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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1456716'
_audit_update_record             
;
2016-03-04 deposited with the CCDC.
2016-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 N4 O22 Sm2 Zn'
_chemical_formula_weight         1182.62

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'
Sm Sm -0.1638 3.4418 '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           orthorhombic
_symmetry_space_group_name_H-M   'I b a 2'

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

_cell_length_a                   13.390(3)
_cell_length_b                   24.074(5)
_cell_length_c                   13.179(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4248.5(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7467
_cell_measurement_theta_min      1.6918
_cell_measurement_theta_max      27.9183

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2296
_exptl_absorpt_coefficient_mu    3.374
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_T_max  0.667
_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  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16610
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3734
_reflns_number_gt                3582
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.3000P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(4)
_refine_ls_number_reflns         3734
_refine_ls_number_parameters     281
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1253
_refine_ls_R_factor_gt           0.1244
_refine_ls_wR_factor_ref         0.2993
_refine_ls_wR_factor_gt          0.2952
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.022
_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
O4 O 0.2986(9) 1.1124(5) 0.2086(10) 0.045(3) Uani 1 1 d . . .
O3 O 0.4325(8) 1.0612(6) 0.2118(11) 0.041(3) Uani 1 1 d . . .
C8 C 0.3413(12) 1.0699(8) 0.2315(12) 0.037(4) Uani 1 1 d . . .
Sm1 Sm 0.44108(4) 0.84298(2) 0.61653(10) 0.0256(4) Uani 1 1 d . . .
Zn1 Zn 0.0000 0.5000 0.6179(3) 0.0363(6) Uani 1 2 d S . .
O6 O 0.5130(8) 0.7388(4) 0.6259(12) 0.035(2) Uani 1 1 d . . .
O5 O 0.3536(8) 0.7574(4) 0.6103(14) 0.041(3) Uani 1 1 d . . .
C13 C 0.3355(11) 0.5523(6) 0.5845(12) 0.030(3) Uani 1 1 d . . .
H13 H 0.3159 0.5158 0.5729 0.036 Uiso 1 1 calc R . .
C10 C 0.3971(10) 0.6615(5) 0.6098(19) 0.033(4) Uani 1 1 d . . .
C14 C 0.2631(10) 0.5933(6) 0.5966(14) 0.036(4) Uani 1 1 d . . .
C16 C 0.2986(12) 0.6476(6) 0.6043(13) 0.031(3) Uani 1 1 d . . .
H16 H 0.2519 0.6762 0.6058 0.037 Uiso 1 1 calc R . .
O8 O 0.1313(7) 0.5323(4) 0.5880(8) 0.035(3) Uani 1 1 d . . .
C15 C 0.1565(10) 0.5816(5) 0.5998(13) 0.032(3) Uani 1 1 d . . .
C11 C 0.4690(11) 0.6192(5) 0.6031(15) 0.033(4) Uani 1 1 d . . .
H11 H 0.5366 0.6277 0.6077 0.040 Uiso 1 1 calc R . .
O10 O 0.4722(12) 0.8197(5) 0.7873(10) 0.041(3) Uani 1 1 d . . .
H10A H 0.4199 0.8255 0.8222 0.062 Uiso 1 1 d R . .
H10B H 0.4883 0.7856 0.7912 0.062 Uiso 1 1 d R . .
O9 O 0.4943(12) 0.8090(6) 0.4518(10) 0.047(3) Uani 1 1 d . . .
H9A H 0.4974 0.7737 0.4532 0.071 Uiso 1 1 d R . .
H9B H 0.4526 0.8192 0.4069 0.071 Uiso 1 1 d R . .
C12 C 0.4392(8) 0.5656(7) 0.5897(12) 0.026(4) Uani 1 1 d . . .
C9 C 0.4268(11) 0.7230(6) 0.6215(18) 0.033(3) Uani 1 1 d U . .
C1 C 0.3406(11) 0.9095(8) 0.4673(12) 0.037(4) Uani 1 1 d . . .
