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

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#                                CCDC 
# 
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#  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.
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#  fide research purposes only. It may contain copyright material
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H33 Er N12 O18'
_chemical_formula_weight         848.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   12.9043(8)
_cell_length_b                   13.7369(8)
_cell_length_c                   18.1170(10)
_cell_angle_alpha                85.446(3)
_cell_angle_beta                 77.264(3)
_cell_angle_gamma                83.393(3)
_cell_volume                     3106.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9514
_cell_measurement_theta_min      27.50
_cell_measurement_theta_max      2.32

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1700.0
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_T_max  0.588
_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            47911
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         27.52
_reflns_number_total             14304
_reflns_number_gt                12323
_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)+(0.0289P)²+3.6951P] 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       0.00025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14304
_refine_ls_number_parameters     818
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0634
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.629193(9) 0.329863(9) 0.883616(6) 0.02353(4) Uani 1 1 d . . .
Er2 Er 0.589520(9) 0.177759(9) 0.379683(6) 0.02394(4) Uani 1 1 d . . .
O1 O 0.70043(18) 0.28995(19) 0.67618(12) 0.0434(6) Uani 1 1 d . . .
O2 O 0.76315(16) 0.32310(17) 0.77524(11) 0.0344(5) Uani 1 1 d . . .
O3 O 0.96763(17) 0.3224(2) 0.75748(12) 0.0443(6) Uani 1 1 d . . .
O4 O 0.36638(15) 0.36682(17) 1.03573(11) 0.0357(5) Uani 1 1 d . . .
O5 O 0.44411(15) 0.33000(16) 0.91829(11) 0.0335(5) Uani 1 1 d . . .
O6 O 0.33392(16) 0.29706(19) 0.82277(12) 0.0412(5) Uani 1 1 d . . .
O7 O 0.64980(17) 0.20889(19) 0.17316(12) 0.0440(6) Uani 1 1 d . . .
O8 O 0.72469(17) 0.19225(17) 0.27312(11) 0.0355(5) Uani 1 1 d . . .
O9 O 0.92886(18) 0.1931(2) 0.25070(12) 0.0460(6) Uani 1 1 d . . .
O10 O 0.33522(15) 0.12917(16) 0.53104(11) 0.0324(5) Uani 1 1 d . . .
O11 O 0.40111(15) 0.17196(16) 0.41030(11) 0.0334(5) Uani 1 1 d . . .
O12 O 0.28289(16) 0.19959(17) 0.31452(11) 0.0373(5) Uani 1 1 d . . .
O13 O 0.55357(17) 0.45141(18) 0.81097(14) 0.0458(6) Uani 1 1 d . . .
O14 O 0.5776(2) 0.22520(18) 0.80626(13) 0.0455(6) Uani 1 1 d . . .
O15 O 0.6150(2) 0.17813(17) 0.95177(14) 0.0490(6) Uani 1 1 d . . .
O16 O 0.57908(16) 0.38484(18) 1.00266(12) 0.0403(5) Uani 1 1 d . . .
O17 O 0.79521(17) 0.28526(16) 0.92161(12) 0.0371(5) Uani 1 1 d . . .
O18 O 0.72310(18) 0.47082(16) 0.88679(13) 0.0408(5) Uani 1 1 d . . .
O19 O 0.54806(17) 0.05206(17) 0.31760(14) 0.0432(6) Uani 1 1 d . . .
O20 O 0.55258(15) 0.10273(16) 0.49857(11) 0.0336(5) Uani 1 1 d . . .
O21 O 0.52603(19) 0.31989(17) 0.44463(13) 0.0423(5) Uani 1 1 d . . .
O22 O 0.72985(17) 0.23217(16) 0.42633(13) 0.0381(5) Uani 1 1 d . . .
O23 O 0.72709(16) 0.04172(15) 0.38760(12) 0.0346(5) Uani 1 1 d . . .
O24 O 0.51362(18) 0.28072(18) 0.29289(12) 0.0449(6) Uani 1 1 d . . .
O25 O 0.45230(13) 0.07846(11) 0.86995(7) 0.0772(9) Uani 1 1 d G . .
H25A H 0.4762 0.0178 0.8746 0.116 Uiso 1 1 d G . .
H25B H 0.3857 0.0861 0.8828 0.116 Uiso 1 1 d G . .
O26 O 0.72885(14) 0.02383(11) 0.88109(7) 0.0784(9) Uani 1 1 d G . .
H26A H 0.7939 0.0362 0.8657 0.118 Uiso 1 1 d G . .
H26B H 0.7010 0.0188 0.8438 0.118 Uiso 1 1 d G . .
O27 O 0.65433(11) 0.57247(8) 0.69917(6) 0.0441(5) Uani 1 1 d G . .
H27B H 0.6612 0.5481 0.6561 0.066 Uiso 1 1 d G . .
H27A H 0.7120 0.5801 0.7046 0.066 Uiso 1 1 d G . .
O28 O 0.54996(8) 0.32974(8) 0.58792(5) 0.0995(13) Uani 1 1 d G . .
H28A H 0.5322 0.2658 0.6087 0.149 Uiso 1 1 d R . .
H28B H 0.5903 0.3275 0.6205 0.149 Uiso 1 1 d R . .
O29 O 0.74748(7) 0.42742(7) 0.43822(5) 0.0626(8) Uani 1 1 d G . .
H29B H 0.7394 0.4469 0.3933 0.094 Uiso 1 1 d G . .
H29A H 0.8129 0.4137 0.4288 0.094 Uiso 1 1 d G . .
O30 O 0.67843(16) 0.88459(11) -0.01152(7) 0.159(2) Uani 1 1 d G . .
H30A H 0.7106 0.9348 -0.0333 0.239 Uiso 1 1 d G . .
H30B H 0.6123 0.8986 -0.0085 0.239 Uiso 1 1 d G . .
O31 O 0.65480(8) 0.54967(7) 0.34361(5) 0.1272(18) Uani 1 1 d G . .
H31A H 0.6421 0.6119 0.3389 0.191 Uiso 1 1 d G . .
H31B H 0.6784 0.5277 0.2994 0.191 Uiso 1 1 d G . .
O32 O 0.65517(10) 0.75014(7) 0.34652(6) 0.1037(13) Uani 1 1 d G . .
H32A H 0.7091 0.7726 0.3148 0.156 Uiso 1 1 d G . .
H32B H 0.6590 0.7615 0.3902 0.156 Uiso 1 1 d G . .
O33 O 0.67408(14) 0.91434(8) 0.23979(7) 0.0606(8) Uani 1 1 d G . .
H33B H 0.7370 0.9251 0.2276 0.091 Uiso 1 1 d G . .
H33A H 0.6571 0.8649 0.2288 0.091 Uiso 1 1 d G . .
O34 O 0.61786(8) 0.51816(7) 0.56565(5) 0.0990(13) Uani 1 1 d G . .
H34A H 0.6487 0.5564 0.5212 0.148 Uiso 1 1 d R . .
H34B H 0.5704 0.4765 0.5529 0.148 Uiso 1 1 d R . .
O35 O 0.52220(17) 0.12706(11) 0.09840(7) 0.0635(7) Uani 1 1 d G . .
H35B H 0.4625 0.1544 0.1192 0.095 Uiso 1 1 d G . .
H35A H 0.5628 0.1440 0.1238 0.095 Uiso 1 1 d G . .
O36 O 0.31278(16) 0.21498(13) 0.15292(8) 0.0999(13) Uani 1 1 d G . .
H36A H 0.3140 0.2159 0.2000 0.150 Uiso 1 1 d G . .
H36B H 0.3046 0.2679 0.1310 0.150 Uiso 1 1 d G . .
C1 C 0.8762(2) 0.3344(2) 0.65434(15) 0.0264(6) Uani 1 1 d . . .
C2 C 0.9683(2) 0.3358(2) 0.68311(16) 0.0310(6) Uani 1 1 d . . .
C3 C 1.0658(2) 0.3515(3) 0.63399(18) 0.0371(7) Uani 1 1 d . . .
C4 C 1.0717(2) 0.3684(2) 0.55780(17) 0.0336(6) Uani 1 1 d . . .
C5 C 0.9798(2) 0.3692(2) 0.52884(15) 0.0285(6) Uani 1 1 d . . .
C6 C 0.8843(2) 0.3516(2) 0.57704(16) 0.0284(6) Uani 1 1 d . . .
C7 C 0.7717(2) 0.3148(2) 0.70424(16) 0.0289(6) Uani 1 1 d . . .
C8 C 1.0484(2) 0.4104(2) 0.33133(16) 0.0300(6) Uani 1 1 d . . .
C9 C 0.2569(2) 0.3425(2) 0.95062(15) 0.0252(5) Uani 1 1 d . . .
C10 C 0.2490(2) 0.3196(2) 0.87793(16) 0.0284(6) Uani 1 1 d . . .
C11 C 0.1483(2) 0.3211(3) 0.86017(17) 0.0359(7) Uani 1 1 d . . .
C12 C 0.0578(2) 0.3444(2) 0.91317(17) 0.0333(7) Uani 1 1 d . . .
C13 C 0.0642(2) 0.3650(2) 0.98608(16) 0.0259(6) Uani 1 1 d . . .
C14 C 0.1634(2) 0.3638(2) 1.00380(15) 0.0259(6) Uani 1 1 d . . .
C15 C 0.3622(2) 0.3468(2) 0.97062(15) 0.0256(6) Uani 1 1 d . . .
C16 C -0.1927(2) 0.4134(2) 1.09726(15) 0.0246(5) Uani 1 1 d . . .
C17 C 0.8367(2) 0.1723(2) 0.15233(15) 0.0271(6) Uani 1 1 d . . .
C18 C 0.9303(2) 0.1740(2) 0.17902(16) 0.0312(6) Uani 1 1 d . . .
C19 C 1.0299(2) 0.1572(3) 0.13014(18) 0.0370(7) Uani 1 1 d . . .
C20 C 1.0372(2) 0.1379(2) 0.05602(17) 0.0338(7) Uani 1 1 d . . .
C21 C 0.9441(2) 0.1362(2) 0.02894(16) 0.0284(6) Uani 1 1 d . . .
C23 C 0.7291(2) 0.1920(2) 0.20190(16) 0.0304(6) Uani 1 1 d . . .
C22 C 0.8457(2) 0.1538(2) 0.07696(16) 0.0285(6) Uani 1 1 d . . .
C24 C 1.0220(2) 0.0857(2) -0.16402(16) 0.0306(6) Uani 1 1 d . . .
C25 C 0.2172(2) 0.15553(19) 0.44618(15) 0.0249(5) Uani 1 1 d . . .
C26 C 0.2032(2) 0.1758(2) 0.37161(16) 0.0271(6) Uani 1 1 d . . .
C27 C 0.1037(2) 0.1704(2) 0.35382(17) 0.0325(6) Uani 1 1 d . . .
C28 C 0.0182(2) 0.1489(2) 0.40985(17) 0.0322(6) Uani 1 1 d . . .
C29 C 0.0301(2) 0.1321(2) 0.48454(16) 0.0267(6) Uani 1 1 d . . .
C30 C 0.1294(2) 0.1339(2) 0.50191(15) 0.0251(5) Uani 1 1 d . . .
C31 C 0.3248(2) 0.1521(2) 0.46514(15) 0.0254(6) Uani 1 1 d . . .
C32 C -0.2156(2) 0.0858(2) 0.60088(16) 0.0260(6) Uani 1 1 d . . .
N1 N 0.9751(2) 0.38563(18) 0.45159(13) 0.0310(5) Uani 1 1 d . . .
N2 N 1.0624(2) 0.39636(18) 0.40632(13) 0.0311(5) Uani 1 1 d . . .
N3 N 0.9583(2) 0.4145(2) 0.30731(14) 0.0355(6) Uani 1 1 d . . .
N4 N 0.9911(2) 0.4276(2) 0.23399(14) 0.0379(6) Uani 1 1 d . . .
N5 N 1.0945(2) 0.4320(2) 0.21211(15) 0.0430(7) Uani 1 1 d . . .
N6 N 1.1329(2) 0.4210(2) 0.27424(15) 0.0393(6) Uani 1 1 d . . .
N7 N -0.02178(18) 0.38927(17) 1.04607(13) 0.0273(5) Uani 1 1 d . . .
N8 N -0.11367(18) 0.38556(17) 1.03374(13) 0.0267(5) Uani 1 1 d . . .
N9 N -0.17797(19) 0.43212(19) 1.16466(14) 0.0328(5) Uani 1 1 d . . .
N10 N -0.2757(2) 0.4581(2) 1.20537(15) 0.0396(6) Uani 1 1 d . . .
N11 N -0.3452(2) 0.4545(2) 1.16312(15) 0.0368(6) Uani 1 1 d . . .
N12 N -0.29468(18) 0.42621(19) 1.09428(14) 0.0314(5) Uani 1 1 d . . .
N13 N 0.94160(19) 0.12122(18) -0.04690(13) 0.0304(5) Uani 1 1 d . . .
N14 N 1.03033(19) 0.09870(18) -0.08955(14) 0.0311(5) Uani 1 1 d . . .
N15 N 0.9335(2) 0.0840(2) -0.18953(14) 0.0359(6) Uani 1 1 d . . .
N16 N 0.9705(2) 0.0664(2) -0.26203(15) 0.0413(7) Uani 1 1 d . . .
N17 N 1.0749(2) 0.0579(2) -0.28005(15) 0.0444(7) Uani 1 1 d . . .
N18 N 1.1095(2) 0.0700(2) -0.21789(15) 0.0393(6) Uani 1 1 d . . .
N19 N -0.05053(18) 0.10889(17) 0.54696(14) 0.0280(5) Uani 1 1 d . . .
N20 N -0.14395(18) 0.11573(18) 0.53478(13) 0.0284(5) Uani 1 1 d . . .
N21 N -0.19457(19) 0.06317(18) 0.66892(14) 0.0303(5) Uani 1 1 d . . .
N22 N -0.2849(2) 0.0358(2) 0.71359(14) 0.0375(6) Uani 1 1 d . . .
N23 N -0.3566(2) 0.0418(2) 0.67253(15) 0.0382(6) Uani 1 1 d . . .
N24 N -0.31549(17) 0.07364(17) 0.60158(13) 0.0319(5) Uani 1 1 d . . .
H1 H 0.9487 0.4326 0.2034 0.048 Uiso 1 1 d R . .
H2 H 0.9075 0.3117 0.7813 0.048 Uiso 1 1 d R . .
H3 H 1.1269 0.3504 0.6538 0.048 Uiso 1 1 d R . .
H4 H 1.1365 0.3791 0.5260 0.048 Uiso 1 1 d R . .
H5 H 0.8237 0.3511 0.5576 0.048 Uiso 1 1 d R . .
H6 H 0.3887 0.3018 0.8381 0.048 Uiso 1 1 d R . .
H7 H 0.1432 0.3059 0.8126 0.048 Uiso 1 1 d R . .
H8 H -0.0085 0.3464 0.9012 0.048 Uiso 1 1 d R . .
H9 H 0.1673 0.3776 1.0529 0.048 Uiso 1 1 d R . .
H10 H 0.3369 0.2016 0.3314 0.048 Uiso 1 1 d R . .
H11 H 0.0958 0.1812 0.3044 0.048 Uiso 1 1 d R . .
H12 H -0.0480 0.1452 0.3987 0.048 Uiso 1 1 d R . .
H13 H 0.1369 0.1203 0.5522 0.048 Uiso 1 1 d R . .
H14 H 0.9304 0.0610 -0.2929 0.048 Uiso 1 1 d R . .
H15 H 0.8669 0.1984 0.2754 0.048 Uiso 1 1 d R . .
H16 H 1.0919 0.1588 0.1485 0.048 Uiso 1 1 d R . .
H17 H 1.1037 0.1259 0.0243 0.048 Uiso 1 1 d R . .
H18 H 0.7842 0.1532 0.0588 0.048 Uiso 1 1 d R . .
H13A H 0.6015 0.4695 0.7727 0.048 Uiso 1 1 d R . .
H13B H 0.5025 0.4301 0.7946 0.048 Uiso 1 1 d R . .
H14A H 0.5505 0.1761 0.8234 0.048 Uiso 1 1 d R . .
H14B H 0.6070 0.2322 0.7622 0.048 Uiso 1 1 d R . .
H15A H 0.5537 0.1779 0.9843 0.048 Uiso 1 1 d R . .
H15B H 0.6200 0.1311 0.9215 0.048 Uiso 1 1 d R . .
H16A H 0.5949 0.4435 1.0027 0.048 Uiso 1 1 d R . .
H16B H 0.5115 0.3836 1.0191 0.048 Uiso 1 1 d R . .
H17A H 0.8176 0.2274 0.9268 0.048 Uiso 1 1 d R . .
H17B H 0.8231 0.3167 0.9481 0.048 Uiso 1 1 d R . .
H18A H 0.7584 0.4857 0.8427 0.048 Uiso 1 1 d R . .
H18B H 0.6781 0.5197 0.9030 0.048 Uiso 1 1 d R . .
H19A H 0.5992 0.0044 0.3135 0.048 Uiso 1 1 d R . .
H19B H 0.4894 0.0290 0.3431 0.048 Uiso 1 1 d R . .
H20A H 0.5934 0.1208 0.5265 0.048 Uiso 1 1 d R . .
H20B H 0.4864 0.1182 0.5212 0.048 Uiso 1 1 d R . .
H21A H 0.5379 0.3647 0.4143 0.048 Uiso 1 1 d R . .
H21B H 0.5603 0.3141 0.4791 0.048 Uiso 1 1 d R . .
H22A H 0.7889 0.1998 0.4075 0.048 Uiso 1 1 d R . .
H22B H 0.7338 0.2931 0.4145 0.048 Uiso 1 1 d R . .
H23A H 0.6979 -0.0102 0.4082 0.048 Uiso 1 1 d R . .
H23B H 0.7638 0.0296 0.3434 0.048 Uiso 1 1 d R . .
H24A H 0.5478 0.2727 0.2492 0.048 Uiso 1 1 d R . .
H24B H 0.4574 0.3152 0.2903 0.048 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
Er1 O16 2.274(2) . ?
Er1 O13 2.305(2) . ?
Er1 O2 2.3125(19) . ?
Er1 O14 2.329(2) . ?
Er1 O5 2.3317(19) . ?
Er1 O15 2.341(2) . ?
Er1 O17 2.392(2) . ?
Er1 O18 2.410(2) . ?
Er2 O20 2.288(2) . ?
Er2 O19 2.306(2) . ?
Er2 O8 2.312(2) . ?
Er2 O24 2.332(2) . ?
Er2 O21 2.332(2) . ?
Er2 O22 2.375(2) . ?
Er2 O11 2.3808(19) . ?
Er2 O23 2.443(2) . ?
O1 C7 1.236(4) . ?
O2 C7 1.280(3) . ?
O3 C2 1.344(3) . ?
O3 H2 0.8239 . ?
O4 C15 1.246(3) . ?
O5 C15 1.268(3) . ?
O6 C10 1.335(3) . ?
O6 H6 0.8245 . ?
O7 C23 1.238(4) . ?
O8 C23 1.279(3) . ?
O9 C18 1.341(3) . ?
O9 H15 0.8238 . ?
O10 C31 1.242(3) . ?
O11 C31 1.272(3) . ?
O12 C26 1.338(3) . ?
O12 H10 0.8242 . ?
O13 H13A 0.8630 . ?
O13 H13B 0.8669 . ?
O14 H14A 0.8037 . ?
O14 H14B 0.8076 . ?
O15 H15A 0.8753 . ?
O15 H15B 0.8670 . ?
O16 H16A 0.8538 . ?
O16 H16B 0.8592 . ?
O17 H17A 0.8196 . ?
O17 H17B 0.8314 . ?
O18 H18A 0.8506 . ?
O18 H18B 0.8608 . ?
O19 H19A 0.8692 . ?
O19 H19B 0.8742 . ?
O20 H20A 0.8720 . ?
O20 H20B 0.8714 . ?
O21 H21A 0.7962 . ?
O21 H21B 0.8359 . ?
O22 H22A 0.8523 . ?
O22 H22B 0.8514 . ?
O23 H23A 0.8646 . ?
O23 H23B 0.8532 . ?
O24 H24A 0.8265 . ?
O24 H24B 0.8278 . ?
O25 H25A 0.8586 . ?
O25 H25B 0.8359 . ?
O26 H26A 0.8561 . ?
O26 H26B 0.8433 . ?
O27 H27B 0.8564 . ?
O27 H27A 0.7920 . ?
O28 H28A 0.9599 . ?
O28 H28B 0.8660 . ?
O29 H29B 0.8607 . ?
O29 H29A 0.8255 . ?
O30 H30A 0.8682 . ?
O30 H30B 0.8431 . ?
O31 H31A 0.8527 . ?
O31 H31B 0.8569 . ?
O32 H32A 0.8683 . ?
O32 H32B 0.8318 . ?
O33 H33B 0.8201 . ?
O33 H33A 0.7899 . ?
O34 H34A 0.9599 . ?
O34 H34B 0.9600 . ?
O35 H35B 0.8397 . ?
O35 H35A 0.8313 . ?
O36 H36A 0.8578 . ?
O36 H36B 0.8075 . ?
C1 C6 1.384(4) . ?
C1 C2 1.401(4) . ?
C1 C7 1.488(4) . ?
C2 C3 1.401(4) . ?
C3 C4 1.368(4) . ?
C3 H3 0.9334 . ?
C4 C5 1.396(4) . ?
C4 H4 0.9251 . ?
C5 C6 1.379(4) . ?
C5 N1 1.414(3) . ?
C6 H5 0.9264 . ?
C8 N3 1.322(4) . ?
C8 N6 1.340(4) . ?
C8 N2 1.405(4) . ?
C9 C14 1.385(4) . ?
C9 C10 1.406(4) . ?
C9 C15 1.490(4) . ?
C10 C11 1.404(4) . ?
C11 C12 1.362(4) . ?
C11 H7 0.9203 . ?
C12 C13 1.395(4) . ?
C12 H8 0.9252 . ?
C13 C14 1.385(4) . ?
C13 N7 1.402(3) . ?
C14 H9 0.9375 . ?
C16 N12 1.320(3) . ?
C16 N9 1.326(3) . ?
C16 N8 1.405(3) . ?
C17 C22 1.386(4) . ?
C17 C18 1.400(4) . ?
C17 C23 1.487(4) . ?
C18 C19 1.397(4) . ?
C19 C20 1.370(4) . ?
C19 H16 0.9346 . ?
C20 C21 1.397(4) . ?
C20 H17 0.9261 . ?
C21 C22 1.379(4) . ?
C21 N13 1.413(4) . ?
C22 H18 0.9255 . ?
C24 N15 1.326(4) . ?
C24 N18 1.329(4) . ?
C24 N14 1.404(4) . ?
C25 C30 1.385(4) . ?
C25 C26 1.404(4) . ?
C25 C31 1.497(4) . ?
C26 C27 1.402(4) . ?
C27 C28 1.368(4) . ?
C27 H11 0.9219 . ?
C28 C29 1.393(4) . ?
C28 H12 0.9275 . ?
C29 C30 1.389(4) . ?
C29 N19 1.401(4) . ?
C30 H13 0.9386 . ?
C32 N24 1.315(3) . ?
C32 N21 1.326(4) . ?
C32 N20 1.407(4) . ?
N1 N2 1.255(3) . ?
N3 N4 1.307(3) . ?
N4 N5 1.312(4) . ?
N4 H1 0.8542 . ?
N5 N6 1.318(4) . ?
N7 N8 1.261(3) . ?
N9 N10 1.338(3) . ?
N10 N11 1.308(4) . ?
N11 N12 1.338(3) . ?
N13 N14 1.253(3) . ?
N15 N16 1.326(3) . ?
N16 N17 1.308(4) . ?
N16 H14 0.8536 . ?
N17 N18 1.328(4) . ?
N19 N20 1.264(3) . ?
N21 N22 1.339(3) . ?
N22 N23 1.300(4) . ?
N23 N24 1.337(3) . ?

