# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


#######################################################################
#
#                 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_shelxl-C1
_database_code_depnum_ccdc_archive 'CCDC 888085'
#TrackingRef '- C1_dv06.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H32 Cu N10 O11 Tb W'
_chemical_formula_weight         1066.93

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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   9.9903(2)
_cell_length_b                   26.4341(7)
_cell_length_c                   13.3220(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.056(2)
_cell_angle_gamma                90.00
_cell_volume                     3452.84(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    60795
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      33.42

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2000
_exptl_absorpt_coefficient_mu    6.029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1792
_exptl_absorpt_correction_T_max  0.3740
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            67798
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         33.42
_reflns_number_total             13337
_reflns_number_gt                10366
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0781P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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     SHELXL
_refine_ls_extinction_coef       0.0045(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         13337
_refine_ls_number_parameters     452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1254
_refine_ls_wR_factor_gt          0.1178
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
C1 C 0.9249(9) 0.0541(3) 0.6269(7) 0.062(2) Uani 1 1 d . . .
H1A H 0.8636 0.0277 0.5977 0.093 Uiso 1 1 calc R . .
H1B H 1.0019 0.0396 0.6718 0.093 Uiso 1 1 calc R . .
H1C H 0.9555 0.0724 0.5733 0.093 Uiso 1 1 calc R . .
C2 C 0.9299(7) 0.1296(3) 0.7302(5) 0.0514(16) Uani 1 1 d . . .
C3 C 1.0622(8) 0.1397(4) 0.7216(7) 0.067(2) Uani 1 1 d . . .
H3 H 1.1083 0.1185 0.6840 0.081 Uiso 1 1 calc R . .
C4 C 1.1258(9) 0.1825(4) 0.7706(8) 0.078(3) Uani 1 1 d . . .
H4 H 1.2153 0.1898 0.7656 0.094 Uiso 1 1 calc R . .
C5 C 1.0583(9) 0.2137(3) 0.8257(8) 0.072(3) Uani 1 1 d . . .
H5 H 1.1024 0.2421 0.8574 0.086 Uiso 1 1 calc R . .
C6 C 0.9226(8) 0.2035(2) 0.8353(6) 0.0556(18) Uani 1 1 d . . .
C7 C 0.8568(6) 0.1602(2) 0.7850(5) 0.0423(12) Uani 1 1 d . . .
C8 C 0.8581(9) 0.2377(3) 0.8974(7) 0.066(2) Uani 1 1 d . . .
H8 H 0.9036 0.2676 0.9193 0.079 Uiso 1 1 calc R . .
C9 C 0.6796(10) 0.2664(2) 0.9837(6) 0.067(2) Uani 1 1 d . . .
H9A H 0.6221 0.2894 0.9378 0.080 Uiso 1 1 calc R . .
H9B H 0.7492 0.2860 1.0277 0.080 Uiso 1 1 calc R . .
C10 C 0.5955(10) 0.2383(2) 1.0472(5) 0.064(2) Uani 1 1 d . . .
H10A H 0.6533 0.2266 1.1099 0.077 Uiso 1 1 calc R . .
H10B H 0.5268 0.2606 1.0652 0.077 Uiso 1 1 calc R . .
C11 C 0.4208(9) 0.1746(3) 1.0085(5) 0.0543(17) Uani 1 1 d . . .
H11 H 0.3779 0.1910 1.0553 0.065 Uiso 1 1 calc R . .
C12 C 0.3597(8) 0.1279(2) 0.9631(5) 0.0476(14) Uani 1 1 d . . .
C13 C 0.2433(9) 0.1083(4) 0.9946(6) 0.065(2) Uani 1 1 d . . .
H13 H 0.2032 0.1270 1.0402 0.078 Uiso 1 1 calc R . .
C14 C 0.1876(9) 0.0632(4) 0.9609(7) 0.067(2) Uani 1 1 d . . .
H14 H 0.1063 0.0528 0.9786 0.080 Uiso 1 1 calc R . .
C15 C 0.2521(8) 0.0325(3) 0.8994(6) 0.0586(17) Uani 1 1 d . . .
H15 H 0.2175 0.0006 0.8795 0.070 Uiso 1 1 calc R . .
C16 C 0.3679(6) 0.0501(2) 0.8687(4) 0.0412(11) Uani 1 1 d . . .
C17 C 0.4184(6) 0.0988(2) 0.8934(4) 0.0366(10) Uani 1 1 d . . .
C18 C 0.4763(9) -0.0276(2) 0.8474(6) 0.0537(16) Uani 1 1 d . . .
H18A H 0.5282 -0.0444 0.8036 0.081 Uiso 1 1 calc R . .
H18B H 0.3943 -0.0463 0.8485 0.081 Uiso 1 1 calc R . .
H18C H 0.5296 -0.0256 0.9154 0.081 Uiso 1 1 calc R . .
C19 C 0.8528(7) 0.1242(2) 1.1125(5) 0.0425(12) Uani 1 1 d . . .
C20 C 1.0263(6) 0.0662(2) 1.2210(4) 0.0379(10) Uani 1 1 d . . .
C21 C 1.1053(6) 0.1605(2) 1.2322(4) 0.0382(10) Uani 1 1 d . . .
C22 C 1.0884(6) 0.1096(2) 1.3999(4) 0.0362(10) Uani 1 1 d . . .
C23 C 0.9070(6) 0.2103(2) 1.2547(5) 0.0407(11) Uani 1 1 d . . .
C24 C 0.8717(6) 0.1571(2) 1.4157(4) 0.0384(10) Uani 1 1 d . . .
C25 C 0.7076(6) 0.14326(19) 1.2474(4) 0.0364(10) Uani 1 1 d . . .
C26 C 0.8348(6) 0.0630(2) 1.3285(4) 0.0365(10) Uani 1 1 d . . .
N1 N 0.7446(7) 0.22989(18) 0.9239(5) 0.0547(15) Uani 1 1 d . . .
N2 N 0.5293(7) 0.19467(19) 0.9886(4) 0.0497(13) Uani 1 1 d . . .
