# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H8 N6 O4 '
_chemical_formula_weight         252.20

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  -P2yn

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

_cell_length_a                   3.9726(2)
_cell_length_b                   10.6370(6)
_cell_length_c                   24.5982(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.158(4)
_cell_angle_gamma                90.00
_cell_volume                     1039.22(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2958
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520.0
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6711
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1835
_reflns_number_gt                1436
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0890P)²+0.6598P] 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     SHELXL
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1835
_refine_ls_number_parameters     174
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1663
_refine_ls_wR_factor_gt          0.1563
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.004

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
N1 N 0.6380(6) 0.2581(2) -0.05473(9) 0.0363(6) Uani 1 1 d . . .
N2 N 0.5555(6) 0.1665(2) -0.08427(9) 0.0363(6) Uani 1 1 d . . .
N3 N 0.8546(6) 0.2775(2) -0.15650(9) 0.0345(6) Uani 1 1 d . . .
N6 N 0.6008(6) 0.1002(2) -0.17624(9) 0.0383(6) Uani 1 1 d . . .
H5 H 0.4894 0.0313 -0.1730 0.046 Uiso 1 1 calc R . .
N5 N 0.7375(6) 0.1445(2) -0.22083(9) 0.0389(6) Uani 1 1 d . . .
N4 N 0.8920(6) 0.2510(2) -0.20890(9) 0.0381(6) Uani 1 1 d . . .
C7 C 0.6815(7) 0.4556(3) 0.12276(11) 0.0311(6) Uani 1 1 d . . .
C3 C 0.2666(7) 0.1545(3) 0.07569(11) 0.0350(7) Uani 1 1 d . . .
H3 H 0.1435 0.0888 0.0904 0.042 Uiso 1 1 calc R . .
C4 C 0.3452(7) 0.1524(3) 0.02165(11) 0.0335(7) Uani 1 1 d . . .
H4 H 0.2738 0.0860 -0.0003 0.040 Uiso 1 1 calc R . .
C1 C 0.5600(6) 0.3526(2) 0.08710(10) 0.0281(6) Uani 1 1 d . . .
C2 C 0.3695(7) 0.2542(2) 0.10876(11) 0.0301(6) Uani 1 1 d . . .
C6 C 0.6366(7) 0.3490(3) 0.03239(11) 0.0303(6) Uani 1 1 d . . .
H6 H 0.7600 0.4143 0.0174 0.036 Uiso 1 1 calc R . .
C8 C 0.6695(7) 0.1827(3) -0.13764(11) 0.0313(6) Uani 1 1 d . . .
C5 C 0.5328(7) 0.2503(3) -0.00024(11) 0.0312(6) Uani 1 1 d . . .
O2 O 0.5998(5) 0.46282(19) 0.17052(8) 0.0434(6) Uani 1 1 d . . .
O1 O 0.8811(5) 0.53420(19) 0.09924(8) 0.0415(6) Uani 1 1 d D . .
H1 H 0.9614 0.5826 0.1220 0.062 Uiso 1 1 calc RD . .
O3 O 0.2787(6) 0.2525(2) 0.16140(8) 0.0411(6) Uani 1 1 d D . .
O4 O 0.8189(6) 0.0921(2) 0.22652(10) 0.0552(7) Uani 1 1 d D . .
H2 H 0.352(10) 0.319(3) 0.1724(17) 0.083 Uiso 1 1 d D . .
H7 H 0.925(9) 0.050(4) 0.2506(13) 0.083 Uiso 1 1 d D . .
H8 H 0.975(8) 0.134(3) 0.2098(14) 0.083 Uiso 1 1 d 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
N1 N2 1.255(3) . ?
N1 C5 1.415(3) . ?
N2 C8 1.408(3) . ?
N3 N4 1.331(3) . ?
N3 C8 1.336(3) . ?
N6 C8 1.318(4) . ?
N6 N5 1.321(3) . ?
N6 H5 0.8600 . ?
N5 N4 1.318(3) . ?
C7 O2 1.228(3) . ?
C7 O1 1.296(3) . ?
C7 C1 1.479(4) . ?
C3 C4 1.372(4) . ?
C3 C2 1.392(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(4) . ?
C4 H4 0.9300 . ?
C1 C6 1.386(4) . ?
C1 C2 1.403(4) . ?
C2 O3 1.351(3) . ?
C6 C5 1.380(4) . ?
C6 H6 0.9300 . ?
O1 H1 0.8200 . ?
O3 H2 0.806(19) . ?
O4 H7 0.850(18) . ?
O4 H8 0.872(18) . ?

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
N2 N1 C5 115.1(2) . . ?
N1 N2 C8 111.1(2) . . ?
N4 N3 C8 104.4(2) . . ?
C8 N6 N5 106.1(2) . . ?
C8 N6 H5 126.9 . . ?
N5 N6 H5 126.9 . . ?
N4 N5 N6 108.6(2) . . ?
N5 N4 N3 109.7(2) . . ?
O2 C7 O1 124.3(3) . . ?
O2 C7 C1 121.6(2) . . ?
O1 C7 C1 114.1(2) . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C1 C2 118.6(2) . . ?
C6 C1 C7 121.4(2) . . ?
C2 C1 C7 120.0(2) . . ?
O3 C2 C3 117.9(2) . . ?
O3 C2 C1 122.0(2) . . ?
C3 C2 C1 120.0(2) . . ?
C5 C6 C1 121.1(2) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
N6 C8 N3 111.1(2) . . ?
N6 C8 N2 121.6(2) . . ?
N3 C8 N2 127.3(2) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 N1 114.6(2) . . ?
C4 C5 N1 125.4(2) . . ?
C7 O1 H1 109.5 . . ?
C2 O3 H2 102(3) . . ?
H7 O4 H8 104(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 922441'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 N6 O7'
_chemical_formula_weight         306.25

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   27.104(10)
_cell_length_b                   3.8044(13)
_cell_length_c                   27.047(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.58(2)
_cell_angle_gamma                90.00
_cell_volume                     2732.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1610
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      21.77

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1280.0
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            10622
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         27.55
_reflns_number_total             3135
_reflns_number_gt                1730
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.1324P)²+1.0209P] 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     SHELXL
_refine_ls_extinction_coef       0.0057(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         30135
_refine_ls_number_parameters     220
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0705
_refine_ls_wR_factor_ref         0.2402
_refine_ls_wR_factor_gt          0.2087
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.083
_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
N1 N 0.20667(9) 1.0190(8) 0.13317(9) 0.0341(7) Uani 1 1 d . . .
N2 N 0.25264(9) 1.0562(8) 0.15298(10) 0.0359(7) Uani 1 1 d . . .
N3 N 0.26639(10) 1.2868(8) 0.07240(10) 0.0377(7) Uani 1 1 d . . .
H1 H 0.2362 1.3480 0.0586 0.045 Uiso 1 1 calc R . .
N6 N 0.33120(9) 1.0813(8) 0.12684(10) 0.0376(7) Uani 1 1 d . . .
N4 N 0.30810(11) 1.3212(8) 0.05371(10) 0.0406(7) Uani 1 1 d . . .
N5 N 0.34690(10) 1.1960(8) 0.08588(10) 0.0401(7) Uani 1 1 d . . .
C6 C 0.12721(11) 0.8231(9) 0.14635(12) 0.0349(8) Uani 1 1 d . . .
H6 H 0.1185 0.7951 0.1115 0.042 Uiso 1 1 calc R . .
C5 C 0.17457(12) 0.9490(9) 0.16762(11) 0.0313(7) Uani 1 1 d . . .
C3 C 0.15391(12) 0.9204(10) 0.24906(12) 0.0392(8) Uani 1 1 d . . .
H3 H 0.1626 0.9556 0.2837 0.047 Uiso 1 1 calc R . .
C2 C 0.10611(12) 0.7865(9) 0.22777(12) 0.0343(8) Uani 1 1 d . . .
C1 C 0.09240(11) 0.7376(9) 0.17547(11) 0.0322(7) Uani 1 1 d . . .
C4 C 0.18791(11) 1.0000(9) 0.21968(12) 0.0350(8) Uani 1 1 d . . .
H4 H 0.2196 1.0870 0.2342 0.042 Uiso 1 1 calc R . .
C8 C 0.28204(11) 1.1357(9) 0.11749(11) 0.0327(8) Uani 1 1 d . . .
C7 C 0.04178(12) 0.5932(10) 0.15185(14) 0.0419(9) Uani 1 1 d D . .
O3 O 0.07396(9) 0.7099(8) 0.25817(9) 0.0506(8) Uani 1 1 d . . .
H5 H 0.0471 0.6424 0.2411 0.076 Uiso 1 1 calc R . .
O2 O 0.01100(9) 0.5524(8) 0.18091(10) 0.0545(8) Uani 1 1 d D . .
O1 O 0.03233(9) 0.5278(8) 0.10585(10) 0.0556(8) Uani 1 1 d D . .
O4 O 0.92443(11) 0.1539(9) 0.15283(12) 0.0626(9) Uani 1 1 d D . .
O5 O 0.09217(11) 0.2955(10) 0.03291(12) 0.0677(9) Uani 1 1 d D . .
O6 O 0.17809(11) 0.7208(9) 0.02910(11) 0.0604(8) Uani 1 1 d D . .
O7 O 0.03886(16) 0.9958(11) 0.94337(16) 0.0899(12) Uani 1 1 d D . .
H7 H 0.925(2) 0.015(15) 0.176(2) 0.135 Uiso 1 1 d D . .
H9 H 0.075(2) 0.331(19) 0.0538(17) 0.135 Uiso 1 1 d D . .
H10 H 0.077(2) 0.22(2) 0.0073(14) 0.135 Uiso 1 1 d D . .
H12 H 0.180(2) 0.860(15) 0.0533(19) 0.135 Uiso 1 1 d D . .
H11 H 0.1496(14) 0.621(16) 0.025(2) 0.135 Uiso 1 1 d D . .
H13 H 0.049(2) 0.798(9) 0.940(3) 0.135 Uiso 1 1 d D . .
H14 H 0.0102(13) 0.980(18) 0.949(3) 0.135 Uiso 1 1 d D . .
H2 H -0.0147(15) 0.417(15) 0.1687(12) 0.135 Uiso 1 1 d D . .
H8 H 0.8971(11) 0.263(11) 0.1481(17) 0.071(15) Uiso 1 1 d 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
N1 N2 1.261(4) . ?
N1 C5 1.422(4) . ?
N2 C8 1.398(4) . ?
N3 N4 1.334(4) . ?
N3 C8 1.338(4) . ?
N3 H1 0.8600 . ?
N6 C8 1.322(4) . ?
N6 N5 1.337(4) . ?
N4 N5 1.312(4) . ?
C6 C5 1.383(4) . ?
C6 C1 1.384(4) . ?
C6 H6 0.9300 . ?
C5 C4 1.395(4) . ?
C3 C4 1.366(4) . ?
C3 C2 1.404(5) . ?
C3 H3 0.9300 . ?
C2 O3 1.344(4) . ?
C2 C1 1.401(4) . ?
C1 C7 1.497(4) . ?
C4 H4 0.9300 . ?
C7 O1 1.244(4) . ?
C7 O2 1.265(4) . ?
O3 H5 0.8200 . ?
O2 H2 0.877(18) . ?
O4 H7 0.82(2) . ?
O4 H8 0.838(19) . ?
O5 H9 0.808(19) . ?
O5 H10 0.788(19) . ?
O6 H12 0.84(2) . ?
O6 H11 0.85(2) . ?
O7 H13 0.81(2) . ?
O7 H14 0.82(2) . ?

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
N2 N1 C5 115.1(2) . . ?
N1 N2 C8 112.5(2) . . ?
N4 N3 C8 104.5(3) . . ?
N4 N3 H1 127.8 . . ?
C8 N3 H1 127.8 . . ?
C8 N6 N5 105.5(3) . . ?
N5 N4 N3 109.9(3) . . ?
N4 N5 N6 108.8(3) . . ?
C5 C6 C1 121.8(3) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 N1 115.5(3) . . ?
C4 C5 N1 124.5(3) . . ?
C4 C3 C2 121.1(3) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
O3 C2 C1 121.1(3) . . ?
O3 C2 C3 119.1(3) . . ?
C1 C2 C3 119.9(3) . . ?
C6 C1 C2 118.1(3) . . ?
C6 C1 C7 121.0(3) . . ?
C2 C1 C7 120.9(3) . . ?
C3 C4 C5 119.2(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N6 C8 N3 111.4(3) . . ?
N6 C8 N2 121.8(3) . . ?
N3 C8 N2 126.8(3) . . ?
O1 C7 O2 124.6(3) . . ?
O1 C7 C1 119.2(3) . . ?
O2 C7 C1 116.2(3) . . ?
C2 O3 H5 109.5 . . ?
C7 O2 H2 114.3(15) . . ?
H7 O4 H8 109(3) . . ?
H9 O5 H10 113(4) . . ?
H12 O6 H11 106(3) . . ?
H13 O7 H14 108(4) . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.071
_database_code_depnum_ccdc_archive 'CCDC 946733'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H46 Dy2 N24 O26'
_chemical_formula_weight         1507.93

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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6459(14)
_cell_length_b                   11.9523(18)
_cell_length_c                   12.8750(19)
_cell_angle_alpha                110.424(2)
_cell_angle_beta                 94.582(2)
_cell_angle_gamma                105.450(2)
_cell_volume                     1316.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8207
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      27.090

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             746.0
_exptl_absorpt_coefficient_mu    2.926
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.304
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11004
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         27.09
_reflns_number_total             5800
_reflns_number_gt                4966
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0197P)²+2.1710P] 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     SHELXL
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5800
_refine_ls_number_parameters     428
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0568
_refine_ls_wR_factor_gt          0.0538
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.027

