# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_y
_audit_block_doi                 10.5517/cc13qg3d
_database_code_depnum_ccdc_archive 'CCDC 1034473'
_audit_update_record             
;
2015-05-21 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H0 La O8 S2'
_chemical_formula_weight         631.28

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'
La La -0.2871 2.4523 '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   C2/c

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

_cell_length_a                   33.400(4)
_cell_length_b                   13.8787(19)
_cell_length_c                   13.5790(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.966(3)
_cell_angle_gamma                90.00
_cell_volume                     6081.0(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4026
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.01

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2424
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7640
_exptl_absorpt_correction_T_max  0.8209
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21624
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         26.67
_reflns_number_total             6316
_reflns_number_gt                4744
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.1166P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6316
_refine_ls_number_parameters     332
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0605
_refine_ls_wR_factor_ref         0.1751
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.006

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
La1 La 0.812078(4) 0.212598(11) 0.561368(11) 0.02077(4) Uani 1 1 d . . .
O1 O 0.76805(6) 0.17953(19) 0.68232(16) 0.0391(6) Uani 1 1 d . . .
O2 O 0.79333(6) 0.24808(17) 0.37414(15) 0.0318(6) Uani 1 1 d . . .
O3 O 0.73352(6) 0.14352(15) 0.46732(15) 0.0292(5) Uani 1 1 d . . .
O4 O 0.78787(6) 0.05402(16) 0.46750(18) 0.0368(6) Uani 1 1 d . A .
O5 O 0.86644(6) 0.32911(17) 0.52088(18) 0.0440(6) Uani 1 1 d . A .
O6 O 0.88019(6) 0.17395(19) 0.51709(18) 0.0448(7) Uani 1 1 d . A .
O7 O 0.84781(9) 0.0809(2) 0.6772(2) 0.0617(9) Uani 1 1 d . . .
O8 O 0.84581(10) 0.2993(2) 0.72257(19) 0.0686(11) Uani 1 1 d D . .
C1 C 0.42611(2) 0.21684(7) 0.96648(6) 0.0332(9) Uani 1 1 d G . .
C2 C 0.45567(2) 0.28786(7) 0.96861(7) 0.0478(11) Uani 1 1 d G . .
C3 C 0.49127(2) 0.26642(6) 0.93794(7) 0.0507(11) Uani 1 1 d G . .
C4 C 0.49732(2) 0.17397(7) 0.90513(6) 0.0355(8) Uani 1 1 d G . .
C5 C 0.46776(2) 0.10295(7) 0.90300(7) 0.0391(9) Uani 1 1 d G . .
C6 C 0.43216(2) 0.12439(7) 0.93367(7) 0.0380(9) Uani 1 1 d G . .
C7 C 0.53665(2) 0.15092(7) 0.87572(7) 0.0332(8) Uani 1 1 d G . .
C8 C 0.56045(2) 0.22227(7) 0.84513(7) 0.0407(9) Uani 1 1 d G . .
C9 C 0.59837(2) 0.20177(8) 0.82653(7) 0.0407(9) Uani 1 1 d G . .
C10 C 0.61407(3) 0.10765(8) 0.83673(8) 0.0296(8) Uani 1 1 d G . .