N3 N 0.8112(7) 0.1183(3) 1.0271(4) 0.0581(15) Uani 1 1 d . . .
N4 N 1.0813(7) 0.03304(18) 1.1918(5) 0.0514(13) Uani 1 1 d . . .
N5 N 1.2019(6) 0.1785(2) 1.2126(5) 0.0550(14) Uani 1 1 d . . .
N6 N 1.1760(6) 0.0990(2) 1.4639(4) 0.0503(12) Uani 1 1 d . . .
N7 N 0.9043(7) 0.25381(19) 1.2463(6) 0.0576(15) Uani 1 1 d . . .
N8 N 0.8380(7) 0.1707(2) 1.4883(4) 0.0545(14) Uani 1 1 d . . .
N9 N 0.5922(5) 0.1492(2) 1.2348(5) 0.0519(13) Uani 1 1 d . . .
N10 N 0.7856(6) 0.02830(19) 1.3581(5) 0.0510(13) Uani 1 1 d . . .
O1 O 0.8550(5) 0.08826(18) 0.6841(4) 0.0489(10) Uani 1 1 d . . .
O2 O 0.7289(4) 0.14801(15) 0.7873(3) 0.0406(8) Uani 1 1 d . . .
O3 O 0.5207(5) 0.11417(14) 0.8510(3) 0.0396(8) Uani 1 1 d . . .
O4 O 0.4417(5) 0.02269(14) 0.8092(3) 0.0412(8) Uani 1 1 d . . .
O5 O 0.7468(5) 0.04376(16) 0.8586(3) 0.0454(9) Uani 1 1 d . . .
O6 O 0.6500(7) -0.00424(18) 0.6619(5) 0.0697(17) Uani 1 1 d . . .
O7 O 0.6225(5) 0.0945(2) 0.5373(4) 0.0518(11) Uani 1 1 d . . .
O8 O 0.3851(5) 0.0545(2) 0.6096(4) 0.0604(14) Uani 1 1 d . . .
O9 O 0.4743(5) 0.15669(14) 0.6450(4) 0.0457(10) Uani 1 1 d . . .
O10 O 0.6397(7) 0.22555(19) 0.5783(5) 0.0665(15) Uani 1 1 d . . .
O11 O 0.4264(6) 0.1067(2) 1.3631(5) 0.0617(13) Uani 1 1 d . . .
Cu1 Cu 0.63531(9) 0.17078(2) 0.89236(6) 0.04312(16) Uani 1 1 d . . .
W1 W 0.924460(19) 0.129730(6) 1.275700(13) 0.02546(6) Uani 1 1 d . . .
Tb1 Tb 0.59834(2) 0.079719(8) 0.712360(17) 0.02983(6) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.063(5) 0.060(4) 0.073(5) 0.021(3) 0.037(4) 0.019(3)
C2 0.038(3) 0.064(4) 0.048(3) 0.024(3) -0.002(2) -0.009(3)
C3 0.040(4) 0.102(6) 0.060(5) 0.027(4) 0.009(3) -0.009(4)
C4 0.046(4) 0.102(7) 0.081(6) 0.039(5) -0.002(4) -0.032(5)
C5 0.054(5) 0.072(5) 0.077(6) 0.025(4) -0.015(4) -0.027(4)
C6 0.050(4) 0.046(3) 0.061(4) 0.012(3) -0.013(3) -0.017(3)
C7 0.030(2) 0.048(3) 0.045(3) 0.015(2) -0.003(2) -0.008(2)
C8 0.073(5) 0.039(3) 0.070(5) 0.009(3) -0.024(4) -0.020(3)
C9 0.087(6) 0.030(2) 0.068(5) -0.010(3) -0.024(4) 0.006(3)
C10 0.095(6) 0.041(3) 0.045(3) -0.012(2) -0.014(4) 0.017(3)
C11 0.068(5) 0.053(3) 0.040(3) -0.008(2) 0.006(3) 0.024(3)
C12 0.052(4) 0.059(3) 0.033(3) 0.001(2) 0.011(2) 0.015(3)
C13 0.055(4) 0.099(6) 0.045(4) 0.002(4) 0.020(3) 0.019(4)
C14 0.052(4) 0.097(6) 0.057(4) 0.004(4) 0.026(4) -0.008(4)
C15 0.051(4) 0.078(5) 0.047(4) 0.005(3) 0.011(3) -0.015(3)
C16 0.042(3) 0.052(3) 0.029(2) 0.003(2) 0.005(2) -0.004(2)
C17 0.038(3) 0.043(2) 0.030(2) 0.0033(18) 0.0088(19) 0.008(2)
C18 0.068(5) 0.039(3) 0.052(4) 0.005(2) 0.007(3) -0.004(3)
C19 0.044(3) 0.040(2) 0.042(3) 0.001(2) 0.004(2) 0.013(2)
C20 0.040(3) 0.038(2) 0.035(2) 0.0035(18) 0.006(2) 0.001(2)
C21 0.042(3) 0.034(2) 0.040(3) 0.0002(18) 0.012(2) 0.0051(19)
C22 0.035(3) 0.040(2) 0.034(2) 0.0034(18) 0.0094(19) 0.0007(19)
C23 0.034(3) 0.044(3) 0.045(3) 0.006(2) 0.011(2) 0.004(2)
C24 0.037(3) 0.037(2) 0.041(3) 0.0033(19) 0.006(2) 0.0045(19)
C25 0.038(3) 0.032(2) 0.038(3) 0.0050(18) 0.004(2) 0.0007(18)
C26 0.030(2) 0.039(2) 0.038(3) -0.0018(19) 0.0028(19) -0.0005(18)
N1 0.066(4) 0.031(2) 0.055(3) -0.0014(19) -0.019(3) -0.004(2)
N2 0.065(4) 0.040(2) 0.038(2) -0.0082(18) -0.005(2) 0.016(2)
N3 0.066(4) 0.069(3) 0.032(2) -0.006(2) -0.008(2) 0.014(3)
N4 0.067(4) 0.035(2) 0.056(3) 0.003(2) 0.023(3) 0.020(2)
N5 0.047(3) 0.050(3) 0.074(4) 0.002(3) 0.025(3) -0.004(2)
N6 0.041(3) 0.064(3) 0.041(3) 0.011(2) -0.004(2) 0.008(2)
N7 0.062(4) 0.031(2) 0.087(4) 0.016(2) 0.030(3) 0.011(2)
N8 0.059(4) 0.069(3) 0.040(3) -0.008(2) 0.019(2) 0.005(3)
N9 0.029(2) 0.062(3) 0.063(4) 0.009(3) 0.005(2) 0.006(2)
N10 0.053(3) 0.039(2) 0.059(3) 0.010(2) 0.007(3) -0.013(2)
O1 0.040(2) 0.062(3) 0.047(2) 0.0038(19) 0.0146(19) -0.0009(19)
O2 0.034(2) 0.0402(18) 0.045(2) -0.0025(15) 0.0027(16) -0.0075(15)
O3 0.046(2) 0.0336(16) 0.041(2) -0.0073(14) 0.0137(17) -0.0047(15)
