# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_importks22-4
_database_code_depnum_ccdc_archive 'CCDC 1407103'
_audit_update_record             
;
2015-06-16 deposited with the CCDC.
2015-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H19 Dy F18 N2 O10 S6'
_chemical_formula_weight         1324.4

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'
F F 0.0171 0.0103 '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   P-1

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

_cell_length_a                   12.4879(3)
_cell_length_b                   13.3816(4)
_cell_length_c                   15.6598(6)
_cell_angle_alpha                100.987(2)
_cell_angle_beta                 90.592(2)
_cell_angle_gamma                107.459(2)
_cell_volume                     2444.19(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10209
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.103

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1334
_exptl_absorpt_coefficient_mu    1.912
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18277
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         27.09
_reflns_number_total             10729
_reflns_number_gt                7750
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0844P)²+0.1841P] 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_number_reflns         10729
_refine_ls_number_parameters     689
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1478
_refine_ls_wR_factor_gt          0.1229
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5321(9) 1.2843(9) 0.7010(9) 0.131(4) Uani 1 1 d . . .
H1A H 0.5251 1.3489 0.7375 0.157 Uiso 1 1 calc R . .
H1B H 0.4772 1.2238 0.7175 0.157 Uiso 1 1 calc R . .
C2 C 0.5062(7) 1.2849(7) 0.6105(9) 0.131(4) Uani 1 1 d . . .
H2A H 0.4289 1.2848 0.6038 0.157 Uiso 1 1 calc R . .
H2B H 0.5541 1.3509 0.5968 0.157 Uiso 1 1 calc R . .
C3 C 0.6085(5) 1.1682(5) 0.5765(6) 0.078(2) Uani 1 1 d . . .
C4 C 0.6645(6) 1.2066(5) 0.6517(6) 0.0784(19) Uani 1 1 d . . .
C5 C 0.7542(5) 1.0710(4) 0.5744(4) 0.0638(15) Uani 1 1 d . . .
C6 C 0.8126(5) 1.0002(4) 0.5573(4) 0.0626(15) Uani 1 1 d . . .
C7 C 0.9470(5) 0.8873(4) 0.5716(4) 0.0586(13) Uani 1 1 d . . .
C8 C 0.8870(5) 0.8414(4) 0.4943(4) 0.0616(14) Uani 1 1 d . . .
C9 C 1.0719(5) 0.8919(5) 0.7231(5) 0.0696(16) Uani 1 1 d . . .
H9A H 1.1428 0.8873 0.7452 0.084 Uiso 1 1 calc R . .
H9B H 1.0755 0.9667 0.7359 0.084 Uiso 1 1 calc R . .
C10 C 0.9804(5) 0.8322(5) 0.7703(4) 0.0645(14) Uani 1 1 d . . .
C11 C 0.9019(7) 0.8735(6) 0.8137(5) 0.086(2) Uani 1 1 d . . .
H11 H 0.9053 0.9439 0.8136 0.103 Uiso 1 1 calc R . .
C12 C 0.8195(7) 0.8138(8) 0.8566(6) 0.105(3) Uani 1 1 d . . .
H12 H 0.7682 0.8431 0.8859 0.125 Uiso 1 1 calc R . .
C13 C 0.8145(7) 0.7088(8) 0.8553(6) 0.105(3) Uani 1 1 d . . .
H13 H 0.7581 0.6658 0.8825 0.126 Uiso 1 1 calc R . .
C14 C 0.8930(6) 0.6689(6) 0.8137(5) 0.085(2) Uani 1 1 d . . .
H14 H 0.8915 0.5993 0.8147 0.103 Uiso 1 1 calc R . .
C15 C 0.7804(5) 0.6265(4) 0.4368(4) 0.0605(14) Uani 1 1 d . . .
H15A H 0.7300 0.6579 0.4712 0.073 Uiso 1 1 calc R . .
H15B H 0.7412 0.5894 0.3806 0.073 Uiso 1 1 calc R . .
C16 C 0.8080(4) 0.5483(4) 0.4814(4) 0.0510(12) Uani 1 1 d . . .
C17 C 0.7897(5) 0.5403(5) 0.5669(4) 0.0692(16) Uani 1 1 d . . .
H17 H 0.7588 0.5878 0.6014 0.083 Uiso 1 1 calc R . .
C18 C 0.8167(5) 0.4627(6) 0.6021(5) 0.0761(18) Uani 1 1 d . . .
H18 H 0.8030 0.4572 0.6596 0.091 Uiso 1 1 calc R . .
C19 C 0.8633(5) 0.3950(5) 0.5519(5) 0.0729(17) Uani 1 1 d . . .
H19 H 0.8812 0.3421 0.5744 0.087 Uiso 1 1 calc R . .
C20 C 0.8838(4) 0.4048(4) 0.4676(4) 0.0594(14) Uani 1 1 d . . .
H20 H 0.9158 0.3583 0.4331 0.071 Uiso 1 1 calc R . .
C21 C 0.4777(7) 0.3677(8) 0.3534(8) 0.106(3) Uani 1 1 d . . .
C22 C 0.5655(5) 0.3177(5) 0.3142(4) 0.0708(16) Uani 1 1 d . . .
C23 C 0.5352(5) 0.2073(6) 0.2916(5) 0.083(2) Uani 1 1 d . . .
H23 H 0.4625 0.1661 0.2987 0.100 Uiso 1 1 calc R . .
C24 C 0.6132(5) 0.1580(5) 0.2584(5) 0.0696(16) Uani 1 1 d . . .
C25 C 0.5759(8) 0.0373(6) 0.2337(7) 0.096(3) Uani 1 1 d . . .
C26 C 0.8275(8) 0.1040(6) -0.0049(5) 0.087(2) Uani 1 1 d . . .
C27 C 0.7773(6) 0.1884(5) 0.0427(4) 0.0666(15) Uani 1 1 d . . .
C28 C 0.6713(6) 0.1865(6) 0.0144(5) 0.0788(18) Uani 1 1 d . . .
H28 H 0.6319 0.1343 -0.0327 0.095 Uiso 1 1 calc R . .
C29 C 0.6242(5) 0.2607(6) 0.0552(5) 0.0797(19) Uani 1 1 d . . .
C30 C 0.5133(11) 0.2625(15) 0.0136(10) 0.155(6) Uani 1 1 d . . .
C31 C 1.1160(7) 0.6016(8) 0.1110(6) 0.090(2) Uani 1 1 d . . .
C32 C 0.9984(5) 0.5729(5) 0.1467(4) 0.0639(14) Uani 1 1 d . . .
C33 C 0.9388(6) 0.6435(5) 0.1509(5) 0.084(2) Uani 1 1 d . . .
H33 H 0.9706 0.7081 0.1336 0.101 Uiso 1 1 calc R . .
C34 C 0.8322(6) 0.6212(6) 0.1802(5) 0.0774(18) Uani 1 1 d . . .
C35 C 0.7683(9) 0.7019(8) 0.1778(8) 0.110(3) Uani 1 1 d . . .
N1 N 0.9726(4) 0.7290(4) 0.7712(3) 0.0627(12) Uani 1 1 d . . .
N2 N 0.8581(3) 0.4809(3) 0.4344(3) 0.0495(10) Uani 1 1 d . . .
O1 O 1.0455(3) 0.6859(3) 0.7290(3) 0.0584(9) Uani 1 1 d . . .
O2 O 0.8853(3) 0.4930(3) 0.3544(3) 0.0575(9) Uani 1 1 d . . .
O3 O 0.6577(3) 0.3840(3) 0.3084(3) 0.0644(10) Uani 1 1 d . . .
O4 O 0.7130(3) 0.2011(3) 0.2442(3) 0.0677(11) Uani 1 1 d . . .
O5 O 0.8424(3) 0.2539(3) 0.1028(3) 0.0656(10) Uani 1 1 d . . .
O6 O 0.6624(3) 0.3327(4) 0.1205(3) 0.0766(12) Uani 1 1 d . . .
O7 O 0.9696(3) 0.4842(3) 0.1677(3) 0.0632(10) Uani 1 1 d . . .
O8 O 0.7793(3) 0.5406(3) 0.2072(3) 0.0723(11) Uani 1 1 d . . .
O9 O 0.6393(5) 1.2780(5) 0.7172(4) 0.1077(18) Uani 1 1 d . . .
O10 O 0.5205(4) 1.1963(4) 0.5482(5) 0.111(2) Uani 1 1 d . . .
F1 F 0.3859(6) 0.2952(7) 0.3745(11) 0.171(5) Uani 0.797(12) 1 d P . .
F1A F 0.384(3) 0.329(4) 0.312(4) 0.171(5) Uani 0.203(12) 1 d P . .
F2 F 0.4466(11) 0.4211(12) 0.3030(10) 0.168(5) Uani 0.797(12) 1 d P . .
F2A F 0.499(5) 0.461(6) 0.357(5) 0.168(5) Uani 0.203(12) 1 d P . .
F3 F 0.5175(9) 0.4351(12) 0.4261(8) 0.186(6) Uani 0.797(12) 1 d P . .
F3A F 0.465(4) 0.365(5) 0.431(3) 0.186(6) Uani 0.203(12) 1 d P . .
F4 F 0.4846(8) -0.0110(6) 0.2693(10) 0.163(5) Uani 0.750(9) 1 d P . .
F4A F 0.474(3) -0.005(2) 0.195(4) 0.163(5) Uani 0.250(9) 1 d P . .
F5 F 0.6507(8) -0.0051(6) 0.2568(10) 0.161(5) Uani 0.750(9) 1 d P . .
F5A F 0.575(3) -0.0088(19) 0.292(3) 0.161(5) Uani 0.250(9) 1 d P . .
F6 F 0.5581(17) 0.0055(8) 0.1509(8) 0.212(9) Uani 0.750(9) 1 d P . .
F6A F 0.636(6) 0.004(3) 0.178(3) 0.212(9) Uani 0.250(9) 1 d P . .
F7 F 0.8334(7) 0.0378(5) 0.0424(5) 0.163(3) Uani 1 1 d . . .
F8 F 0.9320(5) 0.1448(5) -0.0238(5) 0.156(3) Uani 1 1 d . . .
F9 F 0.7758(7) 0.0524(6) -0.0794(4) 0.169(3) Uani 1 1 d . . .
F10 F 0.4327(10) 0.1580(16) 0.0218(14) 0.197(7) Uani 0.578(9) 1 d P . .
F10A F 0.441(2) 0.260(3) 0.076(3) 0.197(7) Uani 0.422(9) 1 d P . .
F11 F 0.4639(14) 0.3203(15) 0.0570(15) 0.168(6) Uani 0.578(9) 1 d P . .
F11A F 0.5329(14) 0.3646(19) -0.0131(13) 0.168(6) Uani 0.422(9) 1 d P . .
F12 F 0.5016(18) 0.242(2) -0.0741(11) 0.171(8) Uani 0.578(9) 1 d P . .
F12A F 0.467(3) 0.197(4) -0.0422(16) 0.171(8) Uani 0.422(9) 1 d P . .
F13 F 1.1886(5) 0.5667(8) 0.1538(7) 0.153(4) Uani 0.830(9) 1 d P . .
F13A F 1.121(3) 0.504(4) 0.057(4) 0.153(4) Uani 0.170(9) 1 d P . .
F14 F 1.1171(7) 0.5641(9) 0.0319(6) 0.169(6) Uani 0.830(9) 1 d P . .
F14A F 1.087(4) 0.632(5) 0.034(3) 0.169(6) Uani 0.170(9) 1 d P . .
F15 F 1.1677(5) 0.7068(5) 0.1245(5) 0.115(2) Uani 0.830(9) 1 d P . .
F15A F 1.184(4) 0.625(3) 0.160(3) 0.115(2) Uani 0.170(9) 1 d P . .
F16 F 0.7042(7) 0.7072(6) 0.2360(7) 0.192(4) Uani 1 1 d . . .
F17 F 0.7150(11) 0.6840(9) 0.1068(6) 0.268(7) Uani 1 1 d . . .
F18 F 0.8363(8) 0.8015(6) 0.1885(8) 0.222(5) Uani 1 1 d . . .
S1 S 0.78024(14) 1.16480(13) 0.67387(12) 0.0731(4) Uani 1 1 d . . .
S2 S 0.65278(17) 1.07696(18) 0.50023(16) 0.0995(7) Uani 1 1 d . . .
S3 S 0.79187(14) 0.90292(13) 0.46139(13) 0.0761(5) Uani 1 1 d . . .
S4 S 0.92363(14) 1.00360(12) 0.62931(12) 0.0720(4) Uani 1 1 d . . .
S5 S 1.05699(14) 0.84514(13) 0.60599(12) 0.0719(4) Uani 1 1 d . . .
S6 S 0.90515(13) 0.73324(11) 0.42068(12) 0.0673(4) Uani 1 1 d . . .
Dy1 Dy 0.813213(18) 0.377369(18) 0.223360(17) 0.05160(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O9 1.389(10) . ?
C1 C2 1.454(15) . ?
C2 O10 1.442(11) . ?
C3 C4 1.294(11) . ?
C3 O10 1.360(8) . ?
C3 S2 1.756(7) . ?
C4 O9 1.370(9) . ?
C4 S1 1.753(7) . ?
C5 C6 1.352(8) . ?
C5 S2 1.738(6) . ?
C5 S1 1.763(7) . ?
C6 S3 1.749(7) . ?
C6 S4 1.762(6) . ?
C7 C8 1.351(9) . ?
C7 S5 1.749(6) . ?
C7 S4 1.751(5) . ?
C8 S6 1.744(6) . ?
C8 S3 1.758(6) . ?
C9 C10 1.478(9) . ?
C9 S5 1.810(7) . ?
C10 N1 1.358(7) . ?
C10 C11 1.386(9) . ?
C11 C12 1.369(11) . ?
C12 C13 1.384(12) . ?
C13 C14 1.365(10) . ?
C14 N1 1.348(8) . ?
C15 C16 1.481(7) . ?
C15 S6 1.828(6) . ?
C16 N2 1.357(6) . ?
C16 C17 1.379(9) . ?
C17 C18 1.386(10) . ?
C18 C19 1.354(10) . ?
C19 C20 1.370(9) . ?
C20 N2 1.343(7) . ?
C21 F2A 1.18(7) . ?
C21 F3A 1.23(6) . ?
C21 F1A 1.24(5) . ?
C21 F2 1.288(16) . ?
C21 F3 1.298(15) . ?
C21 F1 1.352(13) . ?
C21 C22 1.524(9) . ?
C22 O3 1.241(7) . ?
C22 C23 1.384(10) . ?
C23 C24 1.386(9) . ?
C24 O4 1.248(7) . ?
C24 C25 1.511(9) . ?
C25 F5A 1.19(4) . ?
C25 F6A 1.26(7) . ?
C25 F6 1.280(15) . ?
C25 F5 1.309(13) . ?
C25 F4A 1.32(4) . ?
C25 F4 1.317(12) . ?
C26 F7 1.275(9) . ?
C26 F9 1.291(9) . ?
C26 F8 1.316(10) . ?
C26 C27 1.529(9) . ?
C27 O5 1.248(7) . ?
C27 C28 1.383(9) . ?
C28 C29 1.363(10) . ?
C29 O6 1.241(8) . ?
C29 C30 1.533(12) . ?
C30 F12A 1.12(4) . ?
C30 F11 1.24(2) . ?
C30 F10A 1.34(4) . ?
C30 F12 1.35(2) . ?
C30 F11A 1.46(3) . ?
C30 F10 1.49(3) . ?
C31 F15A 1.07(5) . ?
C31 F14 1.247(12) . ?
C31 F15 1.335(11) . ?
C31 F13 1.362(12) . ?
C31 F14A 1.42(6) . ?
C31 F13A 1.43(6) . ?
C31 C32 1.542(10) . ?
C32 O7 1.243(7) . ?
C32 C33 1.359(9) . ?
C33 C34 1.377(10) . ?
C34 O8 1.237(8) . ?
C34 C35 1.529(11) . ?
C35 F16 1.225(11) . ?
C35 F17 1.235(13) . ?
C35 F18 1.326(12) . ?
N1 O1 1.333(6) . ?
N2 O2 1.328(6) . ?
O1 Dy1 2.345(3) 2_766 ?
O2 Dy1 2.309(4) . ?
O3 Dy1 2.380(4) . ?
O4 Dy1 2.402(4) . ?
O5 Dy1 2.370(4) . ?
O6 Dy1 2.323(4) . ?
O7 Dy1 2.335(4) . ?
O8 Dy1 2.404(4) . ?
F1 F1A 1.16(7) . ?
F1 F3A 1.32(4) . ?
F1A F2 1.28(5) . ?
F2 F2A 1.02(7) . ?
F2A F3 1.23(6) . ?
F3 F3A 0.98(6) . ?
F4 F5A 1.17(3) . ?
F4 F4A 1.18(5) . ?
F4A F6 1.26(3) . ?
F5 F5A 1.09(4) . ?
F5 F6A 1.29(5) . ?
F6 F6A 1.06(7) . ?
F10 F12A 1.24(3) . ?
F10 F10A 1.44(4) . ?
F10A F11 0.88(3) . ?
F11 F11A 1.50(3) . ?
F11A F12 1.67(3) . ?
F12 F12A 0.86(4) . ?
F13 F15A 0.79(4) . ?
F13 F13A 1.67(6) . ?
F13A F14 0.98(3) . ?
F14 F14A 1.08(6) . ?
F14A F15 1.69(5) . ?
F15 F15A 1.38(5) . ?
Dy1 O1 2.345(3) 2_766 ?

