# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_at1285a
_database_code_depnum_ccdc_archive 'CCDC 1494777'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25.25 H22.75 Dy N4.25 O3.25'
_chemical_formula_sum            'C25.25 H22.75 Dy N4.25 O3.25'
_chemical_formula_weight         600.23

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   22.269(7)
_cell_length_b                   7.4606(18)
_cell_length_c                   26.014(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4322(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3625
_cell_measurement_theta_min      2
_cell_measurement_theta_max      31

_exptl_crystal_description       'needle '
_exptl_crystal_colour            ' colorless'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2368
_exptl_absorpt_coefficient_mu    3.497
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16502
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         30.72
_reflns_number_total             5823
_reflns_number_gt                3968
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0150P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5823
_refine_ls_number_parameters     301
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.0713
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy Dy 0.719257(10) 0.44767(3) 0.587186(8) 0.00787(6) Uani 1 1 d . . .
O2A O 0.66243(14) 0.5633(4) 0.64928(11) 0.0100(7) Uani 1 1 d . . .
C1A C 0.5576(2) 0.5080(6) 0.64028(18) 0.0094(11) Uani 1 1 d . . .
C2A C 0.6074(2) 0.5733(6) 0.66730(17) 0.0083(10) Uani 1 1 d . . .
C3A C 0.5989(2) 0.6481(6) 0.71668(17) 0.0109(10) Uani 1 1 d . . .
H3A H 0.6328 0.6917 0.7351 0.013 Uiso 1 1 calc R . .
C4A C 0.5440(2) 0.6591(6) 0.73844(18) 0.0145(11) Uani 1 1 d . . .
H4A H 0.5401 0.7096 0.7718 0.017 Uiso 1 1 calc R . .
C5A C 0.4354(2) 0.6098(6) 0.7364(2) 0.0169(12) Uani 1 1 d . . .
H5A H 0.4321 0.6612 0.7697 0.020 Uiso 1 1 calc R . .
C6A C 0.3851(2) 0.5486(7) 0.71204(19) 0.0192(12) Uani 1 1 d . . .
H6A H 0.3470 0.5561 0.7283 0.023 Uiso 1 1 calc R . .
C7A C 0.3903(2) 0.4751(6) 0.66301(19) 0.0150(11) Uani 1 1 d . . .
H7A H 0.3553 0.4331 0.6459 0.018 Uiso 1 1 calc R . .
C8A C 0.4448(2) 0.4624(7) 0.63900(18) 0.0153(11) Uani 1 1 d . . .
H8A H 0.4468 0.4126 0.6054 0.018 Uiso 1 1 calc R . .
C9A C 0.4984(2) 0.5216(6) 0.66291(18) 0.0093(10) Uani 1 1 d . . .
C10A C 0.4920(2) 0.5974(6) 0.71268(19) 0.0126(11) Uani 1 1 d . . .
C11A C 0.5637(2) 0.4287(6) 0.58987(18) 0.0093(9) Uani 1 1 d . . .
H11A H 0.5276 0.3864 0.5746 0.011 Uiso 1 1 calc R . .
N1A N 0.61140(17) 0.4083(4) 0.56333(14) 0.0052(8) Uani 1 1 d . . .
C12A C 0.6041(2) 0.3156(6) 0.51385(17) 0.0112(11) Uani 1 1 d . . .
H12A H 0.5618 0.3246 0.5025 0.013 Uiso 1 1 calc R . .
H12B H 0.6139 0.1870 0.5181 0.013 Uiso 1 1 calc R . .
C12B C 0.6443(2) 0.3960(6) 0.47356(17) 0.0103(11) Uani 1 1 d . . .
H12C H 0.6425 0.3234 0.4417 0.012 Uiso 1 1 calc R . .
H12D H 0.6308 0.5191 0.4653 0.012 Uiso 1 1 calc R . .
N1B N 0.70583(18) 0.4004(5) 0.49302(14) 0.0101(9) Uani 1 1 d . . .
C11B C 0.7476(2) 0.3695(6) 0.46074(18) 0.0106(10) Uani 1 1 d . . .
H11B H 0.7364 0.3460 0.4261 0.013 Uiso 1 1 calc R . .
O2B O 0.79389(14) 0.2543(4) 0.55725(12) 0.0100(7) Uani 1 1 d . . .
C1B C 0.8111(2) 0.3679(6) 0.47326(18) 0.0118(11) Uani 1 1 d . . .
C2B C 0.8317(2) 0.3118(6) 0.52162(17) 0.0088(10) Uiso 1 1 d . . .
C3B C 0.8938(2) 0.3101(6) 0.53140(18) 0.0110(11) Uani 1 1 d . . .
H3B H 0.9079 0.2748 0.5644 0.013 Uiso 1 1 calc R . .
C4B C 0.9339(2) 0.3574(6) 0.49496(18) 0.0120(11) Uani 1 1 d . . .
H4B H 0.9756 0.3513 0.5028 0.014 Uiso 1 1 calc R . .
C5B C 0.9579(2) 0.4738(6) 0.4082(2) 0.0171(11) Uani 1 1 d . . .
H5B H 0.9995 0.4719 0.4163 0.020 Uiso 1 1 calc R . .
C6B C 0.9404(3) 0.5317(7) 0.3614(2) 0.0206(13) Uani 1 1 d . . .
H6B H 0.9693 0.5693 0.3368 0.025 Uiso 1 1 calc R . .
C7B C 0.8790(3) 0.5357(7) 0.34982(19) 0.0206(12) Uani 1 1 d . . .
H7B H 0.8664 0.5751 0.3168 0.025 Uiso 1 1 calc R . .
C8B C 0.8365(3) 0.4840(6) 0.38508(18) 0.0170(12) Uani 1 1 d . . .
H8B H 0.7952 0.4904 0.3764 0.020 Uiso 1 1 calc R . .
C9B C 0.8538(2) 0.4213(6) 0.43429(17) 0.0109(11) Uani 1 1 d . . .
C10B C 0.9161(2) 0.4156(6) 0.44567(18) 0.0115(11) Uani 1 1 d . . .
N1 N 0.6924(4) 0.1353(15) 0.5975(4) 0.0073(11) Uiso 0.75 1 d P . 1
N2 N 0.6470(3) 0.0855(11) 0.6185(3) 0.0088(13) Uiso 0.75 1 d P A 1
N3 N 0.6021(2) 0.0395(7) 0.6376(2) 0.0154(12) Uani 0.75 1 d P A 1
O2 O 0.6972(10) 0.136(4) 0.6032(10) 0.0073(11) Uiso 0.25 1 d PD . 2
C2 C 0.6420(11) 0.091(4) 0.6275(11) 0.0088(13) Uiso 0.25 1 d PD B 2
H2A H 0.6337 0.1753 0.6555 0.013 Uiso 0.25 1 d PR B 2
H2B H 0.6443 -0.0311 0.6413 0.013 Uiso 0.25 1 d PR B 2
H2C H 0.6096 0.0973 0.6020 0.013 Uiso 0.25 1 d PR B 2
O1 O 0.76633(14) 0.3499(4) 0.66920(12) 0.0117(8) Uani 1 1 d . . .
H1 H 0.7925 0.2662 0.6653 0.034(18) Uiso 1 1 d R . .
C1 C 0.7337(2) 0.2912(6) 0.71337(19) 0.0192(13) Uani 1 1 d . . .
H1A H 0.7025 0.3790 0.7217 0.029 Uiso 1 1 calc R . .
H1B H 0.7613 0.2795 0.7426 0.029 Uiso 1 1 calc R . .
H1C H 0.7151 0.1749 0.7062 0.029 Uiso 1 1 calc R . .


_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
Dy O2A 2.226(3) . ?
Dy O2B 2.335(3) . ?
Dy O2 2.37(3) 8_765 ?
Dy N1 2.421(11) . ?
Dy N1 2.429(11) 8_765 ?
Dy O2B 2.434(3) 8_765 ?
Dy O2 2.41(3) . ?
Dy O1 2.487(3) . ?
Dy N1B 2.493(4) . ?
Dy N1A 2.498(4) . ?
O2A C2A 1.314(5) . ?
C1A C2A 1.400(6) . ?
C1A C11A 1.445(6) . ?
C1A C9A 1.448(6) . ?
C2A C3A 1.413(6) . ?
C3A C4A 1.351(7) . ?
C3A H3A 0.9500 . ?
C4A C10A 1.414(7) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.365(7) . ?
C5A C10A 1.408(7) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.393(7) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.369(6) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.415(6) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.420(6) . ?
C11A N1A 1.276(5) . ?
C11A H11A 0.9500 . ?
N1A C12A 1.470(5) . ?
C12A C12B 1.504(6) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C12B N1B 1.460(6) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
N1B C11B 1.274(6) . ?
C11B C1B 1.450(7) . ?
C11B H11B 0.9500 . ?
O2B C2B 1.324(5) . ?
O2B Dy 2.434(3) 8_755 ?
C1B C2B 1.403(6) . ?
C1B C9B 1.446(6) . ?
C2B C3B 1.408(7) . ?
C3B C4B 1.349(6) . ?
C3B H3B 0.9500 . ?
C4B C10B 1.411(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.349(7) . ?
C5B C10B 1.416(6) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.402(7) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.372(7) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.416(6) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.419(7) . ?
N1 N2 1.208(9) . ?
N1 Dy 2.429(11) 8_755 ?
N2 N3 1.168(9) . ?
N2 H2A 1.2087 . ?
N2 H2B 1.0546 . ?
N2 H2C 0.9414 . ?
N3 H2B 1.0824 . ?
N3 H2C 1.0346 . ?
O2 C2 1.423(19) . ?
O2 Dy 2.37(3) 8_755 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O1 C1 1.428(5) . ?
O1 H1 0.8599 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Dy O2B 152.41(11) . . ?
O2A Dy O2 95.1(6) . 8_765 ?
O2B Dy O2 82.3(6) . 8_765 ?
O2A Dy N1 98.7(3) . . ?
O2B Dy N1 67.5(3) . . ?
O2 Dy N1 138.2(6) 8_765 . ?
O2A Dy N1 99.0(3) . 8_765 ?
O2B Dy N1 79.4(3) . 8_765 ?
O2 Dy N1 4.1(8) 8_765 8_765 ?
N1 Dy N1 137.9(3) . 8_765 ?
O2A Dy O2B 78.44(11) . 8_765 ?
O2B Dy O2B 124.03(11) . 8_765 ?
O2 Dy O2B 66.0(6) 8_765 8_765 ?
N1 Dy O2B 155.6(2) . 8_765 ?
N1 Dy O2B 65.9(3) 8_765 8_765 ?
O2A Dy O2 97.6(6) . . ?
O2B Dy O2 66.9(6) . . ?
O2 Dy O2 134.5(8) 8_765 . ?
N1 Dy O2 4.3(8) . . ?
N1 Dy O2 134.5(6) 8_765 . ?
O2B Dy O2 159.5(6) 8_765 . ?
O2A Dy O1 74.38(11) . . ?
O2B Dy O1 78.74(11) . . ?
O2 Dy O1 72.1(6) 8_765 . ?
N1 Dy O1 74.1(2) . . ?
N1 Dy O1 74.5(2) 8_765 . ?
O2B Dy O1 126.94(10) 8_765 . ?
O2 Dy O1 69.8(6) . . ?
O2A Dy N1B 134.41(12) . . ?
O2B Dy N1B 70.74(12) . . ?
O2 Dy N1B 110.6(6) 8_765 . ?
N1 Dy N1B 86.7(2) . . ?
N1 Dy N1B 106.7(2) 8_765 . ?
O2B Dy N1B 78.71(11) 8_765 . ?
O2 Dy N1B 90.5(6) . . ?
O1 Dy N1B 148.44(11) . . ?
O2A Dy N1A 71.30(12) . . ?
O2B Dy N1A 121.93(11) . . ?
O2 Dy N1A 150.3(6) 8_765 . ?
N1 Dy N1A 71.1(2) . . ?
N1 Dy N1A 150.9(3) 8_765 . ?
O2B Dy N1A 85.15(11) 8_765 . ?
O2 Dy N1A 74.6(6) . . ?
O1 Dy N1A 125.73(11) . . ?
N1B Dy N1A 67.91(12) . . ?
O2A Dy Dy 124.04(8) . 8_755 ?
O2B Dy Dy 34.36(7) . 8_755 ?
O2 Dy Dy 106.6(6) 8_765 8_755 ?
N1 Dy Dy 35.1(2) . 8_755 ?
N1 Dy Dy 105.2(2) 8_765 8_755 ?
O2B Dy Dy 157.47(7) 8_765 8_755 ?
O2 Dy Dy 33.4(6) . 8_755 ?
O1 Dy Dy 65.12(7) . 8_755 ?
N1B Dy Dy 84.74(8) . 8_755 ?
N1A Dy Dy 102.76(8) . 8_755 ?
O2A Dy Dy 80.33(8) . 8_765 ?
O2B Dy Dy 109.57(8) . 8_765 ?
O2 Dy Dy 34.1(6) 8_765 8_765 ?
N1 Dy Dy 171.4(2) . 8_765 ?
N1 Dy Dy 34.9(2) 8_765 8_765 ?
O2B Dy Dy 32.78(7) 8_765 8_765 ?
O2 Dy Dy 167.1(6) . 8_765 ?
O1 Dy Dy 97.48(7) . 8_765 ?
N1B Dy Dy 100.04(8) . 8_765 ?
N1A Dy Dy 116.22(8) . 8_765 ?
Dy Dy Dy 139.688(19) 8_755 8_765 ?
C2A O2A Dy 144.2(3) . . ?
C2A C1A C11A 121.6(4) . . ?
C2A C1A C9A 119.5(4) . . ?
C11A C1A C9A 118.8(4) . . ?
O2A C2A C1A 122.6(4) . . ?
O2A C2A C3A 118.1(4) . . ?
C1A C2A C3A 119.2(4) . . ?
C4A C3A C2A 121.7(5) . . ?
C4A C3A H3A 119.1 . . ?
C2A C3A H3A 119.1 . . ?
C3A C4A C10A 121.5(5) . . ?
C3A C4A H4A 119.2 . . ?
C10A C4A H4A 119.2 . . ?
C6A C5A C10A 120.5(5) . . ?
C6A C5A H5A 119.7 . . ?
C10A C5A H5A 119.7 . . ?
C5A C6A C7A 119.3(5) . . ?
C5A C6A H6A 120.3 . . ?
C7A C6A H6A 120.3 . . ?
C8A C7A C6A 121.2(5) . . ?
C8A C7A H7A 119.4 . . ?
C6A C7A H7A 119.4 . . ?
C7A C8A C9A 121.7(5) . . ?
C7A C8A H8A 119.2 . . ?
C9A C8A H8A 119.2 . . ?
C8A C9A C10A 116.2(5) . . ?
C8A C9A C1A 124.6(4) . . ?
C10A C9A C1A 119.3(4) . . ?
C5A C10A C4A 120.2(5) . . ?
C5A C10A C9A 121.0(5) . . ?
C4A C10A C9A 118.7(5) . . ?
N1A C11A C1A 128.1(4) . . ?
N1A C11A H11A 115.9 . . ?
C1A C11A H11A 115.9 . . ?
C11A N1A C12A 116.0(4) . . ?
C11A N1A Dy 130.7(3) . . ?
C12A N1A Dy 112.3(3) . . ?
N1A C12A C12B 110.9(4) . . ?
N1A C12A H12A 109.5 . . ?
C12B C12A H12A 109.5 . . ?
N1A C12A H12B 109.5 . . ?
C12B C12A H12B 109.5 . . ?
H12A C12A H12B 108.0 . . ?
N1B C12B C12A 109.0(4) . . ?
N1B C12B H12C 109.9 . . ?
C12A C12B H12C 109.9 . . ?
N1B C12B H12D 109.9 . . ?
C12A C12B H12D 109.9 . . ?
H12C C12B H12D 108.3 . . ?
C11B N1B C12B 116.9(4) . . ?
C11B N1B Dy 125.8(3) . . ?
C12B N1B Dy 117.1(3) . . ?
N1B C11B C1B 124.4(5) . . ?
N1B C11B H11B 117.8 . . ?
C1B C11B H11B 117.8 . . ?
C2B O2B Dy 119.1(3) . . ?
C2B O2B Dy 127.2(3) . 8_755 ?
Dy O2B Dy 112.86(13) . 8_755 ?
C2B C1B C9B 119.7(5) . . ?
C2B C1B C11B 121.5(5) . . ?
C9B C1B C11B 118.8(4) . . ?
O2B C2B C1B 121.1(4) . . ?
O2B C2B C3B 119.7(4) . . ?
C1B C2B C3B 119.1(4) . . ?
C4B C3B C2B 121.4(5) . . ?
C4B C3B H3B 119.3 . . ?
C2B C3B H3B 119.3 . . ?
C3B C4B C10B 122.2(5) . . ?
C3B C4B H4B 118.9 . . ?
C10B C4B H4B 118.9 . . ?
C6B C5B C10B 122.0(5) . . ?
C6B C5B H5B 119.0 . . ?
C10B C5B H5B 119.0 . . ?
C5B C6B C7B 118.9(5) . . ?
C5B C6B H6B 120.6 . . ?
C7B C6B H6B 120.6 . . ?
C8B C7B C6B 121.5(5) . . ?
C8B C7B H7B 119.3 . . ?
C6B C7B H7B 119.3 . . ?
C7B C8B C9B 120.7(5) . . ?
C7B C8B H8B 119.7 . . ?
C9B C8B H8B 119.7 . . ?
C8B C9B C10B 117.6(4) . . ?
C8B C9B C1B 123.1(5) . . ?
C10B C9B C1B 119.2(4) . . ?
C4B C10B C5B 122.3(5) . . ?
C4B C10B C9B 118.3(4) . . ?
C5B C10B C9B 119.4(5) . . ?
N2 N1 Dy 123.6(8) . . ?
N2 N1 Dy 123.4(8) . 8_755 ?
Dy N1 Dy 110.0(4) . 8_755 ?
N3 N2 N1 178.0(10) . . ?
N3 N2 H2A 67.4 . . ?
N1 N2 H2A 113.2 . . ?
N3 N2 H2B 58.0 . . ?
N1 N2 H2B 123.7 . . ?
H2A N2 H2B 89.7 . . ?
N3 N2 H2C 57.5 . . ?
N1 N2 H2C 120.5 . . ?
H2A N2 H2C 95.4 . . ?
H2B N2 H2C 106.5 . . ?
N2 N3 H2A 57.8 . . ?
N2 N3 H2B 55.7 . . ?
H2A N3 H2B 83.0 . . ?
N2 N3 H2C 50.1 . . ?
H2A N3 H2C 84.8 . . ?
H2B N3 H2C 98.2 . . ?
C2 O2 Dy 128(2) . 8_755 ?
C2 O2 Dy 119(2) . . ?
Dy O2 Dy 112.4(9) 8_755 . ?
O2 C2 H2A 109.8 . . ?
O2 C2 H2B 109.6 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.0 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 O1 Dy 124.5(3) . . ?
C1 O1 H1 102.5 . . ?
Dy O1 H1 113.4 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11A C1A C2A O2A -1.5(7) . . . . ?
C9A C1A C2A O2A 179.1(4) . . . . ?
C11A C1A C2A C3A -179.4(4) . . . . ?
C9A C1A C2A C3A 1.3(7) . . . . ?
O2A C2A C3A C4A -178.4(4) . . . . ?
C1A C2A C3A C4A -0.4(7) . . . . ?
C2A C3A C4A C10A -0.4(7) . . . . ?
C10A C5A C6A C7A -0.6(7) . . . . ?
C5A C6A C7A C8A 0.3(8) . . . . ?
C6A C7A C8A C9A 0.6(8) . . . . ?
C7A C8A C9A C10A -1.1(7) . . . . ?
C7A C8A C9A C1A 178.4(4) . . . . ?
C2A C1A C9A C8A 179.2(4) . . . . ?
C11A C1A C9A C8A -0.2(7) . . . . ?
C2A C1A C9A C10A -1.4(7) . . . . ?
C11A C1A C9A C10A 179.3(4) . . . . ?
C6A C5A C10A C4A -179.3(5) . . . . ?
C6A C5A C10A C9A 0.1(7) . . . . ?
C3A C4A C10A C5A 179.7(4) . . . . ?
C3A C4A C10A C9A 0.3(7) . . . . ?
C8A C9A C10A C5A 0.7(6) . . . . ?
C1A C9A C10A C5A -178.8(4) . . . . ?
C8A C9A C10A C4A -179.9(4) . . . . ?
C1A C9A C10A C4A 0.6(6) . . . . ?
C2A C1A C11A N1A -0.9(7) . . . . ?
C9A C1A C11A N1A 178.5(4) . . . . ?
C1A C11A N1A C12A 177.5(4) . . . . ?
C11A N1A C12A C12B 142.8(4) . . . . ?
N1A C12A C12B N1B 52.8(5) . . . . ?
C12A C12B N1B C11B 143.2(4) . . . . ?
C12B N1B C11B C1B -179.8(4) . . . . ?
N1B C11B C1B C2B 32.5(7) . . . . ?
N1B C11B C1B C9B -149.1(4) . . . . ?
C9B C1B C2B O2B -176.8(4) . . . . ?
C11B C1B C2B O2B 1.6(7) . . . . ?
C9B C1B C2B C3B 0.6(7) . . . . ?
C11B C1B C2B C3B 178.9(4) . . . . ?
O2B C2B C3B C4B 175.9(4) . . . . ?
C1B C2B C3B C4B -1.5(7) . . . . ?
C2B C3B C4B C10B 1.7(7) . . . . ?
C10B C5B C6B C7B 0.5(8) . . . . ?
C5B C6B C7B C8B 0.7(8) . . . . ?
C6B C7B C8B C9B -1.3(8) . . . . ?
C7B C8B C9B C10B 0.5(7) . . . . ?
C7B C8B C9B C1B 178.9(5) . . . . ?
C2B C1B C9B C8B -178.3(4) . . . . ?
C11B C1B C9B C8B 3.3(7) . . . . ?
C2B C1B C9B C10B 0.1(7) . . . . ?
C11B C1B C9B C10B -178.3(4) . . . . ?
C3B C4B C10B C5B 176.8(4) . . . . ?
C3B C4B C10B C9B -1.0(7) . . . . ?
C6B C5B C10B C4B -179.0(5) . . . . ?
C6B C5B C10B C9B -1.2(7) . . . . ?
C8B C9B C10B C4B 178.5(4) . . . . ?
C1B C9B C10B C4B 0.1(6) . . . . ?
C8B C9B C10B C5B 0.7(6) . . . . ?
C1B C9B C10B C5B -177.8(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
O1 H1 O2A 0.86 1.86 2.712(4) 168.9 8_755
C1 H1A O2A 0.98 2.50 3.069(6) 117.1 .