O4 0.049(2) 0.0366(17) 0.040(2) 0.0019(15) 0.0122(17) -0.0045(16)
O5 0.043(2) 0.049(2) 0.041(2) 0.0083(16) 0.0007(17) 0.0131(17)
O6 0.074(4) 0.037(2) 0.109(5) -0.014(2) 0.045(4) 0.002(2)
O7 0.050(3) 0.067(3) 0.040(2) 0.009(2) 0.0125(19) 0.004(2)
O8 0.043(3) 0.064(3) 0.064(3) 0.028(2) -0.016(2) -0.019(2)
O9 0.049(2) 0.0339(17) 0.050(2) 0.0017(16) -0.0005(19) 0.0121(16)
O10 0.080(4) 0.052(3) 0.074(4) -0.002(2) 0.033(3) 0.001(3)
O11 0.052(3) 0.067(3) 0.067(3) 0.003(2) 0.015(3) -0.002(2)
Cu1 0.0513(4) 0.0328(3) 0.0424(4) -0.0078(2) 0.0016(3) -0.0027(3)
W1 0.02588(9) 0.02430(8) 0.02569(9) 0.00146(5) 0.00364(6) 0.00162(5)
Tb1 0.02970(12) 0.02954(10) 0.02940(11) -0.00061(7) 0.00357(8) 0.00105(7)

_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
C1 O1 1.444(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.374(10) . ?
C2 C7 1.386(11) . ?
C2 O1 1.400(9) . ?
C3 C4 1.397(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.424(9) . ?
C6 C8 1.457(13) . ?
C7 O2 1.323(7) . ?
C8 N1 1.267(12) . ?
C8 H8 0.9300 . ?
C9 N1 1.477(11) . ?
C9 C10 1.498(14) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.475(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.279(11) . ?
C11 C12 1.457(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.409(11) . ?
C12 C17 1.417(8) . ?
C13 C14 1.354(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.396(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.380(9) . ?
C15 H15 0.9300 . ?
C16 O4 1.386(7) . ?
C16 C17 1.399(8) . ?
C17 O3 1.322(7) . ?
C18 O4 1.442(7) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.145(8) . ?
C19 W1 2.160(6) . ?
C20 N4 1.142(7) . ?
C20 W1 2.161(6) . ?
C21 N5 1.151(8) . ?
C21 W1 2.158(6) . ?
C22 N6 1.133(7) . ?
C22 W1 2.160(6) . ?
C23 N7 1.154(7) . ?
C23 W1 2.152(6) . ?
C24 N8 1.143(8) . ?
C24 W1 2.157(6) . ?
C25 N9 1.143(8) . ?
C25 W1 2.157(6) . ?
C26 N10 1.147(7) . ?
C26 W1 2.156(5) . ?
N1 Cu1 1.906(5) . ?
N2 Cu1 1.920(6) . ?
O1 Tb1 2.671(5) . ?
O2 Cu1 1.923(4) . ?
O2 Tb1 2.336(4) . ?
O3 Cu1 1.901(4) . ?
O3 Tb1 2.323(4) . ?
O4 Tb1 2.676(4) . ?
O5 Tb1 2.406(4) . ?
O6 Tb1 2.404(4) . ?
O7 Tb1 2.421(5) . ?
O8 Tb1 2.396(5) . ?
O9 Tb1 2.461(4) . ?
Cu1 Tb1 3.3676(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 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 . . ?
C3 C2 C7 123.0(8) . . ?
C3 C2 O1 123.8(8) . . ?
C7 C2 O1 113.2(6) . . ?
C2 C3 C4 118.4(10) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 120.9(8) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 121.0(8) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C7 118.5(8) . . ?
C5 C6 C8 118.1(7) . . ?
C7 C6 C8 123.5(7) . . ?
O2 C7 C2 118.7(6) . . ?
O2 C7 C6 123.1(7) . . ?
C2 C7 C6 118.3(6) . . ?
N1 C8 C6 125.1(6) . . ?
N1 C8 H8 117.5 . . ?
C6 C8 H8 117.5 . . ?
N1 C9 C10 109.5(5) . . ?
N1 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
N1 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 109.4(6) . . ?
N2 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
N2 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
N2 C11 C12 124.8(6) . . ?
N2 C11 H11 117.6 . . ?
C12 C11 H11 117.6 . . ?
C13 C12 C17 117.7(7) . . ?
C13 C12 C11 119.5(6) . . ?
C17 C12 C11 122.6(7) . . ?
C14 C13 C12 122.3(7) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C13 C14 C15 120.0(7) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 119.0(7) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 O4 124.1(6) . . ?
C15 C16 C17 121.7(6) . . ?
O4 C16 C17 114.1(5) . . ?
O3 C17 C16 117.1(5) . . ?
O3 C17 C12 124.3(5) . . ?
C16 C17 C12 118.5(6) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 W1 175.6(6) . . ?
N4 C20 W1 179.2(6) . . ?
N5 C21 W1 176.8(5) . . ?
N6 C22 W1 178.7(5) . . ?
N7 C23 W1 176.5(6) . . ?
N8 C24 W1 176.9(6) . . ?
N9 C25 W1 177.8(5) . . ?
