# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_hkf1005_0m
_database_code_depnum_ccdc_archive 'CCDC 1009151'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 Dy N5 O8'
_chemical_formula_sum            'C20 H24 Dy N5 O8'
_chemical_formula_weight         624.94

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   17.5564(10)
_cell_length_b                   10.6174(6)
_cell_length_c                   25.2308(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4703.1(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      29.5

_exptl_crystal_description       chunk
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2472
_exptl_absorpt_coefficient_mu    3.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6024
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37616
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         29.58
_reflns_number_total             6584
_reflns_number_gt                5345
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0303P)²+5.9006P] 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         6584
_refine_ls_number_parameters     311
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0665
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
Dy1 Dy 0.097676(6) 0.741151(10) 0.362255(5) 0.01731(4) Uani 1 1 d . . .
O7 O 0.04996(11) 0.96194(18) 0.36543(8) 0.0265(4) Uani 1 1 d . . .
O2 O 0.13001(10) 0.57954(16) 0.30171(7) 0.0215(4) Uani 1 1 d . . .
N1 N 0.21752(13) 0.61797(19) 0.38538(8) 0.0191(4) Uani 1 1 d . . .
O3 O 0.17830(10) 0.84997(16) 0.31131(7) 0.0211(4) Uani 1 1 d . . .
C6 C 0.26214(15) 0.7200(2) 0.46572(10) 0.0206(5) Uani 1 1 d . . .
N3 N -0.06525(13) 0.7189(2) 0.22395(9) 0.0226(4) Uani 1 1 d . . .
C13 C 0.19739(15) 0.7840(2) 0.22218(10) 0.0224(5) Uani 1 1 d . . .
H13 H 0.1547 0.7322 0.2240 0.027 Uiso 1 1 calc R . .
O5 O 0.03804(13) 0.56422(19) 0.39917(9) 0.0368(5) Uani 1 1 d U . .
C1 C 0.20080(15) 0.8067(2) 0.47060(10) 0.0209(5) Uani 1 1 d . . .
O1 O 0.14591(11) 0.81312(19) 0.43580(8) 0.0277(4) Uani 1 1 d . . .
C9 C 0.21623(14) 0.4336(2) 0.26216(10) 0.0186(5) Uani 1 1 d . . .
N2 N 0.23596(12) 0.5275(2) 0.34757(9) 0.0204(4) Uani 1 1 d . . .
O6 O -0.01780(11) 0.82398(18) 0.40730(8) 0.0291(4) Uani 1 1 d . . .
C8 C 0.19058(14) 0.5175(2) 0.30479(10) 0.0188(5) Uani 1 1 d . . .
C14 C 0.21845(14) 0.8554(2) 0.26694(10) 0.0188(5) Uani 1 1 d . . .
C2 C 0.20046(16) 0.8874(2) 0.51510(10) 0.0242(5) Uani 1 1 d . . .
H2 H 0.1598 0.9422 0.5199 0.029 Uiso 1 1 calc R . .
C15 C 0.03631(17) 0.4780(3) 0.43193(12) 0.0294(6) Uani 1 1 d U . .
H15 H 0.0768 0.4718 0.4556 0.035 Uiso 1 1 calc R . .
C3 C 0.25879(17) 0.8868(3) 0.55150(11) 0.0259(6) Uani 1 1 d . . .
H3 H 0.2575 0.9421 0.5801 0.031 Uiso 1 1 calc R . .
C19 C -0.0862(2) 0.7574(3) 0.17058(13) 0.0366(7) Uani 1 1 d . . .
H19A H -0.0630 0.8371 0.1627 0.055 Uiso 1 1 calc R . .
H19B H -0.1406 0.7650 0.1682 0.055 Uiso 1 1 calc R . .
H19C H -0.0688 0.6954 0.1457 0.055 Uiso 1 1 calc R . .
C7 C 0.26683(15) 0.6296(2) 0.42301(10) 0.0207(5) Uani 1 1 d . . .
H7 H 0.3086 0.5757 0.4226 0.025 Uiso 1 1 calc R . .
C12 C 0.23870(16) 0.7892(3) 0.17561(11) 0.0247(5) Uani 1 1 d . . .
H12 H 0.2234 0.7412 0.1467 0.030 Uiso 1 1 calc R . .
C20 C -0.10631(19) 0.6126(3) 0.24601(13) 0.0352(7) Uani 1 1 d . . .
H20A H -0.0844 0.5900 0.2795 0.053 Uiso 1 1 calc R . .
H20B H -0.1029 0.5424 0.2222 0.053 Uiso 1 1 calc R . .
H20C H -0.1588 0.6351 0.2509 0.053 Uiso 1 1 calc R . .
N4 N -0.01861(14) 0.3939(2) 0.43591(9) 0.0257(5) Uani 1 1 d . . .
N5 N -0.00824(14) 0.9374(2) 0.39383(10) 0.0278(5) Uani 1 1 d . . .
O4 O 0.00520(13) 0.7479(2) 0.29687(10) 0.0435(6) Uani 1 1 d . . .
C5 C 0.32047(16) 0.7210(3) 0.50362(11) 0.0241(5) Uani 1 1 d . . .
H5 H 0.3606 0.6645 0.5002 0.029 Uiso 1 1 calc R . .
C4 C 0.32003(17) 0.8037(3) 0.54592(11) 0.0266(6) Uani 1 1 d . . .
H4 H 0.3598 0.8040 0.5703 0.032 Uiso 1 1 calc R . .
C18 C -0.01399(17) 0.7777(3) 0.25148(13) 0.0318(6) Uani 1 1 d . . .
H18 H 0.0099 0.8467 0.2360 0.038 Uiso 1 1 calc R . .
O8 O -0.05282(13) 1.0210(2) 0.40646(11) 0.0463(6) Uani 1 1 d . . .
C17 C -0.0833(2) 0.3909(4) 0.40108(15) 0.0476(9) Uani 1 1 d . . .
H17A H -0.0837 0.4655 0.3796 0.071 Uiso 1 1 calc R . .
H17B H -0.1292 0.3872 0.4217 0.071 Uiso 1 1 calc R . .
H17C H -0.0802 0.3180 0.3787 0.071 Uiso 1 1 calc R . .
C16 C -0.0147(2) 0.2938(3) 0.47529(13) 0.0390(7) Uani 1 1 d . . .