_diffrn_measured_fraction_theta_max 0.866
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.88
_refine_diff_density_rms         0.190
####################################################################### 
# 
# 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_at1442a
_database_code_depnum_ccdc_archive 'CCDC 1494778'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C85 H58 Dy2 N6 O7, 2(C H4 O)'
_chemical_formula_sum            'C87 H66 Dy2 N6 O9'
_chemical_formula_weight         1664.46

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.328(4)
_cell_length_b                   17.582(5)
_cell_length_c                   18.751(6)
_cell_angle_alpha                82.66(3)
_cell_angle_beta                 85.97(3)
_cell_angle_gamma                82.48(3)
_cell_volume                     3343(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11082
_cell_measurement_theta_min      3
_cell_measurement_theta_max      29

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1668
_exptl_absorpt_coefficient_mu    2.288
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.6097
_exptl_absorpt_correction_T_max  0.8749
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27996
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         28.82
_reflns_number_total             15179
_reflns_number_gt                9965
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0220P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15179
_refine_ls_number_parameters     937
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.25773(2) 0.777618(12) 0.262878(12) 0.01439(6) Uani 1 1 d . . .
Dy2 Dy 0.60544(2) 0.786896(13) 0.173052(12) 0.01540(7) Uani 1 1 d . . .
C1A C 0.7588(4) 0.9390(3) 0.2483(2) 0.0164(11) Uani 1 1 d . . .
C2A C 0.7554(4) 0.9398(3) 0.1734(3) 0.0172(11) Uani 1 1 d . . .
O2A O 0.7273(3) 0.88149(18) 0.14417(16) 0.0202(8) Uani 1 1 d . . .
C3A C 0.7859(5) 1.0083(3) 0.1283(3) 0.0211(12) Uani 1 1 d . . .
H3A H 0.7932 1.0078 0.0776 0.025 Uiso 1 1 calc R . .
C4A C 0.8043(5) 1.0722(3) 0.1551(3) 0.0229(12) Uani 1 1 d . . .
H4A H 0.8234 1.1164 0.1233 0.027 Uiso 1 1 calc R . .
C5A C 0.8081(5) 1.1453(3) 0.2590(3) 0.0251(12) Uani 1 1 d . . .
H5A H 0.8205 1.1904 0.2267 0.030 Uiso 1 1 calc R . .
C6A C 0.8023(5) 1.1489(3) 0.3313(3) 0.0292(13) Uani 1 1 d . . .
H6A H 0.8145 1.1952 0.3497 0.035 Uiso 1 1 calc R . .
C7A C 0.7783(5) 1.0831(3) 0.3781(3) 0.0252(12) Uani 1 1 d . . .
H7A H 0.7711 1.0858 0.4285 0.030 Uiso 1 1 calc R . .
C8A C 0.7649(4) 1.0148(3) 0.3530(3) 0.0200(11) Uani 1 1 d . . .
H8A H 0.7489 0.9712 0.3864 0.024 Uiso 1 1 calc R . .
C9A C 0.7744(4) 1.0081(3) 0.2785(3) 0.0166(11) Uani 1 1 d . . .
C10A C 0.7958(4) 1.0757(3) 0.2310(3) 0.0181(11) Uani 1 1 d . . .
C11A C 0.7514(4) 0.8683(3) 0.2962(3) 0.0183(11) Uani 1 1 d . . .
H11A H 0.7816 0.8673 0.3431 0.022 Uiso 1 1 calc R . .
N1B N 0.7084(3) 0.8060(2) 0.28245(19) 0.0127(8) Uani 1 1 d . . .
C1B C 0.7095(4) 0.7417(3) 0.3368(2) 0.0142(10) Uani 1 1 d . . .
C2B C 0.7017(4) 0.7476(3) 0.4103(3) 0.0180(11) Uani 1 1 d . . .
H2B H 0.6964 0.7971 0.4263 0.022 Uiso 1 1 calc R . .
C3B C 0.7014(4) 0.6828(3) 0.4603(3) 0.0181(11) Uani 1 1 d . . .
H3B H 0.6985 0.6875 0.5104 0.022 Uiso 1 1 calc R . .
C4B C 0.7054(5) 0.6108(3) 0.4369(3) 0.0216(12) Uani 1 1 d . . .
H4B H 0.7044 0.5661 0.4712 0.026 Uiso 1 1 calc R . .
C5B C 0.7108(4) 0.6037(3) 0.3653(3) 0.0186(12) Uani 1 1 d . . .
H5B H 0.7132 0.5540 0.3500 0.022 Uiso 1 1 calc R . .
C6B C 0.7128(4) 0.6689(3) 0.3137(2) 0.0165(11) Uani 1 1 d . . .
N6B N 0.7106(4) 0.6669(2) 0.2377(2) 0.0158(9) Uani 1 1 d . . .
C11C C 0.7589(4) 0.6033(3) 0.2123(3) 0.0192(11) Uani 1 1 d . . .
H11C H 0.7964 0.5632 0.2463 0.023 Uiso 1 1 calc R . .
C1C C 0.7629(4) 0.5859(3) 0.1391(3) 0.0151(11) Uani 1 1 d . . .
C2C C 0.7417(4) 0.6463(3) 0.0816(3) 0.0185(11) Uani 1 1 d . . .
O2C O 0.7030(3) 0.71796(18) 0.09082(16) 0.0202(8) Uani 1 1 d . . .
C3C C 0.7668(5) 0.6269(3) 0.0100(3) 0.0282(13) Uani 1 1 d . . .
H3C H 0.7552 0.6666 -0.0292 0.034 Uiso 1 1 calc R . .
C4C C 0.8064(5) 0.5542(3) -0.0033(3) 0.0308(14) Uani 1 1 d . . .
H4C H 0.8262 0.5443 -0.0518 0.037 Uiso 1 1 calc R . .
C5C C 0.8565(5) 0.4145(3) 0.0379(3) 0.0368(15) Uani 1 1 d . . .
H5C H 0.8766 0.4047 -0.0105 0.044 Uiso 1 1 calc R . .
C6C C 0.8637(6) 0.3552(3) 0.0907(3) 0.0362(15) Uani 1 1 d . . .
H6C H 0.8905 0.3040 0.0796 0.043 Uiso 1 1 calc R . .
C7C C 0.8316(6) 0.3687(3) 0.1620(3) 0.0396(15) Uani 1 1 d . . .
H7C H 0.8335 0.3266 0.1992 0.048 Uiso 1 1 calc R . .
C8C C 0.7971(5) 0.4431(3) 0.1784(3) 0.0298(13) Uani 1 1 d . . .
H8C H 0.7745 0.4514 0.2270 0.036 Uiso 1 1 calc R . .
C9C C 0.7946(5) 0.5072(3) 0.1247(3) 0.0225(12) Uani 1 1 d . . .
C10C C 0.8200(5) 0.4906(3) 0.0529(3) 0.0276(12) Uani 1 1 d . . .
C1D C 0.4114(4) 0.9289(3) 0.3336(3) 0.0158(11) Uani 1 1 d . . .
C2D C 0.4295(4) 0.9204(3) 0.2602(3) 0.0149(11) Uani 1 1 d . . .
O2D O 0.4302(3) 0.85256(17) 0.23584(16) 0.0142(7) Uani 1 1 d . . .
C3D C 0.4527(4) 0.9856(3) 0.2089(3) 0.0151(11) Uani 1 1 d . . .
H3D H 0.4648 0.9797 0.1591 0.018 Uiso 1 1 calc R . .
C4D C 0.4576(5) 1.0557(3) 0.2311(3) 0.0209(12) Uani 1 1 d . . .
H4D H 0.4745 1.0980 0.1964 0.025 Uiso 1 1 calc R . .
C5D C 0.4392(5) 1.1415(3) 0.3265(3) 0.0231(12) Uani 1 1 d . . .
H5D H 0.4571 1.1833 0.2914 0.028 Uiso 1 1 calc R . .
C6D C 0.4154(5) 1.1540(3) 0.3964(3) 0.0247(12) Uani 1 1 d . . .
H6D H 0.4174 1.2039 0.4104 0.030 Uiso 1 1 calc R . .
C7D C 0.3874(5) 1.0915(3) 0.4483(3) 0.0274(13) Uani 1 1 d . . .
H7D H 0.3698 1.0997 0.4973 0.033 Uiso 1 1 calc R . .
C8D C 0.3853(5) 1.0195(3) 0.4286(3) 0.0220(11) Uani 1 1 d . . .
H8D H 0.3649 0.9786 0.4641 0.026 Uiso 1 1 calc R . .
C9D C 0.4128(5) 1.0047(3) 0.3563(3) 0.0164(11) Uani 1 1 d . . .
C10D C 0.4379(5) 1.0674(3) 0.3049(3) 0.0178(11) Uani 1 1 d . . .
C11D C 0.4029(4) 0.8620(3) 0.3869(2) 0.0159(11) Uani 1 1 d . . .
H11D H 0.4322 0.8646 0.4333 0.019 Uiso 1 1 calc R . .
N1E N 0.3586(4) 0.7992(2) 0.3762(2) 0.0155(9) Uani 1 1 d . . .
C1E C 0.3618(4) 0.7373(3) 0.4334(3) 0.0159(10) Uani 1 1 d . . .
C2E C 0.3574(5) 0.7450(3) 0.5062(2) 0.0184(11) Uani 1 1 d . . .
H2E H 0.3524 0.7951 0.5210 0.022 Uiso 1 1 calc R . .
C3E C 0.3602(5) 0.6815(3) 0.5574(3) 0.0226(12) Uani 1 1 d . . .
H3E H 0.3590 0.6879 0.6070 0.027 Uiso 1 1 calc R . .
C4E C 0.3649(5) 0.6082(3) 0.5369(3) 0.0237(12) Uani 1 1 d . . .
H4E H 0.3673 0.5643 0.5723 0.028 Uiso 1 1 calc R . .
C5E C 0.3659(5) 0.5995(3) 0.4647(3) 0.0208(12) Uani 1 1 d . . .
H5E H 0.3658 0.5495 0.4506 0.025 Uiso 1 1 calc R . .
C6E C 0.3671(4) 0.6632(3) 0.4126(3) 0.0173(11) Uani 1 1 d . . .
N6E N 0.3674(4) 0.6584(2) 0.3368(2) 0.0147(9) Uani 1 1 d . . .
C11F C 0.4194(4) 0.5951(3) 0.3129(3) 0.0175(11) Uani 1 1 d . . .
H11F H 0.4560 0.5546 0.3468 0.021 Uiso 1 1 calc R . .
C1F C 0.4259(5) 0.5813(3) 0.2385(3) 0.0167(11) Uani 1 1 d . . .
C2F C 0.4303(4) 0.6404(3) 0.1824(3) 0.0147(11) Uani 1 1 d . . .
O2F O 0.4290(3) 0.71457(17) 0.19329(16) 0.0150(7) Uani 1 1 d . . .
C3F C 0.4391(4) 0.6227(3) 0.1102(3) 0.0178(11) Uani 1 1 d . . .
H3F H 0.4407 0.6635 0.0717 0.021 Uiso 1 1 calc R . .
C4F C 0.4452(5) 0.5488(3) 0.0950(3) 0.0205(12) Uani 1 1 d . . .
H4F H 0.4503 0.5387 0.0463 0.025 Uiso 1 1 calc R . .
C5F C 0.4474(5) 0.4097(3) 0.1344(3) 0.0234(12) Uani 1 1 d . . .
H5F H 0.4543 0.3997 0.0856 0.028 Uiso 1 1 calc R . .
C6F C 0.4404(5) 0.3495(3) 0.1890(3) 0.0302(13) Uiso 1 1 d . . .
H6F H 0.4430 0.2981 0.1779 0.036 Uiso 1 1 calc R . .
C7F C 0.4295(6) 0.3646(3) 0.2602(3) 0.0330(14) Uani 1 1 d . . .
H7F H 0.4250 0.3230 0.2976 0.040 Uiso 1 1 calc R . .
C8F C 0.4253(5) 0.4385(3) 0.2777(3) 0.0278(13) Uani 1 1 d . . .
H8F H 0.4165 0.4472 0.3268 0.033 Uiso 1 1 calc R . .
C9F C 0.4441(5) 0.4865(3) 0.1511(3) 0.0198(12) Uani 1 1 d . . .
C10F C 0.4338(4) 0.5023(3) 0.2232(3) 0.0178(11) Uani 1 1 d . . .
C1G C 0.1338(4) 0.9841(3) 0.2157(2) 0.0164(10) Uani 1 1 d . . .
C2G C 0.1618(5) 0.9354(3) 0.1613(3) 0.0193(11) Uani 1 1 d . . .
O2G O 0.1757(3) 0.86111(18) 0.17225(16) 0.0196(8) Uani 1 1 d . . .
C3G C 0.1670(5) 0.9724(3) 0.0872(3) 0.0228(12) Uani 1 1 d . . .
H3G H 0.1759 0.9414 0.0488 0.027 Uiso 1 1 calc R . .
C4G C 0.1594(5) 1.0501(3) 0.0721(3) 0.0237(12) Uani 1 1 d . . .
H4G H 0.1611 1.0723 0.0232 0.028 Uiso 1 1 calc R . .
C5G C 0.1529(5) 1.1801(3) 0.1106(3) 0.0298(13) Uani 1 1 d . . .
H5G H 0.1594 1.2021 0.0617 0.036 Uiso 1 1 calc R . .
C6G C 0.1476(5) 1.2263(3) 0.1642(3) 0.0293(13) Uani 1 1 d . . .
H6G H 0.1514 1.2802 0.1525 0.035 Uiso 1 1 calc R . .
C7G C 0.1368(5) 1.1944(3) 0.2360(3) 0.0251(12) Uani 1 1 d . . .
H7G H 0.1331 1.2266 0.2733 0.030 Uiso 1 1 calc R . .
C8G C 0.1313(5) 1.1168(3) 0.2529(3) 0.0217(11) Uani 1 1 d . . .
H8G H 0.1249 1.0959 0.3021 0.026 Uiso 1 1 calc R . .
C9G C 0.1349(4) 1.0670(3) 0.1993(3) 0.0176(11) Uani 1 1 d . . .
C10G C 0.1487(5) 1.0999(3) 0.1273(3) 0.0215(12) Uani 1 1 d . . .
C11G C 0.0944(4) 0.9541(3) 0.2871(3) 0.0159(11) Uani 1 1 d . . .
H11G H 0.0501 0.9900 0.3171 0.019 Uiso 1 1 calc R . .
N1H N 0.1140(3) 0.8812(2) 0.31507(19) 0.0127(8) Uani 1 1 d . . .
C1H C 0.0604(4) 0.8602(3) 0.3858(2) 0.0145(10) Uani 1 1 d . . .
C2H C 0.0269(5) 0.9111(3) 0.4367(3) 0.0235(12) Uani 1 1 d . . .
H2H H 0.0403 0.9638 0.4249 0.028 Uiso 1 1 calc R . .
C3H C -0.0256(5) 0.8865(3) 0.5044(3) 0.0267(12) Uani 1 1 d . . .
H3H H -0.0493 0.9222 0.5386 0.032 Uiso 1 1 calc R . .
C4H C -0.0433(5) 0.8101(3) 0.5219(3) 0.0233(12) Uani 1 1 d . . .
H4H H -0.0809 0.7934 0.5680 0.028 Uiso 1 1 calc R . .
C5H C -0.0077(4) 0.7582(3) 0.4741(2) 0.0191(11) Uani 1 1 d . . .
H5H H -0.0184 0.7053 0.4875 0.023 Uiso 1 1 calc R . .
C6H C 0.0446(4) 0.7824(3) 0.4052(2) 0.0139(10) Uani 1 1 d . . .
N6H N 0.0866(3) 0.7312(2) 0.35223(19) 0.0134(8) Uani 1 1 d . . .
C11I C 0.0389(4) 0.6661(3) 0.3558(2) 0.0152(10) Uani 1 1 d . . .
H11I H -0.0234 0.6560 0.3945 0.018 Uiso 1 1 calc R . .
C1I C 0.0687(5) 0.6080(3) 0.3088(3) 0.0172(11) Uani 1 1 d . . .
C2I C 0.1164(4) 0.6274(3) 0.2376(3) 0.0172(11) Uani 1 1 d . . .
O2I O 0.1514(3) 0.69535(17) 0.21296(16) 0.0171(7) Uani 1 1 d . . .
C3I C 0.1233(5) 0.5717(3) 0.1874(3) 0.0219(12) Uani 1 1 d . . .
H3I H 0.1487 0.5861 0.1384 0.026 Uiso 1 1 calc R . .
C4I C 0.0948(5) 0.4997(3) 0.2084(3) 0.0240(12) Uani 1 1 d . . .
H4I H 0.1032 0.4637 0.1742 0.029 Uiso 1 1 calc R . .
C5I C 0.0212(5) 0.4006(3) 0.3015(3) 0.0277(12) Uani 1 1 d . . .
H5I H 0.0344 0.3641 0.2676 0.033 Uiso 1 1 calc R . .
C6I C -0.0276(6) 0.3781(3) 0.3695(3) 0.0309(14) Uani 1 1 d . . .
H6I H -0.0515 0.3275 0.3823 0.037 Uiso 1 1 calc R . .
C7I C -0.0415(5) 0.4313(3) 0.4200(3) 0.0266(12) Uani 1 1 d . . .
H7I H -0.0757 0.4167 0.4674 0.032 Uiso 1 1 calc R . .
C8I C -0.0065(5) 0.5043(3) 0.4021(3) 0.0214(11) Uani 1 1 d . . .
H8I H -0.0122 0.5381 0.4382 0.026 Uiso 1 1 calc R . .
C9I C 0.0381(4) 0.5305(3) 0.3306(2) 0.0175(10) Uani 1 1 d . . .
C10I C 0.0526(5) 0.4762(3) 0.2800(3) 0.0196(12) Uani 1 1 d . . .
O1M O 0.4887(3) 0.85453(19) 0.07299(16) 0.0251(8) Uani 1 1 d . . .
H1M H 0.4312 0.8284 0.0633 0.038 Uiso 1 1 d R . .
C1M C 0.5500(6) 0.8952(4) 0.0115(3) 0.0479(18) Uani 1 1 d . . .
H1M1 H 0.5934 0.9363 0.0268 0.072 Uiso 1 1 calc R . .
H1M2 H 0.4837 0.9179 -0.0225 0.072 Uiso 1 1 calc R . .
H1M3 H 0.6149 0.8592 -0.0119 0.072 Uiso 1 1 calc R . .
O2M O 0.1317(3) 0.7342(2) 0.06921(18) 0.0294(9) Uani 1 1 d . . .
H2M H 0.1428 0.7160 0.1123 0.044 Uiso 1 1 calc R . .
C2M C 0.0088(6) 0.7836(4) 0.0648(3) 0.0520(19) Uani 1 1 d . . .
H2M1 H -0.0101 0.8079 0.1093 0.078 Uiso 1 1 calc R . .
H2M2 H -0.0612 0.7528 0.0585 0.078 Uiso 1 1 calc R . .
H2M3 H 0.0141 0.8238 0.0237 0.078 Uiso 1 1 calc R . .
O3M O 0.3165(4) 0.8064(2) -0.0014(2) 0.0328(9) Uani 1 1 d . . .
H3M H 0.2611 0.7805 0.0218 0.049 Uiso 1 1 calc R . .
C3M C 0.3846(6) 0.7632(3) -0.0551(3) 0.0381(15) Uani 1 1 d . . .
H3M1 H 0.3478 0.7144 -0.0544 0.057 Uiso 1 1 calc R . .
H3M2 H 0.4775 0.7522 -0.0450 0.057 Uiso 1 1 calc R . .
H3M3 H 0.3753 0.7932 -0.1026 0.057 Uiso 1 1 calc R . .