N10 C26 W1 178.3(6) . . ?
C8 N1 C9 123.6(6) . . ?
C8 N1 Cu1 125.3(5) . . ?
C9 N1 Cu1 111.2(6) . . ?
C11 N2 C10 121.8(6) . . ?
C11 N2 Cu1 126.8(4) . . ?
C10 N2 Cu1 111.2(6) . . ?
C2 O1 C1 116.6(6) . . ?
C2 O1 Tb1 116.8(4) . . ?
C1 O1 Tb1 126.6(5) . . ?
C7 O2 Cu1 123.2(4) . . ?
C7 O2 Tb1 129.8(4) . . ?
Cu1 O2 Tb1 104.08(18) . . ?
C17 O3 Cu1 126.2(3) . . ?
C17 O3 Tb1 128.5(3) . . ?
Cu1 O3 Tb1 105.33(18) . . ?
C16 O4 C18 113.5(5) . . ?
C16 O4 Tb1 113.9(3) . . ?
C18 O4 Tb1 124.5(4) . . ?
O3 Cu1 N1 175.6(2) . . ?
O3 Cu1 N2 94.2(2) . . ?
N1 Cu1 N2 87.1(3) . . ?
O3 Cu1 O2 83.86(17) . . ?
N1 Cu1 O2 94.5(3) . . ?
N2 Cu1 O2 175.3(2) . . ?
O3 Cu1 Tb1 41.70(12) . . ?
N1 Cu1 Tb1 136.3(2) . . ?
N2 Cu1 Tb1 135.36(19) . . ?
O2 Cu1 Tb1 42.29(11) . . ?
C23 W1 C26 145.5(2) . . ?
C23 W1 C25 76.1(2) . . ?
C26 W1 C25 74.1(2) . . ?
C23 W1 C24 75.7(2) . . ?
C26 W1 C24 78.8(2) . . ?
C25 W1 C24 72.0(2) . . ?
C23 W1 C21 69.1(2) . . ?
C26 W1 C21 144.8(2) . . ?
C25 W1 C21 139.0(2) . . ?
C24 W1 C21 117.5(2) . . ?
C23 W1 C22 112.0(2) . . ?
C26 W1 C22 81.4(2) . . ?
C25 W1 C22 139.8(2) . . ?
C24 W1 C22 72.3(2) . . ?
C21 W1 C22 75.4(2) . . ?
C23 W1 C19 86.2(2) . . ?
C26 W1 C19 101.2(2) . . ?
C25 W1 C19 73.0(2) . . ?
C24 W1 C19 143.5(2) . . ?
C21 W1 C19 83.6(2) . . ?
C22 W1 C19 144.2(2) . . ?
C23 W1 C20 139.2(2) . . ?
C26 W1 C20 74.1(2) . . ?
C25 W1 C20 126.3(2) . . ?
C24 W1 C20 139.5(2) . . ?
C21 W1 C20 74.3(2) . . ?
C22 W1 C20 74.4(2) . . ?
C19 W1 C20 72.2(2) . . ?
O3 Tb1 O2 66.51(15) . . ?
O3 Tb1 O8 99.64(19) . . ?
O2 Tb1 O8 145.24(17) . . ?
O3 Tb1 O6 134.99(18) . . ?
O2 Tb1 O6 134.50(19) . . ?
O8 Tb1 O6 78.4(2) . . ?
O3 Tb1 O5 76.06(15) . . ?
O2 Tb1 O5 75.66(15) . . ?
O8 Tb1 O5 134.07(16) . . ?
O6 Tb1 O5 74.3(2) . . ?
O3 Tb1 O7 144.38(16) . . ?
O2 Tb1 O7 97.84(17) . . ?
O8 Tb1 O7 74.71(18) . . ?
O6 Tb1 O7 79.2(2) . . ?
O5 Tb1 O7 133.11(17) . . ?
O3 Tb1 O9 75.17(15) . . ?
O2 Tb1 O9 73.61(15) . . ?
O8 Tb1 O9 71.99(16) . . ?
O6 Tb1 O9 141.4(2) . . ?
O5 Tb1 O9 144.20(15) . . ?
O7 Tb1 O9 69.62(17) . . ?
O3 Tb1 O1 123.72(15) . . ?
O2 Tb1 O1 61.49(15) . . ?
O8 Tb1 O1 135.67(19) . . ?
O6 Tb1 O1 77.01(18) . . ?
O5 Tb1 O1 71.83(16) . . ?
O7 Tb1 O1 64.86(16) . . ?
O9 Tb1 O1 107.98(16) . . ?
O3 Tb1 O4 61.45(13) . . ?
O2 Tb1 O4 124.04(14) . . ?
O8 Tb1 O4 65.20(15) . . ?
O6 Tb1 O4 77.96(16) . . ?
O5 Tb1 O4 73.39(15) . . ?
O7 Tb1 O4 136.92(16) . . ?
O9 Tb1 O4 109.96(15) . . ?
O1 Tb1 O4 141.39(14) . . ?
O3 Tb1 Cu1 32.98(10) . . ?
O2 Tb1 Cu1 33.63(11) . . ?
O8 Tb1 Cu1 124.73(16) . . ?
O6 Tb1 Cu1 149.22(18) . . ?
O5 Tb1 Cu1 74.90(11) . . ?
O7 Tb1 Cu1 123.57(13) . . ?
O9 Tb1 Cu1 69.35(11) . . ?
O1 Tb1 Cu1 93.60(11) . . ?
O4 Tb1 Cu1 93.10(9) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        33.42
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.380
_refine_diff_density_min         -1.849
_refine_diff_density_rms         0.217


data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 888086'
#TrackingRef '- C2_dv11.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H33 Cu N11 O10 Tb W'
_chemical_formula_weight         1089.96

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'
Cu Cu 0.3201 1.2651 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21

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

_cell_length_a                   9.0828(3)
_cell_length_b                   20.1071(6)
_cell_length_c                   10.2803(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.118(2)
_cell_angle_gamma                90.00
_cell_volume                     1869.99(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22181
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      33.44

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1028
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5828
_exptl_absorpt_correction_T_max  0.6350
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39008
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.25
_diffrn_reflns_theta_max         33.44
_reflns_number_total             14415
_reflns_number_gt                12228
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(6)
_refine_ls_number_reflns         14415
_refine_ls_number_parameters     470
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3273(7) 0.6410(4) 0.1671(8) 0.0600(19) Uani 1 1 d . . .