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 0.471937(16) 0.199653(14) 0.118180(12) 0.01483(6) Uani 1 1 d . . .
O8 O 0.6312(2) 0.3075(2) 0.29679(19) 0.0189(5) Uani 1 1 d D . .
O4 O 0.5192(2) 0.0427(2) 0.16876(18) 0.0196(5) Uani 1 1 d . . .
O1 O 0.3759(2) 0.3504(2) 0.25012(17) 0.0173(4) Uani 1 1 d . . .
O11 O 0.1967(3) 0.8358(2) 0.1286(2) 0.0274(5) Uani 1 1 d D . .
O10 O 0.5827(3) 0.3860(2) 0.08970(19) 0.0214(5) Uani 1 1 d D . .
O9 O 0.6914(3) 0.1754(3) 0.0600(2) 0.0250(5) Uani 1 1 d D . .
O5 O 0.3920(2) 0.1089(2) -0.07530(18) 0.0203(5) Uani 1 1 d . . .
O7 O 0.2604(3) 0.0791(2) 0.1558(2) 0.0299(6) Uani 1 1 d D . .
O2 O 0.2682(2) 0.2738(2) 0.07184(18) 0.0214(5) Uani 1 1 d . . .
C7 C 0.2788(3) 0.3440(3) 0.1745(3) 0.0157(6) Uani 1 1 d . . .
C1 C 0.1759(3) 0.4180(3) 0.2039(3) 0.0163(6) Uani 1 1 d . . .
C6 C 0.1778(3) 0.4899(3) 0.3153(3) 0.0161(6) Uani 1 1 d . . .
H3 H 0.2475 0.4933 0.3738 0.019 Uiso 1 1 calc R . .
C4 C -0.0208(4) 0.5543(3) 0.2559(3) 0.0224(7) Uani 1 1 d . . .
H7 H -0.0871 0.6014 0.2737 0.027 Uiso 1 1 calc R . .
C2 C 0.0735(3) 0.4148(3) 0.1178(3) 0.0191(6) Uani 1 1 d . . .
C5 C 0.0791(3) 0.5571(3) 0.3428(3) 0.0176(6) Uani 1 1 d . . .
C3 C -0.0234(4) 0.4839(3) 0.1455(3) 0.0227(7) Uani 1 1 d . . .
H6 H -0.0920 0.4823 0.0873 0.027 Uiso 1 1 calc R . .
O3 O 0.0678(3) 0.3482(2) 0.00784(19) 0.0248(5) Uani 1 1 d D . .
N2 N -0.0070(3) 0.6734(2) 0.4867(2) 0.0179(5) Uani 1 1 d . . .
N1 N 0.0924(3) 0.6247(2) 0.4592(2) 0.0187(5) Uani 1 1 d . . .
C8 C 0.0132(3) 0.7398(3) 0.6041(3) 0.0165(6) Uani 1 1 d . . .
N6 N 0.1184(3) 0.7507(2) 0.6839(2) 0.0178(5) Uani 1 1 d . . .
N3 N -0.0811(3) 0.7977(3) 0.6475(2) 0.0210(6) Uani 1 1 d . . .
H1 H -0.1590 0.8025 0.6109 0.025 Uiso 1 1 calc R . .
N5 N 0.0881(3) 0.8188(3) 0.7807(2) 0.0187(5) Uani 1 1 d . . .
N4 N -0.0314(3) 0.8474(3) 0.7595(2) 0.0202(6) Uani 1 1 d . . .
C15 C 0.5911(3) -0.0303(3) 0.1660(2) 0.0155(6) Uani 1 1 d . . .
C14 C 0.6350(3) 0.0491(3) 0.3750(3) 0.0163(6) Uani 1 1 d . . .
H15 H 0.5712 0.0968 0.3722 0.020 Uiso 1 1 calc R . .
C9 C 0.6614(3) -0.0276(3) 0.2751(3) 0.0158(6) Uani 1 1 d . . .
C13 C 0.6992(3) 0.0582(3) 0.4796(3) 0.0175(6) Uani 1 1 d . . .
C10 C 0.7566(3) -0.0986(3) 0.2790(3) 0.0197(6) Uani 1 1 d . . .
C12 C 0.7926(4) -0.0134(3) 0.4824(3) 0.0218(7) Uani 1 1 d . . .
H11 H 0.8371 -0.0086 0.5530 0.026 Uiso 1 1 calc R . .
C11 C 0.8203(4) -0.0904(3) 0.3843(3) 0.0228(7) Uani 1 1 d . . .
H12 H 0.8832 -0.1386 0.3878 0.027 Uiso 1 1 calc R . .
O6 O 0.7889(3) -0.1740(2) 0.1864(2) 0.0275(5) Uani 1 1 d D . .
N8 N 0.5918(3) 0.1954(2) 0.5819(2) 0.0182(5) Uani 1 1 d . . .
N7 N 0.6791(3) 0.1336(2) 0.5853(2) 0.0201(6) Uani 1 1 d . . .
C16 C 0.5775(3) 0.2697(3) 0.6898(3) 0.0180(6) Uani 1 1 d . . .
N9 N 0.4942(3) 0.3447(3) 0.7011(2) 0.0210(6) Uani 1 1 d . . .
N12 N 0.6392(3) 0.2774(3) 0.7894(2) 0.0208(6) Uani 1 1 d . . .
N10 N 0.5055(3) 0.4009(3) 0.8127(2) 0.0233(6) Uani 1 1 d . . .
N11 N 0.5922(3) 0.3606(3) 0.8650(2) 0.0242(6) Uani 1 1 d . . .
O12 O 0.6793(3) 0.5560(2) 0.4046(2) 0.0309(6) Uani 1 1 d D . .
O13 O 0.4003(4) 0.2570(3) 0.4262(3) 0.0536(8) Uani 1 1 d D . .
H2 H 0.130(5) 0.315(5) 0.003(5) 0.080 Uiso 1 1 d D . .
H4 H 0.751(6) -0.170(6) 0.132(3) 0.080 Uiso 1 1 d D . .
H5 H 0.186(4) 0.096(5) 0.164(5) 0.080 Uiso 1 1 d D . .
H8 H 0.252(6) 0.011(3) 0.155(5) 0.080 Uiso 1 1 d D . .
H9 H 0.649(5) 0.382(2) 0.326(5) 0.080 Uiso 1 1 d D . .
H10 H 0.701(4) 0.287(4) 0.311(5) 0.080 Uiso 1 1 d D . .
H13 H 0.717(5) 0.175(6) 0.002(3) 0.080 Uiso 1 1 d D . .
H14 H 0.759(4) 0.179(6) 0.103(3) 0.080 Uiso 1 1 d D . .
H16 H 0.583(6) 0.369(5) 0.0244(19) 0.080 Uiso 1 1 d D . .
H17 H 0.555(6) 0.445(4) 0.118(4) 0.080 Uiso 1 1 d D . .
H18 H 0.247(5) 0.817(5) 0.167(4) 0.080 Uiso 1 1 d D . .
H19 H 0.120(3) 0.782(4) 0.098(4) 0.080 Uiso 1 1 d D . .
H21 H 0.633(5) 0.581(5) 0.368(4) 0.080 Uiso 1 1 d D . .
H20 H 0.766(2) 0.595(5) 0.417(5) 0.080 Uiso 1 1 d D . .
H23 H 0.394(6) 0.328(3) 0.467(4) 0.080 Uiso 1 1 d D . .
H22 H 0.458(5) 0.271(5) 0.384(4) 0.080 Uiso 1 1 d 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 O5 2.310(2) . ?
Dy1 O4 2.327(2) . ?
Dy1 O9 2.357(2) . ?
Dy1 O7 2.357(2) . ?
Dy1 O10 2.367(2) . ?
Dy1 O8 2.371(2) . ?
Dy1 O1 2.448(2) . ?
Dy1 O2 2.473(2) . ?
Dy1 C7 2.834(3) . ?
O8 H9 0.799(19) . ?
O8 H10 0.808(19) . ?
O4 C15 1.244(4) . ?
O1 C7 1.263(4) . ?
O11 H18 0.797(19) . ?
O11 H19 0.797(19) . ?
O10 H16 0.795(19) . ?
O10 H17 0.798(19) . ?
O9 H13 0.810(19) . ?
O9 H14 0.797(19) . ?
O5 C15 1.273(4) 2_655 ?
O7 H5 0.799(19) . ?
O7 H8 0.798(19) . ?
O2 C7 1.273(4) . ?
C7 C1 1.485(4) . ?
C1 C6 1.387(4) . ?
C1 C2 1.407(4) . ?
C6 C5 1.392(4) . ?
C6 H3 0.9500 . ?
C4 C3 1.370(5) . ?
C4 C5 1.402(5) . ?
C4 H7 0.9500 . ?
C2 O3 1.349(4) . ?
C2 C3 1.394(4) . ?
C5 N1 1.408(4) . ?
C3 H6 0.9500 . ?
O3 H2 0.80(2) . ?
N2 N1 1.262(4) . ?
N2 C8 1.409(4) . ?
C8 N6 1.331(4) . ?
C8 N3 1.330(4) . ?
N6 N5 1.333(4) . ?
N3 N4 1.343(4) . ?
N3 H1 0.8800 . ?
N5 N4 1.321(4) . ?
C15 O5 1.273(4) 2_655 ?
C15 C9 1.495(4) . ?
C14 C9 1.383(4) . ?
C14 C13 1.392(4) . ?
C14 H15 0.9500 . ?
C9 C10 1.415(4) . ?
C13 C12 1.404(4) . ?
C13 N7 1.408(4) . ?
C10 O6 1.338(4) . ?
C10 C11 1.402(5) . ?
C12 C11 1.374(5) . ?
C12 H11 0.9500 . ?
C11 H12 0.9500 . ?
O6 H4 0.79(2) . ?
N8 N7 1.267(4) . ?
N8 C16 1.405(4) . ?
C16 N12 1.331(4) . ?
C16 N9 1.335(4) . ?
N9 N10 1.339(4) . ?
N12 N11 1.334(4) . ?
N10 N11 1.318(4) . ?
O12 H21 0.804(19) . ?
O12 H20 0.815(19) . ?
O13 H23 0.852(19) . ?
O13 H22 0.838(19) . ?

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
O5 Dy1 O4 105.61(8) . . ?
O5 Dy1 O9 80.08(8) . . ?
O4 Dy1 O9 72.96(8) . . ?
O5 Dy1 O7 94.22(9) . . ?
O4 Dy1 O7 68.86(8) . . ?
O9 Dy1 O7 138.21(9) . . ?
O5 Dy1 O10 85.51(8) . . ?
O4 Dy1 O10 144.01(8) . . ?
O9 Dy1 O10 75.58(8) . . ?
O7 Dy1 O10 145.73(8) . . ?
O5 Dy1 O8 160.52(8) . . ?
O4 Dy1 O8 74.87(8) . . ?
O9 Dy1 O8 81.56(8) . . ?
O7 Dy1 O8 103.81(9) . . ?
O10 Dy1 O8 83.69(8) . . ?
O5 Dy1 O1 124.93(7) . . ?
O4 Dy1 O1 118.17(7) . . ?
O9 Dy1 O1 141.92(8) . . ?
O7 Dy1 O1 73.88(8) . . ?
O10 Dy1 O1 78.30(8) . . ?
O8 Dy1 O1 68.38(7) . . ?
O5 Dy1 O2 71.93(7) . . ?
O4 Dy1 O2 141.56(8) . . ?
O9 Dy1 O2 140.05(8) . . ?
O7 Dy1 O2 73.04(8) . . ?
O10 Dy1 O2 74.36(8) . . ?
O8 Dy1 O2 120.16(7) . . ?
O1 Dy1 O2 53.06(7) . . ?
O5 Dy1 C7 98.58(8) . . ?
O4 Dy1 C7 134.27(8) . . ?
O9 Dy1 C7 150.51(9) . . ?
O7 Dy1 C7 71.20(8) . . ?
O10 Dy1 C7 74.95(8) . . ?
O8 Dy1 C7 94.21(8) . . ?
O1 Dy1 C7 26.40(8) . . ?
O2 Dy1 C7 26.67(8) . . ?
Dy1 O8 H9 118(4) . . ?
Dy1 O8 H10 121(4) . . ?
H9 O8 H10 111(3) . . ?
C15 O4 Dy1 150.6(2) . . ?
C7 O1 Dy1 94.09(17) . . ?
H18 O11 H19 113(3) . . ?
Dy1 O10 H16 109(4) . . ?
Dy1 O10 H17 117(4) . . ?
H16 O10 H17 114(3) . . ?
Dy1 O9 H13 128(4) . . ?
Dy1 O9 H14 122(4) . . ?
H13 O9 H14 110(3) . . ?
C15 O5 Dy1 143.3(2) 2_655 . ?
Dy1 O7 H5 126(4) . . ?
Dy1 O7 H8 122(4) . . ?
H5 O7 H8 111(3) . . ?
C7 O2 Dy1 92.70(18) . . ?
O1 C7 O2 120.1(3) . . ?
O1 C7 C1 120.7(3) . . ?
O2 C7 C1 119.2(3) . . ?
O1 C7 Dy1 59.51(15) . . ?
O2 C7 Dy1 60.63(15) . . ?
C1 C7 Dy1 179.2(2) . . ?
C6 C1 C2 119.1(3) . . ?
C6 C1 C7 121.1(3) . . ?
C2 C1 C7 119.8(3) . . ?
C1 C6 C5 121.0(3) . . ?
C1 C6 H3 119.5 . . ?
C5 C6 H3 119.5 . . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H7 119.8 . . ?
C5 C4 H7 119.8 . . ?
O3 C2 C3 118.4(3) . . ?
O3 C2 C1 121.8(3) . . ?
C3 C2 C1 119.7(3) . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 N1 114.9(3) . . ?
C4 C5 N1 125.9(3) . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H6 119.7 . . ?
C2 C3 H6 119.7 . . ?
C2 O3 H2 109(4) . . ?
N1 N2 C8 112.8(3) . . ?
N2 N1 C5 115.8(3) . . ?
N6 C8 N3 111.8(3) . . ?
N6 C8 N2 127.5(3) . . ?
N3 C8 N2 120.6(3) . . ?
C8 N6 N5 104.9(2) . . ?
C8 N3 N4 104.8(3) . . ?
C8 N3 H1 127.6 . . ?
N4 N3 H1 127.6 . . ?
N4 N5 N6 109.5(2) . . ?
N5 N4 N3 109.0(2) . . ?
O4 C15 O5 123.9(3) . 2_655 ?
O4 C15 C9 118.8(3) . . ?
O5 C15 C9 117.3(3) 2_655 . ?
C9 C14 C13 121.8(3) . . ?
C9 C14 H15 119.1 . . ?
C13 C14 H15 119.1 . . ?
C14 C9 C10 119.2(3) . . ?
C14 C9 C15 118.8(3) . . ?
C10 C9 C15 122.0(3) . . ?
C14 C13 C12 118.5(3) . . ?
C14 C13 N7 125.8(3) . . ?
C12 C13 N7 115.8(3) . . ?
O6 C10 C11 118.0(3) . . ?
O6 C10 C9 123.0(3) . . ?
C11 C10 C9 119.0(3) . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H11 119.6 . . ?
C13 C12 H11 119.6 . . ?
C12 C11 C10 120.7(3) . . ?
C12 C11 H12 119.7 . . ?
C10 C11 H12 119.7 . . ?
C10 O6 H4 110(4) . . ?
N7 N8 C16 112.7(3) . . ?
N8 N7 C13 115.4(3) . . ?
N12 C16 N9 111.9(3) . . ?
N12 C16 N8 127.9(3) . . ?
N9 C16 N8 120.2(3) . . ?
C16 N9 N10 104.5(3) . . ?
C16 N12 N11 104.6(3) . . ?
N11 N10 N9 109.2(3) . . ?
N10 N11 N12 109.7(3) . . ?
H21 O12 H20 110(3) . . ?
H23 O13 H22 106(3) . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        27.09
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.106
_database_code_depnum_ccdc_archive 'CCDC 922442'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H46 N24 O26 Tb2'
_chemical_formula_weight         1500.79

