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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_R-Dy1
_database_code_depnum_ccdc_archive 'CCDC 972387'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H87 Dy N10 O8 S4'
_chemical_formula_weight         1295.08
_chemical_absolute_configuration syn

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.2956(7)
_cell_length_b                   11.6900(8)
_cell_length_c                   13.6363(9)
_cell_angle_alpha                106.8860(10)
_cell_angle_beta                 98.2390(10)
_cell_angle_gamma                94.4270(10)
_cell_volume                     1541.95(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    5864
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      26.10

_exptl_crystal_description       stick
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             675
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7569
_exptl_absorpt_correction_T_max  0.8385
_exptl_absorpt_process_details   '(Sadabs;bruker 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8591
_diffrn_reflns_av_R_equivalents  0.0243
__diffrn_reflns_av_unetI/netI    0.0759
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         26.13
_reflns_number_total             7156
_reflns_number_gt                7070
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0850P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(19)
_refine_ls_number_reflns         7156
_refine_ls_number_parameters     698
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1335
_refine_ls_wR_factor_gt          0.1322
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001

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 0.918787(19) -0.059371(19) 0.474661(19) 0.02769(12) Uani 1 1 d . . .
N1 N 0.8872(9) 0.2435(8) 0.7482(7) 0.041(2) Uani 1 1 d . . .
H1A H 0.9171 0.1895 0.6950 0.049 Uiso 1 1 calc R . .
H1B H 0.8990 0.3182 0.7387 0.049 Uiso 1 1 calc R . .
N2 N 1.1284(9) 0.1180(7) 0.7629(6) 0.0357(19) Uani 1 1 d . . .
H2A H 1.1248 0.0614 0.7976 0.043 Uiso 1 1 calc R . .
H2B H 1.0577 0.0964 0.7088 0.043 Uiso 1 1 calc R . .
N3 N 1.1015(9) 0.1346(7) 0.3237(6) 0.0326(18) Uani 1 1 d . . .
H3A H 1.0391 0.1314 0.2671 0.039 Uiso 1 1 calc R . .
H3B H 1.0782 0.0701 0.3460 0.039 Uiso 1 1 calc R . .
N4 N 1.2232(7) -0.0962(7) 0.2755(6) 0.0301(17) Uani 1 1 d . . .
H4A H 1.1644 -0.0723 0.3201 0.036 Uiso 1 1 calc R . .
H4B H 1.3037 -0.0942 0.3156 0.036 Uiso 1 1 calc R . .
N5 N 0.7108(8) -0.1569(7) 0.3459(6) 0.0307(17) Uani 1 1 d . . .
H5 H 0.6441 -0.1163 0.3740 0.037 Uiso 1 1 calc R . .
N6 N 0.8084(8) -0.2423(8) 0.5079(7) 0.0327(18) Uani 1 1 d . . .
H6 H 0.8620 -0.3019 0.4856 0.039 Uiso 1 1 calc R . .
N7 N 1.0903(10) -0.1686(10) 0.5277(10) 0.048(3) Uani 1 1 d . . .
N8 N 0.7975(10) 0.1040(9) 0.4479(8) 0.043(2) Uani 1 1 d . . .
N9 N 0.1805(14) 0.5523(13) 0.8334(11) 0.080(4) Uani 1 1 d . . .
N10 N 0.942(3) 0.033(3) 0.0057(19) 0.184(11) Uani 1 1 d DU . .
O1 O 0.8771(10) 0.0178(9) 0.6360(8) 0.037(3) Uani 1 1 d . . .
O2 O 1.0866(7) 0.0852(6) 0.5236(6) 0.0387(16) Uani 1 1 d . . .
O3 O 0.9880(10) -0.1095(9) 0.3248(8) 0.033(2) Uani 1 1 d . . .
O4 O 0.9600(11) 0.4467(10) 0.7006(7) 0.072(3) Uani 1 1 d . . .
O5 O 0.0037(11) 0.5404(9) 0.3357(9) 0.071(3) Uani 1 1 d . . .
O6 O 0.4611(10) 0.9653(12) 0.4218(9) 0.078(4) Uani 1 1 d D . .
O7 O 0.1029(16) 0.9494(12) 0.8630(11) 0.107(4) Uani 1 1 d DU . .
O8 O 0.625(3) 0.341(3) 1.0134(19) 0.212(10) Uani 1 1 d DU . .
S1 S 1.2746(9) -0.3140(9) 0.5711(8) 0.187(4) Uani 1 1 d U . .
S2 S 0.5917(4) 0.2440(4) 0.4746(4) 0.0808(13) Uani 1 1 d . . .
S3 S 0.4004(5) 0.6462(5) 0.9882(4) 0.0947(15) Uani 1 1 d . . .
S4 S 0.8412(12) 0.1545(10) 0.1733(8) 0.185(4) Uani 1 1 d DU . .
C1 C 0.7760(10) -0.0123(10) 0.6813(8) 0.037(2) Uani 1 1 d . . .
C2 C 0.7435(10) -0.1284(10) 0.6784(8) 0.037(2) Uani 1 1 d . . .
C3 C 0.6434(15) -0.1564(14) 0.7293(11) 0.051(4) Uani 1 1 d . . .
H3 H 0.6193 -0.2383 0.7242 0.061 Uiso 1 1 calc R . .
C4 C 0.5801(15) -0.0718(15) 0.7850(12) 0.063(4) Uani 1 1 d . . .
C5 C 0.6157(13) 0.0482(14) 0.7928(10) 0.065(4) Uani 1 1 d . . .
H5A H 0.5752 0.1091 0.8363 0.079 Uiso 1 1 calc R . .
C6 C 0.7076(12) 0.0806(14) 0.7393(11) 0.041(3) Uani 1 1 d . . .
C7 C 0.477(2) -0.103(2) 0.8489(19) 0.119(9) Uani 1 1 d . . .
H7A H 0.5161 -0.1479 0.8940 0.179 Uiso 1 1 calc R . .
H7B H 0.3991 -0.1531 0.8013 0.179 Uiso 1 1 calc R . .
H7C H 0.4503 -0.0289 0.8917 0.179 Uiso 1 1 calc R . .
C8 C 0.7391(10) 0.2071(10) 0.7410(9) 0.044(3) Uani 1 1 d . . .
H8A H 0.7083 0.2612 0.8013 0.053 Uiso 1 1 calc R . .
H8B H 0.6903 0.2181 0.6770 0.053 Uiso 1 1 calc R . .
C9 C 0.9682(11) 0.2479(9) 0.8484(8) 0.040(2) Uani 1 1 d . . .
H9 H 0.9339 0.1783 0.8701 0.048 Uiso 1 1 calc R . .
C10 C 0.9555(14) 0.3645(11) 0.9309(9) 0.053(3) Uani 1 1 d . . .
H10D H 0.8617 0.3666 0.9394 0.064 Uiso 1 1 calc R . .
H10E H 0.9825 0.4338 0.9072 0.064 Uiso 1 1 calc R . .
C11 C 1.0406(17) 0.3773(12) 1.0361(9) 0.065(4) Uani 1 1 d . . .
H11A H 1.0318 0.4549 1.0872 0.078 Uiso 1 1 calc R . .
H11B H 1.0107 0.3113 1.0628 0.078 Uiso 1 1 calc R . .
C12 C 1.1848(15) 0.3720(11) 1.0218(9) 0.059(4) Uani 1 1 d . . .
H12A H 1.2156 0.4418 1.0002 0.071 Uiso 1 1 calc R . .
H12B H 1.2402 0.3776 1.0891 0.071 Uiso 1 1 calc R . .
C13 C 1.2019(13) 0.2563(12) 0.9407(9) 0.055(3) Uani 1 1 d . . .
H13A H 1.1809 0.1871 0.9661 0.066 Uiso 1 1 calc R . .
H13B H 1.2953 0.2586 0.9308 0.066 Uiso 1 1 calc R . .
C14 C 1.1128(11) 0.2384(9) 0.8364(8) 0.040(2) Uani 1 1 d . . .
H14 H 1.1433 0.3028 0.8071 0.048 Uiso 1 1 calc R . .
C15 C 1.2509(10) 0.1134(10) 0.7190(9) 0.039(2) Uani 1 1 d . . .
H15A H 1.2531 0.0304 0.6741 0.046 Uiso 1 1 calc R . .
H15B H 1.3276 0.1334 0.7765 0.046 Uiso 1 1 calc R . .
C16 C 1.2638(12) 0.2022(13) 0.6539(10) 0.030(3) Uani 1 1 d . . .
C17 C 1.3598(14) 0.3017(12) 0.6923(11) 0.036(3) Uani 1 1 d . . .
H17 H 1.4159 0.3137 0.7571 0.043 Uiso 1 1 calc R . .
C18 C 1.3753(12) 0.3822(11) 0.6390(11) 0.044(3) Uani 1 1 d . . .
C19 C 1.2899(18) 0.3621(15) 0.5459(15) 0.048(5) Uani 1 1 d . . .
H19 H 1.2981 0.4178 0.5078 0.057 Uiso 1 1 calc R . .
C20 C 1.1912(14) 0.2621(12) 0.5054(11) 0.030(3) Uani 1 1 d . . .
C21 C 1.1787(11) 0.1801(9) 0.5611(12) 0.033(3) Uani 1 1 d . . .
C22 C 1.4795(14) 0.4910(12) 0.6810(11) 0.065(4) Uani 1 1 d . . .
H22A H 1.5676 0.4644 0.6825 0.097 Uiso 1 1 calc R . .
H22B H 1.4693 0.5361 0.7516 0.097 Uiso 1 1 calc R . .
H22C H 1.4693 0.5428 0.6360 0.097 Uiso 1 1 calc R . .
C23 C 1.0969(11) 0.2486(9) 0.4090(8) 0.037(2) Uani 1 1 d . . .
H23A H 1.1167 0.3184 0.3839 0.045 Uiso 1 1 calc R . .
H23B H 1.0062 0.2498 0.4251 0.045 Uiso 1 1 calc R . .
C24 C 1.2355(10) 0.1208(9) 0.2884(8) 0.038(2) Uani 1 1 d . . .
H24 H 1.3065 0.1389 0.3510 0.045 Uiso 1 1 calc R . .
C25 C 1.2623(12) 0.2096(10) 0.2274(9) 0.045(3) Uani 1 1 d . . .
H25A H 1.1880 0.1959 0.1690 0.054 Uiso 1 1 calc R . .
H25B H 1.2654 0.2928 0.2738 0.054 Uiso 1 1 calc R . .
C26 C 1.3884(13) 0.1981(11) 0.1853(11) 0.058(3) Uani 1 1 d . . .
H26A H 1.3992 0.2560 0.1457 0.070 Uiso 1 1 calc R . .
H26B H 1.4643 0.2172 0.2434 0.070 Uiso 1 1 calc R . .
C27 C 1.3862(13) 0.0728(13) 0.1158(12) 0.061(4) Uani 1 1 d . . .
H27A H 1.4709 0.0650 0.0894 0.073 Uiso 1 1 calc R . .
H27B H 1.3140 0.0561 0.0553 0.073 Uiso 1 1 calc R . .
C28 C 1.3656(11) -0.0186(10) 0.1733(11) 0.046(3) Uani 1 1 d . . .
H28A H 1.4417 -0.0061 0.2303 0.055 Uiso 1 1 calc R . .
H28B H 1.3618 -0.1009 0.1249 0.055 Uiso 1 1 calc R . .
C29 C 1.2374(13) -0.0074(10) 0.2189(10) 0.033(3) Uani 1 1 d . . .
H29 H 1.1612 -0.0267 0.1600 0.039 Uiso 1 1 calc R . .
C30 C 1.1768(13) -0.2253(12) 0.2096(11) 0.037(3) Uani 1 1 d . . .
H30A H 1.1851 -0.2796 0.2533 0.044 Uiso 1 1 calc R . .
H30B H 1.2312 -0.2502 0.1546 0.044 Uiso 1 1 calc R . .
C31 C 1.0307(11) -0.2321(8) 0.1602(8) 0.034(2) Uani 1 1 d . . .
C32 C 0.9854(10) -0.2958(8) 0.0564(8) 0.034(2) Uani 1 1 d . . .
H32 H 1.0465 -0.3318 0.0145 0.041 Uiso 1 1 calc R . .
C33 C 0.8545(10) -0.3079(9) 0.0126(8) 0.037(2) Uani 1 1 d . . .
C34 C 0.7675(9) -0.2583(9) 0.0767(8) 0.035(2) Uani 1 1 d . . .
H34 H 0.6759 -0.2687 0.0485 0.042 Uiso 1 1 calc R . .
C35 C 0.8097(9) -0.1937(9) 0.1807(7) 0.0294(19) Uani 1 1 d . . .
C36 C 0.9410(9) -0.1777(8) 0.2241(7) 0.0285(19) Uani 1 1 d . . .
C37 C 0.8048(12) -0.3697(13) -0.1030(9) 0.055(3) Uani 1 1 d . . .
H37A H 0.8175 -0.4551 -0.1202 0.083 Uiso 1 1 calc R . .
H37B H 0.8543 -0.3312 -0.1436 0.083 Uiso 1 1 calc R . .
H37C H 0.7105 -0.3627 -0.1196 0.083 Uiso 1 1 calc R . .
C38 C 0.7108(9) -0.1311(10) 0.2449(8) 0.035(2) Uani 1 1 d . . .
H38A H 0.7308 -0.0430 0.2593 0.042 Uiso 1 1 calc R . .
H38B H 0.6209 -0.1562 0.2029 0.042 Uiso 1 1 calc R . .
C39 C 0.6720(10) -0.2838(9) 0.3376(9) 0.030(2) Uani 1 1 d . . .
H39 H 0.7394 -0.3322 0.3054 0.036 Uiso 1 1 calc R . .
C40 C 0.5361(16) -0.3345(16) 0.2678(11) 0.045(4) Uani 1 1 d . . .
H40A H 0.5407 -0.3367 0.1952 0.054 Uiso 1 1 calc R . .
H40B H 0.4687 -0.2822 0.2925 0.054 Uiso 1 1 calc R . .
C41 C 0.497(2) -0.4660(17) 0.2723(14) 0.065(5) Uani 1 1 d . . .
H41A H 0.4058 -0.4959 0.2332 0.078 Uiso 1 1 calc R . .
H41B H 0.5571 -0.5199 0.2375 0.078 Uiso 1 1 calc R . .
C42 C 0.502(2) -0.4723(18) 0.3825(16) 0.062(6) Uani 1 1 d . . .
H42A H 0.4348 -0.4263 0.4152 0.074 Uiso 1 1 calc R . .
H42B H 0.4827 -0.5572 0.3807 0.074 Uiso 1 1 calc R . .
C43 C 0.6328(17) -0.4228(14) 0.4441(13) 0.043(4) Uani 1 1 d . . .
H43A H 0.6985 -0.4744 0.4150 0.052 Uiso 1 1 calc R . .
H43B H 0.6328 -0.4249 0.5161 0.052 Uiso 1 1 calc R . .
C44 C 0.6743(12) -0.2960(11) 0.4469(9) 0.034(3) Uani 1 1 d . . .
H44 H 0.6091 -0.2449 0.4797 0.041 Uiso 1 1 calc R . .
C45 C 0.8200(11) -0.2247(10) 0.6222(9) 0.042(2) Uani 1 1 d . . .
H45A H 0.9146 -0.2035 0.6545 0.050 Uiso 1 1 calc R . .
H45B H 0.7887 -0.3020 0.6323 0.050 Uiso 1 1 calc R . .
C46 C 1.1671(17) -0.2243(15) 0.5443(13) 0.070(4) Uani 1 1 d . . .
C47 C 0.7139(12) 0.1642(10) 0.4571(10) 0.044(3) Uani 1 1 d . . .
C48 C 0.2741(14) 0.5912(13) 0.8980(12) 0.063(4) Uani 1 1 d . . .
C49 C 0.896(3) 0.074(3) 0.0747(18) 0.148(10) Uani 1 1 d DU . .
C50 C 0.9451(17) 0.4648(16) 0.6049(11) 0.073(4) Uani 1 1 d . . .
C51 C 0.124(2) 0.8250(15) 0.8495(18) 0.121(8) Uani 1 1 d D . .
C52 C 0.133(3) 0.517(2) 0.3289(19) 0.133(9) Uani 1 1 d . . .
C53 C 0.421(2) 0.959(2) 0.5183(14) 0.088(6) Uani 1 1 d DU . .
C54 C 0.5620(19) 0.386(2) 0.9316(18) 0.100(6) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O3 2.194(10) . ?
Dy1 O2 2.202(7) . ?
Dy1 O1 2.239(10) . ?
Dy1 N7 2.406(10) . ?
Dy1 N8 2.446(9) . ?
Dy1 N5 2.520(8) . ?
Dy1 N6 2.531(8) . ?
N1 C9 1.480(14) . ?
N1 C8 1.532(14) . ?
N2 C15 1.469(14) . ?
N2 C14 1.508(13) . ?
N3 C23 1.502(12) . ?
N3 C24 1.530(13) . ?
N4 C29 1.472(14) . ?
N4 C30 1.513(15) . ?
N5 C39 1.473(13) . ?
N5 C38 1.492(13) . ?
N6 C44 1.492(14) . ?
N6 C45 1.498(14) . ?
N7 C46 1.101(17) . ?
N8 C47 1.150(14) . ?
N9 C48 1.169(19) . ?
N10 C49 1.112(10) . ?
O1 C1 1.358(14) . ?
O2 C21 1.326(13) . ?
O3 C36 1.367(13) . ?
O4 C50 1.372(16) . ?
O5 C52 1.39(3) . ?
O6 C53 1.452(10) . ?
O7 C51 1.448(10) . ?
O8 C54 1.457(10) . ?
S1 C46 1.657(17) . ?
S2 C47 1.628(12) . ?
S3 C48 1.604(15) . ?
S4 C49 1.607(10) . ?
C1 C2 1.360(15) . ?
C1 C6 1.442(18) . ?
C2 C3 1.391(17) . ?
C2 C45 1.511(16) . ?
C3 C4 1.34(2) . ?
C4 C5 1.39(2) . ?
C4 C7 1.55(2) . ?
C5 C6 1.370(19) . ?
C6 C8 1.48(2) . ?
C9 C10 1.523(14) . ?
C9 C14 1.530(16) . ?
C10 C11 1.531(19) . ?
C11 C12 1.53(2) . ?
C12 C13 1.519(18) . ?
C13 C14 1.526(15) . ?
C15 C16 1.559(17) . ?
C16 C21 1.38(2) . ?
C16 C17 1.39(2) . ?
C17 C18 1.360(18) . ?
C18 C19 1.38(2) . ?
C18 C22 1.512(17) . ?
C19 C20 1.41(2) . ?
C20 C21 1.394(18) . ?
C20 C23 1.479(19) . ?
C24 C29 1.526(15) . ?
C24 C25 1.538(15) . ?
C25 C26 1.493(16) . ?
C26 C27 1.493(18) . ?
C27 C28 1.52(2) . ?
C28 C29 1.536(17) . ?