C3 C 0.3381(9) 0.9889(7) 0.3485(10) 0.034(3) Uani 1 1 d . . .
H3 H 0.4073 0.9910 0.3533 0.041 Uiso 1 1 calc R . .
O7 O 0.0992(7) 0.6221(3) 0.6150(12) 0.036(2) Uani 1 1 d . . .
N2 N 0.5152(9) 0.5239(5) 0.5850(9) 0.029(3) Uani 1 1 d . . .
C4 C 0.2834(11) 1.0273(6) 0.2890(12) 0.032(3) Uani 1 1 d . . .
C2 C 0.2843(10) 0.9476(6) 0.4002(13) 0.034(3) Uani 1 1 d . . .
O1 O 0.3026(8) 0.8636(5) 0.4961(10) 0.038(2) Uani 1 1 d . . .
O2 O 0.4289(9) 0.9255(5) 0.5005(10) 0.034(3) Uani 1 1 d . . .
C7 C 0.1792(10) 0.9434(7) 0.3904(13) 0.037(3) Uani 1 1 d . . .
H7 H 0.1451 0.9138 0.4198 0.044 Uiso 1 1 calc R . .
C5 C 0.1793(10) 1.0268(6) 0.2887(12) 0.030(3) Uani 1 1 d . . .
H5 H 0.1437 1.0550 0.2567 0.037 Uiso 1 1 calc R . .
C6 C 0.1287(9) 0.9828(6) 0.3377(11) 0.026(3) Uani 1 1 d . . .
N1 N 0.0241(10) 0.9769(5) 0.3363(11) 0.035(3) Uani 1 1 d . . .
O0AA O 0.1252(9) 0.8024(6) 0.4487(11) 0.050(3) Uani 1 1 d G . .
H0AA H 0.1287 0.7703 0.4753 0.075 Uiso 1 1 d G . .
H0AB H 0.0747 0.8195 0.4721 0.075 Uiso 1 1 d G . .


_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
O4 C8 1.21(2) . ?
O4 Sm1 2.503(12) 4_574 ?
O3 C8 1.27(2) . ?
O3 Zn1 2.126(13) 5_554 ?
O3 Sm1 2.628(15) 4_574 ?
C8 C4 1.49(2) . ?
C8 Sm1 2.912(18) 4_574 ?
Sm1 O7 2.278(9) 8_564 ?
Sm1 O10 2.356(13) . ?
Sm1 O5 2.371(9) . ?
Sm1 O9 2.427(13) . ?
Sm1 O1 2.491(11) . ?
Sm1 O4 2.503(12) 4_575 ?
Sm1 O2 2.511(12) . ?
Sm1 O3 2.628(15) 4_575 ?
Sm1 O6 2.690(9) . ?
Sm1 C1 2.871(14) . ?
Sm1 C9 2.895(14) . ?
Sm1 C8 2.912(18) 4_575 ?
Zn1 O8 1.962(10) 2_565 ?
Zn1 O8 1.962(10) . ?
Zn1 O3 2.126(13) 6_565 ?
Zn1 O3 2.126(13) 5_445 ?
O6 C9 1.216(18) . ?
O5 C9 1.292(18) . ?
C13 C14 1.393(19) . ?
C13 C12 1.427(19) . ?
C10 C16 1.36(2) . ?
C10 C11 1.405(19) . ?
C10 C9 1.54(2) . ?
C14 C16 1.39(2) . ?
C14 C15 1.456(19) . ?
O8 C15 1.243(17) . ?
C15 O7 1.257(16) . ?
C11 C12 1.36(2) . ?
C12 N2 1.430(17) . ?
C1 O1 1.28(2) . ?
C1 O2 1.32(2) . ?
C1 C2 1.48(2) . ?
C3 C2 1.40(2) . ?
C3 C4 1.42(2) . ?
O7 Sm1 2.278(9) 8_464 ?
N2 N2 1.22(2) 2_665 ?