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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6491(13)
_cell_length_b                   11.9680(17)
_cell_length_c                   12.9137(18)
_cell_angle_alpha                110.617(2)
_cell_angle_beta                 94.603(2)
_cell_angle_gamma                105.596(2)
_cell_volume                     1318.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5783
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      27.030

_exptl_crystal_description       block
_exptl_crystal_colour            light-orange
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744.0
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_T_max  0.473
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            11019
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         27.03
_reflns_number_total             5783
_reflns_number_gt                5183
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0241P)²+2.1988P] 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     SHELXL
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5783
_refine_ls_number_parameters     428
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0609
_refine_ls_wR_factor_gt          0.0567
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.155
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.007

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 0.529269(15) 0.802225(13) 0.382703(11) 0.01522(6) Uani 1 1 d . . .
O4 O 0.4804(2) 0.9579(2) 0.32952(17) 0.0193(4) Uani 1 1 d . . .
O9 O 0.3688(2) 0.6922(2) 0.20301(18) 0.0190(4) Uani 1 1 d D . .
O7 O 0.4172(3) 0.6151(2) 0.41046(18) 0.0224(5) Uani 1 1 d D . .
O1 O 0.6246(2) 0.64999(19) 0.24998(17) 0.0180(4) Uani 1 1 d . . .
O11 O 0.8032(3) 0.1657(2) 0.3725(2) 0.0266(5) Uani 1 1 d D . .
O5 O 0.6086(2) 0.8906(2) 0.57710(17) 0.0218(5) Uani 1 1 d . . .
O3 O 0.9319(2) 0.6511(2) 0.49190(18) 0.0244(5) Uani 1 1 d D . .
O8 O 0.7416(3) 0.9226(2) 0.3439(2) 0.0310(6) Uani 1 1 d D . .
O2 O 0.7326(2) 0.7264(2) 0.42780(17) 0.0209(4) Uani 1 1 d . . .
O10 O 0.3092(3) 0.8279(3) 0.44122(19) 0.0272(5) Uani 1 1 d D . .
O12 O 0.3202(3) 0.4435(2) 0.0954(2) 0.0276(5) Uani 1 1 d D . .
C7 C 0.7215(3) 0.6566(3) 0.3253(2) 0.0156(5) Uani 1 1 d . . .
C6 C 0.8228(3) 0.5106(3) 0.1844(2) 0.0167(6) Uani 1 1 d . . .
H3 H 0.7538 0.5077 0.1259 0.020 Uiso 1 1 calc R . .
C1 C 0.8245(3) 0.5822(3) 0.2958(2) 0.0155(5) Uani 1 1 d . . .
C2 C 0.9269(3) 0.5850(3) 0.3818(2) 0.0190(6) Uani 1 1 d . . .
C5 C 0.9208(3) 0.4429(3) 0.1572(2) 0.0173(6) Uani 1 1 d . . .
C3 C 1.0239(3) 0.5155(3) 0.3546(3) 0.0219(6) Uani 1 1 d . . .
H6 H 1.0923 0.5172 0.4128 0.026 Uiso 1 1 calc R . .
C4 C 1.0202(4) 0.4447(3) 0.2437(3) 0.0235(6) Uani 1 1 d . . .
H7 H 1.0853 0.3967 0.2256 0.028 Uiso 1 1 calc R . .
N2 N 1.0069(3) 0.3262(2) 0.0134(2) 0.0188(5) Uani 1 1 d . . .
N1 N 0.9067(3) 0.3750(2) 0.0404(2) 0.0187(5) Uani 1 1 d . . .
C8 C 0.9865(3) 0.2602(3) -0.1038(2) 0.0165(6) Uani 1 1 d . . .
N3 N 1.0807(3) 0.2018(2) -0.1473(2) 0.0201(5) Uani 1 1 d . . .
H1 H 1.1586 0.1971 -0.1109 0.024 Uiso 1 1 calc R . .
N6 N 0.8807(3) 0.2487(2) -0.1838(2) 0.0178(5) Uani 1 1 d . . .
N5 N 0.9115(3) 0.1807(2) -0.2804(2) 0.0189(5) Uani 1 1 d . . .
N4 N 1.0306(3) 0.1519(2) -0.2590(2) 0.0206(5) Uani 1 1 d . . .
C15 C 0.5921(3) 0.9692(3) 0.6679(2) 0.0153(5) Uani 1 1 d . . .
C14 C 0.6355(3) 1.0490(3) 0.8767(2) 0.0169(6) Uani 1 1 d . . .
H11 H 0.5724 1.0971 0.8741 0.020 Uiso 1 1 calc R . .
C10 C 0.7568(3) 0.9013(3) 0.7809(3) 0.0191(6) Uani 1 1 d . . .
C9 C 0.6620(3) 0.9718(3) 0.7763(2) 0.0163(6) Uani 1 1 d . . .
C11 C 0.8214(3) 0.9100(3) 0.8859(3) 0.0233(6) Uani 1 1 d . . .
H14 H 0.8854 0.8629 0.8894 0.028 Uiso 1 1 calc R . .
C13 C 0.6993(3) 1.0574(3) 0.9806(2) 0.0173(6) Uani 1 1 d . . .
C12 C 0.7925(3) 0.9864(3) 0.9838(3) 0.0217(6) Uani 1 1 d . . .
H13 H 0.8363 0.9910 1.0544 0.026 Uiso 1 1 calc R . .
N8 N 0.5919(3) 1.1951(2) 1.0823(2) 0.0188(5) Uani 1 1 d . . .
N7 N 0.6798(3) 1.1342(2) 1.0864(2) 0.0199(5) Uani 1 1 d . . .
O6 O 0.7890(3) 0.8252(2) 0.68827(19) 0.0274(5) Uani 1 1 d D . .
C16 C 0.5776(3) 1.2705(3) 1.1906(2) 0.0176(6) Uani 1 1 d . . .
N9 N 0.4946(3) 1.3456(2) 1.2012(2) 0.0215(5) Uani 1 1 d . . .
N12 N 0.6387(3) 1.2778(2) 1.2897(2) 0.0206(5) Uani 1 1 d . . .
N10 N 0.5052(3) 1.4016(2) 1.3127(2) 0.0231(5) Uani 1 1 d . . .
N11 N 0.5915(3) 1.3612(3) 1.3653(2) 0.0245(6) Uani 1 1 d . . .
O13 O 0.4015(4) 0.2590(3) 0.9260(3) 0.0484(7) Uani 1 1 d D . .
H8 H 0.812(4) 0.902(5) 0.330(5) 0.073 Uiso 1 1 d D . .
H9 H 0.748(6) 0.991(3) 0.346(5) 0.073 Uiso 1 1 d D . .
H4 H 0.404(6) 0.623(5) 0.473(2) 0.073 Uiso 1 1 d D . .
H5 H 0.443(6) 0.555(4) 0.381(4) 0.073 Uiso 1 1 d D . .
H16 H 0.249(5) 0.835(5) 0.400(3) 0.073 Uiso 1 1 d D . .
H15 H 0.298(4) 0.711(4) 0.188(5) 0.073 Uiso 1 1 d D . .
H19 H 0.759(5) 0.194(5) 0.337(4) 0.073 Uiso 1 1 d D . .
H21 H 0.234(2) 0.403(4) 0.080(5) 0.073 Uiso 1 1 d D . .
H18 H 0.884(3) 0.213(4) 0.400(4) 0.073 Uiso 1 1 d D . .
H20 H 0.368(4) 0.414(5) 0.125(4) 0.073 Uiso 1 1 d D . .
H17 H 0.280(5) 0.821(5) 0.496(3) 0.073 Uiso 1 1 d D . .
H10 H 0.748(6) 0.835(5) 0.638(3) 0.073 Uiso 1 1 d D . .
H2 H 0.877(5) 0.691(5) 0.495(5) 0.073 Uiso 1 1 d D . .
H12 H 0.354(5) 0.618(2) 0.173(4) 0.073 Uiso 1 1 d D . .
H22 H 0.463(5) 0.279(5) 0.887(4) 0.073 Uiso 1 1 d D . .
H23 H 0.441(5) 0.227(5) 0.963(4) 0.073 Uiso 1 1 d 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 O5 2.322(2) . ?
Tb1 O4 2.343(2) . ?
Tb1 O8 2.369(2) . ?
Tb1 O10 2.371(2) . ?
Tb1 O7 2.374(2) . ?
Tb1 O9 2.386(2) . ?
Tb1 O1 2.461(2) . ?
Tb1 O2 2.481(2) . ?
O4 C15 1.249(4) 2_676 ?
O9 H15 0.802(19) . ?
O9 H12 0.800(19) . ?
O7 H4 0.798(19) . ?
O7 H5 0.801(19) . ?
O1 C7 1.260(4) . ?
O11 H19 0.810(19) . ?
O11 H18 0.798(19) . ?
O5 C15 1.273(3) . ?
O3 C2 1.351(4) . ?
O3 H2 0.80(2) . ?
O8 H8 0.797(19) . ?
O8 H9 0.789(19) . ?
O2 C7 1.270(3) . ?
O10 H16 0.804(19) . ?
O10 H17 0.799(19) . ?
O12 H21 0.811(19) . ?
O12 H20 0.800(19) . ?
C7 C1 1.490(4) . ?
C6 C1 1.387(4) . ?
C6 C5 1.393(4) . ?
C6 H3 0.9500 . ?
C1 C2 1.411(4) . ?
C2 C3 1.399(4) . ?
C5 C4 1.403(4) . ?
C5 N1 1.414(4) . ?
C3 C4 1.375(4) . ?
C3 H6 0.9500 . ?
C4 H7 0.9500 . ?
N2 N1 1.269(3) . ?
N2 C8 1.408(4) . ?
C8 N3 1.333(4) . ?
C8 N6 1.335(4) . ?
N3 N4 1.340(4) . ?
N3 H1 0.8800 . ?
N6 N5 1.335(3) . ?
N5 N4 1.321(3) . ?
C15 O4 1.249(3) 2_676 ?
C15 C9 1.490(4) . ?
C14 C13 1.389(4) . ?
C14 C9 1.392(4) . ?
C14 H11 0.9500 . ?
C10 O6 1.341(4) . ?
C10 C11 1.403(4) . ?
C10 C9 1.413(4) . ?
C11 C12 1.375(4) . ?
C11 H14 0.9500 . ?
C13 C12 1.401(4) . ?
C13 N7 1.414(4) . ?
C12 H13 0.9500 . ?
N8 N7 1.267(4) . ?
N8 C16 1.413(4) . ?
O6 H10 0.80(2) . ?
C16 N12 1.330(4) . ?
C16 N9 1.336(4) . ?
N9 N10 1.339(4) . ?
N12 N11 1.337(4) . ?
N10 N11 1.320(4) . ?
O13 H22 0.845(19) . ?
O13 H23 0.838(19) . ?

