# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_uci52
_database_code_depnum_ccdc_archive 'CCDC 1538992'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C85 H121.45 Er K N2 O10'
_chemical_formula_weight         1537.64

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   19.7501(6)
_cell_length_b                   19.7501(6)
_cell_length_c                   19.7501(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7703.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9226
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      28.91

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_F_000             3250
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.203
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6349
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   rotating-anode
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19361
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.786
_diffrn_reflns_theta_max         29.262
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5953
_reflns_number_gt                5352
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_max     0.785
_reflns_Friedel_fraction_full    0.996

_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       'Bruker APEX2 2014.9-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.200 x 0.240 x 0.280 mm was mounted on a glass fiber
and transferred to a Bruker SMART APEX II diffractometer.  The APEX2 program package was used
to determine the unit-cell parameters and for data collection (3 sec/frame scan time for 99
frames of diffraction data).  The raw frame data was processed using SAINT and SADABS to yield
the reflection data file.  Subsequent calculations were carried out using the SHELXTL program.
The systematic absences were consistent with the cubic space group P213 that was later
determined to be correct. The structure was solved by direct methods and refined on F2 by
full-matrix least-squares techniques.  The analytical scattering factors for neutral atoms
were used throughout the analysis.  Hydrogen atoms were included using a riding model.  The
molecule and counter-ion were located on three-fold rotation axes.  The complex appeared to
be a mixed composition of approximately Er2+ (55%) / Er3+( 45%).  There was approximately 45%
of a hydride ligand present bound to Er(2).  The position of the hydride was evident in the
electron density map however it was necessary to fix the Er-H distance and the hydride thermal
parameter during refinement.  An ether solvent molecule was disordered about a three-fold rotation
axis and included with partial site-occupancy-factors. At convergence, wR2 = 0.0827 and
Goof = 1.114 for 301 variables refined against 5953 data (0.73A), R1 = 0.0413 for those 5352
data with I > 2.0sigma(I).  The absolute structure was assigned by refinement of the Flack
parameter.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+4.6163P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1988 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.022(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5953
_refine_ls_number_parameters     301
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.0827
_refine_ls_wR_factor_gt          0.0805
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Er1 Er 0.43761(2) 0.56239(2) 0.06239(2) 0.01189(15) Uani 0.55 3 d S T P . .
Er2 Er 0.45674(3) 0.54326(3) 0.04326(3) 0.0114(2) Uani 0.45 3 d DS T P . .
H1 H 0.5125(19) 0.4875(19) -0.0125(19) 0.060 Uiso 0.45 3 d DS U P . .
O1 O 0.52526(14) 0.53404(14) 0.12249(14) 0.0180(7) Uani 1 1 d . . . . .
C1 C 0.4149(2) 0.6102(2) 0.1830(2) 0.0159(9) Uani 1 1 d . . . . .
C2 C 0.4294(2) 0.6683(2) 0.1430(2) 0.0194(9) Uani 1 1 d . . . . .
C3 C 0.4860(3) 0.7141(2) 0.1637(3) 0.0281(11) Uani 1 1 d . . . . .
H3A H 0.4752 0.7608 0.1506 0.042 Uiso 1 1 calc R U . . .
H3B H 0.5279 0.6999 0.1412 0.042 Uiso 1 1 calc R U . . .
H3C H 0.4921 0.7118 0.2129 0.042 Uiso 1 1 calc R U . . .
C4 C 0.4605(2) 0.5905(2) 0.2414(2) 0.0207(10) Uani 1 1 d . . . . .
H4A H 0.4452 0.5456 0.2578 0.025 Uiso 1 1 calc R U . . .
H4B H 0.4522 0.6232 0.2785 0.025 Uiso 1 1 calc R U . . .
C5 C 0.5368(2) 0.5864(2) 0.2307(2) 0.0179(9) Uani 1 1 d . . . . .
C6 C 0.5657(2) 0.5553(2) 0.17284(19) 0.0145(8) Uani 1 1 d . . . . .
C7 C 0.6371(2) 0.5459(2) 0.1710(2) 0.0169(9) Uani 1 1 d . . . . .
C8 C 0.6745(2) 0.5696(2) 0.2261(2) 0.0183(9) Uani 1 1 d . . . . .
H8A H 0.7222 0.5633 0.2251 0.022 Uiso 1 1 calc R U . . .
C9 C 0.6472(2) 0.6015(2) 0.2821(2) 0.0205(10) Uani 1 1 d . . . . .
C10 C 0.5779(2) 0.6089(2) 0.2830(2) 0.0183(10) Uani 1 1 d . . . . .
H10A H 0.5574 0.6302 0.3210 0.022 Uiso 1 1 calc R U . . .
C11 C 0.6918(3) 0.6239(3) 0.3400(2) 0.0280(11) Uani 1 1 d . . . . .
H11A H 0.6640 0.6313 0.3804 0.042 Uiso 1 1 calc R U . . .
H11B H 0.7148 0.6661 0.3278 0.042 Uiso 1 1 calc R U . . .
H11C H 0.7256 0.5888 0.3494 0.042 Uiso 1 1 calc R U . . .
C12 C 0.6727(2) 0.5084(2) 0.1129(2) 0.0190(9) Uani 1 1 d . . . . .
C13 C 0.7507(2) 0.5081(3) 0.1231(3) 0.0330(13) Uani 1 1 d . . . . .
H13A H 0.7674 0.5554 0.1243 0.040 Uiso 1 1 calc R U . . .
H13B H 0.7616 0.4868 0.1671 0.040 Uiso 1 1 calc R U . . .
C14 C 0.7870(2) 0.4694(3) 0.0659(3) 0.0442(16) Uani 1 1 d . . . . .
H14A H 0.8369 0.4705 0.0740 0.053 Uiso 1 1 calc R U . . .
C15 C 0.7714(3) 0.5026(3) -0.0016(3) 0.0450(16) Uani 1 1 d . . . . .
H15A H 0.7947 0.4780 -0.0385 0.054 Uiso 1 1 calc R U . . .
H15B H 0.7880 0.5500 -0.0014 0.054 Uiso 1 1 calc R U . . .
C16 C 0.6943(2) 0.5015(3) -0.0134(3) 0.0303(12) Uani 1 1 d . . . . .
H16A H 0.6837 0.5227 -0.0582 0.036 Uiso 1 1 calc R U . . .
C17 C 0.6574(2) 0.5400(2) 0.0430(2) 0.0260(11) Uani 1 1 d . . . . .
H17A H 0.6080 0.5386 0.0345 0.031 Uiso 1 1 calc R U . . .
H17B H 0.6718 0.5879 0.0428 0.031 Uiso 1 1 calc R U . . .
C18 C 0.7626(2) 0.3959(3) 0.0663(3) 0.0455(16) Uani 1 1 d . . . . .
H18A H 0.7732 0.3746 0.1104 0.055 Uiso 1 1 calc R U . . .
H18B H 0.7859 0.3700 0.0302 0.055 Uiso 1 1 calc R U . . .
C19 C 0.6858(2) 0.3950(2) 0.0542(3) 0.0303(11) Uani 1 1 d . . . . .
H19A H 0.6697 0.3471 0.0534 0.036 Uiso 1 1 calc R U . . .
C20 C 0.6695(2) 0.4283(3) -0.0129(2) 0.0303(12) Uani 1 1 d . . . . .
H20A H 0.6200 0.4272 -0.0205 0.036 Uiso 1 1 calc R U . . .
H20B H 0.6915 0.4028 -0.0500 0.036 Uiso 1 1 calc R U . . .
C21 C 0.6495(2) 0.4333(2) 0.1117(2) 0.0214(10) Uani 1 1 d . . . . .
H21A H 0.6601 0.4117 0.1557 0.026 Uiso 1 1 calc R U . . .
H21B H 0.5999 0.4311 0.1048 0.026 Uiso 1 1 calc R U . . .
K1 K 0.39814(4) 0.39814(4) 0.39814(4) 0.0140(3) Uani 1 3 d S T P . .
N1 N 0.31292(18) 0.31292(18) 0.31292(18) 0.0187(14) Uani 1 3 d S T P . .
N2 N 0.48568(17) 0.48568(17) 0.48568(17) 0.0170(14) Uani 1 3 d S T P . .
O3 O 0.44900(15) 0.35286(15) 0.27351(14) 0.0193(6) Uani 1 1 d . . . . .
O4 O 0.52169(14) 0.44841(16) 0.34490(14) 0.0187(6) Uani 1 1 d . . . . .
C22 C 0.3553(2) 0.2763(2) 0.2641(2) 0.0235(10) Uani 1 1 d . . . . .
H22A H 0.3255 0.2540 0.2306 0.028 Uiso 1 1 calc R U . . .
H22B H 0.3803 0.2403 0.2885 0.028 Uiso 1 1 calc R U . . .
C23 C 0.4059(2) 0.3202(2) 0.2266(2) 0.0227(10) Uani 1 1 d . . . . .
H23A H 0.4331 0.2919 0.1955 0.027 Uiso 1 1 calc R U . . .
H23B H 0.3815 0.3545 0.1993 0.027 Uiso 1 1 calc R U . . .
C24 C 0.5002(2) 0.3911(2) 0.2412(2) 0.0220(10) Uani 1 1 d . . . . .
H24A H 0.4802 0.4323 0.2207 0.026 Uiso 1 1 calc R U . . .
H24B H 0.5211 0.3640 0.2045 0.026 Uiso 1 1 calc R U . . .
C25 C 0.5531(2) 0.4107(2) 0.2920(2) 0.0212(9) Uani 1 1 d . . . . .
H25A H 0.5747 0.3696 0.3109 0.025 Uiso 1 1 calc R U . . .
H25B H 0.5885 0.4385 0.2700 0.025 Uiso 1 1 calc R U . . .
C26 C 0.5709(2) 0.4690(2) 0.3939(2) 0.0209(9) Uani 1 1 d . . . . .
H26A H 0.6093 0.4916 0.3710 0.025 Uiso 1 1 calc R U . . .
H26B H 0.5885 0.4288 0.4182 0.025 Uiso 1 1 calc R U . . .
C27 C 0.5386(2) 0.5167(2) 0.4432(2) 0.0203(9) Uani 1 1 d . . . . .
H27A H 0.5742 0.5355 0.4730 0.024 Uiso 1 1 calc R U . . .
H27B H 0.5184 0.5548 0.4177 0.024 Uiso 1 1 calc R U . . .
O5 O 0.6867(7) 0.2879(7) 0.2598(8) 0.061(4) Uiso 0.3333 1 d . . P . .
C28 C 0.6878(8) 0.2405(8) 0.2118(8) 0.103(5) Uiso 0.6667 1 d . . P A -1
H28A H 0.6873 0.1959 0.2345 0.124 Uiso 0.6667 1 calc R U P A -1
H28B H 0.7316 0.2443 0.1877 0.124 Uiso 0.6667 1 calc R U P A -1
C29 C 0.6327(7) 0.2407(7) 0.1598(7) 0.094(4) Uiso 0.6667 1 d . . P A -1
H29A H 0.6399 0.2033 0.1280 0.142 Uiso 0.6667 1 calc R U P A -1
H29B H 0.5888 0.2351 0.1822 0.142 Uiso 0.6667 1 calc R U P A -1
H29C H 0.6334 0.2837 0.1352 0.142 Uiso 0.6667 1 calc R U P A -1


_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
Er1 Cnt 2.200 . ?
Er1 Er2 0.6543(8) . ?
Er1 O1 2.172(3) . ?
Er1 O1 2.172(3) 7_564 ?
Er1 O1 2.172(3) 10_655 ?
Er1 C1 2.602(4) . ?
Er1 C1 2.602(4) 7_564 ?
Er1 C1 2.602(4) 10_655 ?
Er1 C2 2.634(4) 7_564 ?
Er1 C2 2.634(4) 10_655 ?
Er1 C2 2.634(4) . ?
Er2 H1 1.91(7) . ?
Er2 O1 2.077(3) 7_564 ?
Er2 O1 2.077(3) 10_655 ?
Er2 O1 2.077(3) . ?
O1 C6 1.343(5) . ?
C1 C2 1.415(6) 7_564 ?
C1 C2 1.423(6) . ?
C1 C4 1.512(6) . ?
C2 C1 1.415(6) 10_655 ?
C2 C3 1.497(6) . ?
C4 C5 1.524(6) . ?
C5 C10 1.387(6) . ?
C5 C6 1.419(6) . ?
C6 C7 1.422(6) . ?
C7 C8 1.396(6) . ?
C7 C12 1.537(6) . ?
C8 C9 1.383(6) . ?
C9 C10 1.377(6) . ?
C9 C11 1.509(6) . ?
C12 C17 1.545(6) . ?
C12 C21 1.552(6) . ?
C12 C13 1.553(6) . ?
C13 C14 1.541(7) . ?
C14 C15 1.517(9) . ?
C14 C18 1.528(8) . ?
C15 C16 1.541(7) . ?
C16 C20 1.528(7) . ?
C16 C17 1.533(6) . ?
C18 C19 1.535(7) . ?
C19 C20 1.514(7) . ?
C19 C21 1.542(6) . ?
K1 O3 2.805(3) 9 ?
K1 O3 2.805(3) 5 ?
K1 O3 2.805(3) . ?
K1 O4 2.837(3) 9 ?
K1 O4 2.837(3) 5 ?
K1 O4 2.837(3) . ?
K1 N1 2.915(6) . ?
K1 N2 2.995(6) . ?
N1 C22 1.467(5) . ?
N1 C22 1.467(5) 5 ?
N1 C22 1.467(5) 9 ?
N2 C27 1.473(5) . ?
N2 C27 1.473(5) 9 ?
N2 C27 1.473(5) 5 ?
O3 C23 1.414(5) . ?
O3 C24 1.415(5) . ?
O4 C25 1.424(5) . ?
O4 C26 1.431(5) . ?
C22 C23 1.517(7) . ?
C24 C25 1.500(6) . ?
C26 C27 1.497(6) . ?
O5 C28 1.331(18) . ?
C28 C29 1.496(18) . ?

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
Cnt Er1 O1 107.1 . . ?
Er2 Er1 O1 72.94(8) . . ?
Er2 Er1 O1 72.94(8) . 7_564 ?
O1 Er1 O1 111.77(7) . 7_564 ?
Er2 Er1 O1 72.94(8) . 10_655 ?
O1 Er1 O1 111.77(7) . 10_655 ?
O1 Er1 O1 111.77(7) 7_564 10_655 ?
Er2 Er1 C1 146.89(9) . . ?
O1 Er1 C1 74.35(12) . . ?
O1 Er1 C1 115.54(12) 7_564 . ?
O1 Er1 C1 125.16(12) 10_655 . ?
Er2 Er1 C1 146.89(9) . 7_564 ?
O1 Er1 C1 125.16(12) . 7_564 ?
O1 Er1 C1 74.35(12) 7_564 7_564 ?
O1 Er1 C1 115.54(12) 10_655 7_564 ?
C1 Er1 C1 56.47(15) . 7_564 ?
Er2 Er1 C1 146.89(9) . 10_655 ?
O1 Er1 C1 115.54(12) . 10_655 ?
O1 Er1 C1 125.16(12) 7_564 10_655 ?
O1 Er1 C1 74.35(12) 10_655 10_655 ?
C1 Er1 C1 56.47(15) . 10_655 ?
C1 Er1 C1 56.47(15) 7_564 10_655 ?
Er2 Er1 C2 147.49(9) . 7_564 ?
O1 Er1 C2 93.64(12) . 7_564 ?
O1 Er1 C2 85.63(12) 7_564 7_564 ?
O1 Er1 C2 139.02(12) 10_655 7_564 ?
C1 Er1 C2 31.36(13) . 7_564 ?
C1 Er1 C2 31.53(13) 7_564 7_564 ?
C1 Er1 C2 65.62(13) 10_655 7_564 ?
Er2 Er1 C2 147.49(10) . 10_655 ?
O1 Er1 C2 139.01(12) . 10_655 ?
O1 Er1 C2 93.64(12) 7_564 10_655 ?
O1 Er1 C2 85.63(12) 10_655 10_655 ?
C1 Er1 C2 65.62(13) . 10_655 ?
C1 Er1 C2 31.36(13) 7_564 10_655 ?
C1 Er1 C2 31.53(13) 10_655 10_655 ?
C2 Er1 C2 55.49(16) 7_564 10_655 ?
Er2 Er1 C2 147.49(10) . . ?
O1 Er1 C2 85.63(12) . . ?
O1 Er1 C2 139.02(12) 7_564 . ?
O1 Er1 C2 93.64(12) 10_655 . ?
C1 Er1 C2 31.53(13) . . ?
C1 Er1 C2 65.62(13) 7_564 . ?
C1 Er1 C2 31.36(13) 10_655 . ?
C2 Er1 C2 55.48(16) 7_564 . ?
C2 Er1 C2 55.49(16) 10_655 . ?
Er1 Er2 H1 180.0(9) . . ?
Er1 Er2 O1 89.53(8) . 7_564 ?
H1 Er2 O1 90.47(8) . 7_564 ?
Er1 Er2 O1 89.53(8) . 10_655 ?
H1 Er2 O1 90.47(8) . 10_655 ?
O1 Er2 O1 119.993(2) 7_564 10_655 ?
Er1 Er2 O1 89.53(8) . . ?
H1 Er2 O1 90.47(8) . . ?
O1 Er2 O1 119.991(2) 7_564 . ?
O1 Er2 O1 119.996(2) 10_655 . ?
C6 O1 Er2 156.7(3) . . ?
C6 O1 Er1 143.0(3) . . ?
Er2 O1 Er1 17.53(3) . . ?
C2 C1 C2 119.5(4) 7_564 . ?
C2 C1 C4 119.7(4) 7_564 . ?
C2 C1 C4 120.8(4) . . ?
C2 C1 Er1 75.6(2) 7_564 . ?
C2 C1 Er1 75.5(2) . . ?
C4 C1 Er1 120.1(3) . . ?
C1 C2 C1 120.3(4) 10_655 . ?
C1 C2 C3 120.6(4) 10_655 . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 Er1 73.1(2) 10_655 . ?
C1 C2 Er1 73.0(2) . . ?
C3 C2 Er1 126.8(3) . . ?
C1 C4 C5 119.8(4) . . ?
C10 C5 C6 120.2(4) . . ?
C10 C5 C4 117.3(4) . . ?
C6 C5 C4 122.2(4) . . ?
O1 C6 C5 119.5(4) . . ?
O1 C6 C7 122.0(4) . . ?
C5 C6 C7 118.4(4) . . ?
C8 C7 C6 117.5(4) . . ?
C8 C7 C12 120.1(4) . . ?
C6 C7 C12 122.4(4) . . ?
C9 C8 C7 124.7(4) . . ?
C10 C9 C8 116.5(4) . . ?
C10 C9 C11 122.7(4) . . ?
C8 C9 C11 120.8(4) . . ?
C9 C10 C5 122.6(4) . . ?
C7 C12 C17 112.5(3) . . ?
C7 C12 C21 109.7(4) . . ?
C17 C12 C21 108.3(4) . . ?
C7 C12 C13 111.0(4) . . ?
C17 C12 C13 108.2(4) . . ?
C21 C12 C13 106.9(4) . . ?
C14 C13 C12 111.6(4) . . ?
C15 C14 C18 110.6(5) . . ?
C15 C14 C13 109.5(5) . . ?
C18 C14 C13 108.8(5) . . ?
C14 C15 C16 109.1(4) . . ?
C20 C16 C17 108.2(4) . . ?
C20 C16 C15 109.2(5) . . ?
C17 C16 C15 110.7(4) . . ?
C16 C17 C12 110.9(4) . . ?
C14 C18 C19 108.8(4) . . ?
C20 C19 C18 110.0(5) . . ?
C20 C19 C21 109.5(4) . . ?
C18 C19 C21 109.9(4) . . ?
C19 C20 C16 110.4(4) . . ?
C19 C21 C12 110.0(4) . . ?
O3 K1 O3 98.55(9) 9 5 ?
O3 K1 O3 98.55(9) 9 . ?
O3 K1 O3 98.55(9) 5 . ?
O3 K1 O4 58.55(8) 9 9 ?
O3 K1 O4 135.58(8) 5 9 ?
O3 K1 O4 120.76(8) . 9 ?
O3 K1 O4 120.75(8) 9 5 ?
O3 K1 O4 58.55(8) 5 5 ?
O3 K1 O4 135.58(8) . 5 ?
O4 K1 O4 98.48(8) 9 5 ?
O3 K1 O4 135.58(8) 9 . ?
O3 K1 O4 120.76(8) 5 . ?
O3 K1 O4 58.55(9) . . ?
O4 K1 O4 98.48(8) 9 . ?
O4 K1 O4 98.48(8) 5 . ?
O3 K1 N1 61.06(7) 9 . ?
O3 K1 N1 61.06(7) 5 . ?
O3 K1 N1 61.06(7) . . ?
O4 K1 N1 119.00(6) 9 . ?
O4 K1 N1 119.00(6) 5 . ?
O4 K1 N1 119.00(6) . . ?
O3 K1 N2 118.94(7) 9 . ?
O3 K1 N2 118.94(7) 5 . ?
O3 K1 N2 118.94(7) . . ?
O4 K1 N2 61.00(6) 9 . ?
O4 K1 N2 61.00(6) 5 . ?
O4 K1 N2 61.00(6) . . ?
N1 K1 N2 180.00(8) . . ?
C22 N1 C22 109.4(3) . 5 ?
C22 N1 C22 109.4(3) . 9 ?
C22 N1 C22 109.4(3) 5 9 ?
C22 N1 K1 109.5(3) . . ?
C22 N1 K1 109.5(3) 5 . ?
C22 N1 K1 109.5(3) 9 . ?
C27 N2 C27 110.3(3) . 9 ?
C27 N2 C27 110.3(3) . 5 ?
C27 N2 C27 110.3(3) 9 5 ?
C27 N2 K1 108.7(3) . . ?
C27 N2 K1 108.7(3) 9 . ?
C27 N2 K1 108.7(3) 5 . ?
C23 O3 C24 112.2(3) . . ?
C23 O3 K1 120.3(2) . . ?
C24 O3 K1 118.8(2) . . ?
C25 O4 C26 110.4(3) . . ?
C25 O4 K1 117.6(2) . . ?
C26 O4 K1 115.7(2) . . ?
N1 C22 C23 114.5(4) . . ?
O3 C23 C22 109.7(3) . . ?
O3 C24 C25 109.4(3) . . ?
O4 C25 C24 108.8(3) . . ?
O4 C26 C27 109.2(3) . . ?
N2 C27 C26 114.3(4) . . ?
O5 C28 C29 118.3(15) . . ?

_refine_diff_density_max         0.807
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_uci51
_database_code_depnum_ccdc_archive 'CCDC 1538993'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C85 H121.60 Dy K N2 O10.60'
_chemical_formula_weight         1542.64

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'
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'
K K 0.2009 0.2494 '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      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   19.7730(7)
_cell_length_b                   19.7730(7)
_cell_length_c                   19.7730(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7730.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2364
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      24.32

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_F_000             3262
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.081
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6531
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   sealed-tube
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7546
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.784
_diffrn_reflns_theta_max         28.259
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measured_fraction_theta_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.647
_diffrn_reflns_point_group_measured_fraction_full 0.707
_reflns_number_total             4155
_reflns_number_gt                3582
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.353
_reflns_Friedel_fraction_max     0.368
_reflns_Friedel_fraction_full    0.445

_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       'Bruker APEX2 2014.9-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.200 x 0.230 x 0.260 mm was mounted on
a glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The APEX2
program package was used to determine the unit-cell parameters and for data
collection (10 sec/frame scan time for 112 frames of data).  The raw frame data
was processed using SAINT and SADABS to yield the reflection data file.  Subsequent
calculations were carried out using the SHELXTL program.  The systematic absences
were consistent with the cubic space group P213 that was later determined to be
correct. The structure was solved by direct methods and refined on F2 by full-matrix
least-squares techniques.  The analytical scattering factors for neutral atoms were
used throughout the analysis.  Hydrogen atoms were included using a riding model.
The molecule was located on a three-fold rotation axis.  The complex was a mixed
composition of approximately Dy2+(40%) / Dy3+(60%).  There was approximately 60%
of a hydroxide ligand present.  An ether solvent molecule was disordered about a
three-fold rotation axis and included with partial  site-occupancy-factors.
At convergence, wR2 = 0.0956 and Goof = 1.043 for 303 variables refined against 4155
data (0.83Å), R1 = 0.0457 for those 3582 data with I > 2.0(I).  The absolute structure
was assigned by refinement of the Flack parameter.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0185P)²+0.2777P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 788 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.009(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4155
_refine_ls_number_parameters     303
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.0956
_refine_ls_wR_factor_gt          0.0916
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.43756(4) 0.56244(4) 0.06244(4) 0.0192(3) Uani 0.4 3 d S T P . .
Dy2 Dy 0.45498(3) 0.54502(3) 0.04502(3) 0.01575(18) Uani 0.6 3 d S T P . .
O2 O 0.5159(4) 0.4841(4) -0.0159(4) 0.051(3) Uani 0.6 3 d S T P . .
H2 H 0.4982 0.4803 -0.0543 0.076 Uiso 0.2 1 calc R U P . .
O1 O 0.52607(17) 0.53177(17) 0.12453(17) 0.0231(8) Uani 1 1 d . . . . .
C1 C 0.4159(3) 0.6094(3) 0.1826(3) 0.0267(12) Uani 1 1 d . . . . .
C2 C 0.4293(3) 0.6670(3) 0.1423(3) 0.0309(13) Uani 1 1 d . . . . .
C3 C 0.4870(3) 0.7124(3) 0.1614(3) 0.0419(16) Uani 1 1 d . . . . .
H3A H 0.4737 0.7596 0.1547 0.063 Uiso 1 1 calc R U . . .
H3B H 0.5262 0.7021 0.1329 0.063 Uiso 1 1 calc R U . . .
H3C H 0.4987 0.7050 0.2090 0.063 Uiso 1 1 calc R U . . .
C4 C 0.4609(3) 0.5901(3) 0.2417(3) 0.0330(14) Uani 1 1 d . . . . .
H4A H 0.4523 0.6230 0.2784 0.040 Uiso 1 1 calc R U . . .
H4B H 0.4454 0.5454 0.2583 0.040 Uiso 1 1 calc R U . . .
C5 C 0.5367(3) 0.5858(3) 0.2320(2) 0.0252(12) Uani 1 1 d . . . . .
C6 C 0.5655(3) 0.5542(3) 0.1749(2) 0.0207(11) Uani 1 1 d . . . . .
C7 C 0.6374(3) 0.5449(3) 0.1737(2) 0.0225(11) Uani 1 1 d . . . . .
C8 C 0.6746(3) 0.5692(3) 0.2283(3) 0.0243(12) Uani 1 1 d . . . . .
H8A H 0.7223 0.5635 0.2272 0.029 Uiso 1 1 calc R U . . .
C9 C 0.6464(3) 0.6015(3) 0.2846(3) 0.0278(13) Uani 1 1 d . . . . .
C10 C 0.5773(3) 0.6090(3) 0.2841(3) 0.0275(13) Uani 1 1 d . . . . .
H10A H 0.5565 0.6313 0.3212 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6909(3) 0.6242(3) 0.3423(3) 0.0398(16) Uani 1 1 d . . . . .
H11A H 0.6651 0.6225 0.3847 0.060 Uiso 1 1 calc R U . . .
H11B H 0.7062 0.6707 0.3341 0.060 Uiso 1 1 calc R U . . .
H11C H 0.7302 0.5942 0.3457 0.060 Uiso 1 1 calc R U . . .
C12 C 0.6730(3) 0.5077(3) 0.1158(3) 0.0244(12) Uani 1 1 d . . . . .
C13 C 0.7501(3) 0.5086(4) 0.1257(3) 0.0437(17) Uani 1 1 d . . . . .
H13A H 0.7659 0.5561 0.1271 0.052 Uiso 1 1 calc R U . . .
H13B H 0.7613 0.4873 0.1696 0.052 Uiso 1 1 calc R U . . .
C14 C 0.7873(3) 0.4710(4) 0.0690(4) 0.061(2) Uani 1 1 d . . . . .
H14A H 0.8371 0.4723 0.0778 0.073 Uiso 1 1 calc R U . . .
C15 C 0.7724(3) 0.5046(4) 0.0017(4) 0.057(2) Uani 1 1 d . . . . .
H15A H 0.7962 0.4804 -0.0351 0.068 Uiso 1 1 calc R U . . .
H15B H 0.7887 0.5520 0.0024 0.068 Uiso 1 1 calc R U . . .
C16 C 0.6957(3) 0.5031(3) -0.0110(3) 0.0410(16) Uani 1 1 d . . . . .
H16A H 0.6853 0.5252 -0.0553 0.049 Uiso 1 1 calc R U . . .
C17 C 0.6598(3) 0.5406(3) 0.0456(3) 0.0323(13) Uani 1 1 d . . . . .
H17A H 0.6106 0.5408 0.0365 0.039 Uiso 1 1 calc R U . . .
H17B H 0.6756 0.5881 0.0465 0.039 Uiso 1 1 calc R U . . .
C18 C 0.7634(3) 0.3974(4) 0.0679(4) 0.062(2) Uani 1 1 d . . . . .
H18A H 0.7741 0.3755 0.1116 0.074 Uiso 1 1 calc R U . . .
H18B H 0.7871 0.3724 0.0316 0.074 Uiso 1 1 calc R U . . .
C19 C 0.6863(3) 0.3952(3) 0.0555(4) 0.0406(16) Uani 1 1 d . . . . .
H19A H 0.6706 0.3471 0.0543 0.049 Uiso 1 1 calc R U . . .
C20 C 0.6703(3) 0.4296(3) -0.0117(3) 0.0334(15) Uani 1 1 d . . . . .
H20A H 0.6209 0.4289 -0.0195 0.040 Uiso 1 1 calc R U . . .
H20B H 0.6923 0.4045 -0.0491 0.040 Uiso 1 1 calc R U . . .
C21 C 0.6500(3) 0.4335(3) 0.1129(3) 0.0290(13) Uani 1 1 d . . . . .
H21A H 0.6005 0.4317 0.1055 0.035 Uiso 1 1 calc R U . . .
H21B H 0.6599 0.4112 0.1567 0.035 Uiso 1 1 calc R U . . .
K1 K 0.39794(5) 0.39794(5) 0.39794(5) 0.0163(4) Uani 1 3 d S T P . .
N1 N 0.3126(2) 0.3126(2) 0.3126(2) 0.0268(18) Uani 1 3 d S T P . .
N2 N 0.4849(2) 0.4849(2) 0.4849(2) 0.0247(17) Uani 1 3 d S T P . .
O3 O 0.4500(2) 0.35056(17) 0.27457(16) 0.0274(8) Uani 1 1 d . . . . .
O4 O 0.52174(16) 0.44673(19) 0.34571(16) 0.0245(8) Uani 1 1 d . . . . .
C22 C 0.3550(3) 0.2755(3) 0.2653(3) 0.0337(14) Uani 1 1 d . . . . .
H22A H 0.3254 0.2528 0.2319 0.040 Uiso 1 1 calc R U . . .
H22B H 0.3795 0.2398 0.2904 0.040 Uiso 1 1 calc R U . . .
C23 C 0.4062(3) 0.3182(3) 0.2274(3) 0.0329(14) Uani 1 1 d . . . . .
H23A H 0.4329 0.2892 0.1966 0.039 Uiso 1 1 calc R U . . .
H23B H 0.3825 0.3526 0.1999 0.039 Uiso 1 1 calc R U . . .
C24 C 0.5005(3) 0.3886(3) 0.2419(3) 0.0301(13) Uani 1 1 d . . . . .
H24A H 0.4802 0.4295 0.2212 0.036 Uiso 1 1 calc R U . . .
H24B H 0.5216 0.3614 0.2056 0.036 Uiso 1 1 calc R U . . .
C25 C 0.5532(3) 0.4090(3) 0.2928(3) 0.0295(12) Uani 1 1 d . . . . .
H25A H 0.5752 0.3682 0.3118 0.035 Uiso 1 1 calc R U . . .
H25B H 0.5884 0.4369 0.2707 0.035 Uiso 1 1 calc R U . . .
C26 C 0.5705(3) 0.4681(3) 0.3942(3) 0.0323(13) Uani 1 1 d . . . . .
H26A H 0.6086 0.4908 0.3710 0.039 Uiso 1 1 calc R U . . .
H26B H 0.5885 0.4283 0.4187 0.039 Uiso 1 1 calc R U . . .
C27 C 0.5383(3) 0.5155(3) 0.4428(3) 0.0292(12) Uani 1 1 d . . . . .
H27A H 0.5737 0.5341 0.4729 0.035 Uiso 1 1 calc R U . . .
H27B H 0.5185 0.5537 0.4172 0.035 Uiso 1 1 calc R U . . .
O5 O 0.6886(8) 0.2884(9) 0.2559(9) 0.067(4) Uiso 0.3333 1 d . . P . .
C28 C 0.6887(11) 0.2448(13) 0.2055(11) 0.144(8) Uiso 0.6667 1 d . . P A -1
H28A H 0.6949 0.1994 0.2257 0.173 Uiso 0.6667 1 calc R U P A -1
H28B H 0.7297 0.2542 0.1784 0.173 Uiso 0.6667 1 calc R U P A -1
C29 C 0.6343(9) 0.2394(9) 0.1594(10) 0.118(6) Uiso 0.6667 1 d . . P A -1
H29A H 0.6444 0.2041 0.1260 0.177 Uiso 0.6667 1 calc R U P A -1
H29B H 0.5929 0.2275 0.1839 0.177 Uiso 0.6667 1 calc R U P A -1
H29C H 0.6280 0.2827 0.1362 0.177 Uiso 0.6667 1 calc R U P A -1


_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 Cnt 2.177 . ?
Dy1 Dy2 0.5965(11) . ?
Dy1 O1 2.222(3) 7_564 ?
Dy1 O1 2.222(3) 10_655 ?
Dy1 O1 2.222(3) . ?
Dy1 C1 2.586(5) 10_655 ?
Dy1 C1 2.586(5) 7_564 ?
Dy1 C1 2.586(5) . ?
Dy1 C2 2.605(6) . ?
Dy1 C2 2.605(6) 10_655 ?
Dy1 C2 2.605(6) 7_564 ?
Dy2 Cnt 2.773 . ?
Dy1 O2 2.683(13) . ?
Dy2 O2 2.087(12) . ?
Dy2 O1 2.125(3) 7_564 ?
Dy2 O1 2.125(3) 10_655 ?
Dy2 O1 2.125(3) . ?
O1 C6 1.339(6) . ?
C1 C2 1.414(8) . ?
C1 C2 1.415(8) 7_564 ?
C1 C4 1.518(8) . ?
C2 C1 1.415(8) 10_655 ?
C2 C3 1.500(8) . ?
C4 C5 1.514(7) . ?
C5 C10 1.385(7) . ?
C5 C6 1.411(7) . ?
C6 C7 1.435(6) . ?
C7 C8 1.390(7) . ?
C7 C12 1.533(7) . ?
C8 C9 1.400(7) . ?
C9 C10 1.374(8) . ?
C9 C11 1.509(7) . ?
C12 C13 1.535(8) . ?
C12 C21 1.537(8) . ?
C12 C17 1.556(7) . ?
C13 C14 1.535(8) . ?
C14 C15 1.517(11) . ?
C14 C18 1.530(11) . ?
C15 C16 1.538(8) . ?
C16 C17 1.517(8) . ?
C16 C20 1.539(9) . ?
C18 C19 1.543(8) . ?
C19 C20 1.526(9) . ?
C19 C21 1.543(8) . ?
K1 O3 2.809(3) . ?
K1 O3 2.809(3) 9 ?
K1 O3 2.809(3) 5 ?
K1 O4 2.827(3) 9 ?
K1 O4 2.827(3) 5 ?
K1 O4 2.827(3) . ?
K1 N1 2.922(8) . ?
K1 N2 2.978(7) . ?
N1 C22 1.455(6) . ?
N1 C22 1.455(6) 9 ?
N1 C22 1.455(6) 5 ?
N2 C27 1.474(6) . ?
N2 C27 1.474(6) 9 ?
N2 C27 1.474(6) 5 ?
O3 C24 1.407(6) . ?
O3 C23 1.425(6) . ?
O4 C26 1.423(6) . ?
O4 C25 1.427(6) . ?
C22 C23 1.516(8) . ?
C24 C25 1.504(8) . ?
C26 C27 1.486(8) . ?
O5 C28 1.32(2) . ?
C28 C29 1.41(2) . ?