C4 C5 1.39(2) . ?
C2 C7 1.417(19) . ?
C7 C6 1.36(2) . ?
C5 C6 1.41(2) . ?
C6 N1 1.409(16) . ?
N1 N1 1.28(3) 2_575 ?

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
C8 O4 Sm1 97.1(10) . 4_574 ?
C8 O3 Zn1 130.1(12) . 5_554 ?
C8 O3 Sm1 89.7(10) . 4_574 ?
Zn1 O3 Sm1 108.2(6) 5_554 4_574 ?
O4 C8 O3 123.0(16) . . ?
O4 C8 C4 117.5(15) . . ?
O3 C8 C4 119.4(14) . . ?
O4 C8 Sm1 58.6(9) . 4_574 ?
O3 C8 Sm1 64.5(9) . 4_574 ?
C4 C8 Sm1 176.0(10) . 4_574 ?
O7 Sm1 O10 86.1(6) 8_564 . ?
O7 Sm1 O5 141.2(3) 8_564 . ?
O10 Sm1 O5 85.1(6) . . ?
O7 Sm1 O9 81.0(5) 8_564 . ?
O10 Sm1 O9 136.2(5) . . ?
O5 Sm1 O9 79.7(5) . . ?
O7 Sm1 O1 127.8(4) 8_564 . ?
O10 Sm1 O1 142.0(5) . . ?
O5 Sm1 O1 77.5(4) . . ?
O9 Sm1 O1 73.5(5) . . ?
O7 Sm1 O4 123.7(4) 8_564 4_575 ?
O10 Sm1 O4 76.9(5) . 4_575 ?
O5 Sm1 O4 90.7(4) . 4_575 ?
O9 Sm1 O4 143.3(5) . 4_575 ?
O1 Sm1 O4 69.9(4) . 4_575 ?
O7 Sm1 O2 76.3(4) 8_564 . ?
O10 Sm1 O2 141.4(5) . . ?
O5 Sm1 O2 129.3(5) . . ?
O9 Sm1 O2 75.0(4) . . ?
O1 Sm1 O2 53.6(4) . . ?
O4 Sm1 O2 84.6(4) 4_575 . ?
O7 Sm1 O3 73.8(4) 8_564 4_575 ?
O10 Sm1 O3 76.1(4) . 4_575 ?
O5 Sm1 O3 139.2(5) . 4_575 ?
O9 Sm1 O3 137.4(4) . 4_575 ?
O1 Sm1 O3 95.6(4) . 4_575 ?
O4 Sm1 O3 50.1(4) 4_575 4_575 ?
O2 Sm1 O3 66.1(4) . 4_575 ?
O7 Sm1 O6 90.7(3) 8_564 . ?
O10 Sm1 O6 70.8(5) . . ?
O5 Sm1 O6 50.8(3) . . ?
O9 Sm1 O6 67.8(4) . . ?
O1 Sm1 O6 118.8(4) . . ?
O4 Sm1 O6 130.6(4) 4_575 . ?
O2 Sm1 O6 142.1(4) . . ?
O3 Sm1 O6 144.3(4) 4_575 . ?
O7 Sm1 C1 102.9(5) 8_564 . ?
O10 Sm1 C1 150.4(5) . . ?
O5 Sm1 C1 103.3(5) . . ?
O9 Sm1 C1 73.3(5) . . ?
O1 Sm1 C1 26.3(4) . . ?
O4 Sm1 C1 74.7(5) 4_575 . ?
O2 Sm1 C1 27.3(5) . . ?
O3 Sm1 C1 79.5(5) 4_575 . ?
O6 Sm1 C1 136.0(5) . . ?
O7 Sm1 C9 115.5(3) 8_564 . ?
O10 Sm1 C9 75.7(6) . . ?
O5 Sm1 C9 26.0(4) . . ?
O9 Sm1 C9 72.7(5) . . ?
O1 Sm1 C9 99.4(5) . . ?