_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 O2G 2.236(3) . ?
Dy1 O2I 2.254(3) . ?
Dy1 O2D 2.342(3) . ?
Dy1 O2F 2.364(3) . ?
Dy1 N1H 2.454(4) . ?
Dy1 N6H 2.492(4) . ?
Dy1 N1E 2.523(4) . ?
Dy1 N6E 2.540(4) . ?
Dy1 Dy2 3.8720(16) . ?
Dy2 O2C 2.191(3) . ?
Dy2 O2A 2.206(3) . ?
Dy2 O2F 2.339(3) . ?
Dy2 O2D 2.344(3) . ?
Dy2 O1M 2.400(3) . ?
Dy2 N1B 2.455(4) . ?
Dy2 N6B 2.456(4) . ?
C1A C2A 1.405(6) . ?
C1A C9A 1.436(6) . ?
C1A C11A 1.446(6) . ?
C2A O2A 1.296(5) . ?
C2A C3A 1.437(6) . ?
C3A C4A 1.329(7) . ?
C3A H3A 0.9500 . ?
C4A C10A 1.428(7) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.363(7) . ?
C5A C10A 1.416(7) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.397(7) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.371(6) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.412(6) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.423(6) . ?
C11A N1B 1.295(6) . ?
C11A H11A 0.9500 . ?
N1B C1B 1.422(5) . ?
C1B C2B 1.391(6) . ?
C1B C6B 1.398(6) . ?
C2B C3B 1.380(6) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.386(7) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.363(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.404(6) . ?
C5B H5B 0.9500 . ?
C6B N6B 1.431(6) . ?
N6B C11C 1.297(6) . ?
C11C C1C 1.441(7) . ?
C11C H11C 0.9500 . ?
C1C C2C 1.421(6) . ?
C1C C9C 1.433(6) . ?
C2C O2C 1.301(5) . ?
C2C C3C 1.424(7) . ?
C3C C4C 1.340(7) . ?
C3C H3C 0.9500 . ?
C4C C10C 1.435(7) . ?
C4C H4C 0.9500 . ?
C5C C6C 1.341(7) . ?
C5C C10C 1.401(7) . ?
C5C H5C 0.9500 . ?
C6C C7C 1.398(8) . ?
C6C H6C 0.9500 . ?
C7C C8C 1.377(7) . ?
C7C H7C 0.9500 . ?
C8C C9C 1.411(7) . ?
C8C H8C 0.9500 . ?
C9C C10C 1.414(7) . ?
C1D C2D 1.400(6) . ?
C1D C11D 1.450(6) . ?
C1D C9D 1.452(6) . ?
C2D O2D 1.330(5) . ?
C2D C3D 1.433(6) . ?
C3D C4D 1.359(6) . ?
C3D H3D 0.9500 . ?
C4D C10D 1.422(7) . ?
C4D H4D 0.9500 . ?
C5D C6D 1.357(7) . ?
C5D C10D 1.415(6) . ?
C5D H5D 0.9500 . ?
C6D C7D 1.417(7) . ?
C6D H6D 0.9500 . ?
C7D C8D 1.367(7) . ?
C7D H7D 0.9500 . ?
C8D C9D 1.414(6) . ?
C8D H8D 0.9500 . ?
C9D C10D 1.407(6) . ?
C11D N1E 1.293(6) . ?
C11D H11D 0.9500 . ?
N1E C1E 1.426(5) . ?
C1E C2E 1.386(6) . ?
C1E C6E 1.400(6) . ?
C2E C3E 1.376(6) . ?
C2E H2E 0.9500 . ?
C3E C4E 1.383(7) . ?
C3E H3E 0.9500 . ?
C4E C5E 1.381(7) . ?
C4E H4E 0.9500 . ?
C5E C6E 1.389(6) . ?
C5E H5E 0.9500 . ?
C6E N6E 1.435(6) . ?
N6E C11F 1.291(6) . ?
C11F C1F 1.441(6) . ?
C11F H11F 0.9500 . ?
C1F C2F 1.383(6) . ?
C1F C10F 1.446(6) . ?
C2F O2F 1.343(5) . ?
C2F C3F 1.423(6) . ?
C3F C4F 1.358(6) . ?
C3F H3F 0.9500 . ?
C4F C9F 1.419(6) . ?
C4F H4F 0.9500 . ?
C5F C6F 1.379(7) . ?
C5F C9F 1.420(6) . ?
C5F H5F 0.9500 . ?
C6F C7F 1.388(7) . ?
C6F H6F 0.9500 . ?
C7F C8F 1.374(7) . ?
C7F H7F 0.9500 . ?
C8F C10F 1.424(6) . ?
C8F H8F 0.9500 . ?
C9F C10F 1.408(7) . ?
C1G C2G 1.404(7) . ?
C1G C11G 1.426(6) . ?
C1G C9G 1.452(6) . ?
C2G O2G 1.286(5) . ?
C2G C3G 1.459(6) . ?
C3G C4G 1.352(6) . ?
C3G H3G 0.9500 . ?
C4G C10G 1.428(7) . ?
C4G H4G 0.9500 . ?
C5G C6G 1.364(7) . ?
C5G C10G 1.411(7) . ?
C5G H5G 0.9500 . ?
C6G C7G 1.395(7) . ?
C6G H6G 0.9500 . ?
C7G C8G 1.368(6) . ?
C7G H7G 0.9500 . ?
C8G C9G 1.410(7) . ?
C8G H8G 0.9500 . ?
C9G C10G 1.405(6) . ?
C11G N1H 1.317(5) . ?
C11G H11G 0.9500 . ?
N1H C1H 1.424(5) . ?
C1H C2H 1.386(6) . ?
C1H C6H 1.398(6) . ?
C2H C3H 1.385(7) . ?
C2H H2H 0.9500 . ?
C3H C4H 1.373(6) . ?
C3H H3H 0.9500 . ?
C4H C5H 1.359(6) . ?
C4H H4H 0.9500 . ?
C5H C6H 1.401(6) . ?
C5H H5H 0.9500 . ?
C6H N6H 1.432(5) . ?
N6H C11I 1.297(5) . ?
C11I C1I 1.423(6) . ?
C11I H11I 0.9500 . ?
C1I C2I 1.407(6) . ?
C1I C9I 1.440(6) . ?
C2I O2I 1.312(5) . ?
C2I C3I 1.434(7) . ?
C3I C4I 1.341(7) . ?
C3I H3I 0.9500 . ?
C4I C10I 1.409(7) . ?
C4I H4I 0.9500 . ?
C5I C6I 1.367(7) . ?
C5I C10I 1.412(6) . ?
C5I H5I 0.9500 . ?
C6I C7I 1.402(7) . ?
C6I H6I 0.9500 . ?
C7I C8I 1.372(6) . ?
C7I H7I 0.9500 . ?
C8I C9I 1.425(6) . ?
C8I H8I 0.9500 . ?
C9I C10I 1.419(7) . ?
O1M C1M 1.430(6) . ?
O1M H1M 0.8399 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
O2M C2M 1.443(7) . ?
O2M H2M 0.8400 . ?
C2M H2M1 0.9800 . ?
C2M H2M2 0.9800 . ?
C2M H2M3 0.9800 . ?
O3M C3M 1.429(6) . ?
O3M H3M 0.8400 . ?
C3M H3M1 0.9800 . ?
C3M H3M2 0.9800 . ?
C3M H3M3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2G Dy1 O2I 82.33(12) . . ?
O2G Dy1 O2D 79.89(11) . . ?
O2I Dy1 O2D 140.22(11) . . ?
O2G Dy1 O2F 96.33(11) . . ?
O2I Dy1 O2F 78.47(11) . . ?
O2D Dy1 O2F 68.57(10) . . ?
O2G Dy1 N1H 72.08(12) . . ?
O2I Dy1 N1H 114.32(12) . . ?
O2D Dy1 N1H 93.48(12) . . ?
O2F Dy1 N1H 160.46(11) . . ?
O2G Dy1 N6H 113.19(12) . . ?
O2I Dy1 N6H 71.53(12) . . ?
O2D Dy1 N6H 148.23(12) . . ?
O2F Dy1 N6H 133.71(11) . . ?
N1H Dy1 N6H 65.81(12) . . ?
O2G Dy1 N1E 131.17(12) . . ?
O2I Dy1 N1E 144.06(12) . . ?
O2D Dy1 N1E 69.09(11) . . ?
O2F Dy1 N1E 105.65(12) . . ?
N1H Dy1 N1E 73.19(12) . . ?
N6H Dy1 N1E 81.51(12) . . ?
O2G Dy1 N6E 163.42(12) . . ?
O2I Dy1 N6E 86.09(12) . . ?
O2D Dy1 N6E 102.01(11) . . ?
O2F Dy1 N6E 69.64(11) . . ?
N1H Dy1 N6E 123.84(12) . . ?
N6H Dy1 N6E 73.84(12) . . ?
N1E Dy1 N6E 63.41(12) . . ?
O2G Dy1 Dy2 89.66(9) . . ?
O2I Dy1 Dy2 110.95(8) . . ?
O2D Dy1 Dy2 34.30(8) . . ?
O2F Dy1 Dy2 34.37(7) . . ?
N1H Dy1 Dy2 127.66(9) . . ?
N6H Dy1 Dy2 157.00(8) . . ?
N1E Dy1 Dy2 85.29(9) . . ?
N6E Dy1 Dy2 83.43(8) . . ?
O2C Dy2 O2A 93.69(12) . . ?
O2C Dy2 O2F 93.84(11) . . ?
O2A Dy2 O2F 163.62(11) . . ?
O2C Dy2 O2D 157.03(11) . . ?
O2A Dy2 O2D 99.53(11) . . ?
O2F Dy2 O2D 68.95(10) . . ?
O2C Dy2 O1M 83.02(12) . . ?
O2A Dy2 O1M 81.21(12) . . ?
O2F Dy2 O1M 85.30(11) . . ?
O2D Dy2 O1M 80.56(11) . . ?
O2C Dy2 N1B 123.59(12) . . ?
O2A Dy2 N1B 72.52(12) . . ?
O2F Dy2 N1B 114.66(11) . . ?
O2D Dy2 N1B 78.58(11) . . ?
O1M Dy2 N1B 142.94(12) . . ?
O2C Dy2 N6B 73.50(12) . . ?
O2A Dy2 N6B 116.78(12) . . ?
O2F Dy2 N6B 79.35(12) . . ?
O2D Dy2 N6B 115.88(12) . . ?
O1M Dy2 N6B 150.82(12) . . ?
N1B Dy2 N6B 66.20(13) . . ?
O2C Dy2 Dy1 127.72(8) . . ?
O2A Dy2 Dy1 133.30(8) . . ?
O2F Dy2 Dy1 34.80(8) . . ?
O2D Dy2 Dy1 34.25(7) . . ?
O1M Dy2 Dy1 83.41(8) . . ?
N1B Dy2 Dy1 95.80(9) . . ?
N6B Dy2 Dy1 97.26(9) . . ?
C2A C1A C9A 120.5(4) . . ?
C2A C1A C11A 120.7(4) . . ?
C9A C1A C11A 118.7(4) . . ?
O2A C2A C1A 122.7(4) . . ?
O2A C2A C3A 119.5(4) . . ?
C1A C2A C3A 117.7(4) . . ?
C2A O2A Dy2 136.9(3) . . ?
C4A C3A C2A 122.3(5) . . ?
C4A C3A H3A 118.8 . . ?
C2A C3A H3A 118.8 . . ?
C3A C4A C10A 121.0(5) . . ?
C3A C4A H4A 119.5 . . ?
C10A C4A H4A 119.5 . . ?
C6A C5A C10A 121.1(5) . . ?
C6A C5A H5A 119.4 . . ?
C10A C5A H5A 119.4 . . ?
C5A C6A C7A 118.8(5) . . ?
C5A C6A H6A 120.6 . . ?
C7A C6A H6A 120.6 . . ?
C8A C7A C6A 121.6(5) . . ?
C8A C7A H7A 119.2 . . ?
C6A C7A H7A 119.2 . . ?
C7A C8A C9A 121.2(5) . . ?
C7A C8A H8A 119.4 . . ?
C9A C8A H8A 119.4 . . ?
C8A C9A C10A 117.0(4) . . ?
C8A C9A C1A 124.3(4) . . ?
C10A C9A C1A 118.7(4) . . ?
C5A C10A C9A 120.1(5) . . ?
C5A C10A C4A 120.7(5) . . ?
C9A C10A C4A 119.2(5) . . ?
N1B C11A C1A 127.4(5) . . ?
N1B C11A H11A 116.3 . . ?
C1A C11A H11A 116.3 . . ?
C11A N1B C1B 119.1(4) . . ?
C11A N1B Dy2 127.2(3) . . ?
C1B N1B Dy2 113.5(3) . . ?
C2B C1B C6B 119.1(4) . . ?
C2B C1B N1B 124.1(4) . . ?
C6B C1B N1B 116.8(4) . . ?
C3B C2B C1B 121.1(4) . . ?
C3B C2B H2B 119.4 . . ?
C1B C2B H2B 119.4 . . ?
C2B C3B C4B 119.4(4) . . ?
C2B C3B H3B 120.3 . . ?
C4B C3B H3B 120.3 . . ?
C5B C4B C3B 120.6(4) . . ?
C5B C4B H4B 119.7 . . ?
C3B C4B H4B 119.7 . . ?
C4B C5B C6B 120.7(5) . . ?
C4B C5B H5B 119.6 . . ?
C6B C5B H5B 119.6 . . ?
C1B C6B C5B 119.0(4) . . ?
C1B C6B N6B 116.7(4) . . ?
C5B C6B N6B 124.2(4) . . ?
C11C N6B C6B 117.7(4) . . ?
C11C N6B Dy2 128.6(3) . . ?
C6B N6B Dy2 113.6(3) . . ?
N6B C11C C1C 128.2(5) . . ?
N6B C11C H11C 115.9 . . ?
C1C C11C H11C 115.9 . . ?
C2C C1C C9C 120.4(4) . . ?
C2C C1C C11C 120.3(4) . . ?
C9C C1C C11C 119.2(4) . . ?
O2C C2C C1C 123.7(4) . . ?
O2C C2C C3C 118.6(4) . . ?
C1C C2C C3C 117.7(4) . . ?
C2C O2C Dy2 140.1(3) . . ?
C4C C3C C2C 121.7(5) . . ?
C4C C3C H3C 119.1 . . ?
C2C C3C H3C 119.1 . . ?
C3C C4C C10C 122.4(5) . . ?
C3C C4C H4C 118.8 . . ?
C10C C4C H4C 118.8 . . ?
C6C C5C C10C 121.3(5) . . ?
C6C C5C H5C 119.3 . . ?
C10C C5C H5C 119.3 . . ?
C5C C6C C7C 119.8(5) . . ?
C5C C6C H6C 120.1 . . ?
C7C C6C H6C 120.1 . . ?
C8C C7C C6C 120.1(5) . . ?
C8C C7C H7C 119.9 . . ?
C6C C7C H7C 119.9 . . ?
C7C C8C C9C 121.6(5) . . ?
C7C C8C H8C 119.2 . . ?
C9C C8C H8C 119.2 . . ?
C8C C9C C10C 116.4(5) . . ?
C8C C9C C1C 123.8(5) . . ?
C10C C9C C1C 119.7(5) . . ?
C5C C10C C9C 120.6(5) . . ?
C5C C10C C4C 121.8(5) . . ?
C9C C10C C4C 117.7(5) . . ?
C2D C1D C11D 120.6(4) . . ?
C2D C1D C9D 119.1(4) . . ?
C11D C1D C9D 120.1(4) . . ?
O2D C2D C1D 122.2(4) . . ?
O2D C2D C3D 117.9(4) . . ?
C1D C2D C3D 119.9(4) . . ?
C2D O2D Dy1 122.2(3) . . ?
C2D O2D Dy2 126.0(3) . . ?
Dy1 O2D Dy2 111.45(13) . . ?
C4D C3D C2D 120.4(4) . . ?
C4D C3D H3D 119.8 . . ?
C2D C3D H3D 119.8 . . ?
C3D C4D C10D 121.7(4) . . ?
C3D C4D H4D 119.1 . . ?
C10D C4D H4D 119.1 . . ?
C6D C5D C10D 121.2(5) . . ?
C6D C5D H5D 119.4 . . ?
C10D C5D H5D 119.4 . . ?
C5D C6D C7D 119.0(5) . . ?
C5D C6D H6D 120.5 . . ?
C7D C6D H6D 120.5 . . ?
C8D C7D C6D 120.7(5) . . ?
C8D C7D H7D 119.6 . . ?
C6D C7D H7D 119.6 . . ?
C7D C8D C9D 121.3(5) . . ?
C7D C8D H8D 119.4 . . ?
C9D C8D H8D 119.4 . . ?
C10D C9D C8D 117.6(4) . . ?
C10D C9D C1D 119.7(4) . . ?
C8D C9D C1D 122.6(4) . . ?
C9D C10D C5D 120.1(5) . . ?
C9D C10D C4D 119.1(4) . . ?
C5D C10D C4D 120.7(4) . . ?
N1E C11D C1D 125.2(4) . . ?
N1E C11D H11D 117.4 . . ?
C1D C11D H11D 117.4 . . ?
C11D N1E C1E 118.3(4) . . ?
C11D N1E Dy1 125.4(3) . . ?
C1E N1E Dy1 116.3(3) . . ?
C2E C1E C6E 118.6(4) . . ?
C2E C1E N1E 125.6(4) . . ?
C6E C1E N1E 115.8(4) . . ?
C3E C2E C1E 121.1(4) . . ?
C3E C2E H2E 119.5 . . ?
C1E C2E H2E 119.5 . . ?
C2E C3E C4E 120.3(5) . . ?
C2E C3E H3E 119.8 . . ?
C4E C3E H3E 119.8 . . ?
C5E C4E C3E 119.5(5) . . ?
C5E C4E H4E 120.3 . . ?
C3E C4E H4E 120.3 . . ?
C4E C5E C6E 120.5(5) . . ?
C4E C5E H5E 119.7 . . ?
C6E C5E H5E 119.7 . . ?
C5E C6E C1E 119.9(4) . . ?
C5E C6E N6E 123.5(4) . . ?
C1E C6E N6E 116.5(4) . . ?
C11F N6E C6E 118.4(4) . . ?
C11F N6E Dy1 126.4(3) . . ?
C6E N6E Dy1 115.2(3) . . ?
N6E C11F C1F 124.8(4) . . ?
N6E C11F H11F 117.6 . . ?
C1F C11F H11F 117.6 . . ?
C2F C1F C11F 122.2(4) . . ?
C2F C1F C10F 119.8(4) . . ?
C11F C1F C10F 117.9(4) . . ?
O2F C2F C1F 122.6(4) . . ?
O2F C2F C3F 118.0(4) . . ?
C1F C2F C3F 119.4(4) . . ?
C2F O2F Dy2 126.3(3) . . ?
C2F O2F Dy1 121.3(3) . . ?
Dy2 O2F Dy1 110.83(12) . . ?
C4F C3F C2F 121.4(5) . . ?
C4F C3F H3F 119.3 . . ?
C2F C3F H3F 119.3 . . ?
C3F C4F C9F 120.9(5) . . ?
C3F C4F H4F 119.6 . . ?
C9F C4F H4F 119.6 . . ?
C6F C5F C9F 120.2(5) . . ?
C6F C5F H5F 119.9 . . ?
C9F C5F H5F 119.9 . . ?
C5F C6F C7F 119.6(5) . . ?
C5F C6F H6F 120.2 . . ?
C7F C6F H6F 120.2 . . ?
C8F C7F C6F 121.4(5) . . ?
C8F C7F H7F 119.3 . . ?
C6F C7F H7F 119.3 . . ?
C7F C8F C10F 121.0(5) . . ?
C7F C8F H8F 119.5 . . ?
C10F C8F H8F 119.5 . . ?
C10F C9F C5F 120.6(5) . . ?
C10F C9F C4F 119.1(4) . . ?
C5F C9F C4F 120.2(5) . . ?
C9F C10F C8F 117.2(4) . . ?
C9F C10F C1F 119.4(4) . . ?
C8F C10F C1F 123.3(5) . . ?
C2G C1G C11G 120.8(4) . . ?
C2G C1G C9G 120.7(4) . . ?
C11G C1G C9G 118.3(4) . . ?
O2G C2G C1G 124.7(4) . . ?
O2G C2G C3G 118.2(4) . . ?
C1G C2G C3G 117.0(4) . . ?
C2G O2G Dy1 131.9(3) . . ?
C4G C3G C2G 121.2(5) . . ?
C4G C3G H3G 119.4 . . ?
C2G C3G H3G 119.4 . . ?
C3G C4G C10G 122.2(5) . . ?
C3G C4G H4G 118.9 . . ?
C10G C4G H4G 118.9 . . ?
C6G C5G C10G 120.5(5) . . ?
C6G C5G H5G 119.7 . . ?
C10G C5G H5G 119.7 . . ?
C5G C6G C7G 120.0(5) . . ?
C5G C6G H6G 120.0 . . ?
C7G C6G H6G 120.0 . . ?
C8G C7G C6G 120.1(5) . . ?
C8G C7G H7G 120.0 . . ?
C6G C7G H7G 120.0 . . ?
C7G C8G C9G 121.9(5) . . ?
C7G C8G H8G 119.0 . . ?
C9G C8G H8G 119.0 . . ?
C10G C9G C8G 117.2(4) . . ?
C10G C9G C1G 119.6(5) . . ?
C8G C9G C1G 123.1(4) . . ?
C9G C10G C5G 120.3(5) . . ?
C9G C10G C4G 118.4(4) . . ?
C5G C10G C4G 121.4(5) . . ?
N1H C11G C1G 125.8(4) . . ?
N1H C11G H11G 117.1 . . ?
C1G C11G H11G 117.1 . . ?
C11G N1H C1H 118.6(4) . . ?
C11G N1H Dy1 126.1(3) . . ?
C1H N1H Dy1 114.9(3) . . ?
C2H C1H C6H 118.4(4) . . ?
C2H C1H N1H 124.4(4) . . ?
C6H C1H N1H 117.1(4) . . ?
C3H C2H C1H 121.2(5) . . ?
C3H C2H H2H 119.4 . . ?
C1H C2H H2H 119.4 . . ?
C4H C3H C2H 119.4(5) . . ?
C4H C3H H3H 120.3 . . ?
C2H C3H H3H 120.3 . . ?
C5H C4H C3H 121.0(5) . . ?
C5H C4H H4H 119.5 . . ?
C3H C4H H4H 119.5 . . ?
C4H C5H C6H 120.2(5) . . ?
C4H C5H H5H 119.9 . . ?
C6H C5H H5H 119.9 . . ?
C1H C6H C5H 119.8(4) . . ?
C1H C6H N6H 116.5(4) . . ?
C5H C6H N6H 123.7(4) . . ?
C11I N6H C6H 119.6(4) . . ?
C11I N6H Dy1 126.4(3) . . ?
C6H N6H Dy1 114.0(3) . . ?
N6H C11I C1I 127.8(4) . . ?
N6H C11I H11I 116.1 . . ?
C1I C11I H11I 116.1 . . ?
C2I C1I C11I 120.1(4) . . ?
C2I C1I C9I 118.8(4) . . ?
C11I C1I C9I 120.8(4) . . ?
O2I C2I C1I 123.6(4) . . ?
O2I C2I C3I 117.1(4) . . ?
C1I C2I C3I 119.2(4) . . ?
C2I O2I Dy1 132.0(3) . . ?
C4I C3I C2I 121.3(5) . . ?
C4I C3I H3I 119.4 . . ?
C2I C3I H3I 119.4 . . ?
C3I C4I C10I 121.6(5) . . ?
C3I C4I H4I 119.2 . . ?
C10I C4I H4I 119.2 . . ?
C6I C5I C10I 122.2(5) . . ?
C6I C5I H5I 118.9 . . ?
C10I C5I H5I 118.9 . . ?
C5I C6I C7I 118.4(5) . . ?
C5I C6I H6I 120.8 . . ?
C7I C6I H6I 120.8 . . ?
C8I C7I C6I 121.1(5) . . ?
C8I C7I H7I 119.4 . . ?
C6I C7I H7I 119.4 . . ?
C7I C8I C9I 121.6(5) . . ?
C7I C8I H8I 119.2 . . ?
C9I C8I H8I 119.2 . . ?
C10I C9I C8I 116.9(4) . . ?
C10I C9I C1I 119.9(4) . . ?
C8I C9I C1I 123.2(4) . . ?
C4I C10I C5I 121.4(5) . . ?
C4I C10I C9I 119.0(5) . . ?
C5I C10I C9I 119.7(5) . . ?
C1M O1M Dy2 123.7(3) . . ?
C1M O1M H1M 114.4 . . ?
Dy2 O1M H1M 109.3 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C2M O2M H2M 109.5 . . ?
O2M C2M H2M1 109.5 . . ?
O2M C2M H2M2 109.5 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.5 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?
C3M O3M H3M 109.5 . . ?
O3M C3M H3M1 109.5 . . ?
O3M C3M H3M2 109.5 . . ?
H3M1 C3M H3M2 109.5 . . ?
O3M C3M H3M3 109.5 . . ?
H3M1 C3M H3M3 109.5 . . ?
H3M2 C3M H3M3 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9A C1A C2A O2A -172.3(4) . . . . ?
C11A C1A C2A O2A 10.0(7) . . . . ?
C9A C1A C2A C3A 8.4(7) . . . . ?
C11A C1A C2A C3A -169.3(4) . . . . ?
O2A C2A C3A C4A 174.0(5) . . . . ?
C1A C2A C3A C4A -6.6(7) . . . . ?
C2A C3A C4A C10A 0.7(8) . . . . ?
C10A C5A C6A C7A -2.8(8) . . . . ?
C5A C6A C7A C8A 2.3(8) . . . . ?
C6A C7A C8A C9A -0.2(7) . . . . ?
C7A C8A C9A C10A -1.2(7) . . . . ?
C7A C8A C9A C1A -178.6(5) . . . . ?
C2A C1A C9A C8A 172.9(4) . . . . ?
C11A C1A C9A C8A -9.3(7) . . . . ?
C2A C1A C9A C10A -4.5(7) . . . . ?
C11A C1A C9A C10A 173.3(4) . . . . ?
C6A C5A C10A C9A 1.3(7) . . . . ?
C6A C5A C10A C4A -178.9(5) . . . . ?
C8A C9A C10A C5A 0.7(7) . . . . ?
C1A C9A C10A C5A 178.3(4) . . . . ?
C8A C9A C10A C4A -179.1(4) . . . . ?
C1A C9A C10A C4A -1.5(7) . . . . ?
C3A C4A C10A C5A -176.3(5) . . . . ?
C3A C4A C10A C9A 3.5(7) . . . . ?
C2A C1A C11A N1B -19.4(7) . . . . ?
C9A C1A C11A N1B 162.8(5) . . . . ?
C1A C11A N1B C1B 179.7(4) . . . . ?
C11A N1B C1B C2B 27.4(6) . . . . ?
C11A N1B C1B C6B -155.5(4) . . . . ?
C6B C1B C2B C3B 2.1(7) . . . . ?
N1B C1B C2B C3B 179.1(4) . . . . ?
C1B C2B C3B C4B -1.8(7) . . . . ?
C2B C3B C4B C5B 0.6(7) . . . . ?
C3B C4B C5B C6B 0.2(7) . . . . ?
C2B C1B C6B C5B -1.3(7) . . . . ?
N1B C1B C6B C5B -178.5(4) . . . . ?
C2B C1B C6B N6B 175.3(4) . . . . ?
N1B C1B C6B N6B -1.9(6) . . . . ?
C4B C5B C6B C1B 0.2(7) . . . . ?
C4B C5B C6B N6B -176.2(4) . . . . ?
C1B C6B N6B C11C 156.0(4) . . . . ?
C5B C6B N6B C11C -27.6(7) . . . . ?
C6B N6B C11C C1C 177.1(4) . . . . ?
Dy2 N6B C11C C1C -0.5(7) . . . . ?
N6B C11C C1C C2C 16.4(8) . . . . ?
N6B C11C C1C C9C -166.5(5) . . . . ?
C9C C1C C2C O2C 174.6(4) . . . . ?
C11C C1C C2C O2C -8.3(7) . . . . ?
C9C C1C C2C C3C -6.7(7) . . . . ?
C11C C1C C2C C3C 170.4(4) . . . . ?
O2C C2C C3C C4C -179.8(5) . . . . ?
C1C C2C C3C C4C 1.4(8) . . . . ?
C2C C3C C4C C10C 3.1(9) . . . . ?
C10C C5C C6C C7C 1.4(9) . . . . ?
C5C C6C C7C C8C -2.3(9) . . . . ?
C6C C7C C8C C9C -0.8(9) . . . . ?
C7C C8C C9C C10C 4.4(8) . . . . ?
C7C C8C C9C C1C -178.2(5) . . . . ?
C2C C1C C9C C8C -169.7(5) . . . . ?
C11C C1C C9C C8C 13.1(7) . . . . ?
C2C C1C C9C C10C 7.5(7) . . . . ?
C11C C1C C9C C10C -169.6(5) . . . . ?
C6C C5C C10C C9C 2.5(9) . . . . ?
C6C C5C C10C C4C -177.2(5) . . . . ?
C8C C9C C10C C5C -5.2(8) . . . . ?
C1C C9C C10C C5C 177.3(5) . . . . ?
C8C C9C C10C C4C 174.4(5) . . . . ?
C1C C9C C10C C4C -3.0(8) . . . . ?
C3C C4C C10C C5C 177.4(6) . . . . ?
C3C C4C C10C C9C -2.2(8) . . . . ?
C11D C1D C2D O2D 4.9(7) . . . . ?
C9D C1D C2D O2D 179.5(4) . . . . ?
C11D C1D C2D C3D -172.8(4) . . . . ?
C9D C1D C2D C3D 1.8(7) . . . . ?
O2D C2D C3D C4D -177.7(4) . . . . ?
C1D C2D C3D C4D 0.1(7) . . . . ?
C2D C3D C4D C10D -1.0(7) . . . . ?
C10D C5D C6D C7D -0.7(7) . . . . ?
C5D C6D C7D C8D 0.5(7) . . . . ?
C6D C7D C8D C9D 1.0(8) . . . . ?
C7D C8D C9D C10D -2.2(7) . . . . ?
C7D C8D C9D C1D 180.0(5) . . . . ?
C2D C1D C9D C10D -2.9(7) . . . . ?
C11D C1D C9D C10D 171.8(4) . . . . ?
C2D C1D C9D C8D 175.0(5) . . . . ?
C11D C1D C9D C8D -10.4(7) . . . . ?
C8D C9D C10D C5D 2.0(7) . . . . ?
C1D C9D C10D C5D 179.9(4) . . . . ?
C8D C9D C10D C4D -176.0(4) . . . . ?
C1D C9D C10D C4D 2.0(7) . . . . ?
C6D C5D C10D C9D -0.6(7) . . . . ?
C6D C5D C10D C4D 177.3(5) . . . . ?
C3D C4D C10D C9D 0.0(7) . . . . ?
C3D C4D C10D C5D -178.0(5) . . . . ?
C2D C1D C11D N1E -29.5(7) . . . . ?
C9D C1D C11D N1E 155.9(5) . . . . ?
C1D C11D N1E C1E 177.5(4) . . . . ?
C11D N1E C1E C2E 27.4(6) . . . . ?
C11D N1E C1E C6E -153.9(4) . . . . ?
C6E C1E C2E C3E 1.0(7) . . . . ?
N1E C1E C2E C3E 179.6(4) . . . . ?
C1E C2E C3E C4E -1.3(7) . . . . ?
C2E C3E C4E C5E -0.4(8) . . . . ?
C3E C4E C5E C6E 2.3(7) . . . . ?
C4E C5E C6E C1E -2.7(7) . . . . ?
C4E C5E C6E N6E -179.6(4) . . . . ?
C2E C1E C6E C5E 1.0(7) . . . . ?
N1E C1E C6E C5E -177.8(4) . . . . ?
C2E C1E C6E N6E 178.1(4) . . . . ?
N1E C1E C6E N6E -0.6(6) . . . . ?
C5E C6E N6E C11F -28.3(7) . . . . ?
C1E C6E N6E C11F 154.6(4) . . . . ?
C6E N6E C11F C1F 179.4(4) . . . . ?
Dy1 N6E C11F C1F 1.0(7) . . . . ?
N6E C11F C1F C2F 28.5(7) . . . . ?
N6E C11F C1F C10F -154.2(5) . . . . ?
C11F C1F C2F O2F 0.1(7) . . . . ?
C10F C1F C2F O2F -177.1(4) . . . . ?
C11F C1F C2F C3F 178.9(4) . . . . ?
C10F C1F C2F C3F 1.6(7) . . . . ?
O2F C2F C3F C4F 177.8(4) . . . . ?
C1F C2F C3F C4F -1.0(7) . . . . ?
C2F C3F C4F C9F -0.5(7) . . . . ?
C9F C5F C6F C7F 0.3(8) . . . . ?
C5F C6F C7F C8F 0.2(8) . . . . ?
C6F C7F C8F C10F -0.9(9) . . . . ?
C6F C5F C9F C10F 0.0(7) . . . . ?
C6F C5F C9F C4F -177.1(5) . . . . ?
C3F C4F C9F C10F 1.4(7) . . . . ?
C3F C4F C9F C5F 178.4(5) . . . . ?
C5F C9F C10F C8F -0.7(7) . . . . ?
C4F C9F C10F C8F 176.4(4) . . . . ?
C5F C9F C10F C1F -177.8(4) . . . . ?
C4F C9F C10F C1F -0.7(7) . . . . ?
C7F C8F C10F C9F 1.2(8) . . . . ?
C7F C8F C10F C1F 178.1(5) . . . . ?
C2F C1F C10F C9F -0.8(7) . . . . ?
C11F C1F C10F C9F -178.2(4) . . . . ?
C2F C1F C10F C8F -177.7(5) . . . . ?
C11F C1F C10F C8F 4.9(7) . . . . ?
C11G C1G C2G O2G -11.8(7) . . . . ?
C9G C1G C2G O2G 172.7(4) . . . . ?
C11G C1G C2G C3G 164.1(4) . . . . ?
C9G C1G C2G C3G -11.4(7) . . . . ?
O2G C2G C3G C4G -176.8(5) . . . . ?
C1G C2G C3G C4G 7.0(7) . . . . ?
C2G C3G C4G C10G 1.3(8) . . . . ?
C10G C5G C6G C7G -0.6(8) . . . . ?
C5G C6G C7G C8G 0.0(8) . . . . ?
C6G C7G C8G C9G -0.7(7) . . . . ?
C7G C8G C9G C10G 2.0(7) . . . . ?
C7G C8G C9G C1G 177.8(4) . . . . ?
C2G C1G C9G C10G 7.7(7) . . . . ?
C11G C1G C9G C10G -168.0(4) . . . . ?
C2G C1G C9G C8G -168.1(5) . . . . ?
C11G C1G C9G C8G 16.3(7) . . . . ?
C8G C9G C10G C5G -2.6(7) . . . . ?
C1G C9G C10G C5G -178.6(4) . . . . ?
C8G C9G C10G C4G 176.9(4) . . . . ?
C1G C9G C10G C4G 0.9(7) . . . . ?
C6G C5G C10G C9G 2.0(8) . . . . ?
C6G C5G C10G C4G -177.5(5) . . . . ?
C3G C4G C10G C9G -5.3(8) . . . . ?
C3G C4G C10G C5G 174.1(5) . . . . ?
C2G C1G C11G N1H 19.9(7) . . . . ?
C9G C1G C11G N1H -164.5(4) . . . . ?
C1G C11G N1H C1H -175.7(4) . . . . ?
C11G N1H C1H C2H -22.3(7) . . . . ?
C11G N1H C1H C6H 159.7(4) . . . . ?
C6H C1H C2H C3H -2.4(7) . . . . ?
N1H C1H C2H C3H 179.6(4) . . . . ?
C1H C2H C3H C4H 0.9(8) . . . . ?
C2H C3H C4H C5H 1.2(8) . . . . ?
C3H C4H C5H C6H -1.7(8) . . . . ?
C2H C1H C6H C5H 1.9(7) . . . . ?
N1H C1H C6H C5H -180.0(4) . . . . ?
C2H C1H C6H N6H -176.9(4) . . . . ?
N1H C1H C6H N6H 1.2(6) . . . . ?
C4H C5H C6H C1H 0.1(7) . . . . ?
C4H C5H C6H N6H 178.9(4) . . . . ?
C1H C6H N6H C11I -157.8(4) . . . . ?
C5H C6H N6H C11I 23.4(6) . . . . ?
C6H N6H C11I C1I -179.6(4) . . . . ?
Dy1 N6H C11I C1I -2.6(7) . . . . ?
N6H C11I C1I C2I -24.7(8) . . . . ?
N6H C11I C1I C9I 161.9(5) . . . . ?
C11I C1I C2I O2I 8.8(7) . . . . ?
C9I C1I C2I O2I -177.6(4) . . . . ?
C11I C1I C2I C3I -168.8(4) . . . . ?
C9I C1I C2I C3I 4.9(7) . . . . ?
O2I C2I C3I C4I 177.2(4) . . . . ?
C1I C2I C3I C4I -5.1(7) . . . . ?
C2I C3I C4I C10I 2.1(8) . . . . ?
C10I C5I C6I C7I -2.7(8) . . . . ?
C5I C6I C7I C8I -0.4(8) . . . . ?
C6I C7I C8I C9I 3.7(8) . . . . ?
C7I C8I C9I C10I -3.9(7) . . . . ?
C7I C8I C9I C1I 176.4(5) . . . . ?
C2I C1I C9I C10I -1.8(7) . . . . ?
C11I C1I C9I C10I 171.7(4) . . . . ?
C2I C1I C9I C8I 177.8(4) . . . . ?
C11I C1I C9I C8I -8.6(7) . . . . ?
C3I C4I C10I C5I 179.2(5) . . . . ?
C3I C4I C10I C9I 1.0(8) . . . . ?
C6I C5I C10I C4I -175.9(5) . . . . ?
C6I C5I C10I C9I 2.3(8) . . . . ?
C8I C9I C10I C4I 179.2(4) . . . . ?
C1I C9I C10I C4I -1.1(7) . . . . ?
C8I C9I C10I C5I 0.9(7) . . . . ?
C1I C9I C10I C5I -179.4(4) . . . . ?