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
O5 Tb1 O4 107.31(7) . . ?
O5 Tb1 O8 95.36(9) . . ?
O4 Tb1 O8 68.96(8) . . ?
O5 Tb1 O10 79.91(8) . . ?
O4 Tb1 O10 72.73(8) . . ?
O8 Tb1 O10 137.96(9) . . ?
O5 Tb1 O7 84.65(8) . . ?
O4 Tb1 O7 143.55(8) . . ?
O8 Tb1 O7 145.76(8) . . ?
O10 Tb1 O7 75.89(8) . . ?
O5 Tb1 O9 160.11(8) . . ?
O4 Tb1 O9 74.32(7) . . ?
O8 Tb1 O9 103.47(9) . . ?
O10 Tb1 O9 81.81(8) . . ?
O7 Tb1 O9 83.36(8) . . ?
O5 Tb1 O1 124.56(7) . . ?
O4 Tb1 O1 117.62(7) . . ?
O8 Tb1 O1 73.75(8) . . ?
O10 Tb1 O1 142.07(8) . . ?
O7 Tb1 O1 78.16(7) . . ?
O9 Tb1 O1 68.06(7) . . ?
O5 Tb1 O2 71.92(7) . . ?
O4 Tb1 O2 142.06(8) . . ?
O8 Tb1 O2 73.32(8) . . ?
O10 Tb1 O2 140.32(8) . . ?
O7 Tb1 O2 74.21(8) . . ?
O9 Tb1 O2 119.47(7) . . ?
O1 Tb1 O2 52.74(7) . . ?
C15 O4 Tb1 150.35(19) 2_676 . ?
Tb1 O9 H15 122(4) . . ?
Tb1 O9 H12 117(4) . . ?
H15 O9 H12 111(3) . . ?
Tb1 O7 H4 117(4) . . ?
Tb1 O7 H5 118(4) . . ?
H4 O7 H5 112(3) . . ?
C7 O1 Tb1 94.01(17) . . ?
H19 O11 H18 110(3) . . ?
C15 O5 Tb1 142.95(19) . . ?
C2 O3 H2 108(4) . . ?
Tb1 O8 H8 126(4) . . ?
Tb1 O8 H9 120(4) . . ?
H8 O8 H9 114(3) . . ?
C7 O2 Tb1 92.83(17) . . ?
Tb1 O10 H16 119(4) . . ?
Tb1 O10 H17 128(4) . . ?
H16 O10 H17 112(3) . . ?
H21 O12 H20 111(3) . . ?
O1 C7 O2 120.4(3) . . ?
O1 C7 C1 120.7(3) . . ?
O2 C7 C1 118.9(3) . . ?
C1 C6 C5 120.8(3) . . ?
C1 C6 H3 119.6 . . ?
C5 C6 H3 119.6 . . ?
C6 C1 C2 118.9(3) . . ?
C6 C1 C7 121.1(3) . . ?
C2 C1 C7 119.9(3) . . ?
O3 C2 C3 118.1(3) . . ?
O3 C2 C1 121.6(3) . . ?
C3 C2 C1 120.2(3) . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 N1 114.5(3) . . ?
C4 C5 N1 125.9(3) . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H6 120.0 . . ?
C2 C3 H6 120.0 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H7 119.8 . . ?
C5 C4 H7 119.8 . . ?
N1 N2 C8 112.3(2) . . ?
N2 N1 C5 115.1(2) . . ?
N3 C8 N6 111.8(3) . . ?
N3 C8 N2 120.5(3) . . ?
N6 C8 N2 127.6(3) . . ?
C8 N3 N4 104.7(2) . . ?
C8 N3 H1 127.7 . . ?
N4 N3 H1 127.7 . . ?
C8 N6 N5 104.7(2) . . ?
N4 N5 N6 109.6(2) . . ?
N5 N4 N3 109.2(2) . . ?
O4 C15 O5 123.7(3) 2_676 . ?
O4 C15 C9 119.0(2) 2_676 . ?
O5 C15 C9 117.3(3) . . ?
C13 C14 C9 121.5(3) . . ?
C13 C14 H11 119.2 . . ?
C9 C14 H11 119.2 . . ?
O6 C10 C11 117.7(3) . . ?
O6 C10 C9 122.8(3) . . ?
C11 C10 C9 119.5(3) . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 C15 118.7(3) . . ?
C10 C9 C15 122.4(3) . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H14 119.8 . . ?
C10 C11 H14 119.8 . . ?
C14 C13 C12 118.9(3) . . ?
C14 C13 N7 125.3(3) . . ?
C12 C13 N7 115.8(3) . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H13 119.6 . . ?
C13 C12 H13 119.6 . . ?
N7 N8 C16 112.5(2) . . ?
N8 N7 C13 115.2(2) . . ?
C10 O6 H10 104(4) . . ?
N12 C16 N9 112.3(3) . . ?
N12 C16 N8 127.6(3) . . ?
N9 C16 N8 120.1(3) . . ?
C16 N9 N10 104.3(2) . . ?
C16 N12 N11 104.4(3) . . ?
N11 N10 N9 109.3(2) . . ?
N10 N11 N12 109.7(2) . . ?
H22 O13 H23 105(3) . . ?

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.03
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.107
_database_code_depnum_ccdc_archive 'CCDC 922443'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H46 Gd2 N24 O26'
_chemical_formula_weight         1497.43

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.76740(10)
_cell_length_b                   11.8082(2)
_cell_length_c                   12.5681(2)
_cell_angle_alpha                109.4910(10)
_cell_angle_beta                 94.4350(10)
_cell_angle_gamma                104.6290(10)
_cell_volume                     1301.27(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5842
_cell_measurement_theta_min      1.75
_cell_measurement_theta_max      26.00

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             742.0
_exptl_absorpt_coefficient_mu    2.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            19222
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5122
_reflns_number_gt                4607
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0290P)²+2.8098P] 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     SHELXL
_refine_ls_extinction_coef       0.0013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5122
_refine_ls_number_parameters     406
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.101
_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
Gd1 Gd 0.53877(2) 0.79753(2) 0.865487(18) 0.04415(10) Uani 1 1 d U . 2
O1 O 0.6346(3) 0.6410(3) 0.7400(2) 0.0389(6) Uani 1 1 d . A 2
O2 O 0.7420(3) 0.7185(3) 0.9190(2) 0.0448(7) Uani 1 1 d . A 2
O3 O 0.9488(4) 0.6491(4) 0.9827(3) 0.0596(9) Uani 1 1 d . A 2
H1 H 0.8865 0.6851 0.9890 0.089 Uiso 1 1 calc R A 2
O4 O 0.4902(4) 0.9736(4) 0.8417(3) 0.0641(10) Uani 1 1 d . B 2
O5 O 0.3875(3) 1.1146(3) 0.9350(2) 0.0433(7) Uani 1 1 d . . 2
O6 O 0.2051(4) 1.1799(3) 0.8237(3) 0.0510(8) Uani 1 1 d . B 2
H2 H 0.2550 1.1831 0.8808 0.077 Uiso 1 1 calc R B 2
O10 O 0.4310(3) 0.6128(3) 0.9049(3) 0.0533(8) Uani 1 1 d . C 2
H16 H 0.4235 0.6219 0.9740 0.064 Uiso 1 1 d R C 2
H17 H 0.4540 0.5458 0.8746 0.064 Uiso 1 1 d R C 2
O7 O 0.3656(3) 0.6920(3) 0.6957(2) 0.0462(7) Uani 1 1 d . D 2
H5 H 0.3705 0.7240 0.6482 0.055 Uiso 1 1 d R D 2
H7 H 0.3488 0.6133 0.6612 0.055 Uiso 1 1 d R D 2
O11 O 0.3205(3) 0.8178(4) 0.9414(3) 0.0618(9) Uani 1 1 d . E 2
H18 H 0.2585 0.8217 0.8924 0.074 Uiso 1 1 d R E 2
H19 H 0.2883 0.7550 0.9607 0.074 Uiso 1 1 d R E 2
O9 O 0.7712(5) 0.9476(4) 0.8893(6) 0.141(2) Uani 1 1 d U F 2
H13 H 0.8320 0.9143 0.8568 0.169 Uiso 1 1 d R F 2
H15 H 0.7802 1.0164 0.8788 0.169 Uiso 1 1 d R F 2
N1 N 0.9151(3) 0.3671(3) 0.5254(3) 0.0391(8) Uani 1 1 d . A 2
N2 N 1.0076(4) 0.3112(3) 0.4978(3) 0.0392(8) Uani 1 1 d . A 2
N3 N 0.8821(3) 0.2386(3) 0.3000(3) 0.0402(8) Uani 1 1 d . A 2
H9 H 0.8133 0.2722 0.3107 0.048 Uiso 1 1 calc R A 2
N4 N 0.9074(4) 0.1682(3) 0.2007(3) 0.0427(8) Uani 1 1 d . A 2
N5 N 1.0223(4) 0.1349(3) 0.2201(3) 0.0433(8) Uani 1 1 d . A 2
N6 N 1.0739(4) 0.1829(3) 0.3325(3) 0.0415(8) Uani 1 1 d . A 2
N7 N 0.3146(4) 0.8738(3) 0.4193(3) 0.0446(8) Uani 1 1 d . B 2
N8 N 0.4004(4) 0.8119(3) 0.4248(3) 0.0433(8) Uani 1 1 d . B 2
N9 N 0.3554(5) 0.7273(4) 0.2143(3) 0.0582(11) Uani 1 1 d . B 2
N10 N 0.4067(6) 0.6442(4) 0.1388(3) 0.0664(13) Uani 1 1 d . B 2
N11 N 0.4937(5) 0.6067(4) 0.1947(4) 0.0620(12) Uani 1 1 d . B 2
N12 N 0.5022(4) 0.6641(4) 0.3075(3) 0.0534(10) Uani 1 1 d . B 2
C1 C 0.8346(4) 0.5739(3) 0.7857(3) 0.0317(8) Uani 1 1 d . A 2
C2 C 0.9400(5) 0.5796(4) 0.8709(3) 0.0411(9) Uani 1 1 d . A 2
C3 C 1.0394(5) 0.5136(5) 0.8424(4) 0.0517(11) Uani 1 1 d . A 2
H3 H 1.1089 0.5177 0.8995 0.062 Uiso 1 1 calc R A 2
C4 C 1.0354(5) 0.4424(4) 0.7304(4) 0.0481(11) Uani 1 1 d . A 2
H4 H 1.1022 0.3984 0.7115 0.058 Uiso 1 1 calc R A 2
C5 C 0.9307(4) 0.4361(4) 0.6443(3) 0.0361(8) Uani 1 1 d . A 2
C6 C 0.8318(4) 0.5014(3) 0.6727(3) 0.0336(8) Uani 1 1 d . A 2
H6 H 0.7623 0.4968 0.6152 0.040 Uiso 1 1 calc R A 2
C7 C 0.7308(4) 0.6470(4) 0.8153(3) 0.0337(8) Uani 1 1 d . A 2
C8 C 0.9852(4) 0.2460(4) 0.3787(3) 0.0337(8) Uani 1 1 d . A 2
C9 C 0.3356(4) 1.0360(3) 0.7333(3) 0.0323(8) Uani 1 1 d . B 2
C10 C 0.2383(4) 1.1054(4) 0.7295(4) 0.0376(9) Uani 1 1 d . B 2
C11 C 0.1725(5) 1.0971(4) 0.6241(4) 0.0458(10) Uani 1 1 d . B 2
H11 H 0.1091 1.1435 0.6211 0.055 Uiso 1 1 calc R B 2
C12 C 0.2004(4) 1.0208(4) 0.5241(4) 0.0440(10) Uani 1 1 d . B 2
H12 H 0.1558 1.0161 0.4540 0.053 Uiso 1 1 calc R B 2
C13 C 0.2940(4) 0.9509(4) 0.5263(3) 0.0380(9) Uani 1 1 d . B 2
C14 C 0.3610(4) 0.9593(4) 0.6312(3) 0.0358(8) Uani 1 1 d . B 2
H14 H 0.4242 0.9125 0.6330 0.043 Uiso 1 1 calc R B 2
C15 C 0.4096(4) 1.0405(4) 0.8433(3) 0.0369(9) Uani 1 1 d . B 2
C16 C 0.4172(5) 0.7368(4) 0.3160(4) 0.0443(10) Uani 1 1 d . B 2
O13 O 0.6721(7) 0.5689(7) 0.4195(6) 0.068(2) Uani 0.50 1 d PD G 1
H22 H 0.6430 0.6167 0.4006 0.082 Uiso 0.50 1 d PRD G 1
H25 H 0.7426 0.5572 0.3951 0.082 Uiso 0.50 1 d PRD G 1
O14 O 0.5483(8) 0.4887(8) 0.4636(6) 0.089(3) Uani 0.50 1 d PD . 2
H23 H 0.5050 0.4877 0.4096 0.107 Uiso 0.50 1 d PRD . 2
H24 H 0.5549 0.4221 0.4627 0.107 Uiso 0.50 1 d PRD . 2
O16 O 0.2032(8) 0.8354(5) 0.1341(6) 0.076(2) Uani 0.50 1 d PD H 1
H26 H 0.2542 0.8038 0.1598 0.091 Uiso 0.50 1 d PRD H 1
H27 H 0.1242 0.7861 0.1051 0.091 Uiso 0.50 1 d PRD H 1
O12 O 0.1340(8) 0.8477(5) 0.1841(6) 0.087(3) Uani 0.50 1 d PRU H 2
H20 H 0.2004 0.8174 0.1938 0.104 Uiso 0.50 1 d PR H 2
H21 H 0.0629 0.7936 0.1352 0.104 Uiso 0.50 1 d PR H 2
O8 O 0.6542(6) 0.8524(6) 0.6876(5) 0.0476(14) Uani 0.50 1 d PU I 1
H8 H 0.7301 0.8288 0.6730 0.057 Uiso 0.50 1 d PR I 1
H10 H 0.5891 0.8041 0.6261 0.057 Uiso 0.50 1 d PR I 1
O15 O 0.6361(10) 0.7460(11) 0.5564(8) 0.102(3) Uani 0.50 1 d P J 2
H28 H 0.6703 0.6917 0.5706 0.123 Uiso 0.50 1 d PR J 2
H29 H 0.5427 0.7327 0.5300 0.123 Uiso 0.50 1 d PR J 2


_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
Gd1 O5 2.343(3) 2_677 ?
Gd1 O4 2.351(3) . ?
Gd1 O7 2.360(3) . ?
Gd1 O10 2.399(3) . ?
Gd1 O9 2.428(5) . ?
Gd1 O11 2.436(3) . ?
Gd1 O1 2.437(3) . ?
Gd1 O2 2.533(3) . ?
Gd1 C7 2.862(4) . ?
O1 C7 1.251(5) . ?
O2 C7 1.273(4) . ?
O3 C2 1.354(5) . ?
O3 H1 0.8200 . ?
O4 C15 1.245(5) . ?
O5 C15 1.265(5) . ?
O5 Gd1 2.343(3) 2_677 ?
O6 C10 1.337(5) . ?
O6 H2 0.8200 . ?
O10 H16 0.8500 . ?
O10 H17 0.8500 . ?
O7 H5 0.8044 . ?
O7 H7 0.8500 . ?
O11 H18 0.8500 . ?
O11 H19 0.8500 . ?
O9 H13 0.8500 . ?
O9 H15 0.8499 . ?
N1 N2 1.252(4) . ?
N1 C5 1.418(5) . ?
N2 C8 1.405(5) . ?
N3 C8 1.321(5) . ?
N3 N4 1.330(5) . ?
N3 H9 0.8600 . ?
N4 N5 1.312(5) . ?
N5 N6 1.335(5) . ?
N6 C8 1.327(5) . ?
N7 N8 1.255(5) . ?
N7 C13 1.412(5) . ?
N8 C16 1.408(5) . ?
N9 C16 1.327(6) . ?
N9 N10 1.347(6) . ?
N10 N11 1.310(7) . ?
N11 N12 1.336(5) . ?
N12 C16 1.324(6) . ?
C1 C6 1.387(5) . ?
C1 C2 1.398(6) . ?
C1 C7 1.483(5) . ?
C2 C3 1.389(6) . ?
C3 C4 1.369(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.399(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.379(5) . ?
C6 H6 0.9300 . ?
C9 C14 1.384(5) . ?
C9 C10 1.410(5) . ?
C9 C15 1.489(5) . ?
C10 C11 1.389(6) . ?
C11 C12 1.374(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.382(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.387(6) . ?
C14 H14 0.9300 . ?
O13 H22 0.7850 . ?
O13 H25 0.8002 . ?
O14 O14 1.378(15) 2_666 ?
O14 H23 0.7666 . ?
O14 H24 0.8011 . ?
O16 H26 0.8006 . ?
O16 H27 0.8093 . ?
O16 H20 0.8463 . ?
O16 H21 1.3370 . ?
O12 H26 1.4132 . ?
O12 H27 0.9971 . ?
O12 H20 0.8351 . ?
O12 H21 0.8464 . ?
O8 H8 0.8670 . ?
O8 H10 0.8792 . ?
O15 H10 1.1270 . ?
O15 H28 0.8536 . ?
O15 H29 0.9017 . ?