H16A H -0.0098 0.2140 0.4577 0.058 Uiso 1 1 calc R . .
H16B H -0.0604 0.2942 0.4962 0.058 Uiso 1 1 calc R . .
H16C H 0.0285 0.3073 0.4979 0.058 Uiso 1 1 calc R . .
C10 C 0.17502(15) 0.4363(2) 0.21450(10) 0.0225(5) Uani 1 1 d . . .
H10 H 0.1320 0.4870 0.2120 0.027 Uiso 1 1 calc R . .
C11 C 0.30308(16) 0.8655(3) 0.17142(11) 0.0246(5) Uani 1 1 d . . .
H11 H 0.3308 0.8685 0.1400 0.030 Uiso 1 1 calc R . .
H2A H 0.2823 0.5566 0.3305 0.037 Uiso 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
Dy1 O1 2.1781(19) . ?
Dy1 O3 2.2340(18) . ?
Dy1 O4 2.316(2) . ?
Dy1 O5 2.344(2) . ?
Dy1 O2 2.3665(18) . ?
Dy1 O6 2.4850(19) . ?
Dy1 O7 2.4906(19) . ?
Dy1 N1 2.545(2) . ?
O7 N5 1.275(3) . ?
O2 C8 1.253(3) . ?
N1 C7 1.291(3) . ?
N1 N2 1.392(3) . ?
O3 C14 1.324(3) . ?
C6 C5 1.401(4) . ?
C6 C1 1.422(4) . ?
C6 C7 1.446(3) . ?
N3 C18 1.297(4) . ?
N3 C20 1.450(4) . ?
N3 C19 1.454(4) . ?
C13 C12 1.382(4) . ?
C13 C14 1.409(3) . ?
O5 C15 1.234(4) . ?
C1 O1 1.305(3) . ?
C1 C2 1.412(4) . ?
C9 C10 1.404(4) . ?
C9 C14 1.421(3) 8_655 ?
C9 C8 1.468(3) . ?
N2 C8 1.346(3) . ?
O6 N5 1.263(3) . ?
C14 C9 1.421(3) 8_665 ?
C2 C3 1.375(4) . ?
C15 N4 1.318(3) . ?
C3 C4 1.398(4) . ?
C12 C11 1.395(4) . ?
N4 C17 1.436(4) . ?
N4 C16 1.456(4) . ?
N5 O8 1.225(3) . ?
O4 C18 1.235(4) . ?
C5 C4 1.382(4) . ?
C10 C11 1.376(4) 8_655 ?
C11 C10 1.376(4) 8_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
O1 Dy1 O3 93.58(7) . . ?
O1 Dy1 O4 150.31(7) . . ?
O3 Dy1 O4 91.05(8) . . ?
O1 Dy1 O5 96.68(8) . . ?
O3 Dy1 O5 157.86(7) . . ?
O4 Dy1 O5 89.69(9) . . ?
O1 Dy1 O2 135.32(7) . . ?
O3 Dy1 O2 81.46(6) . . ?
O4 Dy1 O2 74.37(7) . . ?
O5 Dy1 O2 77.44(7) . . ?
O1 Dy1 O6 78.66(7) . . ?
O3 Dy1 O6 126.66(6) . . ?
O4 Dy1 O6 75.11(8) . . ?
O5 Dy1 O6 74.77(7) . . ?
O2 Dy1 O6 138.38(6) . . ?
O1 Dy1 O7 76.89(7) . . ?
O3 Dy1 O7 75.22(6) . . ?
O4 Dy1 O7 76.01(7) . . ?
O5 Dy1 O7 126.25(7) . . ?
O2 Dy1 O7 141.62(6) . . ?
O6 Dy1 O7 51.52(6) . . ?
O1 Dy1 N1 70.34(7) . . ?
O3 Dy1 N1 82.76(7) . . ?
O4 Dy1 N1 139.35(7) . . ?
O5 Dy1 N1 82.32(8) . . ?
O2 Dy1 N1 64.98(6) . . ?
O6 Dy1 N1 138.71(7) . . ?
O7 Dy1 N1 138.96(7) . . ?
N5 O7 Dy1 95.49(15) . . ?
C8 O2 Dy1 123.01(16) . . ?
C7 N1 N2 114.5(2) . . ?
C7 N1 Dy1 132.37(17) . . ?
N2 N1 Dy1 112.94(15) . . ?
C14 O3 Dy1 147.78(16) . . ?
C5 C6 C1 119.3(2) . . ?
C5 C6 C7 118.2(2) . . ?
C1 C6 C7 122.5(2) . . ?
C18 N3 C20 120.9(3) . . ?
C18 N3 C19 122.4(3) . . ?
C20 N3 C19 116.6(2) . . ?
C12 C13 C14 121.5(2) . . ?
C15 O5 Dy1 150.7(2) . . ?
O1 C1 C2 120.0(2) . . ?
O1 C1 C6 122.3(2) . . ?
C2 C1 C6 117.7(2) . . ?
C1 O1 Dy1 147.34(17) . . ?
C10 C9 C14 120.0(2) . 8_655 ?
C10 C9 C8 117.2(2) . . ?
C14 C9 C8 122.7(2) 8_655 . ?
C8 N2 N1 117.8(2) . . ?
N5 O6 Dy1 96.08(15) . . ?
O2 C8 N2 120.7(2) . . ?
O2 C8 C9 122.3(2) . . ?
N2 C8 C9 117.0(2) . . ?
O3 C14 C13 121.0(2) . . ?
O3 C14 C9 121.8(2) . 8_665 ?
C13 C14 C9 117.3(2) . 8_665 ?
C3 C2 C1 121.7(3) . . ?
O5 C15 N4 124.9(3) . . ?
C2 C3 C4 120.5(3) . . ?
N1 C7 C6 125.0(2) . . ?
C13 C12 C11 120.9(3) . . ?
C15 N4 C17 123.1(3) . . ?
C15 N4 C16 120.8(3) . . ?
C17 N4 C16 116.0(3) . . ?
O8 N5 O6 122.4(3) . . ?
O8 N5 O7 120.7(3) . . ?
O6 N5 O7 116.9(2) . . ?
C18 O4 Dy1 149.3(2) . . ?
C4 C5 C6 121.9(3) . . ?
C5 C4 C3 118.9(3) . . ?
O4 C18 N3 124.3(3) . . ?
C11 C10 C9 121.4(2) 8_655 . ?