C30 C31 1.544(16) . ?
C31 C32 1.386(15) . ?
C31 C36 1.419(13) . ?
C32 C33 1.373(14) . ?
C33 C34 1.383(14) . ?
C33 C37 1.523(15) . ?
C34 C35 1.386(14) . ?
C35 C36 1.372(13) . ?
C35 C38 1.529(13) . ?
C39 C44 1.534(16) . ?
C39 C40 1.542(16) . ?
C40 C41 1.58(2) . ?
C41 C42 1.52(3) . ?
C42 C43 1.45(3) . ?
C43 C44 1.499(17) . ?

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
O3 Dy1 O2 85.1(3) . . ?
O3 Dy1 O1 170.1(4) . . ?
O2 Dy1 O1 85.0(3) . . ?
O3 Dy1 N7 84.7(4) . . ?
O2 Dy1 N7 80.7(3) . . ?
O1 Dy1 N7 93.9(4) . . ?
O3 Dy1 N8 97.3(4) . . ?
O2 Dy1 N8 81.9(3) . . ?
O1 Dy1 N8 81.0(4) . . ?
N7 Dy1 N8 162.3(3) . . ?
O3 Dy1 N5 76.7(3) . . ?
O2 Dy1 N5 146.8(3) . . ?
O1 Dy1 N5 111.9(3) . . ?
N7 Dy1 N5 124.1(3) . . ?
N8 Dy1 N5 73.3(3) . . ?
O3 Dy1 N6 111.0(3) . . ?
O2 Dy1 N6 146.6(3) . . ?
O1 Dy1 N6 77.8(3) . . ?
N7 Dy1 N6 72.3(3) . . ?
N8 Dy1 N6 122.5(3) . . ?
N5 Dy1 N6 66.6(3) . . ?
C9 N1 C8 113.7(8) . . ?
C15 N2 C14 115.4(8) . . ?
C23 N3 C24 115.1(8) . . ?
C29 N4 C30 116.4(9) . . ?
C39 N5 C38 115.4(8) . . ?
C39 N5 Dy1 114.4(6) . . ?
C38 N5 Dy1 111.8(6) . . ?
C44 N6 C45 113.9(8) . . ?
C44 N6 Dy1 118.0(7) . . ?
C45 N6 Dy1 110.9(6) . . ?
C46 N7 Dy1 174.6(13) . . ?
C47 N8 Dy1 154.9(10) . . ?
C1 O1 Dy1 130.6(7) . . ?
C21 O2 Dy1 172.9(7) . . ?
C36 O3 Dy1 138.4(8) . . ?
O1 C1 C2 120.8(10) . . ?
O1 C1 C6 119.8(11) . . ?
C2 C1 C6 119.2(10) . . ?
C1 C2 C3 119.9(11) . . ?
C1 C2 C45 119.2(9) . . ?
C3 C2 C45 121.0(11) . . ?
C4 C3 C2 122.1(13) . . ?
C3 C4 C5 119.0(13) . . ?
C3 C4 C7 121.4(15) . . ?
C5 C4 C7 119.4(15) . . ?
C6 C5 C4 121.5(13) . . ?
C5 C6 C1 118.1(14) . . ?
C5 C6 C8 121.9(13) . . ?
C1 C6 C8 120.0(11) . . ?
C6 C8 N1 113.0(10) . . ?
N1 C9 C10 109.3(10) . . ?
N1 C9 C14 110.4(8) . . ?
C10 C9 C14 110.9(9) . . ?
C9 C10 C11 112.2(11) . . ?
C12 C11 C10 108.7(10) . . ?
C13 C12 C11 111.8(10) . . ?
C12 C13 C14 112.0(11) . . ?
N2 C14 C13 108.7(9) . . ?
N2 C14 C9 111.4(8) . . ?
C13 C14 C9 111.8(9) . . ?
N2 C15 C16 112.6(9) . . ?
C21 C16 C17 122.2(12) . . ?
C21 C16 C15 119.0(11) . . ?
C17 C16 C15 118.8(11) . . ?
C18 C17 C16 121.3(14) . . ?
C17 C18 C19 117.3(13) . . ?
C17 C18 C22 121.3(14) . . ?
C19 C18 C22 121.4(14) . . ?
C18 C19 C20 122.5(15) . . ?
C21 C20 C19 119.0(14) . . ?
C21 C20 C23 120.5(12) . . ?
C19 C20 C23 120.4(13) . . ?
O2 C21 C16 122.8(12) . . ?
O2 C21 C20 119.6(14) . . ?
C16 C21 C20 117.7(12) . . ?
C20 C23 N3 113.3(9) . . ?
C29 C24 N3 110.5(9) . . ?
C29 C24 C25 109.1(9) . . ?
N3 C24 C25 109.8(9) . . ?
C26 C25 C24 113.5(10) . . ?
C27 C26 C25 109.7(10) . . ?
C26 C27 C28 111.1(11) . . ?
C27 C28 C29 111.4(10) . . ?
N4 C29 C24 111.8(10) . . ?
N4 C29 C28 109.4(10) . . ?
C24 C29 C28 110.9(9) . . ?
N4 C30 C31 107.7(9) . . ?
C32 C31 C36 120.1(10) . . ?
C32 C31 C30 120.8(9) . . ?
C36 C31 C30 119.0(9) . . ?
C33 C32 C31 121.6(9) . . ?
C32 C33 C34 117.7(9) . . ?
C32 C33 C37 122.2(10) . . ?
C34 C33 C37 120.1(10) . . ?
C33 C34 C35 122.1(9) . . ?
C36 C35 C34 120.5(9) . . ?
C36 C35 C38 119.7(8) . . ?
C34 C35 C38 119.6(9) . . ?
O3 C36 C35 122.5(9) . . ?
O3 C36 C31 119.5(9) . . ?
C35 C36 C31 118.0(9) . . ?
N5 C38 C35 114.5(8) . . ?
N5 C39 C44 109.5(9) . . ?
N5 C39 C40 112.2(11) . . ?
C44 C39 C40 111.4(10) . . ?
C39 C40 C41 108.6(13) . . ?
C42 C41 C40 113.2(14) . . ?
C43 C42 C41 110.5(16) . . ?
C42 C43 C44 113.4(15) . . ?
N6 C44 C43 115.1(12) . . ?
N6 C44 C39 106.8(9) . . ?
C43 C44 C39 112.3(11) . . ?
N6 C45 C2 114.6(9) . . ?
N7 C46 S1 176.1(18) . . ?
N8 C47 S2 176.2(12) . . ?
N9 C48 S3 178.8(16) . . ?
N10 C49 S4 170(4) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.13
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.128
#######################################################################
#
#                 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_S-Dy1
_database_code_depnum_ccdc_archive 'CCDC 972388'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H85 Dy N10 O8 S4'
_chemical_formula_weight         1281.05
_chemical_absolute_configuration syn
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.409(3)
_cell_length_b                   11.756(3)
_cell_length_c                   13.650(4)
_cell_angle_alpha                106.550(5)
_cell_angle_beta                 98.526(6)
_cell_angle_gamma                94.961(6)
_cell_volume                     1568.9(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3142
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      20.10

_exptl_crystal_description       stick
_exptl_crystal_colour            clourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             667
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7893
_exptl_absorpt_correction_T_max  0.8744
_exptl_absorpt_process_details   ?

_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9742
_diffrn_reflns_av_R_equivalents  0.0472
__diffrn_reflns_av_unetI/netI    0.1026
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         26.13
_reflns_number_total             7624
_reflns_number_gt                6069
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.1178P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.064(19)
_refine_ls_number_reflns         7624
_refine_ls_number_parameters     688
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.1941
_refine_ls_wR_factor_gt          0.1737
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001

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 0.53628(4) 0.89478(4) 0.42593(4) 0.0466(2) Uani 1 1 d . . .
N1 N 0.5664(13) 0.5953(10) 0.1544(9) 0.053(3) Uani 1 1 d . . .
H1A H 0.5550 0.5221 0.1628 0.064 Uiso 1 1 calc R . .
H1B H 0.5367 0.6463 0.2062 0.064 Uiso 1 1 calc R . .
N2 N 0.3258(13) 0.7194(10) 0.1361(9) 0.050(3) Uani 1 1 d . . .
H2A H 0.3949 0.7417 0.1888 0.060 Uiso 1 1 calc R . .
H2B H 0.3285 0.7737 0.1012 0.060 Uiso 1 1 calc R . .
N3 N 0.3484(14) 0.7046(10) 0.5779(9) 0.049(3) Uani 1 1 d . . .
H3A H 0.4082 0.7076 0.6338 0.059 Uiso 1 1 calc R . .
H3B H 0.3718 0.7677 0.5564 0.059 Uiso 1 1 calc R . .
N4 N 0.2346(12) 0.9326(9) 0.6228(9) 0.048(3) Uani 1 1 d . . .
H4A H 0.1549 0.9337 0.5872 0.058 Uiso 1 1 calc R . .
H4B H 0.2864 0.9067 0.5760 0.058 Uiso 1 1 calc R . .
N5 N 0.7433(11) 0.9905(9) 0.5551(9) 0.047(3) Uani 1 1 d . . .
H5 H 0.8077 0.9517 0.5276 0.056 Uiso 1 1 calc R . .
N6 N 0.6472(13) 1.0787(10) 0.3932(10) 0.050(3) Uani 1 1 d . . .
H6 H 0.5962 1.1368 0.4145 0.060 Uiso 1 1 calc R . .
N7 N 0.364(2) 1.0049(17) 0.3745(16) 0.078(5) Uani 1 1 d . . .
N8 N 0.658(2) 0.7333(16) 0.4516(15) 0.076(5) Uani 1 1 d . . .
N9 N 0.266(2) 0.284(3) 1.068(2) 0.172(12) Uani 1 1 d DU . .
N10 N 0.503(6) 0.826(4) 0.917(4) 0.27(2) Uani 1 1 d U . .
O1 O 0.5779(16) 0.8238(13) 0.2644(11) 0.051(4) Uani 1 1 d . . .
O2 O 0.3692(10) 0.7504(8) 0.3771(9) 0.056(3) Uani 1 1 d . . .
O3 O 0.4650(17) 0.9468(15) 0.5768(13) 0.060(5) Uani 1 1 d . . .
O4 O 0.471(5) 0.315(4) 0.574(4) 0.271(18) Uani 1 1 d DU . .
O5 O -0.002(2) 0.8800(19) 0.4802(14) 0.128(6) Uani 1 1 d DU . .
O6 O 0.489(2) 0.3934(14) 0.1980(12) 0.130(7) Uani 1 1 d D . .
O7 O 0.354(2) 0.924(2) 0.0411(18) 0.156(8) Uani 1 1 d U . .
O8 O 0.917(4) 0.437(3) 0.943(3) 0.250(16) Uani 1 1 d DU . .
S1 S 0.1725(16) 1.1343(15) 0.3401(14) 0.232(6) Uani 1 1 d U . .
S2 S 0.8504(9) 0.5883(7) 0.4299(7) 0.143(3) Uani 1 1 d . . .
S3 S 0.0568(10) 0.1866(11) 0.9105(8) 0.171(4) Uani 1 1 d D . .
S4 S 0.600(3) 0.681(2) 0.735(2) 0.319(10) Uani 1 1 d DU . .
C1 C 0.6777(14) 0.8484(12) 0.2193(10) 0.046(3) Uani 1 1 d . . .
C2 C 0.7073(16) 0.9693(13) 0.2226(11) 0.054(4) Uani 1 1 d . . .
C3 C 0.812(2) 0.9938(19) 0.1740(15) 0.067(5) Uani 1 1 d . . .
H3 H 0.8395 1.0733 0.1799 0.081 Uiso 1 1 calc R . .
C4 C 0.874(3) 0.910(2) 0.120(2) 0.088(7) Uani 1 1 d U . .
C5 C 0.838(2) 0.7950(19) 0.1119(15) 0.082(5) Uani 1 1 d U . .
H5B H 0.8783 0.7357 0.0721 0.099 Uiso 1 1 calc R . .
C6 C 0.738(2) 0.7620(16) 0.1632(16) 0.057(5) Uani 1 1 d . . .
C7 C 0.980(4) 0.947(4) 0.050(3) 0.155(15) Uani 1 1 d . . .
H7A H 1.0503 1.0046 0.0954 0.232 Uiso 1 1 calc R . .
H7B H 0.9357 0.9806 0.0004 0.232 Uiso 1 1 calc R . .
H7C H 1.0141 0.8766 0.0145 0.232 Uiso 1 1 calc R . .
C8 C 0.7114(19) 0.6332(17) 0.1649(15) 0.075(5) Uani 1 1 d . . .
H8A H 0.7444 0.5806 0.1083 0.090 Uiso 1 1 calc R . .
H8B H 0.7575 0.6261 0.2296 0.090 Uiso 1 1 calc R . .
C9 C 0.4844(17) 0.5913(13) 0.0532(12) 0.059(4) Uani 1 1 d . . .
H9 H 0.5181 0.6583 0.0307 0.071 Uiso 1 1 calc R . .
C10 C 0.493(2) 0.4747(15) -0.0271(12) 0.075(5) Uani 1 1 d . . .
H10A H 0.4627 0.4087 -0.0030 0.090 Uiso 1 1 calc R . .
H10B H 0.5835 0.4699 -0.0341 0.090 Uiso 1 1 calc R . .
C11 C 0.411(2) 0.4608(16) -0.1335(13) 0.081(6) Uani 1 1 d . . .
H11A H 0.4208 0.3855 -0.1827 0.097 Uiso 1 1 calc R . .
H11B H 0.4403 0.5256 -0.1594 0.097 Uiso 1 1 calc R . .
C12 C 0.268(3) 0.4637(16) -0.1209(14) 0.094(7) Uani 1 1 d . . .
H12A H 0.2381 0.3955 -0.0995 0.113 Uiso 1 1 calc R . .
H12B H 0.2143 0.4575 -0.1871 0.113 Uiso 1 1 calc R . .
C13 C 0.251(2) 0.5801(15) -0.0396(14) 0.074(5) Uani 1 1 d . . .
H13A H 0.2706 0.6474 -0.0653 0.089 Uiso 1 1 calc R . .
H13B H 0.1609 0.5770 -0.0295 0.089 Uiso 1 1 calc R . .
C14 C 0.3411(16) 0.5993(12) 0.0640(10) 0.050(3) Uani 1 1 d . . .
H14 H 0.3118 0.5370 0.0937 0.060 Uiso 1 1 calc R . .
C15 C 0.2041(16) 0.7232(13) 0.1805(12) 0.056(4) Uani 1 1 d . . .
H15A H 0.1297 0.7066 0.1241 0.067 Uiso 1 1 calc R . .
H15B H 0.2044 0.8038 0.2253 0.067 Uiso 1 1 calc R . .
C16 C 0.184(2) 0.6315(19) 0.2456(18) 0.051(6) Uani 1 1 d . . .
C17 C 0.0934(19) 0.5364(18) 0.2103(15) 0.060(6) Uani 1 1 d . . .
H17 H 0.0377 0.5233 0.1470 0.072 Uiso 1 1 calc R . .
C18 C 0.081(2) 0.4603(15) 0.2632(18) 0.066(5) Uani 1 1 d . . .
C19 C 0.160(3) 0.482(2) 0.351(2) 0.063(7) Uani 1 1 d . . .
H19 H 0.1482 0.4285 0.3893 0.076 Uiso 1 1 calc R . .
C20 C 0.2586(19) 0.5739(14) 0.3930(13) 0.041(4) Uani 1 1 d . . .
C21 C 0.2765(16) 0.6570(11) 0.3379(16) 0.042(4) Uani 1 1 d . . .
C22 C -0.030(2) 0.3530(18) 0.220(2) 0.103(8) Uani 1 1 d . . .
H22A H -0.1105 0.3782 0.2404 0.155 Uiso 1 1 calc R . .
H22B H -0.0081 0.2895 0.2482 0.155 Uiso 1 1 calc R . .
H22C H -0.0418 0.3250 0.1459 0.155 Uiso 1 1 calc R . .
C23 C 0.3523(17) 0.5897(11) 0.4916(12) 0.054(4) Uani 1 1 d . . .
H23A H 0.4405 0.5893 0.4766 0.064 Uiso 1 1 calc R . .
H23B H 0.3331 0.5218 0.5165 0.064 Uiso 1 1 calc R . .
C24 C 0.2186(15) 0.7164(13) 0.6101(12) 0.051(3) Uani 1 1 d . . .
H24 H 0.1497 0.7006 0.5488 0.061 Uiso 1 1 calc R . .
C25 C 0.190(2) 0.6270(14) 0.6716(15) 0.074(5) Uani 1 1 d . . .
H25A H 0.1850 0.5460 0.6260 0.089 Uiso 1 1 calc R . .
H25B H 0.2627 0.6393 0.7286 0.089 Uiso 1 1 calc R . .
C26 C 0.066(2) 0.6395(16) 0.7141(17) 0.082(6) Uani 1 1 d . . .
H26A H -0.0081 0.6195 0.6572 0.099 Uiso 1 1 calc R . .
H26B H 0.0559 0.5840 0.7540 0.099 Uiso 1 1 calc R . .
C27 C 0.067(3) 0.762(2) 0.7806(18) 0.094(8) Uani 1 1 d . . .
H27A H 0.1365 0.7782 0.8408 0.113 Uiso 1 1 calc R . .
H27B H -0.0154 0.7675 0.8052 0.113 Uiso 1 1 calc R . .
C28 C 0.0876(18) 0.8537(14) 0.7278(18) 0.073(5) Uani 1 1 d . . .
H28A H 0.0917 0.9327 0.7766 0.087 Uiso 1 1 calc R . .
H28B H 0.0143 0.8429 0.6716 0.087 Uiso 1 1 calc R . .
C29 C 0.221(2) 0.8436(14) 0.6821(16) 0.049(5) Uani 1 1 d . . .
H29 H 0.2961 0.8615 0.7396 0.059 Uiso 1 1 calc R . .
C30 C 0.2902(19) 1.0599(14) 0.6875(14) 0.049(4) Uani 1 1 d . . .
H30A H 0.2852 1.1117 0.6434 0.059 Uiso 1 1 calc R . .
H30B H 0.2382 1.0878 0.7407 0.059 Uiso 1 1 calc R . .
C31 C 0.4296(16) 1.0670(12) 0.7375(11) 0.044(3) Uani 1 1 d . . .
C32 C 0.4730(17) 1.1296(11) 0.8413(12) 0.054(4) Uani 1 1 d . . .
H32 H 0.4126 1.1630 0.8810 0.065 Uiso 1 1 calc R . .
C33 C 0.6019(16) 1.1441(12) 0.8876(10) 0.051(4) Uani 1 1 d . . .
C34 C 0.6882(17) 1.0933(13) 0.8241(12) 0.056(4) Uani 1 1 d . . .
H34 H 0.7768 1.1039 0.8527 0.068 Uiso 1 1 calc R . .
C35 C 0.6479(14) 1.0276(11) 0.7203(10) 0.044(3) Uani 1 1 d . . .
