# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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.
# 
#  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_p131119a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 N12 O36 Tb2 Zn3'
_chemical_formula_weight         1654.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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/m

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

_cell_length_a                   17.3863(12)
_cell_length_b                   17.9923(11)
_cell_length_c                   10.7535(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.455(5)
_cell_angle_gamma                90.00
_cell_volume                     2740.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4095
_cell_measurement_theta_min      3.5500
_cell_measurement_theta_max      28.5130

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    3.953
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.80325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_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  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5939
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2498
_reflns_number_gt                2319
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0336P)²+10.2487P] 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         2498
_refine_ls_number_parameters     201
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0684
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Tb1 Tb 0.5000 0.290923(13) 0.5000 0.01330(10) Uani 1 2 d S . .
Zn2 Zn 0.2500 0.2500 0.5000 0.02007(16) Uani 1 2 d S . .
Zn3 Zn 0.5000 0.5000 0.5000 0.0237(2) Uani 1 4 d S . .
O O 0.2472(2) 0.19717(16) 0.3301(3) 0.0225(6) Uani 1 1 d . . .
O0AA O 0.40010(19) 0.19069(15) 0.4221(3) 0.0214(6) Uani 1 1 d . . .
O1 O 0.36549(19) 0.33040(16) 0.2328(3) 0.0233(6) Uani 1 1 d . . .
O2 O 0.4767(2) 0.25993(17) 0.2587(3) 0.0249(7) Uani 1 1 d . . .
O3 O 0.45272(18) 0.40901(14) 0.5587(3) 0.0170(6) Uani 1 1 d . . .
O4 O 0.3480(2) 0.32689(15) 0.5137(3) 0.0233(6) Uani 1 1 d . . .
O5 O 0.1359(2) 0.31627(19) 0.3258(4) 0.0349(8) Uani 1 1 d . . .
H5A H 0.1480 0.3311 0.2627 0.052 Uiso 1 1 d R . .
H5B H 0.1284 0.3546 0.3657 0.052 Uiso 1 1 d R . .
O6 O 0.3705(3) 0.5000 0.2908(5) 0.0374(11) Uani 1 2 d S . .
H6A H 0.3563 0.4558 0.2550 0.056 Uiso 0.50 1 d PR . .
H6B H 0.3731 0.5279 0.2290 0.056 Uiso 0.50 1 d PR . .
O7 O 0.1844(4) 0.3808(3) 0.1391(7) 0.107(2) Uani 1 1 d . . .
O8 O 0.0816(11) 0.5000 -0.0516(14) 0.219(8) Uani 1 2 d S . .
C5 N 0.3085(2) 0.37168(17) -0.0647(3) 0.0176(7) Uani 1 1 d . . .
C8 N 0.5818(3) 0.5000 0.2676(5) 0.0128(9) Uani 1 2 d S . .
N29 N 0.4473(2) 0.43354(17) 0.0969(3) 0.0150(7) Uani 1 1 d . . .
N30 N 0.3040(3) 0.5000 -0.0766(5) 0.0171(10) Uani 1 2 d S . .
C C 0.3547(3) 0.4373(2) -0.0148(4) 0.0144(8) Uani 1 1 d . . .
C12 C 0.4040(3) 0.2989(2) 0.1767(5) 0.0184(8) Uani 1 1 d . . .
C15 C 0.4897(4) 0.5000 0.1492(6) 0.0123(10) Uani 1 2 d S . .
C18 C 0.3139(3) 0.1777(2) 0.3237(4) 0.0159(8) Uani 1 1 d . . .
C21 C 0.6323(3) 0.5699(2) 0.3292(4) 0.0158(8) Uani 1 1 d . . .
H21A H 0.6177 0.6013 0.2447 0.019 Uiso 1 1 calc R . .
H21B H 0.6995 0.5597 0.3900 0.019 Uiso 1 1 calc R . .
C22 C 0.3620(3) 0.3039(2) 0.0076(4) 0.0201(9) Uani 1 1 d . . .
H22A H 0.4127 0.3010 -0.0053 0.024 Uiso 1 1 calc R . .
H22B H 0.3209 0.2615 -0.0441 0.024 Uiso 1 1 calc R . .