C10 C11 C12 118.9(2) 8_665 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        29.58
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.803
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.101
####################################################################### 
# 
# 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_hkf1045_0m
_database_code_depnum_ccdc_archive 'CCDC 1009152'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 Er N5 O8'
_chemical_formula_sum            'C20 H24 Er N5 O8'
_chemical_formula_weight         629.70

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   17.4707(14)
_cell_length_b                   10.7118(9)
_cell_length_c                   25.398(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4753.1(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5809
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      21.3

_exptl_crystal_description       chunk
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2488
_exptl_absorpt_coefficient_mu    3.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18338
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         27.25
_reflns_number_total             2646
_reflns_number_gt                2231
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0187P)²+35.8708P] 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         2646
_refine_ls_number_parameters     293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0347
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.117
_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
Er1 Er 0.600267(18) 0.24054(3) 0.364564(14) 0.03294(15) Uani 1 1 d . . .
O7 O 0.5527(3) 0.4565(5) 0.3670(2) 0.0447(14) Uani 1 1 d . . .
N1 N 0.7185(3) 0.1193(5) 0.3873(2) 0.0319(15) Uani 1 1 d . . .
O2 O 0.6313(3) 0.0823(5) 0.3046(2) 0.0380(13) Uani 1 1 d . . .
N2 N 0.7361(3) 0.0272(6) 0.3502(2) 0.0336(16) Uani 1 1 d . . .
H2A H 0.7842 0.0440 0.3381 0.040 Uiso 1 1 d . . .
C6 C 0.7623(4) 0.2175(7) 0.4683(3) 0.0349(19) Uani 1 1 d . . .
C2 C 0.7010(5) 0.3831(7) 0.5165(3) 0.042(2) Uani 1 1 d . . .
H2 H 0.6605 0.4385 0.5208 0.050 Uiso 1 1 calc R . .
C12 C 0.7410(5) 0.2915(8) 0.1792(3) 0.043(2) Uani 1 1 d . . .
H12 H 0.7265 0.2432 0.1505 0.051 Uiso 1 1 calc R . .
C1 C 0.7023(5) 0.3053(7) 0.4721(3) 0.037(2) Uani 1 1 d . . .
O6 O 0.4852(3) 0.3220(6) 0.4094(2) 0.0559(16) Uani 1 1 d . . .
O1 O 0.6478(3) 0.3136(5) 0.4370(2) 0.0516(16) Uani 1 1 d . . .
C14 C 0.7197(4) 0.3546(7) 0.2696(3) 0.0330(19) Uani 1 1 d . . .
O5 O 0.5414(4) 0.0680(5) 0.4014(3) 0.070(2) Uani 1 1 d . . .
C9 C 0.7840(4) 0.4347(7) 0.2653(3) 0.0321(19) Uani 1 1 d . . .
C7 C 0.7675(4) 0.1280(7) 0.4250(3) 0.036(2) Uani 1 1 d . . .
H7 H 0.8090 0.0737 0.4247 0.043 Uiso 1 1 calc R . .
C13 C 0.6993(4) 0.2846(7) 0.2249(3) 0.039(2) Uani 1 1 d . . .
H13 H 0.6567 0.2326 0.2264 0.047 Uiso 1 1 calc R . .
N5 N 0.4952(4) 0.4333(7) 0.3958(3) 0.0492(19) Uani 1 1 d . . .
C3 C 0.7574(5) 0.3796(8) 0.5533(3) 0.045(2) Uani 1 1 d . . .
H3 H 0.7553 0.4337 0.5819 0.055 Uiso 1 1 calc R . .
C8 C 0.6905(5) 0.0196(7) 0.3077(3) 0.0327(19) Uani 1 1 d . . .
C11 C 0.8040(5) 0.3688(7) 0.1752(3) 0.043(2) Uani 1 1 d . . .
H11 H 0.8315 0.3733 0.1439 0.052 Uiso 1 1 calc R . .
O8 O 0.4518(4) 0.5166(7) 0.4090(3) 0.086(2) Uani 1 1 d . . .
O4 O 0.5046(4) 0.2407(7) 0.3023(3) 0.079(2) Uani 1 1 d . . .
C4 C 0.8181(5) 0.2964(7) 0.5489(3) 0.046(2) Uani 1 1 d . . .
H4 H 0.8569 0.2953 0.5739 0.055 Uiso 1 1 calc R . .
C10 C 0.8254(4) 0.4386(7) 0.2179(3) 0.041(2) Uani 1 1 d . . .
H10 H 0.8683 0.4898 0.2154 0.049 Uiso 1 1 calc R . .
C5 C 0.8195(5) 0.2158(7) 0.5068(3) 0.043(2) Uani 1 1 d . . .
H5 H 0.8594 0.1587 0.5039 0.051 Uiso 1 1 calc R . .
N3 N 0.4396(4) 0.2132(6) 0.2273(3) 0.0390(16) Uani 1 1 d . . .
N4 N 0.4802(5) -0.0989(7) 0.4339(3) 0.0722(19) Uani 1 1 d . . .
C20 C 0.3977(5) 0.1077(8) 0.2465(4) 0.064(3) Uani 1 1 d . . .
H20A H 0.4167 0.0847 0.2806 0.096 Uiso 1 1 calc R . .
H20B H 0.4038 0.0389 0.2227 0.096 Uiso 1 1 calc R . .
H20C H 0.3444 0.1288 0.2492 0.096 Uiso 1 1 calc R . .
C18 C 0.4882(4) 0.2696(8) 0.2573(4) 0.064(3) Uani 1 1 d . . .
H18 H 0.5131 0.3388 0.2432 0.077 Uiso 1 1 calc R . .
H15 H 0.5670 -0.0226 0.4466 0.077 Uiso 1 1 d R . .
C17 C 0.4106(4) -0.1088(8) 0.4077(4) 0.141(6) Uani 1 1 d R . .
H17A H 0.4022 -0.0353 0.3869 0.211 Uiso 1 1 calc R . .
H17B H 0.3701 -0.1174 0.4330 0.211 Uiso 1 1 calc R . .
H17C H 0.4114 -0.1808 0.3852 0.211 Uiso 1 1 calc R . .
O3 O 0.6787(3) 0.3485(4) 0.31382(19) 0.0347(13) Uani 1 1 d . . .
C19 C 0.4217(7) 0.2546(9) 0.1744(4) 0.079(3) Uani 1 1 d . . .