O4 Sm1 C9 111.5(4) 4_575 . ?
O2 Sm1 C9 143.0(6) . . ?
O3 Sm1 C9 149.5(6) 4_575 . ?
O6 Sm1 C9 24.8(3) . . ?
C1 Sm1 C9 122.8(6) . . ?
O7 Sm1 C8 99.5(4) 8_564 4_575 ?
O10 Sm1 C8 75.9(5) . 4_575 ?
O5 Sm1 C8 114.6(5) . 4_575 ?
O9 Sm1 C8 147.5(5) . 4_575 ?
O1 Sm1 C8 81.2(4) . 4_575 ?
O4 Sm1 C8 24.4(4) 4_575 4_575 ?
O2 Sm1 C8 73.6(4) . 4_575 ?
O3 Sm1 C8 25.8(4) 4_575 4_575 ?
O6 Sm1 C8 144.3(5) . 4_575 ?
C1 Sm1 C8 74.9(6) . 4_575 ?
C9 Sm1 C8 132.6(5) . 4_575 ?
O8 Zn1 O8 156.8(7) 2_565 . ?
O8 Zn1 O3 102.9(5) 2_565 6_565 ?
O8 Zn1 O3 90.6(5) . 6_565 ?
O8 Zn1 O3 90.6(5) 2_565 5_445 ?
O8 Zn1 O3 102.9(5) . 5_445 ?
O3 Zn1 O3 108.8(8) 6_565 5_445 ?
C9 O6 Sm1 87.1(8) . . ?
C9 O5 Sm1 100.3(9) . . ?
C14 C13 C12 120.8(13) . . ?
C16 C10 C11 118.7(13) . . ?
C16 C10 C9 119.5(12) . . ?
C11 C10 C9 121.8(12) . . ?
C13 C14 C16 115.8(13) . . ?
C13 C14 C15 123.2(13) . . ?
C16 C14 C15 121.0(12) . . ?
C10 C16 C14 124.4(14) . . ?
C15 O8 Zn1 126.6(10) . . ?
O8 C15 O7 126.5(12) . . ?
O8 C15 C14 116.6(11) . . ?
O7 C15 C14 116.9(11) . . ?
C12 C11 C10 119.6(13) . . ?
C11 C12 C13 120.3(13) . . ?
C11 C12 N2 117.5(11) . . ?
C13 C12 N2 122.2(13) . . ?
O6 C9 O5 121.7(13) . . ?
O6 C9 C10 123.3(12) . . ?
O5 C9 C10 114.1(13) . . ?
O6 C9 Sm1 68.1(8) . . ?
O5 C9 Sm1 53.7(7) . . ?
C10 C9 Sm1 166.7(13) . . ?
O1 C1 O2 120.8(13) . . ?
O1 C1 C2 120.7(14) . . ?
O2 C1 C2 118.4(15) . . ?
O1 C1 Sm1 60.0(7) . . ?
O2 C1 Sm1 61.0(7) . . ?
C2 C1 Sm1 173.5(12) . . ?
C2 C3 C4 117.7(12) . . ?
C15 O7 Sm1 148.8(9) . 8_464 ?
N2 N2 C12 115.2(14) 2_665 . ?
C5 C4 C3 121.0(15) . . ?
C5 C4 C8 121.5(14) . . ?
C3 C4 C8 117.5(13) . . ?
C3 C2 C7 121.1(14) . . ?
C3 C2 C1 117.8(12) . . ?
C7 C2 C1 121.1(14) . . ?
C1 O1 Sm1 93.7(8) . . ?
C1 O2 Sm1 91.7(9) . . ?
C6 C7 C2 119.5(13) . . ?
C4 C5 C6 118.9(14) . . ?
C7 C6 N1 115.6(12) . . ?
C7 C6 C5 121.3(12) . . ?
N1 C6 C5 123.1(13) . . ?
