# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_w
_database_code_depnum_ccdc_archive 'CCDC 1011116'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H20 N6 O13 Tb2'
_chemical_formula_weight         1038.42

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

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   6.7445(4)
_cell_length_b                   36.3810(19)
_cell_length_c                   13.0378(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3199.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1999
_exptl_absorpt_coefficient_mu    4.469
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  ?
_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            16883
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.12
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2858
_reflns_number_gt                2403
_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)+(0.0495P)²+43.4946P] 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         2858
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1460
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.393
_refine_ls_restrained_S_all      1.393
_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 -0.11523(7) 0.982209(12) 0.62763(3) 0.0129(2) Uani 1 1 d . . .
O2 O -0.1847(11) 0.9881(2) 0.4498(5) 0.0195(16) Uani 1 1 d . . .
O4 O 0.0640(12) 0.93652(19) 0.5414(6) 0.0246(18) Uani 1 1 d . . .
O5 O -0.0800(11) 0.93649(18) 0.7467(5) 0.0190(16) Uani 1 1 d . . .
O6 O -0.4186(10) 0.95500(19) 0.6147(5) 0.0183(15) Uani 1 1 d . . .
O7 O -0.1927(11) 1.04423(18) 0.6073(6) 0.0203(16) Uani 1 1 d . . .
O10 O -0.2111(11) 0.99697(19) 0.2855(5) 0.0184(16) Uani 1 1 d . . .
N1 N 0.2084(16) 0.7690(2) 1.0290(7) 0.029(2) Uani 1 1 d . . .
N2 N 0.068(2) 0.7500 0.8849(10) 0.023(3) Uani 1 2 d S . .
H2 H 0.0097 0.7500 0.8262 0.027 Uiso 1 2 calc SR . .
N3 N 0.2956(16) 0.7688(2) 0.2435(7) 0.025(2) Uani 1 1 d . . .
N4 N 0.233(2) 0.7500 0.3996(10) 0.020(3) Uani 1 2 d S . .
H1 H 0.2084 0.7500 0.4643 0.024 Uiso 1 2 calc SR . .
C1 C 0.0065(15) 0.9299(3) 0.8275(7) 0.013(2) Uani 1 1 d . . .
C2 C 0.0293(15) 0.8909(3) 0.8604(8) 0.015(2) Uani 1 1 d . . .
C3 C 0.1189(17) 0.8818(3) 0.9525(8) 0.022(2) Uani 1 1 d . . .
H3 H 0.1590 0.9004 0.9969 0.026 Uiso 1 1 calc R . .
C4 C 0.1494(16) 0.8453(3) 0.9791(8) 0.021(2) Uani 1 1 d . . .
H4 H 0.2102 0.8395 1.0410 0.026 Uiso 1 1 calc R . .
C5 C 0.0886(16) 0.8176(3) 0.9126(8) 0.020(2) Uani 1 1 d . . .
C6 C 0.1240(17) 0.7793(3) 0.9418(8) 0.023(2) Uani 1 1 d . . .
C7 C -0.0001(16) 0.8263(3) 0.8203(8) 0.021(2) Uani 1 1 d . . .
H7 H -0.0389 0.8078 0.7754 0.025 Uiso 1 1 calc R . .
C8 C -0.0305(17) 0.8626(3) 0.7952(8) 0.022(2) Uani 1 1 d . . .
H8 H -0.0922 0.8684 0.7335 0.026 Uiso 1 1 calc R . .
C9 C 0.1422(16) 0.9310(3) 0.4555(8) 0.021(2) Uani 1 1 d . . .
C10 C 0.1790(16) 0.8914(3) 0.4257(8) 0.018(2) Uani 1 1 d . . .
C11 C 0.1300(17) 0.8631(3) 0.4923(8) 0.023(2) Uani 1 1 d . . .
H11 H 0.0768 0.8687 0.5562 0.027 Uiso 1 1 calc R . .
C12 C 0.2380(15) 0.8177(3) 0.3705(8) 0.016(2) Uani 1 1 d . . .