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
Cnt Dy1 O1 107.1 . . ?
Cnt Dy1 O2 180.0 . . ?
Cnt Dy2 O2 180.0 . . ?
Dy2 Dy1 O1 72.94(9) . 7_564 ?
Dy2 Dy1 O1 72.94(9) . 10_655 ?
O1 Dy1 O1 111.77(8) 7_564 10_655 ?
Dy2 Dy1 O1 72.94(9) . . ?
O1 Dy1 O1 111.77(8) 7_564 . ?
O1 Dy1 O1 111.77(8) 10_655 . ?
Dy2 Dy1 C1 146.43(12) . 10_655 ?
O1 Dy1 C1 124.77(16) 7_564 10_655 ?
O1 Dy1 C1 73.79(15) 10_655 10_655 ?
O1 Dy1 C1 116.23(15) . 10_655 ?
Dy2 Dy1 C1 146.43(12) . 7_564 ?
O1 Dy1 C1 73.79(15) 7_564 7_564 ?
O1 Dy1 C1 116.23(15) 10_655 7_564 ?
O1 Dy1 C1 124.77(16) . 7_564 ?
C1 Dy1 C1 57.23(19) 10_655 7_564 ?
Dy2 Dy1 C1 146.43(12) . . ?
O1 Dy1 C1 116.23(15) 7_564 . ?
O1 Dy1 C1 124.77(16) 10_655 . ?
O1 Dy1 C1 73.80(15) . . ?
C1 Dy1 C1 57.23(19) 10_655 . ?
C1 Dy1 C1 57.23(19) 7_564 . ?
Dy2 Dy1 C2 147.56(13) . . ?
O1 Dy1 C2 139.05(16) 7_564 . ?
O1 Dy1 C2 93.21(16) 10_655 . ?
O1 Dy1 C2 86.07(15) . . ?
C1 Dy1 C2 31.63(17) 10_655 . ?
C1 Dy1 C2 66.01(17) 7_564 . ?
C1 Dy1 C2 31.62(17) . . ?
Dy2 Dy1 C2 147.56(12) . 10_655 ?
O1 Dy1 C2 93.21(16) 7_564 10_655 ?
O1 Dy1 C2 86.07(15) 10_655 10_655 ?
O1 Dy1 C2 139.05(16) . 10_655 ?
C1 Dy1 C2 31.62(17) 10_655 10_655 ?
C1 Dy1 C2 31.63(17) 7_564 10_655 ?
C1 Dy1 C2 66.01(17) . 10_655 ?
C2 Dy1 C2 55.4(2) . 10_655 ?
Dy2 Dy1 C2 147.56(12) . 7_564 ?
O1 Dy1 C2 86.07(15) 7_564 7_564 ?
O1 Dy1 C2 139.05(16) 10_655 7_564 ?
O1 Dy1 C2 93.21(16) . 7_564 ?
C1 Dy1 C2 66.01(17) 10_655 7_564 ?
C1 Dy1 C2 31.62(17) 7_564 7_564 ?
C1 Dy1 C2 31.63(17) . 7_564 ?
C2 Dy1 C2 55.4(2) . 7_564 ?
C2 Dy1 C2 55.4(2) 10_655 7_564 ?
Dy2 Dy1 O2 0.00(17) . . ?
O1 Dy1 O2 72.94(9) 7_564 . ?
O1 Dy1 O2 72.94(9) 10_655 . ?
O1 Dy1 O2 72.94(9) . . ?
C1 Dy1 O2 146.43(12) 10_655 . ?
C1 Dy1 O2 146.43(12) 7_564 . ?
C1 Dy1 O2 146.43(12) . . ?
C2 Dy1 O2 147.56(12) . . ?
C2 Dy1 O2 147.56(12) 10_655 . ?
C2 Dy1 O2 147.56(12) 7_564 . ?
Dy1 Dy2 O2 180.0(2) . . ?
Dy1 Dy2 O1 91.49(9) . 7_564 ?
O2 Dy2 O1 88.51(9) . 7_564 ?
Dy1 Dy2 O1 91.49(9) . 10_655 ?
O2 Dy2 O1 88.51(9) . 10_655 ?
O1 Dy2 O1 119.933(8) 7_564 10_655 ?
Dy1 Dy2 O1 91.49(9) . . ?
O2 Dy2 O1 88.51(9) . . ?
O1 Dy2 O1 119.933(8) 7_564 . ?
O1 Dy2 O1 119.933(8) 10_655 . ?
Dy2 O2 Dy1 0.00(13) . . ?
C6 O1 Dy2 153.4(3) . . ?
C6 O1 Dy1 141.1(3) . . ?
Dy2 O1 Dy1 15.57(4) . . ?
C2 C1 C2 117.6(6) . 7_564 ?
C2 C1 C4 121.8(5) . . ?
C2 C1 C4 120.5(5) 7_564 . ?
C2 C1 Dy1 75.0(3) . . ?
C2 C1 Dy1 75.0(3) 7_564 . ?
C4 C1 Dy1 121.3(3) . . ?
C1 C2 C1 122.2(6) . 10_655 ?
C1 C2 C3 118.8(5) . . ?
C1 C2 C3 119.0(6) 10_655 . ?
C1 C2 Dy1 73.4(3) . . ?
C1 C2 Dy1 73.4(3) 10_655 . ?
C3 C2 Dy1 125.4(4) . . ?
C5 C4 C1 119.8(4) . . ?
C10 C5 C6 120.6(5) . . ?
C10 C5 C4 117.6(5) . . ?
C6 C5 C4 121.7(5) . . ?
O1 C6 C5 120.5(5) . . ?
O1 C6 C7 121.5(4) . . ?
C5 C6 C7 118.0(4) . . ?
C8 C7 C6 117.9(4) . . ?
C8 C7 C12 120.2(5) . . ?
C6 C7 C12 121.9(4) . . ?
C7 C8 C9 124.4(5) . . ?
C10 C9 C8 116.0(5) . . ?
C10 C9 C11 123.5(5) . . ?
C8 C9 C11 120.4(6) . . ?
C9 C10 C5 123.1(5) . . ?
C7 C12 C13 110.8(4) . . ?
C7 C12 C21 110.5(4) . . ?
C13 C12 C21 108.1(5) . . ?
C7 C12 C17 112.8(4) . . ?
C13 C12 C17 106.0(4) . . ?
C21 C12 C17 108.4(4) . . ?
C14 C13 C12 112.1(5) . . ?
C15 C14 C18 110.2(6) . . ?
C15 C14 C13 109.6(6) . . ?
C18 C14 C13 108.8(6) . . ?
C14 C15 C16 109.0(5) . . ?
C17 C16 C15 109.4(5) . . ?
C17 C16 C20 108.4(5) . . ?
C15 C16 C20 110.0(6) . . ?
C16 C17 C12 112.1(5) . . ?
C14 C18 C19 109.6(5) . . ?
C20 C19 C21 109.0(5) . . ?
C20 C19 C18 109.3(6) . . ?
C21 C19 C18 109.2(5) . . ?
C19 C20 C16 110.2(5) . . ?
C12 C21 C19 111.0(5) . . ?
O3 K1 O3 98.67(11) . 9 ?
O3 K1 O3 98.67(11) . 5 ?
O3 K1 O3 98.67(11) 9 5 ?
O3 K1 O4 120.35(10) . 9 ?
O3 K1 O4 58.61(10) 9 9 ?
O3 K1 O4 135.99(10) 5 9 ?
O3 K1 O4 135.99(10) . 5 ?
O3 K1 O4 120.35(10) 9 5 ?
O3 K1 O4 58.61(10) 5 5 ?
O4 K1 O4 98.37(10) 9 5 ?
O3 K1 O4 58.61(10) . . ?
O3 K1 O4 135.99(10) 9 . ?
O3 K1 O4 120.35(10) 5 . ?
O4 K1 O4 98.37(10) 9 . ?
O4 K1 O4 98.37(10) 5 . ?
O3 K1 N1 61.15(8) . . ?
O3 K1 N1 61.15(8) 9 . ?
O3 K1 N1 61.15(8) 5 . ?
O4 K1 N1 119.08(8) 9 . ?
O4 K1 N1 119.08(8) 5 . ?
O4 K1 N1 119.08(8) . . ?
O3 K1 N2 118.85(8) . . ?
O3 K1 N2 118.85(8) 9 . ?
O3 K1 N2 118.85(8) 5 . ?
O4 K1 N2 60.92(8) 9 . ?
O4 K1 N2 60.92(8) 5 . ?
O4 K1 N2 60.92(8) . . ?
N1 K1 N2 180.00(10) . . ?
C22 N1 C22 109.6(4) . 9 ?
C22 N1 C22 109.6(4) . 5 ?
C22 N1 C22 109.6(4) 9 5 ?
C22 N1 K1 109.3(4) . . ?
C22 N1 K1 109.3(4) 9 . ?
C22 N1 K1 109.3(4) 5 . ?
C27 N2 C27 110.0(3) . 9 ?
C27 N2 C27 110.0(3) . 5 ?
C27 N2 C27 110.0(3) 9 5 ?
C27 N2 K1 108.9(3) . . ?
C27 N2 K1 108.9(3) 9 . ?
C27 N2 K1 108.9(3) 5 . ?
C24 O3 C23 111.8(4) . . ?
C24 O3 K1 118.7(3) . . ?
C23 O3 K1 119.7(3) . . ?
C26 O4 C25 110.7(4) . . ?
C26 O4 K1 116.2(3) . . ?
C25 O4 K1 117.9(3) . . ?
N1 C22 C23 114.9(5) . . ?
O3 C23 C22 109.4(4) . . ?
O3 C24 C25 109.2(4) . . ?
O4 C25 C24 109.1(4) . . ?
O4 C26 C27 109.4(4) . . ?
N2 C27 C26 114.4(4) . . ?
O5 C28 C29 122(2) . . ?

_refine_diff_density_max         0.428
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_ctp65
_database_code_depnum_ccdc_archive 'CCDC 1538988'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C63 H75 Dy O3'
_chemical_formula_weight         1042.73

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'
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                   12.7567(11)
_cell_length_b                   15.6646(13)
_cell_length_c                   29.878(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.2651(13)
_cell_angle_gamma                90
_cell_volume                     5934.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6110
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      21.57

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_F_000             2172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.299
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6698
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48246
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_av_R_equivalents  0.1052
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.371
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12128
_reflns_number_gt                8073
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A colorless crystal of approximate dimensions 0.030 x 0.0.050 x 0.100 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters and 
for data collection (90 sec/frame scan time for a sphere of diffraction data).  
The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were consistent 
with the monoclinic space group P21/c that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis.  Hydrogen atoms were included using a riding 
model.

At convergence, wR2 = 0.0943 and Goof = 0.958 for 610 variables refined against 
12128 data (0.80Å), R1 = 0.0444 for those 8073 data with I > 2.0sigma(I).  

There were several high residuals present in the final difference-Fourier map.  
It was not possible to determine the nature of the residuals although it was 
probable that diethyether or hexane solvents were present.  The SQUEEZE routine 
in the PLATON program package was used to account for the electrons in the 
solvent accessible voids.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0349P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12128
_refine_ls_number_parameters     610
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.0943
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_restrained_S_all      0.958
_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 0.56438(2) 0.31432(2) 0.31223(2) 0.01598(7) Uani 1 1 d . . . . .
O1 O 0.4004(2) 0.32765(18) 0.30852(9) 0.0213(7) Uani 1 1 d . . . . .
O2 O 0.6416(2) 0.43068(17) 0.30486(9) 0.0173(7) Uani 1 1 d . . . . .
O3 O 0.6341(2) 0.22819(18) 0.36009(9) 0.0211(7) Uani 1 1 d . . . . .
C1 C 0.5565(4) 0.1671(3) 0.26201(14) 0.0196(11) Uani 1 1 d . . . . .
C2 C 0.4826(3) 0.2234(3) 0.23884(14) 0.0171(10) Uani 1 1 d . . . . .
C3 C 0.5181(3) 0.2982(2) 0.21847(14) 0.0170(10) Uani 1 1 d . . . . .
C4 C 0.6256(3) 0.3218(3) 0.22627(13) 0.0167(9) Uani 1 1 d . . . . .
C5 C 0.6985(3) 0.2667(3) 0.24994(14) 0.0179(10) Uani 1 1 d . . . . .
C6 C 0.6638(3) 0.1900(3) 0.26877(13) 0.0184(9) Uani 1 1 d . . . . .
C7 C 0.5197(4) 0.0822(3) 0.27766(14) 0.0221(11) Uani 1 1 d . . . . .
H7A H 0.4645 0.0597 0.2554 0.033 Uiso 1 1 calc R U . . .
H7B H 0.4915 0.0892 0.3067 0.033 Uiso 1 1 calc R U . . .
H7C H 0.5792 0.0422 0.2811 0.033 Uiso 1 1 calc R U . . .
C8 C 0.4429(4) 0.3489(3) 0.18640(15) 0.0236(10) Uani 1 1 d . . . . .
H8A H 0.3861 0.3115 0.1731 0.035 Uiso 1 1 calc R U . . .
H8B H 0.4808 0.3726 0.1625 0.035 Uiso 1 1 calc R U . . .
H8C H 0.4127 0.3955 0.2027 0.035 Uiso 1 1 calc R U . . .
C9 C 0.8156(3) 0.2870(3) 0.25437(16) 0.0261(11) Uani 1 1 d . . . . .
H9A H 0.8291 0.3314 0.2326 0.039 Uiso 1 1 calc R U . . .
H9B H 0.8552 0.2354 0.2483 0.039 Uiso 1 1 calc R U . . .
H9C H 0.8381 0.3072 0.2850 0.039 Uiso 1 1 calc R U . . .
C10 C 0.3653(3) 0.2049(3) 0.23802(16) 0.0222(11) Uani 1 1 d . . . . .
H10A H 0.3415 0.1778 0.2087 0.027 Uiso 1 1 calc R U . . .
H10B H 0.3568 0.1619 0.2617 0.027 Uiso 1 1 calc R U . . .
C11 C 0.2906(3) 0.2783(3) 0.24461(14) 0.0175(10) Uani 1 1 d . . . . .
C12 C 0.3096(4) 0.3353(3) 0.28094(14) 0.0194(11) Uani 1 1 d . . . . .
C13 C 0.2354(3) 0.4004(3) 0.28750(14) 0.0197(10) Uani 1 1 d . . . . .
C14 C 0.1454(3) 0.4044(3) 0.25684(14) 0.0219(11) Uani 1 1 d . . . . .
H14A H 0.0947 0.4473 0.2610 0.026 Uiso 1 1 calc R U . . .
C15 C 0.1251(4) 0.3494(3) 0.22037(15) 0.0225(11) Uani 1 1 d . . . . .
C16 C 0.1997(4) 0.2868(3) 0.21501(15) 0.0210(11) Uani 1 1 d . . . . .
H16A H 0.1881 0.2485 0.1903 0.025 Uiso 1 1 calc R U . . .
C17 C 0.0279(4) 0.3586(3) 0.18738(15) 0.0311(12) Uani 1 1 d . . . . .
H17A H -0.0235 0.3948 0.2005 0.047 Uiso 1 1 calc R U . . .
H17B H -0.0030 0.3021 0.1806 0.047 Uiso 1 1 calc R U . . .
H17C H 0.0468 0.3848 0.1596 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2529(3) 0.4640(3) 0.32679(14) 0.0181(10) Uani 1 1 d . . . . .
C19 C 0.2656(4) 0.4161(3) 0.37258(14) 0.0222(11) Uani 1 1 d . . . . .
H19A H 0.2007 0.3832 0.3760 0.027 Uiso 1 1 calc R U . . .
H19B H 0.3251 0.3755 0.3733 0.027 Uiso 1 1 calc R U . . .
C20 C 0.2860(4) 0.4800(3) 0.41166(15) 0.0249(11) Uani 1 1 d . . . . .
H20A H 0.2953 0.4481 0.4408 0.030 Uiso 1 1 calc R U . . .
C21 C 0.3860(4) 0.5308(3) 0.40633(15) 0.0262(11) Uani 1 1 d . . . . .
H21A H 0.4467 0.4914 0.4063 0.031 Uiso 1 1 calc R U . . .
H21B H 0.4006 0.5707 0.4319 0.031 Uiso 1 1 calc R U . . .
C22 C 0.3721(4) 0.5810(3) 0.36202(15) 0.0249(11) Uani 1 1 d . . . . .
H22A H 0.4377 0.6144 0.3587 0.030 Uiso 1 1 calc R U . . .
C23 C 0.2789(4) 0.6420(3) 0.36199(16) 0.0280(12) Uani 1 1 d . . . . .
H23A H 0.2917 0.6829 0.3872 0.034 Uiso 1 1 calc R U . . .
H23B H 0.2700 0.6747 0.3335 0.034 Uiso 1 1 calc R U . . .
C24 C 0.1802(4) 0.5901(3) 0.36693(15) 0.0246(11) Uani 1 1 d . . . . .
H24A H 0.1184 0.6295 0.3665 0.030 Uiso 1 1 calc R U . . .
C25 C 0.1610(4) 0.5271(3) 0.32795(15) 0.0246(11) Uani 1 1 d . . . . .
H25A H 0.1513 0.5591 0.2992 0.030 Uiso 1 1 calc R U . . .
H25B H 0.0953 0.4949 0.3309 0.030 Uiso 1 1 calc R U . . .
C26 C 0.3523(3) 0.5179(3) 0.32291(15) 0.0216(11) Uani 1 1 d . . . . .
H26A H 0.4140 0.4797 0.3227 0.026 Uiso 1 1 calc R U . . .
H26B H 0.3439 0.5498 0.2941 0.026 Uiso 1 1 calc R U . . .
C27 C 0.1932(4) 0.5416(3) 0.41174(15) 0.0260(11) Uani 1 1 d . . . . .
H27A H 0.2064 0.5823 0.4371 0.031 Uiso 1 1 calc R U . . .
H27B H 0.1279 0.5094 0.4156 0.031 Uiso 1 1 calc R U . . .
C28 C 0.6583(4) 0.4086(3) 0.20979(14) 0.0193(10) Uani 1 1 d . . . . .
H28A H 0.5931 0.4415 0.2007 0.023 Uiso 1 1 calc R U . . .
H28B H 0.6934 0.3993 0.1822 0.023 Uiso 1 1 calc R U . . .
C29 C 0.7307(3) 0.4649(3) 0.24145(15) 0.0180(10) Uani 1 1 d . . . . .
C30 C 0.7206(3) 0.4722(3) 0.28731(15) 0.0174(10) Uani 1 1 d . . . . .
C31 C 0.7930(3) 0.5234(3) 0.31524(14) 0.0157(10) Uani 1 1 d . . . . .
C32 C 0.8687(3) 0.5680(3) 0.29403(15) 0.0203(10) Uani 1 1 d . . . . .
H32A H 0.9181 0.6019 0.3123 0.024 Uiso 1 1 calc R U . . .
C33 C 0.8762(3) 0.5657(3) 0.24850(15) 0.0219(11) Uani 1 1 d . . . . .
C34 C 0.8071(3) 0.5127(3) 0.22277(15) 0.0211(11) Uani 1 1 d . . . . .
H34A H 0.8119 0.5086 0.1913 0.025 Uiso 1 1 calc R U . . .
C35 C 0.9548(4) 0.6193(3) 0.22677(16) 0.0339(13) Uani 1 1 d . . . . .
H35A H 1.0203 0.6237 0.2471 0.051 Uiso 1 1 calc R U . . .
H35B H 0.9257 0.6765 0.2206 0.051 Uiso 1 1 calc R U . . .
H35C H 0.9697 0.5925 0.1985 0.051 Uiso 1 1 calc R U . . .
C36 C 0.7891(3) 0.5293(3) 0.36606(14) 0.0194(10) Uani 1 1 d . . . . .
C37 C 0.8008(4) 0.4396(3) 0.38802(14) 0.0255(11) Uani 1 1 d . . . . .
H37A H 0.7443 0.4017 0.3741 0.031 Uiso 1 1 calc R U . . .
H37B H 0.8695 0.4146 0.3825 0.031 Uiso 1 1 calc R U . . .
C38 C 0.7940(4) 0.4453(3) 0.43894(15) 0.0308(12) Uani 1 1 d . . . . .
H38A H 0.7999 0.3866 0.4521 0.037 Uiso 1 1 calc R U . . .
C39 C 0.8840(4) 0.4999(4) 0.46085(17) 0.0395(14) Uani 1 1 d . . . . .
H39A H 0.8805 0.5031 0.4937 0.047 Uiso 1 1 calc R U . . .
H39B H 0.9525 0.4742 0.4556 0.047 Uiso 1 1 calc R U . . .
C40 C 0.8749(4) 0.5886(3) 0.44054(17) 0.0380(14) Uani 1 1 d . . . . .
H40A H 0.9343 0.6246 0.4546 0.046 Uiso 1 1 calc R U . . .
C41 C 0.7698(4) 0.6290(3) 0.44993(17) 0.0357(13) Uani 1 1 d . . . . .
H41A H 0.7662 0.6327 0.4828 0.043 Uiso 1 1 calc R U . . .
H41B H 0.7641 0.6875 0.4373 0.043 Uiso 1 1 calc R U . . .
C42 C 0.6794(4) 0.5740(3) 0.42820(15) 0.0279(12) Uani 1 1 d . . . . .
H42A H 0.6107 0.5998 0.4343 0.034 Uiso 1 1 calc R U . . .
C43 C 0.6844(3) 0.5697(3) 0.37679(14) 0.0213(10) Uani 1 1 d . . . . .
H43A H 0.6245 0.5353 0.3627 0.026 Uiso 1 1 calc R U . . .
H43B H 0.6780 0.6280 0.3640 0.026 Uiso 1 1 calc R U . . .
C44 C 0.8796(3) 0.5849(3) 0.38974(15) 0.0258(11) Uani 1 1 d . . . . .
H44A H 0.9483 0.5608 0.3836 0.031 Uiso 1 1 calc R U . . .
H44B H 0.8743 0.6435 0.3773 0.031 Uiso 1 1 calc R U . . .
C45 C 0.6876(4) 0.4836(3) 0.44744(15) 0.0272(12) Uani 1 1 d . . . . .
H45A H 0.6295 0.4480 0.4328 0.033 Uiso 1 1 calc R U . . .
H45B H 0.6815 0.4852 0.4802 0.033 Uiso 1 1 calc R U . . .
C46 C 0.7432(4) 0.1347(3) 0.29706(14) 0.0205(11) Uani 1 1 d . . . . .
H46A H 0.7610 0.0862 0.2781 0.025 Uiso 1 1 calc R U . . .
H46B H 0.8083 0.1688 0.3039 0.025 Uiso 1 1 calc R U . . .
C47 C 0.7147(3) 0.0981(3) 0.34120(15) 0.0201(10) Uani 1 1 d . . . . .
C48 C 0.6623(4) 0.1469(3) 0.37142(14) 0.0190(10) Uani 1 1 d . . . . .
C49 C 0.6375(4) 0.1104(3) 0.41224(15) 0.0232(11) Uani 1 1 d . . . . .
C50 C 0.6720(4) 0.0276(3) 0.42177(15) 0.0260(12) Uani 1 1 d . . . . .
H50A H 0.6573 0.0030 0.4495 0.031 Uiso 1 1 calc R U . . .
C51 C 0.7270(4) -0.0216(3) 0.39321(16) 0.0265(11) Uani 1 1 d . . . . .
C52 C 0.7462(4) 0.0150(3) 0.35283(15) 0.0232(11) Uani 1 1 d . . . . .
H52A H 0.7820 -0.0174 0.3323 0.028 Uiso 1 1 calc R U . . .
C53 C 0.7631(4) -0.1102(3) 0.40615(17) 0.0387(14) Uani 1 1 d . . . . .
H53A H 0.7021 -0.1453 0.4115 0.058 Uiso 1 1 calc R U . . .
H53B H 0.8125 -0.1079 0.4336 0.058 Uiso 1 1 calc R U . . .
H53C H 0.7984 -0.1354 0.3817 0.058 Uiso 1 1 calc R U . . .
C54 C 0.5749(4) 0.1602(3) 0.44504(15) 0.0235(11) Uani 1 1 d . . . . .
C55 C 0.6368(4) 0.2401(3) 0.46209(14) 0.0229(11) Uani 1 1 d . . . . .
H55A H 0.6504 0.2764 0.4362 0.027 Uiso 1 1 calc R U . . .
H55B H 0.7056 0.2231 0.4782 0.027 Uiso 1 1 calc R U . . .
C56 C 0.5729(4) 0.2913(3) 0.49434(15) 0.0318(13) Uani 1 1 d . . . . .
H56A H 0.6126 0.3442 0.5045 0.038 Uiso 1 1 calc R U . . .
C57 C 0.5568(4) 0.2367(3) 0.53503(16) 0.0371(14) Uani 1 1 d . . . . .
H57A H 0.5180 0.2696 0.5562 0.045 Uiso 1 1 calc R U . . .
H57B H 0.6260 0.2199 0.5508 0.045 Uiso 1 1 calc R U . . .
C58 C 0.4934(4) 0.1564(3) 0.51896(16) 0.0352(14) Uani 1 1 d . . . . .
H58A H 0.4831 0.1198 0.5455 0.042 Uiso 1 1 calc R U . . .
C59 C 0.3870(4) 0.1817(3) 0.49539(16) 0.0382(13) Uani 1 1 d . . . . .
H59A H 0.3469 0.2142 0.5163 0.046 Uiso 1 1 calc R U . . .
H59B H 0.3460 0.1300 0.4856 0.046 Uiso 1 1 calc R U . . .
C60 C 0.4038(4) 0.2368(3) 0.45443(16) 0.0330(13) Uani 1 1 d . . . . .
H60A H 0.3338 0.2541 0.4387 0.040 Uiso 1 1 calc R U . . .
C61 C 0.4651(4) 0.1848(3) 0.42192(15) 0.0277(11) Uani 1 1 d . . . . .
H61A H 0.4251 0.1325 0.4125 0.033 Uiso 1 1 calc R U . . .
H61B H 0.4730 0.2191 0.3947 0.033 Uiso 1 1 calc R U . . .
C62 C 0.5566(4) 0.1061(3) 0.48643(15) 0.0298(12) Uani 1 1 d . . . . .
H62A H 0.6255 0.0889 0.5024 0.036 Uiso 1 1 calc R U . . .
H62B H 0.5176 0.0536 0.4765 0.036 Uiso 1 1 calc R U . . .
C63 C 0.4667(4) 0.3160(3) 0.46925(16) 0.0370(13) Uani 1 1 d . . . . .
H63A H 0.4265 0.3509 0.4891 0.044 Uiso 1 1 calc R U . . .
H63B H 0.4781 0.3508 0.4426 0.044 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 Cnt 2.368 . ?
Dy1 O3 2.093(3) . ?
Dy1 O1 2.093(3) . ?
Dy1 O2 2.095(3) . ?
Dy1 C2 2.726(4) . ?
Dy1 C6 2.728(4) . ?
Dy1 C1 2.747(4) . ?
Dy1 C5 2.765(4) . ?
Dy1 C4 2.767(4) . ?
Dy1 C3 2.810(4) . ?
O1 C12 1.352(5) . ?
O2 C30 1.352(5) . ?
O3 C48 1.355(5) . ?
C1 C6 1.408(6) . ?
C1 C2 1.415(6) . ?
C1 C7 1.502(5) . ?
C2 C3 1.418(5) . ?
C2 C10 1.521(6) . ?
C3 C4 1.415(6) . ?
C3 C8 1.506(6) . ?
C4 C5 1.403(6) . ?
C4 C28 1.520(5) . ?
C5 C6 1.418(6) . ?
C5 C9 1.519(6) . ?
C6 C46 1.518(6) . ?
C10 C11 1.520(6) . ?
C11 C16 1.386(6) . ?
C11 C12 1.407(6) . ?
C12 C13 1.419(6) . ?
C13 C14 1.391(6) . ?
C13 C18 1.537(6) . ?
C14 C15 1.391(6) . ?
C15 C16 1.388(6) . ?
C15 C17 1.505(6) . ?
C18 C25 1.537(6) . ?
C18 C26 1.538(6) . ?
C18 C19 1.553(6) . ?
C19 C20 1.538(6) . ?
C20 C21 1.526(6) . ?
C20 C27 1.528(6) . ?
C21 C22 1.534(6) . ?
C22 C23 1.525(6) . ?
C22 C26 1.530(6) . ?
C23 C24 1.520(6) . ?
C24 C25 1.526(6) . ?
C24 C27 1.533(6) . ?
C28 C29 1.529(6) . ?
C29 C34 1.392(6) . ?
C29 C30 1.395(6) . ?
C30 C31 1.423(6) . ?
C31 C32 1.398(6) . ?
C31 C36 1.527(6) . ?
C32 C33 1.374(6) . ?
C33 C34 1.383(6) . ?
C33 C35 1.508(6) . ?
C36 C43 1.543(6) . ?
C36 C37 1.551(6) . ?
C36 C44 1.553(6) . ?
C37 C38 1.536(6) . ?
C38 C39 1.522(6) . ?
C38 C45 1.530(6) . ?
C39 C40 1.515(7) . ?
C40 C44 1.527(6) . ?
C40 C41 1.536(7) . ?
C41 C42 1.526(6) . ?
C42 C45 1.527(6) . ?
C42 C43 1.546(6) . ?
C46 C47 1.518(5) . ?
C47 C52 1.393(6) . ?
C47 C48 1.408(6) . ?
C48 C49 1.414(6) . ?
C49 C50 1.389(6) . ?
C49 C54 1.542(6) . ?
C50 C51 1.395(6) . ?
C51 C52 1.382(6) . ?
C51 C53 1.500(6) . ?
C54 C55 1.537(6) . ?
C54 C62 1.538(6) . ?
C54 C61 1.542(6) . ?
C55 C56 1.552(6) . ?
C56 C57 1.518(6) . ?
C56 C63 1.525(7) . ?
C57 C58 1.544(7) . ?
C58 C59 1.513(7) . ?
C58 C62 1.545(6) . ?
C59 C60 1.532(6) . ?
C60 C63 1.517(7) . ?
C60 C61 1.544(6) . ?