C36 C 0.5126(14) 1.0112(10) 0.6761(11) 0.043(3) Uani 1 1 d . . .
C37 C 0.646(2) 1.2077(18) 1.0005(13) 0.085(6) Uani 1 1 d . . .
H37A H 0.5895 1.2665 1.0230 0.128 Uiso 1 1 calc R . .
H37B H 0.7343 1.2465 1.0123 0.128 Uiso 1 1 calc R . .
H37C H 0.6425 1.1510 1.0390 0.128 Uiso 1 1 calc R . .
C38 C 0.7445(15) 0.9653(13) 0.6550(12) 0.054(4) Uani 1 1 d . . .
H38A H 0.8324 0.9897 0.6956 0.065 Uiso 1 1 calc R . .
H38B H 0.7243 0.8795 0.6412 0.065 Uiso 1 1 calc R . .
C39 C 0.7819(15) 1.1169(12) 0.5639(14) 0.045(4) Uani 1 1 d . . .
H39 H 0.7156 1.1626 0.5945 0.054 Uiso 1 1 calc R . .
C40 C 0.909(3) 1.164(3) 0.635(2) 0.081(9) Uani 1 1 d . . .
H40A H 0.9768 1.1168 0.6112 0.098 Uiso 1 1 calc R . .
H40B H 0.9027 1.1618 0.7047 0.098 Uiso 1 1 calc R . .
C41 C 0.945(3) 1.304(2) 0.635(2) 0.108(11) Uani 1 1 d . . .
H41A H 1.0279 1.3386 0.6805 0.130 Uiso 1 1 calc R . .
H41B H 0.8779 1.3500 0.6609 0.130 Uiso 1 1 calc R . .
C42 C 0.954(4) 1.312(3) 0.513(3) 0.094(11) Uani 1 1 d . . .
H42A H 0.9762 1.3937 0.5129 0.112 Uiso 1 1 calc R . .
H42B H 1.0183 1.2637 0.4826 0.112 Uiso 1 1 calc R . .
C43 C 0.818(3) 1.2609(18) 0.457(2) 0.072(7) Uani 1 1 d . . .
H43A H 0.8093 1.2646 0.3859 0.087 Uiso 1 1 calc R . .
H43B H 0.7571 1.3100 0.4902 0.087 Uiso 1 1 calc R . .
C44 C 0.7789(19) 1.1293(16) 0.4537(13) 0.055(4) Uani 1 1 d . . .
H44 H 0.8421 1.0809 0.4212 0.066 Uiso 1 1 calc R . .
C45 C 0.636(2) 1.0592(14) 0.2787(12) 0.060(4) Uani 1 1 d . . .
H45A H 0.5439 1.0377 0.2472 0.072 Uiso 1 1 calc R . .
H45B H 0.6653 1.1349 0.2684 0.072 Uiso 1 1 calc R . .
C46 C 0.279(3) 1.056(2) 0.364(2) 0.090(6) Uani 1 1 d . . .
C47 C 0.734(2) 0.6715(15) 0.4448(15) 0.064(5) Uani 1 1 d . . .
C48 C 0.180(3) 0.242(3) 1.006(2) 0.159(14) Uani 1 1 d D . .
C49 C 0.530(5) 0.767(4) 0.823(4) 0.21(2) Uani 1 1 d DU . .
C50 C 0.337(5) 0.325(5) 0.582(5) 0.23(2) Uani 1 1 d DU . .
C51 C 0.831(5) 0.500(4) 0.895(4) 0.187(16) Uani 1 1 d DU . .
C52 C 0.505(3) 0.367(2) 0.2937(16) 0.120(9) Uani 1 1 d D . .
C53 C 0.032(3) 0.848(2) 0.3810(16) 0.096(7) Uani 1 1 d DU . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.202(9) . ?
Dy1 O3 2.232(17) . ?
Dy1 O1 2.245(14) . ?
Dy1 N7 2.43(2) . ?
Dy1 N8 2.447(19) . ?
Dy1 N5 2.519(12) . ?
Dy1 N6 2.545(11) . ?
N1 C9 1.50(2) . ?
N1 C8 1.51(2) . ?
N2 C15 1.48(2) . ?
N2 C14 1.510(17) . ?
N3 C24 1.487(19) . ?
N3 C23 1.527(17) . ?
N4 C29 1.50(2) . ?
N4 C30 1.52(2) . ?
N5 C39 1.470(18) . ?
N5 C38 1.474(19) . ?
N6 C44 1.47(2) . ?
N6 C45 1.50(2) . ?
N7 C46 1.13(3) . ?
N8 C47 1.12(2) . ?
N9 C48 1.104(10) . ?
N10 C49 1.36(6) . ?
O1 C1 1.335(19) . ?
O2 C21 1.324(17) . ?
O3 C36 1.34(2) . ?
O4 C50 1.434(10) . ?
O5 C53 1.405(10) . ?
O6 C52 1.414(10) . ?
O8 C51 1.416(10) . ?
S1 C46 1.56(3) . ?
S2 C47 1.62(2) . ?
S3 C48 1.627(10) . ?
S4 C49 1.640(10) . ?
C1 C6 1.35(2) . ?
C1 C2 1.415(19) . ?
C2 C3 1.41(2) . ?
C2 C45 1.45(2) . ?
C3 C4 1.33(3) . ?
C4 C5 1.34(3) . ?
C4 C7 1.66(3) . ?
C5 C6 1.42(3) . ?
C6 C8 1.52(3) . ?
C9 C10 1.51(2) . ?
C9 C14 1.53(2) . ?
C10 C11 1.53(3) . ?
C11 C12 1.53(3) . ?
C12 C13 1.54(3) . ?
C13 C14 1.52(2) . ?
C15 C16 1.60(2) . ?
C16 C17 1.32(3) . ?
C16 C21 1.41(3) . ?
C17 C18 1.31(3) . ?
C18 C19 1.30(3) . ?
C18 C22 1.55(2) . ?
C19 C20 1.35(3) . ?
C20 C21 1.41(2) . ?
C20 C23 1.49(3) . ?
C24 C29 1.53(2) . ?
C24 C25 1.55(2) . ?
C25 C26 1.49(3) . ?
C26 C27 1.46(3) . ?
C27 C28 1.48(3) . ?
C28 C29 1.61(2) . ?
C30 C31 1.49(2) . ?
C31 C36 1.371(19) . ?
C31 C32 1.38(2) . ?
C32 C33 1.37(2) . ?
C33 C34 1.39(2) . ?
C33 C37 1.49(2) . ?
C34 C35 1.39(2) . ?
C35 C36 1.42(2) . ?
C35 C38 1.54(2) . ?
C39 C40 1.48(3) . ?
C39 C44 1.55(2) . ?
C40 C41 1.65(4) . ?
C41 C42 1.71(4) . ?
C42 C43 1.50(4) . ?
C43 C44 1.55(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 85.0(5) . . ?
O2 Dy1 O1 86.3(5) . . ?
O3 Dy1 O1 171.0(7) . . ?
O2 Dy1 N7 80.7(5) . . ?
O3 Dy1 N7 82.8(7) . . ?
O1 Dy1 N7 94.0(7) . . ?
O2 Dy1 N8 82.4(5) . . ?
O3 Dy1 N8 99.1(7) . . ?
O1 Dy1 N8 81.6(6) . . ?
N7 Dy1 N8 162.8(5) . . ?
O2 Dy1 N5 146.3(4) . . ?
O3 Dy1 N5 77.2(5) . . ?
O1 Dy1 N5 111.4(5) . . ?
N7 Dy1 N5 124.1(5) . . ?
N8 Dy1 N5 72.7(5) . . ?
O2 Dy1 N6 146.8(4) . . ?
O3 Dy1 N6 110.3(5) . . ?
O1 Dy1 N6 76.5(5) . . ?
N7 Dy1 N6 72.6(5) . . ?
N8 Dy1 N6 121.8(5) . . ?
N5 Dy1 N6 66.9(4) . . ?
C9 N1 C8 115.2(12) . . ?
C15 N2 C14 115.4(11) . . ?
C24 N3 C23 114.5(12) . . ?
C29 N4 C30 115.8(13) . . ?
C39 N5 C38 114.9(12) . . ?
C39 N5 Dy1 114.0(9) . . ?
C38 N5 Dy1 112.5(8) . . ?
C44 N6 C45 114.2(13) . . ?
C44 N6 Dy1 117.1(10) . . ?
C45 N6 Dy1 110.0(9) . . ?
C46 N7 Dy1 170(2) . . ?
C47 N8 Dy1 159.2(17) . . ?
C1 O1 Dy1 133.0(11) . . ?
C21 O2 Dy1 172.7(11) . . ?
C36 O3 Dy1 137.9(13) . . ?
O1 C1 C6 122.3(15) . . ?
O1 C1 C2 116.2(14) . . ?
C6 C1 C2 121.0(14) . . ?
C3 C2 C1 115.6(15) . . ?
C3 C2 C45 124.5(15) . . ?
C1 C2 C45 119.8(14) . . ?
C4 C3 C2 124(2) . . ?
C3 C4 C5 119(2) . . ?
C3 C4 C7 120(2) . . ?
C5 C4 C7 121(2) . . ?
C4 C5 C6 121.2(18) . . ?
C1 C6 C5 118.9(16) . . ?
C1 C6 C8 120.9(17) . . ?
C5 C6 C8 119.8(17) . . ?
N1 C8 C6 110.7(15) . . ?
N1 C9 C10 108.8(14) . . ?
N1 C9 C14 111.0(11) . . ?
C10 C9 C14 109.0(14) . . ?
C9 C10 C11 113.2(16) . . ?
C10 C11 C12 107.8(14) . . ?
C11 C12 C13 111.0(16) . . ?
C14 C13 C12 111.8(16) . . ?
N2 C14 C13 108.2(13) . . ?
N2 C14 C9 111.1(11) . . ?
C13 C14 C9 112.8(13) . . ?
N2 C15 C16 115.0(13) . . ?
C17 C16 C21 124.2(19) . . ?
C17 C16 C15 122(2) . . ?
C21 C16 C15 113.8(18) . . ?
C18 C17 C16 121(2) . . ?
C19 C18 C17 118.0(19) . . ?
C19 C18 C22 123(2) . . ?
C17 C18 C22 119(2) . . ?
C18 C19 C20 126(2) . . ?
C19 C20 C21 118(2) . . ?
C19 C20 C23 123.8(18) . . ?
C21 C20 C23 118.3(15) . . ?
O2 C21 C20 119.9(18) . . ?
O2 C21 C16 127.0(17) . . ?
C20 C21 C16 113.0(15) . . ?
C20 C23 N3 114.4(13) . . ?
N3 C24 C29 109.0(13) . . ?
N3 C24 C25 109.9(13) . . ?
C29 C24 C25 108.1(13) . . ?
C26 C25 C24 113.5(16) . . ?
C27 C26 C25 110.9(17) . . ?
C26 C27 C28 113.5(18) . . ?
C27 C28 C29 110.3(17) . . ?
N4 C29 C24 110.0(14) . . ?
N4 C29 C28 109.0(15) . . ?
C24 C29 C28 109.7(13) . . ?
C31 C30 N4 111.1(13) . . ?
C36 C31 C32 121.6(16) . . ?
C36 C31 C30 117.4(14) . . ?
C32 C31 C30 120.9(13) . . ?
C33 C32 C31 122.2(14) . . ?
C32 C33 C34 116.4(13) . . ?
C32 C33 C37 121.4(16) . . ?
C34 C33 C37 122.1(16) . . ?
C35 C34 C33 123.1(15) . . ?
C34 C35 C36 118.7(14) . . ?
C34 C35 C38 121.5(14) . . ?
C36 C35 C38 119.6(12) . . ?
O3 C36 C31 119.6(15) . . ?
O3 C36 C35 122.6(14) . . ?
C31 C36 C35 117.8(14) . . ?
N5 C38 C35 114.9(12) . . ?
N5 C39 C40 110.7(17) . . ?
N5 C39 C44 109.1(13) . . ?
C40 C39 C44 114.2(16) . . ?
C39 C40 C41 106(2) . . ?
C40 C41 C42 112(2) . . ?
C43 C42 C41 101(2) . . ?
C42 C43 C44 113(2) . . ?
N6 C44 C39 107.5(13) . . ?
N6 C44 C43 112.6(18) . . ?
C39 C44 C43 112.1(15) . . ?
C2 C45 N6 117.2(13) . . ?
N7 C46 S1 171(3) . . ?
N8 C47 S2 175.4(19) . . ?
N9 C48 S3 176(4) . . ?
N10 C49 S4 161(5) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        26.13
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.257
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.151
#######################################################################
#
#                 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_R-Ho1
_database_code_depnum_ccdc_archive 'CCDC 972389'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H87 Ho N10 O8 S4'
_chemical_formula_weight         1297.51
_chemical_absolute_configuration syn
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.2970(10)
_cell_length_b                   11.6829(11)
_cell_length_c                   13.5696(13)
_cell_angle_alpha                106.808(2)
_cell_angle_beta                 98.496(2)
_cell_angle_gamma                94.203(2)
_cell_volume                     1533.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    5762
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.04

_exptl_crystal_description       stick
_exptl_crystal_colour            pale-orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7557
_exptl_absorpt_correction_T_max  0.8780
_exptl_absorpt_process_details   '(Sadabs; bruker 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7803
_diffrn_reflns_av_R_equivalents  0.0238
__diffrn_reflns_av_unetI/netI    0.0730
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.04
_reflns_number_total             6419
_reflns_number_gt                6387
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0897P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(14)
_refine_ls_number_reflns         6419
_refine_ls_number_parameters     697
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1313
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.014
_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
Ho1 Ho 0.91879(2) -0.05939(2) 0.47467(2) 0.02599(14) Uani 1 1 d . . .
N1 N 0.8875(10) 0.2441(8) 0.7480(6) 0.035(2) Uani 1 1 d . . .
H1A H 0.9170 0.1901 0.6944 0.043 Uiso 1 1 calc R . .
H1B H 0.8988 0.3188 0.7386 0.043 Uiso 1 1 calc R . .
N2 N 1.1291(9) 0.1191(7) 0.7655(6) 0.0284(19) Uani 1 1 d . . .
H2A H 1.1264 0.0633 0.8012 0.034 Uiso 1 1 calc R . .
H2B H 1.0580 0.0969 0.7114 0.034 Uiso 1 1 calc R . .
N3 N 1.1019(9) 0.1355(7) 0.3228(6) 0.0263(18) Uani 1 1 d . . .
H3A H 1.0387 0.1310 0.2659 0.032 Uiso 1 1 calc R . .
H3B H 1.0800 0.0715 0.3462 0.032 Uiso 1 1 calc R . .
N4 N 1.2225(8) -0.0952(7) 0.2776(6) 0.0258(18) Uani 1 1 d . . .
H4A H 1.1642 -0.0704 0.3224 0.031 Uiso 1 1 calc R . .
H4B H 1.3031 -0.0944 0.3176 0.031 Uiso 1 1 calc R . .
N5 N 0.7115(8) -0.1556(7) 0.3471(6) 0.0247(18) Uani 1 1 d . . .
H5 H 0.6452 -0.1148 0.3759 0.030 Uiso 1 1 calc R . .
N6 N 0.8105(8) -0.2431(7) 0.5091(6) 0.0259(18) Uani 1 1 d . . .
H6 H 0.8635 -0.3029 0.4859 0.031 Uiso 1 1 calc R . .
N7 N 1.0907(12) -0.1675(11) 0.5259(11) 0.047(3) Uani 1 1 d . . .
N8 N 0.7976(11) 0.1036(10) 0.4478(9) 0.040(3) Uani 1 1 d . . .
N9 N 0.1820(14) 0.5540(14) 0.8346(10) 0.075(4) Uani 1 1 d . . .
N10 N 0.938(4) 0.027(3) 0.012(3) 0.225(13) Uani 1 1 d DU . .
O1 O 0.8790(10) 0.0160(10) 0.6350(8) 0.030(3) Uani 1 1 d . . .
O2 O 1.0875(7) 0.0857(6) 0.5243(6) 0.0344(17) Uani 1 1 d . . .
O3 O 0.9887(11) -0.1089(10) 0.3252(8) 0.031(3) Uani 1 1 d . . .
O4 O 0.9563(12) 0.4469(9) 0.6993(7) 0.070(3) Uani 1 1 d . . .
O5 O 0.0048(10) 0.5394(8) 0.3348(8) 0.057(2) Uani 1 1 d . . .
O6 O 0.4628(15) 0.9625(19) 0.4281(13) 0.095(5) Uani 1 1 d D . .
O7 O 0.1014(16) 0.9518(15) 0.8634(12) 0.106(5) Uani 1 1 d DU . .
O8 O 0.5686(19) 0.3901(17) 0.9551(17) 0.137(6) Uani 1 1 d DU . .
S1 S 1.2788(10) -0.3075(9) 0.5766(8) 0.184(4) Uani 1 1 d U . .
S2 S 0.5931(4) 0.2454(4) 0.4736(3) 0.0715(12) Uani 1 1 d . . .
S3 S 0.3998(5) 0.6467(5) 0.9872(3) 0.0923(17) Uani 1 1 d . . .
S4 S 0.8462(13) 0.1561(10) 0.1717(8) 0.183(4) Uani 1 1 d DU . .
C1 C 0.7796(10) -0.0135(9) 0.6824(8) 0.028(2) Uani 1 1 d . . .
C2 C 0.7469(11) -0.1298(10) 0.6791(7) 0.032(2) Uani 1 1 d . . .
C3 C 0.6461(15) -0.1547(14) 0.7324(10) 0.044(4) Uani 1 1 d . . .
H3 H 0.6211 -0.2360 0.7287 0.053 Uiso 1 1 calc R . .
C4 C 0.5846(15) -0.0691(14) 0.7875(12) 0.052(4) Uani 1 1 d . . .
C5 C 0.6204(12) 0.0484(14) 0.7942(9) 0.050(3) Uani 1 1 d . . .
H5A H 0.5795 0.1099 0.8367 0.060 Uiso 1 1 calc R . .
C6 C 0.7135(14) 0.0793(13) 0.7416(11) 0.038(3) Uani 1 1 d . . .
C7 C 0.481(2) -0.104(2) 0.8502(15) 0.084(5) Uani 1 1 d U . .
H7A H 0.5085 -0.1701 0.8758 0.126 Uiso 1 1 calc R . .
H7B H 0.3944 -0.1289 0.8047 0.126 Uiso 1 1 calc R . .
H7C H 0.4756 -0.0339 0.9097 0.126 Uiso 1 1 calc R . .
C8 C 0.7410(12) 0.2080(11) 0.7417(10) 0.044(3) Uani 1 1 d . . .
H8A H 0.7101 0.2622 0.8021 0.052 Uiso 1 1 calc R . .
H8B H 0.6909 0.2176 0.6770 0.052 Uiso 1 1 calc R . .
C9 C 0.9707(11) 0.2481(9) 0.8505(7) 0.030(2) Uani 1 1 d . . .
H9 H 0.9376 0.1786 0.8729 0.036 Uiso 1 1 calc R . .
