# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1478314'
_audit_update_record             
;
2016-05-05 deposited with the CCDC.
2016-09-28 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         'C31 H54 N2 Pd S7'
_chemical_formula_sum            'C31 H54 N2 Pd S7'
_chemical_formula_weight         785.58

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.750(10)
_cell_length_b                   16.11(2)
_cell_length_c                   14.900(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.390(10)
_cell_angle_gamma                90
_cell_volume                     3757(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    826
_cell_measurement_theta_min      1.301
_cell_measurement_theta_max      22.028

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_absorpt_coefficient_mu    0.906
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.606
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'TWINABS Bruker AXS Version 2008/4'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed tube'
_diffrn_measurement_device_type  'Bruker Smart APEXII CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4541
_diffrn_reflns_av_unetI/netI     0.2339
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.301
_diffrn_reflns_theta_max         22.028
_diffrn_reflns_theta_full        22.028
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             4541
_reflns_number_gt                1823
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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.
 The crystals under investigation were identified as non-merohedral twins
 using RLATT. Integration of the data was performed with SAINT-Plus using
 both orientation matrices. 3184 reflections involved only the first 
 orientation matrix, 3009 reflections involved the second orientation matrix,
 whereas 17377 reflections were overlapping reflections involving both domains.
 The absorption correction was applied using the program TWINABS, and each
 component was scaled separately.

;

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir97
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0849P)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         4541
_refine_ls_number_parameters     207
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.2472
_refine_ls_R_factor_gt           0.0970
_refine_ls_wR_factor_ref         0.2407
_refine_ls_wR_factor_gt          0.1802
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Pd Pd 0.5002(3) 0.14674(7) 0.13212(11) 0.0493(5) Uani 1 1 d . . . . .
S12 S 0.6015(6) 0.0470(6) 0.1451(7) 0.051(3) Uani 1 1 d D . . . .
S22 S 0.4000(6) 0.0433(6) 0.1208(7) 0.058(3) Uani 1 1 d D . . . .
S11 S 0.6008(6) 0.2469(7) 0.1368(6) 0.051(3) Uani 1 1 d D . . . .
S31 S 0.5870(8) 0.4331(7) 0.1260(7) 0.069(4) Uani 1 1 d D . . . .
S41 S 0.4049(7) 0.4333(6) 0.1076(6) 0.051(3) Uani 1 1 d D . . . .
S51 S 0.4980(11) 0.5945(2) 0.1202(4) 0.075(2) Uani 1 1 d D . . . .
S21 S 0.3929(7) 0.2447(7) 0.1176(7) 0.066(4) Uani 1 1 d D . . . .
C42 C 0.5440(17) -0.1963(17) 0.1464(17) 0.042(8) Uiso 1 1 d . U . . .
H30A H 0.5748 -0.2327 0.1093 0.050 Uiso 1 1 calc R U . . .
H30B H 0.5470 -0.2211 0.2060 0.050 Uiso 1 1 calc R U . . .
C12 C 0.5494(16) -0.0436(13) 0.140(3) 0.071(12) Uiso 1 1 d D U . . .
C22 C 0.4559(13) -0.0462(10) 0.1220(17) 0.018(7) Uiso 1 1 d D U . . .
N12 N 0.5889(15) -0.1158(15) 0.1545(14) 0.047(7) Uiso 1 1 d D . . . .
C52 C 0.6822(13) -0.1220(14) 0.1709(14) 0.034(6) Uiso 1 1 d . . . . .
H5A H 0.6974 -0.1726 0.2041 0.041 Uiso 1 1 calc R U . . .
H5B H 0.7040 -0.0755 0.2080 0.041 Uiso 1 1 calc R U . . .
C62 C 0.7230(14) -0.1221(15) 0.0862(15) 0.052(7) Uiso 1 1 d . . . . .
H6A H 0.7048 -0.1718 0.0526 0.062 Uiso 1 1 calc R U . . .
H6B H 0.7014 -0.0749 0.0503 0.062 Uiso 1 1 calc R U . . .
C32 C 0.4565(18) -0.1944(19) 0.1090(18) 0.051(9) Uiso 1 1 d . U . . .
H8A H 0.4254 -0.2334 0.1427 0.061 Uiso 1 1 calc R U . . .