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
Cnt Dy1 O1 103.6 . . ?
Cnt Dy1 O2 101.4 . . ?
Cnt Dy1 O3 101.6 . . ?
O3 Dy1 O1 116.63(11) . . ?
O3 Dy1 O2 117.59(11) . . ?
O1 Dy1 O2 112.74(11) . . ?
O3 Dy1 C2 108.03(12) . . ?
O1 Dy1 C2 73.55(12) . . ?
O2 Dy1 C2 120.90(11) . . ?
O3 Dy1 C6 71.35(12) . . ?
O1 Dy1 C6 124.03(12) . . ?
O2 Dy1 C6 108.81(11) . . ?
C2 Dy1 C6 53.21(13) . . ?
O3 Dy1 C1 79.60(12) . . ?
O1 Dy1 C1 94.47(12) . . ?
O2 Dy1 C1 131.49(11) . . ?
C2 Dy1 C1 29.97(12) . . ?
C6 Dy1 C1 29.80(13) . . ?
O3 Dy1 C5 92.17(12) . . ?
O1 Dy1 C5 132.82(12) . . ?
O2 Dy1 C5 80.28(11) . . ?
C2 Dy1 C5 61.85(13) . . ?
C6 Dy1 C5 29.90(12) . . ?
C1 Dy1 C5 52.72(12) . . ?
O3 Dy1 C4 121.32(12) . . ?
O1 Dy1 C4 109.16(12) . . ?
O2 Dy1 C4 71.45(11) . . ?
C2 Dy1 C4 52.95(12) . . ?
C6 Dy1 C4 52.83(12) . . ?
C1 Dy1 C4 61.70(12) . . ?
C5 Dy1 C4 29.38(12) . . ?
O3 Dy1 C3 130.60(11) . . ?
O1 Dy1 C3 81.72(11) . . ?
O2 Dy1 C3 91.35(11) . . ?
C2 Dy1 C3 29.63(11) . . ?
C6 Dy1 C3 61.29(12) . . ?
C1 Dy1 C3 52.34(12) . . ?
C5 Dy1 C3 51.91(13) . . ?
C4 Dy1 C3 29.38(12) . . ?
C12 O1 Dy1 145.7(3) . . ?
C30 O2 Dy1 146.9(2) . . ?
C48 O3 Dy1 149.0(3) . . ?
C6 C1 C2 119.8(4) . . ?
C6 C1 C7 120.9(4) . . ?
C2 C1 C7 119.3(4) . . ?
C6 C1 Dy1 74.4(2) . . ?
C2 C1 Dy1 74.2(2) . . ?
C7 C1 Dy1 124.6(3) . . ?
C1 C2 C3 119.9(4) . . ?
C1 C2 C10 119.4(4) . . ?
C3 C2 C10 120.7(4) . . ?
C1 C2 Dy1 75.9(2) . . ?
C3 C2 Dy1 78.5(2) . . ?
C10 C2 Dy1 113.7(3) . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 C8 120.4(4) . . ?
C2 C3 C8 119.9(4) . . ?
C4 C3 Dy1 73.6(2) . . ?
C2 C3 Dy1 71.9(2) . . ?
C8 C3 Dy1 129.6(3) . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 C28 121.6(4) . . ?
C3 C4 C28 118.4(4) . . ?
C5 C4 Dy1 75.2(2) . . ?
C3 C4 Dy1 77.0(2) . . ?
C28 C4 Dy1 117.0(3) . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 C9 120.5(4) . . ?
C6 C5 C9 119.3(4) . . ?
C4 C5 Dy1 75.4(2) . . ?
C6 C5 Dy1 73.6(2) . . ?
C9 C5 Dy1 124.1(3) . . ?
C1 C6 C5 120.0(4) . . ?
C1 C6 C46 120.9(4) . . ?
C5 C6 C46 119.1(4) . . ?
C1 C6 Dy1 75.8(2) . . ?
C5 C6 Dy1 76.5(2) . . ?
C46 C6 Dy1 117.3(3) . . ?
C11 C10 C2 118.9(3) . . ?
C16 C11 C12 119.6(4) . . ?
C16 C11 C10 118.9(4) . . ?
C12 C11 C10 121.5(4) . . ?
O1 C12 C11 118.6(4) . . ?
O1 C12 C13 121.3(4) . . ?
C11 C12 C13 120.1(4) . . ?
C14 C13 C12 117.2(4) . . ?
C14 C13 C18 121.0(4) . . ?
C12 C13 C18 121.8(4) . . ?
C13 C14 C15 123.9(4) . . ?
C16 C15 C14 117.2(4) . . ?
C16 C15 C17 121.2(4) . . ?
C14 C15 C17 121.5(4) . . ?
C11 C16 C15 122.0(4) . . ?
C25 C18 C13 112.7(4) . . ?
C25 C18 C26 106.6(3) . . ?
C13 C18 C26 110.5(3) . . ?
C25 C18 C19 107.3(3) . . ?
C13 C18 C19 110.6(3) . . ?
C26 C18 C19 108.9(4) . . ?
C20 C19 C18 110.3(4) . . ?
C21 C20 C27 109.2(4) . . ?
C21 C20 C19 109.5(4) . . ?
C27 C20 C19 110.1(4) . . ?
C20 C21 C22 109.8(4) . . ?
C23 C22 C26 109.9(4) . . ?
C23 C22 C21 109.8(4) . . ?
C26 C22 C21 108.7(4) . . ?
C24 C23 C22 108.6(4) . . ?
C23 C24 C25 109.7(4) . . ?
C23 C24 C27 109.8(4) . . ?
C25 C24 C27 109.9(4) . . ?
C24 C25 C18 112.0(4) . . ?
C22 C26 C18 111.5(3) . . ?
C20 C27 C24 108.8(4) . . ?
C4 C28 C29 119.0(4) . . ?
C34 C29 C30 119.6(4) . . ?
C34 C29 C28 117.7(4) . . ?
C30 C29 C28 122.7(4) . . ?
O2 C30 C29 119.7(4) . . ?
O2 C30 C31 120.5(4) . . ?
C29 C30 C31 119.9(4) . . ?
C32 C31 C30 116.8(4) . . ?
C32 C31 C36 121.3(4) . . ?
C30 C31 C36 121.8(4) . . ?
C33 C32 C31 124.2(4) . . ?
C32 C33 C34 117.2(4) . . ?
C32 C33 C35 122.2(4) . . ?
C34 C33 C35 120.6(4) . . ?
C33 C34 C29 122.1(4) . . ?
C31 C36 C43 110.8(3) . . ?
C31 C36 C37 110.7(3) . . ?
C43 C36 C37 109.2(4) . . ?
C31 C36 C44 112.5(3) . . ?
C43 C36 C44 107.0(3) . . ?
C37 C36 C44 106.4(4) . . ?
C38 C37 C36 110.7(4) . . ?
C39 C38 C45 110.4(4) . . ?
C39 C38 C37 109.7(4) . . ?
C45 C38 C37 109.5(4) . . ?
C40 C39 C38 108.8(4) . . ?
C39 C40 C44 110.7(4) . . ?
C39 C40 C41 109.6(4) . . ?
C44 C40 C41 109.1(4) . . ?
C42 C41 C40 108.8(4) . . ?
C41 C42 C45 110.2(4) . . ?
C41 C42 C43 109.7(4) . . ?
C45 C42 C43 109.0(4) . . ?
C36 C43 C42 110.8(4) . . ?
C40 C44 C36 111.5(4) . . ?
C42 C45 C38 109.1(4) . . ?
C47 C46 C6 119.4(4) . . ?
C52 C47 C48 119.5(4) . . ?
C52 C47 C46 118.7(4) . . ?
C48 C47 C46 121.8(4) . . ?
O3 C48 C47 118.8(4) . . ?
O3 C48 C49 121.2(4) . . ?
C47 C48 C49 120.0(4) . . ?
C50 C49 C48 117.3(4) . . ?
C50 C49 C54 121.1(4) . . ?
C48 C49 C54 121.6(4) . . ?
C49 C50 C51 124.1(4) . . ?
C52 C51 C50 116.9(4) . . ?
C52 C51 C53 122.1(4) . . ?
C50 C51 C53 121.0(4) . . ?
C51 C52 C47 122.1(4) . . ?
C55 C54 C62 107.4(4) . . ?
C55 C54 C49 109.9(4) . . ?
C62 C54 C49 111.6(4) . . ?
C55 C54 C61 110.7(4) . . ?
C62 C54 C61 106.7(4) . . ?
C49 C54 C61 110.5(4) . . ?
C54 C55 C56 110.0(4) . . ?
C57 C56 C63 110.3(4) . . ?
C57 C56 C55 109.4(4) . . ?
C63 C56 C55 108.9(4) . . ?
C56 C57 C58 108.8(4) . . ?
C59 C58 C57 110.1(4) . . ?
C59 C58 C62 110.1(4) . . ?
C57 C58 C62 108.7(4) . . ?
C58 C59 C60 108.8(4) . . ?
C63 C60 C59 110.1(4) . . ?
C63 C60 C61 109.1(4) . . ?
C59 C60 C61 109.3(4) . . ?
C54 C61 C60 110.4(4) . . ?
C54 C62 C58 111.1(4) . . ?
C60 C63 C56 110.4(4) . . ?

_refine_diff_density_max         0.745
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.114



####################################################################### 
# 
# 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_mef36
_database_code_depnum_ccdc_archive 'CCDC 1538991'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C85 H121.35 Gd K N2 O10'
_chemical_formula_weight         1527.53

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'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   19.7291(9)
_cell_length_b                   19.7291(9)
_cell_length_c                   19.7291(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7679.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.23

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             3233
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.102
_exptl_absorpt_coefficient_mu    0.978
_shelx_estimated_absorpt_T_min   0.843
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8710
_exptl_absorpt_correction_T_max  0.9263
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67649
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.788
_diffrn_reflns_theta_max         26.016
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5062
_reflns_number_gt                4861
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.102 x 0.177 x 0.181 mm was mounted on a
glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The APEX2
program package was used to determine the unit-cell parameters and for data collection
(180 sec/frame scan time for a sphere of diffraction data).  The raw frame data was
processed using SAINT and SADABS to yield the reflection data file.  Subsequent
calculations were carried out using the SHELXTL program.  The systematic absences
were consistent with the cubic space group P213 that was later determined to be correct.
The structure was solved by direct methods and refined on F2 by full-matrix least-squares
techniques.  The analytical scattering factors for neutral atoms were used throughout
the analysis.  Hydrogen atoms were included using a riding model.  The molecule and
counter-ion were located on a three-fold rotation axes.  The complex appeared to be
a mixed composition of approximately Gd2+ (65%) / Gd3+( 35%).  There was approximately
35% of a hydride ligand present bound to Gd(2).  The position of the hydride was
evident in the electron density map however it was necessary to fix the  Gd-H distance
and the hydride thermal parameter during refinement.   An ether solvent molecule was
disordered about a three-fold rotation axis and included with partial site-occupancy-factors.
At convergence, wR2 = 0.0951 and Goof = 1.222 for 301 variables refined against 5062
data (0.81), R1 = 0.0372 for those 4861 data with I > 2.0sigma(I).  The absolute structure
was assigned by refinement of the Flack parameter.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0359P)²+8.1498P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 2074 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.008(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5062
_refine_ls_number_parameters     301
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.222
_refine_ls_restrained_S_all      1.222
_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 0.68990(3) 0.68990(3) 0.68990(3) 0.02117(19) Uani 0.65 3 d S T P . .
Gd2 Gd 0.70680(5) 0.70680(5) 0.70680(5) 0.0200(4) Uani 0.35 3 d DS T P . .
H1 H 0.764(2) 0.764(2) 0.764(2) 0.050 Uiso 0.35 3 d DS U P . .
O1 O 0.62532(17) 0.71888(18) 0.77627(17) 0.0288(8) Uani 1 1 d . . . . .
C1 C 0.5666(3) 0.6398(3) 0.6648(3) 0.0310(11) Uani 1 1 d . . . . .
C2 C 0.6068(3) 0.5811(3) 0.6789(3) 0.0359(12) Uani 1 1 d . . . . .
C3 C 0.5869(3) 0.5368(3) 0.7364(3) 0.0456(15) Uani 1 1 d . . . . .
H3A H 0.6001 0.4899 0.7265 0.068 Uiso 1 1 calc R U . . .
H3B H 0.5377 0.5391 0.7428 0.068 Uiso 1 1 calc R U . . .
H3C H 0.6097 0.5521 0.7777 0.068 Uiso 1 1 calc R U . . .
C4 C 0.5082(3) 0.6596(3) 0.7104(3) 0.0360(12) Uani 1 1 d . . . . .
H4A H 0.4709 0.6271 0.7018 0.043 Uiso 1 1 calc R U . . .
H4B H 0.4921 0.7046 0.6952 0.043 Uiso 1 1 calc R U . . .
C5 C 0.5179(2) 0.6635(3) 0.7868(3) 0.0293(11) Uani 1 1 d . . . . .
C6 C 0.5750(2) 0.6960(3) 0.8165(2) 0.0261(10) Uani 1 1 d . . . . .
C7 C 0.5763(3) 0.7054(2) 0.8878(3) 0.0270(10) Uani 1 1 d . . . . .
C8 C 0.5218(2) 0.6812(3) 0.9252(3) 0.0291(11) Uani 1 1 d . . . . .
H8A H 0.5228 0.6873 0.9730 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4661(3) 0.6487(3) 0.8974(3) 0.0323(12) Uani 1 1 d . . . . .
C10 C 0.4659(2) 0.6405(3) 0.8283(3) 0.0317(12) Uani 1 1 d . . . . .
H10A H 0.4285 0.6180 0.8080 0.038 Uiso 1 1 calc R U . . .
C11 C 0.4081(3) 0.6254(3) 0.9420(3) 0.0442(15) Uani 1 1 d . . . . .
H11A H 0.3673 0.6196 0.9143 0.066 Uiso 1 1 calc R U . . .
H11B H 0.3995 0.6594 0.9772 0.066 Uiso 1 1 calc R U . . .
H11C H 0.4200 0.5822 0.9633 0.066 Uiso 1 1 calc R U . . .
C12 C 0.6351(3) 0.7425(3) 0.9232(3) 0.0289(11) Uani 1 1 d . . . . .
C13 C 0.6364(3) 0.8177(3) 0.9002(3) 0.0306(11) Uani 1 1 d . . . . .
H13A H 0.6428 0.8200 0.8505 0.037 Uiso 1 1 calc R U . . .
H13B H 0.5926 0.8395 0.9115 0.037 Uiso 1 1 calc R U . . .
C14 C 0.6950(3) 0.8556(3) 0.9363(3) 0.0408(13) Uani 1 1 d . . . . .
H14A H 0.6963 0.9038 0.9205 0.049 Uiso 1 1 calc R U . . .
C15 C 0.7620(3) 0.8215(3) 0.9199(3) 0.0396(14) Uani 1 1 d . . . . .
H15A H 0.7993 0.8464 0.9423 0.048 Uiso 1 1 calc R U . . .
H15B H 0.7698 0.8229 0.8704 0.048 Uiso 1 1 calc R U . . .
C16 C 0.7621(3) 0.7480(3) 0.9438(3) 0.0395(13) Uani 1 1 d . . . . .
H16A H 0.8067 0.7265 0.9330 0.047 Uiso 1 1 calc R U . . .
C17 C 0.7047(3) 0.7099(3) 0.9068(3) 0.0392(15) Uani 1 1 d . . . . .
H17A H 0.7045 0.6618 0.9211 0.047 Uiso 1 1 calc R U . . .
H17B H 0.7127 0.7114 0.8573 0.047 Uiso 1 1 calc R U . . .
C18 C 0.6828(4) 0.8539(4) 1.0134(3) 0.058(2) Uani 1 1 d . . . . .
H18A H 0.7189 0.8796 1.0370 0.070 Uiso 1 1 calc R U . . .
H18B H 0.6386 0.8751 1.0242 0.070 Uiso 1 1 calc R U . . .
C19 C 0.6831(4) 0.7801(4) 1.0371(3) 0.057(2) Uani 1 1 d . . . . .
H19A H 0.6751 0.7786 1.0871 0.068 Uiso 1 1 calc R U . . .
C20 C 0.7502(4) 0.7467(4) 1.0213(3) 0.0562(19) Uani 1 1 d . . . . .
H20A H 0.7499 0.6993 1.0377 0.067 Uiso 1 1 calc R U . . .
H20B H 0.7873 0.7712 1.0446 0.067 Uiso 1 1 calc R U . . .
C21 C 0.6251(3) 0.7427(4) 1.0007(3) 0.0446(15) Uani 1 1 d . . . . .
H21A H 0.5815 0.7650 1.0117 0.053 Uiso 1 1 calc R U . . .
H21B H 0.6229 0.6954 1.0173 0.053 Uiso 1 1 calc R U . . .
K1 K 0.64801(5) 0.35199(5) 0.85199(5) 0.0212(3) Uani 1 3 d S T P . .
O3 O 0.52391(16) 0.39828(18) 0.80046(19) 0.0311(8) Uani 1 1 d . . . . .
O4 O 0.59551(17) 0.3031(2) 0.72773(16) 0.0298(7) Uani 1 1 d . . . . .
N1 N 0.5627(2) 0.4373(2) 0.9373(2) 0.0323(17) Uani 1 3 d S T P . .
N2 N 0.7353(2) 0.2647(2) 0.7647(2) 0.0250(15) Uani 1 3 d S T P . .
C22 C 0.5142(3) 0.4743(3) 0.8949(3) 0.0378(13) Uani 1 1 d . . . . .
H22A H 0.5388 0.5103 0.8701 0.045 Uiso 1 1 calc R U . . .
H22B H 0.4805 0.4966 0.9246 0.045 Uiso 1 1 calc R U . . .
C23 C 0.4771(3) 0.4305(3) 0.8442(3) 0.0366(12) Uani 1 1 d . . . . .
H23A H 0.4501 0.3959 0.8685 0.044 Uiso 1 1 calc R U . . .
H23B H 0.4456 0.4589 0.8173 0.044 Uiso 1 1 calc R U . . .
C24 C 0.4916(3) 0.3599(3) 0.7491(3) 0.0355(12) Uani 1 1 d . . . . .
H24A H 0.4548 0.3869 0.7282 0.043 Uiso 1 1 calc R U . . .
H24B H 0.4714 0.3185 0.7689 0.043 Uiso 1 1 calc R U . . .
C25 C 0.5426(3) 0.3410(3) 0.6964(3) 0.0327(11) Uani 1 1 d . . . . .
H25A H 0.5208 0.3134 0.6605 0.039 Uiso 1 1 calc R U . . .
H25B H 0.5615 0.3824 0.6752 0.039 Uiso 1 1 calc R U . . .
C26 C 0.6441(3) 0.2820(3) 0.6785(2) 0.0316(11) Uani 1 1 d . . . . .
H26A H 0.6686 0.3220 0.6605 0.038 Uiso 1 1 calc R U . . .
H26B H 0.6208 0.2593 0.6403 0.038 Uiso 1 1 calc R U . . .
C27 C 0.6933(3) 0.2340(2) 0.7111(2) 0.0307(11) Uani 1 1 d . . . . .
H27A H 0.6677 0.1956 0.7308 0.037 Uiso 1 1 calc R U . . .
H27B H 0.7236 0.2155 0.6756 0.037 Uiso 1 1 calc R U . . .
O5 O 0.5911(9) 1.0102(9) 0.8805(9) 0.074(5) Uiso 0.3333 1 d . . P . .
C28 C 0.5466(12) 1.0079(13) 0.9309(12) 0.137(8) Uiso 0.6667 1 d . . P A -1
H28A H 0.5271 1.0540 0.9336 0.165 Uiso 0.6667 1 calc R U P A -1
H28B H 0.5740 1.0019 0.9726 0.165 Uiso 0.6667 1 calc R U P A -1
C29 C 0.4912(9) 0.9634(9) 0.9382(9) 0.099(5) Uiso 0.6667 1 d . . P A -1
H29A H 0.4673 0.9736 0.9806 0.148 Uiso 0.6667 1 calc R U P A -1
H29B H 0.4601 0.9693 0.8999 0.148 Uiso 0.6667 1 calc R U P A -1
H29C H 0.5076 0.9166 0.9393 0.148 Uiso 0.6667 1 calc R U P A -1


_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 Cnt 2.286 . ?
Gd1 Gd2 0.5773(12) . ?
Gd1 O1 2.203(3) . ?
Gd1 O1 2.203(3) 9 ?
Gd1 O1 2.203(3) 5 ?
Gd1 C1 2.672(5) 9 ?
Gd1 C1 2.672(5) 5 ?
Gd1 C1 2.672(5) . ?
Gd1 C2 2.710(6) 5 ?
Gd1 C2 2.710(6) 9 ?
Gd1 C2 2.710(6) . ?
Gd2 H1 1.94(7) . ?
Gd2 O1 2.126(3) . ?
Gd2 O1 2.126(3) 5 ?
Gd2 O1 2.126(3) 9 ?
O1 C6 1.349(6) . ?
C1 C2 1.409(8) 9 ?
C1 C2 1.431(8) . ?
C1 C4 1.514(8) . ?
C2 C1 1.409(8) 5 ?
C2 C3 1.485(8) . ?
C4 C5 1.520(7) . ?
C5 C10 1.390(7) . ?
C5 C6 1.421(7) . ?
C6 C7 1.420(7) . ?
C7 C8 1.387(7) . ?
C7 C12 1.539(7) . ?
C8 C9 1.386(7) . ?
C9 C10 1.373(8) . ?
C9 C11 1.514(8) . ?
C12 C21 1.541(7) . ?
C12 C17 1.551(8) . ?
C12 C13 1.551(7) . ?
C13 C14 1.551(8) . ?
C14 C15 1.517(9) . ?
C14 C18 1.540(8) . ?
C15 C16 1.525(9) . ?
C16 C17 1.543(7) . ?
C16 C20 1.546(8) . ?
C18 C19 1.530(11) . ?
C19 C20 1.511(11) . ?
C19 C21 1.539(8) . ?
K1 O3 2.804(3) 7_665 ?
K1 O3 2.804(3) 10_646 ?
K1 O3 2.804(3) . ?
K1 O4 2.831(3) 7_665 ?
K1 O4 2.831(3) 10_646 ?
K1 O4 2.831(3) . ?
K1 N1 2.917(8) . ?
K1 N2 2.983(7) . ?
O3 C23 1.416(7) . ?
O3 C24 1.417(6) . ?
O4 C25 1.425(6) . ?
O4 C26 1.426(6) . ?
N1 C22 1.465(6) . ?
N1 C22 1.465(6) 7_665 ?
N1 C22 1.465(6) 10_646 ?
N2 C27 1.473(6) 7_665 ?
N2 C27 1.473(6) 10_646 ?
N2 C27 1.473(6) . ?
C22 C23 1.510(8) . ?
C24 C25 1.495(8) . ?
C26 C27 1.503(7) . ?
O5 C28 1.33(3) . ?
C28 C29 1.41(2) . ?

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
Cnt Gd1 O1 105.2 . . ?
Gd2 Gd1 O1 74.78(9) . . ?
O1 Gd1 O1 113.37(8) . 9 ?
O1 Gd1 O1 113.37(7) . 5 ?
Gd2 Gd1 C1 147.79(12) . 9 ?
O1 Gd1 C1 122.55(15) . 9 ?
O1 Gd1 C1 73.30(15) 9 9 ?
O1 Gd1 C1 114.55(15) 5 9 ?
Gd2 Gd1 C1 147.79(11) . 5 ?
O1 Gd1 C1 114.55(15) . 5 ?
O1 Gd1 C1 122.55(15) 9 5 ?
O1 Gd1 C1 73.30(15) 5 5 ?
C1 Gd1 C1 54.98(19) 9 5 ?
Gd2 Gd1 C1 147.79(12) . . ?
O1 Gd1 C1 73.30(15) . . ?
O1 Gd1 C1 114.55(15) 9 . ?
O1 Gd1 C1 122.55(15) 5 . ?
C1 Gd1 C1 54.98(19) 9 . ?
C1 Gd1 C1 54.98(19) 5 . ?
Gd2 Gd1 C2 148.54(12) . 5 ?
O1 Gd1 C2 136.33(15) . 5 ?
O1 Gd1 C2 91.73(15) 9 5 ?
O1 Gd1 C2 85.30(15) 5 5 ?
C1 Gd1 C2 30.34(17) 9 5 ?
C1 Gd1 C2 30.84(17) 5 5 ?
C1 Gd1 C2 63.67(16) . 5 ?
Gd2 Gd1 C2 148.54(12) . 9 ?
O1 Gd1 C2 91.73(16) . 9 ?
O1 Gd1 C2 85.30(15) 9 9 ?
O1 Gd1 C2 136.33(15) 5 9 ?
C1 Gd1 C2 30.84(17) 9 9 ?
C1 Gd1 C2 63.67(16) 5 9 ?
C1 Gd1 C2 30.34(17) . 9 ?
C2 Gd1 C2 53.74(19) 5 9 ?
Gd2 Gd1 C2 148.54(12) . . ?
O1 Gd1 C2 85.30(15) . . ?
O1 Gd1 C2 136.33(15) 9 . ?
O1 Gd1 C2 91.73(15) 5 . ?
C1 Gd1 C2 63.67(16) 9 . ?
C1 Gd1 C2 30.35(17) 5 . ?
C1 Gd1 C2 30.84(17) . . ?
C2 Gd1 C2 53.74(19) 5 . ?
C2 Gd1 C2 53.74(19) 9 . ?
Gd1 Gd2 H1 180.0(10) . . ?
Gd1 Gd2 O1 90.02(10) . . ?
H1 Gd2 O1 89.98(10) . . ?
Gd1 Gd2 O1 90.02(10) . 5 ?
H1 Gd2 O1 89.98(10) . 5 ?
O1 Gd2 O1 120.0 . 5 ?
Gd1 Gd2 O1 90.02(10) . 9 ?
H1 Gd2 O1 89.98(10) . 9 ?
O1 Gd2 O1 120.003(1) . 9 ?
O1 Gd2 O1 120.0 5 9 ?
C6 O1 Gd2 154.0(3) . . ?
C6 O1 Gd1 142.5(3) . . ?
Gd2 O1 Gd1 15.19(4) . . ?
C2 C1 C2 119.2(6) 9 . ?
C2 C1 C4 119.7(5) 9 . ?
C2 C1 C4 121.1(5) . . ?
C2 C1 Gd1 76.3(3) 9 . ?
C2 C1 Gd1 76.1(3) . . ?
C4 C1 Gd1 119.2(3) . . ?
C1 C2 C1 120.5(6) 5 . ?
C1 C2 C3 121.0(5) 5 . ?
C1 C2 C3 118.5(5) . . ?
C1 C2 Gd1 73.3(3) 5 . ?
C1 C2 Gd1 73.1(3) . . ?
C3 C2 Gd1 124.4(4) . . ?
C1 C4 C5 120.4(5) . . ?
C10 C5 C6 119.3(5) . . ?
C10 C5 C4 118.3(5) . . ?
C6 C5 C4 122.1(5) . . ?
O1 C6 C7 121.7(4) . . ?
O1 C6 C5 119.4(4) . . ?
C7 C6 C5 118.8(4) . . ?
C8 C7 C6 117.9(5) . . ?
C8 C7 C12 120.4(4) . . ?
C6 C7 C12 121.7(4) . . ?
C9 C8 C7 124.3(5) . . ?
C10 C9 C8 116.7(5) . . ?
C10 C9 C11 122.6(5) . . ?
C8 C9 C11 120.7(5) . . ?
C9 C10 C5 123.0(5) . . ?
C7 C12 C21 110.8(4) . . ?
C7 C12 C17 112.0(4) . . ?
C21 C12 C17 108.7(5) . . ?
C7 C12 C13 109.6(4) . . ?
C21 C12 C13 106.8(5) . . ?
C17 C12 C13 108.7(4) . . ?
C14 C13 C12 109.9(4) . . ?
C15 C14 C18 109.7(5) . . ?
C15 C14 C13 109.7(4) . . ?
C18 C14 C13 109.0(5) . . ?
C14 C15 C16 111.0(5) . . ?
C15 C16 C17 108.4(4) . . ?
C15 C16 C20 108.7(6) . . ?
C17 C16 C20 110.4(5) . . ?
C16 C17 C12 110.4(5) . . ?
C19 C18 C14 108.8(5) . . ?
C20 C19 C18 110.8(6) . . ?
C20 C19 C21 110.3(6) . . ?
C18 C19 C21 108.1(6) . . ?
C19 C20 C16 109.3(5) . . ?
C19 C21 C12 111.7(5) . . ?
O3 K1 O3 98.65(11) 7_665 10_646 ?
O3 K1 O3 98.64(11) 7_665 . ?
O3 K1 O3 98.64(11) 10_646 . ?
O3 K1 O4 58.50(11) 7_665 7_665 ?
O3 K1 O4 135.42(11) 10_646 7_665 ?
O3 K1 O4 120.89(10) . 7_665 ?
O3 K1 O4 120.89(10) 7_665 10_646 ?
O3 K1 O4 58.50(11) 10_646 10_646 ?
O3 K1 O4 135.42(11) . 10_646 ?
O4 K1 O4 98.42(10) 7_665 10_646 ?
O3 K1 O4 135.42(11) 7_665 . ?
O3 K1 O4 120.89(11) 10_646 . ?
O3 K1 O4 58.50(11) . . ?
O4 K1 O4 98.42(10) 7_665 . ?
O4 K1 O4 98.42(10) 10_646 . ?
O3 K1 N1 61.13(8) 7_665 . ?
O3 K1 N1 61.13(8) 10_646 . ?
O3 K1 N1 61.13(8) . . ?
O4 K1 N1 119.04(8) 7_665 . ?
O4 K1 N1 119.04(8) 10_646 . ?
O4 K1 N1 119.04(8) . . ?
O3 K1 N2 118.87(8) 7_665 . ?
O3 K1 N2 118.87(8) 10_646 . ?
O3 K1 N2 118.87(8) . . ?
O4 K1 N2 60.96(8) 7_665 . ?
O4 K1 N2 60.96(8) 10_646 . ?
O4 K1 N2 60.96(8) . . ?
N1 K1 N2 180.00(10) . . ?
C23 O3 C24 112.5(4) . . ?
C23 O3 K1 119.7(3) . . ?
C24 O3 K1 118.6(3) . . ?
C25 O4 C26 110.4(4) . . ?
C25 O4 K1 117.7(3) . . ?
C26 O4 K1 116.3(3) . . ?
C22 N1 C22 109.4(4) . 7_665 ?
C22 N1 C22 109.4(4) . 10_646 ?
C22 N1 C22 109.4(4) 7_665 10_646 ?
C22 N1 K1 109.5(4) . . ?
C22 N1 K1 109.5(4) 7_665 . ?
C22 N1 K1 109.5(4) 10_646 . ?
C27 N2 C27 109.8(3) 7_665 10_646 ?
C27 N2 C27 109.8(3) 7_665 . ?
C27 N2 C27 109.8(3) 10_646 . ?
C27 N2 K1 109.1(3) 7_665 . ?
C27 N2 K1 109.1(3) 10_646 . ?
C27 N2 K1 109.1(3) . . ?
N1 C22 C23 114.2(5) . . ?
O3 C23 C22 110.1(4) . . ?
O3 C24 C25 109.2(4) . . ?
O4 C25 C24 108.8(4) . . ?
O4 C26 C27 109.1(4) . . ?
N2 C27 C26 114.3(4) . . ?
O5 C28 C29 128(2) . . ?

_refine_diff_density_max         0.543
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_ctp63
_database_code_depnum_ccdc_archive 'CCDC 1538989'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C63 H75 Gd O3'
_chemical_formula_weight         1037.48

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'
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'

_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                   12.812(3)
_cell_length_b                   15.716(3)
_cell_length_c                   29.962(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.129(2)
_cell_angle_gamma                90
_cell_volume                     5998(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9972
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      26.15

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_F_000             2164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.031
_exptl_absorpt_coefficient_mu    1.145
_shelx_estimated_absorpt_T_min   0.704
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_correction_T_max  0.8013
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62895
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.884
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12284
_reflns_number_gt                9267
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A colorless crystal of approximate dimensions 0.031 x 0.062 x 0.330 mm was mounted 
in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  The APEX2 
program package was used to determine the unit-cell parameters and for data collection 
(90 sec/frame scan time for a sphere of diffraction data).  The raw frame data was 
processed using SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  The diffraction symmetry 
was 2/m and the systematic absences were consistent with the monoclinic space group 
P21/c that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms were 
used throughout the analysis.  Hydrogen atoms were included using a riding model.

At convergence, wR2 = 0.0766 and Goof = 1.014 for 610 variables refined against 12284 
data (0.80Å), R1 = 0.0339 for those 9267 data with I > 2.0sigma(I).  