H19A H 0.4493 0.3301 0.1670 0.119 Uiso 1 1 calc R . .
H19B H 0.3678 0.2700 0.1716 0.119 Uiso 1 1 calc R . .
H19C H 0.4363 0.1913 0.1497 0.119 Uiso 1 1 calc R . .
C16 C 0.4917(6) -0.1947(9) 0.4702(4) 0.0722(19) Uani 1 1 d . . .
H16A H 0.5414 -0.1861 0.4858 0.108 Uiso 1 1 calc R . .
H16B H 0.4883 -0.2739 0.4526 0.108 Uiso 1 1 calc R . .
H16C H 0.4533 -0.1902 0.4971 0.108 Uiso 1 1 calc R . .
C15 C 0.5264 -0.0102 0.4234 0.076 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
Er1 O1 2.165(5) . ?
Er1 O3 2.208(5) . ?
Er1 O4 2.301(6) . ?
Er1 O5 2.313(5) . ?
Er1 O2 2.341(5) . ?
Er1 O7 2.459(5) . ?
Er1 O6 2.469(5) . ?
Er1 N1 2.508(6) . ?
O7 N5 1.268(8) . ?
N1 C7 1.288(9) . ?
N1 N2 1.399(8) . ?
O2 C8 1.237(9) . ?
N2 C8 1.342(9) . ?
C6 C5 1.398(10) . ?
C6 C1 1.412(10) . ?
C6 C7 1.462(10) . ?
C2 C3 1.361(11) . ?
C2 C1 1.401(10) . ?
C12 C13 1.372(10) . ?
C12 C11 1.382(11) . ?
C1 O1 1.307(9) . ?
O6 N5 1.253(9) . ?
C14 O3 1.335(8) . ?
C14 C13 1.405(10) . ?
C14 C9 1.417(10) . ?
O5 C15 1.040(5) . ?
C9 C10 1.406(10) . ?
C9 C8 1.478(10) 8_765 ?
N5 O8 1.218(9) . ?
C3 C4 1.390(11) . ?
C8 C9 1.478(10) 8_755 ?
C11 C10 1.369(11) . ?
O4 C18 1.218(10) . ?
C4 C5 1.374(11) . ?
N3 C18 1.291(10) . ?
N3 C20 1.433(10) . ?
N3 C19 1.447(11) . ?
N4 C15 1.275(8) . ?
N4 C16 1.395(12) . ?
N4 C17 1.389(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Er1 O3 93.9(2) . . ?
O1 Er1 O4 149.6(2) . . ?
O3 Er1 O4 92.8(2) . . ?
O1 Er1 O5 96.6(2) . . ?
O3 Er1 O5 158.51(19) . . ?
O4 Er1 O5 87.4(3) . . ?
O1 Er1 O2 136.50(19) . . ?
O3 Er1 O2 81.71(17) . . ?
O4 Er1 O2 73.8(2) . . ?
O5 Er1 O2 77.7(2) . . ?
O1 Er1 O7 76.61(19) . . ?
O3 Er1 O7 74.46(18) . . ?
O4 Er1 O7 76.8(2) . . ?
O5 Er1 O7 126.2(2) . . ?
O2 Er1 O7 140.84(18) . . ?
O1 Er1 O6 78.0(2) . . ?
O3 Er1 O6 126.11(19) . . ?
O4 Er1 O6 74.1(2) . . ?
O5 Er1 O6 74.6(2) . . ?
O2 Er1 O6 138.04(19) . . ?
O7 Er1 O6 51.74(19) . . ?
O1 Er1 N1 71.07(19) . . ?
O3 Er1 N1 83.91(18) . . ?
O4 Er1 N1 139.2(2) . . ?
O5 Er1 N1 81.9(2) . . ?
O2 Er1 N1 65.43(18) . . ?
O7 Er1 N1 139.46(19) . . ?
O6 Er1 N1 138.4(2) . . ?
N5 O7 Er1 95.6(4) . . ?
C7 N1 N2 114.1(6) . . ?
C7 N1 Er1 132.9(5) . . ?
N2 N1 Er1 113.0(4) . . ?
C8 O2 Er1 123.1(5) . . ?
C8 N2 N1 117.0(6) . . ?
C5 C6 C1 119.5(7) . . ?
C5 C6 C7 118.3(7) . . ?
C1 C6 C7 122.3(7) . . ?
C3 C2 C1 121.7(8) . . ?
C13 C12 C11 121.2(7) . . ?
O1 C1 C2 119.8(7) . . ?
O1 C1 C6 122.6(7) . . ?
C2 C1 C6 117.6(7) . . ?
N5 O6 Er1 95.5(4) . . ?
C1 O1 Er1 146.6(5) . . ?
O3 C14 C13 121.1(7) . . ?
O3 C14 C9 121.2(7) . . ?
C13 C14 C9 117.6(7) . . ?
C15 O5 Er1 166.5(6) . . ?
C10 C9 C14 119.4(7) . . ?
C10 C9 C8 116.8(7) . 8_765 ?
C14 C9 C8 123.8(7) . 8_765 ?
N1 C7 C6 124.5(7) . . ?
C12 C13 C14 121.2(7) . . ?
O8 N5 O6 122.4(8) . . ?
O8 N5 O7 120.5(8) . . ?
O6 N5 O7 117.1(7) . . ?
C2 C3 C4 120.9(8) . . ?
O2 C8 N2 121.0(7) . . ?
O2 C8 C9 122.7(7) . 8_755 ?
N2 C8 C9 116.3(7) . 8_755 ?
C10 C11 C12 119.2(7) . . ?
C18 O4 Er1 144.7(7) . . ?
C5 C4 C3 118.7(8) . . ?
C11 C10 C9 121.4(7) . . ?
C4 C5 C6 121.5(8) . . ?
C18 N3 C20 120.3(8) . . ?
C18 N3 C19 123.0(8) . . ?
C20 N3 C19 116.6(7) . . ?
C15 N4 C16 126.5(9) . . ?
C15 N4 C17 120.8(8) . . ?
C16 N4 C17 112.7(8) . . ?
O4 C18 N3 126.1(9) . . ?
C14 O3 Er1 148.3(4) . . ?