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
O9 C1 C2 113.5(9) . . ?
O10 C2 C1 114.8(8) . . ?
C4 C3 O10 125.9(7) . . ?
C4 C3 S2 118.5(5) . . ?
O10 C3 S2 115.5(6) . . ?
C3 C4 O9 124.7(6) . . ?
C3 C4 S1 118.9(5) . . ?
O9 C4 S1 116.4(6) . . ?
C6 C5 S2 122.7(5) . . ?
C6 C5 S1 120.7(5) . . ?
S2 C5 S1 116.6(3) . . ?
C5 C6 S3 124.2(5) . . ?
C5 C6 S4 121.7(5) . . ?
S3 C6 S4 113.9(3) . . ?
C8 C7 S5 122.0(4) . . ?
C8 C7 S4 116.8(4) . . ?
S5 C7 S4 120.5(4) . . ?
C7 C8 S6 125.1(4) . . ?
C7 C8 S3 117.2(4) . . ?
S6 C8 S3 117.4(4) . . ?
C10 C9 S5 114.6(4) . . ?
N1 C10 C11 117.5(6) . . ?
N1 C10 C9 117.4(5) . . ?
C11 C10 C9 125.1(6) . . ?
C12 C11 C10 122.0(7) . . ?
C11 C12 C13 118.5(7) . . ?
C14 C13 C12 119.4(8) . . ?
N1 C14 C13 121.0(7) . . ?
C16 C15 S6 112.7(4) . . ?
N2 C16 C17 117.7(5) . . ?
N2 C16 C15 116.8(5) . . ?
C17 C16 C15 125.4(5) . . ?
C16 C17 C18 121.0(6) . . ?
C19 C18 C17 119.2(7) . . ?
C18 C19 C20 119.6(6) . . ?
N2 C20 C19 120.7(6) . . ?
F2A C21 F3A 99(4) . . ?
F2A C21 F1A 104(4) . . ?
F3A C21 F1A 109(3) . . ?
F2A C21 F2 49(3) . . ?
F3A C21 F2 132(2) . . ?
F1A C21 F2 61(3) . . ?
F2A C21 F3 59(3) . . ?
F3A C21 F3 46(2) . . ?
F1A C21 F3 135.5(19) . . ?
F2 C21 F3 105.9(12) . . ?
F2A C21 F1 131(2) . . ?
F3A C21 F1 61(2) . . ?
F1A C21 F1 53(3) . . ?
F2 C21 F1 109.3(10) . . ?
F3 C21 F1 104.8(12) . . ?
F2A C21 C22 116(3) . . ?
F3A C21 C22 115(2) . . ?
F1A C21 C22 113.2(19) . . ?
F2 C21 C22 112.3(10) . . ?
F3 C21 C22 111.1(9) . . ?
F1 C21 C22 113.0(8) . . ?
O3 C22 C23 128.4(6) . . ?
O3 C22 C21 113.8(6) . . ?
C23 C22 C21 117.8(6) . . ?
C22 C23 C24 119.9(6) . . ?
O4 C24 C23 128.1(6) . . ?
O4 C24 C25 113.9(6) . . ?
C23 C24 C25 118.0(6) . . ?
F5A C25 F6A 107(3) . . ?
F5A C25 F6 132.8(18) . . ?
F6A C25 F6 49(3) . . ?
F5A C25 F5 51.6(17) . . ?
F6A C25 F5 60(3) . . ?
F6 C25 F5 105.6(13) . . ?
F5A C25 F4A 104(2) . . ?
F6A C25 F4A 103(3) . . ?
F6 C25 F4A 57.9(19) . . ?
F5 C25 F4A 132.3(14) . . ?
F5A C25 F4 55.2(15) . . ?
F6A C25 F4 133(2) . . ?
F6 C25 F4 107.7(11) . . ?
F5 C25 F4 103.6(10) . . ?
F4A C25 F4 53.4(18) . . ?
F5A C25 C24 116.3(17) . . ?
F6A C25 C24 112(2) . . ?
F6 C25 C24 110.8(9) . . ?
F5 C25 C24 113.5(8) . . ?
F4A C25 C24 114.2(15) . . ?
F4 C25 C24 114.9(8) . . ?
F7 C26 F9 109.5(8) . . ?
F7 C26 F8 104.1(8) . . ?
F9 C26 F8 103.7(8) . . ?
F7 C26 C27 111.6(7) . . ?
F9 C26 C27 114.2(7) . . ?
F8 C26 C27 113.0(6) . . ?
O5 C27 C28 128.2(6) . . ?
O5 C27 C26 112.9(6) . . ?
C28 C27 C26 118.9(6) . . ?
C29 C28 C27 120.4(6) . . ?
O6 C29 C28 128.4(6) . . ?
O6 C29 C30 114.0(7) . . ?
C28 C29 C30 117.5(7) . . ?
F12A C30 F11 120(2) . . ?
F12A C30 F10A 106(3) . . ?
F11 C30 F10A 39.6(14) . . ?
F12A C30 F12 40(2) . . ?
F11 C30 F12 120.5(18) . . ?
F10A C30 F12 134.0(17) . . ?
F12A C30 F11A 108(2) . . ?
F11 C30 F11A 67.3(16) . . ?
F10A C30 F11A 107(2) . . ?
F12 C30 F11A 72.9(18) . . ?
F12A C30 F10 54.8(17) . . ?
F11 C30 F10 97(2) . . ?
F10A C30 F10 61(2) . . ?
F12 C30 F10 94.5(16) . . ?
F11A C30 F10 148.4(12) . . ?
F12A C30 C29 120(2) . . ?
F11 C30 C29 116.8(11) . . ?
F10A C30 C29 107.1(18) . . ?
F12 C30 C29 116.7(14) . . ?
F11A C30 C29 108.3(13) . . ?
F10 C30 C29 103.3(14) . . ?
F15A C31 F14 127(2) . . ?
F15A C31 F15 69(2) . . ?
F14 C31 F15 107.8(8) . . ?
F15A C31 F13 35(2) . . ?
F14 C31 F13 106.4(11) . . ?
F15 C31 F13 102.4(9) . . ?
F15A C31 F14A 139(3) . . ?
F14 C31 F14A 47.2(19) . . ?
F15 C31 F14A 75(2) . . ?
F13 C31 F14A 147.7(19) . . ?
F15A C31 F13A 106(3) . . ?
F14 C31 F13A 42.0(18) . . ?
F15 C31 F13A 140.1(17) . . ?
F13 C31 F13A 73.1(19) . . ?
F14A C31 F13A 88(3) . . ?
F15A C31 C32 114(2) . . ?
F14 C31 C32 114.5(8) . . ?
F15 C31 C32 113.2(8) . . ?
F13 C31 C32 111.7(6) . . ?
F14A C31 C32 98.2(17) . . ?
F13A C31 C32 104.9(15) . . ?
O7 C32 C33 127.9(6) . . ?
O7 C32 C31 113.4(6) . . ?
C33 C32 C31 118.7(6) . . ?
C32 C33 C34 121.4(6) . . ?
O8 C34 C33 127.3(6) . . ?
O8 C34 C35 114.7(7) . . ?
C33 C34 C35 118.0(7) . . ?
F16 C35 F17 108.8(11) . . ?
F16 C35 F18 103.3(11) . . ?
F17 C35 F18 105.7(10) . . ?
F16 C35 C34 114.6(8) . . ?
F17 C35 C34 111.4(10) . . ?
F18 C35 C34 112.5(9) . . ?
O1 N1 C14 119.1(5) . . ?
O1 N1 C10 119.3(5) . . ?
C14 N1 C10 121.6(5) . . ?
O2 N2 C20 119.4(4) . . ?
O2 N2 C16 118.8(4) . . ?
C20 N2 C16 121.7(5) . . ?
N1 O1 Dy1 132.7(3) . 2_766 ?
N2 O2 Dy1 128.4(3) . . ?
C22 O3 Dy1 133.5(4) . . ?
C24 O4 Dy1 132.8(4) . . ?
C27 O5 Dy1 132.5(4) . . ?
C29 O6 Dy1 135.4(4) . . ?
C32 O7 Dy1 137.3(4) . . ?
C34 O8 Dy1 135.4(4) . . ?
C4 O9 C1 110.8(8) . . ?
C3 O10 C2 109.7(7) . . ?
F1A F1 F3A 108(4) . . ?
F1A F1 C21 59(2) . . ?
F3A F1 C21 55(3) . . ?
F1 F1A C21 68(4) . . ?
F1 F1A F2 124(5) . . ?
C21 F1A F2 61.5(19) . . ?
F2A F2 F1A 112(6) . . ?
F2A F2 C21 60(4) . . ?
F1A F2 C21 58(3) . . ?
F2 F2A C21 71(5) . . ?
F2 F2A F3 133(7) . . ?
C21 F2A F3 65(3) . . ?
F3A F3 F2A 112(6) . . ?
F3A F3 C21 64(3) . . ?
F2A F3 C21 56(4) . . ?
F3 F3A C21 71(4) . . ?
F3 F3A F1 131(7) . . ?
C21 F3A F1 64(2) . . ?
F5A F4 F4A 114(3) . . ?
F5A F4 C25 57(2) . . ?
F4A F4 C25 63.2(16) . . ?
F4 F4A F6 118(4) . . ?
F4 F4A C25 63(3) . . ?
F6 F4A C25 59.7(15) . . ?
F5A F5 F6A 111(4) . . ?
F5A F5 C25 58.7(18) . . ?
F6A F5 C25 58(4) . . ?
F5 F5A F4 132(4) . . ?
F5 F5A C25 70(3) . . ?
F4 F5A C25 68(2) . . ?
F6A F6 F4A 121(5) . . ?
F6A F6 C25 65(3) . . ?
F4A F6 C25 62(3) . . ?
F6 F6A C25 66(5) . . ?
F6 F6A F5 123(7) . . ?
C25 F6A F5 62(3) . . ?
F12A F10 F10A 93(3) . . ?
F12A F10 C30 47.3(19) . . ?
F10A F10 C30 54.3(15) . . ?
F11 F10A C30 64(3) . . ?
F11 F10A F10 122(5) . . ?
C30 F10A F10 65(3) . . ?
F10A F11 C30 76(3) . . ?
F10A F11 F11A 139(4) . . ?
C30 F11 F11A 63.3(17) . . ?
C30 F11A F11 49.4(12) . . ?
C30 F11A F12 50.5(11) . . ?
F11 F11A F12 89.9(18) . . ?
F12A F12 C30 56(3) . . ?
F12A F12 F11A 107(4) . . ?
C30 F12 F11A 56.6(14) . . ?
F12 F12A C30 84(5) . . ?
F12 F12A F10 162(6) . . ?
C30 F12A F10 77.9(19) . . ?
F15A F13 C31 51(4) . . ?
F15A F13 F13A 104(5) . . ?
C31 F13 F13A 55.5(15) . . ?
F14 F13A C31 59(3) . . ?
F14 F13A F13 101(4) . . ?
C31 F13A F13 51(2) . . ?
F13A F14 F14A 149(5) . . ?
F13A F14 C31 79(4) . . ?
F14A F14 C31 75(3) . . ?
F14 F14A C31 58(3) . . ?
F14 F14A F15 95(4) . . ?
C31 F14A F15 49.9(17) . . ?
C31 F15 F15A 46.2(18) . . ?
C31 F15 F14A 55(2) . . ?
F15A F15 F14A 98(3) . . ?
F13 F15A C31 93(4) . . ?
F13 F15A F15 151(6) . . ?
C31 F15A F15 65(3) . . ?
C4 S1 C5 92.2(3) . . ?
C5 S2 C3 92.8(3) . . ?
C6 S3 C8 95.6(3) . . ?
C7 S4 C6 95.7(3) . . ?
C7 S5 C9 104.1(3) . . ?
C8 S6 C15 100.5(3) . . ?
O2 Dy1 O6 140.31(14) . . ?
O2 Dy1 O7 84.12(14) . . ?
O6 Dy1 O7 107.33(16) . . ?
O2 Dy1 O1 76.26(13) . 2_766 ?
O6 Dy1 O1 142.35(15) . 2_766 ?
O7 Dy1 O1 79.67(13) . 2_766 ?
O2 Dy1 O5 147.46(13) . . ?
O6 Dy1 O5 71.78(15) . . ?
O7 Dy1 O5 78.64(14) . . ?
O1 Dy1 O5 73.65(14) 2_766 . ?
O2 Dy1 O3 73.07(13) . . ?
O6 Dy1 O3 76.03(15) . . ?
O7 Dy1 O3 142.99(14) . . ?
O1 Dy1 O3 120.80(14) 2_766 . ?
O5 Dy1 O3 134.23(13) . . ?
O2 Dy1 O4 111.56(15) . . ?
O6 Dy1 O4 79.86(17) . . ?
O7 Dy1 O4 146.58(14) . . ?
O1 Dy1 O4 76.07(14) 2_766 . ?
O5 Dy1 O4 72.73(14) . . ?
O3 Dy1 O4 70.25(13) . . ?
O2 Dy1 O8 76.28(15) . . ?
O6 Dy1 O8 72.41(16) . . ?
O7 Dy1 O8 70.74(14) . . ?
O1 Dy1 O8 141.21(14) 2_766 . ?
O5 Dy1 O8 122.20(15) . . ?
O3 Dy1 O8 75.69(15) . . ?
O4 Dy1 O8 140.23(14) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.09
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.708
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.118
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_importks22-3
_database_code_depnum_ccdc_archive 'CCDC 1407104'
_audit_update_record             
;
2015-06-16 deposited with the CCDC.
2015-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45.41 H30.54 Cl2.82 Dy F9 N2 O10 S9'
_chemical_formula_weight         1486.2

