# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc1ytjjt
_database_code_depnum_ccdc_archive 'CCDC 1811997'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8NJ01008K 2018
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H23 O5 S Sb W'
_chemical_formula_sum            'C29 H23 O5 S Sb W'
_chemical_formula_weight         789.13

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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.355(8)
_cell_length_b                   28.23(2)
_cell_length_c                   10.896(8)
_cell_angle_alpha                90
_cell_angle_beta                 115.85(3)
_cell_angle_gamma                90
_cell_volume                     2866(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9473
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      30.46

_exptl_crystal_description       block
_exptl_crystal_colour            bronze
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.178
_exptl_absorpt_coefficient_mu    5.061
_shelx_estimated_absorpt_T_min   0.227
_shelx_estimated_absorpt_T_max   0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5833
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\ms micro focus'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83717
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.199
_diffrn_reflns_theta_max         25.252
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5199
_reflns_number_gt                5145
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXTS-2014/15 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXTL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    
; ORTEP-3 for Windows (Farrugia, 1997),
 Mercury (Macrae et al., 2008)
_computing_publication_material   'SHELXL-2014'
  
_refine_special_details
 The thiophenyl and ether moieties attached to the carbene carbon atom are 
 observed in both possible orientations, in a ratio of approximately 0.79 to 0.21. 
 In addition, the ethyl carbon atoms are also disordered. The quality of the 
 data did not allow the modelling of all the atoms in the two orientations, 
 and the anisotropic displacement parameters of some atoms were restrained 
 during the refinement. In addition, the C-C bond lengths in the ether substituent 
 were also constrained during the refinement. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+56.7191P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5199
_refine_ls_number_parameters     314
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1213
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_restrained_S_all      1.326
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.19487(4) 0.41492(2) 0.68526(4) 0.02735(13) Uani 1 1 d . . . . .
Sb1 Sb 0.27221(6) 0.34865(2) 0.54307(6) 0.02114(15) Uani 1 1 d . . . . .
S1 S 0.6219(4) 0.43744(14) 1.1193(4) 0.0441(13) Uani 0.793(10) 1 d . . P A 1
S1A S 0.685(2) 0.4538(9) 0.942(3) 0.100(11) Uani 0.207(10) 1 d . . P A 2
O1 O -0.1199(9) 0.3936(3) 0.4529(10) 0.062(3) Uani 1 1 d . . . . .
O2 O 0.1583(9) 0.3231(3) 0.8388(9) 0.045(2) Uani 1 1 d . . . . .
O3 O 0.0557(11) 0.4803(3) 0.8263(10) 0.062(3) Uani 1 1 d . . . . .
O4 O 0.1915(12) 0.5031(3) 0.5023(9) 0.062(3) Uani 1 1 d . . . . .
O6 O 0.5283(9) 0.4467(3) 0.8370(10) 0.051(2) Uani 1 1 d . . . . .
C1 C -0.0053(13) 0.4012(4) 0.5361(12) 0.043(3) Uani 1 1 d . . . . .
C2 C 0.1774(11) 0.3571(4) 0.7890(11) 0.033(2) Uani 1 1 d . . . . .
C3 C 0.1079(12) 0.4566(4) 0.7763(12) 0.042(3) Uani 1 1 d . . . . .
C4 C 0.1988(13) 0.4713(4) 0.5689(12) 0.041(3) Uani 1 1 d . . . . .
C6 C 0.4089(13) 0.4316(4) 0.8464(13) 0.0422(11) Uani 1 1 d . . . . .
C7 C 0.4512(13) 0.4292(4) 0.9924(13) 0.0422(11) Uani 1 1 d . . . . .
C8 C 0.3620(13) 0.4189(4) 1.0554(13) 0.0422(11) Uani 1 1 d . . . . .
H8 H 0.262025 0.413026 1.006083 0.051 Uiso 1 1 calc R U . . .
C9 C 0.4351(13) 0.4181(4) 1.1994(13) 0.0422(11) Uani 1 1 d . . . . .
H9 H 0.390363 0.412261 1.257717 0.051 Uiso 1 1 calc R U . . .
C10 C 0.5695(13) 0.4261(4) 1.2411(13) 0.0422(11) Uani 1 1 d . . . . .
H10 H 0.634909 0.425708 1.335058 0.051 Uiso 1 1 calc R U . A 1
C11 C 0.5351(11) 0.4535(4) 0.7054(13) 0.0422(11) Uani 0.71(3) 1 d D . P A 3
H11A H 0.486441 0.482965 0.658976 0.051 Uiso 0.71(3) 1 calc R U P A 3
H11B H 0.494721 0.426136 0.643466 0.051 Uiso 0.71(3) 1 calc R U P A 3
C12 C 0.7011(13) 0.4568(6) 0.760(2) 0.0422(11) Uani 0.71(3) 1 d D . P A 3
H12A H 0.724667 0.469660 0.688786 0.063 Uiso 0.71(3) 1 calc R U P A 3
H12B H 0.743241 0.425176 0.786143 0.063 Uiso 0.71(3) 1 calc R U P A 3
H12C H 0.739940 0.477714 0.839910 0.063 Uiso 0.71(3) 1 calc R U P A 3
C11A C 0.5351(11) 0.4535(4) 0.7054(13) 0.0422(11) Uani 0.29(3) 1 d D . P A 4
H11C H 0.474088 0.481384 0.662584 0.051 Uiso 0.29(3) 1 calc R U P A 4
H11D H 0.484809 0.425880 0.648624 0.051 Uiso 0.29(3) 1 calc R U P A 4
C12A C 0.671(4) 0.4602(15) 0.684(6) 0.0422(11) Uani 0.29(3) 1 d D . P A 4
H12D H 0.655088 0.485561 0.617859 0.063 Uiso 0.29(3) 1 calc R U P A 4
H12E H 0.692796 0.430618 0.650002 0.063 Uiso 0.29(3) 1 calc R U P A 4
H12F H 0.751257 0.468587 0.771159 0.063 Uiso 0.29(3) 1 calc R U P A 4
C20 C 0.4881(10) 0.3299(3) 0.5840(10) 0.025(2) Uani 1 1 d . . . . .
C21 C 0.5865(12) 0.3245(4) 0.7204(12) 0.036(2) Uani 1 1 d . . . . .
H21 H 0.557856 0.329932 0.791031 0.044 Uiso 1 1 calc R U . . .
C22 C 0.7270(11) 0.3111(4) 0.7522(13) 0.040(3) Uani 1 1 d . . . . .
H22 H 0.794405 0.307327 0.844841 0.047 Uiso 1 1 calc R U . . .
C23 C 0.7682(12) 0.3032(4) 0.6502(15) 0.050(3) Uani 1 1 d . . . . .
H23 H 0.863725 0.293560 0.672663 0.061 Uiso 1 1 calc R U . . .
C24 C 0.6720(13) 0.3093(5) 0.5147(15) 0.051(3) Uani 1 1 d . . . . .
H24 H 0.702245 0.304434 0.444910 0.061 Uiso 1 1 calc R U . . .
C25 C 0.5303(12) 0.3226(4) 0.4806(12) 0.038(3) Uani 1 1 d . . . . .
H25 H 0.463679 0.326564 0.387844 0.046 Uiso 1 1 calc R U . . .
C30 C 0.1703(10) 0.3572(4) 0.3235(10) 0.026(2) Uani 1 1 d . . . . .
C31 C 0.1093(12) 0.4007(4) 0.2682(11) 0.035(2) Uani 1 1 d . . . . .
H31 H 0.114045 0.426388 0.326370 0.042 Uiso 1 1 calc R U . . .
C32 C 0.0421(14) 0.4063(4) 0.1287(11) 0.045(3) Uani 1 1 d . . . . .
H32 H 0.002589 0.436162 0.090949 0.054 Uiso 1 1 calc R U . . .
C33 C 0.0314(12) 0.3689(4) 0.0434(10) 0.034(2) Uani 1 1 d . . . . .
H33 H -0.016267 0.372962 -0.052692 0.041 Uiso 1 1 calc R U . . .
C34 C 0.0913(12) 0.3249(4) 0.0992(11) 0.034(2) Uani 1 1 d . . . . .
H34 H 0.085805 0.299147 0.040969 0.041 Uiso 1 1 calc R U . . .
C35 C 0.1587(11) 0.3190(4) 0.2399(11) 0.031(2) Uani 1 1 d . . . . .
H35 H 0.196552 0.289051 0.278354 0.037 Uiso 1 1 calc R U . . .
C40 C 0.1948(10) 0.2793(3) 0.5546(10) 0.025(2) Uani 1 1 d . . . . .
C41 C 0.2859(13) 0.2420(4) 0.6190(12) 0.038(3) Uani 1 1 d . . . . .
H41 H 0.386781 0.246069 0.654660 0.046 Uiso 1 1 calc R U . . .
C42 C 0.2288(16) 0.1978(4) 0.6318(14) 0.052(3) Uani 1 1 d . . . . .
H42 H 0.291082 0.172093 0.675554 0.062 Uiso 1 1 calc R U . . .
C43 C 0.0802(17) 0.1921(4) 0.5796(14) 0.056(4) Uani 1 1 d . . . . .
H43 H 0.040985 0.162631 0.588678 0.067 Uiso 1 1 calc R U . . .
C44 C -0.0079(14) 0.2290(5) 0.5158(15) 0.049(3) Uani 1 1 d . . . . .
H44 H -0.108819 0.224766 0.479608 0.059 Uiso 1 1 calc R U . . .
C45 C 0.0448(12) 0.2721(4) 0.5025(13) 0.041(3) Uani 1 1 d . . . . .
H45 H -0.019408 0.297299 0.458086 0.049 Uiso 1 1 calc R U . . .