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
O16 Er1 O13 103.51(9) . . ?
O16 Er1 O2 144.80(7) . . ?
O13 Er1 O2 81.86(8) . . ?
O16 Er1 O14 140.31(8) . . ?
O13 Er1 O14 83.74(9) . . ?
O2 Er1 O14 74.44(8) . . ?
O16 Er1 O5 73.50(7) . . ?
O13 Er1 O5 71.69(8) . . ?
O2 Er1 O5 138.98(7) . . ?
O14 Er1 O5 72.04(8) . . ?
O16 Er1 O15 81.35(9) . . ?
O13 Er1 O15 147.61(9) . . ?
O2 Er1 O15 112.76(8) . . ?
O14 Er1 O15 73.54(9) . . ?
O5 Er1 O15 79.41(8) . . ?
O16 Er1 O17 82.34(7) . . ?
O13 Er1 O17 138.88(8) . . ?
O2 Er1 O17 72.22(7) . . ?
O14 Er1 O17 117.71(8) . . ?
O5 Er1 O17 145.81(8) . . ?
O15 Er1 O17 73.25(8) . . ?
O16 Er1 O18 72.29(8) . . ?
O13 Er1 O18 75.07(9) . . ?
O2 Er1 O18 75.78(7) . . ?
O14 Er1 O18 145.46(8) . . ?
O5 Er1 O18 124.12(7) . . ?
O15 Er1 O18 135.30(9) . . ?
O17 Er1 O18 68.05(8) . . ?
O20 Er2 O19 96.19(8) . . ?
O20 Er2 O8 142.37(7) . . ?
O19 Er2 O8 83.78(8) . . ?
O20 Er2 O24 143.11(7) . . ?
O19 Er2 O24 84.93(9) . . ?
O8 Er2 O24 74.50(8) . . ?
O20 Er2 O21 83.25(8) . . ?
O19 Er2 O21 146.49(8) . . ?
O8 Er2 O21 116.65(8) . . ?
O24 Er2 O21 76.40(8) . . ?
O20 Er2 O22 81.95(7) . . ?
O19 Er2 O22 142.54(8) . . ?
O8 Er2 O22 76.08(8) . . ?
O24 Er2 O22 118.51(9) . . ?
O21 Er2 O22 70.77(8) . . ?
O20 Er2 O11 74.49(7) . . ?
O19 Er2 O11 71.19(7) . . ?
O8 Er2 O11 138.63(7) . . ?
O24 Er2 O11 71.03(8) . . ?
O21 Er2 O11 76.48(8) . . ?
O22 Er2 O11 141.48(7) . . ?
O20 Er2 O23 71.47(7) . . ?
O19 Er2 O23 73.84(8) . . ?
O8 Er2 O23 72.47(7) . . ?
O24 Er2 O23 142.23(7) . . ?
O21 Er2 O23 135.68(7) . . ?
O22 Er2 O23 70.12(7) . . ?
O11 Er2 O23 127.29(7) . . ?
C7 O2 Er1 137.83(18) . . ?
C2 O3 H2 110.0 . . ?
C15 O5 Er1 145.10(18) . . ?
C10 O6 H6 109.1 . . ?
C23 O8 Er2 133.87(19) . . ?
C18 O9 H15 110.0 . . ?
C31 O11 Er2 141.80(17) . . ?
C26 O12 H10 108.8 . . ?
Er1 O13 H13A 109.6 . . ?
Er1 O13 H13B 110.4 . . ?
H13A O13 H13B 109.1 . . ?
Er1 O14 H14A 121.5 . . ?
Er1 O14 H14B 113.1 . . ?
H14A O14 H14B 122.1 . . ?
Er1 O15 H15A 110.9 . . ?
Er1 O15 H15B 110.9 . . ?
H15A O15 H15B 108.4 . . ?
Er1 O16 H16A 110.2 . . ?
Er1 O16 H16B 110.3 . . ?
H16A O16 H16B 109.2 . . ?
Er1 O17 H17A 120.5 . . ?
Er1 O17 H17B 127.1 . . ?
H17A O17 H17B 107.2 . . ?
Er1 O18 H18A 110.0 . . ?
Er1 O18 H18B 109.6 . . ?
H18A O18 H18B 109.7 . . ?
Er2 O19 H19A 109.9 . . ?
Er2 O19 H19B 110.4 . . ?
H19A O19 H19B 108.1 . . ?
Er2 O20 H20A 110.6 . . ?
Er2 O20 H20B 110.9 . . ?
H20A O20 H20B 107.8 . . ?
Er2 O21 H21A 106.1 . . ?
Er2 O21 H21B 102.3 . . ?
H21A O21 H21B 116.1 . . ?
Er2 O22 H22A 109.8 . . ?
Er2 O22 H22B 109.8 . . ?
H22A O22 H22B 109.7 . . ?
Er2 O23 H23A 110.0 . . ?
Er2 O23 H23B 110.2 . . ?
H23A O23 H23B 109.4 . . ?
Er2 O24 H24A 110.8 . . ?
Er2 O24 H24B 140.0 . . ?
H24A O24 H24B 107.8 . . ?
H25A O25 H25B 111.3 . . ?
H26A O26 H26B 110.2 . . ?
H27B O27 H27A 107.9 . . ?
H28A O28 H28B 86.6 . . ?
H29B O29 H29A 99.0 . . ?
H30A O30 H30B 107.9 . . ?
H31A O31 H31B 108.6 . . ?
H32A O32 H32B 108.6 . . ?
H33B O33 H33A 119.3 . . ?
H34A O34 H34B 109.5 . . ?
H35B O35 H35A 102.8 . . ?
H36A O36 H36B 115.9 . . ?
C6 C1 C2 118.2(3) . . ?
C6 C1 C7 119.9(2) . . ?
C2 C1 C7 121.9(2) . . ?
O3 C2 C3 117.3(3) . . ?
O3 C2 C1 122.5(3) . . ?
C3 C2 C1 120.2(3) . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 120.7 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 N1 114.9(3) . . ?
C4 C5 N1 125.3(3) . . ?
C5 C6 C1 121.6(3) . . ?
C5 C6 H5 119.6 . . ?
C1 C6 H5 118.8 . . ?
O1 C7 O2 124.1(3) . . ?
O1 C7 C1 119.6(2) . . ?
O2 C7 C1 116.3(2) . . ?
N3 C8 N6 112.3(3) . . ?
N3 C8 N2 127.7(3) . . ?
N6 C8 N2 120.0(3) . . ?
C14 C9 C10 118.4(2) . . ?
C14 C9 C15 119.9(2) . . ?
C10 C9 C15 121.7(2) . . ?
O6 C10 C11 116.8(3) . . ?
O6 C10 C9 123.2(2) . . ?
C11 C10 C9 120.0(3) . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H7 119.7 . . ?
C10 C11 H7 120.0 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H8 120.3 . . ?
C13 C12 H8 119.4 . . ?
C14 C13 C12 119.5(3) . . ?
C14 C13 N7 114.1(2) . . ?
C12 C13 N7 126.5(2) . . ?
C13 C14 C9 121.5(2) . . ?
C13 C14 H9 119.1 . . ?
C9 C14 H9 119.4 . . ?
O4 C15 O5 123.5(2) . . ?
O4 C15 C9 120.1(2) . . ?
O5 C15 C9 116.4(2) . . ?
N12 C16 N9 111.7(2) . . ?
N12 C16 N8 121.2(2) . . ?
N9 C16 N8 127.1(2) . . ?
C22 C17 C18 118.4(3) . . ?
C22 C17 C23 119.6(2) . . ?
C18 C17 C23 121.9(3) . . ?
O9 C18 C19 117.6(3) . . ?
O9 C18 C17 122.3(3) . . ?
C19 C18 C17 120.1(3) . . ?
C20 C19 C18 120.6(3) . . ?
C20 C19 H16 120.0 . . ?
C18 C19 H16 119.4 . . ?
C19 C20 C21 119.6(3) . . ?
C19 C20 H17 119.9 . . ?
C21 C20 H17 120.5 . . ?
C22 C21 C20 119.8(3) . . ?
C22 C21 N13 115.4(2) . . ?
C20 C21 N13 124.7(3) . . ?
O7 C23 O8 123.6(3) . . ?
O7 C23 C17 119.6(3) . . ?
O8 C23 C17 116.8(3) . . ?
C21 C22 C17 121.4(3) . . ?
C21 C22 H18 119.7 . . ?
C17 C22 H18 118.9 . . ?
N15 C24 N18 112.3(3) . . ?
N15 C24 N14 127.5(3) . . ?
N18 C24 N14 120.2(3) . . ?
C30 C25 C26 118.2(2) . . ?
C30 C25 C31 120.2(2) . . ?
C26 C25 C31 121.5(2) . . ?
O12 C26 C27 117.0(2) . . ?
O12 C26 C25 122.4(2) . . ?
C27 C26 C25 120.7(3) . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H11 119.9 . . ?
C26 C27 H11 120.2 . . ?
C27 C28 C29 119.9(3) . . ?
C27 C28 H12 120.7 . . ?
C29 C28 H12 119.4 . . ?
C30 C29 C28 120.2(3) . . ?
C30 C29 N19 114.1(2) . . ?
C28 C29 N19 125.7(2) . . ?
C25 C30 C29 120.9(3) . . ?
C25 C30 H13 119.7 . . ?
C29 C30 H13 119.4 . . ?
O10 C31 O11 124.3(2) . . ?
O10 C31 C25 119.7(2) . . ?
O11 C31 C25 115.9(2) . . ?
N24 C32 N21 110.4(2) . . ?
N24 C32 N20 122.5(2) . . ?
N21 C32 N20 127.0(2) . . ?
N2 N1 C5 115.8(2) . . ?
N1 N2 C8 110.9(2) . . ?
N4 N3 C8 102.1(2) . . ?
N3 N4 N5 113.8(2) . . ?
N3 N4 H1 122.6 . . ?
N5 N4 H1 123.6 . . ?
N4 N5 N6 106.3(2) . . ?
N5 N6 C8 105.5(2) . . ?
N8 N7 C13 116.1(2) . . ?
N7 N8 C16 110.6(2) . . ?
C16 N9 N10 105.2(2) . . ?
N11 N10 N9 108.7(2) . . ?
N10 N11 N12 109.8(2) . . ?
C16 N12 N11 104.7(2) . . ?
N14 N13 C21 115.7(2) . . ?
N13 N14 C24 112.6(2) . . ?
C24 N15 N16 102.9(2) . . ?
N17 N16 N15 112.0(2) . . ?
N17 N16 H14 124.4 . . ?
N15 N16 H14 123.6 . . ?
N16 N17 N18 107.5(2) . . ?
N17 N18 C24 105.4(2) . . ?
N20 N19 C29 115.8(2) . . ?
N19 N20 C32 109.8(2) . . ?
C32 N21 N22 106.4(2) . . ?
N23 N22 N21 107.7(2) . . ?
N22 N23 N24 110.2(2) . . ?
C32 N24 N23 105.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 975945'
#######################################################################
#
#                 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 Er2 N24 O26'
_chemical_formula_weight         1517.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.7064(14)
_cell_length_b                   12.0080(17)
_cell_length_c                   12.7434(18)
_cell_angle_alpha                110.523(6)
_cell_angle_beta                 94.782(7)
_cell_angle_gamma                105.108(7)
_cell_volume                     1317.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             750.0
_exptl_absorpt_coefficient_mu    3.272
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.346
_exptl_absorpt_correction_T_max  0.537
_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            20387
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0253
_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         1.74
_diffrn_reflns_theta_max         27.58
_reflns_number_total             6112
_reflns_number_gt                5600
_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)+(0.0261P)²+1.2180P] 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       0.00011(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6112
_refine_ls_number_parameters     383
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0220
_refine_ls_wR_factor_ref         0.0539
_refine_ls_wR_factor_gt          0.0529
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.010