_diffrn_measured_fraction_theta_max 0.870
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.151
####################################################################### 
# 
# 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_at1229a
_database_code_depnum_ccdc_archive 'CCDC 1494779'
_audit_update_record             
;
2016-07-19 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25.5 H23 Gd N2 O3.5, (C H4 O)'
_chemical_formula_sum            'C26.50 H27 Gd N2 O4.50'
_chemical_formula_weight         602.75

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   29.660(7)
_cell_length_b                   20.958(5)
_cell_length_c                   7.3955(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4597.1(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10862
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      28.64

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_F_000             2400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    2.925
_shelx_estimated_absorpt_T_min   0.353
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Kuma KM-4-CCD κ-geometry'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22306
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.996
_diffrn_reflns_theta_max         28.703
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             5430
_reflns_number_gt                4226
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis CCD (Agilent, 2013)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2013)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0513P)²+5.4529P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5430
_refine_ls_number_parameters     338
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0911
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_restrained_S_all      1.05
_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
Gd Gd 0.22635(2) 0.44306(2) 0.41039(2) 0.01719(8) Uani 1 1 d . . . . .
O2A O 0.18327(10) 0.36187(13) 0.5210(4) 0.0200(6) Uani 1 1 d . . . . .
C1A C 0.10388(14) 0.38189(19) 0.5081(5) 0.0171(8) Uani 1 1 d . . . . .
C2A C 0.14243(15) 0.34645(18) 0.5601(5) 0.0165(9) Uani 1 1 d . . . . .
C3A C 0.13529(16) 0.2887(2) 0.6618(6) 0.0242(10) Uani 1 1 d . . . . .
H3A H 0.1608 0.2643 0.6974 0.029 Uiso 1 1 calc R U . . .
C4A C 0.09418(17) 0.2680(2) 0.7081(6) 0.0276(10) Uani 1 1 d . . . . .
H4A H 0.0913 0.2295 0.7751 0.033 Uiso 1 1 calc R U . . .
C5A C 0.01166(17) 0.2802(3) 0.7118(6) 0.0325(12) Uani 1 1 d . . . . .
H5A H 0.0092 0.2424 0.7820 0.039 Uiso 1 1 calc R U . . .
C6A C -0.02634(18) 0.3123(3) 0.6636(7) 0.0356(13) Uani 1 1 d . . . . .
H6A H -0.0551 0.2972 0.7012 0.043 Uiso 1 1 calc R U . . .
C7A C -0.02284(18) 0.3679(3) 0.5576(7) 0.0352(12) Uani 1 1 d . . . . .
H7A H -0.0494 0.3899 0.5220 0.042 Uiso 1 1 calc R U . . .
C8A C 0.01855(17) 0.3906(2) 0.5052(6) 0.0301(11) Uani 1 1 d . . . . .
H8A H 0.0201 0.4281 0.4332 0.036 Uiso 1 1 calc R U . . .
C9A C 0.05912(16) 0.3591(2) 0.5563(6) 0.0237(10) Uani 1 1 d . . . . .
C10A C 0.05496(16) 0.3023(2) 0.6590(6) 0.0264(10) Uani 1 1 d . . . . .
C11A C 0.10782(15) 0.44079(19) 0.4077(5) 0.0176(8) Uani 1 1 d . . . . .
H11A H 0.0805 0.4592 0.3658 0.021 Uiso 1 1 calc R U . . .
N1A N 0.14444(13) 0.47119(17) 0.3686(4) 0.0192(8) Uani 1 1 d . . . . .
C12A C 0.13895(15) 0.5298(2) 0.2626(6) 0.0212(9) Uani 1 1 d . . . . .
H12A H 0.1068 0.5422 0.2600 0.025 Uiso 1 1 calc R U . . .
H12B H 0.1490 0.5223 0.1367 0.025 Uiso 1 1 calc R U . . .
C12B C 0.16654(15) 0.5826(2) 0.3462(6) 0.0214(9) Uani 1 1 d . . . . .
H12C H 0.1647 0.6215 0.2706 0.026 Uiso 1 1 calc R U . . .
H12D H 0.1548 0.5928 0.4681 0.026 Uiso 1 1 calc R U . . .
N1B N 0.21347(13) 0.56108(16) 0.3587(5) 0.0181(7) Uani 1 1 d . . . . .
C11B C 0.24454(16) 0.6024(2) 0.3320(5) 0.0198(9) Uani 1 1 d . . . . .
H11B H 0.2353 0.6449 0.3063 0.024 Uiso 1 1 calc R U . . .
C1B C 0.29266(15) 0.58984(19) 0.3377(5) 0.0155(8) Uani 1 1 d . . . . .
C2B C 0.31095(14) 0.53148(19) 0.2786(5) 0.0168(8) Uani 1 1 d . . . . .
O2B O 0.28518(10) 0.48425(13) 0.2191(3) 0.0168(6) Uani 1 1 d . . . . .
C3B C 0.35871(15) 0.5241(2) 0.2791(5) 0.0201(9) Uani 1 1 d . . . . .
H3B H 0.3712 0.4843 0.2433 0.024 Uiso 1 1 calc R U . . .
C4B C 0.38715(16) 0.5723(2) 0.3294(5) 0.0199(9) Uani 1 1 d . . . . .
H4B H 0.4188 0.5661 0.3239 0.024 Uiso 1 1 calc R U . . .
C5B C 0.39846(17) 0.6814(2) 0.4516(6) 0.0253(10) Uani 1 1 d . . . . .
H5B H 0.4302 0.6759 0.4458 0.030 Uiso 1 1 calc R U . . .
C6B C 0.38072(18) 0.7372(2) 0.5194(6) 0.0311(12) Uani 1 1 d . . . . .
H6B H 0.4002 0.7702 0.5603 0.037 Uiso 1 1 calc R U . . .
C7B C 0.33407(16) 0.7451(2) 0.5280(6) 0.0247(10) Uani 1 1 d . . . . .
H7B H 0.3220 0.7837 0.5746 0.030 Uiso 1 1 calc R U . . .
C8B C 0.30534(16) 0.6983(2) 0.4705(5) 0.0209(9) Uani 1 1 d . . . . .
H8B H 0.2737 0.7047 0.4796 0.025 Uiso 1 1 calc R U . . .
C9B C 0.32227(17) 0.6399(2) 0.3970(5) 0.0220(9) Uani 1 1 d . . . . .
C10B C 0.36948(16) 0.6320(2) 0.3901(5) 0.0199(9) Uani 1 1 d . . . . .
O1 O 0.21468(11) 0.42099(16) 0.1049(4) 0.0262(7) Uani 1 1 d . . . . .
C1 C 0.17848(19) 0.3843(2) 0.0436(7) 0.0366(13) Uani 1 1 d . . . . .
H1A H 0.1654 0.4042 -0.0642 0.055 Uiso 1 1 calc R U . . .
H1B H 0.1555 0.3815 0.1386 0.055 Uiso 1 1 calc R U . . .
H1C H 0.1891 0.3413 0.0132 0.055 Uiso 1 1 calc R U . . .
O2 O 0.2542(2) 0.3317(3) 0.2925(7) 0.0186(12) Uani 0.5 1 d . . P A -1
H2 H 0.2784 0.3375 0.2355 0.028 Uiso 0.5 1 d R U P A -1
C2 C 0.2533(4) 0.2682(4) 0.3627(12) 0.023(2) Uani 0.5 1 d . . P A -1
H2A H 0.2828 0.2577 0.4143 0.035 Uiso 0.5 1 calc R U P A -1
H2B H 0.2463 0.2382 0.2650 0.035 Uiso 0.5 1 calc R U P A -1
H2C H 0.2302 0.2651 0.4570 0.035 Uiso 0.5 1 calc R U P A -1
O3 O 0.0051(3) 0.4046(4) -0.0127(12) 0.045(2) Uani 0.5 1 d . . P B 2
H3 H -0.0013 0.3797 -0.0979 0.068 Uiso 0.5 1 calc R U P B 2
C3 C 0.0517(5) 0.4011(8) 0.0236(18) 0.050(4) Uani 0.5 1 d . . P B 2
H3C H 0.0680 0.3903 -0.0877 0.075 Uiso 0.5 1 calc R U P B 2
H3D H 0.0573 0.3682 0.1150 0.075 Uiso 0.5 1 calc R U P B 2
H3E H 0.0623 0.4425 0.0687 0.075 Uiso 0.5 1 calc R U P B 2
O4 O 0.0124(3) 0.4752(4) 0.1447(11) 0.058(2) Uani 0.5 1 d . . P C 3
H4 H 0.0062 0.5111 0.1006 0.087 Uiso 0.5 1 calc R U P C 3
C4 C 0.0291(6) 0.4350(8) 0.008(2) 0.073(5) Uani 0.5 1 d . . P C 3
H4C H 0.0611 0.4444 -0.0126 0.109 Uiso 0.5 1 calc R U P C 3
H4D H 0.0122 0.4423 -0.1039 0.109 Uiso 0.5 1 calc R U P C 3
H4E H 0.0258 0.3904 0.0452 0.109 Uiso 0.5 1 calc R U P C 3


