# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_em45

# ========================================================================= #

_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_audit_creation_date             '07 March 2014'

# ========================================================================= #

_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C87 H120 Gd7 N6 O33, 11(C H4 O)'
_chemical_formula_sum            'C98 H164 Gd7 N6 O44'
_chemical_formula_weight         3231.10

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

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

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

_cell_length_a                   17.237(2)
_cell_length_b                   17.237(2)
_cell_length_c                   25.135(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6467.6(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9314
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      40.08

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3188
_exptl_absorpt_coefficient_mu    3.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2992
_exptl_absorpt_correction_T_max  0.6709
_exptl_absorpt_process_details   
;
 SADABS (Sheldrick, 1997)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            83384
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.66
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5046
_reflns_number_gt                4545
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'APEX2 '
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_computing_structure_refinement  'SHELXTL '
_computing_molecular_graphics    'SHELXTL '
_computing_publication_material  'SHELXTL '

_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)+(0.0197P)²+36.1254P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5046
_refine_ls_number_parameters     237
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0780
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.169
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.566475(13) 0.160213(13) 0.351305(8) 0.01755(7) Uani 1 1 d . . .
Gd2 Gd 0.6667 0.3333 0.2500 0.01272(10) Uani 1 6 d S . .
O5 O 0.5655(3) 0.1636(3) 0.2500 0.0177(8) Uani 1 2 d S . .
O1 O 0.6231(2) 0.0653(2) 0.33074(13) 0.0299(7) Uani 1 1 d . . .
N1 N 0.4788(3) 0.0090(2) 0.39497(15) 0.0282(8) Uani 1 1 d . . .
C7 C 0.3980(3) -0.0263(3) 0.41079(18) 0.0312(10) Uani 1 1 d . . .
H7 H 0.3676 -0.0891 0.4168 0.037 Uiso 1 1 calc R . .
C5 C 0.5835(4) -0.0306(4) 0.4346(2) 0.0368(12) Uani 1 1 d . . .
H5A H 0.5505 -0.0471 0.4687 0.044 Uiso 1 1 calc R . .
H5B H 0.6281 0.0342 0.4358 0.044 Uiso 1 1 calc R . .
C4 C 0.6324(5) -0.0845(4) 0.4278(2) 0.0462(14) Uani 1 1 d . . .
H4A H 0.6764 -0.0694 0.4569 0.055 Uiso 1 1 calc R . .
H4B H 0.5885 -0.1494 0.4298 0.055 Uiso 1 1 calc R . .
C2 C 0.6157(4) -0.0812(4) 0.3287(2) 0.0437(14) Uani 1 1 d . . .
H2A H 0.5722 -0.1462 0.3271 0.052 Uiso 1 1 calc R . .
H2B H 0.6494 -0.0637 0.2948 0.052 Uiso 1 1 calc R . .
C1 C 0.5650(4) -0.0301(3) 0.3348(2) 0.0354(11) Uani 1 1 d . . .
H1 H 0.5186 -0.0499 0.3061 0.042 Uiso 1 1 calc R . .
C3 C 0.6806(4) -0.0630(4) 0.3742(2) 0.0458(14) Uani 1 1 d . . .
H3A H 0.7282 0.0008 0.3735 0.055 Uiso 1 1 calc R . .
H3B H 0.7093 -0.1000 0.3696 0.055 Uiso 1 1 calc R . .
C6 C 0.5181(4) -0.0487(3) 0.3891(2) 0.0322(11) Uani 1 1 d . . .
H6A H 0.4693 -0.1128 0.3905 0.039 Uiso 1 1 calc R . .
C13 C 0.3848(3) 0.1132(3) 0.42079(17) 0.0272(10) Uani 1 1 d . . .
C8 C 0.3469(3) 0.0189(3) 0.42069(18) 0.0304(10) Uani 1 1 d . . .
C12 C 0.3276(3) 0.1479(4) 0.4306(2) 0.0367(11) Uani 1 1 d . . .
H12 H 0.3520 0.2110 0.4312 0.044 Uiso 1 1 calc R . .
C9 C 0.2539(4) -0.0359(4) 0.4313(2) 0.0449(14) Uani 1 1 d . . .
H9 H 0.2287 -0.0991 0.4323 0.054 Uiso 1 1 calc R . .
O2 O 0.4715(2) 0.1681(2) 0.41249(12) 0.0261(7) Uani 1 1 d . . .
C14 C 0.4772(4) 0.1079(4) 0.2500 0.0206(12) Uani 1 2 d S . .
O3 O 0.55725(19) 0.28850(18) 0.31958(11) 0.0174(5) Uani 1 1 d D . .
H3 H 0.5029(19) 0.265(3) 0.3048(19) 0.026 Uiso 1 1 d D . .
C11 C 0.2370(4) 0.0927(4) 0.4393(3) 0.0465(14) Uani 1 1 d . . .
H11 H 0.1999 0.1181 0.4448 0.056 Uiso 1 1 calc R . .
C10 C 0.1995(4) -0.0004(5) 0.4401(3) 0.0531(16) Uani 1 1 d . . .
H10 H 0.1373 -0.0384 0.4467 0.064 Uiso 1 1 calc R . .
O6 O 0.6612(2) 0.2098(2) 0.42832(12) 0.0264(7) Uani 1 1 d D . .
H6 H 0.7213(15) 0.235(4) 0.423(2) 0.040 Uiso 1 1 d D . .
C15 C 0.6432(4) 0.1940(4) 0.48385(19) 0.0391(12) Uani 1 1 d . . .
H15A H 0.5783 0.1606 0.4896 0.059 Uiso 1 1 calc R . .
H15B H 0.6692 0.2514 0.5027 0.059 Uiso 1 1 calc R . .
H15C H 0.6696 0.1591 0.4974 0.059 Uiso 1 1 calc R . .
O4 O 0.4384(2) 0.0830(2) 0.29487(12) 0.0269(7) Uani 1 1 d . . .
O7 O 0.7248(3) 0.1272(3) 0.2500 0.0319(10) Uiso 1 2 d S . .
C16 C 0.8071(7) 0.1234(7) 0.2500 0.061(3) Uiso 1 2 d S . .
C18 C 0.6667 0.3333 0.6206(8) 0.098(5) Uiso 1 3 d S . .
C17 C 0.2135(12) -0.0656(12) 0.2500 0.109(5) Uiso 1 2 d S . .
O8 O 0.2693(8) -0.0667(8) 0.2924(5) 0.076(3) Uiso 0.50 1 d P . .
C19 C 0.3378(17) -0.1985(17) 0.2500 0.159(8) Uiso 1 2 d S . 1
O9 O 0.7017(13) 0.2913(13) 0.6127(8) 0.087(5) Uiso 0.33 1 d P . .
O10 O 0.3225(13) -0.1808(13) 0.2991(7) 0.132(6) Uiso 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O2 2.298(3) . ?
Gd1 O1 2.344(3) . ?
Gd1 O3 2.389(3) 3_655 ?
Gd1 O4 2.392(3) . ?
Gd1 O6 2.398(3) . ?
Gd1 O3 2.430(3) . ?
Gd1 N1 2.518(4) . ?
Gd1 O5 2.5472(4) . ?
Gd2 O3 2.399(3) 12_656 ?
Gd2 O3 2.399(3) 3_655 ?
Gd2 O3 2.399(3) 5_665 ?
Gd2 O3 2.399(3) 10_556 ?
Gd2 O3 2.399(3) 8_666 ?
Gd2 O3 2.399(3) . ?
Gd2 O5 2.550(4) 3_655 ?
Gd2 O5 2.550(4) . ?
Gd2 O5 2.550(4) 8_666 ?
O5 C14 1.333(7) . ?
O5 Gd1 2.5472(4) 10_556 ?
O1 C1 1.438(6) . ?
N1 C7 1.273(6) . ?
N1 C6 1.465(6) . ?
C7 C8 1.459(7) . ?
C7 H7 0.9500 . ?
C5 C6 1.525(7) . ?
C5 C4 1.546(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 C3 1.528(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 C3 1.518(9) . ?
C2 C1 1.529(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 C6 1.536(7) . ?
C1 H1 1.0000 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C6 H6A 1.0000 . ?
C13 O2 1.327(5) . ?
C13 C12 1.406(7) . ?
C13 C8 1.417(7) . ?
C8 C9 1.421(7) . ?
C12 C11 1.380(7) . ?
C12 H12 0.9500 . ?
C9 C10 1.370(9) . ?
C9 H9 0.9500 . ?
C14 O4 1.272(4) 10_556 ?
C14 O4 1.272(4) . ?
O3 Gd1 2.389(3) 5_665 ?
O3 H3 0.895(19) . ?
C11 C10 1.398(9) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
O6 C15 1.426(5) . ?
O6 H6 0.91(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O7 C16 1.452(12) . ?
C18 O9 1.169(19) . ?
C18 O9 1.169(19) 3_655 ?
C18 O9 1.169(19) 5_665 ?
C17 O8 1.442(15) . ?
C17 O8 1.442(15) 10_556 ?
C19 O10 1.330(19) 10_556 ?
C19 O10 1.330(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 O1 138.25(11) . . ?
O2 Gd1 O3 132.38(10) . 3_655 ?
O1 Gd1 O3 80.51(11) . 3_655 ?
O2 Gd1 O4 86.74(11) . . ?
O1 Gd1 O4 94.12(12) . . ?
O3 Gd1 O4 123.45(10) 3_655 . ?
O2 Gd1 O6 79.46(11) . . ?
O1 Gd1 O6 88.83(12) . . ?
O3 Gd1 O6 74.38(10) 3_655 . ?
O4 Gd1 O6 162.17(10) . . ?
O2 Gd1 O3 78.07(10) . . ?
O1 Gd1 O3 143.38(10) . . ?
O3 Gd1 O3 72.35(13) 3_655 . ?
O4 Gd1 O3 81.33(10) . . ?
O6 Gd1 O3 106.47(10) . . ?
O2 Gd1 N1 72.11(12) . . ?
O1 Gd1 N1 67.53(13) . . ?
O3 Gd1 N1 143.85(12) 3_655 . ?
O4 Gd1 N1 76.90(12) . . ?
O6 Gd1 N1 88.07(12) . . ?
O3 Gd1 N1 143.74(12) . . ?
O2 Gd1 O5 130.88(12) . . ?
O1 Gd1 O5 78.76(12) . . ?
O3 Gd1 O5 70.41(11) 3_655 . ?
O4 Gd1 O5 53.49(11) . . ?
O6 Gd1 O5 144.09(12) . . ?
O3 Gd1 O5 69.34(11) . . ?
N1 Gd1 O5 116.87(13) . . ?
O2 Gd1 C14 109.00(14) . . ?
O1 Gd1 C14 86.00(15) . . ?
O3 Gd1 C14 97.84(12) 3_655 . ?
O4 Gd1 C14 25.89(12) . . ?
O6 Gd1 C14 171.30(13) . . ?
O3 Gd1 C14 74.13(13) . . ?
N1 Gd1 C14 96.39(14) . . ?
O5 Gd1 C14 27.61(13) . . ?
O2 Gd1 Gd2 118.69(8) . . ?
O1 Gd1 Gd2 103.05(8) . . ?
O3 Gd1 Gd2 40.70(7) 3_655 . ?
O4 Gd1 Gd2 88.21(7) . . ?
O6 Gd1 Gd2 108.27(8) . . ?
O3 Gd1 Gd2 40.84(6) . . ?
N1 Gd1 Gd2 161.38(9) . . ?
O5 Gd1 Gd2 44.52(9) . . ?
C14 Gd1 Gd2 66.26(11) . . ?
O3 Gd2 O3 93.61(13) 12_656 3_655 ?
O3 Gd2 O3 139.97(5) 12_656 5_665 ?
O3 Gd2 O3 72.71(11) 3_655 5_665 ?
O3 Gd2 O3 72.71(11) 12_656 10_556 ?
O3 Gd2 O3 139.97(5) 3_655 10_556 ?
O3 Gd2 O3 139.97(5) 5_665 10_556 ?
O3 Gd2 O3 72.71(11) 12_656 8_666 ?
O3 Gd2 O3 139.97(5) 3_655 8_666 ?
O3 Gd2 O3 93.61(14) 5_665 8_666 ?
O3 Gd2 O3 72.71(11) 10_556 8_666 ?
O3 Gd2 O3 139.97(5) 12_656 . ?
O3 Gd2 O3 72.71(11) 3_655 . ?
O3 Gd2 O3 72.71(11) 5_665 . ?
O3 Gd2 O3 93.61(13) 10_556 . ?
O3 Gd2 O3 139.97(5) 8_666 . ?
O3 Gd2 O5 69.75(9) 12_656 3_655 ?
O3 Gd2 O5 69.75(9) 3_655 3_655 ?
O3 Gd2 O5 70.22(9) 5_665 3_655 ?
O3 Gd2 O5 133.19(7) 10_556 3_655 ?
O3 Gd2 O5 70.22(9) 8_666 3_655 ?
O3 Gd2 O5 133.19(7) . 3_655 ?
O3 Gd2 O5 70.22(9) 12_656 . ?
O3 Gd2 O5 70.22(9) 3_655 . ?
O3 Gd2 O5 133.19(7) 5_665 . ?
O3 Gd2 O5 69.75(9) 10_556 . ?
O3 Gd2 O5 133.19(7) 8_666 . ?
O3 Gd2 O5 69.75(9) . . ?
O5 Gd2 O5 120.0 3_655 . ?
O3 Gd2 O5 133.19(7) 12_656 8_666 ?
O3 Gd2 O5 133.19(7) 3_655 8_666 ?
O3 Gd2 O5 69.75(9) 5_665 8_666 ?
O3 Gd2 O5 70.22(9) 10_556 8_666 ?
O3 Gd2 O5 69.75(9) 8_666 8_666 ?
O3 Gd2 O5 70.22(9) . 8_666 ?
O5 Gd2 O5 120.000(1) 3_655 8_666 ?
O5 Gd2 O5 120.000(1) . 8_666 ?
O3 Gd2 Gd1 105.78(7) 12_656 3_655 ?
O3 Gd2 Gd1 41.47(7) 3_655 3_655 ?
O3 Gd2 Gd1 40.50(7) 5_665 3_655 ?
O3 Gd2 Gd1 177.59(7) 10_556 3_655 ?
O3 Gd2 Gd1 105.11(7) 8_666 3_655 ?
O3 Gd2 Gd1 88.74(7) . 3_655 ?
O5 Gd2 Gd1 44.469(7) 3_655 3_655 ?
O5 Gd2 Gd1 111.65(6) . 3_655 ?
O5 Gd2 Gd1 110.16(6) 8_666 3_655 ?
O3 Gd2 Gd1 40.50(7) 12_656 10_556 ?
O3 Gd2 Gd1 105.11(7) 3_655 10_556 ?
O3 Gd2 Gd1 177.59(7) 5_665 10_556 ?
O3 Gd2 Gd1 41.47(7) 10_556 10_556 ?
O3 Gd2 Gd1 88.74(7) 8_666 10_556 ?
O3 Gd2 Gd1 105.78(7) . 10_556 ?
O5 Gd2 Gd1 110.16(6) 3_655 10_556 ?
O5 Gd2 Gd1 44.469(7) . 10_556 ?
O5 Gd2 Gd1 111.65(6) 8_666 10_556 ?
Gd1 Gd2 Gd1 138.182(5) 3_655 10_556 ?
O3 Gd2 Gd1 41.47(7) 12_656 12_656 ?
O3 Gd2 Gd1 105.78(7) 3_655 12_656 ?
O3 Gd2 Gd1 105.11(7) 5_665 12_656 ?
O3 Gd2 Gd1 88.74(7) 10_556 12_656 ?
O3 Gd2 Gd1 40.50(7) 8_666 12_656 ?
O3 Gd2 Gd1 177.59(7) . 12_656 ?
O5 Gd2 Gd1 44.469(7) 3_655 12_656 ?
O5 Gd2 Gd1 111.65(6) . 12_656 ?
O5 Gd2 Gd1 110.16(6) 8_666 12_656 ?
Gd1 Gd2 Gd1 88.915(13) 3_655 12_656 ?
Gd1 Gd2 Gd1 76.361(10) 10_556 12_656 ?
C14 O5 Gd1 90.10(9) . 10_556 ?
C14 O5 Gd1 90.10(9) . . ?
Gd1 O5 Gd1 176.95(18) 10_556 . ?
C14 O5 Gd2 134.9(4) . . ?
Gd1 O5 Gd2 91.01(9) 10_556 . ?
Gd1 O5 Gd2 91.01(9) . . ?
C1 O1 Gd1 119.1(3) . . ?
C7 N1 C6 118.3(4) . . ?
C7 N1 Gd1 125.3(3) . . ?
C6 N1 Gd1 114.6(3) . . ?
N1 C7 C8 127.3(4) . . ?
N1 C7 H7 116.4 . . ?
C8 C7 H7 116.4 . . ?
C6 C5 C4 111.3(5) . . ?
C6 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C3 C4 C5 110.2(4) . . ?
C3 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C3 C2 C1 112.4(5) . . ?
C3 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.9 . . ?
O1 C1 C2 112.3(5) . . ?
O1 C1 C6 107.1(4) . . ?
C2 C1 C6 111.2(4) . . ?
O1 C1 H1 108.7 . . ?
C2 C1 H1 108.7 . . ?
C6 C1 H1 108.7 . . ?
C2 C3 C4 111.0(5) . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N1 C6 C5 109.3(4) . . ?
N1 C6 C1 108.8(4) . . ?
C5 C6 C1 111.5(4) . . ?
N1 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C1 C6 H6A 109.1 . . ?
O2 C13 C12 120.3(4) . . ?
O2 C13 C8 121.7(4) . . ?
C12 C13 C8 118.0(4) . . ?
C13 C8 C9 118.8(5) . . ?
C13 C8 C7 123.9(4) . . ?
C9 C8 C7 117.3(5) . . ?
C11 C12 C13 121.8(5) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C10 C9 C8 122.0(6) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C13 O2 Gd1 130.2(3) . . ?
O4 C14 O4 125.0(5) 10_556 . ?
O4 C14 O5 117.5(3) 10_556 . ?
O4 C14 O5 117.5(3) . . ?
O4 C14 Gd1 178.3(4) 10_556 . ?
O4 C14 Gd1 55.21(19) . . ?
O5 C14 Gd1 62.29(10) . . ?
O4 C14 Gd1 55.21(19) 10_556 10_556 ?
O4 C14 Gd1 178.3(4) . 10_556 ?
O5 C14 Gd1 62.29(10) . 10_556 ?
Gd1 C14 Gd1 124.5(2) . 10_556 ?
Gd1 O3 Gd2 98.80(10) 5_665 . ?
Gd1 O3 Gd1 137.73(12) 5_665 . ?
Gd2 O3 Gd1 97.69(10) . . ?
Gd1 O3 H3 106(3) 5_665 . ?
Gd2 O3 H3 109(3) . . ?
Gd1 O3 H3 105(3) . . ?
C12 C11 C10 120.6(6) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C9 C10 C11 118.9(5) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C15 O6 Gd1 132.6(3) . . ?
C15 O6 H6 109(4) . . ?
Gd1 O6 H6 118(4) . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 O4 Gd1 98.9(3) . . ?
O9 C18 O9 117.2(9) . 3_655 ?
O9 C18 O9 117.2(9) . 5_665 ?
O9 C18 O9 117.2(9) 3_655 5_665 ?
O8 C17 O8 95.3(14) . 10_556 ?
O10 C19 O10 136(3) 10_556 . ?

