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


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#                                CCDC 
# 
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# 
#  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. 
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#  fide research purposes only. It may contain copyright material 
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data_1_L
_database_code_depnum_ccdc_archive 'CCDC 885435'
#TrackingRef '- L.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H29 Cl2 Cu4 O32 Tb'
_chemical_formula_weight         1085.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/m '

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

_cell_length_a                   8.4356(19)
_cell_length_b                   18.837(4)
_cell_length_c                   10.116(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.266(2)
_cell_angle_gamma                90.00
_cell_volume                     1476.7(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3798
_cell_measurement_theta_min      2.192
_cell_measurement_theta_max      28.225

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    2.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1060
_exptl_absorpt_coefficient_mu    5.497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2000
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7209
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2673
_reflns_number_gt                2434
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0358P)^2^+4.1455P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2673
_refine_ls_number_parameters     256
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0845
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.066
_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
Tb1 Tb 0.87494(4) 0.7500 0.52684(4) 0.01866(13) Uani 1 2 d S . .
Cu1 Cu 0.44788(11) 0.7500 0.26657(10) 0.0227(2) Uani 1 2 d S . .
Cu2 Cu 0.54019(8) 0.63366(4) 0.50408(7) 0.02323(18) Uani 1 1 d . . .
Cu3 Cu 0.62932(12) 0.7500 0.73637(10) 0.0234(2) Uani 1 2 d S . .
Cl1 Cl 0.7811(2) 0.55266(9) 0.15489(19) 0.0453(4) Uani 1 1 d . . .
O1 O 0.3452(5) 0.5912(2) 0.3439(4) 0.0347(10) Uani 1 1 d . . .
O2 O 0.2757(5) 0.6761(2) 0.1742(4) 0.0376(10) Uani 1 1 d . . .
O3 O 0.5257(5) 0.6770(2) 0.8158(4) 0.0359(10) Uani 1 1 d . . .
O4 O 0.4461(6) 0.5951(2) 0.6408(4) 0.0370(10) Uani 1 1 d . . .
O5 O 1.3997(6) 0.7500 0.4962(6) 0.0278(12) Uani 1 2 d S . .
O6 O 1.1699(7) 0.7500 0.5509(7) 0.0418(16) Uani 1 2 d S . .
O7 O 0.6259(5) 0.68030(19) 0.3715(4) 0.0215(8) Uani 1 1 d D . .
H7A H 0.638(7) 0.652(3) 0.312(5) 0.026 Uiso 1 1 d D . .
O8 O 0.7350(4) 0.68077(19) 0.6534(4) 0.0205(7) Uani 1 1 d D . .
H8A H 0.788(7) 0.651(2) 0.715(5) 0.025 Uiso 1 1 d D . .
O9 O 0.5421(10) 0.7500 0.0700(7) 0.0463(17) Uani 1 2 d SD . .
O10 O 0.7134(6) 0.5321(2) 0.5161(5) 0.0348(9) Uani 1 1 d D . .
H10A H 0.732(8) 0.511(3) 0.594(3) 0.042 Uiso 1 1 d D . .
H10B H 0.659(8) 0.505(3) 0.446(4) 0.042 Uiso 1 1 d D . .
O11 O 0.9251(12) 0.7500 0.9679(8) 0.0559(19) Uani 1 2 d SD . .
H11A H 0.935(11) 0.712(3) 1.015(8) 0.067 Uiso 1 1 d D . .
O12 O 0.8757(8) 0.7500 0.2863(7) 0.0472(18) Uani 1 2 d SD . .
H12A H 0.770(4) 0.7500 0.227(7) 0.057 Uiso 1 2 d SD . .
H12B H 0.936(9) 0.7500 0.235(8) 0.057 Uiso 1 2 d SD . .
O13 O 0.9741(5) 0.6279(2) 0.5322(6) 0.0409(11) Uani 1 1 d D . .
H13A H 1.069(5) 0.611(3) 0.536(8) 0.049 Uiso 1 1 d D . .
H13B H 0.909(6) 0.593(2) 0.530(8) 0.049 Uiso 1 1 d D . .
O14 O 1.0799(8) 0.7500 0.7736(7) 0.0509(19) Uani 1 2 d SD . .
H14A H 1.053(10) 0.7500 0.846(6) 0.061 Uiso 1 2 d SD . .
H14B H 1.189(3) 0.7500 0.803(9) 0.061 Uiso 1 2 d SD . .
O15 O 1.0840(10) 0.4154(5) 0.1480(8) 0.093(2) Uani 1 1 d D . .
H15A H 0.992(8) 0.431(5) 0.151(11) 0.111 Uiso 1 1 d D . .
H15B H 1.109(12) 0.437(5) 0.086(9) 0.111 Uiso 1 1 d D . .
O16 O 0.6275(8) 0.5756(4) 0.1651(9) 0.098(3) Uani 1 1 d . . .
O17 O 0.7479(11) 0.5145(5) 0.0271(9) 0.113(3) Uani 1 1 d . . .
O18 O 0.8839(12) 0.6116(4) 0.1590(11) 0.120(3) Uani 1 1 d . . .
O19 O 0.8687(14) 0.5091(5) 0.2707(10) 0.138(4) Uani 1 1 d . . .
C1 C 0.2679(8) 0.6157(4) 0.2201(7) 0.0363(15) Uani 1 1 d . . .
H1A H 0.183(9) 0.589(4) 0.164(7) 0.044 Uiso 1 1 d . . .
C2 C 0.4598(8) 0.6198(3) 0.7599(7) 0.0373(15) Uani 1 1 d . . .
H2A H 0.4152 0.5919 0.8129 0.045 Uiso 1 1 calc R . .
C3 C 1.2423(11) 0.7500 0.4741(11) 0.062(4) Uani 1 2 d S . .
H3A H 1.1692 0.7500 0.3771 0.074 Uiso 1 2 calc SR . .