C13 C 0.2885(18) 0.8463(3) 0.3043(9) 0.024(3) Uani 1 1 d . . .
H13 H 0.3423 0.8408 0.2404 0.029 Uiso 1 1 calc R . .
C14 C 0.2571(17) 0.7796(3) 0.3372(9) 0.020(2) Uani 1 1 d . . .
C15 C 0.1590(16) 0.8267(3) 0.4653(8) 0.021(2) Uani 1 1 d . . .
H15 H 0.1252 0.8081 0.5111 0.025 Uiso 1 1 calc R . .
C16 C 0.2603(17) 0.8828(3) 0.3317(8) 0.022(2) Uani 1 1 d . . .
H16 H 0.2962 0.9015 0.2866 0.026 Uiso 1 1 calc R . .
C19 C -0.2817(16) 0.9855(3) 0.3689(8) 0.021(2) Uani 1 1 d . . .
H19 H -0.4075 0.9751 0.3701 0.025 Uiso 1 1 calc R . .
O9 O 0.086(4) 0.7500 0.6451(17) 0.099(7) Uani 1 2 d S . .


_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 2.279(7) . ?
Tb1 O5 2.288(7) . ?
Tb1 O7 2.331(7) . ?
Tb1 O4 2.343(7) . ?
Tb1 O2 2.374(7) . ?
Tb1 O10 2.487(7) 2_475 ?
Tb1 O2 2.507(7) 5_576 ?
Tb1 O10 2.589(7) 5_576 ?
Tb1 C19 2.923(11) 5_576 ?
Tb1 Tb1 3.8947(9) 5_576 ?
O2 C19 1.245(12) . ?
O2 Tb1 2.507(7) 5_576 ?
O4 C9 1.254(13) . ?
O5 C1 1.228(12) . ?
O6 C1 1.288(12) 6_557 ?
O7 C9 1.264(13) 5_576 ?
O10 C19 1.257(12) . ?
O10 Tb1 2.487(7) 2_474 ?
O10 Tb1 2.589(7) 5_576 ?
N1 C6 1.325(15) . ?
N1 N1 1.383(18) 8_575 ?
N2 C6 1.352(14) . ?
N2 C6 1.352(14) 8_575 ?
N2 H2 0.8600 . ?
N3 C14 1.308(14) . ?
N3 N3 1.371(17) 8_575 ?
N4 C14 1.358(14) 8_575 ?
N4 C14 1.358(14) . ?
N4 H1 0.8600 . ?
C1 O6 1.288(12) 6_657 ?
C1 C2 1.490(13) . ?
C2 C3 1.384(14) . ?
C2 C8 1.395(14) . ?
C3 C4 1.387(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(15) . ?
C4 H4 0.9300 . ?
C5 C7 1.382(15) . ?
C5 C6 1.464(15) . ?
C7 C8 1.373(15) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 O7 1.264(13) 5_576 ?
C9 C10 1.514(14) . ?
C10 C16 1.379(16) . ?
C10 C11 1.385(15) . ?
C11 C15 1.386(15) . ?
C11 H11 0.9300 . ?
C12 C15 1.385(14) . ?
C12 C13 1.393(14) . ?
C12 C14 1.461(14) . ?
C13 C16 1.390(15) . ?
C13 H13 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C19 Tb1 2.923(11) 5_576 ?
C19 H19 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 O5 80.1(3) . . ?
O6 Tb1 O7 102.2(3) . . ?
O5 Tb1 O7 143.5(3) . . ?
O6 Tb1 O4 96.9(3) . . ?
O5 Tb1 O4 75.9(3) . . ?
O7 Tb1 O4 138.4(3) . . ?
O6 Tb1 O2 77.9(3) . . ?
O5 Tb1 O2 138.4(2) . . ?
O7 Tb1 O2 76.0(3) . . ?
O4 Tb1 O2 72.3(3) . . ?
O6 Tb1 O10 76.7(2) . 2_475 ?
O5 Tb1 O10 73.1(2) . 2_475 ?
O7 Tb1 O10 72.2(2) . 2_475 ?