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.973876(12) 0.702262(11) 0.619475(9) 0.02223(5) Uani 1 1 d . . .
N1 N 0.5939(3) 1.1246(2) 0.9590(2) 0.0295(5) Uani 1 1 d . . .
N2 N 0.4944(3) 1.1730(2) 0.9856(2) 0.0297(5) Uani 1 1 d . . .
N3 N 0.6180(2) 1.2516(2) 1.1843(2) 0.0280(5) Uani 1 1 d . . .
N4 N 0.5856(3) 1.3189(2) 1.2809(2) 0.0312(5) Uani 1 1 d . . .
N5 N 0.4657(3) 1.3451(2) 1.2578(2) 0.0328(5) Uani 1 1 d . . .
N6 N 0.4170(3) 1.2956(2) 1.1452(2) 0.0321(5) Uani 1 1 d . . .
N7 N 0.8204(3) 0.3679(2) -0.08419(19) 0.0301(5) Uani 1 1 d . . .
N8 N 0.9072(3) 0.3063(2) -0.08061(19) 0.0295(5) Uani 1 1 d . . .
N9 N 1.0044(3) 0.1567(2) -0.1990(2) 0.0341(5) Uani 1 1 d . . .
N10 N 0.9941(3) 0.1006(2) -0.3108(2) 0.0385(6) Uani 1 1 d . . .
N11 N 0.9093(3) 0.1419(2) -0.3635(2) 0.0385(6) Uani 1 1 d . . .
H2 H 0.8879 0.1183 -0.4364 0.046 Uiso 1 1 calc R . .
N12 N 0.8609(3) 0.2248(2) -0.28909(19) 0.0329(5) Uani 1 1 d . . .
C1 C 0.6766(3) 0.9177(2) 0.7032(2) 0.0243(5) Uani 1 1 d . . .
C2 C 0.5736(3) 0.9130(3) 0.6168(2) 0.0283(6) Uani 1 1 d . . .
C3 C 0.4762(3) 0.9817(3) 0.6441(3) 0.0375(7) Uani 1 1 d . . .
H3 H 0.4085 0.9788 0.5863 0.045 Uiso 1 1 calc R . .
C4 C 0.4798(3) 1.0526(3) 0.7544(3) 0.0354(7) Uani 1 1 d . . .
H4 H 0.4154 1.0988 0.7719 0.043 Uiso 1 1 calc R . .
C5 C 0.5804(3) 1.0564(3) 0.8420(2) 0.0279(6) Uani 1 1 d . . .
C6 C 0.6790(3) 0.9897(2) 0.8149(2) 0.0253(5) Uani 1 1 d . . .
H6 H 0.7474 0.9939 0.8729 0.030 Uiso 1 1 calc R . .
C7 C 0.7807(3) 0.8444(2) 0.6747(2) 0.0245(5) Uani 1 1 d . . .
C8 C 0.5132(3) 1.2390(3) 1.1033(2) 0.0267(6) Uani 1 1 d . . .
C9 C 0.8382(3) 0.5277(2) 0.2277(2) 0.0230(5) Uani 1 1 d . . .
C10 C 0.7436(3) 0.5990(3) 0.2234(2) 0.0291(6) Uani 1 1 d . . .
C11 C 0.6791(3) 0.5903(3) 0.1178(3) 0.0355(7) Uani 1 1 d . . .
H11 H 0.6168 0.6367 0.1144 0.043 Uiso 1 1 calc R . .
C12 C 0.7068(3) 0.5143(3) 0.0195(2) 0.0337(6) Uani 1 1 d . . .
H12 H 0.6630 0.5092 -0.0504 0.040 Uiso 1 1 calc R . .
C13 C 0.8002(3) 0.4439(3) 0.0225(2) 0.0275(6) Uani 1 1 d . . .
C14 C 0.8644(3) 0.4516(3) 0.1273(2) 0.0260(5) Uani 1 1 d . . .
H14 H 0.9261 0.4045 0.1297 0.031 Uiso 1 1 calc R . .
C15 C 0.9091(3) 0.5301(2) 0.3371(2) 0.0226(5) Uani 1 1 d . . .
C16 C 0.9218(3) 0.2321(3) -0.1889(2) 0.0272(6) Uani 1 1 d . . .
O1 O 0.8778(2) 0.85108(18) 0.75018(16) 0.0279(4) Uani 1 1 d . . .
O2 O 0.7700(2) 0.77414(19) 0.57194(16) 0.0318(4) Uani 1 1 d . . .
O3 O 0.5657(2) 0.8451(2) 0.50643(17) 0.0410(5) Uani 1 1 d . . .
H1 H 0.6317 0.8137 0.5001 0.062 Uiso 1 1 calc R . .
O4 O 0.9802(2) 0.45631(18) 0.33458(16) 0.0293(4) Uani 1 1 d . . .
O5 O 0.8937(2) 0.60873(19) 0.42819(16) 0.0314(4) Uani 1 1 d . . .
O6 O 0.7109(3) 0.6735(2) 0.31589(18) 0.0446(6) Uani 1 1 d . . .
H5 H 0.7541 0.6714 0.3730 0.067 Uiso 1 1 calc R . .
O7 O 0.7663(2) 0.5835(2) 0.6564(2) 0.0431(6) Uani 1 1 d . . .
H7 H 0.7553 0.5085 0.6441 0.065 Uiso 1 1 d R . .
H8 H 0.6902 0.6003 0.6690 0.065 Uiso 1 1 d R . .
O8 O 1.1300(2) 0.80462(19) 0.79619(16) 0.0290(4) Uani 1 1 d . . .
H9 H 1.2077 0.7833 0.7928 0.044 Uiso 1 1 d R . .
H10 H 1.1524 0.8839 0.8148 0.044 Uiso 1 1 d R . .
O9 O 1.1928(2) 0.6821(2) 0.56152(17) 0.0368(5) Uani 1 1 d . . .
H13 H 1.2108 0.6215 0.5736 0.055 Uiso 1 1 d R . .
H15 H 1.1845 0.6677 0.4906 0.055 Uiso 1 1 d R . .
O10 O 1.0785(2) 0.88479(19) 0.58965(17) 0.0327(4) Uani 1 1 d . . .
H17 H 1.1670 0.9020 0.6168 0.049 Uiso 1 1 d R . .
H16 H 1.0556 0.9509 0.6196 0.049 Uiso 1 1 d R . .
O11 O 0.1791(2) 0.05232(19) 0.90408(19) 0.0500(6) Uani 1 1 d G . .
H18 H 0.1300 0.0809 0.8749 0.075 Uiso 1 1 d G . .
H19 H 0.2688 0.0974 0.9208 0.075 Uiso 1 1 d G . .
O12 O 0.8941(3) 0.75255(17) 0.9253(2) 0.0812(10) Uani 1 1 d G . .
H20 H 0.9489 0.8273 0.9663 0.122 Uiso 1 1 d G . .
H21 H 0.8861 0.7597 0.8571 0.122 Uiso 1 1 d G . .
O13 O 0.6979(2) 0.34216(18) 0.63188(15) 0.0473(6) Uani 1 1 d G . .
H22 H 0.7436 0.3115 0.6685 0.071 Uiso 1 1 d G . .
H23 H 0.6126 0.2918 0.6012 0.071 Uiso 1 1 d G . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O5 2.2621(19) . ?
Er1 O4 2.3126(19) 2_766 ?
Er1 O8 2.3233(19) . ?
Er1 O7 2.334(2) . ?
Er1 O10 2.338(2) . ?
Er1 O9 2.350(2) . ?
Er1 O1 2.4243(18) . ?
Er1 O2 2.4669(19) . ?
Er1 C7 2.823(3) . ?
N1 N2 1.262(3) . ?
N1 C5 1.402(4) . ?
N2 C8 1.399(4) . ?
N3 C8 1.326(4) . ?
N3 N4 1.330(3) . ?
N4 N5 1.319(3) . ?
N5 N6 1.333(3) . ?
N6 C8 1.334(3) . ?
N7 N8 1.266(3) . ?
N7 C13 1.410(3) . ?
N8 C16 1.398(3) . ?
N9 N10 1.327(3) . ?
N9 C16 1.340(4) . ?
N10 N11 1.314(4) . ?
N11 N12 1.329(3) . ?
N11 H2 0.8600 . ?
N12 C16 1.325(4) . ?
C1 C6 1.377(4) . ?
C1 C2 1.400(4) . ?
C1 C7 1.492(3) . ?
C2 O3 1.339(3) . ?
C2 C3 1.399(4) . ?
C3 C4 1.356(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(4) . ?
C6 H6 0.9300 . ?
C7 O1 1.255(3) . ?
C7 O2 1.263(3) . ?
C9 C14 1.376(4) . ?
C9 C10 1.418(4) . ?
C9 C15 1.490(4) . ?
C10 O6 1.328(3) . ?
C10 C11 1.393(4) . ?
C11 C12 1.362(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.398(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.387(4) . ?
C14 H14 0.9300 . ?
C15 O4 1.250(3) . ?
C15 O5 1.263(3) . ?
O3 H1 0.8200 . ?
O4 Er1 2.3126(19) 2_766 ?
O6 H5 0.8200 . ?
O7 H7 0.8336 . ?
O7 H8 0.8290 . ?
O8 H9 0.8568 . ?
O8 H10 0.8568 . ?
O9 H13 0.8507 . ?
O9 H15 0.8509 . ?
O10 H17 0.8421 . ?
O10 H16 0.8471 . ?
O11 H18 0.7934 . ?
O11 H19 0.8598 . ?
O12 H20 0.8592 . ?
O12 H21 0.9013 . ?
O13 H22 0.8499 . ?
O13 H23 0.8500 . ?