N1 N1 C6 114.3(15) 2_575 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         3.257
_refine_diff_density_min         -7.447
_refine_diff_density_rms         0.507
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1456717'
_audit_update_record             
;
2016-03-04 deposited with the CCDC.
2016-04-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 N4 O22 Tb2 Zn'
_chemical_formula_weight         1199.76

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           orthorhombic
_symmetry_space_group_name_H-M   Iba2

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

_cell_length_a                   13.368(3)
_cell_length_b                   23.922(5)
_cell_length_c                   13.092(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4186.8(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6405
_cell_measurement_theta_min      1.7026
_cell_measurement_theta_max      27.8505

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2320
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_T_max  0.671
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16849
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3678
_reflns_number_gt                3346
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1350P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_number_reflns         3678
_refine_ls_number_parameters     276
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1631
_refine_ls_wR_factor_gt          0.1562
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.013
_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
O3 O 1.0706(6) 0.4247(4) 0.9972(7) 0.0132(19) Uani 1 1 d U . .
O4 O 1.1964(7) 0.3643(4) 0.9933(7) 0.025(2) Uani 1 1 d . . .
C5 C 1.1578(9) 0.4108(5) 0.9650(9) 0.016(2) Uani 1 1 d U . .
O5 O 0.8693(5) 0.5334(3) 0.5841(6) 0.021(2) Uani 1 1 d . . .
O8 O 0.6450(5) 0.7595(2) 0.6092(12) 0.0261(15) Uani 1 1 d . . .
O7 O 0.4839(5) 0.7399(3) 0.6182(10) 0.0210(16) Uani 1 1 d . . .
C16 C 0.5732(6) 0.7250(4) 0.6111(16) 0.0155(18) Uani 1 1 d U . .
C14 C 0.6015(7) 0.6635(3) 0.6011(12) 0.015(2) Uani 1 1 d U . .
Tb1 Tb 1.05756(2) 0.656500(14) 0.61083(8) 0.0106(2) Uani 1 1 d . . .
Zn1 Zn 1.0000 0.5000 0.6094(3) 0.0210(4) Uani 1 2 d S . .
O1 O 1.0657(6) 0.5617(4) 0.7063(7) 0.019(2) Uani 1 1 d . . .
C11 C 0.6628(7) 0.5523(4) 0.5820(7) 0.014(2) Uani 1 1 d . . .
H11 H 0.6837 0.5156 0.5720 0.016 Uiso 1 1 calc R . .
C10 C 0.7320(7) 0.5945(4) 0.5939(14) 0.025(4) Uani 1 1 d . . .
C15 C 0.7003(7) 0.6503(4) 0.6003(12) 0.019(2) Uani 1 1 d U . .
H15 H 0.7476 0.6787 0.6040 0.022 Uiso 1 1 calc R . .
O9 O 1.0079(7) 0.6901(4) 0.4448(7) 0.0209(19) Uani 1 1 d U . .
H9A H 0.9727 0.6627 0.4027 0.031 Uiso 1 1 d R . .
H9B H 0.9624 0.7220 0.4460 0.031 Uiso 1 1 d R . .
O10 O 1.0230(9) 0.6799(4) 0.7810(8) 0.033(2) Uani 1 1 d U . .
H10A H 0.9594 0.6706 0.7998 0.050 Uiso 1 1 d R . .
H10B H 1.0646 0.6625 0.8263 0.050 Uiso 1 1 d R . .
C9 C 0.8436(7) 0.5830(4) 0.5956(11) 0.017(3) Uani 1 1 d . . .
C12 C 0.5606(6) 0.5652(5) 0.5851(7) 0.012(3) Uani 1 1 d . . .
O2 O 1.1959(7) 0.6160(4) 0.7047(8) 0.027(2) Uani 1 1 d . . .
C8 C 1.3198(7) 0.5273(5) 0.7825(8) 0.015(2) Uani 1 1 d . . .
H8 H 1.3549 0.5555 0.7491 0.017 Uiso 1 1 calc R . .