_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
W1 C3 1.991(12) . ?
W1 C2 2.037(12) . ?
W1 C1 2.037(12) . ?
W1 C4 2.045(12) . ?
W1 C6 2.196(12) . ?
W1 Sb1 2.7609(15) . ?
Sb1 C40 2.140(10) . ?
Sb1 C20 2.146(10) . ?
Sb1 C30 2.167(10) . ?
S1 C10 1.668(13) . ?
S1 C7 1.720(13) . ?
S1A O6 1.53(2) . ?
O1 C1 1.157(14) . ?
O2 C2 1.162(14) . ?
O3 C3 1.137(14) . ?
O4 C4 1.136(14) . ?
O6 C6 1.354(14) . ?
O6 C11A 1.478(15) . ?
O6 C11 1.478(15) . ?
C6 C7 1.456(18) . ?
C7 C8 1.400(17) . ?
C8 C9 1.414(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.282(16) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.558(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C11A C12A 1.532(10) . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C20 C25 1.390(15) . ?
C20 C21 1.396(14) . ?
C21 C22 1.393(15) . ?
C21 H21 0.9500 . ?
C22 C23 1.371(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(19) . ?
C23 H23 0.9500 . ?
C24 C25 1.398(16) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C35 1.382(14) . ?
C30 C31 1.391(14) . ?
C31 C32 1.377(15) . ?
C31 H31 0.9500 . ?
C32 C33 1.377(16) . ?
C32 H32 0.9500 . ?
C33 C34 1.404(16) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(15) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.383(15) . ?
C40 C45 1.417(14) . ?
C41 C42 1.412(16) . ?
C41 H41 0.9500 . ?
C42 C43 1.40(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.359(19) . ?
C43 H43 0.9500 . ?
C44 C45 1.365(16) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

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
C3 W1 C2 91.6(5) . . ?
C3 W1 C1 89.2(5) . . ?
C2 W1 C1 89.2(5) . . ?
C3 W1 C4 89.1(5) . . ?
C2 W1 C4 175.7(4) . . ?
C1 W1 C4 86.6(5) . . ?
C3 W1 C6 89.6(5) . . ?
C2 W1 C6 91.7(4) . . ?
C1 W1 C6 178.5(4) . . ?
C4 W1 C6 92.5(5) . . ?
C3 W1 Sb1 170.3(3) . . ?
C2 W1 Sb1 83.5(3) . . ?
C1 W1 Sb1 82.4(3) . . ?
C4 W1 Sb1 95.2(4) . . ?
C6 W1 Sb1 98.9(3) . . ?
C40 Sb1 C20 98.4(4) . . ?
C40 Sb1 C30 98.8(4) . . ?
C20 Sb1 C30 102.6(4) . . ?
C40 Sb1 W1 112.3(3) . . ?
C20 Sb1 W1 125.5(3) . . ?
C30 Sb1 W1 115.0(3) . . ?
C10 S1 C7 92.1(6) . . ?
C6 O6 C11A 123.1(10) . . ?
C6 O6 C11 123.1(10) . . ?
C6 O6 S1A 133.3(15) . . ?
O1 C1 W1 178.9(12) . . ?
O2 C2 W1 174.6(9) . . ?
O3 C3 W1 178.7(11) . . ?
O4 C4 W1 175.4(12) . . ?
O6 C6 C7 104.4(10) . . ?
O6 C6 W1 130.0(9) . . ?
C7 C6 W1 125.6(9) . . ?
C8 C7 C6 126.6(11) . . ?
C8 C7 S1 107.5(10) . . ?
C6 C7 S1 125.9(10) . . ?
C7 C8 C9 113.5(11) . . ?
C7 C8 H8 123.3 . . ?
C9 C8 H8 123.3 . . ?
C10 C9 C8 111.3(12) . . ?
C10 C9 H9 124.3 . . ?
C8 C9 H9 124.3 . . ?
C9 C10 S1 115.5(11) . . ?
C9 C10 H10 122.2 . . ?
S1 C10 H10 122.2 . . ?
O6 C11 C12 98.5(11) . . ?
O6 C11 H11A 112.1 . . ?
C12 C11 H11A 112.1 . . ?
O6 C11 H11B 112.1 . . ?
C12 C11 H11B 112.1 . . ?
H11A C11 H11B 109.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O6 C11A C12A 127(2) . . ?
O6 C11A H11C 105.7 . . ?
C12A C11A H11C 105.7 . . ?
O6 C11A H11D 105.7 . . ?
C12A C11A H11D 105.7 . . ?
H11C C11A H11D 106.1 . . ?
C11A C12A H12D 109.5 . . ?
C11A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C11A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C25 C20 C21 120.3(10) . . ?
C25 C20 Sb1 122.4(7) . . ?
C21 C20 Sb1 117.3(8) . . ?
C22 C21 C20 119.5(11) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C23 C22 C21 120.1(11) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 120.7(11) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C25 120.0(12) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C20 C25 C24 119.3(11) . . ?
C20 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C35 C30 C31 120.7(9) . . ?
C35 C30 Sb1 120.1(7) . . ?
C31 C30 Sb1 119.1(7) . . ?
C32 C31 C30 119.6(10) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C33 C32 C31 120.7(10) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C32 C33 C34 119.7(10) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C35 C34 C33 119.8(10) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C30 C35 C34 119.5(10) . . ?
C30 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C41 C40 C45 118.7(10) . . ?
C41 C40 Sb1 122.4(7) . . ?
C45 C40 Sb1 118.8(8) . . ?
C40 C41 C42 120.0(11) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 119.7(12) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 119.6(11) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 121.7(12) . . ?
C43 C44 H44 119.1 . . ?
C45 C44 H44 119.1 . . ?
C44 C45 C40 120.3(11) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11A O6 C6 C7 178.9(9) . . . . ?
C11 O6 C6 C7 178.9(9) . . . . ?
S1A O6 C6 C7 9(2) . . . . ?
C11A O6 C6 W1 -2.2(16) . . . . ?
C11 O6 C6 W1 -2.2(16) . . . . ?
S1A O6 C6 W1 -172.0(15) . . . . ?
O6 C6 C7 C8 174.7(11) . . . . ?
W1 C6 C7 C8 -4.3(17) . . . . ?
O6 C6 C7 S1 -6.7(14) . . . . ?
W1 C6 C7 S1 174.3(6) . . . . ?
C10 S1 C7 C8 1.3(9) . . . . ?
C10 S1 C7 C6 -177.6(11) . . . . ?
C6 C7 C8 C9 178.6(11) . . . . ?
S1 C7 C8 C9 -0.3(13) . . . . ?
C7 C8 C9 C10 -1.3(15) . . . . ?
C8 C9 C10 S1 2.3(14) . . . . ?
C7 S1 C10 C9 -2.2(10) . . . . ?
C6 O6 C11 C12 -165.3(11) . . . . ?
C6 O6 C11A C12A -166(2) . . . . ?
C25 C20 C21 C22 -0.8(16) . . . . ?
Sb1 C20 C21 C22 178.2(8) . . . . ?
C20 C21 C22 C23 0.0(17) . . . . ?
C21 C22 C23 C24 1.1(18) . . . . ?
C22 C23 C24 C25 -1(2) . . . . ?
C21 C20 C25 C24 0.6(17) . . . . ?
Sb1 C20 C25 C24 -178.4(9) . . . . ?
C23 C24 C25 C20 0.5(19) . . . . ?
C35 C30 C31 C32 -2.8(17) . . . . ?
Sb1 C30 C31 C32 -178.9(9) . . . . ?
C30 C31 C32 C33 2(2) . . . . ?
C31 C32 C33 C34 -0.8(19) . . . . ?
C32 C33 C34 C35 1.1(17) . . . . ?
C31 C30 C35 C34 3.0(16) . . . . ?
Sb1 C30 C35 C34 179.1(8) . . . . ?
C33 C34 C35 C30 -2.2(16) . . . . ?
C45 C40 C41 C42 0.0(17) . . . . ?
Sb1 C40 C41 C42 175.6(9) . . . . ?
C40 C41 C42 C43 0(2) . . . . ?
C41 C42 C43 C44 1(2) . . . . ?
C42 C43 C44 C45 -1(2) . . . . ?
C43 C44 C45 C40 1(2) . . . . ?
C41 C40 C45 C44 -0.1(17) . . . . ?
Sb1 C40 C45 C44 -175.9(9) . . . . ?