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 Er1 O4 102.80(7) . 2_766 ?
O5 Er1 O8 160.85(7) . . ?
O4 Er1 O8 75.38(7) 2_766 . ?
O5 Er1 O7 92.93(8) . . ?
O4 Er1 O7 68.84(7) 2_766 . ?
O8 Er1 O7 103.82(8) . . ?
O5 Er1 O10 86.51(7) . . ?
O4 Er1 O10 145.07(7) 2_766 . ?
O8 Er1 O10 84.97(7) . . ?
O7 Er1 O10 145.15(7) . . ?
O5 Er1 O9 80.49(7) . . ?
O4 Er1 O9 73.56(7) 2_766 . ?
O8 Er1 O9 80.75(7) . . ?
O7 Er1 O9 139.28(8) . . ?
O10 Er1 O9 74.99(8) . . ?
O5 Er1 O1 125.07(6) . . ?
O4 Er1 O1 119.78(7) 2_766 . ?
O8 Er1 O1 69.60(6) . . ?
O7 Er1 O1 74.00(7) . . ?
O10 Er1 O1 77.94(7) . . ?
O9 Er1 O1 141.20(7) . . ?
O5 Er1 O2 72.26(6) . . ?
O4 Er1 O2 140.87(7) 2_766 . ?
O8 Er1 O2 121.34(6) . . ?
O7 Er1 O2 72.63(7) . . ?
O10 Er1 O2 74.06(7) . . ?
O9 Er1 O2 139.55(7) . . ?
O1 Er1 O2 52.83(6) . . ?
O5 Er1 C7 98.80(7) . . ?
O4 Er1 C7 135.01(7) 2_766 . ?
O8 Er1 C7 95.42(7) . . ?
O7 Er1 C7 71.09(7) . . ?
O10 Er1 C7 74.57(7) . . ?
O9 Er1 C7 149.54(8) . . ?
O1 Er1 C7 26.29(7) . . ?
O2 Er1 C7 26.54(7) . . ?
N2 N1 C5 115.3(2) . . ?
N1 N2 C8 112.7(2) . . ?
C8 N3 N4 104.3(2) . . ?
N5 N4 N3 109.6(2) . . ?
N4 N5 N6 109.6(2) . . ?
N5 N6 C8 103.9(2) . . ?
N8 N7 C13 115.7(2) . . ?
N7 N8 C16 113.0(2) . . ?
N10 N9 C16 104.4(2) . . ?
N11 N10 N9 108.7(2) . . ?
N10 N11 N12 111.0(2) . . ?
N10 N11 H2 124.5 . . ?
N12 N11 H2 124.5 . . ?
C16 N12 N11 103.3(2) . . ?
C6 C1 C2 118.9(2) . . ?
C6 C1 C7 120.6(2) . . ?
C2 C1 C7 120.5(2) . . ?
O3 C2 C3 117.9(3) . . ?
O3 C2 C1 121.9(2) . . ?
C3 C2 C1 120.2(3) . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.1(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 N1 114.9(2) . . ?
C4 C5 N1 125.5(2) . . ?
C1 C6 C5 120.8(3) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
O1 C7 O2 119.6(2) . . ?
O1 C7 C1 121.7(2) . . ?
O2 C7 C1 118.8(2) . . ?
O1 C7 Er1 58.82(13) . . ?
O2 C7 Er1 60.78(13) . . ?
C1 C7 Er1 179.1(2) . . ?
N3 C8 N6 112.6(2) . . ?
N3 C8 N2 127.4(2) . . ?
N6 C8 N2 120.0(2) . . ?
C14 C9 C10 119.2(2) . . ?
C14 C9 C15 118.2(2) . . ?
C10 C9 C15 122.6(2) . . ?
O6 C10 C11 117.4(3) . . ?
O6 C10 C9 123.1(2) . . ?
C11 C10 C9 119.4(3) . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.9(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 N7 124.7(3) . . ?
C12 C13 N7 116.1(2) . . ?
C9 C14 C13 121.0(3) . . ?
C9 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
O4 C15 O5 123.8(2) . . ?
O4 C15 C9 119.4(2) . . ?
O5 C15 C9 116.9(2) . . ?
N12 C16 N9 112.6(2) . . ?
N12 C16 N8 127.5(3) . . ?
N9 C16 N8 119.9(2) . . ?
C7 O1 Er1 94.89(15) . . ?
C7 O2 Er1 92.67(16) . . ?
C2 O3 H1 109.5 . . ?
C15 O4 Er1 151.79(18) . 2_766 ?
C15 O5 Er1 144.18(17) . . ?
C10 O6 H5 109.5 . . ?
Er1 O7 H7 119.6 . . ?
Er1 O7 H8 128.7 . . ?
H7 O7 H8 110.6 . . ?
Er1 O8 H9 109.8 . . ?
Er1 O8 H10 109.5 . . ?
H9 O8 H10 109.1 . . ?
Er1 O9 H13 109.2 . . ?
Er1 O9 H15 109.4 . . ?
H13 O9 H15 109.5 . . ?
Er1 O10 H17 101.9 . . ?
Er1 O10 H16 122.3 . . ?
H17 O10 H16 106.8 . . ?
H18 O11 H19 110.5 . . ?
H20 O12 H21 98.3 . . ?
H22 O13 H23 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 975946'
#######################################################################
#
#                 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 Ho2 N24 O26'
_chemical_formula_weight         1512.79

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'
Ho Ho -0.2175 4.6783 '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           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.6936(4)
_cell_length_b                   11.9920(4)
_cell_length_c                   12.8118(4)
_cell_angle_alpha                110.378(3)
_cell_angle_beta                 94.930(4)
_cell_angle_gamma                104.916(3)
_cell_volume                     1323.48(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8330
_cell_measurement_theta_min      1.40
_cell_measurement_theta_max      27.60

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748.0
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            20025
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0408
_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         1.73
_diffrn_reflns_theta_max         27.60
_reflns_number_total             6153
_reflns_number_gt                5424
_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)+(0.0740P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0011(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6153
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.1058
_refine_ls_wR_factor_gt          0.1015
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.023
_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
Ho1 Ho 0.472897(18) 0.200569(18) 1.118888(14) 0.02301(9) Uani 1 1 d . . .
O1 O 0.3763(3) 0.3509(3) 1.2506(2) 0.0279(7) Uani 1 1 d . . .
O2 O 0.2686(3) 0.2739(3) 1.0723(3) 0.0318(7) Uani 1 1 d . . .
O3 O 0.0662(4) 0.3462(4) 1.0069(3) 0.0422(9) Uani 1 1 d . . .
H1 H 0.1261 0.3081 1.0013 0.063 Uiso 1 1 calc R . .
O4 O 0.4799(3) -0.0425(3) 0.8324(3) 0.0313(7) Uani 1 1 d . . .
O5 O 0.3929(3) 0.1091(3) 0.9255(2) 0.0306(7) Uani 1 1 d . . .
O6 O 0.2116(4) 0.1741(4) 0.8132(3) 0.0456(10) Uani 1 1 d . . .
H2 H 0.2734 0.1906 0.8687 0.068 Uiso 1 1 calc R . .
O7 O 0.6308(3) 0.3051(3) 1.2977(3) 0.0287(7) Uani 1 1 d . . .
O8 O 0.2639(4) 0.0812(3) 1.1578(3) 0.0416(9) Uani 1 1 d . . .
O9 O 0.5797(4) 0.3856(3) 1.0894(3) 0.0339(7) Uani 1 1 d G . .
O10 O 0.6918(3) 0.1771(4) 1.0604(3) 0.0373(8) Uani 1 1 d . . .
O11 O 0.3966(6) 0.2555(7) 0.4265(4) 0.0772(17) Uani 1 1 d G . .
H27 H 0.4570 0.2800 0.3902 0.116 Uiso 1 1 d G . .
H28 H 0.3079 0.2377 0.3917 0.116 Uiso 1 1 d G . .
O12 O 0.6792(4) 0.5526(4) 0.4039(3) 0.0461(9) Uani 1 1 d . . .
O13 O 0.1975(4) 0.8400(4) 0.1310(3) 0.0458(9) Uani 1 1 d . . .
C1 C 0.1769(4) 0.4173(4) 1.2029(3) 0.0231(8) Uani 1 1 d . . .
C2 C 0.0733(5) 0.4135(4) 1.1173(4) 0.0284(9) Uani 1 1 d . . .
C3 C -0.0235(5) 0.4821(5) 1.1445(4) 0.0369(11) Uani 1 1 d . . .
H3 H -0.0906 0.4804 1.0871 0.044 Uiso 1 1 calc R . .
C4 C -0.0204(5) 0.5518(5) 1.2548(4) 0.0353(11) Uani 1 1 d . . .
H4 H -0.0858 0.5971 1.2725 0.042 Uiso 1 1 calc R . .
C5 C 0.0812(5) 0.5558(4) 1.3420(4) 0.0270(9) Uani 1 1 d . . .
C6 C 0.1787(5) 0.4894(4) 1.3145(4) 0.0258(9) Uani 1 1 d . . .
H5 H 0.2471 0.4930 1.3721 0.031 Uiso 1 1 calc R . .
C7 C 0.2801(4) 0.3449(4) 1.1750(4) 0.0245(9) Uani 1 1 d . . .
C8 C 0.0136(4) 0.7392(4) 1.6023(4) 0.0266(9) Uani 1 1 d . . .
C9 C 0.3371(4) 0.0275(4) 0.7257(3) 0.0232(8) Uani 1 1 d . . .
C10 C 0.2436(5) 0.0988(4) 0.7205(4) 0.0275(9) Uani 1 1 d . . .
C11 C 0.1797(5) 0.0899(5) 0.6155(4) 0.0353(11) Uani 1 1 d . . .
H6 H 0.1176 0.1366 0.6120 0.042 Uiso 1 1 calc R . .
C12 C 0.2066(5) 0.0139(5) 0.5176(4) 0.0343(11) Uani 1 1 d . . .
H7 H 0.1626 0.0092 0.4482 0.041 Uiso 1 1 calc R . .
C13 C 0.2991(5) -0.0567(4) 0.5204(4) 0.0280(9) Uani 1 1 d . . .
C14 C 0.3640(5) -0.0486(4) 0.6252(3) 0.0254(9) Uani 1 1 d . . .
H8 H 0.4265 -0.0952 0.6278 0.030 Uiso 1 1 calc R . .
C15 C 0.4078(4) 0.0302(4) 0.8348(3) 0.0221(8) Uani 1 1 d . . .
C16 C 0.4217(5) -0.2685(4) 0.3110(4) 0.0269(9) Uani 1 1 d . . .
N1 N 0.0941(4) 0.6246(4) 1.4591(3) 0.0295(8) Uani 1 1 d . . .
N2 N -0.0060(4) 0.6722(4) 1.4848(3) 0.0299(8) Uani 1 1 d . . .
N3 N 0.1182(4) 0.7517(4) 1.6832(3) 0.0288(8) Uani 1 1 d . . .
N4 N 0.0863(4) 0.8192(4) 1.7796(3) 0.0306(8) Uani 1 1 d . . .
N5 N -0.0337(4) 0.8451(4) 1.7563(3) 0.0323(9) Uani 1 1 d . . .
N6 N -0.0821(4) 0.7957(4) 1.6446(3) 0.0315(9) Uani 1 1 d . . .
N7 N 0.3204(4) -0.1328(4) 0.4141(3) 0.0314(8) Uani 1 1 d . . .
N8 N 0.4058(4) -0.1947(4) 0.4182(3) 0.0289(8) Uani 1 1 d . . .
N9 N 0.5039(4) -0.3437(4) 0.3020(3) 0.0353(9) Uani 1 1 d . . .
N10 N 0.4941(5) -0.3998(4) 0.1891(4) 0.0387(10) Uani 1 1 d . . .
N11 N 0.4102(5) -0.3588(4) 0.1364(3) 0.0370(10) Uani 1 1 d . . .
H9 H 0.3896 -0.3821 0.0639 0.044 Uiso 1 1 calc R . .
N12 N 0.3608(4) -0.2759(4) 0.2100(3) 0.0325(9) Uani 1 1 d . . .
H8A H 0.2422 0.0038 1.1435 0.049 Uiso 1 1 d R . .
H8B H 0.1868 0.1026 1.1678 0.049 Uiso 1 1 d R . .
H10A H 0.7670 0.1883 1.1055 0.049 Uiso 1 1 d R . .
H10B H 0.7166 0.1908 1.0026 0.049 Uiso 1 1 d R . .
H13A H 0.1140 0.7864 0.0990 0.049 Uiso 1 1 d R . .
H13B H 0.2447 0.8120 0.1696 0.049 Uiso 1 1 d R . .
H7A H 0.7035 0.2830 1.3139 0.049 Uiso 1 1 d R . .
H7B H 0.6460 0.3815 1.3372 0.049 Uiso 1 1 d R . .
H12A H 0.6564 0.5898 0.3646 0.049 Uiso 1 1 d R . .
H12B H 0.7694 0.5848 0.4324 0.049 Uiso 1 1 d R . .
H9A H 0.6618 0.3884 1.1042 0.049 Uiso 1 1 d R . .
H9B H 0.5564 0.4481 1.1223 0.049 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
Ho1 O5 2.298(3) . ?
Ho1 O4 2.327(3) 2_657 ?
Ho1 O7 2.360(3) . ?
Ho1 O8 2.362(3) . ?
Ho1 O10 2.362(3) . ?
Ho1 O9 2.369(4) . ?
Ho1 O1 2.449(3) . ?
Ho1 O2 2.472(3) . ?
Ho1 C7 2.835(4) . ?
O1 C7 1.255(5) . ?
O2 C7 1.271(5) . ?
O3 C2 1.347(5) . ?
O3 H1 0.8200 . ?
O4 C15 1.244(5) . ?
O4 Ho1 2.327(3) 2_657 ?
O5 C15 1.265(5) . ?
O6 C10 1.336(5) . ?
O6 H2 0.8200 . ?
O7 H7A 0.8489 . ?
O7 H7B 0.8430 . ?
O8 H8A 0.8457 . ?
O8 H8B 0.8560 . ?
O9 H9A 0.7918 . ?
O9 H9B 0.8205 . ?
O10 H10A 0.8405 . ?
O10 H10B 0.8529 . ?
O11 H27 0.8369 . ?
O11 H28 0.8703 . ?
O12 H12A 0.8308 . ?
O12 H12B 0.8481 . ?
O13 H13A 0.8532 . ?
O13 H13B 0.8500 . ?
C1 C6 1.386(6) . ?
C1 C2 1.402(6) . ?
C1 C7 1.475(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.362(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.378(6) . ?
C5 N1 1.415(5) . ?
C6 H5 0.9300 . ?
C8 N3 1.326(5) . ?
C8 N6 1.329(5) . ?
C8 N2 1.406(6) . ?
C9 C14 1.386(6) . ?
C9 C10 1.409(6) . ?
C9 C15 1.489(6) . ?
C10 C11 1.388(6) . ?
C11 C12 1.362(7) . ?
C11 H6 0.9300 . ?
C12 C13 1.388(7) . ?
C12 H7 0.9300 . ?
C13 C14 1.393(6) . ?
C13 N7 1.418(6) . ?
C14 H8 0.9300 . ?
C16 N9 1.331(6) . ?
C16 N12 1.340(6) . ?
C16 N8 1.398(6) . ?
N1 N2 1.259(5) . ?
N3 N4 1.331(5) . ?
N4 N5 1.316(5) . ?
N5 N6 1.330(5) . ?
N7 N8 1.254(5) . ?
N9 N10 1.349(6) . ?
N10 N11 1.304(6) . ?
N11 N12 1.333(5) . ?
N11 H9 0.8600 . ?

