# 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_z
_database_code_depnum_ccdc_archive 'CCDC 1513084'
_audit_update_record             
;
2016-10-30 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 N2 Ni O14 S2'
_chemical_formula_weight         959.74

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   25.53(3)
_cell_length_b                   11.192(12)
_cell_length_c                   8.628(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.324(14)
_cell_angle_gamma                90.00
_cell_volume                     2464(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4266
_cell_measurement_theta_min      2.3943
_cell_measurement_theta_max      22.9903

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1012
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8948
_exptl_absorpt_correction_T_max  0.9041
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  bruker-CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19078
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4344
_reflns_number_gt                3109
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0859P)²+0.3193P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4344
_refine_ls_number_parameters     335
_refine_ls_number_restraints     237
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1506
_refine_ls_wR_factor_gt          0.1361
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 1.0000 0.0280(2) Uani 1 2 d S . .
O1 O 0.00975(10) 0.4254(2) 0.7839(2) 0.0387(6) Uani 1 1 d D . .
H1A H -0.0168(7) 0.437(4) 0.731(3) 0.058 Uiso 1 1 d D . .
H1B H 0.0375(6) 0.445(4) 0.746(4) 0.058 Uiso 1 1 d D . .
O2 O -0.02100(10) 0.6626(2) 0.9023(3) 0.0420(6) Uani 1 1 d D . .
H2A H -0.0325(15) 0.715(3) 0.959(3) 0.063 Uiso 1 1 d D . .
H2B H -0.0291(14) 0.669(3) 0.8104(14) 0.063 Uiso 1 1 d D . .
O3 O 0.27071(14) 0.5988(4) 0.9800(5) 0.0977(12) Uani 1 1 d U . .
O4 O 0.25161(14) 0.7640(4) 1.1161(6) 0.1144(15) Uani 1 1 d . . .
N1 N 0.07824(11) 0.5593(2) 1.0104(3) 0.0353(7) Uani 1 1 d . . .
C1 C 0.11773(14) 0.4852(3) 0.9763(4) 0.0408(9) Uani 1 1 d . . .
H1 H 0.1093 0.4062 0.9441 0.049 Uiso 1 1 calc R . .
C2 C 0.17012(16) 0.5176(3) 0.9857(5) 0.0502(10) Uani 1 1 d . . .
H2 H 0.1969 0.4628 0.9588 0.060 Uiso 1 1 calc R . .
C3 C 0.18242(15) 0.6325(4) 1.0356(5) 0.0536(11) Uani 1 1 d . . .
C4 C 0.14178(16) 0.7083(4) 1.0723(5) 0.0598(11) Uani 1 1 d . . .
H4 H 0.1491 0.7868 1.1089 0.072 Uiso 1 1 calc R . .
C5 C 0.09113(16) 0.6705(3) 1.0560(5) 0.0499(10) Uani 1 1 d . . .
H5 H 0.0638 0.7251 1.0778 0.060 Uiso 1 1 calc R . .
C6 C 0.23790(19) 0.6736(5) 1.0516(7) 0.0780(15) Uani 1 1 d . . .
C7 C 0.3258(2) 0.6342(6) 0.9757(8) 0.1110(18) Uani 1 1 d U A .
H7A H 0.3418 0.6348 1.0814 0.133 Uiso 1 1 calc R . .
H7B H 0.3294 0.7149 0.9300 0.133 Uiso 1 1 calc R . .
C8 C 0.3518(3) 0.5412(8) 0.8755(10) 0.140(3) Uani 1 1 d DU . .