H9A H 0.516(13) 0.7135(5) 0.017(4) 0.11(4) Uiso 1 1 d 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
Tb1 0.01447(19) 0.0219(2) 0.0224(2) 0.000 0.01015(15) 0.000
Cu1 0.0187(4) 0.0236(5) 0.0233(5) 0.000 0.0058(4) 0.000
Cu2 0.0237(3) 0.0227(4) 0.0243(4) 0.0003(3) 0.0106(3) -0.0056(3)
Cu3 0.0295(5) 0.0219(5) 0.0260(5) 0.000 0.0187(4) 0.000
Cl1 0.0514(10) 0.0411(10) 0.0534(10) -0.0083(7) 0.0314(9) 0.0030(7)
O1 0.031(2) 0.035(2) 0.031(2) 0.0008(18) 0.0047(19) -0.0136(18)
O2 0.034(2) 0.035(3) 0.032(2) 0.0029(19) 0.0003(19) -0.0118(19)
O3 0.046(2) 0.037(3) 0.034(2) -0.0020(19) 0.026(2) -0.009(2)
O4 0.049(3) 0.036(2) 0.035(2) -0.0028(19) 0.026(2) -0.016(2)
O5 0.018(3) 0.038(3) 0.032(3) 0.000 0.015(2) 0.000
O6 0.020(3) 0.070(5) 0.039(3) 0.000 0.016(3) 0.000
O7 0.0248(18) 0.019(2) 0.0232(19) -0.0010(14) 0.0120(16) 0.0012(15)
O8 0.0211(18) 0.0176(19) 0.0223(19) 0.0008(14) 0.0081(16) 0.0028(15)
O9 0.072(5) 0.043(4) 0.029(3) 0.000 0.026(3) 0.000
O10 0.046(3) 0.022(2) 0.034(2) 0.0003(17) 0.014(2) -0.0023(19)
O11 0.086(5) 0.047(5) 0.033(4) 0.000 0.021(4) 0.000
O12 0.024(3) 0.086(5) 0.038(4) 0.000 0.020(3) 0.000
O13 0.032(2) 0.029(2) 0.068(3) 0.002(2) 0.027(2) 0.0069(19)
O14 0.023(3) 0.094(6) 0.034(4) 0.000 0.009(3) 0.000
O15 0.093(5) 0.119(6) 0.082(5) 0.062(4) 0.052(4) 0.068(5)
O16 0.061(4) 0.125(6) 0.123(6) -0.065(5) 0.051(4) -0.005(4)
O17 0.116(6) 0.125(7) 0.115(6) -0.075(5) 0.062(5) -0.014(5)
O18 0.139(7) 0.085(6) 0.183(9) -0.041(6) 0.114(7) -0.045(5)
O19 0.183(9) 0.131(8) 0.110(7) 0.065(6) 0.068(7) 0.093(7)
C1 0.028(3) 0.037(4) 0.037(4) -0.008(3) 0.004(3) -0.011(3)
C2 0.047(4) 0.036(4) 0.036(3) 0.000(3) 0.024(3) -0.015(3)
C3 0.012(4) 0.137(12) 0.039(6) 0.000 0.013(4) 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O6 2.402(5) . ?
Tb1 O14 2.411(6) . ?
Tb1 O8 2.434(4) 4_575 ?
Tb1 O8 2.434(4) . ?
Tb1 O12 2.436(6) . ?
Tb1 O13 2.440(4) . ?
Tb1 O13 2.440(4) 4_575 ?
Tb1 O7 2.449(4) . ?
Tb1 O7 2.449(4) 4_575 ?
Tb1 Cu3 3.5007(10) . ?
Tb1 Cu2 3.5094(9) . ?
Tb1 Cu2 3.5094(9) 4_575 ?
Cu1 O7 1.961(4) 4_575 ?
Cu1 O7 1.961(4) . ?
Cu1 O2 1.962(4) . ?
Cu1 O2 1.962(4) 4_575 ?
Cu1 O9 2.415(6) . ?
Cu2 O8 1.952(4) . ?
Cu2 O7 1.965(4) . ?
Cu2 O1 1.967(4) . ?
Cu2 O4 1.984(4) . ?
Cu2 O10 2.381(4) . ?
Cu3 O8 1.947(4) . ?
Cu3 O8 1.947(4) 4_575 ?
Cu3 O3 1.964(4) 4_575 ?
Cu3 O3 1.964(4) . ?
Cu3 O5 2.437(6) 1_455 ?
Cl1 O19 1.381(7) . ?
Cl1 O18 1.400(7) . ?
Cl1 O17 1.407(6) . ?
Cl1 O16 1.408(6) . ?
O1 C1 1.250(8) . ?
O2 C1 1.240(8) . ?
O3 C2 1.241(7) . ?
O4 C2 1.254(7) . ?
O5 C3 1.257(10) . ?
O5 Cu3 2.437(5) 1_655 ?
O6 C3 1.163(11) . ?
O7 H7A 0.84(2) . ?
O8 H8A 0.84(2) . ?
O9 H9A 0.84(2) . ?
O10 H10A 0.84(2) . ?
O10 H10B 0.84(2) . ?
O11 H11A 0.84(2) . ?
O12 H12A 0.85(2) . ?
O12 H12B 0.86(2) . ?
O13 H13A 0.85(2) . ?
O13 H13B 0.86(2) . ?
O14 H14A 0.85(2) . ?
O14 H14B 0.85(2) . ?
O15 H15A 0.85(2) . ?
O15 H15B 0.84(2) . ?
C1 H1A 0.87(7) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?

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
O6 Tb1 O14 66.7(2) . . ?
O6 Tb1 O8 130.13(14) . 4_575 ?
O14 Tb1 O8 75.75(15) . 4_575 ?
O6 Tb1 O8 130.13(13) . . ?
O14 Tb1 O8 75.75(15) . . ?
O8 Tb1 O8 64.79(17) 4_575 . ?
O6 Tb1 O12 72.0(2) . . ?
O14 Tb1 O12 138.6(2) . . ?
O8 Tb1 O12 135.92(12) 4_575 . ?
O8 Tb1 O12 135.92(12) . . ?
O6 Tb1 O13 70.47(10) . . ?
O14 Tb1 O13 82.97(13) . . ?
O8 Tb1 O13 136.58(14) 4_575 . ?
O8 Tb1 O13 73.53(13) . . ?
O12 Tb1 O13 83.46(13) . . ?
O6 Tb1 O13 70.47(10) . 4_575 ?
O14 Tb1 O13 82.97(13) . 4_575 ?
O8 Tb1 O13 73.53(13) 4_575 4_575 ?
O8 Tb1 O13 136.58(14) . 4_575 ?