C10 C 0.9555(14) 0.3672(11) 0.9325(9) 0.048(3) Uani 1 1 d . . .
H10D H 0.9830 0.4362 0.9085 0.057 Uiso 1 1 calc R . .
H10E H 0.8615 0.3694 0.9402 0.057 Uiso 1 1 calc R . .
C11 C 1.0404(15) 0.3785(12) 1.0382(8) 0.049(3) Uani 1 1 d . . .
H11A H 1.0308 0.4556 1.0898 0.059 Uiso 1 1 calc R . .
H11B H 1.0100 0.3119 1.0640 0.059 Uiso 1 1 calc R . .
C12 C 1.1853(15) 0.3739(12) 1.0270(8) 0.054(4) Uani 1 1 d . . .
H12A H 1.2171 0.4440 1.0061 0.065 Uiso 1 1 calc R . .
H12B H 1.2390 0.3790 1.0953 0.065 Uiso 1 1 calc R . .
C13 C 1.2035(13) 0.2585(11) 0.9458(8) 0.043(3) Uani 1 1 d . . .
H13A H 1.1821 0.1890 0.9710 0.052 Uiso 1 1 calc R . .
H13B H 1.2973 0.2607 0.9370 0.052 Uiso 1 1 calc R . .
C14 C 1.1143(11) 0.2407(9) 0.8385(8) 0.033(2) Uani 1 1 d . . .
H14 H 1.1442 0.3050 0.8088 0.039 Uiso 1 1 calc R . .
C15 C 1.2543(12) 0.1149(11) 0.7203(9) 0.036(2) Uani 1 1 d . . .
H15A H 1.2569 0.0320 0.6750 0.043 Uiso 1 1 calc R . .
H15B H 1.3314 0.1350 0.7779 0.043 Uiso 1 1 calc R . .
C16 C 1.2647(15) 0.2047(15) 0.6549(11) 0.029(3) Uani 1 1 d . . .
C17 C 1.3606(14) 0.3047(13) 0.6916(10) 0.033(3) Uani 1 1 d . . .
H17 H 1.4162 0.3178 0.7572 0.040 Uiso 1 1 calc R . .
C18 C 1.3777(13) 0.3824(12) 0.6391(11) 0.040(3) Uani 1 1 d . . .
C19 C 1.2907(18) 0.3654(15) 0.5428(12) 0.037(4) Uani 1 1 d . . .
H19 H 1.2986 0.4209 0.5042 0.044 Uiso 1 1 calc R . .
C20 C 1.1913(14) 0.2631(12) 0.5051(10) 0.024(3) Uani 1 1 d . . .
C21 C 1.1773(11) 0.1809(9) 0.5612(11) 0.025(2) Uani 1 1 d . . .
C22 C 1.4836(15) 0.4881(13) 0.6818(10) 0.056(4) Uani 1 1 d . . .
H22A H 1.5703 0.4604 0.6754 0.084 Uiso 1 1 calc R . .
H22B H 1.4809 0.5275 0.7557 0.084 Uiso 1 1 calc R . .
H22C H 1.4687 0.5456 0.6424 0.084 Uiso 1 1 calc R . .
C23 C 1.0952(11) 0.2500(9) 0.4076(8) 0.029(2) Uani 1 1 d . . .
H23A H 1.1140 0.3197 0.3822 0.035 Uiso 1 1 calc R . .
H23B H 1.0045 0.2504 0.4237 0.035 Uiso 1 1 calc R . .
C24 C 1.2344(10) 0.1211(9) 0.2865(8) 0.026(2) Uani 1 1 d . . .
H24 H 1.3054 0.1389 0.3496 0.032 Uiso 1 1 calc R . .
C25 C 1.2607(12) 0.2115(10) 0.2285(9) 0.038(3) Uani 1 1 d . . .
H25A H 1.1860 0.2004 0.1702 0.046 Uiso 1 1 calc R . .
H25B H 1.2656 0.2941 0.2767 0.046 Uiso 1 1 calc R . .
C26 C 1.3885(13) 0.1977(10) 0.1851(9) 0.043(3) Uani 1 1 d . . .
H26A H 1.3984 0.2539 0.1435 0.052 Uiso 1 1 calc R . .
H26B H 1.4646 0.2185 0.2435 0.052 Uiso 1 1 calc R . .
C27 C 1.3878(13) 0.0717(13) 0.1177(10) 0.048(3) Uani 1 1 d . . .
H27A H 1.4734 0.0635 0.0929 0.057 Uiso 1 1 calc R . .
H27B H 1.3169 0.0539 0.0557 0.057 Uiso 1 1 calc R . .
C28 C 1.3661(11) -0.0172(10) 0.1755(10) 0.039(3) Uani 1 1 d . . .
H28A H 1.4409 -0.0034 0.2342 0.047 Uiso 1 1 calc R . .
H28B H 1.3645 -0.0997 0.1279 0.047 Uiso 1 1 calc R . .
C29 C 1.2370(12) -0.0079(11) 0.2183(10) 0.028(3) Uani 1 1 d . . .
H29 H 1.1616 -0.0282 0.1581 0.033 Uiso 1 1 calc R . .
C30 C 1.1741(13) -0.2229(11) 0.2094(10) 0.029(3) Uani 1 1 d . . .
H30A H 1.1836 -0.2788 0.2519 0.034 Uiso 1 1 calc R . .
H30B H 1.2277 -0.2466 0.1535 0.034 Uiso 1 1 calc R . .
C31 C 1.0298(11) -0.2302(9) 0.1611(8) 0.029(2) Uani 1 1 d . . .
C32 C 0.9846(10) -0.2943(9) 0.0562(8) 0.027(2) Uani 1 1 d . . .
H32 H 1.0456 -0.3303 0.0142 0.033 Uiso 1 1 calc R . .
C33 C 0.8523(11) -0.3064(10) 0.0121(8) 0.032(2) Uani 1 1 d . . .
C34 C 0.7653(11) -0.2570(9) 0.0768(8) 0.031(2) Uani 1 1 d . . .
H34 H 0.6735 -0.2686 0.0487 0.037 Uiso 1 1 calc R . .
C35 C 0.8079(10) -0.1904(9) 0.1825(7) 0.027(2) Uani 1 1 d . . .
C36 C 0.9403(10) -0.1765(9) 0.2238(8) 0.027(2) Uani 1 1 d . . .
C37 C 0.8047(14) -0.3710(13) -0.1036(9) 0.050(3) Uani 1 1 d . . .
H37A H 0.8773 -0.4088 -0.1342 0.076 Uiso 1 1 calc R . .
H37B H 0.7752 -0.3128 -0.1390 0.076 Uiso 1 1 calc R . .
H37C H 0.7308 -0.4330 -0.1122 0.076 Uiso 1 1 calc R . .
C38 C 0.7088(10) -0.1300(9) 0.2450(8) 0.029(2) Uani 1 1 d . . .
H38A H 0.7265 -0.0418 0.2587 0.035 Uiso 1 1 calc R . .
H38B H 0.6190 -0.1570 0.2027 0.035 Uiso 1 1 calc R . .
C39 C 0.6701(12) -0.2845(10) 0.3363(10) 0.029(3) Uani 1 1 d . . .
H39 H 0.7353 -0.3345 0.3021 0.035 Uiso 1 1 calc R . .
C40 C 0.5347(19) -0.3294(18) 0.2707(13) 0.046(5) Uani 1 1 d . . .
H40A H 0.5351 -0.3279 0.1982 0.055 Uiso 1 1 calc R . .
H40B H 0.4690 -0.2777 0.3000 0.055 Uiso 1 1 calc R . .
C41 C 0.497(2) -0.4660(17) 0.2719(14) 0.064(6) Uani 1 1 d . . .
H41A H 0.4062 -0.4961 0.2333 0.077 Uiso 1 1 calc R . .
H41B H 0.5580 -0.5182 0.2355 0.077 Uiso 1 1 calc R . .
C42 C 0.507(2) -0.4737(16) 0.3796(13) 0.046(5) Uani 1 1 d . . .
H42A H 0.4375 -0.4302 0.4127 0.055 Uiso 1 1 calc R . .
H42B H 0.4891 -0.5592 0.3765 0.055 Uiso 1 1 calc R . .
C43 C 0.6341(17) -0.4235(14) 0.4431(13) 0.038(4) Uani 1 1 d . . .
H43A H 0.7013 -0.4741 0.4150 0.046 Uiso 1 1 calc R . .
H43B H 0.6325 -0.4269 0.5150 0.046 Uiso 1 1 calc R . .
C44 C 0.6757(10) -0.2949(10) 0.4481(9) 0.024(2) Uani 1 1 d . . .
H44 H 0.6108 -0.2440 0.4817 0.029 Uiso 1 1 calc R . .
C45 C 0.8218(13) -0.2277(10) 0.6239(8) 0.033(2) Uani 1 1 d . . .
H45A H 0.9163 -0.2088 0.6570 0.040 Uiso 1 1 calc R . .
H45B H 0.7879 -0.3048 0.6332 0.040 Uiso 1 1 calc R . .
C46 C 1.1699(18) -0.2189(15) 0.5478(15) 0.080(6) Uani 1 1 d . . .
C47 C 0.7153(13) 0.1628(11) 0.4556(9) 0.038(3) Uani 1 1 d . . .
C48 C 0.2718(16) 0.5941(13) 0.8978(12) 0.060(4) Uani 1 1 d . . .
C49 C 0.869(5) 0.053(3) 0.070(3) 0.223(15) Uani 1 1 d DU . .
C50 C 0.9472(17) 0.4606(17) 0.6038(12) 0.069(4) Uani 1 1 d . . .
C51 C 0.1300(19) 0.8309(17) 0.8544(16) 0.102(8) Uani 1 1 d D . .
C52 C 0.143(3) 0.520(2) 0.3326(16) 0.103(7) Uani 1 1 d . . .
C53 C 0.641(3) 0.326(3) 1.018(2) 0.131(9) Uani 1 1 d DU . .
C54 C 0.417(2) 0.951(3) 0.5217(16) 0.119(14) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O3 2.186(12) . ?
Ho1 O1 2.211(10) . ?
Ho1 O2 2.215(7) . ?
Ho1 N7 2.384(12) . ?
Ho1 N8 2.436(11) . ?
Ho1 N5 2.500(8) . ?
Ho1 N6 2.540(8) . ?
N1 C9 1.508(14) . ?
N1 C8 1.519(15) . ?
N2 C15 1.505(14) . ?
N2 C14 1.511(13) . ?
N3 C23 1.504(12) . ?
N3 C24 1.522(13) . ?
N4 C29 1.482(15) . ?
N4 C30 1.512(14) . ?
N5 C39 1.494(14) . ?
N5 C38 1.496(13) . ?
N6 C44 1.492(13) . ?
N6 C45 1.502(13) . ?
N7 C46 1.10(2) . ?
N8 C47 1.130(16) . ?
N9 C48 1.131(19) . ?
N10 C49 1.119(11) . ?
O1 C1 1.361(14) . ?
O2 C21 1.317(13) . ?
O3 C36 1.370(14) . ?
O4 C50 1.342(17) . ?
O5 C52 1.46(3) . ?
O6 C54 1.454(10) . ?
O7 C51 1.438(10) . ?
O8 C53 1.449(10) . ?
S1 C46 1.66(2) . ?
S2 C47 1.645(13) . ?
S3 C48 1.601(17) . ?
S4 C49 1.612(11) . ?
C1 C2 1.362(15) . ?
C1 C6 1.431(18) . ?
C2 C3 1.409(16) . ?
C2 C45 1.506(16) . ?
C3 C4 1.33(2) . ?
C4 C5 1.37(2) . ?
C4 C7 1.56(2) . ?
C5 C6 1.364(19) . ?
C6 C8 1.51(2) . ?
C9 C14 1.518(16) . ?
C9 C10 1.545(15) . ?
C10 C11 1.531(18) . ?
C11 C12 1.52(2) . ?
C12 C13 1.518(18) . ?
C13 C14 1.552(15) . ?
C15 C16 1.566(19) . ?
C16 C21 1.39(2) . ?
C16 C17 1.39(2) . ?
C17 C18 1.32(2) . ?
C18 C19 1.42(2) . ?
C18 C22 1.501(17) . ?
C19 C20 1.43(2) . ?
C20 C21 1.399(19) . ?
C20 C23 1.492(18) . ?
C24 C25 1.520(15) . ?
C24 C29 1.528(15) . ?
C25 C26 1.520(16) . ?
C26 C27 1.491(17) . ?
C27 C28 1.49(2) . ?
C28 C29 1.527(17) . ?
C30 C31 1.518(16) . ?
C31 C32 1.393(15) . ?
C31 C36 1.405(15) . ?
C32 C33 1.384(15) . ?
C33 C34 1.387(16) . ?
C33 C37 1.518(14) . ?
C34 C35 1.405(14) . ?
C35 C36 1.374(14) . ?
C35 C38 1.508(14) . ?
C39 C40 1.506(19) . ?
C39 C44 1.549(16) . ?
C40 C41 1.62(3) . ?
C41 C42 1.48(3) . ?
C42 C43 1.44(2) . ?
C43 C44 1.511(17) . ?

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
O3 Ho1 O1 169.7(4) . . ?
O3 Ho1 O2 84.7(3) . . ?
O1 Ho1 O2 85.0(3) . . ?
O3 Ho1 N7 83.7(4) . . ?
O1 Ho1 N7 94.2(4) . . ?
O2 Ho1 N7 80.3(4) . . ?
O3 Ho1 N8 97.5(4) . . ?
O1 Ho1 N8 81.4(4) . . ?
O2 Ho1 N8 82.0(3) . . ?
N7 Ho1 N8 162.0(3) . . ?
O3 Ho1 N5 77.4(3) . . ?
O1 Ho1 N5 111.8(3) . . ?
O2 Ho1 N5 147.1(3) . . ?
N7 Ho1 N5 124.2(4) . . ?
N8 Ho1 N5 73.3(3) . . ?
O3 Ho1 N6 111.2(3) . . ?
O1 Ho1 N6 77.6(3) . . ?
O2 Ho1 N6 146.1(3) . . ?
N7 Ho1 N6 72.4(3) . . ?
N8 Ho1 N6 123.0(3) . . ?
N5 Ho1 N6 66.9(3) . . ?
C9 N1 C8 113.3(9) . . ?
C15 N2 C14 114.5(8) . . ?
C23 N3 C24 116.2(8) . . ?
C29 N4 C30 114.0(9) . . ?
C39 N5 C38 114.0(8) . . ?
C39 N5 Ho1 115.8(6) . . ?
C38 N5 Ho1 112.3(6) . . ?
C44 N6 C45 113.3(8) . . ?
C44 N6 Ho1 117.0(6) . . ?
C45 N6 Ho1 112.1(6) . . ?
C46 N7 Ho1 178.7(15) . . ?
C47 N8 Ho1 155.5(11) . . ?
C1 O1 Ho1 131.5(7) . . ?
C21 O2 Ho1 172.3(7) . . ?
C36 O3 Ho1 137.6(8) . . ?
O1 C1 C2 120.7(10) . . ?
O1 C1 C6 119.8(11) . . ?
C2 C1 C6 119.4(11) . . ?
C1 C2 C3 118.3(12) . . ?
C1 C2 C45 120.4(10) . . ?
C3 C2 C45 121.2(11) . . ?
C4 C3 C2 122.6(13) . . ?
C3 C4 C5 119.3(13) . . ?
C3 C4 C7 119.1(14) . . ?
C5 C4 C7 121.4(15) . . ?
C6 C5 C4 121.6(13) . . ?
C5 C6 C1 118.7(13) . . ?
C5 C6 C8 120.4(13) . . ?
C1 C6 C8 120.9(12) . . ?
C6 C8 N1 111.6(10) . . ?
N1 C9 C14 110.2(8) . . ?
N1 C9 C10 107.7(10) . . ?
C14 C9 C10 110.9(9) . . ?
C11 C10 C9 110.4(11) . . ?
C12 C11 C10 110.0(10) . . ?
C13 C12 C11 111.3(10) . . ?
C12 C13 C14 111.9(10) . . ?
N2 C14 C9 110.2(8) . . ?
N2 C14 C13 108.5(9) . . ?
C9 C14 C13 110.8(9) . . ?
N2 C15 C16 112.0(10) . . ?
C21 C16 C17 122.2(14) . . ?
C21 C16 C15 118.3(13) . . ?
C17 C16 C15 119.6(13) . . ?
C18 C17 C16 122.9(13) . . ?
C17 C18 C19 118.4(13) . . ?
C17 C18 C22 120.7(14) . . ?
C19 C18 C22 120.8(15) . . ?
C18 C19 C20 118.8(14) . . ?
C21 C20 C19 121.5(13) . . ?
C21 C20 C23 119.8(12) . . ?
C19 C20 C23 118.6(12) . . ?
O2 C21 C16 123.0(13) . . ?
O2 C21 C20 120.8(13) . . ?
C16 C21 C20 116.1(12) . . ?
C20 C23 N3 112.1(9) . . ?
C25 C24 N3 109.4(9) . . ?
C25 C24 C29 111.4(9) . . ?
N3 C24 C29 110.8(8) . . ?
C26 C25 C24 112.2(10) . . ?
C27 C26 C25 110.4(9) . . ?
C26 C27 C28 111.6(10) . . ?
C27 C28 C29 112.2(11) . . ?
N4 C29 C28 110.0(10) . . ?
N4 C29 C24 111.4(10) . . ?
C28 C29 C24 109.7(9) . . ?
N4 C30 C31 109.1(9) . . ?
C32 C31 C36 119.8(10) . . ?
C32 C31 C30 120.4(9) . . ?
C36 C31 C30 119.8(10) . . ?
C33 C32 C31 121.2(10) . . ?
C32 C33 C34 117.7(9) . . ?
C32 C33 C37 120.9(10) . . ?
C34 C33 C37 121.3(10) . . ?
C33 C34 C35 122.4(10) . . ?
C36 C35 C34 118.7(9) . . ?
C36 C35 C38 122.0(9) . . ?
C34 C35 C38 119.1(9) . . ?
O3 C36 C35 121.5(10) . . ?
O3 C36 C31 118.5(10) . . ?
C35 C36 C31 120.0(10) . . ?
N5 C38 C35 113.7(8) . . ?
N5 C39 C40 112.1(12) . . ?
N5 C39 C44 107.4(9) . . ?
C40 C39 C44 111.6(11) . . ?
C39 C40 C41 107.3(14) . . ?
C42 C41 C40 112.0(13) . . ?
C43 C42 C41 112.5(16) . . ?
C42 C43 C44 114.0(15) . . ?
N6 C44 C43 115.0(11) . . ?
N6 C44 C39 108.1(9) . . ?
C43 C44 C39 110.2(10) . . ?
N6 C45 C2 113.3(9) . . ?
N7 C46 S1 174.7(18) . . ?
N8 C47 S2 176.1(12) . . ?
N9 C48 S3 178.2(16) . . ?