H8B H 0.4535 -0.2149 0.0475 0.061 Uiso 1 1 calc R U . . .
N22 N 0.4122(14) -0.1169(13) 0.1069(12) 0.037(6) Uiso 1 1 d D . . . .
C172 C 0.3207(17) -0.1198(18) 0.0816(18) 0.064(8) Uiso 1 1 d . . . . .
H10A H 0.3057 -0.1695 0.0465 0.076 Uiso 1 1 calc R U . . .
H10B H 0.3025 -0.0719 0.0450 0.076 Uiso 1 1 calc R U . . .
C11 C 0.5351(13) 0.3347(10) 0.1306(18) 0.028(8) Uiso 1 1 d D . . . .
C31 C 0.4954(13) 0.4916(7) 0.1188(13) 0.045(4) Uiso 1 1 d D . . . .
C21 C 0.4488(13) 0.3354(10) 0.1107(19) 0.047(10) Uiso 1 1 d D . . . .
C202 C 0.1469(17) -0.1187(17) 0.2484(17) 0.075(9) Uiso 1 1 d . . . . .
H35A H 0.1690 -0.0704 0.2821 0.090 Uiso 1 1 calc R U . . .
H35B H 0.1711 -0.1673 0.2802 0.090 Uiso 1 1 calc R U . . .
C192 C 0.1793(16) -0.1163(16) 0.1587(17) 0.066(8) Uiso 1 1 d . . . . .
H34A H 0.1604 -0.0656 0.1276 0.079 Uiso 1 1 calc R U . . .
H34B H 0.1562 -0.1629 0.1225 0.079 Uiso 1 1 calc R U . . .
C72 C 0.8169(17) -0.1190(17) 0.0952(16) 0.072(9) Uiso 1 1 d . . . . .
H32A H 0.8398 -0.1659 0.1308 0.087 Uiso 1 1 calc R U . . .
H32B H 0.8363 -0.0686 0.1268 0.087 Uiso 1 1 calc R U . . .
C82 C 0.8510(19) -0.1209(19) 0.0004(19) 0.088(10) Uiso 1 1 d . . . . .
H36A H 0.8277 -0.1702 -0.0307 0.105 Uiso 1 1 calc R U . . .
H36B H 0.8268 -0.0735 -0.0334 0.105 Uiso 1 1 calc R U . . .
C182 C 0.2761(15) -0.1203(16) 0.1687(16) 0.062(8) Uiso 1 1 d . . . . .
H33A H 0.2935 -0.1703 0.2021 0.074 Uiso 1 1 calc R U . . .
H33B H 0.2977 -0.0735 0.2054 0.074 Uiso 1 1 calc R U . . .
C232 C -0.0680(18) -0.122(2) 0.3603(18) 0.090(12) Uiso 1 1 d D . . . .
H39A H -0.0968 -0.0736 0.3316 0.108 Uiso 1 1 calc R U . . .
H39B H -0.0943 -0.1713 0.3333 0.108 Uiso 1 1 calc R U . . .
C222 C 0.031(2) -0.119(2) 0.347(2) 0.116(12) Uiso 1 1 d . . . . .
H38A H 0.0558 -0.0696 0.3752 0.139 Uiso 1 1 calc R U . . .
H38B H 0.0585 -0.1668 0.3778 0.139 Uiso 1 1 calc R U . . .
C212 C 0.047(2) -0.121(2) 0.251(2) 0.086(10) Uiso 1 1 d . . . . .
H37A H 0.0211 -0.0734 0.2192 0.103 Uiso 1 1 calc R U . . .
H37B H 0.0237 -0.1710 0.2218 0.103 Uiso 1 1 calc R U . . .
C122 C 1.078(2) -0.121(2) -0.208(2) 0.113(12) Uiso 1 1 d . . . . .
H3S1 H 1.0480 -0.1683 -0.2370 0.135 Uiso 1 1 calc R U . . .
H3S2 H 1.0500 -0.0715 -0.2342 0.135 Uiso 1 1 calc R U . . .
C132 C 1.166(2) -0.122(2) -0.232(2) 0.136(15) Uiso 1 1 d D . . . .
H2S1 H 1.1964 -0.1702 -0.2063 0.163 Uiso 1 1 calc R U . . .
H2S2 H 1.1965 -0.0726 -0.2089 0.163 Uiso 1 1 calc R U . . .
