0.63052(13) 0.0308(4) Uani 1 1 d . . . . .
H2S H 0.7282 0.2152 0.6671 0.037 Uiso 1 1 calc R U . . .
C2S C 0.5505(3) 0.2316(3) 0.7007(2) 0.0414(6) Uani 1 1 d . . . . .
H2S1 H 0.5619 0.1573 0.7670 0.062 Uiso 1 1 calc R U . . .
H2S2 H 0.4824 0.2307 0.6637 0.062 Uiso 1 1 calc R U . . .
H2S3 H 0.5271 0.3033 0.7199 0.062 Uiso 1 1 calc R U . . .
O3S O 0.1522(2) 0.8244(2) 0.23982(19) 0.0627(7) Uani 1 1 d . . . . .
H3S H 0.0969 0.8884 0.2165 0.075 Uiso 1 1 calc R U . . .
C3S C 0.1419(4) 0.7438(3) 0.1982(3) 0.0736(11) Uani 1 1 d . . . . .
H3SC H 0.1886 0.6623 0.2399 0.088 Uiso 1 1 calc R U . . .
H3SA H 0.1783 0.7699 0.1219 0.088 Uiso 1 1 calc R U . . .
H3SB H 0.0516 0.7413 0.2030 0.088 Uiso 1 1 calc R 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 O1 2.2475(14) . ?
Dy1 O5 2.2794(14) . ?
Dy1 O4 2.2927(13) . ?
Dy1 O2 2.3122(13) . ?
Dy1 O2 2.3792(13) 2_656 ?
Dy1 O6 2.4587(14) . ?
Dy1 N1 2.4791(17) . ?
Dy1 O3 2.4896(13) 2_656 ?
Dy1 Dy1 3.8086(2) 2_656 ?
O1 C1 1.329(3) . ?
O2 C9 1.334(2) . ?
O2 Dy1 2.3792(13) 2_656 ?
O3 C10 1.382(2) . ?
O3 C14 1.439(2) . ?
O3 Dy1 2.4896(13) 2_656 ?
O4 C23 1.266(2) . ?
O5 C21 1.276(2) . ?
O6 C30 1.429(3) . ?
O6 H6S 0.8400 . ?
N1 C7 1.278(3) . ?
N1 C6 1.424(3) . ?
C1 C2 1.399(3) . ?
C1 C6 1.407(3) . ?
C2 C3 1.378(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.454(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.406(3) . ?
C8 C9 1.412(3) . ?
C9 C10 1.409(3) . ?
C10 C11 1.372(3) . ?
C11 C12 1.390(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.366(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.383(3) . ?
C15 C20 1.390(3) . ?
C15 C21 1.496(3) . ?
C16 C17 1.386(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.370(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.394(3) . ?
C22 C23 1.395(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.503(3) . ?
C24 C29 1.388(3) . ?
C24 C25 1.393(3) . ?
C25 C26 1.383(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(3) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O1S C1S 1.418(3) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.419(3) . ?
O2S H2S 0.8400 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
O3S C3S 1.365(4) . ?
O3S H3S 0.8400 . ?
C3S H3SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 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
O1 Dy1 O5 83.61(5) . . ?
O1 Dy1 O4 89.76(5) . . ?
O5 Dy1 O4 73.77(5) . . ?
O1 Dy1 O2 144.34(5) . . ?
O5 Dy1 O2 123.76(5) . . ?
O4 Dy1 O2 78.54(5) . . ?
O1 Dy1 O2 141.30(5) . 2_656 ?
O5 Dy1 O2 80.73(5) . 2_656 ?
O4 Dy1 O2 118.91(5) . 2_656 ?
O2 Dy1 O2 71.46(5) . 2_656 ?
O1 Dy1 O6 88.58(5) . . ?
O5 Dy1 O6 144.29(5) . . ?
O4 Dy1 O6 141.18(5) . . ?
O2 Dy1 O6 80.51(5) . . ?
O2 Dy1 O6 84.03(5) 2_656 . ?
O1 Dy1 N1 68.56(5) . . ?
O5 Dy1 N1 138.13(5) . . ?
O4 Dy1 N1 75.44(5) . . ?
O2 Dy1 N1 75.89(5) . . ?
O2 Dy1 N1 139.85(5) 2_656 . ?
O6 Dy1 N1 67.92(5) . . ?
O1 Dy1 O3 77.12(5) . 2_656 ?
O5 Dy1 O3 74.87(5) . 2_656 ?
O4 Dy1 O3 147.10(5) . 2_656 ?
O2 Dy1 O3 128.39(4) . 2_656 ?
O2 Dy1 O3 64.70(4) 2_656 2_656 ?
O6 Dy1 O3 69.43(5) . 2_656 ?
N1 Dy1 O3 124.84(5) . 2_656 ?
O1 Dy1 Dy1 168.74(4) . 2_656 ?
O5 Dy1 Dy1 103.69(4) . 2_656 ?
O4 Dy1 Dy1 100.45(4) . 2_656 ?
O2 Dy1 Dy1 36.32(3) . 2_656 ?
O2 Dy1 Dy1 35.14(3) 2_656 2_656 ?
O6 Dy1 Dy1 80.50(3) . 2_656 ?
N1 Dy1 Dy1 109.24(4) . 2_656 ?
O3 Dy1 Dy1 96.32(3) 2_656 2_656 ?
C1 O1 Dy1 121.35(13) . . ?
C9 O2 Dy1 131.05(12) . . ?
C9 O2 Dy1 120.01(12) . 2_656 ?
Dy1 O2 Dy1 108.54(5) . 2_656 ?
C10 O3 C14 117.46(15) . . ?
C10 O3 Dy1 116.26(11) . 2_656 ?
C14 O3 Dy1 126.25(12) . 2_656 ?
C23 O4 Dy1 134.53(13) . . ?
C21 O5 Dy1 135.38(13) . . ?
C30 O6 Dy1 131.75(13) . . ?
C30 O6 H6S 109.5 . . ?
Dy1 O6 H6S 113.3 . . ?
C7 N1 C6 119.73(18) . . ?
C7 N1 Dy1 127.56(14) . . ?
C6 N1 Dy1 112.09(13) . . ?
O1 C1 C2 122.2(2) . . ?
O1 C1 C6 119.78(19) . . ?
C2 C1 C6 118.1(2) . . ?
C3 C2 C1 120.7(2) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.6(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 120.5(2) . . ?
C5 C6 N1 124.7(2) . . ?
C1 C6 N1 114.80(19) . . ?
N1 C7 C8 127.2(2) . . ?
N1 C7 H7 116.4 . . ?
C8 C7 H7 116.4 . . ?
C13 C8 C9 119.04(19) . . ?
C13 C8 C7 115.38(19) . . ?
C9 C8 C7 125.58(18) . . ?
O2 C9 C10 118.16(18) . . ?
O2 C9 C8 124.54(18) . . ?
C10 C9 C8 117.29(18) . . ?
C11 C10 O3 123.18(19) . . ?
C11 C10 C9 122.61(19) . . ?
O3 C10 C9 114.21(17) . . ?
C10 C11 C12 119.5(2) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 119.6(2) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C8 122.0(2) . . ?
C12 C13 H13 119.0 . . ?
C8 C13 H13 119.0 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 117.9(2) . . ?
C16 C15 C21 119.04(19) . . ?
C20 C15 C21 123.1(2) . . ?
C15 C16 C17 120.8(2) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 120.8(2) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C19 C18 C17 119.0(2) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 120.8(2) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C15 120.8(2) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
O5 C21 C22 123.6(2) . . ?
O5 C21 C15 116.10(18) . . ?
C22 C21 C15 120.30(18) . . ?
C21 C22 C23 124.45(19) . . ?
C21 C22 H22 117.8 . . ?
C23 C22 H22 117.8 . . ?
O4 C23 C22 124.35(19) . . ?
O4 C23 C24 116.54(19) . . ?
C22 C23 C24 119.04(18) . . ?
C29 C24 C25 118.9(2) . . ?
C29 C24 C23 118.79(19) . . ?
C25 C24 C23 122.3(2) . . ?
C26 C25 C24 120.4(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 120.4(2) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 119.7(2) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 C29 120.4(2) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C24 120.2(2) . . ?
C28 C29 H29 119.9 . . ?
C24 C29 H29 119.9 . . ?
O6 C30 H30A 109.5 . . ?
O6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C3S O3S H3S 109.5 . . ?
O3S C3S H3SC 109.5 . . ?
O3S C3S H3SA 109.5 . . ?