O5 C15 N4 150.6(6) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.439
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_hkf1038_0m
_database_code_depnum_ccdc_archive 'CCDC 1009153'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 Ho N5 O8'
_chemical_formula_sum            'C20 H24 Ho N5 O8'
_chemical_formula_weight         627.37

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   17.497(2)
_cell_length_b                   10.6651(12)
_cell_length_c                   25.333(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4727.4(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6823
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.9

_exptl_crystal_description       chunk
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    3.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5914
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34501
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         28.33
_reflns_number_total             5867
_reflns_number_gt                4203
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0229P)²+7.8349P] 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         5867
_refine_ls_number_parameters     311
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0690
_refine_ls_wR_factor_gt          0.0612
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
C10 C 0.1753(2) 1.0629(3) 0.21624(16) 0.0305(9) Uani 1 1 d . . .
H10 H 0.1326 1.0112 0.2137 0.037 Uiso 1 1 calc R . .
C9 C 0.2163(2) 1.0670(3) 0.26386(15) 0.0252(8) Uani 1 1 d . . .
C13 C 0.1982(2) 0.7158(3) 0.22399(16) 0.0313(9) Uani 1 1 d . . .
H13 H 0.1556 0.7678 0.2257 0.038 Uiso 1 1 calc R . .
C14 C 0.2189(2) 0.6452(3) 0.26888(15) 0.0261(8) Uani 1 1 d . . .
Ho1 Ho 0.098544(9) 0.759771(13) 0.363051(7) 0.02428(6) Uani 1 1 d . . .
O6 O 0.05141(16) 0.5417(2) 0.36596(12) 0.0351(6) Uani 1 1 d . . .
N1 N 0.21792(19) 0.8825(3) 0.38662(12) 0.0261(7) Uani 1 1 d . . .
O2 O 0.13059(15) 0.9196(2) 0.30321(10) 0.0287(6) Uani 1 1 d . . .
N2 N 0.23672(19) 0.9723(3) 0.34854(12) 0.0289(7) Uani 1 1 d . . .
H2A H 0.2365 1.0479 0.3650 0.035 Uiso 1 1 d . . .
C8 C 0.1906(2) 0.9826(3) 0.30613(15) 0.0257(8) Uani 1 1 d . . .
C6 C 0.2616(2) 0.7822(3) 0.46721(14) 0.0266(8) Uani 1 1 d . . .
O7 O -0.01675(16) 0.6780(3) 0.40773(13) 0.0419(7) Uani 1 1 d . . .
C1 C 0.2005(2) 0.6954(3) 0.47141(15) 0.0291(8) Uani 1 1 d . . .
C7 C 0.2665(2) 0.8716(3) 0.42423(15) 0.0281(8) Uani 1 1 d . . .
H7 H 0.3083 0.9255 0.4239 0.034 Uiso 1 1 calc R . .
C2 C 0.1998(2) 0.6155(3) 0.51554(15) 0.0317(9) Uani 1 1 d . . .
H2 H 0.1593 0.5600 0.5199 0.038 Uiso 1 1 calc R . .
O1 O 0.14621(17) 0.6883(3) 0.43640(11) 0.0386(7) Uani 1 1 d . . .
N5 N -0.0067(2) 0.5651(3) 0.39496(15) 0.0391(9) Uani 1 1 d . . .
C3 C 0.2573(3) 0.6171(4) 0.55241(16) 0.0353(10) Uani 1 1 d . . .
H3 H 0.2554 0.5626 0.5810 0.042 Uiso 1 1 calc R . .
C4 C 0.3187(3) 0.7001(4) 0.54728(16) 0.0359(10) Uani 1 1 d . . .
H4 H 0.3583 0.6999 0.5718 0.043 Uiso 1 1 calc R . .
C5 C 0.3194(2) 0.7819(4) 0.50540(16) 0.0328(9) Uani 1 1 d . . .
H5 H 0.3595 0.8387 0.5023 0.039 Uiso 1 1 calc R . .
O8 O -0.0508(2) 0.4822(3) 0.40769(16) 0.0667(11) Uani 1 1 d . . .
O4 O 0.00523(18) 0.7554(3) 0.29875(15) 0.0620(11) Uani 1 1 d . . .
O5 O 0.0386(2) 0.9343(3) 0.39968(14) 0.0537(9) Uani 1 1 d U . .
C18 C -0.0130(3) 0.7254(4) 0.2534(2) 0.0489(12) Uani 1 1 d . . .
H18 H 0.0109 0.6560 0.2385 0.059 Uiso 1 1 calc R . .
N3 N -0.06367(19) 0.7848(3) 0.22507(13) 0.0312(7) Uani 1 1 d . . .
C19 C -0.0833(3) 0.7456(4) 0.17198(18) 0.0557(14) Uani 1 1 d . . .
H19A H -0.0631 0.8046 0.1470 0.084 Uiso 1 1 calc R . .
H19B H -0.1379 0.7419 0.1685 0.084 Uiso 1 1 calc R . .
H19C H -0.0620 0.6642 0.1653 0.084 Uiso 1 1 calc R . .
C20 C -0.1046(3) 0.8911(4) 0.24649(19) 0.0485(12) Uani 1 1 d . . .
H20A H -0.0806 0.9176 0.2787 0.073 Uiso 1 1 calc R . .
H20B H -0.1566 0.8676 0.2535 0.073 Uiso 1 1 calc R . .
H20C H -0.1037 0.9587 0.2215 0.073 Uiso 1 1 calc R . .
O3 O 0.17892(15) 0.6520(2) 0.31297(10) 0.0274(6) Uani 1 1 d . . .
N4 N -0.0194(2) 1.1023(3) 0.43487(15) 0.0389(9) Uani 1 1 d . . .
C15 C 0.0365(3) 1.0207(4) 0.4307(2) 0.0493(12) Uani 1 1 d U . .
H15 H 0.0778 1.0299 0.4534 0.059 Uiso 1 1 calc R . .
C17 C -0.0856(4) 1.1059(6) 0.4031(3) 0.082(2) Uani 1 1 d . . .
H17A H -0.0826 1.1757 0.3793 0.123 Uiso 1 1 calc R . .
H17B H -0.1299 1.1150 0.4252 0.123 Uiso 1 1 calc R . .
H17C H -0.0895 1.0294 0.3833 0.123 Uiso 1 1 calc R . .
C16 C -0.0122(4) 1.2024(5) 0.4733(2) 0.0688(16) Uani 1 1 d . . .
H16A H 0.0341 1.1914 0.4931 0.103 Uiso 1 1 calc R . .