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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.4634(8)
_cell_length_b                   12.1092(10)
_cell_length_c                   23.9781(18)
_cell_angle_alpha                77.004(2)
_cell_angle_beta                 86.822(2)
_cell_angle_gamma                74.808(2)
_cell_volume                     2856.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4487
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      21.81

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1522
_exptl_absorpt_coefficient_mu    1.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6193
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29912
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_sigmaI/netI    0.1423
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         0.87
_diffrn_reflns_theta_max         27.54
_reflns_number_total             12500
_reflns_number_gt                7773
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1083P)²+17.4267P] 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_number_reflns         12500
_refine_ls_number_parameters     711
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0882
_refine_ls_wR_factor_ref         0.2413
_refine_ls_wR_factor_gt          0.2008
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_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
C1 C 0.2761(11) 0.4536(12) 0.7194(5) 0.037(3) Uani 1 1 d . . .
H1A H 0.2729 0.3856 0.7050 0.045 Uiso 1 1 calc R . .
H1B H 0.3108 0.5058 0.6892 0.045 Uiso 1 1 calc R . .
C2 C 0.1404(13) 0.5145(11) 0.7335(6) 0.042(3) Uani 1 1 d . . .
H2A H 0.1429 0.5848 0.7460 0.050 Uiso 1 1 calc R . .
H2B H 0.0856 0.5382 0.6994 0.050 Uiso 1 1 calc R . .
C3 C 0.1714(11) 0.3820(11) 0.8203(5) 0.032(3) Uani 1 1 d . . .
C4 C 0.3006(10) 0.3726(10) 0.8156(5) 0.031(3) Uani 1 1 d . . .
C5 C 0.2654(12) 0.2741(11) 0.9187(5) 0.037(3) Uani 1 1 d . . .
C6 C 0.2745(11) 0.2314(11) 0.9763(5) 0.034(3) Uani 1 1 d . . .
C7 C 0.3611(11) 0.1748(11) 1.0808(5) 0.034(3) Uani 1 1 d . . .
C8 C 0.2249(11) 0.2017(11) 1.0840(5) 0.036(3) Uani 1 1 d . . .
C9 C 0.4403(11) 0.0107(10) 1.1836(5) 0.033(3) Uani 1 1 d . . .
H9A H 0.3484 0.0283 1.1955 0.040 Uiso 1 1 calc R . .
H9B H 0.4556 -0.0530 1.1636 0.040 Uiso 1 1 calc R . .
C10 C 0.5283(9) -0.0241(10) 1.2341(5) 0.026(2) Uani 1 1 d . . .
C11 C 0.6419(10) -0.1189(11) 1.2429(5) 0.032(3) Uani 1 1 d . . .
H11 H 0.6654 -0.1652 1.2159 0.038 Uiso 1 1 calc R . .
C12 C 0.7173(11) -0.1431(11) 1.2905(6) 0.040(3) Uani 1 1 d . . .
H12 H 0.7929 -0.2053 1.2957 0.048 Uiso 1 1 calc R . .
C13 C 0.6829(10) -0.0760(10) 1.3319(5) 0.030(3) Uani 1 1 d . . .
H13 H 0.7334 -0.0946 1.3650 0.036 Uiso 1 1 calc R . .
C14 C 0.5739(10) 0.0177(10) 1.3230(5) 0.028(3) Uani 1 1 d . . .
H14 H 0.5517 0.0649 1.3496 0.034 Uiso 1 1 calc R . .
C15 C 0.0968(10) 0.3649(11) 1.1434(5) 0.032(3) Uani 1 1 d . . .
H15A H 0.0601 0.4079 1.1062 0.039 Uiso 1 1 calc R . .
H15B H 0.0321 0.3863 1.1722 0.039 Uiso 1 1 calc R . .
C16 C 0.2174(11) 0.3955(10) 1.1528(5) 0.030(3) Uani 1 1 d . . .
C21 C 0.4549(11) 0.3627(10) 1.3931(5) 0.030(3) Uani 1 1 d . . .
C22 C 0.3282(10) 0.3326(9) 1.3836(5) 0.022(2) Uani 1 1 d . . .
C23 C 0.2111(10) 0.4063(10) 1.3967(5) 0.032(3) Uani 1 1 d . B .
H23 H 0.2136 0.4729 1.4094 0.038 Uiso 1 1 calc R . .
C24 C 0.0867(10) 0.3823(10) 1.3912(5) 0.027(2) Uani 1 1 d . . .
C29 C 0.4183(10) -0.2027(10) 1.4224(5) 0.028(3) Uani 1 1 d . . .
C30 C 0.2986(9) -0.0993(9) 1.4070(5) 0.022(2) Uani 1 1 d . . .
C31 C 0.1761(10) -0.1149(9) 1.4245(5) 0.026(2) Uani 1 1 d . A .
H31 H 0.1702 -0.1889 1.4441 0.031 Uiso 1 1 calc R . .
C32 C 0.0596(10) -0.0243(10) 1.4140(5) 0.027(2) Uani 1 1 d . . .
N1 N 0.4977(8) 0.0419(8) 1.2752(4) 0.0231(19) Uani 1 1 d . . .
N2 N 0.2639(8) 0.3700(8) 1.2076(4) 0.027(2) Uani 1 1 d . . .
O1 O 0.3928(6) 0.1334(6) 1.2669(3) 0.0272(17) Uani 1 1 d . A .
O2 O 0.1904(7) 0.3332(6) 1.2507(3) 0.0262(17) Uani 1 1 d . A .
O3 O 0.3452(6) 0.2401(6) 1.3652(3) 0.0244(16) Uani 1 1 d . A .
O4 O 0.0709(7) 0.3034(6) 1.3696(3) 0.0261(17) Uani 1 1 d . A .
O5 O 0.3275(6) -0.0060(6) 1.3812(3) 0.0236(16) Uani 1 1 d . A .
O6 O 0.0562(7) 0.0758(6) 1.3834(3) 0.0255(16) Uani 1 1 d . A .
O7 O -0.0018(6) 0.2025(6) 1.2694(3) 0.0251(17) Uani 1 1 d . A .
O10 O 0.0806(7) 0.4404(7) 0.7786(4) 0.0352(19) Uani 1 1 d . . .
O9 O 0.3640(8) 0.4166(8) 0.7678(3) 0.040(2) Uani 1 1 d . . .
F4 F 0.4774(6) -0.2330(6) 1.3742(3) 0.0431(18) Uani 1 1 d . . .
F5 F 0.3921(6) -0.3014(6) 1.4537(3) 0.0459(19) Uani 1 1 d . . .
F6 F 0.5111(6) -0.1790(6) 1.4499(3) 0.0391(17) Uani 1 1 d . . .
S1 S 0.4028(3) 0.2859(3) 0.87407(14) 0.0372(7) Uani 1 1 d . . .
S2 S 0.1113(3) 0.3126(3) 0.88433(14) 0.0433(8) Uani 1 1 d . . .
S3 S 0.1371(3) 0.2273(3) 1.02020(14) 0.0400(8) Uani 1 1 d . . .
S4 S 0.4279(3) 0.1741(3) 1.01247(14) 0.0417(8) Uani 1 1 d . . .
S5 S 0.4759(3) 0.1417(3) 1.13553(13) 0.0361(7) Uani 1 1 d . . .
S6 S 0.1315(3) 0.2052(3) 1.14712(13) 0.0328(7) Uani 1 1 d . . .
Dy1 Dy 0.19895(5) 0.16121(5) 1.32089(2) 0.02178(16) Uani 1 1 d . . .
F3 F 0.4428(7) 0.4559(8) 1.4149(5) 0.070(3) Uani 1 1 d . . .
F1 F 0.5217(7) 0.3818(8) 1.3443(3) 0.059(2) Uani 1 1 d . . .
F2 F 0.5378(7) 0.2746(7) 1.4280(4) 0.057(2) Uani 1 1 d . . .
C45 C -0.2263(17) 0.3067(15) 1.0605(7) 0.069(5) Uani 1 1 d D . .
H45A H -0.1425 0.2586 1.0776 0.083 Uiso 1 1 calc R . .
H45B H -0.2960 0.2861 1.0859 0.083 Uiso 1 1 calc R . .
Cl1 Cl -0.2320(11) 0.4551(10) 1.0578(5) 0.196(3) Uani 1 1 d D . .
Cl2 Cl -0.2425(11) 0.2719(10) 0.9991(5) 0.196(3) Uani 1 1 d D . .
C46 C -0.072(4) 0.065(6) 0.9336(16) 0.14(3) Uiso 0.410(15) 1 d PD . .
H46A H -0.0809 -0.0012 0.9634 0.167 Uiso 1 1 calc R . .
H46B H -0.0564 0.1235 0.9523 0.167 Uiso 1 1 calc R . .
Cl3 Cl -0.215(3) 0.121(3) 0.8995(16) 0.270(15) Uiso 0.410(15) 1 d PD . .
Cl4 Cl 0.066(3) 0.019(3) 0.8951(16) 0.270(15) Uiso 0.410(15) 1 d PD . .
C20 C 0.3865(10) 0.3801(10) 1.2190(5) 0.029(3) Uani 1 1 d . . .
H20 H 0.4199 0.3544 1.2561 0.035 Uiso 1 1 calc R . .
C19 C 0.4615(11) 0.4289(10) 1.1751(6) 0.034(3) Uani 1 1 d . . .
H19 H 0.5434 0.4387 1.1829 0.041 Uiso 1 1 calc R . .
C17 C 0.2905(13) 0.4425(12) 1.1094(5) 0.042(3) Uani 1 1 d . . .
H17 H 0.2590 0.4618 1.0720 0.051 Uiso 1 1 calc R . .
C18 C 0.4125(13) 0.4622(12) 1.1202(6) 0.046(3) Uani 1 1 d . . .
H18 H 0.4595 0.4974 1.0905 0.055 Uiso 1 1 calc R . .
O8 O 0.2024(6) -0.0016(7) 1.2815(3) 0.0261(17) Uani 1 1 d . A .
C38 C -0.0630(10) 0.1350(10) 1.2568(5) 0.027(2) Uani 1 1 d . . .
C42 C 0.2943(11) -0.2360(10) 1.2678(5) 0.034(3) Uani 1 1 d . A .
H42 H 0.3661 -0.2087 1.2742 0.041 Uiso 1 1 calc R . .
C39 C -0.0191(10) 0.0173(10) 1.2567(5) 0.030(3) Uani 1 1 d . A .
H39 H -0.0794 -0.0220 1.2493 0.036 Uiso 1 1 calc R . .
C40 C 0.1146(10) -0.0456(9) 1.2675(5) 0.024(2) Uani 1 1 d . . .
C41 C 0.1611(11) -0.1691(9) 1.2624(5) 0.028(2) Uani 1 1 d . A .
C37 C -0.2052(10) 0.1967(9) 1.2357(5) 0.026(2) Uani 1 1 d . A .
S9 S 0.0563(3) -0.2492(3) 1.25035(19) 0.0500(10) Uani 1 1 d . . .
F9 F -0.2054(6) 0.2911(6) 1.1931(3) 0.0414(17) Uani 1 1 d . . .
F7 F -0.2793(6) 0.2374(7) 1.2779(3) 0.0468(19) Uani 1 1 d . . .
F8 F -0.2682(6) 0.1325(6) 1.2156(3) 0.0448(19) Uani 1 1 d . . .
C43 C 0.1849(12) -0.3711(12) 1.2532(7) 0.049(4) Uani 1 1 d . A .
H43 H 0.1752 -0.4431 1.2492 0.059 Uiso 1 1 calc R . .
C44 C 0.3014(11) -0.3511(12) 1.2618(7) 0.050(4) Uani 1 1 d . . .
H44 H 0.3809 -0.4085 1.2638 0.060 Uiso 1 1 calc R A .
C33A C -0.0683(9) -0.0377(8) 1.4410(4) 0.023(2) Uani 0.746(9) 1 d PD A 1
C34A C -0.1029(16) -0.1272(19) 1.4798(10) 0.034(5) Uani 0.746(9) 1 d PD A 1
H34A H -0.0425 -0.1986 1.4936 0.041 Uiso 0.746(9) 1 calc PR A 1
C35A C -0.2361(10) -0.1035(10) 1.4971(5) 0.0333(19) Uani 0.746(9) 1 d PD A 1
H35A H -0.2749 -0.1529 1.5241 0.040 Uiso 0.746(9) 1 calc PR A 1
C36A C -0.2965(10) 0.0032(10) 1.4676(5) 0.0333(19) Uani 0.746(9) 1 d PD A 1
H36A H -0.3871 0.0343 1.4708 0.040 Uiso 0.746(9) 1 calc PR A 1
S8A S -0.2038(4) 0.0779(4) 1.4252(2) 0.0288(13) Uani 0.746(9) 1 d PD A 1
C33B C -0.0683(9) -0.0377(8) 1.4410(4) 0.023(2) Uani 0.254(9) 1 d PD A 2
C34B C -0.192(3) 0.042(4) 1.436(3) 0.034(5) Uani 0.254(9) 1 d PD A 2
H34B H -0.2049 0.1172 1.4129 0.041 Uiso 0.254(9) 1 calc PR A 2
C35B C -0.2965(10) 0.0032(10) 1.4676(5) 0.0333(19) Uani 0.254(9) 1 d PD A 2
C36B C -0.2361(10) -0.1035(10) 1.4971(5) 0.0333(19) Uani 0.254(9) 1 d PD A 2
S8B S -0.0789(13) -0.1600(14) 1.4884(8) 0.0288(13) Uani 0.254(9) 1 d PD A 2
C25A C -0.0352(10) 0.4562(8) 1.4129(5) 0.029(3) Uani 0.524(8) 1 d PD B 1
C26A C -0.052(3) 0.564(3) 1.4324(19) 0.039(11) Uani 0.524(8) 1 d PD B 1
H26A H 0.0143 0.5991 1.4363 0.046 Uiso 0.524(8) 1 calc PR B 1
C27A C -0.1964(11) 0.6081(12) 1.4453(6) 0.045(2) Uani 0.524(8) 1 d PD B 1
H27A H -0.2376 0.6820 1.4518 0.054 Uiso 0.524(8) 1 calc PR B 1
C28A C -0.2556(11) 0.5197(11) 1.4457(6) 0.045(2) Uani 0.524(8) 1 d PD B 1
H28A H -0.3440 0.5283 1.4561 0.054 Uiso 0.524(8) 1 calc PR B 1
S7A S -0.1711(9) 0.3995(10) 1.4280(6) 0.037(2) Uani 0.524(8) 1 d PD B 1
C25B C -0.0352(10) 0.4562(8) 1.4129(5) 0.029(3) Uani 0.476(8) 1 d PD B 2
C26B C -0.161(3) 0.427(3) 1.421(2) 0.039(11) Uani 0.476(8) 1 d PD B 2
H26B H -0.1798 0.3621 1.4126 0.046 Uiso 0.476(8) 1 calc PR B 2
C27B C -0.2556(11) 0.5197(11) 1.4457(6) 0.045(2) Uani 0.476(8) 1 d PD B 2
C28B C -0.1964(11) 0.6081(12) 1.4453(6) 0.045(2) Uani 0.476(8) 1 d PD B 2
S7B S -0.0436(9) 0.5943(10) 1.4229(5) 0.037(2) Uani 0.476(8) 1 d PD B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O9 1.437(14) . ?
C1 C2 1.478(16) . ?
C2 O10 1.466(15) . ?
C3 C4 1.327(15) . ?
C3 O10 1.356(13) . ?
C3 S2 1.745(12) . ?
C4 O9 1.365(14) . ?
C4 S1 1.768(12) . ?
C5 C6 1.361(17) . ?
C5 S2 1.754(12) . ?
C5 S1 1.760(13) . ?
C6 S3 1.739(12) . ?
C6 S4 1.764(12) . ?
C7 C8 1.378(16) . ?
C7 S5 1.736(12) . ?
C7 S4 1.745(12) . ?
C8 S3 1.753(12) . ?
C8 S6 1.759(12) . ?
C9 C10 1.479(15) . ?
C9 S5 1.850(13) . ?
C10 N1 1.376(13) . ?
C10 C11 1.406(14) . ?
C11 C12 1.358(17) . ?
C12 C13 1.394(17) . ?
C13 C14 1.369(14) . ?
C14 N1 1.367(14) . ?
C15 C16 1.448(15) . ?
C15 S6 1.854(12) . ?
C16 N2 1.366(14) . ?
C16 C17 1.367(17) . ?
C21 F3 1.320(12) . ?
C21 F1 1.336(14) . ?
C21 F2 1.336(13) . ?
C21 C22 1.506(15) . ?
C22 O3 1.260(12) . ?
C22 C23 1.381(14) . ?
C23 C24 1.426(14) . ?
C24 O4 1.234(12) . ?
C24 C25A 1.495(14) . ?
C29 F6 1.328(12) . ?
C29 F5 1.345(13) . ?
C29 F4 1.359(13) . ?
C29 C30 1.514(14) . ?
C30 O5 1.262(12) . ?
C30 C31 1.374(14) . ?
C31 C32 1.401(14) . ?
C32 O6 1.260(13) . ?
C32 C33A 1.485(14) . ?
N1 O1 1.326(10) . ?
N2 O2 1.321(11) . ?
N2 C20 1.368(13) . ?
O1 Dy1 2.334(7) . ?
O2 Dy1 2.349(7) . ?
O3 Dy1 2.406(7) . ?
O4 Dy1 2.376(7) . ?
O5 Dy1 2.339(7) . ?
O6 Dy1 2.327(7) . ?
O7 C38 1.257(13) . ?
O7 Dy1 2.375(7) . ?
Dy1 O8 2.362(7) . ?
C45 Cl2 1.649(17) . ?
C45 Cl1 1.768(18) . ?
C46 Cl3 1.649(19) . ?
C46 Cl4 1.707(19) . ?
C20 C19 1.394(16) . ?
C19 C18 1.374(18) . ?
C17 C18 1.406(18) . ?
O8 C40 1.268(12) . ?
C38 C39 1.378(16) . ?
C38 C37 1.535(14) . ?
C42 C41 1.413(15) . ?
C42 C44 1.414(17) . ?
C39 C40 1.414(14) . ?
C40 C41 1.478(14) . ?
C41 S9 1.717(11) . ?
C37 F8 1.320(12) . ?
C37 F7 1.344(13) . ?
C37 F9 1.350(13) . ?
S9 C43 1.708(12) . ?
C43 C44 1.339(17) . ?
C33A C34A 1.37(2) . ?
C33A S8A 1.701(9) . ?
C34A C35A 1.406(19) . ?
C35A C36A 1.333(17) . ?
C36A S8A 1.652(11) . ?
C25A C26A 1.44(4) . ?
C25A S7A 1.723(14) . ?
C26A C27A 1.50(3) . ?
C27A C28A 1.368(19) . ?
C28A S7A 1.626(14) . ?