_refine_diff_density_max         2.640
_refine_diff_density_min         -2.235
_refine_diff_density_rms         0.198

####################################################################### 
# 
# 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_compound4
_audit_block_doi                 10.5517/ccdc.csd.cc1ytjmx
_database_code_depnum_ccdc_archive 'CCDC 1812000'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8NJ01008K 2018
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H25 O5 S2 Sb W'
_chemical_formula_sum            'C33 H25 O5 S2 Sb W'
_chemical_formula_weight         871.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.587(6)
_cell_length_b                   11.959(7)
_cell_length_c                   15.924(12)
_cell_angle_alpha                71.22(3)
_cell_angle_beta                 75.47(3)
_cell_angle_gamma                66.92(2)
_cell_volume                     1573.7(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9720
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.33
_exptl_crystal_description       block
_exptl_crystal_colour            bronze
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_F_000             840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.143
_exptl_absorpt_coefficient_mu    4.682
_shelx_estimated_absorpt_T_min   0.459
_shelx_estimated_absorpt_T_max   0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6565
_exptl_absorpt_correction_T_max  0.7899
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\ms micro focus'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52111
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.333
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5772
_reflns_number_gt                5489
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    
; 
ORTEP-3 for Windows (Farrugia, 1997), 
Mercury (Macrae et al., 2008) 
;
_computing_publication_material  
; 
SHELXL-2013, 
PLATON (Spek, 2009) 
;
_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0139P)²+0.9829P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5772
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0136
_refine_ls_wR_factor_ref         0.0329
_refine_ls_wR_factor_gt          0.0320
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.27654(2) 0.86646(2) 0.19257(2) 0.01692(3) Uani 1 1 d . . . . .
Sb1 Sb 0.56425(2) 0.68991(2) 0.21306(2) 0.01785(4) Uani 1 1 d . . . . .
S1 S 0.14136(6) 0.84159(5) 0.50983(4) 0.02333(12) Uani 1 1 d . . . . .
S2 S -0.19352(8) 0.68083(6) 0.68712(4) 0.03483(14) Uani 1 1 d . . . . .
O1 O 0.3186(2) 0.83703(17) -0.00394(11) 0.0332(4) Uani 1 1 d . . . . .
O2 O 0.3995(2) 1.09240(16) 0.08476(12) 0.0353(4) Uani 1 1 d . . . . .
O3 O -0.06586(19) 1.03450(16) 0.17736(12) 0.0347(4) Uani 1 1 d . . . . .
O4 O 0.1596(2) 0.63336(17) 0.26350(13) 0.0422(5) Uani 1 1 d . . . . .
O6 O 0.31622(17) 0.93689(14) 0.36181(10) 0.0235(3) Uani 1 1 d . . . . .
C1 C 0.3050(2) 0.8450(2) 0.06812(16) 0.0229(5) Uani 1 1 d . . . . .
C2 C 0.3562(2) 1.0122(2) 0.12807(15) 0.0234(5) Uani 1 1 d . . . . .
C3 C 0.0603(3) 0.9755(2) 0.18149(14) 0.0231(5) Uani 1 1 d . . . . .
C4 C 0.2024(3) 0.7172(2) 0.24069(15) 0.0253(5) Uani 1 1 d . . . . .
C6 C 0.2411(2) 0.89359(19) 0.32635(14) 0.0195(4) Uani 1 1 d . . . . .
C7 C 0.1260(2) 0.8598(2) 0.39879(14) 0.0210(4) Uani 1 1 d . . . . .
C8 C -0.0026(3) 0.8363(2) 0.39610(15) 0.0261(5) Uani 1 1 d . . . . .
H8 H -0.031893 0.841367 0.341909 0.031 Uiso 1 1 calc R U . . .
C9 C -0.0858(3) 0.8045(2) 0.48062(15) 0.0272(5) Uani 1 1 d . . . . .
H9 H -0.177520 0.786774 0.489300 0.033 Uiso 1 1 calc R U . . .
C10 C -0.0213(2) 0.8013(2) 0.54984(15) 0.0232(5) Uani 1 1 d . . . . .
C11 C 0.4426(3) 0.9781(2) 0.31093(16) 0.0256(5) Uani 1 1 d . . . . .
H11A H 0.404191 1.062292 0.270113 0.031 Uiso 1 1 calc R U . . .
H11B H 0.511645 0.918775 0.274583 0.031 Uiso 1 1 calc R U . . .
C12 C 0.5268(3) 0.9825(3) 0.37720(19) 0.0422(7) Uani 1 1 d . . . . .
H12A H 0.613776 1.010165 0.344961 0.063 Uiso 1 1 calc R U . . .
H12B H 0.457297 1.041494 0.412662 0.063 Uiso 1 1 calc R U . . .
H12C H 0.564282 0.898605 0.417112 0.063 Uiso 1 1 calc R U . . .
C14 C -0.0704(3) 0.7657(2) 0.64531(15) 0.0246(5) Uani 1 1 d . . . . .
C15 C -0.0293(3) 0.7878(2) 0.71386(15) 0.0268(5) Uani 1 1 d . . . . .
H15 H 0.037023 0.833685 0.704773 0.032 Uiso 1 1 calc R U . . .
C16 C -0.0965(3) 0.7346(2) 0.79885(17) 0.0366(6) Uani 1 1 d . . . . .
H16 H -0.079671 0.740260 0.853409 0.044 Uiso 1 1 calc R U . . .
C17 C -0.1872(3) 0.6748(3) 0.79493(17) 0.0394(6) Uani 1 1 d . . . . .
H17 H -0.241428 0.634036 0.846119 0.047 Uiso 1 1 calc R U . . .
C20 C 0.5840(2) 0.5110(2) 0.20176(15) 0.0210(4) Uani 1 1 d . . . . .
C21 C 0.5342(3) 0.5049(2) 0.12945(17) 0.0387(6) Uani 1 1 d . . . . .
H21 H 0.491846 0.579919 0.086113 0.046 Uiso 1 1 calc R U . . .
C22 C 0.5453(3) 0.3905(2) 0.11954(18) 0.0410(7) Uani 1 1 d . . . . .
H22 H 0.513341 0.387559 0.068665 0.049 Uiso 1 1 calc R U . . .
C23 C 0.6022(3) 0.2816(2) 0.18262(17) 0.0312(5) Uani 1 1 d . . . . .
H23 H 0.609719 0.203374 0.175711 0.037 Uiso 1 1 calc R U . . .
C24 C 0.6481(3) 0.2867(2) 0.25596(18) 0.0319(6) Uani 1 1 d . . . . .
H24 H 0.684944 0.211772 0.300678 0.038 Uiso 1 1 calc R U . . .
C25 C 0.6413(3) 0.4004(2) 0.26547(16) 0.0259(5) Uani 1 1 d . . . . .
H25 H 0.676002 0.402431 0.315684 0.031 Uiso 1 1 calc R U . . .
C30 C 0.7658(2) 0.7112(2) 0.12576(14) 0.0213(4) Uani 1 1 d . . . . .
C31 C 0.7864(3) 0.8269(2) 0.09828(16) 0.0264(5) Uani 1 1 d . . . . .
H31 H 0.708953 0.897082 0.116660 0.032 Uiso 1 1 calc R U . . .
C32 C 0.9194(3) 0.8403(2) 0.04423(17) 0.0326(6) Uani 1 1 d . . . . .
H32 H 0.933513 0.919469 0.026193 0.039 Uiso 1 1 calc R U . . .
C33 C 1.0321(3) 0.7388(2) 0.01633(16) 0.0301(5) Uani 1 1 d . . . . .
H33 H 1.122724 0.748392 -0.021514 0.036 Uiso 1 1 calc R U . . .
C34 C 1.0121(3) 0.6234(2) 0.04376(16) 0.0314(5) Uani 1 1 d . . . . .
H34 H 1.089736 0.553545 0.024991 0.038 Uiso 1 1 calc R U . . .
C35 C 0.8799(3) 0.6088(2) 0.09843(16) 0.0280(5) Uani 1 1 d . . . . .
H35 H 0.867001 0.529127 0.117227 0.034 Uiso 1 1 calc R U . . .
C40 C 0.6471(2) 0.63248(19) 0.33810(14) 0.0202(4) Uani 1 1 d . . . . .
C41 C 0.5427(3) 0.6412(2) 0.41560(15) 0.0255(5) Uani 1 1 d . . . . .
H41 H 0.436017 0.674011 0.412258 0.031 Uiso 1 1 calc R U . . .
C42 C 0.5930(3) 0.6024(2) 0.49809(16) 0.0318(5) Uani 1 1 d . . . . .
H42 H 0.520695 0.610010 0.550852 0.038 Uiso 1 1 calc R U . . .
C43 C 0.7474(3) 0.5530(2) 0.50381(17) 0.0348(6) Uani 1 1 d . . . . .
H43 H 0.781578 0.525778 0.560462 0.042 Uiso 1 1 calc R U . . .
C44 C 0.8529(3) 0.5430(3) 0.42671(19) 0.0424(7) Uani 1 1 d . . . . .
H44 H 0.959478 0.508111 0.430578 0.051 Uiso 1 1 calc R U . . .
C45 C 0.8030(3) 0.5838(3) 0.34390(16) 0.0328(6) Uani 1 1 d . . . . .
H45 H 0.875540 0.578591 0.291023 0.039 Uiso 1 1 calc R U . . .