H8AA H 0.3315 0.5350 0.7767 0.168 Uiso 0.559(12) 1 calc PR A 1
H8AB H 0.3493 0.4630 0.9284 0.168 Uiso 0.559(12) 1 calc PR A 1
H8BC H 0.3399 0.5489 0.7659 0.168 Uiso 0.441(12) 1 d PR A 2
H8BD H 0.3439 0.4594 0.9119 0.168 Uiso 0.441(12) 1 d PR A 2
C9 C 0.4092(5) 0.563(2) 0.837(3) 0.200(5) Uani 0.559(12) 1 d PDU A 1
H9A H 0.4293 0.5849 0.9321 0.240 Uiso 0.559(12) 1 calc PR A 1
H9B H 0.4118 0.6288 0.7615 0.240 Uiso 0.559(12) 1 calc PR A 1
C10 C 0.4321(7) 0.445(2) 0.767(3) 0.199(5) Uani 0.559(12) 1 d PDU A 1
H10A H 0.4253 0.3764 0.8357 0.238 Uiso 0.559(12) 1 calc PR A 1
H10B H 0.4155 0.4286 0.6641 0.238 Uiso 0.559(12) 1 calc PR A 1
C11 C 0.4917(7) 0.4630(17) 0.750(3) 0.216(5) Uani 0.559(12) 1 d PDU A 1
H11A H 0.5082 0.4908 0.8486 0.259 Uiso 0.559(12) 1 calc PR A 1
H11B H 0.4992 0.5213 0.6672 0.259 Uiso 0.559(12) 1 calc PR A 1
C12 C 0.5110(9) 0.3364(18) 0.707(3) 0.222(8) Uani 0.559(12) 1 d PDU A 1
H12A H 0.5491 0.3376 0.6963 0.333 Uiso 0.559(12) 1 calc PR A 1
H12B H 0.4943 0.3115 0.6089 0.333 Uiso 0.559(12) 1 calc PR A 1
H12C H 0.5018 0.2801 0.7891 0.333 Uiso 0.559(12) 1 calc PR A 1
C9B C 0.4111(5) 0.570(3) 0.892(3) 0.201(6) Uani 0.441(12) 1 d PDU A 2
H9BA H 0.4273 0.5278 0.9823 0.242 Uiso 0.441(12) 1 calc PR A 2
H9BB H 0.4173 0.6567 0.9028 0.242 Uiso 0.441(12) 1 calc PR A 2
C10B C 0.4320(13) 0.521(2) 0.735(3) 0.223(6) Uani 0.441(12) 1 d PDU A 2
H10C H 0.4043 0.5072 0.6551 0.267 Uiso 0.441(12) 1 calc PR A 2
H10D H 0.4612 0.5679 0.6933 0.267 Uiso 0.441(12) 1 calc PR A 2
C11B C 0.4498(11) 0.406(2) 0.821(3) 0.205(6) Uani 0.441(12) 1 d PDU A 2
H11C H 0.4205 0.3541 0.8526 0.246 Uiso 0.441(12) 1 calc PR A 2
H11D H 0.4748 0.4202 0.9081 0.246 Uiso 0.441(12) 1 calc PR A 2
C12B C 0.4767(13) 0.363(3) 0.667(3) 0.244(8) Uani 0.441(12) 1 d PDU A 2
H12D H 0.4922 0.2840 0.6835 0.366 Uiso 0.441(12) 1 calc PR A 2
H12E H 0.5042 0.4200 0.6398 0.366 Uiso 0.441(12) 1 calc PR A 2
H12F H 0.4504 0.3593 0.5826 0.366 Uiso 0.441(12) 1 calc PR A 2
S1 S 0.09723(3) 0.43453(8) 0.45464(9) 0.0374(3) Uani 1 1 d . . .
O5 O 0.08238(10) 0.5480(2) 0.3852(3) 0.0489(7) Uani 1 1 d . . .
O6 O 0.10311(10) 0.4398(3) 0.6217(3) 0.0575(8) Uani 1 1 d . . .
O7 O 0.06281(10) 0.3373(2) 0.4042(3) 0.0533(7) Uani 1 1 d . . .
C13 C 0.16055(15) 0.3983(3) 0.3850(4) 0.0423(9) Uani 1 1 d . . .
C14 C 0.16680(19) 0.2971(4) 0.2882(5) 0.0590(11) Uani 1 1 d . . .
H14 H 0.1372 0.2503 0.2586 0.071 Uiso 1 1 calc R . .