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
O2 Gd1 O5 C14 -43.4(4) . . . . ?
O1 Gd1 O5 C14 103.1(3) . . . . ?
O3 Gd1 O5 C14 -173.1(3) 3_655 . . . ?
O4 Gd1 O5 C14 -0.7(3) . . . . ?
O6 Gd1 O5 C14 175.0(3) . . . . ?
O3 Gd1 O5 C14 -95.2(3) . . . . ?
N1 Gd1 O5 C14 45.6(3) . . . . ?
Gd2 Gd1 O5 C14 -134.9(4) . . . . ?
O2 Gd1 O5 Gd2 91.46(15) . . . . ?
O1 Gd1 O5 Gd2 -122.03(13) . . . . ?
O3 Gd1 O5 Gd2 -38.21(10) 3_655 . . . ?
O4 Gd1 O5 Gd2 134.20(18) . . . . ?
O6 Gd1 O5 Gd2 -50.1(2) . . . . ?
O3 Gd1 O5 Gd2 39.68(10) . . . . ?
N1 Gd1 O5 Gd2 -179.52(12) . . . . ?
C14 Gd1 O5 Gd2 134.9(4) . . . . ?
O3 Gd2 O5 C14 -129.22(8) 12_656 . . . ?
O3 Gd2 O5 C14 129.22(8) 3_655 . . . ?
O3 Gd2 O5 C14 89.65(12) 5_665 . . . ?
O3 Gd2 O5 C14 -50.99(8) 10_556 . . . ?
O3 Gd2 O5 C14 -89.65(12) 8_666 . . . ?
O3 Gd2 O5 C14 50.99(8) . . . . ?
O5 Gd2 O5 C14 180.0 3_655 . . . ?
O5 Gd2 O5 C14 0.0 8_666 . . . ?
Gd1 Gd2 O5 C14 131.10(3) 3_655 . . . ?
Gd1 Gd2 O5 C14 -91.14(9) 10_556 . . . ?
Gd1 Gd2 O5 C14 -131.10(3) 12_656 . . . ?
O3 Gd2 O5 Gd1 -38.07(10) 12_656 . . 10_556 ?
O3 Gd2 O5 Gd1 -139.64(14) 3_655 . . 10_556 ?
O3 Gd2 O5 Gd1 -179.20(9) 5_665 . . 10_556 ?
O3 Gd2 O5 Gd1 40.16(10) 10_556 . . 10_556 ?
O3 Gd2 O5 Gd1 1.5(2) 8_666 . . 10_556 ?
O3 Gd2 O5 Gd1 142.13(14) . . . 10_556 ?
O5 Gd2 O5 Gd1 -88.86(9) 3_655 . . 10_556 ?
O5 Gd2 O5 Gd1 91.14(9) 8_666 . . 10_556 ?
Gd1 Gd2 O5 Gd1 -137.75(7) 3_655 . . 10_556 ?
Gd1 Gd2 O5 Gd1 -39.96(12) 12_656 . . 10_556 ?
O3 Gd2 O5 Gd1 139.64(14) 12_656 . . . ?
O3 Gd2 O5 Gd1 38.07(10) 3_655 . . . ?
O3 Gd2 O5 Gd1 -1.5(2) 5_665 . . . ?
O3 Gd2 O5 Gd1 -142.13(14) 10_556 . . . ?
O3 Gd2 O5 Gd1 179.20(9) 8_666 . . . ?
O3 Gd2 O5 Gd1 -40.16(10) . . . . ?
O5 Gd2 O5 Gd1 88.86(9) 3_655 . . . ?
O5 Gd2 O5 Gd1 -91.14(9) 8_666 . . . ?
Gd1 Gd2 O5 Gd1 39.96(12) 3_655 . . . ?
Gd1 Gd2 O5 Gd1 177.71(18) 10_556 . . . ?
Gd1 Gd2 O5 Gd1 137.75(7) 12_656 . . . ?
O2 Gd1 O1 C1 38.9(4) . . . . ?
O3 Gd1 O1 C1 -174.0(3) 3_655 . . . ?
O4 Gd1 O1 C1 -50.8(3) . . . . ?
O6 Gd1 O1 C1 111.6(3) . . . . ?
O3 Gd1 O1 C1 -131.8(3) . . . . ?
N1 Gd1 O1 C1 23.2(3) . . . . ?
O5 Gd1 O1 C1 -102.3(3) . . . . ?
C14 Gd1 O1 C1 -75.4(3) . . . . ?
Gd2 Gd1 O1 C1 -139.9(3) . . . . ?
O2 Gd1 N1 C7 34.0(4) . . . . ?
O1 Gd1 N1 C7 -157.0(4) . . . . ?
O3 Gd1 N1 C7 173.3(3) 3_655 . . . ?
O4 Gd1 N1 C7 -56.8(4) . . . . ?
O6 Gd1 N1 C7 113.5(4) . . . . ?
O3 Gd1 N1 C7 -2.2(5) . . . . ?
O5 Gd1 N1 C7 -93.4(4) . . . . ?
C14 Gd1 N1 C7 -74.0(4) . . . . ?
Gd2 Gd1 N1 C7 -94.5(5) . . . . ?
O2 Gd1 N1 C6 -161.6(3) . . . . ?
O1 Gd1 N1 C6 7.5(3) . . . . ?
O3 Gd1 N1 C6 -22.2(4) 3_655 . . . ?
O4 Gd1 N1 C6 107.6(3) . . . . ?
O6 Gd1 N1 C6 -82.0(3) . . . . ?
O3 Gd1 N1 C6 162.3(3) . . . . ?
O5 Gd1 N1 C6 71.0(3) . . . . ?
C14 Gd1 N1 C6 90.5(3) . . . . ?
Gd2 Gd1 N1 C6 70.0(5) . . . . ?
C6 N1 C7 C8 178.2(4) . . . . ?
Gd1 N1 C7 C8 -17.8(7) . . . . ?
C6 C5 C4 C3 56.6(7) . . . . ?
Gd1 O1 C1 C2 -170.8(3) . . . . ?
Gd1 O1 C1 C6 -48.6(5) . . . . ?
C3 C2 C1 O1 66.0(6) . . . . ?
C3 C2 C1 C6 -54.0(6) . . . . ?
C1 C2 C3 C4 56.0(6) . . . . ?
C5 C4 C3 C2 -56.5(7) . . . . ?
C7 N1 C6 C5 -105.8(5) . . . . ?
Gd1 N1 C6 C5 88.5(4) . . . . ?
C7 N1 C6 C1 132.2(5) . . . . ?
Gd1 N1 C6 C1 -33.4(5) . . . . ?
C4 C5 C6 N1 -175.5(4) . . . . ?
C4 C5 C6 C1 -55.2(6) . . . . ?
O1 C1 C6 N1 51.0(5) . . . . ?
C2 C1 C6 N1 174.0(4) . . . . ?
O1 C1 C6 C5 -69.6(5) . . . . ?
C2 C1 C6 C5 53.4(6) . . . . ?
O2 C13 C8 C9 178.3(4) . . . . ?
C12 C13 C8 C9 -1.0(7) . . . . ?
O2 C13 C8 C7 -1.1(7) . . . . ?
C12 C13 C8 C7 179.6(5) . . . . ?
N1 C7 C8 C13 -8.9(8) . . . . ?
N1 C7 C8 C9 171.7(5) . . . . ?
O2 C13 C12 C11 179.9(5) . . . . ?
C8 C13 C12 C11 -0.7(8) . . . . ?
C13 C8 C9 C10 1.8(8) . . . . ?
C7 C8 C9 C10 -178.8(5) . . . . ?
C12 C13 O2 Gd1 -137.7(4) . . . . ?
C8 C13 O2 Gd1 43.0(6) . . . . ?
O1 Gd1 O2 C13 -63.1(4) . . . . ?
O3 Gd1 O2 C13 163.4(3) 3_655 . . . ?
O4 Gd1 O2 C13 29.4(4) . . . . ?
O6 Gd1 O2 C13 -139.3(4) . . . . ?
O3 Gd1 O2 C13 111.2(4) . . . . ?
N1 Gd1 O2 C13 -47.9(4) . . . . ?
O5 Gd1 O2 C13 62.5(4) . . . . ?
C14 Gd1 O2 C13 42.8(4) . . . . ?
Gd2 Gd1 O2 C13 115.6(4) . . . . ?
Gd1 O5 C14 O4 -1.2(5) 10_556 . . 10_556 ?
Gd1 O5 C14 O4 -178.1(5) . . . 10_556 ?
Gd2 O5 C14 O4 90.4(5) . . . 10_556 ?
Gd1 O5 C14 O4 178.1(5) 10_556 . . . ?
Gd1 O5 C14 O4 1.2(5) . . . . ?
Gd2 O5 C14 O4 -90.4(5) . . . . ?
Gd1 O5 C14 Gd1 176.96(18) 10_556 . . . ?
Gd2 O5 C14 Gd1 -91.52(9) . . . . ?
Gd1 O5 C14 Gd1 -176.96(18) . . . 10_556 ?
Gd2 O5 C14 Gd1 91.52(9) . . . 10_556 ?
O2 Gd1 C14 O4 -32.1(4) . . . . ?
O1 Gd1 C14 O4 108.0(3) . . . . ?
O3 Gd1 C14 O4 -172.2(3) 3_655 . . . ?
O3 Gd1 C14 O4 -103.1(3) . . . . ?
N1 Gd1 C14 O4 41.1(3) . . . . ?
O5 Gd1 C14 O4 -178.7(5) . . . . ?
Gd2 Gd1 C14 O4 -145.9(3) . . . . ?
O2 Gd1 C14 O5 146.7(3) . . . . ?
O1 Gd1 C14 O5 -73.3(3) . . . . ?
O3 Gd1 C14 O5 6.6(3) 3_655 . . . ?
O4 Gd1 C14 O5 178.7(5) . . . . ?
O3 Gd1 C14 O5 75.6(3) . . . . ?
N1 Gd1 C14 O5 -140.1(3) . . . . ?
Gd2 Gd1 C14 O5 32.9(3) . . . . ?
O2 Gd1 C14 Gd1 149.9(2) . . . 10_556 ?
O1 Gd1 C14 Gd1 -70.0(2) . . . 10_556 ?
O3 Gd1 C14 Gd1 9.8(3) 3_655 . . 10_556 ?
O4 Gd1 C14 Gd1 -178.0(5) . . . 10_556 ?
O3 Gd1 C14 Gd1 78.9(2) . . . 10_556 ?
N1 Gd1 C14 Gd1 -136.8(2) . . . 10_556 ?
O5 Gd1 C14 Gd1 3.27(19) . . . 10_556 ?
Gd2 Gd1 C14 Gd1 36.14(18) . . . 10_556 ?
O3 Gd2 O3 Gd1 -176.35(11) 12_656 . . 5_665 ?
O3 Gd2 O3 Gd1 109.20(6) 3_655 . . 5_665 ?
O3 Gd2 O3 Gd1 32.45(11) 5_665 . . 5_665 ?
O3 Gd2 O3 Gd1 -109.18(9) 10_556 . . 5_665 ?
O3 Gd2 O3 Gd1 -42.00(7) 8_666 . . 5_665 ?
O5 Gd2 O3 Gd1 71.33(17) 3_655 . . 5_665 ?
O5 Gd2 O3 Gd1 -176.04(13) . . . 5_665 ?
O5 Gd2 O3 Gd1 -41.70(10) 8_666 . . 5_665 ?
Gd1 Gd2 O3 Gd1 70.29(8) 3_655 . . 5_665 ?
Gd1 Gd2 O3 Gd1 -149.50(6) 10_556 . . 5_665 ?
O3 Gd2 O3 Gd1 42.71(7) 12_656 . . . ?
O3 Gd2 O3 Gd1 -31.74(11) 3_655 . . . ?
O3 Gd2 O3 Gd1 -108.50(6) 5_665 . . . ?
O3 Gd2 O3 Gd1 109.88(9) 10_556 . . . ?
O3 Gd2 O3 Gd1 177.05(10) 8_666 . . . ?
O5 Gd2 O3 Gd1 -69.62(17) 3_655 . . . ?
O5 Gd2 O3 Gd1 43.01(10) . . . . ?
O5 Gd2 O3 Gd1 177.36(12) 8_666 . . . ?
Gd1 Gd2 O3 Gd1 -70.66(8) 3_655 . . . ?
Gd1 Gd2 O3 Gd1 69.55(8) 10_556 . . . ?
O2 Gd1 O3 Gd1 61.95(18) . . . 5_665 ?
O1 Gd1 O3 Gd1 -124.4(2) . . . 5_665 ?
O3 Gd1 O3 Gd1 -80.25(19) 3_655 . . 5_665 ?
O4 Gd1 O3 Gd1 150.43(19) . . . 5_665 ?
O6 Gd1 O3 Gd1 -13.1(2) . . . 5_665 ?
N1 Gd1 O3 Gd1 97.0(2) . . . 5_665 ?
O5 Gd1 O3 Gd1 -155.4(2) . . . 5_665 ?
C14 Gd1 O3 Gd1 175.9(2) . . . 5_665 ?
Gd2 Gd1 O3 Gd1 -112.2(2) . . . 5_665 ?
O2 Gd1 O3 Gd2 174.17(12) . . . . ?
O1 Gd1 O3 Gd2 -12.1(2) . . . . ?
O3 Gd1 O3 Gd2 31.96(11) 3_655 . . . ?
O4 Gd1 O3 Gd2 -97.36(11) . . . . ?
O6 Gd1 O3 Gd2 99.09(11) . . . . ?
N1 Gd1 O3 Gd2 -150.81(16) . . . . ?
O5 Gd1 O3 Gd2 -43.21(11) . . . . ?
C14 Gd1 O3 Gd2 -71.88(13) . . . . ?
C13 C12 C11 C10 1.8(9) . . . . ?
C8 C9 C10 C11 -0.8(10) . . . . ?
C12 C11 C10 C9 -1.0(10) . . . . ?
O2 Gd1 O6 C15 32.0(4) . . . . ?
O1 Gd1 O6 C15 -107.7(4) . . . . ?
O3 Gd1 O6 C15 171.8(5) 3_655 . . . ?
O4 Gd1 O6 C15 -7.8(7) . . . . ?
O3 Gd1 O6 C15 106.1(4) . . . . ?
N1 Gd1 O6 C15 -40.1(4) . . . . ?
O5 Gd1 O6 C15 -176.5(4) . . . . ?
Gd2 Gd1 O6 C15 149.0(4) . . . . ?
O4 C14 O4 Gd1 178.0(5) 10_556 . . . ?
O5 C14 O4 Gd1 -1.2(5) . . . . ?
O2 Gd1 O4 C14 149.8(3) . . . . ?
O1 Gd1 O4 C14 -72.0(3) . . . . ?
O3 Gd1 O4 C14 9.3(4) 3_655 . . . ?
O6 Gd1 O4 C14 -171.1(4) . . . . ?
O3 Gd1 O4 C14 71.4(3) . . . . ?
N1 Gd1 O4 C14 -137.8(3) . . . . ?
O5 Gd1 O4 C14 0.7(3) . . . . ?
Gd2 Gd1 O4 C14 30.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         2.045
_refine_diff_density_min         -2.267
_refine_diff_density_rms         0.133