N10 C49 S4 144(5) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.137
#######################################################################
#
#                 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_S-Ho1
_database_code_depnum_ccdc_archive 'CCDC 972390'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H87 Ho N10 O8 S4'
_chemical_formula_weight         1297.51
_chemical_absolute_configuration syn
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.2833(8)
_cell_length_b                   11.6475(8)
_cell_length_c                   13.6139(10)
_cell_angle_alpha                106.8000(10)
_cell_angle_beta                 98.1310(10)
_cell_angle_gamma                94.3980(10)
_cell_volume                     1533.38(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    4828
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      26.12

_exptl_crystal_description       stick
_exptl_crystal_colour            pale-orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             676
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7556
_exptl_absorpt_correction_T_max  0.8905
_exptl_absorpt_process_details   '(Sadabs;bruker 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8586
_diffrn_reflns_av_R_equivalents  0.0310
__diffrn_reflns_av_unetI/netI    0.0925
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         26.19
_reflns_number_total             7160
_reflns_number_gt                7041
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0704P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(18)
_refine_ls_number_reflns         7160
_refine_ls_number_parameters     698
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1298
_refine_ls_wR_factor_gt          0.1284
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.014
_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
Ho1 Ho 0.53627(2) 0.89474(2) 0.42594(2) 0.02373(12) Uani 1 1 d . . .
N1 N 0.5702(8) 0.5916(8) 0.1555(6) 0.032(2) Uani 1 1 d . . .
H1A H 0.5417 0.6487 0.2075 0.039 Uiso 1 1 calc R . .
H1B H 0.5550 0.5181 0.1670 0.039 Uiso 1 1 calc R . .
N2 N 0.3291(9) 0.7172(8) 0.1363(6) 0.0304(19) Uani 1 1 d . . .
H2A H 0.4002 0.7396 0.1900 0.036 Uiso 1 1 calc R . .
H2B H 0.3323 0.7732 0.1005 0.036 Uiso 1 1 calc R . .
N3 N 0.3543(9) 0.7016(8) 0.5786(7) 0.030(2) Uani 1 1 d . . .
H3A H 0.3770 0.7665 0.5561 0.037 Uiso 1 1 calc R . .
H3B H 0.4176 0.7044 0.6345 0.037 Uiso 1 1 calc R . .
N4 N 0.2325(8) 0.9318(7) 0.6269(7) 0.0256(17) Uani 1 1 d . . .
H4A H 0.1515 0.9315 0.5882 0.031 Uiso 1 1 calc R . .
H4B H 0.2902 0.9081 0.5811 0.031 Uiso 1 1 calc R . .
N5 N 0.7437(7) 0.9888(7) 0.5546(6) 0.0249(17) Uani 1 1 d . . .
H5 H 0.8107 0.9483 0.5264 0.030 Uiso 1 1 calc R . .
N6 N 0.6472(8) 1.0776(8) 0.3925(7) 0.0288(19) Uani 1 1 d . . .
H6 H 0.5938 1.1373 0.4153 0.035 Uiso 1 1 calc R . .
N7 N 0.3676(10) 1.0064(9) 0.3734(9) 0.035(2) Uani 1 1 d . . .
N8 N 0.6547(10) 0.7297(10) 0.4518(9) 0.041(3) Uani 1 1 d . . .
N9 N 0.2744(12) 0.2852(11) 1.0691(10) 0.060(3) Uani 1 1 d . . .
N10 N 0.503(2) 0.7978(19) 0.8863(14) 0.129(7) Uani 1 1 d DU . .
O1 O 0.5780(10) 0.8168(10) 0.2650(8) 0.030(2) Uani 1 1 d . . .
O2 O 0.3678(7) 0.7508(6) 0.3771(6) 0.0331(16) Uani 1 1 d . . .
O3 O 0.4656(10) 0.9467(10) 0.5765(9) 0.030(2) Uani 1 1 d . . .
O4 O 0.4534(12) 0.2999(11) 0.5711(10) 0.083(3) Uani 1 1 d U . .
O5 O 0.3571(13) 0.8890(11) 0.0387(10) 0.090(4) Uani 1 1 d . . .
O6 O 0.4958(10) 0.3843(9) 0.2006(7) 0.064(3) Uani 1 1 d . . .
O7 O 0.8901(14) 0.4530(15) 0.9663(13) 0.115(5) Uani 1 1 d DU . .
O8 O -0.0066(10) 0.8690(11) 0.4795(9) 0.064(3) Uani 1 1 d DU . .
S1 S 0.1869(6) 1.1551(6) 0.3254(6) 0.125(2) Uani 1 1 d . . .
S2 S 0.8610(4) 0.5895(4) 0.4308(3) 0.0634(10) Uani 1 1 d . . .
S3 S 0.0504(4) 0.1928(5) 0.9146(3) 0.0811(14) Uani 1 1 d . . .
S4 S 0.6196(9) 0.6785(7) 0.7268(6) 0.138(3) Uani 1 1 d D . .
C1 C 0.6810(9) 0.8449(9) 0.2201(7) 0.025(2) Uani 1 1 d . . .
C2 C 0.7141(10) 0.9634(9) 0.2235(7) 0.028(2) Uani 1 1 d . . .
C3 C 0.8169(14) 0.9913(15) 0.1726(11) 0.044(3) Uani 1 1 d . . .
H3 H 0.8427 1.0731 0.1775 0.053 Uiso 1 1 calc R . .
C4 C 0.8795(15) 0.9026(13) 0.1167(11) 0.050(4) Uani 1 1 d . . .
C5 C 0.8445(11) 0.7847(13) 0.1113(9) 0.049(3) Uani 1 1 d . . .
H5B H 0.8866 0.7228 0.0703 0.058 Uiso 1 1 calc R . .
C6 C 0.7468(13) 0.7535(15) 0.1657(11) 0.039(4) Uani 1 1 d . . .
C7 C 0.9863(18) 0.9320(17) 0.0543(16) 0.089(7) Uani 1 1 d . . .
H7A H 1.0652 0.9781 0.1029 0.133 Uiso 1 1 calc R . .
H7B H 0.9511 0.9800 0.0105 0.133 Uiso 1 1 calc R . .
H7C H 1.0098 0.8566 0.0102 0.133 Uiso 1 1 calc R . .
C8 C 0.7166(10) 0.6221(10) 0.1620(9) 0.039(3) Uani 1 1 d . . .
H8A H 0.7462 0.5686 0.1006 0.047 Uiso 1 1 calc R . .
H8B H 0.7652 0.6091 0.2253 0.047 Uiso 1 1 calc R . .
C9 C 0.4899(10) 0.5861(9) 0.0517(8) 0.028(2) Uani 1 1 d . . .
H9 H 0.5247 0.6553 0.0293 0.034 Uiso 1 1 calc R . .
C10 C 0.5038(13) 0.4677(11) -0.0290(9) 0.046(3) Uani 1 1 d . . .
H10A H 0.4746 0.3989 -0.0051 0.055 Uiso 1 1 calc R . .
H10B H 0.5981 0.4645 -0.0363 0.055 Uiso 1 1 calc R . .
C11 C 0.4208(13) 0.4562(12) -0.1353(9) 0.050(3) Uani 1 1 d . . .
H11A H 0.4521 0.5226 -0.1612 0.061 Uiso 1 1 calc R . .
H11B H 0.4299 0.3784 -0.1864 0.061 Uiso 1 1 calc R . .
C12 C 0.2766(12) 0.4620(12) -0.1226(10) 0.050(3) Uani 1 1 d . . .
H12A H 0.2446 0.3924 -0.1008 0.060 Uiso 1 1 calc R . .
H12B H 0.2225 0.4561 -0.1905 0.060 Uiso 1 1 calc R . .
C13 C 0.2585(12) 0.5803(10) -0.0414(8) 0.040(3) Uani 1 1 d . . .
H13A H 0.2822 0.6496 -0.0664 0.048 Uiso 1 1 calc R . .
H13B H 0.1644 0.5793 -0.0330 0.048 Uiso 1 1 calc R . .
C14 C 0.3449(10) 0.5964(9) 0.0641(8) 0.030(2) Uani 1 1 d . . .
H14 H 0.3130 0.5317 0.0930 0.036 Uiso 1 1 calc R . .
C15 C 0.2051(10) 0.7229(10) 0.1816(9) 0.034(2) Uani 1 1 d . . .
H15A H 0.1279 0.7032 0.1246 0.040 Uiso 1 1 calc R . .
H15B H 0.2035 0.8063 0.2266 0.040 Uiso 1 1 calc R . .
C16 C 0.1934(13) 0.6358(13) 0.2454(12) 0.030(3) Uani 1 1 d . . .
C17 C 0.0958(12) 0.5376(13) 0.2082(9) 0.032(3) Uani 1 1 d . . .
H17 H 0.0392 0.5260 0.1437 0.038 Uiso 1 1 calc R . .
C18 C 0.0791(11) 0.4550(10) 0.2637(12) 0.034(3) Uani 1 1 d . . .
C19 C 0.1610(14) 0.4743(13) 0.3550(12) 0.031(3) Uani 1 1 d . . .
H19 H 0.1518 0.4190 0.3937 0.037 Uiso 1 1 calc R . .
C20 C 0.2589(12) 0.5735(11) 0.3940(10) 0.023(3) Uani 1 1 d . . .
C21 C 0.2759(10) 0.6567(9) 0.3379(12) 0.025(2) Uani 1 1 d . . .
C22 C -0.0279(12) 0.3471(12) 0.2187(11) 0.052(3) Uani 1 1 d . . .
H22A H -0.0180 0.2916 0.2606 0.078 Uiso 1 1 calc R . .
H22B H -0.0193 0.3051 0.1468 0.078 Uiso 1 1 calc R . .
H22C H -0.1152 0.3752 0.2198 0.078 Uiso 1 1 calc R . .
C23 C 0.3571(10) 0.5870(9) 0.4922(8) 0.030(2) Uani 1 1 d . . .
H23A H 0.3378 0.5170 0.5175 0.036 Uiso 1 1 calc R . .
H23B H 0.4474 0.5854 0.4749 0.036 Uiso 1 1 calc R . .
C24 C 0.2195(10) 0.7151(9) 0.6156(8) 0.026(2) Uani 1 1 d . . .
H24 H 0.1480 0.6972 0.5534 0.032 Uiso 1 1 calc R . .
C25 C 0.1953(11) 0.6248(10) 0.6738(9) 0.038(3) Uani 1 1 d . . .
H25A H 0.1923 0.5420 0.6260 0.046 Uiso 1 1 calc R . .
H25B H 0.2702 0.6374 0.7317 0.046 Uiso 1 1 calc R . .
C26 C 0.0675(13) 0.6355(11) 0.7172(10) 0.047(3) Uani 1 1 d . . .
H26A H -0.0088 0.6156 0.6594 0.057 Uiso 1 1 calc R . .
H26B H 0.0579 0.5780 0.7576 0.057 Uiso 1 1 calc R . .
C27 C 0.0696(13) 0.7628(12) 0.7865(10) 0.046(3) Uani 1 1 d . . .
H27A H -0.0149 0.7710 0.8132 0.055 Uiso 1 1 calc R . .
H27B H 0.1422 0.7802 0.8468 0.055 Uiso 1 1 calc R . .
C28 C 0.0893(11) 0.8522(10) 0.7281(10) 0.037(3) Uani 1 1 d . . .
H28A H 0.0912 0.9349 0.7754 0.045 Uiso 1 1 calc R . .
H28B H 0.0136 0.8378 0.6704 0.045 Uiso 1 1 calc R . .
C29 C 0.2192(13) 0.8425(11) 0.6831(10) 0.029(3) Uani 1 1 d . . .
H29 H 0.2951 0.8618 0.7423 0.034 Uiso 1 1 calc R . .
C30 C 0.2808(12) 1.0587(12) 0.6944(10) 0.029(3) Uani 1 1 d . . .
H30A H 0.2693 1.1149 0.6523 0.034 Uiso 1 1 calc R . .
H30B H 0.2276 1.0815 0.7507 0.034 Uiso 1 1 calc R . .
C31 C 0.4237(10) 1.0696(9) 0.7409(8) 0.027(2) Uani 1 1 d . . .
C32 C 0.4700(10) 1.1318(9) 0.8457(8) 0.028(2) Uani 1 1 d . . .
H32 H 0.4096 1.1676 0.8886 0.034 Uiso 1 1 calc R . .
C33 C 0.6004(10) 1.1423(10) 0.8877(8) 0.031(2) Uani 1 1 d . . .
C34 C 0.6861(9) 1.0895(9) 0.8224(8) 0.029(2) Uani 1 1 d . . .
H34 H 0.7774 1.0970 0.8507 0.035 Uiso 1 1 calc R . .
C35 C 0.6445(9) 1.0265(8) 0.7185(7) 0.0217(19) Uani 1 1 d . . .
C36 C 0.5143(9) 1.0136(8) 0.6769(8) 0.024(2) Uani 1 1 d . . .
C37 C 0.6494(12) 1.2029(12) 1.0032(9) 0.048(3) Uani 1 1 d . . .
H37A H 0.5735 1.2203 1.0389 0.073 Uiso 1 1 calc R . .
H37B H 0.7058 1.2785 1.0132 0.073 Uiso 1 1 calc R . .
H37C H 0.7005 1.1489 1.0320 0.073 Uiso 1 1 calc R . .
C38 C 0.7422(9) 0.9628(9) 0.6543(8) 0.027(2) Uani 1 1 d . . .
H38A H 0.8322 0.9867 0.6964 0.033 Uiso 1 1 calc R . .
H38B H 0.7208 0.8745 0.6397 0.033 Uiso 1 1 calc R . .
C39 C 0.7833(12) 1.1197(11) 0.5653(10) 0.032(3) Uani 1 1 d . . .
H39 H 0.7172 1.1691 0.5992 0.038 Uiso 1 1 calc R . .
C40 C 0.9198(16) 1.1674(16) 0.6294(12) 0.040(4) Uani 1 1 d . . .
H40A H 0.9847 1.1144 0.6004 0.048 Uiso 1 1 calc R . .
H40B H 0.9195 1.1668 0.7019 0.048 Uiso 1 1 calc R . .
C41 C 0.9604(15) 1.2962(13) 0.6288(11) 0.043(3) Uani 1 1 d U . .
H41A H 0.9011 1.3502 0.6656 0.051 Uiso 1 1 calc R . .
H41B H 1.0516 1.3237 0.6679 0.051 Uiso 1 1 calc R . .
C42 C 0.9553(17) 1.3081(17) 0.5215(14) 0.050(5) Uani 1 1 d . . .
H42A H 1.0229 1.2631 0.4874 0.060 Uiso 1 1 calc R . .
H42B H 0.9757 1.3942 0.5264 0.060 Uiso 1 1 calc R . .
C43 C 0.8205(15) 1.2594(13) 0.4567(12) 0.036(3) Uani 1 1 d . . .
H43A H 0.8213 1.2625 0.3849 0.043 Uiso 1 1 calc R . .
H43B H 0.7547 1.3111 0.4861 0.043 Uiso 1 1 calc R . .
C44 C 0.7799(11) 1.1307(11) 0.4536(10) 0.030(3) Uani 1 1 d . . .
H44 H 0.8458 1.0801 0.4209 0.036 Uiso 1 1 calc R . .
C45 C 0.6351(11) 1.0621(10) 0.2791(9) 0.034(2) Uani 1 1 d . . .
H45A H 0.6670 1.1398 0.2694 0.040 Uiso 1 1 calc R . .
H45B H 0.5406 1.0410 0.2466 0.040 Uiso 1 1 calc R . .
C46 C 0.2891(13) 1.0622(13) 0.3553(12) 0.053(4) Uani 1 1 d . . .
C47 C 0.7381(11) 0.6702(10) 0.4464(9) 0.031(2) Uani 1 1 d . . .
C48 C 0.1818(12) 0.2452(11) 1.0053(10) 0.045(3) Uani 1 1 d . . .
C49 C 0.554(2) 0.756(2) 0.8200(15) 0.113(7) Uani 1 1 d DU . .
C50 C 0.3110(18) 0.3176(16) 0.5721(15) 0.082(5) Uani 1 1 d . . .
C51 C 0.3381(15) 1.0023(15) 0.0523(15) 0.074(5) Uani 1 1 d . . .
C52 C 0.5080(14) 0.3709(14) 0.3008(10) 0.056(4) Uani 1 1 d . . .
C53 C 0.820(2) 0.483(3) 0.8784(17) 0.128(8) Uani 1 1 d DU . .
C54 C 0.0344(17) 0.878(2) 0.3840(12) 0.077(6) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O2 2.199(7) . ?
Ho1 O3 2.206(11) . ?
Ho1 O1 2.233(10) . ?
Ho1 N7 2.397(10) . ?
Ho1 N8 2.436(11) . ?
Ho1 N5 2.509(8) . ?
Ho1 N6 2.526(8) . ?
N1 C8 1.504(13) . ?
N1 C9 1.515(13) . ?
N2 C15 1.491(13) . ?
N2 C14 1.501(12) . ?
N3 C23 1.507(13) . ?
N3 C24 1.545(12) . ?
N4 C29 1.468(14) . ?
N4 C30 1.500(15) . ?
N5 C38 1.475(12) . ?
N5 C39 1.507(14) . ?
N6 C44 1.479(15) . ?
N6 C45 1.486(14) . ?
N7 C46 1.118(16) . ?
N8 C47 1.140(14) . ?
N9 C48 1.158(16) . ?
N10 C49 1.118(9) . ?
O1 C1 1.359(13) . ?
O2 C21 1.319(12) . ?
O3 C36 1.363(14) . ?
O4 C50 1.50(2) . ?
O5 C51 1.313(19) . ?
O6 C52 1.406(15) . ?
O7 C53 1.454(10) . ?
O8 C54 1.449(9) . ?
S1 C46 1.658(14) . ?
S2 C47 1.634(11) . ?
S3 C48 1.640(14) . ?
S4 C49 1.597(9) . ?
C1 C2 1.382(14) . ?
C1 C6 1.391(17) . ?
C2 C3 1.410(16) . ?
C2 C45 1.539(15) . ?
C3 C4 1.359(19) . ?
C4 C5 1.371(19) . ?
C4 C7 1.555(17) . ?
C5 C6 1.414(16) . ?
C6 C8 1.523(19) . ?
C9 C10 1.526(14) . ?
C9 C14 1.534(14) . ?
C10 C11 1.536(18) . ?
C11 C12 1.521(18) . ?
C12 C13 1.540(17) . ?
C13 C14 1.531(14) . ?
C15 C16 1.523(18) . ?
C16 C21 1.36(2) . ?
C16 C17 1.384(19) . ?
C17 C18 1.398(18) . ?
C18 C19 1.35(2) . ?
C18 C22 1.522(16) . ?
C19 C20 1.395(19) . ?
C20 C21 1.412(17) . ?
C20 C23 1.519(17) . ?
C24 C29 1.503(15) . ?
C24 C25 1.514(14) . ?
C25 C26 1.515(15) . ?
C26 C27 1.506(17) . ?
C27 C28 1.499(18) . ?
C28 C29 1.545(16) . ?
C30 C31 1.497(15) . ?