There were several high residuals present in the final difference-Fourier map.  It was 
not possible to determine the nature of the residuals although it was probable that 
diethyether or hexane solvents were present.  The SQUEEZE routine 
in the PLATON program package was used to account for the electrons in the solvent 
accessible voids.  
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12284
_refine_ls_number_parameters     610
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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 0.56415(2) 0.31532(2) 0.31361(2) 0.01614(5) Uani 1 1 d . . . . .
O1 O 0.39744(15) 0.32518(12) 0.30965(7) 0.0209(4) Uani 1 1 d . . . . .
O2 O 0.64152(15) 0.43333(12) 0.30452(7) 0.0192(4) Uani 1 1 d . . . . .
O3 O 0.63777(16) 0.22764(12) 0.36136(7) 0.0215(5) Uani 1 1 d . . . . .
C1 C 0.5564(2) 0.16719(17) 0.26222(10) 0.0188(7) Uani 1 1 d . . . . .
C2 C 0.4828(2) 0.22306(18) 0.23920(10) 0.0192(7) Uani 1 1 d . . . . .
C3 C 0.5186(2) 0.29757(17) 0.21881(10) 0.0187(7) Uani 1 1 d . . . . .
C4 C 0.6257(2) 0.32103(17) 0.22663(9) 0.0177(6) Uani 1 1 d . . . . .
C5 C 0.6987(2) 0.26601(17) 0.25055(10) 0.0180(6) Uani 1 1 d . . . . .
C6 C 0.6644(2) 0.18952(18) 0.26922(10) 0.0191(6) Uani 1 1 d . . . . .
C7 C 0.5197(2) 0.08191(17) 0.27800(10) 0.0232(7) Uani 1 1 d . . . . .
H7A H 0.4653 0.0591 0.2557 0.035 Uiso 1 1 calc R U . . .
H7B H 0.4908 0.0890 0.3068 0.035 Uiso 1 1 calc R U . . .
H7C H 0.5791 0.0424 0.2818 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4434(2) 0.34826(18) 0.18679(11) 0.0232(7) Uani 1 1 d . . . . .
H8A H 0.3849 0.3118 0.1749 0.035 Uiso 1 1 calc R U . . .
H8B H 0.4802 0.3693 0.1620 0.035 Uiso 1 1 calc R U . . .
H8C H 0.4163 0.3965 0.2028 0.035 Uiso 1 1 calc R U . . .
C9 C 0.8153(2) 0.28715(19) 0.25465(11) 0.0254(7) Uani 1 1 d . . . . .
H9A H 0.8283 0.3304 0.2323 0.038 Uiso 1 1 calc R U . . .
H9B H 0.8554 0.2356 0.2494 0.038 Uiso 1 1 calc R U . . .
H9C H 0.8372 0.3091 0.2848 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3655(2) 0.20392(18) 0.23851(11) 0.0233(7) Uani 1 1 d . . . . .
H10A H 0.3420 0.1763 0.2095 0.028 Uiso 1 1 calc R U . . .
H10B H 0.3571 0.1616 0.2623 0.028 Uiso 1 1 calc R U . . .
C11 C 0.2905(2) 0.27747(19) 0.24474(10) 0.0218(7) Uani 1 1 d . . . . .
C12 C 0.3084(2) 0.33383(17) 0.28152(10) 0.0189(7) Uani 1 1 d . . . . .
C13 C 0.2334(2) 0.39873(18) 0.28797(10) 0.0191(6) Uani 1 1 d . . . . .
C14 C 0.1442(2) 0.4032(2) 0.25736(10) 0.0245(7) Uani 1 1 d . . . . .
H14A H 0.0935 0.4458 0.2615 0.029 Uiso 1 1 calc R U . . .
C15 C 0.1253(2) 0.3480(2) 0.22076(11) 0.0237(7) Uani 1 1 d . . . . .
C16 C 0.1999(2) 0.28587(19) 0.21499(11) 0.0240(7) Uani 1 1 d . . . . .
H16A H 0.1888 0.2482 0.1901 0.029 Uiso 1 1 calc R U . . .
C17 C 0.0283(3) 0.3578(2) 0.18733(11) 0.0311(8) Uani 1 1 d . . . . .
H17A H -0.0236 0.3930 0.2005 0.047 Uiso 1 1 calc R U . . .
H17B H -0.0019 0.3016 0.1799 0.047 Uiso 1 1 calc R U . . .
H17C H 0.0476 0.3851 0.1600 0.047 Uiso 1 1 calc R U . . .
C18 C 0.2517(2) 0.46261(18) 0.32712(10) 0.0205(7) Uani 1 1 d . . . . .
C19 C 0.2637(2) 0.41557(19) 0.37299(10) 0.0228(7) Uani 1 1 d . . . . .
H19A H 0.1987 0.3833 0.3765 0.027 Uiso 1 1 calc R U . . .
H19B H 0.3225 0.3745 0.3737 0.027 Uiso 1 1 calc R U . . .
C20 C 0.2849(2) 0.4790(2) 0.41185(10) 0.0258(7) Uani 1 1 d . . . . .
H20A H 0.2942 0.4474 0.4410 0.031 Uiso 1 1 calc R U . . .
C21 C 0.3855(2) 0.5303(2) 0.40603(10) 0.0268(7) Uani 1 1 d . . . . .
H21A H 0.3999 0.5705 0.4314 0.032 Uiso 1 1 calc R U . . .
H21B H 0.4460 0.4911 0.4062 0.032 Uiso 1 1 calc R U . . .
C22 C 0.3720(2) 0.57978(19) 0.36179(10) 0.0239(7) Uani 1 1 d . . . . .
H22A H 0.4373 0.6128 0.3583 0.029 Uiso 1 1 calc R U . . .
C23 C 0.2785(2) 0.64128(19) 0.36200(11) 0.0270(7) Uani 1 1 d . . . . .
H23A H 0.2917 0.6821 0.3872 0.032 Uiso 1 1 calc R U . . .
H23B H 0.2695 0.6739 0.3336 0.032 Uiso 1 1 calc R U . . .
C24 C 0.1788(3) 0.5895(2) 0.36724(10) 0.0273(8) Uani 1 1 d . . . . .
H24A H 0.1174 0.6289 0.3669 0.033 Uiso 1 1 calc R U . . .
C25 C 0.1594(2) 0.52564(19) 0.32811(10) 0.0225(7) Uani 1 1 d . . . . .
H25A H 0.1496 0.5572 0.2994 0.027 Uiso 1 1 calc R U . . .
H25B H 0.0941 0.4935 0.3312 0.027 Uiso 1 1 calc R U . . .
C26 C 0.3512(2) 0.51677(18) 0.32272(10) 0.0208(7) Uani 1 1 d . . . . .
H26A H 0.4126 0.4786 0.3221 0.025 Uiso 1 1 calc R U . . .
H26B H 0.3423 0.5486 0.2940 0.025 Uiso 1 1 calc R U . . .
C27 C 0.1924(3) 0.5414(2) 0.41198(11) 0.0299(8) Uani 1 1 d . . . . .
H27A H 0.1274 0.5098 0.4162 0.036 Uiso 1 1 calc R U . . .
H27B H 0.2063 0.5822 0.4371 0.036 Uiso 1 1 calc R U . . .
C28 C 0.6592(2) 0.40852(17) 0.20990(10) 0.0198(7) Uani 1 1 d . . . . .
H28A H 0.6939 0.3989 0.1823 0.024 Uiso 1 1 calc R U . . .
H28B H 0.5945 0.4415 0.2010 0.024 Uiso 1 1 calc R U . . .
C29 C 0.7318(2) 0.46476(17) 0.24105(10) 0.0180(6) Uani 1 1 d . . . . .
C30 C 0.7208(2) 0.47399(16) 0.28717(10) 0.0170(6) Uani 1 1 d . . . . .
C31 C 0.7937(2) 0.52489(17) 0.31476(10) 0.0166(6) Uani 1 1 d . . . . .
C32 C 0.8700(2) 0.56851(18) 0.29366(11) 0.0215(7) Uani 1 1 d . . . . .
H32A H 0.9197 0.6022 0.3117 0.026 Uiso 1 1 calc R U . . .
C33 C 0.8767(2) 0.56510(19) 0.24769(11) 0.0241(7) Uani 1 1 d . . . . .
C34 C 0.8083(2) 0.51166(18) 0.22221(11) 0.0216(7) Uani 1 1 d . . . . .
H34A H 0.8136 0.5068 0.1909 0.026 Uiso 1 1 calc R U . . .
C35 C 0.9566(3) 0.6188(2) 0.22642(12) 0.0340(8) Uani 1 1 d . . . . .
H35A H 1.0234 0.6184 0.2457 0.051 Uiso 1 1 calc R U . . .
H35B H 0.9308 0.6774 0.2229 0.051 Uiso 1 1 calc R U . . .
H35C H 0.9672 0.5953 0.1969 0.051 Uiso 1 1 calc R U . . .
C36 C 0.7895(2) 0.53109(18) 0.36578(10) 0.0192(7) Uani 1 1 d . . . . .
C37 C 0.8018(2) 0.44123(19) 0.38768(10) 0.0249(7) Uani 1 1 d . . . . .
H37A H 0.7461 0.4032 0.3736 0.030 Uiso 1 1 calc R U . . .
H37B H 0.8705 0.4169 0.3822 0.030 Uiso 1 1 calc R U . . .
C38 C 0.7944(2) 0.4457(2) 0.43861(11) 0.0307(8) Uani 1 1 d . . . . .
H38A H 0.8004 0.3871 0.4517 0.037 Uiso 1 1 calc R U . . .
C39 C 0.8840(3) 0.5015(2) 0.46033(12) 0.0406(9) Uani 1 1 d . . . . .
H39A H 0.8805 0.5047 0.4931 0.049 Uiso 1 1 calc R U . . .
H39B H 0.9524 0.4765 0.4550 0.049 Uiso 1 1 calc R U . . .
C40 C 0.8739(3) 0.5908(2) 0.44003(12) 0.0374(9) Uani 1 1 d . . . . .
H40A H 0.9330 0.6268 0.4540 0.045 Uiso 1 1 calc R U . . .
C41 C 0.7697(3) 0.6306(2) 0.44969(12) 0.0364(9) Uani 1 1 d . . . . .
H41A H 0.7639 0.6891 0.4373 0.044 Uiso 1 1 calc R U . . .
H41B H 0.7663 0.6338 0.4825 0.044 Uiso 1 1 calc R U . . .
C42 C 0.6792(3) 0.5753(2) 0.42773(10) 0.0277(8) Uani 1 1 d . . . . .
H42A H 0.6106 0.6007 0.4339 0.033 Uiso 1 1 calc R U . . .
C43 C 0.6848(2) 0.57168(18) 0.37664(10) 0.0206(7) Uani 1 1 d . . . . .
H43A H 0.6789 0.6300 0.3641 0.025 Uiso 1 1 calc R U . . .
H43B H 0.6252 0.5378 0.3624 0.025 Uiso 1 1 calc R U . . .
C44 C 0.8796(2) 0.5865(2) 0.38925(10) 0.0274(7) Uani 1 1 d . . . . .
H44A H 0.9481 0.5623 0.3833 0.033 Uiso 1 1 calc R U . . .
H44B H 0.8747 0.6448 0.3766 0.033 Uiso 1 1 calc R U . . .
C45 C 0.6882(3) 0.4851(2) 0.44707(11) 0.0283(8) Uani 1 1 d . . . . .
H45A H 0.6302 0.4495 0.4328 0.034 Uiso 1 1 calc R U . . .
H45B H 0.6823 0.4870 0.4797 0.034 Uiso 1 1 calc R U . . .
C46 C 0.7441(2) 0.13392(18) 0.29730(10) 0.0220(7) Uani 1 1 d . . . . .
H46A H 0.8089 0.1679 0.3041 0.026 Uiso 1 1 calc R U . . .
H46B H 0.7617 0.0857 0.2782 0.026 Uiso 1 1 calc R U . . .
C47 C 0.7155(2) 0.09701(18) 0.34156(10) 0.0205(7) Uani 1 1 d . . . . .
C48 C 0.6649(2) 0.14621(19) 0.37202(10) 0.0217(7) Uani 1 1 d . . . . .
C49 C 0.6402(2) 0.10938(18) 0.41298(10) 0.0241(7) Uani 1 1 d . . . . .
C50 C 0.6740(3) 0.02568(19) 0.42202(11) 0.0280(8) Uani 1 1 d . . . . .
H50A H 0.6596 0.0008 0.4496 0.034 Uiso 1 1 calc R U . . .
C51 C 0.7274(3) -0.02326(19) 0.39316(11) 0.0278(8) Uani 1 1 d . . . . .
C52 C 0.7465(2) 0.01377(19) 0.35269(11) 0.0251(7) Uani 1 1 d . . . . .
H52A H 0.7816 -0.0184 0.3320 0.030 Uiso 1 1 calc R U . . .
C53 C 0.7620(3) -0.1133(2) 0.40530(12) 0.0382(9) Uani 1 1 d . . . . .
H53A H 0.7008 -0.1473 0.4111 0.057 Uiso 1 1 calc R U . . .
H53B H 0.8125 -0.1123 0.4323 0.057 Uiso 1 1 calc R U . . .
H53C H 0.7951 -0.1385 0.3804 0.057 Uiso 1 1 calc R U . . .
C54 C 0.5779(3) 0.15888(19) 0.44577(10) 0.0259(7) Uani 1 1 d . . . . .
C55 C 0.6396(3) 0.23982(19) 0.46298(11) 0.0284(8) Uani 1 1 d . . . . .
H55A H 0.7081 0.2231 0.4790 0.034 Uiso 1 1 calc R U . . .
H55B H 0.6532 0.2760 0.4372 0.034 Uiso 1 1 calc R U . . .
C56 C 0.5756(3) 0.2906(2) 0.49495(11) 0.0330(9) Uani 1 1 d . . . . .
H56A H 0.6153 0.3431 0.5051 0.040 Uiso 1 1 calc R U . . .
C57 C 0.5599(3) 0.2359(2) 0.53581(11) 0.0394(9) Uani 1 1 d . . . . .
H57A H 0.5212 0.2685 0.5570 0.047 Uiso 1 1 calc R U . . .
H57B H 0.6288 0.2192 0.5515 0.047 Uiso 1 1 calc R U . . .
C58 C 0.4970(3) 0.1562(2) 0.51978(11) 0.0367(9) Uani 1 1 d . . . . .
H58A H 0.4869 0.1196 0.5463 0.044 Uiso 1 1 calc R U . . .
C59 C 0.3895(3) 0.1811(2) 0.49604(12) 0.0408(9) Uani 1 1 d . . . . .
H59A H 0.3493 0.2135 0.5168 0.049 Uiso 1 1 calc R U . . .
H59B H 0.3491 0.1293 0.4864 0.049 Uiso 1 1 calc R U . . .
C60 C 0.4063(3) 0.2362(2) 0.45481(11) 0.0347(9) Uani 1 1 d . . . . .
H60A H 0.3368 0.2531 0.4390 0.042 Uiso 1 1 calc R U . . .
C61 C 0.4681(2) 0.1843(2) 0.42270(11) 0.0289(7) Uani 1 1 d . . . . .
H61A H 0.4765 0.2185 0.3956 0.035 Uiso 1 1 calc R U . . .
H61B H 0.4282 0.1323 0.4132 0.035 Uiso 1 1 calc R U . . .
C62 C 0.5596(3) 0.1059(2) 0.48723(11) 0.0325(8) Uani 1 1 d . . . . .
H62A H 0.6282 0.0888 0.5031 0.039 Uiso 1 1 calc R U . . .
H62B H 0.5206 0.0535 0.4776 0.039 Uiso 1 1 calc R U . . .
C63 C 0.4691(3) 0.3160(2) 0.47011(12) 0.0382(9) Uani 1 1 d . . . . .
H63A H 0.4291 0.3501 0.4903 0.046 Uiso 1 1 calc R U . . .
H63B H 0.4803 0.3514 0.4437 0.046 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 Cnt 2.413 . ?
Gd1 O1 2.1320(19) . ?
Gd1 O3 2.132(2) . ?
Gd1 O2 2.1339(19) . ?
Gd1 C2 2.768(3) . ?
Gd1 C6 2.774(3) . ?
Gd1 C1 2.787(3) . ?
Gd1 C5 2.800(3) . ?
Gd1 C4 2.804(3) . ?
Gd1 C3 2.852(3) . ?
O1 C12 1.350(4) . ?
O2 C30 1.350(3) . ?
O3 C48 1.355(3) . ?
C1 C2 1.413(4) . ?
C1 C6 1.422(4) . ?
C1 C7 1.513(4) . ?
C2 C3 1.419(4) . ?
C2 C10 1.532(4) . ?
C3 C4 1.415(4) . ?
C3 C8 1.512(4) . ?
C4 C5 1.412(4) . ?
C4 C28 1.540(4) . ?
C5 C6 1.415(4) . ?
C5 C9 1.522(4) . ?
C6 C46 1.526(4) . ?
C10 C11 1.527(4) . ?
C11 C16 1.393(4) . ?
C11 C12 1.414(4) . ?
C12 C13 1.428(4) . ?
C13 C14 1.389(4) . ?
C13 C18 1.542(4) . ?
C14 C15 1.399(4) . ?
C15 C16 1.389(4) . ?
C15 C17 1.519(4) . ?
C18 C25 1.545(4) . ?
C18 C26 1.551(4) . ?
C18 C19 1.554(4) . ?
C19 C20 1.535(4) . ?
C20 C27 1.538(4) . ?
C20 C21 1.546(4) . ?
C21 C22 1.530(4) . ?
C22 C26 1.534(4) . ?
C22 C23 1.539(4) . ?
C23 C24 1.537(4) . ?
C24 C27 1.532(4) . ?
C24 C25 1.543(4) . ?
C28 C29 1.527(4) . ?
C29 C34 1.393(4) . ?
C29 C30 1.412(4) . ?
C30 C31 1.425(4) . ?
C31 C32 1.399(4) . ?
C31 C36 1.538(4) . ?
C32 C33 1.390(4) . ?
C33 C34 1.384(4) . ?
C33 C35 1.518(4) . ?
C36 C43 1.551(4) . ?
C36 C44 1.553(4) . ?
C36 C37 1.558(4) . ?
C37 C38 1.540(4) . ?
C38 C39 1.534(5) . ?
C38 C45 1.541(4) . ?
C39 C40 1.528(5) . ?
C40 C41 1.530(5) . ?
C40 C44 1.532(4) . ?
C41 C42 1.541(4) . ?
C42 C45 1.530(4) . ?
C42 C43 1.541(4) . ?
C46 C47 1.528(4) . ?
C47 C52 1.397(4) . ?
C47 C48 1.406(4) . ?
C48 C49 1.423(4) . ?
C49 C50 1.402(4) . ?
C49 C54 1.541(4) . ?
C50 C51 1.390(4) . ?
C51 C52 1.390(4) . ?
C51 C53 1.515(4) . ?
C54 C62 1.534(4) . ?
C54 C61 1.552(5) . ?
C54 C55 1.556(4) . ?
C55 C56 1.547(4) . ?
C56 C57 1.526(4) . ?
C56 C63 1.536(5) . ?
C57 C58 1.538(5) . ?
C58 C59 1.533(5) . ?
C58 C62 1.544(4) . ?
C59 C60 1.543(5) . ?
C60 C63 1.534(5) . ?
C60 C61 1.543(4) . ?

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
Cnt Gd1 O1 102.7 . . ?
Cnt Gd1 O2 100.5 . . ?
Cnt Gd1 O3 100.5 . . ?
O1 Gd1 O3 116.94(8) . . ?
O1 Gd1 O2 113.95(7) . . ?
O3 Gd1 O2 117.97(8) . . ?
O1 Gd1 C2 72.82(8) . . ?
O3 Gd1 C2 107.66(8) . . ?
O2 Gd1 C2 119.50(8) . . ?
O1 Gd1 C6 122.52(8) . . ?
O3 Gd1 C6 70.53(8) . . ?
O2 Gd1 C6 108.24(8) . . ?
C2 Gd1 C6 52.71(9) . . ?
O1 Gd1 C1 93.07(8) . . ?
O3 Gd1 C1 79.51(8) . . ?
O2 Gd1 C1 130.17(8) . . ?
C2 Gd1 C1 29.46(9) . . ?
C6 Gd1 C1 29.62(8) . . ?
O1 Gd1 C5 131.91(8) . . ?
O3 Gd1 C5 90.79(8) . . ?
O2 Gd1 C5 80.01(7) . . ?
C2 Gd1 C5 61.14(9) . . ?
C6 Gd1 C5 29.42(8) . . ?
C1 Gd1 C5 51.99(8) . . ?
O1 Gd1 C4 108.98(8) . . ?
O3 Gd1 C4 119.75(8) . . ?
O2 Gd1 C4 70.92(8) . . ?
C2 Gd1 C4 52.20(8) . . ?
C6 Gd1 C4 52.15(8) . . ?
C1 Gd1 C4 60.67(8) . . ?
C5 Gd1 C4 29.19(8) . . ?
O1 Gd1 C3 81.63(8) . . ?
O3 Gd1 C3 129.33(8) . . ?
O2 Gd1 C3 90.36(8) . . ?
C2 Gd1 C3 29.21(8) . . ?
C6 Gd1 C3 60.57(8) . . ?
C1 Gd1 C3 51.43(8) . . ?
C5 Gd1 C3 51.39(9) . . ?
C4 Gd1 C3 28.97(8) . . ?
C12 O1 Gd1 144.71(18) . . ?
C30 O2 Gd1 147.07(17) . . ?
C48 O3 Gd1 148.45(19) . . ?
C2 C1 C6 120.4(2) . . ?
C2 C1 C7 119.3(3) . . ?
C6 C1 C7 120.2(3) . . ?
C2 C1 Gd1 74.52(16) . . ?
C6 C1 Gd1 74.66(15) . . ?
C7 C1 Gd1 124.14(19) . . ?
C1 C2 C3 119.6(3) . . ?
C1 C2 C10 119.2(2) . . ?
C3 C2 C10 121.2(3) . . ?
C1 C2 Gd1 76.02(17) . . ?
C3 C2 Gd1 78.67(17) . . ?
C10 C2 Gd1 113.47(18) . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 C8 120.6(2) . . ?
C2 C3 C8 119.6(3) . . ?
C4 C3 Gd1 73.62(16) . . ?
C2 C3 Gd1 72.12(17) . . ?
C8 C3 Gd1 128.98(18) . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 C28 121.2(3) . . ?
C3 C4 C28 118.5(3) . . ?
C5 C4 Gd1 75.26(16) . . ?
C3 C4 Gd1 77.41(16) . . ?
C28 C4 Gd1 116.55(17) . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 C9 119.9(2) . . ?
C6 C5 C9 119.8(3) . . ?
C4 C5 Gd1 75.54(15) . . ?
C6 C5 Gd1 74.26(15) . . ?
C9 C5 Gd1 123.69(19) . . ?
C5 C6 C1 119.3(3) . . ?
C5 C6 C46 119.1(3) . . ?
C1 C6 C46 121.5(3) . . ?
C5 C6 Gd1 76.32(16) . . ?
C1 C6 Gd1 75.72(15) . . ?
C46 C6 Gd1 117.43(18) . . ?
C11 C10 C2 118.6(2) . . ?
C16 C11 C12 119.6(3) . . ?
C16 C11 C10 119.1(3) . . ?
C12 C11 C10 121.2(3) . . ?
O1 C12 C11 118.6(3) . . ?
O1 C12 C13 121.5(3) . . ?
C11 C12 C13 119.8(3) . . ?
C14 C13 C12 117.7(3) . . ?
C14 C13 C18 121.1(3) . . ?
C12 C13 C18 121.2(3) . . ?
C13 C14 C15 123.2(3) . . ?
C16 C15 C14 118.0(3) . . ?
C16 C15 C17 121.0(3) . . ?
C14 C15 C17 121.0(3) . . ?
C15 C16 C11 121.6(3) . . ?
C13 C18 C25 112.2(2) . . ?
C13 C18 C26 110.6(2) . . ?
C25 C18 C26 106.7(2) . . ?
C13 C18 C19 110.8(2) . . ?
C25 C18 C19 107.0(2) . . ?
C26 C18 C19 109.3(2) . . ?
C20 C19 C18 110.8(2) . . ?
C19 C20 C27 110.0(3) . . ?
C19 C20 C21 109.6(2) . . ?
C27 C20 C21 108.6(3) . . ?
C22 C21 C20 110.1(3) . . ?
C21 C22 C26 109.1(2) . . ?
C21 C22 C23 109.3(2) . . ?
C26 C22 C23 109.7(3) . . ?
C24 C23 C22 108.9(2) . . ?
C27 C24 C23 109.4(3) . . ?
C27 C24 C25 109.8(3) . . ?
C23 C24 C25 109.6(2) . . ?
C24 C25 C18 111.7(2) . . ?
C22 C26 C18 111.5(2) . . ?
C24 C27 C20 109.2(2) . . ?
C29 C28 C4 119.4(2) . . ?
C34 C29 C30 119.4(3) . . ?
C34 C29 C28 117.9(3) . . ?
C30 C29 C28 122.6(2) . . ?
O2 C30 C29 119.1(3) . . ?
O2 C30 C31 121.1(3) . . ?
C29 C30 C31 119.8(3) . . ?
C32 C31 C30 117.3(3) . . ?
C32 C31 C36 121.2(3) . . ?
C30 C31 C36 121.5(2) . . ?
C33 C32 C31 123.3(3) . . ?
C34 C33 C32 117.8(3) . . ?
C34 C33 C35 121.5(3) . . ?
C32 C33 C35 120.7(3) . . ?
C33 C34 C29 122.0(3) . . ?
C31 C36 C43 110.9(2) . . ?
C31 C36 C44 112.5(2) . . ?
C43 C36 C44 107.0(2) . . ?
C31 C36 C37 110.4(2) . . ?
C43 C36 C37 109.6(2) . . ?
C44 C36 C37 106.4(2) . . ?
C38 C37 C36 111.2(3) . . ?
C39 C38 C37 108.9(3) . . ?
C39 C38 C45 109.5(3) . . ?
C37 C38 C45 109.2(3) . . ?
C40 C39 C38 109.2(3) . . ?
C39 C40 C41 109.8(3) . . ?
C39 C40 C44 110.2(3) . . ?
C41 C40 C44 109.9(3) . . ?
C40 C41 C42 108.7(3) . . ?
C45 C42 C41 109.7(3) . . ?
C45 C42 C43 109.4(3) . . ?
C41 C42 C43 109.4(3) . . ?
C42 C43 C36 110.9(2) . . ?
C40 C44 C36 111.2(2) . . ?
C42 C45 C38 110.1(3) . . ?
C6 C46 C47 119.2(2) . . ?
C52 C47 C48 119.9(3) . . ?
C52 C47 C46 118.3(3) . . ?
C48 C47 C46 121.7(3) . . ?
O3 C48 C47 119.4(3) . . ?
O3 C48 C49 120.8(3) . . ?
C47 C48 C49 119.8(3) . . ?
C50 C49 C48 117.1(3) . . ?
C50 C49 C54 121.4(3) . . ?
C48 C49 C54 121.5(3) . . ?
C51 C50 C49 124.1(3) . . ?
C52 C51 C50 117.1(3) . . ?
C52 C51 C53 121.7(3) . . ?
C50 C51 C53 121.2(3) . . ?
C51 C52 C47 121.9(3) . . ?
C62 C54 C49 112.1(2) . . ?
C62 C54 C61 106.9(3) . . ?
C49 C54 C61 110.6(3) . . ?
C62 C54 C55 106.9(3) . . ?
C49 C54 C55 110.2(3) . . ?
C61 C54 C55 110.0(3) . . ?
C56 C55 C54 110.1(3) . . ?
C57 C56 C63 110.4(3) . . ?
C57 C56 C55 109.3(3) . . ?
C63 C56 C55 109.7(3) . . ?
C56 C57 C58 108.5(3) . . ?
C59 C58 C57 110.6(3) . . ?
C59 C58 C62 109.8(3) . . ?
C57 C58 C62 108.9(3) . . ?
C58 C59 C60 108.6(3) . . ?
C63 C60 C61 109.4(3) . . ?
C63 C60 C59 109.5(3) . . ?
C61 C60 C59 109.1(3) . . ?
C60 C61 C54 111.1(3) . . ?
C54 C62 C58 111.6(3) . . ?
C60 C63 C56 110.0(3) . . ?

_refine_diff_density_max         1.333
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.082



####################################################################### 
# 
# 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_ctp71
_database_code_depnum_ccdc_archive 'CCDC 1538994'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C91 H131.50 Dy K O13'
_chemical_formula_weight         1635.05

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_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+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   21.7362(14)
_cell_length_b                   30.6130(19)
_cell_length_c                   25.4472(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     16932.8(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9703
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      25.42

_exptl_crystal_description       rectangular
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             6932
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.128
_exptl_absorpt_coefficient_mu    0.992
_shelx_estimated_absorpt_T_min   0.803
_shelx_estimated_absorpt_T_max   0.884
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            170974
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.149
_diffrn_reflns_theta_max         25.744
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16156
_reflns_number_gt                12496
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A brown crystal of approximate dimensions 0.128 x 0.194 x 0.231 mm was mounted 
in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  The APEX2 
program package was used to determine the unit-cell parameters and for data 
collection (90 sec/frame scan time for a sphere of diffraction data).  The raw frame 
data was processed using SAINT and SADABS to yield the reflection data file.  
Subsequent calculations were carried out using the SHELXTL program.  The diffraction 
symmetry was mmm and the systematic absences were consistent with the orthorhombic 
space group Pbcn that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix least-squares 
techniques.  The analytical scattering factors for neutral atoms were used throughout 
the analysis.  The complex appeared to be a mixed composition of approximately 
Dy2+ (50%) / Dy3+( 50%).  There was approximately 50% of a hydride ligand present which 
was located from a difference-Fourier map and refined (x,y,z and Uiso).  Hydrogen atoms 
were included using a riding model.  There were two molecules of tetrahydrofuran solvent 
present.

Least-squares analysis yielded wR2 = 0.1486 and Goof = 1.101 for 949 variables refined 
against 16156 data (0.82Å), R1 = 0.0583 for those 12496 data with I > 2.0sigma(I).  