C24 C 0.2092(3) 0.3664(2) -0.1850(4) 0.0194(8) Uani 1 1 d . . .
H24A H 0.1838 0.4162 -0.2176 0.023 Uiso 1 1 calc R . .
H24B H 0.1777 0.3432 -0.1444 0.023 Uiso 1 1 calc R . .
C31 C 0.3891(3) 0.3872(2) 0.5737(4) 0.0142(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O0AA 2.299(3) . ?
Tb1 O0AA 2.299(3) 2_656 ?
Tb1 O2 2.447(3) 2_656 ?
Tb1 O2 2.447(3) . ?
Tb1 O3 2.488(3) 2_656 ?
Tb1 O3 2.488(3) . ?
Tb1 O1 2.537(3) 2_656 ?
Tb1 O1 2.537(3) . ?
Zn2 O 2.035(3) . ?
Zn2 O 2.035(3) 7_556 ?
Zn2 O4 2.132(3) 7_556 ?
Zn2 O4 2.132(3) . ?
Zn2 O5 2.134(3) 7_556 ?
Zn2 O5 2.134(3) . ?
Zn3 O6 2.063(4) . ?
Zn3 O6 2.063(4) 5_666 ?
Zn3 O3 2.087(2) 5_666 ?
Zn3 O3 2.087(2) 2_656 ?
Zn3 O3 2.087(2) 6_565 ?
Zn3 O3 2.087(2) . ?
O C18 1.251(5) . ?
O0AA C18 1.257(5) . ?
O1 C12 1.265(5) . ?
O2 C12 1.255(5) . ?
O3 C31 1.270(4) . ?
O4 C31 1.252(5) . ?
C5 C 1.352(5) . ?
C5 C24 1.439(5) . ?
C5 C22 1.455(5) . ?
C8 C15 1.348(7) . ?
C8 C21 1.455(4) . ?
C8 C21 1.455(4) 6_565 ?
N29 C 1.341(5) . ?
N29 C15 1.345(4) . ?
N30 C 1.345(4) . ?
N30 C 1.345(4) 6_565 ?
C12 C22 1.519(5) . ?
C15 N29 1.345(4) 6_565 ?
C18 C24 1.523(5) 7 ?
C21 C31 1.508(5) 5_666 ?
C24 C18 1.523(5) 7 ?
C31 C21 1.508(5) 5_666 ?

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
O0AA Tb1 O0AA 76.63(14) . 2_656 ?
O0AA Tb1 O2 80.38(10) . 2_656 ?
O0AA Tb1 O2 79.02(10) 2_656 2_656 ?
O0AA Tb1 O2 79.02(10) . . ?
O0AA Tb1 O2 80.37(10) 2_656 . ?
O2 Tb1 O2 153.65(14) 2_656 . ?
O0AA Tb1 O3 150.31(9) . 2_656 ?
O0AA Tb1 O3 118.13(9) 2_656 2_656 ?
O2 Tb1 O3 125.99(9) 2_656 2_656 ?
O2 Tb1 O3 78.56(9) . 2_656 ?
O0AA Tb1 O3 118.13(9) . . ?
O0AA Tb1 O3 150.31(10) 2_656 . ?
O2 Tb1 O3 78.56(9) 2_656 . ?
O2 Tb1 O3 125.99(9) . . ?
O3 Tb1 O3 62.70(11) 2_656 . ?
O0AA Tb1 O1 129.61(9) . 2_656 ?
O0AA Tb1 O1 78.56(10) 2_656 2_656 ?
O2 Tb1 O1 52.11(9) 2_656 2_656 ?
O2 Tb1 O1 137.89(9) . 2_656 ?
O3 Tb1 O1 79.93(9) 2_656 2_656 ?
O3 Tb1 O1 72.35(9) . 2_656 ?
O0AA Tb1 O1 78.57(10) . . ?
O0AA Tb1 O1 129.61(9) 2_656 . ?
O2 Tb1 O1 137.89(9) 2_656 . ?
O2 Tb1 O1 52.11(9) . . ?
O3 Tb1 O1 72.34(9) 2_656 . ?