C11 C 0.58999(3) 0.03437(8) 0.86093(9) 0.0336(8) Uani 1 1 d G . .
C12 C 0.55188(2) 0.05554(7) 0.88176(8) 0.0369(9) Uani 1 1 d G . .
C13 C 0.65639(3) 0.08990(9) 0.82510(9) 0.0263(7) Uani 1 1 d G . .
C14 C 0.67299(3) 0.14593(10) 0.76086(9) 0.0294(8) Uani 1 1 d G . .
C15 C 0.71407(3) 0.13567(11) 0.75604(10) 0.0275(7) Uani 1 1 d G . .
C16 C 0.73919(3) 0.06726(11) 0.81805(11) 0.0280(8) Uani 1 1 d G . .
C17 C 0.72259(3) 0.00772(10) 0.87922(11) 0.0268(7) Uani 1 1 d G . .
C18 C 0.68127(3) 0.01675(9) 0.88314(10) 0.0274(8) Uani 1 1 d G . .
C19 C 0.73097(9) 0.1940(2) 0.6816(2) 0.0301(8) Uani 1 1 d . . .
C20 C 0.74994(8) 0.0676(2) 0.4429(2) 0.0264(7) Uani 1 1 d . . .
C21 C 0.88851(9) 0.2617(3) 0.5045(3) 0.0351(9) Uani 1 1 d . . .
C22 C 0.8131(2) -0.0442(5) 0.6936(5) 0.1100(15) Uani 0.694(2) 1 d PDU A 1
C22' C 0.8122(3) -0.0844(10) 0.6734(13) 0.110(2) Uani 0.306(2) 1 d PDU A 2
S1 S 0.84120(6) 0.02561(14) 0.76452(14) 0.0851(5) Uani 0.694(2) 1 d PDU A 1
S1' S 0.85064(15) -0.0285(4) 0.6850(4) 0.0987(12) Uani 0.306(2) 1 d PDU A 2
S2 S 0.85670(11) 0.2963(3) 0.83016(19) 0.1102(10) Uani 0.50 1 d PDU A 1
S2' S 0.82653(12) 0.3258(3) 0.8153(2) 0.1287(12) Uani 0.50 1 d PDU A 2
C23 C 0.8757(3) -0.0455(7) 0.8225(8) 0.1522(18) Uani 0.694(2) 1 d PDU A 1
C23' C 0.8850(5) -0.0526(18) 0.7831(11) 0.151(2) Uani 0.306(2) 1 d PDU A 2
C24 C 0.90361(19) 0.2877(10) 0.8786(9) 0.2639(18) Uani 0.50 1 d PDU A 1
C24' C 0.8305(3) 0.2495(6) 0.8978(6) 0.150(4) Uani 0.50 1 d PDU A 2
C25 C 0.8508(3) 0.3983(5) 0.8833(7) 0.2612(18) Uani 0.50 1 d PDU A 1
C25' C 0.8689(4) 0.3832(14) 0.859(2) 0.2622(16) Uani 0.50 1 d PDU A 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
La1 O3 2.480(2) 7_656 ?
La1 O8 2.497(3) . ?
La1 O2 2.505(2) . ?
La1 O7 2.503(3) . ?
La1 O1 2.514(2) . ?
La1 O6 2.556(2) . ?
La1 O4 2.567(2) . ?
La1 O5 2.594(2) . ?
La1 O3 2.7756(19) . ?
La1 C21 2.932(3) . ?
La1 C20 3.037(3) . ?
La1 La1 4.1812(5) 7_656 ?
O1 C19 1.252(4) . ?
O2 C19 1.250(4) 7_656 ?
O3 C20 1.271(4) . ?
O3 La1 2.480(2) 7_656 ?
O4 C20 1.238(3) . ?
O5 C21 1.247(4) . ?
O6 C21 1.270(4) . ?
O7 S1 1.477(3) . ?
O7 S1' 1.524(6) . ?
O8 S2 1.412(4) . ?
O8 S2' 1.598(5) . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C1 C21 1.506(3) 8_456 ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C7 1.5028 . ?
C5 C6 1.3900 . ?
C7 C8 1.3984 . ?
C7 C12 1.4129 . ?
C8 C9 1.3836 . ?
C9 C10 1.4009 . ?
C10 C11 1.3876 . ?
C10 C13 1.4831 . ?
C11 C12 1.4045 . ?
C13 C14 1.3866 . ?
C13 C18 1.4156 . ?
C14 C15 1.3978 . ?
C15 C16 1.3963 . ?
C15 C19 1.513(3) . ?
C16 C17 1.3850 . ?
C17 C18 1.4004 . ?
C17 C20 1.506(3) 6_556 ?
C19 O2 1.249(4) 7_656 ?
C20 C17 1.506(4) 6 ?
C21 C1 1.506(3) 8 ?
C22 S1 1.510(7) . ?
C22' S1' 1.472(12) . ?
S1 C23 1.566(9) . ?
S1' C23' 1.553(13) . ?
S2 C24 1.539(7) . ?
S2 C25 1.624(8) . ?
S2' C24' 1.521(8) . ?
S2' C25' 1.599(13) . ?