_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
Gd O2A 2.280(3) . ?
Gd O1 2.311(3) 8_656 ?
Gd O1 2.332(3) . ?
Gd O2B 2.406(3) . ?
Gd O2B 2.465(3) 8_656 ?
Gd N1A 2.519(4) . ?
Gd N1B 2.532(3) . ?
Gd O2 2.624(5) . ?
Gd Gd 3.9548(9) 8_656 ?
Gd Gd 3.9549(9) 8_655 ?
O2A C2A 1.287(5) . ?
C1A C2A 1.417(6) . ?
C1A C11A 1.445(6) . ?
C1A C9A 1.455(6) . ?
C2A C3A 1.441(6) . ?
C3A C4A 1.339(6) . ?
C3A H3A 0.9500 . ?
C4A C10A 1.415(7) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.359(7) . ?
C5A C10A 1.419(6) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.409(7) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.372(7) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.424(7) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.418(6) . ?
C11A N1A 1.292(5) . ?
C11A H11A 0.9500 . ?
N1A C12A 1.465(5) . ?
C12A C12B 1.509(6) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C12B N1B 1.466(6) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
N1B C11B 1.280(5) . ?
C11B C1B 1.452(6) . ?
C11B H11B 0.9500 . ?
C1B C2B 1.408(6) . ?
C1B C9B 1.436(6) . ?
C2B O2B 1.326(5) . ?
C2B C3B 1.425(6) . ?
O2B Gd 2.465(3) 8_655 ?
C3B C4B 1.369(6) . ?
C3B H3B 0.9500 . ?
C4B C10B 1.429(6) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.377(7) . ?
C5B C10B 1.420(6) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.395(7) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.367(6) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.431(6) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.411(7) . ?
O1 C1 1.397(5) . ?
O1 Gd 2.311(3) 8_655 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O2 C2 1.430(9) . ?
O2 H2 0.8400 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C3 1.411(16) . ?
O3 H3 0.8400 . ?
C3 H3C 0.9800 . ?
C3 H3D 0.9800 . ?
C3 H3E 0.9800 . ?
O4 C4 1.407(19) . ?
O4 H4 0.8400 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Gd O1 92.95(12) . 8_656 ?
O2A Gd O1 96.68(11) . . ?
O1 Gd O1 132.50(9) 8_656 . ?
O2A Gd O2B 152.27(10) . . ?
O1 Gd O2B 83.63(11) 8_656 . ?
O1 Gd O2B 67.00(10) . . ?
O2A Gd O2B 81.45(10) . 8_656 ?
O1 Gd O2B 66.33(9) 8_656 8_656 ?
O1 Gd O2B 161.14(11) . 8_656 ?
O2B Gd O2B 121.29(9) . 8_656 ?
O2A Gd N1A 71.23(11) . . ?
O1 Gd N1A 148.55(10) 8_656 . ?
O1 Gd N1A 77.54(11) . . ?
O2B Gd N1A 122.89(10) . . ?
O2B Gd N1A 84.14(10) 8_656 . ?
O2A Gd N1B 134.32(11) . . ?
O1 Gd N1B 113.81(12) 8_656 . ?
O1 Gd N1B 91.44(12) . . ?
O2B Gd N1B 70.74(11) . . ?
O2B Gd N1B 77.09(10) 8_656 . ?
N1A Gd N1B 66.87(12) . . ?
O2A Gd O2 68.44(15) . . ?
O1 Gd O2 77.90(14) 8_656 . ?
O1 Gd O2 63.16(14) . . ?
O2B Gd O2 83.98(14) . . ?
O2B Gd O2 131.53(13) 8_656 . ?
N1A Gd O2 118.12(15) . . ?
N1B Gd O2 149.98(14) . . ?
O2A Gd Gd 82.14(7) . 8_656 ?
O1 Gd Gd 31.76(7) 8_656 8_656 ?
O1 Gd Gd 163.43(9) . 8_656 ?
O2B Gd Gd 107.01(7) . 8_656 ?
O2B Gd Gd 35.23(6) 8_656 8_656 ?
N1A Gd Gd 117.19(7) . 8_656 ?
N1B Gd Gd 101.22(8) . 8_656 ?
O2 Gd Gd 101.47(12) . 8_656 ?
O2A Gd Gd 122.29(7) . 8_655 ?
O1 Gd Gd 108.27(8) 8_656 8_655 ?
O1 Gd Gd 31.44(8) . 8_655 ?
O2B Gd Gd 36.22(6) . 8_655 ?
O2B Gd Gd 156.25(7) 8_656 8_655 ?
N1A Gd Gd 103.13(7) . 8_655 ?
N1B Gd Gd 84.98(8) . 8_655 ?
O2 Gd Gd 65.00(12) . 8_655 ?
Gd Gd Gd 138.453(17) 8_656 8_655 ?
C2A O2A Gd 142.7(3) . . ?
C2A C1A C11A 121.5(4) . . ?
C2A C1A C9A 119.9(4) . . ?
C11A C1A C9A 118.7(4) . . ?
O2A C2A C1A 124.6(4) . . ?
O2A C2A C3A 117.8(4) . . ?
C1A C2A C3A 117.6(4) . . ?
C4A C3A C2A 122.7(4) . . ?
C4A C3A H3A 118.7 . . ?
C2A C3A H3A 118.7 . . ?
C3A C4A C10A 121.2(4) . . ?
C3A C4A H4A 119.4 . . ?
C10A C4A H4A 119.4 . . ?
C6A C5A C10A 121.2(5) . . ?
C6A C5A H5A 119.4 . . ?
C10A C5A H5A 119.4 . . ?
C5A C6A C7A 119.5(5) . . ?
C5A C6A H6A 120.2 . . ?
C7A C6A H6A 120.2 . . ?
C8A C7A C6A 120.7(5) . . ?
C8A C7A H7A 119.7 . . ?
C6A C7A H7A 119.7 . . ?
C7A C8A C9A 121.4(5) . . ?
C7A C8A H8A 119.3 . . ?
C9A C8A H8A 119.3 . . ?
C10A C9A C8A 117.2(4) . . ?
C10A C9A C1A 119.1(4) . . ?
C8A C9A C1A 123.7(4) . . ?
C4A C10A C9A 119.5(4) . . ?
C4A C10A C5A 120.5(4) . . ?
C9A C10A C5A 120.0(5) . . ?
N1A C11A C1A 127.2(4) . . ?
N1A C11A H11A 116.4 . . ?
C1A C11A H11A 116.4 . . ?
C11A N1A C12A 116.1(4) . . ?
C11A N1A Gd 131.9(3) . . ?
C12A N1A Gd 111.6(3) . . ?
N1A C12A C12B 109.6(3) . . ?
N1A C12A H12A 109.8 . . ?
C12B C12A H12A 109.8 . . ?
N1A C12A H12B 109.8 . . ?
C12B C12A H12B 109.8 . . ?
H12A C12A H12B 108.2 . . ?
N1B C12B C12A 108.4(4) . . ?
N1B C12B H12C 110.0 . . ?
C12A C12B H12C 110.0 . . ?
N1B C12B H12D 110.0 . . ?
C12A C12B H12D 110.0 . . ?
H12C C12B H12D 108.4 . . ?
C11B N1B C12B 117.8(4) . . ?
C11B N1B Gd 125.2(3) . . ?
C12B N1B Gd 116.9(2) . . ?
N1B C11B C1B 125.5(4) . . ?
N1B C11B H11B 117.3 . . ?
C1B C11B H11B 117.3 . . ?
C2B C1B C9B 119.6(4) . . ?
C2B C1B C11B 121.8(4) . . ?
C9B C1B C11B 118.5(4) . . ?
O2B C2B C1B 122.0(4) . . ?
O2B C2B C3B 119.5(4) . . ?
C1B C2B C3B 118.5(4) . . ?
C2B O2B Gd 119.4(2) . . ?
C2B O2B Gd 130.5(2) . 8_655 ?
Gd O2B Gd 108.55(11) . 8_655 ?
C4B C3B C2B 122.2(4) . . ?
C4B C3B H3B 118.9 . . ?
C2B C3B H3B 118.9 . . ?
C3B C4B C10B 120.4(4) . . ?
C3B C4B H4B 119.8 . . ?
C10B C4B H4B 119.8 . . ?
C6B C5B C10B 120.3(5) . . ?
C6B C5B H5B 119.9 . . ?
C10B C5B H5B 119.9 . . ?
C5B C6B C7B 119.8(4) . . ?
C5B C6B H6B 120.1 . . ?
C7B C6B H6B 120.1 . . ?
C8B C7B C6B 121.3(5) . . ?
C8B C7B H7B 119.4 . . ?
C6B C7B H7B 119.4 . . ?
C7B C8B C9B 120.9(4) . . ?
C7B C8B H8B 119.6 . . ?
C9B C8B H8B 119.6 . . ?
C10B C9B C8B 117.5(4) . . ?
C10B C9B C1B 120.7(4) . . ?
C8B C9B C1B 121.8(4) . . ?
C9B C10B C5B 120.3(4) . . ?
C9B C10B C4B 118.5(4) . . ?
C5B C10B C4B 121.1(4) . . ?
C1 O1 Gd 119.3(3) . 8_655 ?
C1 O1 Gd 122.5(3) . . ?
Gd O1 Gd 116.81(13) 8_655 . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 O2 Gd 134.5(5) . . ?
C2 O2 H2 109.4 . . ?
Gd O2 H2 107.9 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 O3 H3 109.5 . . ?
O3 C3 H3C 109.5 . . ?
O3 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
O3 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
C4 O4 H4 109.5 . . ?
O4 C4 H4C 109.5 . . ?
O4 C4 H4D 109.5 . . ?
H4C C4 H4D 109.5 . . ?
O4 C4 H4E 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd O2A C2A C1A 12.0(7) . . . . ?
Gd O2A C2A C3A -168.8(3) . . . . ?
C11A C1A C2A O2A -1.6(6) . . . . ?
C9A C1A C2A O2A 178.6(4) . . . . ?
C11A C1A C2A C3A 179.3(4) . . . . ?
C9A C1A C2A C3A -0.6(5) . . . . ?
O2A C2A C3A C4A -179.4(4) . . . . ?
C1A C2A C3A C4A -0.2(6) . . . . ?
C2A C3A C4A C10A -0.1(7) . . . . ?
C10A C5A C6A C7A 0.8(7) . . . . ?
C5A C6A C7A C8A -1.1(8) . . . . ?
C6A C7A C8A C9A -0.3(7) . . . . ?
C7A C8A C9A C10A 1.9(7) . . . . ?
C7A C8A C9A C1A -178.5(4) . . . . ?
C2A C1A C9A C10A 1.5(6) . . . . ?
C11A C1A C9A C10A -178.3(4) . . . . ?
C2A C1A C9A C8A -178.0(4) . . . . ?
C11A C1A C9A C8A 2.1(6) . . . . ?
C3A C4A C10A C9A 1.1(7) . . . . ?
C3A C4A C10A C5A -178.9(4) . . . . ?
C8A C9A C10A C4A 177.8(4) . . . . ?
C1A C9A C10A C4A -1.7(6) . . . . ?
C8A C9A C10A C5A -2.2(6) . . . . ?
C1A C9A C10A C5A 178.3(4) . . . . ?
C6A C5A C10A C4A -179.1(4) . . . . ?
C6A C5A C10A C9A 0.9(7) . . . . ?
C2A C1A C11A N1A -7.0(6) . . . . ?
C9A C1A C11A N1A 172.8(4) . . . . ?
C1A C11A N1A C12A 179.3(4) . . . . ?
C1A C11A N1A Gd 7.1(6) . . . . ?
C11A N1A C12A C12B 133.1(4) . . . . ?
Gd N1A C12A C12B -53.1(4) . . . . ?
N1A C12A C12B N1B 55.8(4) . . . . ?
C12A C12B N1B C11B 143.7(4) . . . . ?
C12A C12B N1B Gd -32.2(4) . . . . ?
C12B N1B C11B C1B -179.6(4) . . . . ?
Gd N1B C11B C1B -4.1(6) . . . . ?
N1B C11B C1B C2B 34.7(6) . . . . ?
N1B C11B C1B C9B -148.5(4) . . . . ?
C9B C1B C2B O2B -178.6(3) . . . . ?
C11B C1B C2B O2B -1.8(6) . . . . ?
C9B C1B C2B C3B -0.2(5) . . . . ?
C11B C1B C2B C3B 176.6(3) . . . . ?
C1B C2B O2B Gd -56.3(4) . . . . ?
C3B C2B O2B Gd 125.3(3) . . . . ?
C1B C2B O2B Gd 107.6(4) . . . 8_655 ?
C3B C2B O2B Gd -70.8(4) . . . 8_655 ?
O2B C2B C3B C4B 176.3(3) . . . . ?
C1B C2B C3B C4B -2.1(6) . . . . ?
C2B C3B C4B C10B 2.2(6) . . . . ?
C10B C5B C6B C7B 0.1(6) . . . . ?
C5B C6B C7B C8B 0.2(7) . . . . ?
C6B C7B C8B C9B -1.0(6) . . . . ?
C7B C8B C9B C10B 1.4(6) . . . . ?
C7B C8B C9B C1B 179.3(4) . . . . ?
C2B C1B C9B C10B 2.4(5) . . . . ?
C11B C1B C9B C10B -174.4(3) . . . . ?
C2B C1B C9B C8B -175.4(4) . . . . ?
C11B C1B C9B C8B 7.8(6) . . . . ?
C8B C9B C10B C5B -1.1(5) . . . . ?
C1B C9B C10B C5B -179.0(4) . . . . ?
C8B C9B C10B C4B 175.6(4) . . . . ?
C1B C9B C10B C4B -2.3(5) . . . . ?
C6B C5B C10B C9B 0.4(6) . . . . ?
C6B C5B C10B C4B -176.2(4) . . . . ?
C3B C4B C10B C9B 0.0(6) . . . . ?
C3B C4B C10B C5B 176.7(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
C11A H11A O4 0.95 2.62 3.510(10) 156.0 .
C1 H1C O2 0.98 2.35 2.940(8) 117.9 8_655
C4 H4D O4 0.98 1.90 2.52(2) 118.2 5_565
O2 H2 O2A 0.84 2.02 2.804(6) 155.7 8_655

_refine_diff_density_max         0.991
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.142

_shelxl_version_number           2013-2
####################################################################### 
# 
# 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_at2854ra
_database_code_depnum_ccdc_archive 'CCDC 1505018'
_audit_update_record             
;
2016-09-19 deposited with the CCDC.
2016-10-25 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         'C25.50 H21.50 N2 O3.50 Tb'
_chemical_formula_sum            'C25.50 H21.50 N2 O3.50 Tb'
_chemical_formula_weight         570.87

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.270(8)
_cell_length_b                   26.500(9)
_cell_length_c                   7.373(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4351(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1737
_cell_measurement_theta_min      2.85
_cell_measurement_theta_max      31.61