O3 Tb1 O1 79.93(9) . . ?
O1 Tb1 O1 147.48(13) 2_656 . ?
O Zn2 O 180.00(17) . 7_556 ?
O Zn2 O4 91.89(11) . 7_556 ?
O Zn2 O4 88.11(11) 7_556 7_556 ?
O Zn2 O4 88.11(10) . . ?
O Zn2 O4 91.89(11) 7_556 . ?
O4 Zn2 O4 180.0 7_556 . ?
O Zn2 O5 93.04(12) . 7_556 ?
O Zn2 O5 86.96(12) 7_556 7_556 ?
O4 Zn2 O5 89.83(12) 7_556 7_556 ?
O4 Zn2 O5 90.17(12) . 7_556 ?
O Zn2 O5 86.96(12) . . ?
O Zn2 O5 93.04(12) 7_556 . ?
O4 Zn2 O5 90.17(12) 7_556 . ?
O4 Zn2 O5 89.83(12) . . ?
O5 Zn2 O5 180.0 7_556 . ?
O6 Zn3 O6 179.999(1) . 5_666 ?
O6 Zn3 O3 92.43(11) . 5_666 ?
O6 Zn3 O3 87.57(11) 5_666 5_666 ?
O6 Zn3 O3 92.43(11) . 2_656 ?
O6 Zn3 O3 87.57(11) 5_666 2_656 ?
O3 Zn3 O3 103.35(14) 5_666 2_656 ?
O6 Zn3 O3 87.57(11) . 6_565 ?
O6 Zn3 O3 92.43(11) 5_666 6_565 ?
O3 Zn3 O3 76.66(14) 5_666 6_565 ?
O3 Zn3 O3 180.0 2_656 6_565 ?
O6 Zn3 O3 87.57(11) . . ?
O6 Zn3 O3 92.43(11) 5_666 . ?
O3 Zn3 O3 180.00(14) 5_666 . ?
O3 Zn3 O3 76.65(14) 2_656 . ?
O3 Zn3 O3 103.34(14) 6_565 . ?
C18 O Zn2 129.8(3) . . ?
C18 O0AA Tb1 137.1(3) . . ?
C12 O1 Tb1 91.1(2) . . ?
C12 O2 Tb1 95.6(2) . . ?
C31 O3 Zn3 143.8(2) . . ?
C31 O3 Tb1 102.0(2) . . ?
Zn3 O3 Tb1 110.32(10) . . ?
C31 O4 Zn2 142.3(3) . . ?
C C5 C24 122.8(3) . . ?
C C5 C22 118.1(3) . . ?
C24 C5 C22 119.1(3) . . ?
C15 C8 C21 120.1(2) . . ?
C15 C8 C21 120.1(2) . 6_565 ?
C21 C8 C21 119.6(4) . 6_565 ?
C N29 C15 114.3(3) . . ?
C N30 C 113.9(4) . 6_565 ?
N29 C N30 126.0(3) . . ?
N29 C C5 116.1(3) . . ?
N30 C C5 117.9(3) . . ?
O2 C12 O1 120.7(4) . . ?
O2 C12 C22 117.6(4) . . ?
O1 C12 C22 121.6(4) . . ?
N29 C15 N29 125.5(5) 6_565 . ?
N29 C15 C8 117.2(2) 6_565 . ?
N29 C15 C8 117.2(2) . . ?
O C18 O0AA 126.3(4) . . ?
O C18 C24 118.3(3) . 7 ?
O0AA C18 C24 115.5(3) . 7 ?
C8 C21 C31 115.6(3) . 5_666 ?
C5 C22 C12 113.8(3) . . ?
C5 C24 C18 114.3(3) . 7 ?
O4 C31 O3 118.8(3) . . ?
O4 C31 C21 120.3(3) . 5_666 ?