H3SC C3S H3SA 109.5 . . ?
O3S C3S H3SB 109.5 . . ?
H3SC C3S H3SB 109.5 . . ?
H3SA C3S H3SB 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
Dy1 O1 C1 C2 167.25(15) . . . . ?
Dy1 O1 C1 C6 -12.9(2) . . . . ?
O1 C1 C2 C3 -176.82(19) . . . . ?
C6 C1 C2 C3 3.4(3) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 C1 3.4(3) . . . . ?
C4 C5 C6 N1 -178.50(19) . . . . ?
O1 C1 C6 C5 175.11(18) . . . . ?
C2 C1 C6 C5 -5.1(3) . . . . ?
O1 C1 C6 N1 -3.2(3) . . . . ?
C2 C1 C6 N1 176.65(17) . . . . ?
C7 N1 C6 C5 25.3(3) . . . . ?
Dy1 N1 C6 C5 -163.05(16) . . . . ?
C7 N1 C6 C1 -156.52(18) . . . . ?
Dy1 N1 C6 C1 15.1(2) . . . . ?
C6 N1 C7 C8 -179.60(19) . . . . ?
Dy1 N1 C7 C8 10.2(3) . . . . ?
N1 C7 C8 C13 -172.8(2) . . . . ?
N1 C7 C8 C9 7.2(3) . . . . ?
Dy1 O2 C9 C10 151.67(14) . . . . ?
Dy1 O2 C9 C10 -20.2(2) 2_656 . . . ?
Dy1 O2 C9 C8 -28.8(3) . . . . ?
Dy1 O2 C9 C8 159.37(15) 2_656 . . . ?
C13 C8 C9 O2 -178.79(19) . . . . ?
C7 C8 C9 O2 1.3(3) . . . . ?
C13 C8 C9 C10 0.8(3) . . . . ?
C7 C8 C9 C10 -179.15(19) . . . . ?
C14 O3 C10 C11 18.0(3) . . . . ?
Dy1 O3 C10 C11 -159.99(16) 2_656 . . . ?
C14 O3 C10 C9 -162.08(17) . . . . ?
Dy1 O3 C10 C9 20.0(2) 2_656 . . . ?
O2 C9 C10 C11 179.02(19) . . . . ?
C8 C9 C10 C11 -0.6(3) . . . . ?
O2 C9 C10 O3 -0.9(3) . . . . ?
C8 C9 C10 O3 179.48(16) . . . . ?
O3 C10 C11 C12 -179.6(2) . . . . ?
C9 C10 C11 C12 0.4(3) . . . . ?
C10 C11 C12 C13 -0.5(4) . . . . ?
C11 C12 C13 C8 0.7(4) . . . . ?
C9 C8 C13 C12 -0.9(3) . . . . ?
C7 C8 C13 C12 179.0(2) . . . . ?
C20 C15 C16 C17 -1.3(4) . . . . ?
C21 C15 C16 C17 177.7(2) . . . . ?
C15 C16 C17 C18 1.0(4) . . . . ?
C16 C17 C18 C19 0.0(4) . . . . ?
C17 C18 C19 C20 -0.7(4) . . . . ?
C18 C19 C20 C15 0.3(4) . . . . ?
C16 C15 C20 C19 0.7(3) . . . . ?
C21 C15 C20 C19 -178.3(2) . . . . ?
Dy1 O5 C21 C22 -13.4(3) . . . . ?
Dy1 O5 C21 C15 168.30(13) . . . . ?
C16 C15 C21 O5 -0.7(3) . . . . ?
C20 C15 C21 O5 178.3(2) . . . . ?
C16 C15 C21 C22 -179.0(2) . . . . ?
C20 C15 C21 C22 0.0(3) . . . . ?
O5 C21 C22 C23 -4.2(3) . . . . ?
C15 C21 C22 C23 173.97(19) . . . . ?
Dy1 O4 C23 C22 14.4(3) . . . . ?
Dy1 O4 C23 C24 -168.71(13) . . . . ?
C21 C22 C23 O4 3.6(3) . . . . ?
C21 C22 C23 C24 -173.17(19) . . . . ?
O4 C23 C24 C29 -22.2(3) . . . . ?
C22 C23 C24 C29 154.8(2) . . . . ?
O4 C23 C24 C25 157.7(2) . . . . ?
C22 C23 C24 C25 -25.2(3) . . . . ?
C29 C24 C25 C26 -0.5(3) . . . . ?
C23 C24 C25 C26 179.6(2) . . . . ?
C24 C25 C26 C27 -0.9(4) . . . . ?
C25 C26 C27 C28 1.1(4) . . . . ?
C26 C27 C28 C29 0.1(4) . . . . ?
C27 C28 C29 C24 -1.4(4) . . . . ?
C25 C24 C29 C28 1.6(3) . . . . ?
C23 C24 C29 C28 -178.4(2) . . . . ?

_refine_diff_density_max         0.712
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.068

####################################################################### 
# 
# 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_Gd_DMF
_database_code_depnum_ccdc_archive 'CCDC 1574222'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H58 Gd2 N4 O12'
_chemical_formula_weight         1389.64

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   11.2606(13)
_cell_length_b                   15.9046(15)
_cell_length_c                   15.5822(17)
_cell_angle_alpha                90
_cell_angle_beta                 96.903(5)
_cell_angle_gamma                90
_cell_volume                     2770.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9868
_cell_measurement_theta_min      2.4750
_cell_measurement_theta_max      26.3352

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             1388
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.443
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40304
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.227
_diffrn_reflns_theta_max         26.417
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5677
_reflns_number_gt                4599
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'XT, VERSION 2014/5'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0116P)²+7.0925P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5677
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0592
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Gd1 Gd 0.52127(2) 0.38808(2) 0.54311(2) 0.01571(6) Uani 1 1 d . . . . .
O1 O 0.6269(2) 0.51118(16) 0.51427(16) 0.0168(6) Uani 1 1 d . . . . .
O2 O 0.5448(2) 0.24826(17) 0.5552(2) 0.0295(7) Uani 1 1 d . . . . .
O3 O 0.6610(2) 0.67351(17) 0.54167(18) 0.0252(7) Uani 1 1 d . . . . .
O4 O 0.6098(2) 0.43686(17) 0.67658(17) 0.0209(6) Uani 1 1 d . . . . .
O5 O 0.3805(2) 0.37873(18) 0.64203(16) 0.0216(6) Uani 1 1 d . . . . .
O6 O 0.5556(3) 0.36553(18) 0.39362(18) 0.0293(7) Uani 1 1 d . . . . .
N1 N 0.7378(3) 0.3431(2) 0.5425(2) 0.0185(7) Uani 1 1 d . . . . .
N2 N 0.6783(4) 0.3268(2) 0.2959(2) 0.0350(9) Uani 1 1 d . . . . .
C1 C 0.7371(3) 0.5356(2) 0.5446(2) 0.0187(9) Uani 1 1 d . . . . .
C2 C 0.7603(3) 0.6219(3) 0.5586(2) 0.0210(9) Uani 1 1 d . . . . .
C3 C 0.8725(4) 0.6531(3) 0.5865(3) 0.0299(10) Uani 1 1 d . . . . .
H3 H 0.8842 0.7119 0.5945 0.036 Uiso 1 1 calc R U . . .
C4 C 0.9682(4) 0.5982(3) 0.6028(3) 0.0354(11) Uani 1 1 d . . . . .
H4 H 1.0460 0.6190 0.6217 0.043 Uiso 1 1 calc R U . . .
C5 C 0.9493(4) 0.5138(3) 0.5913(3) 0.0309(10) Uani 1 1 d . . . . .
H5 H 1.0153 0.4765 0.6025 0.037 Uiso 1 1 calc R U . . .
C6 C 0.8354(3) 0.4804(3) 0.5634(3) 0.0219(9) Uani 1 1 d . . . . .
C7 C 0.8316(3) 0.3889(3) 0.5549(2) 0.0228(8) Uani 1 1 d . . . . .
H7 H 0.9064 0.3606 0.5589 0.027 Uiso 1 1 calc R U . . .
C8 C 0.7485(4) 0.2545(3) 0.5291(3) 0.0216(9) Uani 1 1 d . . . . .
C9 C 0.8502(4) 0.2138(3) 0.5081(3) 0.0279(10) Uani 1 1 d . . . . .
H9 H 0.9214 0.2449 0.5043 0.033 Uiso 1 1 calc R U . . .
C10 C 0.8483(4) 0.1282(3) 0.4925(3) 0.0327(11) Uani 1 1 d . . . . .
