# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1038101'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-19 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         'C84 H87 N24 O3 Tb2, 3(N O3)'
_chemical_formula_sum            'C84 H87 N27 O12 Tb2'
_chemical_formula_weight         1984.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   26.2088(6)
_cell_length_b                   26.2088(6)
_cell_length_c                   48.2544(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     28705.3(15)
_cell_formula_units_Z            12
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    8867
_cell_measurement_theta_min      2.6706
_cell_measurement_theta_max      75.6259

_exptl_crystal_description       block
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             12072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    7.747
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.22919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21t (release 14-08-2012 CrysAlis171 .NET)
(compiled Aug 14 2012,18:12:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_detector_area_resol_mean 10.5357
_diffrn_measurement_method       ω-scan
_diffrn_reflns_number            23031
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_theta_min         2.673
_diffrn_reflns_theta_max         75.915
_diffrn_reflns_theta_full        67.500
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6555
_reflns_number_gt                4491
_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       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0923P)²+2.5911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6555
_refine_ls_number_parameters     381
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1553
_refine_ls_wR_factor_gt          0.1388
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.186
_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
Tb1 Tb 0.3333 0.6667 0.07384(2) 0.04610(14) Uani 1 3 d S T P . .
Tb2 Tb 0.3333 0.6667 0.00020(2) 0.04161(13) Uani 1 3 d S T P . .
N1 N 0.24422(16) 0.61174(14) 0.10384(7) 0.0591(8) Uani 1 1 d . . . . .
C2 C 0.19659(19) 0.61375(18) 0.09731(9) 0.0590(10) Uani 1 1 d . . . . .
N3 N 0.14566(17) 0.56717(14) 0.10692(9) 0.0675(10) Uani 1 1 d . . . . .
H3 H 0.1105 0.5609 0.1045 0.081 Uiso 1 1 calc R U . . .
C4 C 0.16193(19) 0.53222(18) 0.12139(9) 0.0667(11) Uani 1 1 d . . . . .
C5 C 0.1279(2) 0.4801(2) 0.13563(11) 0.0858(14) Uani 1 1 d . . . . .
H5 H 0.0870 0.4615 0.1360 0.103 Uiso 1 1 calc R U . . .
C6 C 0.1583(3) 0.4573(2) 0.14915(12) 0.0985(17) Uani 1 1 d . . . . .
H6 H 0.1374 0.4223 0.1589 0.118 Uiso 1 1 calc R U . . .
C7 C 0.2192(3) 0.4852(3) 0.14856(12) 0.0955(16) Uani 1 1 d . . . . .
H7 H 0.2381 0.4683 0.1579 0.115 Uiso 1 1 calc R U . . .
C8 C 0.2528(2) 0.5380(2) 0.13436(11) 0.0821(14) Uani 1 1 d . . . . .
H8 H 0.2938 0.5574 0.1346 0.098 Uiso 1 1 calc R U . . .
C9 C 0.22282(19) 0.56029(18) 0.11987(9) 0.0625(10) Uani 1 1 d . . . . .
N10 N 0.19649(14) 0.65797(14) 0.08231(8) 0.0648(9) Uani 1 1 d . . . . .
C10A C 0.1451(2) 0.6649(2) 0.07956(13) 0.1015(17) Uani 1 1 d . U . . .
H10A H 0.1100 0.6269 0.0801 0.152 Uiso 1 1 calc R U . . .
H10B H 0.1469 0.6837 0.0622 0.152 Uiso 1 1 calc R U . . .
H10C H 0.1444 0.6887 0.0945 0.152 Uiso 1 1 calc R U . . .
N11 N 0.25151(13) 0.69936(13) 0.07226(6) 0.0524(7) Uani 1 1 d . . . . .
C12 C 0.25760(17) 0.74899(16) 0.06394(10) 0.0588(10) Uani 1 1 d . . . . .
H12 H 0.2262 0.7556 0.0666 0.071 Uiso 1 1 calc R U . . .
C13 C 0.31041(16) 0.79492(15) 0.05074(8) 0.0509(8) Uani 1 1 d . . . . .
C14 C 0.35036(15) 0.78205(15) 0.03713(7) 0.0454(7) Uani 1 1 d . . . . .
O14 O 0.34225(10) 0.72819(10) 0.03692(5) 0.0450(5) Uani 1 1 d . . . . .
C15 C 0.39926(17) 0.82892(16) 0.02379(8) 0.0502(8) Uani 1 1 d . . . . .
C16 C 0.40750(17) 0.88541(15) 0.02472(9) 0.0574(9) Uani 1 1 d . . . . .
H16 H 0.4409 0.9158 0.0164 0.069 Uiso 1 1 calc R U . . .
C17 C 0.36827(17) 0.89861(16) 0.03749(9) 0.0586(10) Uani 1 1 d . . . . .
C17A C 0.3783(2) 0.96111(18) 0.03860(11) 0.0766(13) Uani 1 1 d . . . . .
C17B C 0.4003(3) 0.9846(2) 0.06848(16) 0.125(2) Uani 1 1 d . . . . .
H17A H 0.4089 1.0247 0.0698 0.188 Uiso 1 1 calc R U . . .
H17B H 0.4353 0.9828 0.0723 0.188 Uiso 1 1 calc R U . . .
H17C H 0.3703 0.9608 0.0816 0.188 Uiso 1 1 calc R U . . .
C17C C 0.3231(3) 0.9629(3) 0.03361(15) 0.135(3) Uani 1 1 d . . . . .
H17D H 0.3314 1.0029 0.0345 0.203 Uiso 1 1 calc R U . . .
H17E H 0.2945 0.9400 0.0475 0.203 Uiso 1 1 calc R U . . .
H17F H 0.3077 0.9469 0.0156 0.203 Uiso 1 1 calc R U . . .
C17D C 0.4278(3) 1.0030(2) 0.02012(15) 0.123(2) Uani 1 1 d . U . . .
H17G H 0.4186 0.9901 0.0012 0.185 Uiso 1 1 calc R U . . .
H17H H 0.4635 1.0039 0.0255 0.185 Uiso 1 1 calc R U . . .
H17I H 0.4328 1.0418 0.0219 0.185 Uiso 1 1 calc R U . . .
C18 C 0.31973(18) 0.85213(17) 0.05010(9) 0.0604(10) Uani 1 1 d . . . . .
H18 H 0.2921 0.8595 0.0585 0.072 Uiso 1 1 calc R U . . .
C19 C 0.44423(16) 0.82003(15) 0.01067(8) 0.0534(9) Uani 1 1 d . . . . .
H19 H 0.4814 0.8529 0.0082 0.064 Uiso 1 1 calc R U . . .
N20 N 0.43614(12) 0.76964(12) 0.00226(6) 0.0484(7) Uani 1 1 d . . . . .
N21 N 0.48498(13) 0.76834(14) -0.00772(7) 0.0589(8) Uani 1 1 d . . . . .
C21A C 0.54341(19) 0.8192(2) -0.00767(13) 0.0933(16) Uani 1 1 d . U . . .
H21A H 0.5719 0.8068 -0.0105 0.140 Uiso 1 1 calc R U . . .
H21B H 0.5507 0.8390 0.0098 0.140 Uiso 1 1 calc R U . . .
H21C H 0.5466 0.8455 -0.0223 0.140 Uiso 1 1 calc R U . . .
N22 N 0.41788(12) 0.67693(12) -0.02909(6) 0.0507(7) Uani 1 1 d . . . . .
C23 C 0.47183(16) 0.71821(17) -0.02190(8) 0.0510(9) Uani 1 1 d . . . . .
N24 N 0.51398(13) 0.70641(13) -0.02989(7) 0.0588(8) Uani 1 1 d . . . . .
H24 H 0.5512 0.7277 -0.0268 0.071 Uiso 1 1 calc R U . . .
C25 C 0.48618(18) 0.65363(17) -0.04392(8) 0.0590(9) Uani 1 1 d . . . . .
C26 C 0.5088(2) 0.62119(19) -0.05629(9) 0.0707(12) Uani 1 1 d . . . . .
H26 H 0.5489 0.6336 -0.0559 0.085 Uiso 1 1 calc R U . . .
C27 C 0.4682(2) 0.5691(2) -0.06921(10) 0.0776(13) Uani 1 1 d . . . . .
H27 H 0.4811 0.5456 -0.0776 0.093 Uiso 1 1 calc R U . . .
C28 C 0.4091(2) 0.5516(2) -0.06988(10) 0.0788(13) Uani 1 1 d . . . . .
H28 H 0.3833 0.5170 -0.0791 0.095 Uiso 1 1 calc R U . . .
C29 C 0.3868(2) 0.5841(2) -0.05720(10) 0.0667(11) Uani 1 1 d . . . . .
H29 H 0.3468 0.5718 -0.0576 0.080 Uiso 1 1 calc R U . . .
C30 C 0.42705(17) 0.63580(16) -0.04387(8) 0.0542(9) Uani 1 1 d . . . . .
N1A N 0.4620(4) 0.4662(4) 0.12776(14) 0.116(2) Uani 1 1 d . . . . .
O1A O 0.5062(4) 0.5118(4) 0.13264(19) 0.209(4) Uani 1 1 d . . . . .
O2A O 0.4556(2) 0.4242(3) 0.13951(14) 0.167(3) Uani 1 1 d . . . . .
O3A O 0.4331(3) 0.4705(3) 0.11048(14) 0.191(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O14 2.335(2) 2_665 ?
Tb1 O14 2.335(2) 3_565 ?
Tb1 O14 2.335(2) . ?
Tb1 N1 2.502(3) 3_565 ?
Tb1 N1 2.502(3) . ?
Tb1 N1 2.502(3) 2_665 ?
Tb1 N11 2.679(3) . ?
Tb1 N11 2.679(3) 3_565 ?
Tb1 N11 2.679(3) 2_665 ?
Tb1 Tb2 3.5533(5) . ?
Tb2 O14 2.327(2) . ?
Tb2 O14 2.327(2) 2_665 ?
Tb2 O14 2.327(2) 3_565 ?
Tb2 N22 2.527(3) 2_665 ?
Tb2 N22 2.527(3) 3_565 ?
Tb2 N22 2.527(3) . ?
Tb2 N20 2.698(3) 2_665 ?
Tb2 N20 2.698(3) 3_565 ?
Tb2 N20 2.698(3) . ?
N1 C2 1.314(6) . ?
N1 C9 1.405(5) . ?
C2 N3 1.363(5) . ?
C2 N10 1.367(5) . ?
N3 C4 1.378(5) . ?
N3 H3 0.8600 . ?
C4 C5 1.385(6) . ?
C4 C9 1.385(6) . ?
C5 C6 1.374(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.393(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(6) . ?
C8 H8 0.9300 . ?
N10 N11 1.388(4) . ?
N10 C10A 1.453(5) . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9600 . ?
C10A H10C 0.9600 . ?
N11 C12 1.293(5) . ?
C12 C13 1.451(5) . ?
C12 H12 0.9300 . ?
C13 C18 1.394(5) . ?
C13 C14 1.412(5) . ?
C14 O14 1.318(4) . ?
C14 C15 1.411(5) . ?
C15 C16 1.386(5) . ?
C15 C19 1.456(5) . ?
C16 C17 1.383(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(5) . ?
C17 C17A 1.525(5) . ?
C17A C17C 1.490(7) . ?
C17A C17D 1.503(7) . ?
C17A C17B 1.561(8) . ?
C17B H17A 0.9600 . ?
C17B H17B 0.9600 . ?
C17B H17C 0.9600 . ?
C17C H17D 0.9600 . ?
C17C H17E 0.9600 . ?
C17C H17F 0.9600 . ?
C17D H17G 0.9600 . ?
C17D H17H 0.9600 . ?
C17D H17I 0.9600 . ?
C18 H18 0.9300 . ?
C19 N20 1.294(4) . ?
C19 H19 0.9300 . ?
N20 N21 1.384(4) . ?
N21 C23 1.364(5) . ?
N21 C21A 1.442(5) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
N22 C23 1.327(5) . ?
N22 C30 1.410(4) . ?
C23 N24 1.344(4) . ?
N24 C25 1.376(5) . ?
N24 H24 0.8600 . ?
C25 C30 1.377(5) . ?
C25 C26 1.392(5) . ?
C26 C27 1.390(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.378(7) . ?
C27 H27 0.9300 . ?
C28 C29 1.393(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.390(6) . ?
C29 H29 0.9300 . ?
N1A O3A 1.167(7) . ?
N1A O2A 1.175(7) . ?
N1A O1A 1.200(10) . ?

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
O14 Tb1 O14 68.08(9) 2_665 3_565 ?
O14 Tb1 O14 68.08(9) 2_665 . ?
O14 Tb1 O14 68.08(9) 3_565 . ?
O14 Tb1 N1 144.27(9) 2_665 3_565 ?
O14 Tb1 N1 125.53(10) 3_565 3_565 ?
O14 Tb1 N1 86.06(10) . 3_565 ?
O14 Tb1 N1 86.06(10) 2_665 . ?
O14 Tb1 N1 144.28(9) 3_565 . ?
O14 Tb1 N1 125.53(10) . . ?
N1 Tb1 N1 89.89(12) 3_565 . ?
O14 Tb1 N1 125.53(10) 2_665 2_665 ?
O14 Tb1 N1 86.06(10) 3_565 2_665 ?
O14 Tb1 N1 144.27(9) . 2_665 ?
N1 Tb1 N1 89.89(12) 3_565 2_665 ?
N1 Tb1 N1 89.89(12) . 2_665 ?
O14 Tb1 N11 74.94(9) 2_665 . ?
O14 Tb1 N11 128.14(9) 3_565 . ?
O14 Tb1 N11 64.98(8) . . ?
N1 Tb1 N11 71.83(10) 3_565 . ?
N1 Tb1 N11 62.24(10) . . ?
N1 Tb1 N11 145.79(11) 2_665 . ?
O14 Tb1 N11 128.14(9) 2_665 3_565 ?
O14 Tb1 N11 64.99(8) 3_565 3_565 ?
O14 Tb1 N11 74.95(9) . 3_565 ?
N1 Tb1 N11 62.24(10) 3_565 3_565 ?
N1 Tb1 N11 145.78(11) . 3_565 ?
N1 Tb1 N11 71.83(10) 2_665 3_565 ?
N11 Tb1 N11 119.920(7) . 3_565 ?
O14 Tb1 N11 64.99(8) 2_665 2_665 ?
O14 Tb1 N11 74.95(9) 3_565 2_665 ?
O14 Tb1 N11 128.14(9) . 2_665 ?
N1 Tb1 N11 145.79(11) 3_565 2_665 ?
N1 Tb1 N11 71.83(10) . 2_665 ?
N1 Tb1 N11 62.24(10) 2_665 2_665 ?
N11 Tb1 N11 119.919(7) . 2_665 ?
N11 Tb1 N11 119.920(7) 3_565 2_665 ?
O14 Tb1 Tb2 40.27(6) 2_665 . ?
O14 Tb1 Tb2 40.27(6) 3_565 . ?
O14 Tb1 Tb2 40.27(6) . . ?
N1 Tb1 Tb2 125.34(9) 3_565 . ?
N1 Tb1 Tb2 125.35(9) . . ?
N1 Tb1 Tb2 125.34(9) 2_665 . ?
N11 Tb1 Tb2 88.37(7) . . ?
N11 Tb1 Tb2 88.37(7) 3_565 . ?
N11 Tb1 Tb2 88.37(7) 2_665 . ?
O14 Tb2 O14 68.34(9) . 2_665 ?
O14 Tb2 O14 68.34(9) . 3_565 ?
O14 Tb2 O14 68.34(9) 2_665 3_565 ?
O14 Tb2 N22 84.52(9) . 2_665 ?
O14 Tb2 N22 124.97(9) 2_665 2_665 ?
O14 Tb2 N22 143.12(9) 3_565 2_665 ?
O14 Tb2 N22 143.12(9) . 3_565 ?
O14 Tb2 N22 84.52(9) 2_665 3_565 ?
O14 Tb2 N22 124.97(9) 3_565 3_565 ?
N22 Tb2 N22 91.75(10) 2_665 3_565 ?
O14 Tb2 N22 124.97(9) . . ?
O14 Tb2 N22 143.12(9) 2_665 . ?
O14 Tb2 N22 84.52(9) 3_565 . ?
N22 Tb2 N22 91.75(10) 2_665 . ?
N22 Tb2 N22 91.75(10) 3_565 . ?
O14 Tb2 N20 74.16(8) . 2_665 ?
O14 Tb2 N20 64.84(8) 2_665 2_665 ?
O14 Tb2 N20 127.89(9) 3_565 2_665 ?
N22 Tb2 N20 61.97(9) 2_665 2_665 ?
N22 Tb2 N20 71.81(9) 3_565 2_665 ?
N22 Tb2 N20 147.55(10) . 2_665 ?
O14 Tb2 N20 127.89(9) . 3_565 ?
O14 Tb2 N20 74.16(8) 2_665 3_565 ?
O14 Tb2 N20 64.84(8) 3_565 3_565 ?
N22 Tb2 N20 147.55(10) 2_665 3_565 ?
N22 Tb2 N20 61.97(9) 3_565 3_565 ?
N22 Tb2 N20 71.81(9) . 3_565 ?
N20 Tb2 N20 119.866(8) 2_665 3_565 ?
O14 Tb2 N20 64.84(8) . . ?
O14 Tb2 N20 127.88(9) 2_665 . ?
O14 Tb2 N20 74.16(8) 3_565 . ?
N22 Tb2 N20 71.81(9) 2_665 . ?
N22 Tb2 N20 147.55(10) 3_565 . ?
N22 Tb2 N20 61.97(9) . . ?
N20 Tb2 N20 119.865(8) 2_665 . ?
N20 Tb2 N20 119.867(9) 3_565 . ?
O14 Tb2 Tb1 40.43(6) . . ?
O14 Tb2 Tb1 40.43(6) 2_665 . ?
O14 Tb2 Tb1 40.43(6) 3_565 . ?
N22 Tb2 Tb1 124.02(7) 2_665 . ?
N22 Tb2 Tb1 124.02(7) 3_565 . ?
N22 Tb2 Tb1 124.02(7) . . ?
N20 Tb2 Tb1 87.89(6) 2_665 . ?
N20 Tb2 Tb1 87.89(6) 3_565 . ?
N20 Tb2 Tb1 87.89(6) . . ?
C2 N1 C9 103.8(4) . . ?
C2 N1 Tb1 118.1(3) . . ?
C9 N1 Tb1 132.9(3) . . ?
N1 C2 N3 114.0(4) . . ?
N1 C2 N10 124.4(4) . . ?
N3 C2 N10 121.5(4) . . ?
C2 N3 C4 106.1(4) . . ?
C2 N3 H3 126.9 . . ?
C4 N3 H3 126.9 . . ?
N3 C4 C5 130.4(4) . . ?
N3 C4 C9 106.1(4) . . ?
C5 C4 C9 123.5(4) . . ?
C6 C5 C4 115.9(5) . . ?
C6 C5 H5 122.0 . . ?
C4 C5 H5 122.0 . . ?
C5 C6 C7 121.8(5) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C6 C7 C8 121.6(5) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 117.2(5) . . ?
C9 C8 H8 121.4 . . ?
C7 C8 H8 121.4 . . ?
C8 C9 C4 119.8(4) . . ?
C8 C9 N1 130.2(4) . . ?
C4 C9 N1 109.9(4) . . ?
C2 N10 N11 113.9(3) . . ?
C2 N10 C10A 123.3(4) . . ?
N11 N10 C10A 122.4(3) . . ?
N10 C10A H10A 109.5 . . ?
N10 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
N10 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C12 N11 N10 116.9(3) . . ?
C12 N11 Tb1 127.9(3) . . ?
N10 N11 Tb1 115.1(2) . . ?
N11 C12 C13 123.9(4) . . ?
N11 C12 H12 118.0 . . ?
C13 C12 H12 118.0 . . ?
C18 C13 C14 119.6(3) . . ?
C18 C13 C12 118.9(3) . . ?
C14 C13 C12 121.3(3) . . ?
O14 C14 C15 121.2(3) . . ?
O14 C14 C13 121.2(3) . . ?
C15 C14 C13 117.6(3) . . ?
C14 O14 Tb2 130.9(2) . . ?
C14 O14 Tb1 129.8(2) . . ?
Tb2 O14 Tb1 99.30(9) . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 C19 118.6(3) . . ?
C14 C15 C19 121.0(3) . . ?
C17 C16 C15 122.9(3) . . ?
C17 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C16 C17 C18 116.5(3) . . ?
C16 C17 C17A 122.3(4) . . ?
C18 C17 C17A 121.2(4) . . ?
C17C C17A C17D 112.2(5) . . ?
C17C C17A C17 112.3(4) . . ?
C17D C17A C17 112.7(4) . . ?
C17C C17A C17B 108.0(5) . . ?
C17D C17A C17B 104.2(5) . . ?
C17 C17A C17B 106.7(4) . . ?
C17A C17B H17A 109.5 . . ?
C17A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C17A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C17A C17C H17D 109.5 . . ?
C17A C17C H17E 109.5 . . ?
H17D C17C H17E 109.5 . . ?
C17A C17C H17F 109.5 . . ?
H17D C17C H17F 109.5 . . ?
H17E C17C H17F 109.5 . . ?
C17A C17D H17G 109.5 . . ?
C17A C17D H17H 109.5 . . ?
H17G C17D H17H 109.5 . . ?
C17A C17D H17I 109.5 . . ?
H17G C17D H17I 109.5 . . ?
H17H C17D H17I 109.5 . . ?
C17 C18 C13 123.0(3) . . ?
C17 C18 H18 118.5 . . ?
C13 C18 H18 118.5 . . ?
N20 C19 C15 124.6(3) . . ?
N20 C19 H19 117.7 . . ?
C15 C19 H19 117.7 . . ?
C19 N20 N21 116.9(3) . . ?
C19 N20 Tb2 127.2(2) . . ?
N21 N20 Tb2 115.8(2) . . ?
C23 N21 N20 114.0(3) . . ?
C23 N21 C21A 122.0(3) . . ?
N20 N21 C21A 123.0(3) . . ?
N21 C21A H21A 109.5 . . ?
N21 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
N21 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23 N22 C30 103.7(3) . . ?
C23 N22 Tb2 117.4(2) . . ?
C30 N22 Tb2 132.6(2) . . ?
N22 C23 N24 113.6(3) . . ?
N22 C23 N21 124.7(3) . . ?
N24 C23 N21 121.7(3) . . ?
C23 N24 C25 106.8(3) . . ?
C23 N24 H24 126.6 . . ?
C25 N24 H24 126.6 . . ?
N24 C25 C30 106.3(3) . . ?
N24 C25 C26 130.7(4) . . ?
C30 C25 C26 123.0(4) . . ?
C27 C26 C25 116.1(4) . . ?
C27 C26 H26 121.9 . . ?
C25 C26 H26 121.9 . . ?
C28 C27 C26 121.3(4) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C27 C28 C29 122.1(5) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C30 C29 C28 117.0(5) . . ?
C30 C29 H29 121.5 . . ?
C28 C29 H29 121.5 . . ?
C25 C30 C29 120.5(4) . . ?
C25 C30 N22 109.5(3) . . ?
C29 C30 N22 130.0(4) . . ?
O3A N1A O2A 129.7(10) . . ?
O3A N1A O1A 113.2(8) . . ?
O2A N1A O1A 116.9(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N3 -2.0(5) . . . . ?
Tb1 N1 C2 N3 155.8(3) . . . . ?
C9 N1 C2 N10 177.9(4) . . . . ?
Tb1 N1 C2 N10 -24.4(6) . . . . ?
N1 C2 N3 C4 1.0(5) . . . . ?
N10 C2 N3 C4 -178.8(4) . . . . ?
C2 N3 C4 C5 179.1(5) . . . . ?
C2 N3 C4 C9 0.4(5) . . . . ?
N3 C4 C5 C6 -177.0(5) . . . . ?
C9 C4 C5 C6 1.4(8) . . . . ?
C4 C5 C6 C7 0.2(9) . . . . ?
C5 C6 C7 C8 0.4(10) . . . . ?
C6 C7 C8 C9 -2.5(9) . . . . ?
C7 C8 C9 C4 4.1(8) . . . . ?
C7 C8 C9 N1 -180.0(5) . . . . ?
N3 C4 C9 C8 175.0(5) . . . . ?
C5 C4 C9 C8 -3.7(7) . . . . ?
N3 C4 C9 N1 -1.6(5) . . . . ?
C5 C4 C9 N1 179.6(4) . . . . ?
C2 N1 C9 C8 -174.1(5) . . . . ?
Tb1 N1 C9 C8 33.1(7) . . . . ?
C2 N1 C9 C4 2.2(5) . . . . ?
Tb1 N1 C9 C4 -150.7(3) . . . . ?
N1 C2 N10 N11 5.1(6) . . . . ?
N3 C2 N10 N11 -175.0(4) . . . . ?
N1 C2 N10 C10A -168.5(5) . . . . ?
N3 C2 N10 C10A 11.3(7) . . . . ?
C2 N10 N11 C12 -163.6(4) . . . . ?
C10A N10 N11 C12 10.1(6) . . . . ?
C2 N10 N11 Tb1 14.9(4) . . . . ?
C10A N10 N11 Tb1 -171.4(4) . . . . ?
N10 N11 C12 C13 -174.6(4) . . . . ?
Tb1 N11 C12 C13 7.1(6) . . . . ?
N11 C12 C13 C18 -160.9(4) . . . . ?
N11 C12 C13 C14 23.0(7) . . . . ?
C18 C13 C14 O14 -178.8(4) . . . . ?
C12 C13 C14 O14 -2.8(6) . . . . ?
C18 C13 C14 C15 1.2(6) . . . . ?
C12 C13 C14 C15 177.3(4) . . . . ?
C15 C14 O14 Tb2 -57.2(5) . . . . ?
C13 C14 O14 Tb2 122.9(3) . . . . ?
C15 C14 O14 Tb1 122.3(3) . . . . ?
C13 C14 O14 Tb1 -57.7(4) . . . . ?
O14 C14 C15 C16 -178.8(4) . . . . ?
C13 C14 C15 C16 1.2(6) . . . . ?
O14 C14 C15 C19 -3.5(6) . . . . ?
C13 C14 C15 C19 176.4(4) . . . . ?
C14 C15 C16 C17 -2.5(7) . . . . ?
C19 C15 C16 C17 -177.9(4) . . . . ?
C15 C16 C17 C18 1.2(6) . . . . ?
C15 C16 C17 C17A 179.3(4) . . . . ?
C16 C17 C17A C17C 138.8(5) . . . . ?
C18 C17 C17A C17C -43.2(7) . . . . ?
C16 C17 C17A C17D 10.8(7) . . . . ?
C18 C17 C17A C17D -171.2(5) . . . . ?
C16 C17 C17A C17B -103.0(5) . . . . ?
C18 C17 C17A C17B 75.0(6) . . . . ?
C16 C17 C18 C13 1.3(6) . . . . ?
C17A C17 C18 C13 -176.8(4) . . . . ?
C14 C13 C18 C17 -2.6(6) . . . . ?
C12 C13 C18 C17 -178.7(4) . . . . ?
C16 C15 C19 N20 -162.0(4) . . . . ?
C14 C15 C19 N20 22.7(6) . . . . ?
C15 C19 N20 N21 -174.9(4) . . . . ?
C15 C19 N20 Tb2 7.5(6) . . . . ?
C19 N20 N21 C23 -165.9(4) . . . . ?
Tb2 N20 N21 C23 12.0(4) . . . . ?
C19 N20 N21 C21A 3.3(6) . . . . ?
Tb2 N20 N21 C21A -178.8(4) . . . . ?
C30 N22 C23 N24 -1.9(4) . . . . ?
Tb2 N22 C23 N24 153.8(3) . . . . ?
C30 N22 C23 N21 178.1(4) . . . . ?
Tb2 N22 C23 N21 -26.2(5) . . . . ?
N20 N21 C23 N22 8.5(6) . . . . ?
C21A N21 C23 N22 -160.8(4) . . . . ?
N20 N21 C23 N24 -171.4(3) . . . . ?
C21A N21 C23 N24 19.3(7) . . . . ?
N22 C23 N24 C25 1.0(5) . . . . ?
N21 C23 N24 C25 -179.0(4) . . . . ?
C23 N24 C25 C30 0.4(4) . . . . ?
C23 N24 C25 C26 -179.4(4) . . . . ?
N24 C25 C26 C27 -179.4(4) . . . . ?
C30 C25 C26 C27 0.8(7) . . . . ?
C25 C26 C27 C28 0.8(7) . . . . ?
C26 C27 C28 C29 -1.5(8) . . . . ?
C27 C28 C29 C30 0.5(8) . . . . ?
N24 C25 C30 C29 178.3(4) . . . . ?
C26 C25 C30 C29 -1.9(7) . . . . ?
N24 C25 C30 N22 -1.6(4) . . . . ?
C26 C25 C30 N22 178.3(4) . . . . ?
C28 C29 C30 C25 1.1(7) . . . . ?
C28 C29 C30 N22 -179.0(4) . . . . ?
C23 N22 C30 C25 2.1(4) . . . . ?
Tb2 N22 C30 C25 -148.1(3) . . . . ?
C23 N22 C30 C29 -177.7(4) . . . . ?
Tb2 N22 C30 C29 32.0(6) . . . . ?