_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
W1 C3 1.986(3) . ?
W1 C1 2.017(3) . ?
W1 C4 2.030(3) . ?
W1 C2 2.043(3) . ?
W1 C6 2.180(3) . ?
W1 Sb1 2.7593(15) . ?
Sb1 C30 2.131(2) . ?
Sb1 C40 2.133(3) . ?
Sb1 C20 2.135(2) . ?
S1 C10 1.721(2) . ?
S1 C7 1.747(2) . ?
S2 C17 1.710(3) . ?
S2 C14 1.725(3) . ?
O1 C1 1.153(3) . ?
O2 C2 1.145(3) . ?
O3 C3 1.143(3) . ?
O4 C4 1.148(3) . ?
O6 C6 1.338(3) . ?
O6 C11 1.444(3) . ?
C6 C7 1.457(3) . ?
C7 C8 1.380(3) . ?
C8 C9 1.401(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.377(3) . ?
C9 H9 0.9500 . ?
C10 C14 1.448(3) . ?
C11 C12 1.505(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 C15 1.378(3) . ?
C15 C16 1.408(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.347(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C20 C21 1.384(3) . ?
C20 C25 1.388(3) . ?
C21 C22 1.387(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.370(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C31 1.388(3) . ?
C30 C35 1.392(3) . ?
C31 C32 1.383(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.384(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.381(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(3) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.384(3) . ?
C40 C45 1.391(3) . ?
C41 C42 1.387(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.377(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.387(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

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
C3 W1 C1 90.01(9) . . ?
C3 W1 C4 87.79(10) . . ?
C1 W1 C4 88.51(10) . . ?
C3 W1 C2 92.62(10) . . ?
C1 W1 C2 84.01(9) . . ?
C4 W1 C2 172.50(9) . . ?
C3 W1 C6 88.71(9) . . ?
C1 W1 C6 178.65(8) . . ?
C4 W1 C6 91.90(9) . . ?
C2 W1 C6 95.59(9) . . ?
C3 W1 Sb1 172.82(6) . . ?
C1 W1 Sb1 88.81(7) . . ?
C4 W1 Sb1 85.10(8) . . ?
C2 W1 Sb1 94.30(8) . . ?
C6 W1 Sb1 92.51(6) . . ?
C30 Sb1 C40 98.74(9) . . ?
C30 Sb1 C20 99.37(9) . . ?
C40 Sb1 C20 99.21(9) . . ?
C30 Sb1 W1 122.78(7) . . ?
C40 Sb1 W1 119.59(7) . . ?
C20 Sb1 W1 112.96(7) . . ?
C10 S1 C7 92.28(11) . . ?
C17 S2 C14 91.54(13) . . ?
C6 O6 C11 122.39(17) . . ?
O1 C1 W1 177.7(2) . . ?
O2 C2 W1 173.73(19) . . ?
O3 C3 W1 177.3(2) . . ?
O4 C4 W1 176.5(2) . . ?
O6 C6 C7 105.47(18) . . ?
O6 C6 W1 130.61(16) . . ?
C7 C6 W1 123.87(15) . . ?
C8 C7 C6 130.2(2) . . ?
C8 C7 S1 109.69(17) . . ?
C6 C7 S1 120.14(16) . . ?
C7 C8 C9 113.8(2) . . ?
C7 C8 H8 123.1 . . ?
C9 C8 H8 123.1 . . ?
C10 C9 C8 113.2(2) . . ?
C10 C9 H9 123.4 . . ?
C8 C9 H9 123.4 . . ?
C9 C10 C14 128.5(2) . . ?
C9 C10 S1 111.01(18) . . ?
C14 C10 S1 120.50(17) . . ?
O6 C11 C12 107.1(2) . . ?
O6 C11 H11A 110.3 . . ?
C12 C11 H11A 110.3 . . ?
O6 C11 H11B 110.3 . . ?
C12 C11 H11B 110.3 . . ?
H11A C11 H11B 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 C14 C10 128.7(2) . . ?
C15 C14 S2 110.77(18) . . ?
C10 C14 S2 120.51(18) . . ?
C14 C15 C16 112.4(2) . . ?
C14 C15 H15 123.8 . . ?
C16 C15 H15 123.8 . . ?
C17 C16 C15 113.1(2) . . ?
C17 C16 H16 123.4 . . ?
C15 C16 H16 123.4 . . ?
C16 C17 S2 112.2(2) . . ?
C16 C17 H17 123.9 . . ?
S2 C17 H17 123.9 . . ?
C21 C20 C25 118.5(2) . . ?
C21 C20 Sb1 118.99(17) . . ?
C25 C20 Sb1 122.49(17) . . ?
C20 C21 C22 120.8(2) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 120.4(2) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 119.4(2) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 120.7(2) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C20 C25 C24 120.1(2) . . ?
C20 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C31 C30 C35 119.5(2) . . ?
C31 C30 Sb1 119.89(17) . . ?
C35 C30 Sb1 120.56(17) . . ?
C32 C31 C30 120.2(2) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 120.2(2) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 119.7(2) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.5(2) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C34 C35 C30 119.8(2) . . ?
C34 C35 H35 120.1 . . ?
C30 C35 H35 120.1 . . ?
C41 C40 C45 119.3(2) . . ?
C41 C40 Sb1 119.04(16) . . ?
C45 C40 Sb1 121.68(17) . . ?
C40 C41 C42 120.4(2) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C43 C42 C41 120.3(2) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C44 119.8(2) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C45 120.1(2) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C40 120.2(2) . . ?
C44 C45 H45 119.9 . . ?
C40 C45 H45 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 O6 C6 C7 178.78(18) . . . . ?
C11 O6 C6 W1 1.2(3) . . . . ?
O6 C6 C7 C8 164.3(2) . . . . ?
W1 C6 C7 C8 -17.9(3) . . . . ?
O6 C6 C7 S1 -16.5(2) . . . . ?
W1 C6 C7 S1 161.27(11) . . . . ?
C10 S1 C7 C8 0.77(18) . . . . ?
C10 S1 C7 C6 -178.59(18) . . . . ?
C6 C7 C8 C9 179.1(2) . . . . ?
S1 C7 C8 C9 -0.1(3) . . . . ?
C7 C8 C9 C10 -0.8(3) . . . . ?
C8 C9 C10 C14 -176.3(2) . . . . ?
C8 C9 C10 S1 1.4(3) . . . . ?
C7 S1 C10 C9 -1.21(18) . . . . ?
C7 S1 C10 C14 176.65(18) . . . . ?
C6 O6 C11 C12 -163.3(2) . . . . ?
C9 C10 C14 C15 -164.2(2) . . . . ?
S1 C10 C14 C15 18.3(3) . . . . ?
C9 C10 C14 S2 17.5(3) . . . . ?
S1 C10 C14 S2 -159.99(13) . . . . ?
C17 S2 C14 C15 -0.47(18) . . . . ?
C17 S2 C14 C10 178.11(19) . . . . ?
C10 C14 C15 C16 -177.8(2) . . . . ?
S2 C14 C15 C16 0.6(3) . . . . ?
C14 C15 C16 C17 -0.5(3) . . . . ?
C15 C16 C17 S2 0.2(3) . . . . ?
C14 S2 C17 C16 0.2(2) . . . . ?
C25 C20 C21 C22 -1.8(4) . . . . ?
Sb1 C20 C21 C22 179.8(2) . . . . ?
C20 C21 C22 C23 1.8(5) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
C22 C23 C24 C25 -1.7(4) . . . . ?
C21 C20 C25 C24 0.1(4) . . . . ?
Sb1 C20 C25 C24 178.39(17) . . . . ?
C23 C24 C25 C20 1.7(4) . . . . ?
C35 C30 C31 C32 -0.1(3) . . . . ?
Sb1 C30 C31 C32 177.67(17) . . . . ?
C30 C31 C32 C33 0.7(4) . . . . ?
C31 C32 C33 C34 -0.9(4) . . . . ?
C32 C33 C34 C35 0.5(4) . . . . ?
C33 C34 C35 C30 0.2(4) . . . . ?
C31 C30 C35 C34 -0.4(3) . . . . ?
Sb1 C30 C35 C34 -178.14(18) . . . . ?
C45 C40 C41 C42 0.3(3) . . . . ?
Sb1 C40 C41 C42 178.78(17) . . . . ?
C40 C41 C42 C43 -1.0(4) . . . . ?
C41 C42 C43 C44 0.6(4) . . . . ?
C42 C43 C44 C45 0.6(4) . . . . ?
C43 C44 C45 C40 -1.4(4) . . . . ?
C41 C40 C45 C44 0.9(4) . . . . ?
Sb1 C40 C45 C44 -177.6(2) . . . . ?