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_F_000             2252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    3.284
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur R with Ruby CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18244
_diffrn_reflns_av_unetI/netI     0.1894
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.850
_diffrn_reflns_theta_max         31.609
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6760
_reflns_number_gt                3486
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6760
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1861
_refine_ls_R_factor_gt           0.0890
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Tb Tb 0.78089(2) -0.09506(2) 0.06017(5) 0.01691(11) Uani 1 1 d . . . . .
O2A O 0.8384(3) -0.1588(2) -0.0470(8) 0.0210(14) Uani 1 1 d . . . . .
N1A N 0.8894(3) -0.0714(3) 0.0997(8) 0.0155(16) Uani 1 1 d . . . . .
C1A C 0.9449(3) -0.1456(3) -0.0141(9) 0.0069(16) Uiso 1 1 d . . . . .
C2A C 0.8939(4) -0.1735(3) -0.0683(11) 0.0181(19) Uani 1 1 d . . . . .
C3A C 0.9034(4) -0.2211(4) -0.1531(11) 0.022(2) Uani 1 1 d . . . . .
H3A H 0.8698 -0.2399 -0.1947 0.026 Uiso 1 1 calc R U . . .
C4A C 0.9591(4) -0.2400(3) -0.1755(11) 0.022(2) Uani 1 1 d . . . . .
H4A H 0.9633 -0.2718 -0.2329 0.027 Uiso 1 1 calc R U . . .
C5A C 1.0686(4) -0.2351(4) -0.1429(11) 0.024(2) Uani 1 1 d . . . . .
H5A H 1.0725 -0.2668 -0.2022 0.029 Uiso 1 1 calc R U . . .
C6A C 1.1195(4) -0.2113(4) -0.0851(11) 0.023(2) Uani 1 1 d . . . . .
H6A H 1.1577 -0.2268 -0.0974 0.028 Uiso 1 1 calc R U . . .
C7A C 1.1139(4) -0.1628(4) -0.0063(11) 0.027(2) Uani 1 1 d . . . . .
H7A H 1.1487 -0.1449 0.0317 0.032 Uiso 1 1 calc R U . . .
C8A C 1.0582(4) -0.1417(4) 0.0150(10) 0.018(2) Uani 1 1 d . . . . .
H8A H 1.0554 -0.1091 0.0680 0.021 Uiso 1 1 calc R U . . .
C9A C 1.0051(4) -0.1661(4) -0.0378(10) 0.0167(19) Uani 1 1 d . . . . .
C10A C 1.0105(4) -0.2150(4) -0.1188(10) 0.016(2) Uani 1 1 d . . . . .
C11A C 0.9385(3) -0.0962(3) 0.0711(10) 0.0134(16) Uiso 1 1 d . . . . .
H11A H 0.9746 -0.0804 0.1101 0.016 Uiso 1 1 calc R U . . .
C12A C 0.8956(4) -0.0227(4) 0.1968(11) 0.018(2) Uani 1 1 d . . . . .
H12A H 0.9380 -0.0117 0.1927 0.022 Uiso 1 1 calc R U . . .
H12B H 0.8843 -0.0273 0.3256 0.022 Uiso 1 1 calc R U . . .
O2B O 0.7031(2) -0.0640(2) 0.2502(7) 0.0157(14) Uani 1 1 d . . . . .
N1B N 0.7941(3) -0.0009(3) 0.1073(8) 0.0196(18) Uani 1 1 d . . . . .
C1B C 0.6885(4) 0.0202(3) 0.1402(11) 0.0133(19) Uiso 1 1 d . . . . .
C2B C 0.6667(4) -0.0281(4) 0.1928(10) 0.018(2) Uani 1 1 d . . . . .
C3B C 0.6038(4) -0.0360(3) 0.1935(10) 0.0146(19) Uani 1 1 d . . . . .
H3B H 0.5886 -0.0682 0.2265 0.017 Uiso 1 1 calc R U . . .
C4B C 0.5648(4) 0.0011(3) 0.1483(10) 0.0160(19) Uiso 1 1 d . . . . .
H4B H 0.5230 -0.0060 0.1515 0.019 Uiso 1 1 calc R U . . .
C5B C 0.5435(4) 0.0877(4) 0.0437(11) 0.024(2) Uani 1 1 d . . . . .
H5B H 0.5016 0.0809 0.0455 0.029 Uiso 1 1 calc R U . . .
C6B C 0.5626(5) 0.1341(4) -0.0104(11) 0.029(3) Uani 1 1 d . . . . .
H6B H 0.5345 0.1591 -0.0464 0.035 Uiso 1 1 calc R U . . .
C7B C 0.6240(5) 0.1447(4) -0.0126(11) 0.026(2) Uani 1 1 d . . . . .
H7B H 0.6374 0.1772 -0.0486 0.032 Uiso 1 1 calc R U . . .
C8B C 0.6654(4) 0.1086(3) 0.0366(10) 0.018(2) Uani 1 1 d . . . . .
H8B H 0.7070 0.1164 0.0318 0.022 Uiso 1 1 calc R U . . .
C9B C 0.6469(4) 0.0592(3) 0.0950(9) 0.0153(19) Uani 1 1 d . . . . .
C10B C 0.5836(4) 0.0496(3) 0.0969(10) 0.0160(19) Uiso 1 1 d . . . . .
C11B C 0.7520(4) 0.0317(4) 0.1420(10) 0.017(2) Uani 1 1 d . . . . .
H20A H 0.7638 0.0653 0.1704 0.021 Uiso 1 1 calc R U . . .
C12B C 0.8566(4) 0.0171(3) 0.1136(10) 0.0142(19) Uani 1 1 d . . . . .
H12C H 0.8590 0.0484 0.1864 0.017 Uiso 1 1 calc R U . . .
H12D H 0.8708 0.0248 -0.0106 0.017 Uiso 1 1 calc R U . . .
O1 O 0.7981(3) -0.1123(3) 0.3657(7) 0.0259(17) Uani 1 1 d . . . . .
C1 C 0.8469(4) -0.1423(4) 0.4242(13) 0.036(3) Uiso 1 1 d . . . . .
H1A H 0.8759 -0.1459 0.3250 0.054 Uiso 0.5 1 calc R U P . .
H1B H 0.8323 -0.1756 0.4604 0.054 Uiso 0.5 1 calc R U P . .
H1C H 0.8665 -0.1260 0.5279 0.054 Uiso 0.5 1 calc R U P . .
O2 O 0.7424(6) -0.1828(5) 0.1775(16) 0.028(3) Uani 0.5 1 d . . P A -1
H2 H 0.7264 -0.1691 0.2650 0.034 Uiso 0.5 1 d R U P A -1
C2 C 0.7460(13) -0.2325(8) 0.123(3) 0.046(7) Uani 0.5 1 d . . P A -1
H2A H 0.7067 -0.2435 0.0775 0.069 Uiso 0.5 1 calc R U P A -1
H2B H 0.7576 -0.2536 0.2264 0.069 Uiso 0.5 1 calc R U P A -1
H2C H 0.7760 -0.2358 0.0266 0.069 Uiso 0.5 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb O2A 2.261(6) . ?
Tb O1 2.315(5) 7_755 ?
Tb O1 2.331(5) . ?
Tb O2B 2.375(5) . ?
Tb O2B 2.455(5) 7_755 ?
Tb N1A 2.513(7) . ?
Tb N1B 2.536(8) . ?
Tb O2 2.625(12) . ?
Tb Tb 3.9349(14) 7_756 ?
Tb Tb 3.9349(14) 7_755 ?
O2A C2A 1.305(10) . ?
N1A C11A 1.294(10) . ?
N1A C12A 1.481(11) . ?
C1A C2A 1.414(11) . ?
C1A C9A 1.456(10) . ?
C1A C11A 1.459(11) . ?
C2A C3A 1.423(12) . ?
C3A C4A 1.348(12) . ?
C3A H3A 0.9500 . ?
C4A C10A 1.387(12) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.366(12) . ?
C5A C10A 1.410(11) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.415(13) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.370(12) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.403(11) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.431(12) . ?
C11A H11A 0.9500 . ?
C12A C12B 1.497(11) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
O2B C2B 1.320(10) . ?
O2B Tb 2.455(5) 7_756 ?
N1B C11B 1.301(10) . ?
N1B C12B 1.473(10) . ?
C1B C2B 1.423(12) . ?
C1B C9B 1.427(11) . ?
C1B C11B 1.448(10) . ?
C2B C3B 1.416(11) . ?
C3B C4B 1.353(11) . ?
C3B H3B 0.9500 . ?
C4B C10B 1.406(12) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.361(13) . ?
C5B C10B 1.405(12) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.394(12) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.378(12) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.438(12) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.432(11) . ?
C11B H20A 0.9500 . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
O1 C1 1.413(11) . ?
O1 Tb 2.315(5) 7_756 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O2 C2 1.38(2) . ?
O2 H2 0.8212 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Tb O1 93.8(2) . 7_755 ?
O2A Tb O1 95.6(2) . . ?
O1 Tb O1 133.2(2) 7_755 . ?
O2A Tb O2B 151.4(2) . . ?
O1 Tb O2B 83.1(2) 7_755 . ?
O1 Tb O2B 67.53(19) . . ?
O2A Tb O2B 81.0(2) . 7_755 ?
O1 Tb O2B 66.44(19) 7_755 7_755 ?
O1 Tb O2B 160.4(2) . 7_755 ?
O2B Tb O2B 122.6(2) . 7_755 ?
O2A Tb N1A 71.5(2) . . ?
O1 Tb N1A 148.40(19) 7_755 . ?
O1 Tb N1A 77.2(2) . . ?
O2B Tb N1A 123.1(2) . . ?
O2B Tb N1A 83.38(19) 7_755 . ?
O2A Tb N1B 135.8(2) . . ?
O1 Tb N1B 111.6(2) 7_755 . ?
O1 Tb N1B 92.4(2) . . ?
O2B Tb N1B 70.3(2) . . ?
O2B Tb N1B 77.3(2) 7_755 . ?
N1A Tb N1B 68.1(2) . . ?
O2A Tb O2 68.8(3) . . ?
O1 Tb O2 77.3(3) 7_755 . ?
O1 Tb O2 63.9(3) . . ?
O2B Tb O2 82.8(3) . . ?
O2B Tb O2 130.6(3) 7_755 . ?
N1A Tb O2 119.8(3) . . ?
N1B Tb O2 149.8(3) . . ?
O2A Tb Tb 121.68(14) . 7_756 ?
O1 Tb Tb 108.33(14) 7_755 7_756 ?
O1 Tb Tb 31.99(14) . 7_756 ?
O2B Tb Tb 36.13(13) . 7_756 ?
O2B Tb Tb 157.36(14) 7_755 7_756 ?
N1A Tb Tb 103.14(14) . 7_756 ?
N1B Tb Tb 84.96(14) . 7_756 ?
O2 Tb Tb 65.0(3) . 7_756 ?
O2A Tb Tb 82.57(14) . 7_755 ?
O1 Tb Tb 32.23(14) 7_755 7_755 ?
O1 Tb Tb 164.38(16) . 7_755 ?
O2B Tb Tb 107.31(13) . 7_755 ?
O2B Tb Tb 34.79(13) 7_755 7_755 ?
N1A Tb Tb 116.42(14) . 7_755 ?
N1B Tb Tb 99.73(14) . 7_755 ?
O2 Tb Tb 101.2(3) . 7_755 ?
Tb Tb Tb 139.07(3) 7_756 7_755 ?
C2A O2A Tb 143.3(6) . . ?
C11A N1A C12A 116.2(7) . . ?
C11A N1A Tb 131.8(6) . . ?
C12A N1A Tb 111.3(5) . . ?
C2A C1A C9A 120.7(8) . . ?
C2A C1A C11A 120.8(7) . . ?
C9A C1A C11A 118.5(7) . . ?
O2A C2A C1A 124.8(8) . . ?
O2A C2A C3A 117.3(8) . . ?
C1A C2A C3A 117.9(8) . . ?
C4A C3A C2A 121.3(9) . . ?
C4A C3A H3A 119.3 . . ?
C2A C3A H3A 119.3 . . ?
C3A C4A C10A 123.1(9) . . ?
C3A C4A H4A 118.5 . . ?
C10A C4A H4A 118.5 . . ?
C6A C5A C10A 123.1(9) . . ?
C6A C5A H5A 118.4 . . ?
C10A C5A H5A 118.4 . . ?
C5A C6A C7A 118.4(9) . . ?
C5A C6A H6A 120.8 . . ?
C7A C6A H6A 120.8 . . ?
C8A C7A C6A 119.7(9) . . ?
C8A C7A H7A 120.1 . . ?
C6A C7A H7A 120.1 . . ?
C7A C8A C9A 123.0(9) . . ?
C7A C8A H8A 118.5 . . ?
C9A C8A H8A 118.5 . . ?
C8A C9A C10A 117.5(8) . . ?
C8A C9A C1A 124.8(9) . . ?
C10A C9A C1A 117.7(8) . . ?
C4A C10A C5A 122.6(9) . . ?
C4A C10A C9A 119.2(8) . . ?
C5A C10A C9A 118.2(9) . . ?
N1A C11A C1A 127.5(8) . . ?
N1A C11A H11A 116.2 . . ?
C1A C11A H11A 116.2 . . ?
N1A C12A C12B 111.2(7) . . ?
N1A C12A H12A 109.4 . . ?
C12B C12A H12A 109.4 . . ?
N1A C12A H12B 109.4 . . ?
C12B C12A H12B 109.4 . . ?
H12A C12A H12B 108.0 . . ?
C2B O2B Tb 120.6(5) . . ?
C2B O2B Tb 129.0(5) . 7_756 ?
Tb O2B Tb 109.1(2) . 7_756 ?
C11B N1B C12B 117.3(8) . . ?
C11B N1B Tb 126.7(6) . . ?
C12B N1B Tb 115.6(5) . . ?
C2B C1B C9B 119.6(8) . . ?
C2B C1B C11B 121.4(8) . . ?
C9B C1B C11B 118.9(8) . . ?
O2B C2B C3B 120.0(8) . . ?
O2B C2B C1B 121.8(8) . . ?
C3B C2B C1B 118.2(8) . . ?
C4B C3B C2B 121.7(9) . . ?
C4B C3B H3B 119.1 . . ?
C2B C3B H3B 119.1 . . ?
C3B C4B C10B 122.7(8) . . ?
C3B C4B H4B 118.6 . . ?
C10B C4B H4B 118.6 . . ?
C6B C5B C10B 122.1(9) . . ?
C6B C5B H5B 118.9 . . ?
C10B C5B H5B 118.9 . . ?
C5B C6B C7B 119.5(9) . . ?
C5B C6B H6B 120.3 . . ?
C7B C6B H6B 120.3 . . ?
C8B C7B C6B 120.9(10) . . ?
C8B C7B H7B 119.5 . . ?
C6B C7B H7B 119.5 . . ?
C7B C8B C9B 121.2(9) . . ?
C7B C8B H8B 119.4 . . ?
C9B C8B H8B 119.4 . . ?
C1B C9B C10B 120.6(8) . . ?
C1B C9B C8B 122.8(8) . . ?
C10B C9B C8B 116.5(8) . . ?
C5B C10B C4B 123.0(8) . . ?
C5B C10B C9B 119.8(8) . . ?
C4B C10B C9B 117.2(8) . . ?
N1B C11B C1B 124.2(9) . . ?
N1B C11B H20A 117.9 . . ?
C1B C11B H20A 117.9 . . ?
N1B C12B C12A 109.4(7) . . ?
N1B C12B H12C 109.8 . . ?
C12A C12B H12C 109.8 . . ?
N1B C12B H12D 109.8 . . ?
C12A C12B H12D 109.8 . . ?
H12C C12B H12D 108.2 . . ?
C1 O1 Tb 120.4(5) . 7_756 ?
C1 O1 Tb 122.1(5) . . ?
Tb O1 Tb 115.8(2) 7_756 . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 O2 Tb 137.0(11) . . ?
C2 O2 H2 132.4 . . ?
Tb O2 H2 90.6 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb O2A C2A C1A 0.4(14) . . . . ?
Tb O2A C2A C3A -179.4(6) . . . . ?
C9A C1A C2A O2A 177.8(7) . . . . ?
C11A C1A C2A O2A -0.7(12) . . . . ?
C9A C1A C2A C3A -2.5(11) . . . . ?
C11A C1A C2A C3A 179.0(7) . . . . ?
O2A C2A C3A C4A -177.9(8) . . . . ?
C1A C2A C3A C4A 2.3(13) . . . . ?
C2A C3A C4A C10A 0.0(14) . . . . ?
C10A C5A C6A C7A -3.6(13) . . . . ?
C5A C6A C7A C8A 1.9(13) . . . . ?
C6A C7A C8A C9A 0.1(13) . . . . ?
C7A C8A C9A C10A -0.5(12) . . . . ?
C7A C8A C9A C1A 178.6(7) . . . . ?
C2A C1A C9A C8A -178.6(7) . . . . ?
C11A C1A C9A C8A -0.1(12) . . . . ?
C2A C1A C9A C10A 0.4(11) . . . . ?
C11A C1A C9A C10A 178.9(7) . . . . ?
C3A C4A C10A C5A 180.0(8) . . . . ?
C3A C4A C10A C9A -2.2(13) . . . . ?
C6A C5A C10A C4A -178.9(8) . . . . ?
C6A C5A C10A C9A 3.2(12) . . . . ?
C8A C9A C10A C4A -179.0(7) . . . . ?
C1A C9A C10A C4A 1.9(11) . . . . ?
C8A C9A C10A C5A -1.0(11) . . . . ?
C1A C9A C10A C5A 179.8(7) . . . . ?
C12A N1A C11A C1A 177.4(7) . . . . ?
Tb N1A C11A C1A 7.2(12) . . . . ?
C2A C1A C11A N1A -3.3(13) . . . . ?
C9A C1A C11A N1A 178.2(7) . . . . ?
C11A N1A C12A C12B 138.0(7) . . . . ?
Tb N1A C12A C12B -49.9(8) . . . . ?
Tb O2B C2B C3B 124.1(7) . . . . ?
Tb O2B C2B C3B -70.6(10) 7_756 . . . ?
Tb O2B C2B C1B -60.0(10) . . . . ?
Tb O2B C2B C1B 105.3(8) 7_756 . . . ?
C9B C1B C2B O2B -174.3(7) . . . . ?
C11B C1B C2B O2B 1.8(13) . . . . ?
C9B C1B C2B C3B 1.7(12) . . . . ?
C11B C1B C2B C3B 177.9(7) . . . . ?
O2B C2B C3B C4B 175.1(7) . . . . ?
C1B C2B C3B C4B -1.0(12) . . . . ?
C2B C3B C4B C10B 0.4(13) . . . . ?
C10B C5B C6B C7B -0.4(13) . . . . ?
C5B C6B C7B C8B 1.0(13) . . . . ?
C6B C7B C8B C9B -1.2(12) . . . . ?
C2B C1B C9B C10B -1.9(12) . . . . ?
C11B C1B C9B C10B -178.2(7) . . . . ?
C2B C1B C9B C8B -178.5(7) . . . . ?
C11B C1B C9B C8B 5.3(12) . . . . ?
C7B C8B C9B C1B 177.5(7) . . . . ?
C7B C8B C9B C10B 0.7(11) . . . . ?
C6B C5B C10B C4B -178.1(8) . . . . ?
C6B C5B C10B C9B 0.0(12) . . . . ?
C3B C4B C10B C5B 177.7(8) . . . . ?
C3B C4B C10B C9B -0.5(12) . . . . ?
C1B C9B C10B C5B -176.9(7) . . . . ?
C8B C9B C10B C5B -0.1(11) . . . . ?
C1B C9B C10B C4B 1.3(11) . . . . ?
C8B C9B C10B C4B 178.1(7) . . . . ?
C12B N1B C11B C1B 179.6(7) . . . . ?
Tb N1B C11B C1B -7.1(12) . . . . ?
C2B C1B C11B N1B 33.1(13) . . . . ?
C9B C1B C11B N1B -150.7(8) . . . . ?
C11B N1B C12B C12A 141.2(7) . . . . ?
Tb N1B C12B C12A -32.9(8) . . . . ?
N1A C12A C12B N1B 54.9(9) . . . . ?

_refine_diff_density_max         1.703
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.241

####################################################################### 
# 
# 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_at2856a
_database_code_depnum_ccdc_archive 'CCDC 1505019'
_audit_update_record             
;
2016-09-19 deposited with the CCDC.
2016-10-25 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         'C25.25 H22.75 N4.25 O3.25 Tb'
_chemical_formula_sum            'C25.25 H22.75 N4.25 O3.25 Tb'
_chemical_formula_weight         596.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.386(9)
_cell_length_b                   7.523(3)
_cell_length_c                   26.158(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4405(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2193
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      31.55