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
N3 H3 O3A 0.86 2.02 2.840(6) 158.9 3_565
C10A H10A O3A 0.96 2.29 3.090(8) 140.0 3_565
C21A H21A O1A 0.96 2.57 3.346(8) 138.5 29
N24 H24 O2A 0.86 1.93 2.766(5) 162.3 29

_refine_diff_density_max         0.544
_refine_diff_density_min         -1.041
_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_2
_database_code_depnum_ccdc_archive 'CCDC 1038102'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-19 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         'C84 H87 Dy2 N24 O3, 3(N O3)'
_chemical_formula_sum            'C84 H87 Dy2 N27 O12'
_chemical_formula_weight         1991.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   26.1377(11)
_cell_length_b                   26.1377(11)
_cell_length_c                   47.2565(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     27959(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    5316
_cell_measurement_theta_min      3.1140
_cell_measurement_theta_max      27.8620

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_F_000             12096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    1.663
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.38045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       ω-scan

_diffrn_reflns_number            17460
_diffrn_reflns_av_unetI/netI     0.0714
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         3.020
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5460
_reflns_number_gt                3178
_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       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0410P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5460
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1064
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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 0.3333 0.6667 0.07534(2) 0.01877(13) Uani 1 3 d S T P . .
Dy2 Dy 0.3333 0.6667 0.00075(2) 0.01730(13) Uani 1 3 d S T P . .
N1 N 0.24425(19) 0.61105(18) 0.10556(9) 0.0239(11) Uani 1 1 d . . . . .
C2 C 0.1956(3) 0.6129(3) 0.09831(12) 0.0269(14) Uani 1 1 d . . . . .
N3 N 0.14512(19) 0.56595(19) 0.10761(9) 0.0244(11) Uani 1 1 d . . . . .
H3 H 0.1090 0.5592 0.1048 0.029 Uiso 1 1 calc R U . . .
C4 C 0.1610(3) 0.5303(2) 0.12249(11) 0.0252(14) Uani 1 1 d . . . . .
C5 C 0.1271(3) 0.4768(3) 0.13656(12) 0.0319(15) Uani 1 1 d . . . . .
H5 H 0.0852 0.4576 0.1368 0.038 Uiso 1 1 calc R U . . .
C6 C 0.1567(3) 0.4534(3) 0.14983(12) 0.0353(16) Uani 1 1 d . . . . .
H6 H 0.1350 0.4165 0.1592 0.042 Uiso 1 1 calc R U . . .
C7 C 0.2192(3) 0.4824(3) 0.15005(11) 0.0344(16) Uani 1 1 d . . . . .
H7 H 0.2386 0.4653 0.1600 0.041 Uiso 1 1 calc R U . . .
C8 C 0.2524(3) 0.5356(3) 0.13593(11) 0.0296(15) Uani 1 1 d . . . . .
H8 H 0.2944 0.5556 0.1362 0.036 Uiso 1 1 calc R U . . .
C9 C 0.2225(3) 0.5585(3) 0.12146(11) 0.0291(15) Uani 1 1 d . . . . .
N10 N 0.1963(2) 0.6573(2) 0.08310(10) 0.0286(12) Uani 1 1 d . . . . .
C10A C 0.1452(3) 0.6649(3) 0.08097(17) 0.072(3) Uani 1 1 d . . . . .
H10A H 0.1094 0.6274 0.0852 0.108 Uiso 1 1 calc R U . . .
H10B H 0.1426 0.6775 0.0617 0.108 Uiso 1 1 calc R U . . .
H10C H 0.1491 0.6950 0.0945 0.108 Uiso 1 1 calc R U . . .
N11 N 0.25197(19) 0.6993(2) 0.07332(9) 0.0233(11) Uani 1 1 d . . . . .
C12 C 0.2578(3) 0.7488(2) 0.06507(10) 0.0250(13) Uani 1 1 d . . . . .
H12 H 0.2255 0.7553 0.0678 0.030 Uiso 1 1 calc R U . . .
C13 C 0.3107(2) 0.7949(2) 0.05198(11) 0.0211(13) Uani 1 1 d . . . . .
C14 C 0.3509(2) 0.7826(2) 0.03789(10) 0.0177(12) Uani 1 1 d . . . . .
O14 O 0.34232(15) 0.72852(16) 0.03787(7) 0.0210(9) Uani 1 1 d . . . . .
C15 C 0.4004(2) 0.8286(2) 0.02464(11) 0.0213(14) Uani 1 1 d . . . . .
C16 C 0.4090(2) 0.8857(2) 0.02548(10) 0.0226(13) Uani 1 1 d . . . . .
H16 H 0.4432 0.9167 0.0168 0.027 Uiso 1 1 calc R U . . .
C17 C 0.3696(2) 0.8993(2) 0.03848(11) 0.0242(13) Uani 1 1 d . . . . .
C17A C 0.3805(3) 0.9626(2) 0.04014(12) 0.0300(15) Uani 1 1 d . . . . .
C17B C 0.3993(3) 0.9843(3) 0.07060(12) 0.0394(17) Uani 1 1 d . . . . .
H17A H 0.4077 1.0251 0.0722 0.059 Uiso 1 1 calc R U . . .
H17B H 0.4349 0.9825 0.0754 0.059 Uiso 1 1 calc R U . . .
H17C H 0.3674 0.9591 0.0836 0.059 Uiso 1 1 calc R U . . .
C17C C 0.3238(3) 0.9644(3) 0.03360(14) 0.0480(19) Uani 1 1 d . . . . .
H17D H 0.3316 1.0050 0.0354 0.072 Uiso 1 1 calc R U . . .
H17E H 0.2928 0.9389 0.0470 0.072 Uiso 1 1 calc R U . . .
H17F H 0.3109 0.9503 0.0143 0.072 Uiso 1 1 calc R U . . .
C17D C 0.4290(3) 1.0042(2) 0.01982(13) 0.0461(19) Uani 1 1 d . . . . .
H17G H 0.4190 0.9884 0.0006 0.069 Uiso 1 1 calc R U . . .
H17H H 0.4667 1.0077 0.0254 0.069 Uiso 1 1 calc R U . . .
H17I H 0.4323 1.0432 0.0204 0.069 Uiso 1 1 calc R U . . .
C18 C 0.3205(2) 0.8527(2) 0.05117(11) 0.0265(14) Uani 1 1 d . . . . .
H18 H 0.2922 0.8603 0.0597 0.032 Uiso 1 1 calc R U . . .
C19 C 0.4450(2) 0.8194(2) 0.01135(11) 0.0261(14) Uani 1 1 d . . . . .
H19 H 0.4832 0.8528 0.0087 0.031 Uiso 1 1 calc R U . . .
N20 N 0.43615(19) 0.7687(2) 0.00289(9) 0.0217(11) Uani 1 1 d . . . . .
N21 N 0.4847(2) 0.7665(2) -0.00725(10) 0.0263(12) Uani 1 1 d . . . . .
C21A C 0.5442(2) 0.8185(3) -0.00654(14) 0.0476(19) Uani 1 1 d . . . . .
H21A H 0.5733 0.8067 -0.0114 0.071 Uiso 1 1 calc R U . . .
H21B H 0.5524 0.8357 0.0125 0.071 Uiso 1 1 calc R U . . .
H21C H 0.5467 0.8477 -0.0203 0.071 Uiso 1 1 calc R U . . .
N22 N 0.41731(19) 0.67551(19) -0.02882(8) 0.0221(11) Uani 1 1 d . . . . .
C23 C 0.4718(3) 0.7165(2) -0.02161(11) 0.0235(14) Uani 1 1 d . . . . .
N24 N 0.5138(2) 0.7051(2) -0.02999(9) 0.0275(12) Uani 1 1 d . . . . .
H24 H 0.5521 0.7274 -0.0271 0.033 Uiso 1 1 calc R U . . .
C25 C 0.4859(2) 0.6514(2) -0.04411(11) 0.0209(13) Uani 1 1 d . . . . .
C26 C 0.5082(2) 0.6188(2) -0.05645(11) 0.0257(14) Uani 1 1 d . . . . .
H26 H 0.5491 0.6312 -0.0558 0.031 Uiso 1 1 calc R U . . .
C27 C 0.4683(3) 0.5674(2) -0.06968(12) 0.0327(15) Uani 1 1 d . . . . .
H27 H 0.4816 0.5437 -0.0787 0.039 Uiso 1 1 calc R U . . .
C28 C 0.4086(3) 0.5498(3) -0.07006(12) 0.0325(15) Uani 1 1 d . . . . .
H28 H 0.3819 0.5138 -0.0792 0.039 Uiso 1 1 calc R U . . .
C29 C 0.3867(3) 0.5831(3) -0.05744(11) 0.0311(15) Uani 1 1 d . . . . .
H29 H 0.3459 0.5712 -0.0583 0.037 Uiso 1 1 calc R U . . .
C30 C 0.4260(2) 0.6332(3) -0.04393(11) 0.0245(14) Uani 1 1 d . . . . .
N1A N 0.4680(3) 0.4715(3) 0.12799(12) 0.0419(15) Uani 1 1 d . . . . .
O1A O 0.5119(2) 0.5166(2) 0.13331(13) 0.084(2) Uani 1 1 d . . . . .
O2A O 0.4554(2) 0.4246(2) 0.14067(9) 0.0540(13) Uani 1 1 d . . . . .
O3A O 0.4349(2) 0.4722(2) 0.10998(11) 0.0747(18) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O14 2.329(3) 2_665 ?
Dy1 O14 2.329(3) 3_565 ?
Dy1 O14 2.329(3) . ?
Dy1 N1 2.488(4) . ?
Dy1 N1 2.488(4) 3_565 ?
Dy1 N1 2.488(4) 2_665 ?
Dy1 N11 2.659(4) . ?
Dy1 N11 2.659(4) 3_565 ?
Dy1 N11 2.659(4) 2_665 ?
Dy1 Dy2 3.5249(6) . ?
Dy2 O14 2.317(3) . ?
Dy2 O14 2.317(3) 2_665 ?
Dy2 O14 2.317(3) 3_565 ?
Dy2 N22 2.513(4) 2_665 ?
Dy2 N22 2.513(4) 3_565 ?
Dy2 N22 2.513(4) . ?
Dy2 N20 2.679(4) 3_565 ?
Dy2 N20 2.679(4) . ?
Dy2 N20 2.679(4) 2_665 ?
N1 C2 1.341(7) . ?
N1 C9 1.412(6) . ?
C2 N3 1.350(7) . ?
C2 N10 1.357(7) . ?
N3 C4 1.386(7) . ?
N3 H3 0.8800 . ?
C4 C9 1.395(7) . ?
C4 C5 1.395(7) . ?
C5 C6 1.357(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.415(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(7) . ?
C8 H8 0.9500 . ?
N10 N11 1.393(6) . ?
N10 C10A 1.448(7) . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
N11 C12 1.285(6) . ?
C12 C13 1.442(7) . ?
C12 H12 0.9500 . ?
C13 C18 1.398(7) . ?
C13 C14 1.412(7) . ?
C14 O14 1.315(6) . ?
C14 C15 1.399(7) . ?
C15 C16 1.396(7) . ?
C15 C19 1.447(7) . ?
C16 C17 1.389(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(7) . ?
C17 C17A 1.532(7) . ?
C17A C17D 1.527(8) . ?
C17A C17B 1.535(7) . ?
C17A C17C 1.538(8) . ?
C17B H17A 0.9800 . ?
C17B H17B 0.9800 . ?
C17B H17C 0.9800 . ?
C17C H17D 0.9800 . ?
C17C H17E 0.9800 . ?
C17C H17F 0.9800 . ?
C17D H17G 0.9800 . ?
C17D H17H 0.9800 . ?
C17D H17I 0.9800 . ?
C18 H18 0.9500 . ?
C19 N20 1.289(6) . ?
C19 H19 0.9500 . ?
N20 N21 1.385(6) . ?
N21 C23 1.357(7) . ?
N21 C21A 1.466(7) . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
N22 C23 1.329(7) . ?
N22 C30 1.426(7) . ?
C23 N24 1.336(7) . ?
N24 C25 1.388(6) . ?
N24 H24 0.8800 . ?
C25 C26 1.380(7) . ?
C25 C30 1.389(7) . ?
C26 C27 1.371(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.394(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.355(7) . ?
C29 H29 0.9500 . ?
N1A O1A 1.192(7) . ?
N1A O3A 1.221(6) . ?
N1A O2A 1.252(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
O14 Dy1 O14 68.47(13) 2_665 3_565 ?
O14 Dy1 O14 68.47(13) 2_665 . ?
O14 Dy1 O14 68.47(13) 3_565 . ?
O14 Dy1 N1 85.44(13) 2_665 . ?
O14 Dy1 N1 143.77(13) 3_565 . ?
O14 Dy1 N1 125.60(13) . . ?
O14 Dy1 N1 143.77(13) 2_665 3_565 ?
O14 Dy1 N1 125.60(13) 3_565 3_565 ?
O14 Dy1 N1 85.45(13) . 3_565 ?
N1 Dy1 N1 90.32(14) . 3_565 ?
O14 Dy1 N1 125.60(13) 2_665 2_665 ?
O14 Dy1 N1 85.44(13) 3_565 2_665 ?
O14 Dy1 N1 143.77(13) . 2_665 ?
N1 Dy1 N1 90.32(14) . 2_665 ?
N1 Dy1 N1 90.32(14) 3_565 2_665 ?
O14 Dy1 N11 74.55(12) 2_665 . ?
O14 Dy1 N11 127.95(13) 3_565 . ?
O14 Dy1 N11 64.49(13) . . ?
N1 Dy1 N11 62.81(14) . . ?
N1 Dy1 N11 71.58(13) 3_565 . ?
N1 Dy1 N11 146.60(14) 2_665 . ?
O14 Dy1 N11 127.95(13) 2_665 3_565 ?
O14 Dy1 N11 64.50(13) 3_565 3_565 ?
O14 Dy1 N11 74.56(12) . 3_565 ?
N1 Dy1 N11 146.60(14) . 3_565 ?
N1 Dy1 N11 62.81(14) 3_565 3_565 ?
N1 Dy1 N11 71.58(13) 2_665 3_565 ?
N11 Dy1 N11 119.873(12) . 3_565 ?
O14 Dy1 N11 64.49(13) 2_665 2_665 ?
O14 Dy1 N11 74.56(12) 3_565 2_665 ?
O14 Dy1 N11 127.94(13) . 2_665 ?
N1 Dy1 N11 71.57(13) . 2_665 ?
N1 Dy1 N11 146.60(14) 3_565 2_665 ?
N1 Dy1 N11 62.81(14) 2_665 2_665 ?
N11 Dy1 N11 119.870(12) . 2_665 ?
N11 Dy1 N11 119.872(12) 3_565 2_665 ?
O14 Dy1 Dy2 40.51(8) 2_665 . ?
O14 Dy1 Dy2 40.51(8) 3_565 . ?
O14 Dy1 Dy2 40.51(8) . . ?
N1 Dy1 Dy2 125.03(10) . . ?
N1 Dy1 Dy2 125.04(10) 3_565 . ?
N1 Dy1 Dy2 125.04(10) 2_665 . ?
N11 Dy1 Dy2 87.94(9) . . ?
N11 Dy1 Dy2 87.94(9) 3_565 . ?
N11 Dy1 Dy2 87.94(9) 2_665 . ?
O14 Dy2 O14 68.89(13) . 2_665 ?
O14 Dy2 O14 68.89(13) . 3_565 ?
O14 Dy2 O14 68.89(13) 2_665 3_565 ?
O14 Dy2 N22 83.83(13) . 2_665 ?
O14 Dy2 N22 125.29(13) 2_665 2_665 ?
O14 Dy2 N22 142.46(13) 3_565 2_665 ?
O14 Dy2 N22 142.46(13) . 3_565 ?
O14 Dy2 N22 83.84(13) 2_665 3_565 ?
O14 Dy2 N22 125.29(13) 3_565 3_565 ?
N22 Dy2 N22 92.08(13) 2_665 3_565 ?
O14 Dy2 N22 125.29(13) . . ?
O14 Dy2 N22 142.46(13) 2_665 . ?
O14 Dy2 N22 83.84(13) 3_565 . ?
N22 Dy2 N22 92.08(13) 2_665 . ?
N22 Dy2 N22 92.08(13) 3_565 . ?
O14 Dy2 N20 128.22(12) . 3_565 ?
O14 Dy2 N20 73.76(12) 2_665 3_565 ?
O14 Dy2 N20 64.87(12) 3_565 3_565 ?
N22 Dy2 N20 147.91(13) 2_665 3_565 ?
N22 Dy2 N20 62.25(13) 3_565 3_565 ?
N22 Dy2 N20 71.42(13) . 3_565 ?
O14 Dy2 N20 64.87(12) . . ?
O14 Dy2 N20 128.22(12) 2_665 . ?
O14 Dy2 N20 73.75(12) 3_565 . ?
N22 Dy2 N20 71.42(13) 2_665 . ?
N22 Dy2 N20 147.91(13) 3_565 . ?
N22 Dy2 N20 62.25(13) . . ?
N20 Dy2 N20 119.859(12) 3_565 . ?
O14 Dy2 N20 73.75(12) . 2_665 ?
O14 Dy2 N20 64.87(12) 2_665 2_665 ?
O14 Dy2 N20 128.22(12) 3_565 2_665 ?
N22 Dy2 N20 62.25(13) 2_665 2_665 ?
N22 Dy2 N20 71.42(13) 3_565 2_665 ?
N22 Dy2 N20 147.91(13) . 2_665 ?
N20 Dy2 N20 119.859(12) 3_565 2_665 ?
N20 Dy2 N20 119.858(12) . 2_665 ?
O14 Dy2 Dy1 40.78(8) . . ?
O14 Dy2 Dy1 40.78(8) 2_665 . ?
O14 Dy2 Dy1 40.78(8) 3_565 . ?
N22 Dy2 Dy1 123.78(10) 2_665 . ?
N22 Dy2 Dy1 123.78(10) 3_565 . ?
N22 Dy2 Dy1 123.78(10) . . ?
N20 Dy2 Dy1 87.84(9) 3_565 . ?
N20 Dy2 Dy1 87.84(9) . . ?
N20 Dy2 Dy1 87.84(9) 2_665 . ?
C2 N1 C9 104.1(5) . . ?
C2 N1 Dy1 117.3(4) . . ?
C9 N1 Dy1 132.6(3) . . ?
N1 C2 N3 113.4(5) . . ?
N1 C2 N10 124.0(5) . . ?
N3 C2 N10 122.6(5) . . ?
C2 N3 C4 106.9(5) . . ?
C2 N3 H3 126.5 . . ?
C4 N3 H3 126.5 . . ?
N3 C4 C9 106.3(5) . . ?
N3 C4 C5 131.5(5) . . ?
C9 C4 C5 122.2(6) . . ?
C6 C5 C4 116.9(6) . . ?
C6 C5 H5 121.5 . . ?
C4 C5 H5 121.5 . . ?
C5 C6 C7 121.8(6) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 120.7(6) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C9 C8 C7 117.8(6) . . ?
C9 C8 H8 121.1 . . ?
C7 C8 H8 121.1 . . ?
C8 C9 C4 120.5(5) . . ?
C8 C9 N1 130.3(6) . . ?
C4 C9 N1 109.2(5) . . ?
C2 N10 N11 114.2(5) . . ?
C2 N10 C10A 122.4(5) . . ?
N11 N10 C10A 122.7(5) . . ?
N10 C10A H10A 109.5 . . ?
N10 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
N10 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C12 N11 N10 116.4(5) . . ?
C12 N11 Dy1 128.5(4) . . ?
N10 N11 Dy1 115.1(3) . . ?
N11 C12 C13 123.6(5) . . ?
N11 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C18 C13 C14 118.5(5) . . ?
C18 C13 C12 119.8(5) . . ?
C14 C13 C12 121.5(5) . . ?
O14 C14 C15 120.8(5) . . ?
O14 C14 C13 120.0(5) . . ?
C15 C14 C13 119.2(5) . . ?
C14 O14 Dy2 130.8(3) . . ?
C14 O14 Dy1 130.5(3) . . ?
Dy2 O14 Dy1 98.71(13) . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 C19 118.6(5) . . ?
C14 C15 C19 121.8(5) . . ?
C17 C16 C15 122.9(5) . . ?
C17 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
C18 C17 C16 116.3(5) . . ?
C18 C17 C17A 121.2(5) . . ?
C16 C17 C17A 122.4(5) . . ?
C17D C17A C17 112.2(5) . . ?
C17D C17A C17B 109.2(5) . . ?
C17 C17A C17B 107.4(5) . . ?
C17D C17A C17C 108.7(5) . . ?
C17 C17A C17C 111.0(5) . . ?
C17B C17A C17C 108.2(5) . . ?
C17A C17B H17A 109.5 . . ?
C17A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C17A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C17A C17C H17D 109.5 . . ?
C17A C17C H17E 109.5 . . ?
H17D C17C H17E 109.5 . . ?
C17A C17C H17F 109.5 . . ?