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
O5 Gd1 O4 97.45(11) 2_677 . ?
O5 Gd1 O7 153.85(10) 2_677 . ?
O4 Gd1 O7 81.42(12) . . ?
O5 Gd1 O10 82.60(11) 2_677 . ?
O4 Gd1 O10 142.27(12) . . ?
O7 Gd1 O10 82.68(11) . . ?
O5 Gd1 O9 77.16(18) 2_677 . ?
O4 Gd1 O9 74.03(15) . . ?
O7 Gd1 O9 126.60(19) . . ?
O10 Gd1 O9 140.95(16) . . ?
O5 Gd1 O11 75.28(10) 2_677 . ?
O4 Gd1 O11 72.51(13) . . ?
O7 Gd1 O11 79.54(10) . . ?
O10 Gd1 O11 71.06(12) . . ?
O9 Gd1 O11 132.82(14) . . ?
O5 Gd1 O1 123.01(9) 2_677 . ?
O4 Gd1 O1 129.64(10) . . ?
O7 Gd1 O1 74.19(9) . . ?
O10 Gd1 O1 77.31(10) . . ?
O9 Gd1 O1 86.22(13) . . ?
O11 Gd1 O1 140.96(11) . . ?
O5 Gd1 O2 71.11(9) 2_677 . ?
O4 Gd1 O2 142.55(13) . . ?
O7 Gd1 O2 124.36(9) . . ?
O10 Gd1 O2 73.27(10) . . ?
O9 Gd1 O2 68.70(14) . . ?
O11 Gd1 O2 133.30(11) . . ?
O1 Gd1 O2 52.13(9) . . ?
O5 Gd1 C7 97.45(10) 2_677 . ?
O4 Gd1 C7 142.13(12) . . ?
O7 Gd1 C7 99.21(10) . . ?
O10 Gd1 C7 74.26(11) . . ?
O9 Gd1 C7 75.68(12) . . ?
O11 Gd1 C7 145.19(12) . . ?
O1 Gd1 C7 25.75(10) . . ?
O2 Gd1 C7 26.40(10) . . ?
C7 O1 Gd1 96.5(2) . . ?
C7 O2 Gd1 91.4(2) . . ?
C2 O3 H1 109.5 . . ?
C15 O4 Gd1 151.2(3) . . ?
C15 O5 Gd1 143.6(3) . 2_677 ?
C10 O6 H2 109.5 . . ?
Gd1 O10 H16 117.7 . . ?
Gd1 O10 H17 120.2 . . ?
H16 O10 H17 108.4 . . ?
Gd1 O7 H5 116.6 . . ?
Gd1 O7 H7 119.4 . . ?
H5 O7 H7 107.9 . . ?
Gd1 O11 H18 111.4 . . ?
Gd1 O11 H19 107.5 . . ?
H18 O11 H19 111.4 . . ?
Gd1 O9 H13 113.6 . . ?
Gd1 O9 H15 122.6 . . ?
H13 O9 H15 108.1 . . ?
N2 N1 C5 115.2(3) . . ?
N1 N2 C8 111.6(3) . . ?
C8 N3 N4 105.3(3) . . ?
C8 N3 H9 127.3 . . ?
N4 N3 H9 127.3 . . ?
N5 N4 N3 109.0(3) . . ?
N4 N5 N6 109.4(3) . . ?
C8 N6 N5 104.6(3) . . ?
N8 N7 C13 115.1(4) . . ?
N7 N8 C16 112.7(4) . . ?
C16 N9 N10 104.1(4) . . ?
N11 N10 N9 109.4(4) . . ?
N10 N11 N12 109.5(4) . . ?
C16 N12 N11 104.7(4) . . ?
C6 C1 C2 118.7(3) . . ?
C6 C1 C7 120.6(3) . . ?
C2 C1 C7 120.7(3) . . ?
O3 C2 C3 118.1(4) . . ?
O3 C2 C1 121.5(4) . . ?
C3 C2 C1 120.4(4) . . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.9(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 N1 114.4(4) . . ?
C4 C5 N1 125.7(4) . . ?
C5 C6 C1 120.9(4) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O1 C7 O2 119.9(3) . . ?
O1 C7 C1 121.2(3) . . ?
O2 C7 C1 118.9(3) . . ?
O1 C7 Gd1 57.77(18) . . ?
O2 C7 Gd1 62.2(2) . . ?
C1 C7 Gd1 176.6(3) . . ?
N3 C8 N6 111.6(3) . . ?
N3 C8 N2 127.7(3) . . ?
N6 C8 N2 120.7(4) . . ?
C14 C9 C10 119.0(4) . . ?
C14 C9 C15 118.8(3) . . ?
C10 C9 C15 122.2(3) . . ?
O6 C10 C11 117.5(4) . . ?
O6 C10 C9 123.0(4) . . ?
C11 C10 C9 119.5(4) . . ?
C12 C11 C10 120.3(4) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 N7 116.9(4) . . ?
C14 C13 N7 123.9(4) . . ?
C9 C14 C13 121.1(4) . . ?
C9 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
O4 C15 O5 123.2(4) . . ?
O4 C15 C9 119.6(3) . . ?
O5 C15 C9 117.2(3) . . ?
N12 C16 N9 112.4(4) . . ?
N12 C16 N8 120.0(4) . . ?
N9 C16 N8 127.7(4) . . ?
H22 O13 H25 114.2 . . ?
O14 O14 H23 98.5 2_666 . ?
O14 O14 H24 102.5 2_666 . ?
H23 O14 H24 116.0 . . ?
H26 O16 H27 111.1 . . ?
H26 O16 H20 51.7 . . ?
H27 O16 H20 90.9 . . ?
H26 O16 H21 116.2 . . ?
H27 O16 H21 29.0 . . ?
H20 O16 H21 75.7 . . ?
H26 O12 H27 64.2 . . ?
H26 O12 H20 22.7 . . ?
H27 O12 H20 79.6 . . ?
H26 O12 H21 106.0 . . ?
H27 O12 H21 46.6 . . ?
H20 O12 H21 112.0 . . ?
H8 O8 H10 103.6 . . ?
H10 O15 H28 117.1 . . ?
H10 O15 H29 70.9 . . ?
H28 O15 H29 124.7 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.733
_refine_diff_density_rms         0.082
_database_code_depnum_ccdc_archive 'CCDC 922444'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H46 N24 O26 Sm2'
_chemical_formula_weight         1483.65

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6865(12)
_cell_length_b                   11.7997(14)
_cell_length_c                   13.1112(16)
_cell_angle_alpha                111.997(2)
_cell_angle_beta                 95.839(2)
_cell_angle_gamma                104.792(2)
_cell_volume                     1310.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5577
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      27.070

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             738.0
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.425
_exptl_absorpt_correction_T_max  0.546
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            10980
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         27.07
_reflns_number_total             5770
_reflns_number_gt                5071
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0418P)²+0.7549P] 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     SHELXL
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5770
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0236
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0667
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_restrained_S_all      1.194
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.012

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
Sm1 Sm 0.943845(16) 0.161113(14) 0.602172(12) 0.01199(7) Uani 1 1 d . . .
O7 O 1.1606(2) 0.0988(2) 0.53402(18) 0.0161(5) Uani 1 1 d . . .
O4 O 1.0169(2) 0.0318(2) 0.68794(18) 0.0155(4) Uani 1 1 d . . .
O10 O 1.1196(2) 0.2954(2) 0.78310(19) 0.0186(5) Uani 1 1 d . . .
O5 O 0.8842(3) 0.1163(2) 0.40550(18) 0.0175(5) Uani 1 1 d . . .
O9 O 1.0726(3) 0.3560(2) 0.58250(19) 0.0188(5) Uani 1 1 d . . .
O8 O 0.7448(3) 0.0621(2) 0.6701(2) 0.0253(6) Uani 1 1 d . . .
O13 O 0.2862(3) 0.1853(2) 0.3950(2) 0.0212(5) Uani 1 1 d . . .
O12 O 0.1794(3) 0.5535(2) 0.9104(2) 0.0258(5) Uani 1 1 d . . .
N7 N 1.1806(3) 0.1397(3) 1.1014(2) 0.0176(6) Uani 1 1 d . . .
C15 C 1.0942(3) -0.0392(3) 0.6852(3) 0.0127(6) Uani 1 1 d . . .
C14 C 1.1400(3) 0.0476(3) 0.8921(3) 0.0157(6) Uani 1 1 d . . .
H14 H 1.0776 0.0969 0.8880 0.019 Uiso 1 1 calc R . .
C9 C 1.1659(3) -0.0333(3) 0.7939(3) 0.0142(6) Uani 1 1 d . . .
N8 N 1.0962(3) 0.2028(3) 1.0925(2) 0.0167(5) Uani 1 1 d . . .
N12 N 1.1282(3) 0.2900(3) 1.2992(2) 0.0192(6) Uani 1 1 d . . .
C16 C 1.0765(3) 0.2813(3) 1.1973(3) 0.0153(6) Uani 1 1 d . . .
C13 C 1.2034(3) 0.0590(3) 0.9976(3) 0.0159(6) Uani 1 1 d . . .
C12 C 1.2947(4) -0.0137(3) 1.0030(3) 0.0186(7) Uani 1 1 d . . .
H12 H 1.3381 -0.0073 1.0741 0.022 Uiso 1 1 calc R . .
O11 O 0.9078(4) 0.2541(3) 0.9205(3) 0.0441(8) Uani 1 1 d . . .
C11 C 1.3224(4) -0.0950(3) 0.9057(3) 0.0190(7) Uani 1 1 d . . .
H11 H 1.3840 -0.1447 0.9103 0.023 Uiso 1 1 calc R . .
N9 N 0.9940(3) 0.3578(3) 1.2027(2) 0.0193(6) Uani 1 1 d . . .
N11 N 1.0772(3) 0.3762(3) 1.3705(2) 0.0226(6) Uani 1 1 d . . .
N10 N 0.9971(3) 0.4168(3) 1.3127(2) 0.0217(6) Uani 1 1 d . . .
C10 C 1.2603(4) -0.1048(3) 0.7999(3) 0.0169(6) Uani 1 1 d . . .
O6 O 1.2922(3) -0.1833(2) 0.7082(2) 0.0248(5) Uani 1 1 d . . .
H5 H 1.2471 -0.1825 0.6504 0.037 Uiso 1 1 calc R . .
O1 O 0.8628(2) 0.3311(2) 0.74177(18) 0.0164(5) Uani 1 1 d . . .
O2 O 0.7434(2) 0.2509(2) 0.56527(19) 0.0185(5) Uani 1 1 d . . .
O3 O 0.5622(3) 0.3486(2) 0.50830(19) 0.0214(5) Uani 1 1 d . . .
H4 H 0.6215 0.3066 0.5002 0.032 Uiso 1 1 calc R . .
C7 C 0.7648(3) 0.3270(3) 0.6693(3) 0.0146(6) Uani 1 1 d . . .
C6 C 0.6758(3) 0.4814(3) 0.8150(3) 0.0147(6) Uani 1 1 d . . .
H6 H 0.7444 0.4806 0.8718 0.018 Uiso 1 1 calc R . .
C1 C 0.6692(3) 0.4091(3) 0.7021(3) 0.0140(6) Uani 1 1 d . . .
C5 C 0.5822(3) 0.5554(3) 0.8459(3) 0.0153(6) Uani 1 1 d . . .
C2 C 0.5708(3) 0.4145(3) 0.6193(3) 0.0160(6) Uani 1 1 d . . .
C4 C 0.4852(4) 0.5600(3) 0.7616(3) 0.0219(7) Uani 1 1 d . . .
H2 H 0.4231 0.6116 0.7822 0.026 Uiso 1 1 calc R . .
C3 C 0.4790(4) 0.4908(3) 0.6500(3) 0.0221(7) Uani 1 1 d . . .
H3 H 0.4128 0.4944 0.5934 0.027 Uiso 1 1 calc R . .
N2 N 0.4997(3) 0.6739(3) 0.9908(2) 0.0169(5) Uani 1 1 d . . .
N1 N 0.5989(3) 0.6239(3) 0.9634(2) 0.0173(6) Uani 1 1 d . . .
C8 C 0.5227(3) 0.7449(3) 1.1079(3) 0.0153(6) Uani 1 1 d . . .
N6 N 0.6318(3) 0.7599(3) 1.1884(2) 0.0165(5) Uani 1 1 d . . .
N3 N 0.4303(3) 0.8053(3) 1.1507(2) 0.0180(6) Uani 1 1 d . . .
H1 H 0.3510 0.8081 1.1138 0.022 Uiso 1 1 calc R . .
N5 N 0.6042(3) 0.8341(3) 1.2847(2) 0.0170(5) Uani 1 1 d . . .
N4 N 0.4836(3) 0.8610(3) 1.2624(2) 0.0183(6) Uani 1 1 d . . .
H7 H 0.6790 0.0933 0.6832 0.022 Uiso 1 1 d R . .
H8 H 0.7211 -0.0090 0.6636 0.022 Uiso 1 1 d R . .
H9 H 1.0620 0.4236 0.6217 0.022 Uiso 1 1 d R . .
H10 H 1.0732 0.3540 0.5199 0.022 Uiso 1 1 d R . .
H17 H 1.2295 0.1081 0.5816 0.022 Uiso 1 1 d R . .
H18 H 1.1893 0.1379 0.4980 0.022 Uiso 1 1 d R . .
H19 H 1.1950 0.2837 0.7988 0.022 Uiso 1 1 d R . .
H20 H 1.1263 0.3709 0.8210 0.022 Uiso 1 1 d R . .
H15 H 0.3726 0.2245 0.4171 0.022 Uiso 1 1 d R . .
H16 H 0.2435 0.2132 0.3598 0.022 Uiso 1 1 d R . .
H21 H 0.2613 0.6032 0.9263 0.022 Uiso 1 1 d R . .
H22 H 0.1249 0.5756 0.8749 0.022 Uiso 1 1 d R . .
H23 H 0.8807 0.3191 0.9539 0.022 Uiso 1 1 d R . .
H24 H 0.9668 0.2762 0.8853 0.022 Uiso 1 1 d 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
Sm1 O4 2.402(2) . ?
Sm1 O5 2.405(2) . ?
Sm1 O8 2.419(2) . ?
Sm1 O9 2.440(2) . ?
Sm1 O10 2.454(2) . ?
Sm1 O1 2.518(2) . ?
Sm1 O2 2.524(2) . ?
Sm1 O7 2.535(2) . ?
Sm1 O7 2.750(2) 2_756 ?
O7 Sm1 2.750(2) 2_756 ?
O7 H17 0.8200 . ?
O7 H18 0.7988 . ?
O4 C15 1.252(4) . ?
O10 H19 0.7987 . ?
O10 H20 0.8225 . ?
O5 C15 1.274(4) 2_756 ?
O9 H9 0.8107 . ?
O9 H10 0.8128 . ?
O8 H7 0.8159 . ?
O8 H8 0.7806 . ?
O13 H15 0.8068 . ?
O13 H16 0.7977 . ?
O12 H21 0.8084 . ?
O12 H22 0.8206 . ?
N7 N8 1.262(4) . ?
N7 C13 1.415(4) . ?
C15 O5 1.274(4) 2_756 ?
C15 C9 1.489(4) . ?
C14 C9 1.378(4) . ?
C14 C13 1.398(4) . ?
C14 H14 0.9500 . ?
C9 C10 1.408(4) . ?
N8 C16 1.403(4) . ?
N12 C16 1.335(4) . ?
N12 N11 1.338(4) . ?
C16 N9 1.338(4) . ?
C13 C12 1.395(5) . ?
C12 C11 1.379(5) . ?
C12 H12 0.9500 . ?
O11 H23 0.8512 . ?
O11 H24 0.8218 . ?
C11 C10 1.405(5) . ?
C11 H11 0.9500 . ?
N9 N10 1.340(4) . ?
N11 N10 1.321(4) . ?
C10 O6 1.337(4) . ?
O6 H5 0.8400 . ?
O1 C7 1.251(4) . ?
O2 C7 1.280(4) . ?
O3 C2 1.351(4) . ?
O3 H4 0.8400 . ?
C7 C1 1.486(4) . ?
C6 C1 1.389(4) . ?
C6 C5 1.402(4) . ?
C6 H6 0.9500 . ?
C1 C2 1.401(4) . ?
C5 C4 1.402(5) . ?
C5 N1 1.414(4) . ?
C2 C3 1.405(5) . ?
C4 C3 1.369(5) . ?
C4 H2 0.9500 . ?
C3 H3 0.9500 . ?
N2 N1 1.265(4) . ?
N2 C8 1.406(4) . ?
C8 N3 1.324(4) . ?
C8 N6 1.342(4) . ?
N6 N5 1.338(4) . ?
N3 N4 1.340(4) . ?
N3 H1 0.8800 . ?
N5 N4 1.320(4) . ?