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_F_000             2360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    3.249
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur R with Ruby CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17678
_diffrn_reflns_av_unetI/netI     0.1536
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.961
_diffrn_reflns_theta_max         31.548
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6841
_reflns_number_gt                3839
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0043P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6841
_refine_ls_number_parameters     295
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0730
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Tb Tb 0.71931(2) 0.44652(4) 0.58753(2) 0.01057(8) Uani 1 1 d . . . . .
O2A O 0.66205(18) 0.5625(6) 0.65001(19) 0.0132(10) Uani 1 1 d . . . . .
C1A C 0.5567(3) 0.5094(8) 0.6406(3) 0.0126(16) Uani 1 1 d . . . . .
C2A C 0.6067(3) 0.5719(8) 0.6677(3) 0.0096(14) Uani 1 1 d . . . . .
C3A C 0.5972(3) 0.6468(8) 0.7164(3) 0.0179(17) Uani 1 1 d . . . . .
H3A H 0.6308 0.6914 0.7345 0.022 Uiso 1 1 calc R U . . .
C4A C 0.5426(3) 0.6588(8) 0.7389(3) 0.0198(18) Uani 1 1 d . . . . .
H4A H 0.5390 0.7079 0.7722 0.024 Uiso 1 1 calc R U . . .
C5A C 0.4344(3) 0.6095(8) 0.7364(3) 0.0223(19) Uani 1 1 d . . . . .
H5A H 0.4306 0.6599 0.7696 0.027 Uiso 1 1 calc R U . . .
C6A C 0.3850(3) 0.5475(9) 0.7114(3) 0.0227(18) Uani 1 1 d . . . . .
H6A H 0.3471 0.5542 0.7276 0.027 Uiso 1 1 calc R U . . .
C7A C 0.3893(3) 0.4738(8) 0.6621(3) 0.0213(19) Uani 1 1 d . . . . .
H7A H 0.3545 0.4332 0.6449 0.026 Uiso 1 1 calc R U . . .
C8A C 0.4441(3) 0.4611(9) 0.6391(3) 0.0186(17) Uani 1 1 d . . . . .
H8A H 0.4466 0.4110 0.6058 0.022 Uiso 1 1 calc R U . . .
C9A C 0.4976(3) 0.5202(7) 0.6632(3) 0.0157(17) Uani 1 1 d . . . . .
C10A C 0.4910(3) 0.5983(7) 0.7127(3) 0.0163(17) Uani 1 1 d . . . . .
C11A C 0.5635(3) 0.4295(7) 0.5897(3) 0.0142(14) Uani 1 1 d . . . . .
H11A H 0.5278 0.3875 0.5743 0.017 Uiso 1 1 calc R U . . .
N1A N 0.6119(2) 0.4087(6) 0.5631(2) 0.0113(13) Uani 1 1 d . . . . .
C12A C 0.6041(3) 0.3142(8) 0.5137(3) 0.0124(16) Uani 1 1 d . . . . .
H12A H 0.5620 0.3234 0.5024 0.015 Uiso 1 1 calc R U . . .
H12B H 0.6139 0.1868 0.5180 0.015 Uiso 1 1 calc R U . . .
C12B C 0.6445(3) 0.3953(8) 0.4738(3) 0.0126(16) Uani 1 1 d . . . . .
H12C H 0.6425 0.3249 0.4419 0.015 Uiso 1 1 calc R U . . .
H12D H 0.6313 0.5180 0.4661 0.015 Uiso 1 1 calc R U . . .
N1B N 0.7060(2) 0.3979(6) 0.4931(2) 0.0124(13) Uani 1 1 d . . . . .
C11B C 0.7470(3) 0.3656(7) 0.4607(3) 0.0137(16) Uani 1 1 d . . . . .
H11B H 0.7356 0.3395 0.4265 0.016 Uiso 1 1 calc R U . . .
O2B O 0.79440(19) 0.2523(5) 0.5573(2) 0.0143(11) Uani 1 1 d . . . . .
C1B C 0.8107(3) 0.3665(8) 0.4730(3) 0.0134(16) Uani 1 1 d . . . . .
C2B C 0.8319(3) 0.3090(8) 0.5212(3) 0.0110(15) Uiso 1 1 d . . . . .
C3B C 0.8941(3) 0.3091(7) 0.5315(3) 0.0120(15) Uiso 1 1 d . . . . .
H3B H 0.9081 0.2747 0.5643 0.014 Uiso 1 1 calc R U . . .
C4B C 0.9335(3) 0.3579(8) 0.4948(3) 0.0168(18) Uani 1 1 d . . . . .
H4B H 0.9750 0.3536 0.5025 0.020 Uiso 1 1 calc R U . . .
C5B C 0.9568(3) 0.4748(8) 0.4077(4) 0.0230(19) Uani 1 1 d . . . . .
H5B H 0.9982 0.4730 0.4155 0.028 Uiso 1 1 calc R U . . .
C6B C 0.9395(4) 0.5334(9) 0.3613(4) 0.030(2) Uani 1 1 d . . . . .
H6B H 0.9682 0.5726 0.3370 0.036 Uiso 1 1 calc R U . . .
C7B C 0.8779(4) 0.5357(9) 0.3494(3) 0.026(2) Uani 1 1 d . . . . .
H7B H 0.8652 0.5738 0.3165 0.032 Uiso 1 1 calc R U . . .
C8B C 0.8359(4) 0.4831(8) 0.3850(3) 0.0213(18) Uani 1 1 d . . . . .
H8B H 0.7946 0.4892 0.3766 0.026 Uiso 1 1 calc R U . . .
C9B C 0.8536(3) 0.4199(8) 0.4340(3) 0.0183(17) Uani 1 1 d . . . . .
C10B C 0.9157(3) 0.4156(7) 0.4452(3) 0.0170(17) Uani 1 1 d . . . . .
N1 N 0.6950(6) 0.1343(18) 0.6008(5) 0.0062(15) Uiso 0.75 1 d . . P A 1
N2 N 0.6467(5) 0.0859(18) 0.6196(4) 0.0140(17) Uiso 0.75 1 d . . P A 1
N3 N 0.6016(4) 0.0408(10) 0.6372(4) 0.025(2) Uani 0.75 1 d . . P A 1
O2 O 0.6897(13) 0.132(4) 0.5939(12) 0.0062(15) Uiso 0.25 1 d D . P A 2
C2 C 0.6427(18) 0.087(7) 0.6285(16) 0.0140(17) Uiso 0.25 1 d D . P A 2
H2A H 0.6345 0.1718 0.6565 0.021 Uiso 0.25 1 d R U P A 2
H2B H 0.6451 -0.0345 0.6424 0.021 Uiso 0.25 1 d R U P A 2
H2C H 0.6104 0.0938 0.6031 0.021 Uiso 0.25 1 d R U P A 2
O1 O 0.7667(2) 0.3478(5) 0.6702(2) 0.0163(12) Uani 1 1 d . . . . .
H1 H 0.7929 0.2641 0.6663 0.024 Uiso 1 1 d R U . . .
C1 C 0.7334(3) 0.2886(8) 0.7141(3) 0.0217(19) Uani 1 1 d . . . . .
H1A H 0.7000 0.3702 0.7203 0.033 Uiso 1 1 calc R U . . .
H1B H 0.7596 0.2867 0.7441 0.033 Uiso 1 1 calc R U . . .
H1C H 0.7179 0.1688 0.7078 0.033 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb O2A 2.253(5) . ?
Tb O2B 2.363(4) . ?
Tb N1 2.407(14) 8_765 ?
Tb N1 2.436(14) . ?
Tb O2B 2.452(4) 8_765 ?
Tb O2 2.46(3) . ?
Tb O2 2.47(3) 8_765 ?
Tb N1A 2.504(6) . ?
Tb N1B 2.516(6) . ?
Tb O1 2.520(5) . ?
Tb Tb 4.0046(14) 8_755 ?
Tb Tb 4.0046(14) 8_765 ?
O2A C2A 1.324(7) . ?
C1A C2A 1.407(9) . ?
C1A C9A 1.452(9) . ?
C1A C11A 1.467(10) . ?
C2A C3A 1.410(10) . ?
C3A C4A 1.359(9) . ?
C3A H3A 0.9500 . ?
C4A C10A 1.418(10) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.367(10) . ?
C5A C10A 1.413(10) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.407(11) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.370(9) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.423(9) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.431(11) . ?
C11A N1A 1.298(8) . ?
C11A H11A 0.9500 . ?
N1A C12A 1.485(9) . ?
C12A C12B 1.510(9) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C12B N1B 1.465(8) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
N1B C11B 1.272(9) . ?
C11B C1B 1.462(9) . ?
C11B H11B 0.9500 . ?
O2B C2B 1.334(8) . ?
O2B Tb 2.452(4) 8_755 ?
C1B C2B 1.417(10) . ?
C1B C9B 1.457(10) . ?
C2B C3B 1.417(9) . ?
C3B C4B 1.355(10) . ?
C3B H3B 0.9500 . ?
C4B C10B 1.425(11) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.348(12) . ?
C5B C10B 1.417(10) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.414(10) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.381(10) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.424(10) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.422(10) . ?
N1 N2 1.242(13) . ?
N1 Tb 2.407(13) 8_755 ?
N2 N3 1.160(13) . ?
O2 C2 1.426(19) . ?
O2 Tb 2.47(3) 8_755 ?
C2 H2A 0.9866 . ?
C2 H2B 0.9878 . ?
C2 H2C 0.9853 . ?
O1 C1 1.441(8) . ?
O1 H1 0.8659 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Tb O2B 152.47(18) . . ?
O2A Tb N1 97.0(3) . 8_765 ?
O2B Tb N1 81.1(3) . 8_765 ?
O2A Tb N1 98.2(3) . . ?
O2B Tb N1 67.1(3) . . ?
N1 Tb N1 136.3(4) 8_765 . ?
O2A Tb O2B 78.41(16) . 8_765 ?
O2B Tb O2B 124.16(18) . 8_765 ?
N1 Tb O2B 66.1(3) 8_765 8_765 ?
N1 Tb O2B 157.3(3) . 8_765 ?
O2A Tb O2 99.8(7) . . ?
O2B Tb O2 67.7(7) . . ?
O2B Tb O2 152.8(8) 8_765 . ?
O2A Tb O2 101.6(8) . 8_765 ?
O2B Tb O2 77.6(8) . 8_765 ?
O2B Tb O2 66.2(7) 8_765 8_765 ?
O2 Tb O2 139.3(9) . 8_765 ?
O2A Tb N1A 71.54(18) . . ?
O2B Tb N1A 121.82(16) . . ?
N1 Tb N1A 150.3(3) 8_765 . ?
N1 Tb N1A 73.3(3) . . ?
O2B Tb N1A 84.49(15) 8_765 . ?
O2 Tb N1A 69.5(7) . . ?
O2 Tb N1A 150.7(7) 8_765 . ?
O2A Tb N1B 134.56(17) . . ?
O2B Tb N1B 70.47(17) . . ?
N1 Tb N1B 108.8(3) 8_765 . ?
N1 Tb N1B 88.5(3) . . ?
O2B Tb N1B 78.77(17) 8_765 . ?
O2 Tb N1B 84.0(8) . . ?
O2 Tb N1B 104.2(7) 8_765 . ?
N1A Tb N1B 67.58(19) . . ?
O2A Tb O1 74.42(16) . . ?
O2B Tb O1 78.76(16) . . ?
N1 Tb O1 73.4(3) 8_765 . ?
N1 Tb O1 71.8(3) . . ?
O2B Tb O1 127.28(15) 8_765 . ?
O2 Tb O1 76.8(8) . . ?
O2 Tb O1 76.2(7) 8_765 . ?
N1A Tb O1 126.16(17) . . ?
N1B Tb O1 148.16(15) . . ?
O2A Tb Tb 123.99(12) . 8_755 ?
O2B Tb Tb 34.43(11) . 8_755 ?
N1 Tb Tb 106.1(3) 8_765 8_755 ?
N1 Tb Tb 34.0(3) . 8_755 ?
O2B Tb Tb 157.57(12) 8_765 8_755 ?
O2 Tb Tb 35.9(7) . 8_755 ?
O2 Tb Tb 104.3(7) 8_765 8_755 ?
N1A Tb Tb 102.87(10) . 8_755 ?
N1B Tb Tb 84.48(11) . 8_755 ?
O1 Tb Tb 65.08(9) . 8_755 ?
O2A Tb Tb 80.29(11) . 8_765 ?
O2B Tb Tb 109.67(10) . 8_765 ?
N1 Tb Tb 34.5(3) 8_765 8_765 ?
N1 Tb Tb 169.2(3) . 8_765 ?
O2B Tb Tb 33.03(11) 8_765 8_765 ?
O2 Tb Tb 174.1(8) . 8_765 ?
O2 Tb Tb 35.7(7) 8_765 8_765 ?
N1A Tb Tb 115.85(10) . 8_765 ?
N1B Tb Tb 100.21(11) . 8_765 ?
O1 Tb Tb 97.61(9) . 8_765 ?
Tb Tb Tb 139.87(3) 8_755 8_765 ?
C2A O2A Tb 143.7(4) . . ?
C2A C1A C9A 120.1(7) . . ?
C2A C1A C11A 120.7(6) . . ?
C9A C1A C11A 119.2(7) . . ?
O2A C2A C1A 123.4(6) . . ?
O2A C2A C3A 118.6(6) . . ?
C1A C2A C3A 118.0(6) . . ?
C4A C3A C2A 123.6(7) . . ?
C4A C3A H3A 118.2 . . ?
C2A C3A H3A 118.2 . . ?
C3A C4A C10A 120.2(7) . . ?
C3A C4A H4A 119.9 . . ?
C10A C4A H4A 119.9 . . ?
C6A C5A C10A 119.7(8) . . ?
C6A C5A H5A 120.2 . . ?
C10A C5A H5A 120.2 . . ?
C5A C6A C7A 121.2(7) . . ?
C5A C6A H6A 119.4 . . ?
C7A C6A H6A 119.4 . . ?
C8A C7A C6A 119.5(7) . . ?
C8A C7A H7A 120.3 . . ?
C6A C7A H7A 120.3 . . ?
C7A C8A C9A 122.5(8) . . ?
C7A C8A H8A 118.8 . . ?
C9A C8A H8A 118.8 . . ?
C8A C9A C10A 116.3(7) . . ?
C8A C9A C1A 124.6(8) . . ?
C10A C9A C1A 119.1(7) . . ?
C5A C10A C4A 120.0(8) . . ?
C5A C10A C9A 121.0(7) . . ?
C4A C10A C9A 119.0(7) . . ?
N1A C11A C1A 128.6(7) . . ?
N1A C11A H11A 115.7 . . ?
C1A C11A H11A 115.7 . . ?
C11A N1A C12A 115.2(6) . . ?
C11A N1A Tb 130.5(5) . . ?
C12A N1A Tb 113.0(4) . . ?
N1A C12A C12B 109.6(5) . . ?
N1A C12A H12A 109.7 . . ?
C12B C12A H12A 109.7 . . ?
N1A C12A H12B 109.7 . . ?
C12B C12A H12B 109.7 . . ?
H12A C12A H12B 108.2 . . ?
N1B C12B C12A 109.4(6) . . ?
N1B C12B H12C 109.8 . . ?
C12A C12B H12C 109.8 . . ?
N1B C12B H12D 109.8 . . ?
C12A C12B H12D 109.8 . . ?
H12C C12B H12D 108.3 . . ?
C11B N1B C12B 116.5(6) . . ?
C11B N1B Tb 126.6(5) . . ?
C12B N1B Tb 116.8(4) . . ?
N1B C11B C1B 123.8(7) . . ?
N1B C11B H11B 118.1 . . ?
C1B C11B H11B 118.1 . . ?
C2B O2B Tb 119.1(4) . . ?
C2B O2B Tb 127.4(4) . 8_755 ?
Tb O2B Tb 112.54(19) . 8_755 ?
C2B C1B C11B 121.4(7) . . ?
C2B C1B C9B 119.2(7) . . ?
C11B C1B C9B 119.4(7) . . ?
O2B C2B C3B 118.9(7) . . ?
O2B C2B C1B 121.2(6) . . ?
C3B C2B C1B 119.9(7) . . ?
C4B C3B C2B 120.4(7) . . ?
C4B C3B H3B 119.8 . . ?
C2B C3B H3B 119.8 . . ?
C3B C4B C10B 123.0(7) . . ?
C3B C4B H4B 118.5 . . ?
C10B C4B H4B 118.5 . . ?
C6B C5B C10B 122.7(8) . . ?
C6B C5B H5B 118.6 . . ?
C10B C5B H5B 118.6 . . ?
C5B C6B C7B 118.8(8) . . ?
C5B C6B H6B 120.6 . . ?
C7B C6B H6B 120.6 . . ?
C8B C7B C6B 120.9(8) . . ?
C8B C7B H7B 119.6 . . ?
C6B C7B H7B 119.6 . . ?
C7B C8B C9B 120.8(8) . . ?
C7B C8B H8B 119.6 . . ?
C9B C8B H8B 119.6 . . ?
C10B C9B C8B 117.8(7) . . ?
C10B C9B C1B 119.6(7) . . ?
C8B C9B C1B 122.6(7) . . ?
C9B C10B C5B 118.9(8) . . ?
C9B C10B C4B 118.0(7) . . ?
C5B C10B C4B 123.0(7) . . ?
N2 N1 Tb 125.4(11) . 8_755 ?
N2 N1 Tb 122.2(11) . . ?
Tb N1 Tb 111.6(5) 8_755 . ?
N3 N2 N1 180.0(19) . . ?
C2 O2 Tb 118(3) . . ?
C2 O2 Tb 121(3) . 8_755 ?
Tb O2 Tb 108.4(11) . 8_755 ?
O2 C2 H2A 117.2 . . ?
O2 C2 H2B 114.2 . . ?
H2A C2 H2B 109.6 . . ?
O2 C2 H2C 95.9 . . ?
H2A C2 H2C 109.4 . . ?
H2B C2 H2C 109.4 . . ?
C1 O1 Tb 123.9(4) . . ?
C1 O1 H1 102.7 . . ?
Tb O1 H1 113.5 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb O2A C2A C1A -9.8(11) . . . . ?
Tb O2A C2A C3A 169.6(5) . . . . ?
C9A C1A C2A O2A 178.3(6) . . . . ?
C11A C1A C2A O2A -0.4(10) . . . . ?
C9A C1A C2A C3A -1.1(9) . . . . ?
C11A C1A C2A C3A -179.8(6) . . . . ?
O2A C2A C3A C4A -178.2(6) . . . . ?
C1A C2A C3A C4A 1.3(10) . . . . ?
C2A C3A C4A C10A -1.6(10) . . . . ?
C10A C5A C6A C7A -0.6(11) . . . . ?
C5A C6A C7A C8A 1.2(11) . . . . ?
C6A C7A C8A C9A -0.1(11) . . . . ?
C7A C8A C9A C10A -1.4(10) . . . . ?
C7A C8A C9A C1A 179.9(7) . . . . ?
C2A C1A C9A C8A 180.0(6) . . . . ?
C11A C1A C9A C8A -1.3(10) . . . . ?
C2A C1A C9A C10A 1.3(9) . . . . ?
C11A C1A C9A C10A -179.9(6) . . . . ?
C6A C5A C10A C4A -178.6(6) . . . . ?
C6A C5A C10A C9A -1.0(10) . . . . ?
C3A C4A C10A C5A 179.4(6) . . . . ?
C3A C4A C10A C9A 1.8(10) . . . . ?
C8A C9A C10A C5A 2.0(9) . . . . ?
C1A C9A C10A C5A -179.2(6) . . . . ?
C8A C9A C10A C4A 179.6(6) . . . . ?
C1A C9A C10A C4A -1.6(9) . . . . ?
C2A C1A C11A N1A -1.8(10) . . . . ?
C9A C1A C11A N1A 179.5(6) . . . . ?
C1A C11A N1A C12A 177.1(6) . . . . ?
C1A C11A N1A Tb 10.8(10) . . . . ?
C11A N1A C12A C12B 142.9(6) . . . . ?
Tb N1A C12A C12B -48.3(6) . . . . ?
N1A C12A C12B N1B 53.6(7) . . . . ?
C12A C12B N1B C11B 142.2(6) . . . . ?
C12A C12B N1B Tb -34.1(6) . . . . ?
C12B N1B C11B C1B 178.6(5) . . . . ?
Tb N1B C11B C1B -5.5(9) . . . . ?
N1B C11B C1B C2B 34.6(10) . . . . ?
N1B C11B C1B C9B -148.3(6) . . . . ?
Tb O2B C2B C3B 121.5(5) . . . . ?
Tb O2B C2B C3B -70.5(7) 8_755 . . . ?
Tb O2B C2B C1B -59.4(8) . . . . ?
Tb O2B C2B C1B 108.6(6) 8_755 . . . ?
C11B C1B C2B O2B -0.1(10) . . . . ?
C9B C1B C2B O2B -177.3(5) . . . . ?
C11B C1B C2B C3B 179.0(6) . . . . ?
C9B C1B C2B C3B 1.8(10) . . . . ?
O2B C2B C3B C4B 176.9(6) . . . . ?
C1B C2B C3B C4B -2.3(10) . . . . ?
C2B C3B C4B C10B 1.7(10) . . . . ?
C10B C5B C6B C7B -0.2(11) . . . . ?
C5B C6B C7B C8B 1.6(11) . . . . ?
C6B C7B C8B C9B -2.0(11) . . . . ?
C7B C8B C9B C10B 1.0(10) . . . . ?
C7B C8B C9B C1B 178.7(6) . . . . ?
C2B C1B C9B C10B -0.8(9) . . . . ?
C11B C1B C9B C10B -178.0(6) . . . . ?
C2B C1B C9B C8B -178.5(6) . . . . ?
C11B C1B C9B C8B 4.2(10) . . . . ?
C8B C9B C10B C5B 0.4(9) . . . . ?
C1B C9B C10B C5B -177.4(6) . . . . ?
C8B C9B C10B C4B 178.0(6) . . . . ?
C1B C9B C10B C4B 0.1(9) . . . . ?
C6B C5B C10B C9B -0.8(10) . . . . ?
C6B C5B C10B C4B -178.2(7) . . . . ?
C3B C4B C10B C9B -0.6(10) . . . . ?
C3B C4B C10B C5B 176.9(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
O1 H1 O2A 0.87 1.87 2.725(6) 168.9 8_755
C1 H1A O2A 0.98 2.49 3.100(8) 120.1 .
C1 H1C O1 0.98 2.63 3.510(8) 149.4 8_755

_refine_diff_density_max         1.660
_refine_diff_density_min         -1.757
_refine_diff_density_rms         0.249


# start Validation Reply Form
_vrf_PLAT973_at2856a             
;
PROBLEM: Check Calcd Positive Residual Density on      Gd       2.58 eA-3  
RESPONSE:  Caused by  small, less than 1%, disorder of the molecule.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_at2855a
_database_code_depnum_ccdc_archive 'CCDC 1505020'
_audit_update_record             
;
2016-09-19 deposited with the CCDC.
2016-10-25 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         'C25.25 H22.75 Gd N4.25 O3.25'
_chemical_formula_sum            'C25.25 H22.75 Gd N4.25 O3.25'
_chemical_formula_weight         594.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   22.387(8)
_cell_length_b                   7.560(3)
_cell_length_c                   26.153(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4426(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1016
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      28.85