H17D C17C H17F 109.5 . . ?
H17E C17C H17F 109.5 . . ?
C17A C17D H17G 109.5 . . ?
C17A C17D H17H 109.5 . . ?
H17G C17D H17H 109.5 . . ?
C17A C17D H17I 109.5 . . ?
H17G C17D H17I 109.5 . . ?
H17H C17D H17I 109.5 . . ?
C17 C18 C13 123.5(5) . . ?
C17 C18 H18 118.3 . . ?
C13 C18 H18 118.3 . . ?
N20 C19 C15 124.0(5) . . ?
N20 C19 H19 118.0 . . ?
C15 C19 H19 118.0 . . ?
C19 N20 N21 116.9(5) . . ?
C19 N20 Dy2 127.6(4) . . ?
N21 N20 Dy2 115.4(3) . . ?
C23 N21 N20 114.9(4) . . ?
C23 N21 C21A 122.8(5) . . ?
N20 N21 C21A 121.6(4) . . ?
N21 C21A H21A 109.5 . . ?
N21 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
N21 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23 N22 C30 103.4(4) . . ?
C23 N22 Dy2 117.7(3) . . ?
C30 N22 Dy2 132.7(3) . . ?
N22 C23 N24 114.4(5) . . ?
N22 C23 N21 123.8(5) . . ?
N24 C23 N21 121.8(5) . . ?
C23 N24 C25 107.0(5) . . ?
C23 N24 H24 126.5 . . ?
C25 N24 H24 126.5 . . ?
C26 C25 N24 131.0(5) . . ?
C26 C25 C30 122.9(5) . . ?
N24 C25 C30 106.0(5) . . ?
C27 C26 C25 116.5(5) . . ?
C27 C26 H26 121.7 . . ?
C25 C26 H26 121.7 . . ?
C26 C27 C28 120.7(5) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C29 122.1(6) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C30 C29 C28 117.1(6) . . ?
C30 C29 H29 121.5 . . ?
C28 C29 H29 121.5 . . ?
C29 C30 C25 120.5(5) . . ?
C29 C30 N22 130.3(5) . . ?
C25 C30 N22 109.1(5) . . ?
O1A N1A O3A 118.1(6) . . ?
O1A N1A O2A 121.3(6) . . ?
O3A N1A O2A 120.5(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N3 -1.3(6) . . . . ?
Dy1 N1 C2 N3 155.1(3) . . . . ?
C9 N1 C2 N10 178.8(5) . . . . ?
Dy1 N1 C2 N10 -24.8(7) . . . . ?
N1 C2 N3 C4 0.8(6) . . . . ?
N10 C2 N3 C4 -179.3(5) . . . . ?
C2 N3 C4 C9 0.0(6) . . . . ?
C2 N3 C4 C5 179.9(6) . . . . ?
N3 C4 C5 C6 -178.6(5) . . . . ?
C9 C4 C5 C6 1.2(8) . . . . ?
C4 C5 C6 C7 1.5(9) . . . . ?
C5 C6 C7 C8 -1.7(9) . . . . ?
C6 C7 C8 C9 -0.9(9) . . . . ?
C7 C8 C9 C4 3.5(8) . . . . ?
C7 C8 C9 N1 179.7(5) . . . . ?
N3 C4 C9 C8 176.1(5) . . . . ?
C5 C4 C9 C8 -3.8(8) . . . . ?
N3 C4 C9 N1 -0.8(6) . . . . ?
C5 C4 C9 N1 179.3(5) . . . . ?
C2 N1 C9 C8 -175.2(6) . . . . ?
Dy1 N1 C9 C8 33.7(8) . . . . ?
C2 N1 C9 C4 1.3(6) . . . . ?
Dy1 N1 C9 C4 -149.9(4) . . . . ?
N1 C2 N10 N11 5.2(8) . . . . ?
N3 C2 N10 N11 -174.7(5) . . . . ?
N1 C2 N10 C10A -165.9(6) . . . . ?
N3 C2 N10 C10A 14.2(9) . . . . ?
C2 N10 N11 C12 -163.4(5) . . . . ?
C10A N10 N11 C12 7.7(8) . . . . ?
C2 N10 N11 Dy1 15.3(5) . . . . ?
C10A N10 N11 Dy1 -173.7(5) . . . . ?
N10 N11 C12 C13 -174.1(5) . . . . ?
Dy1 N11 C12 C13 7.4(8) . . . . ?
N11 C12 C13 C18 -161.3(5) . . . . ?
N11 C12 C13 C14 23.7(8) . . . . ?
C18 C13 C14 O14 -178.9(5) . . . . ?
C12 C13 C14 O14 -3.9(8) . . . . ?
C18 C13 C14 C15 2.6(8) . . . . ?
C12 C13 C14 C15 177.7(5) . . . . ?
C15 C14 O14 Dy2 -57.9(6) . . . . ?
C13 C14 O14 Dy2 123.6(4) . . . . ?
C15 C14 O14 Dy1 120.8(5) . . . . ?
C13 C14 O14 Dy1 -57.7(6) . . . . ?
O14 C14 C15 C16 -178.8(5) . . . . ?
C13 C14 C15 C16 -0.3(8) . . . . ?
O14 C14 C15 C19 -2.3(8) . . . . ?
C13 C14 C15 C19 176.2(5) . . . . ?
C14 C15 C16 C17 -1.5(8) . . . . ?
C19 C15 C16 C17 -178.1(5) . . . . ?
C15 C16 C17 C18 0.7(8) . . . . ?
C15 C16 C17 C17A 177.8(5) . . . . ?
C18 C17 C17A C17D -168.0(5) . . . . ?
C16 C17 C17A C17D 15.1(8) . . . . ?
C18 C17 C17A C17B 72.0(7) . . . . ?
C16 C17 C17A C17B -104.9(6) . . . . ?
C18 C17 C17A C17C -46.1(7) . . . . ?
C16 C17 C17A C17C 136.9(5) . . . . ?
C16 C17 C18 C13 1.8(8) . . . . ?
C17A C17 C18 C13 -175.3(5) . . . . ?
C14 C13 C18 C17 -3.5(8) . . . . ?
C12 C13 C18 C17 -178.6(5) . . . . ?
C16 C15 C19 N20 -161.7(5) . . . . ?
C14 C15 C19 N20 21.7(8) . . . . ?
C15 C19 N20 N21 -174.7(5) . . . . ?
C15 C19 N20 Dy2 7.7(8) . . . . ?
C19 N20 N21 C23 -166.0(5) . . . . ?
Dy2 N20 N21 C23 11.9(5) . . . . ?
C19 N20 N21 C21A 4.2(7) . . . . ?
Dy2 N20 N21 C21A -177.9(4) . . . . ?
C30 N22 C23 N24 -0.8(6) . . . . ?
Dy2 N22 C23 N24 155.1(4) . . . . ?
C30 N22 C23 N21 178.4(5) . . . . ?
Dy2 N22 C23 N21 -25.7(7) . . . . ?
N20 N21 C23 N22 8.2(7) . . . . ?
C21A N21 C23 N22 -161.8(6) . . . . ?
N20 N21 C23 N24 -172.6(5) . . . . ?
C21A N21 C23 N24 17.3(8) . . . . ?
N22 C23 N24 C25 -0.3(6) . . . . ?
N21 C23 N24 C25 -179.5(5) . . . . ?
C23 N24 C25 C26 -178.6(6) . . . . ?
C23 N24 C25 C30 1.2(6) . . . . ?
N24 C25 C26 C27 -178.1(5) . . . . ?
C30 C25 C26 C27 2.1(8) . . . . ?
C25 C26 C27 C28 -0.7(8) . . . . ?
C26 C27 C28 C29 0.6(9) . . . . ?
C27 C28 C29 C30 -1.7(9) . . . . ?
C28 C29 C30 C25 3.1(8) . . . . ?
C28 C29 C30 N22 -178.9(5) . . . . ?
C26 C25 C30 C29 -3.4(9) . . . . ?
N24 C25 C30 C29 176.7(5) . . . . ?
C26 C25 C30 N22 178.1(5) . . . . ?
N24 C25 C30 N22 -1.7(6) . . . . ?
C23 N22 C30 C29 -176.7(6) . . . . ?
Dy2 N22 C30 C29 32.8(8) . . . . ?
C23 N22 C30 C25 1.5(6) . . . . ?
Dy2 N22 C30 C25 -149.0(4) . . . . ?

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
N3 H3 O3A 0.88 1.97 2.809(6) 158.8 3_565
C5 H5 O1A 0.95 2.60 3.360(8) 137.1 3_565
C10A H10A O3A 0.98 2.12 3.046(8) 156.6 3_565
C21A H21A O1A 0.98 2.46 3.256(7) 138.5 29
C21A H21A O2A 0.98 2.62 3.588(7) 170.5 29
N24 H24 O2A 0.88 1.92 2.775(6) 163.8 29

_refine_diff_density_max         1.564
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.105



####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1038103'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-19 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         'C84 H87 Ho2 N24 O3, 3(N O3)'
_chemical_formula_sum            'C84 H87 Ho2 N27 O12'
_chemical_formula_weight         1996.66

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   26.1368(10)
_cell_length_b                   26.1368(10)
_cell_length_c                   48.150(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     28486(2)
_cell_formula_units_Z            12
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2769
_cell_measurement_theta_min      3.1740
_cell_measurement_theta_max      25.4380

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_F_000             12120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    1.725
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.93928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       ω-scan
_diffrn_reflns_number            18209
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_theta_min         2.921
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5577
_reflns_number_gt                2877
_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       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0419P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5577
_refine_ls_number_parameters     381
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_restrained_S_all      0.952
_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
Ho1 Ho 0.3333 0.6667 0.07324(2) 0.03784(13) Uani 1 3 d S T P . .
Ho2 Ho 0.3333 0.6667 0.00017(2) 0.03486(13) Uani 1 3 d S T P . .
N1 N 0.2452(2) 0.6108(2) 0.10315(9) 0.0490(13) Uani 1 1 d . . . . .
C2 C 0.1967(3) 0.6129(3) 0.09699(12) 0.0480(17) Uani 1 1 d . . . . .
N3 N 0.1470(2) 0.5662(2) 0.10669(9) 0.0522(13) Uani 1 1 d . . . . .
H3 H 0.1116 0.5594 0.1043 0.063 Uiso 1 1 calc R U . . .
C4 C 0.1635(3) 0.5318(3) 0.12117(13) 0.0561(17) Uani 1 1 d . . . . .
C5 C 0.1301(3) 0.4796(3) 0.13538(13) 0.0686(19) Uani 1 1 d . . . . .
H5 H 0.0891 0.4603 0.1357 0.082 Uiso 1 1 calc R U . . .
C6 C 0.1617(4) 0.4576(3) 0.14909(15) 0.086(2) Uani 1 1 d . . . . .
H6 H 0.1411 0.4227 0.1591 0.104 Uiso 1 1 calc R U . . .
C7 C 0.2232(4) 0.4857(3) 0.14850(14) 0.081(2) Uani 1 1 d . . . . .
H7 H 0.2428 0.4697 0.1581 0.097 Uiso 1 1 calc R U . . .
C8 C 0.2550(3) 0.5376(3) 0.13364(13) 0.066(2) Uani 1 1 d . . . . .
H8 H 0.2961 0.5569 0.1332 0.079 Uiso 1 1 calc R U . . .
C9 C 0.2248(3) 0.5601(3) 0.11957(12) 0.0529(17) Uani 1 1 d . . . . .
N10 N 0.1962(2) 0.6561(2) 0.08168(10) 0.0516(13) Uani 1 1 d . . . . .
C10A C 0.1441(3) 0.6621(3) 0.07926(16) 0.097(3) Uani 1 1 d . . . . .
H10A H 0.1093 0.6241 0.0818 0.146 Uiso 1 1 calc R U . . .
H10B H 0.1432 0.6771 0.0612 0.146 Uiso 1 1 calc R U . . .
H10C H 0.1452 0.6889 0.0932 0.146 Uiso 1 1 calc R U . . .
N11 N 0.25101(19) 0.6979(2) 0.07150(9) 0.0443(12) Uani 1 1 d . . . . .
C12 C 0.2560(3) 0.7469(3) 0.06341(11) 0.0495(14) Uani 1 1 d . . . . .
H12 H 0.2241 0.7529 0.0659 0.059 Uiso 1 1 calc R U . . .
C13 C 0.3096(2) 0.7940(2) 0.05043(11) 0.0407(14) Uani 1 1 d . . . . .
C14 C 0.3502(2) 0.7821(2) 0.03695(11) 0.0389(14) Uani 1 1 d . . . . .
O14 O 0.34194(14) 0.72771(15) 0.03653(6) 0.0382(9) Uani 1 1 d . . . . .
C15 C 0.3986(2) 0.8284(2) 0.02355(11) 0.0391(14) Uani 1 1 d . . . . .
C16 C 0.4071(3) 0.8854(2) 0.02440(11) 0.0483(15) Uani 1 1 d . . . . .
H16 H 0.4407 0.9160 0.0161 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3673(3) 0.8981(3) 0.03716(12) 0.0528(16) Uani 1 1 d . U . . .
C17A C 0.3770(3) 0.9612(3) 0.03836(16) 0.076(2) Uani 1 1 d . U . . .
C17B C 0.3985(4) 0.9851(3) 0.06762(18) 0.117(3) Uani 1 1 d . U . . .
H17A H 0.4049 1.0245 0.0690 0.175 Uiso 1 1 calc R U . . .
H17B H 0.4349 0.9857 0.0713 0.175 Uiso 1 1 calc R U . . .
H17C H 0.3694 0.9602 0.0810 0.175 Uiso 1 1 calc R U . . .
C17C C 0.3221(3) 0.9629(3) 0.03346(18) 0.118(3) Uani 1 1 d . U . . .
H17D H 0.3288 1.0018 0.0376 0.178 Uiso 1 1 calc R U . . .
H17E H 0.2914 0.9346 0.0453 0.178 Uiso 1 1 calc R U . . .
H17F H 0.3105 0.9536 0.0144 0.178 Uiso 1 1 calc R U . . .
C17D C 0.4241(4) 1.0026(3) 0.01840(18) 0.126(3) Uani 1 1 d . U . . .
H17G H 0.4144 0.9865 0.0000 0.189 Uiso 1 1 calc R U . . .
H17H H 0.4616 1.0073 0.0238 0.189 Uiso 1 1 calc R U . . .
H17I H 0.4262 1.0403 0.0188 0.189 Uiso 1 1 calc R U . . .
C18 C 0.3183(3) 0.8511(2) 0.04980(11) 0.0517(16) Uani 1 1 d . . . . .
H18 H 0.2904 0.8582 0.0582 0.062 Uiso 1 1 calc R U . . .
C19 C 0.4437(2) 0.8197(2) 0.01054(11) 0.0447(15) Uani 1 1 d . . . . .
H19 H 0.4809 0.8527 0.0079 0.054 Uiso 1 1 calc R U . . .
N20 N 0.43580(18) 0.76928(19) 0.00240(9) 0.0401(11) Uani 1 1 d . . . . .
N21 N 0.4844(2) 0.7680(2) -0.00806(10) 0.0511(14) Uani 1 1 d . . . . .
C21A C 0.5434(3) 0.8194(3) -0.00773(16) 0.094(3) Uani 1 1 d . . . . .
H21A H 0.5718 0.8075 -0.0121 0.141 Uiso 1 1 calc R U . . .
H21B H 0.5516 0.8371 0.0104 0.141 Uiso 1 1 calc R U . . .
H21C H 0.5458 0.8475 -0.0212 0.141 Uiso 1 1 calc R U . . .
N22 N 0.4164(2) 0.6761(2) -0.02933(9) 0.0471(12) Uani 1 1 d . . . . .
C23 C 0.4713(3) 0.7180(3) -0.02201(12) 0.0445(15) Uani 1 1 d . . . . .
N24 N 0.5139(2) 0.7062(2) -0.03038(9) 0.0519(13) Uani 1 1 d . . . . .
H24 H 0.5513 0.7280 -0.0276 0.062 Uiso 1 1 calc R U . . .
C25 C 0.4862(3) 0.6528(3) -0.04412(12) 0.0500(16) Uani 1 1 d . . . . .
C26 C 0.5090(3) 0.6209(3) -0.05625(13) 0.0621(18) Uani 1 1 d . . . . .
H26 H 0.5491 0.6333 -0.0556 0.074 Uiso 1 1 calc R U . . .
C27 C 0.4695(3) 0.5699(3) -0.06927(13) 0.070(2) Uani 1 1 d . . . . .
H27 H 0.4829 0.5469 -0.0778 0.084 Uiso 1 1 calc R U . . .
C28 C 0.4096(4) 0.5517(3) -0.06999(13) 0.072(2) Uani 1 1 d . . . . .
H28 H 0.3840 0.5169 -0.0792 0.087 Uiso 1 1 calc R U . . .
C29 C 0.3866(3) 0.5838(3) -0.05729(12) 0.0576(18) Uani 1 1 d . . . . .
H29 H 0.3465 0.5714 -0.0579 0.069 Uiso 1 1 calc R U . . .
C30 C 0.4266(3) 0.6353(3) -0.04373(11) 0.0417(14) Uani 1 1 d . . . . .
N1A N 0.4648(4) 0.4687(4) 0.12781(17) 0.094(2) Uani 1 1 d . . . . .
O1A O 0.5072(4) 0.5144(4) 0.13353(19) 0.182(4) Uani 1 1 d . . . . .
O2A O 0.4582(3) 0.4267(3) 0.14010(14) 0.135(3) Uani 1 1 d . . . . .
O3A O 0.4351(4) 0.4734(3) 0.11115(16) 0.171(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O14 2.315(3) . ?
Ho1 O14 2.316(3) 2_665 ?
Ho1 O14 2.316(3) 3_565 ?
Ho1 N1 2.480(4) 3_565 ?
Ho1 N1 2.480(4) . ?
Ho1 N1 2.480(4) 2_665 ?
Ho1 N11 2.656(5) . ?
Ho1 N11 2.656(5) 3_565 ?
Ho1 N11 2.656(5) 2_665 ?
Ho1 Ho2 3.5182(5) . ?
Ho2 O14 2.303(3) 2_665 ?
Ho2 O14 2.303(3) 3_565 ?
Ho2 O14 2.303(3) . ?
Ho2 N22 2.501(4) . ?
Ho2 N22 2.501(4) 2_665 ?
Ho2 N22 2.501(4) 3_565 ?
Ho2 N20 2.682(4) 2_665 ?
Ho2 N20 2.682(4) . ?
Ho2 N20 2.682(4) 3_565 ?
N1 C2 1.328(7) . ?
N1 C9 1.399(7) . ?
C2 N3 1.345(7) . ?
C2 N10 1.355(7) . ?
N3 C4 1.368(7) . ?
N3 H3 0.8600 . ?
C4 C5 1.379(8) . ?
C4 C9 1.391(8) . ?
C5 C6 1.386(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.393(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.384(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.376(8) . ?
C8 H8 0.9300 . ?
N10 N11 1.386(6) . ?
N10 C10A 1.451(7) . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9600 . ?
C10A H10C 0.9600 . ?
N11 C12 1.283(7) . ?
C12 C13 1.463(7) . ?
C12 H12 0.9300 . ?
C13 C18 1.393(7) . ?
C13 C14 1.407(7) . ?
C14 O14 1.327(6) . ?
C14 C15 1.396(7) . ?
C15 C16 1.394(7) . ?
C15 C19 1.450(7) . ?
C16 C17 1.385(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.393(7) . ?
C17 C17A 1.539(8) . ?
C17A C17C 1.477(8) . ?
C17A C17D 1.509(9) . ?
C17A C17B 1.530(9) . ?
C17B H17A 0.9600 . ?
C17B H17B 0.9600 . ?
C17B H17C 0.9600 . ?
C17C H17D 0.9600 . ?
C17C H17E 0.9600 . ?
C17C H17F 0.9600 . ?
C17D H17G 0.9600 . ?
C17D H17H 0.9600 . ?
C17D H17I 0.9600 . ?
C18 H18 0.9300 . ?
C19 N20 1.288(6) . ?
C19 H19 0.9300 . ?
N20 N21 1.383(5) . ?
N21 C23 1.352(7) . ?
N21 C21A 1.453(7) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
N22 C23 1.345(7) . ?
N22 C30 1.405(6) . ?
C23 N24 1.357(6) . ?
N24 C25 1.377(7) . ?
N24 H24 0.8600 . ?
C25 C26 1.375(7) . ?
C25 C30 1.387(7) . ?
C26 C27 1.363(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.390(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.396(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.387(7) . ?
C29 H29 0.9300 . ?
N1A O3A 1.164(8) . ?
N1A O2A 1.182(8) . ?
N1A O1A 1.187(10) . ?