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 Sm1 O5 128.95(7) . . ?
O4 Sm1 O8 69.49(8) . . ?
O5 Sm1 O8 114.40(9) . . ?
O4 Sm1 O9 134.20(8) . . ?
O5 Sm1 O9 72.97(8) . . ?
O8 Sm1 O9 145.39(8) . . ?
O4 Sm1 O10 68.57(8) . . ?
O5 Sm1 O10 145.93(8) . . ?
O8 Sm1 O10 98.85(9) . . ?
O9 Sm1 O10 75.44(8) . . ?
O4 Sm1 O1 110.00(7) . . ?
O5 Sm1 O1 119.01(7) . . ?
O8 Sm1 O1 69.67(8) . . ?
O9 Sm1 O1 77.32(7) . . ?
O10 Sm1 O1 64.76(7) . . ?
O4 Sm1 O2 144.73(8) . . ?
O5 Sm1 O2 69.83(7) . . ?
O8 Sm1 O2 75.46(8) . . ?
O9 Sm1 O2 76.16(8) . . ?
O10 Sm1 O2 114.31(7) . . ?
O1 Sm1 O2 51.77(7) . . ?
O4 Sm1 O7 69.04(7) . . ?
O5 Sm1 O7 78.01(7) . . ?
O8 Sm1 O7 133.63(8) . . ?
O9 Sm1 O7 80.46(8) . . ?
O10 Sm1 O7 84.55(7) . . ?
O1 Sm1 O7 145.66(7) . . ?
O2 Sm1 O7 144.49(7) . . ?
O4 Sm1 O7 66.53(7) . 2_756 ?
O5 Sm1 O7 67.45(7) . 2_756 ?
O8 Sm1 O7 71.48(7) . 2_756 ?
O9 Sm1 O7 136.16(7) . 2_756 ?
O10 Sm1 O7 134.60(7) . 2_756 ?
O1 Sm1 O7 139.10(7) . 2_756 ?
O2 Sm1 O7 106.04(7) . 2_756 ?
O7 Sm1 O7 73.74(8) . 2_756 ?
Sm1 O7 Sm1 106.26(8) . 2_756 ?
Sm1 O7 H17 117.7 . . ?
Sm1 O7 H17 105.4 2_756 . ?
Sm1 O7 H18 107.9 . . ?
Sm1 O7 H18 110.0 2_756 . ?
H17 O7 H18 109.5 . . ?
C15 O4 Sm1 144.89(19) . . ?
Sm1 O10 H19 123.0 . . ?
Sm1 O10 H20 123.0 . . ?
H19 O10 H20 109.4 . . ?
C15 O5 Sm1 135.7(2) 2_756 . ?
Sm1 O9 H9 118.6 . . ?
Sm1 O9 H10 119.6 . . ?
H9 O9 H10 107.9 . . ?
Sm1 O8 H7 120.1 . . ?
Sm1 O8 H8 126.1 . . ?
H7 O8 H8 110.9 . . ?
H15 O13 H16 113.3 . . ?
H21 O12 H22 108.1 . . ?
N8 N7 C13 114.7(3) . . ?
O4 C15 O5 123.8(3) . 2_756 ?
O4 C15 C9 118.4(3) . . ?
O5 C15 C9 117.8(3) 2_756 . ?
C9 C14 C13 121.6(3) . . ?
C9 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C9 C10 119.3(3) . . ?
C14 C9 C15 118.0(3) . . ?
C10 C9 C15 122.7(3) . . ?
N7 N8 C16 112.8(3) . . ?
C16 N12 N11 105.0(3) . . ?
N12 C16 N9 111.5(3) . . ?
N12 C16 N8 128.3(3) . . ?
N9 C16 N8 120.1(3) . . ?
C12 C13 C14 118.9(3) . . ?
C12 C13 N7 116.7(3) . . ?
C14 C13 N7 124.4(3) . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
H23 O11 H24 106.1 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C16 N9 N10 104.7(3) . . ?
N10 N11 N12 109.2(3) . . ?
N11 N10 N9 109.6(3) . . ?
O6 C10 C11 118.4(3) . . ?
O6 C10 C9 122.4(3) . . ?
C11 C10 C9 119.2(3) . . ?
C10 O6 H5 109.5 . . ?
C7 O1 Sm1 94.24(18) . . ?
C7 O2 Sm1 93.18(18) . . ?
C2 O3 H4 109.5 . . ?
O1 C7 O2 120.8(3) . . ?
O1 C7 C1 120.7(3) . . ?
O2 C7 C1 118.4(3) . . ?
C1 C6 C5 120.6(3) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C1 C2 119.0(3) . . ?
C6 C1 C7 120.6(3) . . ?
C2 C1 C7 120.3(3) . . ?
C6 C5 C4 119.4(3) . . ?
C6 C5 N1 115.2(3) . . ?
C4 C5 N1 125.4(3) . . ?
O3 C2 C1 121.5(3) . . ?
O3 C2 C3 117.9(3) . . ?
C1 C2 C3 120.6(3) . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H2 119.6 . . ?
C5 C4 H2 119.6 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
N1 N2 C8 113.0(3) . . ?
N2 N1 C5 114.6(3) . . ?
N3 C8 N6 111.9(3) . . ?
N3 C8 N2 120.7(3) . . ?
N6 C8 N2 127.4(3) . . ?
N5 N6 C8 104.3(3) . . ?
C8 N3 N4 105.0(3) . . ?
C8 N3 H1 127.5 . . ?
N4 N3 H1 127.5 . . ?
N4 N5 N6 109.6(3) . . ?
N5 N4 N3 109.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        27.07
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.130
_database_code_depnum_ccdc_archive 'CCDC 922445'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H92 Eu4 N48 O52 '
_chemical_formula_weight         2973.74

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8805(2)
_cell_length_b                   14.6591(3)
_cell_length_c                   16.4889(3)
_cell_angle_alpha                99.9840(10)
_cell_angle_beta                 95.9560(10)
_cell_angle_gamma                110.3260(10)
_cell_volume                     2609.93(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11918
_cell_measurement_theta_min      1.27
_cell_measurement_theta_max      27.58

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480.0
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            41058
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         27.58
_reflns_number_total             12090
_reflns_number_gt                10514
_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 SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0274P)²+2.8236P] 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     SHELXL
_refine_ls_extinction_coef       0.0011(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         12090
_refine_ls_number_parameters     762
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0621
_refine_ls_wR_factor_gt          0.0594
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.005