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             2352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.035
_shelx_estimated_absorpt_T_min   0.473
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur R with Ruby CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19296
_diffrn_reflns_av_unetI/netI     0.2686
_diffrn_reflns_av_R_equivalents  0.2038
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.949
_diffrn_reflns_theta_max         28.847
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5283
_reflns_number_gt                2491
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPRO, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5283
_refine_ls_number_parameters     250
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2338
_refine_ls_R_factor_gt           0.1073
_refine_ls_wR_factor_ref         0.1948
_refine_ls_wR_factor_gt          0.1514
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.71930(3) 0.44540(10) 0.58774(3) 0.0139(2) Uani 1 1 d . . . . .
O2A O 0.6613(4) 0.5595(14) 0.6503(3) 0.021(2) Uani 1 1 d . . . . .
C1A C 0.5569(6) 0.5081(18) 0.6396(5) 0.014(3) Uani 1 1 d . . . . .
C2A C 0.6062(5) 0.570(2) 0.6679(5) 0.013(3) Uiso 1 1 d . . . . .
C3A C 0.5977(6) 0.6435(19) 0.7164(5) 0.017(3) Uiso 1 1 d . . . . .
H3A H 0.6312 0.6871 0.7348 0.021 Uiso 1 1 calc R U . . .
C4A C 0.5422(6) 0.654(2) 0.7378(6) 0.026(4) Uani 1 1 d . . . . .
H4A H 0.5387 0.7020 0.7712 0.031 Uiso 1 1 calc R U . . .
C5A C 0.4345(6) 0.605(2) 0.7359(6) 0.026(4) Uiso 1 1 d . . . . .
H5A H 0.4313 0.6527 0.7694 0.032 Uiso 1 1 calc R U . . .
C6A C 0.3839(6) 0.547(2) 0.7122(6) 0.032(4) Uani 1 1 d . . . . .
H6A H 0.3461 0.5559 0.7285 0.039 Uiso 1 1 calc R U . . .
C7A C 0.3891(6) 0.473(2) 0.6634(7) 0.032(5) Uani 1 1 d . . . . .
H7A H 0.3545 0.4298 0.6465 0.038 Uiso 1 1 calc R U . . .
C8A C 0.4443(6) 0.462(2) 0.6391(6) 0.023(4) Uani 1 1 d . . . . .
H8A H 0.4468 0.4150 0.6055 0.028 Uiso 1 1 calc R U . . .
C9A C 0.4967(5) 0.5204(19) 0.6641(5) 0.016(4) Uani 1 1 d . . . . .
C10A C 0.4907(6) 0.5963(19) 0.7132(6) 0.018(4) Uani 1 1 d . . . . .
C11A C 0.5626(5) 0.4266(18) 0.5896(6) 0.015(3) Uani 1 1 d . . . . .
H11A H 0.5268 0.3821 0.5748 0.018 Uiso 1 1 calc R U . . .
N1A N 0.6097(5) 0.4080(14) 0.5634(4) 0.014(3) Uani 1 1 d . . . . .
C12A C 0.6024(6) 0.315(2) 0.5136(5) 0.018(4) Uani 1 1 d . . . . .
H12A H 0.5604 0.3251 0.5021 0.022 Uiso 1 1 calc R U . . .
H12B H 0.6119 0.1882 0.5178 0.022 Uiso 1 1 calc R U . . .
C12B C 0.6428(5) 0.394(2) 0.4741(5) 0.019(4) Uani 1 1 d . . . . .
H12C H 0.6408 0.3236 0.4422 0.023 Uiso 1 1 calc R U . . .
H12D H 0.6301 0.5164 0.4662 0.023 Uiso 1 1 calc R U . . .
N1B N 0.7051(5) 0.3938(15) 0.4945(4) 0.016(3) Uani 1 1 d . . . . .
C11B C 0.7457(6) 0.3669(19) 0.4610(6) 0.018(4) Uiso 1 1 d . . . . .
H11B H 0.7332 0.3449 0.4269 0.022 Uiso 1 1 calc R U . . .
O2B O 0.7945(3) 0.2500(12) 0.5569(4) 0.019(2) Uani 1 1 d . . . . .
C1B C 0.8108(6) 0.367(2) 0.4714(6) 0.020(4) Uiso 1 1 d . . . . .
C2B C 0.8308(6) 0.3100(19) 0.5201(5) 0.014(3) Uiso 1 1 d . . . . .
C3B C 0.8930(6) 0.3118(19) 0.5308(5) 0.017(4) Uiso 1 1 d . . . . .
H3B H 0.9065 0.2789 0.5639 0.020 Uiso 1 1 calc R U . . .
C4B C 0.9334(6) 0.359(2) 0.4948(6) 0.022(4) Uiso 1 1 d . . . . .
H4B H 0.9749 0.3533 0.5024 0.026 Uiso 1 1 calc R U . . .
C5B C 0.9563(6) 0.476(2) 0.4086(6) 0.027(4) Uiso 1 1 d . . . . .
H5B H 0.9977 0.4742 0.4166 0.032 Uiso 1 1 calc R U . . .
C6B C 0.9379(7) 0.533(2) 0.3618(6) 0.035(5) Uani 1 1 d . . . . .
H6B H 0.9665 0.5716 0.3374 0.042 Uiso 1 1 calc R U . . .
C7B C 0.8764(7) 0.536(2) 0.3495(6) 0.031(4) Uani 1 1 d . . . . .
H7B H 0.8640 0.5734 0.3165 0.037 Uiso 1 1 calc R U . . .
C8B C 0.8343(7) 0.485(2) 0.3852(6) 0.032(4) Uani 1 1 d . . . . .
H8B H 0.7930 0.4920 0.3772 0.038 Uiso 1 1 calc R U . . .
C9B C 0.8529(6) 0.422(2) 0.4342(5) 0.018(3) Uiso 1 1 d . . . . .
C10B C 0.9144(6) 0.4186(19) 0.4452(5) 0.016(3) Uiso 1 1 d . . . . .
N1 N 0.6904(10) 0.129(4) 0.5973(9) 0.010(4) Uiso 0.75 1 d . . P A 1
N2 N 0.6432(10) 0.083(4) 0.6187(8) 0.028(5) Uiso 0.75 1 d . . P A 1
N3 N 0.6010(7) 0.038(2) 0.6387(7) 0.036(5) Uani 0.75 1 d . . P A 1
O2 O 0.700(2) 0.126(9) 0.603(2) 0.010(4) Uiso 0.25 1 d D . P A 2
C2 C 0.647(3) 0.084(15) 0.631(3) 0.028(5) Uiso 0.25 1 d D . P A 2
H2A H 0.6390 0.1681 0.6587 0.043 Uiso 0.25 1 d R U P A 2
H2B H 0.6496 -0.0383 0.6445 0.043 Uiso 0.25 1 d R U P A 2
H2C H 0.6148 0.0901 0.6052 0.043 Uiso 0.25 1 d R U P A 2
O1 O 0.7673(4) 0.3454(13) 0.6702(4) 0.019(2) Uani 1 1 d . . . . .
H1 H 0.7935 0.2616 0.6663 0.029 Uiso 1 1 d R U . . .
C1 C 0.7351(6) 0.2895(19) 0.7139(6) 0.026(4) Uani 1 1 d . . . . .
H1A H 0.6982 0.3588 0.7169 0.039 Uiso 1 1 calc R U . . .
H1B H 0.7596 0.3074 0.7446 0.039 Uiso 1 1 calc R U . . .
H1C H 0.7251 0.1638 0.7106 0.039 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O2A 2.260(9) . ?
Gd O2 2.30(6) 8_765 ?
Gd O2B 2.380(8) . ?
Gd O2B 2.459(9) 8_765 ?
Gd N1 2.46(2) 8_765 ?
Gd O2 2.49(7) . ?
Gd N1B 2.491(11) . ?
Gd N1 2.49(3) . ?
Gd O1 2.526(9) . ?
Gd N1A 2.549(11) . ?
Gd Gd 4.0221(15) 8_755 ?
Gd Gd 4.0222(15) 8_765 ?
O2A C2A 1.321(14) . ?
C1A C2A 1.409(18) . ?
C1A C11A 1.451(18) . ?
C1A C9A 1.496(16) . ?
C2A C3A 1.395(17) . ?
C3A C4A 1.365(17) . ?
C3A H3A 0.9500 . ?
C4A C10A 1.391(19) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.364(19) . ?
C5A C10A 1.390(18) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.40(2) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.392(18) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.412(18) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.414(18) . ?
C11A N1A 1.267(15) . ?
C11A H11A 0.9500 . ?
N1A C12A 1.489(16) . ?
C12A C12B 1.495(18) . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?
C12B N1B 1.494(15) . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
N1B C11B 1.277(16) . ?
C11B C1B 1.482(17) . ?
C11B H11B 0.9500 . ?
O2B C2B 1.340(15) . ?
O2B Gd 2.459(9) 8_755 ?
C1B C2B 1.417(18) . ?
C1B C9B 1.417(18) . ?
C2B C3B 1.421(17) . ?
C3B C4B 1.355(18) . ?
C3B H3B 0.9500 . ?
C4B C10B 1.436(18) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.36(2) . ?
C5B C10B 1.408(19) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.41(2) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.38(2) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.429(19) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.406(17) . ?
N1 N2 1.24(2) . ?
N1 Gd 2.46(2) 8_755 ?
N2 N3 1.13(3) . ?
O2 C2 1.42(2) . ?
O2 Gd 2.30(6) 8_755 ?
C2 H2A 0.9885 . ?
C2 H2B 0.9920 . ?
C2 H2C 0.9852 . ?
O1 C1 1.417(15) . ?
O1 H1 0.8682 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Gd O2 95.8(15) . 8_765 ?
O2A Gd O2B 152.7(3) . . ?
O2 Gd O2B 82.5(15) 8_765 . ?
O2A Gd O2B 78.9(3) . 8_765 ?
O2 Gd O2B 66.4(16) 8_765 8_765 ?
O2B Gd O2B 124.0(3) . 8_765 ?
O2A Gd N1 100.5(6) . 8_765 ?
O2B Gd N1 78.7(6) . 8_765 ?
O2B Gd N1 67.0(7) 8_765 8_765 ?
O2A Gd O2 98.8(14) . . ?
O2 Gd O2 133.4(19) 8_765 . ?
O2B Gd O2 64.9(14) . . ?
O2B Gd O2 160.0(12) 8_765 . ?
O2A Gd N1B 134.1(3) . . ?
O2 Gd N1B 111.3(15) 8_765 . ?
O2B Gd N1B 70.2(3) . . ?
O2B Gd N1B 79.0(3) 8_765 . ?
N1 Gd N1B 107.0(6) 8_765 . ?
O2 Gd N1B 89.0(14) . . ?
O2A Gd N1 98.3(7) . . ?
O2B Gd N1 67.8(6) . . ?
O2B Gd N1 154.1(5) 8_765 . ?
N1 Gd N1 138.0(7) 8_765 . ?
N1B Gd N1 85.1(6) . . ?
O2A Gd O1 75.0(3) . . ?
O2 Gd O1 72.3(16) 8_765 . ?
O2B Gd O1 78.6(3) . . ?
O2B Gd O1 127.9(3) 8_765 . ?
N1 Gd O1 74.5(6) 8_765 . ?
O2 Gd O1 69.4(13) . . ?
N1B Gd O1 147.5(3) . . ?
N1 Gd O1 74.7(5) . . ?
O2A Gd N1A 70.8(3) . . ?
O2 Gd N1A 149.9(16) 8_765 . ?
O2B Gd N1A 121.8(3) . . ?
O2B Gd N1A 84.3(3) 8_765 . ?
N1 Gd N1A 151.3(7) 8_765 . ?
O2 Gd N1A 76.3(12) . . ?
N1B Gd N1A 67.4(4) . . ?
N1 Gd N1A 70.7(5) . . ?
O1 Gd N1A 126.1(3) . . ?
O2A Gd Gd 123.7(3) . 8_755 ?
O2 Gd Gd 106.8(15) 8_765 8_755 ?
O2B Gd Gd 34.4(2) . 8_755 ?
O2B Gd Gd 157.4(2) 8_765 8_755 ?
N1 Gd Gd 104.4(6) 8_765 8_755 ?
O2 Gd Gd 31.5(13) . 8_755 ?
N1B Gd Gd 84.1(3) . 8_755 ?
N1 Gd Gd 35.5(5) . 8_755 ?
O1 Gd Gd 64.7(2) . 8_755 ?
N1A Gd Gd 103.0(2) . 8_755 ?
O2A Gd Gd 80.7(3) . 8_765 ?
O2 Gd Gd 34.3(16) 8_765 8_765 ?
O2B Gd Gd 110.0(2) . 8_765 ?
O2B Gd Gd 33.16(19) 8_765 8_765 ?
N1 Gd Gd 36.0(6) 8_765 8_765 ?
O2 Gd Gd 166.7(12) . 8_765 ?
N1B Gd Gd 101.0(3) . 8_765 ?
N1 Gd Gd 172.5(5) . 8_765 ?
O1 Gd Gd 97.8(2) . 8_765 ?
N1A Gd Gd 115.7(2) . 8_765 ?
Gd Gd Gd 140.03(4) 8_755 8_765 ?
C2A O2A Gd 144.4(9) . . ?
C2A C1A C11A 123.1(12) . . ?
C2A C1A C9A 117.4(13) . . ?
C11A C1A C9A 119.4(12) . . ?
O2A C2A C3A 117.9(12) . . ?
O2A C2A C1A 121.9(13) . . ?
C3A C2A C1A 120.2(12) . . ?
C4A C3A C2A 121.2(13) . . ?
C4A C3A H3A 119.4 . . ?
C2A C3A H3A 119.4 . . ?
C3A C4A C10A 123.3(15) . . ?
C3A C4A H4A 118.4 . . ?
C10A C4A H4A 118.4 . . ?
C6A C5A C10A 122.8(15) . . ?
C6A C5A H5A 118.6 . . ?
C10A C5A H5A 118.6 . . ?
C5A C6A C7A 118.3(13) . . ?
C5A C6A H6A 120.9 . . ?
C7A C6A H6A 120.8 . . ?
C8A C7A C6A 120.9(15) . . ?
C8A C7A H7A 119.5 . . ?
C6A C7A H7A 119.5 . . ?
C7A C8A C9A 120.4(15) . . ?
C7A C8A H8A 119.8 . . ?
C9A C8A H8A 119.8 . . ?
C8A C9A C10A 118.0(12) . . ?
C8A C9A C1A 122.0(13) . . ?
C10A C9A C1A 120.0(12) . . ?
C5A C10A C4A 122.6(15) . . ?
C5A C10A C9A 119.5(13) . . ?
C4A C10A C9A 117.9(13) . . ?
N1A C11A C1A 127.4(12) . . ?
N1A C11A H11A 116.3 . . ?
C1A C11A H11A 116.3 . . ?
C11A N1A C12A 115.7(12) . . ?
C11A N1A Gd 130.9(10) . . ?
C12A N1A Gd 112.1(8) . . ?
N1A C12A C12B 110.5(12) . . ?
N1A C12A H12A 109.5 . . ?
C12B C12A H12A 109.5 . . ?
N1A C12A H12B 109.5 . . ?
C12B C12A H12B 109.5 . . ?
H12A C12A H12B 108.1 . . ?
N1B C12B C12A 108.5(11) . . ?
N1B C12B H12C 110.0 . . ?
C12A C12B H12C 110.0 . . ?
N1B C12B H12D 110.0 . . ?
C12A C12B H12D 110.0 . . ?
H12C C12B H12D 108.4 . . ?
C11B N1B C12B 114.9(12) . . ?
C11B N1B Gd 127.2(10) . . ?
C12B N1B Gd 117.9(8) . . ?
N1B C11B C1B 125.0(14) . . ?
N1B C11B H11B 117.5 . . ?
C1B C11B H11B 117.5 . . ?
C2B O2B Gd 117.5(8) . . ?
C2B O2B Gd 129.0(8) . 8_755 ?
Gd O2B Gd 112.4(3) . 8_755 ?
C2B C1B C9B 119.7(13) . . ?
C2B C1B C11B 118.3(13) . . ?
C9B C1B C11B 122.0(14) . . ?
O2B C2B C1B 124.0(12) . . ?
O2B C2B C3B 117.1(12) . . ?
C1B C2B C3B 119.0(13) . . ?
C4B C3B C2B 121.3(14) . . ?
C4B C3B H3B 119.3 . . ?
C2B C3B H3B 119.3 . . ?
C3B C4B C10B 120.8(13) . . ?
C3B C4B H4B 119.6 . . ?
C10B C4B H4B 119.6 . . ?
C6B C5B C10B 120.4(14) . . ?
C6B C5B H5B 119.8 . . ?
C10B C5B H5B 119.8 . . ?
C5B C6B C7B 120.3(14) . . ?
C5B C6B H6B 119.8 . . ?
C7B C6B H6B 119.8 . . ?
C8B C7B C6B 120.4(16) . . ?
C8B C7B H7B 119.8 . . ?
C6B C7B H7B 119.8 . . ?
C7B C8B C9B 119.9(15) . . ?
C7B C8B H8B 120.0 . . ?
C9B C8B H8B 120.0 . . ?
C10B C9B C1B 120.4(13) . . ?
C10B C9B C8B 118.4(13) . . ?
C1B C9B C8B 121.2(13) . . ?
C9B C10B C5B 120.5(13) . . ?
C9B C10B C4B 118.7(12) . . ?
C5B C10B C4B 120.8(13) . . ?
N2 N1 Gd 126(2) . 8_755 ?
N2 N1 Gd 122(2) . . ?
Gd N1 Gd 108.5(9) 8_755 . ?
N3 N2 N1 178(3) . . ?
C2 O2 Gd 127(6) . 8_755 ?
C2 O2 Gd 117(6) . . ?
Gd O2 Gd 114(2) 8_755 . ?
O2 C2 H2A 112.8 . . ?
O2 C2 H2B 110.6 . . ?
H2A C2 H2B 109.8 . . ?
O2 C2 H2C 104.7 . . ?
H2A C2 H2C 109.4 . . ?
H2B C2 H2C 109.4 . . ?
C1 O1 Gd 124.2(8) . . ?
C1 O1 H1 102.8 . . ?
Gd O1 H1 113.9 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd O2A C2A C3A 169.8(11) . . . . ?
Gd O2A C2A C1A -9(2) . . . . ?
C11A C1A C2A O2A 0(2) . . . . ?
C9A C1A C2A O2A 177.6(12) . . . . ?
C11A C1A C2A C3A -178.4(13) . . . . ?
C9A C1A C2A C3A -1(2) . . . . ?
O2A C2A C3A C4A -177.7(13) . . . . ?
C1A C2A C3A C4A 1(2) . . . . ?
C2A C3A C4A C10A -1(2) . . . . ?
C10A C5A C6A C7A 1(3) . . . . ?
C5A C6A C7A C8A -1(3) . . . . ?
C6A C7A C8A C9A 2(2) . . . . ?
C7A C8A C9A C10A -3(2) . . . . ?
C7A C8A C9A C1A 179.0(14) . . . . ?
C2A C1A C9A C8A 179.9(14) . . . . ?
C11A C1A C9A C8A -3(2) . . . . ?
C2A C1A C9A C10A 2(2) . . . . ?
C11A C1A C9A C10A 178.8(13) . . . . ?
C6A C5A C10A C4A -179.1(15) . . . . ?
C6A C5A C10A C9A -2(2) . . . . ?
C3A C4A C10A C5A 178.9(14) . . . . ?
C3A C4A C10A C9A 2(2) . . . . ?
C8A C9A C10A C5A 3(2) . . . . ?
C1A C9A C10A C5A -179.0(13) . . . . ?
C8A C9A C10A C4A 179.9(13) . . . . ?
C1A C9A C10A C4A -2(2) . . . . ?
C2A C1A C11A N1A -4(2) . . . . ?
C9A C1A C11A N1A 178.9(13) . . . . ?
C1A C11A N1A C12A 178.7(13) . . . . ?
C1A C11A N1A Gd 13(2) . . . . ?
C11A N1A C12A C12B 143.8(12) . . . . ?
Gd N1A C12A C12B -47.6(13) . . . . ?
N1A C12A C12B N1B 53.6(15) . . . . ?
C12A C12B N1B C11B 145.1(13) . . . . ?
C12A C12B N1B Gd -35.0(14) . . . . ?
C12B N1B C11B C1B 177.6(13) . . . . ?
Gd N1B C11B C1B -2(2) . . . . ?
N1B C11B C1B C2B 32(2) . . . . ?
N1B C11B C1B C9B -148.8(15) . . . . ?
Gd O2B C2B C1B -60.0(17) . . . . ?
Gd O2B C2B C1B 107.2(15) 8_755 . . . ?
Gd O2B C2B C3B 121.3(11) . . . . ?
Gd O2B C2B C3B -71.5(15) 8_755 . . . ?
C9B C1B C2B O2B -177.4(13) . . . . ?
C11B C1B C2B O2B 2(2) . . . . ?
C9B C1B C2B C3B 1(2) . . . . ?
C11B C1B C2B C3B -179.3(13) . . . . ?
O2B C2B C3B C4B 175.7(14) . . . . ?
C1B C2B C3B C4B -3(2) . . . . ?
C2B C3B C4B C10B 3(2) . . . . ?
C10B C5B C6B C7B 0(2) . . . . ?
C5B C6B C7B C8B 2(2) . . . . ?
C6B C7B C8B C9B -3(2) . . . . ?
C2B C1B C9B C10B 0(2) . . . . ?
C11B C1B C9B C10B -179.2(13) . . . . ?
C2B C1B C9B C8B -178.3(14) . . . . ?
C11B C1B C9B C8B 2(2) . . . . ?
C7B C8B C9B C10B 2(2) . . . . ?
C7B C8B C9B C1B -179.5(15) . . . . ?
C1B C9B C10B C5B -178.8(14) . . . . ?
C8B C9B C10B C5B 0(2) . . . . ?
C1B C9B C10B C4B 0(2) . . . . ?
C8B C9B C10B C4B 178.5(14) . . . . ?
C6B C5B C10B C9B -1(2) . . . . ?
C6B C5B C10B C4B -179.4(15) . . . . ?
C3B C4B C10B C9B -2(2) . . . . ?
C3B C4B C10B C5B 177.0(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O2A 0.87 1.88 2.738(14) 169.0 8_755
C1 H1A O2A 0.98 2.45 3.108(18) 123.9 .
C1 H1C O1 0.98 2.63 3.548(18) 155.1 8_755

_refine_diff_density_max         3.179
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.294


# start Validation Reply Form
_vrf_PLAT201_at2855a             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         13 Report
RESPONSE: Due to the low quality of data it was impossible to refine part of the atoms 
with anisotropic displacement parameters
;
_vrf_PLAT973_at2855a             
;
PROBLEM: Check Calcd Positive Residual Density on      Gd       2.58 eA-3  
RESPONSE:  Caused by  small, less than 1%, disorder of the molecule.
;
# end Validation Reply Form