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
O9 C1 C2 112.5(10) . . ?
O10 C2 C1 112.3(10) . . ?
C4 C3 O10 125.1(11) . . ?
C4 C3 S2 118.6(9) . . ?
O10 C3 S2 116.3(8) . . ?
C3 C4 O9 125.9(11) . . ?
C3 C4 S1 117.7(9) . . ?
O9 C4 S1 116.2(8) . . ?
C6 C5 S2 119.9(10) . . ?
C6 C5 S1 123.8(9) . . ?
S2 C5 S1 116.2(7) . . ?
C5 C6 S3 123.2(9) . . ?
C5 C6 S4 122.4(9) . . ?
S3 C6 S4 114.4(7) . . ?
C8 C7 S5 128.8(10) . . ?
C8 C7 S4 115.9(9) . . ?
S5 C7 S4 115.4(6) . . ?
C7 C8 S3 117.3(9) . . ?
C7 C8 S6 125.6(10) . . ?
S3 C8 S6 116.9(7) . . ?
C10 C9 S5 108.6(8) . . ?
N1 C10 C11 117.8(10) . . ?
N1 C10 C9 117.6(9) . . ?
C11 C10 C9 124.6(10) . . ?
C12 C11 C10 120.2(11) . . ?
C11 C12 C13 120.9(11) . . ?
C14 C13 C12 119.1(11) . . ?
N1 C14 C13 120.0(10) . . ?
C16 C15 S6 110.1(8) . . ?
N2 C16 C17 118.6(11) . . ?
N2 C16 C15 118.1(11) . . ?
C17 C16 C15 123.2(11) . . ?
F3 C21 F1 105.9(10) . . ?
F3 C21 F2 105.8(10) . . ?
F1 C21 F2 105.0(10) . . ?
F3 C21 C22 116.3(9) . . ?
F1 C21 C22 111.2(9) . . ?
F2 C21 C22 111.9(9) . . ?
O3 C22 C23 128.8(10) . . ?
O3 C22 C21 113.9(9) . . ?
C23 C22 C21 117.3(9) . . ?
C22 C23 C24 121.3(10) . . ?
O4 C24 C23 124.7(10) . . ?
O4 C24 C25A 116.3(9) . . ?
C23 C24 C25A 119.1(9) . . ?
F6 C29 F5 107.5(9) . . ?
F6 C29 F4 105.5(8) . . ?
F5 C29 F4 105.0(9) . . ?
F6 C29 C30 112.9(9) . . ?
F5 C29 C30 115.1(9) . . ?
F4 C29 C30 110.1(9) . . ?
O5 C30 C31 128.1(9) . . ?
O5 C30 C29 113.5(9) . . ?
C31 C30 C29 118.3(10) . . ?
C30 C31 C32 122.9(10) . . ?
O6 C32 C31 123.0(10) . . ?
O6 C32 C33A 115.0(9) . . ?
C31 C32 C33A 122.0(10) . . ?
O1 N1 C14 119.4(9) . . ?
O1 N1 C10 118.6(9) . . ?
C14 N1 C10 122.0(9) . . ?
O2 N2 C16 119.8(9) . . ?
O2 N2 C20 118.7(9) . . ?
C16 N2 C20 121.5(10) . . ?
N1 O1 Dy1 128.0(6) . . ?
N2 O2 Dy1 137.5(6) . . ?
C22 O3 Dy1 132.8(6) . . ?
C24 O4 Dy1 138.4(7) . . ?
C30 O5 Dy1 130.3(6) . . ?
C32 O6 Dy1 136.5(7) . . ?
C38 O7 Dy1 130.8(7) . . ?
C3 O10 C2 109.4(9) . . ?
C4 O9 C1 110.0(9) . . ?
C5 S1 C4 92.2(6) . . ?
C3 S2 C5 92.9(6) . . ?
C6 S3 C8 94.7(6) . . ?
C7 S4 C6 95.3(5) . . ?
C7 S5 C9 102.9(6) . . ?
C8 S6 C15 97.7(6) . . ?
O6 Dy1 O1 147.4(3) . . ?
O6 Dy1 O5 72.3(2) . . ?
O1 Dy1 O5 80.6(2) . . ?
O6 Dy1 O2 138.7(2) . . ?
O1 Dy1 O2 71.4(2) . . ?
O5 Dy1 O2 148.4(2) . . ?
O6 Dy1 O8 79.8(3) . . ?
O1 Dy1 O8 74.8(2) . . ?
O5 Dy1 O8 72.3(3) . . ?
O2 Dy1 O8 112.8(3) . . ?
O6 Dy1 O7 73.9(3) . . ?
O1 Dy1 O7 115.9(3) . . ?
O5 Dy1 O7 134.1(2) . . ?
O2 Dy1 O7 73.5(2) . . ?
O8 Dy1 O7 71.9(2) . . ?
O6 Dy1 O4 71.5(3) . . ?
O1 Dy1 O4 138.2(3) . . ?
O5 Dy1 O4 114.1(3) . . ?
O2 Dy1 O4 79.8(3) . . ?
O8 Dy1 O4 145.9(2) . . ?
O7 Dy1 O4 82.7(2) . . ?
O6 Dy1 O3 114.9(3) . . ?
O1 Dy1 O3 75.2(2) . . ?
O5 Dy1 O3 77.5(2) . . ?
O2 Dy1 O3 81.2(3) . . ?
O8 Dy1 O3 140.2(2) . . ?
O7 Dy1 O3 146.2(2) . . ?
O4 Dy1 O3 70.9(2) . . ?
Cl2 C45 Cl1 116.6(11) . . ?
Cl3 C46 Cl4 118.4(19) . . ?
N2 C20 C19 120.1(11) . . ?
C18 C19 C20 119.0(11) . . ?
C16 C17 C18 121.2(12) . . ?
C19 C18 C17 119.3(12) . . ?
C40 O8 Dy1 134.8(6) . . ?
O7 C38 C39 129.5(10) . . ?
O7 C38 C37 113.7(10) . . ?
C39 C38 C37 116.8(10) . . ?
C41 C42 C44 109.4(10) . . ?
C38 C39 C40 122.2(10) . . ?
O8 C40 C39 123.6(10) . . ?
O8 C40 C41 115.5(9) . . ?
C39 C40 C41 120.9(10) . . ?
C42 C41 C40 125.0(9) . . ?
C42 C41 S9 111.9(8) . . ?
C40 C41 S9 123.0(8) . . ?
F8 C37 F7 107.5(8) . . ?
F8 C37 F9 106.3(9) . . ?
F7 C37 F9 106.3(9) . . ?
F8 C37 C38 115.9(9) . . ?
F7 C37 C38 110.4(9) . . ?
F9 C37 C38 110.0(9) . . ?
C43 S9 C41 91.4(6) . . ?
C44 C43 S9 112.2(10) . . ?
C43 C44 C42 115.0(11) . . ?
C34A C33A C32 132.7(10) . . ?
C34A C33A S8A 109.1(9) . . ?
C32 C33A S8A 118.1(7) . . ?
C33A C34A C35A 115.4(15) . . ?
C36A C35A C34A 107.2(12) . . ?
C35A C36A S8A 117.3(7) . . ?
C36A S8A C33A 90.8(6) . . ?
C26A C25A C24 129.3(15) . . ?
C26A C25A S7A 111.9(13) . . ?
C24 C25A S7A 118.0(7) . . ?
C25A C26A C27A 108(3) . . ?
C28A C27A C26A 107.3(17) . . ?
C27A C28A S7A 119.9(8) . . ?
C28A S7A C25A 90.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         2.307
_refine_diff_density_min         -2.705
_refine_diff_density_rms         0.270
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_import-ks22-2
_database_code_depnum_ccdc_archive 'CCDC 1407105'
_audit_update_record             
;
2015-06-16 deposited with the CCDC.
2015-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H32 Cl4 F9 N2 O10 S9 Yb'
_chemical_formula_weight         1547.12

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'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.4473(3)
_cell_length_b                   12.0946(4)
_cell_length_c                   23.9969(7)
_cell_angle_alpha                76.5010(10)
_cell_angle_beta                 86.0280(10)
_cell_angle_gamma                74.7470(10)
_cell_volume                     2844.42(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9848
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.45