H16B H -0.0551 1.2005 0.4968 0.103 Uiso 1 1 calc R . .
H16C H -0.0108 1.2817 0.4554 0.103 Uiso 1 1 calc R . .
C12 C 0.2394(2) 0.7098(4) 0.17759(16) 0.0353(9) Uani 1 1 d . . .
H12 H 0.2241 0.7576 0.1487 0.042 Uiso 1 1 calc R . .
C11 C 0.1966(2) 1.1334(4) 0.17347(16) 0.0348(9) Uani 1 1 d . . .
H11 H 0.1688 1.1300 0.1422 0.042 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
C10 C11 1.370(5) . ?
C10 C9 1.405(5) . ?
C9 C14 1.414(5) 8_665 ?
C9 C8 1.469(5) . ?
C13 C12 1.381(6) . ?
C13 C14 1.411(5) . ?
C14 O3 1.319(4) . ?
C14 C9 1.414(5) 8_655 ?
Ho1 O1 2.175(3) . ?
Ho1 O3 2.216(2) . ?
Ho1 O4 2.307(3) . ?
Ho1 O5 2.329(3) . ?
Ho1 O2 2.349(2) . ?
Ho1 O6 2.469(3) . ?
Ho1 O7 2.472(3) . ?
Ho1 N1 2.536(3) . ?
O6 N5 1.278(4) . ?
N1 C7 1.282(5) . ?
N1 N2 1.399(4) . ?
O2 C8 1.250(4) . ?
N2 C8 1.348(5) . ?
C6 C5 1.400(5) . ?
C6 C1 1.419(5) . ?
C6 C7 1.450(5) . ?
O7 N5 1.259(4) . ?
C1 O1 1.302(5) . ?
C1 C2 1.405(5) . ?
C2 C3 1.373(6) . ?
N5 O8 1.218(4) . ?
C3 C4 1.398(6) . ?
C4 C5 1.374(5) . ?
O4 C18 1.234(6) . ?
O5 C15 1.212(5) . ?
C18 N3 1.306(6) . ?
N3 C20 1.446(5) . ?
N3 C19 1.450(6) . ?
N4 C15 1.313(5) . ?
N4 C17 1.412(7) . ?
N4 C16 1.450(6) . ?
C12 C11 1.389(6) 8_655 ?
C11 C12 1.389(6) 8_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
C11 C10 C9 121.5(4) . . ?
C10 C9 C14 120.4(3) . 8_665 ?
C10 C9 C8 116.8(3) . . ?
C14 C9 C8 122.8(3) 8_665 . ?
C12 C13 C14 121.8(4) . . ?
O3 C14 C13 121.1(3) . . ?
O3 C14 C9 122.3(3) . 8_655 ?
C13 C14 C9 116.6(4) . 8_655 ?
O1 Ho1 O3 93.66(11) . . ?
O1 Ho1 O4 150.19(11) . . ?
O3 Ho1 O4 91.97(13) . . ?
O1 Ho1 O5 96.47(12) . . ?
O3 Ho1 O5 158.22(10) . . ?
O4 Ho1 O5 88.77(14) . . ?
O1 Ho1 O2 135.58(10) . . ?
O3 Ho1 O2 81.69(9) . . ?
O4 Ho1 O2 74.21(10) . . ?
O5 Ho1 O2 77.57(10) . . ?
O1 Ho1 O6 76.83(10) . . ?
O3 Ho1 O6 74.95(9) . . ?
O4 Ho1 O6 76.45(11) . . ?
O5 Ho1 O6 126.17(11) . . ?
O2 Ho1 O6 141.51(9) . . ?
O1 Ho1 O7 78.35(10) . . ?
O3 Ho1 O7 126.66(9) . . ?
O4 Ho1 O7 74.85(12) . . ?
O5 Ho1 O7 74.44(10) . . ?
O2 Ho1 O7 138.26(9) . . ?
O6 Ho1 O7 51.79(9) . . ?
O1 Ho1 N1 70.37(10) . . ?
O3 Ho1 N1 83.09(10) . . ?
O4 Ho1 N1 139.43(10) . . ?
O5 Ho1 N1 82.25(11) . . ?
O2 Ho1 N1 65.22(9) . . ?
O6 Ho1 N1 138.96(10) . . ?
O7 Ho1 N1 138.28(10) . . ?
N5 O6 Ho1 95.7(2) . . ?
C7 N1 N2 114.7(3) . . ?
C7 N1 Ho1 132.4(2) . . ?
N2 N1 Ho1 112.6(2) . . ?
C8 O2 Ho1 123.6(2) . . ?
C8 N2 N1 117.7(3) . . ?
O2 C8 N2 120.4(3) . . ?
O2 C8 C9 122.9(3) . . ?
N2 C8 C9 116.6(3) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 118.5(3) . . ?
C1 C6 C7 122.0(3) . . ?
N5 O7 Ho1 96.0(2) . . ?
O1 C1 C2 120.1(4) . . ?
O1 C1 C6 122.5(3) . . ?
C2 C1 C6 117.5(4) . . ?
N1 C7 C6 125.3(3) . . ?
C3 C2 C1 121.9(4) . . ?
C1 O1 Ho1 147.3(2) . . ?
O8 N5 O7 122.5(4) . . ?
O8 N5 O6 121.0(4) . . ?
O7 N5 O6 116.5(3) . . ?
C2 C3 C4 120.5(4) . . ?
C5 C4 C3 118.8(4) . . ?
C4 C5 C6 121.9(4) . . ?
C18 O4 Ho1 147.7(4) . . ?
C15 O5 Ho1 151.6(4) . . ?
O4 C18 N3 124.1(5) . . ?
C18 N3 C20 120.7(4) . . ?
C18 N3 C19 122.1(4) . . ?
C20 N3 C19 117.2(4) . . ?
C14 O3 Ho1 148.2(2) . . ?
C15 N4 C17 125.7(5) . . ?
C15 N4 C16 118.5(5) . . ?
C17 N4 C16 115.7(4) . . ?
O5 C15 N4 125.4(5) . . ?
C13 C12 C11 120.8(4) . 8_655 ?