C31 C32 1.395(15) . ?
C31 C36 1.431(13) . ?
C32 C33 1.362(14) . ?
C33 C34 1.390(14) . ?
C33 C37 1.518(15) . ?
C34 C35 1.380(14) . ?
C35 C36 1.357(13) . ?
C35 C38 1.520(13) . ?
C39 C40 1.515(18) . ?
C39 C44 1.559(16) . ?
C40 C41 1.53(2) . ?
C41 C42 1.50(2) . ?
C42 C43 1.50(2) . ?
C43 C44 1.512(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ho1 O3 85.1(3) . . ?
O2 Ho1 O1 84.9(3) . . ?
O3 Ho1 O1 170.0(4) . . ?
O2 Ho1 N7 81.1(3) . . ?
O3 Ho1 N7 84.4(4) . . ?
O1 Ho1 N7 94.1(4) . . ?
O2 Ho1 N8 81.6(3) . . ?
O3 Ho1 N8 97.8(4) . . ?
O1 Ho1 N8 80.8(4) . . ?
N7 Ho1 N8 162.3(3) . . ?
O2 Ho1 N5 146.2(3) . . ?
O3 Ho1 N5 76.7(3) . . ?
O1 Ho1 N5 112.0(3) . . ?
N7 Ho1 N5 124.2(3) . . ?
N8 Ho1 N5 73.1(3) . . ?
O2 Ho1 N6 146.4(3) . . ?
O3 Ho1 N6 110.7(3) . . ?
O1 Ho1 N6 78.0(3) . . ?
N7 Ho1 N6 71.7(3) . . ?
N8 Ho1 N6 122.9(3) . . ?
N5 Ho1 N6 67.3(3) . . ?
C8 N1 C9 113.3(8) . . ?
C15 N2 C14 115.6(8) . . ?
C23 N3 C24 114.6(9) . . ?
C29 N4 C30 115.1(9) . . ?
C38 N5 C39 114.5(8) . . ?
C38 N5 Ho1 112.0(6) . . ?
C39 N5 Ho1 114.1(6) . . ?
C44 N6 C45 114.4(8) . . ?
C44 N6 Ho1 117.8(7) . . ?
C45 N6 Ho1 111.6(6) . . ?
C46 N7 Ho1 175.6(12) . . ?
C47 N8 Ho1 156.2(10) . . ?
C1 O1 Ho1 130.5(8) . . ?
C21 O2 Ho1 172.1(7) . . ?
C36 O3 Ho1 137.7(8) . . ?
O1 C1 C2 119.5(9) . . ?
O1 C1 C6 119.9(10) . . ?
C2 C1 C6 120.5(10) . . ?
C1 C2 C3 119.3(11) . . ?
C1 C2 C45 119.7(8) . . ?
C3 C2 C45 121.0(11) . . ?
C4 C3 C2 120.8(13) . . ?
C3 C4 C5 119.8(12) . . ?
C3 C4 C7 120.9(13) . . ?
C5 C4 C7 119.2(13) . . ?
C4 C5 C6 121.2(13) . . ?
C1 C6 C5 118.2(13) . . ?
C1 C6 C8 122.5(11) . . ?
C5 C6 C8 119.2(12) . . ?
N1 C8 C6 109.7(9) . . ?
N1 C9 C10 109.0(9) . . ?
N1 C9 C14 109.1(8) . . ?
C10 C9 C14 111.4(9) . . ?
C9 C10 C11 111.0(11) . . ?
C12 C11 C10 108.8(10) . . ?
C11 C12 C13 111.6(10) . . ?
C14 C13 C12 111.3(10) . . ?
N2 C14 C13 108.0(8) . . ?
N2 C14 C9 111.6(8) . . ?
C13 C14 C9 110.5(8) . . ?
N2 C15 C16 112.1(9) . . ?
C21 C16 C17 121.4(13) . . ?
C21 C16 C15 120.0(13) . . ?
C17 C16 C15 118.5(12) . . ?
C16 C17 C18 121.2(12) . . ?
C19 C18 C17 117.8(12) . . ?
C19 C18 C22 122.8(14) . . ?
C17 C18 C22 119.4(13) . . ?
C18 C19 C20 121.6(14) . . ?
C19 C20 C21 120.6(12) . . ?
C19 C20 C23 120.3(12) . . ?
C21 C20 C23 118.8(11) . . ?
O2 C21 C16 123.2(13) . . ?
O2 C21 C20 119.5(13) . . ?
C16 C21 C20 117.3(11) . . ?
N3 C23 C20 113.6(8) . . ?
C29 C24 C25 111.5(9) . . ?
C29 C24 N3 109.7(9) . . ?
C25 C24 N3 109.0(8) . . ?
C26 C25 C24 112.5(9) . . ?
C27 C26 C25 109.2(10) . . ?
C28 C27 C26 110.9(10) . . ?
C27 C28 C29 111.8(10) . . ?
N4 C29 C24 112.9(10) . . ?
N4 C29 C28 109.2(10) . . ?
C24 C29 C28 109.3(9) . . ?
C31 C30 N4 110.5(9) . . ?
C32 C31 C36 119.3(9) . . ?
C32 C31 C30 121.3(9) . . ?
C36 C31 C30 119.3(10) . . ?
C33 C32 C31 121.2(9) . . ?
C32 C33 C34 117.8(9) . . ?
C32 C33 C37 121.2(9) . . ?
C34 C33 C37 120.8(9) . . ?
C35 C34 C33 122.9(9) . . ?
C36 C35 C34 119.4(9) . . ?
C36 C35 C38 120.6(9) . . ?
C34 C35 C38 119.8(8) . . ?
C35 C36 O3 122.4(9) . . ?
C35 C36 C31 119.2(9) . . ?
O3 C36 C31 118.4(9) . . ?
N5 C38 C35 114.6(7) . . ?
N5 C39 C40 112.6(11) . . ?
N5 C39 C44 107.7(10) . . ?
C40 C39 C44 109.8(10) . . ?
C39 C40 C41 110.4(13) . . ?
C42 C41 C40 113.6(13) . . ?
C41 C42 C43 110.7(13) . . ?
C42 C43 C44 111.7(13) . . ?
N6 C44 C43 114.6(11) . . ?
N6 C44 C39 107.8(9) . . ?
C43 C44 C39 111.4(11) . . ?
N6 C45 C2 112.8(8) . . ?
N7 C46 S1 173.2(14) . . ?
N8 C47 S2 175.1(11) . . ?
N9 C48 S3 178.2(12) . . ?
N10 C49 S4 172(3) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        26.19
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.133
#######################################################################
#
#                 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_R-Er1
_database_code_depnum_ccdc_archive 'CCDC 972391'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H87 Er N10 O8 S4'
_chemical_formula_weight         1299.84
_chemical_absolute_configuration syn
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'
S S 0.1246 0.1234 '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   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.2722(8)
_cell_length_b                   11.6628(9)
_cell_length_c                   13.4833(11)
_cell_angle_alpha                106.8210(10)
_cell_angle_beta                 98.7730(10)
_cell_angle_gamma                94.0620(10)
_cell_volume                     1516.8(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    4444
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.44

_exptl_crystal_description       stick
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             677
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7429
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_process_details   '(sadabs;bruker 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8409
_diffrn_reflns_av_R_equivalents  0.0314
__diffrn_reflns_av_unetI/netI    0.0909
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         26.08
_reflns_number_total             7007
_reflns_number_gt                6827
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.1154P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_number_reflns         7007
_refine_ls_number_parameters     698
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1693
_refine_ls_wR_factor_gt          0.1650
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.051
_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 0.09674(3) 0.75630(3) 0.08798(3) 0.02823(16) Uani 1 1 d . . .
N1 N 0.3997(9) 0.7203(8) -0.1064(8) 0.025(2) Uani 1 1 d . . .
H1A H 0.3428 0.7467 -0.0604 0.030 Uiso 1 1 calc R . .
H1B H 0.4807 0.7190 -0.0670 0.030 Uiso 1 1 calc R . .
N2 N 0.2792(10) 0.9490(8) -0.0658(7) 0.0216(19) Uani 1 1 d . . .
H2A H 0.2563 0.8846 -0.0430 0.026 Uiso 1 1 calc R . .
H2B H 0.2176 0.9444 -0.1245 0.026 Uiso 1 1 calc R . .
N3 N 0.3134(11) 0.9365(9) 0.3788(7) 0.030(2) Uani 1 1 d . . .
H3A H 0.2406 0.9138 0.3253 0.036 Uiso 1 1 calc R . .
H3B H 0.3129 0.8808 0.4151 0.036 Uiso 1 1 calc R . .
N4 N 0.0713(11) 1.0577(10) 0.3630(8) 0.035(2) Uani 1 1 d . . .
H4A H 0.1006 1.0039 0.3088 0.042 Uiso 1 1 calc R . .
H4B H 0.0812 1.1326 0.3534 0.042 Uiso 1 1 calc R . .
N5 N -0.0080(10) 0.5717(10) 0.1226(8) 0.029(2) Uani 1 1 d . . .
H5 H 0.0457 0.5125 0.0984 0.035 Uiso 1 1 calc R . .
N6 N -0.1131(9) 0.6601(8) -0.0384(8) 0.024(2) Uani 1 1 d . . .
H6 H -0.1798 0.7006 -0.0094 0.029 Uiso 1 1 calc R . .
N7 N 0.2711(13) 0.6478(14) 0.1376(12) 0.045(3) Uani 1 1 d . . .
N8 N -0.0259(15) 0.9170(13) 0.0635(11) 0.048(3) Uani 1 1 d . . .
N9 N 0.357(3) 0.380(2) 0.452(2) 0.117(8) Uani 1 1 d U . .
N10 N -0.004(4) 0.181(3) 0.814(3) 0.174(12) Uani 1 1 d DU . .
O1 O 0.1654(11) 0.7087(10) -0.0648(9) 0.029(3) Uani 1 1 d U . .
O2 O 0.2651(9) 0.9027(7) 0.1363(7) 0.0313(19) Uani 1 1 d . . .
O3 O 0.0600(12) 0.8297(11) 0.2442(11) 0.037(3) Uani 1 1 d . . .
O4 O 0.134(2) 0.2660(17) 0.3158(11) 0.086(5) Uani 1 1 d DU . .
O5 O 0.6437(16) 0.781(2) 0.0543(16) 0.107(8) Uani 1 1 d D . .
O6 O 0.3012(15) 0.723(2) 0.4687(11) 0.117(8) Uani 1 1 d D . .
O7 O 0.050(2) 0.9659(17) 0.7779(13) 0.115(6) Uani 1 1 d U . .
O8 O 0.7594(17) 0.2085(17) 0.5980(15) 0.101(5) Uani 1 1 d DU . .
S1 S 0.4880(14) 0.5418(14) 0.1832(12) 0.216(6) Uani 1 1 d U . .
S2 S -0.2298(5) 1.0609(5) 0.0929(4) 0.0734(15) Uani 1 1 d . . .
S3 S 0.5703(7) 0.4638(7) 0.6006(5) 0.096(2) Uani 1 1 d . . .
S4 S 0.1863(9) 0.3594(7) 0.9538(6) 0.109(2) Uani 1 1 d DU . .
C1 C 0.1173(12) 0.6392(10) -0.1628(9) 0.025(2) Uani 1 1 d . . .
C2 C -0.0186(10) 0.6240(9) -0.2052(9) 0.021(2) Uani 1 1 d . . .
C3 C -0.0600(11) 0.5580(11) -0.3113(10) 0.029(3) Uani 1 1 d . . .
H3 H -0.1515 0.5478 -0.3416 0.035 Uiso 1 1 calc R . .
C4 C 0.0303(13) 0.5065(12) -0.3739(9) 0.032(3) Uani 1 1 d . . .
C5 C 0.1628(13) 0.5180(11) -0.3288(10) 0.030(3) Uani 1 1 d . . .
H5A H 0.2244 0.4807 -0.3699 0.036 Uiso 1 1 calc R . .
C6 C 0.2057(12) 0.5841(10) -0.2233(10) 0.024(2) Uani 1 1 d . . .
C7 C -0.0200(17) 0.4407(17) -0.4906(11) 0.054(4) Uani 1 1 d . . .
H7A H 0.0438 0.3866 -0.5180 0.082 Uiso 1 1 calc R . .
H7B H -0.0301 0.4997 -0.5294 0.082 Uiso 1 1 calc R . .
H7C H -0.1060 0.3934 -0.4993 0.082 Uiso 1 1 calc R . .
C8 C 0.3466(16) 0.5920(13) -0.1755(12) 0.032(3) Uani 1 1 d . . .
H8A H 0.3996 0.5669 -0.2319 0.039 Uiso 1 1 calc R . .
H8B H 0.3559 0.5363 -0.1324 0.039 Uiso 1 1 calc R . .
C9 C 0.4155(13) 0.8078(11) -0.1657(10) 0.023(3) Uani 1 1 d . . .
H9 H 0.3408 0.7874 -0.2273 0.028 Uiso 1 1 calc R . .
C10 C 0.5460(12) 0.7959(12) -0.2067(11) 0.035(3) Uani 1 1 d . . .
H10A H 0.6196 0.8091 -0.1464 0.041 Uiso 1 1 calc R . .
H10B H 0.5436 0.7127 -0.2537 0.041 Uiso 1 1 calc R . .
C11 C 0.5738(16) 0.8845(15) -0.2664(12) 0.051(4) Uani 1 1 d . . .
H11A H 0.5063 0.8658 -0.3315 0.061 Uiso 1 1 calc R . .
H11B H 0.6620 0.8765 -0.2869 0.061 Uiso 1 1 calc R . .
C12 C 0.5706(14) 1.0132(13) -0.1985(11) 0.041(3) Uani 1 1 d . . .
H12A H 0.6451 1.0353 -0.1379 0.049 Uiso 1 1 calc R . .
H12B H 0.5818 1.0693 -0.2403 0.049 Uiso 1 1 calc R . .
C13 C 0.4405(13) 1.0259(11) -0.1587(10) 0.030(3) Uani 1 1 d . . .
H13A H 0.3672 1.0122 -0.2194 0.036 Uiso 1 1 calc R . .
H13B H 0.4427 1.1093 -0.1121 0.036 Uiso 1 1 calc R . .
C14 C 0.4125(10) 0.9366(10) -0.0978(9) 0.022(2) Uani 1 1 d . . .
H14 H 0.4823 0.9553 -0.0330 0.026 Uiso 1 1 calc R . .
C15 C 0.2705(12) 1.0645(10) 0.0198(9) 0.028(3) Uani 1 1 d . . .
H15A H 0.2864 1.1339 -0.0070 0.034 Uiso 1 1 calc R . .
H15B H 0.1795 1.0630 0.0356 0.034 Uiso 1 1 calc R . .
C16 C 0.3669(17) 1.0830(14) 0.1191(12) 0.021(3) Uani 1 1 d . . .
C17 C 0.4633(16) 1.1814(15) 0.1559(12) 0.027(3) Uani 1 1 d . . .
H17 H 0.4690 1.2366 0.1165 0.032 Uiso 1 1 calc R . .
C18 C 0.5526(14) 1.2013(13) 0.2500(12) 0.036(3) Uani 1 1 d . . .
C19 C 0.5402(17) 1.1184(14) 0.3036(12) 0.031(4) Uani 1 1 d . . .
H19 H 0.5991 1.1308 0.3684 0.037 Uiso 1 1 calc R . .
C20 C 0.4476(15) 1.0189(15) 0.2683(12) 0.025(3) Uani 1 1 d . . .
C21 C 0.3571(15) 0.9967(12) 0.1729(14) 0.031(3) Uani 1 1 d . . .
C22 C 0.6540(19) 1.3114(17) 0.2906(13) 0.062(5) Uani 1 1 d . . .
H22A H 0.6105 1.3831 0.2891 0.093 Uiso 1 1 calc R . .
H22B H 0.7219 1.3030 0.2461 0.093 Uiso 1 1 calc R . .
H22C H 0.6957 1.3198 0.3632 0.093 Uiso 1 1 calc R . .
C23 C 0.4364(14) 0.9312(13) 0.3303(10) 0.038(3) Uani 1 1 d . . .
H23A H 0.4361 0.8484 0.2832 0.046 Uiso 1 1 calc R . .
H23B H 0.5154 0.9487 0.3870 0.046 Uiso 1 1 calc R . .
C24 C 0.2986(13) 1.0570(11) 0.4522(9) 0.030(3) Uani 1 1 d . . .
H24 H 0.3273 1.1221 0.4228 0.037 Uiso 1 1 calc R . .
C25 C 0.3898(16) 1.0735(14) 0.5605(10) 0.047(4) Uani 1 1 d . . .
H25A H 0.3690 1.0037 0.5855 0.056 Uiso 1 1 calc R . .
H25B H 0.4838 1.0767 0.5518 0.056 Uiso 1 1 calc R . .
C26 C 0.369(2) 1.1903(16) 0.6425(11) 0.067(6) Uani 1 1 d . . .
H26A H 0.4244 1.1965 0.7113 0.080 Uiso 1 1 calc R . .
H26B H 0.3998 1.2604 0.6209 0.080 Uiso 1 1 calc R . .
C27 C 0.2292(18) 1.1952(14) 0.6550(10) 0.055(4) Uani 1 1 d . . .
H27A H 0.2209 1.2722 0.7077 0.065 Uiso 1 1 calc R . .
H27B H 0.1999 1.1283 0.6811 0.065 Uiso 1 1 calc R . .
C28 C 0.1383(16) 1.1846(12) 0.5474(10) 0.042(3) Uani 1 1 d . . .
H28A H 0.1641 1.2534 0.5226 0.050 Uiso 1 1 calc R . .
H28B H 0.0445 1.1859 0.5564 0.050 Uiso 1 1 calc R . .
C29 C 0.1552(12) 1.0623(10) 0.4647(8) 0.027(2) Uani 1 1 d . . .
H29 H 0.1237 0.9929 0.4880 0.032 Uiso 1 1 calc R . .
C30 C -0.0750(15) 1.0205(14) 0.3577(12) 0.049(4) Uani 1 1 d . . .
H30A H -0.1054 1.0742 0.4190 0.058 Uiso 1 1 calc R . .
H30B H -0.1270 1.0298 0.2930 0.058 Uiso 1 1 calc R . .
C31 C -0.0991(18) 0.8956(13) 0.3576(12) 0.036(4) Uani 1 1 d . . .
C32 C -0.1934(14) 0.8651(15) 0.4112(9) 0.044(4) Uani 1 1 d . . .
H32 H -0.2369 0.9265 0.4515 0.052 Uiso 1 1 calc R . .
C33 C -0.2267(16) 0.7428(18) 0.4068(13) 0.052(4) Uani 1 1 d . . .
C34 C -0.1651(17) 0.6599(17) 0.3508(11) 0.045(4) Uani 1 1 d . . .
H34 H -0.1879 0.5785 0.3480 0.054 Uiso 1 1 calc R . .
C35 C -0.0668(12) 0.6841(12) 0.2943(9) 0.031(3) Uani 1 1 d . . .