H10 H 0.9189 0.1003 0.4801 0.039 Uiso 1 1 calc R U . . .
C11 C 0.7439(4) 0.0832(3) 0.4951(3) 0.0301(11) Uani 1 1 d . . . . .
H11 H 0.7425 0.0247 0.4827 0.036 Uiso 1 1 calc R U . . .
C12 C 0.6413(4) 0.1225(3) 0.5154(3) 0.0279(10) Uani 1 1 d . . . . .
H12 H 0.5701 0.0907 0.5168 0.034 Uiso 1 1 calc R U . . .
C13 C 0.6412(4) 0.2091(2) 0.5340(3) 0.0226(9) Uani 1 1 d . . . . .
C14 C 0.6597(5) 0.7471(3) 0.5956(3) 0.0426(13) Uani 1 1 d . . . . .
H14A H 0.7213 0.7867 0.5815 0.064 Uiso 1 1 calc R U . . .
H14B H 0.6759 0.7307 0.6565 0.064 Uiso 1 1 calc R U . . .
H14C H 0.5810 0.7741 0.5854 0.064 Uiso 1 1 calc R U . . .
C15 C 0.3682(3) 0.4100(2) 0.7154(3) 0.0181(9) Uani 1 1 d . . . . .
C16 C 0.2486(3) 0.3951(2) 0.7471(2) 0.0179(8) Uani 1 1 d . . . . .
C17 C 0.1698(4) 0.3399(3) 0.7016(3) 0.0264(10) Uani 1 1 d . . . . .
H17 H 0.1911 0.3143 0.6505 0.032 Uiso 1 1 calc R U . . .
C18 C 0.0599(4) 0.3211(3) 0.7292(3) 0.0313(10) Uani 1 1 d . . . . .
H18 H 0.0076 0.2819 0.6979 0.038 Uiso 1 1 calc R U . . .
C19 C 0.0268(4) 0.3596(3) 0.8024(3) 0.0289(10) Uani 1 1 d . . . . .
H19 H -0.0486 0.3476 0.8212 0.035 Uiso 1 1 calc R U . . .
C20 C 0.1039(4) 0.4155(3) 0.8475(3) 0.0300(10) Uani 1 1 d . . . . .
H20 H 0.0811 0.4424 0.8974 0.036 Uiso 1 1 calc R U . . .
C21 C 0.2142(4) 0.4330(3) 0.8212(3) 0.0267(10) Uani 1 1 d . . . . .
H21 H 0.2670 0.4710 0.8536 0.032 Uiso 1 1 calc R U . . .
C22 C 0.4561(3) 0.4576(2) 0.7644(3) 0.0203(9) Uani 1 1 d . . . . .
H22 H 0.4372 0.4816 0.8169 0.024 Uiso 1 1 calc R U . . .
C23 C 0.5707(3) 0.4718(2) 0.7405(2) 0.0174(8) Uani 1 1 d . . . . .
C24 C 0.6555(4) 0.5296(2) 0.7931(3) 0.0193(9) Uani 1 1 d . . . . .
C25 C 0.6156(4) 0.5941(3) 0.8422(3) 0.0292(10) Uani 1 1 d . . . . .
H25 H 0.5322 0.6015 0.8438 0.035 Uiso 1 1 calc R U . . .
C26 C 0.6962(4) 0.6481(3) 0.8892(3) 0.0354(11) Uani 1 1 d . . . . .
H26 H 0.6679 0.6925 0.9221 0.042 Uiso 1 1 calc R U . . .
C27 C 0.8183(4) 0.6366(3) 0.8876(3) 0.0326(11) Uani 1 1 d . . . . .
H27 H 0.8738 0.6719 0.9212 0.039 Uiso 1 1 calc R U . . .
C28 C 0.8591(4) 0.5735(3) 0.8371(3) 0.0278(10) Uani 1 1 d . . . . .
H28 H 0.9425 0.5665 0.8350 0.033 Uiso 1 1 calc R U . . .
C29 C 0.7784(4) 0.5209(3) 0.7900(3) 0.0224(9) Uani 1 1 d . . . . .
H29 H 0.8068 0.4782 0.7550 0.027 Uiso 1 1 calc R U . . .
C30 C 0.6403(4) 0.3789(3) 0.3543(3) 0.0265(9) Uani 1 1 d . . . . .
H30 H 0.6828 0.4300 0.3659 0.032 Uiso 1 1 calc R U . . .
C31 C 0.6196(5) 0.2469(3) 0.2776(3) 0.0525(16) Uani 1 1 d . . . . .
H31A H 0.5645 0.2514 0.2241 0.079 Uiso 1 1 calc R U . . .
H31B H 0.5748 0.2316 0.3254 0.079 Uiso 1 1 calc R U . . .
H31C H 0.6797 0.2037 0.2707 0.079 Uiso 1 1 calc R U . . .
C32 C 0.7744(5) 0.3507(4) 0.2463(3) 0.0448(13) Uani 1 1 d . . . . .
H32A H 0.7432 0.3551 0.1850 0.067 Uiso 1 1 calc R U . . .
H32B H 0.8376 0.3080 0.2536 0.067 Uiso 1 1 calc R U . . .
H32C H 0.8073 0.4051 0.2668 0.067 Uiso 1 1 calc R 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
Gd1 O2 2.245(3) . ?
Gd1 O4 2.329(3) . ?
Gd1 O5 2.345(3) . ?
Gd1 O1 2.362(3) . ?
Gd1 O1 2.406(3) 3_666 ?
Gd1 O6 2.433(3) . ?
Gd1 O3 2.503(3) 3_666 ?
Gd1 N1 2.542(3) . ?
Gd1 Gd1 3.8151(5) 3_666 ?
O1 C1 1.331(5) . ?
O1 Gd1 2.406(3) 3_666 ?
O2 C13 1.327(5) . ?
O3 C2 1.386(5) . ?
O3 C14 1.442(5) . ?
O3 Gd1 2.503(3) 3_666 ?
O4 C23 1.265(5) . ?
O5 C15 1.270(5) . ?
O6 C30 1.212(5) . ?
N1 C7 1.279(5) . ?
N1 C8 1.432(5) . ?
N2 C30 1.339(5) . ?
N2 C31 1.444(6) . ?
N2 C32 1.455(6) . ?
C1 C2 1.410(6) . ?
C1 C6 1.416(6) . ?
C2 C3 1.379(5) . ?
C3 C4 1.387(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.408(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.461(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.389(6) . ?
C8 C13 1.418(6) . ?
C9 C10 1.383(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.408(6) . ?
C12 H12 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C22 1.398(5) . ?
C15 C16 1.507(5) . ?
C16 C17 1.383(6) . ?
C16 C21 1.397(5) . ?
C17 C18 1.391(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.404(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.496(5) . ?
C24 C25 1.386(6) . ?
C24 C29 1.398(6) . ?
C25 C26 1.392(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.391(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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 O4 102.80(10) . . ?
O2 Gd1 O5 87.95(10) . . ?
O4 Gd1 O5 71.61(9) . . ?
O2 Gd1 O1 141.28(9) . . ?
O4 Gd1 O1 73.89(9) . . ?
O5 Gd1 O1 124.98(9) . . ?
O2 Gd1 O1 139.50(9) . 3_666 ?
O4 Gd1 O1 108.25(9) . 3_666 ?
O5 Gd1 O1 78.07(9) . 3_666 ?
O1 Gd1 O1 73.72(10) . 3_666 ?
O2 Gd1 O6 84.47(11) . . ?
O4 Gd1 O6 143.51(10) . . ?
O5 Gd1 O6 144.86(9) . . ?
O1 Gd1 O6 78.37(9) . . ?
O1 Gd1 O6 85.71(9) 3_666 . ?
O2 Gd1 O3 74.79(10) . 3_666 ?
O4 Gd1 O3 146.88(9) . 3_666 ?
O5 Gd1 O3 75.28(9) . 3_666 ?
O1 Gd1 O3 128.58(9) . 3_666 ?
O1 Gd1 O3 64.95(9) 3_666 3_666 ?
O6 Gd1 O3 69.61(10) . 3_666 ?
O2 Gd1 N1 67.55(10) . . ?
O4 Gd1 N1 77.84(10) . . ?
O5 Gd1 N1 135.16(9) . . ?
O1 Gd1 N1 74.18(10) . . ?
O1 Gd1 N1 143.92(9) 3_666 . ?
O6 Gd1 N1 72.07(10) . . ?
O3 Gd1 N1 127.88(10) 3_666 . ?