C15 C 0.2152(2) 0.2669(5) 0.2375(6) 0.0803(15) Uani 1 1 d . . .
H15 H 0.2189 0.1984 0.1737 0.096 Uiso 1 1 calc R . .
C16 C 0.2584(2) 0.3328(5) 0.2763(6) 0.0732(13) Uani 1 1 d . . .
C17 C 0.3105(3) 0.3003(7) 0.2239(9) 0.116(2) Uani 1 1 d . . .
H17 H 0.3146 0.2324 0.1592 0.139 Uiso 1 1 calc R . .
C18 C 0.3519(3) 0.3642(9) 0.2655(11) 0.137(3) Uani 1 1 d . . .
H18 H 0.3856 0.3423 0.2303 0.164 Uiso 1 1 calc R . .
C19 C 0.3465(3) 0.4638(8) 0.3609(12) 0.145(3) Uani 1 1 d . . .
H19 H 0.3768 0.5086 0.3902 0.174 Uiso 1 1 calc R . .
C20 C 0.2981(2) 0.4988(5) 0.4140(9) 0.109(2) Uani 1 1 d . . .
H20 H 0.2953 0.5667 0.4792 0.130 Uiso 1 1 calc R . .
C21 C 0.25411(19) 0.4341(4) 0.3715(6) 0.0674(13) Uani 1 1 d . . .
C22 C 0.20250(17) 0.4661(4) 0.4257(5) 0.0572(11) Uani 1 1 d . . .
H22 H 0.1982 0.5345 0.4894 0.069 Uiso 1 1 calc R . .


_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
Ni1 O1 2.063(3) 3_567 ?
Ni1 O1 2.063(3) . ?
Ni1 O2 2.071(3) 3_567 ?
Ni1 O2 2.071(3) . ?
Ni1 N1 2.104(3) 3_567 ?
Ni1 N1 2.104(3) . ?
O1 H1A 0.817(10) . ?
O1 H1B 0.817(10) . ?
O2 H2A 0.824(10) . ?
O2 H2B 0.818(10) . ?
O3 C6 1.344(7) . ?
O3 C7 1.463(6) . ?
O4 C6 1.203(6) . ?
N1 C1 1.343(5) . ?
N1 C5 1.344(5) . ?
C1 C2 1.386(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(6) . ?
C3 C6 1.492(6) . ?
C4 C5 1.365(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C7 C8 1.516(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.527(10) . ?
C8 C9B 1.550(10) . ?
C8 H8AA 0.9900 . ?
C8 H8AB 0.9900 . ?
C8 H8BC 0.9901 . ?
C8 H8BD 0.9900 . ?
C9 C10 1.569(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.544(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.548(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C9B C10B 1.568(10) . ?
C9B H9BA 0.9900 . ?
C9B H9BB 0.9900 . ?
C10B C11B 1.544(10) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11B C12B 1.579(10) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
S1 O6 1.447(3) . ?
S1 O5 1.451(3) . ?
S1 O7 1.459(3) . ?
S1 C13 1.784(4) . ?
C13 C22 1.353(5) . ?
C13 C14 1.418(5) . ?
C14 C15 1.362(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.362(7) . ?
C15 H15 0.9500 . ?
C16 C21 1.406(7) . ?
C16 C17 1.460(8) . ?
C17 C18 1.319(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.379(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.453(6) . ?
C22 H22 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
O1 Ni1 O1 180.0 3_567 . ?
O1 Ni1 O2 91.35(11) 3_567 3_567 ?
O1 Ni1 O2 88.65(11) . 3_567 ?
O1 Ni1 O2 88.65(11) 3_567 . ?
O1 Ni1 O2 91.35(11) . . ?
O2 Ni1 O2 180.0 3_567 . ?
O1 Ni1 N1 91.82(10) 3_567 3_567 ?
O1 Ni1 N1 88.18(10) . 3_567 ?
O2 Ni1 N1 88.66(11) 3_567 3_567 ?