There were several high residuals present in the final difference-Fourier map.  It was 
not possible to determine the nature of the residuals although it was probable based on 
the observed geometry that diethylether solvent was present.  The SQUEEZE routine in 
the PLATON program package was used to account for the electrons in the solvent 
accessible voids.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0573P)²+47.6570P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16156
_refine_ls_number_parameters     949
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1486
_refine_ls_wR_factor_gt          0.1389
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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 0.81044(3) 0.10178(3) 0.74684(3) 0.01942(15) Uani 0.5 1 d . . P A 1
Dy2 Dy 0.78588(3) 0.09965(2) 0.74099(3) 0.01758(14) Uani 0.5 1 d . . P A 2
H1 H 0.696(4) 0.093(3) 0.721(4) 0.04(3) Uiso 0.5 1 d . . P . .
O1 O 0.79593(14) 0.03565(10) 0.71668(13) 0.0354(8) Uani 1 1 d . . . . .
O2 O 0.79481(12) 0.15047(9) 0.68618(11) 0.0268(6) Uani 1 1 d . . . . .
O3 O 0.76667(13) 0.11566(10) 0.81980(11) 0.0292(7) Uani 1 1 d . . . . .
C1 C 0.9002(2) 0.08090(15) 0.81214(18) 0.0306(10) Uani 1 1 d . . . . .
C2 C 0.91189(19) 0.05969(15) 0.76421(18) 0.0306(10) Uani 1 1 d . . . . .
C3 C 0.92284(19) 0.08468(15) 0.71820(18) 0.0309(10) Uani 1 1 d . . . . .
C4 C 0.91929(19) 0.13067(15) 0.72053(16) 0.0281(9) Uani 1 1 d . . . . .
C5 C 0.91075(18) 0.15201(14) 0.76930(16) 0.0255(9) Uani 1 1 d . . . . .
C6 C 0.89735(18) 0.12692(14) 0.81424(16) 0.0241(9) Uani 1 1 d . . . . .
C7 C 0.8916(2) 0.05554(16) 0.8625(2) 0.0405(12) Uani 1 1 d . . . . .
H7A H 0.8978 0.0750 0.8926 0.061 Uiso 1 1 calc R U . . .
H7B H 0.9217 0.0317 0.8640 0.061 Uiso 1 1 calc R U . . .
H7C H 0.8499 0.0434 0.8636 0.061 Uiso 1 1 calc R U . . .
C8 C 0.9387(2) 0.06183(17) 0.66744(18) 0.0390(12) Uani 1 1 d . . . . .
H8A H 0.9683 0.0796 0.6476 0.058 Uiso 1 1 calc R U . . .
H8B H 0.9013 0.0578 0.6465 0.058 Uiso 1 1 calc R U . . .
H8C H 0.9570 0.0333 0.6752 0.058 Uiso 1 1 calc R U . . .
C9 C 0.9177(2) 0.20077(14) 0.77326(17) 0.0309(10) Uani 1 1 d . . . . .
H9A H 0.9428 0.2114 0.7439 0.046 Uiso 1 1 calc R U . . .
H9B H 0.9378 0.2082 0.8065 0.046 Uiso 1 1 calc R U . . .
H9C H 0.8770 0.2145 0.7719 0.046 Uiso 1 1 calc R U . . .
C10 C 0.9099(3) 0.01014(17) 0.7647(2) 0.0530(15) Uani 1 1 d . . . . .
H10A H 0.9530 -0.0001 0.7654 0.064 Uiso 1 1 calc R U . . .
H10B H 0.8912 0.0014 0.7986 0.064 Uiso 1 1 calc R U . . .
C11 C 0.8775(2) -0.01538(14) 0.72247(17) 0.0292(10) Uani 1 1 d . . . . .
C12 C 0.8204(2) -0.00257(14) 0.70164(16) 0.0274(9) Uani 1 1 d . . . . .
C13 C 0.78958(19) -0.03041(13) 0.66531(15) 0.0237(9) Uani 1 1 d . . . . .
C14 C 0.8172(2) -0.07034(14) 0.65357(16) 0.0262(9) Uani 1 1 d . . . . .
H14A H 0.7965 -0.0894 0.6301 0.031 Uiso 1 1 calc R U . . .
C15 C 0.8727(2) -0.08375(14) 0.67393(16) 0.0278(9) Uani 1 1 d . . . . .
C16 C 0.9023(2) -0.05586(14) 0.70818(17) 0.0289(9) Uani 1 1 d . . . . .
H16A H 0.9408 -0.0644 0.7225 0.035 Uiso 1 1 calc R U . . .
C17 C 0.8997(2) -0.12759(15) 0.6585(2) 0.0365(11) Uani 1 1 d . . . . .
H17A H 0.8674 -0.1500 0.6598 0.055 Uiso 1 1 calc R U . . .
H17B H 0.9328 -0.1353 0.6829 0.055 Uiso 1 1 calc R U . . .
H17C H 0.9162 -0.1258 0.6227 0.055 Uiso 1 1 calc R U . . .
C18 C 0.72983(18) -0.01649(13) 0.63801(16) 0.0238(9) Uani 1 1 d . . . . .
C19 C 0.67781(18) -0.00665(15) 0.67764(16) 0.0268(9) Uani 1 1 d . . . . .
H19A H 0.6682 -0.0333 0.6980 0.032 Uiso 1 1 calc R U . . .
H19B H 0.6915 0.0162 0.7025 0.032 Uiso 1 1 calc R U . . .
C20 C 0.6198(2) 0.00893(15) 0.64861(18) 0.0321(10) Uani 1 1 d . . . . .
H20A H 0.5869 0.0159 0.6748 0.039 Uiso 1 1 calc R U . . .
C21 C 0.6342(2) 0.04931(15) 0.61644(19) 0.0354(11) Uani 1 1 d . . . . .
H21A H 0.6485 0.0730 0.6400 0.042 Uiso 1 1 calc R U . . .
H21B H 0.5965 0.0595 0.5984 0.042 Uiso 1 1 calc R U . . .
C22 C 0.6839(2) 0.03946(16) 0.57567(19) 0.0366(11) Uani 1 1 d . . . . .
H22A H 0.6929 0.0663 0.5547 0.044 Uiso 1 1 calc R U . . .
C23 C 0.6614(2) 0.00293(16) 0.53909(17) 0.0363(11) Uani 1 1 d . . . . .
H23A H 0.6239 0.0125 0.5202 0.044 Uiso 1 1 calc R U . . .
H23B H 0.6935 -0.0039 0.5127 0.044 Uiso 1 1 calc R U . . .
C24 C 0.6473(2) -0.03730(15) 0.57160(17) 0.0337(10) Uani 1 1 d . . . . .
H24A H 0.6330 -0.0613 0.5478 0.040 Uiso 1 1 calc R U . . .
C25 C 0.7061(2) -0.05202(15) 0.60018(17) 0.0292(9) Uani 1 1 d . . . . .
H25A H 0.7383 -0.0588 0.5739 0.035 Uiso 1 1 calc R U . . .
H25B H 0.6974 -0.0790 0.6203 0.035 Uiso 1 1 calc R U . . .
C26 C 0.7422(2) 0.02459(15) 0.60453(17) 0.0300(10) Uani 1 1 d . . . . .
H26A H 0.7570 0.0485 0.6275 0.036 Uiso 1 1 calc R U . . .
H26B H 0.7749 0.0182 0.5786 0.036 Uiso 1 1 calc R U . . .
C27 C 0.5969(2) -0.02714(16) 0.61144(18) 0.0339(11) Uani 1 1 d . . . . .
H27A H 0.5867 -0.0537 0.6318 0.041 Uiso 1 1 calc R U . . .
H27B H 0.5592 -0.0173 0.5930 0.041 Uiso 1 1 calc R U . . .
C28 C 0.9237(2) 0.15719(16) 0.66991(17) 0.0329(10) Uani 1 1 d . . . . .
H28A H 0.9179 0.1369 0.6400 0.039 Uiso 1 1 calc R U . . .
H28B H 0.9660 0.1689 0.6673 0.039 Uiso 1 1 calc R U . . .
C29 C 0.87895(19) 0.19530(15) 0.66281(15) 0.0287(10) Uani 1 1 d . . . . .
C30 C 0.8153(2) 0.18936(14) 0.66963(15) 0.0251(9) Uani 1 1 d . . . . .
C31 C 0.77415(19) 0.22446(14) 0.65893(15) 0.0246(9) Uani 1 1 d . . . . .
C32 C 0.7996(2) 0.26437(14) 0.64403(15) 0.0282(9) Uani 1 1 d . . . . .
H32A H 0.7726 0.2881 0.6373 0.034 Uiso 1 1 calc R U . . .
C33 C 0.8625(2) 0.27135(15) 0.63843(16) 0.0325(10) Uani 1 1 d . . . . .
C34 C 0.9009(2) 0.23597(16) 0.64714(17) 0.0344(11) Uani 1 1 d . . . . .
H34A H 0.9439 0.2396 0.6422 0.041 Uiso 1 1 calc R U . . .
C35 C 0.8878(2) 0.31547(17) 0.6230(2) 0.0462(13) Uani 1 1 d . . . . .
H35A H 0.8757 0.3373 0.6492 0.069 Uiso 1 1 calc R U . . .
H35B H 0.8713 0.3238 0.5885 0.069 Uiso 1 1 calc R U . . .
H35C H 0.9328 0.3140 0.6211 0.069 Uiso 1 1 calc R U . . .
C36 C 0.70402(19) 0.21897(13) 0.66328(15) 0.0225(9) Uani 1 1 d . . . . .
C37 C 0.68467(19) 0.21248(14) 0.72116(15) 0.0248(9) Uani 1 1 d . . . . .
H37A H 0.7059 0.1865 0.7357 0.030 Uiso 1 1 calc R U . . .
H37B H 0.6974 0.2382 0.7420 0.030 Uiso 1 1 calc R U . . .
C38 C 0.61509(19) 0.20632(14) 0.72601(16) 0.0274(9) Uani 1 1 d . . . . .
H38A H 0.6040 0.2018 0.7638 0.033 Uiso 1 1 calc R U . . .
C39 C 0.5822(2) 0.24666(14) 0.70532(17) 0.0301(10) Uani 1 1 d . . . . .
H39A H 0.5945 0.2726 0.7261 0.036 Uiso 1 1 calc R U . . .
H39B H 0.5372 0.2429 0.7089 0.036 Uiso 1 1 calc R U . . .
C40 C 0.5989(2) 0.25353(14) 0.64738(17) 0.0283(9) Uani 1 1 d . . . . .
H40A H 0.5778 0.2803 0.6339 0.034 Uiso 1 1 calc R U . . .
C41 C 0.5783(2) 0.21389(14) 0.61546(16) 0.0277(9) Uani 1 1 d . . . . .
H41A H 0.5333 0.2098 0.6191 0.033 Uiso 1 1 calc R U . . .
H41B H 0.5879 0.2184 0.5778 0.033 Uiso 1 1 calc R U . . .
C42 C 0.61203(19) 0.17354(13) 0.63580(16) 0.0242(9) Uani 1 1 d . . . . .
H42A H 0.5989 0.1475 0.6149 0.029 Uiso 1 1 calc R U . . .
C43 C 0.68114(18) 0.17949(13) 0.63032(15) 0.0223(8) Uani 1 1 d . . . . .
H43A H 0.6916 0.1842 0.5929 0.027 Uiso 1 1 calc R U . . .
H43B H 0.7023 0.1526 0.6422 0.027 Uiso 1 1 calc R U . . .
C44 C 0.66871(19) 0.25936(13) 0.64286(16) 0.0264(9) Uani 1 1 d . . . . .
H44A H 0.6814 0.2854 0.6633 0.032 Uiso 1 1 calc R U . . .
H44B H 0.6797 0.2645 0.6056 0.032 Uiso 1 1 calc R U . . .
C45 C 0.59521(19) 0.16628(14) 0.69383(16) 0.0262(9) Uani 1 1 d . . . . .
H45A H 0.5503 0.1619 0.6973 0.031 Uiso 1 1 calc R U . . .
H45B H 0.6162 0.1398 0.7072 0.031 Uiso 1 1 calc R U . . .
C46 C 0.8809(2) 0.14988(16) 0.86449(17) 0.0355(11) Uani 1 1 d . . . . .
H46A H 0.8776 0.1814 0.8563 0.043 Uiso 1 1 calc R U . . .
H46B H 0.9163 0.1465 0.8886 0.043 Uiso 1 1 calc R U . . .
C47 C 0.8236(2) 0.13745(13) 0.89500(16) 0.0263(9) Uani 1 1 d . . . . .
C48 C 0.76943(19) 0.12131(13) 0.87194(15) 0.0240(9) Uani 1 1 d . . . . .
C49 C 0.7176(2) 0.11229(13) 0.90426(16) 0.0256(9) Uani 1 1 d . . . . .
C50 C 0.7215(2) 0.12196(14) 0.95777(16) 0.0285(10) Uani 1 1 d . . . . .
H50A H 0.6869 0.1160 0.9795 0.034 Uiso 1 1 calc R U . . .
C51 C 0.7738(2) 0.13991(14) 0.98051(16) 0.0315(10) Uani 1 1 d . . . . .
C52 C 0.8247(2) 0.14659(14) 0.94852(16) 0.0296(10) Uani 1 1 d . . . . .
H52A H 0.8614 0.1578 0.9637 0.035 Uiso 1 1 calc R U . . .
C53 C 0.7753(3) 0.15328(17) 1.03736(18) 0.0449(13) Uani 1 1 d . . . . .
H53A H 0.7408 0.1396 1.0560 0.067 Uiso 1 1 calc R U . . .
H53B H 0.7718 0.1851 1.0399 0.067 Uiso 1 1 calc R U . . .
H53C H 0.8142 0.1438 1.0532 0.067 Uiso 1 1 calc R U . . .
C54 C 0.65791(19) 0.09363(14) 0.88111(17) 0.0269(9) Uani 1 1 d . . . . .
C55 C 0.62861(19) 0.12630(14) 0.84163(16) 0.0267(9) Uani 1 1 d . . . . .
H55A H 0.6183 0.1538 0.8601 0.032 Uiso 1 1 calc R U . . .
H55B H 0.6586 0.1332 0.8135 0.032 Uiso 1 1 calc R U . . .
C56 C 0.5702(2) 0.10691(16) 0.81719(18) 0.0338(11) Uani 1 1 d . . . . .
H56A H 0.5525 0.1282 0.7915 0.041 Uiso 1 1 calc R U . . .
C57 C 0.5230(2) 0.09775(18) 0.8605(2) 0.0409(12) Uani 1 1 d . . . . .
H57A H 0.4849 0.0857 0.8449 0.049 Uiso 1 1 calc R U . . .
H57B H 0.5126 0.1252 0.8789 0.049 Uiso 1 1 calc R U . . .
C58 C 0.5504(2) 0.06479(17) 0.8996(2) 0.0431(13) Uani 1 1 d . . . . .
H58A H 0.5199 0.0589 0.9282 0.052 Uiso 1 1 calc R U . . .
C59 C 0.5647(2) 0.02242(17) 0.8708(2) 0.0468(14) Uani 1 1 d . . . . .
H59A H 0.5812 0.0006 0.8958 0.056 Uiso 1 1 calc R U . . .
H59B H 0.5266 0.0105 0.8550 0.056 Uiso 1 1 calc R U . . .
C60 C 0.6119(2) 0.03136(16) 0.8279(2) 0.0377(11) Uani 1 1 d . . . . .
H60A H 0.6220 0.0035 0.8092 0.045 Uiso 1 1 calc R U . . .
C61 C 0.6705(2) 0.05007(14) 0.85306(18) 0.0302(10) Uani 1 1 d . . . . .
H61A H 0.7020 0.0546 0.8255 0.036 Uiso 1 1 calc R U . . .
H61B H 0.6870 0.0288 0.8787 0.036 Uiso 1 1 calc R U . . .
C62 C 0.6090(2) 0.08415(16) 0.92369(18) 0.0356(11) Uani 1 1 d . . . . .
H62A H 0.6261 0.0634 0.9497 0.043 Uiso 1 1 calc R U . . .
H62B H 0.5987 0.1116 0.9423 0.043 Uiso 1 1 calc R U . . .
C63 C 0.5857(2) 0.06430(16) 0.78886(19) 0.0382(11) Uani 1 1 d . . . . .
H63A H 0.5481 0.0522 0.7724 0.046 Uiso 1 1 calc R U . . .
H63B H 0.6161 0.0700 0.7608 0.046 Uiso 1 1 calc R U . . .
K1 K 1.22967(5) 0.15115(3) 1.09720(3) 0.0279(2) Uani 1 1 d . . . . .
O4 O 1.22921(17) 0.23808(10) 1.06876(13) 0.0418(8) Uani 1 1 d . . . . .
O5 O 1.25295(15) 0.21464(10) 1.17512(12) 0.0361(8) Uani 1 1 d . . . . .
O6 O 1.26905(15) 0.12606(10) 1.19679(11) 0.0341(7) Uani 1 1 d . . . . .
O7 O 1.21504(14) 0.06314(10) 1.12941(12) 0.0324(7) Uani 1 1 d . . . . .
O8 O 1.19720(14) 0.08737(10) 1.02274(12) 0.0315(7) Uani 1 1 d . . . . .
O9 O 1.17738(16) 0.17454(10) 1.00070(11) 0.0373(8) Uani 1 1 d . . . . .
O10 O 1.10893(18) 0.17756(13) 1.11722(14) 0.0532(10) Uani 1 1 d . . . . .
O11 O 1.35040(19) 0.13730(17) 1.07196(17) 0.0713(13) Uani 1 1 d . . . . .
C64 C 1.2236(3) 0.26759(15) 1.11170(19) 0.0456(13) Uani 1 1 d . . . . .
H64A H 1.1816 0.2659 1.1266 0.055 Uiso 1 1 calc R U . . .
H64B H 1.2309 0.2979 1.0996 0.055 Uiso 1 1 calc R U . . .
C65 C 1.2699(3) 0.25534(16) 1.1525(2) 0.0431(13) Uani 1 1 d . . . . .
H65A H 1.3111 0.2530 1.1363 0.052 Uiso 1 1 calc R U . . .
H65B H 1.2715 0.2781 1.1801 0.052 Uiso 1 1 calc R U . . .
C66 C 1.2955(2) 0.19990(17) 1.21329(18) 0.0398(12) Uani 1 1 d . . . . .
H66A H 1.3003 0.2222 1.2411 0.048 Uiso 1 1 calc R U . . .
H66B H 1.3361 0.1949 1.1968 0.048 Uiso 1 1 calc R U . . .
C67 C 1.2722(2) 0.15853(17) 1.23652(17) 0.0397(12) Uani 1 1 d . . . . .
H67A H 1.3000 0.1488 1.2650 0.048 Uiso 1 1 calc R U . . .
H67B H 1.2308 0.1633 1.2518 0.048 Uiso 1 1 calc R U . . .
C68 C 1.2453(2) 0.08550(16) 1.21518(18) 0.0380(11) Uani 1 1 d . . . . .
H68A H 1.2013 0.0888 1.2244 0.046 Uiso 1 1 calc R U . . .
H68B H 1.2678 0.0763 1.2471 0.046 Uiso 1 1 calc R U . . .
C69 C 1.2523(2) 0.05218(16) 1.17364(18) 0.0391(11) Uani 1 1 d . . . . .
H69A H 1.2960 0.0505 1.1628 0.047 Uiso 1 1 calc R U . . .
H69B H 1.2399 0.0232 1.1874 0.047 Uiso 1 1 calc R U . . .
C70 C 1.2241(2) 0.03459(15) 1.08609(18) 0.0343(11) Uani 1 1 d . . . . .
H70A H 1.2172 0.0040 1.0973 0.041 Uiso 1 1 calc R U . . .
H70B H 1.2670 0.0371 1.0733 0.041 Uiso 1 1 calc R U . . .
C71 C 1.1809(2) 0.04594(14) 1.04322(18) 0.0348(11) Uani 1 1 d . . . . .
H71A H 1.1830 0.0236 1.0151 0.042 Uiso 1 1 calc R U . . .
H71B H 1.1383 0.0468 1.0569 0.042 Uiso 1 1 calc R U . . .
C72 C 1.1594(2) 0.10056(15) 0.97976(17) 0.0338(10) Uani 1 1 d . . . . .
H72A H 1.1161 0.1035 0.9914 0.041 Uiso 1 1 calc R U . . .
H72B H 1.1612 0.0785 0.9514 0.041 Uiso 1 1 calc R U . . .
C73 C 1.1824(2) 0.14303(16) 0.96025(17) 0.0371(11) Uani 1 1 d . . . . .
H73A H 1.2259 0.1401 0.9493 0.045 Uiso 1 1 calc R U . . .
H73B H 1.1581 0.1524 0.9294 0.045 Uiso 1 1 calc R U . . .
C74 C 1.1953(3) 0.21700(16) 0.98433(19) 0.0453(13) Uani 1 1 d . . . . .
H74A H 1.1704 0.2263 0.9537 0.054 Uiso 1 1 calc R U . . .
H74B H 1.2392 0.2170 0.9739 0.054 Uiso 1 1 calc R U . . .
C75 C 1.1857(3) 0.24759(16) 1.02890(19) 0.0480(14) Uani 1 1 d . . . . .
H75A H 1.1908 0.2781 1.0168 0.058 Uiso 1 1 calc R U . . .
H75B H 1.1434 0.2443 1.0429 0.058 Uiso 1 1 calc R U . . .
C76 C 1.0908(3) 0.19186(18) 1.1682(2) 0.0510(14) Uani 1 1 d . . . . .
H76A H 1.0533 0.2101 1.1660 0.061 Uiso 1 1 calc R U . . .
H76B H 1.1240 0.2093 1.1847 0.061 Uiso 1 1 calc R U . . .
C77 C 1.0786(3) 0.15085(19) 1.1995(2) 0.0507(14) Uani 1 1 d . . . . .
H77A H 1.0402 0.1537 1.2202 0.061 Uiso 1 1 calc R U . . .
H77B H 1.1131 0.1446 1.2237 0.061 Uiso 1 1 calc R U . . .
C78 C 1.0724(3) 0.11494(19) 1.1583(2) 0.0508(14) Uani 1 1 d . . . . .
H78A H 1.1074 0.0943 1.1599 0.061 Uiso 1 1 calc R U . . .
H78B H 1.0335 0.0985 1.1627 0.061 Uiso 1 1 calc R U . . .
C79 C 1.0727(3) 0.1405(2) 1.1076(2) 0.0554(16) Uani 1 1 d . . . . .
H79A H 1.0906 0.1228 1.0788 0.066 Uiso 1 1 calc R U . . .
H79B H 1.0304 0.1491 1.0977 0.066 Uiso 1 1 calc R U . . .
C80 C 1.3978(4) 0.1228(4) 1.1041(4) 0.137(5) Uani 1 1 d . . . . .
H80A H 1.3841 0.0970 1.1244 0.165 Uiso 1 1 calc R U . . .
H80B H 1.4095 0.1460 1.1291 0.165 Uiso 1 1 calc R U . . .
C81 C 1.4506(4) 0.1111(3) 1.0715(4) 0.093(3) Uani 1 1 d . . . . .
H81A H 1.4632 0.0805 1.0780 0.112 Uiso 1 1 calc R U . . .
H81B H 1.4859 0.1306 1.0789 0.112 Uiso 1 1 calc R U . . .
C82 C 1.4290(4) 0.1167(3) 1.0157(4) 0.110(3) Uani 1 1 d . . . . .
H82A H 1.4581 0.1351 0.9955 0.132 Uiso 1 1 calc R U . . .
H82B H 1.4251 0.0880 0.9980 0.132 Uiso 1 1 calc R U . . .
C83 C 1.3693(4) 0.1380(4) 1.0201(3) 0.106(3) Uani 1 1 d . . . . .
H83A H 1.3723 0.1685 1.0077 0.127 Uiso 1 1 calc R U . . .
H83B H 1.3388 0.1225 0.9980 0.127 Uiso 1 1 calc R U . . .
O12 O 0.99201(18) -0.06147(15) 0.96181(18) 0.0646(12) Uani 1 1 d . . . . .
C84 C 1.0401(3) -0.0796(2) 0.9913(3) 0.0656(18) Uani 1 1 d . . . . .
H84A H 1.0462 -0.1105 0.9811 0.079 Uiso 1 1 calc R U . . .
H84B H 1.0296 -0.0786 1.0291 0.079 Uiso 1 1 calc R U . . .
C85 C 1.0963(3) -0.0548(2) 0.9817(3) 0.0637(17) Uani 1 1 d . . . . .
H85A H 1.1274 -0.0732 0.9639 0.076 Uiso 1 1 calc R U . . .
H85B H 1.1138 -0.0440 1.0152 0.076 Uiso 1 1 calc R U . . .
C86 C 1.0778(2) -0.01709(17) 0.9470(2) 0.0421(12) Uani 1 1 d . . . . .
H86A H 1.0748 0.0104 0.9673 0.050 Uiso 1 1 calc R U . . .
H86B H 1.1073 -0.0130 0.9178 0.050 Uiso 1 1 calc R U . . .
C87 C 1.0164(3) -0.03086(19) 0.9270(2) 0.0492(13) Uani 1 1 d . . . . .
H87A H 0.9887 -0.0053 0.9244 0.059 Uiso 1 1 calc R U . . .
H87B H 1.0206 -0.0439 0.8916 0.059 Uiso 1 1 calc R U . . .
O13 O 1.4814(4) 0.2221(3) 1.0392(4) 0.152(3) Uiso 1 1 d . . . . .
C88 C 1.5291(5) 0.2312(3) 1.0061(4) 0.106(3) Uiso 1 1 d . . . . .
H88A H 1.5305 0.2103 0.9764 0.128 Uiso 1 1 calc R U . . .
H88B H 1.5690 0.2305 1.0249 0.128 Uiso 1 1 calc R U . . .
C89 C 1.5133(5) 0.2780(4) 0.9872(5) 0.130(4) Uiso 1 1 d . . . . .
H89A H 1.5513 0.2948 0.9801 0.156 Uiso 1 1 calc R U . . .
H89B H 1.4884 0.2769 0.9546 0.156 Uiso 1 1 calc R U . . .
C90 C 1.4832(10) 0.2953(7) 1.0236(9) 0.269(10) Uiso 1 1 d . . . . .
H90A H 1.4532 0.3164 1.0091 0.323 Uiso 1 1 calc R U . . .
H90B H 1.5112 0.3111 1.0477 0.323 Uiso 1 1 calc R U . . .
C91 C 1.4475(5) 0.2561(3) 1.0550(4) 0.122(3) Uiso 1 1 d . . . . .
H91A H 1.4494 0.2602 1.0936 0.147 Uiso 1 1 calc R U . . .
H91B H 1.4040 0.2534 1.0438 0.147 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 Cnt 2.232 . ?
Dy1 Dy2 0.5582(5) . ?
Dy1 O3 2.129(3) . ?
Dy1 O2 2.173(3) . ?
Dy1 O1 2.188(3) . ?
Dy1 C2 2.592(4) . ?
Dy1 C3 2.603(4) . ?
Dy1 C4 2.613(4) . ?
Dy1 C1 2.641(4) . ?
Dy1 C6 2.665(4) . ?
Dy1 C5 2.728(4) . ?
Dy2 H1 2.03(10) . ?
Dy2 O1 2.066(3) . ?
Dy2 O2 2.098(3) . ?
Dy2 O3 2.106(3) . ?
O1 C12 1.341(5) . ?
O2 C30 1.339(5) . ?
O3 C48 1.340(5) . ?
C1 C2 1.405(6) . ?
C1 C6 1.411(6) . ?
C1 C7 1.510(6) . ?
C2 C3 1.419(7) . ?
C2 C10 1.518(7) . ?
C3 C4 1.411(6) . ?
C3 C8 1.509(6) . ?
C4 C5 1.415(6) . ?
C4 C28 1.526(6) . ?
C5 C6 1.408(6) . ?
C5 C9 1.504(6) . ?
C6 C46 1.503(6) . ?
C10 C11 1.503(6) . ?
C11 C16 1.399(6) . ?
C11 C12 1.407(6) . ?
C12 C13 1.424(6) . ?
C13 C14 1.394(6) . ?
C13 C18 1.533(6) . ?
C14 C15 1.375(6) . ?
C15 C16 1.379(6) . ?
C15 C17 1.516(6) . ?
C18 C25 1.541(6) . ?
C18 C26 1.543(6) . ?
C18 C19 1.545(6) . ?
C19 C20 1.538(6) . ?
C20 C21 1.516(7) . ?
C20 C27 1.537(6) . ?
C21 C22 1.527(7) . ?
C22 C26 1.534(6) . ?
C22 C23 1.535(7) . ?
C23 C24 1.515(7) . ?
C24 C27 1.525(6) . ?
C24 C25 1.538(6) . ?
C28 C29 1.529(6) . ?
C29 C34 1.391(6) . ?
C29 C30 1.406(6) . ?
C30 C31 1.424(6) . ?
C31 C32 1.394(6) . ?
C31 C36 1.537(6) . ?
C32 C33 1.391(6) . ?
C33 C34 1.385(7) . ?
C33 C35 1.510(6) . ?
C36 C37 1.545(5) . ?
C36 C44 1.545(6) . ?
C36 C43 1.553(5) . ?
C37 C38 1.529(6) . ?
C38 C39 1.521(6) . ?
C38 C45 1.536(6) . ?
C39 C40 1.533(6) . ?
C40 C41 1.528(6) . ?
C40 C44 1.531(6) . ?
C41 C42 1.527(6) . ?
C42 C43 1.520(6) . ?
C42 C45 1.538(6) . ?
C46 C47 1.515(6) . ?
C47 C52 1.391(6) . ?
C47 C48 1.406(6) . ?
C48 C49 1.422(6) . ?
C49 C50 1.396(6) . ?
C49 C54 1.535(6) . ?
C50 C51 1.390(7) . ?
C51 C52 1.388(6) . ?
C51 C53 1.504(6) . ?
C54 C61 1.537(6) . ?
C54 C62 1.545(6) . ?
C54 C55 1.554(6) . ?
C55 C56 1.534(6) . ?
C56 C63 1.528(7) . ?
C56 C57 1.530(6) . ?
C57 C58 1.538(6) . ?
C58 C59 1.522(8) . ?
C58 C62 1.533(7) . ?
C59 C60 1.522(7) . ?
C60 C63 1.526(7) . ?
C60 C61 1.536(6) . ?
K1 O11 2.735(4) . ?
K1 O4 2.758(3) . ?
K1 O6 2.783(3) . ?
K1 O10 2.793(4) . ?
K1 O9 2.799(3) . ?
K1 O8 2.811(3) . ?
K1 O5 2.822(3) . ?
K1 O7 2.834(3) . ?
K1 C79 3.438(6) . ?
O4 C75 1.418(6) . ?
O4 C64 1.423(6) . ?
O5 C66 1.414(6) . ?
O5 C65 1.421(6) . ?
O6 C67 1.420(5) . ?
O6 C68 1.424(6) . ?
O7 C70 1.421(5) . ?
O7 C69 1.426(6) . ?
O8 C71 1.416(5) . ?
O8 C72 1.427(5) . ?
O9 C73 1.415(5) . ?
O9 C74 1.419(6) . ?
O10 C79 1.403(6) . ?
O10 C76 1.424(6) . ?
O11 C83 1.381(8) . ?
O11 C80 1.388(9) . ?
C64 C65 1.494(8) . ?
C66 C67 1.487(7) . ?
C68 C69 1.477(7) . ?
C70 C71 1.482(7) . ?
C72 C73 1.479(7) . ?
C74 C75 1.486(7) . ?
C76 C77 1.511(8) . ?
C77 C78 1.525(7) . ?
C78 C79 1.508(8) . ?
C80 C81 1.459(11) . ?
C81 C82 1.503(12) . ?
C82 C83 1.457(12) . ?
O12 C87 1.394(7) . ?
O12 C84 1.400(7) . ?
C84 C85 1.460(9) . ?
C85 C86 1.508(7) . ?
C86 C87 1.488(7) . ?
O13 C91 1.338(11) . ?
O13 C88 1.365(11) . ?
C88 C89 1.551(13) . ?
C89 C90 1.25(2) . ?
C90 C91 1.64(2) . ?