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
O14 Ho1 O14 68.03(13) . 2_665 ?
O14 Ho1 O14 68.03(13) . 3_565 ?
O14 Ho1 O14 68.03(13) 2_665 3_565 ?
O14 Ho1 N1 86.14(14) . 3_565 ?
O14 Ho1 N1 143.79(13) 2_665 3_565 ?
O14 Ho1 N1 126.21(13) 3_565 3_565 ?
O14 Ho1 N1 126.21(13) . . ?
O14 Ho1 N1 86.14(14) 2_665 . ?
O14 Ho1 N1 143.79(13) 3_565 . ?
N1 Ho1 N1 89.65(15) 3_565 . ?
O14 Ho1 N1 143.79(13) . 2_665 ?
O14 Ho1 N1 126.21(13) 2_665 2_665 ?
O14 Ho1 N1 86.14(14) 3_565 2_665 ?
N1 Ho1 N1 89.65(15) 3_565 2_665 ?
N1 Ho1 N1 89.65(15) . 2_665 ?
O14 Ho1 N11 65.10(13) . . ?
O14 Ho1 N11 74.54(13) 2_665 . ?
O14 Ho1 N11 127.98(13) 3_565 . ?
N1 Ho1 N11 71.62(14) 3_565 . ?
N1 Ho1 N11 62.78(14) . . ?
N1 Ho1 N11 145.87(15) 2_665 . ?
O14 Ho1 N11 74.54(13) . 3_565 ?
O14 Ho1 N11 127.98(13) 2_665 3_565 ?
O14 Ho1 N11 65.10(13) 3_565 3_565 ?
N1 Ho1 N11 62.78(14) 3_565 3_565 ?
N1 Ho1 N11 145.87(15) . 3_565 ?
N1 Ho1 N11 71.62(14) 2_665 3_565 ?
N11 Ho1 N11 119.900(11) . 3_565 ?
O14 Ho1 N11 127.98(13) . 2_665 ?
O14 Ho1 N11 65.10(13) 2_665 2_665 ?
O14 Ho1 N11 74.54(13) 3_565 2_665 ?
N1 Ho1 N11 145.87(15) 3_565 2_665 ?
N1 Ho1 N11 71.62(14) . 2_665 ?
N1 Ho1 N11 62.78(14) 2_665 2_665 ?
N11 Ho1 N11 119.903(11) . 2_665 ?
N11 Ho1 N11 119.901(11) 3_565 2_665 ?
O14 Ho1 Ho2 40.24(8) . . ?
O14 Ho1 Ho2 40.24(8) 2_665 . ?
O14 Ho1 Ho2 40.24(8) 3_565 . ?
N1 Ho1 Ho2 125.51(11) 3_565 . ?
N1 Ho1 Ho2 125.51(11) . . ?
N1 Ho1 Ho2 125.51(11) 2_665 . ?
N11 Ho1 Ho2 88.19(10) . . ?
N11 Ho1 Ho2 88.19(10) 3_565 . ?
N11 Ho1 Ho2 88.19(10) 2_665 . ?
O14 Ho2 O14 68.47(13) 2_665 3_565 ?
O14 Ho2 O14 68.47(13) 2_665 . ?
O14 Ho2 O14 68.47(13) 3_565 . ?
O14 Ho2 N22 143.05(13) 2_665 . ?
O14 Ho2 N22 84.93(14) 3_565 . ?
O14 Ho2 N22 125.76(13) . . ?
O14 Ho2 N22 125.76(13) 2_665 2_665 ?
O14 Ho2 N22 143.05(13) 3_565 2_665 ?
O14 Ho2 N22 84.93(14) . 2_665 ?
N22 Ho2 N22 90.94(15) . 2_665 ?
O14 Ho2 N22 84.93(14) 2_665 3_565 ?
O14 Ho2 N22 125.76(13) 3_565 3_565 ?
O14 Ho2 N22 143.05(13) . 3_565 ?
N22 Ho2 N22 90.94(15) . 3_565 ?
N22 Ho2 N22 90.94(15) 2_665 3_565 ?
O14 Ho2 N20 64.78(12) 2_665 2_665 ?
O14 Ho2 N20 127.80(12) 3_565 2_665 ?
O14 Ho2 N20 73.84(12) . 2_665 ?
N22 Ho2 N20 147.25(14) . 2_665 ?
N22 Ho2 N20 62.68(14) 2_665 2_665 ?
N22 Ho2 N20 71.72(14) 3_565 2_665 ?
O14 Ho2 N20 127.80(12) 2_665 . ?
O14 Ho2 N20 73.84(12) 3_565 . ?
O14 Ho2 N20 64.78(12) . . ?
N22 Ho2 N20 62.68(14) . . ?
N22 Ho2 N20 71.72(14) 2_665 . ?
N22 Ho2 N20 147.24(14) 3_565 . ?
N20 Ho2 N20 119.841(13) 2_665 . ?
O14 Ho2 N20 73.84(12) 2_665 3_565 ?
O14 Ho2 N20 64.78(12) 3_565 3_565 ?
O14 Ho2 N20 127.80(12) . 3_565 ?
N22 Ho2 N20 71.72(14) . 3_565 ?
N22 Ho2 N20 147.24(14) 2_665 3_565 ?
N22 Ho2 N20 62.68(14) 3_565 3_565 ?
N20 Ho2 N20 119.840(13) 2_665 3_565 ?
N20 Ho2 N20 119.840(13) . 3_565 ?
O14 Ho2 Ho1 40.51(8) 2_665 . ?
O14 Ho2 Ho1 40.51(8) 3_565 . ?
O14 Ho2 Ho1 40.51(8) . . ?
N22 Ho2 Ho1 124.60(10) . . ?
N22 Ho2 Ho1 124.60(10) 2_665 . ?
N22 Ho2 Ho1 124.60(10) 3_565 . ?
N20 Ho2 Ho1 87.70(9) 2_665 . ?
N20 Ho2 Ho1 87.70(9) . . ?
N20 Ho2 Ho1 87.70(9) 3_565 . ?
C2 N1 C9 104.3(5) . . ?
C2 N1 Ho1 118.0(4) . . ?
C9 N1 Ho1 133.4(4) . . ?
N1 C2 N3 113.2(5) . . ?
N1 C2 N10 124.3(5) . . ?
N3 C2 N10 122.5(6) . . ?
C2 N3 C4 107.1(5) . . ?
C2 N3 H3 126.4 . . ?
C4 N3 H3 126.4 . . ?
N3 C4 C5 130.7(6) . . ?
N3 C4 C9 106.2(6) . . ?
C5 C4 C9 123.1(7) . . ?
C4 C5 C6 115.6(7) . . ?
C4 C5 H5 122.2 . . ?
C6 C5 H5 122.2 . . ?
C5 C6 C7 122.7(7) . . ?
C5 C6 H6 118.6 . . ?
C7 C6 H6 118.6 . . ?
C8 C7 C6 119.9(7) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C9 C8 C7 118.8(7) . . ?
C9 C8 H8 120.6 . . ?
C7 C8 H8 120.6 . . ?
C8 C9 C4 119.9(6) . . ?
C8 C9 N1 131.0(6) . . ?
C4 C9 N1 109.1(6) . . ?
C2 N10 N11 114.3(5) . . ?
C2 N10 C10A 122.3(5) . . ?
N11 N10 C10A 123.0(5) . . ?
N10 C10A H10A 109.5 . . ?
N10 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
N10 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C12 N11 N10 116.3(5) . . ?
C12 N11 Ho1 128.5(4) . . ?
N10 N11 Ho1 115.1(3) . . ?
N11 C12 C13 123.2(5) . . ?
N11 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C18 C13 C14 119.3(5) . . ?
C18 C13 C12 119.1(5) . . ?
C14 C13 C12 121.4(5) . . ?
O14 C14 C15 120.8(5) . . ?
O14 C14 C13 120.5(5) . . ?
C15 C14 C13 118.6(5) . . ?
C14 O14 Ho2 131.4(3) . . ?
C14 O14 Ho1 129.4(3) . . ?
Ho2 O14 Ho1 99.25(13) . . ?
C16 C15 C14 120.2(5) . . ?
C16 C15 C19 118.2(5) . . ?
C14 C15 C19 121.3(5) . . ?
C17 C16 C15 122.1(5) . . ?
C17 C16 H16 118.9 . . ?
C15 C16 H16 118.9 . . ?
C16 C17 C18 116.9(5) . . ?
C16 C17 C17A 122.1(5) . . ?
C18 C17 C17A 121.0(5) . . ?
C17C C17A C17D 109.4(7) . . ?
C17C C17A C17B 107.4(6) . . ?
C17D C17A C17B 106.9(7) . . ?
C17C C17A C17 112.6(6) . . ?
C17D C17A C17 112.5(6) . . ?
C17B C17A C17 107.6(6) . . ?
C17A C17B H17A 109.5 . . ?
C17A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C17A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C17A C17C H17D 109.5 . . ?
C17A C17C H17E 109.5 . . ?
H17D C17C H17E 109.5 . . ?
C17A C17C H17F 109.5 . . ?
H17D C17C H17F 109.5 . . ?
H17E C17C H17F 109.5 . . ?
C17A C17D H17G 109.5 . . ?
C17A C17D H17H 109.5 . . ?
H17G C17D H17H 109.5 . . ?
C17A C17D H17I 109.5 . . ?
H17G C17D H17I 109.5 . . ?
H17H C17D H17I 109.5 . . ?
C13 C18 C17 122.7(5) . . ?
C13 C18 H18 118.6 . . ?
C17 C18 H18 118.6 . . ?
N20 C19 C15 124.3(5) . . ?
N20 C19 H19 117.8 . . ?
C15 C19 H19 117.8 . . ?
C19 N20 N21 117.1(5) . . ?
C19 N20 Ho2 127.2(4) . . ?
N21 N20 Ho2 115.5(3) . . ?
C23 N21 N20 114.3(5) . . ?
C23 N21 C21A 122.6(5) . . ?
N20 N21 C21A 122.4(5) . . ?
N21 C21A H21A 109.5 . . ?
N21 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
N21 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23 N22 C30 102.5(5) . . ?
C23 N22 Ho2 116.8(3) . . ?
C30 N22 Ho2 133.7(4) . . ?
N22 C23 N21 124.7(5) . . ?
N22 C23 N24 113.6(5) . . ?
N21 C23 N24 121.7(6) . . ?
C23 N24 C25 107.3(5) . . ?
C23 N24 H24 126.3 . . ?
C25 N24 H24 126.3 . . ?
N24 C25 C26 130.7(6) . . ?
N24 C25 C30 105.2(5) . . ?
C26 C25 C30 124.1(6) . . ?
C27 C26 C25 116.3(6) . . ?
C27 C26 H26 121.8 . . ?
C25 C26 H26 121.8 . . ?
C26 C27 C28 121.2(6) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C27 C28 C29 122.3(6) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C30 C29 C28 116.5(6) . . ?
C30 C29 H29 121.8 . . ?
C28 C29 H29 121.8 . . ?
C29 C30 C25 119.5(5) . . ?
C29 C30 N22 129.1(6) . . ?
C25 C30 N22 111.4(5) . . ?
O3A N1A O2A 130.4(11) . . ?
O3A N1A O1A 113.0(10) . . ?
O2A N1A O1A 116.6(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N3 -3.6(6) . . . . ?
Ho1 N1 C2 N3 156.2(4) . . . . ?
C9 N1 C2 N10 178.6(5) . . . . ?
Ho1 N1 C2 N10 -21.6(7) . . . . ?
N1 C2 N3 C4 2.3(7) . . . . ?
N10 C2 N3 C4 -179.8(5) . . . . ?
C2 N3 C4 C5 179.3(6) . . . . ?
C2 N3 C4 C9 0.1(6) . . . . ?
N3 C4 C5 C6 -176.9(6) . . . . ?
C9 C4 C5 C6 2.3(10) . . . . ?
C4 C5 C6 C7 -0.6(11) . . . . ?
C5 C6 C7 C8 -0.4(12) . . . . ?
C6 C7 C8 C9 -0.3(11) . . . . ?
C7 C8 C9 C4 2.0(10) . . . . ?
C7 C8 C9 N1 -179.9(6) . . . . ?
N3 C4 C9 C8 176.3(6) . . . . ?
C5 C4 C9 C8 -3.1(10) . . . . ?
N3 C4 C9 N1 -2.2(7) . . . . ?
C5 C4 C9 N1 178.4(6) . . . . ?
C2 N1 C9 C8 -174.8(7) . . . . ?
Ho1 N1 C9 C8 30.0(10) . . . . ?
C2 N1 C9 C4 3.5(6) . . . . ?
Ho1 N1 C9 C4 -151.7(4) . . . . ?
N1 C2 N10 N11 3.0(8) . . . . ?
N3 C2 N10 N11 -174.7(5) . . . . ?
N1 C2 N10 C10A -169.6(6) . . . . ?
N3 C2 N10 C10A 12.7(9) . . . . ?
C2 N10 N11 C12 -162.2(5) . . . . ?
C10A N10 N11 C12 10.3(8) . . . . ?
C2 N10 N11 Ho1 15.4(6) . . . . ?
C10A N10 N11 Ho1 -172.0(5) . . . . ?
N10 N11 C12 C13 -175.8(5) . . . . ?
Ho1 N11 C12 C13 6.9(8) . . . . ?
N11 C12 C13 C18 -161.1(5) . . . . ?
N11 C12 C13 C14 23.3(8) . . . . ?
C18 C13 C14 O14 -178.0(5) . . . . ?
C12 C13 C14 O14 -2.4(8) . . . . ?
C18 C13 C14 C15 0.7(8) . . . . ?
C12 C13 C14 C15 176.3(5) . . . . ?
C15 C14 O14 Ho2 -56.3(6) . . . . ?
C13 C14 O14 Ho2 122.3(5) . . . . ?
C15 C14 O14 Ho1 122.6(5) . . . . ?
C13 C14 O14 Ho1 -58.7(6) . . . . ?
O14 C14 C15 C16 -179.3(5) . . . . ?
C13 C14 C15 C16 2.0(8) . . . . ?
O14 C14 C15 C19 -4.6(8) . . . . ?
C13 C14 C15 C19 176.7(5) . . . . ?
C14 C15 C16 C17 -3.1(9) . . . . ?
C19 C15 C16 C17 -178.0(5) . . . . ?
C15 C16 C17 C18 1.4(9) . . . . ?
C15 C16 C17 C17A 179.3(6) . . . . ?
C16 C17 C17A C17C 139.1(7) . . . . ?
C18 C17 C17A C17C -43.0(9) . . . . ?
C16 C17 C17A C17D 14.8(10) . . . . ?
C18 C17 C17A C17D -167.3(7) . . . . ?
C16 C17 C17A C17B -102.8(7) . . . . ?
C18 C17 C17A C17B 75.1(8) . . . . ?
C14 C13 C18 C17 -2.5(9) . . . . ?
C12 C13 C18 C17 -178.2(5) . . . . ?
C16 C17 C18 C13 1.4(9) . . . . ?
C17A C17 C18 C13 -176.6(6) . . . . ?
C16 C15 C19 N20 -162.6(5) . . . . ?
C14 C15 C19 N20 22.6(8) . . . . ?
C15 C19 N20 N21 -176.1(5) . . . . ?
C15 C19 N20 Ho2 8.4(8) . . . . ?
C19 N20 N21 C23 -165.5(5) . . . . ?
Ho2 N20 N21 C23 10.6(6) . . . . ?
C19 N20 N21 C21A 5.6(8) . . . . ?
Ho2 N20 N21 C21A -178.4(5) . . . . ?
C30 N22 C23 N21 178.4(5) . . . . ?
Ho2 N22 C23 N21 -26.8(7) . . . . ?
C30 N22 C23 N24 -0.6(6) . . . . ?
Ho2 N22 C23 N24 154.2(4) . . . . ?
N20 N21 C23 N22 9.9(8) . . . . ?
C21A N21 C23 N22 -161.1(6) . . . . ?
N20 N21 C23 N24 -171.1(5) . . . . ?
C21A N21 C23 N24 17.8(9) . . . . ?
N22 C23 N24 C25 -0.3(7) . . . . ?
N21 C23 N24 C25 -179.3(5) . . . . ?
C23 N24 C25 C26 -179.0(6) . . . . ?
C23 N24 C25 C30 1.1(6) . . . . ?
N24 C25 C26 C27 -177.7(6) . . . . ?
C30 C25 C26 C27 2.1(10) . . . . ?
C25 C26 C27 C28 -0.2(10) . . . . ?
C26 C27 C28 C29 -0.7(11) . . . . ?
C27 C28 C29 C30 -0.1(9) . . . . ?
C28 C29 C30 C25 1.9(8) . . . . ?
C28 C29 C30 N22 179.9(5) . . . . ?
N24 C25 C30 C29 176.8(5) . . . . ?
C26 C25 C30 C29 -3.1(9) . . . . ?
N24 C25 C30 N22 -1.5(6) . . . . ?
C26 C25 C30 N22 178.6(5) . . . . ?
C23 N22 C30 C29 -176.8(6) . . . . ?
Ho2 N22 C30 C29 34.8(9) . . . . ?
C23 N22 C30 C25 1.3(6) . . . . ?
Ho2 N22 C30 C25 -147.0(4) . . . . ?