C142 C 1.164(2) -0.124(2) -0.3355(19) 0.119(13) Uiso 1 1 d D . . . .
H1S1 H 1.1365 -0.1756 -0.3576 0.143 Uiso 1 1 calc R U . . .
H1S2 H 1.1285 -0.0786 -0.3610 0.143 Uiso 1 1 calc R U . . .
C162 C 1.242(2) -0.131(3) -0.468(2) 0.131(16) Uiso 1 1 d D . . . .
H4S1 H 1.2226 -0.1860 -0.4825 0.196 Uiso 1 1 calc R U . . .
H4S2 H 1.2972 -0.1224 -0.4881 0.196 Uiso 1 1 calc R U . . .
H4S3 H 1.2023 -0.0914 -0.4970 0.196 Uiso 1 1 calc R U . . .
C112 C 1.0632(19) -0.123(2) -0.106(2) 0.092(12) Uiso 1 1 d . . . . .
H6S1 H 1.0882 -0.1729 -0.0776 0.110 Uiso 1 1 calc R U . . .
H6S2 H 1.0895 -0.0751 -0.0749 0.110 Uiso 1 1 calc R U . . .
C102 C 0.9709(16) -0.1223(16) -0.1020(16) 0.072(8) Uiso 1 1 d . . . . .
H7S1 H 0.9463 -0.1713 -0.1327 0.087 Uiso 1 1 calc R U . . .
H7S2 H 0.9469 -0.0741 -0.1345 0.087 Uiso 1 1 calc R U . . .
C262 C -0.161(2) -0.117(3) 0.583(2) 0.145(16) Uiso 1 1 d D . . . .
H42A H -0.1239 -0.1602 0.6108 0.174 Uiso 1 1 calc R U . . .
H42B H -0.1365 -0.0639 0.6014 0.174 Uiso 1 1 calc R U . . .
C252 C -0.1650(19) -0.125(3) 0.481(2) 0.142(15) Uiso 1 1 d D . . . .
H41A H -0.1907 -0.1772 0.4606 0.170 Uiso 1 1 calc R U . . .
H41B H -0.1982 -0.0798 0.4515 0.170 Uiso 1 1 calc R U . . .
C152 C 1.248(2) -0.118(3) -0.367(2) 0.153(19) Uiso 1 1 d D . . . .
H5S1 H 1.2857 -0.1605 -0.3374 0.183 Uiso 1 1 calc R U . . .
H5S2 H 1.2730 -0.0645 -0.3518 0.183 Uiso 1 1 calc R U . . .
C242 C -0.0748(18) -0.120(2) 0.4610(18) 0.111(12) Uiso 1 1 d D . . . .
H40A H -0.0434 -0.1672 0.4890 0.133 Uiso 1 1 calc R U . . .
H40B H -0.0489 -0.0700 0.4868 0.133 Uiso 1 1 calc R U . . .
C282 C -0.243(2) -0.134(3) 0.712(2) 0.127(15) Uiso 1 1 d . . . . .
H45A H -0.2152 -0.1856 0.7300 0.191 Uiso 1 1 calc R U . . .
H45B H -0.3003 -0.1351 0.7292 0.191 Uiso 1 1 calc R U . . .
H45C H -0.2122 -0.0889 0.7412 0.191 Uiso 1 1 calc R U . . .
C92 C 0.9451(19) -0.120(2) -0.006(2) 0.084(11) Uiso 1 1 d . . . . .
H43A H 0.9703 -0.1682 0.0264 0.100 Uiso 1 1 calc R U . . .
H43B H 0.9694 -0.0712 0.0239 0.100 Uiso 1 1 calc R U . . .
C272 C -0.247(3) -0.125(3) 0.614(3) 0.17(2) Uiso 1 1 d D . . . .
H44A H -0.2803 -0.0759 0.5953 0.206 Uiso 1 1 calc R U . . .
H44B H -0.2760 -0.1725 0.5846 0.206 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
Pd S11 2.257(11) . ?
Pd S12 2.258(11) . ?
Pd S22 2.288(11) . ?
Pd S21 2.304(11) . ?
S12 C12 1.671(16) . ?
S22 C22 1.689(14) . ?
S11 C11 1.749(14) . ?
S31 C31 1.717(15) . ?