O3 C31 C21 120.8(3) . 5_666 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.113
# 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 0.321 -0.001 9 0 ' '
2 0.000 0.679 -0.001 9 0 ' '
3 0.500 0.179 -0.001 9 0 ' '
4 0.500 0.821 -0.001 9 0 ' '
5 0.000 0.500 0.500 147 8 ' '
6 0.500 0.000 0.500 147 8 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 1017363'
#######################################################################
#
#                 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_p130722c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H36 Co3 N12 O36 Tb2'
_chemical_formula_weight         1635.34

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'
Co Co 0.3494 0.9721 '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           monoclinic
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   17.3855(15)
_cell_length_b                   17.8778(17)
_cell_length_c                   10.7117(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.437(6)
_cell_angle_gamma                90.00
_cell_volume                     2712.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1809
_cell_measurement_theta_min      3.3490
_cell_measurement_theta_max      26.5530

_exptl_crystal_description       neddle
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1598
_exptl_absorpt_coefficient_mu    3.583
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.38527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_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  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5463
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2466
_reflns_number_gt                1939
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0681P)²+0.0000P] 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         2466
_refine_ls_number_parameters     195
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1552
_refine_ls_wR_factor_gt          0.1288
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.080
_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
Tb1 Tb 0.5000 0.29118(4) 0.0000 0.0145(2) Uani 1 2 d S . .
Co2 Co 0.2500 0.2500 0.0000 0.0129(4) Uani 1 2 d S . .
Co3 Co 0.5000 0.5000 0.0000 0.0109(5) Uani 1 4 d S . .
O O 0.4547(4) 0.4080(3) 0.0615(7) 0.0106(14) Uani 1 1 d . . .
O1 O 0.4764(4) 0.2612(4) -0.2419(7) 0.0222(16) Uani 1 1 d . . .
O2 O 0.2511(4) 0.3041(4) 0.1692(7) 0.0192(11) Uani 1 1 d . . .
O3 O 0.3472(4) 0.3272(4) 0.0127(6) 0.0126(14) Uani 1 1 d . . .
O4 O 0.6266(6) 0.5000 0.2084(10) 0.028(3) Uani 1 2 d S . .
H4A H 0.6668 0.4522 0.3029 0.042 Uiso 0.50 1 d PR . .
H4B H 0.6856 0.5487 0.2792 0.042 Uiso 0.50 1 d PR . .
O5 O 0.3636(4) 0.3292(4) -0.2689(7) 0.0222(16) Uani 1 1 d . . .
O6 O 0.4029(4) 0.1896(4) -0.0736(7) 0.0192(11) Uani 1 1 d . . .
O20 O 0.3628(4) 0.1863(4) 0.1744(7) 0.0253(17) Uani 1 1 d . . .
H20A H 0.3585 0.1794 0.2514 0.038 Uiso 1 1 d R . .
H20B H 0.4170 0.2086 0.2105 0.038 Uiso 1 1 d R . .
O25 O 0.1847(8) 0.3790(7) -0.3608(13) 0.099(4) Uani 1 1 d . . .
O26 O 0.900(2) 0.5000 0.568(3) 0.194(13) Uani 1 2 d S . .
C3 N 0.6989(6) 0.5000 0.5788(10) 0.0075(19) Uani 1 2 d SU . .
C4 N 0.5545(4) 0.5670(4) 0.4064(7) 0.0071(13) Uani 1 1 d U . .
C6 N 0.6937(5) 0.6284(4) 0.5656(8) 0.0111(14) Uani 1 1 d U . .
C7 N 0.4203(6) 0.5000 0.2377(11) 0.0063(17) Uani 1 2 d SU . .
C5 C 0.4013(6) 0.2985(5) -0.3251(10) 0.013(2) Uani 1 1 d . . .
C9 C 0.6484(5) 0.5624(5) 0.5167(9) 0.0079(14) Uani 1 1 d U . .
C15 C 0.5121(8) 0.5000 0.3509(13) 0.0070(19) Uani 1 2 d SU . .
C18 C 0.3917(6) 0.3865(5) 0.0759(10) 0.0092(19) Uani 1 1 d U . .
C19 C 0.3688(6) 0.4305(5) 0.1743(10) 0.0085(16) Uani 1 1 d U . .
H19A H 0.3017 0.4415 0.1120 0.010 Uiso 1 1 calc R . .
H19B H 0.3820 0.3987 0.2581 0.010 Uiso 1 1 calc R . .