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
Eu1 Eu 0.844263(11) 1.048387(9) 0.404693(8) 0.02402(4) Uani 1 1 d . . .
Eu2 Eu 0.347660(11) 0.547551(9) 0.923298(8) 0.02589(4) Uani 1 1 d . . .
O18 O 0.40988(18) 0.71909(14) 0.91411(13) 0.0364(5) Uani 1 1 d D . .
O20 O 0.19470(18) 0.57970(16) 0.99395(13) 0.0400(5) Uani 1 1 d D . .
O11 O 0.29461(17) 0.40418(14) 0.97812(12) 0.0339(4) Uani 1 1 d . . .
O10 O 0.56116(16) 0.60119(14) 0.92855(12) 0.0336(4) Uani 1 1 d . . .
O7 O 0.21673(16) 0.56576(14) 0.80466(11) 0.0313(4) Uani 1 1 d . . .
O8 O 0.14815(17) 0.42214(14) 0.84042(12) 0.0371(5) Uani 1 1 d . . .
O19 O 0.4432(2) 0.61826(16) 1.06705(13) 0.0457(5) Uani 1 1 d D . .
O5 O 0.79939(17) 0.91577(14) 0.47465(11) 0.0318(4) Uani 1 1 d . . .
O16 O 0.69702(17) 1.08555(16) 0.48294(12) 0.0361(4) Uani 1 1 d D . .
O14 O 0.91444(19) 1.22234(14) 0.41419(13) 0.0404(5) Uani 1 1 d D . .
O4 O 1.05485(16) 1.07152(15) 0.42430(12) 0.0356(5) Uani 1 1 d D . .
O1 O 0.69236(17) 1.05927(15) 0.30043(12) 0.0343(4) Uani 1 1 d . . .
O15 O 0.9307(2) 1.12298(16) 0.55674(13) 0.0449(5) Uani 1 1 d D . .
O2 O 0.62924(18) 0.91662(15) 0.33772(12) 0.0391(5) Uani 1 1 d . . .
C7 C 0.6138(2) 0.9733(2) 0.29151(16) 0.0290(5) Uani 1 1 d . . .
C1 C 0.5045(2) 0.93598(19) 0.22499(15) 0.0263(5) Uani 1 1 d . . .
C6 C 0.4905(2) 0.9937(2) 0.16949(16) 0.0277(5) Uani 1 1 d . . .
H6 H 0.5489 1.0573 0.1755 0.033 Uiso 1 1 calc R . .
C2 C 0.4154(3) 0.8407(2) 0.21576(17) 0.0328(6) Uani 1 1 d . . .
C31 C 0.3325(2) 0.36553(18) 1.03265(16) 0.0255(5) Uani 1 1 d . . .
C25 C 0.2422(2) 0.27450(18) 1.05046(15) 0.0244(5) Uani 1 1 d . . .
C26 C 0.1225(2) 0.22730(19) 1.00427(16) 0.0279(5) Uani 1 1 d . . .
C17 C 0.0263(2) 0.44449(19) 0.72802(16) 0.0273(5) Uani 1 1 d . . .
C23 C 0.1359(2) 0.48042(19) 0.79410(16) 0.0273(5) Uani 1 1 d . . .
C22 C 0.0113(2) 0.5029(2) 0.67310(16) 0.0279(5) Uani 1 1 d . . .
H22 H 0.0703 0.5661 0.6784 0.033 Uiso 1 1 calc R . .
C29 C 0.1977(2) 0.15055(19) 1.13369(16) 0.0273(5) Uani 1 1 d . . .
C30 C 0.2773(2) 0.23450(19) 1.11365(16) 0.0270(5) Uani 1 1 d . . .
H30 H 0.3565 0.2647 1.1437 0.032 Uiso 1 1 calc R . .
C28 C 0.0788(2) 0.1063(2) 1.08925(18) 0.0328(6) Uani 1 1 d . . .
H28 H 0.0239 0.0507 1.1029 0.039 Uiso 1 1 calc R . .
C27 C 0.0423(2) 0.1441(2) 1.02551(18) 0.0332(6) Uani 1 1 d . . .
H27 H -0.0373 0.1136 0.9960 0.040 Uiso 1 1 calc R . .
C21 C -0.0903(2) 0.4681(2) 0.61047(17) 0.0312(6) Uani 1 1 d . . .
C20 C -0.1796(3) 0.3737(2) 0.6028(2) 0.0432(7) Uani 1 1 d . . .
H20 H -0.2482 0.3505 0.5610 0.052 Uiso 1 1 calc R . .
C18 C -0.0639(3) 0.3497(2) 0.71906(18) 0.0354(6) Uani 1 1 d . . .
C5 C 0.3912(2) 0.9583(2) 0.10530(16) 0.0286(5) Uani 1 1 d . . .
C4 C 0.3024(3) 0.8628(2) 0.09647(18) 0.0359(6) Uani 1 1 d . . .
H4 H 0.2352 0.8386 0.0534 0.043 Uiso 1 1 calc R . .
O12 O 0.08228(18) 0.25896(15) 0.93914(13) 0.0396(5) Uani 1 1 d . . .
H8 H 0.1357 0.3100 0.9341 0.048 Uiso 1 1 calc R . .
O3 O 0.4235(2) 0.78118(16) 0.26789(14) 0.0477(6) Uani 1 1 d . . .
H2 H 0.4873 0.8088 0.3018 0.057 Uiso 1 1 calc R . .
O9 O -0.0547(2) 0.28902(17) 0.77006(16) 0.0531(6) Uani 1 1 d . . .
H7 H 0.0089 0.3168 0.8043 0.064 Uiso 1 1 calc R . .
N2 N 0.3058(2) 0.99388(17) -0.00844(14) 0.0305(5) Uani 1 1 d . . .
N14 N -0.1858(2) 0.50148(18) 0.50089(14) 0.0348(5) Uani 1 1 d . . .
N1 N 0.3906(2) 1.02568(17) 0.05406(14) 0.0305(5) Uani 1 1 d . . .
N13 N -0.0942(2) 0.53450(18) 0.55827(14) 0.0330(5) Uani 1 1 d . . .
N19 N 0.2291(2) 0.10511(17) 1.19720(14) 0.0312(5) Uani 1 1 d . . .
N3 N 0.3981(2) 1.15782(17) -0.04088(14) 0.0302(5) Uani 1 1 d . . .
N6 N 0.2324(2) 1.04705(18) -0.12394(14) 0.0332(5) Uani 1 1 d . . .
H1 H 0.1706 0.9928 -0.1452 0.040 Uiso 1 1 calc R . .
N15 N -0.1026(2) 0.66112(18) 0.45943(14) 0.0346(5) Uani 1 1 d . . .
N18 N -0.2711(2) 0.54542(19) 0.38442(15) 0.0375(5) Uani 1 1 d . . .
H18 H -0.3330 0.4902 0.3670 0.045 Uiso 1 1 calc R . .
N7 N 0.7614(2) 0.62765(17) 0.70183(14) 0.0328(5) Uani 1 1 d . . .
N20 N 0.3352(2) 0.15075(17) 1.23788(14) 0.0312(5) Uani 1 1 d . . .
N21 N 0.2985(2) 0.02443(19) 1.32309(15) 0.0373(6) Uani 1 1 d . . .
C8 C 0.3138(2) 1.06618(19) -0.05567(15) 0.0268(5) Uani 1 1 d . . .
C24 C -0.1840(2) 0.5699(2) 0.45056(16) 0.0307(6) Uani 1 1 d . . .
C13 C 0.7247(2) 0.66868(19) 0.63707(16) 0.0286(5) Uani 1 1 d . . .
C9 C 0.7558(2) 0.79214(19) 0.55301(15) 0.0244(5) Uani 1 1 d . . .
C32 C 0.3669(2) 0.1058(2) 1.30047(16) 0.0304(6) Uani 1 1 d . . .
C10 C 0.6368(2) 0.7385(2) 0.50673(17) 0.0305(6) Uani 1 1 d . . .
C3 C 0.3146(3) 0.8052(2) 0.15118(19) 0.0391(7) Uani 1 1 d . . .
H3 H 0.2554 0.7420 0.1453 0.047 Uiso 1 1 calc R . .
C12 C 0.6083(3) 0.6166(2) 0.59096(19) 0.0364(6) Uani 1 1 d . . .
H12 H 0.5593 0.5577 0.6035 0.044 Uiso 1 1 calc R . .
C11 C 0.5645(3) 0.6507(2) 0.52709(19) 0.0388(7) Uani 1 1 d . . .
H11 H 0.4860 0.6151 0.4971 0.047 Uiso 1 1 calc R . .
C15 C 0.8394(2) 0.88442(19) 0.53375(15) 0.0250(5) Uani 1 1 d . . .
C14 C 0.7970(2) 0.75612(19) 0.61751(16) 0.0271(5) Uani 1 1 d . . .
H14 H 0.8751 0.7914 0.6484 0.032 Uiso 1 1 calc R . .
C16 C 0.8974(3) 0.6287(2) 0.80376(17) 0.0320(6) Uani 1 1 d . . .
N5 N 0.2677(2) 1.13073(18) -0.15237(14) 0.0337(5) Uani 1 1 d . . .
N17 N -0.2416(2) 0.62500(19) 0.35100(15) 0.0380(6) Uani 1 1 d . . .
N4 N 0.3669(2) 1.19652(17) -0.10302(14) 0.0333(5) Uani 1 1 d . . .
N16 N -0.1410(2) 0.69444(18) 0.39582(15) 0.0378(5) Uani 1 1 d . . .
N8 N 0.8684(2) 0.67421(17) 0.74028(14) 0.0317(5) Uani 1 1 d . . .
N24 N 0.4783(2) 0.14723(19) 1.34564(15) 0.0379(6) Uani 1 1 d . . .
N9 N 0.8239(2) 0.5498(2) 0.82634(16) 0.0406(6) Uani 1 1 d . . .
N23 N 0.4788(2) 0.0877(2) 1.39851(16) 0.0428(6) Uani 1 1 d . . .
N22 N 0.3719(2) 0.0148(2) 1.38501(16) 0.0433(6) Uani 1 1 d . . .
C19 C -0.1668(3) 0.3154(2) 0.6564(2) 0.0452(8) Uani 1 1 d . . .
H19 H -0.2267 0.2526 0.6512 0.054 Uiso 1 1 calc R . .
N12 N 1.0084(2) 0.66462(19) 0.84958(16) 0.0399(6) Uani 1 1 d . . .
N11 N 1.0027(3) 0.6045(2) 0.90241(16) 0.0463(7) Uani 1 1 d . . .
N10 N 0.8927(3) 0.5362(2) 0.88852(17) 0.0470(7) Uani 1 1 d . . .
O6 O 0.58862(19) 0.76711(16) 0.44361(14) 0.0433(5) Uani 1 1 d . . .
H5 H 0.6378 0.8197 0.4376 0.052 Uiso 1 1 calc R . .
O17 O 0.84984(18) 0.88924(15) 0.31140(12) 0.0386(5) Uani 1 1 d D . .
O21 O 0.3918(2) 0.46230(19) 0.80203(13) 0.0531(6) Uani 1 1 d D . .
O13 O 0.92506(18) 1.08163(16) 0.26718(12) 0.0421(5) Uani 1 1 d D . .
O25 O 0.5916(2) 0.42092(19) 0.78096(17) 0.0579(6) Uani 1 1 d D . .
O26 O 0.2401(2) 0.7988(2) 0.8724(2) 0.0730(8) Uani 1 1 d D . .
O24 O 0.0622(3) 0.9080(2) 0.2329(2) 0.0925(11) Uani 1 1 d D . .
O22 O 0.7590(3) 0.2542(2) 0.2954(2) 0.1007(12) Uani 1 1 d D . .
O23 O 0.5921(3) 0.3451(2) 0.28946(19) 0.0966(11) Uani 1 1 d D . .
H10 H 0.9655 1.0549 0.2555 0.116 Uiso 1 1 d RD . .
H9 H 0.9377 1.1311 0.2502 0.116 Uiso 1 1 d RD . .
H13 H 0.9683 1.2618 0.4510 0.116 Uiso 1 1 d RD . .
H15 H 0.8905 1.2494 0.3831 0.116 Uiso 1 1 d RD . .
H16 H 0.9472 1.0855 0.5801 0.116 Uiso 1 1 d RD . .
H17 H 0.9792 1.1780 0.5689 0.116 Uiso 1 1 d RD . .
H24 H 0.8086 0.8826 0.2678 0.116 Uiso 1 1 d RD . .
H23 H 0.8175 0.8426 0.3325 0.116 Uiso 1 1 d RD . .
H21 H 0.6331 1.0839 0.4614 0.116 Uiso 1 1 d RD . .
H25 H 0.6889 1.0622 0.5244 0.116 Uiso 1 1 d RD . .
H26 H 0.3598 0.7426 0.9085 0.116 Uiso 1 1 d RD . .
H29 H 0.4709 0.7581 0.9457 0.116 Uiso 1 1 d RD . .
H31 H 0.5065 0.6637 1.0772 0.116 Uiso 1 1 d RD . .
H32 H 0.4224 0.6035 1.1104 0.116 Uiso 1 1 d RD . .
H33 H 0.1759 0.5470 1.0289 0.116 Uiso 1 1 d RD . .
H34 H 0.1383 0.5873 0.9705 0.116 Uiso 1 1 d RD . .
H36 H 0.3412 0.4312 0.7620 0.116 Uiso 1 1 d RD . .
H35 H 0.4549 0.4563 0.8003 0.116 Uiso 1 1 d RD . .
H37 H 0.7436 0.2798 0.3501 0.116 Uiso 1 1 d RD . .
H40 H 0.5191 0.3112 0.2882 0.116 Uiso 1 1 d RD . .
H42 H 0.1334 0.9324 0.2583 0.116 Uiso 1 1 d RD . .
H41 H 0.0142 0.8975 0.2648 0.116 Uiso 1 1 d RD . .
H43 H 0.5675 0.4070 0.7313 0.116 Uiso 1 1 d RD . .
H44 H 0.6638 0.4505 0.7906 0.116 Uiso 1 1 d RD . .
H45 H 0.2523 0.7817 0.8178 0.116 Uiso 1 1 d RD . .
H38 H 0.7169 0.1942 0.2963 0.116 Uiso 1 1 d RD . .
H46 H 0.1633 0.7648 0.8611 0.116 Uiso 1 1 d RD . .
H39 H 0.6325 0.3139 0.2706 0.116 Uiso 1 1 d RD . .


_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
Eu1 O5 2.3620(17) . ?
Eu1 O14 2.3621(19) . ?
Eu1 O4 2.3840(18) . ?
Eu1 O1 2.4268(18) . ?
Eu1 O16 2.431(2) . ?
Eu1 O15 2.504(2) . ?
Eu1 O17 2.588(2) . ?
Eu1 O2 2.593(2) . ?
Eu1 O13 2.610(2) . ?
Eu1 C7 2.886(3) . ?
Eu2 O11 2.3427(17) . ?
Eu2 O10 2.3674(18) . ?
Eu2 O21 2.375(2) . ?
Eu2 O20 2.393(2) . ?
Eu2 O19 2.399(2) . ?
Eu2 O18 2.3993(18) . ?
Eu2 O7 2.4811(17) . ?
Eu2 O8 2.5090(19) . ?
Eu2 C23 2.877(3) . ?
Eu2 H33 2.8160 . ?
O18 H26 0.7892 . ?
O18 H29 0.8090 . ?
O20 H33 0.8134 . ?
O20 H34 0.7898 . ?
O11 C31 1.265(3) . ?
O10 C31 1.241(3) 2_667 ?
O7 C23 1.254(3) . ?
O8 C23 1.274(3) . ?
O19 H31 0.7900 . ?
O19 H32 0.8193 . ?
O5 C15 1.264(3) . ?
O16 H21 0.7949 . ?
O16 H25 0.8168 . ?
O14 H13 0.8084 . ?
O14 H15 0.7863 . ?
O4 C15 1.255(3) 2_776 ?
O1 C7 1.253(3) . ?
O15 H16 0.7884 . ?
O15 H17 0.7872 . ?
O2 C7 1.266(3) . ?
C7 C1 1.480(3) . ?
C1 C6 1.384(3) . ?
C1 C2 1.400(4) . ?
C6 C5 1.381(3) . ?
C6 H6 0.9300 . ?
C2 O3 1.345(3) . ?
C2 C3 1.396(4) . ?
C31 O10 1.241(3) 2_667 ?
C31 C25 1.491(3) . ?
C25 C30 1.377(3) . ?
C25 C26 1.410(3) . ?
C26 O12 1.348(3) . ?
C26 C27 1.389(4) . ?
C17 C22 1.388(4) . ?
C17 C18 1.400(4) . ?
C17 C23 1.481(3) . ?
C22 C21 1.384(4) . ?
C22 H22 0.9300 . ?
C29 C30 1.384(3) . ?
C29 C28 1.391(4) . ?
C29 N19 1.419(3) . ?
C30 H30 0.9300 . ?
C28 C27 1.369(4) . ?
C28 H28 0.9300 . ?
C27 H27 0.9300 . ?
C21 C20 1.396(4) . ?
C21 N13 1.415(3) . ?
C20 C19 1.364(4) . ?
C20 H20 0.9300 . ?
C18 O9 1.349(3) . ?
C18 C19 1.394(4) . ?
C5 C4 1.402(4) . ?
C5 N1 1.409(3) . ?
C4 C3 1.367(4) . ?
C4 H4 0.9300 . ?
O12 H8 0.8200 . ?
O3 H2 0.8200 . ?
O9 H7 0.8200 . ?
N2 N1 1.260(3) . ?
N2 C8 1.404(3) . ?
N14 N13 1.255(3) . ?
N14 C24 1.405(4) . ?
N19 N20 1.252(3) . ?
N3 C8 1.330(3) . ?
N3 N4 1.333(3) . ?
N6 C8 1.326(3) . ?
N6 N5 1.335(3) . ?
N6 H1 0.8600 . ?
N15 C24 1.322(4) . ?
N15 N16 1.334(3) . ?
N18 C24 1.327(3) . ?
N18 N17 1.329(3) . ?
N18 H18 0.8600 . ?
N7 N8 1.251(3) . ?
N7 C13 1.414(3) . ?
N20 C32 1.403(3) . ?
N21 C32 1.329(3) . ?
N21 N22 1.332(3) . ?
C13 C12 1.386(4) . ?
C13 C14 1.386(3) . ?
C9 C14 1.384(3) . ?
C9 C10 1.412(3) . ?
C9 C15 1.483(3) . ?
C32 N24 1.325(4) . ?
C10 O6 1.335(3) . ?
C10 C11 1.395(4) . ?
C3 H3 0.9300 . ?
C12 C11 1.371(4) . ?
C12 H12 0.9300 . ?
C11 H11 0.9300 . ?
C15 O4 1.255(3) 2_776 ?
C14 H14 0.9300 . ?
C16 N9 1.324(4) . ?
C16 N12 1.326(4) . ?
C16 N8 1.410(3) . ?
N5 N4 1.311(3) . ?
N17 N16 1.312(3) . ?
N24 N23 1.337(3) . ?
N9 N10 1.330(3) . ?
N23 N22 1.311(4) . ?
C19 H19 0.9300 . ?
N12 N11 1.333(3) . ?
N11 N10 1.309(4) . ?
O6 H5 0.8200 . ?
O17 H24 0.7983 . ?
O17 H23 0.8139 . ?
O21 H36 0.7928 . ?
O21 H35 0.7880 . ?
O13 H10 0.7377 . ?
O13 H9 0.7948 . ?
O25 H43 0.8047 . ?
O25 H44 0.7986 . ?
O26 H45 0.9322 . ?
O26 H46 0.8551 . ?
O24 H42 0.8261 . ?
O24 H41 0.8102 . ?
O22 H37 0.9756 . ?
O22 H38 0.8515 . ?
O23 H40 0.8324 . ?
O23 H39 0.8186 . ?