S31 C11 1.79(2) . ?
S41 C31 1.700(15) . ?
S41 C21 1.721(17) . ?
S51 C31 1.658(12) . ?
S21 C21 1.715(15) . ?
C42 C32 1.43(2) . ?
C42 N12 1.48(3) . ?
C42 H30A 0.9700 . ?
C42 H30B 0.9700 . ?
C12 N12 1.325(17) . ?
C12 C22 1.468(15) . ?
C22 N22 1.336(15) . ?
N12 C52 1.47(3) . ?
C52 C62 1.48(3) . ?
C52 H5A 0.9700 . ?
C52 H5B 0.9700 . ?
C62 C72 1.47(3) . ?
C62 H6A 0.9700 . ?
C62 H6B 0.9700 . ?
C32 N22 1.43(3) . ?
C32 H8A 0.9700 . ?
C32 H8B 0.9700 . ?
N22 C172 1.45(3) . ?
C172 C182 1.54(3) . ?
C172 H10A 0.9700 . ?
C172 H10B 0.9700 . ?
C11 C21 1.359(15) . ?
C202 C192 1.48(3) . ?
C202 C212 1.57(4) . ?
C202 H35A 0.9700 . ?
C202 H35B 0.9700 . ?
C192 C182 1.52(3) . ?
C192 H34A 0.9700 . ?
C192 H34B 0.9700 . ?
C72 C82 1.57(4) . ?
C72 H32A 0.9700 . ?
C72 H32B 0.9700 . ?
C82 C92 1.50(4) . ?
C82 H36A 0.9700 . ?
C82 H36B 0.9700 . ?
C182 H33A 0.9700 . ?
C182 H33B 0.9700 . ?
C232 C242 1.516(18) . ?
C232 C222 1.59(4) . ?
C232 H39A 0.9700 . ?
C232 H39B 0.9700 . ?
C222 C212 1.49(4) . ?
C222 H38A 0.9700 . ?
C222 H38B 0.9700 . ?
C212 H37A 0.9700 . ?
C212 H37B 0.9700 . ?
C122 C132 1.48(4) . ?
C122 C112 1.56(4) . ?
C122 H3S1 0.9700 . ?
C122 H3S2 0.9700 . ?
C132 C142 1.533(18) . ?
C132 H2S1 0.9700 . ?
C132 H2S2 0.9700 . ?
C142 C152 1.469(19) . ?
C142 H1S1 0.9700 . ?
C142 H1S2 0.9700 . ?
C162 C152 1.503(19) . ?
C162 H4S1 0.9600 . ?
C162 H4S2 0.9600 . ?
C162 H4S3 0.9600 . ?
C112 C102 1.46(3) . ?
C112 H6S1 0.9700 . ?
C112 H6S2 0.9700 . ?
C102 C92 1.53(4) . ?
C102 H7S1 0.9700 . ?
C102 H7S2 0.9700 . ?
C262 C272 1.486(19) . ?
C262 C252 1.514(18) . ?
C262 H42A 0.9700 . ?
C262 H42B 0.9700 . ?
C252 C242 1.485(18) . ?
C252 H41A 0.9700 . ?
C252 H41B 0.9700 . ?
C152 H5S1 0.9700 . ?
C152 H5S2 0.9700 . ?
C242 H40A 0.9700 . ?
C242 H40B 0.9700 . ?
C282 C272 1.47(4) . ?
C282 H45A 0.9600 . ?
C282 H45B 0.9600 . ?
C282 H45C 0.9600 . ?
C92 H43A 0.9700 . ?
C92 H43B 0.9700 . ?
C272 H44A 0.9700 . ?
C272 H44B 0.9700 . ?

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
S11 Pd S12 91.1(4) . . ?
S11 Pd S22 177.3(4) . . ?
S12 Pd S22 87.88(18) . . ?
S11 Pd S21 91.02(19) . . ?
S12 Pd S21 177.8(4) . . ?
S22 Pd S21 90.0(4) . . ?
C12 S12 Pd 106.2(11) . . ?
C22 S22 Pd 105.5(9) . . ?
C11 S11 Pd 99.7(8) . . ?
C31 S31 C11 96.0(9) . . ?
C31 S41 C21 100.0(9) . . ?
C21 S21 Pd 102.3(9) . . ?
C32 C42 N12 116(3) . . ?