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.003 662 397 ' '
_platon_squeeze_details          
;
;

#============================================================================#
#      Luis Cunha-Silva @ REQUIMTE & DQB FCUP  *  12/03/2014  *   END        #
#============================================================================#  
_database_code_depnum_ccdc_archive 'CCDC 991355'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_em112c

# ========================================================================= #

_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_audit_creation_date             '07 March 2014'

# ========================================================================= #

_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C87 H120 N6 O33 Tb7, 3(C H4 O)'
_chemical_formula_sum            'C90 H132 N6 O36 Tb7'
_chemical_formula_weight         2986.46

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

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

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

_cell_length_a                   15.7469(9)
_cell_length_b                   15.7469(9)
_cell_length_c                   27.835(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5977.5(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9254
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.39

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2914
_exptl_absorpt_coefficient_mu    4.156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6813
_exptl_absorpt_correction_T_max  0.7886
_exptl_absorpt_process_details   
;
 SADABS (Sheldrick, 1997)
;


_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            64198
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.71
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3555
_reflns_number_gt                3256
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'APEX2 '
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_computing_structure_refinement  'SHELXTL '
_computing_molecular_graphics    'SHELXTL '
_computing_publication_material  'SHELXTL '

_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)+(0.1068P)²+119.8300P] 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         3555
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0893
_refine_ls_wR_factor_ref         0.2228
_refine_ls_wR_factor_gt          0.2180
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb2 Tb 0.3333 0.6667 0.7500 0.0241(3) Uani 1 6 d S . .
Tb1 Tb 0.50991(5) 0.70542(5) 0.65703(2) 0.0440(3) Uani 1 1 d . . .
O5 O 0.5102(9) 0.7055(9) 0.7500 0.042(3) Uani 1 2 d S . .
O4 O 0.6358(7) 0.8195(7) 0.7090(3) 0.046(2) Uani 1 1 d . . .
O1 O 0.5526(7) 0.5866(8) 0.6759(4) 0.052(2) Uani 1 1 d . . .
O2 O 0.5560(7) 0.8303(7) 0.6034(3) 0.051(2) Uani 1 1 d . . .
N1 N 0.6651(10) 0.7316(10) 0.6155(4) 0.060(3) Uani 1 1 d . . .
O6 O 0.4371(9) 0.6088(9) 0.5875(4) 0.073(3) Uani 1 1 d . . .
H6 H 0.3840 0.5456 0.5950 0.087 Uiso 1 1 calc R . .
C3 C 0.6089(14) 0.4403(16) 0.6401(7) 0.076(5) Uani 1 1 d . . .
H3A H 0.6174 0.3829 0.6456 0.091 Uiso 1 1 calc R . .
H3B H 0.5378 0.4174 0.6417 0.091 Uiso 1 1 calc R . .
C6 C 0.6896(12) 0.6539(13) 0.6230(6) 0.062(4) Uani 1 1 d . . .
H2 H 0.7623 0.6822 0.6219 0.075 Uiso 1 1 calc R . .
C8 C 0.7237(11) 0.8928(12) 0.5809(5) 0.053(4) Uani 1 1 d . . .
C1 C 0.6496(13) 0.6064(14) 0.6718(7) 0.067(4) Uani 1 1 d . . .
H1 H 0.6891 0.6555 0.6971 0.081 Uiso 1 1 calc R . .
C4 C 0.6462(17) 0.4808(16) 0.5907(10) 0.099(8) Uani 1 1 d . . .
H4A H 0.6063 0.4316 0.5661 0.118 Uiso 1 1 calc R . .
H4B H 0.7151 0.4963 0.5872 0.118 Uiso 1 1 calc R . .
C7 C 0.7320(11) 0.8097(12) 0.5946(6) 0.058(4) Uani 1 1 d . . .
H7 H 0.7923 0.8122 0.5876 0.069 Uiso 1 1 calc R . .
C9 C 0.8112(13) 0.9719(13) 0.5608(7) 0.071(5) Uani 1 1 d . . .
H9 H 0.8687 0.9669 0.5578 0.086 Uiso 1 1 calc R . .
C2 C 0.6609(15) 0.5145(16) 0.6798(8) 0.075(5) Uani 1 1 d . . .
H2A H 0.7313 0.5344 0.6800 0.090 Uiso 1 1 calc R . .
H2B H 0.6326 0.4845 0.7113 0.090 Uiso 1 1 calc R . .
O7 O 0.4560(11) 0.4894(11) 0.7500 0.056(4) Uiso 1 2 d S . .
C14 C 0.5950(13) 0.7833(13) 0.7500 0.038(4) Uani 1 2 d S . .
C12 C 0.6469(15) 0.9906(13) 0.5696(7) 0.072(5) Uani 1 1 d . . .
H12 H 0.5911 0.9986 0.5725 0.087 Uiso 1 1 calc R . .
C13 C 0.6392(11) 0.9029(13) 0.5848(5) 0.055(4) Uani 1 1 d . . .
C16 C 0.4541(14) 0.6232(14) 0.5380(5) 0.068(5) Uani 1 1 d . . .
H16A H 0.4282 0.6642 0.5260 0.101 Uiso 1 1 calc R . .
H16B H 0.4212 0.5596 0.5216 0.101 Uiso 1 1 calc R . .
H16C H 0.5247 0.6557 0.5318 0.101 Uiso 1 1 calc R . .
C17 C 0.415(3) 0.379(3) 0.7500 0.097(10) Uiso 1 2 d S . .
C11 C 0.7286(17) 1.0636(15) 0.5512(6) 0.086(7) Uani 1 1 d . . .
H11 H 0.7297 1.1220 0.5416 0.103 Uiso 1 1 calc R . .
C10 C 0.8112(16) 1.0568(14) 0.5457(7) 0.080(6) Uani 1 1 d . . .
H10 H 0.8683 1.1093 0.5316 0.096 Uiso 1 1 calc R . .
C5 C 0.6398(15) 0.5749(14) 0.5836(7) 0.075(5) Uani 1 1 d . . .
H5A H 0.6699 0.6043 0.5523 0.090 Uiso 1 1 calc R . .
H5B H 0.5697 0.5561 0.5819 0.090 Uiso 1 1 calc R . .
O3 O 0.4229(6) 0.7812(6) 0.6882(3) 0.038(2) Uani 1 1 d . . .
H3 H 0.4718 0.8439 0.7040 0.045 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
Tb2 O3 2.379(8) 3_665 ?
Tb2 O3 2.379(8) 12_667 ?
Tb2 O3 2.379(8) 10_557 ?
Tb2 O3 2.379(8) . ?
Tb2 O3 2.379(8) 5_565 ?
Tb2 O3 2.379(8) 8_567 ?
Tb2 O5 2.535(13) 3_665 ?
Tb2 O5 2.535(13) 8_567 ?
Tb2 O5 2.535(13) . ?
Tb1 O2 2.280(9) . ?
Tb1 O1 2.342(10) . ?
Tb1 O6 2.373(11) . ?
Tb1 O4 2.385(10) . ?
Tb1 O3 2.386(8) . ?
Tb1 O3 2.389(9) 5_565 ?
Tb1 N1 2.543(12) . ?
Tb1 O5 2.5879(7) . ?
O5 C14 1.28(2) . ?
O5 Tb1 2.5879(7) 10_557 ?
O4 C14 1.293(12) . ?
O1 C1 1.40(2) . ?
O2 C13 1.339(18) . ?
N1 C7 1.29(2) . ?
N1 C6 1.47(2) . ?
O6 C16 1.400(18) . ?
O6 H6 0.9500 . ?
C3 C4 1.51(3) . ?
C3 C2 1.52(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C6 C1 1.53(2) . ?
C6 C5 1.55(3) . ?
C6 H2 1.0000 . ?
C8 C13 1.42(2) . ?
C8 C9 1.43(2) . ?
C8 C7 1.43(2) . ?
C1 C2 1.56(3) . ?
C1 H1 1.0000 . ?
C4 C5 1.55(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 H7 0.9500 . ?
C9 C10 1.40(3) . ?
C9 H9 0.9500 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O7 C17 1.52(4) . ?
C14 O4 1.293(12) 10_557 ?
C12 C11 1.33(3) . ?
C12 C13 1.39(2) . ?
C12 H12 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C11 C10 1.37(3) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
O3 Tb1 2.389(9) 3_665 ?
O3 H3 1.0000 . ?