_refine_diff_density_max         0.294
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_shelx_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc1ytjkv
_database_code_depnum_ccdc_archive 'CCDC 1811998'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8NJ01008K 2018
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H23 O6 Sb W'
_chemical_formula_sum            'C29 H23 O6 Sb W'
_chemical_formula_weight         773.07

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.584(10)
_cell_length_b                   10.930(11)
_cell_length_c                   14.073(12)
_cell_angle_alpha                101.23(5)
_cell_angle_beta                 91.88(5)
_cell_angle_gamma                118.69(3)
_cell_volume                     1386(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9002
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      37.98

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_F_000             740
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.633
_exptl_crystal_size_mid          0.422
_exptl_crystal_size_min          0.296
_exptl_absorpt_coefficient_mu    5.162
_shelx_estimated_absorpt_T_min   0.139
_shelx_estimated_absorpt_T_max   0.310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3621
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\ms micro focus'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42619
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.211
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5077
_reflns_number_gt                4587
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
; 
ORTEP-3 for Windows (Farrugia, 1997), 
Mercury (Macrae et al., 2008) 
;
_computing_publication_material  
; 
SHELXL-2013, 
PLATON (Spek, 2009) 
;
_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+9.3866P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5077
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.23695(2) 0.73750(2) 0.16979(2) 0.01891(7) Uani 1 1 d . . . . .
Sb1 Sb 0.34389(3) 0.64225(3) 0.30381(2) 0.01678(9) Uani 1 1 d . . . . .
O1 O -0.0740(5) 0.5018(5) 0.2053(3) 0.0464(12) Uani 1 1 d . . . . .
O2 O 0.2546(5) 0.9594(5) 0.3612(3) 0.0371(10) Uani 1 1 d . . . . .
O3 O 0.0789(5) 0.8320(4) 0.0340(3) 0.0364(10) Uani 1 1 d . . . . .
O4 O 0.2031(5) 0.4912(4) -0.0116(3) 0.0358(10) Uani 1 1 d . . . . .
O6 O 0.5136(5) 1.0181(5) 0.1333(3) 0.0404(11) Uani 1 1 d . . . . .
O7 O 0.5246(5) 0.6955(6) 0.1152(4) 0.0495(12) Uani 1 1 d . . . . .
C1 C 0.0380(6) 0.5884(6) 0.1929(4) 0.0250(12) Uani 1 1 d . . . . .
C2 C 0.2507(6) 0.8840(6) 0.2905(4) 0.0236(11) Uani 1 1 d . . . . .
C3 C 0.1378(6) 0.7992(6) 0.0856(4) 0.0270(12) Uani 1 1 d . . . . .
C4 C 0.2192(6) 0.5817(6) 0.0539(4) 0.0255(12) Uani 1 1 d . . . . .
C6 C 0.4519(6) 0.8814(6) 0.1390(4) 0.0245(12) Uani 1 1 d . . . . .
C7 C 0.5632(6) 0.8426(8) 0.1179(4) 0.0410(17) Uani 1 1 d . . . . .
C8 C 0.7034(8) 0.9055(10) 0.1052(6) 0.058(2) Uani 1 1 d . . . . .
H8 H 0.7615 1.0041 0.1054 0.070 Uiso 1 1 calc R U . . .
C9 C 0.7525(8) 0.8065(9) 0.0916(5) 0.0499(18) Uani 1 1 d . . . . .
H9 H 0.8475 0.8255 0.0801 0.060 Uiso 1 1 calc R U . . .
C10 C 0.6425(9) 0.6807(10) 0.0976(6) 0.059(2) Uani 1 1 d . . . . .
H10 H 0.6458 0.5941 0.0906 0.071 Uiso 1 1 calc R U . . .
C11 C 0.4267(9) 1.0913(7) 0.1424(5) 0.049(2) Uani 1 1 d . . . . .
H11A H 0.3866 1.0896 0.2050 0.059 Uiso 1 1 calc R U . . .
H11B H 0.3461 1.0478 0.0872 0.059 Uiso 1 1 calc R U . . .
C12 C 0.5462(10) 1.2503(8) 0.1391(6) 0.058(2) Uani 1 1 d . . . . .
H12A H 0.5015 1.3112 0.1446 0.087 Uiso 1 1 calc R U . . .
H12B H 0.6254 1.2893 0.1936 0.087 Uiso 1 1 calc R U . . .
H12C H 0.5853 1.2479 0.0770 0.087 Uiso 1 1 calc R U . . .
C20 C 0.2938(6) 0.6939(6) 0.4476(4) 0.0223(11) Uani 1 1 d . . . . .
C21 C 0.3995(7) 0.7644(8) 0.5295(5) 0.0455(18) Uani 1 1 d . . . . .
H21 H 0.4975 0.7887 0.5235 0.055 Uiso 1 1 calc R U . . .
C22 C 0.3620(9) 0.7996(10) 0.6202(5) 0.067(3) Uani 1 1 d . . . . .
H22 H 0.4351 0.8486 0.6761 0.080 Uiso 1 1 calc R U . . .
C23 C 0.2196(9) 0.7644(8) 0.6306(5) 0.0486(18) Uani 1 1 d . . . . .
H23 H 0.1948 0.7878 0.6932 0.058 Uiso 1 1 calc R U . . .
C24 C 0.1154(8) 0.6960(8) 0.5500(5) 0.0436(17) Uani 1 1 d . . . . .
H24 H 0.0175 0.6715 0.5562 0.052 Uiso 1 1 calc R U . . .
C25 C 0.1522(7) 0.6622(7) 0.4592(5) 0.0369(14) Uani 1 1 d . . . . .
H25 H 0.0790 0.6162 0.4033 0.044 Uiso 1 1 calc R U . . .
C30 C 0.2443(5) 0.4141(5) 0.2830(4) 0.0197(10) Uani 1 1 d . . . . .
C31 C 0.2487(6) 0.3542(6) 0.3609(4) 0.0263(12) Uani 1 1 d . . . . .
H31 H 0.2970 0.4152 0.4239 0.032 Uiso 1 1 calc R U . . .
C32 C 0.1826(7) 0.2050(6) 0.3474(4) 0.0304(13) Uani 1 1 d . . . . .
H32 H 0.1864 0.1650 0.4009 0.036 Uiso 1 1 calc R U . . .
C33 C 0.1120(7) 0.1159(6) 0.2561(5) 0.0337(14) Uani 1 1 d . . . . .
H33 H 0.0665 0.0147 0.2470 0.040 Uiso 1 1 calc R U . . .
C34 C 0.1075(7) 0.1739(7) 0.1781(5) 0.0404(16) Uani 1 1 d . . . . .
H34 H 0.0597 0.1124 0.1153 0.049 Uiso 1 1 calc R U . . .
C35 C 0.1729(7) 0.3223(6) 0.1912(4) 0.0346(14) Uani 1 1 d . . . . .
H35 H 0.1689 0.3614 0.1373 0.042 Uiso 1 1 calc R U . . .
C40 C 0.5684(5) 0.7040(6) 0.3412(4) 0.0221(11) Uani 1 1 d . . . . .
C41 C 0.6721(6) 0.8511(7) 0.3656(4) 0.0330(13) Uani 1 1 d . . . . .
H41 H 0.6425 0.9206 0.3663 0.040 Uiso 1 1 calc R U . . .
C42 C 0.8192(7) 0.8943(7) 0.3889(5) 0.0410(16) Uani 1 1 d . . . . .
H42 H 0.8896 0.9937 0.4053 0.049 Uiso 1 1 calc R U . . .
C43 C 0.8634(7) 0.7930(9) 0.3882(5) 0.0448(18) Uani 1 1 d . . . . .
H43 H 0.9638 0.8235 0.4035 0.054 Uiso 1 1 calc R U . . .
C44 C 0.7617(7) 0.6479(8) 0.3652(5) 0.0412(16) Uani 1 1 d . . . . .
H44 H 0.7919 0.5789 0.3655 0.049 Uiso 1 1 calc R U . . .
C45 C 0.6135(6) 0.6032(7) 0.3415(4) 0.0319(13) Uani 1 1 d . . . . .
H45 H 0.5436 0.5037 0.3255 0.038 Uiso 1 1 calc R U . . .