O4 Tb1 O10 148.9(2) . 2_475 ?
O2 Tb1 O10 133.5(3) . 2_475 ?
O6 Tb1 O2 151.9(2) . 5_576 ?
O5 Tb1 O2 120.2(3) . 5_576 ?
O7 Tb1 O2 73.6(3) . 5_576 ?
O4 Tb1 O2 72.3(3) . 5_576 ?
O2 Tb1 O2 74.2(3) . 5_576 ?
O10 Tb1 O2 125.6(2) 2_475 5_576 ?
O6 Tb1 O10 157.3(2) . 5_576 ?
O5 Tb1 O10 80.1(2) . 5_576 ?
O7 Tb1 O10 87.5(2) . 5_576 ?
O4 Tb1 O10 88.8(3) . 5_576 ?
O2 Tb1 O10 124.6(2) . 5_576 ?
O10 Tb1 O10 87.09(13) 2_475 5_576 ?
O2 Tb1 O10 50.5(2) 5_576 5_576 ?
O6 Tb1 C19 176.0(3) . 5_576 ?
O5 Tb1 C19 100.7(3) . 5_576 ?
O7 Tb1 C19 79.5(3) . 5_576 ?
O4 Tb1 C19 79.6(3) . 5_576 ?
O2 Tb1 C19 99.2(3) . 5_576 ?
O10 Tb1 C19 107.2(3) 2_475 5_576 ?
O2 Tb1 C19 25.0(3) 5_576 5_576 ?
O10 Tb1 C19 25.4(2) 5_576 5_576 ?
O6 Tb1 Tb1 116.08(18) . 5_576 ?
O5 Tb1 Tb1 141.26(19) . 5_576 ?
O7 Tb1 Tb1 70.77(19) . 5_576 ?
O4 Tb1 Tb1 67.64(18) . 5_576 ?
O2 Tb1 Tb1 38.25(18) . 5_576 ?
O10 Tb1 Tb1 142.57(16) 2_475 5_576 ?
O2 Tb1 Tb1 35.91(16) 5_576 5_576 ?
O10 Tb1 Tb1 86.39(15) 5_576 5_576 ?
C19 Tb1 Tb1 60.9(2) 5_576 5_576 ?
C19 O2 Tb1 157.6(7) . . ?
C19 O2 Tb1 96.5(6) . 5_576 ?
Tb1 O2 Tb1 105.8(3) . 5_576 ?
C9 O4 Tb1 139.4(7) . . ?
C1 O5 Tb1 140.7(7) . . ?
C1 O6 Tb1 128.1(6) 6_557 . ?
C9 O7 Tb1 134.7(7) 5_576 . ?
C19 O10 Tb1 129.7(7) . 2_474 ?
C19 O10 Tb1 92.3(6) . 5_576 ?
Tb1 O10 Tb1 132.3(3) 2_474 5_576 ?
C6 N1 N1 106.4(6) . 8_575 ?
C6 N2 C6 103.9(13) . 8_575 ?
C6 N2 H2 128.1 . . ?
C6 N2 H2 128.1 8_575 . ?
C14 N3 N3 107.3(6) . 8_575 ?
C14 N4 C14 104.7(13) 8_575 . ?
C14 N4 H1 127.6 8_575 . ?
C14 N4 H1 127.6 . . ?
O5 C1 O6 123.3(9) . 6_657 ?
O5 C1 C2 118.9(9) . . ?
O6 C1 C2 117.8(9) 6_657 . ?
C3 C2 C8 118.6(9) . . ?
C3 C2 C1 121.5(9) . . ?
C8 C2 C1 119.8(9) . . ?
C2 C3 C4 120.7(10) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 119.6(10) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C7 C5 C4 120.1(10) . . ?
C7 C5 C6 121.1(10) . . ?
C4 C5 C6 118.7(10) . . ?
N1 C6 N2 111.7(10) . . ?
N1 C6 C5 124.1(10) . . ?
N2 C6 C5 124.1(10) . . ?
C8 C7 C5 119.6(10) . . ?
C8 C7 H7 120.2 . . ?