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
N3 H3 O3A 0.86 2.02 2.834(8) 157.7 3_565
C10A H10A O3A 0.96 2.23 3.071(9) 145.7 3_565
C21A H21A O1A 0.96 2.54 3.338(10) 141.0 29
N24 H24 O2A 0.86 1.92 2.757(7) 164.8 29

_refine_diff_density_max         0.870
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.077



####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1038105'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-19 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         'C84 H87 N24 O3 Tm2, 3(N O3)'
_chemical_formula_sum            'C84 H87 N27 O12 Tm2'
_chemical_formula_weight         2004.66

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'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   26.1210(5)
_cell_length_b                   26.1210(5)
_cell_length_c                   47.7029(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     28187.4(13)
_cell_formula_units_Z            12
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    14499
_cell_measurement_theta_min      3.1890
_cell_measurement_theta_max      28.2040

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             12168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.947
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.90730
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       ω-scan
_diffrn_reflns_number            32539
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         2.931
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_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             5515
_reflns_number_gt                3653
_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       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0964P)²+3.9341P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5515
_refine_ls_number_parameters     381
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1583
_refine_ls_wR_factor_gt          0.1370
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.130
_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
Tm1 Tm 0.3333 0.6667 0.07417(2) 0.02834(17) Uani 1 3 d S T P . .
Tm2 Tm 0.3333 0.6667 0.00095(2) 0.02733(16) Uani 1 3 d S T P . .
N1 N 0.2460(2) 0.60996(18) 0.10383(10) 0.0404(11) Uani 1 1 d . . . . .
C2 C 0.1973(2) 0.6110(2) 0.09779(12) 0.0363(13) Uani 1 1 d . . . . .
N3 N 0.1476(2) 0.56370(19) 0.10736(11) 0.0437(12) Uani 1 1 d . . . . .
H3 H 0.1120 0.5566 0.1050 0.052 Uiso 1 1 calc R U . . .
C4 C 0.1647(2) 0.5289(2) 0.12158(12) 0.0446(14) Uani 1 1 d . . . . .
C5 C 0.1320(3) 0.4756(3) 0.13594(13) 0.0598(17) Uani 1 1 d . . . . .
H5 H 0.0909 0.4563 0.1364 0.072 Uiso 1 1 calc R U . . .
C6 C 0.1624(3) 0.4529(3) 0.14934(15) 0.071(2) Uani 1 1 d . . . . .
H6 H 0.1419 0.4172 0.1589 0.085 Uiso 1 1 calc R U . . .
C7 C 0.2246(4) 0.4832(3) 0.14874(15) 0.070(2) Uani 1 1 d . . . . .
H7 H 0.2445 0.4673 0.1583 0.083 Uiso 1 1 calc R U . . .
C8 C 0.2572(3) 0.5360(3) 0.13447(13) 0.0521(17) Uani 1 1 d . . . . .
H8 H 0.2983 0.5558 0.1344 0.063 Uiso 1 1 calc R U . . .
C9 C 0.2257(2) 0.5584(2) 0.12003(12) 0.0390(13) Uani 1 1 d . . . . .
N10 N 0.19575(18) 0.65450(18) 0.08281(10) 0.0424(11) Uani 1 1 d . . . . .
C10A C 0.1445(2) 0.6613(3) 0.08177(17) 0.079(2) Uani 1 1 d . . . . .
H10A H 0.1094 0.6232 0.0828 0.119 Uiso 1 1 calc R U . . .
H10B H 0.1444 0.6802 0.0645 0.119 Uiso 1 1 calc R U . . .
H10C H 0.1453 0.6852 0.0973 0.119 Uiso 1 1 calc R U . . .
N11 N 0.25071(17) 0.69709(18) 0.07236(9) 0.0352(10) Uani 1 1 d . . . . .
C12 C 0.2552(2) 0.7458(2) 0.06426(13) 0.0386(14) Uani 1 1 d . . . . .
H12 H 0.2229 0.7511 0.0668 0.046 Uiso 1 1 calc R U . . .
C13 C 0.3077(2) 0.7935(2) 0.05128(11) 0.0335(12) Uani 1 1 d . . . . .
C14 C 0.3493(2) 0.7818(2) 0.03764(11) 0.0311(11) Uani 1 1 d . . . . .
O14 O 0.34178(14) 0.72754(14) 0.03738(7) 0.0341(8) Uani 1 1 d . . . . .
C15 C 0.3980(2) 0.8283(2) 0.02401(12) 0.0344(12) Uani 1 1 d . . . . .
C16 C 0.4050(2) 0.8847(2) 0.02465(11) 0.0398(13) Uani 1 1 d . . . . .
H16 H 0.4383 0.9154 0.0162 0.048 Uiso 1 1 calc R U . . .
C17 C 0.3649(2) 0.8972(2) 0.03719(13) 0.0449(14) Uani 1 1 d . U . . .
C17A C 0.3735(3) 0.9598(2) 0.03763(15) 0.0636(16) Uani 1 1 d . U . . .
C17B C 0.4008(3) 0.9871(3) 0.06654(18) 0.098(2) Uani 1 1 d . U . . .
H17A H 0.4042 1.0254 0.0682 0.147 Uiso 1 1 calc R U . . .
H17B H 0.4392 0.9910 0.0681 0.147 Uiso 1 1 calc R U . . .
H17C H 0.3757 0.9619 0.0812 0.147 Uiso 1 1 calc R U . . .
C17C C 0.3177(3) 0.9602(3) 0.03441(19) 0.098(2) Uani 1 1 d . U . . .
H17D H 0.3255 1.0002 0.0347 0.148 Uiso 1 1 calc R U . . .
H17E H 0.2914 0.9384 0.0495 0.148 Uiso 1 1 calc R U . . .
H17F H 0.2996 0.9421 0.0169 0.148 Uiso 1 1 calc R U . . .
C17D C 0.4193(4) 1.0001(3) 0.0165(2) 0.128(3) Uani 1 1 d . U . . .
H17G H 0.4066 0.9845 -0.0020 0.192 Uiso 1 1 calc R U . . .
H17H H 0.4564 1.0024 0.0205 0.192 Uiso 1 1 calc R U . . .
H17I H 0.4239 1.0388 0.0176 0.192 Uiso 1 1 calc R U . . .
C18 C 0.3161(2) 0.8501(2) 0.05020(12) 0.0415(13) Uani 1 1 d . . . . .
H18 H 0.2880 0.8571 0.0585 0.050 Uiso 1 1 calc R U . . .
C19 C 0.4438(2) 0.8204(2) 0.01131(11) 0.0384(13) Uani 1 1 d . . . . .
H19 H 0.4811 0.8535 0.0090 0.046 Uiso 1 1 calc R U . . .
N20 N 0.43577(16) 0.76947(17) 0.00286(9) 0.0343(10) Uani 1 1 d . . . . .
N21 N 0.48460(17) 0.76793(19) -0.00703(10) 0.0434(12) Uani 1 1 d . . . . .
C21A C 0.5440(2) 0.8183(2) -0.00597(17) 0.074(2) Uani 1 1 d . . . . .
H21A H 0.5720 0.8052 -0.0089 0.111 Uiso 1 1 calc R U . . .
H21B H 0.5507 0.8370 0.0120 0.111 Uiso 1 1 calc R U . . .
H21C H 0.5486 0.8459 -0.0204 0.111 Uiso 1 1 calc R U . . .
N22 N 0.41656(18) 0.67616(18) -0.02839(9) 0.0406(11) Uani 1 1 d . . . . .
C23 C 0.4714(2) 0.7183(2) -0.02123(12) 0.0384(13) Uani 1 1 d . . . . .
N24 N 0.51386(18) 0.70704(18) -0.02983(10) 0.0448(12) Uani 1 1 d . . . . .
H24 H 0.5513 0.7290 -0.0272 0.054 Uiso 1 1 calc R U . . .
C25 C 0.4859(2) 0.6534(2) -0.04376(12) 0.0460(14) Uani 1 1 d . . . . .
C26 C 0.5090(3) 0.6210(3) -0.05664(14) 0.0574(17) Uani 1 1 d . . . . .
H26 H 0.5493 0.6339 -0.0567 0.069 Uiso 1 1 calc R U . . .
C27 C 0.4680(3) 0.5684(3) -0.06938(14) 0.0632(18) Uani 1 1 d . . . . .
H27 H 0.4807 0.5446 -0.0778 0.076 Uiso 1 1 calc R U . . .
C28 C 0.4088(3) 0.5511(3) -0.06976(14) 0.0619(18) Uani 1 1 d . . . . .
H28 H 0.3828 0.5161 -0.0789 0.074 Uiso 1 1 calc R U . . .
C29 C 0.3860(3) 0.5834(3) -0.05711(13) 0.0533(16) Uani 1 1 d . . . . .
H29 H 0.3458 0.5708 -0.0577 0.064 Uiso 1 1 calc R U . . .
C30 C 0.4260(2) 0.6355(2) -0.04344(12) 0.0410(13) Uani 1 1 d . . . . .
N1A N 0.4699(4) 0.4740(4) 0.12867(15) 0.081(2) Uani 1 1 d . . . . .
O1A O 0.5115(5) 0.5200(4) 0.1364(2) 0.181(4) Uani 1 1 d . . . . .
O2A O 0.4611(3) 0.4298(3) 0.14039(16) 0.129(3) Uani 1 1 d . . . . .
O3A O 0.4438(4) 0.4787(3) 0.10970(16) 0.146(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O14 2.304(3) . ?
Tm1 O14 2.304(3) 2_665 ?
Tm1 O14 2.304(3) 3_565 ?
Tm1 N1 2.454(4) . ?
Tm1 N1 2.454(4) 3_565 ?
Tm1 N1 2.454(4) 2_665 ?
Tm1 N11 2.648(4) . ?
Tm1 N11 2.648(4) 3_565 ?
Tm1 N11 2.648(4) 2_665 ?
Tm1 Tm2 3.4927(5) . ?
Tm2 O14 2.290(3) 2_665 ?
Tm2 O14 2.290(3) 3_565 ?
Tm2 O14 2.290(3) . ?
Tm2 N22 2.491(4) 2_665 ?
Tm2 N22 2.491(4) . ?
Tm2 N22 2.491(4) 3_565 ?
Tm2 N20 2.682(4) 2_665 ?
Tm2 N20 2.682(4) 3_565 ?
Tm2 N20 2.682(4) . ?
N1 C2 1.319(7) . ?
N1 C9 1.407(6) . ?
C2 N3 1.348(7) . ?
C2 N10 1.359(7) . ?
N3 C4 1.378(7) . ?
N3 H3 0.8600 . ?
C4 C5 1.395(7) . ?
C4 C9 1.381(7) . ?
C5 C6 1.364(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.408(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.383(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.407(8) . ?
C8 H8 0.9300 . ?
N10 N11 1.396(5) . ?
N10 C10A 1.438(6) . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9600 . ?
C10A H10C 0.9600 . ?
N11 C12 1.278(7) . ?
C12 C13 1.452(7) . ?
C12 H12 0.9300 . ?
C13 C18 1.383(6) . ?
C13 C14 1.425(7) . ?
C14 O14 1.330(5) . ?
C14 C15 1.403(7) . ?
C15 C16 1.392(7) . ?
C15 C19 1.445(7) . ?
C16 C17 1.381(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.398(7) . ?
C17 C17A 1.535(7) . ?
C17A C17C 1.473(9) . ?
C17A C17D 1.515(10) . ?
C17A C17B 1.552(9) . ?
C17B H17A 0.9600 . ?
C17B H17B 0.9600 . ?
C17B H17C 0.9600 . ?
C17C H17D 0.9600 . ?
C17C H17E 0.9600 . ?
C17C H17F 0.9600 . ?
C17D H17G 0.9600 . ?
C17D H17H 0.9600 . ?
C17D H17I 0.9600 . ?
C18 H18 0.9300 . ?
C19 N20 1.302(6) . ?
C19 H19 0.9300 . ?
N20 N21 1.379(5) . ?
N21 C23 1.345(7) . ?
N21 C21A 1.448(6) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
N22 C23 1.343(7) . ?
N22 C30 1.403(6) . ?
C23 N24 1.348(6) . ?
N24 C25 1.384(6) . ?
N24 H24 0.8600 . ?
C25 C30 1.389(7) . ?
C25 C26 1.404(7) . ?
C26 C27 1.390(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.378(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.390(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.397(8) . ?
C29 H29 0.9300 . ?
N1A O3A 1.175(8) . ?
N1A O2A 1.199(8) . ?
N1A O1A 1.206(12) . ?

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
O14 Tm1 O14 68.25(12) . 2_665 ?
O14 Tm1 O14 68.25(12) . 3_565 ?
O14 Tm1 O14 68.25(12) 2_665 3_565 ?
O14 Tm1 N1 126.53(13) . . ?
O14 Tm1 N1 85.60(13) 2_665 . ?
O14 Tm1 N1 143.06(12) 3_565 . ?
O14 Tm1 N1 85.60(13) . 3_565 ?
O14 Tm1 N1 143.06(12) 2_665 3_565 ?
O14 Tm1 N1 126.53(13) 3_565 3_565 ?
N1 Tm1 N1 90.07(16) . 3_565 ?
O14 Tm1 N1 143.06(12) . 2_665 ?
O14 Tm1 N1 126.53(13) 2_665 2_665 ?
O14 Tm1 N1 85.61(13) 3_565 2_665 ?
N1 Tm1 N1 90.07(16) . 2_665 ?
N1 Tm1 N1 90.07(16) 3_565 2_665 ?
O14 Tm1 N11 65.11(12) . . ?
O14 Tm1 N11 74.32(12) 2_665 . ?
O14 Tm1 N11 128.08(12) 3_565 . ?
N1 Tm1 N11 63.17(14) . . ?
N1 Tm1 N11 71.07(13) 3_565 . ?
N1 Tm1 N11 146.31(15) 2_665 . ?
O14 Tm1 N11 74.32(12) . 3_565 ?
O14 Tm1 N11 128.08(12) 2_665 3_565 ?
O14 Tm1 N11 65.11(12) 3_565 3_565 ?
N1 Tm1 N11 146.31(15) . 3_565 ?
N1 Tm1 N11 63.17(14) 3_565 3_565 ?
N1 Tm1 N11 71.07(13) 2_665 3_565 ?
N11 Tm1 N11 119.896(11) . 3_565 ?
O14 Tm1 N11 128.08(12) . 2_665 ?
O14 Tm1 N11 65.11(12) 2_665 2_665 ?
O14 Tm1 N11 74.32(12) 3_565 2_665 ?
N1 Tm1 N11 71.07(13) . 2_665 ?
N1 Tm1 N11 146.31(15) 3_565 2_665 ?
N1 Tm1 N11 63.17(14) 2_665 2_665 ?
N11 Tm1 N11 119.894(11) . 2_665 ?
N11 Tm1 N11 119.895(11) 3_565 2_665 ?
O14 Tm1 Tm2 40.37(8) . . ?
O14 Tm1 Tm2 40.37(8) 2_665 . ?
O14 Tm1 Tm2 40.37(8) 3_565 . ?
N1 Tm1 Tm2 125.21(11) . . ?
N1 Tm1 Tm2 125.21(11) 3_565 . ?
N1 Tm1 Tm2 125.21(11) 2_665 . ?
N11 Tm1 Tm2 88.14(9) . . ?
N11 Tm1 Tm2 88.14(9) 3_565 . ?
N11 Tm1 Tm2 88.14(9) 2_665 . ?
O14 Tm2 O14 68.69(13) 2_665 3_565 ?
O14 Tm2 O14 68.69(13) 2_665 . ?
O14 Tm2 O14 68.69(13) 3_565 . ?
O14 Tm2 N22 125.50(13) 2_665 2_665 ?
O14 Tm2 N22 142.75(12) 3_565 2_665 ?
O14 Tm2 N22 84.36(13) . 2_665 ?
O14 Tm2 N22 142.75(12) 2_665 . ?
O14 Tm2 N22 84.36(13) 3_565 . ?
O14 Tm2 N22 125.50(13) . . ?
N22 Tm2 N22 91.53(14) 2_665 . ?
O14 Tm2 N22 84.36(13) 2_665 3_565 ?
O14 Tm2 N22 125.50(13) 3_565 3_565 ?
O14 Tm2 N22 142.76(12) . 3_565 ?
N22 Tm2 N22 91.53(14) 2_665 3_565 ?
N22 Tm2 N22 91.53(14) . 3_565 ?
O14 Tm2 N20 65.01(11) 2_665 2_665 ?
O14 Tm2 N20 128.29(12) 3_565 2_665 ?
O14 Tm2 N20 74.06(12) . 2_665 ?
N22 Tm2 N20 62.32(13) 2_665 2_665 ?
N22 Tm2 N20 147.32(14) . 2_665 ?
N22 Tm2 N20 71.35(12) 3_565 2_665 ?
O14 Tm2 N20 74.06(12) 2_665 3_565 ?
O14 Tm2 N20 65.01(11) 3_565 3_565 ?
O14 Tm2 N20 128.29(12) . 3_565 ?
N22 Tm2 N20 147.32(14) 2_665 3_565 ?
N22 Tm2 N20 71.35(12) . 3_565 ?
N22 Tm2 N20 62.31(13) 3_565 3_565 ?
N20 Tm2 N20 119.885(11) 2_665 3_565 ?
O14 Tm2 N20 128.29(12) 2_665 . ?
O14 Tm2 N20 74.06(12) 3_565 . ?
O14 Tm2 N20 65.01(11) . . ?
N22 Tm2 N20 71.35(12) 2_665 . ?
N22 Tm2 N20 62.32(13) . . ?
N22 Tm2 N20 147.32(14) 3_565 . ?
N20 Tm2 N20 119.884(11) 2_665 . ?
N20 Tm2 N20 119.886(11) 3_565 . ?
O14 Tm2 Tm1 40.65(8) 2_665 . ?
O14 Tm2 Tm1 40.65(8) 3_565 . ?
O14 Tm2 Tm1 40.65(8) . . ?
N22 Tm2 Tm1 124.18(10) 2_665 . ?
N22 Tm2 Tm1 124.18(10) . . ?
N22 Tm2 Tm1 124.17(10) 3_565 . ?
N20 Tm2 Tm1 88.05(9) 2_665 . ?
N20 Tm2 Tm1 88.05(9) 3_565 . ?
N20 Tm2 Tm1 88.05(9) . . ?
C2 N1 C9 103.6(4) . . ?
C2 N1 Tm1 118.5(4) . . ?
C9 N1 Tm1 133.3(3) . . ?
N1 C2 N3 113.8(5) . . ?
N1 C2 N10 124.4(5) . . ?
N3 C2 N10 121.8(5) . . ?
C2 N3 C4 106.9(5) . . ?
C2 N3 H3 126.6 . . ?
C4 N3 H3 126.6 . . ?
N3 C4 C5 131.4(5) . . ?
N3 C4 C9 105.7(4) . . ?
C5 C4 C9 122.9(5) . . ?
C6 C5 C4 117.7(6) . . ?
C6 C5 H5 121.2 . . ?
C4 C5 H5 121.2 . . ?
C5 C6 C7 120.3(6) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 122.3(6) . . ?
C8 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C7 C8 C9 117.2(6) . . ?
C7 C8 H8 121.4 . . ?
C9 C8 H8 121.4 . . ?
C4 C9 C8 119.6(5) . . ?
C4 C9 N1 110.0(5) . . ?
C8 C9 N1 130.4(5) . . ?
C2 N10 N11 113.9(4) . . ?
C2 N10 C10A 122.7(4) . . ?
N11 N10 C10A 122.6(4) . . ?
N10 C10A H10A 109.5 . . ?
N10 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
N10 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C12 N11 N10 116.6(4) . . ?
C12 N11 Tm1 128.7(3) . . ?
N10 N11 Tm1 114.6(3) . . ?
N11 C12 C13 124.1(5) . . ?
N11 C12 H12 117.9 . . ?
C13 C12 H12 117.9 . . ?
C18 C13 C14 118.9(4) . . ?
C18 C13 C12 120.7(5) . . ?
C14 C13 C12 120.3(4) . . ?
O14 C14 C15 120.3(4) . . ?
O14 C14 C13 120.7(4) . . ?
C15 C14 C13 119.0(4) . . ?
C14 O14 Tm2 131.2(3) . . ?
C14 O14 Tm1 129.8(3) . . ?
Tm2 O14 Tm1 98.98(12) . . ?
C16 C15 C14 119.2(5) . . ?
C16 C15 C19 118.7(5) . . ?
C14 C15 C19 121.9(4) . . ?
C17 C16 C15 123.2(5) . . ?
C17 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
C16 C17 C18 116.7(4) . . ?
C16 C17 C17A 122.2(5) . . ?
C18 C17 C17A 121.1(5) . . ?
C17C C17A C17D 111.5(6) . . ?
C17C C17A C17 112.7(5) . . ?
C17D C17A C17 112.1(5) . . ?
C17C C17A C17B 108.5(6) . . ?
C17D C17A C17B 104.5(6) . . ?
C17 C17A C17B 107.0(5) . . ?
C17A C17B H17A 109.5 . . ?
C17A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C17A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C17A C17C H17D 109.5 . . ?
C17A C17C H17E 109.5 . . ?
H17D C17C H17E 109.5 . . ?
C17A C17C H17F 109.5 . . ?
H17D C17C H17F 109.5 . . ?
H17E C17C H17F 109.5 . . ?
C17A C17D H17G 109.5 . . ?
C17A C17D H17H 109.5 . . ?
H17G C17D H17H 109.5 . . ?
C17A C17D H17I 109.5 . . ?
H17G C17D H17I 109.5 . . ?
H17H C17D H17I 109.5 . . ?
C13 C18 C17 123.0(5) . . ?
C13 C18 H18 118.5 . . ?
C17 C18 H18 118.5 . . ?
N20 C19 C15 123.6(4) . . ?
N20 C19 H19 118.2 . . ?
C15 C19 H19 118.2 . . ?
C19 N20 N21 117.1(4) . . ?
C19 N20 Tm2 127.1(3) . . ?
N21 N20 Tm2 115.7(3) . . ?
C23 N21 N20 113.8(4) . . ?
C23 N21 C21A 122.3(4) . . ?
N20 N21 C21A 123.2(4) . . ?
N21 C21A H21A 109.5 . . ?
N21 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
N21 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23 N22 C30 103.4(4) . . ?
C23 N22 Tm2 117.3(3) . . ?
C30 N22 Tm2 133.5(3) . . ?
N22 C23 N21 125.0(5) . . ?
N22 C23 N24 113.6(5) . . ?
N21 C23 N24 121.4(5) . . ?
C23 N24 C25 107.0(4) . . ?
C23 N24 H24 126.5 . . ?
C25 N24 H24 126.5 . . ?
N24 C25 C30 105.7(4) . . ?
N24 C25 C26 130.7(5) . . ?
C30 C25 C26 123.6(5) . . ?
C27 C26 C25 115.8(5) . . ?
C27 C26 H26 122.1 . . ?
C25 C26 H26 122.1 . . ?
C26 C27 C28 121.0(6) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C27 C28 C29 123.1(6) . . ?
C27 C28 H28 118.4 . . ?
C29 C28 H28 118.4 . . ?
C30 C29 C28 117.0(6) . . ?
C30 C29 H29 121.5 . . ?
C28 C29 H29 121.5 . . ?
C25 C30 C29 119.4(5) . . ?
C25 C30 N22 110.2(5) . . ?
C29 C30 N22 130.3(5) . . ?
O3A N1A O2A 128.2(10) . . ?
O3A N1A O1A 114.3(9) . . ?
O2A N1A O1A 117.5(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N3 -3.1(6) . . . . ?
Tm1 N1 C2 N3 156.0(4) . . . . ?
C9 N1 C2 N10 178.3(5) . . . . ?
Tm1 N1 C2 N10 -22.6(7) . . . . ?
N1 C2 N3 C4 1.6(7) . . . . ?
N10 C2 N3 C4 -179.8(5) . . . . ?
C2 N3 C4 C5 178.9(6) . . . . ?
C2 N3 C4 C9 0.7(6) . . . . ?
N3 C4 C5 C6 -176.7(6) . . . . ?
C9 C4 C5 C6 1.2(10) . . . . ?
C4 C5 C6 C7 0.8(11) . . . . ?
C5 C6 C7 C8 -1.0(12) . . . . ?
C6 C7 C8 C9 -0.8(11) . . . . ?
N3 C4 C9 C8 175.3(5) . . . . ?
C5 C4 C9 C8 -3.0(9) . . . . ?
N3 C4 C9 N1 -2.6(6) . . . . ?
C5 C4 C9 N1 179.0(5) . . . . ?
C7 C8 C9 C4 2.7(9) . . . . ?
C7 C8 C9 N1 -179.8(6) . . . . ?
C2 N1 C9 C4 3.5(6) . . . . ?
Tm1 N1 C9 C4 -151.0(4) . . . . ?
C2 N1 C9 C8 -174.2(6) . . . . ?
Tm1 N1 C9 C8 31.3(9) . . . . ?
N1 C2 N10 N11 4.3(8) . . . . ?
N3 C2 N10 N11 -174.2(5) . . . . ?
N1 C2 N10 C10A -166.0(6) . . . . ?
N3 C2 N10 C10A 15.5(9) . . . . ?
C2 N10 N11 C12 -163.3(5) . . . . ?
C10A N10 N11 C12 6.9(8) . . . . ?
C2 N10 N11 Tm1 14.2(5) . . . . ?
C10A N10 N11 Tm1 -175.6(5) . . . . ?
N10 N11 C12 C13 -176.1(5) . . . . ?
Tm1 N11 C12 C13 6.8(8) . . . . ?
N11 C12 C13 C18 -161.8(6) . . . . ?
N11 C12 C13 C14 22.9(9) . . . . ?
C18 C13 C14 O14 -177.7(5) . . . . ?
C12 C13 C14 O14 -2.2(8) . . . . ?
C18 C13 C14 C15 1.2(8) . . . . ?
C12 C13 C14 C15 176.7(5) . . . . ?
C15 C14 O14 Tm2 -57.2(6) . . . . ?
C13 C14 O14 Tm2 121.7(5) . . . . ?
C15 C14 O14 Tm1 122.8(5) . . . . ?
C13 C14 O14 Tm1 -58.3(6) . . . . ?
O14 C14 C15 C16 -179.9(5) . . . . ?
C13 C14 C15 C16 1.2(8) . . . . ?
O14 C14 C15 C19 -5.1(8) . . . . ?
C13 C14 C15 C19 176.0(5) . . . . ?
C14 C15 C16 C17 -2.7(9) . . . . ?
C19 C15 C16 C17 -177.6(5) . . . . ?
C15 C16 C17 C18 1.4(9) . . . . ?
C15 C16 C17 C17A 180.0(6) . . . . ?
C16 C17 C17A C17C 142.9(7) . . . . ?
C18 C17 C17A C17C -38.6(9) . . . . ?
C16 C17 C17A C17D 16.1(10) . . . . ?
C18 C17 C17A C17D -165.4(7) . . . . ?
C16 C17 C17A C17B -97.9(7) . . . . ?
C18 C17 C17A C17B 80.6(7) . . . . ?
C14 C13 C18 C17 -2.5(8) . . . . ?
C12 C13 C18 C17 -177.9(5) . . . . ?
C16 C17 C18 C13 1.2(9) . . . . ?
C17A C17 C18 C13 -177.3(5) . . . . ?
C16 C15 C19 N20 -161.1(5) . . . . ?
C14 C15 C19 N20 24.1(9) . . . . ?
C15 C19 N20 N21 -175.4(5) . . . . ?
C15 C19 N20 Tm2 6.7(8) . . . . ?
C19 N20 N21 C23 -165.4(5) . . . . ?
Tm2 N20 N21 C23 12.8(6) . . . . ?
C19 N20 N21 C21A 5.9(8) . . . . ?
Tm2 N20 N21 C21A -176.0(5) . . . . ?
C30 N22 C23 N21 178.1(5) . . . . ?
Tm2 N22 C23 N21 -25.2(7) . . . . ?
C30 N22 C23 N24 -1.5(6) . . . . ?
Tm2 N22 C23 N24 155.2(4) . . . . ?
N20 N21 C23 N22 7.2(8) . . . . ?
C21A N21 C23 N22 -164.1(6) . . . . ?
N20 N21 C23 N24 -173.1(5) . . . . ?
C21A N21 C23 N24 15.5(9) . . . . ?
N22 C23 N24 C25 -0.1(6) . . . . ?
N21 C23 N24 C25 -179.7(5) . . . . ?
C23 N24 C25 C30 1.7(6) . . . . ?
C23 N24 C25 C26 -179.5(6) . . . . ?
N24 C25 C26 C27 -178.9(6) . . . . ?
C30 C25 C26 C27 -0.3(9) . . . . ?
C25 C26 C27 C28 1.9(10) . . . . ?
C26 C27 C28 C29 -1.7(11) . . . . ?
C27 C28 C29 C30 -0.2(11) . . . . ?
N24 C25 C30 C29 177.3(5) . . . . ?
C26 C25 C30 C29 -1.6(9) . . . . ?
N24 C25 C30 N22 -2.7(6) . . . . ?
C26 C25 C30 N22 178.4(5) . . . . ?
C28 C29 C30 C25 1.8(9) . . . . ?
C28 C29 C30 N22 -178.2(6) . . . . ?
C23 N22 C30 C25 2.6(6) . . . . ?
Tm2 N22 C30 C25 -148.5(4) . . . . ?
C23 N22 C30 C29 -177.4(6) . . . . ?
Tm2 N22 C30 C29 31.6(9) . . . . ?