H1A H 0.3671 0.6094 0.2308 0.090 Uiso 1 1 calc R . .
H1B H 0.2906 0.6181 0.0890 0.090 Uiso 1 1 calc R . .
H1C H 0.2480 0.6651 0.2013 0.090 Uiso 1 1 calc R . .
C2 C 0.4037(6) 0.7351(3) 0.0433(5) 0.0363(11) Uani 1 1 d . . .
C3 C 0.2735(7) 0.7367(4) -0.0345(6) 0.0491(15) Uani 1 1 d . . .
H3 H 0.2006 0.7050 -0.0254 0.059 Uiso 1 1 calc R . .
C4 C 0.2522(8) 0.7876(4) -0.1291(7) 0.0590(19) Uani 1 1 d . . .
H4 H 0.1647 0.7889 -0.1835 0.071 Uiso 1 1 calc R . .
C5 C 0.3573(8) 0.8346(4) -0.1419(6) 0.0512(16) Uani 1 1 d . . .
H5 H 0.3417 0.8674 -0.2055 0.061 Uiso 1 1 calc R . .
C6 C 0.4890(7) 0.8340(3) -0.0600(5) 0.0409(12) Uani 1 1 d . . .
C7 C 0.5128(6) 0.7833(3) 0.0337(4) 0.0339(10) Uani 1 1 d . . .
C8 C 0.5987(8) 0.8851(3) -0.0828(5) 0.0454(14) Uani 1 1 d . . .
H8 H 0.5720 0.9176 -0.1449 0.055 Uiso 1 1 calc R . .
C9 C 0.8333(9) 0.9410(3) -0.0487(8) 0.0590(18) Uani 1 1 d . . .
H9A H 0.8251 0.9773 0.0125 0.071 Uiso 1 1 calc R . .
H9B H 0.8122 0.9583 -0.1365 0.071 Uiso 1 1 calc R . .
C10 C 0.9892(9) 0.9121(3) -0.0326(8) 0.063(2) Uani 1 1 d . . .
H10A H 1.0081 0.8862 -0.1091 0.075 Uiso 1 1 calc R . .
H10B H 1.0618 0.9475 -0.0219 0.075 Uiso 1 1 calc R . .
C11 C 1.1174(7) 0.8586(3) 0.1532(7) 0.0494(15) Uani 1 1 d . . .
H11 H 1.2020 0.8798 0.1297 0.059 Uiso 1 1 calc R . .
C12 C 1.1322(6) 0.8154(3) 0.2674(6) 0.0431(13) Uani 1 1 d . . .
C13 C 1.2625(7) 0.8194(4) 0.3532(8) 0.0593(19) Uani 1 1 d . . .
H13 H 1.3373 0.8485 0.3343 0.071 Uiso 1 1 calc R . .
C14 C 1.2801(7) 0.7816(5) 0.4627(9) 0.069(2) Uani 1 1 d . . .
H14 H 1.3687 0.7837 0.5155 0.082 Uiso 1 1 calc R . .
C15 C 1.1680(7) 0.7395(4) 0.4976(7) 0.0536(16) Uani 1 1 d . . .
H15 H 1.1794 0.7153 0.5750 0.064 Uiso 1 1 calc R . .
C16 C 1.0390(5) 0.7345(3) 0.4147(6) 0.0348(11) Uani 1 1 d . . .
C17 C 1.0198(5) 0.7715(3) 0.2984(5) 0.0330(10) Uani 1 1 d . . .
C18 C 0.9180(7) 0.6683(4) 0.5673(6) 0.0544(17) Uani 1 1 d . . .
H18A H 0.8307 0.6418 0.5720 0.082 Uiso 1 1 calc R . .
H18B H 0.9179 0.7042 0.6289 0.082 Uiso 1 1 calc R . .
H18C H 1.0040 0.6412 0.5875 0.082 Uiso 1 1 calc R . .
C19 C 0.5412(6) 0.5951(3) 0.4904(5) 0.0325(10) Uani 1 1 d . . .
C20 C 0.2594(6) 0.5591(3) 0.4961(5) 0.0339(10) Uani 1 1 d . . .
C21 C 0.2625(7) 0.5762(3) 0.7442(6) 0.0431(13) Uani 1 1 d . . .
C22 C 0.6721(6) 0.5113(3) 0.6680(6) 0.0404(12) Uani 1 1 d . . .
C23 C 0.4691(7) 0.4685(3) 0.4850(5) 0.0386(11) Uani 1 1 d . . .
C24 C 0.5198(6) 0.6340(3) 0.7176(5) 0.0357(11) Uani 1 1 d . . .
C25 C 0.3296(6) 0.4490(3) 0.6865(5) 0.0338(10) Uani 1 1 d . . .
C26 C 0.5008(7) 0.5208(3) 0.8445(5) 0.0428(13) Uani 1 1 d . . .
C27 C 0.9113(8) 0.4446(4) 0.3774(8) 0.0542(16) Uani 1 1 d . . .
C28 C 1.0122(11) 0.4122(5) 0.4707(11) 0.089(3) Uani 1 1 d . . .
H28A H 1.0238 0.4381 0.5493 0.133 Uiso 1 1 calc R . .
H28B H 1.1062 0.4075 0.4357 0.133 Uiso 1 1 calc R . .
H28C H 0.9746 0.3690 0.4899 0.133 Uiso 1 1 calc R . .
Cu1 Cu 0.80907(8) 0.82932(3) 0.10967(7) 0.03659(14) Uani 1 1 d . . .
Tb1 Tb 0.71391(2) 0.681787(11) 0.235095(19) 0.02396(4) Uani 1 1 d . . .
N1 N 0.7277(6) 0.8883(2) -0.0240(5) 0.0447(11) Uani 1 1 d . . .