O2 Gd1 Gd1 164.28(8) . 3_666 ?
O4 Gd1 Gd1 91.48(7) . 3_666 ?
O5 Gd1 Gd1 102.97(7) . 3_666 ?
O1 Gd1 Gd1 37.26(6) . 3_666 ?
O1 Gd1 Gd1 36.46(6) 3_666 3_666 ?
O6 Gd1 Gd1 80.10(7) . 3_666 ?
O3 Gd1 Gd1 96.84(7) 3_666 3_666 ?
N1 Gd1 Gd1 109.94(7) . 3_666 ?
C1 O1 Gd1 130.0(2) . . ?
C1 O1 Gd1 120.9(2) . 3_666 ?
Gd1 O1 Gd1 106.28(10) . 3_666 ?
C13 O2 Gd1 122.4(2) . . ?
C2 O3 C14 115.7(3) . . ?
C2 O3 Gd1 117.4(2) . 3_666 ?
C14 O3 Gd1 124.0(3) . 3_666 ?
C23 O4 Gd1 134.3(2) . . ?
C15 O5 Gd1 136.3(2) . . ?
C30 O6 Gd1 133.0(3) . . ?
C7 N1 C8 120.0(3) . . ?
C7 N1 Gd1 127.9(3) . . ?
C8 N1 Gd1 112.0(2) . . ?
C30 N2 C31 120.2(4) . . ?
C30 N2 C32 121.2(4) . . ?
C31 N2 C32 118.5(4) . . ?
O1 C1 C2 119.1(3) . . ?
O1 C1 C6 124.4(4) . . ?
C2 C1 C6 116.5(4) . . ?
C3 C2 O3 122.3(4) . . ?
C3 C2 C1 123.1(4) . . ?
O3 C2 C1 114.6(3) . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.3(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 122.1(4) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 119.4(4) . . ?
C5 C6 C7 114.8(4) . . ?
C1 C6 C7 125.8(4) . . ?
N1 C7 C6 126.5(4) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
C9 C8 C13 120.5(4) . . ?
C9 C8 N1 125.5(4) . . ?
C13 C8 N1 114.0(3) . . ?
C10 C9 C8 120.4(4) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C9 120.0(4) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.7(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
O2 C13 C12 122.1(4) . . ?
O2 C13 C8 120.2(4) . . ?
C12 C13 C8 117.8(4) . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O5 C15 C22 123.8(4) . . ?
O5 C15 C16 115.6(3) . . ?
C22 C15 C16 120.5(4) . . ?
C17 C16 C21 118.2(4) . . ?
C17 C16 C15 118.4(4) . . ?
C21 C16 C15 123.4(4) . . ?
C16 C17 C18 121.2(4) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 119.8(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C20 C19 C18 119.4(4) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 120.8(4) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C20 C21 C16 120.5(4) . . ?
C20 C21 H21 119.8 . . ?
C16 C21 H21 119.8 . . ?
C15 C22 C23 123.8(4) . . ?
C15 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
O4 C23 C22 123.8(4) . . ?
O4 C23 C24 116.2(3) . . ?
C22 C23 C24 120.0(3) . . ?
C25 C24 C29 118.7(4) . . ?
C25 C24 C23 121.9(4) . . ?
C29 C24 C23 119.3(4) . . ?
C24 C25 C26 120.9(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C27 C26 C25 119.5(4) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 120.1(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C29 C28 C27 119.9(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C24 120.9(4) . . ?
C28 C29 H29 119.5 . . ?
C24 C29 H29 119.5 . . ?
O6 C30 N2 124.7(4) . . ?
O6 C30 H30 117.6 . . ?
N2 C30 H30 117.6 . . ?
N2 C31 H31A 109.5 . . ?
N2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N2 C32 H32A 109.5 . . ?
N2 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N2 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_refine_diff_density_max         0.619
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_Tb_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1574221'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H76 N2 O18 Tb2'
_chemical_formula_weight         1503.12

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'
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'
Tb Tb -0.1723 4.1537 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8918(2)
_cell_length_b                   12.2785(2)
_cell_length_c                   13.6668(3)
_cell_angle_alpha                65.133(2)
_cell_angle_beta                 78.645(2)
_cell_angle_gamma                75.204(2)
_cell_volume                     1594.92(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    17318
_cell_measurement_theta_min      2.9242
_cell_measurement_theta_max      33.1504

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    2.272
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.788
_exptl_absorpt_correction_T_min  0.80545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15235
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.934
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5605
_reflns_number_gt                5227
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0283P)²+0.0391P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5605
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0177
_refine_ls_wR_factor_ref         0.0443
_refine_ls_wR_factor_gt          0.0439
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.003
_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_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
Tb1 Tb 0.63060(2) 0.06945(2) 0.39227(2) 0.01398(4) Uani 1 1 d . . . . .
O1 O 0.80618(13) 0.14200(13) 0.29404(11) 0.0220(3) Uani 1 1 d . . . . .
O2 O 0.43769(12) 0.11707(12) 0.48842(10) 0.0149(3) Uani 1 1 d . . . . .
O3 O 0.19505(12) 0.11450(13) 0.54549(11) 0.0187(3) Uani 1 1 d . . . . .
O4 O 0.51121(13) 0.20621(13) 0.25285(11) 0.0192(3) Uani 1 1 d . . . . .
O5 O 0.65528(14) -0.01933(13) 0.26980(11) 0.0200(3) Uani 1 1 d . . . . .
O6 O 0.70958(14) 0.05301(13) 0.55640(11) 0.0216(3) Uani 1 1 d . . . . .
H6S H 0.6926 0.1194 0.5648 0.026 Uiso 1 1 calc R U . . .
N1 N 0.63060(15) 0.27361(15) 0.38917(13) 0.0169(4) Uani 1 1 d . . . . .
C1 C 0.8398(2) 0.2346(2) 0.30168(17) 0.0221(5) Uani 1 1 d . . . . .
C2 C 0.9596(2) 0.2663(2) 0.25868(18) 0.0283(5) Uani 1 1 d . . . . .
H2 H 1.0179 0.2232 0.2195 0.034 Uiso 1 1 calc R U . . .
C3 C 0.9939(2) 0.3588(2) 0.2724(2) 0.0344(6) Uani 1 1 d . . . . .
H3 H 1.0759 0.3783 0.2433 0.041 Uiso 1 1 calc R U . . .
C4 C 0.9104(2) 0.4242(2) 0.3282(2) 0.0333(6) Uani 1 1 d . . . . .
H4 H 0.9355 0.4868 0.3387 0.040 Uiso 1 1 calc R U . . .
C5 C 0.7902(2) 0.3974(2) 0.36845(18) 0.0261(5) Uani 1 1 d . . . . .
H5 H 0.7325 0.4418 0.4068 0.031 Uiso 1 1 calc R U . . .
C6 C 0.7533(2) 0.30611(19) 0.35312(17) 0.0201(5) Uani 1 1 d . . . . .
C7 C 0.5338(2) 0.35328(19) 0.40262(16) 0.0202(5) Uani 1 1 d . . . . .
H7 H 0.5495 0.4319 0.3868 0.024 Uiso 1 1 calc R U . . .
C8 C 0.40291(19) 0.33636(19) 0.43934(16) 0.0191(4) Uani 1 1 d . . . . .
C9 C 0.36146(19) 0.22432(18) 0.47825(15) 0.0157(4) Uani 1 1 d . . . . .
C10 C 0.22928(19) 0.22670(19) 0.50940(16) 0.0176(4) Uani 1 1 d . . . . .
C11 C 0.1433(2) 0.3325(2) 0.50333(19) 0.0270(5) Uani 1 1 d . . . . .
H11 H 0.0552 0.3306 0.5254 0.032 Uiso 1 1 calc R U . . .
C12 C 0.1856(2) 0.4419(2) 0.4649(2) 0.0318(6) Uani 1 1 d . . . . .
H12 H 0.1268 0.5156 0.4599 0.038 Uiso 1 1 calc R U . . .
C13 C 0.3130(2) 0.4430(2) 0.43433(19) 0.0274(5) Uani 1 1 d . . . . .
H13 H 0.3415 0.5182 0.4090 0.033 Uiso 1 1 calc R U . . .
C14 C 0.06247(19) 0.1135(2) 0.54868(19) 0.0273(5) Uani 1 1 d . . . . .
H14A H 0.0129 0.1390 0.6061 0.041 Uiso 1 1 calc R U . . .
H14B H 0.0529 0.0306 0.5634 0.041 Uiso 1 1 calc R U . . .