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
N3 H3 O3A 0.86 2.02 2.853(8) 162.7 3_565
C10A H10A O3A 0.96 2.26 3.106(9) 147.2 3_565
C21A H21A O1A 0.96 2.55 3.286(9) 133.5 29
C21A H21A O2A 0.96 2.54 3.485(8) 168.1 29
N24 H24 O2A 0.86 1.91 2.755(7) 166.1 29

_refine_diff_density_max         1.638
_refine_diff_density_min         -1.713
_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_6
_database_code_depnum_ccdc_archive 'CCDC 1038106'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-19 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         'C84 H87 N24 O3 Yb2, 3(N O3)'
_chemical_formula_sum            'C84 H87 N27 O12 Yb2'
_chemical_formula_weight         2012.88

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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   25.9543(5)
_cell_length_b                   25.9543(5)
_cell_length_c                   48.9988(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     28584.8(13)
_cell_formula_units_Z            12
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    19815
_cell_measurement_theta_min      3.1800
_cell_measurement_theta_max      26.8400

_exptl_crystal_description       block
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             12192
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    2.021
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.67165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       ω-scan

_diffrn_reflns_number            60274
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         2.918
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_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             5595
_reflns_number_gt                3270
_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       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0190P)²+92.1995P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5595
_refine_ls_number_parameters     381
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0435
_refine_ls_wR_factor_ref         0.1113
_refine_ls_wR_factor_gt          0.1009
_refine_ls_goodness_of_fit_ref   1.432
_refine_ls_restrained_S_all      1.447
_refine_ls_shift/su_max          0.006
_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
Yb1 Yb 0.3333 0.6667 0.07105(2) 0.03489(15) Uani 1 3 d S T P . .
Yb2 Yb 0.3333 0.6667 0.00029(2) 0.03131(14) Uani 1 3 d S T P . .
N1 N 0.2475(2) 0.6111(2) 0.10049(10) 0.0469(14) Uani 1 1 d . . . . .
C2 C 0.1976(3) 0.6110(3) 0.09451(12) 0.0482(18) Uani 1 1 d . . . . .
N3 N 0.1477(2) 0.5650(2) 0.10529(11) 0.0548(16) Uani 1 1 d . . . . .
H3 H 0.1118 0.5582 0.1034 0.066 Uiso 1 1 calc R U . . .
C4 C 0.1658(3) 0.5311(3) 0.11995(14) 0.0541(19) Uani 1 1 d . . . . .
C5 C 0.1343(4) 0.4803(3) 0.13493(15) 0.073(2) Uani 1 1 d . . . . .
H5 H 0.0929 0.4606 0.1357 0.087 Uiso 1 1 calc R U . . .
C6 C 0.1660(5) 0.4598(4) 0.14872(17) 0.088(3) Uani 1 1 d . . . . .
H6 H 0.1461 0.4252 0.1591 0.106 Uiso 1 1 calc R U . . .
C7 C 0.2281(4) 0.4899(4) 0.14751(16) 0.081(3) Uani 1 1 d . . . . .
H7 H 0.2484 0.4753 0.1575 0.097 Uiso 1 1 calc R U . . .
C8 C 0.2606(3) 0.5407(4) 0.13203(13) 0.065(2) Uani 1 1 d . . . . .
H8 H 0.3020 0.5602 0.1313 0.078 Uiso 1 1 calc R U . . .
C9 C 0.2278(3) 0.5612(3) 0.11759(13) 0.0517(18) Uani 1 1 d . . . . .
N10 N 0.1955(2) 0.6540(3) 0.07930(11) 0.0515(15) Uani 1 1 d . . . . .
C10A C 0.1417(3) 0.6580(4) 0.07672(18) 0.091(3) Uani 1 1 d . . . . .
H10A H 0.1074 0.6194 0.0794 0.137 Uiso 1 1 calc R U . . .
H10B H 0.1402 0.6723 0.0588 0.137 Uiso 1 1 calc R U . . .
H10C H 0.1420 0.6849 0.0902 0.137 Uiso 1 1 calc R U . . .
N11 N 0.2505(2) 0.6970(2) 0.06977(10) 0.0448(13) Uani 1 1 d . . . . .
C12 C 0.2549(3) 0.7457(3) 0.06181(12) 0.0468(16) Uani 1 1 d . . . . .
H12 H 0.2223 0.7510 0.0641 0.056 Uiso 1 1 calc R U . . .
C13 C 0.3083(3) 0.7937(3) 0.04921(12) 0.0442(16) Uani 1 1 d . . . . .
C14 C 0.3492(3) 0.7817(3) 0.03569(12) 0.0395(15) Uani 1 1 d . . . . .
O14 O 0.34093(17) 0.72715(18) 0.03549(7) 0.0393(10) Uani 1 1 d . . . . .
C15 C 0.3974(3) 0.8288(3) 0.02299(12) 0.0429(16) Uani 1 1 d . . . . .
C16 C 0.4059(3) 0.8861(3) 0.02404(13) 0.0474(17) Uani 1 1 d . . . . .
H16 H 0.4396 0.9172 0.0161 0.057 Uiso 1 1 calc R U . . .
C17 C 0.3657(3) 0.8979(3) 0.03654(14) 0.0532(18) Uani 1 1 d . U . . .
C17A C 0.3744(4) 0.9607(3) 0.03786(18) 0.077(2) Uani 1 1 d . U . . .
C17B C 0.3995(5) 0.9850(4) 0.0669(2) 0.117(3) Uani 1 1 d . U . . .
H17A H 0.3708 0.9606 0.0804 0.176 Uiso 1 1 calc R U . . .
H17B H 0.4074 1.0252 0.0685 0.176 Uiso 1 1 calc R U . . .
H17C H 0.4357 0.9842 0.0696 0.176 Uiso 1 1 calc R U . . .
C17C C 0.3162(4) 0.9603(4) 0.0350(2) 0.116(3) Uani 1 1 d . U . . .
H17D H 0.3234 1.0002 0.0362 0.174 Uiso 1 1 calc R U . . .
H17E H 0.2897 0.9368 0.0494 0.174 Uiso 1 1 calc R U . . .
H17F H 0.2986 0.9435 0.0177 0.174 Uiso 1 1 calc R U . . .
C17D C 0.4223(5) 1.0036(4) 0.0179(2) 0.147(4) Uani 1 1 d . U . . .
H17G H 0.4275 1.0427 0.0199 0.220 Uiso 1 1 calc R U . . .
H17H H 0.4101 0.9901 -0.0005 0.220 Uiso 1 1 calc R U . . .
H17I H 0.4592 1.0049 0.0216 0.220 Uiso 1 1 calc R U . . .
C18 C 0.3169(3) 0.8508(3) 0.04856(13) 0.0547(19) Uani 1 1 d . . . . .
H18 H 0.2884 0.8577 0.0566 0.066 Uiso 1 1 calc R U . . .
C19 C 0.4431(3) 0.8204(3) 0.01007(12) 0.0500(18) Uani 1 1 d . . . . .
H19 H 0.4802 0.8538 0.0072 0.060 Uiso 1 1 calc R U . . .
N20 N 0.4353(2) 0.7692(2) 0.00228(10) 0.0398(13) Uani 1 1 d . . . . .
N21 N 0.4846(2) 0.7681(2) -0.00778(11) 0.0492(15) Uani 1 1 d . . . . .
C21A C 0.5431(3) 0.8190(3) -0.00758(19) 0.092(3) Uani 1 1 d . . . . .
H21A H 0.5715 0.8072 -0.0125 0.139 Uiso 1 1 calc R U . . .
H21B H 0.5520 0.8362 0.0104 0.139 Uiso 1 1 calc R U . . .
H21C H 0.5450 0.8478 -0.0205 0.139 Uiso 1 1 calc R U . . .
N22 N 0.4161(2) 0.6761(2) -0.02851(10) 0.0405(13) Uani 1 1 d . . . . .
C23 C 0.4705(3) 0.7181(3) -0.02169(13) 0.0411(16) Uani 1 1 d . . . . .
N24 N 0.5130(2) 0.7067(2) -0.03042(10) 0.0494(14) Uani 1 1 d . . . . .
H24 H 0.5507 0.7288 -0.0279 0.059 Uiso 1 1 calc R U . . .
C25 C 0.4849(3) 0.6531(3) -0.04410(13) 0.0484(17) Uani 1 1 d . . . . .
C26 C 0.5077(3) 0.6209(3) -0.05644(14) 0.061(2) Uani 1 1 d . . . . .
H26 H 0.5481 0.6335 -0.0561 0.074 Uiso 1 1 calc R U . . .
C27 C 0.4676(4) 0.5695(4) -0.06910(15) 0.071(2) Uani 1 1 d . . . . .
H27 H 0.4808 0.5461 -0.0775 0.085 Uiso 1 1 calc R U . . .
C28 C 0.4076(4) 0.5513(4) -0.06967(15) 0.071(2) Uani 1 1 d . . . . .
H28 H 0.3815 0.5166 -0.0789 0.085 Uiso 1 1 calc R U . . .
C29 C 0.3855(3) 0.5840(3) -0.05676(13) 0.060(2) Uani 1 1 d . . . . .
H29 H 0.3451 0.5716 -0.0572 0.072 Uiso 1 1 calc R U . . .
C30 C 0.4250(3) 0.6352(3) -0.04339(13) 0.0457(17) Uani 1 1 d . . . . .
N1A N 0.4645(5) 0.4702(5) 0.1280(2) 0.103(3) Uani 1 1 d . . . . .
O1A O 0.5101(5) 0.5156(5) 0.1310(2) 0.187(5) Uani 1 1 d . . . . .
O2A O 0.4581(3) 0.4275(4) 0.13994(17) 0.134(3) Uani 1 1 d . . . . .
O3A O 0.4327(5) 0.4737(4) 0.11254(19) 0.188(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O14 2.287(4) . ?
Yb1 O14 2.287(4) 2_665 ?
Yb1 O14 2.287(4) 3_565 ?
Yb1 N1 2.432(5) . ?
Yb1 N1 2.432(5) 2_665 ?
Yb1 N1 2.432(5) 3_565 ?
Yb1 N11 2.635(5) 2_665 ?
Yb1 N11 2.635(5) 3_565 ?
Yb1 N11 2.635(5) . ?
Yb1 Yb2 3.4669(6) . ?
Yb2 O14 2.273(4) . ?
Yb2 O14 2.273(4) 2_665 ?
Yb2 O14 2.273(4) 3_565 ?
Yb2 N22 2.477(5) 2_665 ?
Yb2 N22 2.477(5) 3_565 ?
Yb2 N22 2.477(5) . ?
Yb2 N20 2.655(5) 2_665 ?
Yb2 N20 2.655(5) 3_565 ?
Yb2 N20 2.655(5) . ?
N1 C2 1.326(8) . ?
N1 C9 1.407(8) . ?
C2 N3 1.354(8) . ?
C2 N10 1.366(8) . ?
N3 C4 1.388(8) . ?
N3 H3 0.8600 . ?
C4 C5 1.366(9) . ?
C4 C9 1.398(9) . ?
C5 C6 1.364(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.397(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.383(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.401(9) . ?
C8 H8 0.9300 . ?
N10 N11 1.381(7) . ?
N10 C10A 1.458(8) . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9600 . ?
C10A H10C 0.9600 . ?
N11 C12 1.272(7) . ?
C12 C13 1.459(9) . ?
C12 H12 0.9300 . ?
C13 C18 1.384(8) . ?
C13 C14 1.411(8) . ?
C14 O14 1.323(7) . ?
C14 C15 1.385(8) . ?
C15 C16 1.391(8) . ?
C15 C19 1.453(8) . ?
C16 C17 1.369(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(9) . ?
C17 C17A 1.533(9) . ?
C17A C17C 1.510(11) . ?
C17A C17D 1.537(11) . ?
C17A C17B 1.558(11) . ?
C17B H17A 0.9600 . ?
C17B H17B 0.9600 . ?
C17B H17C 0.9600 . ?
C17C H17D 0.9600 . ?
C17C H17E 0.9600 . ?
C17C H17F 0.9600 . ?
C17D H17G 0.9600 . ?
C17D H17H 0.9600 . ?
C17D H17I 0.9600 . ?
C18 H18 0.9300 . ?
C19 N20 1.297(7) . ?
C19 H19 0.9300 . ?
N20 N21 1.386(6) . ?
N21 C23 1.345(7) . ?
N21 C21A 1.430(8) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
N22 C23 1.325(7) . ?
N22 C30 1.400(7) . ?
C23 N24 1.345(7) . ?
N24 C25 1.380(8) . ?
N24 H24 0.8600 . ?
C25 C30 1.383(9) . ?
C25 C26 1.381(9) . ?
C26 C27 1.364(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.383(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.391(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.372(9) . ?
C29 H29 0.9300 . ?
N1A O3A 1.157(10) . ?
N1A O2A 1.190(11) . ?
N1A O1A 1.190(12) . ?