O12 Tb1 O13 83.46(13) . 4_575 ?
O13 Tb1 O13 140.9(2) . 4_575 ?
O6 Tb1 O7 131.04(13) . . ?
O14 Tb1 O7 138.34(12) . . ?
O8 Tb1 O7 98.83(12) 4_575 . ?
O8 Tb1 O7 65.11(12) . . ?
O12 Tb1 O7 72.48(14) . . ?
O13 Tb1 O7 73.06(14) . . ?
O13 Tb1 O7 135.97(14) 4_575 . ?
O6 Tb1 O7 131.04(13) . 4_575 ?
O14 Tb1 O7 138.34(12) . 4_575 ?
O8 Tb1 O7 65.11(12) 4_575 4_575 ?
O8 Tb1 O7 98.83(12) . 4_575 ?
O12 Tb1 O7 72.48(14) . 4_575 ?
O13 Tb1 O7 135.97(15) . 4_575 ?
O13 Tb1 O7 73.06(14) 4_575 4_575 ?
O7 Tb1 O7 64.83(17) . 4_575 ?
O6 Tb1 Cu3 140.85(15) . . ?
O14 Tb1 Cu3 74.16(15) . . ?
O8 Tb1 Cu3 32.41(8) 4_575 . ?
O8 Tb1 Cu3 32.41(8) . . ?
O12 Tb1 Cu3 147.19(14) . . ?
O13 Tb1 Cu3 105.44(11) . . ?
O13 Tb1 Cu3 105.44(11) 4_575 . ?
O7 Tb1 Cu3 79.96(8) . . ?
O7 Tb1 Cu3 79.96(8) 4_575 . ?
O6 Tb1 Cu2 141.347(15) . . ?
O14 Tb1 Cu2 107.30(11) . . ?
O8 Tb1 Cu2 79.89(8) 4_575 . ?
O8 Tb1 Cu2 32.36(8) . . ?
O12 Tb1 Cu2 104.71(11) . . ?
O13 Tb1 Cu2 70.90(10) . . ?
O13 Tb1 Cu2 148.18(10) 4_575 . ?
O7 Tb1 Cu2 32.77(8) . . ?
O7 Tb1 Cu2 80.13(9) 4_575 . ?
Cu3 Tb1 Cu2 52.149(17) . . ?
O6 Tb1 Cu2 141.347(15) . 4_575 ?
O14 Tb1 Cu2 107.30(11) . 4_575 ?
O8 Tb1 Cu2 32.36(8) 4_575 4_575 ?
O8 Tb1 Cu2 79.89(8) . 4_575 ?
O12 Tb1 Cu2 104.71(11) . 4_575 ?
O13 Tb1 Cu2 148.18(10) . 4_575 ?
O13 Tb1 Cu2 70.90(10) 4_575 4_575 ?
O7 Tb1 Cu2 80.13(8) . 4_575 ?
O7 Tb1 Cu2 32.77(8) 4_575 4_575 ?
Cu3 Tb1 Cu2 52.149(17) . 4_575 ?
Cu2 Tb1 Cu2 77.29(3) . 4_575 ?
O7 Cu1 O7 84.1(2) 4_575 . ?
O7 Cu1 O2 175.87(17) 4_575 . ?
O7 Cu1 O2 92.69(17) . . ?
O7 Cu1 O2 92.69(17) 4_575 4_575 ?
O7 Cu1 O2 175.87(17) . 4_575 ?
O2 Cu1 O2 90.4(3) . 4_575 ?
O7 Cu1 O9 90.85(17) 4_575 . ?
O7 Cu1 O9 90.85(17) . . ?
O2 Cu1 O9 91.75(19) . . ?
O2 Cu1 O9 91.75(19) 4_575 . ?
O7 Cu1 Tb1 42.05(11) 4_575 . ?
O7 Cu1 Tb1 42.05(11) . . ?
O2 Cu1 Tb1 134.57(13) . . ?
O2 Cu1 Tb1 134.57(13) 4_575 . ?
O9 Cu1 Tb1 92.49(19) . . ?
O8 Cu2 O7 84.29(15) . . ?
O8 Cu2 O1 175.93(16) . . ?
O7 Cu2 O1 91.90(16) . . ?
O8 Cu2 O4 94.22(16) . . ?
O7 Cu2 O4 174.79(17) . . ?
O1 Cu2 O4 89.46(17) . . ?
O8 Cu2 O10 90.78(15) . . ?
O7 Cu2 O10 90.60(15) . . ?
O1 Cu2 O10 90.67(17) . . ?
O4 Cu2 O10 94.41(17) . . ?
O8 Cu2 Tb1 41.87(10) . . ?
O7 Cu2 Tb1 42.44(11) . . ?
O1 Cu2 Tb1 134.26(12) . . ?
O4 Cu2 Tb1 135.71(12) . . ?
O10 Cu2 Tb1 92.11(11) . . ?
O8 Cu3 O8 84.1(2) . 4_575 ?
O8 Cu3 O3 177.55(16) . 4_575 ?
O8 Cu3 O3 93.49(16) 4_575 4_575 ?
O8 Cu3 O3 93.49(17) . . ?
O8 Cu3 O3 177.55(16) 4_575 . ?
O3 Cu3 O3 88.9(3) 4_575 . ?
O8 Cu3 O5 83.63(14) . 1_455 ?
O8 Cu3 O5 83.63(14) 4_575 1_455 ?
O3 Cu3 O5 95.80(16) 4_575 1_455 ?
O3 Cu3 O5 95.80(16) . 1_455 ?
O8 Cu3 Tb1 42.06(11) . . ?
O8 Cu3 Tb1 42.06(11) 4_575 . ?
O3 Cu3 Tb1 135.49(13) 4_575 . ?
O3 Cu3 Tb1 135.49(13) . . ?
O5 Cu3 Tb1 79.84(12) 1_455 . ?
O19 Cl1 O18 109.1(7) . . ?
O19 Cl1 O17 108.7(6) . . ?
O18 Cl1 O17 109.2(5) . . ?
O19 Cl1 O16 108.7(6) . . ?
O18 Cl1 O16 109.4(5) . . ?
O17 Cl1 O16 111.7(5) . . ?
C1 O1 Cu2 127.6(4) . . ?