N2 N 0.9985(6) 0.8693(2) 0.0843(5) 0.0456(11) Uani 1 1 d . . .
N3 N 0.5994(6) 0.6258(2) 0.4160(5) 0.0378(10) Uani 1 1 d . . .
N4 N 0.1651(5) 0.5702(3) 0.4185(6) 0.0509(13) Uani 1 1 d . . .
N5 N 0.1694(7) 0.5942(4) 0.8009(7) 0.0642(17) Uani 1 1 d . . .
N6 N 0.7941(7) 0.4975(4) 0.6887(8) 0.072(2) Uani 1 1 d . . .
N7 N 0.4746(8) 0.4298(3) 0.4052(6) 0.0620(16) Uani 1 1 d . . .
N8 N 0.5652(6) 0.6825(3) 0.7622(5) 0.0474(11) Uani 1 1 d . . .
N9 N 0.2724(7) 0.4015(3) 0.7145(5) 0.0497(12) Uani 1 1 d . . .
N10 N 0.5314(9) 0.5117(3) 0.9517(5) 0.070(2) Uani 1 1 d . . .
N11 N 0.8323(9) 0.4689(4) 0.3023(9) 0.084(2) Uani 1 1 d . . .
O1 O 0.4419(3) 0.6869(2) 0.1374(3) 0.0369(7) Uani 1 1 d . . .
O2 O 0.6341(4) 0.77697(18) 0.1141(4) 0.0337(7) Uani 1 1 d . . .
O1W O 0.7517(5) 0.6675(2) 0.0080(4) 0.0480(10) Uani 1 1 d . . .
O3 O 0.8948(4) 0.76234(18) 0.2241(4) 0.0326(7) Uani 1 1 d . . .
O2W O 0.9355(4) 0.6137(2) 0.2228(5) 0.0473(11) Uani 1 1 d . . .
O4 O 0.9203(4) 0.69489(19) 0.4377(4) 0.0368(8) Uani 1 1 d . . .
O3W O 0.6395(5) 0.5686(2) 0.1812(4) 0.0436(9) Uani 1 1 d . . .
O4W O 0.6354(5) 0.7665(2) 0.3792(4) 0.0405(9) Uani 1 1 d . . .
O5W O 0.6778(6) 0.8007(3) 0.6380(5) 0.0609(13) Uani 1 1 d . . .
O6W O 0.9181(5) 0.5679(3) -0.0678(6) 0.0622(13) Uani 1 1 d . . .
W1 W 0.442875(18) 0.539414(8) 0.639804(15) 0.02332(4) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.036(3) 0.064(5) 0.081(5) 0.011(4) 0.004(3) -0.012(3)
C2 0.038(3) 0.037(3) 0.032(2) -0.006(2) -0.0012(19) 0.008(2)
C3 0.044(3) 0.057(4) 0.044(3) -0.009(3) -0.009(2) 0.009(3)
C4 0.058(4) 0.071(5) 0.044(3) -0.004(3) -0.016(3) 0.030(4)
C5 0.063(4) 0.050(4) 0.038(3) 0.003(3) -0.007(3) 0.026(3)
C6 0.055(3) 0.038(3) 0.030(2) 0.000(2) 0.002(2) 0.017(2)
C7 0.044(3) 0.033(3) 0.024(2) -0.0024(18) 0.0015(19) 0.014(2)
C8 0.082(4) 0.029(3) 0.027(2) 0.009(2) 0.013(3) 0.015(3)
C9 0.094(5) 0.030(3) 0.056(4) 0.013(3) 0.023(4) -0.006(3)
C10 0.090(5) 0.032(3) 0.073(5) 0.016(3) 0.044(4) -0.004(3)
C11 0.051(3) 0.037(3) 0.063(4) -0.008(3) 0.026(3) -0.011(3)
C12 0.034(2) 0.040(3) 0.057(3) -0.008(3) 0.013(2) -0.006(2)
C13 0.033(3) 0.056(4) 0.089(6) -0.004(4) 0.006(3) -0.015(3)
C14 0.036(3) 0.078(6) 0.089(6) -0.005(5) -0.017(3) -0.008(3)
C15 0.037(3) 0.062(4) 0.060(4) -0.004(3) -0.010(3) -0.001(3)
C16 0.028(2) 0.035(3) 0.041(3) -0.009(2) -0.0006(19) 0.0010(19)
C17 0.029(2) 0.030(2) 0.041(3) -0.0080(19) 0.0092(18) -0.0036(18)
C18 0.045(3) 0.077(5) 0.040(3) 0.016(3) 0.001(2) -0.004(3)
C19 0.036(2) 0.031(3) 0.029(2) -0.0011(18) -0.0034(18) -0.0066(19)
C20 0.036(2) 0.033(3) 0.033(2) 0.0038(18) 0.0054(18) -0.0032(18)
C21 0.048(3) 0.044(3) 0.039(3) -0.010(2) 0.009(2) -0.005(2)
C22 0.043(3) 0.036(3) 0.041(3) -0.002(2) -0.004(2) 0.003(2)
C23 0.047(3) 0.039(3) 0.030(2) -0.001(2) 0.002(2) -0.003(2)
C24 0.051(3) 0.028(2) 0.029(2) -0.0021(18) 0.011(2) -0.005(2)
C25 0.047(3) 0.025(2) 0.029(2) -0.0003(17) 0.0003(19) -0.005(2)
C26 0.057(3) 0.041(3) 0.030(2) 0.0006(19) -0.002(2) -0.015(2)
C27 0.061(4) 0.043(4) 0.057(4) 0.001(3) -0.004(3) -0.007(3)
C28 0.076(5) 0.083(7) 0.103(8) 0.034(6) -0.016(5) -0.004(5)
Cu1 0.0445(3) 0.0283(3) 0.0380(3) 0.0091(3) 0.0095(3) -0.0011(3)
Tb1 0.02699(9) 0.02351(10) 0.02135(9) 0.00181(8) 0.00195(7) -0.00055(8)
N1 0.070(3) 0.029(2) 0.036(2) 0.0065(18) 0.012(2) 0.007(2)
N2 0.057(3) 0.033(2) 0.050(3) 0.003(2) 0.023(2) -0.005(2)
N3 0.050(3) 0.034(2) 0.030(2) 0.0037(17) 0.0096(19) -0.009(2)
N4 0.040(2) 0.061(3) 0.051(3) 0.012(3) -0.004(2) 0.001(2)
N5 0.053(3) 0.080(5) 0.062(4) -0.024(3) 0.021(3) 0.000(3)
N6 0.048(3) 0.078(5) 0.086(5) 0.003(4) -0.014(3) 0.017(3)
N7 0.086(4) 0.048(3) 0.054(3) -0.023(3) 0.013(3) -0.007(3)
N8 0.069(3) 0.029(2) 0.044(2) -0.010(2) 0.009(2) -0.010(3)
N9 0.071(3) 0.036(3) 0.041(3) 0.008(2) 0.003(2) -0.016(3)