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
O14 Yb1 O14 68.24(16) . 2_665 ?
O14 Yb1 O14 68.24(16) . 3_565 ?
O14 Yb1 O14 68.24(16) 2_665 3_565 ?
O14 Yb1 N1 126.71(16) . . ?
O14 Yb1 N1 86.87(16) 2_665 . ?
O14 Yb1 N1 144.35(15) 3_565 . ?
O14 Yb1 N1 144.35(15) . 2_665 ?
O14 Yb1 N1 126.71(16) 2_665 2_665 ?
O14 Yb1 N1 86.87(16) 3_565 2_665 ?
N1 Yb1 N1 88.41(18) . 2_665 ?
O14 Yb1 N1 86.87(16) . 3_565 ?
O14 Yb1 N1 144.35(15) 2_665 3_565 ?
O14 Yb1 N1 126.71(16) 3_565 3_565 ?
N1 Yb1 N1 88.41(18) . 3_565 ?
N1 Yb1 N1 88.41(18) 2_665 3_565 ?
O14 Yb1 N11 128.51(15) . 2_665 ?
O14 Yb1 N11 65.15(15) 2_665 2_665 ?
O14 Yb1 N11 75.15(15) 3_565 2_665 ?
N1 Yb1 N11 71.24(17) . 2_665 ?
N1 Yb1 N11 63.14(17) 2_665 2_665 ?
N1 Yb1 N11 144.62(17) 3_565 2_665 ?
O14 Yb1 N11 75.14(15) . 3_565 ?
O14 Yb1 N11 128.51(15) 2_665 3_565 ?
O14 Yb1 N11 65.15(15) 3_565 3_565 ?
N1 Yb1 N11 144.62(17) . 3_565 ?
N1 Yb1 N11 71.25(17) 2_665 3_565 ?
N1 Yb1 N11 63.14(17) 3_565 3_565 ?
N11 Yb1 N11 119.949(10) 2_665 3_565 ?
O14 Yb1 N11 65.15(15) . . ?
O14 Yb1 N11 75.14(15) 2_665 . ?
O14 Yb1 N11 128.51(15) 3_565 . ?
N1 Yb1 N11 63.14(17) . . ?
N1 Yb1 N11 144.62(17) 2_665 . ?
N1 Yb1 N11 71.24(17) 3_565 . ?
N11 Yb1 N11 119.943(9) 2_665 . ?
N11 Yb1 N11 119.942(9) 3_565 . ?
O14 Yb1 Yb2 40.37(10) . . ?
O14 Yb1 Yb2 40.37(10) 2_665 . ?
O14 Yb1 Yb2 40.37(10) 3_565 . ?
N1 Yb1 Yb2 126.38(12) . . ?
N1 Yb1 Yb2 126.38(12) 2_665 . ?
N1 Yb1 Yb2 126.38(12) 3_565 . ?
N11 Yb1 Yb2 88.65(11) 2_665 . ?
N11 Yb1 Yb2 88.65(11) 3_565 . ?
N11 Yb1 Yb2 88.65(11) . . ?
O14 Yb2 O14 68.70(16) . 2_665 ?
O14 Yb2 O14 68.69(16) . 3_565 ?
O14 Yb2 O14 68.69(16) 2_665 3_565 ?
O14 Yb2 N22 84.81(15) . 2_665 ?
O14 Yb2 N22 126.32(15) 2_665 2_665 ?
O14 Yb2 N22 142.62(15) 3_565 2_665 ?
O14 Yb2 N22 142.62(15) . 3_565 ?
O14 Yb2 N22 84.81(15) 2_665 3_565 ?
O14 Yb2 N22 126.31(15) 3_565 3_565 ?
N22 Yb2 N22 90.77(16) 2_665 3_565 ?
O14 Yb2 N22 126.32(15) . . ?
O14 Yb2 N22 142.62(15) 2_665 . ?
O14 Yb2 N22 84.81(15) 3_565 . ?
N22 Yb2 N22 90.76(16) 2_665 . ?
N22 Yb2 N22 90.76(16) 3_565 . ?
O14 Yb2 N20 73.54(14) . 2_665 ?
O14 Yb2 N20 65.24(14) 2_665 2_665 ?
O14 Yb2 N20 128.20(14) 3_565 2_665 ?
N22 Yb2 N20 62.72(15) 2_665 2_665 ?
N22 Yb2 N20 71.52(16) 3_565 2_665 ?
N22 Yb2 N20 146.96(15) . 2_665 ?
O14 Yb2 N20 128.20(14) . 3_565 ?
O14 Yb2 N20 73.54(14) 2_665 3_565 ?
O14 Yb2 N20 65.24(14) 3_565 3_565 ?
N22 Yb2 N20 146.96(15) 2_665 3_565 ?
N22 Yb2 N20 62.72(15) 3_565 3_565 ?
N22 Yb2 N20 71.52(16) . 3_565 ?
N20 Yb2 N20 119.865(13) 2_665 3_565 ?
O14 Yb2 N20 65.24(14) . . ?
O14 Yb2 N20 128.20(14) 2_665 . ?
O14 Yb2 N20 73.54(14) 3_565 . ?
N22 Yb2 N20 71.52(16) 2_665 . ?
N22 Yb2 N20 146.96(15) 3_565 . ?
N22 Yb2 N20 62.72(15) . . ?
N20 Yb2 N20 119.867(13) 2_665 . ?
N20 Yb2 N20 119.864(14) 3_565 . ?
O14 Yb2 Yb1 40.65(10) . . ?
O14 Yb2 Yb1 40.65(10) 2_665 . ?
O14 Yb2 Yb1 40.65(10) 3_565 . ?
N22 Yb2 Yb1 124.72(11) 2_665 . ?
N22 Yb2 Yb1 124.72(11) 3_565 . ?
N22 Yb2 Yb1 124.72(11) . . ?
N20 Yb2 Yb1 87.89(10) 2_665 . ?
N20 Yb2 Yb1 87.89(10) 3_565 . ?
N20 Yb2 Yb1 87.89(10) . . ?
C2 N1 C9 103.0(6) . . ?
C2 N1 Yb1 118.4(4) . . ?
C9 N1 Yb1 134.6(4) . . ?
N1 C2 N3 114.8(6) . . ?
N1 C2 N10 123.7(6) . . ?
N3 C2 N10 121.5(7) . . ?
C2 N3 C4 106.4(6) . . ?
C2 N3 H3 126.8 . . ?
C4 N3 H3 126.8 . . ?
C5 C4 N3 131.3(7) . . ?
C5 C4 C9 123.4(8) . . ?
N3 C4 C9 105.2(6) . . ?
C4 C5 C6 117.1(8) . . ?
C4 C5 H5 121.4 . . ?
C6 C5 H5 121.4 . . ?
C5 C6 C7 120.9(8) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 122.7(8) . . ?
C8 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C7 C8 C9 116.2(7) . . ?
C7 C8 H8 121.9 . . ?
C9 C8 H8 121.9 . . ?
C4 C9 C8 119.6(7) . . ?
C4 C9 N1 110.5(6) . . ?
C8 C9 N1 129.8(7) . . ?
C2 N10 N11 113.5(5) . . ?
C2 N10 C10A 122.4(6) . . ?
N11 N10 C10A 123.5(6) . . ?
N10 C10A H10A 109.5 . . ?
N10 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
N10 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C12 N11 N10 116.8(6) . . ?
C12 N11 Yb1 128.5(5) . . ?
N10 N11 Yb1 114.7(4) . . ?
N11 C12 C13 123.6(6) . . ?
N11 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C18 C13 C14 119.3(6) . . ?
C18 C13 C12 119.9(6) . . ?
C14 C13 C12 120.5(6) . . ?
O14 C14 C15 122.1(6) . . ?
O14 C14 C13 120.2(6) . . ?
C15 C14 C13 117.7(6) . . ?
C14 O14 Yb2 131.1(4) . . ?
C14 O14 Yb1 129.9(4) . . ?
Yb2 O14 Yb1 98.98(16) . . ?
C14 C15 C16 121.0(6) . . ?
C14 C15 C19 120.6(6) . . ?
C16 C15 C19 118.2(6) . . ?
C17 C16 C15 121.6(6) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 117.3(6) . . ?
C16 C17 C17A 122.2(7) . . ?
C18 C17 C17A 120.5(7) . . ?
C17C C17A C17 111.9(7) . . ?
C17C C17A C17D 113.0(8) . . ?
C17 C17A C17D 112.3(7) . . ?
C17C C17A C17B 107.5(7) . . ?
C17 C17A C17B 106.2(7) . . ?
C17D C17A C17B 105.4(8) . . ?
C17A C17B H17A 109.5 . . ?
C17A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C17A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C17A C17C H17D 109.5 . . ?
C17A C17C H17E 109.5 . . ?
H17D C17C H17E 109.5 . . ?
C17A C17C H17F 109.5 . . ?
H17D C17C H17F 109.5 . . ?
H17E C17C H17F 109.5 . . ?
C17A C17D H17G 109.5 . . ?
C17A C17D H17H 109.5 . . ?
H17G C17D H17H 109.5 . . ?
C17A C17D H17I 109.5 . . ?
H17G C17D H17I 109.5 . . ?
H17H C17D H17I 109.5 . . ?
C17 C18 C13 122.9(6) . . ?
C17 C18 H18 118.6 . . ?
C13 C18 H18 118.6 . . ?
N20 C19 C15 124.1(6) . . ?
N20 C19 H19 118.0 . . ?
C15 C19 H19 118.0 . . ?
C19 N20 N21 116.9(5) . . ?
C19 N20 Yb2 127.2(4) . . ?
N21 N20 Yb2 115.8(3) . . ?
C23 N21 N20 113.1(5) . . ?
C23 N21 C21A 123.1(5) . . ?
N20 N21 C21A 122.9(5) . . ?
N21 C21A H21A 109.5 . . ?
N21 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
N21 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23 N22 C30 104.0(5) . . ?
C23 N22 Yb2 116.9(4) . . ?
C30 N22 Yb2 133.3(4) . . ?
N22 C23 N24 113.2(6) . . ?
N22 C23 N21 125.8(6) . . ?
N24 C23 N21 121.0(6) . . ?
C23 N24 C25 107.4(6) . . ?
C23 N24 H24 126.3 . . ?
C25 N24 H24 126.3 . . ?
C30 C25 N24 105.3(6) . . ?
C30 C25 C26 123.9(7) . . ?
N24 C25 C26 130.9(7) . . ?
C27 C26 C25 116.3(7) . . ?
C27 C26 H26 121.9 . . ?
C25 C26 H26 121.9 . . ?
C26 C27 C28 121.4(7) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C27 C28 C29 121.3(8) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C30 C29 C28 118.1(7) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
C29 C30 C25 118.9(6) . . ?
C29 C30 N22 130.9(7) . . ?
C25 C30 N22 110.1(6) . . ?
O3A N1A O2A 128.5(13) . . ?
O3A N1A O1A 113.5(13) . . ?
O2A N1A O1A 117.9(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N3 -2.1(7) . . . . ?
Yb1 N1 C2 N3 158.6(4) . . . . ?
C9 N1 C2 N10 176.4(6) . . . . ?
Yb1 N1 C2 N10 -23.0(8) . . . . ?
N1 C2 N3 C4 0.1(8) . . . . ?
N10 C2 N3 C4 -178.4(6) . . . . ?
C2 N3 C4 C5 179.5(8) . . . . ?
C2 N3 C4 C9 1.9(7) . . . . ?
N3 C4 C5 C6 -175.4(7) . . . . ?
C9 C4 C5 C6 1.8(12) . . . . ?
C4 C5 C6 C7 0.3(13) . . . . ?
C5 C6 C7 C8 -1.6(14) . . . . ?
C6 C7 C8 C9 0.6(13) . . . . ?
C5 C4 C9 C8 -2.8(11) . . . . ?
N3 C4 C9 C8 175.0(6) . . . . ?
C5 C4 C9 N1 178.9(7) . . . . ?
N3 C4 C9 N1 -3.3(8) . . . . ?
C7 C8 C9 C4 1.5(11) . . . . ?
C7 C8 C9 N1 179.4(7) . . . . ?
C2 N1 C9 C4 3.3(7) . . . . ?
Yb1 N1 C9 C4 -152.5(5) . . . . ?
C2 N1 C9 C8 -174.8(7) . . . . ?
Yb1 N1 C9 C8 29.4(11) . . . . ?
N1 C2 N10 N11 2.2(9) . . . . ?
N3 C2 N10 N11 -179.4(6) . . . . ?
N1 C2 N10 C10A -169.8(7) . . . . ?
N3 C2 N10 C10A 8.5(10) . . . . ?
C2 N10 N11 C12 -162.1(6) . . . . ?
C10A N10 N11 C12 9.8(10) . . . . ?
C2 N10 N11 Yb1 17.3(6) . . . . ?
C10A N10 N11 Yb1 -170.7(6) . . . . ?
N10 N11 C12 C13 -174.9(5) . . . . ?
Yb1 N11 C12 C13 5.7(9) . . . . ?
N11 C12 C13 C18 -160.6(6) . . . . ?
N11 C12 C13 C14 24.6(10) . . . . ?
C18 C13 C14 O14 -178.3(6) . . . . ?
C12 C13 C14 O14 -3.4(9) . . . . ?
C18 C13 C14 C15 2.0(9) . . . . ?
C12 C13 C14 C15 176.8(6) . . . . ?
C15 C14 O14 Yb2 -56.4(8) . . . . ?
C13 C14 O14 Yb2 123.9(5) . . . . ?
C15 C14 O14 Yb1 121.1(5) . . . . ?
C13 C14 O14 Yb1 -58.6(7) . . . . ?
O14 C14 C15 C16 -178.5(6) . . . . ?
C13 C14 C15 C16 1.3(9) . . . . ?
O14 C14 C15 C19 -3.4(9) . . . . ?
C13 C14 C15 C19 176.3(6) . . . . ?
C14 C15 C16 C17 -3.0(10) . . . . ?
C19 C15 C16 C17 -178.1(6) . . . . ?
C15 C16 C17 C18 1.2(11) . . . . ?
C15 C16 C17 C17A 180.0(7) . . . . ?
C16 C17 C17A C17C 143.2(8) . . . . ?
C18 C17 C17A C17C -38.1(11) . . . . ?
C16 C17 C17A C17D 14.9(12) . . . . ?
C18 C17 C17A C17D -166.4(8) . . . . ?
C16 C17 C17A C17B -99.8(9) . . . . ?
C18 C17 C17A C17B 78.9(9) . . . . ?
C16 C17 C18 C13 2.2(11) . . . . ?
C17A C17 C18 C13 -176.6(7) . . . . ?
C14 C13 C18 C17 -3.9(11) . . . . ?
C12 C13 C18 C17 -178.7(6) . . . . ?
C14 C15 C19 N20 21.0(10) . . . . ?
C16 C15 C19 N20 -163.8(6) . . . . ?
C15 C19 N20 N21 -175.2(6) . . . . ?
C15 C19 N20 Yb2 9.3(9) . . . . ?
C19 N20 N21 C23 -163.9(6) . . . . ?
Yb2 N20 N21 C23 12.1(6) . . . . ?
C19 N20 N21 C21A 5.6(9) . . . . ?
Yb2 N20 N21 C21A -178.4(6) . . . . ?
C30 N22 C23 N24 -1.4(7) . . . . ?
Yb2 N22 C23 N24 155.5(4) . . . . ?
C30 N22 C23 N21 177.9(6) . . . . ?
Yb2 N22 C23 N21 -25.2(8) . . . . ?
N20 N21 C23 N22 7.8(9) . . . . ?
C21A N21 C23 N22 -161.7(7) . . . . ?
N20 N21 C23 N24 -173.0(5) . . . . ?
C21A N21 C23 N24 17.6(10) . . . . ?
N22 C23 N24 C25 -0.1(7) . . . . ?
N21 C23 N24 C25 -179.4(6) . . . . ?
C23 N24 C25 C30 1.5(7) . . . . ?
C23 N24 C25 C26 -178.5(7) . . . . ?
C30 C25 C26 C27 1.9(11) . . . . ?
N24 C25 C26 C27 -178.2(7) . . . . ?
C25 C26 C27 C28 0.6(11) . . . . ?
C26 C27 C28 C29 -1.6(13) . . . . ?
C27 C28 C29 C30 0.2(11) . . . . ?
C28 C29 C30 C25 2.2(10) . . . . ?
C28 C29 C30 N22 -179.0(7) . . . . ?
N24 C25 C30 C29 176.7(6) . . . . ?
C26 C25 C30 C29 -3.3(11) . . . . ?
N24 C25 C30 N22 -2.4(7) . . . . ?
C26 C25 C30 N22 177.6(6) . . . . ?
C23 N22 C30 C29 -176.6(7) . . . . ?
Yb2 N22 C30 C29 32.2(10) . . . . ?
C23 N22 C30 C25 2.3(7) . . . . ?
Yb2 N22 C30 C25 -148.9(5) . . . . ?

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
N3 H3 O3A 0.86 2.02 2.821(10) 155.1 3_565
C8 H8 N1 0.93 2.61 3.371(9) 139.5 2_665
C10A H10A O3A 0.96 2.26 3.049(11) 138.9 3_565
C21A H21A O1A 0.96 2.54 3.335(12) 140.1 29
C21A H21A O2A 0.96 2.60 3.554(11) 172.2 29
N24 H24 O2A 0.86 1.94 2.780(9) 164.7 29

_refine_diff_density_max         1.984
_refine_diff_density_min         -1.173
_refine_diff_density_rms         0.107



####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1038936'
_audit_update_record             
;
2015-07-22 deposited with the CCDC.
2015-08-19 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         'C84 H87 Er2 N24 O3, 3(N O3)'
_chemical_formula_sum            'C84 H87 Er2 N27 O12'
_chemical_formula_weight         2001.32

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

_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c :H'
_space_group_name_Hall           '-R 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   26.1100(7)
_cell_length_b                   26.1100(7)
_cell_length_c                   48.0953(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     28395.3(17)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    8313
_cell_measurement_theta_min      3.3110
_cell_measurement_theta_max      27.9890

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             12144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.832
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.86336
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.1544
_diffrn_measurement_method       ω-scan

_diffrn_reflns_number            17425
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_theta_min         2.924
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5547
_reflns_number_gt                4227
_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       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_cell_refinement       'CrysAlis Pro (Agilent Technologies (2011))'
_computing_data_reduction        'CrysAlis Pro (Agilent Technologies (2011))'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0976P)²+3.8970P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5547
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0392
_refine_ls_wR_factor_ref         0.1660
_refine_ls_wR_factor_gt          0.1521
_refine_ls_goodness_of_fit_ref   1.286
_refine_ls_restrained_S_all      1.286
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.006