H14C H 0.0314 0.1700 0.4787 0.041 Uiso 1 1 calc R U . . .
C15 C 0.69043(19) -0.0719(2) 0.11801(17) 0.0190(5) Uani 1 1 d . . . . .
C16 C 0.7527(2) -0.1879(2) 0.17928(19) 0.0313(6) Uani 1 1 d . . . . .
H16 H 0.7639 -0.2078 0.2525 0.038 Uiso 1 1 calc R U . . .
C17 C 0.7990(3) -0.2755(2) 0.1346(2) 0.0367(6) Uani 1 1 d . . . . .
H17 H 0.8408 -0.3549 0.1778 0.044 Uiso 1 1 calc R U . . .
C18 C 0.7846(2) -0.2481(2) 0.0289(2) 0.0313(6) Uani 1 1 d . . . . .
H18 H 0.8160 -0.3082 -0.0013 0.038 Uiso 1 1 calc R U . . .
C19 C 0.7247(2) -0.1334(2) -0.0326(2) 0.0339(6) Uani 1 1 d . . . . .
H19 H 0.7153 -0.1136 -0.1062 0.041 Uiso 1 1 calc R U . . .
C20 C 0.6776(2) -0.0456(2) 0.01105(19) 0.0282(5) Uani 1 1 d . . . . .
H20 H 0.6359 0.0336 -0.0328 0.034 Uiso 1 1 calc R U . . .
C21 C 0.63780(19) 0.01828(19) 0.17066(16) 0.0182(4) Uani 1 1 d . . . . .
C22 C 0.5714(2) 0.1343(2) 0.11195(17) 0.0216(5) Uani 1 1 d . . . . .
H22 H 0.5677 0.1561 0.0370 0.026 Uiso 1 1 calc R U . . .
C23 C 0.50948(19) 0.22136(19) 0.15588(17) 0.0183(4) Uani 1 1 d . . . . .
C24 C 0.4294(2) 0.33753(19) 0.08625(17) 0.0203(5) Uani 1 1 d . . . . .
C25 C 0.4501(2) 0.3857(2) -0.02601(18) 0.0252(5) Uani 1 1 d . . . . .
H25 H 0.5173 0.3445 -0.0614 0.030 Uiso 1 1 calc R U . . .
C26 C 0.3739(2) 0.4933(2) -0.08701(19) 0.0319(6) Uani 1 1 d . . . . .
H26 H 0.3899 0.5261 -0.1638 0.038 Uiso 1 1 calc R U . . .
C27 C 0.2750(2) 0.5527(2) -0.0368(2) 0.0345(6) Uani 1 1 d . . . . .
H27 H 0.2219 0.6258 -0.0789 0.041 Uiso 1 1 calc R U . . .
C28 C 0.2532(2) 0.5058(2) 0.0748(2) 0.0310(6) Uani 1 1 d . . . . .
H28 H 0.1847 0.5466 0.1094 0.037 Uiso 1 1 calc R U . . .
C29 C 0.3307(2) 0.3994(2) 0.13675(19) 0.0254(5) Uani 1 1 d . . . . .
H29 H 0.3164 0.3687 0.2136 0.030 Uiso 1 1 calc R U . . .
C30 C 0.7312(2) -0.0466(2) 0.65842(18) 0.0280(5) Uani 1 1 d . . . . .
H30A H 0.6558 -0.0427 0.7103 0.042 Uiso 1 1 calc R U . . .
H30B H 0.8053 -0.0413 0.6857 0.042 Uiso 1 1 calc R U . . .
H30C H 0.7474 -0.1242 0.6491 0.042 Uiso 1 1 calc R U . . .
O1S O 0.97919(17) 0.03118(17) 0.17923(15) 0.0430(5) Uani 1 1 d . . . . .
H1S H 0.9271 0.0576 0.2221 0.052 Uiso 1 1 calc R U . . .
C1S C 0.9505(3) 0.1051(3) 0.0718(2) 0.0397(7) Uani 1 1 d . . . . .
H1S1 H 0.9372 0.1915 0.0601 0.060 Uiso 1 1 calc R U . . .
H1S2 H 0.8728 0.0883 0.0596 0.060 Uiso 1 1 calc R U . . .
H1S3 H 1.0216 0.0868 0.0212 0.060 Uiso 1 1 calc R U . . .
O2S O 0.66591(15) 0.23566(15) 0.63059(13) 0.0305(4) Uani 1 1 d . . . . .
H2S H 0.7280 0.2145 0.6670 0.037 Uiso 1 1 calc R U . . .
C2S C 0.5507(3) 0.2300(3) 0.7007(2) 0.0417(7) Uani 1 1 d . . . . .
H2S1 H 0.5633 0.1566 0.7676 0.063 Uiso 1 1 calc R U . . .
H2S2 H 0.4831 0.2266 0.6647 0.063 Uiso 1 1 calc R U . . .
H2S3 H 0.5262 0.3029 0.7181 0.063 Uiso 1 1 calc R U . . .
O3S O 0.1516(2) 0.8245(2) 0.24122(18) 0.0618(6) Uani 1 1 d . . . . .
H3S H 0.0967 0.8890 0.2185 0.074 Uiso 1 1 calc R U . . .
C3S C 0.1410(4) 0.7456(3) 0.1975(3) 0.0739(11) Uani 1 1 d . . . . .
H3SC H 0.1900 0.6641 0.2364 0.089 Uiso 1 1 calc R U . . .
H3SA H 0.1743 0.7752 0.1208 0.089 Uiso 1 1 calc R U . . .
H3SB H 0.0510 0.7411 0.2041 0.089 Uiso 1 1 calc R 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
Tb1 O1 2.2597(14) . ?
Tb1 O5 2.2955(14) . ?
Tb1 O4 2.3045(13) . ?
Tb1 O2 2.3270(13) . ?
Tb1 O2 2.3894(13) 2_656 ?
Tb1 O6 2.4705(13) . ?
Tb1 N1 2.4893(17) . ?
Tb1 O3 2.5022(13) 2_656 ?
Tb1 Tb1 3.8249(2) 2_656 ?
O1 C1 1.328(3) . ?
O2 C9 1.333(2) . ?
O2 Tb1 2.3894(13) 2_656 ?
O3 C10 1.378(3) . ?
O3 C14 1.439(2) . ?
O3 Tb1 2.5021(13) 2_656 ?
O4 C23 1.262(2) . ?
O5 C21 1.271(2) . ?
O6 C30 1.430(3) . ?
O6 H6S 0.8400 . ?
N1 C7 1.285(3) . ?
N1 C6 1.427(3) . ?
C1 C2 1.401(3) . ?
C1 C6 1.410(3) . ?
C2 C3 1.375(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.452(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.405(3) . ?
C8 C9 1.409(3) . ?
C9 C10 1.415(3) . ?
C10 C11 1.375(3) . ?
C11 C12 1.386(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.370(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.384(3) . ?
C15 C20 1.386(3) . ?
C15 C21 1.502(3) . ?
C16 C17 1.392(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.366(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.386(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.392(3) . ?
C22 C23 1.403(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.500(3) . ?
C24 C25 1.387(3) . ?
C24 C29 1.393(3) . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.379(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(3) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O1S C1S 1.411(3) . ?
O1S H1S 0.8400 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.418(3) . ?
O2S H2S 0.8400 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
O3S C3S 1.371(4) . ?
O3S H3S 0.8400 . ?
C3S H3SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 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
O1 Tb1 O5 83.29(5) . . ?
O1 Tb1 O4 89.39(5) . . ?
O5 Tb1 O4 73.46(5) . . ?
O1 Tb1 O2 143.77(5) . . ?
O5 Tb1 O2 124.54(5) . . ?
O4 Tb1 O2 78.97(5) . . ?
O1 Tb1 O2 141.50(5) . 2_656 ?
O5 Tb1 O2 81.47(5) . 2_656 ?
O4 Tb1 O2 119.31(5) . 2_656 ?
O2 Tb1 O2 71.62(5) . 2_656 ?
O1 Tb1 O6 88.74(5) . . ?
O5 Tb1 O6 144.34(5) . . ?
O4 Tb1 O6 141.36(5) . . ?
O2 Tb1 O6 80.05(5) . . ?
O2 Tb1 O6 83.54(5) 2_656 . ?
O1 Tb1 N1 68.44(5) . . ?
O5 Tb1 N1 137.86(5) . . ?
O4 Tb1 N1 75.56(5) . . ?
O2 Tb1 N1 75.43(5) . . ?