N10 0.112(5) 0.065(4) 0.029(2) 0.009(2) -0.012(3) -0.037(4)
N11 0.091(5) 0.063(4) 0.092(6) 0.014(4) -0.030(4) -0.006(4)
O1 0.0326(15) 0.0386(19) 0.0386(18) 0.006(2) -0.0024(13) -0.0023(19)
O2 0.0391(18) 0.0303(18) 0.0310(17) 0.0092(14) -0.0015(14) -0.0007(15)
O1W 0.060(2) 0.055(3) 0.0286(17) -0.0037(17) 0.0061(16) 0.013(2)
O3 0.0329(17) 0.0288(18) 0.0357(18) 0.0031(14) 0.0009(14) -0.0013(14)
O2W 0.038(2) 0.042(2) 0.059(3) -0.011(2) -0.0084(19) 0.0135(18)
O4 0.0325(16) 0.041(2) 0.0361(18) 0.0066(15) 0.0002(13) -0.0022(15)
O3W 0.058(2) 0.0299(19) 0.041(2) -0.0066(16) -0.0077(18) -0.0049(17)
O4W 0.050(2) 0.036(2) 0.037(2) -0.0031(16) 0.0120(17) 0.0068(17)
O5W 0.093(4) 0.042(3) 0.049(3) 0.001(2) 0.016(3) -0.002(3)
O6W 0.056(3) 0.061(3) 0.072(3) -0.013(3) 0.019(2) 0.010(2)
W1 0.03074(7) 0.01999(7) 0.01910(6) 0.00044(7) 0.00148(5) -0.00316(8)

_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
C1 O1 1.444(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.368(8) . ?
C2 O1 1.390(7) . ?
C2 C7 1.396(8) . ?
C3 C4 1.413(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.359(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.401(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.406(8) . ?
C6 C8 1.465(10) . ?
C7 O2 1.323(6) . ?
C8 N1 1.271(9) . ?
C8 H8 0.9300 . ?
C9 N1 1.467(8) . ?
C9 C10 1.526(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.475(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.256(9) . ?
C11 C12 1.457(10) . ?
C11 H11 0.9300 . ?
C12 C17 1.407(7) . ?
C12 C13 1.414(9) . ?
C13 C14 1.356(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.395(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.390(8) . ?
C15 H15 0.9300 . ?
C16 O4 1.378(6) . ?
C16 C17 1.406(8) . ?
C17 O3 1.324(6) . ?
C18 O4 1.437(7) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.148(7) . ?
C19 W1 2.157(5) . ?
C20 N4 1.139(7) . ?
C20 W1 2.162(5) . ?
C21 N5 1.129(8) . ?
C21 W1 2.167(6) . ?
C22 N6 1.143(8) . ?
C22 W1 2.152(6) . ?
C23 N7 1.135(8) . ?
C23 W1 2.166(6) . ?
C24 N8 1.138(7) . ?
C24 W1 2.156(5) . ?
C25 N9 1.137(7) . ?
C25 W1 2.164(5) . ?
C26 N10 1.127(8) . ?
C26 W1 2.156(5) . ?
C27 N11 1.119(10) . ?
C27 C28 1.424(11) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cu1 O3 1.908(4) . ?
Cu1 O2 1.910(4) . ?
Cu1 N1 1.914(5) . ?
Cu1 N2 1.937(5) . ?
Cu1 Tb1 3.3776(7) . ?
Tb1 O3 2.317(4) . ?
Tb1 O2 2.361(4) . ?
Tb1 O4W 2.406(4) . ?
Tb1 O1W 2.407(4) . ?
Tb1 O3W 2.425(4) . ?
Tb1 O2W 2.447(4) . ?
Tb1 N3 2.481(4) . ?
Tb1 O1 2.585(3) . ?
Tb1 O4 2.688(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
C3 C2 O1 124.9(6) . . ?
C3 C2 C7 121.6(6) . . ?
O1 C2 C7 113.5(4) . . ?
C2 C3 C4 118.5(7) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 121.1(6) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 120.4(6) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 119.3(6) . . ?
C5 C6 C8 117.0(6) . . ?
C7 C6 C8 123.6(5) . . ?
O2 C7 C2 116.5(5) . . ?
O2 C7 C6 124.5(5) . . ?
C2 C7 C6 119.1(5) . . ?
N1 C8 C6 124.8(5) . . ?
N1 C8 H8 117.6 . . ?
C6 C8 H8 117.6 . . ?
N1 C9 C10 108.7(5) . . ?
N1 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
N1 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
N2 C10 C9 107.2(5) . . ?
N2 C10 H10A 110.3 . . ?
C9 C10 H10A 110.3 . . ?
N2 C10 H10B 110.3 . . ?
C9 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
N2 C11 C12 124.7(5) . . ?
N2 C11 H11 117.6 . . ?
C12 C11 H11 117.6 . . ?
C17 C12 C13 118.6(6) . . ?
C17 C12 C11 122.7(5) . . ?
C13 C12 C11 118.7(6) . . ?
C14 C13 C12 121.1(6) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 121.2(6) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C16 C15 C14 118.7(7) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
O4 C16 C15 124.5(6) . . ?
O4 C16 C17 114.3(4) . . ?
C15 C16 C17 121.1(6) . . ?