C5 C7 H7 120.2 . . ?
C7 C8 C2 121.4(10) . . ?
C7 C8 H8 119.3 . . ?
C2 C8 H8 119.3 . . ?
O4 C9 O7 125.3(10) . 5_576 ?
O4 C9 C10 116.7(9) . . ?
O7 C9 C10 117.9(9) 5_576 . ?
C16 C10 C11 119.0(9) . . ?
C16 C10 C9 120.5(9) . . ?
C11 C10 C9 120.5(10) . . ?
C10 C11 C15 121.2(10) . . ?
C10 C11 H11 119.4 . . ?
C15 C11 H11 119.4 . . ?
C15 C12 C13 118.2(9) . . ?
C15 C12 C14 121.5(10) . . ?
C13 C12 C14 120.2(10) . . ?
C16 C13 C12 121.3(10) . . ?
C16 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
N3 C14 N4 110.3(9) . . ?
N3 C14 C12 125.3(10) . . ?
N4 C14 C12 124.4(10) . . ?
C12 C15 C11 120.3(10) . . ?
C12 C15 H15 119.8 . . ?
C11 C15 H15 119.8 . . ?
C10 C16 C13 119.9(10) . . ?
C10 C16 H16 120.0 . . ?
C13 C16 H16 120.0 . . ?
O2 C19 O10 120.6(10) . . ?
O2 C19 Tb1 58.4(5) . 5_576 ?
O10 C19 Tb1 62.2(5) . 5_576 ?
O2 C19 H19 119.7 . . ?
O10 C19 H19 119.7 . . ?
Tb1 C19 H19 178.1 5_576 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.381
_refine_diff_density_min         -2.863
_refine_diff_density_rms         0.286
####################################################################### 
# 
# 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_y
_database_code_depnum_ccdc_archive 'CCDC 1428248'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H20 Gd2 N6 O13'
_chemical_formula_weight         1035.06

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

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   6.7503(4)
_cell_length_b                   36.407(3)
_cell_length_c                   13.0761(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3213.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1991
_exptl_absorpt_coefficient_mu    4.175
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  ?
_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            17349
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.32
_reflns_number_total             2956
_reflns_number_gt                2214
_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)+(0.0280P)²+17.2711P] 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         2956
_refine_ls_number_parameters     254
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.0959
_refine_ls_wR_factor_gt          0.0903
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8562(12) 1.0693(2) 0.0447(6) 0.0203(17) Uani 1 1 d . . .
C2 C 0.8209(11) 1.1085(2) 0.0739(6) 0.0199(18) Uani 1 1 d . . .
C3 C 0.8711(12) 1.1369(2) 0.0087(6) 0.0234(18) Uani 1 1 d . . .
H5 H 0.9243 1.1314 -0.0550 0.028 Uiso 1 1 calc R . .
C4 C 0.8447(12) 1.1732(2) 0.0355(6) 0.0231(19) Uani 1 1 d . . .
H6 H 0.8795 1.1917 -0.0103 0.028 Uiso 1 1 calc R . .
C5 C 0.7662(11) 1.1824(2) 0.1305(6) 0.0183(17) Uani 1 1 d . . .
C6 C 0.7457(12) 1.2205(2) 0.1614(6) 0.0209(18) Uani 1 1 d . . .
C7 C 0.7119(13) 1.1537(2) 0.1967(6) 0.026(2) Uani 1 1 d . . .
H9 H 0.6573 1.1592 0.2602 0.031 Uiso 1 1 calc R . .
C8 C 0.7387(12) 1.1173(2) 0.1688(6) 0.0237(19) Uani 1 1 d . . .
H10 H 0.7016 1.0987 0.2134 0.028 Uiso 1 1 calc R . .
C9 C 0.5047(10) 0.9292(2) 0.1716(6) 0.0163(17) Uani 1 1 d . . .
C10 C 0.5298(11) 0.8910(2) 0.1389(6) 0.0185(17) Uani 1 1 d . . .
C11 C 0.6170(12) 0.8816(2) 0.0466(6) 0.0232(18) Uani 1 1 d . . .