C3 C 1.1634(6) 0.4892(4) 0.8451(8) 0.010(2) Uani 1 1 d . . .
H3 H 1.0940 0.4912 0.8485 0.012 Uiso 1 1 calc R . .
O6 O 0.8991(4) 0.6239(2) 0.6049(9) 0.0182(14) Uani 1 1 d U . .
C13 C 0.5295(7) 0.6208(4) 0.5992(10) 0.016(2) Uani 1 1 d U . .
H13 H 0.4620 0.6291 0.6071 0.019 Uiso 1 1 calc R . .
N1 N 1.4767(7) 0.4778(4) 0.8306(7) 0.0166(18) Uani 1 1 d . . .
N2 N 0.4831(7) 0.5240(3) 0.5811(6) 0.015(2) Uani 1 1 d . . .
C2 C 1.2162(8) 0.5276(5) 0.7843(9) 0.020(3) Uani 1 1 d . . .
C4 C 1.2131(8) 0.4485(5) 0.8999(10) 0.020(2) Uani 1 1 d . . .
C7 C 1.3710(8) 0.4835(4) 0.8321(8) 0.016(2) Uani 1 1 d . . .
C6 C 1.3177(8) 0.4438(5) 0.8865(9) 0.019(2) Uani 1 1 d . . .
H6 H 1.3513 0.4135 0.9148 0.023 Uiso 1 1 calc R . .
C1 C 1.1559(8) 0.5717(5) 0.7261(9) 0.017(2) Uani 1 1 d . . .
O0AA O 1.387(2) 0.7032(13) 0.792(3) 0.172(10) Uiso 1 1 d G . .
H0AA H 1.4393 0.7194 0.7708 0.258 Uiso 1 1 d G . .
H0AB H 1.3358 0.7170 0.7625 0.258 Uiso 1 1 d G . .


_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
O3 C5 1.283(15) . ?
O3 Tb1 2.453(9) 4_565 ?
O4 C5 1.281(15) . ?
O4 Tb1 2.461(9) 4_565 ?
C5 C4 1.445(16) . ?
C5 Tb1 2.834(11) 4_565 ?
O5 C9 1.243(12) . ?
O5 Zn1 1.950(7) . ?
O8 C16 1.267(11) . ?
O8 Tb1 2.324(6) 8_464 ?
O7 C16 1.250(11) . ?
O7 Tb1 2.668(6) 8_464 ?
C16 C14 1.524(12) . ?
C16 Tb1 2.844(9) 8_464 ?
C14 C15 1.357(13) . ?
C14 C13 1.405(13) . ?
Tb1 O6 2.259(6) . ?
Tb1 O8 2.324(6) 8_564 ?
Tb1 O10 2.343(11) . ?
Tb1 O9 2.411(9) . ?
Tb1 O2 2.423(9) . ?
Tb1 O3 2.453(9) 4_564 ?
Tb1 O4 2.461(9) 4_564 ?
Tb1 O1 2.591(9) . ?
Tb1 O7 2.668(6) 8_564 ?
Tb1 C5 2.834(11) 4_564 ?
Tb1 C16 2.844(9) 8_564 ?
Tb1 C1 2.850(11) . ?
Zn1 O5 1.950(7) 2_765 ?
Zn1 O1 2.136(9) 2_765 ?
Zn1 O1 2.136(9) . ?
O1 C1 1.255(13) . ?
C11 C10 1.378(14) . ?
C11 C12 1.402(13) . ?
C10 C15 1.403(12) . ?
C10 C9 1.517(13) . ?
C9 O6 1.234(11) . ?
C12 C13 1.404(14) . ?
C12 N2 1.430(13) . ?
O2 C1 1.220(14) . ?
C8 C2 1.385(15) . ?
C8 C7 1.410(14) . ?
C3 C4 1.380(16) . ?
C3 C2 1.406(16) . ?
N1 N1 1.230(18) 2_865 ?
N1 C7 1.419(13) . ?
N2 N2 1.235(17) 2_665 ?