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 Ho1 O4 104.38(11) . 2_657 ?
O5 Ho1 O7 160.71(12) . . ?
O4 Ho1 O7 75.03(11) 2_657 . ?
O5 Ho1 O8 94.15(13) . . ?
O4 Ho1 O8 68.59(12) 2_657 . ?
O7 Ho1 O8 103.26(13) . . ?
O5 Ho1 O10 80.07(11) . . ?
O4 Ho1 O10 73.21(12) 2_657 . ?
O7 Ho1 O10 81.38(11) . . ?
O8 Ho1 O10 138.55(13) . . ?
O5 Ho1 O9 85.79(12) . . ?
O4 Ho1 O9 144.73(12) 2_657 . ?
O7 Ho1 O9 84.53(12) . . ?
O8 Ho1 O9 145.43(12) . . ?
O10 Ho1 O9 75.56(12) . . ?
O5 Ho1 O1 124.96(10) . . ?
O4 Ho1 O1 118.93(11) 2_657 . ?
O7 Ho1 O1 68.97(10) . . ?
O8 Ho1 O1 73.79(12) . . ?
O10 Ho1 O1 141.78(12) . . ?
O9 Ho1 O1 78.04(11) . . ?
O5 Ho1 O2 72.21(10) . . ?
O4 Ho1 O2 141.03(12) 2_657 . ?
O7 Ho1 O2 120.66(10) . . ?
O8 Ho1 O2 72.91(12) . . ?
O10 Ho1 O2 140.02(12) . . ?
O9 Ho1 O2 74.22(11) . . ?
O1 Ho1 O2 52.80(10) . . ?
O5 Ho1 C7 98.80(12) . . ?
O4 Ho1 C7 134.62(12) 2_657 . ?
O7 Ho1 C7 94.64(12) . . ?
O8 Ho1 C7 71.31(12) . . ?
O10 Ho1 C7 150.07(13) . . ?
O9 Ho1 C7 74.54(12) . . ?
O1 Ho1 C7 26.19(11) . . ?
O2 Ho1 C7 26.61(11) . . ?
C7 O1 Ho1 94.3(3) . . ?
C7 O2 Ho1 92.8(3) . . ?
C2 O3 H1 109.5 . . ?
C15 O4 Ho1 150.9(3) . 2_657 ?
C15 O5 Ho1 144.0(3) . . ?
C10 O6 H2 109.5 . . ?
Ho1 O7 H7A 121.7 . . ?
Ho1 O7 H7B 122.8 . . ?
H7A O7 H7B 109.9 . . ?
Ho1 O8 H8A 125.1 . . ?
Ho1 O8 H8B 124.5 . . ?
H8A O8 H8B 107.8 . . ?
Ho1 O9 H9A 97.0 . . ?
Ho1 O9 H9B 118.4 . . ?
H9A O9 H9B 118.1 . . ?
Ho1 O10 H10A 123.2 . . ?
Ho1 O10 H10B 122.0 . . ?
H10A O10 H10B 109.0 . . ?
H27 O11 H28 111.1 . . ?
H12A O12 H12B 108.8 . . ?
H13A O13 H13B 109.2 . . ?
C6 C1 C2 118.4(4) . . ?
C6 C1 C7 120.8(4) . . ?
C2 C1 C7 120.8(4) . . ?
O3 C2 C3 118.1(4) . . ?
O3 C2 C1 121.5(4) . . ?
C3 C2 C1 120.4(4) . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.3(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 N1 115.6(4) . . ?
C4 C5 N1 125.1(4) . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H5 119.3 . . ?
C1 C6 H5 119.3 . . ?
O1 C7 O2 120.1(4) . . ?
O1 C7 C1 121.3(4) . . ?
O2 C7 C1 118.6(4) . . ?
O1 C7 Ho1 59.5(2) . . ?
O2 C7 Ho1 60.6(2) . . ?
C1 C7 Ho1 178.6(3) . . ?
N3 C8 N6 111.8(4) . . ?
N3 C8 N2 127.7(4) . . ?
N6 C8 N2 120.4(4) . . ?
C14 C9 C10 118.7(4) . . ?
C14 C9 C15 118.6(4) . . ?
C10 C9 C15 122.7(4) . . ?
O6 C10 C11 118.1(4) . . ?
O6 C10 C9 122.5(4) . . ?
C11 C10 C9 119.4(4) . . ?
C12 C11 C10 121.0(5) . . ?
C12 C11 H6 119.5 . . ?
C10 C11 H6 119.5 . . ?
C11 C12 C13 120.7(4) . . ?
C11 C12 H7 119.6 . . ?
C13 C12 H7 119.6 . . ?
C12 C13 C14 118.9(4) . . ?
C12 C13 N7 116.5(4) . . ?
C14 C13 N7 124.7(4) . . ?
C9 C14 C13 121.3(4) . . ?
C9 C14 H8 119.4 . . ?
C13 C14 H8 119.4 . . ?
O4 C15 O5 123.6(4) . . ?
O4 C15 C9 119.0(4) . . ?
O5 C15 C9 117.4(4) . . ?
N9 C16 N12 112.7(4) . . ?
N9 C16 N8 119.9(4) . . ?
N12 C16 N8 127.5(4) . . ?
N2 N1 C5 115.3(4) . . ?
N1 N2 C8 112.3(4) . . ?
C8 N3 N4 104.9(4) . . ?
N5 N4 N3 109.2(4) . . ?
N4 N5 N6 109.6(3) . . ?
C8 N6 N5 104.6(4) . . ?
N8 N7 C13 115.7(4) . . ?
N7 N8 C16 113.1(4) . . ?
C16 N9 N10 103.9(4) . . ?
N11 N10 N9 109.1(4) . . ?
N10 N11 N12 110.9(4) . . ?
N10 N11 H9 124.5 . . ?
N12 N11 H9 124.5 . . ?
N11 N12 C16 103.4(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Ho1 O1 C7 3.1(3) . . . . ?
O4 Ho1 O1 C7 -134.0(3) 2_657 . . . ?
O7 Ho1 O1 C7 167.9(3) . . . . ?
O8 Ho1 O1 C7 -80.5(3) . . . . ?
O10 Ho1 O1 C7 126.3(3) . . . . ?
O9 Ho1 O1 C7 79.2(3) . . . . ?
O2 Ho1 O1 C7 0.1(2) . . . . ?
O5 Ho1 O2 C7 -177.5(3) . . . . ?
O4 Ho1 O2 C7 91.5(3) 2_657 . . . ?
O7 Ho1 O2 C7 -13.3(3) . . . . ?
O8 Ho1 O2 C7 82.3(3) . . . . ?
O10 Ho1 O2 C7 -129.1(3) . . . . ?
O9 Ho1 O2 C7 -86.9(3) . . . . ?
O1 Ho1 O2 C7 -0.1(2) . . . . ?
O4 Ho1 O5 C15 -34.5(5) 2_657 . . . ?
O7 Ho1 O5 C15 51.2(7) . . . . ?
O8 Ho1 O5 C15 -103.5(5) . . . . ?
O10 Ho1 O5 C15 35.2(5) . . . . ?
O9 Ho1 O5 C15 111.2(5) . . . . ?
O1 Ho1 O5 C15 -176.6(5) . . . . ?
O2 Ho1 O5 C15 -174.0(5) . . . . ?
C7 Ho1 O5 C15 -175.2(5) . . . . ?
C6 C1 C2 O3 179.4(4) . . . . ?
C7 C1 C2 O3 -1.5(7) . . . . ?
C6 C1 C2 C3 0.9(7) . . . . ?
C7 C1 C2 C3 -180.0(4) . . . . ?
O3 C2 C3 C4 -179.8(5) . . . . ?
C1 C2 C3 C4 -1.3(8) . . . . ?
C2 C3 C4 C5 0.5(8) . . . . ?
C3 C4 C5 C6 0.7(8) . . . . ?
C3 C4 C5 N1 -179.9(5) . . . . ?
C4 C5 C6 C1 -1.1(7) . . . . ?
N1 C5 C6 C1 179.5(4) . . . . ?
C2 C1 C6 C5 0.3(7) . . . . ?
C7 C1 C6 C5 -178.8(4) . . . . ?
Ho1 O1 C7 O2 -0.1(4) . . . . ?
Ho1 O1 C7 C1 178.7(4) . . . . ?
Ho1 O2 C7 O1 0.1(4) . . . . ?
Ho1 O2 C7 C1 -178.7(3) . . . . ?
C6 C1 C7 O1 -3.3(7) . . . . ?
C2 C1 C7 O1 177.6(4) . . . . ?
C6 C1 C7 O2 175.6(4) . . . . ?
C2 C1 C7 O2 -3.5(7) . . . . ?
C6 C1 C7 Ho1 122(13) . . . . ?
C2 C1 C7 Ho1 -57(13) . . . . ?
O5 Ho1 C7 O1 -177.4(3) . . . . ?
O4 Ho1 C7 O1 62.2(3) 2_657 . . . ?
O7 Ho1 C7 O1 -11.3(3) . . . . ?
O8 Ho1 C7 O1 91.1(3) . . . . ?
O10 Ho1 C7 O1 -92.1(3) . . . . ?
O9 Ho1 C7 O1 -94.3(3) . . . . ?
O2 Ho1 C7 O1 -179.9(4) . . . . ?
O5 Ho1 C7 O2 2.4(3) . . . . ?
O4 Ho1 C7 O2 -118.0(3) 2_657 . . . ?
O7 Ho1 C7 O2 168.6(3) . . . . ?
O8 Ho1 C7 O2 -89.0(3) . . . . ?
O10 Ho1 C7 O2 87.8(3) . . . . ?
O9 Ho1 C7 O2 85.5(3) . . . . ?
O1 Ho1 C7 O2 179.9(4) . . . . ?
O5 Ho1 C7 C1 57(13) . . . . ?
O4 Ho1 C7 C1 -64(13) 2_657 . . . ?
O7 Ho1 C7 C1 -137(13) . . . . ?
O8 Ho1 C7 C1 -35(13) . . . . ?
O10 Ho1 C7 C1 142(13) . . . . ?
O9 Ho1 C7 C1 140(13) . . . . ?
O1 Ho1 C7 C1 -126(13) . . . . ?
O2 Ho1 C7 C1 54(13) . . . . ?
C14 C9 C10 O6 179.8(4) . . . . ?
C15 C9 C10 O6 0.0(7) . . . . ?
C14 C9 C10 C11 0.8(7) . . . . ?
C15 C9 C10 C11 -179.0(4) . . . . ?
O6 C10 C11 C12 -179.3(5) . . . . ?
C9 C10 C11 C12 -0.4(7) . . . . ?
C10 C11 C12 C13 -0.1(8) . . . . ?
C11 C12 C13 C14 0.1(7) . . . . ?
C11 C12 C13 N7 -179.9(4) . . . . ?
C10 C9 C14 C13 -0.8(7) . . . . ?
C15 C9 C14 C13 179.0(4) . . . . ?
C12 C13 C14 C9 0.4(7) . . . . ?
N7 C13 C14 C9 -179.6(4) . . . . ?
Ho1 O4 C15 O5 58.0(8) 2_657 . . . ?
Ho1 O4 C15 C9 -123.4(5) 2_657 . . . ?
Ho1 O5 C15 O4 9.4(8) . . . . ?
Ho1 O5 C15 C9 -169.3(3) . . . . ?
C14 C9 C15 O4 -5.3(6) . . . . ?
C10 C9 C15 O4 174.5(4) . . . . ?
C14 C9 C15 O5 173.4(4) . . . . ?
C10 C9 C15 O5 -6.8(6) . . . . ?
C6 C5 N1 N2 -171.5(4) . . . . ?
C4 C5 N1 N2 9.0(7) . . . . ?
C5 N1 N2 C8 -180.0(4) . . . . ?
N3 C8 N2 N1 -2.6(7) . . . . ?
N6 C8 N2 N1 -180.0(4) . . . . ?
N6 C8 N3 N4 -0.2(6) . . . . ?
N2 C8 N3 N4 -177.8(5) . . . . ?
C8 N3 N4 N5 0.3(5) . . . . ?
N3 N4 N5 N6 -0.3(5) . . . . ?
N3 C8 N6 N5 0.0(6) . . . . ?
N2 C8 N6 N5 177.8(4) . . . . ?
N4 N5 N6 C8 0.1(5) . . . . ?
C12 C13 N7 N8 179.1(4) . . . . ?
C14 C13 N7 N8 -0.9(7) . . . . ?
C13 N7 N8 C16 179.5(4) . . . . ?
N9 C16 N8 N7 -177.0(4) . . . . ?
N12 C16 N8 N7 2.1(7) . . . . ?
N12 C16 N9 N10 0.5(5) . . . . ?
N8 C16 N9 N10 179.7(4) . . . . ?
C16 N9 N10 N11 -0.1(5) . . . . ?
N9 N10 N11 N12 -0.3(6) . . . . ?
N10 N11 N12 C16 0.6(5) . . . . ?
N9 C16 N12 N11 -0.7(5) . . . . ?
N8 C16 N12 N11 -179.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.183
_database_code_depnum_ccdc_archive 'CCDC 993757'
#######################################################################
#
#                 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_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H17 N12 Nd O10'
_chemical_formula_weight         681.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   Cc

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'

_cell_length_a                   16.2248(7)
_cell_length_b                   14.2682(6)
_cell_length_c                   10.0232(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.746(2)
_cell_angle_gamma                90.00
_cell_volume                     2233.28(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3581
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.08

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1348.0
_exptl_absorpt_coefficient_mu    2.410
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_T_max  0.633
_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            8855
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.57
_reflns_number_total             5133
_reflns_number_gt                3835
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0392P)²+5.4729P] 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       0.00013(1)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.050(2)
_refine_ls_number_reflns         5133
_refine_ls_number_parameters     355
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0774
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.014