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 La1 O8 82.50(8) 7_656 . ?
O3 La1 O2 72.54(7) 7_656 . ?
O8 La1 O2 137.14(9) . . ?
O3 La1 O7 149.32(8) 7_656 . ?
O8 La1 O7 76.53(9) . . ?
O2 La1 O7 137.28(9) . . ?
O3 La1 O1 79.08(7) 7_656 . ?
O8 La1 O1 73.91(9) . . ?
O2 La1 O1 131.60(7) . . ?
O7 La1 O1 73.78(9) . . ?
O3 La1 O6 132.83(8) 7_656 . ?
O8 La1 O6 94.58(10) . . ?
O2 La1 O6 78.87(7) . . ?
O7 La1 O6 71.68(9) . . ?
O1 La1 O6 145.28(7) . . ?
O3 La1 O4 120.69(6) 7_656 . ?
O8 La1 O4 149.46(8) . . ?
O2 La1 O4 72.57(8) . . ?
O7 La1 O4 73.97(8) . . ?
O1 La1 O4 90.32(8) . . ?
O6 La1 O4 83.60(7) . . ?
O3 La1 O5 84.25(7) 7_656 . ?
O8 La1 O5 72.75(9) . . ?
O2 La1 O5 70.59(7) . . ?
O7 La1 O5 110.00(8) . . ?
O1 La1 O5 144.28(8) . . ?
O6 La1 O5 50.70(8) . . ?
O4 La1 O5 125.25(8) . . ?
O3 La1 O3 74.73(7) 7_656 . ?
O8 La1 O3 136.78(9) . . ?
O2 La1 O3 69.03(7) . . ?
O7 La1 O3 106.11(8) . . ?
O1 La1 O3 66.08(6) . . ?
O6 La1 O3 127.76(7) . . ?
O4 La1 O3 48.42(6) . . ?
O5 La1 O3 138.42(6) . . ?
O3 La1 C21 108.22(9) 7_656 . ?
O8 La1 C21 83.84(10) . . ?
O2 La1 C21 72.14(8) . . ?
O7 La1 C21 91.66(10) . . ?
O1 La1 C21 155.61(8) . . ?
O6 La1 C21 25.61(9) . . ?
O4 La1 C21 104.61(9) . . ?
O5 La1 C21 25.13(9) . . ?
O3 La1 C21 137.98(8) . . ?
O3 La1 C20 98.19(7) 7_656 . ?
O8 La1 C20 151.13(9) . . ?
O2 La1 C20 68.59(8) . . ?
O7 La1 C20 89.93(8) . . ?
O1 La1 C20 77.88(8) . . ?
O6 La1 C20 105.33(8) . . ?
O4 La1 C20 23.69(7) . . ?
O5 La1 C20 136.12(8) . . ?
O3 La1 C20 24.74(7) . . ?
C21 La1 C20 122.46(9) . . ?
O3 La1 La1 39.82(4) 7_656 7_656 ?
O8 La1 La1 113.98(8) . 7_656 ?
O2 La1 La1 65.44(5) . 7_656 ?
O7 La1 La1 133.98(7) . 7_656 ?
O1 La1 La1 67.57(4) . 7_656 ?
O6 La1 La1 144.08(5) . 7_656 ?
O4 La1 La1 82.08(4) . 7_656 ?
O5 La1 La1 115.92(5) . 7_656 ?
O3 La1 La1 34.91(4) . 7_656 ?
C21 La1 La1 132.74(6) . 7_656 ?
C20 La1 La1 58.77(5) . 7_656 ?
C19 O1 La1 135.25(19) . . ?
C19 O2 La1 134.0(2) 7_656 . ?
C20 O3 La1 156.26(17) . 7_656 ?
C20 O3 La1 89.20(15) . . ?
La1 O3 La1 105.27(7) 7_656 . ?
C20 O4 La1 99.94(18) . . ?
C21 O5 La1 92.8(2) . . ?
C21 O6 La1 94.0(2) . . ?