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 0.3333 0.6667 0.07369(2) 0.01932(17) Uani 1 3 d S T P . .
Er2 Er 0.3333 0.6667 0.00071(2) 0.01606(17) Uani 1 3 d S T P . .
N1 N 0.24523(17) 0.61076(16) 0.10340(8) 0.0283(9) Uani 1 1 d . . . . .
C2 C 0.1967(2) 0.6125(2) 0.09721(10) 0.0304(11) Uani 1 1 d . . . . .
N3 N 0.14571(19) 0.56518(16) 0.10704(9) 0.0321(10) Uani 1 1 d . . . . .
H3 H 0.1094 0.5584 0.1046 0.039 Uiso 1 1 calc R U . . .
C4 C 0.1625(2) 0.53043(19) 0.12151(9) 0.0345(11) Uani 1 1 d . . . . .
C5 C 0.1292(2) 0.4775(2) 0.13627(10) 0.0435(12) Uani 1 1 d . . . . .
H5 H 0.0872 0.4581 0.1367 0.052 Uiso 1 1 calc R U . . .
C6 C 0.1594(3) 0.4551(2) 0.14995(11) 0.0532(15) Uani 1 1 d . . . . .
H6 H 0.1382 0.4192 0.1600 0.064 Uiso 1 1 calc R U . . .
C7 C 0.2231(3) 0.4851(2) 0.14933(11) 0.0461(13) Uani 1 1 d . . . . .
H7 H 0.2432 0.4689 0.1592 0.055 Uiso 1 1 calc R U . . .
C8 C 0.2553(2) 0.5369(2) 0.13458(11) 0.0388(12) Uani 1 1 d . . . . .
H8 H 0.2973 0.5568 0.1344 0.047 Uiso 1 1 calc R U . . .
C9 C 0.2246(2) 0.55975(19) 0.11988(10) 0.0325(10) Uani 1 1 d . . . . .
N10 N 0.19583(15) 0.65601(16) 0.08154(8) 0.0330(9) Uani 1 1 d . . . . .
C10A C 0.1435(2) 0.6609(3) 0.07821(16) 0.073(2) Uani 1 1 d . . . . .
H10A H 0.1083 0.6215 0.0793 0.110 Uiso 1 1 calc R U . . .
H10B H 0.1446 0.6787 0.0601 0.110 Uiso 1 1 calc R U . . .
H10C H 0.1420 0.6860 0.0930 0.110 Uiso 1 1 calc R U . . .
N11 N 0.25145(15) 0.69847(15) 0.07197(7) 0.0258(8) Uani 1 1 d . . . . .
C12 C 0.25687(19) 0.74842(19) 0.06414(12) 0.0295(12) Uani 1 1 d . . . . .
H12 H 0.2245 0.7548 0.0669 0.035 Uiso 1 1 calc R U . . .
C13 C 0.31065(18) 0.79535(18) 0.05122(9) 0.0244(9) Uani 1 1 d . . . . .
C14 C 0.35070(17) 0.78263(17) 0.03716(8) 0.0196(9) Uani 1 1 d . . . . .
O14 O 0.34201(12) 0.72792(11) 0.03709(5) 0.0218(6) Uani 1 1 d . . . . .
C15 C 0.3996(2) 0.82927(19) 0.02404(10) 0.0236(10) Uani 1 1 d . . . . .
C16 C 0.40883(18) 0.88632(18) 0.02526(9) 0.0284(10) Uani 1 1 d . . . . .
H16 H 0.4433 0.9174 0.0168 0.034 Uiso 1 1 calc R U . . .
C17 C 0.36974(18) 0.89992(18) 0.03826(9) 0.0285(10) Uani 1 1 d . . . . .
C17A C 0.3815(2) 0.96389(19) 0.04063(10) 0.0375(11) Uani 1 1 d . . . . .
C17B C 0.3995(2) 0.9847(2) 0.07068(11) 0.0468(13) Uani 1 1 d . . . . .
H17A H 0.4047 1.0244 0.0729 0.070 Uiso 1 1 calc R U . . .
H17B H 0.4367 0.9858 0.0750 0.070 Uiso 1 1 calc R U . . .
H17C H 0.3685 0.9573 0.0834 0.070 Uiso 1 1 calc R U . . .
C17C C 0.3250(2) 0.9652(2) 0.03375(13) 0.0554(15) Uani 1 1 d . . . . .
H17D H 0.3336 1.0063 0.0334 0.083 Uiso 1 1 calc R U . . .
H17E H 0.2950 0.9431 0.0479 0.083 Uiso 1 1 calc R U . . .
H17F H 0.3103 0.9471 0.0155 0.083 Uiso 1 1 calc R U . . .
C17D C 0.4320(3) 1.0063(2) 0.02146(13) 0.0567(15) Uani 1 1 d . . . . .
H17G H 0.4240 0.9907 0.0025 0.085 Uiso 1 1 calc R U . . .
H17H H 0.4693 1.0102 0.0280 0.085 Uiso 1 1 calc R U . . .
H17I H 0.4348 1.0452 0.0217 0.085 Uiso 1 1 calc R U . . .
C18 C 0.3202(2) 0.85286(19) 0.05099(10) 0.0318(10) Uani 1 1 d . . . . .
H18 H 0.2921 0.8605 0.0598 0.038 Uiso 1 1 calc R U . . .
C19 C 0.44491(18) 0.82011(18) 0.01105(9) 0.0271(10) Uani 1 1 d . . . . .
H19 H 0.4831 0.8536 0.0084 0.032 Uiso 1 1 calc R U . . .
N20 N 0.43610(14) 0.76859(14) 0.00288(7) 0.0237(8) Uani 1 1 d . . . . .
N21 N 0.48492(14) 0.76689(15) -0.00689(8) 0.0290(9) Uani 1 1 d . . . . .
C21A C 0.54439(19) 0.8181(2) -0.00653(15) 0.0609(18) Uani 1 1 d . . . . .
H21A H 0.5730 0.8057 -0.0116 0.091 Uiso 1 1 calc R U . . .
H21B H 0.5534 0.8353 0.0122 0.091 Uiso 1 1 calc R U . . .
H21C H 0.5468 0.8476 -0.0199 0.091 Uiso 1 1 calc R U . . .
N22 N 0.41665(14) 0.67505(14) -0.02849(7) 0.0229(8) Uani 1 1 d . . . . .
C23 C 0.47132(19) 0.7163(2) -0.02128(9) 0.0261(10) Uani 1 1 d . . . . .
N24 N 0.51407(15) 0.70504(14) -0.02978(8) 0.0292(8) Uani 1 1 d . . . . .
H24 H 0.5524 0.7271 -0.0269 0.035 Uiso 1 1 calc R U . . .
C25 C 0.48521(18) 0.65161(18) -0.04391(9) 0.0272(10) Uani 1 1 d . . . . .
C26 C 0.5086(2) 0.61931(19) -0.05644(9) 0.0330(11) Uani 1 1 d . . . . .
H26 H 0.5497 0.6321 -0.0559 0.040 Uiso 1 1 calc R U . . .
C27 C 0.4679(2) 0.5672(2) -0.06980(10) 0.0326(10) Uani 1 1 d . . . . .
H27 H 0.4813 0.5437 -0.0788 0.039 Uiso 1 1 calc R U . . .
C28 C 0.4076(2) 0.5492(2) -0.07014(9) 0.0343(11) Uani 1 1 d . . . . .
H28 H 0.3808 0.5136 -0.0794 0.041 Uiso 1 1 calc R U . . .
C29 C 0.3861(2) 0.5822(2) -0.05718(10) 0.0342(11) Uani 1 1 d . . . . .
H29 H 0.3450 0.5695 -0.0577 0.041 Uiso 1 1 calc R U . . .
C30 C 0.42548(18) 0.63420(18) -0.04336(9) 0.0254(10) Uani 1 1 d . . . . .
N1A N 0.4672(3) 0.4718(3) 0.12868(9) 0.0533(15) Uani 1 1 d . . . . .
O1A O 0.5127(2) 0.5176(3) 0.13358(15) 0.111(2) Uani 1 1 d . . . . .
O2A O 0.45442(17) 0.42378(18) 0.14109(9) 0.0625(11) Uani 1 1 d . . . . .
O3A O 0.4320(3) 0.4712(2) 0.11125(11) 0.110(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O14 2.312(3) 2_665 ?
Er1 O14 2.312(3) 3_565 ?
Er1 O14 2.312(3) . ?
Er1 N1 2.471(4) 3_565 ?
Er1 N1 2.471(4) . ?
Er1 N1 2.471(4) 2_665 ?
Er1 N11 2.654(3) . ?
Er1 N11 2.654(3) 3_565 ?
Er1 N11 2.654(3) 2_665 ?
Er1 Er2 3.5101(5) . ?
Er2 O14 2.304(3) . ?
Er2 O14 2.304(3) 2_665 ?
Er2 O14 2.304(3) 3_565 ?
Er2 N22 2.505(3) 2_665 ?
Er2 N22 2.505(3) 3_565 ?
Er2 N22 2.505(3) . ?
Er2 N20 2.674(3) 2_665 ?
Er2 N20 2.674(3) . ?
Er2 N20 2.674(3) 3_565 ?
N1 C2 1.322(6) . ?
N1 C9 1.405(6) . ?
C2 N10 1.374(6) . ?
C2 N3 1.371(6) . ?
N3 C4 1.378(6) . ?
N3 H3 0.8800 . ?
C4 C5 1.402(6) . ?
C4 C9 1.406(6) . ?
C5 C6 1.365(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.440(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.381(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.406(7) . ?
C8 H8 0.9500 . ?
N10 N11 1.393(5) . ?
N10 C10A 1.445(6) . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
N11 C12 1.295(6) . ?
C12 C13 1.462(6) . ?
C12 H12 0.9500 . ?
C13 C18 1.394(6) . ?
C13 C14 1.417(6) . ?
C14 O14 1.330(4) . ?
C14 C15 1.399(6) . ?
C15 C16 1.387(6) . ?
C15 C19 1.458(6) . ?
C16 C17 1.386(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.403(6) . ?
C17 C17A 1.544(6) . ?
C17A C17C 1.527(7) . ?
C17A C17D 1.535(6) . ?
C17A C17B 1.533(7) . ?
C17B H17A 0.9800 . ?
C17B H17B 0.9800 . ?
C17B H17C 0.9800 . ?
C17C H17D 0.9800 . ?
C17C H17E 0.9800 . ?
C17C H17F 0.9800 . ?
C17D H17G 0.9800 . ?
C17D H17H 0.9800 . ?
C17D H17I 0.9800 . ?
C18 H18 0.9500 . ?
C19 N20 1.307(5) . ?
C19 H19 0.9500 . ?
N20 N21 1.380(5) . ?
N21 C23 1.370(6) . ?
N21 C21A 1.457(5) . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
N22 C23 1.335(5) . ?
N22 C30 1.396(5) . ?
C23 N24 1.353(5) . ?
N24 C25 1.387(5) . ?
N24 H24 0.8800 . ?
C25 C30 1.389(6) . ?
C25 C26 1.401(6) . ?
C26 C27 1.395(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.400(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(6) . ?
C29 H29 0.9500 . ?
N1A O1A 1.215(9) . ?
N1A O3A 1.238(6) . ?
N1A O2A 1.274(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
O14 Er1 O14 68.32(10) 2_665 3_565 ?
O14 Er1 O14 68.32(10) 2_665 . ?
O14 Er1 O14 68.32(10) 3_565 . ?
O14 Er1 N1 143.64(11) 2_665 3_565 ?
O14 Er1 N1 126.09(11) 3_565 3_565 ?
O14 Er1 N1 85.77(11) . 3_565 ?
O14 Er1 N1 85.76(11) 2_665 . ?
O14 Er1 N1 143.64(11) 3_565 . ?
O14 Er1 N1 126.09(11) . . ?
N1 Er1 N1 89.92(13) 3_565 . ?
O14 Er1 N1 126.09(11) 2_665 2_665 ?
O14 Er1 N1 85.76(11) 3_565 2_665 ?
O14 Er1 N1 143.64(11) . 2_665 ?
N1 Er1 N1 89.92(13) 3_565 2_665 ?
N1 Er1 N1 89.92(13) . 2_665 ?
O14 Er1 N11 74.68(10) 2_665 . ?
O14 Er1 N11 128.15(10) 3_565 . ?
O14 Er1 N11 64.88(10) . . ?
N1 Er1 N11 71.28(11) 3_565 . ?
N1 Er1 N11 62.94(11) . . ?
N1 Er1 N11 146.08(12) 2_665 . ?
O14 Er1 N11 128.15(10) 2_665 3_565 ?
O14 Er1 N11 64.87(10) 3_565 3_565 ?
O14 Er1 N11 74.68(10) . 3_565 ?
N1 Er1 N11 62.95(11) 3_565 3_565 ?
N1 Er1 N11 146.08(12) . 3_565 ?
N1 Er1 N11 71.28(11) 2_665 3_565 ?
N11 Er1 N11 119.906(9) . 3_565 ?
O14 Er1 N11 64.88(10) 2_665 2_665 ?
O14 Er1 N11 74.68(10) 3_565 2_665 ?
O14 Er1 N11 128.14(10) . 2_665 ?
N1 Er1 N11 146.08(12) 3_565 2_665 ?
N1 Er1 N11 71.28(11) . 2_665 ?
N1 Er1 N11 62.94(11) 2_665 2_665 ?
N11 Er1 N11 119.905(9) . 2_665 ?
N11 Er1 N11 119.900(9) 3_565 2_665 ?
O14 Er1 Er2 40.42(6) 2_665 . ?
O14 Er1 Er2 40.42(6) 3_565 . ?
O14 Er1 Er2 40.41(6) . . ?
N1 Er1 Er2 125.32(9) 3_565 . ?
N1 Er1 Er2 125.32(9) . . ?
N1 Er1 Er2 125.32(9) 2_665 . ?
N11 Er1 Er2 88.22(8) . . ?
N11 Er1 Er2 88.21(8) 3_565 . ?
N11 Er1 Er2 88.21(8) 2_665 . ?
O14 Er2 O14 68.59(10) . 2_665 ?
O14 Er2 O14 68.59(10) . 3_565 ?
O14 Er2 O14 68.59(10) 2_665 3_565 ?
O14 Er2 N22 84.27(10) . 2_665 ?
O14 Er2 N22 125.83(10) 2_665 2_665 ?
O14 Er2 N22 142.32(10) 3_565 2_665 ?
O14 Er2 N22 142.33(10) . 3_565 ?
O14 Er2 N22 84.27(10) 2_665 3_565 ?
O14 Er2 N22 125.83(10) 3_565 3_565 ?
N22 Er2 N22 91.65(11) 2_665 3_565 ?
O14 Er2 N22 125.83(10) . . ?
O14 Er2 N22 142.32(10) 2_665 . ?
O14 Er2 N22 84.27(10) 3_565 . ?
N22 Er2 N22 91.64(11) 2_665 . ?
N22 Er2 N22 91.64(11) 3_565 . ?
O14 Er2 N20 73.59(10) . 2_665 ?
O14 Er2 N20 65.05(9) 2_665 2_665 ?
O14 Er2 N20 127.99(10) 3_565 2_665 ?
N22 Er2 N20 62.58(10) 2_665 2_665 ?
N22 Er2 N20 71.39(10) 3_565 2_665 ?
N22 Er2 N20 147.71(11) . 2_665 ?
O14 Er2 N20 65.05(9) . . ?
O14 Er2 N20 127.99(10) 2_665 . ?
O14 Er2 N20 73.59(10) 3_565 . ?
N22 Er2 N20 71.38(10) 2_665 . ?
N22 Er2 N20 147.71(11) 3_565 . ?
N22 Er2 N20 62.58(10) . . ?
N20 Er2 N20 119.847(10) 2_665 . ?
O14 Er2 N20 127.99(10) . 3_565 ?
O14 Er2 N20 73.59(10) 2_665 3_565 ?
O14 Er2 N20 65.05(9) 3_565 3_565 ?
N22 Er2 N20 147.71(11) 2_665 3_565 ?
N22 Er2 N20 62.58(10) 3_565 3_565 ?
N22 Er2 N20 71.38(10) . 3_565 ?
N20 Er2 N20 119.849(10) 2_665 3_565 ?
N20 Er2 N20 119.851(10) . 3_565 ?
O14 Er2 Er1 40.59(7) . . ?
O14 Er2 Er1 40.59(7) 2_665 . ?
O14 Er2 Er1 40.59(7) 3_565 . ?
N22 Er2 Er1 124.09(8) 2_665 . ?
N22 Er2 Er1 124.09(8) 3_565 . ?
N22 Er2 Er1 124.09(8) . . ?
N20 Er2 Er1 87.76(7) 2_665 . ?
N20 Er2 Er1 87.76(7) . . ?
N20 Er2 Er1 87.76(7) 3_565 . ?
C2 N1 C9 103.8(4) . . ?
C2 N1 Er1 118.3(3) . . ?
C9 N1 Er1 133.5(3) . . ?
N1 C2 N10 124.3(4) . . ?
N1 C2 N3 114.1(4) . . ?
N10 C2 N3 121.5(4) . . ?
C2 N3 C4 106.3(4) . . ?
C2 N3 H3 126.8 . . ?
C4 N3 H3 126.8 . . ?
N3 C4 C5 131.2(4) . . ?
N3 C4 C9 105.8(4) . . ?
C5 C4 C9 122.9(4) . . ?
C6 C5 C4 117.3(5) . . ?
C6 C5 H5 121.3 . . ?
C4 C5 H5 121.3 . . ?
C5 C6 C7 121.0(5) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 121.0(5) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 118.5(5) . . ?
C7 C8 H8 120.8 . . ?
C9 C8 H8 120.8 . . ?
C8 C9 C4 119.2(4) . . ?
C8 C9 N1 130.9(4) . . ?
C4 C9 N1 109.8(4) . . ?
C2 N10 N11 113.4(3) . . ?
C2 N10 C10A 122.9(4) . . ?
N11 N10 C10A 123.3(4) . . ?
N10 C10A H10A 109.5 . . ?
N10 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
N10 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C12 N11 N10 116.3(4) . . ?
C12 N11 Er1 128.6(3) . . ?
N10 N11 Er1 115.0(2) . . ?
N11 C12 C13 122.9(4) . . ?
N11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C18 C13 C14 119.5(4) . . ?
C18 C13 C12 119.1(4) . . ?
C14 C13 C12 121.2(4) . . ?
O14 C14 C15 121.6(4) . . ?
O14 C14 C13 120.2(4) . . ?
C15 C14 C13 118.1(4) . . ?
C14 O14 Er2 130.7(2) . . ?
C14 O14 Er1 130.2(2) . . ?
Er2 O14 Er1 99.00(10) . . ?
C16 C15 C14 120.5(4) . . ?
C16 C15 C19 118.4(4) . . ?
C14 C15 C19 120.9(4) . . ?
C15 C16 C17 122.7(4) . . ?
C15 C16 H16 118.6 . . ?
C17 C16 H16 118.6 . . ?
C16 C17 C18 116.6(4) . . ?
C16 C17 C17A 122.5(4) . . ?
C18 C17 C17A 120.8(4) . . ?
C17C C17A C17D 110.1(4) . . ?
C17C C17A C17B 108.9(4) . . ?
C17D C17A C17B 108.0(4) . . ?
C17C C17A C17 109.7(4) . . ?
C17D C17A C17 111.8(4) . . ?
C17B C17A C17 108.2(4) . . ?
C17A C17B H17A 109.5 . . ?
C17A C17B H17B 109.5 . . ?
H17A C17B H17B 109.5 . . ?
C17A C17B H17C 109.5 . . ?
H17A C17B H17C 109.5 . . ?
H17B C17B H17C 109.5 . . ?
C17A C17C H17D 109.5 . . ?
C17A C17C H17E 109.5 . . ?
H17D C17C H17E 109.5 . . ?
C17A C17C H17F 109.5 . . ?
H17D C17C H17F 109.5 . . ?
H17E C17C H17F 109.5 . . ?
C17A C17D H17G 109.5 . . ?
C17A C17D H17H 109.5 . . ?
H17G C17D H17H 109.5 . . ?
C17A C17D H17I 109.5 . . ?
H17G C17D H17I 109.5 . . ?
H17H C17D H17I 109.5 . . ?
C13 C18 C17 122.5(4) . . ?
C13 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
N20 C19 C15 123.9(4) . . ?
N20 C19 H19 118.0 . . ?
C15 C19 H19 118.0 . . ?
C19 N20 N21 116.5(3) . . ?
C19 N20 Er2 127.5(3) . . ?
N21 N20 Er2 116.0(2) . . ?
C23 N21 N20 113.8(3) . . ?
C23 N21 C21A 122.3(3) . . ?
N20 N21 C21A 123.0(3) . . ?
N21 C21A H21A 109.5 . . ?
N21 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
N21 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
C23 N22 C30 103.4(3) . . ?
C23 N22 Er2 117.1(3) . . ?
C30 N22 Er2 133.5(3) . . ?
N22 C23 N24 114.3(4) . . ?
N22 C23 N21 124.5(4) . . ?
N24 C23 N21 121.2(4) . . ?
C23 N24 C25 106.0(3) . . ?
C23 N24 H24 127.0 . . ?
C25 N24 H24 127.0 . . ?
C30 C25 N24 106.0(3) . . ?
C30 C25 C26 124.6(4) . . ?
N24 C25 C26 129.4(4) . . ?
C27 C26 C25 115.9(4) . . ?
C27 C26 H26 122.1 . . ?
C25 C26 H26 122.1 . . ?
C28 C27 C26 120.9(4) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C29 C28 C27 121.5(4) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C30 C29 C28 119.1(5) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C25 C30 C29 118.0(4) . . ?
C25 C30 N22 110.3(4) . . ?
C29 C30 N22 131.7(4) . . ?
O1A N1A O3A 119.9(6) . . ?
O1A N1A O2A 121.5(5) . . ?
O3A N1A O2A 118.6(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N1 C2 N10 178.9(4) . . . . ?
Er1 N1 C2 N10 -21.4(6) . . . . ?
C9 N1 C2 N3 -3.2(5) . . . . ?
Er1 N1 C2 N3 156.5(3) . . . . ?
N1 C2 N3 C4 1.7(6) . . . . ?
N10 C2 N3 C4 179.6(4) . . . . ?
C2 N3 C4 C5 178.7(5) . . . . ?
C2 N3 C4 C9 0.7(5) . . . . ?
N3 C4 C5 C6 -176.3(5) . . . . ?
C9 C4 C5 C6 1.4(7) . . . . ?
C4 C5 C6 C7 0.5(8) . . . . ?
C5 C6 C7 C8 -0.9(8) . . . . ?
C6 C7 C8 C9 -0.6(8) . . . . ?
C7 C8 C9 C4 2.4(7) . . . . ?
C7 C8 C9 N1 179.9(5) . . . . ?
N3 C4 C9 C8 175.3(4) . . . . ?
C5 C4 C9 C8 -2.9(7) . . . . ?
N3 C4 C9 N1 -2.7(5) . . . . ?
C5 C4 C9 N1 179.1(4) . . . . ?
C2 N1 C9 C8 -174.1(5) . . . . ?
Er1 N1 C9 C8 30.8(8) . . . . ?
C2 N1 C9 C4 3.6(5) . . . . ?
Er1 N1 C9 C4 -151.5(3) . . . . ?
N1 C2 N10 N11 1.4(6) . . . . ?
N3 C2 N10 N11 -176.3(4) . . . . ?
N1 C2 N10 C10A -171.6(5) . . . . ?
N3 C2 N10 C10A 10.8(8) . . . . ?
C2 N10 N11 C12 -161.0(4) . . . . ?
C10A N10 N11 C12 11.9(7) . . . . ?
C2 N10 N11 Er1 17.3(4) . . . . ?
C10A N10 N11 Er1 -169.8(4) . . . . ?
N10 N11 C12 C13 -174.2(4) . . . . ?
Er1 N11 C12 C13 7.8(7) . . . . ?
N11 C12 C13 C18 -161.0(5) . . . . ?
N11 C12 C13 C14 23.9(7) . . . . ?
C18 C13 C14 O14 -179.7(4) . . . . ?
C12 C13 C14 O14 -4.6(6) . . . . ?
C18 C13 C14 C15 1.6(6) . . . . ?
C12 C13 C14 C15 176.7(4) . . . . ?
C15 C14 O14 Er2 -57.1(5) . . . . ?
C13 C14 O14 Er2 124.3(3) . . . . ?
C15 C14 O14 Er1 121.3(4) . . . . ?
C13 C14 O14 Er1 -57.4(5) . . . . ?
O14 C14 C15 C16 -177.7(4) . . . . ?
C13 C14 C15 C16 1.0(6) . . . . ?
O14 C14 C15 C19 -3.5(7) . . . . ?
C13 C14 C15 C19 175.2(4) . . . . ?
C14 C15 C16 C17 -2.7(7) . . . . ?
C19 C15 C16 C17 -177.0(4) . . . . ?
C15 C16 C17 C18 1.5(6) . . . . ?
C15 C16 C17 C17A 177.4(4) . . . . ?
C16 C17 C17A C17C 135.8(5) . . . . ?
C18 C17 C17A C17C -48.5(6) . . . . ?
C16 C17 C17A C17D 13.4(6) . . . . ?
C18 C17 C17A C17D -170.9(4) . . . . ?
C16 C17 C17A C17B -105.5(5) . . . . ?
C18 C17 C17A C17B 70.2(5) . . . . ?
C14 C13 C18 C17 -2.8(7) . . . . ?
C12 C13 C18 C17 -178.0(4) . . . . ?
C16 C17 C18 C13 1.2(7) . . . . ?
C17A C17 C18 C13 -174.7(4) . . . . ?
C16 C15 C19 N20 -163.5(4) . . . . ?
C14 C15 C19 N20 22.1(7) . . . . ?
C15 C19 N20 N21 -174.8(4) . . . . ?
C15 C19 N20 Er2 8.2(6) . . . . ?
C19 N20 N21 C23 -164.9(4) . . . . ?
Er2 N20 N21 C23 12.4(5) . . . . ?
C19 N20 N21 C21A 4.3(6) . . . . ?
Er2 N20 N21 C21A -178.4(4) . . . . ?
C30 N22 C23 N24 -1.1(5) . . . . ?
Er2 N22 C23 N24 155.5(3) . . . . ?
C30 N22 C23 N21 177.9(4) . . . . ?
Er2 N22 C23 N21 -25.5(6) . . . . ?
N20 N21 C23 N22 7.8(7) . . . . ?
C21A N21 C23 N22 -161.5(5) . . . . ?
N20 N21 C23 N24 -173.2(4) . . . . ?
C21A N21 C23 N24 17.5(8) . . . . ?
N22 C23 N24 C25 0.1(5) . . . . ?
N21 C23 N24 C25 -178.9(4) . . . . ?
C23 N24 C25 C30 0.9(5) . . . . ?
C23 N24 C25 C26 -178.6(4) . . . . ?
C30 C25 C26 C27 2.0(7) . . . . ?
N24 C25 C26 C27 -178.5(4) . . . . ?
C25 C26 C27 C28 -0.5(7) . . . . ?
C26 C27 C28 C29 -0.2(7) . . . . ?
C27 C28 C29 C30 -0.5(7) . . . . ?
N24 C25 C30 C29 177.6(4) . . . . ?
C26 C25 C30 C29 -2.8(7) . . . . ?
N24 C25 C30 N22 -1.6(5) . . . . ?
C26 C25 C30 N22 178.0(4) . . . . ?
C28 C29 C30 C25 1.9(7) . . . . ?
C28 C29 C30 N22 -179.0(4) . . . . ?
C23 N22 C30 C25 1.6(5) . . . . ?
Er2 N22 C30 C25 -149.1(3) . . . . ?
C23 N22 C30 C29 -177.5(5) . . . . ?
Er2 N22 C30 C29 31.7(7) . . . . ?

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
N3 H3 O3A 0.88 2.00 2.825(6) 156.4 3_565
C10A H10A O3A 0.98 2.25 3.036(7) 136.7 3_565
C21A H21A O1A 0.98 2.46 3.247(6) 137.2 29
N24 H24 O2A 0.88 1.92 2.775(5) 164.2 29

_refine_diff_density_max         1.051
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.106



_exptl_crystal_preparation       'Magnetic properties'