C1 O2 Cu1 127.7(4) . . ?
C2 O3 Cu3 127.8(4) . . ?
C2 O4 Cu2 128.6(4) . . ?
C3 O5 Cu3 123.0(6) . 1_655 ?
C3 O6 Tb1 136.8(6) . . ?
Cu1 O7 Cu2 105.03(16) . . ?
Cu1 O7 Tb1 105.53(15) . . ?
Cu2 O7 Tb1 104.79(15) . . ?
Cu1 O7 H7A 108(4) . . ?
Cu2 O7 H7A 113(4) . . ?
Tb1 O7 H7A 119(4) . . ?
Cu3 O8 Cu2 104.42(16) . . ?
Cu3 O8 Tb1 105.53(15) . . ?
Cu2 O8 Tb1 105.77(15) . . ?
Cu3 O8 H8A 110(4) . . ?
Cu2 O8 H8A 108(4) . . ?
Tb1 O8 H8A 122(4) . . ?
Cu1 O9 H9A 116(6) . . ?
Cu2 O10 H10A 109(4) . . ?
Cu2 O10 H10B 109(5) . . ?
H10A O10 H10B 110(3) . . ?
Tb1 O12 H12A 107(6) . . ?
Tb1 O12 H12B 147(6) . . ?
H12A O12 H12B 106(3) . . ?
Tb1 O13 H13A 132(4) . . ?
Tb1 O13 H13B 121(4) . . ?
H13A O13 H13B 107(3) . . ?
Tb1 O14 H14A 125(6) . . ?
Tb1 O14 H14B 127(6) . . ?
H14A O14 H14B 108(3) . . ?
H15A O15 H15B 111(4) . . ?
O2 C1 O1 129.1(6) . . ?
O2 C1 H1A 115(5) . . ?
O1 C1 H1A 114(5) . . ?
O3 C2 O4 127.9(5) . . ?
O3 C2 H2A 116.1 . . ?
O4 C2 H2A 116.0 . . ?
O6 C3 O5 132.7(10) . . ?
O6 C3 H3A 113.6 . . ?
O5 C3 H3A 113.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O16 0.84(2) 2.05(2) 2.876(7) 170(6) .
O8 H8A O15 0.84(2) 1.85(2) 2.688(7) 177(6) 3_766
O10 H10A O1 0.84(2) 2.20(4) 2.862(6) 136(5) 3_666
O10 H10B O4 0.84(2) 2.13(4) 2.896(6) 152(5) 3_666
O11 H11A O18 0.84(2) 2.53(3) 3.344(10) 164(8) 1_556
O12 H12A O9 0.85(2) 1.96(3) 2.800(10) 172(8) .
O13 H13B O10 0.86(2) 1.97(2) 2.800(6) 165(6) .
O14 H14A O11 0.85(2) 1.94(3) 2.756(10) 163(8) .
O15 H15A O19 0.85(2) 2.38(7) 3.120(11) 146(10) .
O15 H15A O17 0.85(2) 2.49(6) 3.206(11) 143(8) .
O15 H15B O17 0.84(2) 2.17(3) 2.980(11) 162(9) 3_765
O9 H9A O3 0.84(2) 2.18(6) 2.872(7) 139(6) 1_554

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.163


data_1_Z
_database_code_depnum_ccdc_archive 'CCDC 885436'
#TrackingRef '- Z.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H30 Cl5 Cu4 Na2 O43 Tb'
_chemical_formula_weight         1402.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c '

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

_cell_length_a                   13.117(4)
_cell_length_b                   14.410(4)
_cell_length_c                   21.239(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.672(4)
_cell_angle_gamma                90.00
_cell_volume                     3917(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9359
_cell_measurement_theta_min      2.193
_cell_measurement_theta_max      28.204

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2744
_exptl_absorpt_coefficient_mu    4.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2000
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9569
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3450
_reflns_number_gt                3297
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0558P)^2^+41.7289P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3450
_refine_ls_number_parameters     312
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1112
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.092
_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
Tb1 Tb 1.0000 0.55680(2) 0.2500 0.03154(14) Uani 1 2 d S . .
Cu1 Cu 1.05575(6) 0.75096(5) 0.35509(3) 0.03204(19) Uani 1 1 d . . .
Cu2 Cu 0.83260(5) 0.74671(5) 0.26367(3) 0.03117(19) Uani 1 1 d . A .
Cl1 Cl 1.0000 0.95521(15) 0.2500 0.0447(5) Uani 1 2 d S . .
Cl2 Cl 1.10460(15) 0.86118(14) 0.57227(9) 0.0575(5) Uani 1 1 d . A .
Cl3 Cl 1.29814(19) 1.09727(16) 0.45490(11) 0.0678(6) Uani 1 1 d . . .
Na1 Na 1.0942(2) 0.96114(19) 0.43217(14) 0.0510(7) Uani 1 1 d U . .
O1 O 0.8093(3) 0.8220(3) 0.3364(2) 0.0442(10) Uani 1 1 d . . .
O2 O 0.9735(3) 0.8378(3) 0.3956(2) 0.0392(9) Uani 1 1 d . . .
O3 O 0.7436(3) 0.8307(3) 0.2019(2) 0.0385(9) Uani 1 1 d . . .
O4 O 0.8237(3) 0.8350(3) 0.1181(2) 0.0443(10) Uani 1 1 d . . .
O5 O 0.9364(3) 0.6699(3) 0.32025(19) 0.0315(8) Uani 1 1 d D . .
H5A H 0.908(5) 0.648(4) 0.349(2) 0.038 Uiso 1 1 d D . .
O6 O 0.8710(3) 0.6722(3) 0.19514(18) 0.0312(8) Uani 1 1 d D . .
H6A H 0.818(3) 0.649(4) 0.170(3) 0.037 Uiso 1 1 d D . .
O7 O 1.1009(4) 0.6576(4) 0.4474(2) 0.0556(12) Uani 1 1 d D . .
H7A H 1.056(4) 0.638(5) 0.468(4) 0.067 Uiso 1 1 d D . .
H7B H 1.158(3) 0.628(5) 0.460(4) 0.067 Uiso 1 1 d D . .
O8 O 0.6921(4) 0.6535(5) 0.2694(3) 0.0643(15) Uani 1 1 d D . .