C21 C 0.1842(7) 0.3235(5) 0.1750(11) 0.018(2) Uani 1 1 d . . .
C22 C 0.7929(6) 0.6343(5) 0.6859(10) 0.0137(17) Uani 1 1 d U . .
H22A H 0.8238 0.6590 0.6454 0.016 Uiso 1 1 calc R . .
H22B H 0.8190 0.5843 0.7170 0.016 Uiso 1 1 calc R . .
C24 C 0.3596(6) 0.3036(5) -0.4927(10) 0.016(2) Uani 1 1 d . . .
H24A H 0.4103 0.3004 -0.5058 0.020 Uiso 1 1 calc R . .
H24B H 0.3184 0.2609 -0.5444 0.020 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
Tb1 O6 2.285(6) 2_655 ?
Tb1 O6 2.285(6) . ?
Tb1 O1 2.436(6) . ?
Tb1 O1 2.436(6) 2_655 ?
Tb1 O 2.453(6) 2_655 ?
Tb1 O 2.453(6) . ?
Tb1 O5 2.542(6) . ?
Tb1 O5 2.542(6) 2_655 ?
Co2 O2 2.045(7) 7 ?
Co2 O2 2.045(7) . ?
Co2 O20 2.094(6) 7 ?
Co2 O20 2.094(6) . ?
Co2 O3 2.124(6) 7 ?
Co2 O3 2.124(6) . ?
Co3 O4 2.032(8) . ?
Co3 O4 2.032(8) 5_665 ?
Co3 O 2.089(6) 5_665 ?
Co3 O 2.089(6) 6_565 ?
Co3 O 2.089(6) 2_655 ?
Co3 O 2.089(6) . ?
O C18 1.251(10) . ?
O1 C5 1.263(10) . ?
O2 C21 1.250(11) . ?
O3 C18 1.254(10) . ?
O5 C5 1.245(11) . ?
O6 C21 1.273(11) 7 ?
C3 C9 1.335(10) . ?
C3 C9 1.335(10) 6_565 ?
C4 C15 1.350(8) . ?
C4 C9 1.352(10) . ?
C6 C9 1.346(11) . ?
C6 C22 1.439(10) . ?
C6 C24 1.452(11) 5_665 ?
C7 C15 1.332(14) . ?
C7 C19 1.451(9) 6_565 ?
C7 C19 1.451(9) . ?
C5 C24 1.499(12) . ?
C15 C4 1.350(8) 6_565 ?
C18 C19 1.541(12) . ?
C21 O6 1.273(11) 7 ?
C21 C22 1.502(12) 5_666 ?
C22 C21 1.502(12) 5_666 ?
C24 C6 1.451(11) 5_665 ?

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 O6 74.8(3) 2_655 . ?
O6 Tb1 O1 80.1(2) 2_655 . ?
O6 Tb1 O1 79.8(2) . . ?
O6 Tb1 O1 79.8(2) 2_655 2_655 ?
O6 Tb1 O1 80.1(2) . 2_655 ?
O1 Tb1 O1 154.6(3) . 2_655 ?
O6 Tb1 O 118.7(2) 2_655 2_655 ?
O6 Tb1 O 150.6(2) . 2_655 ?
O1 Tb1 O 77.5(2) . 2_655 ?
O1 Tb1 O 126.2(2) 2_655 2_655 ?
O6 Tb1 O 150.6(2) 2_655 . ?
O6 Tb1 O 118.7(2) . . ?
O1 Tb1 O 126.2(2) . . ?
O1 Tb1 O 77.5(2) 2_655 . ?
O Tb1 O 63.3(3) 2_655 . ?
O6 Tb1 O5 128.4(2) 2_655 . ?
O6 Tb1 O5 78.7(2) . . ?
O1 Tb1 O5 51.9(2) . . ?
O1 Tb1 O5 137.3(2) 2_655 . ?
O Tb1 O5 72.7(2) 2_655 . ?
O Tb1 O5 81.0(2) . . ?
O6 Tb1 O5 78.7(2) 2_655 2_655 ?
O6 Tb1 O5 128.4(2) . 2_655 ?
O1 Tb1 O5 137.3(2) . 2_655 ?