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
Nd1 Nd 0.18733(7) 0.026254(18) 0.77860(10) 0.02527(10) Uani 1 1 d . . .
O1 O 0.1479(7) 0.0863(6) 0.4249(11) 0.040(2) Uani 1 1 d . . .
O2 O 0.1543(6) 0.1606(7) 0.6224(9) 0.0345(19) Uani 1 1 d . . .
O3 O 0.1555(7) 0.3445(8) 0.6176(10) 0.058(3) Uani 1 1 d . . .
H2 H 0.1704 0.2932 0.6526 0.087 Uiso 1 1 calc R . .
O4 O 0.2233(6) -0.0915(6) 0.6368(11) 0.040(2) Uani 1 1 d . . .
O5 O 0.2309(6) -0.1549(7) 0.4395(9) 0.043(2) Uani 1 1 d . . .
O6 O 0.2371(7) -0.3349(9) 0.4224(10) 0.062(3) Uani 1 1 d . . .
H5 H 0.2289 -0.2813 0.3923 0.094 Uiso 1 1 calc R . .
O7 O 0.0455(8) -0.0212(6) 0.6037(14) 0.045(3) Uani 1 1 d . . .
O8 O 0.0585(7) 0.0948(7) 0.8383(9) 0.053(3) Uani 1 1 d . . .
O9 O 0.3162(8) -0.0341(7) 0.9518(13) 0.046(3) Uani 1 1 d . . .
O10 O 0.3229(5) 0.0811(6) 0.7274(9) 0.0362(19) Uani 1 1 d . . .
C1 C 0.1249(7) 0.2495(9) 0.4166(12) 0.029(2) Uani 1 1 d . . .
C2 C 0.1299(8) 0.3360(10) 0.4783(13) 0.039(3) Uani 1 1 d . . .
C3 C 0.1138(7) 0.4184(7) 0.3964(11) 0.051(3) Uani 1 1 d . . .
H3 H 0.1213 0.4770 0.4386 0.061 Uiso 1 1 calc R . .
C4 C 0.0869(7) 0.4115(7) 0.2543(9) 0.048(2) Uani 1 1 d . . .
H4 H 0.0759 0.4654 0.2002 0.058 Uiso 1 1 calc R . .
C5 C 0.0763(7) 0.3248(8) 0.1925(11) 0.039(2) Uani 1 1 d . . .
C6 C 0.0948(8) 0.2461(10) 0.2693(13) 0.036(3) Uani 1 1 d . . .
H6 H 0.0877 0.1882 0.2250 0.043 Uiso 1 1 calc R . .
C7 C 0.1420(8) 0.1582(9) 0.4934(14) 0.030(3) Uani 1 1 d . . .
C8 C -0.0142(6) 0.3642(6) -0.1661(8) 0.0331(18) Uani 1 1 d . . .
C9 C 0.2674(6) -0.2501(8) 0.6385(12) 0.022(2) Uani 1 1 d . . .
C10 C 0.2634(7) -0.3326(9) 0.5583(12) 0.035(2) Uani 1 1 d . . .
C11 C 0.2882(8) -0.4171(8) 0.6216(12) 0.062(3) Uani 1 1 d . . .
H11 H 0.2852 -0.4710 0.5683 0.074 Uiso 1 1 calc R . .
C12 C 0.3167(7) -0.4224(7) 0.7596(10) 0.060(3) Uani 1 1 d . . .
H12 H 0.3341 -0.4800 0.8014 0.072 Uiso 1 1 calc R . .
C13 C 0.3209(7) -0.3429(10) 0.8417(12) 0.052(3) Uani 1 1 d . . .
C14 C 0.2949(7) -0.2563(9) 0.7791(13) 0.033(3) Uani 1 1 d . . .
H14 H 0.2965 -0.2031 0.8333 0.040 Uiso 1 1 calc R . .
C15 C 0.2376(8) -0.1609(9) 0.5703(12) 0.024(3) Uani 1 1 d . . .
C16 C 0.3906(6) -0.3182(8) 1.2002(9) 0.044(2) Uani 1 1 d . . .
N1 N 0.0451(6) 0.3078(7) 0.0443(10) 0.039(2) Uani 1 1 d . . .
N2 N 0.0134(4) 0.3805(4) -0.0231(5) 0.0355(14) Uani 1 1 d . . .
N3 N -0.0557(5) 0.4316(5) -0.2516(7) 0.0408(18) Uani 1 1 d . . .
N4 N -0.0708(8) 0.3935(9) -0.3701(14) 0.049(3) Uani 1 1 d . . .
N5 N -0.0411(7) 0.3087(9) -0.3588(10) 0.044(3) Uani 1 1 d . . .
N6 N 0.0000(7) 0.2816(9) -0.2333(11) 0.048(3) Uani 1 1 d . . .
N7 N 0.3542(5) -0.3621(6) 0.9842(8) 0.0588(19) Uani 1 1 d . . .
N8 N 0.3544(6) -0.2928(7) 1.0534(10) 0.050(3) Uani 1 1 d . . .
N9 N 0.4325(5) -0.3957(6) 1.2575(9) 0.049(2) Uani 1 1 d . . .
N10 N 0.4541(8) -0.3802(10) 1.4031(16) 0.062(4) Uani 1 1 d . . .
N11 N 0.4251(7) -0.2966(8) 1.4188(12) 0.048(3) Uani 1 1 d . . .
N12 N 0.3885(6) -0.2586(9) 1.2935(11) 0.052(3) Uani 1 1 d . . .
H7 H 0.0130 -0.0308 0.6465 0.078 Uiso 1 1 d R . .
H8 H 0.0319 0.0237 0.5514 0.078 Uiso 1 1 d R . .
H10 H 0.0186 0.0618 0.8106 0.078 Uiso 1 1 d R . .
H13 H 0.3587 0.0004 0.9602 0.078 Uiso 1 1 d R . .
H15 H 0.3097 -0.0451 1.0250 0.078 Uiso 1 1 d R . .
H16 H 0.3588 0.0433 0.7397 0.078 Uiso 1 1 d R . .
H17 H 0.3384 0.1321 0.7590 0.078 Uiso 1 1 d R . .
H9 H 0.0692 0.1056 0.9183 0.078 Uiso 1 1 d R . .
H1 H 0.4534 -0.2622 1.4951 0.078 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
Nd1 O4 2.373(9) . ?
Nd1 O1 2.376(9) 2 ?
Nd1 O5 2.419(10) 2 ?
Nd1 O2 2.440(9) . ?
Nd1 O9 2.481(13) . ?
Nd1 O10 2.516(8) . ?
Nd1 O8 2.522(10) . ?
Nd1 O7 2.577(12) . ?
O1 C7 1.253(16) . ?
O1 Nd1 2.376(9) 2_554 ?
O2 C7 1.254(16) . ?
O3 C2 1.350(16) . ?
O3 H2 0.8200 . ?
O4 C15 1.251(15) . ?
O5 C15 1.289(15) . ?
O5 Nd1 2.419(10) 2_554 ?
O6 C10 1.313(16) . ?
O6 H5 0.8200 . ?
O7 H7 0.7768 . ?
O7 H8 0.8197 . ?
O8 H10 0.7874 . ?
O8 H9 0.7886 . ?
O9 H13 0.8329 . ?
O9 H15 0.7852 . ?
O10 H16 0.7782 . ?
O10 H17 0.8064 . ?
C1 C2 1.374(19) . ?
C1 C6 1.425(18) . ?
C1 C7 1.501(18) . ?
C2 C3 1.416(17) . ?
C3 C4 1.375(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(16) . ?
C4 H4 0.9300 . ?
C5 C6 1.348(17) . ?
C5 N1 1.454(14) . ?
C6 H6 0.9300 . ?
C8 N3 1.341(11) . ?
C8 N2 1.400(9) . ?
C8 N6 1.407(15) . ?
C9 C14 1.361(18) . ?
C9 C10 1.417(17) . ?
C9 C15 1.463(17) . ?
C10 C11 1.371(17) . ?
C11 C12 1.336(15) . ?
C11 H11 0.9300 . ?
C12 C13 1.392(18) . ?
C12 H12 0.9300 . ?
C13 C14 1.399(17) . ?
C13 N7 1.409(13) . ?
C14 H14 0.9300 . ?
C16 N12 1.272(15) . ?
C16 N9 1.342(12) . ?
C16 N8 1.474(13) . ?
N1 N2 1.268(11) . ?
N3 N4 1.269(15) . ?
N4 N5 1.296(18) . ?
N5 N6 1.312(16) . ?
N7 N8 1.208(12) . ?
N9 N10 1.422(17) . ?
N10 N11 1.307(17) . ?
N11 N12 1.349(15) . ?
N11 H1 0.9191 . ?

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 Nd1 O1 92.43(15) . 2 ?
O4 Nd1 O5 149.5(4) . 2 ?
O1 Nd1 O5 100.4(3) 2 2 ?
O4 Nd1 O2 102.6(3) . . ?
O1 Nd1 O2 151.3(3) 2 . ?
O5 Nd1 O2 78.76(15) 2 . ?
O4 Nd1 O9 82.9(4) . . ?
O1 Nd1 O9 69.5(4) 2 . ?
O5 Nd1 O9 76.1(3) 2 . ?
O2 Nd1 O9 135.9(3) . . ?
O4 Nd1 O10 74.2(3) . . ?
O1 Nd1 O10 137.1(3) 2 . ?
O5 Nd1 O10 77.7(3) 2 . ?
O2 Nd1 O10 71.1(3) . . ?
O9 Nd1 O10 68.5(4) . . ?
O4 Nd1 O8 140.4(4) . . ?
O1 Nd1 O8 74.7(3) 2 . ?
O5 Nd1 O8 70.0(3) 2 . ?
O2 Nd1 O8 78.2(3) . . ?
O9 Nd1 O8 124.3(4) . . ?
O10 Nd1 O8 139.00(18) . . ?
O4 Nd1 O7 74.1(4) . . ?
O1 Nd1 O7 84.4(4) 2 . ?
O5 Nd1 O7 134.3(3) 2 . ?
O2 Nd1 O7 76.7(3) . . ?
O9 Nd1 O7 144.3(2) . . ?
O10 Nd1 O7 127.7(3) . . ?
O8 Nd1 O7 67.6(4) . . ?
C7 O1 Nd1 164.8(9) . 2_554 ?
C7 O2 Nd1 125.9(9) . . ?
C2 O3 H2 109.5 . . ?
C15 O4 Nd1 172.5(8) . . ?
C15 O5 Nd1 131.1(9) . 2_554 ?
C10 O6 H5 109.5 . . ?
Nd1 O7 H7 106.5 . . ?
Nd1 O7 H8 105.3 . . ?
H7 O7 H8 112.7 . . ?
Nd1 O8 H10 109.9 . . ?
Nd1 O8 H9 110.5 . . ?
H10 O8 H9 114.1 . . ?
Nd1 O9 H13 112.5 . . ?
Nd1 O9 H15 115.0 . . ?
H13 O9 H15 109.9 . . ?
Nd1 O10 H16 114.2 . . ?
Nd1 O10 H17 113.4 . . ?
H16 O10 H17 115.0 . . ?
C2 C1 C6 117.3(11) . . ?
C2 C1 C7 124.7(12) . . ?
C6 C1 C7 117.8(11) . . ?
O3 C2 C1 120.7(12) . . ?
O3 C2 C3 118.8(12) . . ?
C1 C2 C3 120.4(11) . . ?
C4 C3 C2 119.9(10) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 119.8(10) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 120.8(10) . . ?
C6 C5 N1 113.9(11) . . ?
C4 C5 N1 125.3(10) . . ?
C5 C6 C1 121.6(12) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
O1 C7 O2 125.0(13) . . ?
O1 C7 C1 117.4(12) . . ?
O2 C7 C1 117.4(12) . . ?
N3 C8 N2 120.0(8) . . ?
N3 C8 N6 114.4(8) . . ?
N2 C8 N6 125.5(9) . . ?
C14 C9 C10 119.0(11) . . ?
C14 C9 C15 120.9(11) . . ?
C10 C9 C15 120.0(11) . . ?
O6 C10 C11 115.5(11) . . ?
O6 C10 C9 124.1(12) . . ?
C11 C10 C9 120.4(11) . . ?
C12 C11 C10 120.3(11) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.9(10) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 119.6(10) . . ?
C12 C13 N7 112.6(10) . . ?
C14 C13 N7 127.8(13) . . ?
C9 C14 C13 119.8(12) . . ?
C9 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
O4 C15 O5 120.9(12) . . ?
O4 C15 C9 121.7(11) . . ?
O5 C15 C9 117.3(11) . . ?
N12 C16 N9 110.3(9) . . ?
N12 C16 N8 119.1(10) . . ?
N9 C16 N8 130.4(9) . . ?
N2 N1 C5 112.7(8) . . ?
N1 N2 C8 112.3(7) . . ?
N4 N3 C8 103.1(9) . . ?
N3 N4 N5 110.2(12) . . ?
N4 N5 N6 116.0(12) . . ?
N5 N6 C8 96.1(10) . . ?
N8 N7 C13 111.3(10) . . ?
N7 N8 C16 108.1(9) . . ?
C16 N9 N10 105.4(9) . . ?
N11 N10 N9 105.6(12) . . ?
N10 N11 N12 109.7(12) . . ?
N10 N11 H1 118.2 . . ?
N12 N11 H1 123.7 . . ?
C16 N12 N11 108.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.109
_database_code_depnum_ccdc_archive 'CCDC 975949'
#######################################################################
#
#                 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            'C16 H17 Gd N12 O10'
_chemical_formula_weight         694.67

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           monoclinic
_symmetry_space_group_name_H-M   Cc

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'

_cell_length_a                   16.3059(18)
_cell_length_b                   14.2088(16)
_cell_length_c                   10.0240(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.473(6)
_cell_angle_gamma                90.00
_cell_volume                     2238.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5863
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1364.0
_exptl_absorpt_coefficient_mu    3.048
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_T_max  0.633
_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            8969
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.48
_reflns_number_total             5107
_reflns_number_gt                3852
_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)+(0.0258P)²+9.1432P] 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       0.00013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.042(3)
_refine_ls_number_reflns         5107
_refine_ls_number_parameters     375
_refine_ls_number_restraints     261
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.014