C2 C1 1.530(16) . ?
C4 C6 1.413(15) . ?
C7 C6 1.386(16) . ?

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
C5 O3 Tb1 93.4(7) . 4_565 ?
C5 O4 Tb1 93.0(7) . 4_565 ?
O4 C5 O3 119.7(10) . . ?
O4 C5 C4 120.4(10) . . ?
O3 C5 C4 119.9(10) . . ?
O4 C5 Tb1 60.1(6) . 4_565 ?
O3 C5 Tb1 59.8(6) . 4_565 ?
C4 C5 Tb1 173.8(9) . 4_565 ?
C9 O5 Zn1 128.2(7) . . ?
C16 O8 Tb1 100.6(5) . 8_464 ?
C16 O7 Tb1 84.9(5) . 8_464 ?
O7 C16 O8 122.5(8) . . ?
O7 C16 C14 121.3(7) . . ?
O8 C16 C14 116.1(7) . . ?
O7 C16 Tb1 69.2(5) . 8_464 ?
O8 C16 Tb1 53.5(4) . 8_464 ?
C14 C16 Tb1 168.7(8) . 8_464 ?
C15 C14 C13 119.8(8) . . ?
C15 C14 C16 117.8(8) . . ?
C13 C14 C16 122.3(8) . . ?
O6 Tb1 O8 140.3(2) . 8_564 ?
O6 Tb1 O10 86.0(4) . . ?
O8 Tb1 O10 84.4(5) 8_564 . ?
O6 Tb1 O9 80.0(4) . . ?
O8 Tb1 O9 80.9(4) 8_564 . ?
O10 Tb1 O9 136.3(3) . . ?
O6 Tb1 O2 126.5(3) . . ?
O8 Tb1 O2 88.1(3) 8_564 . ?
O10 Tb1 O2 76.3(4) . . ?
O9 Tb1 O2 143.2(3) . . ?
O6 Tb1 O3 76.9(3) . 4_564 ?
O8 Tb1 O3 130.0(4) 8_564 4_564 ?
O10 Tb1 O3 141.2(3) . 4_564 ?
O9 Tb1 O3 74.7(3) . 4_564 ?
O2 Tb1 O3 86.4(3) . 4_564 ?
O6 Tb1 O4 128.0(3) . 4_564 ?
O8 Tb1 O4 77.9(3) 8_564 4_564 ?
O10 Tb1 O4 142.3(4) . 4_564 ?
O9 Tb1 O4 73.3(3) . 4_564 ?
O2 Tb1 O4 70.1(3) . 4_564 ?
O3 Tb1 O4 53.6(3) 4_564 4_564 ?
O6 Tb1 O1 75.8(3) . . ?
O8 Tb1 O1 137.7(4) 8_564 . ?
O10 Tb1 O1 76.0(3) . . ?
O9 Tb1 O1 137.6(3) . . ?
O2 Tb1 O1 51.2(3) . . ?
O3 Tb1 O1 66.2(3) 4_564 . ?
O4 Tb1 O1 95.3(3) 4_564 . ?
O6 Tb1 O7 88.6(2) . 8_564 ?
O8 Tb1 O7 51.9(2) 8_564 8_564 ?
O10 Tb1 O7 70.8(4) . 8_564 ?
O9 Tb1 O7 67.8(3) . 8_564 ?
O2 Tb1 O7 129.4(3) . 8_564 ?
O3 Tb1 O7 141.6(3) 4_564 8_564 ?
O4 Tb1 O7 119.3(3) 4_564 8_564 ?
O1 Tb1 O7 144.2(3) . 8_564 ?
O6 Tb1 C5 103.0(3) . 4_564 ?
O8 Tb1 C5 104.3(4) 8_564 4_564 ?
O10 Tb1 C5 150.4(3) . 4_564 ?
O9 Tb1 C5 73.3(3) . 4_564 ?
O2 Tb1 C5 75.7(3) . 4_564 ?