S1 O7 S1' 56.3(2) . . ?
S1 O7 La1 137.58(19) . . ?
S1' O7 La1 141.5(2) . . ?
S2 O8 S2' 40.5(2) . . ?
S2 O8 La1 146.1(2) . . ?
S2' O8 La1 128.3(2) . . ?
C2 C1 C6 120.0 . . ?
C2 C1 C21 120.21(14) . 8_456 ?
C6 C1 C21 119.72(14) . 8_456 ?
C3 C2 C1 120.0 . . ?
C2 C3 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 C7 120.6 . . ?
C3 C4 C7 119.4 . . ?
C4 C5 C6 120.0 . . ?
C5 C6 C1 120.0 . . ?
C8 C7 C12 117.2 . . ?
C8 C7 C4 122.1 . . ?
C12 C7 C4 120.7 . . ?
C9 C8 C7 121.7 . . ?
C8 C9 C10 120.7 . . ?
C11 C10 C9 118.8 . . ?
C11 C10 C13 122.0 . . ?
C9 C10 C13 119.1 . . ?
C10 C11 C12 120.3 . . ?
C11 C12 C7 121.0 . . ?
C14 C13 C18 118.7 . . ?
C14 C13 C10 121.4 . . ?
C18 C13 C10 119.9 . . ?
C13 C14 C15 121.9 . . ?
C16 C15 C14 119.0 . . ?
C16 C15 C19 119.79(12) . . ?
C14 C15 C19 121.12(12) . . ?
C17 C16 C15 119.7 . . ?
C16 C17 C18 121.4 . . ?
C16 C17 C20 118.75(12) . 6_556 ?
C18 C17 C20 119.88(12) . 6_556 ?
C17 C18 C13 119.0 . . ?
O2 C19 O1 126.4(3) 7_656 . ?
O2 C19 C15 117.0(3) 7_656 . ?
O1 C19 C15 116.6(2) . . ?
O4 C20 O3 122.4(3) . . ?
O4 C20 C17 118.4(2) . 6 ?
O3 C20 C17 119.1(2) . 6 ?
O4 C20 La1 56.38(15) . . ?
O3 C20 La1 66.06(14) . . ?
C17 C20 La1 174.10(18) 6 . ?
O5 C21 O6 122.4(3) . . ?
O5 C21 C1 119.8(3) . 8 ?
O6 C21 C1 117.8(3) . 8 ?
O5 C21 La1 62.09(17) . . ?
O6 C21 La1 60.40(17) . . ?
C1 C21 La1 175.12(19) 8 . ?
O7 S1 C22 91.1(3) . . ?
O7 S1 C23 119.2(5) . . ?
C22 S1 C23 99.9(5) . . ?
C22' S1' O7 118.8(6) . . ?
C22' S1' C23' 114.1(11) . . ?
O7 S1' C23' 107.0(10) . . ?
O8 S2 C24 113.9(5) . . ?
O8 S2 C25 114.0(4) . . ?
C24 S2 C25 96.0(6) . . ?
C24' S2' O8 116.3(5) . . ?
C24' S2' C25' 99.9(9) . . ?
O8 S2' C25' 84.8(10) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.67
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         2.509
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.187


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.007 567 120 ' '
2 0.250 0.750 0.000 33 2 ' '
3 0.500 0.500 0.038 567 120 ' '
4 0.750 0.250 0.000 33 2 ' '
5 0.250 0.250 0.500 33 1 ' '
6 0.750 0.750 0.500 33 1 ' '
_platon_squeeze_details          
;
;