C32 C42 H30A 108.2 . . ?
N12 C42 H30A 108.2 . . ?
C32 C42 H30B 108.2 . . ?
N12 C42 H30B 108.2 . . ?
H30A C42 H30B 107.3 . . ?
N12 C12 C22 117(2) . . ?
N12 C12 S12 123(2) . . ?
C22 C12 S12 121(2) . . ?
N22 C22 C12 122.9(19) . . ?
N22 C22 S22 117.9(18) . . ?
C12 C22 S22 119.2(19) . . ?
C12 N12 C52 122(2) . . ?
C12 N12 C42 123(2) . . ?
C52 N12 C42 115(2) . . ?
N12 C52 C62 112.4(19) . . ?
N12 C52 H5A 109.1 . . ?
C62 C52 H5A 109.1 . . ?
N12 C52 H5B 109.1 . . ?
C62 C52 H5B 109.1 . . ?
H5A C52 H5B 107.9 . . ?
C72 C62 C52 116.8(19) . . ?
C72 C62 H6A 108.1 . . ?
C52 C62 H6A 108.1 . . ?
C72 C62 H6B 108.1 . . ?
C52 C62 H6B 108.1 . . ?
H6A C62 H6B 107.3 . . ?
C42 C32 N22 118(3) . . ?
C42 C32 H8A 107.7 . . ?
N22 C32 H8A 107.7 . . ?
C42 C32 H8B 107.7 . . ?
N22 C32 H8B 107.7 . . ?
H8A C32 H8B 107.1 . . ?
C22 N22 C32 120(2) . . ?
C22 N22 C172 123(2) . . ?
C32 N22 C172 116(2) . . ?
N22 C172 C182 108(2) . . ?
N22 C172 H10A 110.0 . . ?
C182 C172 H10A 110.0 . . ?
N22 C172 H10B 110.0 . . ?
C182 C172 H10B 110.0 . . ?
H10A C172 H10B 108.4 . . ?
C21 C11 S11 126.1(18) . . ?
C21 C11 S31 115.8(15) . . ?
S11 C11 S31 116.7(13) . . ?
S51 C31 S41 124.9(14) . . ?
S51 C31 S31 122.0(13) . . ?
S41 C31 S31 113.1(7) . . ?
C11 C21 S21 119.2(18) . . ?
C11 C21 S41 113.7(15) . . ?
S21 C21 S41 125.1(14) . . ?
C192 C202 C212 118(2) . . ?
C192 C202 H35A 107.9 . . ?
C212 C202 H35A 107.9 . . ?
C192 C202 H35B 107.9 . . ?
C212 C202 H35B 107.9 . . ?
H35A C202 H35B 107.2 . . ?
C202 C192 C182 111(2) . . ?
C202 C192 H34A 109.5 . . ?
C182 C192 H34A 109.5 . . ?
C202 C192 H34B 109.5 . . ?
C182 C192 H34B 109.5 . . ?
H34A C192 H34B 108.1 . . ?
C62 C72 C82 111(2) . . ?
C62 C72 H32A 109.4 . . ?
C82 C72 H32A 109.4 . . ?
C62 C72 H32B 109.4 . . ?
C82 C72 H32B 109.4 . . ?
H32A C72 H32B 108.0 . . ?
C92 C82 C72 120(2) . . ?
C92 C82 H36A 107.3 . . ?
C72 C82 H36A 107.3 . . ?
C92 C82 H36B 107.3 . . ?
C72 C82 H36B 107.3 . . ?
H36A C82 H36B 106.9 . . ?
C192 C182 C172 118(2) . . ?
C192 C182 H33A 107.9 . . ?
C172 C182 H33A 107.9 . . ?
C192 C182 H33B 107.9 . . ?
C172 C182 H33B 107.9 . . ?
H33A C182 H33B 107.2 . . ?
C242 C232 C222 108(2) . . ?
C242 C232 H39A 110.2 . . ?
C222 C232 H39A 110.2 . . ?
C242 C232 H39B 110.2 . . ?
C222 C232 H39B 110.2 . . ?
H39A C232 H39B 108.5 . . ?
C212 C222 C232 114(3) . . ?
C212 C222 H38A 108.8 . . ?
C232 C222 H38A 108.8 . . ?
C212 C222 H38B 108.8 . . ?