H8A H 0.637(4) 0.671(7) 0.243(3) 0.077 Uiso 1 1 d D . .
H8B H 0.682(6) 0.656(7) 0.3071(15) 0.077 Uiso 1 1 d D . .
O9 O 1.0545(5) 0.5017(3) 0.3597(2) 0.0542(12) Uani 1 1 d D . .
H9A H 1.078(6) 0.448(2) 0.371(3) 0.065 Uiso 1 1 d D . .
H9B H 1.061(7) 0.536(4) 0.393(2) 0.065 Uiso 1 1 d D . .
O10 O 0.8307(4) 0.5011(3) 0.2555(3) 0.0532(12) Uani 1 1 d D . .
H10A H 0.810(5) 0.4455(18) 0.253(4) 0.064 Uiso 1 1 d D . .
H10B H 0.781(4) 0.537(4) 0.257(4) 0.064 Uiso 1 1 d D . .
O11 O 1.0000 0.3872(5) 0.2500 0.058(2) Uani 1 2 d S . .
H11A H 1.017(7) 0.364(6) 0.286(4) 0.069 Uiso 1 1 d . . .
O12 O 1.0000 0.8531(4) 0.2500 0.0434(14) Uani 1 2 d S . .
O13 O 1.0775(10) 0.9887(7) 0.3089(6) 0.061(3) Uani 0.50 1 d P . .
O14 O 0.9836(15) 0.9943(8) 0.3019(6) 0.081(4) Uani 0.50 1 d P A .
O15 O 0.8998(9) 0.9777(8) 0.2647(8) 0.078(4) Uani 0.50 1 d P . .
O16 O 1.0318(6) 0.9307(5) 0.5468(3) 0.091(2) Uani 1 1 d . . .
O17 O 1.1689(5) 0.8495(7) 0.5264(3) 0.099(2) Uani 1 1 d . . .
O18 O 1.1687(8) 0.8889(8) 0.6299(3) 0.150(5) Uani 1 1 d . . .
O19 O 1.0581(8) 0.7723(7) 0.5721(6) 0.149(4) Uani 1 1 d . . .
O20 O 1.2660(8) 1.0369(8) 0.4946(5) 0.107(4) Uiso 0.83(2) 1 d PU A .
O21 O 1.1981(15) 1.1083(16) 0.4073(9) 0.178(7) Uiso 0.83(2) 1 d P A 1
O21' O 1.216(3) 1.061(3) 0.3974(18) 0.065(13) Uiso 0.17(2) 1 d P A 2
O22 O 1.3674(12) 1.0638(10) 0.4214(8) 0.190(6) Uiso 1 1 d . A .
O23 O 1.3266(16) 1.1798(15) 0.4747(10) 0.257(8) Uiso 1 1 d . A .
O24 O 1.1013(5) 0.3102(6) 0.3637(3) 0.086(2) Uani 1 1 d D . .
H24A H 1.159(4) 0.319(9) 0.391(3) 0.103 Uiso 1 1 d D . .
H24B H 1.052(5) 0.309(8) 0.384(4) 0.103 Uiso 1 1 d D . .
C1 C 0.8766(5) 0.8510(5) 0.3834(3) 0.0445(15) Uani 1 1 d . A .
H1A H 0.847(6) 0.890(5) 0.412(4) 0.053 Uiso 1 1 d . . .
C2 C 0.7520(5) 0.8553(4) 0.1473(3) 0.0397(14) Uani 1 1 d . . .
H2B H 0.706(6) 0.895(5) 0.129(4) 0.048 Uiso 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
Tb1 0.0430(2) 0.0211(2) 0.0331(2) 0.000 0.01398(16) 0.000
Cu1 0.0384(4) 0.0283(4) 0.0327(4) -0.0050(3) 0.0149(3) -0.0023(3)
Cu2 0.0348(4) 0.0280(4) 0.0338(4) -0.0023(3) 0.0142(3) 0.0005(3)
Cl1 0.0422(11) 0.0295(10) 0.0614(14) 0.000 0.0095(10) 0.000
Cl2 0.0592(10) 0.0598(11) 0.0547(10) 0.0160(8) 0.0150(8) 0.0200(9)
Cl3 0.0889(15) 0.0621(12) 0.0620(12) -0.0037(9) 0.0377(11) -0.0231(11)
Na1 0.0533(16) 0.0438(14) 0.0571(16) -0.0123(12) 0.0144(13) -0.0002(12)
O1 0.036(2) 0.051(3) 0.048(3) -0.015(2) 0.0156(19) 0.001(2)
O2 0.038(2) 0.040(2) 0.042(2) -0.0117(18) 0.0144(18) -0.0012(18)
O3 0.038(2) 0.035(2) 0.046(2) 0.0008(18) 0.0155(18) 0.0067(17)
O4 0.046(2) 0.041(2) 0.051(3) 0.013(2) 0.021(2) 0.010(2)
O5 0.038(2) 0.028(2) 0.032(2) 0.0008(16) 0.0148(16) -0.0017(16)
O6 0.039(2) 0.0254(19) 0.031(2) -0.0003(15) 0.0120(16) -0.0016(16)
O7 0.063(3) 0.060(3) 0.045(3) 0.010(2) 0.014(2) 0.005(3)
O8 0.059(3) 0.080(4) 0.058(3) -0.007(3) 0.021(3) -0.030(3)
O9 0.084(4) 0.036(3) 0.044(3) 0.008(2) 0.016(3) 0.009(2)
O10 0.052(3) 0.034(2) 0.079(4) 0.004(2) 0.026(3) -0.011(2)
O11 0.089(6) 0.028(3) 0.055(4) 0.000 0.012(4) 0.000
O12 0.056(4) 0.029(3) 0.047(4) 0.000 0.016(3) 0.000
O13 0.064(7) 0.038(5) 0.071(7) -0.003(5) -0.006(6) -0.010(5)
O14 0.136(14) 0.047(7) 0.062(8) -0.015(6) 0.030(8) 0.014(8)
O15 0.049(6) 0.047(6) 0.142(13) -0.012(7) 0.030(7) 0.009(5)
O16 0.101(5) 0.087(5) 0.073(4) -0.002(3) -0.008(4) 0.051(4)
O17 0.073(4) 0.156(8) 0.074(4) -0.026(5) 0.027(3) 0.002(5)
O18 0.162(8) 0.215(11) 0.052(4) -0.037(5) -0.019(5) 0.126(8)
O19 0.133(8) 0.108(7) 0.216(12) 0.069(8) 0.059(8) -0.015(6)
O24 0.065(4) 0.100(5) 0.097(5) 0.034(4) 0.027(3) 0.022(4)
C1 0.050(4) 0.045(4) 0.044(4) -0.015(3) 0.022(3) -0.003(3)
C2 0.038(3) 0.034(3) 0.048(4) 0.005(3) 0.011(3) 0.007(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O10 2.388(5) . ?