O3 Tb1 C5 26.9(3) 4_564 4_564 ?
O4 Tb1 C5 26.8(3) 4_564 4_564 ?
O1 Tb1 C5 78.9(3) . 4_564 ?
O7 Tb1 C5 136.6(3) 8_564 4_564 ?
O6 Tb1 C16 114.4(2) . 8_564 ?
O8 Tb1 C16 26.0(2) 8_564 8_564 ?
O10 Tb1 C16 77.0(5) . 8_564 ?
O9 Tb1 C16 71.9(5) . 8_564 ?
O2 Tb1 C16 110.0(3) . 8_564 ?
O3 Tb1 C16 141.7(5) 4_564 8_564 ?
O4 Tb1 C16 98.5(4) 4_564 8_564 ?
O1 Tb1 C16 150.3(5) . 8_564 ?
O7 Tb1 C16 26.0(2) 8_564 8_564 ?
C5 Tb1 C16 122.2(4) 4_564 8_564 ?
O6 Tb1 C1 101.8(3) . . ?
O8 Tb1 C1 112.9(3) 8_564 . ?
O10 Tb1 C1 76.0(3) . . ?
O9 Tb1 C1 147.3(3) . . ?
O2 Tb1 C1 25.1(3) . . ?
O3 Tb1 C1 74.0(3) 4_564 . ?
O4 Tb1 C1 80.7(3) 4_564 . ?
O1 Tb1 C1 26.1(3) . . ?
O7 Tb1 C1 144.3(4) 8_564 . ?
C5 Tb1 C1 74.6(4) 4_564 . ?
C16 Tb1 C1 132.5(4) 8_564 . ?
O5 Zn1 O5 160.4(5) 2_765 . ?
O5 Zn1 O1 100.7(3) 2_765 2_765 ?
O5 Zn1 O1 90.9(3) . 2_765 ?
O5 Zn1 O1 90.9(3) 2_765 . ?
O5 Zn1 O1 100.7(3) . . ?
O1 Zn1 O1 107.1(5) 2_765 . ?
C1 O1 Zn1 130.4(8) . . ?
C1 O1 Tb1 88.5(7) . . ?
Zn1 O1 Tb1 107.5(4) . . ?
C10 C11 C12 119.3(9) . . ?
C11 C10 C15 120.0(9) . . ?
C11 C10 C9 122.0(9) . . ?
C15 C10 C9 118.0(8) . . ?
C14 C15 C10 121.1(9) . . ?
O6 C9 O5 127.0(8) . . ?
O6 C9 C10 116.7(8) . . ?
O5 C9 C10 116.3(8) . . ?
C11 C12 C13 120.1(9) . . ?
C11 C12 N2 123.5(10) . . ?
C13 C12 N2 116.3(8) . . ?
C1 O2 Tb1 97.4(7) . . ?
C2 C8 C7 118.8(10) . . ?
C4 C3 C2 120.9(9) . . ?
C9 O6 Tb1 147.2(6) . . ?
C12 C13 C14 119.2(8) . . ?
N1 N1 C7 114.9(11) 2_865 . ?
N2 N2 C12 112.2(11) 2_665 . ?
C8 C2 C3 120.6(11) . . ?
C8 C2 C1 121.4(10) . . ?
C3 C2 C1 117.9(9) . . ?
C3 C4 C6 117.9(10) . . ?
C3 C4 C5 120.0(10) . . ?
C6 C4 C5 122.0(11) . . ?
C6 C7 C8 119.8(10) . . ?
C6 C7 N1 117.0(9) . . ?
C8 C7 N1 123.3(9) . . ?
C7 C6 C4 121.2(10) . . ?
O2 C1 O1 122.6(11) . . ?
O2 C1 C2 118.8(10) . . ?
O1 C1 C2 118.6(10) . . ?
O2 C1 Tb1 57.5(6) . . ?
O1 C1 Tb1 65.3(6) . . ?
C2 C1 Tb1 175.6(7) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.533
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.235