_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
W1 C3 1.967(6) . ?
W1 C1 2.038(6) . ?
W1 C2 2.043(6) . ?
W1 C4 2.046(6) . ?
W1 C6 2.175(6) . ?
W1 Sb1 2.7710(18) . ?
Sb1 C30 2.142(5) . ?
Sb1 C20 2.147(5) . ?
Sb1 C40 2.149(6) . ?
O1 C1 1.154(7) . ?
O2 C2 1.147(7) . ?
O3 C3 1.153(7) . ?
O4 C4 1.154(7) . ?
O6 C6 1.334(7) . ?
O6 C11 1.475(9) . ?
O7 C10 1.357(9) . ?
O7 C7 1.448(9) . ?
C6 C7 1.452(9) . ?
C7 C8 1.339(10) . ?
C8 C9 1.394(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.329(12) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.596(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C20 C21 1.383(8) . ?
C20 C25 1.390(8) . ?
C21 C22 1.388(9) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.363(10) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(9) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C31 1.393(7) . ?
C30 C35 1.396(8) . ?
C31 C32 1.401(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(9) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.393(8) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C45 1.396(8) . ?
C40 C41 1.404(8) . ?
C41 C42 1.398(9) . ?
C41 H41 0.9500 . ?
C42 C43 1.393(10) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(10) . ?
C43 H43 0.9500 . ?
C44 C45 1.406(8) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

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
C3 W1 C1 88.6(2) . . ?
C3 W1 C2 91.7(2) . . ?
C1 W1 C2 91.1(2) . . ?
C3 W1 C4 90.8(2) . . ?
C1 W1 C4 86.5(2) . . ?
C2 W1 C4 176.5(2) . . ?
C3 W1 C6 93.6(2) . . ?
C1 W1 C6 175.1(2) . . ?
C2 W1 C6 93.3(2) . . ?
C4 W1 C6 89.0(2) . . ?
C3 W1 Sb1 171.78(16) . . ?
C1 W1 Sb1 84.50(17) . . ?
C2 W1 Sb1 84.02(17) . . ?
C4 W1 Sb1 93.20(17) . . ?
C6 W1 Sb1 93.67(16) . . ?
C30 Sb1 C20 98.9(2) . . ?
C30 Sb1 C40 100.3(2) . . ?
C20 Sb1 C40 99.4(2) . . ?
C30 Sb1 W1 116.11(15) . . ?
C20 Sb1 W1 111.91(15) . . ?
C40 Sb1 W1 125.91(15) . . ?
C6 O6 C11 119.3(5) . . ?
C10 O7 C7 108.1(6) . . ?
O1 C1 W1 178.6(5) . . ?
O2 C2 W1 175.7(5) . . ?
O3 C3 W1 178.0(5) . . ?
O4 C4 W1 177.2(5) . . ?
O6 C6 C7 103.8(5) . . ?
O6 C6 W1 131.2(4) . . ?
C7 C6 W1 125.0(4) . . ?
C8 C7 O7 104.2(7) . . ?
C8 C7 C6 139.1(8) . . ?
O7 C7 C6 116.5(5) . . ?
C7 C8 C9 110.8(8) . . ?
C7 C8 H8 124.6 . . ?
C9 C8 H8 124.6 . . ?
C10 C9 C8 107.6(7) . . ?
C10 C9 H9 126.2 . . ?
C8 C9 H9 126.2 . . ?
C9 C10 O7 109.3(8) . . ?
C9 C10 H10 125.4 . . ?
O7 C10 H10 125.4 . . ?
O6 C11 C12 101.2(6) . . ?
O6 C11 H11A 111.5 . . ?
C12 C11 H11A 111.5 . . ?
O6 C11 H11B 111.5 . . ?
C12 C11 H11B 111.5 . . ?
H11A C11 H11B 109.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 C20 C25 118.3(5) . . ?
C21 C20 Sb1 122.2(4) . . ?
C25 C20 Sb1 119.4(4) . . ?
C20 C21 C22 119.8(6) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 H21 120.1 . . ?
C23 C22 C21 121.1(7) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 119.3(6) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.0(6) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 121.5(6) . . ?
C24 C25 H25 119.3 . . ?
C20 C25 H25 119.3 . . ?
C31 C30 C35 118.6(5) . . ?
C31 C30 Sb1 120.6(4) . . ?
C35 C30 Sb1 120.7(4) . . ?
C30 C31 C32 120.6(5) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C33 C32 C31 119.9(5) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.1(6) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.2(6) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C30 C35 C34 120.6(5) . . ?
C30 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C45 C40 C41 119.5(5) . . ?
C45 C40 Sb1 122.2(4) . . ?
C41 C40 Sb1 118.3(4) . . ?
C42 C41 C40 119.5(6) . . ?
C42 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
C43 C42 C41 120.6(6) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C44 C43 C42 120.3(6) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 119.6(6) . . ?
C43 C44 H44 120.2 . . ?
C45 C44 H44 120.2 . . ?
C40 C45 C44 120.5(6) . . ?
C40 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 O6 C6 C7 174.8(5) . . . . ?
C11 O6 C6 W1 -4.4(7) . . . . ?
C10 O7 C7 C8 -2.2(7) . . . . ?
C10 O7 C7 C6 -178.2(6) . . . . ?
O6 C6 C7 C8 8.3(11) . . . . ?
W1 C6 C7 C8 -172.5(8) . . . . ?
O6 C6 C7 O7 -177.7(5) . . . . ?
W1 C6 C7 O7 1.5(7) . . . . ?
O7 C7 C8 C9 2.0(8) . . . . ?
C6 C7 C8 C9 176.4(7) . . . . ?
C7 C8 C9 C10 -1.1(10) . . . . ?
C8 C9 C10 O7 -0.4(9) . . . . ?
C7 O7 C10 C9 1.7(8) . . . . ?
C6 O6 C11 C12 176.0(5) . . . . ?
C25 C20 C21 C22 0.9(11) . . . . ?
Sb1 C20 C21 C22 177.8(6) . . . . ?
C20 C21 C22 C23 0.4(14) . . . . ?
C21 C22 C23 C24 -0.9(14) . . . . ?
C22 C23 C24 C25 0.1(12) . . . . ?
C23 C24 C25 C20 1.3(11) . . . . ?
C21 C20 C25 C24 -1.8(10) . . . . ?
Sb1 C20 C25 C24 -178.7(5) . . . . ?
C35 C30 C31 C32 -0.1(8) . . . . ?
Sb1 C30 C31 C32 179.5(4) . . . . ?
C30 C31 C32 C33 -0.2(9) . . . . ?
C31 C32 C33 C34 0.5(9) . . . . ?
C32 C33 C34 C35 -0.6(10) . . . . ?
C31 C30 C35 C34 0.0(9) . . . . ?
Sb1 C30 C35 C34 -179.6(5) . . . . ?
C33 C34 C35 C30 0.4(11) . . . . ?
C45 C40 C41 C42 0.6(9) . . . . ?
Sb1 C40 C41 C42 -179.1(5) . . . . ?
C40 C41 C42 C43 -0.1(9) . . . . ?
C41 C42 C43 C44 -0.6(10) . . . . ?
C42 C43 C44 C45 0.7(10) . . . . ?
C41 C40 C45 C44 -0.5(9) . . . . ?
Sb1 C40 C45 C44 179.2(4) . . . . ?
C43 C44 C45 C40 -0.2(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C9 H9 O3 0.95 2.53 3.466(9) 170.3 1_655
C10 H10 O4 0.95 2.41 3.139(9) 133.4 2_665
C11 H11B O3 0.99 2.63 3.441(9) 139.8 .