H13 H 0.6548 0.9001 0.0015 0.028 Uiso 1 1 calc R . .
C12 C 0.6485(12) 0.8456(2) 0.0204(6) 0.0243(19) Uani 1 1 d . . .
H14 H 0.7100 0.8399 -0.0412 0.029 Uiso 1 1 calc R . .
C13 C 0.5879(12) 0.8173(2) 0.0866(6) 0.0224(18) Uani 1 1 d . . .
C14 C 0.4982(12) 0.8263(2) 0.1789(6) 0.0241(19) Uani 1 1 d . . .
H16 H 0.4594 0.8078 0.2236 0.029 Uiso 1 1 calc R . .
C15 C 0.6214(13) 0.7792(2) 0.0574(6) 0.0258(18) Uani 1 1 d . . .
C16 C 0.4667(12) 0.8626(2) 0.2042(6) 0.0225(18) Uani 1 1 d . . .
H18 H 0.4031 0.8683 0.2652 0.027 Uiso 1 1 calc R . .
C17 C 0.7190(11) 0.9854(2) -0.1312(6) 0.0209(17) Uani 1 1 d . . .
H17 H 0.5933 0.9749 -0.1307 0.025 Uiso 1 1 calc R . .
Gd1 Gd 0.88368(5) 0.982019(9) 0.12746(2) 0.01401(13) Uani 1 1 d . . .
N1 N 0.5667(14) 0.7500 0.1136(7) 0.027(2) Uani 1 2 d S . .
H1 H 0.5096 0.7500 0.1724 0.033 Uiso 1 2 calc SR . .
N2 N 0.7068(11) 0.76886(19) -0.0290(5) 0.0300(18) Uani 1 1 d . . .
N4 N 0.7702(14) 1.2500 0.1001(7) 0.022(2) Uani 1 2 d S . .
H4 H 0.7959 1.2500 0.0357 0.026 Uiso 1 2 calc SR . .
N5 N 0.7091(11) 1.23126(18) 0.2563(5) 0.0270(17) Uani 1 1 d . . .
O1 O 0.5796(7) 0.95482(13) 0.1152(4) 0.0193(12) Uani 1 1 d . . .
O2 O 0.8073(8) 1.04441(14) 0.1072(4) 0.0250(13) Uani 1 1 d . . .
O3 O 0.582(2) 0.7500 0.3558(10) 0.088(4) Uani 1 2 d S . .
O4 O 1.0645(8) 0.93645(15) 0.0412(4) 0.0272(14) Uani 1 1 d . . .
O5 O 0.8136(8) 0.98769(15) -0.0504(4) 0.0231(13) Uani 1 1 d . . .
O6 O 0.7089(8) 1.00299(14) 0.2856(4) 0.0186(12) Uani 1 1 d . . .
O7 O 0.4188(8) 0.93607(15) 0.2535(4) 0.0209(13) 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
C1 O4 1.261(9) 5_775 ?
C1 O2 1.266(9) . ?
C1 C2 1.497(11) . ?
C2 C3 1.382(11) . ?
C2 C8 1.396(11) . ?
C3 C4 1.377(11) . ?
C3 H5 0.9300 . ?
C4 C5 1.392(11) . ?
C4 H6 0.9300 . ?
C5 C7 1.405(11) . ?
C5 C6 1.452(11) . ?
C6 N5 1.324(10) . ?
C6 N4 1.350(10) . ?
C7 C8 1.386(11) . ?
C7 H9 0.9300 . ?
C8 H10 0.9300 . ?
C9 O7 1.243(9) . ?
C9 O1 1.293(9) . ?
C9 C10 1.465(10) . ?
C10 C11 1.386(10) . ?
C10 C16 1.408(11) . ?
C11 C12 1.369(11) . ?
C11 H13 0.9300 . ?
C12 C13 1.407(11) . ?
C12 H14 0.9300 . ?
C13 C14 1.389(11) . ?
C13 C15 1.458(11) . ?
C14 C16 1.378(11) . ?
C14 H16 0.9300 . ?