O3 C17 C16 116.9(4) . . ?
O3 C17 C12 123.9(5) . . ?
C16 C17 C12 119.2(5) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 W1 176.3(4) . . ?
N4 C20 W1 178.3(5) . . ?
N5 C21 W1 178.2(7) . . ?
N6 C22 W1 176.9(6) . . ?
N7 C23 W1 175.8(6) . . ?
N8 C24 W1 176.9(6) . . ?
N9 C25 W1 178.0(5) . . ?
N10 C26 W1 179.4(6) . . ?
N11 C27 C28 178.4(10) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 Cu1 O2 83.76(15) . . ?
O3 Cu1 N1 172.19(19) . . ?
O2 Cu1 N1 95.1(2) . . ?
O3 Cu1 N2 93.3(2) . . ?
O2 Cu1 N2 169.3(2) . . ?
N1 Cu1 N2 86.4(2) . . ?
O3 Cu1 Tb1 41.33(11) . . ?
O2 Cu1 Tb1 42.72(11) . . ?
N1 Cu1 Tb1 136.32(17) . . ?
N2 Cu1 Tb1 132.55(16) . . ?
O3 Tb1 O2 66.01(12) . . ?
O3 Tb1 O4W 77.63(14) . . ?
O2 Tb1 O4W 69.94(14) . . ?
O3 Tb1 O1W 82.69(14) . . ?
O2 Tb1 O1W 69.47(14) . . ?
O4W Tb1 O1W 139.22(14) . . ?
O3 Tb1 O3W 146.05(14) . . ?
O2 Tb1 O3W 125.04(14) . . ?
O4W Tb1 O3W 135.50(15) . . ?
O1W Tb1 O3W 74.17(16) . . ?
O3 Tb1 O2W 78.38(15) . . ?
O2 Tb1 O2W 129.93(16) . . ?
O4W Tb1 O2W 135.89(14) . . ?
O1W Tb1 O2W 72.18(15) . . ?
O3W Tb1 O2W 71.13(15) . . ?
O3 Tb1 N3 134.47(15) . . ?
O2 Tb1 N3 129.28(15) . . ?
O4W Tb1 N3 72.08(16) . . ?
O1W Tb1 N3 141.15(16) . . ?
O3W Tb1 N3 67.57(16) . . ?
O2W Tb1 N3 100.76(17) . . ?
O3 Tb1 O1 127.61(12) . . ?
O2 Tb1 O1 61.62(12) . . ?
O4W Tb1 O1 83.43(13) . . ?
O1W Tb1 O1 80.90(13) . . ?
O3W Tb1 O1 73.23(14) . . ?
O2W Tb1 O1 139.85(14) . . ?
N3 Tb1 O1 81.91(14) . . ?
O3 Tb1 O4 61.37(12) . . ?
O2 Tb1 O4 119.28(12) . . ?
O4W Tb1 O4 71.21(13) . . ?
O1W Tb1 O4 127.83(13) . . ?
O3W Tb1 O4 115.48(13) . . ?
O2W Tb1 O4 64.85(13) . . ?
N3 Tb1 O4 76.91(14) . . ?
O1 Tb1 O4 150.88(11) . . ?
O3 Tb1 Cu1 32.93(9) . . ?
O2 Tb1 Cu1 33.28(9) . . ?
O4W Tb1 Cu1 73.35(10) . . ?
O1W Tb1 Cu1 70.79(11) . . ?
O3W Tb1 Cu1 144.38(10) . . ?
O2W Tb1 Cu1 103.43(12) . . ?
N3 Tb1 Cu1 145.42(12) . . ?
O1 Tb1 Cu1 94.86(9) . . ?
O4 Tb1 Cu1 91.45(8) . . ?
C8 N1 C9 122.9(5) . . ?
C8 N1 Cu1 126.2(4) . . ?
C9 N1 Cu1 110.8(5) . . ?
C11 N2 C10 122.9(6) . . ?
C11 N2 Cu1 125.6(4) . . ?
C10 N2 Cu1 111.4(5) . . ?
C19 N3 Tb1 172.9(4) . . ?
C2 O1 C1 116.9(4) . . ?
C2 O1 Tb1 118.0(3) . . ?
C1 O1 Tb1 125.0(4) . . ?
C7 O2 Cu1 125.5(3) . . ?
C7 O2 Tb1 127.3(3) . . ?
Cu1 O2 Tb1 104.00(15) . . ?
C17 O3 Cu1 122.7(3) . . ?
C17 O3 Tb1 130.1(3) . . ?
Cu1 O3 Tb1 105.74(15) . . ?
C16 O4 C18 116.7(4) . . ?
C16 O4 Tb1 115.2(3) . . ?
C18 O4 Tb1 128.0(3) . . ?
C22 W1 C26 71.0(2) . . ?
C22 W1 C24 84.5(2) . . ?
C26 W1 C24 75.4(2) . . ?
C22 W1 C19 77.0(2) . . ?
C26 W1 C19 134.8(2) . . ?
C24 W1 C19 70.46(19) . . ?
C22 W1 C20 144.8(2) . . ?
C26 W1 C20 143.6(2) . . ?
C24 W1 C20 107.2(2) . . ?
C19 W1 C20 76.19(19) . . ?
C22 W1 C25 102.9(2) . . ?
C26 W1 C25 73.6(2) . . ?
C24 W1 C25 143.49(19) . . ?
C19 W1 C25 146.00(19) . . ?
C20 W1 C25 87.29(19) . . ?
C22 W1 C23 76.0(2) . . ?
C26 W1 C23 124.8(2) . . ?
C24 W1 C23 143.2(2) . . ?
C19 W1 C23 74.8(2) . . ?
C20 W1 C23 75.3(2) . . ?
C25 W1 C23 72.3(2) . . ?
C22 W1 C21 142.0(2) . . ?
C26 W1 C21 72.8(2) . . ?
C24 W1 C21 75.5(2) . . ?
C19 W1 C21 123.7(2) . . ?
C20 W1 C21 72.9(2) . . ?
C25 W1 C21 77.4(2) . . ?
C23 W1 C21 136.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        33.44
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.884
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.141