_refine_diff_density_max         1.893
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.138

####################################################################### 
# 
# 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_shelx_CCDC2
_audit_block_doi                 10.5517/ccdc.csd.cc1ytjlw
_database_code_depnum_ccdc_archive 'CCDC 1811999'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C8NJ01008K 2018
_audit_update_record             
;
2017-12-18 deposited with the CCDC.
2018-05-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H26 N O5 Sb W'
_chemical_formula_sum            'C30 H26 N O5 Sb W'
_chemical_formula_weight         786.12

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.482(7)
_cell_length_b                   28.043(14)
_cell_length_c                   10.666(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.58(3)
_cell_angle_gamma                90
_cell_volume                     2828(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9335
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.42

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_F_000             1512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.146
_exptl_absorpt_coefficient_mu    5.058
_shelx_estimated_absorpt_T_min   0.431
_shelx_estimated_absorpt_T_max   0.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6262
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\ms micro focus'
_diffrn_radiation_monochromator  'Quazar multi-layer optics'
_diffrn_measurement_device_type  'Bruker kappa Proton CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            111070
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.238
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5170
_reflns_number_gt                5006
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXTS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXTL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
; ORTEP-3 for Windows (Farrugia, 1997),
 Mercury (Macrae et al., 2008)
_computing_publication_material   'SHELXL-2014'
  
_refine_special_details
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5170
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0673
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.605
_refine_ls_restrained_S_all      1.605
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.81759(2) 0.41293(2) 0.31833(2) 0.01691(7) Uani 1 1 d . . . . .
Sb1 Sb 0.73741(2) 0.34751(2) 0.46349(2) 0.01589(8) Uani 1 1 d . . . . .
O1 O 1.1203(3) 0.38938(10) 0.5545(3) 0.0382(7) Uani 1 1 d . . . . .
O2 O 0.8442(3) 0.31949(9) 0.1606(3) 0.0338(6) Uani 1 1 d . . . . .
O3 O 0.9724(3) 0.47271(9) 0.1776(3) 0.0322(6) Uani 1 1 d . . . . .
O4 O 0.8265(3) 0.50469(9) 0.4970(3) 0.0349(6) Uani 1 1 d . . . . .
O6 O 0.4896(2) 0.44613(9) 0.1765(3) 0.0299(6) Uani 1 1 d . . . . .
N1 N 0.4237(3) 0.43371(12) -0.0970(3) 0.0349(7) Uani 1 1 d . . . . .
C1 C 1.0099(4) 0.39780(12) 0.4666(4) 0.0242(7) Uani 1 1 d . . . . .
C2 C 0.8303(4) 0.35383(12) 0.2129(3) 0.0228(7) Uani 1 1 d . . . . .
C3 C 0.9109(3) 0.45156(12) 0.2279(4) 0.0240(7) Uani 1 1 d . . . . .
C4 C 0.8188(4) 0.47139(12) 0.4320(4) 0.0233(7) Uani 1 1 d . . . . .
C6 C 0.6016(3) 0.43060(11) 0.1573(4) 0.0200(7) Uani 1 1 d . . . . .
C7 C 0.5592(3) 0.42777(11) 0.0114(3) 0.0158(6) Uani 1 1 d . . . . .
C8 C 0.6465(4) 0.41854(12) -0.0552(4) 0.0238(8) Uani 1 1 d . . . . .
H8 H 0.7453 0.4125 -0.0099 0.029 Uiso 1 1 calc R U . . .
C9 C 0.5642(4) 0.41962(12) -0.1991(4) 0.0281(8) Uani 1 1 d . . . . .
H9 H 0.5970 0.4153 -0.2686 0.034 Uiso 1 1 calc R U . . .
C10 C 0.4285(5) 0.42799(16) -0.2208(4) 0.0399(10) Uani 1 1 d . . . . .
H10 H 0.3494 0.4296 -0.3091 0.048 Uiso 1 1 calc R U . . .
C11 C 0.4922(4) 0.45422(14) 0.3109(4) 0.0326(9) Uani 1 1 d . . . . .
H11A H 0.5441 0.4840 0.3523 0.039 Uiso 1 1 calc R U . . .
H11B H 0.5396 0.4274 0.3743 0.039 Uiso 1 1 calc R U . . .
C12 C 0.3431(5) 0.45807(16) 0.2886(5) 0.0460(11) Uani 1 1 d . . . . .
H12A H 0.3398 0.4636 0.3779 0.069 Uiso 1 1 calc R U . . .
H12B H 0.2976 0.4847 0.2257 0.069 Uiso 1 1 calc R U . . .
H12C H 0.2931 0.4284 0.2475 0.069 Uiso 1 1 calc R U . . .
C13 C 0.2891(4) 0.44178(17) -0.0841(5) 0.0442(11) Uani 1 1 d . . . . .
H13A H 0.3096 0.4450 0.0143 0.066 Uiso 1 1 calc R U . . .
H13B H 0.2438 0.4710 -0.1337 0.066 Uiso 1 1 calc R U . . .
H13C H 0.2255 0.4147 -0.1244 0.066 Uiso 1 1 calc R U . . .
C20 C 0.5253(3) 0.32919(11) 0.4234(4) 0.0210(7) Uani 1 1 d . . . . .
C21 C 0.4267(4) 0.32549(12) 0.2860(4) 0.0275(8) Uani 1 1 d . . . . .
H21 H 0.4542 0.3315 0.2135 0.033 Uiso 1 1 calc R U . . .
C22 C 0.2891(4) 0.31315(14) 0.2541(5) 0.0378(10) Uani 1 1 d . . . . .
H22 H 0.2221 0.3103 0.1597 0.045 Uiso 1 1 calc R U . . .
C23 C 0.2486(4) 0.30488(15) 0.3591(5) 0.0435(11) Uani 1 1 d . . . . .
H23 H 0.1532 0.2968 0.3367 0.052 Uiso 1 1 calc R U . . .
C24 C 0.3458(4) 0.30828(16) 0.4966(5) 0.0433(10) Uani 1 1 d . . . . .
H24 H 0.3175 0.3023 0.5686 0.052 Uiso 1 1 calc R U . . .
C25 C 0.4847(4) 0.32045(14) 0.5294(4) 0.0318(9) Uani 1 1 d . . . . .
H25 H 0.5519 0.3228 0.6238 0.038 Uiso 1 1 calc R U . . .
C30 C 0.8128(3) 0.27757(11) 0.4506(3) 0.0191(7) Uani 1 1 d . . . . .
C31 C 0.9583(4) 0.27065(13) 0.5016(4) 0.0299(8) Uani 1 1 d . . . . .
H31 H 1.0216 0.2956 0.5506 0.036 Uiso 1 1 calc R U . . .
C32 C 1.0104(5) 0.22773(15) 0.4813(5) 0.0433(11) Uani 1 1 d . . . . .
H32 H 1.1095 0.2233 0.5145 0.052 Uiso 1 1 calc R U . . .
C33 C 0.9185(5) 0.19098(13) 0.4124(4) 0.0386(10) Uani 1 1 d . . . . .
H33 H 0.9548 0.1615 0.3983 0.046 Uiso 1 1 calc R U . . .
C34 C 0.7763(5) 0.19700(13) 0.3649(4) 0.0398(10) Uani 1 1 d . . . . .
H34 H 0.7138 0.1715 0.3194 0.048 Uiso 1 1 calc R U . . .
C35 C 0.7221(4) 0.24069(12) 0.3830(4) 0.0284(8) Uani 1 1 d . . . . .
H35 H 0.6228 0.2450 0.3487 0.034 Uiso 1 1 calc R U . . .
C40 C 0.8378(3) 0.35712(12) 0.6843(3) 0.0184(7) Uani 1 1 d . . . . .
C41 C 0.8841(4) 0.40221(12) 0.7378(3) 0.0226(7) Uani 1 1 d . . . . .
H41 H 0.8690 0.4284 0.6764 0.027 Uiso 1 1 calc R U . . .
C42 C 0.9527(4) 0.40939(12) 0.8814(4) 0.0237(8) Uani 1 1 d . . . . .
H42 H 0.9816 0.4405 0.9182 0.028 Uiso 1 1 calc R U . . .
C43 C 0.9782(4) 0.37035(13) 0.9699(3) 0.0257(8) Uani 1 1 d . . . . .
H43 H 1.0268 0.3748 1.0675 0.031 Uiso 1 1 calc R U . . .
C44 C 0.9342(4) 0.32565(13) 0.9177(4) 0.0271(8) Uani 1 1 d . . . . .
H44 H 0.9520 0.2993 0.9791 0.033 Uiso 1 1 calc R U . . .
C45 C 0.8622(4) 0.31863(12) 0.7727(4) 0.0248(7) Uani 1 1 d . . . . .
H45 H 0.8307 0.2877 0.7361 0.030 Uiso 1 1 calc R U . . .