O1 Tb1 O5 51.9(2) 2_655 2_655 ?
O Tb1 O5 81.0(2) 2_655 2_655 ?
O Tb1 O5 72.7(2) . 2_655 ?
O5 Tb1 O5 149.0(3) . 2_655 ?
O2 Co2 O2 179.998(1) 7 . ?
O2 Co2 O20 86.8(3) 7 7 ?
O2 Co2 O20 93.2(3) . 7 ?
O2 Co2 O20 93.2(3) 7 . ?
O2 Co2 O20 86.8(3) . . ?
O20 Co2 O20 179.998(1) 7 . ?
O2 Co2 O3 92.2(2) 7 7 ?
O2 Co2 O3 87.8(2) . 7 ?
O20 Co2 O3 89.8(2) 7 7 ?
O20 Co2 O3 90.2(2) . 7 ?
O2 Co2 O3 87.8(2) 7 . ?
O2 Co2 O3 92.2(2) . . ?
O20 Co2 O3 90.2(2) 7 . ?
O20 Co2 O3 89.8(2) . . ?
O3 Co2 O3 179.998(1) 7 . ?
O4 Co3 O4 179.999(1) . 5_665 ?
O4 Co3 O 88.9(2) . 5_665 ?
O4 Co3 O 91.1(2) 5_665 5_665 ?
O4 Co3 O 91.1(2) . 6_565 ?
O4 Co3 O 88.9(2) 5_665 6_565 ?
O Co3 O 76.1(3) 5_665 6_565 ?
O4 Co3 O 88.9(2) . 2_655 ?
O4 Co3 O 91.1(2) 5_665 2_655 ?
O Co3 O 103.9(3) 5_665 2_655 ?
O Co3 O 179.999(1) 6_565 2_655 ?
O4 Co3 O 91.1(2) . . ?
O4 Co3 O 88.9(2) 5_665 . ?
O Co3 O 180.0 5_665 . ?
O Co3 O 103.9(3) 6_565 . ?
O Co3 O 76.1(3) 2_655 . ?
C18 O Co3 142.9(6) . . ?
C18 O Tb1 102.2(5) . . ?
Co3 O Tb1 110.3(2) . . ?
C5 O1 Tb1 95.8(6) . . ?
C21 O2 Co2 130.2(6) . . ?
C18 O3 Co2 143.4(6) . . ?
C5 O5 Tb1 91.3(5) . . ?
C21 O6 Tb1 135.8(6) 7 . ?
C9 C3 C9 113.4(9) . 6_565 ?
C15 C4 C9 113.9(8) . . ?
C9 C6 C22 122.7(8) . . ?
C9 C6 C24 118.6(7) . 5_665 ?
C22 C6 C24 118.7(7) . 5_665 ?
C15 C7 C19 121.0(4) . 6_565 ?
C15 C7 C19 121.0(4) . . ?
C19 C7 C19 118.0(9) 6_565 . ?
O5 C5 O1 120.7(8) . . ?
O5 C5 C24 121.9(8) . . ?
O1 C5 C24 117.4(8) . . ?
C3 C9 C6 118.1(7) . . ?
C3 C9 C4 126.7(8) . . ?
C6 C9 C4 115.1(8) . . ?
C7 C15 C4 117.5(5) . 6_565 ?
C7 C15 C4 117.5(5) . . ?
C4 C15 C4 125.0(10) 6_565 . ?
O C18 O3 120.2(8) . . ?
O C18 C19 121.3(7) . . ?
O3 C18 C19 118.5(7) . . ?
C7 C19 C18 115.0(7) . . ?
O2 C21 O6 125.9(9) . 7 ?
O2 C21 C22 118.0(8) . 5_666 ?
O6 C21 C22 116.1(8) 7 5_666 ?
C6 C22 C21 114.6(8) . 5_666 ?
C6 C24 C5 114.2(8) 5_665 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.355
_refine_diff_density_min         -2.025
_refine_diff_density_rms         0.246
# 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 0.500 0.000 169 42 ' '
2 0.500 0.000 0.000 169 42 ' '
_platon_squeeze_details          
;
;

_database_code_depnum_ccdc_archive 'CCDC 1017364'