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 0.15328(13) 0.027608(13) 0.62151(17) 0.02669(8) Uani 1 1 d . . .
N10 N 0.4161(8) 0.3868(10) 1.7586(13) 0.049(2) Uani 1 1 d U . .
N11 N 0.3875(7) 0.3068(8) 1.7610(10) 0.0354(18) Uani 1 1 d U . .
H9 H 0.3918 0.2770 1.8372 0.043 Uiso 1 1 calc R . .
N5 N -0.0795(8) 0.3015(8) -0.5185(11) 0.038(2) Uani 1 1 d U . .
N12 N 0.3490(7) 0.2684(8) 1.6361(11) 0.0433(18) Uani 1 1 d U . .
N6 N -0.0412(7) 0.2826(8) -0.3862(11) 0.0437(19) Uani 1 1 d U . .
N3 N -0.0961(5) 0.4315(5) -0.4124(7) 0.0409(16) Uani 1 1 d U . .
N1 N 0.0015(8) 0.3052(8) -0.1179(11) 0.041(2) Uani 1 1 d U . .
N4 N -0.1113(8) 0.3916(9) -0.5270(13) 0.047(2) Uani 1 1 d U . .
N2 N -0.0284(7) 0.3773(8) -0.1766(12) 0.0448(18) Uani 1 1 d U . .
N9 N 0.3973(6) 0.4109(6) 1.6189(9) 0.0522(17) Uani 1 1 d U . .
N13 N 0.3146(7) 0.3627(8) 1.3237(9) 0.0298(17) Uani 0.50 1 d PU . .
N14 N 0.3006(13) 0.3087(14) 1.3469(18) 0.027(2) Uani 0.50 1 d PU . .
N7 N 0.3151(12) 0.2947(13) 1.3983(16) 0.036(2) Uani 0.50 1 d PU . .
N8 N 0.3277(13) 0.3811(16) 1.420(2) 0.033(2) Uani 0.50 1 d PU . .
C1 C 0.0818(7) 0.2485(8) 0.2623(11) 0.026(3) Uani 1 1 d . . .
C7 C 0.1068(7) 0.1538(9) 0.3296(11) 0.029(3) Uani 1 1 d . . .
C6 C 0.0539(9) 0.2470(10) 0.1172(14) 0.036(3) Uani 1 1 d U . .
H2 H 0.0525 0.1914 0.0677 0.043 Uiso 1 1 calc R . .
C5 C 0.0279(9) 0.3337(11) 0.0493(13) 0.049(3) Uani 1 1 d U . .
C2 C 0.0870(8) 0.3288(10) 0.3269(12) 0.041(3) Uani 1 1 d . . .
C4 C 0.0332(8) 0.4172(9) 0.1264(13) 0.062(3) Uani 1 1 d U . .
H3 H 0.0113 0.4729 0.0822 0.074 Uiso 1 1 calc R . .
C3 C 0.0668(13) 0.4171(10) 0.2522(17) 0.066(5) Uani 1 1 d . . .
H4 H 0.0792 0.4738 0.2996 0.079 Uiso 1 1 calc R . .
C8 C -0.0569(7) 0.3686(5) -0.3252(9) 0.033(2) Uani 1 1 d . . .
C9 C 0.2246(7) 0.2450(8) 0.9861(11) 0.024(3) Uani 1 1 d . . .
C14 C 0.2543(8) 0.2472(9) 1.1293(12) 0.028(3) Uani 1 1 d . . .
H8 H 0.2617 0.1897 1.1751 0.033 Uiso 1 1 calc R . .
C16 C 0.3559(6) 0.3345(9) 1.5528(9) 0.051(3) Uani 1 1 d U . .
C11 C 0.2387(11) 0.4145(10) 0.9890(19) 0.065(5) Uani 1 1 d U . .
H6 H 0.2384 0.4725 0.9458 0.078 Uiso 1 1 calc R . .
C13 C 0.2729(8) 0.3235(10) 1.2063(12) 0.036(2) Uani 1 1 d . . .
C10 C 0.2187(9) 0.3346(8) 0.9115(14) 0.036(3) Uani 1 1 d . . .
C12 C 0.2613(7) 0.4085(7) 1.1447(10) 0.041(2) Uani 1 1 d U . .
H7 H 0.2672 0.4631 1.1977 0.049 Uiso 1 1 calc R . .
C15 C 0.2006(7) 0.1576(8) 0.9106(12) 0.025(3) Uani 1 1 d . . .
O4 O 0.1928(7) 0.0837(6) 0.9838(11) 0.040(2) Uani 1 1 d . . .
O7 O 0.0173(9) -0.0265(6) 0.4500(13) 0.062(4) Uani 1 1 d . . .
O10 O 0.2788(7) -0.0293(5) 0.7943(11) 0.0324(19) Uani 1 1 d . . .
O5 O 0.1890(6) 0.1566(7) 0.7795(9) 0.039(2) Uani 1 1 d . . .
O2 O 0.1185(7) 0.1521(6) 0.4605(9) 0.037(2) Uani 1 1 d . . .
O9 O 0.2867(7) 0.0854(6) 0.5713(11) 0.045(3) Uani 1 1 d . . .
H9A H 0.2874 0.0782 0.4771 0.067 Uiso 1 1 d R . .
H9B H 0.2971 0.1506 0.5902 0.067 Uiso 1 1 d R . .
O8 O 0.0218(6) 0.0889(7) 0.6713(11) 0.045(3) Uani 1 1 d . . .
H8A H -0.0178 0.0439 0.6637 0.067 Uiso 1 1 d R . .
H8B H 0.0327 0.1118 0.7576 0.067 Uiso 1 1 d R . .
O3 O 0.1157(8) 0.3381(8) 0.4715(10) 0.056(3) Uani 1 1 d . . .
H1 H 0.1108 0.2875 0.5080 0.083 Uiso 1 1 calc R . .
O6 O 0.1949(8) 0.3395(8) 0.7796(11) 0.058(3) Uani 1 1 d . . .
H5 H 0.1769 0.2880 0.7477 0.088 Uiso 1 1 calc R . .
O1 O 0.1163(7) 0.0859(6) 0.2653(10) 0.039(2) Uani 1 1 d . . .
H7A H -0.0291 -0.0228 0.4746 0.058 Uiso 1 1 d R . .
H7B H 0.0118 0.0133 0.3850 0.058 Uiso 1 1 d R . .
H10A H 0.3127 0.0172 0.8198 0.058 Uiso 1 1 d R . .
H10B H 0.3140 -0.0734 0.7730 0.058 Uiso 1 1 d R . .


_geom_special_details            
; 
SIMU 0.01 0.02 3.8 $N, because Large Non-Solvent  N  Ueq(max)/Ueq(min) Range        7.3 Ratio
ISOR 0.01 0.01 N14,because ADP of Atom N14     is N.P.D. or (nearly) 2D
ISOR 0.01 0.01 C5 C16, because Atom C5,C16              has ADP max/min Ratio 4.1,4.8 prolat
ISOR 0.005 0.005 C12 C4 C6, because Atom C12,C4,C6      has ADP max/min Ratio 4.1,4.6,4.0 prolat
DELU 0.02 C11 C12, because Hirshfeld Test Diff for    C11    --  C12     ..        7.2 su 
;

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 O4 2.301(9) 2_554 ?
Gd1 O1 2.347(9) 2 ?
Gd1 O2 2.360(9) . ?
Gd1 O5 2.391(9) . ?
Gd1 O10 2.439(10) . ?
Gd1 O8 2.485(10) . ?
Gd1 O9 2.499(11) . ?
Gd1 O7 2.536(13) . ?
N10 N11 1.231(18) . ?
N10 N9 1.394(14) . ?
N11 N12 1.356(16) . ?
N11 H9 0.8600 . ?
N5 N6 1.334(15) . ?
N5 N4 1.376(18) . ?
N12 C16 1.281(15) . ?
N6 C8 1.421(14) . ?
N3 N4 1.245(14) . ?
N3 C8 1.294(11) . ?
N1 N2 1.217(16) . ?
N1 C5 1.665(17) . ?
N2 C8 1.442(14) . ?
N9 C16 1.354(14) . ?
N13 N14 0.85(2) . ?
N13 N8 0.97(2) . ?
N13 N7 1.221(19) . ?
N13 C13 1.315(15) . ?
N13 C12 1.889(14) . ?
N14 N7 0.544(18) . ?
N14 N8 1.27(3) . ?
N14 C13 1.38(2) . ?
N7 N8 1.25(3) . ?
N7 C16 1.616(18) . ?
N7 C13 1.908(19) . ?
N8 C16 1.45(2) . ?
C1 C2 1.304(18) . ?
C1 C6 1.403(17) . ?
C1 C7 1.512(16) . ?
C7 O1 1.192(15) . ?
C7 O2 1.274(14) . ?
C6 C5 1.42(2) . ?
C6 H2 0.9300 . ?
C5 C4 1.41(2) . ?
C2 O3 1.405(15) . ?
C2 C3 1.453(18) . ?
C4 C3 1.23(2) . ?
C4 H3 0.9300 . ?
C3 H4 0.9300 . ?
C9 C14 1.388(15) . ?
C9 C15 1.452(17) . ?
C9 C10 1.467(15) . ?
C14 C13 1.319(19) . ?
C14 H8 0.9300 . ?
C11 C10 1.37(2) . ?
C11 C12 1.51(2) . ?
C11 H6 0.9300 . ?
C13 C12 1.347(18) . ?
C10 O6 1.276(17) . ?
C12 H7 0.9300 . ?
C15 O5 1.277(15) . ?
C15 O4 1.307(15) . ?
O4 Gd1 2.301(9) 2 ?
O7 H7A 0.8572 . ?
O7 H7B 0.8499 . ?
O10 H10A 0.8566 . ?
O10 H10B 0.9141 . ?
O9 H9A 0.9537 . ?
O9 H9B 0.9514 . ?
O8 H8A 0.8969 . ?
O8 H8B 0.8963 . ?
O3 H1 0.8200 . ?
O6 H5 0.8200 . ?
O1 Gd1 2.347(9) 2_554 ?

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 Gd1 O1 93.18(12) 2_554 2 ?
O4 Gd1 O2 99.2(3) 2_554 . ?
O1 Gd1 O2 151.8(4) 2 . ?
O4 Gd1 O5 150.1(4) 2_554 . ?
O1 Gd1 O5 100.2(3) 2 . ?
O2 Gd1 O5 81.37(12) . . ?
O4 Gd1 O10 83.2(4) 2_554 . ?
O1 Gd1 O10 68.9(4) 2 . ?
O2 Gd1 O10 137.5(3) . . ?
O5 Gd1 O10 76.9(3) . . ?
O4 Gd1 O8 139.1(4) 2_554 . ?
O1 Gd1 O8 74.9(3) 2 . ?
O2 Gd1 O8 79.2(3) . . ?
O5 Gd1 O8 70.7(4) . . ?
O10 Gd1 O8 125.4(4) . . ?
O4 Gd1 O9 73.0(3) 2_554 . ?
O1 Gd1 O9 136.9(4) 2 . ?
O2 Gd1 O9 71.3(4) . . ?
O5 Gd1 O9 79.0(3) . . ?
O10 Gd1 O9 69.0(4) . . ?
O8 Gd1 O9 140.30(12) . . ?
O4 Gd1 O7 73.7(4) 2_554 . ?
O1 Gd1 O7 83.5(4) 2 . ?
O2 Gd1 O7 75.9(3) . . ?
O5 Gd1 O7 134.1(4) . . ?
O10 Gd1 O7 142.84(14) . . ?
O8 Gd1 O7 66.2(4) . . ?
O9 Gd1 O7 127.9(4) . . ?
N11 N10 N9 105.3(11) . . ?
N10 N11 N12 116.0(11) . . ?
N10 N11 H9 122.0 . . ?
N12 N11 H9 122.0 . . ?
N6 N5 N4 108.5(11) . . ?
C16 N12 N11 101.9(11) . . ?
N5 N6 C8 99.4(9) . . ?
N4 N3 C8 104.5(9) . . ?
N2 N1 C5 104.2(11) . . ?
N3 N4 N5 112.8(11) . . ?
N1 N2 C8 113.9(11) . . ?
C16 N9 N10 104.0(9) . . ?
N14 N13 N8 88.6(19) . . ?
N14 N13 N7 22.6(15) . . ?
N8 N13 N7 68.9(16) . . ?
N14 N13 C13 75.6(16) . . ?
N8 N13 C13 158.7(16) . . ?
N7 N13 C13 97.5(13) . . ?
N14 N13 C12 118.8(16) . . ?
N8 N13 C12 141.1(16) . . ?
N7 N13 C12 141.4(12) . . ?
C13 N13 C12 45.5(7) . . ?
N7 N14 N13 121(4) . . ?
N7 N14 N8 76(3) . . ?
N13 N14 N8 49.4(15) . . ?
N7 N14 C13 165(4) . . ?
N13 N14 C13 67.7(13) . . ?
N8 N14 C13 115.7(17) . . ?
N14 N7 N13 37(3) . . ?
N14 N7 N8 79(3) . . ?
N13 N7 N8 45.9(11) . . ?
N14 N7 C16 138(4) . . ?
N13 N7 C16 104.1(13) . . ?
N8 N7 C16 59.0(12) . . ?
N14 N7 C13 11(3) . . ?
N13 N7 C13 43.1(8) . . ?
N8 N7 C13 87.8(13) . . ?
C16 N7 C13 146.8(13) . . ?
N13 N8 N7 65.2(17) . . ?
N13 N8 N14 41.9(13) . . ?
N7 N8 N14 24.9(10) . . ?
N13 N8 C16 136(2) . . ?
N7 N8 C16 73.0(13) . . ?
N14 N8 C16 97.8(16) . . ?
C2 C1 C6 119.2(10) . . ?
C2 C1 C7 125.7(10) . . ?
C6 C1 C7 115.0(11) . . ?
O1 C7 O2 122.4(11) . . ?
O1 C7 C1 122.5(11) . . ?
O2 C7 C1 115.1(10) . . ?
C1 C6 C5 117.2(13) . . ?
C1 C6 H2 121.4 . . ?
C5 C6 H2 121.4 . . ?
C4 C5 C6 120.3(12) . . ?
C4 C5 N1 136.0(10) . . ?
C6 C5 N1 103.7(12) . . ?
C1 C2 O3 123.6(11) . . ?
C1 C2 C3 121.6(11) . . ?
O3 C2 C3 114.7(12) . . ?
C3 C4 C5 120.3(12) . . ?
C3 C4 H3 119.8 . . ?
C5 C4 H3 119.8 . . ?
C4 C3 C2 120.4(14) . . ?
C4 C3 H4 119.8 . . ?
C2 C3 H4 119.8 . . ?
N3 C8 N6 114.7(9) . . ?
N3 C8 N2 127.2(9) . . ?
N6 C8 N2 118.2(9) . . ?
C14 C9 C15 122.0(10) . . ?
C14 C9 C10 117.7(11) . . ?
C15 C9 C10 120.3(10) . . ?
C13 C14 C9 125.9(12) . . ?
C13 C14 H8 117.0 . . ?
C9 C14 H8 117.0 . . ?
N12 C16 N9 112.8(9) . . ?
N12 C16 N8 150.9(14) . . ?
N9 C16 N8 94.4(12) . . ?
N12 C16 N7 106.4(11) . . ?
N9 C16 N7 140.6(11) . . ?
N8 C16 N7 48.0(12) . . ?
C10 C11 C12 119.8(12) . . ?
C10 C11 H6 120.1 . . ?
C12 C11 H6 120.1 . . ?
N13 C13 C14 148.7(14) . . ?
N13 C13 C12 90.4(11) . . ?
C14 C13 C12 119.1(11) . . ?
N13 C13 N14 36.7(10) . . ?
C14 C13 N14 115.8(14) . . ?
C12 C13 N14 125.1(13) . . ?
N13 C13 N7 39.4(8) . . ?
C14 C13 N7 112.2(12) . . ?
C12 C13 N7 128.7(11) . . ?
N14 C13 N7 4.2(11) . . ?
O6 C10 C11 120.3(11) . . ?
O6 C10 C9 122.4(11) . . ?
C11 C10 C9 117.3(12) . . ?
C13 C12 C11 119.5(10) . . ?
C13 C12 N13 44.1(7) . . ?
C11 C12 N13 157.9(10) . . ?
C13 C12 H7 120.3 . . ?
C11 C12 H7 120.3 . . ?
N13 C12 H7 78.1 . . ?
O5 C15 O4 124.0(11) . . ?
O5 C15 C9 119.4(10) . . ?
O4 C15 C9 116.6(10) . . ?
C15 O4 Gd1 166.9(9) . 2 ?
Gd1 O7 H7A 117.7 . . ?
Gd1 O7 H7B 102.2 . . ?
H7A O7 H7B 104.9 . . ?
Gd1 O10 H10A 108.0 . . ?
Gd1 O10 H10B 121.5 . . ?
H10A O10 H10B 101.7 . . ?
C15 O5 Gd1 129.3(8) . . ?
C7 O2 Gd1 131.3(8) . . ?
Gd1 O9 H9A 113.9 . . ?
Gd1 O9 H9B 113.5 . . ?
H9A O9 H9B 104.6 . . ?
Gd1 O8 H8A 111.9 . . ?
Gd1 O8 H8B 111.1 . . ?
H8A O8 H8B 107.2 . . ?
C2 O3 H1 109.5 . . ?
C10 O6 H5 109.5 . . ?
C7 O1 Gd1 168.3(9) . 2_554 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.098
_database_code_depnum_ccdc_archive 'CCDC 993758'
#######################################################################
#
#                 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_7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H23 Dy N6 O13'
_chemical_formula_weight         573.82

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'
Dy Dy -0.1892 4.4098 '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/c

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

_cell_length_a                   10.8529(13)
_cell_length_b                   6.9013(9)
_cell_length_c                   27.181(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.490(6)
_cell_angle_gamma                90.00
_cell_volume                     1881.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4573
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      26.78