_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
W1 C3 1.969(4) . ?
W1 C1 1.998(4) . ?
W1 C4 2.036(4) . ?
W1 C2 2.039(4) . ?
W1 C6 2.228(3) . ?
W1 Sb1 2.7555(10) . ?
Sb1 C40 2.142(3) . ?
Sb1 C30 2.141(3) . ?
Sb1 C20 2.138(4) . ?
O1 C1 1.156(4) . ?
O2 C2 1.153(4) . ?
O3 C3 1.164(4) . ?
O4 C4 1.145(4) . ?
O6 C6 1.349(4) . ?
O6 C11 1.439(5) . ?
N1 C10 1.353(5) . ?
N1 C7 1.401(4) . ?
N1 C13 1.492(5) . ?
C6 C7 1.424(5) . ?
C7 C8 1.404(5) . ?
C8 C9 1.400(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.359(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.480(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C20 C21 1.385(5) . ?
C20 C25 1.391(5) . ?
C21 C22 1.375(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(5) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C30 C35 1.379(5) . ?
C30 C31 1.394(5) . ?
C31 C32 1.377(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.385(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.361(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.399(5) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C40 C41 1.386(5) . ?
C40 C45 1.382(5) . ?
C41 C42 1.398(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.394(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.368(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.412(5) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

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
C3 W1 C1 87.69(15) . . ?
C3 W1 C4 88.39(14) . . ?
C1 W1 C4 87.42(14) . . ?
C3 W1 C2 90.73(14) . . ?
C1 W1 C2 88.86(14) . . ?
C4 W1 C2 176.21(13) . . ?
C3 W1 C6 93.12(13) . . ?
C1 W1 C6 178.47(13) . . ?
C4 W1 C6 91.31(13) . . ?
C2 W1 C6 92.42(13) . . ?
C3 W1 Sb1 168.04(10) . . ?
C1 W1 Sb1 82.07(11) . . ?
C4 W1 Sb1 97.27(10) . . ?
C2 W1 Sb1 82.93(10) . . ?
C6 W1 Sb1 97.26(9) . . ?
C40 Sb1 C30 99.55(12) . . ?
C40 Sb1 C20 103.01(13) . . ?
C30 Sb1 C20 98.49(12) . . ?
C40 Sb1 W1 114.20(9) . . ?
C30 Sb1 W1 111.31(9) . . ?
C20 Sb1 W1 126.22(9) . . ?
C6 O6 C11 124.0(3) . . ?
C10 N1 C7 109.8(3) . . ?
C10 N1 C13 122.9(3) . . ?
C7 N1 C13 127.2(3) . . ?
O1 C1 W1 178.6(3) . . ?
O2 C2 W1 175.9(3) . . ?
O3 C3 W1 176.2(3) . . ?
O4 C4 W1 176.5(3) . . ?
O6 C6 C7 107.6(3) . . ?
O6 C6 W1 128.0(2) . . ?
C7 C6 W1 124.3(2) . . ?
C8 C7 N1 104.8(3) . . ?
C8 C7 C6 126.8(3) . . ?
N1 C7 C6 128.4(3) . . ?
C9 C8 C7 108.8(3) . . ?
C9 C8 H8 125.6 . . ?
C7 C8 H8 125.6 . . ?
C10 C9 C8 107.1(4) . . ?
C10 C9 H9 126.4 . . ?
C8 C9 H9 126.4 . . ?
C9 C10 N1 109.4(4) . . ?
C9 C10 H10 125.3 . . ?
N1 C10 H10 125.3 . . ?
O6 C11 C12 106.7(3) . . ?
O6 C11 H11A 110.4 . . ?
C12 C11 H11A 110.4 . . ?
O6 C11 H11B 110.4 . . ?
C12 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C21 C20 C25 119.8(3) . . ?
C21 C20 Sb1 117.8(3) . . ?
C25 C20 Sb1 122.5(3) . . ?
C20 C21 C22 120.3(4) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 120.0(4) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 119.9(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C20 119.7(4) . . ?
C24 C25 H25 120.1 . . ?
C20 C25 H25 120.1 . . ?
C35 C30 C31 119.4(3) . . ?
C35 C30 Sb1 122.1(2) . . ?
C31 C30 Sb1 118.3(2) . . ?
C32 C31 C30 120.1(4) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C31 120.1(4) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.3(4) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C33 C34 C35 120.1(4) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C30 C35 C34 120.0(3) . . ?
C30 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C41 C40 C45 120.2(3) . . ?
C41 C40 Sb1 119.1(2) . . ?
C45 C40 Sb1 120.7(2) . . ?
C40 C41 C42 120.4(3) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C43 C42 C41 119.1(3) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C42 C43 C44 120.8(3) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C45 C44 C43 120.0(3) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C45 C40 119.5(3) . . ?
C44 C45 H45 120.3 . . ?
C40 C45 H45 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 O6 C6 C7 -179.0(3) . . . . ?
C11 O6 C6 W1 0.2(5) . . . . ?
C10 N1 C7 C8 0.6(4) . . . . ?
C13 N1 C7 C8 176.5(4) . . . . ?
C10 N1 C7 C6 -179.8(3) . . . . ?
C13 N1 C7 C6 -3.8(6) . . . . ?
O6 C6 C7 C8 172.1(3) . . . . ?
W1 C6 C7 C8 -7.0(5) . . . . ?
O6 C6 C7 N1 -7.4(5) . . . . ?
W1 C6 C7 N1 173.4(3) . . . . ?
N1 C7 C8 C9 0.7(4) . . . . ?
C6 C7 C8 C9 -179.0(3) . . . . ?
C7 C8 C9 C10 -1.6(4) . . . . ?
C8 C9 C10 N1 2.0(5) . . . . ?
C7 N1 C10 C9 -1.6(5) . . . . ?
C13 N1 C10 C9 -177.8(4) . . . . ?
C6 O6 C11 C12 -165.0(3) . . . . ?
C25 C20 C21 C22 -0.1(5) . . . . ?
Sb1 C20 C21 C22 179.1(3) . . . . ?
C20 C21 C22 C23 0.7(6) . . . . ?
C21 C22 C23 C24 -0.9(6) . . . . ?
C22 C23 C24 C25 0.5(7) . . . . ?
C23 C24 C25 C20 0.0(6) . . . . ?
C21 C20 C25 C24 -0.2(5) . . . . ?
Sb1 C20 C25 C24 -179.4(3) . . . . ?
C35 C30 C31 C32 1.7(5) . . . . ?
Sb1 C30 C31 C32 -172.6(3) . . . . ?
C30 C31 C32 C33 -1.3(6) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C32 C33 C34 C35 1.3(6) . . . . ?
C31 C30 C35 C34 -0.6(5) . . . . ?
Sb1 C30 C35 C34 173.5(3) . . . . ?
C33 C34 C35 C30 -0.8(6) . . . . ?
C45 C40 C41 C42 -1.5(5) . . . . ?
Sb1 C40 C41 C42 -178.6(3) . . . . ?
C40 C41 C42 C43 2.1(5) . . . . ?
C41 C42 C43 C44 -1.5(5) . . . . ?
C42 C43 C44 C45 0.1(5) . . . . ?
C43 C44 C45 C40 0.5(5) . . . . ?
C41 C40 C45 C44 0.1(5) . . . . ?
Sb1 C40 C45 C44 177.2(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C10 H10 O1 0.95 2.48 3.267(5) 140.4 1_454
C13 H13A O6 0.98 1.93 2.667(5) 129.7 .
C13 H13B O3 0.98 2.63 3.450(5) 140.9 3_665

_refine_diff_density_max         1.396
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.099