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
Cnt Dy1 O1 105.7 . . ?
Cnt Dy1 O2 105.8 . . ?
Cnt Dy1 O3 103.2 . . ?
Dy2 Dy1 O3 80.11(15) . . ?
Dy2 Dy1 O2 75.00(16) . . ?
O3 Dy1 O2 114.39(12) . . ?
Dy2 Dy1 O1 70.14(16) . . ?
O3 Dy1 O1 115.22(13) . . ?
O2 Dy1 O1 111.28(12) . . ?
Dy2 Dy1 C2 143.24(19) . . ?
O3 Dy1 C2 109.31(13) . . ?
O2 Dy1 C2 126.53(13) . . ?
O1 Dy1 C2 73.89(13) . . ?
Dy2 Dy1 C3 143.11(17) . . ?
O3 Dy1 C3 134.74(13) . . ?
O2 Dy1 C3 94.92(13) . . ?
O1 Dy1 C3 81.43(13) . . ?
C2 Dy1 C3 31.70(15) . . ?
Dy2 Dy1 C4 146.87(18) . . ?
O3 Dy1 C4 124.10(12) . . ?
O2 Dy1 C4 74.18(12) . . ?
O1 Dy1 C4 110.72(13) . . ?
C2 Dy1 C4 56.06(14) . . ?
C3 Dy1 C4 31.40(14) . . ?
Dy2 Dy1 C1 147.79(19) . . ?
O3 Dy1 C1 80.21(13) . . ?
O2 Dy1 C1 136.77(13) . . ?
O1 Dy1 C1 95.92(13) . . ?
C2 Dy1 C1 31.12(14) . . ?
C3 Dy1 C1 55.53(14) . . ?
C4 Dy1 C1 64.80(14) . . ?
Dy2 Dy1 C6 152.07(17) . . ?
O3 Dy1 C6 72.42(12) . . ?
O2 Dy1 C6 111.72(12) . . ?
O1 Dy1 C6 126.52(12) . . ?
C2 Dy1 C6 55.30(13) . . ?
C3 Dy1 C6 64.72(13) . . ?
C4 Dy1 C6 54.93(13) . . ?
C1 Dy1 C6 30.84(13) . . ?
Dy2 Dy1 C5 152.40(19) . . ?
O3 Dy1 C5 93.56(12) . . ?
O2 Dy1 C5 83.52(12) . . ?
O1 Dy1 C5 135.25(12) . . ?
C2 Dy1 C5 64.19(13) . . ?
C3 Dy1 C5 54.68(13) . . ?
C4 Dy1 C5 30.62(13) . . ?
C1 Dy1 C5 54.15(13) . . ?
C6 Dy1 C5 30.24(12) . . ?
Dy1 Dy2 H1 179(3) . . ?
Dy1 Dy2 O1 95.14(17) . . ?
H1 Dy2 O1 86(3) . . ?
Dy1 Dy2 O2 90.11(16) . . ?
H1 Dy2 O2 90(3) . . ?
O1 Dy2 O2 119.61(13) . . ?
Dy1 Dy2 O3 84.75(15) . . ?
H1 Dy2 O3 94(3) . . ?
O1 Dy2 O3 121.78(13) . . ?
O2 Dy2 O3 118.61(12) . . ?
C12 O1 Dy2 162.7(3) . . ?
C12 O1 Dy1 148.3(3) . . ?
C30 O2 Dy2 154.0(3) . . ?
C30 O2 Dy1 141.4(2) . . ?
C48 O3 Dy2 164.7(3) . . ?
C48 O3 Dy1 150.4(3) . . ?
C2 C1 C6 120.2(4) . . ?
C2 C1 C7 121.5(4) . . ?
C6 C1 C7 118.4(4) . . ?
C2 C1 Dy1 72.5(2) . . ?
C6 C1 Dy1 75.5(2) . . ?
C7 C1 Dy1 124.6(3) . . ?
C1 C2 C3 119.8(4) . . ?
C1 C2 C10 116.7(4) . . ?
C3 C2 C10 123.4(4) . . ?
C1 C2 Dy1 76.4(2) . . ?
C3 C2 Dy1 74.6(2) . . ?
C10 C2 Dy1 118.3(3) . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 C8 120.7(4) . . ?
C2 C3 C8 119.7(4) . . ?
C4 C3 Dy1 74.7(2) . . ?
C2 C3 Dy1 73.7(2) . . ?
C8 C3 Dy1 123.2(3) . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 C28 119.5(4) . . ?
C5 C4 C28 120.2(4) . . ?
C3 C4 Dy1 73.9(2) . . ?
C5 C4 Dy1 79.2(2) . . ?
C28 C4 Dy1 116.9(3) . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 C9 120.5(4) . . ?
C4 C5 C9 120.3(4) . . ?
C6 C5 Dy1 72.4(2) . . ?
C4 C5 Dy1 70.2(2) . . ?
C9 C5 Dy1 130.8(3) . . ?
C5 C6 C1 120.3(4) . . ?
C5 C6 C46 119.0(4) . . ?
C1 C6 C46 120.7(4) . . ?
C5 C6 Dy1 77.4(2) . . ?
C1 C6 Dy1 73.7(2) . . ?
C46 C6 Dy1 120.9(3) . . ?
C11 C10 C2 121.8(4) . . ?
C16 C11 C12 119.3(4) . . ?
C16 C11 C10 117.8(4) . . ?
C12 C11 C10 122.5(4) . . ?
O1 C12 C11 119.1(4) . . ?
O1 C12 C13 121.4(4) . . ?
C11 C12 C13 119.5(4) . . ?
C14 C13 C12 117.5(4) . . ?
C14 C13 C18 120.8(4) . . ?
C12 C13 C18 121.7(4) . . ?
C15 C14 C13 124.0(4) . . ?
C14 C15 C16 117.6(4) . . ?
C14 C15 C17 120.4(4) . . ?
C16 C15 C17 122.1(4) . . ?
C15 C16 C11 122.2(4) . . ?
C13 C18 C25 111.8(3) . . ?
C13 C18 C26 109.2(3) . . ?
C25 C18 C26 106.8(3) . . ?
C13 C18 C19 112.2(3) . . ?
C25 C18 C19 107.5(3) . . ?
C26 C18 C19 109.2(3) . . ?
C20 C19 C18 110.3(3) . . ?
C21 C20 C27 108.7(4) . . ?
C21 C20 C19 110.0(4) . . ?
C27 C20 C19 109.8(4) . . ?
C20 C21 C22 110.7(4) . . ?
C21 C22 C26 108.5(4) . . ?
C21 C22 C23 109.3(4) . . ?
C26 C22 C23 109.8(4) . . ?
C24 C23 C22 109.0(4) . . ?
C23 C24 C27 110.0(4) . . ?
C23 C24 C25 109.2(4) . . ?
C27 C24 C25 110.0(4) . . ?
C24 C25 C18 111.5(4) . . ?
C22 C26 C18 111.2(4) . . ?
C24 C27 C20 108.9(4) . . ?
C4 C28 C29 117.8(4) . . ?
C34 C29 C30 119.2(4) . . ?
C34 C29 C28 119.9(4) . . ?
C30 C29 C28 120.8(4) . . ?
O2 C30 C29 118.8(4) . . ?
O2 C30 C31 121.5(4) . . ?
C29 C30 C31 119.8(4) . . ?
C32 C31 C30 117.6(4) . . ?
C32 C31 C36 120.6(4) . . ?
C30 C31 C36 121.8(4) . . ?
C33 C32 C31 123.6(4) . . ?
C34 C33 C32 117.1(4) . . ?
C34 C33 C35 121.5(4) . . ?
C32 C33 C35 121.5(4) . . ?
C33 C34 C29 122.7(4) . . ?
C31 C36 C37 110.7(3) . . ?
C31 C36 C44 112.4(3) . . ?
C37 C36 C44 106.8(3) . . ?
C31 C36 C43 111.3(3) . . ?
C37 C36 C43 109.1(3) . . ?
C44 C36 C43 106.4(3) . . ?
C38 C37 C36 111.2(3) . . ?
C39 C38 C37 109.7(4) . . ?
C39 C38 C45 109.3(3) . . ?
C37 C38 C45 109.5(3) . . ?
C38 C39 C40 109.4(3) . . ?
C41 C40 C44 110.1(4) . . ?
C41 C40 C39 109.4(4) . . ?
C44 C40 C39 108.9(3) . . ?
C42 C41 C40 108.8(3) . . ?
C43 C42 C41 110.3(3) . . ?
C43 C42 C45 109.9(3) . . ?
C41 C42 C45 109.2(3) . . ?
C42 C43 C36 111.1(3) . . ?
C40 C44 C36 111.9(3) . . ?
C38 C45 C42 109.3(3) . . ?
C6 C46 C47 121.0(4) . . ?
C52 C47 C48 119.6(4) . . ?
C52 C47 C46 116.0(4) . . ?
C48 C47 C46 124.2(4) . . ?
O3 C48 C47 119.8(4) . . ?
O3 C48 C49 120.8(4) . . ?
C47 C48 C49 119.4(4) . . ?
C50 C49 C48 118.4(4) . . ?
C50 C49 C54 120.3(4) . . ?
C48 C49 C54 121.3(4) . . ?
C51 C50 C49 122.6(4) . . ?
C52 C51 C50 117.8(4) . . ?
C52 C51 C53 120.5(4) . . ?
C50 C51 C53 121.7(4) . . ?
C51 C52 C47 122.1(4) . . ?
C49 C54 C61 110.5(3) . . ?
C49 C54 C62 112.5(4) . . ?
C61 C54 C62 106.6(4) . . ?
C49 C54 C55 110.8(3) . . ?
C61 C54 C55 109.3(4) . . ?
C62 C54 C55 107.0(3) . . ?
C56 C55 C54 110.6(3) . . ?
C63 C56 C57 109.3(4) . . ?
C63 C56 C55 109.8(4) . . ?
C57 C56 C55 109.5(4) . . ?
C56 C57 C58 109.1(4) . . ?
C59 C58 C62 110.6(4) . . ?
C59 C58 C57 109.0(4) . . ?
C62 C58 C57 109.1(4) . . ?
C60 C59 C58 109.3(4) . . ?
C59 C60 C63 109.5(4) . . ?
C59 C60 C61 109.1(4) . . ?
C63 C60 C61 109.5(4) . . ?
C60 C61 C54 111.7(4) . . ?
C58 C62 C54 111.4(4) . . ?
C60 C63 C56 109.8(4) . . ?
O11 K1 O4 95.25(14) . . ?
O11 K1 O6 82.87(12) . . ?
O4 K1 O6 120.43(10) . . ?
O11 K1 O10 171.65(14) . . ?
O4 K1 O10 76.42(11) . . ?
O6 K1 O10 101.70(11) . . ?
O11 K1 O9 102.90(12) . . ?
O4 K1 O9 61.41(10) . . ?
O6 K1 O9 173.93(11) . . ?
O10 K1 O9 72.81(11) . . ?
O11 K1 O8 88.56(12) . . ?
O4 K1 O8 119.51(10) . . ?
O6 K1 O8 119.95(10) . . ?
O10 K1 O8 95.05(10) . . ?
O9 K1 O8 58.96(9) . . ?
O11 K1 O5 95.72(13) . . ?
O4 K1 O5 61.35(9) . . ?
O6 K1 O5 59.68(9) . . ?
O10 K1 O5 80.86(11) . . ?
O9 K1 O5 120.87(10) . . ?
O8 K1 O5 175.56(10) . . ?
O11 K1 O7 91.61(13) . . ?
O4 K1 O7 173.13(11) . . ?
O6 K1 O7 60.57(9) . . ?
O10 K1 O7 96.71(11) . . ?
O9 K1 O7 116.83(10) . . ?
O8 K1 O7 60.42(9) . . ?
O5 K1 O7 118.13(9) . . ?
O11 K1 C79 162.88(15) . . ?
O4 K1 C79 96.22(14) . . ?
O6 K1 C79 102.05(12) . . ?
O10 K1 C79 23.20(13) . . ?
O9 K1 C79 71.87(12) . . ?
O8 K1 C79 74.73(11) . . ?
O5 K1 C79 100.92(12) . . ?
O7 K1 C79 77.05(13) . . ?
C75 O4 C64 111.2(4) . . ?
C75 O4 K1 112.9(3) . . ?
C64 O4 K1 114.3(3) . . ?
C66 O5 C65 112.9(4) . . ?
C66 O5 K1 112.3(3) . . ?
C65 O5 K1 111.4(2) . . ?
C67 O6 C68 113.2(3) . . ?
C67 O6 K1 118.0(3) . . ?
C68 O6 K1 115.4(3) . . ?
C70 O7 C69 112.9(3) . . ?
C70 O7 K1 110.2(2) . . ?
C69 O7 K1 112.8(3) . . ?
C71 O8 C72 113.0(3) . . ?
C71 O8 K1 115.9(2) . . ?
C72 O8 K1 117.7(2) . . ?
C73 O9 C74 112.9(3) . . ?
C73 O9 K1 115.6(3) . . ?
C74 O9 K1 112.3(3) . . ?
C79 O10 C76 104.6(4) . . ?
C79 O10 K1 105.2(3) . . ?
C76 O10 K1 121.0(3) . . ?
C83 O11 C80 110.2(6) . . ?
C83 O11 K1 120.5(4) . . ?
C80 O11 K1 128.6(4) . . ?
O4 C64 C65 108.4(4) . . ?
O5 C65 C64 109.1(4) . . ?
O5 C66 C67 108.8(4) . . ?
O6 C67 C66 109.2(4) . . ?
O6 C68 C69 109.2(4) . . ?
O7 C69 C68 110.1(4) . . ?
O7 C70 C71 109.8(4) . . ?
O8 C71 C70 108.8(4) . . ?
O8 C72 C73 108.1(4) . . ?
O9 C73 C72 109.2(4) . . ?
O9 C74 C75 108.3(4) . . ?
O4 C75 C74 108.8(4) . . ?
O10 C76 C77 105.9(4) . . ?
C76 C77 C78 104.6(4) . . ?
C79 C78 C77 102.4(5) . . ?
O10 C79 C78 105.8(4) . . ?
O10 C79 K1 51.6(3) . . ?
C78 C79 K1 96.9(4) . . ?
O11 C80 C81 109.1(7) . . ?
C80 C81 C82 105.3(7) . . ?
C83 C82 C81 104.8(7) . . ?
O11 C83 C82 109.4(7) . . ?
C87 O12 C84 108.8(4) . . ?
O12 C84 C85 109.3(5) . . ?
C84 C85 C86 105.7(5) . . ?
C87 C86 C85 102.9(5) . . ?
O12 C87 C86 108.3(4) . . ?
C91 O13 C88 116.5(9) . . ?
O13 C88 C89 102.1(9) . . ?
C90 C89 C88 106.1(14) . . ?
C89 C90 C91 107.4(17) . . ?
O13 C91 C90 99.3(11) . . ?

_refine_diff_density_max         1.718
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.095



####################################################################### 
# 
# 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_ctp82
_database_code_depnum_ccdc_archive 'CCDC 1538995'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C75 H108 O6'
_chemical_formula_weight         1105.61

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'
O O 0.0106 0.0060 '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                   13.904(3)
_cell_length_b                   15.774(3)
_cell_length_c                   16.856(3)
_cell_angle_alpha                99.238(3)
_cell_angle_beta                 109.444(2)
_cell_angle_gamma                106.032(3)
_cell_volume                     3217.6(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    5679
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.24

_exptl_crystal_description       irregular
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_F_000             1212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.172
_exptl_absorpt_coefficient_mu    0.070
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7226
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30722
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.334
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.350
_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             11758
_reflns_number_gt                7122
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A colorless crystal of approximate dimensions 0.172 x 0.200 x 0.292 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters and 
for data collection (90 sec/frame scan time for a sphere of diffraction data).  
The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
There were no systematic absences nor any diffraction symmetry other than the 
Friedel condition.  The centrosymmetric triclinic space group P-1 was assigned 
and later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis. Hydrogen atoms H(1), H(2) and H(3) were located 
from a difference-Fourier map and refined (x,y,z and Uiso).  The remaining hydrogen 
atoms were included using a riding model.  There were three molecules of 
diethylether present.  

Least-squares analysis yielded wR2 = 0.1517 and Goof = 0.96 for 754 variables 
refined against 11758 data (0.83 Å), R1 = 0.0570 for those 7122 data 
with I > 2.0sigma(I).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0758P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11758
_refine_ls_number_parameters     754
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1517
_refine_ls_wR_factor_gt          0.1267
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
O1 O 0.59542(13) 0.33632(11) 0.67555(11) 0.0218(4) Uani 1 1 d . . . . .
O2 O 0.29265(14) 0.72865(12) 0.92974(12) 0.0239(4) Uani 1 1 d . . . . .
O3 O 0.99455(15) 0.74661(12) 1.31437(11) 0.0283(4) Uani 1 1 d . . . . .
C1 C 0.62273(18) 0.51054(15) 0.91404(15) 0.0186(5) Uani 1 1 d . . . . .
C2 C 0.53783(18) 0.54500(15) 0.90312(15) 0.0188(5) Uani 1 1 d . . . . .
C3 C 0.54199(18) 0.60971(15) 0.97277(15) 0.0181(5) Uani 1 1 d . . . . .
C4 C 0.63305(18) 0.64208(15) 1.05275(15) 0.0181(5) Uani 1 1 d . . . . .
C5 C 0.71720(18) 0.60695(15) 1.06401(15) 0.0181(5) Uani 1 1 d . . . . .
C6 C 0.71330(18) 0.54219(15) 0.99433(15) 0.0191(5) Uani 1 1 d . . . . .
C7 C 0.44365(18) 0.51604(16) 0.81523(15) 0.0220(5) Uani 1 1 d . . . . .
H7A H 0.4216 0.5686 0.8053 0.033 Uiso 1 1 calc R U . . .
H7B H 0.3821 0.4666 0.8144 0.033 Uiso 1 1 calc R U . . .
H7C H 0.4661 0.4941 0.7690 0.033 Uiso 1 1 calc R U . . .
C8 C 0.6408(2) 0.71745(16) 1.12529(15) 0.0242(6) Uani 1 1 d . . . . .
H8A H 0.7175 0.7502 1.1650 0.036 Uiso 1 1 calc R U . . .
H8B H 0.5999 0.6904 1.1580 0.036 Uiso 1 1 calc R U . . .
H8C H 0.6102 0.7606 1.0998 0.036 Uiso 1 1 calc R U . . .
C9 C 0.8080(2) 0.50949(17) 1.00463(16) 0.0274(6) Uani 1 1 d . . . . .
H9A H 0.8754 0.5574 1.0481 0.041 Uiso 1 1 calc R U . . .
H9B H 0.8146 0.4961 0.9483 0.041 Uiso 1 1 calc R U . . .
H9C H 0.7954 0.4537 1.0242 0.041 Uiso 1 1 calc R U . . .
C10 C 0.61867(19) 0.44221(15) 0.83770(15) 0.0214(5) Uani 1 1 d . . . . .
H10A H 0.5425 0.3993 0.8045 0.026 Uiso 1 1 calc R U . . .
H10B H 0.6636 0.4058 0.8609 0.026 Uiso 1 1 calc R U . . .
C11 C 0.65891(18) 0.48611(15) 0.77520(15) 0.0189(5) Uani 1 1 d . . . . .
C12 C 0.64337(18) 0.43091(15) 0.69468(15) 0.0185(5) Uani 1 1 d . . . . .
C13 C 0.66957(18) 0.46839(15) 0.63169(15) 0.0187(5) Uani 1 1 d . . . . .
C14 C 0.71716(18) 0.56401(16) 0.65439(15) 0.0209(5) Uani 1 1 d . . . . .
H14A H 0.7363 0.5914 0.6129 0.025 Uiso 1 1 calc R U . . .
C15 C 0.73784(18) 0.62107(15) 0.73486(16) 0.0210(5) Uani 1 1 d . . . . .
C16 C 0.70758(18) 0.58096(16) 0.79409(15) 0.0208(5) Uani 1 1 d . . . . .
H16A H 0.7203 0.6190 0.8490 0.025 Uiso 1 1 calc R U . . .
C17 C 0.7895(2) 0.72391(16) 0.75588(17) 0.0271(6) Uani 1 1 d . . . . .
H17A H 0.8551 0.7465 0.8104 0.041 Uiso 1 1 calc R U . . .
H17B H 0.7376 0.7527 0.7628 0.041 Uiso 1 1 calc R U . . .
H17C H 0.8094 0.7394 0.7081 0.041 Uiso 1 1 calc R U . . .
C18 C 0.64609(18) 0.40903(16) 0.54108(15) 0.0202(5) Uani 1 1 d . . . . .
C19 C 0.70807(19) 0.34124(16) 0.54790(15) 0.0231(6) Uani 1 1 d . . . . .
H19A H 0.7875 0.3759 0.5774 0.028 Uiso 1 1 calc R U . . .
H19B H 0.6873 0.3014 0.5837 0.028 Uiso 1 1 calc R U . . .
C20 C 0.6815(2) 0.28164(16) 0.45664(15) 0.0241(6) Uani 1 1 d . . . . .
H20A H 0.7219 0.2379 0.4626 0.029 Uiso 1 1 calc R U . . .
C21 C 0.5583(2) 0.22702(17) 0.41101(16) 0.0281(6) Uani 1 1 d . . . . .
H21A H 0.5411 0.1874 0.3526 0.034 Uiso 1 1 calc R U . . .
H21B H 0.5355 0.1872 0.4461 0.034 Uiso 1 1 calc R U . . .
C22 C 0.4966(2) 0.29428(17) 0.40117(15) 0.0260(6) Uani 1 1 d . . . . .
H22A H 0.4165 0.2587 0.3716 0.031 Uiso 1 1 calc R U . . .
C23 C 0.5302(2) 0.35498(17) 0.34590(16) 0.0273(6) Uani 1 1 d . . . . .
H23A H 0.4900 0.3981 0.3392 0.033 Uiso 1 1 calc R U . . .
H23B H 0.5128 0.3166 0.2869 0.033 Uiso 1 1 calc R U . . .
C24 C 0.6531(2) 0.40860(17) 0.39213(15) 0.0241(6) Uani 1 1 d . . . . .
H24A H 0.6762 0.4492 0.3569 0.029 Uiso 1 1 calc R U . . .
C25 C 0.6795(2) 0.46778(16) 0.48327(15) 0.0225(6) Uani 1 1 d . . . . .
H25A H 0.6406 0.5119 0.4774 0.027 Uiso 1 1 calc R U . . .
H25B H 0.7587 0.5034 0.5121 0.027 Uiso 1 1 calc R U . . .
C26 C 0.7153(2) 0.34206(17) 0.40104(16) 0.0277(6) Uani 1 1 d . . . . .
H26A H 0.7948 0.3769 0.4292 0.033 Uiso 1 1 calc R U . . .
H26B H 0.6984 0.3032 0.3424 0.033 Uiso 1 1 calc R U . . .
C27 C 0.52222(19) 0.35414(16) 0.49208(15) 0.0225(5) Uani 1 1 d . . . . .
H27A H 0.4974 0.3146 0.5267 0.027 Uiso 1 1 calc R U . . .
H27B H 0.4821 0.3973 0.4858 0.027 Uiso 1 1 calc R U . . .
C28 C 0.44990(19) 0.64660(15) 0.96057(15) 0.0210(5) Uani 1 1 d . . . . .
H28A H 0.4456 0.6644 1.0180 0.025 Uiso 1 1 calc R U . . .
H28B H 0.3804 0.5967 0.9211 0.025 Uiso 1 1 calc R U . . .
C29 C 0.46108(19) 0.72878(15) 0.92315(14) 0.0196(5) Uani 1 1 d . . . . .
C30 C 0.37807(19) 0.76565(15) 0.90522(15) 0.0193(5) Uani 1 1 d . . . . .
C31 C 0.38415(19) 0.84091(15) 0.86988(15) 0.0202(5) Uani 1 1 d . . . . .
C32 C 0.47759(19) 0.87710(15) 0.85426(15) 0.0209(5) Uani 1 1 d . . . . .
H32A H 0.4838 0.9280 0.8303 0.025 Uiso 1 1 calc R U . . .
C33 C 0.56183(19) 0.84283(16) 0.87177(15) 0.0204(5) Uani 1 1 d . . . . .
C34 C 0.55204(19) 0.76852(16) 0.90616(15) 0.0210(5) Uani 1 1 d . . . . .
H34A H 0.6089 0.7440 0.9185 0.025 Uiso 1 1 calc R U . . .
C35 C 0.6596(2) 0.88543(17) 0.85237(17) 0.0292(6) Uani 1 1 d . . . . .
H35A H 0.7213 0.8705 0.8875 0.044 Uiso 1 1 calc R U . . .
H35B H 0.6788 0.9523 0.8670 0.044 Uiso 1 1 calc R U . . .
H35C H 0.6423 0.8613 0.7900 0.044 Uiso 1 1 calc R U . . .
C36 C 0.29442(19) 0.88266(16) 0.84871(15) 0.0213(5) Uani 1 1 d . . . . .
C37 C 0.2764(2) 0.91876(16) 0.93152(16) 0.0254(6) Uani 1 1 d . . . . .
H37A H 0.2567 0.8678 0.9573 0.030 Uiso 1 1 calc R U . . .
H37B H 0.3450 0.9666 0.9755 0.030 Uiso 1 1 calc R U . . .
C38 C 0.1860(2) 0.95904(17) 0.90959(17) 0.0296(6) Uani 1 1 d . . . . .
H38A H 0.1751 0.9807 0.9640 0.036 Uiso 1 1 calc R U . . .
C39 C 0.2167(2) 1.03976(18) 0.8724(2) 0.0381(7) Uani 1 1 d . . . . .
H39A H 0.2846 1.0884 0.9162 0.046 Uiso 1 1 calc R U . . .
H39B H 0.1580 1.0659 0.8585 0.046 Uiso 1 1 calc R U . . .
C40 C 0.2331(2) 1.00588(18) 0.78955(19) 0.0352(7) Uani 1 1 d . . . . .
H40A H 0.2547 1.0588 0.7656 0.042 Uiso 1 1 calc R U . . .
C41 C 0.1265(2) 0.93311(19) 0.72113(18) 0.0364(7) Uani 1 1 d . . . . .
H41A H 0.0681 0.9595 0.7072 0.044 Uiso 1 1 calc R U . . .
H41B H 0.1360 0.9122 0.6666 0.044 Uiso 1 1 calc R U . . .
C42 C 0.0949(2) 0.85186(17) 0.75781(17) 0.0279(6) Uani 1 1 d . . . . .
H42A H 0.0253 0.8038 0.7135 0.033 Uiso 1 1 calc R U . . .
C43 C 0.18567(19) 0.81121(16) 0.77876(16) 0.0231(6) Uani 1 1 d . . . . .
H43A H 0.1960 0.7902 0.7246 0.028 Uiso 1 1 calc R U . . .
H43B H 0.1639 0.7572 0.8004 0.028 Uiso 1 1 calc R U . . .
C44 C 0.0795(2) 0.88491(17) 0.84154(17) 0.0290(6) Uani 1 1 d . . . . .
H44A H 0.0586 0.8326 0.8654 0.035 Uiso 1 1 calc R U . . .
H44B H 0.0202 0.9104 0.8282 0.035 Uiso 1 1 calc R U . . .
C45 C 0.3229(2) 0.96516(17) 0.81098(18) 0.0284(6) Uani 1 1 d . . . . .
H45A H 0.3919 1.0131 0.8541 0.034 Uiso 1 1 calc R U . . .
H45B H 0.3341 0.9447 0.7572 0.034 Uiso 1 1 calc R U . . .
C46 C 0.81565(18) 0.64230(15) 1.15103(15) 0.0203(5) Uani 1 1 d . . . . .
H46A H 0.8497 0.5949 1.1574 0.024 Uiso 1 1 calc R U . . .
H46B H 0.7904 0.6513 1.1991 0.024 Uiso 1 1 calc R U . . .
C47 C 0.90168(19) 0.73197(15) 1.16093(15) 0.0201(5) Uani 1 1 d . . . . .
C48 C 0.98460(19) 0.78180(16) 1.24364(15) 0.0208(5) Uani 1 1 d . . . . .
C49 C 1.06221(19) 0.86750(16) 1.25638(16) 0.0221(5) Uani 1 1 d . . . . .
C50 C 1.0566(2) 0.89694(16) 1.18202(16) 0.0240(6) Uani 1 1 d . . . . .
H50A H 1.1089 0.9539 1.1886 0.029 Uiso 1 1 calc R U . . .
C51 C 0.97835(19) 0.84737(16) 1.09847(16) 0.0229(6) Uani 1 1 d . . . . .
C52 C 0.9008(2) 0.76576(16) 1.09017(16) 0.0227(6) Uani 1 1 d . . . . .
H52A H 0.8452 0.7319 1.0340 0.027 Uiso 1 1 calc R U . . .
C53 C 0.9761(2) 0.88296(18) 1.02039(17) 0.0341(7) Uani 1 1 d . . . . .
H53A H 0.9354 0.8319 0.9667 0.051 Uiso 1 1 calc R U . . .
H53B H 1.0509 0.9115 1.0255 0.051 Uiso 1 1 calc R U . . .
H53C H 0.9404 0.9287 1.0181 0.051 Uiso 1 1 calc R U . . .
C54 C 1.14826(19) 0.92575(16) 1.34747(16) 0.0251(6) Uani 1 1 d . . . . .
C55 C 1.2170(2) 1.01986(16) 1.34444(17) 0.0314(6) Uani 1 1 d . . . . .
H55A H 1.2547 1.0102 1.3051 0.038 Uiso 1 1 calc R U . . .
H55B H 1.1683 1.0531 1.3204 0.038 Uiso 1 1 calc R U . . .
C56 C 1.3019(2) 1.07809(18) 1.43647(19) 0.0382(7) Uani 1 1 d . . . . .
H56A H 1.3446 1.1386 1.4326 0.046 Uiso 1 1 calc R U . . .
C57 C 1.3789(2) 1.02818(18) 1.47169(19) 0.0374(7) Uani 1 1 d . . . . .
H57A H 1.4348 1.0657 1.5305 0.045 Uiso 1 1 calc R U . . .
H57B H 1.4165 1.0184 1.4323 0.045 Uiso 1 1 calc R U . . .
C58 C 1.3131(2) 0.93523(16) 1.47746(17) 0.0293(6) Uani 1 1 d . . . . .
H58A H 1.3635 0.9023 1.5012 0.035 Uiso 1 1 calc R U . . .
C59 C 1.2545(2) 0.95041(18) 1.53743(17) 0.0329(6) Uani 1 1 d . . . . .
H59A H 1.3087 0.9863 1.5972 0.039 Uiso 1 1 calc R U . . .
H59B H 1.2117 0.8904 1.5407 0.039 Uiso 1 1 calc R U . . .
C60 C 1.1785(2) 1.00200(17) 1.50266(17) 0.0337(7) Uani 1 1 d . . . . .
H60A H 1.1411 1.0124 1.5428 0.040 Uiso 1 1 calc R U . . .
C61 C 1.0933(2) 0.94506(17) 1.41083(16) 0.0295(6) Uani 1 1 d . . . . .
H61A H 1.0445 0.9787 1.3879 0.035 Uiso 1 1 calc R U . . .
H61B H 1.0483 0.8861 1.4143 0.035 Uiso 1 1 calc R U . . .
C62 C 1.2451(2) 1.09440(18) 1.49745(19) 0.0409(7) Uani 1 1 d . . . . .
H62A H 1.1964 1.1283 1.4751 0.049 Uiso 1 1 calc R U . . .
H62B H 1.2999 1.1319 1.5566 0.049 Uiso 1 1 calc R U . . .
C63 C 1.2282(2) 0.87709(16) 1.38534(16) 0.0269(6) Uani 1 1 d . . . . .
H63A H 1.1871 0.8164 1.3884 0.032 Uiso 1 1 calc R U . . .
H63B H 1.2659 0.8670 1.3461 0.032 Uiso 1 1 calc R U . . .
O4 O 0.69415(17) 0.25090(12) 0.79151(12) 0.0418(5) Uani 1 1 d . . . . .
C64 C 0.8648(3) 0.3553(2) 0.8075(3) 0.0672(11) Uani 1 1 d . . . . .
H64A H 0.9430 0.3820 0.8447 0.101 Uiso 1 1 calc R U . . .
H64B H 0.8339 0.4041 0.8049 0.101 Uiso 1 1 calc R U . . .
H64C H 0.8542 0.3244 0.7483 0.101 Uiso 1 1 calc R U . . .
C65 C 0.8094(3) 0.2876(3) 0.8447(2) 0.0674(12) Uani 1 1 d . . . . .
H65A H 0.8390 0.2373 0.8460 0.081 Uiso 1 1 calc R U . . .
H65B H 0.8226 0.3179 0.9055 0.081 Uiso 1 1 calc R U . . .
C66 C 0.6306(4) 0.1860(3) 0.8217(2) 0.0805(14) Uani 1 1 d . . . . .
H66A H 0.6371 0.2156 0.8806 0.097 Uiso 1 1 calc R U . . .
H66B H 0.6568 0.1339 0.8254 0.097 Uiso 1 1 calc R U . . .
C67 C 0.5135(4) 0.1524(3) 0.7571(3) 0.0917(15) Uani 1 1 d . . . . .
H67A H 0.4677 0.1092 0.7771 0.138 Uiso 1 1 calc R U . . .
H67B H 0.5076 0.1215 0.6995 0.138 Uiso 1 1 calc R U . . .
H67C H 0.4890 0.2047 0.7528 0.138 Uiso 1 1 calc R U . . .
O5 O 0.08509(13) 0.59034(11) 0.81508(11) 0.0297(4) Uani 1 1 d . . . . .
C68 C 0.1687(2) 0.5404(2) 0.7244(2) 0.0414(7) Uani 1 1 d . . . . .
H68A H 0.1544 0.5044 0.6660 0.062 Uiso 1 1 calc R U . . .
H68B H 0.1996 0.5106 0.7682 0.062 Uiso 1 1 calc R U . . .
H68C H 0.2205 0.6024 0.7373 0.062 Uiso 1 1 calc R U . . .
C69 C 0.0646(2) 0.5463(2) 0.72726(18) 0.0403(7) Uani 1 1 d . . . . .
H69A H 0.0367 0.5819 0.6876 0.048 Uiso 1 1 calc R U . . .
H69B H 0.0090 0.4839 0.7077 0.048 Uiso 1 1 calc R U . . .
C70 C -0.0065(2) 0.60966(19) 0.82139(17) 0.0329(6) Uani 1 1 d . . . . .
H70A H -0.0722 0.5531 0.7941 0.039 Uiso 1 1 calc R U . . .
H70B H -0.0203 0.6559 0.7901 0.039 Uiso 1 1 calc R U . . .
C71 C 0.0163(2) 0.64564(19) 0.91628(18) 0.0374(7) Uani 1 1 d . . . . .
H71A H -0.0449 0.6622 0.9212 0.056 Uiso 1 1 calc R U . . .
H71B H 0.0832 0.7000 0.9436 0.056 Uiso 1 1 calc R U . . .
H71C H 0.0254 0.5981 0.9461 0.056 Uiso 1 1 calc R U . . .
O6 O 0.84772(14) 0.67470(13) 1.38963(11) 0.0345(5) Uani 1 1 d . . . . .
C72 C 1.0096(2) 0.6753(2) 1.4986(2) 0.0541(9) Uani 1 1 d . . . . .
H72A H 1.0614 0.7036 1.5597 0.081 Uiso 1 1 calc R U . . .
H72B H 1.0478 0.6867 1.4598 0.081 Uiso 1 1 calc R U . . .
H72C H 0.9770 0.6089 1.4889 0.081 Uiso 1 1 calc R U . . .
C73 C 0.9217(2) 0.7158(2) 1.47958(17) 0.0403(7) Uani 1 1 d . . . . .
H73A H 0.8823 0.7040 1.5182 0.048 Uiso 1 1 calc R U . . .
H73B H 0.9542 0.7831 1.4907 0.048 Uiso 1 1 calc R U . . .
C74 C 0.7601(2) 0.70865(18) 1.36543(17) 0.0300(6) Uani 1 1 d . . . . .
H74A H 0.7250 0.6921 1.3007 0.036 Uiso 1 1 calc R U . . .
H74B H 0.7904 0.7765 1.3874 0.036 Uiso 1 1 calc R U . . .
C75 C 0.6747(2) 0.67252(17) 1.39985(17) 0.0310(6) Uani 1 1 d . . . . .
H75A H 0.6143 0.6943 1.3764 0.046 Uiso 1 1 calc R U . . .
H75B H 0.7068 0.6945 1.4640 0.046 Uiso 1 1 calc R U . . .
H75C H 0.6474 0.6052 1.3816 0.046 Uiso 1 1 calc R U . . .
H1 H 0.622(2) 0.3099(19) 0.7174(19) 0.046(9) Uiso 1 1 d . . . . .
H2 H 0.238(3) 0.688(3) 0.893(3) 0.107(17) Uiso 1 1 d . . . . .
H3 H 0.937(3) 0.715(2) 1.321(2) 0.067(11) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C12 1.388(3) . ?
O2 C30 1.394(3) . ?
O3 C48 1.376(3) . ?
C1 C2 1.402(3) . ?
C1 C6 1.403(3) . ?
C1 C10 1.514(3) . ?
C2 C3 1.400(3) . ?
C2 C7 1.510(3) . ?
C3 C4 1.402(3) . ?
C3 C28 1.515(3) . ?
C4 C5 1.398(3) . ?
C4 C8 1.515(3) . ?
C5 C6 1.403(3) . ?
C5 C46 1.521(3) . ?
C6 C9 1.510(3) . ?
C10 C11 1.522(3) . ?
C11 C16 1.394(3) . ?
C11 C12 1.403(3) . ?
C12 C13 1.396(3) . ?
C13 C14 1.398(3) . ?
C13 C18 1.535(3) . ?
C14 C15 1.392(3) . ?
C15 C16 1.382(3) . ?
C15 C17 1.508(3) . ?
C18 C25 1.542(3) . ?
C18 C19 1.543(3) . ?
C18 C27 1.548(3) . ?
C19 C20 1.534(3) . ?
C20 C26 1.530(3) . ?
C20 C21 1.538(3) . ?
C21 C22 1.533(3) . ?
C22 C23 1.527(3) . ?
C22 C27 1.534(3) . ?
C23 C24 1.532(3) . ?
C24 C26 1.528(3) . ?
C24 C25 1.530(3) . ?
C28 C29 1.523(3) . ?
C29 C34 1.391(3) . ?
C29 C30 1.399(3) . ?
C30 C31 1.406(3) . ?
C31 C32 1.396(3) . ?
C31 C36 1.533(3) . ?
C32 C33 1.386(3) . ?
C33 C34 1.382(3) . ?
C33 C35 1.506(3) . ?
C36 C43 1.547(3) . ?
C36 C37 1.547(3) . ?
C36 C45 1.550(3) . ?
C37 C38 1.526(3) . ?
C38 C39 1.526(4) . ?
C38 C44 1.536(4) . ?
C39 C40 1.527(4) . ?
C40 C45 1.522(3) . ?
C40 C41 1.531(4) . ?
C41 C42 1.530(3) . ?
C42 C44 1.528(3) . ?
C42 C43 1.533(3) . ?
C46 C47 1.522(3) . ?
C47 C52 1.380(3) . ?
C47 C48 1.403(3) . ?
C48 C49 1.409(3) . ?
C49 C50 1.391(3) . ?
C49 C54 1.533(3) . ?
C50 C51 1.391(3) . ?
C51 C52 1.384(3) . ?
C51 C53 1.506(3) . ?
C54 C61 1.544(3) . ?
C54 C63 1.545(3) . ?
C54 C55 1.547(3) . ?
C55 C56 1.539(4) . ?
C56 C57 1.520(4) . ?
C56 C62 1.521(4) . ?
C57 C58 1.536(3) . ?
C58 C59 1.524(4) . ?
C58 C63 1.540(3) . ?
C59 C60 1.529(3) . ?
C60 C62 1.529(4) . ?
C60 C61 1.533(4) . ?
O4 C66 1.433(4) . ?
O4 C65 1.439(4) . ?
C64 C65 1.486(5) . ?
C66 C67 1.508(6) . ?
O5 C70 1.422(3) . ?
O5 C69 1.427(3) . ?
C68 C69 1.491(4) . ?
C70 C71 1.501(4) . ?
O6 C74 1.427(3) . ?
O6 C73 1.434(3) . ?
C72 C73 1.496(4) . ?
C74 C75 1.504(3) . ?