C15 N2 1.323(10) . ?
C15 N1 1.344(10) . ?
C16 H18 0.9300 . ?
C17 O5 1.237(8) . ?
C17 O6 1.266(9) 2_674 ?
C17 Gd1 2.933(8) 5_775 ?
C17 H17 0.9300 . ?
Gd1 O1 2.285(5) . ?
Gd1 O7 2.298(5) 6_656 ?
Gd1 O2 2.344(5) . ?
Gd1 O4 2.348(5) . ?
Gd1 O5 2.382(5) . ?
Gd1 O6 2.500(5) . ?
Gd1 O5 2.531(5) 5_775 ?
Gd1 O6 2.587(5) 6_656 ?
Gd1 C17 2.933(8) 5_775 ?
Gd1 Gd1 3.9104(7) 5_775 ?
N1 C15 1.344(10) 8_575 ?
N1 H1 0.8600 . ?
N2 N2 1.373(14) 8_575 ?
N4 C6 1.350(10) 8_585 ?
N4 H4 0.8600 . ?
N5 N5 1.365(13) 8_585 ?
O4 C1 1.261(9) 5_775 ?
O5 Gd1 2.531(5) 5_775 ?
O6 C17 1.266(9) 2_675 ?
O6 Gd1 2.587(5) 6_556 ?
O7 Gd1 2.298(5) 6_556 ?

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
O4 C1 O2 124.4(7) 5_775 . ?
O4 C1 C2 117.0(7) 5_775 . ?
O2 C1 C2 118.5(7) . . ?
C3 C2 C8 118.3(7) . . ?
C3 C2 C1 121.1(7) . . ?
C8 C2 C1 120.6(7) . . ?
C4 C3 C2 121.9(7) . . ?
C4 C3 H5 119.0 . . ?
C2 C3 H5 119.0 . . ?
C3 C4 C5 120.4(7) . . ?
C3 C4 H6 119.8 . . ?
C5 C4 H6 119.8 . . ?
C4 C5 C7 118.1(7) . . ?
C4 C5 C6 121.0(7) . . ?
C7 C5 C6 120.9(7) . . ?
N5 C6 N4 110.2(7) . . ?
N5 C6 C5 124.1(7) . . ?
N4 C6 C5 125.7(8) . . ?
C8 C7 C5 120.9(7) . . ?
C8 C7 H9 119.5 . . ?
C5 C7 H9 119.5 . . ?
C7 C8 C2 120.3(8) . . ?
C7 C8 H10 119.8 . . ?
C2 C8 H10 119.8 . . ?
O7 C9 O1 121.9(7) . . ?
O7 C9 C10 119.8(7) . . ?
O1 C9 C10 118.3(6) . . ?
C11 C10 C16 118.4(7) . . ?
C11 C10 C9 122.5(7) . . ?
C16 C10 C9 119.0(7) . . ?
C12 C11 C10 121.3(7) . . ?
C12 C11 H13 119.3 . . ?
C10 C11 H13 119.3 . . ?
C11 C12 C13 120.0(7) . . ?
C11 C12 H14 120.0 . . ?
C13 C12 H14 120.0 . . ?
C14 C13 C12 119.3(7) . . ?
C14 C13 C15 121.3(7) . . ?
C12 C13 C15 119.4(7) . . ?
C16 C14 C13 120.1(8) . . ?
C16 C14 H16 120.0 . . ?
C13 C14 H16 120.0 . . ?
N2 C15 N1 111.2(8) . . ?
N2 C15 C13 124.2(8) . . ?
N1 C15 C13 124.6(7) . . ?
C14 C16 C10 120.8(7) . . ?
C14 C16 H18 119.6 . . ?
C10 C16 H18 119.6 . . ?
O5 C17 O6 120.9(7) . 2_674 ?
O5 C17 Gd1 59.1(4) . 5_775 ?
O6 C17 Gd1 61.8(4) 2_674 5_775 ?
O5 C17 H17 119.6 . . ?
O6 C17 H17 119.6 2_674 . ?
Gd1 C17 H17 178.7 5_775 . ?