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
O3 Tb2 O3 92.6(4) 3_665 12_667 ?
O3 Tb2 O3 139.60(17) 3_665 10_557 ?
O3 Tb2 O3 73.5(3) 12_667 10_557 ?
O3 Tb2 O3 73.5(3) 3_665 . ?
O3 Tb2 O3 139.60(17) 12_667 . ?
O3 Tb2 O3 92.6(5) 10_557 . ?
O3 Tb2 O3 73.5(3) 3_665 5_565 ?
O3 Tb2 O3 139.60(18) 12_667 5_565 ?
O3 Tb2 O3 139.60(18) 10_557 5_565 ?
O3 Tb2 O3 73.5(3) . 5_565 ?
O3 Tb2 O3 139.60(18) 3_665 8_567 ?
O3 Tb2 O3 73.5(3) 12_667 8_567 ?
O3 Tb2 O3 73.5(3) 10_557 8_567 ?
O3 Tb2 O3 139.60(18) . 8_567 ?
O3 Tb2 O3 92.6(4) 5_565 8_567 ?
O3 Tb2 O5 69.8(3) 3_665 3_665 ?
O3 Tb2 O5 69.8(3) 12_667 3_665 ?
O3 Tb2 O5 69.8(3) 10_557 3_665 ?
O3 Tb2 O5 69.8(3) . 3_665 ?
O3 Tb2 O5 133.7(2) 5_565 3_665 ?
O3 Tb2 O5 133.7(2) 8_567 3_665 ?
O3 Tb2 O5 69.8(3) 3_665 8_567 ?
O3 Tb2 O5 69.8(3) 12_667 8_567 ?
O3 Tb2 O5 133.7(2) 10_557 8_567 ?
O3 Tb2 O5 133.7(2) . 8_567 ?
O3 Tb2 O5 69.8(3) 5_565 8_567 ?
O3 Tb2 O5 69.8(3) 8_567 8_567 ?
O5 Tb2 O5 120.000(3) 3_665 8_567 ?
O3 Tb2 O5 133.7(2) 3_665 . ?
O3 Tb2 O5 133.7(2) 12_667 . ?
O3 Tb2 O5 69.8(3) 10_557 . ?
O3 Tb2 O5 69.8(3) . . ?
O3 Tb2 O5 69.8(3) 5_565 . ?
O3 Tb2 O5 69.8(3) 8_567 . ?
O5 Tb2 O5 120.000(3) 3_665 . ?
O5 Tb2 O5 120.000(1) 8_567 . ?
O3 Tb2 Tb1 40.6(2) 3_665 3_665 ?
O3 Tb2 Tb1 106.0(2) 12_667 3_665 ?
O3 Tb2 Tb1 106.0(2) 10_557 3_665 ?
O3 Tb2 Tb1 40.7(2) . 3_665 ?
O3 Tb2 Tb1 88.0(2) 5_565 3_665 ?
O3 Tb2 Tb1 179.3(2) 8_567 3_665 ?
O5 Tb2 Tb1 45.635(12) 3_665 3_665 ?
O5 Tb2 Tb1 110.47(19) 8_567 3_665 ?
O5 Tb2 Tb1 110.45(19) . 3_665 ?
O3 Tb2 Tb1 106.0(2) 3_665 12_667 ?
O3 Tb2 Tb1 40.6(2) 12_667 12_667 ?
O3 Tb2 Tb1 40.7(2) 10_557 12_667 ?
O3 Tb2 Tb1 106.0(2) . 12_667 ?
O3 Tb2 Tb1 179.3(2) 5_565 12_667 ?
O3 Tb2 Tb1 88.0(2) 8_567 12_667 ?
O5 Tb2 Tb1 45.635(12) 3_665 12_667 ?
O5 Tb2 Tb1 110.47(19) 8_567 12_667 ?
O5 Tb2 Tb1 110.45(19) . 12_667 ?
Tb1 Tb2 Tb1 91.27(2) 3_665 12_667 ?
O3 Tb2 Tb1 40.7(2) 3_665 5_565 ?
O3 Tb2 Tb1 106.0(2) 12_667 5_565 ?
O3 Tb2 Tb1 179.3(2) 10_557 5_565 ?
O3 Tb2 Tb1 88.0(2) . 5_565 ?
O3 Tb2 Tb1 40.6(2) 5_565 5_565 ?
O3 Tb2 Tb1 106.0(2) 8_567 5_565 ?
O5 Tb2 Tb1 110.45(19) 3_665 5_565 ?
O5 Tb2 Tb1 45.635(13) 8_567 5_565 ?
O5 Tb2 Tb1 110.47(19) . 5_565 ?
Tb1 Tb2 Tb1 74.537(19) 3_665 5_565 ?
Tb1 Tb2 Tb1 139.073(10) 12_667 5_565 ?
O2 Tb1 O1 137.9(3) . . ?
O2 Tb1 O6 82.1(4) . . ?
O1 Tb1 O6 84.9(4) . . ?
O2 Tb1 O4 87.8(3) . . ?
O1 Tb1 O4 90.2(3) . . ?
O6 Tb1 O4 158.6(4) . . ?
O2 Tb1 O3 79.7(3) . . ?
O1 Tb1 O3 141.6(3) . . ?
O6 Tb1 O3 113.8(4) . . ?
O4 Tb1 O3 82.6(3) . . ?
O2 Tb1 O3 136.0(3) . 5_565 ?
O1 Tb1 O3 78.9(3) . 5_565 ?
O6 Tb1 O3 78.2(3) . 5_565 ?
O4 Tb1 O3 121.3(3) . 5_565 ?
O3 Tb1 O3 73.2(4) . 5_565 ?
O2 Tb1 N1 72.3(4) . . ?
O1 Tb1 N1 66.1(4) . . ?
O6 Tb1 N1 81.4(4) . . ?
O4 Tb1 N1 77.6(4) . . ?
O3 Tb1 N1 146.1(4) . . ?
O3 Tb1 N1 140.8(4) 5_565 . ?
O2 Tb1 O5 130.9(4) . . ?
O1 Tb1 O5 77.0(4) . . ?
O6 Tb1 O5 144.7(4) . . ?
O4 Tb1 O5 52.6(3) . . ?
O3 Tb1 O5 68.7(3) . . ?
O3 Tb1 O5 68.8(3) 5_565 . ?
N1 Tb1 O5 117.0(4) . . ?
O2 Tb1 C14 109.9(4) . . ?
O1 Tb1 C14 83.1(4) . . ?
O6 Tb1 C14 167.2(5) . . ?
O4 Tb1 C14 26.2(4) . . ?
O3 Tb1 C14 73.9(4) . . ?
O3 Tb1 C14 95.1(4) 5_565 . ?
N1 Tb1 C14 97.7(4) . . ?
O5 Tb1 C14 26.4(4) . . ?
O2 Tb1 Tb2 120.0(2) . . ?
O1 Tb1 Tb2 102.0(2) . . ?
O6 Tb1 Tb2 113.0(3) . . ?
O4 Tb1 Tb2 88.4(2) . . ?
O3 Tb1 Tb2 40.49(19) . . ?
O3 Tb1 Tb2 40.50(18) 5_565 . ?
N1 Tb1 Tb2 161.3(3) . . ?
O5 Tb1 Tb2 44.5(3) . . ?
C14 Tb1 Tb2 65.5(3) . . ?
C14 O5 Tb2 136.4(11) . . ?
C14 O5 Tb1 90.1(3) . . ?
Tb2 O5 Tb1 89.9(3) . . ?
C14 O5 Tb1 90.1(3) . 10_557 ?
Tb2 O5 Tb1 89.9(3) . 10_557 ?
Tb1 O5 Tb1 179.8(5) . 10_557 ?
C14 O4 Tb1 99.3(9) . . ?
C1 O1 Tb1 121.3(10) . . ?
C13 O2 Tb1 138.0(9) . . ?
C7 N1 C6 115.3(13) . . ?
C7 N1 Tb1 128.3(11) . . ?
C6 N1 Tb1 115.6(10) . . ?
C16 O6 Tb1 135.0(11) . . ?
C16 O6 H6 112.5 . . ?
Tb1 O6 H6 112.5 . . ?
C4 C3 C2 113.1(19) . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N1 C6 C1 108.5(13) . . ?
N1 C6 C5 109.3(14) . . ?
C1 C6 C5 108.5(15) . . ?
N1 C6 H2 110.2 . . ?
C1 C6 H2 110.2 . . ?
C5 C6 H2 110.2 . . ?
C13 C8 C9 118.8(16) . . ?
C13 C8 C7 127.0(14) . . ?
C9 C8 C7 114.3(15) . . ?
O1 C1 C6 108.6(15) . . ?
O1 C1 C2 113.6(15) . . ?
C6 C1 C2 111.7(15) . . ?
O1 C1 H1 107.6 . . ?
C6 C1 H1 107.6 . . ?
C2 C1 H1 107.6 . . ?
C3 C4 C5 108.9(16) . . ?
C3 C4 H4A 109.9 . . ?
C5 C4 H4A 109.9 . . ?
C3 C4 H4B 109.9 . . ?
C5 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N1 C7 C8 125.9(14) . . ?
N1 C7 H7 117.0 . . ?
C8 C7 H7 117.0 . . ?
C10 C9 C8 119.2(19) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C3 C2 C1 110.1(16) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
O5 C14 O4 118.1(8) . 10_557 ?
O5 C14 O4 118.1(8) . . ?
O4 C14 O4 123.8(16) 10_557 . ?
O5 C14 Tb1 63.6(3) . . ?
O4 C14 Tb1 178.2(11) 10_557 . ?
O4 C14 Tb1 54.5(6) . . ?
O5 C14 Tb1 63.6(3) . 10_557 ?
O4 C14 Tb1 54.5(6) 10_557 10_557 ?
O4 C14 Tb1 178.2(11) . 10_557 ?
Tb1 C14 Tb1 127.1(6) . 10_557 ?
C11 C12 C13 123(2) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
O2 C13 C12 121.8(15) . . ?
O2 C13 C8 120.4(15) . . ?
C12 C13 C8 117.8(15) . . ?
O6 C16 H16A 109.5 . . ?
O6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C11 C10 122(2) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C10 C9 119.7(18) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C6 C5 C4 115.5(17) . . ?
C6 C5 H5A 108.4 . . ?
C4 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
C4 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
Tb2 O3 Tb1 98.9(3) . . ?
Tb2 O3 Tb1 98.8(3) . 3_665 ?
Tb1 O3 Tb1 133.3(4) . 3_665 ?
Tb2 O3 H3 107.6 . . ?
Tb1 O3 H3 107.6 . . ?
Tb1 O3 H3 107.6 3_665 . ?