O2 Tb1 N1 139.46(5) 2_656 . ?
O6 Tb1 N1 67.93(5) . . ?
O1 Tb1 O3 77.56(5) . 2_656 ?
O5 Tb1 O3 75.03(5) . 2_656 ?
O4 Tb1 O3 147.05(5) . 2_656 ?
O2 Tb1 O3 128.15(5) . 2_656 ?
O2 Tb1 O3 64.40(4) 2_656 2_656 ?
O6 Tb1 O3 69.31(5) . 2_656 ?
N1 Tb1 O3 124.87(5) . 2_656 ?
O1 Tb1 Tb1 168.40(4) . 2_656 ?
O5 Tb1 Tb1 104.61(4) . 2_656 ?
O4 Tb1 Tb1 100.92(3) . 2_656 ?
O2 Tb1 Tb1 36.36(3) . 2_656 ?
O2 Tb1 Tb1 35.27(3) 2_656 2_656 ?
O6 Tb1 Tb1 79.89(3) . 2_656 ?
N1 Tb1 Tb1 108.76(4) . 2_656 ?
O3 Tb1 Tb1 96.08(3) 2_656 2_656 ?
C1 O1 Tb1 121.12(12) . . ?
C9 O2 Tb1 131.07(12) . . ?
C9 O2 Tb1 120.14(11) . 2_656 ?
Tb1 O2 Tb1 108.38(5) . 2_656 ?
C10 O3 C14 117.49(16) . . ?
C10 O3 Tb1 116.36(11) . 2_656 ?
C14 O3 Tb1 126.08(12) . 2_656 ?
C23 O4 Tb1 134.93(13) . . ?
C21 O5 Tb1 135.61(13) . . ?
C30 O6 Tb1 132.02(13) . . ?
C30 O6 H6S 109.5 . . ?
Tb1 O6 H6S 113.3 . . ?
C7 N1 C6 119.55(18) . . ?
C7 N1 Tb1 127.67(14) . . ?
C6 N1 Tb1 112.15(12) . . ?
O1 C1 C2 122.3(2) . . ?
O1 C1 C6 120.15(18) . . ?
C2 C1 C6 117.5(2) . . ?
C3 C2 C1 120.9(2) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 120.9(2) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.4(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.7(2) . . ?
C5 C6 N1 124.6(2) . . ?
C1 C6 N1 114.65(18) . . ?
N1 C7 C8 127.1(2) . . ?
N1 C7 H7 116.4 . . ?
C8 C7 H7 116.4 . . ?
C13 C8 C9 119.22(19) . . ?
C13 C8 C7 115.22(19) . . ?
C9 C8 C7 125.56(18) . . ?
O2 C9 C8 124.75(18) . . ?
O2 C9 C10 118.09(18) . . ?
C8 C9 C10 117.16(18) . . ?
C11 C10 O3 123.41(19) . . ?
C11 C10 C9 122.4(2) . . ?
O3 C10 C9 114.18(17) . . ?
C10 C11 C12 119.7(2) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.5(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C8 122.0(2) . . ?
C12 C13 H13 119.0 . . ?
C8 C13 H13 119.0 . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 118.0(2) . . ?
C16 C15 C21 118.81(19) . . ?
C20 C15 C21 123.2(2) . . ?
C15 C16 C17 120.6(2) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 120.6(2) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C19 C18 C17 119.2(2) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 120.7(2) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C15 120.8(2) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
O5 C21 C22 123.78(19) . . ?
O5 C21 C15 116.14(18) . . ?
C22 C21 C15 120.06(18) . . ?
C21 C22 C23 124.48(19) . . ?
C21 C22 H22 117.8 . . ?
C23 C22 H22 117.8 . . ?
O4 C23 C22 124.24(19) . . ?
O4 C23 C24 116.89(19) . . ?
C22 C23 C24 118.77(18) . . ?
C25 C24 C29 118.9(2) . . ?
C25 C24 C23 122.6(2) . . ?
C29 C24 C23 118.48(19) . . ?
C26 C25 C24 120.6(2) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C27 C26 C25 120.2(2) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 119.8(2) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C29 120.5(2) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C24 120.0(2) . . ?
C28 C29 H29 120.0 . . ?
C24 C29 H29 120.0 . . ?
O6 C30 H30A 109.5 . . ?
O6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C3S O3S H3S 109.5 . . ?
O3S C3S H3SC 109.5 . . ?
O3S C3S H3SA 109.5 . . ?
H3SC C3S H3SA 109.5 . . ?
O3S C3S H3SB 109.5 . . ?
H3SC C3S H3SB 109.5 . . ?
H3SA C3S H3SB 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
Tb1 O1 C1 C2 167.47(15) . . . . ?
Tb1 O1 C1 C6 -13.4(2) . . . . ?
O1 C1 C2 C3 -176.9(2) . . . . ?
C6 C1 C2 C3 4.0(3) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 C1 3.5(3) . . . . ?
C4 C5 C6 N1 -178.4(2) . . . . ?
O1 C1 C6 C5 175.42(19) . . . . ?
C2 C1 C6 C5 -5.4(3) . . . . ?
O1 C1 C6 N1 -2.8(3) . . . . ?
C2 C1 C6 N1 176.36(18) . . . . ?
C7 N1 C6 C5 25.3(3) . . . . ?
Tb1 N1 C6 C5 -163.05(17) . . . . ?
C7 N1 C6 C1 -156.55(19) . . . . ?
Tb1 N1 C6 C1 15.1(2) . . . . ?
C6 N1 C7 C8 -179.49(19) . . . . ?
Tb1 N1 C7 C8 10.3(3) . . . . ?
N1 C7 C8 C13 -172.6(2) . . . . ?
N1 C7 C8 C9 7.4(3) . . . . ?
Tb1 O2 C9 C8 -29.1(3) . . . . ?
Tb1 O2 C9 C8 159.19(15) 2_656 . . . ?
Tb1 O2 C9 C10 151.48(14) . . . . ?
Tb1 O2 C9 C10 -20.3(2) 2_656 . . . ?
C13 C8 C9 O2 -178.87(19) . . . . ?
C7 C8 C9 O2 1.1(3) . . . . ?
C13 C8 C9 C10 0.6(3) . . . . ?
C7 C8 C9 C10 -179.42(19) . . . . ?
C14 O3 C10 C11 17.3(3) . . . . ?
Tb1 O3 C10 C11 -159.91(17) 2_656 . . . ?
C14 O3 C10 C9 -162.38(17) . . . . ?
Tb1 O3 C10 C9 20.4(2) 2_656 . . . ?
O2 C9 C10 C11 179.10(19) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
O2 C9 C10 O3 -1.2(3) . . . . ?
C8 C9 C10 O3 179.31(17) . . . . ?
O3 C10 C11 C12 -179.3(2) . . . . ?
C9 C10 C11 C12 0.4(3) . . . . ?
C10 C11 C12 C13 -0.6(4) . . . . ?
C11 C12 C13 C8 0.8(4) . . . . ?
C9 C8 C13 C12 -0.8(3) . . . . ?
C7 C8 C13 C12 179.2(2) . . . . ?
C20 C15 C16 C17 -1.0(4) . . . . ?
C21 C15 C16 C17 177.8(2) . . . . ?
C15 C16 C17 C18 0.6(4) . . . . ?
C16 C17 C18 C19 0.3(4) . . . . ?
C17 C18 C19 C20 -0.7(4) . . . . ?
C18 C19 C20 C15 0.3(4) . . . . ?
C16 C15 C20 C19 0.6(4) . . . . ?
C21 C15 C20 C19 -178.1(2) . . . . ?
Tb1 O5 C21 C22 -12.5(3) . . . . ?
Tb1 O5 C21 C15 169.15(13) . . . . ?
C16 C15 C21 O5 0.3(3) . . . . ?
C20 C15 C21 O5 179.0(2) . . . . ?
C16 C15 C21 C22 -178.1(2) . . . . ?
C20 C15 C21 C22 0.6(3) . . . . ?
O5 C21 C22 C23 -3.8(3) . . . . ?
C15 C21 C22 C23 174.42(19) . . . . ?
Tb1 O4 C23 C22 14.1(3) . . . . ?
Tb1 O4 C23 C24 -169.52(13) . . . . ?
C21 C22 C23 O4 3.0(3) . . . . ?
C21 C22 C23 C24 -173.32(19) . . . . ?
O4 C23 C24 C25 157.8(2) . . . . ?
C22 C23 C24 C25 -25.6(3) . . . . ?