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1530
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5769
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39778
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         0.87
_diffrn_reflns_theta_max         27.50
_reflns_number_total             12653
_reflns_number_gt                11826
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0567P)²+10.8149P] 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_number_reflns         12653
_refine_ls_number_parameters     732
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.1187
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_restrained_S_all      1.191
_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
C1 C 0.7778(6) 0.4436(5) -0.2829(2) 0.0303(11) Uani 1 1 d . . .
H1A H 0.7737 0.3742 -0.2957 0.036 Uiso 1 1 calc R . .
H1B H 0.8130 0.4944 -0.3142 0.036 Uiso 1 1 calc R . .
C2 C 0.6402(6) 0.5073(5) -0.2677(2) 0.0332(12) Uani 1 1 d . . .
H2A H 0.6443 0.5774 -0.2555 0.040 Uiso 1 1 calc R . .
H2B H 0.5846 0.5318 -0.3013 0.040 Uiso 1 1 calc R . .
C3 C 0.6713(5) 0.3769(4) -0.1807(2) 0.0232(9) Uani 1 1 d . . .
C4 C 0.8015(5) 0.3658(4) -0.1856(2) 0.0235(9) Uani 1 1 d . . .
C5 C 0.7652(5) 0.2687(5) -0.0818(2) 0.0260(10) Uani 1 1 d . . .
C6 C 0.7750(5) 0.2304(5) -0.0247(2) 0.0271(10) Uani 1 1 d . . .
C7 C 0.8590(5) 0.1785(4) 0.0799(2) 0.0251(10) Uani 1 1 d . . .
C8 C 0.7253(5) 0.2051(4) 0.0845(2) 0.0241(9) Uani 1 1 d . . .
C9 C 0.9399(5) 0.0181(4) 0.1828(2) 0.0227(9) Uani 1 1 d . . .
H9A H 0.8478 0.0355 0.1952 0.027 Uiso 1 1 calc R . .
H9B H 0.9555 -0.0459 0.1631 0.027 Uiso 1 1 calc R . .
C10 C 1.0291(4) -0.0164(4) 0.23342(19) 0.0191(8) Uani 1 1 d . . .
C11 C 1.1427(5) -0.1083(4) 0.2412(2) 0.0244(10) Uani 1 1 d . . .
H11 H 1.1683 -0.1520 0.2133 0.029 Uiso 1 1 calc R . .
C12 C 1.2188(5) -0.1361(4) 0.2899(2) 0.0273(10) Uani 1 1 d . . .
H12 H 1.2934 -0.1995 0.2954 0.033 Uiso 1 1 calc R . .
C13 C 1.1823(5) -0.0682(4) 0.3304(2) 0.0244(10) Uani 1 1 d . . .
H13 H 1.2328 -0.0851 0.3632 0.029 Uiso 1 1 calc R . .
C14 C 1.0710(4) 0.0242(4) 0.32168(19) 0.0196(9) Uani 1 1 d . . .
H14 H 1.0467 0.0706 0.3485 0.023 Uiso 1 1 calc R . .
C15 C 0.5961(5) 0.3713(4) 0.1445(2) 0.0240(9) Uani 1 1 d . . .
H15A H 0.5599 0.4158 0.1075 0.029 Uiso 1 1 calc R . .
H15B H 0.5311 0.3917 0.1738 0.029 Uiso 1 1 calc R . .
C16 C 0.7204(5) 0.4016(4) 0.1542(2) 0.0216(9) Uani 1 1 d . . .
C17 C 0.7947(5) 0.4529(5) 0.1103(2) 0.0289(10) Uani 1 1 d . . .
H17 H 0.7629 0.4758 0.0730 0.035 Uiso 1 1 calc R . .
C18 C 0.9146(6) 0.4701(5) 0.1213(2) 0.0319(11) Uani 1 1 d . . .
H18 H 0.9634 0.5052 0.0918 0.038 Uiso 1 1 calc R . .
C19 C 0.9616(5) 0.4344(4) 0.1770(2) 0.0263(10) Uani 1 1 d . . .
H19 H 1.0437 0.4433 0.1851 0.032 Uiso 1 1 calc R . .
C20 C 0.8860(5) 0.3857(4) 0.2203(2) 0.0213(9) Uani 1 1 d . . .
H20 H 0.9173 0.3615 0.2577 0.026 Uiso 1 1 calc R . .
C21 C 0.9543(5) 0.3614(4) 0.3933(2) 0.0234(9) Uani 1 1 d . . .
C22 C 0.8243(4) 0.3329(4) 0.38294(18) 0.0173(8) Uani 1 1 d . . .
C23 C 0.7075(5) 0.4060(4) 0.3970(2) 0.0215(9) Uani 1 1 d . A .
H23 H 0.7099 0.4711 0.4108 0.026 Uiso 1 1 calc R . .
C24 C 0.5838(4) 0.3828(4) 0.39054(18) 0.0183(8) Uani 1 1 d . . .
C29 C 0.9201(5) -0.1974(4) 0.4208(2) 0.0240(9) Uani 1 1 d . . .
C30 C 0.7981(4) -0.0927(4) 0.40654(19) 0.0191(9) Uani 1 1 d . . .
C31 C 0.6761(5) -0.1124(4) 0.4240(2) 0.0211(9) Uani 1 1 d . B .
H31 H 0.6703 -0.1875 0.4428 0.025 Uiso 1 1 calc R . .
C32 C 0.5590(4) -0.0187(4) 0.41347(18) 0.0177(8) Uani 1 1 d . . .
C37 C 0.2975(4) 0.2049(4) 0.2372(2) 0.0222(9) Uani 1 1 d . . .
C38 C 0.4396(4) 0.1405(4) 0.25802(19) 0.0192(9) Uani 1 1 d . . .
C39 C 0.4830(4) 0.0226(4) 0.2582(2) 0.0217(9) Uani 1 1 d . . .
H39 H 0.4228 -0.0168 0.2510 0.026 Uiso 1 1 calc R . .
C40 C 0.6173(4) -0.0402(4) 0.26914(18) 0.0177(8) Uani 1 1 d . . .
C41 C 0.6630(5) -0.1631(4) 0.2636(2) 0.0221(9) Uani 1 1 d . . .
C42 C 0.7974(5) -0.2297(4) 0.2688(2) 0.0258(10) Uani 1 1 d . . .
H42 H 0.8692 -0.2023 0.2751 0.031 Uiso 1 1 calc R . .
C43 C 0.8038(5) -0.3468(5) 0.2627(3) 0.0368(13) Uani 1 1 d . . .
H43 H 0.8831 -0.4049 0.2645 0.044 Uiso 1 1 calc R . .
C44 C 0.6844(6) -0.3656(5) 0.2540(3) 0.0414(15) Uani 1 1 d . . .
H44 H 0.6736 -0.4370 0.2497 0.050 Uiso 1 1 calc R . .
C45 C 0.7330(8) 0.6848(7) -0.0656(3) 0.0565(18) Uani 1 1 d . . .
H45A H 0.7966 0.7040 -0.0953 0.068 Uiso 1 1 calc R . .
H45B H 0.6464 0.7355 -0.0778 0.068 Uiso 1 1 calc R . .
C46 C 0.599(2) 0.9122(17) 0.0670(13) 0.225(13) Uani 1 1 d . . .
H46A H 0.5873 0.8377 0.0625 0.271 Uiso 1 1 calc R . .
H46B H 0.6135 0.9579 0.0293 0.271 Uiso 1 1 calc R . .
N1 N 0.9964(3) 0.0483(3) 0.27431(15) 0.0152(7) Uani 1 1 d . . .
N2 N 0.7662(4) 0.3727(3) 0.20882(16) 0.0183(7) Uani 1 1 d . . .
O1 O 0.8900(3) 0.1387(3) 0.26652(13) 0.0175(6) Uani 1 1 d . A .
O2 O 0.6894(3) 0.3351(3) 0.25148(13) 0.0207(6) Uani 1 1 d . A .
O3 O 0.8428(3) 0.2416(3) 0.36356(13) 0.0186(6) Uani 1 1 d . A .
O4 O 0.5695(3) 0.3034(3) 0.36794(13) 0.0192(6) Uani 1 1 d . A .
O5 O 0.8267(3) 0.0011(3) 0.38007(13) 0.0178(6) Uani 1 1 d . A .
O6 O 0.5565(3) 0.0812(3) 0.38242(13) 0.0190(6) Uani 1 1 d . A .
O7 O 0.5014(3) 0.2079(3) 0.27102(13) 0.0186(6) Uani 1 1 d . A .
O8 O 0.7037(3) 0.0049(3) 0.28228(13) 0.0188(6) Uani 1 1 d . A .
O9 O 0.8648(4) 0.4093(4) -0.23439(15) 0.0322(8) Uani 1 1 d . . .
O10 O 0.5815(4) 0.4342(3) -0.22249(15) 0.0287(8) Uani 1 1 d . . .
F1 F 1.0332(4) 0.2726(4) 0.42835(19) 0.0554(11) Uani 1 1 d . . .