Tb1 O10 2.388(5) 2_755 ?
Tb1 O9 2.417(5) . ?
Tb1 O9 2.417(5) 2_755 ?
Tb1 O11 2.444(7) . ?
Tb1 O6 2.474(4) 2_755 ?
Tb1 O6 2.474(4) . ?
Tb1 O5 2.475(4) . ?
Tb1 O5 2.475(4) 2_755 ?
Cu1 O6 1.949(4) 2_755 ?
Cu1 O5 1.963(4) . ?
Cu1 O2 1.969(4) . ?
Cu1 O4 1.974(4) 2_755 ?
Cu1 O7 2.345(5) . ?
Cu1 Na1 3.427(3) . ?
Cu2 O5 1.950(4) . ?
Cu2 O6 1.961(4) . ?
Cu2 O1 1.966(4) . ?
Cu2 O3 1.969(4) . ?
Cu2 O8 2.304(5) . ?
Cl1 O14 1.298(11) . ?
Cl1 O14 1.298(11) 2_755 ?
Cl1 O15 1.453(11) . ?
Cl1 O15 1.453(11) 2_755 ?
Cl1 O12 1.472(6) . ?
Cl1 O13 1.508(11) . ?
Cl1 O13 1.508(10) 2_755 ?
Cl2 O18 1.383(8) . ?
Cl2 O16 1.407(6) . ?
Cl2 O19 1.418(10) . ?
Cl2 O17 1.431(7) . ?
Cl2 Na1 3.282(4) . ?
Cl3 O23 1.29(2) . ?
Cl3 O20 1.343(11) . ?
Cl3 O22 1.359(16) . ?
Cl3 O21 1.479(18) . ?
Cl3 O21' 1.53(4) . ?
Cl3 Na1 3.266(4) . ?
Na1 O21' 2.38(4) . ?
Na1 O16 2.385(7) 5_776 ?
Na1 O2 2.394(5) . ?
Na1 O4 2.471(5) 2_755 ?
Na1 O17 2.588(9) . ?
Na1 O20 2.591(11) . ?
Na1 O13 2.609(12) . ?
Na1 O21 2.64(2) . ?
Na1 O16 2.769(9) . ?
Na1 O14 2.868(15) . ?
O1 C1 1.250(8) . ?
O2 C1 1.255(8) . ?
O3 C2 1.240(8) . ?
O4 C2 1.270(8) . ?
O4 Cu1 1.974(4) 2_755 ?
O4 Na1 2.471(5) 2_755 ?
O5 H5A 0.84(2) . ?
O6 Cu1 1.949(4) 2_755 ?
O6 H6A 0.85(2) . ?
O7 H7A 0.85(2) . ?
O7 H7B 0.85(2) . ?
O8 H8A 0.85(2) . ?
O8 H8B 0.84(2) . ?
O9 H9A 0.85(2) . ?
O9 H9B 0.85(2) . ?
O10 H10A 0.84(2) . ?
O10 H10B 0.84(2) . ?
O11 H11A 0.81(8) . ?
O13 O14 1.211(19) . ?
O13 O15 1.66(2) 2_755 ?
O14 O15 1.228(19) . ?
O15 O13 1.66(2) 2_755 ?
O16 Na1 2.385(7) 5_776 ?
O24 H24A 0.85(2) . ?
O24 H24B 0.85(2) . ?
C1 H1A 0.97(8) . ?
C2 H2B 0.86(8) . ?

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
O10 Tb1 O10 140.7(2) . 2_755 ?
O10 Tb1 O9 85.6(2) . . ?
O10 Tb1 O9 81.69(19) 2_755 . ?
O10 Tb1 O9 81.69(19) . 2_755 ?
O10 Tb1 O9 85.6(2) 2_755 2_755 ?
O9 Tb1 O9 141.6(2) . 2_755 ?
O10 Tb1 O11 70.37(12) . . ?
O10 Tb1 O11 70.37(12) 2_755 . ?
O9 Tb1 O11 70.82(12) . . ?
O9 Tb1 O11 70.82(12) 2_755 . ?
O10 Tb1 O6 138.58(16) . 2_755 ?
O10 Tb1 O6 72.64(15) 2_755 2_755 ?
O9 Tb1 O6 74.90(16) . 2_755 ?
O9 Tb1 O6 134.59(15) 2_755 2_755 ?
O11 Tb1 O6 132.23(9) . 2_755 ?
O10 Tb1 O6 72.64(15) . . ?
O10 Tb1 O6 138.58(16) 2_755 . ?
O9 Tb1 O6 134.59(15) . . ?
O9 Tb1 O6 74.90(16) 2_755 . ?
O11 Tb1 O6 132.23(9) . . ?
O6 Tb1 O6 95.54(18) 2_755 . ?
O10 Tb1 O5 75.61(16) . . ?
O10 Tb1 O5 133.71(16) 2_755 . ?
O9 Tb1 O5 72.70(15) . . ?
O9 Tb1 O5 136.89(17) 2_755 . ?
O11 Tb1 O5 131.20(9) . . ?
O6 Tb1 O5 63.87(13) 2_755 . ?
O6 Tb1 O5 63.58(13) . . ?
O10 Tb1 O5 133.71(16) . 2_755 ?
O10 Tb1 O5 75.61(16) 2_755 2_755 ?
O9 Tb1 O5 136.89(17) . 2_755 ?
O9 Tb1 O5 72.70(15) 2_755 2_755 ?
O11 Tb1 O5 131.20(9) . 2_755 ?
O6 Tb1 O5 63.58(13) 2_755 2_755 ?
O6 Tb1 O5 63.87(13) . 2_755 ?
O5 Tb1 O5 97.60(18) . 2_755 ?