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
O3 Tb2 Tb1 O2 60.5(4) 3_665 . . . ?
O3 Tb2 Tb1 O2 -81.0(4) 10_557 . . . ?
O3 Tb2 Tb1 O2 -6.1(4) . . . . ?
O3 Tb2 Tb1 O2 127.1(5) 5_565 . . . ?
O3 Tb2 Tb1 O2 -157.9(4) 8_567 . . . ?
O5 Tb2 Tb1 O2 -7.0(4) 3_665 . . . ?
O5 Tb2 Tb1 O2 128.2(4) 8_567 . . . ?
O5 Tb2 Tb1 O2 -119.4(5) . . . . ?
Tb1 Tb2 Tb1 O2 21.6(3) 3_665 . . . ?
Tb1 Tb2 Tb1 O2 -51.9(3) 12_667 . . . ?
Tb1 Tb2 Tb1 O2 99.5(3) 5_565 . . . ?
O3 Tb2 Tb1 O1 -123.1(3) 3_665 . . . ?
O3 Tb2 Tb1 O1 95.4(3) 10_557 . . . ?
O3 Tb2 Tb1 O1 170.3(4) . . . . ?
O3 Tb2 Tb1 O1 -56.5(4) 5_565 . . . ?
O3 Tb2 Tb1 O1 18.4(3) 8_567 . . . ?
O5 Tb2 Tb1 O1 169.4(4) 3_665 . . . ?
O5 Tb2 Tb1 O1 -55.5(4) 8_567 . . . ?
O5 Tb2 Tb1 O1 57.0(5) . . . . ?
Tb1 Tb2 Tb1 O1 -162.0(3) 3_665 . . . ?
Tb1 Tb2 Tb1 O1 124.5(3) 12_667 . . . ?
Tb1 Tb2 Tb1 O1 -84.1(3) 5_565 . . . ?
O3 Tb2 Tb1 O6 -33.6(4) 3_665 . . . ?
O3 Tb2 Tb1 O6 -175.1(4) 10_557 . . . ?
O3 Tb2 Tb1 O6 -100.2(5) . . . . ?
O3 Tb2 Tb1 O6 33.0(5) 5_565 . . . ?
O3 Tb2 Tb1 O6 107.9(4) 8_567 . . . ?
O5 Tb2 Tb1 O6 -101.1(4) 3_665 . . . ?
O5 Tb2 Tb1 O6 34.0(4) 8_567 . . . ?
O5 Tb2 Tb1 O6 146.5(5) . . . . ?
Tb1 Tb2 Tb1 O6 -72.5(4) 3_665 . . . ?
Tb1 Tb2 Tb1 O6 -146.0(4) 12_667 . . . ?
Tb1 Tb2 Tb1 O6 5.4(4) 5_565 . . . ?
O3 Tb2 Tb1 O4 147.1(3) 3_665 . . . ?
O3 Tb2 Tb1 O4 5.6(3) 10_557 . . . ?
O3 Tb2 Tb1 O4 80.5(4) . . . . ?
O3 Tb2 Tb1 O4 -146.3(4) 5_565 . . . ?
O3 Tb2 Tb1 O4 -71.4(3) 8_567 . . . ?
O5 Tb2 Tb1 O4 79.6(3) 3_665 . . . ?
O5 Tb2 Tb1 O4 -145.3(3) 8_567 . . . ?
O5 Tb2 Tb1 O4 -32.9(5) . . . . ?
Tb1 Tb2 Tb1 O4 108.2(2) 3_665 . . . ?
Tb1 Tb2 Tb1 O4 34.7(2) 12_667 . . . ?
Tb1 Tb2 Tb1 O4 -174.0(2) 5_565 . . . ?
O3 Tb2 Tb1 O3 66.6(3) 3_665 . . . ?
O3 Tb2 Tb1 O3 -74.9(5) 10_557 . . . ?
O3 Tb2 Tb1 O3 133.2(6) 5_565 . . . ?
O3 Tb2 Tb1 O3 -151.89(18) 8_567 . . . ?
O5 Tb2 Tb1 O3 -0.9(4) 3_665 . . . ?
O5 Tb2 Tb1 O3 134.2(4) 8_567 . . . ?
O5 Tb2 Tb1 O3 -113.4(5) . . . . ?
Tb1 Tb2 Tb1 O3 27.7(3) 3_665 . . . ?
Tb1 Tb2 Tb1 O3 -45.8(3) 12_667 . . . ?
Tb1 Tb2 Tb1 O3 105.5(3) 5_565 . . . ?
O3 Tb2 Tb1 O3 -66.6(3) 3_665 . . 5_565 ?
O3 Tb2 Tb1 O3 151.87(18) 10_557 . . 5_565 ?
O3 Tb2 Tb1 O3 -133.2(6) . . . 5_565 ?
O3 Tb2 Tb1 O3 74.9(5) 8_567 . . 5_565 ?
O5 Tb2 Tb1 O3 -134.1(4) 3_665 . . 5_565 ?
O5 Tb2 Tb1 O3 1.0(4) 8_567 . . 5_565 ?
O5 Tb2 Tb1 O3 113.5(5) . . . 5_565 ?
Tb1 Tb2 Tb1 O3 -105.5(3) 3_665 . . 5_565 ?
Tb1 Tb2 Tb1 O3 -179.0(3) 12_667 . . 5_565 ?
Tb1 Tb2 Tb1 O3 -27.6(3) 5_565 . . 5_565 ?
O3 Tb2 Tb1 N1 -171.7(10) 3_665 . . . ?
O3 Tb2 Tb1 N1 46.8(10) 10_557 . . . ?
O3 Tb2 Tb1 N1 121.7(11) . . . . ?
O3 Tb2 Tb1 N1 -105.1(11) 5_565 . . . ?
O3 Tb2 Tb1 N1 -30.2(10) 8_567 . . . ?
O5 Tb2 Tb1 N1 120.8(10) 3_665 . . . ?
O5 Tb2 Tb1 N1 -104.1(10) 8_567 . . . ?
O5 Tb2 Tb1 N1 8.3(11) . . . . ?
Tb1 Tb2 Tb1 N1 149.4(10) 3_665 . . . ?
Tb1 Tb2 Tb1 N1 75.9(10) 12_667 . . . ?
Tb1 Tb2 Tb1 N1 -132.8(10) 5_565 . . . ?
O3 Tb2 Tb1 O5 179.9(5) 3_665 . . . ?
O3 Tb2 Tb1 O5 38.4(5) 10_557 . . . ?
O3 Tb2 Tb1 O5 113.4(5) . . . . ?
O3 Tb2 Tb1 O5 -113.5(5) 5_565 . . . ?
O3 Tb2 Tb1 O5 -38.5(5) 8_567 . . . ?
O5 Tb2 Tb1 O5 112.42(17) 3_665 . . . ?
O5 Tb2 Tb1 O5 -112.44(17) 8_567 . . . ?
Tb1 Tb2 Tb1 O5 141.1(4) 3_665 . . . ?
Tb1 Tb2 Tb1 O5 67.5(4) 12_667 . . . ?
Tb1 Tb2 Tb1 O5 -141.1(4) 5_565 . . . ?
O3 Tb2 Tb1 C14 160.3(4) 3_665 . . . ?
O3 Tb2 Tb1 C14 93.7(5) . . . . ?
O5 Tb2 Tb1 C14 92.7(4) 3_665 . . . ?
O5 Tb2 Tb1 C14 -132.1(4) 8_567 . . . ?
O5 Tb2 Tb1 C14 -19.7(5) . . . . ?
Tb1 Tb2 Tb1 C14 121.4(4) 3_665 . . . ?
Tb1 Tb2 Tb1 C14 47.9(4) 12_667 . . . ?
Tb1 Tb2 Tb1 C14 -160.8(4) 5_565 . . . ?
O3 Tb2 O5 C14 89.9(4) 3_665 . . . ?
O3 Tb2 O5 C14 -89.9(4) 12_667 . . . ?
O3 Tb2 O5 C14 -50.4(2) 10_557 . . . ?
O3 Tb2 O5 C14 50.4(2) . . . . ?
O3 Tb2 O5 C14 129.6(2) 5_565 . . . ?
O3 Tb2 O5 C14 -129.6(2) 8_567 . . . ?
O5 Tb2 O5 C14 0.0 3_665 . . . ?
O5 Tb2 O5 C14 180.0 8_567 . . . ?
Tb1 Tb2 O5 C14 49.73(8) 3_665 . . . ?
Tb1 Tb2 O5 C14 -49.73(8) 12_667 . . . ?
Tb1 Tb2 O5 C14 130.26(8) 5_565 . . . ?
O3 Tb2 O5 Tb1 -0.1(6) 3_665 . . . ?
O3 Tb2 O5 Tb1 -179.9(3) 12_667 . . . ?
O3 Tb2 O5 Tb1 -140.4(4) 10_557 . . . ?
O3 Tb2 O5 Tb1 -39.6(3) . . . . ?
O3 Tb2 O5 Tb1 39.6(3) 5_565 . . . ?
O3 Tb2 O5 Tb1 140.4(4) 8_567 . . . ?
O5 Tb2 O5 Tb1 -90.0(3) 3_665 . . . ?
O5 Tb2 O5 Tb1 90.0(3) 8_567 . . . ?
Tb1 Tb2 O5 Tb1 -40.3(4) 3_665 . . . ?
Tb1 Tb2 O5 Tb1 -139.7(2) 12_667 . . . ?
Tb1 Tb2 O5 Tb1 40.2(4) 5_565 . . . ?
O3 Tb2 O5 Tb1 179.9(3) 3_665 . . 10_557 ?
O3 Tb2 O5 Tb1 0.1(6) 12_667 . . 10_557 ?
O3 Tb2 O5 Tb1 39.6(3) 10_557 . . 10_557 ?
O3 Tb2 O5 Tb1 140.4(4) . . . 10_557 ?
O3 Tb2 O5 Tb1 -140.4(4) 5_565 . . 10_557 ?
O3 Tb2 O5 Tb1 -39.6(3) 8_567 . . 10_557 ?
O5 Tb2 O5 Tb1 90.0(3) 3_665 . . 10_557 ?
O5 Tb2 O5 Tb1 -90.0(3) 8_567 . . 10_557 ?
Tb1 Tb2 O5 Tb1 139.7(2) 3_665 . . 10_557 ?
Tb1 Tb2 O5 Tb1 40.3(4) 12_667 . . 10_557 ?
Tb1 Tb2 O5 Tb1 -139.7(2) 5_565 . . 10_557 ?
O2 Tb1 O5 C14 -42.8(11) . . . . ?
O1 Tb1 O5 C14 101.0(10) . . . . ?
O6 Tb1 O5 C14 162.0(10) . . . . ?
O4 Tb1 O5 C14 0.6(9) . . . . ?
O3 Tb1 O5 C14 -96.6(10) . . . . ?
O3 Tb1 O5 C14 -176.1(11) 5_565 . . . ?
N1 Tb1 O5 C14 46.6(11) . . . . ?
Tb2 Tb1 O5 C14 -136.4(11) . . . . ?
O2 Tb1 O5 Tb2 93.5(5) . . . . ?
O1 Tb1 O5 Tb2 -122.7(4) . . . . ?
O6 Tb1 O5 Tb2 -61.7(9) . . . . ?
O4 Tb1 O5 Tb2 136.9(6) . . . . ?
O3 Tb1 O5 Tb2 39.8(3) . . . . ?
O3 Tb1 O5 Tb2 -39.7(3) 5_565 . . . ?
N1 Tb1 O5 Tb2 -177.0(4) . . . . ?
C14 Tb1 O5 Tb2 136.4(11) . . . . ?
O2 Tb1 O4 C14 148.2(9) . . . . ?
O1 Tb1 O4 C14 -74.0(9) . . . . ?
O6 Tb1 O4 C14 -150.3(12) . . . . ?
O3 Tb1 O4 C14 68.3(9) . . . . ?
O3 Tb1 O4 C14 3.1(10) 5_565 . . . ?
N1 Tb1 O4 C14 -139.4(10) . . . . ?
O5 Tb1 O4 C14 -0.6(9) . . . . ?
Tb2 Tb1 O4 C14 28.0(9) . . . . ?
O2 Tb1 O1 C1 34.6(14) . . . . ?
O6 Tb1 O1 C1 106.8(12) . . . . ?
O4 Tb1 O1 C1 -52.4(12) . . . . ?
O3 Tb1 O1 C1 -130.6(11) . . . . ?
O3 Tb1 O1 C1 -174.3(12) 5_565 . . . ?
N1 Tb1 O1 C1 23.9(11) . . . . ?
O5 Tb1 O1 C1 -103.7(12) . . . . ?
C14 Tb1 O1 C1 -77.7(12) . . . . ?
Tb2 Tb1 O1 C1 -140.8(11) . . . . ?
O1 Tb1 O2 C13 -42.6(16) . . . . ?
O6 Tb1 O2 C13 -115.8(14) . . . . ?
O4 Tb1 O2 C13 45.3(14) . . . . ?
O3 Tb1 O2 C13 128.2(14) . . . . ?
O3 Tb1 O2 C13 -179.6(12) 5_565 . . . ?
N1 Tb1 O2 C13 -32.4(13) . . . . ?
O5 Tb1 O2 C13 78.3(14) . . . . ?
C14 Tb1 O2 C13 59.6(14) . . . . ?
Tb2 Tb1 O2 C13 132.2(13) . . . . ?
O2 Tb1 N1 C7 23.5(13) . . . . ?
O1 Tb1 N1 C7 -163.9(14) . . . . ?
O6 Tb1 N1 C7 107.9(14) . . . . ?
O4 Tb1 N1 C7 -68.1(13) . . . . ?
O3 Tb1 N1 C7 -12.4(17) . . . . ?
O3 Tb1 N1 C7 167.1(12) 5_565 . . . ?
O5 Tb1 N1 C7 -104.0(14) . . . . ?
C14 Tb1 N1 C7 -85.0(14) . . . . ?
Tb2 Tb1 N1 C7 -110.5(15) . . . . ?
O2 Tb1 N1 C6 -167.3(12) . . . . ?
O1 Tb1 N1 C6 5.2(10) . . . . ?
O6 Tb1 N1 C6 -83.0(11) . . . . ?
O4 Tb1 N1 C6 101.0(11) . . . . ?
O3 Tb1 N1 C6 156.7(10) . . . . ?
O3 Tb1 N1 C6 -23.8(14) 5_565 . . . ?
O5 Tb1 N1 C6 65.1(12) . . . . ?
C14 Tb1 N1 C6 84.2(11) . . . . ?
Tb2 Tb1 N1 C6 58.6(16) . . . . ?
O2 Tb1 O6 C16 24.2(17) . . . . ?
O1 Tb1 O6 C16 -115.7(17) . . . . ?
O4 Tb1 O6 C16 -38(2) . . . . ?
O3 Tb1 O6 C16 99.2(17) . . . . ?
O3 Tb1 O6 C16 164.7(18) 5_565 . . . ?
N1 Tb1 O6 C16 -49.1(17) . . . . ?
O5 Tb1 O6 C16 -174.5(15) . . . . ?
C14 Tb1 O6 C16 -136(2) . . . . ?
Tb2 Tb1 O6 C16 143.5(16) . . . . ?
C7 N1 C6 C1 141.7(15) . . . . ?
Tb1 N1 C6 C1 -28.9(17) . . . . ?
C7 N1 C6 C5 -100.1(16) . . . . ?
Tb1 N1 C6 C5 89.3(14) . . . . ?
Tb1 O1 C1 C6 -47.8(17) . . . . ?
Tb1 O1 C1 C2 -172.7(11) . . . . ?
N1 C6 C1 O1 46.8(19) . . . . ?
C5 C6 C1 O1 -71.9(17) . . . . ?
N1 C6 C1 C2 172.8(15) . . . . ?
C5 C6 C1 C2 54.1(19) . . . . ?
C2 C3 C4 C5 -55(2) . . . . ?
C6 N1 C7 C8 176.3(15) . . . . ?
Tb1 N1 C7 C8 -15(2) . . . . ?
C13 C8 C7 N1 -4(3) . . . . ?
C9 C8 C7 N1 176.4(15) . . . . ?
C13 C8 C9 C10 0(2) . . . . ?
C7 C8 C9 C10 179.3(16) . . . . ?
C4 C3 C2 C1 58(2) . . . . ?
O1 C1 C2 C3 65(2) . . . . ?
C6 C1 C2 C3 -58(2) . . . . ?
Tb2 O5 C14 O4 90.9(14) . . . 10_557 ?
Tb1 O5 C14 O4 -179.2(14) . . . 10_557 ?
Tb1 O5 C14 O4 0.9(15) 10_557 . . 10_557 ?
Tb2 O5 C14 O4 -90.9(14) . . . . ?
Tb1 O5 C14 O4 -0.9(15) . . . . ?
Tb1 O5 C14 O4 179.2(14) 10_557 . . . ?
Tb2 O5 C14 Tb1 -90.0(3) . . . . ?
Tb1 O5 C14 Tb1 -179.9(6) 10_557 . . . ?
Tb2 O5 C14 Tb1 90.0(3) . . . 10_557 ?
Tb1 O5 C14 Tb1 179.9(6) . . . 10_557 ?
Tb1 O4 C14 O5 1.0(16) . . . . ?
Tb1 O4 C14 O4 179.2(14) . . . 10_557 ?
O2 Tb1 C14 O5 146.9(9) . . . . ?
O1 Tb1 C14 O5 -74.5(10) . . . . ?
O6 Tb1 C14 O5 -54(2) . . . . ?
O4 Tb1 C14 O5 -179.0(16) . . . . ?
O3 Tb1 C14 O5 74.5(10) . . . . ?
O3 Tb1 C14 O5 3.7(10) 5_565 . . . ?
N1 Tb1 C14 O5 -139.2(10) . . . . ?
Tb2 Tb1 C14 O5 32.1(9) . . . . ?
O2 Tb1 C14 O4 -34.1(10) . . . . ?
O1 Tb1 C14 O4 104.5(9) . . . . ?
O6 Tb1 C14 O4 124.9(19) . . . . ?
O3 Tb1 C14 O4 -106.5(9) . . . . ?
O3 Tb1 C14 O4 -177.3(9) 5_565 . . . ?
N1 Tb1 C14 O4 39.8(10) . . . . ?
O5 Tb1 C14 O4 179.0(16) . . . . ?
Tb2 Tb1 C14 O4 -148.9(10) . . . . ?
O2 Tb1 C14 Tb1 146.8(6) . . . 10_557 ?
O1 Tb1 C14 Tb1 -74.6(7) . . . 10_557 ?
O6 Tb1 C14 Tb1 -54(2) . . . 10_557 ?
O4 Tb1 C14 Tb1 -179.1(15) . . . 10_557 ?
O3 Tb1 C14 Tb1 74.4(7) . . . 10_557 ?
O3 Tb1 C14 Tb1 3.6(8) 5_565 . . 10_557 ?
N1 Tb1 C14 Tb1 -139.3(7) . . . 10_557 ?
O5 Tb1 C14 Tb1 -0.1(7) . . . 10_557 ?
Tb2 Tb1 C14 Tb1 32.0(6) . . . 10_557 ?
Tb1 O2 C13 C12 -150.8(13) . . . . ?
Tb1 O2 C13 C8 28(2) . . . . ?
C11 C12 C13 O2 179.9(16) . . . . ?
C11 C12 C13 C8 1(3) . . . . ?
C9 C8 C13 O2 179.9(14) . . . . ?
C7 C8 C13 O2 1(2) . . . . ?
C9 C8 C13 C12 -1(2) . . . . ?
C7 C8 C13 C12 179.6(16) . . . . ?
C13 C12 C11 C10 0(3) . . . . ?
C12 C11 C10 C9 -2(3) . . . . ?
C8 C9 C10 C11 1(3) . . . . ?
N1 C6 C5 C4 -171.5(15) . . . . ?
C1 C6 C5 C4 -53(2) . . . . ?
C3 C4 C5 C6 53(2) . . . . ?
O3 Tb2 O3 Tb1 -106.93(18) 3_665 . . . ?
O3 Tb2 O3 Tb1 179.0(3) 12_667 . . . ?
O3 Tb2 O3 Tb1 111.7(3) 10_557 . . . ?
O3 Tb2 O3 Tb1 -29.7(4) 5_565 . . . ?
O3 Tb2 O3 Tb1 44.3(2) 8_567 . . . ?
O5 Tb2 O3 Tb1 179.1(4) 3_665 . . . ?
O5 Tb2 O3 Tb1 -68.2(5) 8_567 . . . ?
O5 Tb2 O3 Tb1 44.4(3) . . . . ?
Tb1 Tb2 O3 Tb1 -136.6(5) 3_665 . . . ?
Tb1 Tb2 O3 Tb1 150.7(2) 12_667 . . . ?
Tb1 Tb2 O3 Tb1 -68.3(3) 5_565 . . . ?
O3 Tb2 O3 Tb1 29.7(4) 3_665 . . 3_665 ?
O3 Tb2 O3 Tb1 -44.4(2) 12_667 . . 3_665 ?
O3 Tb2 O3 Tb1 -111.7(3) 10_557 . . 3_665 ?
O3 Tb2 O3 Tb1 106.89(19) 5_565 . . 3_665 ?
O3 Tb2 O3 Tb1 -179.0(3) 8_567 . . 3_665 ?
O5 Tb2 O3 Tb1 -44.3(3) 3_665 . . 3_665 ?
O5 Tb2 O3 Tb1 68.4(5) 8_567 . . 3_665 ?
O5 Tb2 O3 Tb1 -179.0(4) . . . 3_665 ?
Tb1 Tb2 O3 Tb1 -72.6(3) 12_667 . . 3_665 ?
Tb1 Tb2 O3 Tb1 68.3(3) 5_565 . . 3_665 ?
O2 Tb1 O3 Tb2 174.7(4) . . . . ?
O1 Tb1 O3 Tb2 -15.4(7) . . . . ?
O6 Tb1 O3 Tb2 98.2(4) . . . . ?
O4 Tb1 O3 Tb2 -96.2(3) . . . . ?
O3 Tb1 O3 Tb2 29.7(4) 5_565 . . . ?
N1 Tb1 O3 Tb2 -150.7(6) . . . . ?
O5 Tb1 O3 Tb2 -43.6(4) . . . . ?
C14 Tb1 O3 Tb2 -70.9(4) . . . . ?
O2 Tb1 O3 Tb1 63.6(5) . . . 3_665 ?
O1 Tb1 O3 Tb1 -126.5(5) . . . 3_665 ?
O6 Tb1 O3 Tb1 -12.9(6) . . . 3_665 ?
O4 Tb1 O3 Tb1 152.7(5) . . . 3_665 ?
O3 Tb1 O3 Tb1 -81.4(5) 5_565 . . 3_665 ?
N1 Tb1 O3 Tb1 98.2(8) . . . 3_665 ?
O5 Tb1 O3 Tb1 -154.7(6) . . . 3_665 ?
C14 Tb1 O3 Tb1 178.0(6) . . . 3_665 ?
Tb2 Tb1 O3 Tb1 -111.1(6) . . . 3_665 ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         6.336
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.248