F2 F 1.0222(4) 0.3811(4) 0.34474(16) 0.0512(10) Uani 1 1 d . . .
F3 F 0.9395(4) 0.4540(4) 0.4156(2) 0.0596(12) Uani 1 1 d . . .
F4 F 0.8947(3) -0.2947(3) 0.45375(16) 0.0400(8) Uani 1 1 d . . .
F5 F 0.9795(3) -0.2266(3) 0.37300(14) 0.0357(7) Uani 1 1 d . . .
F6 F 1.0122(3) -0.1712(3) 0.44814(14) 0.0337(7) Uani 1 1 d . . .
F7 F 0.2358(3) 0.1406(3) 0.21622(15) 0.0358(7) Uani 1 1 d . . .
F8 F 0.2984(3) 0.3007(3) 0.19552(13) 0.0326(7) Uani 1 1 d . . .
F9 F 0.2210(3) 0.2431(3) 0.27948(14) 0.0354(7) Uani 1 1 d . . .
S1 S 0.90323(12) 0.27973(12) -0.12765(5) 0.0274(3) Uani 1 1 d . . .
S2 S 0.60969(14) 0.30892(14) -0.11545(5) 0.0333(3) Uani 1 1 d . . .
S3 S 0.63651(13) 0.22859(13) 0.02101(5) 0.0316(3) Uani 1 1 d . . .
S4 S 0.92763(13) 0.17363(14) 0.01132(5) 0.0342(3) Uani 1 1 d . . .
S5 S 0.97533(12) 0.14898(12) 0.13419(5) 0.0269(3) Uani 1 1 d . . .
S6 S 0.63061(12) 0.21282(11) 0.14726(5) 0.0234(2) Uani 1 1 d . . .
S9 S 0.55799(14) -0.24369(13) 0.25194(8) 0.0423(4) Uani 1 1 d . . .
Yb1 Yb 0.699046(17) 0.164779(15) 0.320662(7) 0.01378(6) Uani 1 1 d . . .
Cl1 Cl 0.7726(6) 0.7133(3) -0.00577(14) 0.165(2) Uani 1 1 d . . .
Cl2 Cl 0.7290(2) 0.53735(18) -0.05963(9) 0.0649(5) Uani 1 1 d . . .
Cl3 Cl 0.7193(9) 0.8897(7) 0.1044(3) 0.240(4) Uani 1 1 d . . .
Cl4 Cl 0.4399(10) 0.9952(4) 0.1000(3) 0.233(4) Uani 1 1 d . . .
C25A C 0.4631(5) 0.4539(4) 0.4129(2) 0.0223(9) Uani 0.536(4) 1 d PD A 1
C26A C 0.4366(15) 0.5609(13) 0.4323(8) 0.039(4) Uani 0.536(4) 1 d PD A 1
H26A H 0.5016 0.5988 0.4355 0.046 Uiso 0.536(4) 1 calc PR A 1
C27A C 0.2988(6) 0.6040(6) 0.4465(3) 0.0403(10) Uani 0.536(4) 1 d PD A 1
H27A H 0.2584 0.6776 0.4537 0.048 Uiso 0.536(4) 1 calc PR A 1
C28A C 0.2404(6) 0.5174(6) 0.4473(3) 0.0403(10) Uani 0.536(4) 1 d PD A 1
H28A H 0.1522 0.5254 0.4588 0.048 Uiso 0.536(4) 1 calc PR A 1
S7A S 0.3252(3) 0.3972(3) 0.4279(2) 0.0285(7) Uani 0.536(4) 1 d PD A 1
C25B C 0.4631(5) 0.4539(4) 0.4129(2) 0.0223(9) Uani 0.464(4) 1 d PD A 2
C26B C 0.3387(17) 0.4301(14) 0.4249(10) 0.039(4) Uani 0.464(4) 1 d PD A 2
H26B H 0.3207 0.3625 0.4189 0.046 Uiso 0.464(4) 1 calc PR A 2
C27B C 0.2404(6) 0.5174(6) 0.4473(3) 0.0403(10) Uani 0.464(4) 1 d PD A 2
H27B H 0.1548 0.5144 0.4597 0.048 Uiso 0.464(4) 1 calc PR A 2
C28B C 0.2988(6) 0.6040(6) 0.4465(3) 0.0403(10) Uani 0.464(4) 1 d PD A 2
H28B H 0.2522 0.6710 0.4588 0.048 Uiso 0.464(4) 1 calc PR A 2
S7B S 0.4533(4) 0.5918(4) 0.4238(2) 0.0285(7) Uani 0.464(4) 1 d PD A 2
C33A C 0.4322(4) -0.0348(4) 0.44022(18) 0.0185(8) Uani 0.752(5) 1 d PD B 1
C34A C 0.3989(9) -0.1274(10) 0.4810(5) 0.030(2) Uani 0.752(5) 1 d PD B 1
H34A H 0.4606 -0.1969 0.4966 0.036 Uiso 0.752(5) 1 calc PR B 1
C35A C 0.2614(5) -0.1043(5) 0.4959(2) 0.0288(7) Uani 0.752(5) 1 d PD B 1
H35A H 0.2206 -0.1561 0.5209 0.035 Uiso 0.752(5) 1 calc PR B 1
C36A C 0.2004(5) 0.0058(5) 0.4676(2) 0.0288(7) Uani 0.752(5) 1 d PD B 1
H36A H 0.1100 0.0377 0.4718 0.035 Uiso 0.752(5) 1 calc PR B 1
S8A S 0.29606(18) 0.08111(16) 0.42480(9) 0.0225(5) Uani 0.752(5) 1 d PD B 1
C33B C 0.4322(4) -0.0348(4) 0.44022(18) 0.0185(8) Uani 0.248(5) 1 d PD B 2
C34B C 0.3057(19) 0.046(2) 0.4326(13) 0.030(2) Uani 0.248(5) 1 d PD B 2
H34B H 0.2911 0.1189 0.4072 0.036 Uiso 0.248(5) 1 calc PR B 2
C35B C 0.2004(5) 0.0058(5) 0.4676(2) 0.0288(7) Uani 0.248(5) 1 d PD B 2
H35B H 0.1119 0.0462 0.4700 0.035 Uiso 0.248(5) 1 calc PR B 2
C36B C 0.2614(5) -0.1043(5) 0.4959(2) 0.0288(7) Uani 0.248(5) 1 d PD B 2
H36B H 0.2130 -0.1489 0.5212 0.035 Uiso 0.248(5) 1 calc PR B 2
S8B S 0.4169(8) -0.1586(7) 0.4861(4) 0.0225(5) Uani 0.248(5) 1 d PD B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O9 1.441(6) . ?
C1 C2 1.507(8) . ?
C2 O10 1.442(6) . ?
C3 C4 1.331(7) . ?
C3 O10 1.353(6) . ?
C3 S2 1.755(5) . ?
C4 O9 1.368(6) . ?
C4 S1 1.760(5) . ?
C5 C6 1.341(7) . ?
C5 S2 1.764(5) . ?
C5 S1 1.766(5) . ?
C6 S3 1.756(5) . ?
C6 S4 1.761(5) . ?
C7 C8 1.350(7) . ?
C7 S5 1.754(5) . ?
C7 S4 1.756(5) . ?
C8 S6 1.752(5) . ?
C8 S3 1.765(5) . ?
C9 C10 1.495(6) . ?
C9 S5 1.841(5) . ?
C10 N1 1.365(5) . ?
C10 C11 1.385(6) . ?
C11 C12 1.384(7) . ?
C12 C13 1.385(7) . ?
C13 C14 1.374(6) . ?
C14 N1 1.354(6) . ?
C15 C16 1.485(7) . ?
C15 S6 1.841(5) . ?
C16 N2 1.362(6) . ?
C16 C17 1.389(7) . ?
C17 C18 1.375(8) . ?
C18 C19 1.388(8) . ?
C19 C20 1.377(7) . ?
C20 N2 1.356(6) . ?
C21 F3 1.320(6) . ?
C21 F1 1.324(6) . ?
C21 F2 1.328(6) . ?
C21 C22 1.535(6) . ?
C22 O3 1.260(5) . ?
C22 C23 1.378(6) . ?
C23 C24 1.418(6) . ?
C24 O4 1.253(5) . ?
C24 C25A 1.472(6) . ?
C29 F4 1.335(6) . ?
C29 F6 1.341(6) . ?
C29 F5 1.343(6) . ?
C29 C30 1.535(6) . ?
C30 O5 1.263(5) . ?
C30 C31 1.377(6) . ?
C31 C32 1.424(6) . ?
C32 O6 1.257(5) . ?
C32 C33A 1.471(6) . ?
C37 F7 1.329(5) . ?
C37 F9 1.339(6) . ?
C37 F8 1.344(6) . ?
C37 C38 1.541(6) . ?
C38 O7 1.265(5) . ?
C38 C39 1.378(6) . ?
C39 C40 1.418(6) . ?
C40 O8 1.262(5) . ?
C40 C41 1.471(6) . ?
C41 C42 1.421(7) . ?
C41 S9 1.722(5) . ?
C42 C43 1.443(7) . ?
C43 C44 1.363(8) . ?
C44 S9 1.694(6) . ?
C45 Cl1 1.657(8) . ?
C45 Cl2 1.766(8) . ?
C46 Cl3 1.53(2) . ?
C46 Cl4 1.92(2) . ?
N1 O1 1.327(5) . ?
N2 O2 1.326(5) . ?
O1 Yb1 2.295(3) . ?
O2 Yb1 2.308(3) . ?
O3 Yb1 2.361(3) . ?
O4 Yb1 2.326(3) . ?
O5 Yb1 2.299(3) . ?
O6 Yb1 2.286(3) . ?
O7 Yb1 2.332(3) . ?
O8 Yb1 2.316(3) . ?
C25A C26A 1.430(15) . ?
C25A S7A 1.735(6) . ?
C26A C27A 1.442(14) . ?
C27A C28A 1.340(9) . ?
C28A S7A 1.642(6) . ?
C33A C34A 1.406(12) . ?
C33A S8A 1.705(5) . ?
C34A C35A 1.426(11) . ?
C35A C36A 1.353(8) . ?
C36A S8A 1.669(5) . ?