C232 C222 H38B 108.8 . . ?
H38A C222 H38B 107.7 . . ?
C222 C212 C202 108(3) . . ?
C222 C212 H37A 110.1 . . ?
C202 C212 H37A 110.1 . . ?
C222 C212 H37B 110.1 . . ?
C202 C212 H37B 110.1 . . ?
H37A C212 H37B 108.4 . . ?
C132 C122 C112 119(3) . . ?
C132 C122 H3S1 107.6 . . ?
C112 C122 H3S1 107.6 . . ?
C132 C122 H3S2 107.6 . . ?
C112 C122 H3S2 107.6 . . ?
H3S1 C122 H3S2 107.0 . . ?
C122 C132 C142 109(3) . . ?
C122 C132 H2S1 109.9 . . ?
C142 C132 H2S1 109.9 . . ?
C122 C132 H2S2 109.9 . . ?
C142 C132 H2S2 109.9 . . ?
H2S1 C132 H2S2 108.3 . . ?
C152 C142 C132 113(3) . . ?
C152 C142 H1S1 108.9 . . ?
C132 C142 H1S1 108.9 . . ?
C152 C142 H1S2 108.9 . . ?
C132 C142 H1S2 108.9 . . ?
H1S1 C142 H1S2 107.7 . . ?
C152 C162 H4S1 109.5 . . ?
C152 C162 H4S2 109.5 . . ?
H4S1 C162 H4S2 109.5 . . ?
C152 C162 H4S3 109.5 . . ?
H4S1 C162 H4S3 109.5 . . ?
H4S2 C162 H4S3 109.5 . . ?
C102 C112 C122 107(3) . . ?
C102 C112 H6S1 110.3 . . ?
C122 C112 H6S1 110.3 . . ?
C102 C112 H6S2 110.3 . . ?
C122 C112 H6S2 110.3 . . ?
H6S1 C112 H6S2 108.6 . . ?
C112 C102 C92 114(2) . . ?
C112 C102 H7S1 108.7 . . ?
C92 C102 H7S1 108.7 . . ?
C112 C102 H7S2 108.7 . . ?
C92 C102 H7S2 108.7 . . ?
H7S1 C102 H7S2 107.6 . . ?
C272 C262 C252 111(3) . . ?
C272 C262 H42A 109.3 . . ?
C252 C262 H42A 109.3 . . ?
C272 C262 H42B 109.3 . . ?
C252 C262 H42B 109.3 . . ?
H42A C262 H42B 108.0 . . ?
C242 C252 C262 105(3) . . ?
C242 C252 H41A 110.7 . . ?
C262 C252 H41A 110.7 . . ?
C242 C252 H41B 110.7 . . ?
C262 C252 H41B 110.7 . . ?
H41A C252 H41B 108.8 . . ?
C142 C152 C162 110(3) . . ?
C142 C152 H5S1 109.6 . . ?
C162 C152 H5S1 109.6 . . ?
C142 C152 H5S2 109.6 . . ?
C162 C152 H5S2 109.6 . . ?
H5S1 C152 H5S2 108.1 . . ?
C252 C242 C232 112(2) . . ?
C252 C242 H40A 109.2 . . ?
C232 C242 H40A 109.2 . . ?
C252 C242 H40B 109.2 . . ?
C232 C242 H40B 109.2 . . ?
H40A C242 H40B 107.9 . . ?
C272 C282 H45A 109.5 . . ?
C272 C282 H45B 109.5 . . ?
H45A C282 H45B 109.5 . . ?
C272 C282 H45C 109.5 . . ?
H45A C282 H45C 109.5 . . ?
H45B C282 H45C 109.5 . . ?
C82 C92 C102 115(3) . . ?
C82 C92 H43A 108.4 . . ?
C102 C92 H43A 108.4 . . ?
C82 C92 H43B 108.4 . . ?
C102 C92 H43B 108.4 . . ?
H43A C92 H43B 107.5 . . ?
C282 C272 C262 113(3) . . ?
C282 C272 H44A 109.1 . . ?
C262 C272 H44A 109.1 . . ?
C282 C272 H44B 109.1 . . ?
C262 C272 H44B 109.1 . . ?
H44A C272 H44B 107.8 . . ?

_refine_diff_density_max         0.842
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.127


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method acetonitrile