C36 C -0.0374(10) 0.8020(12) 0.2969(8) 0.026(3) Uani 1 1 d . . .
C37 C -0.330(2) 0.707(3) 0.4661(19) 0.096(9) Uani 1 1 d . . .
H37A H -0.2891 0.6660 0.5145 0.144 Uiso 1 1 calc R . .
H37B H -0.4036 0.6532 0.4157 0.144 Uiso 1 1 calc R . .
H37C H -0.3632 0.7800 0.5062 0.144 Uiso 1 1 calc R . .
C38 C 0.0054(14) 0.5853(12) 0.2386(10) 0.035(3) Uani 1 1 d . . .
H38A H -0.0300 0.5083 0.2474 0.041 Uiso 1 1 calc R . .
H38B H 0.1005 0.6024 0.2714 0.041 Uiso 1 1 calc R . .
C39 C -0.1448(12) 0.5183(13) 0.0600(11) 0.027(3) Uani 1 1 d . . .
H39 H -0.2091 0.5704 0.0937 0.033 Uiso 1 1 calc R . .
C40 C -0.186(3) 0.392(2) 0.0613(18) 0.050(6) Uani 1 1 d . . .
H40A H -0.1177 0.3400 0.0367 0.060 Uiso 1 1 calc R . .
H40B H -0.1890 0.3936 0.1347 0.060 Uiso 1 1 calc R . .
C41 C -0.317(2) 0.3369(19) -0.0053(15) 0.051(5) Uani 1 1 d . . .
H41A H -0.3877 0.3767 0.0282 0.061 Uiso 1 1 calc R . .
H41B H -0.3303 0.2503 -0.0104 0.061 Uiso 1 1 calc R . .
C42 C -0.326(3) 0.3492(18) -0.1142(15) 0.057(6) Uani 1 1 d . . .
H42A H -0.4177 0.3194 -0.1533 0.068 Uiso 1 1 calc R . .
H42B H -0.2658 0.2970 -0.1517 0.068 Uiso 1 1 calc R . .
C43 C -0.291(2) 0.480(2) -0.1161(15) 0.051(6) Uani 1 1 d . . .
H43A H -0.3576 0.5308 -0.0875 0.062 Uiso 1 1 calc R . .
H43B H -0.2911 0.4800 -0.1894 0.062 Uiso 1 1 calc R . .
C44 C -0.1506(14) 0.5299(11) -0.0477(12) 0.032(3) Uani 1 1 d . . .
H44 H -0.0840 0.4814 -0.0818 0.038 Uiso 1 1 calc R . .
C45 C -0.1152(12) 0.6851(11) -0.1425(9) 0.030(3) Uani 1 1 d . . .
H45A H -0.2056 0.6591 -0.1850 0.035 Uiso 1 1 calc R . .
H45B H -0.0962 0.7732 -0.1288 0.035 Uiso 1 1 calc R . .
C46 C 0.355(2) 0.6042(19) 0.1574(17) 0.072(5) Uani 1 1 d U . .
C47 C -0.1081(16) 0.9811(12) 0.0727(11) 0.041(3) Uani 1 1 d . . .
C48 C 0.455(3) 0.417(2) 0.514(2) 0.091(7) Uani 1 1 d U . .
C49 C 0.066(5) 0.265(5) 0.870(4) 0.184(16) Uani 1 1 d DU . .
C50 C 0.121(2) 0.279(2) 0.2110(13) 0.081(6) Uani 1 1 d DU . .
C51 C 0.210(3) 0.768(3) 0.542(2) 0.137(12) Uani 1 1 d DU . .
C52 C -0.001(4) 0.856(3) 0.681(3) 0.131(11) Uani 1 1 d U . .
C53 C 0.828(3) 0.114(2) 0.627(2) 0.117(9) Uani 1 1 d DU . .
C54 C 0.596(3) 0.758(3) 0.144(2) 0.096(10) Uani 1 1 d DU . .


_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 O3 2.135(14) . ?
Er1 O1 2.210(12) . ?
Er1 O2 2.219(8) . ?
Er1 N7 2.388(12) . ?
Er1 N8 2.403(15) . ?
Er1 N6 2.498(9) . ?
Er1 N5 2.533(11) . ?
N1 C9 1.482(16) . ?
N1 C8 1.525(17) . ?
N2 C14 1.501(14) . ?
N2 C15 1.518(13) . ?
N3 C24 1.500(15) . ?
N3 C23 1.505(18) . ?
N4 C29 1.489(15) . ?
N4 C30 1.52(2) . ?
N5 C38 1.511(16) . ?
N5 C39 1.512(16) . ?
N6 C44 1.504(16) . ?
N6 C45 1.512(15) . ?
N7 C46 1.07(2) . ?
N8 C47 1.165(19) . ?
N9 C48 1.17(3) . ?
N10 C49 1.165(19) . ?
O1 C1 1.332(16) . ?
O2 C21 1.318(17) . ?
O3 C36 1.383(15) . ?
O4 C50 1.451(10) . ?
O5 C54 1.459(10) . ?
O6 C51 1.471(10) . ?
O7 C52 1.53(4) . ?
O8 C53 1.459(10) . ?
S1 C46 1.63(2) . ?
S2 C47 1.620(15) . ?
S3 C48 1.48(3) . ?
S4 C49 1.63(2) . ?
C1 C6 1.381(17) . ?
C1 C2 1.403(16) . ?
C2 C3 1.397(16) . ?
C2 C45 1.488(16) . ?
C3 C4 1.399(18) . ?
C4 C5 1.384(18) . ?
C4 C7 1.526(17) . ?
C5 C6 1.393(17) . ?
C6 C8 1.476(18) . ?
C9 C14 1.522(17) . ?
C9 C10 1.527(18) . ?
C10 C11 1.52(2) . ?
C11 C12 1.52(2) . ?
C12 C13 1.516(18) . ?
C13 C14 1.539(16) . ?
C15 C16 1.49(2) . ?
C16 C17 1.38(2) . ?
C16 C21 1.41(2) . ?
C17 C18 1.40(2) . ?
C18 C19 1.37(2) . ?
C18 C22 1.50(2) . ?
C19 C20 1.36(2) . ?
C20 C21 1.41(2) . ?
C20 C23 1.51(2) . ?
C24 C29 1.512(18) . ?
C24 C25 1.562(17) . ?
C25 C26 1.54(2) . ?
C26 C27 1.48(3) . ?
C27 C28 1.57(2) . ?
C28 C29 1.575(16) . ?
C30 C31 1.46(2) . ?
C31 C32 1.38(2) . ?
C31 C36 1.42(2) . ?
C32 C33 1.43(2) . ?
C33 C34 1.31(3) . ?
C33 C37 1.52(2) . ?
C34 C35 1.41(2) . ?
C35 C36 1.375(18) . ?
C35 C38 1.494(19) . ?
C39 C44 1.49(2) . ?
C39 C40 1.51(2) . ?
C40 C41 1.48(3) . ?
C41 C42 1.51(3) . ?
C42 C43 1.55(3) . ?
C43 C44 1.56(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Er1 O1 169.2(4) . . ?
O3 Er1 O2 85.1(4) . . ?
O1 Er1 O2 84.1(4) . . ?
O3 Er1 N7 94.8(5) . . ?
O1 Er1 N7 83.9(5) . . ?
O2 Er1 N7 80.6(4) . . ?
O3 Er1 N8 80.6(5) . . ?
O1 Er1 N8 97.4(5) . . ?
O2 Er1 N8 81.9(4) . . ?
N7 Er1 N8 162.2(4) . . ?
O3 Er1 N6 111.3(4) . . ?
O1 Er1 N6 78.0(4) . . ?
O2 Er1 N6 146.8(3) . . ?
N7 Er1 N6 124.2(4) . . ?
N8 Er1 N6 73.1(4) . . ?
O3 Er1 N5 78.0(4) . . ?
O1 Er1 N5 111.5(4) . . ?
O2 Er1 N5 146.3(3) . . ?
N7 Er1 N5 72.1(4) . . ?
N8 Er1 N5 122.9(4) . . ?
N6 Er1 N5 66.8(3) . . ?
C9 N1 C8 114.2(10) . . ?
C14 N2 C15 115.4(9) . . ?
C24 N3 C23 115.6(10) . . ?
C29 N4 C30 113.1(11) . . ?
C38 N5 C39 113.6(10) . . ?
C38 N5 Er1 112.7(7) . . ?
C39 N5 Er1 116.7(8) . . ?
C44 N6 C45 114.5(10) . . ?
C44 N6 Er1 114.4(7) . . ?
C45 N6 Er1 111.3(7) . . ?
C46 N7 Er1 174.7(18) . . ?
C47 N8 Er1 157.7(14) . . ?
C1 O1 Er1 136.5(9) . . ?
C21 O2 Er1 173.4(8) . . ?
C36 O3 Er1 133.5(9) . . ?
O1 C1 C6 118.0(11) . . ?
O1 C1 C2 121.5(11) . . ?
C6 C1 C2 120.5(10) . . ?
C3 C2 C1 118.1(10) . . ?
C3 C2 C45 120.2(10) . . ?
C1 C2 C45 121.4(10) . . ?
C2 C3 C4 121.4(10) . . ?
C5 C4 C3 119.2(11) . . ?
C5 C4 C7 121.8(12) . . ?
C3 C4 C7 119.0(12) . . ?
C4 C5 C6 120.0(11) . . ?
C1 C6 C5 120.6(11) . . ?
C1 C6 C8 120.1(11) . . ?
C5 C6 C8 119.3(11) . . ?
C6 C8 N1 111.0(11) . . ?
N1 C9 C14 111.6(10) . . ?
N1 C9 C10 108.9(11) . . ?
C14 C9 C10 110.4(10) . . ?
C11 C10 C9 113.1(12) . . ?
C10 C11 C12 110.5(11) . . ?
C13 C12 C11 110.8(11) . . ?
C12 C13 C14 112.5(11) . . ?
N2 C14 C9 109.6(9) . . ?
N2 C14 C13 109.8(9) . . ?
C9 C14 C13 110.3(9) . . ?
C16 C15 N2 113.6(10) . . ?
C17 C16 C21 121.5(15) . . ?
C17 C16 C15 120.5(13) . . ?
C21 C16 C15 118.0(14) . . ?
C16 C17 C18 121.2(15) . . ?
C19 C18 C17 117.0(14) . . ?
C19 C18 C22 122.6(16) . . ?
C17 C18 C22 120.4(16) . . ?
C20 C19 C18 123.2(15) . . ?
C19 C20 C21 120.6(15) . . ?
C19 C20 C23 121.4(14) . . ?
C21 C20 C23 117.9(14) . . ?
O2 C21 C16 120.8(15) . . ?
O2 C21 C20 122.8(14) . . ?
C16 C21 C20 116.4(15) . . ?
N3 C23 C20 113.1(11) . . ?
N3 C24 C29 109.7(9) . . ?
N3 C24 C25 108.1(11) . . ?
C29 C24 C25 110.7(10) . . ?
C26 C25 C24 110.6(13) . . ?
C27 C26 C25 112.5(13) . . ?
C26 C27 C28 110.7(12) . . ?
C27 C28 C29 108.4(12) . . ?
N4 C29 C24 110.1(10) . . ?
N4 C29 C28 106.8(10) . . ?
C24 C29 C28 110.9(10) . . ?
C31 C30 N4 111.4(13) . . ?
C32 C31 C36 118.3(14) . . ?
C32 C31 C30 119.2(15) . . ?
C36 C31 C30 122.3(15) . . ?
C31 C32 C33 120.9(14) . . ?
C34 C33 C32 118.3(14) . . ?
C34 C33 C37 119.9(19) . . ?
C32 C33 C37 121.8(19) . . ?
C33 C34 C35 124.0(16) . . ?
C36 C35 C34 117.3(13) . . ?
C36 C35 C38 122.1(12) . . ?
C34 C35 C38 120.5(14) . . ?
C35 C36 O3 119.1(12) . . ?
C35 C36 C31 121.1(12) . . ?
O3 C36 C31 119.7(13) . . ?
C35 C38 N5 112.3(10) . . ?
C44 C39 C40 114.0(13) . . ?
C44 C39 N5 107.7(11) . . ?
C40 C39 N5 113.9(14) . . ?
C41 C40 C39 113.8(19) . . ?
C40 C41 C42 111.5(18) . . ?
C41 C42 C43 114.2(15) . . ?
C42 C43 C44 108.7(16) . . ?
C39 C44 N6 108.8(11) . . ?
C39 C44 C43 110.6(14) . . ?
N6 C44 C43 112.1(13) . . ?
C2 C45 N6 114.4(9) . . ?
N7 C46 S1 177(3) . . ?
N8 C47 S2 173.4(16) . . ?
N9 C48 S3 174(3) . . ?
N10 C49 S4 166(6) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        26.08
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.675
_refine_diff_density_min         -1.639
_refine_diff_density_rms         0.209
#######################################################################
#
#                 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_S-Er1
_database_code_depnum_ccdc_archive 'CCDC 972392'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C53 H85 Er N10 O8 S4'
_chemical_formula_weight         1285.81
_chemical_absolute_configuration syn
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'
S S 0.1246 0.1234 '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   p1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'

_cell_length_a                   10.2345(6)
_cell_length_b                   11.6666(7)
_cell_length_c                   13.5492(8)
_cell_angle_alpha                107.0270(10)
_cell_angle_beta                 98.8810(10)
_cell_angle_gamma                94.1180(10)
_cell_volume                     1516.57(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    3844
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.74

_exptl_crystal_description       stick
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             669
_exptl_absorpt_coefficient_mu    1.579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7642
_exptl_absorpt_correction_T_max  0.8841
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      185(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8472
_diffrn_reflns_av_R_equivalents  0.0336
__diffrn_reflns_av_unetI/netI    0.1005
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         26.07
_reflns_number_total             7034
_reflns_number_gt                6770
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0687P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.028(18)
_refine_ls_number_reflns         7034
_refine_ls_number_parameters     689
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0577
_refine_ls_wR_factor_ref         0.1344
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.90336(3) 0.24373(3) 0.91208(3) 0.02604(13) Uani 1 1 d . . .
N1 N 0.5984(8) 0.2831(7) 1.1023(7) 0.0262(19) Uani 1 1 d . . .
H1A H 0.6558 0.2558 1.0571 0.031 Uiso 1 1 calc R . .
H1B H 0.5175 0.2847 1.0624 0.031 Uiso 1 1 calc R . .
N2 N 0.7231(9) 0.0525(7) 1.0678(6) 0.0232(18) Uani 1 1 d . . .
H2A H 0.7486 0.1165 1.0454 0.028 Uiso 1 1 calc R . .
H2B H 0.7823 0.0576 1.1278 0.028 Uiso 1 1 calc R . .
N3 N 0.6814(10) 0.0678(8) 0.6250(8) 0.035(2) Uani 1 1 d . . .
H3A H 0.7564 0.0883 0.6767 0.041 Uiso 1 1 calc R . .
H3B H 0.6800 0.1257 0.5912 0.041 Uiso 1 1 calc R . .
N4 N 0.9231(10) -0.0552(8) 0.6320(8) 0.040(2) Uani 1 1 d . . .
H4A H 0.9122 -0.1295 0.6424 0.047 Uiso 1 1 calc R . .
H4B H 0.8972 0.0002 0.6869 0.047 Uiso 1 1 calc R . .
N5 N 1.0034(8) 0.4266(8) 0.8776(8) 0.028(2) Uani 1 1 d . . .
H5 H 0.9493 0.4853 0.9020 0.033 Uiso 1 1 calc R . .
N6 N 1.1124(8) 0.3433(7) 1.0392(7) 0.0250(19) Uani 1 1 d . . .
H6 H 1.1798 0.3039 1.0103 0.030 Uiso 1 1 calc R . .
N7 N 0.7225(10) 0.3488(11) 0.8656(10) 0.041(3) Uani 1 1 d . . .
N8 N 1.0313(10) 0.0879(9) 0.9355(9) 0.038(3) Uani 1 1 d . . .
N9 N 0.639(3) 0.549(3) 0.542(2) 0.185(9) Uani 1 1 d DU . .
N10 N 0.9933(19) 0.8224(16) 0.1789(18) 0.122(8) Uani 1 1 d D . .
O1 O 0.8362(9) 0.2898(9) 1.0626(8) 0.026(2) Uani 1 1 d U . .
O2 O 0.7352(8) 0.0989(6) 0.8659(6) 0.0347(18) Uani 1 1 d . . .
O3 O 0.9341(10) 0.1673(9) 0.7486(9) 0.034(3) Uani 1 1 d . . .
O4 O 0.8451(17) 0.7434(15) 0.6809(10) 0.085(5) Uani 1 1 d DU . .
O5 O 0.3691(10) 0.2361(11) 0.9450(8) 0.065(3) Uani 1 1 d . . .
O6 O 0.6849(13) 0.2645(13) 0.5372(11) 0.093(4) Uani 1 1 d . . .
O7 O 0.9143(13) 0.0446(10) 0.2338(10) 0.095(5) Uani 1 1 d . . .
O8 O 0.2321(16) 0.7793(14) 0.3925(15) 0.130(6) Uani 1 1 d DU . .
S1 S 0.4760(7) 0.4195(8) 0.8196(6) 0.130(2) Uani 1 1 d U . .
S2 S 1.2367(4) -0.0545(4) 0.8966(4) 0.0722(13) Uani 1 1 d . . .
S3 S 0.4374(5) 0.5306(4) 0.3971(4) 0.0814(14) Uani 1 1 d DU . .
S4 S 0.8131(5) 0.6390(4) 0.0435(4) 0.0779(13) Uani 1 1 d . . .
C1 C 0.8819(11) 0.3639(8) 1.1626(9) 0.027(2) Uani 1 1 d . . .
C2 C 1.0196(11) 0.3796(9) 1.2061(9) 0.028(2) Uani 1 1 d . . .
C3 C 1.0589(11) 0.4479(9) 1.3103(9) 0.031(3) Uani 1 1 d . . .
H3 H 1.1511 0.4608 1.3400 0.037 Uiso 1 1 calc R . .
C4 C 0.9714(11) 0.4981(9) 1.3733(8) 0.030(2) Uani 1 1 d . . .
C5 C 0.8357(11) 0.4844(9) 1.3268(8) 0.028(2) Uani 1 1 d . . .
H5A H 0.7730 0.5198 1.3677 0.033 Uiso 1 1 calc R . .
C6 C 0.7939(11) 0.4194(9) 1.2216(9) 0.025(2) Uani 1 1 d . . .
C7 C 1.0170(15) 0.5619(12) 1.4894(10) 0.050(3) Uani 1 1 d . . .
H7A H 0.9437 0.5531 1.5266 0.075 Uiso 1 1 calc R . .
H7B H 1.0437 0.6478 1.5008 0.075 Uiso 1 1 calc R . .
H7C H 1.0929 0.5260 1.5163 0.075 Uiso 1 1 calc R . .
C8 C 0.6515(11) 0.4086(10) 1.1701(10) 0.027(3) Uani 1 1 d . . .
H8A H 0.5967 0.4343 1.2250 0.033 Uiso 1 1 calc R . .