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
O9 C1 C2 111.0(4) . . ?
O10 C2 C1 111.7(4) . . ?
C4 C3 O10 125.5(4) . . ?
C4 C3 S2 118.0(4) . . ?
O10 C3 S2 116.5(4) . . ?
C3 C4 O9 124.8(4) . . ?
C3 C4 S1 118.5(4) . . ?
O9 C4 S1 116.5(4) . . ?
C6 C5 S2 120.6(4) . . ?
C6 C5 S1 123.3(4) . . ?
S2 C5 S1 116.1(3) . . ?
C5 C6 S3 123.1(4) . . ?
C5 C6 S4 123.3(4) . . ?
S3 C6 S4 113.6(3) . . ?
C8 C7 S5 128.1(4) . . ?
C8 C7 S4 117.1(4) . . ?
S5 C7 S4 114.8(3) . . ?
C7 C8 S6 126.9(4) . . ?
C7 C8 S3 116.7(4) . . ?
S6 C8 S3 116.3(3) . . ?
C10 C9 S5 108.3(3) . . ?
N1 C10 C11 118.1(4) . . ?
N1 C10 C9 117.4(4) . . ?
C11 C10 C9 124.5(4) . . ?
C12 C11 C10 121.0(4) . . ?
C11 C12 C13 119.1(4) . . ?
C14 C13 C12 119.5(4) . . ?
N1 C14 C13 120.4(4) . . ?
C16 C15 S6 109.8(3) . . ?
N2 C16 C17 118.6(4) . . ?
N2 C16 C15 117.7(4) . . ?
C17 C16 C15 123.6(4) . . ?
C18 C17 C16 120.9(5) . . ?
C17 C18 C19 119.0(5) . . ?
C20 C19 C18 119.5(5) . . ?
N2 C20 C19 120.5(4) . . ?
F3 C21 F1 106.1(4) . . ?
F3 C21 F2 106.7(4) . . ?
F1 C21 F2 106.1(4) . . ?
F3 C21 C22 114.9(4) . . ?
F1 C21 C22 111.6(4) . . ?
F2 C21 C22 111.0(4) . . ?
O3 C22 C23 129.7(4) . . ?
O3 C22 C21 112.9(4) . . ?
C23 C22 C21 117.4(4) . . ?
C22 C23 C24 120.6(4) . . ?
O4 C24 C23 124.5(4) . . ?
O4 C24 C25A 116.7(4) . . ?
C23 C24 C25A 118.8(4) . . ?
F4 C29 F6 106.6(4) . . ?
F4 C29 F5 106.8(4) . . ?
F6 C29 F5 105.9(4) . . ?
F4 C29 C30 114.6(4) . . ?
F6 C29 C30 111.3(4) . . ?
F5 C29 C30 111.1(4) . . ?
O5 C30 C31 129.5(4) . . ?
O5 C30 C29 113.2(4) . . ?
C31 C30 C29 117.3(4) . . ?
C30 C31 C32 120.4(4) . . ?
O6 C32 C31 123.5(4) . . ?
O6 C32 C33A 116.2(4) . . ?
C31 C32 C33A 120.3(4) . . ?
F7 C37 F9 107.2(4) . . ?
F7 C37 F8 106.7(4) . . ?
F9 C37 F8 106.4(4) . . ?
F7 C37 C38 114.5(4) . . ?
F9 C37 C38 111.3(4) . . ?
F8 C37 C38 110.4(4) . . ?
O7 C38 C39 129.4(4) . . ?
O7 C38 C37 112.9(4) . . ?
C39 C38 C37 117.6(4) . . ?
C38 C39 C40 121.6(4) . . ?
O8 C40 C39 123.2(4) . . ?
O8 C40 C41 116.6(4) . . ?
C39 C40 C41 120.2(4) . . ?
C42 C41 C40 124.2(4) . . ?
C42 C41 S9 112.4(3) . . ?
C40 C41 S9 123.5(3) . . ?
C41 C42 C43 108.6(4) . . ?
C44 C43 C42 114.5(5) . . ?
C43 C44 S9 112.2(4) . . ?
Cl1 C45 Cl2 114.4(5) . . ?
Cl3 C46 Cl4 111.4(16) . . ?
O1 N1 C14 119.4(3) . . ?
O1 N1 C10 118.7(4) . . ?
C14 N1 C10 121.9(4) . . ?
O2 N2 C20 119.9(4) . . ?
O2 N2 C16 118.9(4) . . ?
C20 N2 C16 121.2(4) . . ?
N1 O1 Yb1 128.6(2) . . ?
N2 O2 Yb1 136.6(3) . . ?
C22 O3 Yb1 132.3(3) . . ?
C24 O4 Yb1 138.2(3) . . ?
C30 O5 Yb1 130.1(3) . . ?
C32 O6 Yb1 136.5(3) . . ?
C38 O7 Yb1 130.6(3) . . ?
C40 O8 Yb1 135.1(3) . . ?
C4 O9 C1 110.5(4) . . ?
C3 O10 C2 109.9(4) . . ?
C4 S1 C5 92.3(2) . . ?
C3 S2 C5 92.9(2) . . ?
C6 S3 C8 95.1(2) . . ?
C7 S4 C6 95.2(2) . . ?
C7 S5 C9 101.6(2) . . ?
C8 S6 C15 100.2(2) . . ?
C44 S9 C41 92.3(3) . . ?
O6 Yb1 O1 147.97(11) . . ?
O6 Yb1 O5 73.21(11) . . ?
O1 Yb1 O5 80.66(11) . . ?
O6 Yb1 O2 137.79(11) . . ?
O1 Yb1 O2 71.61(11) . . ?
O5 Yb1 O2 148.30(11) . . ?
O6 Yb1 O8 80.09(11) . . ?
O1 Yb1 O8 74.63(11) . . ?
O5 Yb1 O8 72.76(11) . . ?
O2 Yb1 O8 112.82(11) . . ?
O6 Yb1 O4 70.65(11) . . ?
O1 Yb1 O4 138.94(11) . . ?
O5 Yb1 O4 114.39(11) . . ?
O2 Yb1 O4 79.58(11) . . ?
O8 Yb1 O4 145.19(11) . . ?
O6 Yb1 O7 73.66(11) . . ?
O1 Yb1 O7 115.92(11) . . ?
O5 Yb1 O7 135.37(11) . . ?
O2 Yb1 O7 72.71(11) . . ?
O8 Yb1 O7 72.80(11) . . ?
O4 Yb1 O7 81.05(11) . . ?
O6 Yb1 O3 115.10(11) . . ?
O1 Yb1 O3 75.27(11) . . ?
O5 Yb1 O3 76.66(11) . . ?
O2 Yb1 O3 81.60(11) . . ?
O8 Yb1 O3 139.84(11) . . ?
O4 Yb1 O3 72.05(11) . . ?
O7 Yb1 O3 145.66(11) . . ?
C26A C25A C24 132.6(7) . . ?
C26A C25A S7A 108.3(7) . . ?
C24 C25A S7A 118.7(3) . . ?
C25A C26A C27A 113.2(12) . . ?
C28A C27A C26A 106.7(8) . . ?
C27A C28A S7A 119.7(5) . . ?
C28A S7A C25A 90.7(3) . . ?
C34A C33A C32 132.5(5) . . ?
C34A C33A S8A 109.9(5) . . ?
C32 C33A S8A 117.4(3) . . ?
C33A C34A C35A 113.5(8) . . ?
C36A C35A C34A 108.5(6) . . ?
C35A C36A S8A 116.4(4) . . ?
C36A S8A C33A 91.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         2.496
_refine_diff_density_min         -2.492
_refine_diff_density_rms         0.209
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_import-ks-edo-ttf-2pynoxide
_database_code_depnum_ccdc_archive 'CCDC 1407106'
_audit_update_record             
;
2015-06-16 deposited with the CCDC.
2015-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H16 N2 O5 S6'
_chemical_formula_weight         556.71