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 7 0 ' '
2 0.000 0.000 0.250 485 186 ' '
3 0.000 0.000 0.500 7 0 ' '
4 0.000 0.000 0.750 485 186 ' '
5 0.333 0.667 0.250 40 34 ' '
6 0.667 0.333 0.750 40 34 ' '
_platon_squeeze_details          
;
;


#============================================================================#
#      Luis Cunha-Silva @ REQUIMTE & DQB FCUP  *  13/03/2014  *   END        #
#============================================================================#  
_database_code_depnum_ccdc_archive 'CCDC 991356'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_em44c

# ========================================================================= #

_audit_creation_method           'SHELXL-97, manual editing plus enCIFer'
_audit_creation_date             '07 March 2014'

# ========================================================================= #

_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C87 H120 Dy7 N6 O33, 6(C H4 O)'
_chemical_formula_sum            'C93 H144 Dy7 N6 O39'
_chemical_formula_weight         3107.64

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

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'

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

_cell_length_a                   15.5912(7)
_cell_length_b                   15.5912(7)
_cell_length_c                   28.0106(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5896.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9997
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      33.00

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3036
_exptl_absorpt_coefficient_mu    4.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_process_details   
;
 SADABS (Sheldrick, 1997)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  'Bruker X8 Kappa CCD APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61297
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.72
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3537
_reflns_number_gt                3315
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'APEX2 '
_computing_data_reduction        'SAINT+ (Bruker, 1997-2005)'
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_computing_structure_refinement  'SHELXTL '
_computing_molecular_graphics    'SHELXTL '
_computing_publication_material  'SHELXTL '