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
O5 Eu1 O14 148.05(7) . . ?
O5 Eu1 O4 91.10(6) . . ?
O14 Eu1 O4 85.25(7) . . ?
O5 Eu1 O1 121.68(6) . . ?
O14 Eu1 O1 78.74(7) . . ?
O4 Eu1 O1 138.66(6) . . ?
O5 Eu1 O16 81.10(7) . . ?
O14 Eu1 O16 81.42(7) . . ?
O4 Eu1 O16 139.78(7) . . ?
O1 Eu1 O16 75.06(6) . . ?
O5 Eu1 O15 72.72(7) . . ?
O14 Eu1 O15 75.92(7) . . ?
O4 Eu1 O15 72.60(7) . . ?
O1 Eu1 O15 137.09(7) . . ?
O16 Eu1 O15 67.38(7) . . ?
O5 Eu1 O17 68.97(7) . . ?
O14 Eu1 O17 139.41(7) . . ?
O4 Eu1 O17 75.78(7) . . ?
O1 Eu1 O17 92.21(6) . . ?
O16 Eu1 O17 134.67(7) . . ?
O15 Eu1 O17 129.02(7) . . ?
O5 Eu1 O2 70.75(6) . . ?
O14 Eu1 O2 127.50(6) . . ?
O4 Eu1 O2 142.11(7) . . ?
O1 Eu1 O2 51.42(6) . . ?
O16 Eu1 O2 71.70(7) . . ?
O15 Eu1 O2 128.18(7) . . ?
O17 Eu1 O2 66.76(7) . . ?
O5 Eu1 O13 136.06(7) . . ?
O14 Eu1 O13 72.38(7) . . ?
O4 Eu1 O13 71.64(6) . . ?
O1 Eu1 O13 67.24(6) . . ?
O16 Eu1 O13 137.27(6) . . ?
O15 Eu1 O13 133.46(7) . . ?
O17 Eu1 O13 67.70(7) . . ?
O2 Eu1 O13 98.24(6) . . ?
O5 Eu1 C7 96.67(7) . . ?
O14 Eu1 C7 103.37(7) . . ?
O4 Eu1 C7 147.49(7) . . ?
O1 Eu1 C7 25.46(7) . . ?
O16 Eu1 C7 72.72(7) . . ?
O15 Eu1 C7 139.78(7) . . ?
O17 Eu1 C7 77.71(7) . . ?
O2 Eu1 C7 26.02(7) . . ?
O13 Eu1 C7 81.11(7) . . ?
O11 Eu2 O10 105.40(6) . . ?
O11 Eu2 O21 91.18(8) . . ?
O10 Eu2 O21 69.77(7) . . ?
O11 Eu2 O20 84.05(7) . . ?
O10 Eu2 O20 142.81(7) . . ?
O21 Eu2 O20 147.07(7) . . ?
O11 Eu2 O19 79.19(7) . . ?
O10 Eu2 O19 72.54(7) . . ?
O21 Eu2 O19 136.85(8) . . ?
O20 Eu2 O19 74.22(8) . . ?
O11 Eu2 O18 161.36(7) . . ?
O10 Eu2 O18 75.34(7) . . ?
O21 Eu2 O18 106.19(9) . . ?
O20 Eu2 O18 84.82(7) . . ?
O19 Eu2 O18 83.43(7) . . ?
O11 Eu2 O7 122.97(6) . . ?
O10 Eu2 O7 119.85(6) . . ?
O21 Eu2 O7 75.33(7) . . ?
O20 Eu2 O7 80.09(7) . . ?
O19 Eu2 O7 144.03(7) . . ?
O18 Eu2 O7 69.41(6) . . ?
O11 Eu2 O8 71.01(6) . . ?
O10 Eu2 O8 142.52(7) . . ?
O21 Eu2 O8 72.99(7) . . ?
O20 Eu2 O8 74.66(7) . . ?
O19 Eu2 O8 138.57(7) . . ?
O18 Eu2 O8 120.01(6) . . ?
O7 Eu2 O8 51.98(6) . . ?
O11 Eu2 C23 97.24(7) . . ?
O10 Eu2 C23 135.96(7) . . ?
O21 Eu2 C23 72.54(7) . . ?
O20 Eu2 C23 75.78(7) . . ?
O19 Eu2 C23 149.99(8) . . ?
O18 Eu2 C23 94.44(7) . . ?
O7 Eu2 C23 25.74(7) . . ?
O8 Eu2 C23 26.25(6) . . ?
O11 Eu2 H33 69.3 . . ?
O10 Eu2 H33 140.5 . . ?
O21 Eu2 H33 146.4 . . ?
O20 Eu2 H33 15.4 . . ?
O19 Eu2 H33 68.0 . . ?
O18 Eu2 H33 98.0 . . ?
O7 Eu2 H33 92.2 . . ?
O8 Eu2 H33 74.8 . . ?
C23 Eu2 H33 82.7 . . ?
Eu2 O18 H26 119.0 . . ?
Eu2 O18 H29 116.7 . . ?
H26 O18 H29 111.5 . . ?
Eu2 O20 H33 113.4 . . ?
Eu2 O20 H34 122.6 . . ?
H33 O20 H34 112.1 . . ?
C31 O11 Eu2 142.67(17) . . ?
C31 O10 Eu2 152.04(18) 2_667 . ?
C23 O7 Eu2 95.04(15) . . ?
C23 O8 Eu2 93.20(15) . . ?
Eu2 O19 H31 118.4 . . ?
Eu2 O19 H32 131.4 . . ?
H31 O19 H32 110.3 . . ?
C15 O5 Eu1 144.06(17) . . ?
Eu1 O16 H21 123.4 . . ?
Eu1 O16 H25 114.5 . . ?
H21 O16 H25 109.9 . . ?
Eu1 O14 H13 122.4 . . ?
Eu1 O14 H15 126.1 . . ?
H13 O14 H15 111.5 . . ?
C15 O4 Eu1 149.50(19) 2_776 . ?
C7 O1 Eu1 98.20(15) . . ?
Eu1 O15 H16 112.7 . . ?
Eu1 O15 H17 117.5 . . ?
H16 O15 H17 114.7 . . ?
C7 O2 Eu1 90.01(16) . . ?
O1 C7 O2 120.1(2) . . ?
O1 C7 C1 120.4(2) . . ?
O2 C7 C1 119.5(2) . . ?
O1 C7 Eu1 56.34(13) . . ?
O2 C7 Eu1 63.97(14) . . ?
C1 C7 Eu1 172.90(18) . . ?
C6 C1 C2 119.0(2) . . ?
C6 C1 C7 120.4(2) . . ?
C2 C1 C7 120.5(2) . . ?
C5 C6 C1 121.0(2) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O3 C2 C3 118.3(3) . . ?
O3 C2 C1 121.8(2) . . ?
C3 C2 C1 119.9(2) . . ?
O10 C31 O11 124.0(2) 2_667 . ?
O10 C31 C25 118.9(2) 2_667 . ?
O11 C31 C25 117.0(2) . . ?
C30 C25 C26 118.8(2) . . ?
C30 C25 C31 118.8(2) . . ?
C26 C25 C31 122.4(2) . . ?
O12 C26 C27 118.0(2) . . ?
O12 C26 C25 122.7(2) . . ?
C27 C26 C25 119.3(2) . . ?
C22 C17 C18 118.7(2) . . ?
C22 C17 C23 121.0(2) . . ?
C18 C17 C23 120.3(2) . . ?
O7 C23 O8 119.8(2) . . ?
O7 C23 C17 121.6(2) . . ?
O8 C23 C17 118.6(2) . . ?
O7 C23 Eu2 59.22(13) . . ?
O8 C23 Eu2 60.55(13) . . ?
C17 C23 Eu2 179.16(19) . . ?
C21 C22 C17 120.7(3) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
C30 C29 C28 119.0(2) . . ?
C30 C29 N19 124.2(2) . . ?
C28 C29 N19 116.8(2) . . ?
C25 C30 C29 121.7(2) . . ?
C25 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
C27 C28 C29 120.3(2) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C28 C27 C26 120.8(3) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C22 C21 C20 119.8(3) . . ?
C22 C21 N13 115.2(2) . . ?
C20 C21 N13 125.0(2) . . ?
C19 C20 C21 120.3(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
O9 C18 C19 117.9(3) . . ?
O9 C18 C17 121.7(2) . . ?
C19 C18 C17 120.4(3) . . ?
C6 C5 C4 119.7(2) . . ?
C6 C5 N1 114.1(2) . . ?
C4 C5 N1 126.2(2) . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C26 O12 H8 109.5 . . ?
C2 O3 H2 109.5 . . ?
C18 O9 H7 109.5 . . ?
N1 N2 C8 111.7(2) . . ?
N13 N14 C24 112.1(2) . . ?
N2 N1 C5 116.1(2) . . ?
N14 N13 C21 114.6(2) . . ?
N20 N19 C29 114.1(2) . . ?
C8 N3 N4 104.6(2) . . ?
C8 N6 N5 104.7(2) . . ?
C8 N6 H1 127.6 . . ?
N5 N6 H1 127.6 . . ?
C24 N15 N16 104.8(2) . . ?
C24 N18 N17 104.8(2) . . ?
C24 N18 H18 127.6 . . ?
N17 N18 H18 127.6 . . ?
N8 N7 C13 115.2(2) . . ?
N19 N20 C32 114.3(2) . . ?
C32 N21 N22 104.2(2) . . ?
N6 C8 N3 111.8(2) . . ?
N6 C8 N2 120.9(2) . . ?
N3 C8 N2 127.3(2) . . ?
N15 C24 N18 111.8(2) . . ?
N15 C24 N14 128.0(2) . . ?
N18 C24 N14 120.2(3) . . ?
C12 C13 C14 119.0(2) . . ?
C12 C13 N7 116.6(2) . . ?
C14 C13 N7 124.4(2) . . ?
C14 C9 C10 118.9(2) . . ?
C14 C9 C15 118.7(2) . . ?
C10 C9 C15 122.4(2) . . ?
N24 C32 N21 112.6(2) . . ?
N24 C32 N20 118.8(2) . . ?
N21 C32 N20 128.6(3) . . ?
O6 C10 C11 117.4(2) . . ?
O6 C10 C9 123.4(2) . . ?
C11 C10 C9 119.2(2) . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C11 C12 C13 120.9(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
O4 C15 O5 122.5(2) 2_776 . ?
O4 C15 C9 120.1(2) 2_776 . ?
O5 C15 C9 117.4(2) . . ?
C9 C14 C13 121.5(2) . . ?
C9 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
N9 C16 N12 111.9(2) . . ?
N9 C16 N8 127.3(3) . . ?
N12 C16 N8 120.8(3) . . ?
N4 N5 N6 109.4(2) . . ?
N16 N17 N18 109.4(2) . . ?
N5 N4 N3 109.5(2) . . ?
N17 N16 N15 109.2(2) . . ?
N7 N8 C16 111.6(2) . . ?
C32 N24 N23 104.0(2) . . ?
C16 N9 N10 104.7(3) . . ?
N22 N23 N24 109.7(2) . . ?
N23 N22 N21 109.6(2) . . ?
C20 C19 C18 120.0(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C16 N12 N11 104.5(3) . . ?
N10 N11 N12 109.4(2) . . ?
N11 N10 N9 109.5(2) . . ?
C10 O6 H5 109.5 . . ?
Eu1 O17 H24 104.5 . . ?
Eu1 O17 H23 107.5 . . ?
H24 O17 H23 109.3 . . ?
Eu2 O21 H36 122.4 . . ?
Eu2 O21 H35 123.1 . . ?
H36 O21 H35 114.0 . . ?
Eu1 O13 H10 113.0 . . ?
Eu1 O13 H9 126.7 . . ?
H10 O13 H9 113.8 . . ?
H43 O25 H44 109.6 . . ?
H45 O26 H46 94.6 . . ?
H42 O24 H41 111.3 . . ?
H37 O22 H38 92.2 . . ?
H40 O23 H39 115.4 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.472
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.079
_database_code_depnum_ccdc_archive 'CCDC 922446'