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/a

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

_cell_length_a                   13.2244(3)
_cell_length_b                   12.1843(4)
_cell_length_c                   15.3079(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.908(2)
_cell_angle_gamma                90.00
_cell_volume                     2347.06(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9997
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.103

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27589
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.10
_reflns_number_total             5151
_reflns_number_gt                3539
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0789P)²+0.9775P] 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_number_reflns         5151
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1519
_refine_ls_wR_factor_gt          0.1327
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
S6 S 0.45559(6) 0.99724(7) 0.66680(5) 0.0503(2) Uani 1 1 d . . .
S4 S 0.60193(7) 0.75252(7) 0.87301(6) 0.0535(2) Uani 1 1 d . . .
S1 S 0.81977(7) 0.74621(7) 1.04271(6) 0.0590(2) Uani 1 1 d . . .
S5 S 0.41827(6) 0.73333(7) 0.70076(6) 0.0513(2) Uani 1 1 d . . .
S2 S 0.85244(7) 0.98533(8) 1.01418(6) 0.0618(3) Uani 1 1 d . . .
S3 S 0.63888(7) 0.98677(7) 0.84241(6) 0.0594(2) Uani 1 1 d . . .
O3 O 0.9976(2) 0.7469(2) 1.18334(19) 0.0719(7) Uani 1 1 d . . .
O1 O 0.68519(17) 1.22345(18) 0.59818(17) 0.0584(6) Uani 1 1 d . . .
C9 C 0.6250(2) 1.0451(2) 0.59936(19) 0.0420(6) Uani 1 1 d . . .
N1 N 0.69179(18) 1.1192(2) 0.57872(17) 0.0461(6) Uani 1 1 d . . .
O2 O 0.15235(19) 0.8171(2) 0.63675(18) 0.0701(7) Uani 1 1 d . . .
O4 O 1.02833(19) 0.9799(2) 1.15644(18) 0.0745(7) Uani 1 1 d . . .
N2 N 0.2003(2) 0.8887(2) 0.70001(19) 0.0553(7) Uani 1 1 d . . .
C5 C 0.7745(2) 0.8667(3) 0.97858(19) 0.0471(7) Uani 1 1 d . . .
C4 C 0.9331(2) 0.8114(3) 1.1151(2) 0.0555(8) Uani 1 1 d . . .
C15 C 0.3244(3) 0.7424(3) 0.7687(2) 0.0552(8) Uani 1 1 d . . .
H15A H 0.2642 0.6945 0.7421 0.066 Uiso 1 1 calc R . .
H15B H 0.3594 0.7180 0.8310 0.066 Uiso 1 1 calc R . .
C14 C 0.5207(2) 0.8137(3) 0.77121(19) 0.0440(6) Uani 1 1 d . . .
C7 C 0.5379(2) 0.9197(2) 0.75754(19) 0.0433(6) Uani 1 1 d . . .
C12 C 0.7789(3) 0.9788(3) 0.5237(2) 0.0618(9) Uani 1 1 d . . .
H12 H 0.8316 0.9573 0.4987 0.074 Uiso 1 1 calc R . .
C8 C 0.5481(2) 1.0932(2) 0.6431(2) 0.0446(6) Uani 1 1 d . . .
H8A H 0.5077 1.1502 0.6032 0.053 Uiso 1 1 calc R . .
H8B H 0.5882 1.1278 0.7004 0.053 Uiso 1 1 calc R . .
C16 C 0.2863(2) 0.8569(3) 0.7702(2) 0.0511(7) Uani 1 1 d . . .
C17 C 0.3353(3) 0.9332(3) 0.8364(2) 0.0622(9) Uani 1 1 d . . .
H17 H 0.3923 0.9116 0.8862 0.075 Uiso 1 1 calc R . .
C11 C 0.7130(3) 0.9016(3) 0.5426(2) 0.0600(8) Uani 1 1 d . . .
H11 H 0.7202 0.8278 0.5302 0.072 Uiso 1 1 calc R . .
C10 C 0.6352(3) 0.9358(3) 0.5807(2) 0.0515(7) Uani 1 1 d . . .
H10 H 0.5897 0.8844 0.5936 0.062 Uiso 1 1 calc R . .
C3 C 0.9464(2) 0.9165(3) 1.1024(2) 0.0542(8) Uani 1 1 d . . .
C6 C 0.6844(2) 0.8679(3) 0.9082(2) 0.0479(7) Uani 1 1 d . . .
C13 C 0.7674(2) 1.0854(3) 0.5414(2) 0.0577(8) Uani 1 1 d . . .
H13 H 0.8121 1.1370 0.5277 0.069 Uiso 1 1 calc R . .
C20 C 0.1657(3) 0.9936(3) 0.6939(3) 0.0664(10) Uani 1 1 d . . .
H20 H 0.1066 1.0140 0.6455 0.080 Uiso 1 1 calc R . .
C19 C 0.2159(4) 1.0697(4) 0.7574(3) 0.0762(11) Uani 1 1 d . . .
H19 H 0.1919 1.1419 0.7514 0.091 Uiso 1 1 calc R . .
C18 C 0.3016(4) 1.0404(4) 0.8301(3) 0.0753(11) Uani 1 1 d . . .
H18 H 0.3361 1.0918 0.8741 0.090 Uiso 1 1 calc R . .
C1 C 1.0803(5) 0.8100(5) 1.2397(5) 0.150(3) Uani 1 1 d . . .
H1A H 1.0683 0.8138 1.2990 0.180 Uiso 1 1 calc R . .
H1B H 1.1448 0.7678 1.2486 0.180 Uiso 1 1 calc R . .
C2 C 1.1019(4) 0.9117(6) 1.2194(4) 0.153(3) Uani 1 1 d . . .
H2A H 1.1636 0.9066 1.1979 0.183 Uiso 1 1 calc R . .
H2B H 1.1246 0.9516 1.2770 0.183 Uiso 1 1 calc R . .
O1W O 0.99811(19) 0.8469(2) 0.46763(18) 0.0724(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S6 C7 1.754(3) . ?
S6 C8 1.807(3) . ?
S4 C6 1.759(3) . ?
S4 C14 1.763(3) . ?
S1 C4 1.756(3) . ?
S1 C5 1.765(3) . ?
S5 C14 1.749(3) . ?
S5 C15 1.852(3) . ?
S2 C3 1.743(3) . ?
S2 C5 1.761(3) . ?
S3 C7 1.752(3) . ?
S3 C6 1.761(3) . ?
O3 C4 1.374(4) . ?
O3 C1 1.396(5) . ?
O1 N1 1.313(3) . ?
C9 N1 1.366(4) . ?
C9 C10 1.378(4) . ?
C9 C8 1.499(4) . ?
N1 C13 1.359(4) . ?
O2 N2 1.312(4) . ?
O4 C3 1.380(4) . ?
O4 C2 1.410(6) . ?
N2 C20 1.351(5) . ?
N2 C16 1.359(4) . ?
C5 C6 1.338(4) . ?
C4 C3 1.315(5) . ?
C15 C16 1.485(5) . ?
C14 C7 1.340(4) . ?
C12 C13 1.345(5) . ?
C12 C11 1.371(5) . ?
C16 C17 1.381(5) . ?
C17 C18 1.374(6) . ?
C11 C10 1.394(5) . ?
C20 C19 1.359(6) . ?
C19 C18 1.370(6) . ?
C1 C2 1.331(7) . ?

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
C7 S6 C8 102.34(14) . . ?
C6 S4 C14 94.87(14) . . ?
C4 S1 C5 93.00(16) . . ?
C14 S5 C15 98.41(15) . . ?
C3 S2 C5 93.15(15) . . ?
C7 S3 C6 95.12(14) . . ?
C4 O3 C1 109.9(3) . . ?
N1 C9 C10 118.7(3) . . ?
N1 C9 C8 114.9(3) . . ?
C10 C9 C8 126.4(3) . . ?
O1 N1 C13 119.8(3) . . ?
O1 N1 C9 119.6(2) . . ?
C13 N1 C9 120.5(3) . . ?
C3 O4 C2 109.3(3) . . ?
O2 N2 C20 120.1(3) . . ?
O2 N2 C16 119.4(3) . . ?
C20 N2 C16 120.5(3) . . ?
C6 C5 S2 122.1(2) . . ?
C6 C5 S1 121.5(2) . . ?
S2 C5 S1 116.38(16) . . ?
C3 C4 O3 126.1(3) . . ?
C3 C4 S1 118.3(2) . . ?
O3 C4 S1 115.5(3) . . ?
C16 C15 S5 110.7(2) . . ?
C7 C14 S5 125.5(2) . . ?
C7 C14 S4 117.3(2) . . ?
S5 C14 S4 117.03(17) . . ?
C14 C7 S3 117.5(2) . . ?
C14 C7 S6 123.3(2) . . ?
S3 C7 S6 118.82(17) . . ?
C13 C12 C11 120.1(3) . . ?
C9 C8 S6 115.6(2) . . ?
N2 C16 C17 118.6(3) . . ?
N2 C16 C15 117.4(3) . . ?
C17 C16 C15 124.0(3) . . ?
C18 C17 C16 121.3(4) . . ?
C12 C11 C10 118.8(3) . . ?
C9 C10 C11 120.5(3) . . ?
C4 C3 O4 124.9(3) . . ?
C4 C3 S2 119.2(2) . . ?
O4 C3 S2 115.9(3) . . ?
C5 C6 S4 123.5(2) . . ?
C5 C6 S3 122.2(3) . . ?
S4 C6 S3 114.28(16) . . ?
C12 C13 N1 121.4(3) . . ?
N2 C20 C19 121.0(4) . . ?
C20 C19 C18 120.2(4) . . ?
C19 C18 C17 118.3(4) . . ?
C2 C1 O3 123.5(5) . . ?
C1 C2 O4 123.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.064