_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)+(0.0060P)²+175.2583P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3537
_refine_ls_number_parameters     229
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.1554
_refine_ls_wR_factor_gt          0.1541
_refine_ls_goodness_of_fit_ref   1.275
_refine_ls_restrained_S_all      1.275
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy2 Dy 0.6667 0.3333 0.2500 0.0201(3) Uani 1 6 d S . .
Dy1 Dy 0.70742(5) 0.19372(5) 0.34229(2) 0.0362(2) Uani 1 1 d . . .
O5 O 0.7087(8) 0.1960(8) 0.2500 0.026(2) Uani 1 2 d S . .
O3 O 0.5766(6) 0.2167(5) 0.3124(3) 0.0254(17) Uani 1 1 d D . .
H3 H 0.534(8) 0.161(6) 0.296(4) 0.038 Uiso 1 1 d D . .
O2 O 0.8320(7) 0.2740(7) 0.3974(3) 0.043(2) Uani 1 1 d . . .
N1 N 0.7338(9) 0.0640(9) 0.3841(4) 0.043(3) Uani 1 1 d . . .
O1 O 0.5884(7) 0.0312(6) 0.3227(3) 0.041(2) Uani 1 1 d . . .
O4 O 0.8252(7) 0.1861(7) 0.2903(3) 0.039(2) Uani 1 1 d . . .
O6 O 0.6100(8) 0.1747(10) 0.4116(4) 0.060(3) Uani 1 1 d D . .
H6 H 0.548(6) 0.166(14) 0.415(7) 0.091 Uiso 1 1 d D . .
C14 C 0.7888(12) 0.1897(12) 0.2500 0.029(4) Uani 1 2 d S . .
C8 C 0.8972(11) 0.1697(11) 0.4199(5) 0.042(3) Uani 1 1 d . . .
C6 C 0.6558(11) -0.0384(11) 0.3764(6) 0.050(4) Uani 1 1 d . . .
H6A H 0.6846 -0.0830 0.3780 0.060 Uiso 1 1 calc R . .
C7 C 0.8123(10) 0.0782(10) 0.4058(5) 0.042(3) Uani 1 1 d . . .
H7 H 0.8145 0.0201 0.4135 0.050 Uiso 1 1 calc R . .
C9 C 0.9771(12) 0.1644(14) 0.4403(5) 0.053(4) Uani 1 1 d . . .
H9 H 0.9728 0.1017 0.4432 0.063 Uiso 1 1 calc R . .
C2 C 0.5159(13) -0.1515(12) 0.3203(7) 0.065(5) Uani 1 1 d . . .
H2A H 0.4859 -0.1549 0.2887 0.077 Uiso 1 1 calc R . .
H2B H 0.5354 -0.2029 0.3214 0.077 Uiso 1 1 calc R . .
C13 C 0.9055(10) 0.2649(10) 0.4154(4) 0.037(3) Uani 1 1 d . . .
C10 C 1.0612(12) 0.2474(16) 0.4561(5) 0.060(5) Uani 1 1 d . . .
H10 H 1.1140 0.2421 0.4700 0.071 Uiso 1 1 calc R . .
C12 C 0.9928(11) 0.3461(12) 0.4313(5) 0.048(4) Uani 1 1 d . . .
H12 H 1.0009 0.4104 0.4279 0.058 Uiso 1 1 calc R . .
C1 C 0.6090(13) -0.0473(12) 0.3273(6) 0.058(4) Uani 1 1 d . . .
H1 H 0.6589 -0.0384 0.3024 0.070 Uiso 1 1 calc R . .
C3 C 0.4422(14) -0.1704(14) 0.3586(7) 0.072(5) Uani 1 1 d . . .
H3A H 0.3828 -0.2362 0.3534 0.087 Uiso 1 1 calc R . .
H3B H 0.4215 -0.1199 0.3567 0.087 Uiso 1 1 calc R . .
C11 C 1.0674(13) 0.3369(16) 0.4515(5) 0.061(5) Uani 1 1 d . . .
H11 H 1.1250 0.3944 0.4625 0.074 Uiso 1 1 calc R . .
C5 C 0.5767(13) -0.0677(13) 0.4155(6) 0.064(5) Uani 1 1 d . . .
H5A H 0.6068 -0.0680 0.4466 0.077 Uiso 1 1 calc R . .
H5B H 0.5573 -0.0163 0.4171 0.077 Uiso 1 1 calc R . .
C4 C 0.4840(14) -0.1675(12) 0.4086(8) 0.087(7) Uani 1 1 d . . .
H4A H 0.4343 -0.1774 0.4332 0.104 Uiso 1 1 calc R . .
H4B H 0.5002 -0.2211 0.4119 0.104 Uiso 1 1 calc R . .
O7 O 0.4912(9) 0.0300(10) 0.2500 0.038(3) Uiso 1 2 d S . .
H7A H 0.5136 0.0326 0.2224 0.046 Uiso 0.50 1 calc PR . .
C15 C 0.6278(14) 0.1723(16) 0.4624(5) 0.068(5) Uani 1 1 d . . .
H15A H 0.6979 0.1944 0.4677 0.102 Uiso 1 1 calc R . .
H15B H 0.5872 0.1045 0.4743 0.102 Uiso 1 1 calc R . .
H15C H 0.6102 0.2163 0.4794 0.102 Uiso 1 1 calc R . .
C16 C 0.386(2) -0.036(2) 0.2500 0.082(8) Uiso 1 2 d S . .
H16A H 0.3592 -0.0378 0.2820 0.123 Uiso 0.50 1 calc PR . .
H16B H 0.3711 -0.1027 0.2410 0.123 Uiso 0.50 1 calc PR . .
H16C H 0.3546 -0.0125 0.2270 0.123 Uiso 0.50 1 calc PR . .
C17 C 0.969(3) 0.132(3) 0.3082(13) 0.061(9) Uiso 0.50 1 d P . .
H17A H 0.9746 0.0845 0.3295 0.091 Uiso 0.50 1 calc PR . .
H17B H 0.9641 0.1093 0.2751 0.091 Uiso 0.50 1 calc PR . .
H17C H 0.9101 0.1352 0.3165 0.091 Uiso 0.50 1 calc PR . .
O8 O 1.045(3) 0.216(3) 0.3128(16) 0.143(14) Uiso 0.50 1 d P . .
H8 H 1.0761 0.2334 0.2868 0.172 Uiso 0.50 1 calc PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy2 O3 2.405(7) 3_655 ?
Dy2 O3 2.405(7) 10_556 ?
Dy2 O3 2.405(7) 12_656 ?
Dy2 O3 2.405(7) . ?
Dy2 O3 2.405(7) 5_665 ?
Dy2 O3 2.405(7) 8_666 ?
Dy2 O5 2.533(11) . ?
Dy2 O5 2.533(11) 3_655 ?
Dy2 O5 2.533(11) 8_666 ?
Dy1 O2 2.299(9) . ?
Dy1 O1 2.338(9) . ?
Dy1 O6 2.391(11) . ?
Dy1 O3 2.392(8) . ?
Dy1 O4 2.392(9) . ?
Dy1 O3 2.397(8) 3_655 ?
Dy1 N1 2.543(11) . ?
Dy1 O5 2.5853(6) . ?
O5 C14 1.301(19) . ?
O5 Dy1 2.5853(6) 10_556 ?
O3 Dy1 2.397(8) 5_665 ?
O3 H3 0.91(2) . ?
O2 C13 1.325(16) . ?
N1 C7 1.281(17) . ?
N1 C6 1.460(18) . ?
O1 C1 1.419(18) . ?
O4 C14 1.276(11) . ?
O6 C15 1.453(18) . ?
O6 H6 0.92(2) . ?
C14 O4 1.276(11) 10_556 ?
C14 Dy1 2.894(7) 10_556 ?
C8 C9 1.411(19) . ?
C8 C13 1.429(19) . ?
C8 C7 1.43(2) . ?
C6 C1 1.53(2) . ?
C6 C5 1.54(2) . ?
C6 H6A 1.0000 . ?
C7 H7 0.9500 . ?
C9 C10 1.38(2) . ?
C9 H9 0.9500 . ?
C2 C3 1.49(2) . ?
C2 C1 1.56(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C13 C12 1.39(2) . ?
C10 C11 1.36(3) . ?
C10 H10 0.9500 . ?
C12 C11 1.36(2) . ?
C12 H12 0.9500 . ?
C1 H1 1.0000 . ?
C3 C4 1.54(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C11 H11 0.9500 . ?
C5 C4 1.52(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O7 C16 1.44(3) . ?
O7 H7A 0.8400 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 O8 1.26(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O8 H8 0.8400 . ?