C10 C11 C12 118.8(4) . 8_665 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.108
####################################################################### 
# 
# 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_hkf1039_0m
_database_code_depnum_ccdc_archive 'CCDC 1009154'
_audit_update_record             
;
2014-11-28 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H24 N5 O8 Tb'
_chemical_formula_sum            'C20 H24 N5 O8 Tb'
_chemical_formula_weight         621.36

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           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   17.5789(15)
_cell_length_b                   10.6997(9)
_cell_length_c                   25.330(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4764.3(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7322
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      28.1

_exptl_crystal_description       chunk
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_absorpt_coefficient_mu    3.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6589
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33893
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         28.28
_reflns_number_total             5908
_reflns_number_gt                4192
_reflns_threshold_expression     >2sigma(I)

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

_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+6.0111P] 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         5908
_refine_ls_number_parameters     311
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0640
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.097494(8) 0.741918(13) 0.137644(7) 0.02463(6) Uani 1 1 d . . .
O6 O 0.05045(15) 0.9619(2) 0.13311(12) 0.0378(6) Uani 1 1 d . . .
N1 N 0.21687(17) 0.6170(2) 0.11395(12) 0.0265(6) Uani 1 1 d . . .
O2 O 0.13049(13) 0.5805(2) 0.19759(10) 0.0308(6) Uani 1 1 d . . .
C6 C 0.2612(2) 0.7162(3) 0.03335(14) 0.0263(7) Uani 1 1 d . . .
C8 C 0.19068(19) 0.5182(3) 0.19442(14) 0.0257(7) Uani 1 1 d . . .
O3 O 0.17920(13) 0.8502(2) 0.18787(10) 0.0293(6) Uani 1 1 d . . .
N2 N 0.23616(17) 0.5284(3) 0.15196(12) 0.0289(7) Uani 1 1 d . . .
H2A H 0.2363 0.4528 0.1357 0.035 Uiso 1 1 d . . .
C7 C 0.26532(19) 0.6272(3) 0.07601(15) 0.0281(8) Uani 1 1 d . . .
H7 H 0.3065 0.5725 0.0762 0.034 Uiso 1 1 calc R . .
O1 O 0.14518(15) 0.8096(3) 0.06313(11) 0.0396(7) Uani 1 1 d . . .
C10 C 0.1758(2) 0.4386(3) 0.28443(15) 0.0320(8) Uani 1 1 d . . .
H10 H 0.1332 0.4898 0.2871 0.038 Uiso 1 1 calc R . .
C3 C 0.2579(2) 0.8807(3) -0.05193(16) 0.0353(9) Uani 1 1 d . . .
H3 H 0.2566 0.9352 -0.0805 0.042 Uiso 1 1 calc R . .
C1 C 0.2002(2) 0.8034(3) 0.02837(15) 0.0295(8) Uani 1 1 d . . .
O7 O -0.01812(15) 0.8251(3) 0.09288(13) 0.0428(7) Uani 1 1 d . . .
N3 N -0.06529(17) 0.7175(3) 0.27597(13) 0.0318(7) Uani 1 1 d . . .
C2 C 0.2003(2) 0.8824(3) -0.01583(15) 0.0329(8) Uani 1 1 d . . .
H2 H 0.1600 0.9375 -0.0207 0.039 Uiso 1 1 calc R . .
C19 C -0.0878(3) 0.7537(4) 0.32881(18) 0.0533(12) Uani 1 1 d . . .
H19A H -0.0697 0.6928 0.3536 0.080 Uiso 1 1 calc R . .
H19B H -0.1423 0.7584 0.3307 0.080 Uiso 1 1 calc R . .
H19C H -0.0664 0.8338 0.3371 0.080 Uiso 1 1 calc R . .
C9 C 0.21595(19) 0.4351(3) 0.23693(14) 0.0259(7) Uani 1 1 d . . .
C5 C 0.3188(2) 0.7167(3) -0.00465(16) 0.0335(8) Uani 1 1 d . . .
H5 H 0.3586 0.6598 -0.0015 0.040 Uiso 1 1 calc R . .
C20 C -0.1036(3) 0.6105(4) 0.25325(19) 0.0538(12) Uani 1 1 d . . .
H20A H -0.1563 0.6302 0.2477 0.081 Uiso 1 1 calc R . .
H20B H -0.0995 0.5407 0.2769 0.081 Uiso 1 1 calc R . .
H20C H -0.0804 0.5897 0.2201 0.081 Uiso 1 1 calc R . .
N5 N -0.00778(19) 0.9375(3) 0.10505(15) 0.0409(8) Uani 1 1 d . . .
C18 C -0.0150(2) 0.7788(4) 0.2489(2) 0.0470(11) Uani 1 1 d . . .
H18 H 0.0069 0.8486 0.2647 0.056 Uiso 1 1 calc R . .
C11 C 0.1973(2) 0.3688(3) 0.32748(16) 0.0345(9) Uani 1 1 d . . .
H11 H 0.1698 0.3727 0.3588 0.041 Uiso 1 1 calc R . .
O8 O -0.05188(19) 1.0210(3) 0.09268(17) 0.0739(12) Uani 1 1 d . . .
C4 C 0.3186(2) 0.7981(3) -0.04645(16) 0.0363(9) Uani 1 1 d . . .
H4 H 0.3583 0.7982 -0.0707 0.044 Uiso 1 1 calc R . .
O4 O 0.00591(17) 0.7517(3) 0.20413(15) 0.0647(11) Uani 1 1 d . . .
N4 N -0.01818(18) 0.3965(3) 0.06462(14) 0.0374(8) Uani 1 1 d . . .
C15 C 0.0354(3) 0.4797(4) 0.06918(18) 0.0464(10) Uani 1 1 d U . .
H15 H 0.0766 0.4732 0.0463 0.056 Uiso 1 1 calc R . .
C17 C -0.0847(3) 0.3943(5) 0.0973(2) 0.0714(16) Uani 1 1 d . . .
H17A H -0.0875 0.4703 0.1173 0.107 Uiso 1 1 calc R . .
H17B H -0.0821 0.3243 0.1209 0.107 Uiso 1 1 calc R . .
H17C H -0.1292 0.3869 0.0754 0.107 Uiso 1 1 calc R . .
C16 C -0.0115(3) 0.2956(4) 0.0266(2) 0.0629(14) Uani 1 1 d . . .
H16A H 0.0342 0.3062 0.0064 0.094 Uiso 1 1 calc R . .
H16B H -0.0547 0.2967 0.0034 0.094 Uiso 1 1 calc R . .