O4 C23 C24 C29 -21.9(3) . . . . ?
C22 C23 C24 C29 154.7(2) . . . . ?
C29 C24 C25 C26 -0.2(3) . . . . ?
C23 C24 C25 C26 -179.9(2) . . . . ?
C24 C25 C26 C27 -1.0(4) . . . . ?
C25 C26 C27 C28 1.0(4) . . . . ?
C26 C27 C28 C29 0.3(4) . . . . ?
C27 C28 C29 C24 -1.5(4) . . . . ?
C25 C24 C29 C28 1.5(3) . . . . ?
C23 C24 C29 C28 -178.8(2) . . . . ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.073

####################################################################### 
# 
# 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_Tb_DMF
_database_code_depnum_ccdc_archive 'CCDC 1574220'
_audit_update_record             
;
2017-10-30 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H58 N4 O12 Tb2'
_chemical_formula_weight         1392.98

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   11.2720(3)
_cell_length_b                   15.8900(3)
_cell_length_c                   15.5373(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.596(2)
_cell_angle_gamma                90
_cell_volume                     2764.50(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    13167
_cell_measurement_theta_min      2.9329
_cell_measurement_theta_max      33.1937

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.607
_shelx_estimated_absorpt_T_min   0.529
_shelx_estimated_absorpt_T_max   0.624
_exptl_absorpt_correction_T_min  0.74282
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17456
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.144
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4868
_reflns_number_gt                3894
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+3.3368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4868
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0671
_refine_ls_wR_factor_gt          0.0627
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C18 C 0.0269(4) 0.6408(3) 0.8012(3) 0.0363(10) Uani 1 1 d . . . . .
H18 H -0.0485 0.6532 0.8200 0.044 Uiso 1 1 calc R U . . .
C25 C 0.6963(4) 0.3516(3) 0.8876(3) 0.0424(11) Uani 1 1 d . . . . .
H25 H 0.6683 0.3066 0.9199 0.051 Uiso 1 1 calc R U . . .
C26 C 0.8171(4) 0.3641(3) 0.8872(3) 0.0399(11) Uani 1 1 d . . . . .
H26 H 0.8723 0.3290 0.9212 0.048 Uiso 1 1 calc R U . . .
C32 C 0.3423(4) 0.7481(3) 0.4043(3) 0.0479(13) Uani 1 1 d . . . . .
H32A H 0.3265 0.7318 0.3433 0.072 Uiso 1 1 calc R U . . .
H32B H 0.4205 0.7756 0.4145 0.072 Uiso 1 1 calc R U . . .
H32C H 0.2803 0.7872 0.4187 0.072 Uiso 1 1 calc R U . . .
C1 C 0.7358(3) 0.4640(2) 0.5442(2) 0.0237(8) Uani 1 1 d . . . . .
C2 C 0.2424(4) 0.6228(2) 0.4417(2) 0.0266(9) Uani 1 1 d . . . . .
C3 C 0.1311(4) 0.6547(3) 0.4139(3) 0.0373(10) Uani 1 1 d . . . . .
H3 H 0.1200 0.7135 0.4060 0.045 Uiso 1 1 calc R U . . .
C4 C 0.0348(4) 0.5999(3) 0.3976(3) 0.0425(11) Uani 1 1 d . . . . .
H4 H -0.0428 0.6210 0.3790 0.051 Uiso 1 1 calc R U . . .
C5 C 0.0531(4) 0.5156(3) 0.4086(3) 0.0385(10) Uani 1 1 d . . . . .
H5 H -0.0129 0.4784 0.3967 0.046 Uiso 1 1 calc R U . . .
C6 C 0.8339(3) 0.5185(3) 0.5631(2) 0.0276(9) Uani 1 1 d . . . . .
C7 C 0.8299(4) 0.6095(3) 0.5546(3) 0.0301(9) Uani 1 1 d . . . . .
H7 H 0.9048 0.6376 0.5585 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7475(4) 0.7449(2) 0.5288(2) 0.0263(9) Uani 1 1 d . . . . .
C9 C 0.8495(4) 0.7861(3) 0.5084(3) 0.0350(10) Uani 1 1 d . . . . .
H9 H 0.9209 0.7550 0.5052 0.042 Uiso 1 1 calc R U . . .
C10 C 0.8481(4) 0.8719(3) 0.4929(3) 0.0393(11) Uani 1 1 d . . . . .
H10 H 0.9187 0.8998 0.4805 0.047 Uiso 1 1 calc R U . . .
C11 C 0.7429(4) 0.9170(3) 0.4956(3) 0.0351(10) Uani 1 1 d . . . . .
H11 H 0.7412 0.9756 0.4834 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6412(4) 0.8774(2) 0.5158(3) 0.0341(10) Uani 1 1 d . . . . .
H12 H 0.5700 0.9091 0.5170 0.041 Uiso 1 1 calc R U . . .
C13 C 0.6403(4) 0.7910(2) 0.5346(3) 0.0291(9) Uani 1 1 d . . . . .
C14 C 0.3691(3) 0.5899(2) 0.7148(2) 0.0242(8) Uani 1 1 d . . . . .
C15 C 0.2493(3) 0.6052(2) 0.7461(2) 0.0242(8) Uani 1 1 d . . . . .
C16 C 0.1702(4) 0.6596(3) 0.7000(3) 0.0314(9) Uani 1 1 d . . . . .
H16 H 0.1913 0.6847 0.6483 0.038 Uiso 1 1 calc R U . . .
C17 C 0.0600(4) 0.6782(3) 0.7278(3) 0.0363(10) Uani 1 1 d . . . . .
H17 H 0.0077 0.7169 0.6961 0.044 Uiso 1 1 calc R U . . .
C19 C 0.1041(4) 0.5851(3) 0.8475(3) 0.0383(11) Uani 1 1 d . . . . .
H19 H 0.0811 0.5585 0.8978 0.046 Uiso 1 1 calc R U . . .
C20 C 0.2151(4) 0.5678(3) 0.8208(3) 0.0320(10) Uani 1 1 d . . . . .
H20 H 0.2682 0.5303 0.8536 0.038 Uiso 1 1 calc R U . . .
C21 C 0.4555(3) 0.5423(2) 0.7638(2) 0.0261(9) Uani 1 1 d . . . . .
H21 H 0.4358 0.5175 0.8159 0.031 Uiso 1 1 calc R U . . .
C22 C 0.5709(3) 0.5289(2) 0.7400(2) 0.0232(8) Uani 1 1 d . . . . .
C23 C 0.6557(3) 0.4711(2) 0.7925(2) 0.0245(8) Uani 1 1 d . . . . .
C24 C 0.6158(4) 0.4048(3) 0.8408(3) 0.0360(10) Uani 1 1 d . . . . .
H24 H 0.5325 0.3962 0.8415 0.043 Uiso 1 1 calc R U . . .
C27 C 0.8586(4) 0.4276(3) 0.8373(3) 0.0332(10) Uani 1 1 d . . . . .
H27 H 0.9420 0.4351 0.8359 0.040 Uiso 1 1 calc R U . . .
C28 C 0.7779(3) 0.4801(2) 0.7894(3) 0.0287(9) Uani 1 1 d . . . . .
H28 H 0.8063 0.5228 0.7542 0.034 Uiso 1 1 calc R U . . .
C29 C 0.6425(4) 0.6200(3) 0.3546(3) 0.0338(10) Uani 1 1 d . . . . .
H29 H 0.6846 0.5687 0.3662 0.041 Uiso 1 1 calc R U . . .
C30 C 0.6239(5) 0.7518(3) 0.2779(3) 0.0566(15) Uani 1 1 d . . . . .
H30A H 0.5678 0.7474 0.2250 0.085 Uiso 1 1 calc R U . . .
H30B H 0.6849 0.7940 0.2696 0.085 Uiso 1 1 calc R U . . .
H30C H 0.5806 0.7686 0.3264 0.085 Uiso 1 1 calc R U . . .
C31 C 0.7767(5) 0.6481(4) 0.2464(3) 0.0518(13) Uani 1 1 d . . . . .
H31A H 0.8034 0.5909 0.2623 0.078 Uiso 1 1 calc R U . . .
H31B H 0.8436 0.6873 0.2588 0.078 Uiso 1 1 calc R U . . .
H31C H 0.7481 0.6500 0.1844 0.078 Uiso 1 1 calc R U . . .
N1 N 0.7367(3) 0.6566(2) 0.54233(19) 0.0240(7) Uani 1 1 d . . . . .