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
O3 Dy2 O3 139.86(14) 3_655 10_556 ?
O3 Dy2 O3 93.3(4) 3_655 12_656 ?
O3 Dy2 O3 72.9(3) 10_556 12_656 ?
O3 Dy2 O3 72.9(3) 3_655 . ?
O3 Dy2 O3 93.3(4) 10_556 . ?
O3 Dy2 O3 139.86(14) 12_656 . ?
O3 Dy2 O3 72.9(3) 3_655 5_665 ?
O3 Dy2 O3 139.86(14) 10_556 5_665 ?
O3 Dy2 O3 139.86(14) 12_656 5_665 ?
O3 Dy2 O3 72.9(3) . 5_665 ?
O3 Dy2 O3 139.86(14) 3_655 8_666 ?
O3 Dy2 O3 72.9(3) 10_556 8_666 ?
O3 Dy2 O3 72.9(3) 12_656 8_666 ?
O3 Dy2 O3 139.86(14) . 8_666 ?
O3 Dy2 O3 93.3(4) 5_665 8_666 ?
O3 Dy2 O5 69.7(2) 3_655 . ?
O3 Dy2 O5 70.2(2) 10_556 . ?
O3 Dy2 O5 69.7(2) 12_656 . ?
O3 Dy2 O5 70.2(2) . . ?
O3 Dy2 O5 133.34(18) 5_665 . ?
O3 Dy2 O5 133.34(18) 8_666 . ?
O3 Dy2 O5 70.2(2) 3_655 3_655 ?
O3 Dy2 O5 133.34(18) 10_556 3_655 ?
O3 Dy2 O5 70.2(2) 12_656 3_655 ?
O3 Dy2 O5 133.34(18) . 3_655 ?
O3 Dy2 O5 69.7(2) 5_665 3_655 ?
O3 Dy2 O5 69.7(2) 8_666 3_655 ?
O5 Dy2 O5 120.000(1) . 3_655 ?
O3 Dy2 O5 133.34(18) 3_655 8_666 ?
O3 Dy2 O5 69.7(2) 10_556 8_666 ?
O3 Dy2 O5 133.34(18) 12_656 8_666 ?
O3 Dy2 O5 69.7(2) . 8_666 ?
O3 Dy2 O5 70.2(2) 5_665 8_666 ?
O3 Dy2 O5 70.2(2) 8_666 8_666 ?
O5 Dy2 O5 120.000(1) . 8_666 ?
O5 Dy2 O5 120.000(1) 3_655 8_666 ?
O3 Dy2 Dy1 106.07(19) 3_655 10_556 ?
O3 Dy2 Dy1 40.60(19) 10_556 10_556 ?
O3 Dy2 Dy1 40.73(19) 12_656 10_556 ?
O3 Dy2 Dy1 105.98(18) . 10_556 ?
O3 Dy2 Dy1 178.68(18) 5_665 10_556 ?
O3 Dy2 Dy1 88.00(18) 8_666 10_556 ?
O5 Dy2 Dy1 45.344(11) . 10_556 ?
O5 Dy2 Dy1 110.90(16) 3_655 10_556 ?
O5 Dy2 Dy1 110.25(16) 8_666 10_556 ?
O3 Dy2 Dy1 40.60(19) 3_655 3_655 ?
O3 Dy2 Dy1 178.68(19) 10_556 3_655 ?
O3 Dy2 Dy1 105.98(18) 12_656 3_655 ?
O3 Dy2 Dy1 88.00(19) . 3_655 ?
O3 Dy2 Dy1 40.73(19) 5_665 3_655 ?
O3 Dy2 Dy1 106.07(19) 8_666 3_655 ?
O5 Dy2 Dy1 110.25(16) . 3_655 ?
O5 Dy2 Dy1 45.344(11) 3_655 3_655 ?
O5 Dy2 Dy1 110.90(16) 8_666 3_655 ?
Dy1 Dy2 Dy1 138.849(8) 10_556 3_655 ?
O3 Dy2 Dy1 105.98(18) 3_655 12_656 ?
O3 Dy2 Dy1 88.00(18) 10_556 12_656 ?
O3 Dy2 Dy1 40.60(19) 12_656 12_656 ?
O3 Dy2 Dy1 178.68(19) . 12_656 ?
O3 Dy2 Dy1 106.07(19) 5_665 12_656 ?
O3 Dy2 Dy1 40.73(19) 8_666 12_656 ?
O5 Dy2 Dy1 110.25(16) . 12_656 ?
O5 Dy2 Dy1 45.344(11) 3_655 12_656 ?
O5 Dy2 Dy1 110.90(16) 8_666 12_656 ?
Dy1 Dy2 Dy1 74.993(17) 10_556 12_656 ?
Dy1 Dy2 Dy1 90.68(2) 3_655 12_656 ?
O2 Dy1 O1 138.1(3) . . ?
O2 Dy1 O6 80.4(4) . . ?
O1 Dy1 O6 86.9(4) . . ?
O2 Dy1 O3 134.8(3) . . ?
O1 Dy1 O3 78.8(3) . . ?
O6 Dy1 O3 76.5(3) . . ?
O2 Dy1 O4 88.6(3) . . ?
O1 Dy1 O4 90.9(3) . . ?
O6 Dy1 O4 160.8(3) . . ?
O3 Dy1 O4 121.8(3) . . ?
O2 Dy1 O3 79.6(3) . 3_655 ?
O1 Dy1 O3 141.7(3) . 3_655 ?
O6 Dy1 O3 110.9(4) . 3_655 ?
O3 Dy1 O3 73.3(4) . 3_655 ?
O4 Dy1 O3 82.2(3) . 3_655 ?
O2 Dy1 N1 72.3(4) . . ?
O1 Dy1 N1 66.6(3) . . ?
O6 Dy1 N1 82.7(4) . . ?
O3 Dy1 N1 140.3(3) . . ?
O4 Dy1 N1 78.9(3) . . ?
O3 Dy1 N1 146.3(3) 3_655 . ?
O2 Dy1 O5 131.7(3) . . ?
O1 Dy1 O5 77.1(3) . . ?
O6 Dy1 O5 144.5(3) . . ?
O3 Dy1 O5 69.5(3) . . ?
O4 Dy1 O5 52.5(3) . . ?
O3 Dy1 O5 68.9(3) 3_655 . ?
N1 Dy1 O5 117.9(4) . . ?
C14 O5 Dy2 136.7(10) . . ?
C14 O5 Dy1 90.0(2) . . ?
Dy2 O5 Dy1 90.5(2) . . ?
C14 O5 Dy1 90.0(2) . 10_556 ?
Dy2 O5 Dy1 90.5(2) . 10_556 ?
Dy1 O5 Dy1 178.6(5) . 10_556 ?
Dy1 O3 Dy1 135.0(3) . 5_665 ?
Dy1 O3 Dy2 98.5(3) . . ?
Dy1 O3 Dy2 98.4(3) 5_665 . ?
Dy1 O3 H3 108(8) . . ?
Dy1 O3 H3 109(8) 5_665 . ?
Dy2 O3 H3 103(8) . . ?
C13 O2 Dy1 137.6(8) . . ?
C7 N1 C6 117.5(12) . . ?
C7 N1 Dy1 126.9(9) . . ?
C6 N1 Dy1 115.0(9) . . ?
C1 O1 Dy1 120.9(9) . . ?
C14 O4 Dy1 99.7(8) . . ?
C15 O6 Dy1 132.9(10) . . ?
C15 O6 H6 96(10) . . ?
Dy1 O6 H6 131(10) . . ?
O4 C14 O4 124.3(15) 10_556 . ?
O4 C14 O5 117.9(8) 10_556 . ?
O4 C14 O5 117.9(8) . . ?
O4 C14 Dy1 54.6(5) 10_556 10_556 ?
O4 C14 Dy1 178.4(11) . 10_556 ?
O5 C14 Dy1 63.3(3) . 10_556 ?
C9 C8 C13 118.1(15) . . ?
C9 C8 C7 117.2(14) . . ?
C13 C8 C7 124.6(12) . . ?
N1 C6 C1 109.3(12) . . ?
N1 C6 C5 109.0(13) . . ?
C1 C6 C5 109.8(13) . . ?
N1 C6 H6A 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N1 C7 C8 129.0(12) . . ?
N1 C7 H7 115.5 . . ?
C8 C7 H7 115.5 . . ?
C10 C9 C8 122.0(16) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C3 C2 C1 110.0(16) . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
O2 C13 C12 122.0(13) . . ?
O2 C13 C8 120.7(12) . . ?
C12 C13 C8 117.3(13) . . ?
C11 C10 C9 118.7(14) . . ?
C11 C10 H10 120.6 . . ?
C9 C10 H10 120.6 . . ?
C11 C12 C13 122.3(16) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
O1 C1 C6 107.8(13) . . ?
O1 C1 C2 113.1(14) . . ?
C6 C1 C2 111.1(14) . . ?
O1 C1 H1 108.2 . . ?
C6 C1 H1 108.2 . . ?
C2 C1 H1 108.2 . . ?
C2 C3 C4 112.1(16) . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C10 C11 C12 121.6(17) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C4 C5 C6 115.2(17) . . ?
C4 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
C4 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C4 C3 108.6(14) . . ?
C5 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
C5 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C16 O7 H7A 109.5 . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O8 C17 H17A 109.5 . . ?
O8 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O8 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C17 O8 H8 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
O3 Dy2 O5 C14 -50.9(2) 3_655 . . . ?
O3 Dy2 O5 C14 129.4(2) 10_556 . . . ?
O3 Dy2 O5 C14 50.9(2) 12_656 . . . ?
O3 Dy2 O5 C14 -129.4(2) . . . . ?
O3 Dy2 O5 C14 -89.6(3) 5_665 . . . ?
O3 Dy2 O5 C14 89.6(3) 8_666 . . . ?
O5 Dy2 O5 C14 0.0 3_655 . . . ?
O5 Dy2 O5 C14 180.0 8_666 . . . ?
Dy1 Dy2 O5 C14 90.5(2) 10_556 . . . ?
Dy1 Dy2 O5 C14 -49.30(7) 3_655 . . . ?
Dy1 Dy2 O5 C14 49.30(7) 12_656 . . . ?
O3 Dy2 O5 Dy1 39.6(3) 3_655 . . . ?
O3 Dy2 O5 Dy1 -140.1(4) 10_556 . . . ?
O3 Dy2 O5 Dy1 141.4(4) 12_656 . . . ?
O3 Dy2 O5 Dy1 -38.9(3) . . . . ?
O3 Dy2 O5 Dy1 0.9(5) 5_665 . . . ?
O3 Dy2 O5 Dy1 -179.9(3) 8_666 . . . ?
O5 Dy2 O5 Dy1 90.5(2) 3_655 . . . ?
O5 Dy2 O5 Dy1 -89.5(2) 8_666 . . . ?
Dy1 Dy2 O5 Dy1 -179.0(5) 10_556 . . . ?
Dy1 Dy2 O5 Dy1 41.2(3) 3_655 . . . ?
Dy1 Dy2 O5 Dy1 139.80(17) 12_656 . . . ?
O3 Dy2 O5 Dy1 -141.4(4) 3_655 . . 10_556 ?
O3 Dy2 O5 Dy1 38.9(3) 10_556 . . 10_556 ?
O3 Dy2 O5 Dy1 -39.6(3) 12_656 . . 10_556 ?
O3 Dy2 O5 Dy1 140.1(4) . . . 10_556 ?
O3 Dy2 O5 Dy1 179.9(3) 5_665 . . 10_556 ?
O3 Dy2 O5 Dy1 -0.9(5) 8_666 . . 10_556 ?
O5 Dy2 O5 Dy1 -90.5(2) 3_655 . . 10_556 ?
O5 Dy2 O5 Dy1 89.5(2) 8_666 . . 10_556 ?
Dy1 Dy2 O5 Dy1 -139.80(17) 3_655 . . 10_556 ?
Dy1 Dy2 O5 Dy1 -41.2(3) 12_656 . . 10_556 ?
O2 Dy1 O5 C14 43.7(10) . . . . ?
O1 Dy1 O5 C14 -101.3(9) . . . . ?
O6 Dy1 O5 C14 -166.6(9) . . . . ?
O3 Dy1 O5 C14 176.0(9) . . . . ?
O4 Dy1 O5 C14 0.1(8) . . . . ?
O3 Dy1 O5 C14 96.6(9) 3_655 . . . ?
N1 Dy1 O5 C14 -46.9(10) . . . . ?
O2 Dy1 O5 Dy2 -93.0(4) . . . . ?
O1 Dy1 O5 Dy2 122.0(4) . . . . ?
O6 Dy1 O5 Dy2 56.7(8) . . . . ?
O3 Dy1 O5 Dy2 39.3(3) . . . . ?
O4 Dy1 O5 Dy2 -136.6(5) . . . . ?
O3 Dy1 O5 Dy2 -40.0(3) 3_655 . . . ?
N1 Dy1 O5 Dy2 176.4(3) . . . . ?
O2 Dy1 O5 Dy1 134(20) . . . 10_556 ?
O2 Dy1 O3 Dy1 -24.5(7) . . . 5_665 ?
O1 Dy1 O3 Dy1 126.3(5) . . . 5_665 ?
O6 Dy1 O3 Dy1 36.8(5) . . . 5_665 ?
O4 Dy1 O3 Dy1 -149.7(4) . . . 5_665 ?
O3 Dy1 O3 Dy1 -80.3(5) 3_655 . . 5_665 ?
N1 Dy1 O3 Dy1 97.1(6) . . . 5_665 ?
O5 Dy1 O3 Dy1 -153.5(6) . . . 5_665 ?
O2 Dy1 O3 Dy2 86.5(4) . . . . ?
O1 Dy1 O3 Dy2 -122.7(3) . . . . ?
O6 Dy1 O3 Dy2 147.8(4) . . . . ?
O4 Dy1 O3 Dy2 -38.7(4) . . . . ?
O3 Dy1 O3 Dy2 30.7(3) 3_655 . . . ?
N1 Dy1 O3 Dy2 -151.9(4) . . . . ?
O5 Dy1 O3 Dy2 -42.5(3) . . . . ?
O3 Dy2 O3 Dy1 -30.7(3) 3_655 . . . ?
O3 Dy2 O3 Dy1 110.9(2) 10_556 . . . ?
O3 Dy2 O3 Dy1 43.65(19) 12_656 . . . ?
O3 Dy2 O3 Dy1 -107.57(17) 5_665 . . . ?
O3 Dy2 O3 Dy1 178.1(3) 8_666 . . . ?
O5 Dy2 O3 Dy1 43.3(3) . . . . ?
O5 Dy2 O3 Dy1 -69.7(5) 3_655 . . . ?
O5 Dy2 O3 Dy1 177.8(3) 8_666 . . . ?
Dy1 Dy2 O3 Dy1 71.6(2) 10_556 . . . ?
Dy1 Dy2 O3 Dy1 -69.1(2) 3_655 . . . ?
O3 Dy2 O3 Dy1 107.49(16) 3_655 . . 5_665 ?
O3 Dy2 O3 Dy1 -111.0(2) 10_556 . . 5_665 ?
O3 Dy2 O3 Dy1 -178.2(3) 12_656 . . 5_665 ?
O3 Dy2 O3 Dy1 30.6(3) 5_665 . . 5_665 ?
O3 Dy2 O3 Dy1 -43.74(18) 8_666 . . 5_665 ?
O5 Dy2 O3 Dy1 -178.5(3) . . . 5_665 ?
O5 Dy2 O3 Dy1 68.5(5) 3_655 . . 5_665 ?
O5 Dy2 O3 Dy1 -44.1(3) 8_666 . . 5_665 ?
Dy1 Dy2 O3 Dy1 -150.20(17) 10_556 . . 5_665 ?
Dy1 Dy2 O3 Dy1 69.1(2) 3_655 . . 5_665 ?
O1 Dy1 O2 C13 45.4(14) . . . . ?
O6 Dy1 O2 C13 119.7(13) . . . . ?
O3 Dy1 O2 C13 179.6(11) . . . . ?
O4 Dy1 O2 C13 -44.4(12) . . . . ?
O3 Dy1 O2 C13 -126.8(13) 3_655 . . . ?
N1 Dy1 O2 C13 34.4(12) . . . . ?
O5 Dy1 O2 C13 -77.5(13) . . . . ?
O2 Dy1 N1 C7 -22.8(12) . . . . ?
O1 Dy1 N1 C7 165.2(13) . . . . ?
O6 Dy1 N1 C7 -105.0(12) . . . . ?
O3 Dy1 N1 C7 -163.4(10) . . . . ?
O4 Dy1 N1 C7 69.3(12) . . . . ?
O3 Dy1 N1 C7 12.1(16) 3_655 . . . ?
O5 Dy1 N1 C7 105.6(12) . . . . ?
O2 Dy1 N1 C6 166.3(11) . . . . ?
O1 Dy1 N1 C6 -5.7(9) . . . . ?
O6 Dy1 N1 C6 84.1(10) . . . . ?
O3 Dy1 N1 C6 25.7(12) . . . . ?
O4 Dy1 N1 C6 -101.6(10) . . . . ?
O3 Dy1 N1 C6 -158.8(8) 3_655 . . . ?
O5 Dy1 N1 C6 -65.3(10) . . . . ?
O2 Dy1 O1 C1 -35.1(12) . . . . ?
O6 Dy1 O1 C1 -107.1(11) . . . . ?
O3 Dy1 O1 C1 176.1(11) . . . . ?
O4 Dy1 O1 C1 53.8(11) . . . . ?
O3 Dy1 O1 C1 132.4(10) 3_655 . . . ?
N1 Dy1 O1 C1 -23.7(10) . . . . ?
O5 Dy1 O1 C1 104.8(11) . . . . ?
O2 Dy1 O4 C14 -149.1(9) . . . . ?
O1 Dy1 O4 C14 72.7(9) . . . . ?
O6 Dy1 O4 C14 155.9(12) . . . . ?
O3 Dy1 O4 C14 -4.6(10) . . . . ?
O3 Dy1 O4 C14 -69.4(9) 3_655 . . . ?
N1 Dy1 O4 C14 138.7(9) . . . . ?
O5 Dy1 O4 C14 -0.1(9) . . . . ?
O2 Dy1 O6 C15 -25.9(16) . . . . ?
O1 Dy1 O6 C15 114.0(16) . . . . ?
O3 Dy1 O6 C15 -166.8(17) . . . . ?
O4 Dy1 O6 C15 30(2) . . . . ?
O3 Dy1 O6 C15 -100.9(16) 3_655 . . . ?
N1 Dy1 O6 C15 47.2(16) . . . . ?
O5 Dy1 O6 C15 176.5(14) . . . . ?
Dy1 O4 C14 O4 -178.7(13) . . . 10_556 ?
Dy1 O4 C14 O5 0.2(15) . . . . ?
Dy2 O5 C14 O4 -90.5(13) . . . 10_556 ?
Dy1 O5 C14 O4 178.8(13) . . . 10_556 ?
Dy1 O5 C14 O4 0.2(14) 10_556 . . 10_556 ?
Dy2 O5 C14 O4 90.5(13) . . . . ?
Dy1 O5 C14 O4 -0.2(14) . . . . ?
Dy1 O5 C14 O4 -178.8(13) 10_556 . . . ?
Dy2 O5 C14 Dy1 -90.7(2) . . . 10_556 ?
Dy1 O5 C14 Dy1 178.6(5) . . . 10_556 ?
C7 N1 C6 C1 -141.8(14) . . . . ?
Dy1 N1 C6 C1 30.0(15) . . . . ?
C7 N1 C6 C5 98.1(15) . . . . ?
Dy1 N1 C6 C5 -90.1(13) . . . . ?
C6 N1 C7 C8 -176.7(14) . . . . ?
Dy1 N1 C7 C8 13(2) . . . . ?
C9 C8 C7 N1 -175.4(14) . . . . ?
C13 C8 C7 N1 6(2) . . . . ?
C13 C8 C9 C10 0(2) . . . . ?
C7 C8 C9 C10 -178.5(13) . . . . ?
Dy1 O2 C13 C12 149.9(11) . . . . ?
Dy1 O2 C13 C8 -30.8(19) . . . . ?
C9 C8 C13 O2 -178.7(12) . . . . ?
C7 C8 C13 O2 0(2) . . . . ?
C9 C8 C13 C12 0.6(19) . . . . ?
C7 C8 C13 C12 179.5(13) . . . . ?
C8 C9 C10 C11 -1(2) . . . . ?
O2 C13 C12 C11 177.7(13) . . . . ?
C8 C13 C12 C11 -2(2) . . . . ?
Dy1 O1 C1 C6 47.6(15) . . . . ?
Dy1 O1 C1 C2 170.8(11) . . . . ?
N1 C6 C1 O1 -47.6(17) . . . . ?
C5 C6 C1 O1 72.0(16) . . . . ?
N1 C6 C1 C2 -172.1(13) . . . . ?
C5 C6 C1 C2 -52.5(18) . . . . ?
C3 C2 C1 O1 -63.7(19) . . . . ?
C3 C2 C1 C6 57.7(19) . . . . ?
C1 C2 C3 C4 -60(2) . . . . ?
C9 C10 C11 C12 0(2) . . . . ?
C13 C12 C11 C10 2(2) . . . . ?
N1 C6 C5 C4 172.3(14) . . . . ?
C1 C6 C5 C4 52.5(19) . . . . ?
C6 C5 C4 C3 -53(2) . . . . ?
C2 C3 C4 C5 57(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.030
_refine_diff_density_min         -3.869
_refine_diff_density_rms         0.230

#============================================================================#
#      Luis Cunha-Silva @ REQUIMTE & DQB FCUP  *  13/03/2014  *   END        #
#============================================================================#  
_database_code_depnum_ccdc_archive 'CCDC 991357'