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1132
_exptl_absorpt_coefficient_mu    4.050
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  '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            16013
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         27.57
_reflns_number_total             4338
_reflns_number_gt                3590
_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)+(0.0592P)²+0.7516P] 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       0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4338
_refine_ls_number_parameters     269
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0944
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy -0.13744(2) 0.36124(3) 0.798652(8) 0.01899(10) Uani 1 1 d . . .
O1 O 0.0672(3) 0.5293(5) 0.82659(13) 0.0301(8) Uani 1 1 d . . .
O2 O 0.0746(3) 0.7346(6) 0.76570(14) 0.0373(9) Uani 1 1 d . . .
O3 O 0.3312(3) 0.8080(5) 0.77649(13) 0.0253(7) Uani 1 1 d . . .
O4 O 0.0464(4) 0.1316(5) 0.84329(16) 0.0356(9) Uani 1 1 d . . .
H4A H 0.0618 0.0536 0.8170 0.053 Uiso 1 1 d R . .
H4B H 0.1259 0.2028 0.8633 0.053 Uiso 1 1 d R . .
O5 O -0.0624(4) 0.4187(6) 0.89347(14) 0.0385(9) Uani 1 1 d . . .
H5A H 0.0300 0.4552 0.9071 0.058 Uiso 1 1 d R . .
H5B H -0.0303 0.3190 0.9075 0.058 Uiso 1 1 d R . .
O6 O -0.2354(4) 0.0849(6) 0.82022(16) 0.0385(9) Uani 1 1 d . . .
H6B H -0.2172 -0.0275 0.8033 0.058 Uiso 1 1 d R . .
H6A H -0.3299 0.1039 0.8084 0.058 Uiso 1 1 d R . .
O7 O -0.3072(3) 0.5151(5) 0.82105(13) 0.0291(8) Uani 1 1 d . . .
H7A H -0.3580 0.6047 0.8029 0.044 Uiso 1 1 d R . .
H7B H -0.3427 0.4470 0.8352 0.044 Uiso 1 1 d R . .
O8 O -0.1740(3) 0.6643(5) 0.75736(15) 0.0299(8) Uani 1 1 d . . .
H8A H -0.0966 0.7096 0.7605 0.045 Uiso 1 1 d R . .
H8B H -0.2216 0.6479 0.7243 0.045 Uiso 1 1 d R . .
O9 O 0.1747(4) 0.2900(8) 0.97132(19) 0.0536(12) Uani 1 1 d . . .
H9A H 0.1793 0.3327 1.0056 0.080 Uiso 1 1 d R . .
H9B H 0.2491 0.3411 0.9646 0.080 Uiso 1 1 d R . .
O10 O 0.5622(3) 0.8280(5) 0.76195(15) 0.0320(8) Uani 1 1 d . . .
H10A H 0.4965 0.8348 0.7677 0.048 Uiso 1 1 d R . .
H10B H 0.5510 0.8109 0.7321 0.048 Uiso 1 1 d R . .
O11 O 0.8003(5) 0.4033(9) 0.9567(2) 0.0706(16) Uani 1 1 d . . .
H11A H 0.7851 0.4245 0.9198 0.106 Uiso 1 1 d R . .
H11B H 0.7317 0.3379 0.9644 0.106 Uiso 1 1 d R . .
O12 O 0.9406(8) 0.8507(7) 0.8972(3) 0.107(3) Uani 1 1 d . . .
H12A H 0.9619 0.9556 0.8786 0.161 Uiso 1 1 d R . .
H12B H 0.9395 0.7251 0.8818 0.161 Uiso 1 1 d R . .
O13 O 0.0841(16) 0.953(2) 0.0019(7) 0.110(5) Uani 0.50 1 d PG A 1
H13A H 0.1633 1.0220 0.0046 0.165 Uiso 0.50 1 d PR A 1
H13B H 0.0828 0.8290 -0.0143 0.165 Uiso 0.50 1 d PR A 1
O14 O 0.165(3) 0.906(3) -0.0136(10) 0.161(9) Uani 0.50 1 d PG B 2
H14A H 0.1718 1.0251 0.0008 0.242 Uiso 0.50 1 d PR B 2
H14B H 0.1547 0.9318 -0.0440 0.242 Uiso 0.50 1 d PR B 2
N1 N 0.4375(4) 0.7302(6) 0.99129(16) 0.0257(9) Uani 1 1 d . . .
N2 N 0.5542(4) 0.7570(6) 1.02551(15) 0.0238(9) Uani 1 1 d . . .
N3 N 0.6744(4) 0.7700(6) 1.11881(16) 0.0269(9) Uani 1 1 d . . .
N4 N 0.6437(4) 0.7367(6) 1.16165(16) 0.0291(9) Uani 1 1 d . . .
N5 N 0.5185(5) 0.6856(6) 1.14645(17) 0.0295(10) Uani 1 1 d . . .
N6 N 0.4619(4) 0.6834(6) 1.09329(17) 0.0276(9) Uani 1 1 d . . .
C1 C 0.2624(4) 0.7136(7) 0.84688(18) 0.0203(9) Uani 1 1 d . . .
C2 C 0.3570(4) 0.7873(7) 0.82724(18) 0.0193(9) Uani 1 1 d U . .
C3 C 0.4854(5) 0.8365(6) 0.86546(19) 0.0206(9) Uani 1 1 d U . .
H1 H 0.5503 0.8814 0.8537 0.025 Uiso 1 1 calc R . .
C4 C 0.5156(5) 0.8194(7) 0.91882(19) 0.0217(10) Uani 1 1 d . . .
H2 H 0.5997 0.8552 0.9429 0.026 Uiso 1 1 calc R . .
C5 C 0.4210(5) 0.7486(7) 0.93763(18) 0.0224(10) Uani 1 1 d . . .
C6 C 0.2965(5) 0.6961(7) 0.90126(19) 0.0220(9) Uani 1 1 d . . .
H3 H 0.2339 0.6477 0.9137 0.026 Uiso 1 1 calc R . .
C7 C 0.1282(5) 0.6532(6) 0.81088(19) 0.0223(10) Uani 1 1 d . . .
C8 C 0.5599(5) 0.7366(6) 1.07772(18) 0.0214(9) Uani 1 1 d . . .


_geom_special_details            
; 
DELU 0.001 C12 C3, because Hirshfeld Test Diff for    C2    --  C3     ..        5.2 su
;

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 O2 2.280(3) 2_546 ?
Dy1 O3 2.333(3) 2_546 ?
Dy1 O8 2.334(3) . ?
Dy1 O1 2.358(3) . ?
Dy1 O6 2.364(4) . ?
Dy1 O7 2.398(3) . ?
Dy1 O5 2.420(4) . ?
Dy1 O4 2.473(4) . ?
O1 C7 1.252(5) . ?
O2 C7 1.271(6) . ?
O2 Dy1 2.280(3) 2_556 ?
O3 C2 1.306(6) . ?
O3 Dy1 2.333(3) 2_556 ?
O4 H4A 0.9600 . ?
O4 H4B 0.9602 . ?
O5 H5A 0.9600 . ?
O5 H5B 0.7990 . ?
O6 H6B 0.9595 . ?
O6 H6A 0.9602 . ?
O7 H7A 0.8505 . ?
O7 H7B 0.7945 . ?
O8 H8A 0.8688 . ?
O8 H8B 0.8562 . ?
O9 H9A 0.9607 . ?
O9 H9B 0.9604 . ?
O10 H10A 0.7871 . ?
O10 H10B 0.7827 . ?
O11 H11A 0.9615 . ?
O11 H11B 0.9597 . ?
O12 H12A 0.9598 . ?
O12 H12B 0.9599 . ?
O13 H13A 0.9596 . ?
O13 H13B 0.9600 . ?
O13 H14A 1.0830 . ?
O14 H13A 0.9420 . ?
O14 H13B 1.0335 . ?
O14 H14A 0.8983 . ?
O14 H14B 0.8090 . ?
N1 N2 1.266(5) . ?
N1 C5 1.406(6) . ?
N2 C8 1.404(6) . ?
N3 C8 1.336(6) . ?
N3 N4 1.348(6) . ?
N4 N5 1.308(6) . ?
N5 N6 1.337(6) . ?
N6 C8 1.337(6) . ?
C1 C6 1.385(6) . ?
C1 C2 1.420(6) . ?
C1 C7 1.471(7) . ?
C2 C3 1.425(7) . ?
C3 C4 1.364(7) . ?
C3 H1 0.9300 . ?
C4 C5 1.398(6) . ?
C4 H2 0.9300 . ?
C5 C6 1.383(7) . ?
C6 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 72.65(12) 2_546 2_546 ?
O2 Dy1 O8 91.15(14) 2_546 . ?
O3 Dy1 O8 77.87(13) 2_546 . ?
O2 Dy1 O1 85.10(13) 2_546 . ?
O3 Dy1 O1 141.41(12) 2_546 . ?
O8 Dy1 O1 71.34(12) . . ?
O2 Dy1 O6 100.12(15) 2_546 . ?
O3 Dy1 O6 75.51(13) 2_546 . ?
O8 Dy1 O6 146.34(13) . . ?
O1 Dy1 O6 140.73(12) . . ?
O2 Dy1 O7 148.06(12) 2_546 . ?
O3 Dy1 O7 76.67(12) 2_546 . ?
O8 Dy1 O7 73.73(12) . . ?
O1 Dy1 O7 114.87(13) . . ?
O6 Dy1 O7 80.35(13) . . ?
O2 Dy1 O5 143.33(13) 2_546 . ?
O3 Dy1 O5 141.40(12) 2_546 . ?
O8 Dy1 O5 106.93(14) . . ?
O1 Dy1 O5 71.62(13) . . ?
O6 Dy1 O5 82.42(14) . . ?
O7 Dy1 O5 68.61(12) . . ?
O2 Dy1 O4 73.07(14) 2_546 . ?
O3 Dy1 O4 128.06(13) 2_546 . ?
O8 Dy1 O4 140.07(13) . . ?
O1 Dy1 O4 70.95(12) . . ?
O6 Dy1 O4 73.51(13) . . ?
O7 Dy1 O4 135.52(12) . . ?
O5 Dy1 O4 72.71(14) . . ?
C7 O1 Dy1 141.4(3) . . ?
C7 O2 Dy1 138.6(3) . 2_556 ?
C2 O3 Dy1 134.4(3) . 2_556 ?
Dy1 O4 H4A 109.4 . . ?
Dy1 O4 H4B 109.3 . . ?
H4A O4 H4B 109.5 . . ?
Dy1 O5 H5A 109.3 . . ?
Dy1 O5 H5B 105.9 . . ?
H5A O5 H5B 80.9 . . ?
Dy1 O6 H6B 109.9 . . ?
Dy1 O6 H6A 109.3 . . ?
H6B O6 H6A 109.8 . . ?
Dy1 O7 H7A 124.4 . . ?
Dy1 O7 H7B 115.1 . . ?
H7A O7 H7B 112.6 . . ?
Dy1 O8 H8A 107.2 . . ?
Dy1 O8 H8B 108.1 . . ?
H8A O8 H8B 108.9 . . ?
H9A O9 H9B 109.7 . . ?
H10A O10 H10B 114.9 . . ?
H11A O11 H11B 117.4 . . ?
H12A O12 H12B 114.7 . . ?
H13A O13 H13B 109.5 . . ?
H13A O13 H14A 6.0 . . ?
H13B O13 H14A 104.9 . . ?
H13A O14 H13B 104.9 . . ?
H13A O14 H14A 9.8 . . ?
H13B O14 H14A 113.9 . . ?
H13A O14 H14B 109.3 . . ?
H13B O14 H14B 108.2 . . ?
H14A O14 H14B 101.8 . . ?
N2 N1 C5 116.3(4) . . ?
N1 N2 C8 111.9(4) . . ?
C8 N3 N4 103.5(4) . . ?
N5 N4 N3 110.1(4) . . ?
N4 N5 N6 109.7(4) . . ?
N5 N6 C8 104.3(4) . . ?
C6 C1 C2 119.7(4) . . ?
C6 C1 C7 118.6(4) . . ?
C2 C1 C7 121.7(4) . . ?
O3 C2 C1 122.8(4) . . ?
O3 C2 C3 119.9(4) . . ?
C1 C2 C3 117.2(4) . . ?
C4 C3 C2 121.7(4) . . ?
C4 C3 H1 119.2 . . ?
C2 C3 H1 119.2 . . ?
C3 C4 C5 120.5(4) . . ?
C3 C4 H2 119.8 . . ?
C5 C4 H2 119.8 . . ?
C6 C5 C4 118.9(4) . . ?
C6 C5 N1 114.8(4) . . ?
C4 C5 N1 126.2(4) . . ?
C5 C6 C1 122.0(4) . . ?
C5 C6 H3 119.0 . . ?
C1 C6 H3 119.0 . . ?
O1 C7 O2 121.7(5) . . ?
O1 C7 C1 119.0(4) . . ?
O2 C7 C1 119.2(4) . . ?
N3 C8 N6 112.4(4) . . ?
N3 C8 N2 119.6(4) . . ?
N6 C8 N2 128.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Dy1 O1 C7 62.7(5) 2_546 . . . ?
O3 Dy1 O1 C7 8.6(6) 2_546 . . . ?
O8 Dy1 O1 C7 -30.2(5) . . . . ?
O6 Dy1 O1 C7 162.7(5) . . . . ?
O7 Dy1 O1 C7 -91.4(5) . . . . ?
O5 Dy1 O1 C7 -146.1(5) . . . . ?
O4 Dy1 O1 C7 136.4(5) . . . . ?
C5 N1 N2 C8 179.6(4) . . . . ?
C8 N3 N4 N5 0.3(5) . . . . ?
N3 N4 N5 N6 -0.1(6) . . . . ?
N4 N5 N6 C8 -0.2(5) . . . . ?
Dy1 O3 C2 C1 27.5(7) 2_556 . . . ?
Dy1 O3 C2 C3 -153.6(3) 2_556 . . . ?
C6 C1 C2 O3 -179.8(4) . . . . ?
C7 C1 C2 O3 0.7(7) . . . . ?
C6 C1 C2 C3 1.2(7) . . . . ?
C7 C1 C2 C3 -178.3(4) . . . . ?
O3 C2 C3 C4 179.1(4) . . . . ?
C1 C2 C3 C4 -1.9(7) . . . . ?
C2 C3 C4 C5 1.3(7) . . . . ?
C3 C4 C5 C6 0.0(7) . . . . ?
C3 C4 C5 N1 -177.7(4) . . . . ?
N2 N1 C5 C6 172.7(4) . . . . ?
N2 N1 C5 C4 -9.5(7) . . . . ?
C4 C5 C6 C1 -0.7(7) . . . . ?
N1 C5 C6 C1 177.2(4) . . . . ?
C2 C1 C6 C5 0.0(7) . . . . ?
C7 C1 C6 C5 179.6(4) . . . . ?
Dy1 O1 C7 O2 2.5(8) . . . . ?
Dy1 O1 C7 C1 179.0(3) . . . . ?
Dy1 O2 C7 O1 -148.8(4) 2_556 . . . ?
Dy1 O2 C7 C1 34.6(8) 2_556 . . . ?
C6 C1 C7 O1 -25.2(7) . . . . ?
C2 C1 C7 O1 154.3(5) . . . . ?
C6 C1 C7 O2 151.4(5) . . . . ?
C2 C1 C7 O2 -29.1(7) . . . . ?
N4 N3 C8 N6 -0.5(5) . . . . ?
N4 N3 C8 N2 -179.8(4) . . . . ?
N5 N6 C8 N3 0.5(5) . . . . ?
N5 N6 C8 N2 179.7(5) . . . . ?
N1 N2 C8 N3 -176.6(4) . . . . ?
N1 N2 C8 N6 4.2(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.264
_database_code_depnum_ccdc_archive 'CCDC 993759'