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
C2 C1 C6 120.1(2) . . ?
C2 C1 C10 119.8(2) . . ?
C6 C1 C10 120.1(2) . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 C7 119.3(2) . . ?
C1 C2 C7 120.4(2) . . ?
C2 C3 C4 119.7(2) . . ?
C2 C3 C28 119.9(2) . . ?
C4 C3 C28 120.3(2) . . ?
C5 C4 C3 120.1(2) . . ?
C5 C4 C8 120.6(2) . . ?
C3 C4 C8 119.3(2) . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 C46 119.8(2) . . ?
C6 C5 C46 119.9(2) . . ?
C1 C6 C5 119.6(2) . . ?
C1 C6 C9 120.2(2) . . ?
C5 C6 C9 120.2(2) . . ?
C1 C10 C11 113.95(19) . . ?
C16 C11 C12 118.4(2) . . ?
C16 C11 C10 121.7(2) . . ?
C12 C11 C10 119.9(2) . . ?
O1 C12 C13 119.1(2) . . ?
O1 C12 C11 118.8(2) . . ?
C13 C12 C11 122.0(2) . . ?
C12 C13 C14 116.6(2) . . ?
C12 C13 C18 122.5(2) . . ?
C14 C13 C18 120.9(2) . . ?
C15 C14 C13 123.1(2) . . ?
C16 C15 C14 118.1(2) . . ?
C16 C15 C17 121.0(2) . . ?
C14 C15 C17 120.9(2) . . ?
C15 C16 C11 121.6(2) . . ?
C13 C18 C25 111.92(19) . . ?
C13 C18 C19 111.72(18) . . ?
C25 C18 C19 107.33(18) . . ?
C13 C18 C27 109.91(18) . . ?
C25 C18 C27 106.77(18) . . ?
C19 C18 C27 109.02(19) . . ?
C20 C19 C18 110.62(19) . . ?
C26 C20 C19 110.2(2) . . ?
C26 C20 C21 109.1(2) . . ?
C19 C20 C21 109.62(19) . . ?
C22 C21 C20 109.2(2) . . ?
C23 C22 C21 110.1(2) . . ?
C23 C22 C27 109.8(2) . . ?
C21 C22 C27 109.44(19) . . ?
C22 C23 C24 108.35(19) . . ?
C26 C24 C25 109.3(2) . . ?
C26 C24 C23 110.0(2) . . ?
C25 C24 C23 109.76(19) . . ?
C24 C25 C18 111.80(19) . . ?
C24 C26 C20 109.01(19) . . ?
C22 C27 C18 110.89(19) . . ?
C3 C28 C29 114.64(19) . . ?
C34 C29 C30 118.8(2) . . ?
C34 C29 C28 121.7(2) . . ?
C30 C29 C28 119.5(2) . . ?
O2 C30 C29 116.9(2) . . ?
O2 C30 C31 121.3(2) . . ?
C29 C30 C31 121.6(2) . . ?
C32 C31 C30 116.5(2) . . ?
C32 C31 C36 120.5(2) . . ?
C30 C31 C36 123.1(2) . . ?
C33 C32 C31 123.6(2) . . ?
C34 C33 C32 117.9(2) . . ?
C34 C33 C35 121.8(2) . . ?
C32 C33 C35 120.2(2) . . ?
C33 C34 C29 121.7(2) . . ?
C31 C36 C43 110.82(19) . . ?
C31 C36 C37 111.43(19) . . ?
C43 C36 C37 109.14(19) . . ?
C31 C36 C45 112.03(19) . . ?
C43 C36 C45 106.53(19) . . ?
C37 C36 C45 106.68(19) . . ?
C38 C37 C36 111.0(2) . . ?
C37 C38 C39 110.1(2) . . ?
C37 C38 C44 109.5(2) . . ?
C39 C38 C44 109.3(2) . . ?
C38 C39 C40 108.8(2) . . ?
C45 C40 C39 109.8(2) . . ?
C45 C40 C41 109.9(2) . . ?
C39 C40 C41 109.5(2) . . ?
C42 C41 C40 108.9(2) . . ?
C44 C42 C41 109.3(2) . . ?
C44 C42 C43 109.4(2) . . ?
C41 C42 C43 109.5(2) . . ?
C42 C43 C36 111.30(19) . . ?
C42 C44 C38 109.7(2) . . ?
C40 C45 C36 111.8(2) . . ?
C5 C46 C47 114.06(18) . . ?
C52 C47 C48 118.7(2) . . ?
C52 C47 C46 121.6(2) . . ?
C48 C47 C46 119.7(2) . . ?
O3 C48 C47 120.6(2) . . ?
O3 C48 C49 118.0(2) . . ?
C47 C48 C49 121.4(2) . . ?
C50 C49 C48 116.6(2) . . ?
C50 C49 C54 121.6(2) . . ?
C48 C49 C54 121.9(2) . . ?
C49 C50 C51 123.5(2) . . ?
C52 C51 C50 117.6(2) . . ?
C52 C51 C53 121.3(2) . . ?
C50 C51 C53 121.1(2) . . ?
C47 C52 C51 122.1(2) . . ?
C49 C54 C61 110.56(19) . . ?
C49 C54 C63 111.00(19) . . ?
C61 C54 C63 109.3(2) . . ?
C49 C54 C55 111.5(2) . . ?
C61 C54 C55 107.1(2) . . ?
C63 C54 C55 107.16(19) . . ?
C56 C55 C54 110.9(2) . . ?
C57 C56 C62 110.0(2) . . ?
C57 C56 C55 109.2(2) . . ?
C62 C56 C55 110.1(2) . . ?
C56 C57 C58 109.1(2) . . ?
C59 C58 C57 109.8(2) . . ?
C59 C58 C63 109.2(2) . . ?
C57 C58 C63 109.2(2) . . ?
C58 C59 C60 110.2(2) . . ?
C62 C60 C59 109.4(2) . . ?
C62 C60 C61 109.2(2) . . ?
C59 C60 C61 109.3(2) . . ?
C60 C61 C54 111.2(2) . . ?
C56 C62 C60 109.3(2) . . ?
C58 C63 C54 110.7(2) . . ?
C66 O4 C65 114.8(3) . . ?
O4 C65 C64 109.2(2) . . ?
O4 C66 C67 107.8(3) . . ?
C70 O5 C69 112.01(19) . . ?
O5 C69 C68 108.5(2) . . ?
O5 C70 C71 108.9(2) . . ?
C74 O6 C73 112.79(19) . . ?
O6 C73 C72 108.7(2) . . ?
O6 C74 C75 114.1(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O4 0.90(3) 1.87(3) 2.757(2) 168(3) .
O2 H2 O5 0.81(4) 2.08(4) 2.877(3) 169(4) .
O3 H3 O6 0.87(3) 2.01(3) 2.823(3) 155(3) .

_refine_diff_density_max         0.289
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_ctp64
_database_code_depnum_ccdc_archive 'CCDC 1538990'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C63 H75 Er O3'
_chemical_formula_weight         1047.49

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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                   12.7631(14)
_cell_length_b                   15.6460(17)
_cell_length_c                   29.910(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.4368(15)
_cell_angle_gamma                90
_cell_volume                     5935.2(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9996
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      26.24

_exptl_crystal_description       rod
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_F_000             2180
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.454
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6949
_exptl_absorpt_correction_T_max  0.8013
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64185
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.370
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12175
_reflns_number_gt                9178
_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. 
  
 Structure factors included contributions from the .fab file. 
  
 _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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A pink crystal of approximate dimensions 0.030 x 0.035 x 0.224 mm was mounted 
in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  The 
APEX2 program package was used to determine the unit-cell parameters and for 
data collection (90 sec/frame scan time for a sphere of diffraction data).  The 
raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were consistent 
with the monoclinic space group P21/c that was later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis.  Hydrogen atoms were included using a riding
model.

At convergence, wR2 = 0.0741 and Goof = 0.985 for 610 variables refined against 
12175 data (0.80Å), R1 = 0.0335 for those 9178 data with I > 2.0sigma(I).  

There were several high residuals present in the final difference-Fourier map.  
It was not possible to determine the nature of the residuals although it was 
probable that diethyether or hexane solvents were present.  The 
SQUEEZE routine in the PLATON program package was used to account for the 
electrons in the solvent accessible voids.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12175
_refine_ls_number_parameters     610
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0741
_refine_ls_wR_factor_gt          0.0672
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_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
Er1 Er 0.56429(2) 0.31245(2) 0.31072(2) 0.01589(5) Uani 1 1 d . . . . .
O1 O 0.40162(16) 0.32706(13) 0.30776(7) 0.0194(5) Uani 1 1 d . . . . .
O2 O 0.64266(16) 0.42771(13) 0.30509(7) 0.0184(5) Uani 1 1 d . . . . .
O3 O 0.63085(17) 0.22774(13) 0.35940(7) 0.0210(5) Uani 1 1 d . . . . .
C1 C 0.5556(3) 0.16627(19) 0.26138(10) 0.0196(7) Uani 1 1 d . . . . .
C2 C 0.4822(2) 0.2227(2) 0.23808(11) 0.0208(7) Uani 1 1 d . . . . .
C3 C 0.5178(2) 0.29710(18) 0.21801(10) 0.0184(7) Uani 1 1 d . . . . .
C4 C 0.6248(2) 0.32057(19) 0.22590(10) 0.0185(7) Uani 1 1 d . . . . .
C5 C 0.6990(2) 0.26557(19) 0.24990(10) 0.0186(7) Uani 1 1 d . . . . .
C6 C 0.6633(2) 0.1888(2) 0.26824(10) 0.0198(7) Uani 1 1 d . . . . .
C7 C 0.5188(3) 0.08086(19) 0.27715(11) 0.0230(8) Uani 1 1 d . . . . .
H7A H 0.4641 0.0579 0.2548 0.034 Uiso 1 1 calc R U . . .
H7B H 0.4899 0.0881 0.3059 0.034 Uiso 1 1 calc R U . . .
H7C H 0.5785 0.0411 0.2810 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4427(3) 0.3485(2) 0.18590(11) 0.0256(8) Uani 1 1 d . . . . .
H8A H 0.3854 0.3115 0.1727 0.038 Uiso 1 1 calc R U . . .
H8B H 0.4807 0.3718 0.1619 0.038 Uiso 1 1 calc R U . . .
H8C H 0.4134 0.3955 0.2022 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8149(2) 0.2863(2) 0.25415(12) 0.0253(8) Uani 1 1 d . . . . .
H9A H 0.8274 0.3322 0.2331 0.038 Uiso 1 1 calc R U . . .
H9B H 0.8546 0.2353 0.2472 0.038 Uiso 1 1 calc R U . . .
H9C H 0.8380 0.3049 0.2850 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3648(2) 0.20403(19) 0.23757(11) 0.0233(8) Uani 1 1 d . . . . .
H10A H 0.3403 0.1767 0.2084 0.028 Uiso 1 1 calc R U . . .
H10B H 0.3566 0.1613 0.2614 0.028 Uiso 1 1 calc R U . . .
C11 C 0.2910(3) 0.2780(2) 0.24418(11) 0.0213(7) Uani 1 1 d . . . . .
C12 C 0.3115(2) 0.33493(19) 0.28050(11) 0.0201(7) Uani 1 1 d . . . . .
C13 C 0.2361(2) 0.4000(2) 0.28728(10) 0.0195(7) Uani 1 1 d . . . . .
C14 C 0.1455(3) 0.4040(2) 0.25652(11) 0.0237(8) Uani 1 1 d . . . . .
H14A H 0.0946 0.4467 0.2608 0.028 Uiso 1 1 calc R U . . .
C15 C 0.1258(2) 0.3495(2) 0.22034(11) 0.0234(8) Uani 1 1 d . . . . .
C16 C 0.1993(3) 0.2861(2) 0.21489(11) 0.0237(8) Uani 1 1 d . . . . .
H16A H 0.1865 0.2473 0.1905 0.028 Uiso 1 1 calc R U . . .
C17 C 0.0279(3) 0.3584(2) 0.18707(12) 0.0318(9) Uani 1 1 d . . . . .
H17A H -0.0218 0.3974 0.1993 0.048 Uiso 1 1 calc R U . . .
H17B H -0.0052 0.3022 0.1818 0.048 Uiso 1 1 calc R U . . .
H17C H 0.0473 0.3813 0.1586 0.048 Uiso 1 1 calc R U . . .
C18 C 0.2542(2) 0.4633(2) 0.32662(10) 0.0201(7) Uani 1 1 d . . . . .
C19 C 0.2662(3) 0.4153(2) 0.37195(11) 0.0235(8) Uani 1 1 d . . . . .
H19A H 0.2011 0.3825 0.3751 0.028 Uiso 1 1 calc R U . . .
H19B H 0.3255 0.3744 0.3727 0.028 Uiso 1 1 calc R U . . .
C20 C 0.2868(3) 0.4784(2) 0.41138(11) 0.0266(8) Uani 1 1 d . . . . .
H20A H 0.2961 0.4460 0.4404 0.032 Uiso 1 1 calc R U . . .
C21 C 0.3874(3) 0.5302(2) 0.40624(11) 0.0278(8) Uani 1 1 d . . . . .
H21A H 0.4019 0.5699 0.4320 0.033 Uiso 1 1 calc R U . . .
H21B H 0.4483 0.4910 0.4061 0.033 Uiso 1 1 calc R U . . .
C22 C 0.3730(3) 0.5806(2) 0.36249(11) 0.0250(8) Uani 1 1 d . . . . .
H22A H 0.4384 0.6144 0.3594 0.030 Uiso 1 1 calc R U . . .
C23 C 0.2794(3) 0.6413(2) 0.36256(12) 0.0277(8) Uani 1 1 d . . . . .
H23A H 0.2705 0.6746 0.3342 0.033 Uiso 1 1 calc R U . . .
H23B H 0.2921 0.6819 0.3880 0.033 Uiso 1 1 calc R U . . .
C24 C 0.1799(3) 0.5891(2) 0.36711(11) 0.0266(8) Uani 1 1 d . . . . .
H24A H 0.1179 0.6283 0.3667 0.032 Uiso 1 1 calc R U . . .
C25 C 0.1615(3) 0.5258(2) 0.32770(11) 0.0252(8) Uani 1 1 d . . . . .
H25A H 0.1517 0.5580 0.2991 0.030 Uiso 1 1 calc R U . . .
H25B H 0.0962 0.4930 0.3304 0.030 Uiso 1 1 calc R U . . .
C26 C 0.3530(2) 0.5180(2) 0.32271(11) 0.0222(7) Uani 1 1 d . . . . .
H26A H 0.3437 0.5506 0.2942 0.027 Uiso 1 1 calc R U . . .
H26B H 0.4150 0.4802 0.3220 0.027 Uiso 1 1 calc R U . . .
C27 C 0.1934(3) 0.5397(2) 0.41142(11) 0.0305(9) Uani 1 1 d . . . . .
H27A H 0.1284 0.5071 0.4150 0.037 Uiso 1 1 calc R U . . .
H27B H 0.2061 0.5801 0.4369 0.037 Uiso 1 1 calc R U . . .
C28 C 0.6585(2) 0.40795(19) 0.20945(10) 0.0193(7) Uani 1 1 d . . . . .
H28A H 0.6943 0.3984 0.1822 0.023 Uiso 1 1 calc R U . . .
H28B H 0.5936 0.4411 0.2001 0.023 Uiso 1 1 calc R U . . .
C29 C 0.7304(2) 0.46388(19) 0.24148(11) 0.0196(7) Uani 1 1 d . . . . .
C30 C 0.7204(2) 0.47074(18) 0.28794(11) 0.0170(7) Uani 1 1 d . . . . .
C31 C 0.7929(2) 0.52116(19) 0.31562(11) 0.0191(7) Uani 1 1 d . . . . .
C32 C 0.8681(2) 0.5670(2) 0.29497(11) 0.0208(7) Uani 1 1 d . . . . .
H32A H 0.9172 0.6011 0.3133 0.025 Uiso 1 1 calc R U . . .
C33 C 0.8750(2) 0.5651(2) 0.24883(12) 0.0249(8) Uani 1 1 d . . . . .
C34 C 0.8065(2) 0.51200(19) 0.22318(11) 0.0216(7) Uani 1 1 d . . . . .
H34A H 0.8114 0.5081 0.1918 0.026 Uiso 1 1 calc R U . . .
C35 C 0.9540(3) 0.6202(2) 0.22808(13) 0.0368(9) Uani 1 1 d . . . . .
H35A H 1.0074 0.6409 0.2517 0.055 Uiso 1 1 calc R U . . .
H35B H 0.9177 0.6690 0.2128 0.055 Uiso 1 1 calc R U . . .
H35C H 0.9882 0.5864 0.2063 0.055 Uiso 1 1 calc R U . . .
C36 C 0.7891(2) 0.5274(2) 0.36660(11) 0.0215(7) Uani 1 1 d . . . . .
C37 C 0.8010(3) 0.4384(2) 0.38880(11) 0.0248(8) Uani 1 1 d . . . . .
H37A H 0.7451 0.4001 0.3746 0.030 Uiso 1 1 calc R U . . .
H37B H 0.8700 0.4137 0.3836 0.030 Uiso 1 1 calc R U . . .
C38 C 0.7935(3) 0.4431(2) 0.43947(11) 0.0305(8) Uani 1 1 d . . . . .
H38A H 0.7994 0.3843 0.4526 0.037 Uiso 1 1 calc R U . . .
C39 C 0.8833(3) 0.4986(3) 0.46153(12) 0.0403(10) Uani 1 1 d . . . . .
H39A H 0.8792 0.5023 0.4943 0.048 Uiso 1 1 calc R U . . .
H39B H 0.9520 0.4729 0.4567 0.048 Uiso 1 1 calc R U . . .
C40 C 0.8743(3) 0.5877(2) 0.44077(12) 0.0372(10) Uani 1 1 d . . . . .
H40A H 0.9337 0.6240 0.4547 0.045 Uiso 1 1 calc R U . . .
C41 C 0.7694(3) 0.6277(3) 0.44991(12) 0.0393(10) Uani 1 1 d . . . . .
H41A H 0.7659 0.6313 0.4828 0.047 Uiso 1 1 calc R U . . .
H41B H 0.7638 0.6863 0.4374 0.047 Uiso 1 1 calc R U . . .
C42 C 0.6783(3) 0.5730(2) 0.42811(11) 0.0272(8) Uani 1 1 d . . . . .
H42A H 0.6096 0.5989 0.4341 0.033 Uiso 1 1 calc R U . . .
C43 C 0.6844(2) 0.5687(2) 0.37717(10) 0.0218(7) Uani 1 1 d . . . . .
H43A H 0.6788 0.6271 0.3644 0.026 Uiso 1 1 calc R U . . .
H43B H 0.6243 0.5348 0.3628 0.026 Uiso 1 1 calc R U . . .
C44 C 0.8785(3) 0.5833(2) 0.39017(11) 0.0308(9) Uani 1 1 d . . . . .
H44A H 0.9474 0.5594 0.3841 0.037 Uiso 1 1 calc R U . . .
H44B H 0.8728 0.6417 0.3775 0.037 Uiso 1 1 calc R U . . .
C45 C 0.6875(3) 0.4825(2) 0.44788(11) 0.0324(9) Uani 1 1 d . . . . .
H45A H 0.6822 0.4848 0.4806 0.039 Uiso 1 1 calc R U . . .
H45B H 0.6291 0.4466 0.4337 0.039 Uiso 1 1 calc R U . . .
C46 C 0.7432(3) 0.1338(2) 0.29712(11) 0.0215(7) Uani 1 1 d . . . . .
H46A H 0.7616 0.0849 0.2784 0.026 Uiso 1 1 calc R U . . .
H46B H 0.8081 0.1682 0.3041 0.026 Uiso 1 1 calc R U . . .
C47 C 0.7136(2) 0.0978(2) 0.34124(11) 0.0214(7) Uani 1 1 d . . . . .
C48 C 0.6605(2) 0.1470(2) 0.37105(11) 0.0199(7) Uani 1 1 d . . . . .
C49 C 0.6364(3) 0.1103(2) 0.41193(11) 0.0231(7) Uani 1 1 d . . . . .
C50 C 0.6718(3) 0.0274(2) 0.42154(11) 0.0280(8) Uani 1 1 d . . . . .
H50A H 0.6571 0.0027 0.4492 0.034 Uiso 1 1 calc R U . . .
C51 C 0.7270(3) -0.0211(2) 0.39350(12) 0.0284(8) Uani 1 1 d . . . . .
C52 C 0.7461(3) 0.0151(2) 0.35302(11) 0.0256(8) Uani 1 1 d . . . . .
H52A H 0.7823 -0.0174 0.3327 0.031 Uiso 1 1 calc R U . . .
C53 C 0.7649(3) -0.1102(2) 0.40655(13) 0.0397(10) Uani 1 1 d . . . . .
H53A H 0.7042 -0.1464 0.4110 0.060 Uiso 1 1 calc R U . . .
H53B H 0.8127 -0.1076 0.4345 0.060 Uiso 1 1 calc R U . . .
H53C H 0.8022 -0.1343 0.3826 0.060 Uiso 1 1 calc R U . . .
C54 C 0.5741(3) 0.1598(2) 0.44475(11) 0.0238(8) Uani 1 1 d . . . . .
C55 C 0.6354(3) 0.2408(2) 0.46189(11) 0.0264(8) Uani 1 1 d . . . . .
H55A H 0.7046 0.2243 0.4777 0.032 Uiso 1 1 calc R U . . .
H55B H 0.6479 0.2775 0.4360 0.032 Uiso 1 1 calc R U . . .
C56 C 0.5723(3) 0.2910(2) 0.49405(12) 0.0354(10) Uani 1 1 d . . . . .
H56A H 0.6122 0.3437 0.5043 0.042 Uiso 1 1 calc R U . . .
C57 C 0.5576(3) 0.2356(2) 0.53482(12) 0.0405(10) Uani 1 1 d . . . . .
H57A H 0.5196 0.2682 0.5564 0.049 Uiso 1 1 calc R U . . .
H57B H 0.6272 0.2185 0.5502 0.049 Uiso 1 1 calc R U . . .
C58 C 0.4938(3) 0.1558(2) 0.51860(12) 0.0379(10) Uani 1 1 d . . . . .
H58A H 0.4835 0.1189 0.5450 0.046 Uiso 1 1 calc R U . . .
C59 C 0.3864(3) 0.1818(3) 0.49487(13) 0.0435(10) Uani 1 1 d . . . . .
H59A H 0.3451 0.1301 0.4852 0.052 Uiso 1 1 calc R U . . .
H59B H 0.3468 0.2145 0.5158 0.052 Uiso 1 1 calc R U . . .
C60 C 0.4026(3) 0.2365(2) 0.45406(12) 0.0358(9) Uani 1 1 d . . . . .
H60A H 0.3327 0.2539 0.4383 0.043 Uiso 1 1 calc R U . . .
C61 C 0.4640(3) 0.1850(2) 0.42181(11) 0.0295(8) Uani 1 1 d . . . . .
H61A H 0.4719 0.2197 0.3947 0.035 Uiso 1 1 calc R U . . .
H61B H 0.4239 0.1328 0.4122 0.035 Uiso 1 1 calc R U . . .
C62 C 0.5563(3) 0.1059(2) 0.48604(11) 0.0326(9) Uani 1 1 d . . . . .
H62A H 0.6254 0.0887 0.5019 0.039 Uiso 1 1 calc R U . . .
H62B H 0.5173 0.0533 0.4761 0.039 Uiso 1 1 calc R U . . .
C63 C 0.4664(3) 0.3164(2) 0.46971(13) 0.0420(10) Uani 1 1 d . . . . .
H63A H 0.4772 0.3523 0.4434 0.050 Uiso 1 1 calc R U . . .
H63B H 0.4267 0.3504 0.4901 0.050 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
Er1 Cnt 2.336 . ?
Er1 O2 2.078(2) . ?
Er1 O3 2.079(2) . ?
Er1 O1 2.081(2) . ?
Er1 C2 2.698(3) . ?
Er1 C6 2.704(3) . ?
Er1 C1 2.717(3) . ?
Er1 C4 2.736(3) . ?
Er1 C5 2.739(3) . ?
Er1 C3 2.780(3) . ?
O1 C12 1.339(4) . ?
O2 C30 1.348(3) . ?
O3 C48 1.353(4) . ?
C1 C6 1.411(4) . ?
C1 C2 1.413(4) . ?
C1 C7 1.510(4) . ?
C2 C3 1.408(4) . ?
C2 C10 1.525(4) . ?
C3 C4 1.409(4) . ?
C3 C8 1.510(4) . ?
C4 C5 1.414(4) . ?
C4 C28 1.531(4) . ?
C5 C6 1.416(4) . ?
C5 C9 1.506(4) . ?
C6 C46 1.527(4) . ?
C10 C11 1.518(4) . ?
C11 C16 1.387(4) . ?
C11 C12 1.407(4) . ?
C12 C13 1.431(4) . ?
C13 C14 1.396(4) . ?
C13 C18 1.535(4) . ?
C14 C15 1.379(4) . ?
C15 C16 1.387(5) . ?
C15 C17 1.514(4) . ?
C18 C25 1.538(4) . ?
C18 C26 1.540(4) . ?
C18 C19 1.542(4) . ?
C19 C20 1.538(4) . ?
C20 C27 1.531(4) . ?
C20 C21 1.541(5) . ?
C21 C22 1.521(4) . ?
C22 C23 1.527(4) . ?
C22 C26 1.541(4) . ?
C23 C24 1.530(5) . ?
C24 C27 1.527(5) . ?
C24 C25 1.537(4) . ?
C28 C29 1.526(4) . ?
C29 C34 1.389(4) . ?
C29 C30 1.414(4) . ?
C30 C31 1.411(4) . ?
C31 C32 1.396(4) . ?
C31 C36 1.534(4) . ?
C32 C33 1.393(4) . ?
C33 C34 1.376(4) . ?
C33 C35 1.511(4) . ?
C36 C44 1.543(4) . ?
C36 C37 1.544(4) . ?
C36 C43 1.548(4) . ?
C37 C38 1.531(4) . ?
C38 C39 1.528(5) . ?
C38 C45 1.533(5) . ?
C39 C40 1.525(5) . ?
C40 C44 1.522(5) . ?
C40 C41 1.530(5) . ?
C41 C42 1.529(5) . ?
C42 C45 1.534(5) . ?
C42 C43 1.536(4) . ?
C46 C47 1.521(4) . ?
C47 C52 1.392(4) . ?
C47 C48 1.408(4) . ?
C48 C49 1.416(4) . ?
C49 C50 1.392(4) . ?
C49 C54 1.540(4) . ?
C50 C51 1.382(5) . ?
C51 C52 1.383(4) . ?
C51 C53 1.511(4) . ?
C54 C62 1.533(4) . ?
C54 C61 1.544(5) . ?
C54 C55 1.547(4) . ?
C55 C56 1.537(4) . ?
C56 C63 1.515(5) . ?
C56 C57 1.524(5) . ?
C57 C58 1.540(5) . ?
C58 C59 1.526(6) . ?
C58 C62 1.539(5) . ?
C59 C60 1.524(5) . ?
C60 C63 1.535(5) . ?
C60 C61 1.537(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cnt Er1 O1 104.6 . . ?
Cnt Er1 O2 102.4 . . ?
Cnt Er1 O3 102.8 . . ?
O2 Er1 O3 116.58(8) . . ?
O2 Er1 O1 112.85(8) . . ?
O3 Er1 O1 115.29(8) . . ?
O2 Er1 C2 122.24(9) . . ?
O3 Er1 C2 108.87(9) . . ?
O1 Er1 C2 74.16(9) . . ?
O2 Er1 C6 109.15(9) . . ?
O3 Er1 C6 72.38(9) . . ?
O1 Er1 C6 125.11(9) . . ?
C2 Er1 C6 53.79(9) . . ?
O2 Er1 C1 132.61(8) . . ?
O3 Er1 C1 80.34(9) . . ?
O1 Er1 C1 95.14(9) . . ?
C2 Er1 C1 30.26(9) . . ?
C6 Er1 C1 30.18(9) . . ?
O2 Er1 C4 72.31(8) . . ?
O3 Er1 C4 122.91(8) . . ?
O1 Er1 C4 109.84(9) . . ?
C2 Er1 C4 53.29(9) . . ?
C6 Er1 C4 53.29(9) . . ?
C1 Er1 C4 62.23(9) . . ?
O2 Er1 C5 80.50(8) . . ?
O3 Er1 C5 93.26(9) . . ?
O1 Er1 C5 134.32(9) . . ?
C2 Er1 C5 62.74(9) . . ?
C6 Er1 C5 30.15(9) . . ?
C1 Er1 C5 53.44(9) . . ?
C4 Er1 C5 29.93(9) . . ?
O2 Er1 C3 92.58(8) . . ?
O3 Er1 C3 131.94(8) . . ?
O1 Er1 C3 82.33(8) . . ?
C2 Er1 C3 29.74(9) . . ?
C6 Er1 C3 61.86(9) . . ?
C1 Er1 C3 52.74(9) . . ?
C4 Er1 C3 29.57(9) . . ?
C5 Er1 C3 52.72(9) . . ?
C12 O1 Er1 145.17(19) . . ?
C30 O2 Er1 147.80(18) . . ?
C48 O3 Er1 148.90(19) . . ?
C6 C1 C2 119.8(3) . . ?
C6 C1 C7 120.5(3) . . ?
C2 C1 C7 119.6(3) . . ?
C6 C1 Er1 74.38(17) . . ?
C2 C1 Er1 74.12(17) . . ?
C7 C1 Er1 124.8(2) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C10 121.2(3) . . ?
C1 C2 C10 118.8(3) . . ?
C3 C2 Er1 78.36(18) . . ?
C1 C2 Er1 75.62(18) . . ?
C10 C2 Er1 113.61(19) . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 C8 119.9(3) . . ?
C4 C3 C8 120.1(3) . . ?
C2 C3 Er1 71.90(18) . . ?
C4 C3 Er1 73.49(17) . . ?
C8 C3 Er1 129.6(2) . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 C28 118.7(3) . . ?
C5 C4 C28 120.7(3) . . ?
C3 C4 Er1 76.94(17) . . ?
C5 C4 Er1 75.13(17) . . ?
C28 C4 Er1 117.26(19) . . ?
C4 C5 C6 119.1(3) . . ?
C4 C5 C9 120.5(3) . . ?
C6 C5 C9 120.4(3) . . ?
C4 C5 Er1 74.93(17) . . ?
C6 C5 Er1 73.55(16) . . ?
C9 C5 Er1 124.7(2) . . ?
C1 C6 C5 120.4(3) . . ?
C1 C6 C46 121.2(3) . . ?
C5 C6 C46 118.3(3) . . ?
C1 C6 Er1 75.44(17) . . ?
C5 C6 Er1 76.30(17) . . ?
C46 C6 Er1 117.11(19) . . ?
C11 C10 C2 118.4(3) . . ?
C16 C11 C12 120.0(3) . . ?
C16 C11 C10 118.6(3) . . ?
C12 C11 C10 121.3(3) . . ?
O1 C12 C11 119.0(3) . . ?
O1 C12 C13 121.6(3) . . ?
C11 C12 C13 119.4(3) . . ?
C14 C13 C12 117.3(3) . . ?
C14 C13 C18 121.2(3) . . ?
C12 C13 C18 121.4(3) . . ?
C15 C14 C13 123.7(3) . . ?
C14 C15 C16 117.9(3) . . ?
C14 C15 C17 121.6(3) . . ?
C16 C15 C17 120.5(3) . . ?
C11 C16 C15 121.7(3) . . ?
C13 C18 C25 112.1(3) . . ?
C13 C18 C26 110.8(2) . . ?
C25 C18 C26 106.6(3) . . ?
C13 C18 C19 110.6(3) . . ?
C25 C18 C19 106.9(2) . . ?
C26 C18 C19 109.6(3) . . ?
C20 C19 C18 110.7(3) . . ?
C27 C20 C19 109.6(3) . . ?
C27 C20 C21 109.2(3) . . ?
C19 C20 C21 109.5(3) . . ?
C22 C21 C20 109.7(3) . . ?
C21 C22 C23 109.9(3) . . ?
C21 C22 C26 109.2(3) . . ?
C23 C22 C26 109.6(3) . . ?
C22 C23 C24 109.0(3) . . ?
C27 C24 C23 109.5(3) . . ?
C27 C24 C25 109.4(3) . . ?
C23 C24 C25 109.4(3) . . ?
C24 C25 C18 112.0(3) . . ?
C18 C26 C22 111.2(2) . . ?
C24 C27 C20 109.2(3) . . ?
C29 C28 C4 118.7(3) . . ?
C34 C29 C30 119.3(3) . . ?
C34 C29 C28 117.5(3) . . ?
C30 C29 C28 123.2(3) . . ?
O2 C30 C31 121.2(3) . . ?
O2 C30 C29 119.2(3) . . ?
C31 C30 C29 119.6(3) . . ?
C32 C31 C30 117.7(3) . . ?
C32 C31 C36 120.4(3) . . ?
C30 C31 C36 121.8(3) . . ?
C33 C32 C31 123.4(3) . . ?
C34 C33 C32 117.2(3) . . ?
C34 C33 C35 121.8(3) . . ?
C32 C33 C35 121.0(3) . . ?
C33 C34 C29 122.5(3) . . ?
C31 C36 C44 112.7(3) . . ?
C31 C36 C37 110.9(3) . . ?
C44 C36 C37 106.4(3) . . ?
C31 C36 C43 110.7(3) . . ?
C44 C36 C43 106.4(3) . . ?
C37 C36 C43 109.5(3) . . ?
C38 C37 C36 111.6(3) . . ?
C39 C38 C37 109.1(3) . . ?
C39 C38 C45 109.5(3) . . ?
C37 C38 C45 109.7(3) . . ?
C40 C39 C38 109.0(3) . . ?
C44 C40 C39 110.7(3) . . ?
C44 C40 C41 109.0(3) . . ?
C39 C40 C41 109.2(3) . . ?
C42 C41 C40 109.5(3) . . ?
C41 C42 C45 109.3(3) . . ?
C41 C42 C43 109.1(3) . . ?
C45 C42 C43 109.4(3) . . ?
C42 C43 C36 111.2(3) . . ?
C40 C44 C36 111.9(3) . . ?
C38 C45 C42 109.8(3) . . ?
C47 C46 C6 119.0(3) . . ?
C52 C47 C48 119.9(3) . . ?
C52 C47 C46 117.9(3) . . ?
C48 C47 C46 122.1(3) . . ?
O3 C48 C47 119.2(3) . . ?
O3 C48 C49 121.3(3) . . ?
C47 C48 C49 119.4(3) . . ?
C50 C49 C48 117.3(3) . . ?
C50 C49 C54 121.1(3) . . ?
C48 C49 C54 121.6(3) . . ?
C51 C50 C49 124.2(3) . . ?
C50 C51 C52 117.3(3) . . ?
C50 C51 C53 121.3(3) . . ?
C52 C51 C53 121.4(3) . . ?
C51 C52 C47 121.7(3) . . ?
C62 C54 C49 111.7(3) . . ?
C62 C54 C61 106.8(3) . . ?
C49 C54 C61 110.8(3) . . ?
C62 C54 C55 107.4(3) . . ?
C49 C54 C55 110.2(3) . . ?
C61 C54 C55 109.8(3) . . ?
C56 C55 C54 110.2(3) . . ?
C63 C56 C57 110.5(3) . . ?
C63 C56 C55 109.6(3) . . ?
C57 C56 C55 109.3(3) . . ?
C56 C57 C58 108.5(3) . . ?
C59 C58 C62 110.1(3) . . ?
C59 C58 C57 110.3(3) . . ?
C62 C58 C57 108.5(3) . . ?
C60 C59 C58 109.1(3) . . ?
C59 C60 C63 109.2(3) . . ?
C59 C60 C61 109.4(3) . . ?
C63 C60 C61 109.2(3) . . ?
C60 C61 C54 110.9(3) . . ?
C54 C62 C58 111.3(3) . . ?
C56 C63 C60 110.3(3) . . ?