H16C H -0.0097 0.2171 0.0449 0.094 Uiso 1 1 calc R . .
O5 O 0.03637(19) 0.5659(3) 0.10116(14) 0.0551(9) Uani 1 1 d U . .
C13 C 0.3019(2) 0.2861(3) 0.27686(15) 0.0304(8) Uani 1 1 d . . .
H13 H 0.3443 0.2343 0.2750 0.037 Uiso 1 1 calc R . .
C12 C 0.2612(2) 0.2917(4) 0.32309(16) 0.0347(9) Uani 1 1 d . . .
H12 H 0.2764 0.2436 0.3518 0.042 Uiso 1 1 calc R . .
C14 C 0.21893(19) 0.8567(3) 0.23228(14) 0.0246(7) 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 O1 2.188(3) . ?
Tb1 O3 2.242(2) . ?
Tb1 O4 2.332(3) . ?
Tb1 O5 2.357(3) . ?
Tb1 O2 2.372(2) . ?
Tb1 O7 2.492(3) . ?
Tb1 O6 2.497(2) . ?
Tb1 N1 2.559(3) . ?
O6 N5 1.273(4) . ?
N1 C7 1.289(4) . ?
N1 N2 1.394(4) . ?
O2 C8 1.253(4) . ?
C6 C5 1.397(5) . ?
C6 C1 1.427(5) . ?
C6 C7 1.442(5) . ?
C8 N2 1.344(4) . ?
C8 C9 1.465(5) . ?
O3 C14 1.326(4) . ?
O1 C1 1.310(4) . ?
C10 C11 1.374(5) . ?
C10 C9 1.395(5) . ?
C3 C2 1.364(5) . ?
C3 C4 1.392(5) . ?
C1 C2 1.403(5) . ?
O7 N5 1.255(4) . ?
N3 C18 1.297(5) . ?
N3 C20 1.448(5) . ?
N3 C19 1.448(5) . ?
C9 C14 1.424(4) 8_655 ?
C5 C4 1.372(5) . ?
N5 O8 1.224(4) . ?
C18 O4 1.228(6) . ?
C11 C12 1.400(5) . ?
N4 C15 1.301(5) . ?
N4 C17 1.433(6) . ?
N4 C16 1.451(6) . ?
C15 O5 1.228(5) . ?
C13 C12 1.373(5) . ?
C13 C14 1.407(5) 8_655 ?
C14 C13 1.407(5) 8_665 ?
C14 C9 1.424(4) 8_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
O1 Tb1 O3 94.19(10) . . ?
O1 Tb1 O4 150.73(10) . . ?
O3 Tb1 O4 90.53(12) . . ?
O1 Tb1 O5 95.78(12) . . ?
O3 Tb1 O5 158.09(9) . . ?
O4 Tb1 O5 90.25(13) . . ?
O1 Tb1 O2 134.38(9) . . ?
O3 Tb1 O2 81.74(8) . . ?
O4 Tb1 O2 74.88(9) . . ?
O5 Tb1 O2 77.33(10) . . ?
O1 Tb1 O7 78.57(10) . . ?
O3 Tb1 O7 126.61(9) . . ?
O4 Tb1 O7 75.49(11) . . ?
O5 Tb1 O7 74.63(10) . . ?
O2 Tb1 O7 138.67(9) . . ?
O1 Tb1 O6 77.02(9) . . ?
O3 Tb1 O6 75.58(8) . . ?
O4 Tb1 O6 76.25(10) . . ?
O5 Tb1 O6 125.73(10) . . ?
O2 Tb1 O6 142.82(9) . . ?
O7 Tb1 O6 51.13(9) . . ?
O1 Tb1 N1 69.90(9) . . ?
O3 Tb1 N1 82.97(9) . . ?
O4 Tb1 N1 139.37(10) . . ?
O5 Tb1 N1 82.22(10) . . ?
O2 Tb1 N1 64.50(9) . . ?
O7 Tb1 N1 138.47(10) . . ?
O6 Tb1 N1 138.83(9) . . ?
N5 O6 Tb1 95.7(2) . . ?
C7 N1 N2 114.3(3) . . ?
C7 N1 Tb1 132.3(2) . . ?
N2 N1 Tb1 113.1(2) . . ?
C8 O2 Tb1 123.6(2) . . ?
C5 C6 C1 118.8(3) . . ?
C5 C6 C7 118.8(3) . . ?
C1 C6 C7 122.4(3) . . ?
O2 C8 N2 120.7(3) . . ?
O2 C8 C9 122.1(3) . . ?
N2 C8 C9 117.2(3) . . ?
C14 O3 Tb1 147.8(2) . . ?
C8 N2 N1 117.6(3) . . ?
N1 C7 C6 125.5(3) . . ?
C1 O1 Tb1 147.8(2) . . ?
C11 C10 C9 122.1(3) . . ?
C2 C3 C4 120.7(4) . . ?
O1 C1 C2 120.5(3) . . ?
O1 C1 C6 121.9(3) . . ?
C2 C1 C6 117.6(3) . . ?
N5 O7 Tb1 96.5(2) . . ?
C18 N3 C20 120.5(4) . . ?
C18 N3 C19 122.6(4) . . ?
C20 N3 C19 116.8(4) . . ?
C3 C2 C1 121.8(3) . . ?
C10 C9 C14 119.6(3) . 8_655 ?
C10 C9 C8 117.7(3) . . ?
C14 C9 C8 122.7(3) 8_655 . ?
C4 C5 C6 122.1(4) . . ?
O8 N5 O7 123.0(4) . . ?
O8 N5 O6 120.2(4) . . ?
O7 N5 O6 116.7(3) . . ?
O4 C18 N3 125.0(4) . . ?
C10 C11 C12 118.5(4) . . ?
C5 C4 C3 118.8(4) . . ?
C18 O4 Tb1 152.2(3) . . ?
C15 N4 C17 123.5(4) . . ?
C15 N4 C16 120.6(4) . . ?
C17 N4 C16 115.9(4) . . ?
O5 C15 N4 125.6(5) . . ?
C15 O5 Tb1 149.9(3) . . ?
C12 C13 C14 121.8(3) . 8_655 ?
C13 C12 C11 120.8(4) . . ?
O3 C14 C13 121.1(3) . 8_665 ?
O3 C14 C9 121.6(3) . 8_665 ?
C13 C14 C9 117.3(3) 8_665 8_665 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.101