O6 Cu1 O5 84.00(17) 2_755 . ?
O6 Cu1 O2 172.89(17) 2_755 . ?
O5 Cu1 O2 94.28(17) . . ?
O6 Cu1 O4 93.17(18) 2_755 2_755 ?
O5 Cu1 O4 174.78(18) . 2_755 ?
O2 Cu1 O4 88.00(18) . 2_755 ?
O6 Cu1 O7 93.39(18) 2_755 . ?
O5 Cu1 O7 90.49(18) . . ?
O2 Cu1 O7 93.52(19) . . ?
O4 Cu1 O7 94.1(2) 2_755 . ?
O6 Cu1 Na1 137.51(13) 2_755 . ?
O5 Cu1 Na1 136.67(13) . . ?
O2 Cu1 Na1 42.87(13) . . ?
O4 Cu1 Na1 45.19(14) 2_755 . ?
O7 Cu1 Na1 97.11(15) . . ?
O5 Cu2 O6 83.60(16) . . ?
O5 Cu2 O1 92.08(18) . . ?
O6 Cu2 O1 174.18(18) . . ?
O5 Cu2 O3 172.27(17) . . ?
O6 Cu2 O3 93.06(17) . . ?
O1 Cu2 O3 90.75(19) . . ?
O5 Cu2 O8 95.5(2) . . ?
O6 Cu2 O8 93.35(19) . . ?
O1 Cu2 O8 90.9(2) . . ?
O3 Cu2 O8 91.7(2) . . ?
O14 Cl1 O14 128.5(12) . 2_755 ?
O14 Cl1 O15 52.7(9) . . ?
O14 Cl1 O15 114.3(9) 2_755 . ?
O14 Cl1 O15 114.3(9) . 2_755 ?
O14 Cl1 O15 52.7(9) 2_755 2_755 ?
O15 Cl1 O15 154.2(10) . 2_755 ?
O14 Cl1 O12 115.7(6) . . ?
O14 Cl1 O12 115.7(6) 2_755 . ?
O15 Cl1 O12 102.9(5) . . ?
O15 Cl1 O12 102.9(5) 2_755 . ?
O14 Cl1 O13 50.4(9) . . ?
O14 Cl1 O13 111.0(8) 2_755 . ?
O15 Cl1 O13 103.1(8) . . ?
O15 Cl1 O13 68.3(8) 2_755 . ?
O12 Cl1 O13 108.6(4) . . ?
O14 Cl1 O13 111.0(8) . 2_755 ?
O14 Cl1 O13 50.4(9) 2_755 2_755 ?
O15 Cl1 O13 68.3(8) . 2_755 ?
O15 Cl1 O13 103.1(8) 2_755 2_755 ?
O12 Cl1 O13 108.6(4) . 2_755 ?
O13 Cl1 O13 142.7(8) . 2_755 ?
O18 Cl2 O16 111.3(5) . . ?
O18 Cl2 O19 116.2(8) . . ?
O16 Cl2 O19 112.7(6) . . ?
O18 Cl2 O17 107.5(5) . . ?
O16 Cl2 O17 105.9(5) . . ?
O19 Cl2 O17 102.1(7) . . ?
O18 Cl2 Na1 124.9(6) . . ?
O16 Cl2 Na1 56.6(3) . . ?
O19 Cl2 Na1 117.5(5) . . ?
O17 Cl2 Na1 49.3(4) . . ?
O23 Cl3 O20 120.1(10) . . ?
O23 Cl3 O22 108.6(11) . . ?
O20 Cl3 O22 115.9(8) . . ?
O23 Cl3 O21 105.9(13) . . ?
O20 Cl3 O21 98.4(9) . . ?
O22 Cl3 O21 106.0(11) . . ?
O23 Cl3 O21' 132.8(18) . . ?
O20 Cl3 O21' 90.9(15) . . ?
O22 Cl3 O21' 83.9(17) . . ?
O21 Cl3 O21' 29.5(15) . . ?
O23 Cl3 Na1 140.5(9) . . ?
O20 Cl3 Na1 49.0(5) . . ?
O22 Cl3 Na1 109.2(7) . . ?
O21 Cl3 Na1 52.3(8) . . ?
O21' Cl3 Na1 42.9(14) . . ?
O21' Na1 O16 101.8(11) . 5_776 ?
O21' Na1 O2 142.0(10) . . ?
O16 Na1 O2 96.3(2) 5_776 . ?
O21' Na1 O4 85.6(11) . 2_755 ?
O16 Na1 O4 161.3(2) 5_776 2_755 ?
O2 Na1 O4 68.50(15) . 2_755 ?
O21' Na1 O17 116.6(9) . . ?
O16 Na1 O17 115.0(3) 5_776 . ?
O2 Na1 O17 84.3(2) . . ?
O4 Na1 O17 75.5(2) 2_755 . ?
O21' Na1 O20 48.5(9) . . ?
O16 Na1 O20 100.9(3) 5_776 . ?
O2 Na1 O20 156.6(3) . . ?
O4 Na1 O20 96.8(3) 2_755 . ?
O17 Na1 O20 74.2(3) . . ?
O21' Na1 O13 60.8(9) . . ?
O16 Na1 O13 100.3(3) 5_776 . ?
O2 Na1 O13 83.3(3) . . ?
O4 Na1 O13 68.1(3) 2_755 . ?
O17 Na1 O13 143.6(3) . . ?
O20 Na1 O13 108.8(4) . . ?
O21' Na1 O21 16.7(10) . . ?
O16 Na1 O21 85.5(6) 5_776 . ?
O2 Na1 O21 150.0(4) . . ?
O4 Na1 O21 102.2(5) 2_755 . ?
O17 Na1 O21 122.1(5) . . ?
O20 Na1 O21 48.3(5) . . ?
O13 Na1 O21 67.0(5) . . ?
O21' Na1 O16 135.7(10) . . ?
O16 Na1 O16 65.7(3) 5_776 . ?
O2 Na1 O16 82.3(2) . . ?
O4 Na1 O16 120.3(2) 2_755 . ?
O17 Na1 O16 49.9(2) . . ?
O20 Na1 O16 90.5(3) . . ?
O13 Na1 O16 158.5(3) . . ?
O21 Na1 O16 124.7(5) . . ?
O21' Na1 O14 80.4(10) . . ?