_refine_diff_density_max         0.751
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.090



####################################################################### 
# 
# 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_mef38
_database_code_depnum_ccdc_archive 'CCDC 1538987'
_audit_update_record             
;
2017-03-19 deposited with the CCDC.
2017-09-07 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            'C63 H75 Nd O3'
_chemical_formula_weight         1024.47

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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                   11.5124(10)
_cell_length_b                   36.810(3)
_cell_length_c                   11.9512(10)
_cell_angle_alpha                90
_cell_angle_beta                 106.7298(9)
_cell_angle_gamma                90
_cell_volume                     4850.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      26.35

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             2148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.071
_exptl_absorpt_coefficient_mu    1.119
_shelx_estimated_absorpt_T_min   0.729
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6830
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44017
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.847
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8875
_reflns_number_gt                7703
_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       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A blue crystal of approximate dimensions 0.301 x 0.088 x 0.071 mm 
was mounted on a glass fiber and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine 
the unit-cell parameters and for data collection (120 sec/frame 
scan time for a sphere of diffraction data).  The raw frame data 
was processed using SAINT and SADABS to yield the reflection data 
file.  Subsequent calculations were carried out using the SHELXTL 
program.  The diffraction symmetry was 2/m and the systematic 
absences were consistent with the monoclinic space group P21/c 
that was later determined to be correct.

The structure was solved using the coordinates from mef30, the La 
analog.  The analytical scattering factors for neutral atoms were 
used throughout the analysis.  Hydrogen atoms were included using 
a riding model.

At convergence, wR2 = 0.0850 and Goof = 1.228 for 610 variables 
refined against 8875 data (0.83 Å), R1 = 0.0453 for those 7703 
data with I > 2.0sigma(I).  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0177P)²+10.9217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8875
_refine_ls_number_parameters     610
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_restrained_S_all      1.228
_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
Nd1 Nd 0.36874(2) 0.09893(2) 0.80119(2) 0.01309(6) Uani 1 1 d . . . . .
O1 O 0.2956(2) 0.04431(7) 0.7671(2) 0.0158(6) Uani 1 1 d . . . . .
O2 O 0.3206(2) 0.13976(7) 0.6624(2) 0.0193(6) Uani 1 1 d . . . . .
O3 O 0.4230(2) 0.11087(7) 0.9896(2) 0.0185(6) Uani 1 1 d . . . . .
C1 C 0.5961(3) 0.06369(11) 0.8822(3) 0.0160(8) Uani 1 1 d . . . . .
C2 C 0.5450(3) 0.04936(10) 0.7678(3) 0.0147(8) Uani 1 1 d . . . . .
C3 C 0.5194(3) 0.07280(11) 0.6697(3) 0.0160(8) Uani 1 1 d . . . . .
C4 C 0.5544(3) 0.10983(10) 0.6843(3) 0.0145(8) Uani 1 1 d . . . . .
C5 C 0.6098(3) 0.12381(11) 0.7982(3) 0.0165(8) Uani 1 1 d . . . . .
C6 C 0.6269(3) 0.10123(11) 0.8962(3) 0.0164(8) Uani 1 1 d . . . . .
C7 C 0.6102(4) 0.03967(11) 0.9881(3) 0.0228(9) Uani 1 1 d . . . . .
H7A H 0.5756 0.0519 1.0439 0.034 Uiso 1 1 calc R U . . .
H7B H 0.6965 0.0349 1.0252 0.034 Uiso 1 1 calc R U . . .
H7C H 0.5677 0.0166 0.9639 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4508(4) 0.05801(11) 0.5506(3) 0.0207(9) Uani 1 1 d . . . . .
H8A H 0.4057 0.0362 0.5603 0.031 Uiso 1 1 calc R U . . .
H8B H 0.5083 0.0518 0.5070 0.031 Uiso 1 1 calc R U . . .
H8C H 0.3940 0.0765 0.5075 0.031 Uiso 1 1 calc R U . . .
C9 C 0.6479(4) 0.16351(11) 0.8127(4) 0.0224(9) Uani 1 1 d . . . . .
H9A H 0.6702 0.1716 0.7435 0.034 Uiso 1 1 calc R U . . .
H9B H 0.7176 0.1662 0.8822 0.034 Uiso 1 1 calc R U . . .
H9C H 0.5803 0.1783 0.8217 0.034 Uiso 1 1 calc R U . . .
C10 C 0.5242(3) 0.00873(11) 0.7489(3) 0.0180(8) Uani 1 1 d . . . . .
H10A H 0.5795 -0.0035 0.8175 0.022 Uiso 1 1 calc R U . . .
H10B H 0.5525 0.0022 0.6808 0.022 Uiso 1 1 calc R U . . .
C11 C 0.3985(3) -0.00891(10) 0.7290(3) 0.0152(8) Uani 1 1 d . . . . .
C12 C 0.2926(3) 0.00873(10) 0.7372(3) 0.0146(8) Uani 1 1 d . . . . .
C13 C 0.1820(3) -0.01182(10) 0.7150(3) 0.0132(8) Uani 1 1 d . . . . .
C14 C 0.1852(3) -0.04844(10) 0.6884(3) 0.0145(8) Uani 1 1 d . . . . .
H14A H 0.1121 -0.0620 0.6738 0.017 Uiso 1 1 calc R U . . .
C15 C 0.2906(3) -0.06658(11) 0.6817(3) 0.0164(8) Uani 1 1 d . . . . .
C16 C 0.3957(3) -0.04624(11) 0.7027(3) 0.0148(8) Uani 1 1 d . . . . .
H16A H 0.4683 -0.0578 0.6991 0.018 Uiso 1 1 calc R U . . .
C17 C 0.2889(4) -0.10631(10) 0.6500(3) 0.0210(9) Uani 1 1 d . . . . .
H17A H 0.2175 -0.1180 0.6634 0.032 Uiso 1 1 calc R U . . .
H17B H 0.3626 -0.1181 0.6985 0.032 Uiso 1 1 calc R U . . .
H17C H 0.2855 -0.1087 0.5674 0.032 Uiso 1 1 calc R U . . .
C18 C 0.0630(3) 0.00573(10) 0.7235(3) 0.0134(8) Uani 1 1 d . . . . .
C19 C 0.0765(3) 0.01724(10) 0.8524(3) 0.0146(8) Uani 1 1 d . . . . .
H19A H 0.0961 -0.0044 0.9038 0.017 Uiso 1 1 calc R U . . .
H19B H 0.1441 0.0348 0.8786 0.017 Uiso 1 1 calc R U . . .
C20 C -0.0417(3) 0.03475(10) 0.8631(3) 0.0160(8) Uani 1 1 d . . . . .
H20A H -0.0307 0.0421 0.9461 0.019 Uiso 1 1 calc R U . . .
C21 C -0.0709(4) 0.06851(11) 0.7840(3) 0.0195(9) Uani 1 1 d . . . . .
H21A H -0.0034 0.0862 0.8081 0.023 Uiso 1 1 calc R U . . .
H21B H -0.1454 0.0803 0.7920 0.023 Uiso 1 1 calc R U . . .
C22 C -0.0894(3) 0.05723(11) 0.6559(3) 0.0193(9) Uani 1 1 d . . . . .
H22A H -0.1089 0.0792 0.6049 0.023 Uiso 1 1 calc R U . . .
C23 C -0.1948(3) 0.03017(11) 0.6190(3) 0.0190(9) Uani 1 1 d . . . . .
H23A H -0.2702 0.0415 0.6262 0.023 Uiso 1 1 calc R U . . .
H23B H -0.2078 0.0230 0.5364 0.023 Uiso 1 1 calc R U . . .
C24 C -0.1636(3) -0.00326(11) 0.6979(3) 0.0149(8) Uani 1 1 d . . . . .
H24A H -0.2314 -0.0212 0.6735 0.018 Uiso 1 1 calc R U . . .
C25 C -0.0458(3) -0.02100(10) 0.6882(3) 0.0157(8) Uani 1 1 d . . . . .
H25A H -0.0574 -0.0292 0.6069 0.019 Uiso 1 1 calc R U . . .
H25B H -0.0275 -0.0426 0.7396 0.019 Uiso 1 1 calc R U . . .
C26 C 0.0271(3) 0.03947(11) 0.6429(3) 0.0178(8) Uani 1 1 d . . . . .
H26A H 0.0940 0.0574 0.6631 0.021 Uiso 1 1 calc R U . . .
H26B H 0.0142 0.0320 0.5606 0.021 Uiso 1 1 calc R U . . .
C27 C -0.1467(3) 0.00766(11) 0.8255(3) 0.0162(8) Uani 1 1 d . . . . .
H27A H -0.2221 0.0189 0.8334 0.019 Uiso 1 1 calc R U . . .
H27B H -0.1288 -0.0141 0.8761 0.019 Uiso 1 1 calc R U . . .
C28 C 0.5364(4) 0.13450(11) 0.5785(3) 0.0194(9) Uani 1 1 d . . . . .
H28A H 0.5056 0.1192 0.5079 0.023 Uiso 1 1 calc R U . . .
H28B H 0.6174 0.1434 0.5781 0.023 Uiso 1 1 calc R U . . .
C29 C 0.4525(3) 0.16769(10) 0.5645(3) 0.0160(8) Uani 1 1 d . . . . .
C30 C 0.3450(3) 0.16779(11) 0.5976(3) 0.0170(8) Uani 1 1 d . . . . .
C31 C 0.2625(3) 0.19763(11) 0.5647(3) 0.0175(8) Uani 1 1 d . . . . .
C32 C 0.2999(4) 0.22707(11) 0.5078(3) 0.0180(8) Uani 1 1 d . . . . .
H32A H 0.2465 0.2472 0.4862 0.022 Uiso 1 1 calc R U . . .
C33 C 0.4096(4) 0.22858(11) 0.4814(3) 0.0179(8) Uani 1 1 d . . . . .
C34 C 0.4836(4) 0.19797(11) 0.5090(3) 0.0187(8) Uani 1 1 d . . . . .
H34A H 0.5579 0.1977 0.4893 0.022 Uiso 1 1 calc R U . . .
C35 C 0.4453(4) 0.26120(11) 0.4218(4) 0.0232(9) Uani 1 1 d . . . . .
H35A H 0.4060 0.2830 0.4410 0.035 Uiso 1 1 calc R U . . .
H35B H 0.4195 0.2575 0.3370 0.035 Uiso 1 1 calc R U . . .
H35C H 0.5335 0.2643 0.4488 0.035 Uiso 1 1 calc R U . . .
C36 C 0.1391(3) 0.19795(11) 0.5911(3) 0.0179(8) Uani 1 1 d . . . . .
C37 C 0.1590(3) 0.20282(11) 0.7245(3) 0.0209(9) Uani 1 1 d . . . . .
H37A H 0.2112 0.1830 0.7673 0.025 Uiso 1 1 calc R U . . .
H37B H 0.2011 0.2261 0.7503 0.025 Uiso 1 1 calc R U . . .
C38 C 0.0376(4) 0.20247(12) 0.7536(4) 0.0253(9) Uani 1 1 d . . . . .
H38A H 0.0525 0.2052 0.8398 0.030 Uiso 1 1 calc R U . . .
C39 C -0.0407(4) 0.23432(12) 0.6899(4) 0.0277(10) Uani 1 1 d . . . . .
H39A H -0.1184 0.2349 0.7097 0.033 Uiso 1 1 calc R U . . .
H39B H 0.0020 0.2576 0.7153 0.033 Uiso 1 1 calc R U . . .
C40 C -0.0653(4) 0.22985(12) 0.5575(4) 0.0246(9) Uani 1 1 d . . . . .
H40A H -0.1160 0.2506 0.5163 0.029 Uiso 1 1 calc R U . . .
C41 C -0.1324(4) 0.19410(12) 0.5185(4) 0.0296(10) Uani 1 1 d . . . . .
H41A H -0.1499 0.1913 0.4328 0.036 Uiso 1 1 calc R U . . .
H41B H -0.2104 0.1941 0.5379 0.036 Uiso 1 1 calc R U . . .
C42 C -0.0533(4) 0.16255(12) 0.5807(4) 0.0270(10) Uani 1 1 d . . . . .
H42A H -0.0967 0.1391 0.5554 0.032 Uiso 1 1 calc R U . . .
C43 C 0.0663(4) 0.16260(11) 0.5484(3) 0.0208(9) Uani 1 1 d . . . . .
H43A H 0.0489 0.1606 0.4626 0.025 Uiso 1 1 calc R U . . .
H43B H 0.1155 0.1413 0.5844 0.025 Uiso 1 1 calc R U . . .
C44 C 0.0577(4) 0.22972(11) 0.5291(3) 0.0213(9) Uani 1 1 d . . . . .
H44A H 0.1000 0.2530 0.5544 0.026 Uiso 1 1 calc R U . . .
H44B H 0.0430 0.2275 0.4436 0.026 Uiso 1 1 calc R U . . .
C45 C -0.0264(4) 0.16672(12) 0.7138(4) 0.0270(10) Uani 1 1 d . . . . .
H45A H -0.1032 0.1659 0.7352 0.032 Uiso 1 1 calc R U . . .
H45B H 0.0254 0.1464 0.7536 0.032 Uiso 1 1 calc R U . . .
C46 C 0.6814(3) 0.11699(11) 1.0179(3) 0.0180(8) Uani 1 1 d . . . . .
H46A H 0.7592 0.1287 1.0192 0.022 Uiso 1 1 calc R U . . .
H46B H 0.7009 0.0965 1.0737 0.022 Uiso 1 1 calc R U . . .
C47 C 0.6063(3) 0.14468(11) 1.0642(3) 0.0169(8) Uani 1 1 d . . . . .
C48 C 0.4841(3) 0.13829(10) 1.0577(3) 0.0156(8) Uani 1 1 d . . . . .
C49 C 0.4259(3) 0.16015(11) 1.1244(3) 0.0163(8) Uani 1 1 d . . . . .
C50 C 0.4911(4) 0.18979(11) 1.1839(3) 0.0181(8) Uani 1 1 d . . . . .
H50A H 0.4528 0.2049 1.2272 0.022 Uiso 1 1 calc R U . . .
C51 C 0.6080(3) 0.19855(11) 1.1838(3) 0.0202(9) Uani 1 1 d . . . . .
C52 C 0.6654(4) 0.17501(11) 1.1249(3) 0.0204(9) Uani 1 1 d . . . . .
H52A H 0.7469 0.1797 1.1262 0.024 Uiso 1 1 calc R U . . .
C53 C 0.6694(4) 0.23257(12) 1.2435(4) 0.0280(10) Uani 1 1 d . . . . .
H53A H 0.6440 0.2372 1.3137 0.042 Uiso 1 1 calc R U . . .
H53B H 0.6464 0.2532 1.1900 0.042 Uiso 1 1 calc R U . . .
H53C H 0.7576 0.2293 1.2655 0.042 Uiso 1 1 calc R U . . .
C54 C 0.3012(3) 0.15010(10) 1.1385(3) 0.0155(8) Uani 1 1 d . . . . .
C55 C 0.2595(3) 0.17671(11) 1.2201(3) 0.0177(8) Uani 1 1 d . . . . .
H55A H 0.3220 0.1777 1.2968 0.021 Uiso 1 1 calc R U . . .
H55B H 0.2512 0.2014 1.1858 0.021 Uiso 1 1 calc R U . . .
C56 C 0.1380(4) 0.16509(11) 1.2379(3) 0.0192(9) Uani 1 1 d . . . . .
H56A H 0.1144 0.1828 1.2910 0.023 Uiso 1 1 calc R U . . .
C57 C 0.0390(4) 0.16417(11) 1.1199(3) 0.0211(9) Uani 1 1 d . . . . .
H57A H -0.0389 0.1562 1.1315 0.025 Uiso 1 1 calc R U . . .
H57B H 0.0277 0.1888 1.0849 0.025 Uiso 1 1 calc R U . . .
C58 C 0.0774(3) 0.13763(11) 1.0382(3) 0.0207(9) Uani 1 1 d . . . . .
H58A H 0.0137 0.1369 0.9610 0.025 Uiso 1 1 calc R U . . .
C59 C 0.0926(4) 0.09963(12) 1.0930(3) 0.0229(9) Uani 1 1 d . . . . .
H59A H 0.1172 0.0823 1.0406 0.028 Uiso 1 1 calc R U . . .
H59B H 0.0143 0.0913 1.1028 0.028 Uiso 1 1 calc R U . . .
C60 C 0.1892(4) 0.10042(12) 1.2122(3) 0.0219(8) Uani 1 1 d . . . . .
H60A H 0.1974 0.0756 1.2475 0.026 Uiso 1 1 calc R U . . .
C61 C 0.3107(4) 0.11182(11) 1.1955(3) 0.0180(8) Uani 1 1 d . . . . .
H61A H 0.3356 0.0939 1.1451 0.022 Uiso 1 1 calc R U . . .
H61B H 0.3734 0.1122 1.2721 0.022 Uiso 1 1 calc R U . . .
C62 C 0.1991(3) 0.14984(11) 1.0205(3) 0.0185(9) Uani 1 1 d . . . . .
H62A H 0.1900 0.1745 0.9861 0.022 Uiso 1 1 calc R U . . .
H62B H 0.2217 0.1331 0.9654 0.022 Uiso 1 1 calc R U . . .
C63 C 0.1508(4) 0.12708(11) 1.2933(3) 0.0209(9) Uani 1 1 d . . . . .
H63A H 0.2125 0.1275 1.3706 0.025 Uiso 1 1 calc R U . . .
H63B H 0.0726 0.1194 1.3044 0.025 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
Nd1 Cnt1 2.489 . ?
Nd1 O1 2.172(3) . ?
Nd1 O2 2.188(3) . ?
Nd1 O3 2.200(2) . ?
Nd1 C3 2.823(4) . ?
Nd1 C1 2.830(4) . ?
Nd1 C2 2.841(4) . ?
Nd1 C6 2.861(3) . ?
Nd1 C4 2.898(4) . ?
Nd1 C5 2.932(4) . ?
O1 C12 1.356(4) . ?
O2 C30 1.366(5) . ?
O3 C48 1.359(5) . ?
C1 C6 1.425(6) . ?
C1 C2 1.425(5) . ?
C1 C7 1.515(5) . ?
C2 C3 1.416(5) . ?
C2 C10 1.521(5) . ?
C3 C4 1.418(6) . ?
C3 C8 1.516(5) . ?
C4 C5 1.423(5) . ?
C4 C28 1.522(5) . ?
C5 C6 1.403(5) . ?
C5 C9 1.521(6) . ?
C6 C46 1.523(5) . ?
C10 C11 1.541(5) . ?
C11 C16 1.408(5) . ?
C11 C12 1.409(5) . ?
C12 C13 1.438(5) . ?
C13 C14 1.388(5) . ?
C13 C18 1.544(5) . ?
C14 C15 1.407(5) . ?
C15 C16 1.383(5) . ?
C15 C17 1.510(5) . ?
C18 C26 1.553(5) . ?
C18 C25 1.553(5) . ?
C18 C19 1.563(5) . ?
C19 C20 1.544(5) . ?
C20 C27 1.531(5) . ?
C20 C21 1.539(5) . ?
C21 C22 1.541(5) . ?
C22 C23 1.533(5) . ?
C22 C26 1.540(5) . ?
C23 C24 1.529(5) . ?
C24 C27 1.534(5) . ?
C24 C25 1.539(5) . ?
C28 C29 1.536(5) . ?
C29 C34 1.396(5) . ?
C29 C30 1.404(5) . ?
C30 C31 1.431(5) . ?
C31 C32 1.411(6) . ?
C31 C36 1.541(5) . ?
C32 C33 1.387(6) . ?
C33 C34 1.394(6) . ?
C33 C35 1.513(5) . ?
C36 C44 1.548(5) . ?
C36 C43 1.553(5) . ?
C36 C37 1.555(5) . ?
C37 C38 1.534(6) . ?
C38 C45 1.516(6) . ?
C38 C39 1.540(6) . ?
C39 C40 1.534(6) . ?
C40 C41 1.529(6) . ?
C40 C44 1.548(6) . ?
C41 C42 1.530(6) . ?
C42 C43 1.533(6) . ?
C42 C45 1.538(6) . ?
C46 C47 1.539(5) . ?
C47 C52 1.397(6) . ?
C47 C48 1.406(5) . ?
C48 C49 1.428(5) . ?
C49 C50 1.397(5) . ?
C49 C54 1.538(5) . ?
C50 C51 1.385(5) . ?
C51 C52 1.396(6) . ?
C51 C53 1.512(6) . ?
C54 C55 1.552(5) . ?
C54 C62 1.554(5) . ?
C54 C61 1.555(5) . ?
C55 C56 1.535(5) . ?
C56 C63 1.536(6) . ?
C56 C57 1.537(5) . ?
C57 C58 1.533(5) . ?
C58 C59 1.533(6) . ?
C58 C62 1.543(5) . ?
C59 C60 1.535(5) . ?
C60 C61 1.527(6) . ?
C60 C63 1.530(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cnt1 Nd1 O1 98.4 . . ?
Cnt1 Nd1 O2 95.6 . . ?
Cnt1 Nd1 O3 97.3 . . ?
O1 Nd1 O2 119.58(10) . . ?
O1 Nd1 O3 110.95(10) . . ?
O2 Nd1 O3 125.00(10) . . ?
O1 Nd1 C3 81.21(10) . . ?
O2 Nd1 C3 82.77(10) . . ?
O3 Nd1 C3 126.75(10) . . ?
O1 Nd1 C1 84.85(10) . . ?
O2 Nd1 C1 125.54(10) . . ?
O3 Nd1 C1 77.25(10) . . ?
C3 Nd1 C1 51.57(11) . . ?
O1 Nd1 C2 68.48(10) . . ?
O2 Nd1 C2 111.70(10) . . ?
O3 Nd1 C2 105.55(10) . . ?
C3 Nd1 C2 28.96(11) . . ?
C1 Nd1 C2 29.10(10) . . ?
O1 Nd1 C6 113.83(11) . . ?
O2 Nd1 C6 106.73(11) . . ?
O3 Nd1 C6 68.37(10) . . ?
C3 Nd1 C6 59.78(11) . . ?
C1 Nd1 C6 28.99(11) . . ?
C2 Nd1 C6 51.14(11) . . ?
O1 Nd1 C4 109.73(10) . . ?
O2 Nd1 C4 66.45(10) . . ?
O3 Nd1 C4 115.69(10) . . ?
C3 Nd1 C4 28.67(11) . . ?
C1 Nd1 C4 59.37(11) . . ?
C2 Nd1 C4 50.62(11) . . ?
C6 Nd1 C4 50.29(10) . . ?
O1 Nd1 C5 127.15(10) . . ?
O2 Nd1 C5 79.06(10) . . ?
O3 Nd1 C5 87.63(10) . . ?
C3 Nd1 C5 50.55(11) . . ?
C1 Nd1 C5 50.36(11) . . ?
C2 Nd1 C5 58.83(11) . . ?
C6 Nd1 C5 27.99(11) . . ?
C4 Nd1 C5 28.24(10) . . ?
C12 O1 Nd1 157.3(2) . . ?
C30 O2 Nd1 154.1(2) . . ?
C48 O3 Nd1 135.0(2) . . ?
C6 C1 C2 119.5(3) . . ?
C6 C1 C7 120.3(3) . . ?
C2 C1 C7 120.1(4) . . ?
C6 C1 Nd1 76.7(2) . . ?
C2 C1 Nd1 75.9(2) . . ?
C7 C1 Nd1 114.8(2) . . ?
C3 C2 C1 119.9(4) . . ?
C3 C2 C10 119.3(3) . . ?
C1 C2 C10 120.7(3) . . ?
C3 C2 Nd1 74.8(2) . . ?
C1 C2 Nd1 75.0(2) . . ?
C10 C2 Nd1 124.3(2) . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 C8 119.1(3) . . ?
C4 C3 C8 120.9(3) . . ?
C2 C3 Nd1 76.2(2) . . ?
C4 C3 Nd1 78.6(2) . . ?
C8 C3 Nd1 114.0(2) . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 C28 120.3(3) . . ?
C5 C4 C28 119.7(3) . . ?
C3 C4 Nd1 72.7(2) . . ?
C5 C4 Nd1 77.2(2) . . ?
C28 C4 Nd1 122.7(2) . . ?
C6 C5 C4 120.0(4) . . ?
C6 C5 C9 120.5(3) . . ?
C4 C5 C9 119.4(3) . . ?
C6 C5 Nd1 73.2(2) . . ?
C4 C5 Nd1 74.6(2) . . ?
C9 C5 Nd1 122.8(2) . . ?
C5 C6 C1 120.4(3) . . ?
C5 C6 C46 119.4(4) . . ?
C1 C6 C46 120.1(3) . . ?
C5 C6 Nd1 78.8(2) . . ?
C1 C6 Nd1 74.3(2) . . ?
C46 C6 Nd1 119.1(2) . . ?
C2 C10 C11 122.5(3) . . ?
C16 C11 C12 120.1(3) . . ?
C16 C11 C10 113.9(3) . . ?
C12 C11 C10 126.0(3) . . ?
O1 C12 C11 120.4(3) . . ?
O1 C12 C13 120.7(3) . . ?
C11 C12 C13 118.8(3) . . ?
C14 C13 C12 118.2(3) . . ?
C14 C13 C18 120.2(3) . . ?
C12 C13 C18 121.5(3) . . ?
C13 C14 C15 123.6(4) . . ?
C16 C15 C14 117.2(4) . . ?
C16 C15 C17 121.1(3) . . ?
C14 C15 C17 121.7(3) . . ?
C15 C16 C11 122.1(4) . . ?
C13 C18 C26 112.1(3) . . ?
C13 C18 C25 112.3(3) . . ?
C26 C18 C25 106.8(3) . . ?
C13 C18 C19 109.9(3) . . ?
C26 C18 C19 109.1(3) . . ?
C25 C18 C19 106.4(3) . . ?
C20 C19 C18 110.8(3) . . ?
C27 C20 C21 109.3(3) . . ?
C27 C20 C19 110.1(3) . . ?
C21 C20 C19 109.1(3) . . ?
C20 C21 C22 109.6(3) . . ?
C23 C22 C26 109.6(3) . . ?
C23 C22 C21 109.5(3) . . ?
C26 C22 C21 109.8(3) . . ?
C24 C23 C22 108.6(3) . . ?
C23 C24 C27 110.0(3) . . ?
C23 C24 C25 110.5(3) . . ?
C27 C24 C25 108.9(3) . . ?
C24 C25 C18 111.7(3) . . ?
C22 C26 C18 111.2(3) . . ?
C20 C27 C24 109.0(3) . . ?
C4 C28 C29 119.7(3) . . ?
C34 C29 C30 120.0(4) . . ?
C34 C29 C28 116.6(3) . . ?
C30 C29 C28 123.3(3) . . ?
O2 C30 C29 119.9(3) . . ?
O2 C30 C31 120.5(3) . . ?
C29 C30 C31 119.5(4) . . ?
C32 C31 C30 116.9(4) . . ?
C32 C31 C36 121.3(3) . . ?
C30 C31 C36 121.8(3) . . ?
C33 C32 C31 124.3(4) . . ?
C32 C33 C34 116.7(4) . . ?
C32 C33 C35 121.8(4) . . ?
C34 C33 C35 121.5(4) . . ?
C33 C34 C29 122.3(4) . . ?
C31 C36 C44 112.0(3) . . ?
C31 C36 C43 111.7(3) . . ?
C44 C36 C43 106.3(3) . . ?
C31 C36 C37 109.8(3) . . ?
C44 C36 C37 107.1(3) . . ?
C43 C36 C37 109.8(3) . . ?
C38 C37 C36 110.9(3) . . ?
C45 C38 C37 109.2(3) . . ?
C45 C38 C39 110.1(4) . . ?
C37 C38 C39 108.9(3) . . ?
C40 C39 C38 109.7(3) . . ?
C41 C40 C39 109.5(4) . . ?
C41 C40 C44 110.1(4) . . ?
C39 C40 C44 108.5(3) . . ?
C40 C41 C42 109.1(3) . . ?
C41 C42 C43 109.2(4) . . ?
C41 C42 C45 110.0(4) . . ?
C43 C42 C45 109.4(3) . . ?
C42 C43 C36 111.0(3) . . ?
C40 C44 C36 111.3(3) . . ?
C38 C45 C42 110.2(3) . . ?
C6 C46 C47 118.4(3) . . ?
C52 C47 C48 119.5(4) . . ?
C52 C47 C46 118.4(3) . . ?
C48 C47 C46 121.8(3) . . ?
O3 C48 C47 119.6(3) . . ?
O3 C48 C49 120.5(3) . . ?
C47 C48 C49 119.9(3) . . ?
C50 C49 C48 117.0(4) . . ?
C50 C49 C54 120.9(3) . . ?
C48 C49 C54 121.9(3) . . ?
C51 C50 C49 124.1(4) . . ?
C50 C51 C52 117.2(4) . . ?
C50 C51 C53 121.0(4) . . ?
C52 C51 C53 121.8(4) . . ?
C51 C52 C47 121.8(4) . . ?
C49 C54 C55 112.6(3) . . ?
C49 C54 C62 112.8(3) . . ?
C55 C54 C62 106.5(3) . . ?
C49 C54 C61 108.4(3) . . ?
C55 C54 C61 107.0(3) . . ?
C62 C54 C61 109.3(3) . . ?
C56 C55 C54 111.7(3) . . ?
C55 C56 C63 109.6(3) . . ?
C55 C56 C57 110.1(3) . . ?
C63 C56 C57 109.2(3) . . ?
C58 C57 C56 108.9(3) . . ?
C59 C58 C57 109.2(3) . . ?
C59 C58 C62 109.1(3) . . ?
C57 C58 C62 110.0(3) . . ?
C58 C59 C60 110.0(3) . . ?
C61 C60 C63 110.4(3) . . ?
C61 C60 C59 109.2(3) . . ?
C63 C60 C59 109.6(3) . . ?
C60 C61 C54 110.8(3) . . ?
C58 C62 C54 110.9(3) . . ?
C60 C63 C56 108.7(3) . . ?

_refine_diff_density_max         0.736
_refine_diff_density_min         -1.856
_refine_diff_density_rms         0.088