O1 Gd1 O7 79.92(18) . 6_656 ?
O1 Gd1 O2 102.38(18) . . ?
O7 Gd1 O2 143.60(19) 6_656 . ?
O1 Gd1 O4 97.29(19) . . ?
O7 Gd1 O4 75.96(19) 6_656 . ?
O2 Gd1 O4 138.11(19) . . ?
O1 Gd1 O5 77.91(18) . . ?
O7 Gd1 O5 138.17(18) 6_656 . ?
O2 Gd1 O5 76.22(19) . . ?
O4 Gd1 O5 72.28(19) . . ?
O1 Gd1 O6 76.49(18) . . ?
O7 Gd1 O6 73.18(18) 6_656 . ?
O2 Gd1 O6 72.18(18) . . ?
O4 Gd1 O6 149.12(18) . . ?
O5 Gd1 O6 133.41(19) . . ?
O1 Gd1 O5 152.38(17) . 5_775 ?
O7 Gd1 O5 120.25(18) 6_656 5_775 ?
O2 Gd1 O5 73.16(18) . 5_775 ?
O4 Gd1 O5 72.36(19) . 5_775 ?
O5 Gd1 O5 74.56(19) . 5_775 ?
O6 Gd1 O5 125.26(17) . 5_775 ?
O1 Gd1 O6 157.08(17) . 6_656 ?
O7 Gd1 O6 80.18(17) 6_656 6_656 ?
O2 Gd1 O6 87.16(18) . 6_656 ?
O4 Gd1 O6 88.77(19) . 6_656 ?
O5 Gd1 O6 124.89(18) . 6_656 ?
O6 Gd1 O6 86.96(9) . 6_656 ?
O5 Gd1 O6 50.33(16) 5_775 6_656 ?
O1 Gd1 C17 176.4(2) . 5_775 ?
O7 Gd1 C17 100.91(19) 6_656 5_775 ?
O2 Gd1 C17 79.1(2) . 5_775 ?
O4 Gd1 C17 79.6(2) . 5_775 ?
O5 Gd1 C17 99.4(2) . 5_775 ?
O6 Gd1 C17 107.12(19) . 5_775 ?
O5 Gd1 C17 24.80(17) 5_775 5_775 ?
O6 Gd1 C17 25.54(17) 6_656 5_775 ?
O1 Gd1 Gd1 116.48(13) . 5_775 ?
O7 Gd1 Gd1 141.26(13) 6_656 5_775 ?
O2 Gd1 Gd1 70.57(13) . 5_775 ?
O4 Gd1 Gd1 67.57(13) . 5_775 ?
O5 Gd1 Gd1 38.60(13) . 5_775 ?
O6 Gd1 Gd1 142.40(12) . 5_775 ?
O5 Gd1 Gd1 35.95(11) 5_775 5_775 ?
O6 Gd1 Gd1 86.28(11) 6_656 5_775 ?
C17 Gd1 Gd1 60.75(14) 5_775 5_775 ?
C15 N1 C15 104.5(10) 8_575 . ?
C15 N1 H1 127.7 8_575 . ?
C15 N1 H1 127.7 . . ?
C15 N2 N2 106.5(5) . 8_575 ?
C6 N4 C6 105.3(10) . 8_585 ?
C6 N4 H4 127.3 . . ?
C6 N4 H4 127.3 8_585 . ?
C6 N5 N5 107.2(5) . 8_585 ?
C9 O1 Gd1 128.6(5) . . ?
C1 O2 Gd1 135.3(5) . . ?
C1 O4 Gd1 140.0(5) 5_775 . ?
C17 O5 Gd1 158.4(5) . . ?
C17 O5 Gd1 96.1(5) . 5_775 ?
Gd1 O5 Gd1 105.44(19) . 5_775 ?
C17 O6 Gd1 129.2(5) 2_675 . ?
C17 O6 Gd1 92.7(4) 2_675 6_556 ?
Gd1 O6 Gd1 132.4(2) . 6_556 ?
C9 O7 Gd1 141.1(5) . 6_556 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.32
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.170