O16 Na1 O14 81.2(3) 5_776 . ?
O2 Na1 O14 69.6(3) . . ?
O4 Na1 O14 83.2(3) 2_755 . ?
O17 Na1 O14 151.1(3) . . ?
O20 Na1 O14 128.5(4) . . ?
O13 Na1 O14 25.0(4) . . ?
O21 Na1 O14 81.2(5) . . ?
O16 Na1 O14 133.6(4) . . ?
O21' Na1 Cl3 25.9(9) . . ?
O16 Na1 Cl3 99.1(2) 5_776 . ?
O2 Na1 Cl3 162.91(15) . . ?
O4 Na1 Cl3 94.91(14) 2_755 . ?
O17 Na1 Cl3 95.8(2) . . ?
O20 Na1 Cl3 23.0(2) . . ?
O13 Na1 Cl3 86.7(3) . . ?
O21 Na1 Cl3 26.4(4) . . ?
O16 Na1 Cl3 110.85(19) . . ?
O14 Na1 Cl3 105.5(4) . . ?
O21' Na1 Cl2 130.4(9) . . ?
O16 Na1 Cl2 90.6(2) 5_776 . ?
O2 Na1 Cl2 82.02(14) . . ?
O4 Na1 Cl2 97.67(15) 2_755 . ?
O17 Na1 Cl2 24.80(15) . . ?
O20 Na1 Cl2 82.1(3) . . ?
O13 Na1 Cl2 162.6(2) . . ?
O21 Na1 Cl2 127.9(4) . . ?
O16 Na1 Cl2 25.10(13) . . ?
O14 Na1 Cl2 149.2(4) . . ?
Cl3 Na1 Cl2 105.07(10) . . ?
C1 O1 Cu2 127.4(4) . . ?
C1 O2 Cu1 129.3(4) . . ?
C1 O2 Na1 121.5(4) . . ?
Cu1 O2 Na1 103.10(18) . . ?
C2 O3 Cu2 129.6(4) . . ?
C2 O4 Cu1 129.2(4) . 2_755 ?
C2 O4 Na1 118.8(4) . 2_755 ?
Cu1 O4 Na1 100.30(19) 2_755 2_755 ?
Cu2 O5 Cu1 106.63(18) . . ?
Cu2 O5 Tb1 106.51(16) . . ?
Cu1 O5 Tb1 105.82(16) . . ?
Cu2 O5 H5A 107(5) . . ?
Cu1 O5 H5A 113(5) . . ?
Tb1 O5 H5A 117(5) . . ?
Cu1 O6 Cu2 108.97(18) 2_755 . ?
Cu1 O6 Tb1 106.31(17) 2_755 . ?
Cu2 O6 Tb1 106.20(16) . . ?
Cu1 O6 H6A 109(5) 2_755 . ?
Cu2 O6 H6A 111(5) . . ?
Tb1 O6 H6A 114(5) . . ?
Cu1 O7 H7A 123(5) . . ?
Cu1 O7 H7B 127(5) . . ?
H7A O7 H7B 109(3) . . ?
Cu2 O8 H8A 111(7) . . ?
Cu2 O8 H8B 109(6) . . ?
H8A O8 H8B 109(3) . . ?
Tb1 O9 H9A 126(5) . . ?
Tb1 O9 H9B 124(5) . . ?
H9A O9 H9B 109(3) . . ?
Tb1 O10 H10A 127(5) . . ?
Tb1 O10 H10B 123(5) . . ?
H10A O10 H10B 110(3) . . ?
Tb1 O11 H11A 114(7) . . ?
O14 O13 Cl1 55.7(7) . . ?
O14 O13 O15 106.1(10) . 2_755 ?
Cl1 O13 O15 54.3(6) . 2_755 ?
O14 O13 Na1 89.6(10) . . ?
Cl1 O13 Na1 132.6(7) . . ?
O15 O13 Na1 159.5(8) 2_755 . ?
O13 O14 O15 144.0(13) . . ?
O13 O14 Cl1 73.8(10) . . ?
O15 O14 Cl1 70.1(9) . . ?
O13 O14 Na1 65.4(9) . . ?
O15 O14 Na1 141.3(12) . . ?
Cl1 O14 Na1 127.2(9) . . ?
O14 O15 Cl1 57.2(7) . . ?
O14 O15 O13 105.5(11) . 2_755 ?
Cl1 O15 O13 57.4(6) . 2_755 ?
Cl2 O16 Na1 146.4(5) . 5_776 ?
Cl2 O16 Na1 98.3(4) . . ?
Na1 O16 Na1 114.3(3) 5_776 . ?
Cl2 O17 Na1 105.9(4) . . ?
Cl3 O20 Na1 108.0(6) . . ?
Cl3 O21 Na1 101.3(10) . . ?
Cl3 O21' Na1 111.2(19) . . ?
H24A O24 H24B 109(4) . . ?
O1 C1 O2 128.3(6) . . ?
O1 C1 H1A 112(4) . . ?
O2 C1 H1A 119(4) . . ?
O3 C2 O4 128.2(6) . . ?
O3 C2 H2B 114(5) . . ?
O4 C2 H2B 117(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O22 0.84(2) 2.12(3) 2.938(16) 164(6) 3_445
O6 H6A O18 0.85(2) 2.03(3) 2.851(9) 163(6) 8_465
O7 H7B O17 0.85(2) 2.25(5) 2.949(9) 139(7) 7_766
O8 H8B O21 0.84(2) 2.20(4) 2.98(2) 155(8) 3_445
O9 H9A O24 0.85(2) 2.02(3) 2.825(10) 157(7) .
O9 H9B O7 0.85(2) 2.11(4) 2.896(8) 155(7) .
O10 H10A O3 0.84(2) 2.12(5) 2.861(6) 147(8) 4_645
O10 H10B O8 0.84(2) 2.09(3) 2.906(8) 163(7) .
O10 H10B O15 0.84(2) 2.46(6) 2.979(12) 121(5) 4_645
O11 H11A O24 0.81(8) 1.95(8) 2.725(7) 161(9) .
O24 H24A O1 0.85(2) 2.50(8) 2.916(8) 112(7) 3_545
O24 H24B O19 0.85(2) 2.22(7) 2.982(12) 150(11) 5_766

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.136