H8B H 0.6434 0.4639 1.1269 0.033 Uiso 1 1 calc R . .
C9 C 0.5802(12) 0.1951(9) 1.1635(9) 0.025(2) Uani 1 1 d . . .
H9 H 0.6535 0.2164 1.2262 0.030 Uiso 1 1 calc R . .
C10 C 0.4480(11) 0.2071(10) 1.2000(10) 0.036(3) Uani 1 1 d . . .
H10A H 0.3759 0.1930 1.1384 0.043 Uiso 1 1 calc R . .
H10B H 0.4491 0.2903 1.2466 0.043 Uiso 1 1 calc R . .
C11 C 0.4188(15) 0.1169(12) 1.2593(11) 0.049(4) Uani 1 1 d . . .
H11A H 0.4865 0.1351 1.3243 0.059 Uiso 1 1 calc R . .
H11B H 0.3303 0.1252 1.2796 0.059 Uiso 1 1 calc R . .
C12 C 0.4212(13) -0.0109(12) 1.1913(11) 0.048(3) Uani 1 1 d . . .
H12A H 0.3464 -0.0324 1.1307 0.058 Uiso 1 1 calc R . .
H12B H 0.4091 -0.0672 1.2324 0.058 Uiso 1 1 calc R . .
C13 C 0.5536(11) -0.0247(10) 1.1512(9) 0.032(2) Uani 1 1 d . . .
H13A H 0.6266 -0.0145 1.2115 0.038 Uiso 1 1 calc R . .
H13B H 0.5492 -0.1074 1.1026 0.038 Uiso 1 1 calc R . .
C14 C 0.5854(9) 0.0655(8) 1.0953(8) 0.021(2) Uani 1 1 d . . .
H14 H 0.5185 0.0474 1.0289 0.026 Uiso 1 1 calc R . .
C15 C 0.7341(10) -0.0640(9) 0.9839(9) 0.028(2) Uani 1 1 d . . .
H15A H 0.8253 -0.0616 0.9680 0.034 Uiso 1 1 calc R . .
H15B H 0.7193 -0.1329 1.0111 0.034 Uiso 1 1 calc R . .
C16 C 0.6354(14) -0.0832(11) 0.8851(11) 0.025(3) Uani 1 1 d . . .
C17 C 0.5442(12) -0.1825(12) 0.8468(11) 0.029(3) Uani 1 1 d . . .
H17 H 0.5402 -0.2381 0.8856 0.035 Uiso 1 1 calc R . .
C18 C 0.4571(13) -0.2055(11) 0.7535(12) 0.035(3) Uani 1 1 d . . .
C19 C 0.4626(18) -0.1169(15) 0.6982(12) 0.042(4) Uani 1 1 d . . .
H19 H 0.4012 -0.1285 0.6349 0.050 Uiso 1 1 calc R . .
C20 C 0.5547(14) -0.0172(12) 0.7360(12) 0.027(3) Uani 1 1 d . . .
C21 C 0.6459(12) 0.0038(10) 0.8273(13) 0.028(3) Uani 1 1 d . . .
C22 C 0.3536(15) -0.3220(11) 0.7061(11) 0.054(4) Uani 1 1 d . . .
H22A H 0.3904 -0.3891 0.7259 0.082 Uiso 1 1 calc R . .
H22B H 0.3347 -0.3424 0.6294 0.082 Uiso 1 1 calc R . .
H22C H 0.2710 -0.3073 0.7334 0.082 Uiso 1 1 calc R . .
C23 C 0.5613(12) 0.0692(10) 0.6753(10) 0.037(3) Uani 1 1 d . . .
H23A H 0.5606 0.1517 0.7228 0.044 Uiso 1 1 calc R . .
H23B H 0.4805 0.0503 0.6200 0.044 Uiso 1 1 calc R . .
C24 C 0.6908(11) -0.0515(9) 0.5478(8) 0.030(2) Uani 1 1 d . . .
H24 H 0.6621 -0.1173 0.5762 0.036 Uiso 1 1 calc R . .
C25 C 0.5984(14) -0.0655(12) 0.4449(10) 0.050(3) Uani 1 1 d . . .
H25A H 0.6202 0.0044 0.4204 0.060 Uiso 1 1 calc R . .
H25B H 0.5053 -0.0654 0.4567 0.060 Uiso 1 1 calc R . .
C26 C 0.6096(17) -0.1821(12) 0.3599(11) 0.060(4) Uani 1 1 d . . .
H26A H 0.5523 -0.1850 0.2930 0.072 Uiso 1 1 calc R . .
H26B H 0.5779 -0.2525 0.3804 0.072 Uiso 1 1 calc R . .
C27 C 0.7542(18) -0.1889(12) 0.3442(10) 0.061(4) Uani 1 1 d . . .
H27A H 0.7604 -0.2664 0.2912 0.073 Uiso 1 1 calc R . .
H27B H 0.7835 -0.1224 0.3179 0.073 Uiso 1 1 calc R . .
C28 C 0.8438(14) -0.1792(11) 0.4464(9) 0.043(3) Uani 1 1 d . . .
H28A H 0.9371 -0.1821 0.4355 0.052 Uiso 1 1 calc R . .
H28B H 0.8179 -0.2487 0.4702 0.052 Uiso 1 1 calc R . .
C29 C 0.8343(13) -0.0600(10) 0.5321(8) 0.036(3) Uani 1 1 d . . .
H29 H 0.8653 0.0097 0.5091 0.043 Uiso 1 1 calc R . .
C30 C 1.0695(13) -0.0216(12) 0.6338(11) 0.052(4) Uani 1 1 d . . .
H30A H 1.1240 -0.0335 0.6962 0.062 Uiso 1 1 calc R . .
H30B H 1.0962 -0.0743 0.5703 0.062 Uiso 1 1 calc R . .
C31 C 1.0927(16) 0.1045(13) 0.6370(11) 0.042(3) Uani 1 1 d . . .
C32 C 1.1876(12) 0.1410(15) 0.5841(10) 0.054(4) Uani 1 1 d . . .
H32 H 1.2314 0.0812 0.5421 0.065 Uiso 1 1 calc R . .
C33 C 1.2199(13) 0.2604(15) 0.5906(12) 0.051(4) Uani 1 1 d . . .
C34 C 1.1559(14) 0.3460(12) 0.6501(10) 0.043(3) Uani 1 1 d . . .
H34 H 1.1764 0.4281 0.6539 0.051 Uiso 1 1 calc R . .
C35 C 1.0622(11) 0.3171(11) 0.7048(9) 0.034(3) Uani 1 1 d . . .
C36 C 1.0292(11) 0.1967(10) 0.7001(9) 0.032(3) Uani 1 1 d . . .
C37 C 1.3227(17) 0.2932(18) 0.5299(14) 0.079(5) Uani 1 1 d . . .
H37A H 1.2772 0.3113 0.4681 0.119 Uiso 1 1 calc R . .
H37B H 1.3735 0.2251 0.5074 0.119 Uiso 1 1 calc R . .
H37C H 1.3835 0.3642 0.5751 0.119 Uiso 1 1 calc R . .
C38 C 0.9875(13) 0.4111(11) 0.7619(10) 0.040(3) Uani 1 1 d . . .
H38A H 0.8917 0.3901 0.7301 0.047 Uiso 1 1 calc R . .
H38B H 1.0179 0.4892 0.7526 0.047 Uiso 1 1 calc R . .
C39 C 1.1404(12) 0.4805(12) 0.9391(10) 0.028(3) Uani 1 1 d . . .
H39 H 1.2058 0.4297 0.9054 0.033 Uiso 1 1 calc R . .
C40 C 1.1761(19) 0.6105(14) 0.9366(15) 0.043(5) Uani 1 1 d U . .
H40A H 1.1749 0.6090 0.8630 0.052 Uiso 1 1 calc R . .
H40B H 1.1078 0.6609 0.9637 0.052 Uiso 1 1 calc R . .
C41 C 1.3127(18) 0.6671(16) 1.0021(13) 0.052(5) Uani 1 1 d . . .
H41A H 1.3254 0.7542 1.0088 0.062 Uiso 1 1 calc R . .
H41B H 1.3830 0.6282 0.9666 0.062 Uiso 1 1 calc R . .
C42 C 1.3249(18) 0.6514(15) 1.1115(14) 0.052(5) Uani 1 1 d . . .
H42A H 1.4183 0.6777 1.1485 0.063 Uiso 1 1 calc R . .
H42B H 1.2683 0.7056 1.1516 0.063 Uiso 1 1 calc R . .
C43 C 1.2860(18) 0.5248(15) 1.1126(13) 0.041(4) Uani 1 1 d U . .
H43A H 1.2877 0.5256 1.1861 0.049 Uiso 1 1 calc R . .
H43B H 1.3523 0.4727 1.0844 0.049 Uiso 1 1 calc R . .
C44 C 1.1480(13) 0.4712(10) 1.0483(10) 0.030(3) Uani 1 1 d . . .
H44 H 1.0807 0.5192 1.0820 0.037 Uiso 1 1 calc R . .
C45 C 1.1160(10) 0.3174(10) 1.1406(8) 0.026(2) Uani 1 1 d . . .
H45A H 1.2075 0.3423 1.1822 0.032 Uiso 1 1 calc R . .
H45B H 1.0961 0.2291 1.1259 0.032 Uiso 1 1 calc R . .
C46 C 0.6282(15) 0.3852(13) 0.8481(13) 0.061(4) Uani 1 1 d . . .
C47 C 1.1129(12) 0.0253(10) 0.9221(10) 0.036(3) Uani 1 1 d . . .
C48 C 0.5664(18) 0.583(2) 0.4905(16) 0.109(6) Uani 1 1 d DU . .
C49 C 0.9148(18) 0.7472(17) 0.1302(19) 0.068(6) Uani 1 1 d D . .
C50 C 1.0073(19) 0.1312(17) 0.3083(16) 0.078(5) Uani 1 1 d U . .
C51 C 0.776(3) 0.259(2) 0.473(2) 0.106(7) Uani 1 1 d U . .
C52 C 0.8845(19) 0.7265(16) 0.7834(11) 0.074(5) Uani 1 1 d D . .
C53 C 0.174(2) 0.8827(12) 0.3762(14) 0.079(6) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.182(11) . ?
Er1 O2 2.200(7) . ?
Er1 O3 2.213(11) . ?
Er1 N8 2.382(11) . ?
Er1 N7 2.396(11) . ?
Er1 N6 2.496(8) . ?
Er1 N5 2.497(8) . ?
N1 C8 1.492(13) . ?
N1 C9 1.515(13) . ?
N2 C15 1.519(12) . ?
N2 C14 1.519(12) . ?
N3 C23 1.493(15) . ?
N3 C24 1.496(14) . ?
N4 C29 1.493(14) . ?
N4 C30 1.516(16) . ?
N5 C39 1.503(14) . ?
N5 C38 1.506(15) . ?
N6 C44 1.474(14) . ?
N6 C45 1.487(14) . ?
N7 C46 1.103(17) . ?
N8 C47 1.149(14) . ?
N9 C48 1.120(10) . ?
N10 C49 1.117(10) . ?
O1 C1 1.365(13) . ?
O2 C21 1.307(14) . ?
O3 C36 1.334(15) . ?
O4 C52 1.459(10) . ?
O6 C51 1.36(3) . ?
O7 C50 1.38(2) . ?
O8 C53 1.442(10) . ?
S1 C46 1.652(15) . ?
S2 C47 1.646(12) . ?
S3 C48 1.623(10) . ?
S4 C49 1.619(18) . ?
C1 C6 1.368(15) . ?
C1 C2 1.418(15) . ?
C2 C3 1.382(15) . ?
C2 C45 1.511(15) . ?
C3 C4 1.375(16) . ?
C4 C5 1.411(15) . ?
C4 C7 1.512(16) . ?
C5 C6 1.387(15) . ?
C6 C8 1.495(14) . ?
C9 C10 1.513(16) . ?
C9 C14 1.533(14) . ?
C10 C11 1.538(19) . ?
C11 C12 1.511(19) . ?
C12 C13 1.537(16) . ?
C13 C14 1.511(15) . ?
C15 C16 1.495(18) . ?
C16 C17 1.351(18) . ?
C16 C21 1.46(2) . ?
C17 C18 1.372(18) . ?
C18 C19 1.44(2) . ?
C18 C22 1.566(17) . ?
C19 C20 1.36(2) . ?
C20 C21 1.38(2) . ?
C20 C23 1.480(19) . ?
C24 C25 1.517(16) . ?
C24 C29 1.522(17) . ?
C25 C26 1.528(19) . ?
C26 C27 1.53(2) . ?
C27 C28 1.508(19) . ?
C28 C29 1.549(15) . ?
C30 C31 1.46(2) . ?
C31 C32 1.40(2) . ?
C31 C36 1.430(18) . ?
C32 C33 1.38(2) . ?
C33 C34 1.36(2) . ?
C33 C37 1.52(2) . ?
C34 C35 1.379(17) . ?
C35 C36 1.402(16) . ?
C35 C38 1.481(18) . ?
C39 C44 1.505(17) . ?
C39 C40 1.546(19) . ?
C40 C41 1.52(2) . ?
C41 C42 1.53(2) . ?
C42 C43 1.51(2) . ?
C43 C44 1.523(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Er1 O2 83.3(3) . . ?
O1 Er1 O3 167.8(3) . . ?
O2 Er1 O3 84.5(3) . . ?
O1 Er1 N8 97.9(4) . . ?
O2 Er1 N8 83.5(3) . . ?
O3 Er1 N8 81.3(4) . . ?
O1 Er1 N7 82.7(4) . . ?
O2 Er1 N7 79.1(3) . . ?
O3 Er1 N7 94.3(4) . . ?
N8 Er1 N7 162.4(3) . . ?
O1 Er1 N6 77.4(3) . . ?
O2 Er1 N6 146.7(3) . . ?
O3 Er1 N6 113.7(3) . . ?
N8 Er1 N6 72.8(3) . . ?
N7 Er1 N6 124.2(3) . . ?
O1 Er1 N5 111.7(3) . . ?
O2 Er1 N5 146.0(3) . . ?
O3 Er1 N5 78.5(3) . . ?
N8 Er1 N5 122.0(3) . . ?
N7 Er1 N5 73.2(3) . . ?
N6 Er1 N5 67.2(3) . . ?
C8 N1 C9 113.6(9) . . ?
C15 N2 C14 115.2(8) . . ?
C23 N3 C24 113.8(8) . . ?
C29 N4 C30 113.8(10) . . ?
C39 N5 C38 114.2(9) . . ?
C39 N5 Er1 116.3(7) . . ?
C38 N5 Er1 112.0(6) . . ?
C44 N6 C45 115.2(9) . . ?
C44 N6 Er1 114.6(7) . . ?
C45 N6 Er1 111.5(6) . . ?
C46 N7 Er1 169.7(13) . . ?
C47 N8 Er1 156.4(11) . . ?
C1 O1 Er1 137.6(7) . . ?
C21 O2 Er1 170.9(8) . . ?
C36 O3 Er1 130.7(8) . . ?
O1 C1 C6 119.8(10) . . ?
O1 C1 C2 119.8(10) . . ?
C6 C1 C2 120.3(10) . . ?
C3 C2 C1 117.4(11) . . ?
C3 C2 C45 122.5(10) . . ?
C1 C2 C45 120.0(10) . . ?
C4 C3 C2 123.4(10) . . ?
C3 C4 C5 117.8(10) . . ?
C3 C4 C7 121.6(11) . . ?
C5 C4 C7 120.5(11) . . ?
C6 C5 C4 120.0(10) . . ?
C1 C6 C5 120.8(10) . . ?
C1 C6 C8 118.6(11) . . ?
C5 C6 C8 120.6(10) . . ?
N1 C8 C6 112.7(9) . . ?
C10 C9 N1 108.4(10) . . ?
C10 C9 C14 110.9(8) . . ?
N1 C9 C14 110.6(9) . . ?
C9 C10 C11 111.9(11) . . ?
C12 C11 C10 110.5(11) . . ?
C11 C12 C13 111.0(10) . . ?
C14 C13 C12 112.9(9) . . ?
C13 C14 N2 108.9(8) . . ?
C13 C14 C9 111.3(9) . . ?
N2 C14 C9 110.1(8) . . ?
C16 C15 N2 112.1(9) . . ?
C17 C16 C21 120.7(13) . . ?
C17 C16 C15 120.9(13) . . ?
C21 C16 C15 118.3(12) . . ?
C16 C17 C18 122.1(14) . . ?
C17 C18 C19 117.6(13) . . ?
C17 C18 C22 122.8(13) . . ?
C19 C18 C22 119.6(14) . . ?
C20 C19 C18 120.6(15) . . ?
C19 C20 C21 122.0(14) . . ?
C19 C20 C23 119.3(14) . . ?
C21 C20 C23 118.7(12) . . ?
O2 C21 C20 123.5(13) . . ?
O2 C21 C16 119.6(13) . . ?
C20 C21 C16 116.9(11) . . ?
C20 C23 N3 114.0(10) . . ?
N3 C24 C25 109.3(10) . . ?
N3 C24 C29 109.8(8) . . ?
C25 C24 C29 111.1(10) . . ?
C24 C25 C26 112.2(12) . . ?
C25 C26 C27 110.6(11) . . ?
C28 C27 C26 110.3(11) . . ?
C27 C28 C29 111.1(11) . . ?
N4 C29 C24 110.8(9) . . ?
N4 C29 C28 109.1(10) . . ?
C24 C29 C28 110.4(9) . . ?
C31 C30 N4 109.6(11) . . ?
C32 C31 C36 117.3(14) . . ?
C32 C31 C30 120.5(14) . . ?
C36 C31 C30 122.0(13) . . ?
C33 C32 C31 122.7(13) . . ?
C34 C33 C32 118.5(12) . . ?
C34 C33 C37 121.7(15) . . ?
C32 C33 C37 119.8(15) . . ?
C33 C34 C35 122.0(13) . . ?
C34 C35 C36 120.3(12) . . ?
C34 C35 C38 120.4(12) . . ?
C36 C35 C38 119.1(11) . . ?
O3 C36 C35 120.6(11) . . ?
O3 C36 C31 120.2(12) . . ?
C35 C36 C31 119.1(12) . . ?
C35 C38 N5 113.9(9) . . ?
N5 C39 C44 108.1(10) . . ?
N5 C39 C40 111.8(12) . . ?
C44 C39 C40 113.6(12) . . ?
C41 C40 C39 112.0(14) . . ?
C40 C41 C42 110.1(14) . . ?
C43 C42 C41 115.2(14) . . ?
C42 C43 C44 112.5(14) . . ?
N6 C44 C39 107.9(10) . . ?
N6 C44 C43 113.8(11) . . ?
C39 C44 C43 109.5(12) . . ?
N6 C45 C2 114.4(8) . . ?
N7 C46 S1 171.5(16) . . ?
N8 C47 S2 173.8(13) . . ?
N9 C48 S3 138(3) . . ?
N10 C49 S4 171(3) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.07
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.579
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.142