N2 N 0.6798(4) 0.6721(2) 0.2965(2) 0.0404(9) Uani 1 1 d . . . . .
O1 O 0.6258(2) 0.48846(15) 0.51402(16) 0.0225(6) Uani 1 1 d . . . . .
O2 O 0.5451(2) 0.75125(17) 0.5560(2) 0.0360(7) Uani 1 1 d . . . . .
O3 O 0.3815(2) 0.62151(16) 0.64108(17) 0.0270(6) Uani 1 1 d . . . . .
O4 O 0.6102(2) 0.56362(16) 0.67567(16) 0.0263(6) Uani 1 1 d . . . . .
O5 O 0.3418(2) 0.67424(17) 0.45802(18) 0.0313(6) Uani 1 1 d . . . . .
O6 O 0.5569(3) 0.63434(18) 0.39406(18) 0.0353(7) Uani 1 1 d . . . . .
Tb1 Tb 0.52199(2) 0.61182(2) 0.54268(2) 0.02144(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C18 C17 1.375(6) . ?
C18 C19 1.384(6) . ?
C18 H18 0.9500 . ?
C25 C26 1.376(6) . ?
C25 C24 1.383(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(6) . ?
C26 H26 0.9500 . ?
C32 O5 1.440(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C1 O1 1.332(4) . ?
C1 C6 1.409(5) . ?
C1 C2 1.413(5) 3_666 ?
C2 C3 1.375(6) . ?
C2 O5 1.387(5) . ?
C2 C1 1.413(5) 3_666 ?
C3 C4 1.391(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.407(6) 3_666 ?
C5 H5 0.9500 . ?
C6 C5 1.407(6) 3_666 ?
C6 C7 1.453(6) . ?
C7 N1 1.285(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(6) . ?
C8 C13 1.424(6) . ?
C8 N1 1.426(5) . ?
C9 C10 1.384(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.391(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.403(6) . ?
C12 H12 0.9500 . ?
C13 O2 1.321(5) . ?
C14 O3 1.273(5) . ?
C14 C21 1.390(5) . ?
C14 C15 1.508(5) . ?
C15 C16 1.382(6) . ?
C15 C20 1.397(5) . ?
C16 C17 1.393(6) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C19 C20 1.391(6) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.408(5) . ?
C21 H21 0.9500 . ?
C22 O4 1.265(4) . ?
C22 C23 1.498(5) . ?
C23 C28 1.391(5) . ?
C23 C24 1.397(6) . ?
C24 H24 0.9500 . ?
C27 C28 1.386(6) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 O6 1.222(5) . ?
C29 N2 1.329(5) . ?
C29 H29 0.9500 . ?
C30 N2 1.430(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 N2 1.463(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
N1 Tb1 2.523(3) . ?
O1 Tb1 2.351(2) . ?
O1 Tb1 2.398(2) 3_666 ?
O2 Tb1 2.238(3) . ?
O3 Tb1 2.329(2) . ?
O4 Tb1 2.318(3) . ?
O5 Tb1 2.495(3) . ?
O6 Tb1 2.413(3) . ?
Tb1 O1 2.398(2) 3_666 ?
Tb1 Tb1 3.8054(3) 3_666 ?

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
C17 C18 C19 119.6(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C26 C25 C24 120.0(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 120.3(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
O5 C32 H32A 109.5 . . ?
O5 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O5 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O1 C1 C6 124.8(3) . . ?
O1 C1 C2 118.6(3) . 3_666 ?
C6 C1 C2 116.7(3) . 3_666 ?
C3 C2 O5 122.0(4) . . ?
C3 C2 C1 123.0(4) . 3_666 ?
O5 C2 C1 115.1(3) . 3_666 ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 122.4(4) . 3_666 ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 3_666 . ?
C5 C6 C1 119.3(4) 3_666 . ?
C5 C6 C7 115.4(4) 3_666 . ?
C1 C6 C7 125.3(3) . . ?
N1 C7 C6 127.5(4) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
C9 C8 C13 120.1(4) . . ?
C9 C8 N1 125.7(4) . . ?
C13 C8 N1 114.2(3) . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 120.4(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 121.4(4) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
O2 C13 C12 123.0(4) . . ?
O2 C13 C8 119.3(3) . . ?
C12 C13 C8 117.6(4) . . ?
O3 C14 C21 124.4(3) . . ?
O3 C14 C15 115.0(3) . . ?
C21 C14 C15 120.5(3) . . ?
C16 C15 C20 118.3(4) . . ?
C16 C15 C14 118.8(3) . . ?
C20 C15 C14 122.9(4) . . ?
C15 C16 C17 121.1(4) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C18 C17 C16 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C18 C19 C20 120.3(4) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C19 C20 C15 120.5(4) . . ?
C19 C20 H20 119.8 . . ?
C15 C20 H20 119.8 . . ?
C14 C21 C22 123.3(4) . . ?
C14 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
O4 C22 C21 124.0(4) . . ?
O4 C22 C23 116.0(3) . . ?
C21 C22 C23 120.0(3) . . ?
C28 C23 C24 118.5(4) . . ?
C28 C23 C22 119.3(3) . . ?
C24 C23 C22 122.0(4) . . ?
C25 C24 C23 120.7(4) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C27 C28 119.7(4) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C23 120.7(4) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
O6 C29 N2 123.6(4) . . ?
O6 C29 H29 118.2 . . ?
N2 C29 H29 118.2 . . ?
N2 C30 H30A 109.5 . . ?
N2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 C31 H31A 109.5 . . ?
N2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C7 N1 C8 120.8(3) . . ?
C7 N1 Tb1 127.1(3) . . ?
C8 N1 Tb1 112.1(2) . . ?
C29 N2 C30 121.5(4) . . ?
C29 N2 C31 120.9(4) . . ?
C30 N2 C31 117.5(4) . . ?
C1 O1 Tb1 129.8(2) . . ?
C1 O1 Tb1 120.9(2) . 3_666 ?
Tb1 O1 Tb1 106.48(9) . 3_666 ?
C13 O2 Tb1 122.7(2) . . ?
C14 O3 Tb1 135.9(2) . . ?
C22 O4 Tb1 134.0(2) . . ?
C2 O5 C32 115.5(3) . . ?
C2 O5 Tb1 117.0(2) . . ?
C32 O5 Tb1 124.9(3) . . ?
C29 O6 Tb1 132.6(3) . . ?
O2 Tb1 O4 102.20(10) . . ?
O2 Tb1 O3 87.39(10) . . ?
O4 Tb1 O3 72.00(9) . . ?
O2 Tb1 O1 141.99(9) . . ?
O4 Tb1 O1 73.84(9) . . ?
O3 Tb1 O1 124.75(9) . . ?
O2 Tb1 O1 139.48(9) . 3_666 ?
O4 Tb1 O1 108.46(9) . 3_666 ?
O3 Tb1 O1 77.83(9) . 3_666 ?
O1 Tb1 O1 73.52(9) . 3_666 ?
O2 Tb1 O6 84.93(11) . . ?
O4 Tb1 O6 143.27(9) . . ?
O3 Tb1 O6 144.72(10) . . ?
O1 Tb1 O6 78.64(9) . . ?
O1 Tb1 O6 85.98(9) 3_666 . ?
O2 Tb1 O5 74.57(10) . . ?
O4 Tb1 O5 147.26(9) . . ?
O3 Tb1 O5 75.29(9) . . ?
O1 Tb1 O5 128.62(9) . . ?
O1 Tb1 O5 65.26(8) 3_666 . ?
O6 Tb1 O5 69.46(9) . . ?
O2 Tb1 N1 67.65(10) . . ?
O4 Tb1 N1 77.40(9) . . ?
O3 Tb1 N1 135.02(9) . . ?
O1 Tb1 N1 74.72(9) . . ?
O1 Tb1 N1 144.33(9) 3_666 . ?
O6 Tb1 N1 72.18(10) . . ?
O5 Tb1 N1 127.57(9) . . ?
O2 Tb1 Tb1 165.00(8) . 3_666 ?
O4 Tb1 Tb1 91.58(7) . 3_666 ?
O3 Tb1 Tb1 102.67(7) . 3_666 ?
O1 Tb1 Tb1 37.18(6) . 3_666 ?
O1 Tb1 Tb1 36.34(6) 3_666 3_666 ?
O6 Tb1 Tb1 80.45(7) . 3_666 ?
O5 Tb1 Tb1 97.00(6) . 3_666 ?
N1 Tb1 Tb1 110.44(7) . 3_666 ?

_refine_diff_density_max         1.670
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.098