O2 Ni1 N1 91.34(11) . 3_567 ?
O1 Ni1 N1 88.18(10) 3_567 . ?
O1 Ni1 N1 91.82(10) . . ?
O2 Ni1 N1 91.34(11) 3_567 . ?
O2 Ni1 N1 88.66(11) . . ?
N1 Ni1 N1 180.00(5) 3_567 . ?
Ni1 O1 H1A 109(3) . . ?
Ni1 O1 H1B 112(3) . . ?
H1A O1 H1B 116.6(19) . . ?
Ni1 O2 H2A 119(2) . . ?
Ni1 O2 H2B 122(2) . . ?
H2A O2 H2B 115.0(19) . . ?
C6 O3 C7 116.9(5) . . ?
C1 N1 C5 117.1(3) . . ?
C1 N1 Ni1 120.8(2) . . ?
C5 N1 Ni1 122.0(3) . . ?
N1 C1 C2 123.6(3) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 118.1(4) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 118.3(4) . . ?
C4 C3 C6 120.3(4) . . ?
C2 C3 C6 121.4(4) . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 122.9(4) . . ?
N1 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
O4 C6 O3 124.0(5) . . ?
O4 C6 C3 124.6(5) . . ?
O3 C6 C3 111.4(5) . . ?
O3 C7 C8 105.2(5) . . ?
O3 C7 H7A 110.7 . . ?
C8 C7 H7A 110.7 . . ?
O3 C7 H7B 110.7 . . ?
C8 C7 H7B 110.7 . . ?
H7A C7 H7B 108.8 . . ?
C7 C8 C9 116.8(10) . . ?
C7 C8 C9B 104.1(12) . . ?
C9 C8 C9B 18.1(16) . . ?
C7 C8 H8AA 108.1 . . ?
C9 C8 H8AA 108.1 . . ?
C9B C8 H8AA 125.9 . . ?
C7 C8 H8AB 108.1 . . ?
C9 C8 H8AB 108.1 . . ?
C9B C8 H8AB 102.2 . . ?
H8AA C8 H8AB 107.3 . . ?
C7 C8 H8BC 110.9 . . ?
C9 C8 H8BC 93.0 . . ?
C9B C8 H8BC 110.4 . . ?
H8AA C8 H8BC 16.5 . . ?
H8AB C8 H8BC 119.8 . . ?
C7 C8 H8BD 111.0 . . ?
C9 C8 H8BD 114.7 . . ?
C9B C8 H8BD 111.5 . . ?
H8AA C8 H8BD 95.8 . . ?
H8AB C8 H8BD 11.6 . . ?
H8BC C8 H8BD 108.9 . . ?
C8 C9 C10 108.7(15) . . ?
C8 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C11 C10 C9 107.7(15) . . ?
C11 C10 H10A 110.2 . . ?
C9 C10 H10A 110.2 . . ?
C11 C10 H10B 110.2 . . ?
C9 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C10 C11 C12 102.8(16) . . ?
C10 C11 H11A 111.2 . . ?
C12 C11 H11A 111.2 . . ?
C10 C11 H11B 111.2 . . ?
C12 C11 H11B 111.2 . . ?
H11A C11 H11B 109.1 . . ?
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 . . ?
C8 C9B C10B 101.4(18) . . ?
C8 C9B H9BA 111.5 . . ?
C10B C9B H9BA 111.5 . . ?
C8 C9B H9BB 111.5 . . ?
C10B C9B H9BB 111.5 . . ?
H9BA C9B H9BB 109.3 . . ?
C11B C10B C9B 89(2) . . ?
C11B C10B H10C 113.8 . . ?
C9B C10B H10C 113.8 . . ?
C11B C10B H10D 113.8 . . ?
C9B C10B H10D 113.8 . . ?
H10C C10B H10D 111.0 . . ?
C10B C11B C12B 89(2) . . ?
C10B C11B H11C 113.8 . . ?
C12B C11B H11C 113.8 . . ?
C10B C11B H11D 113.8 . . ?
C12B C11B H11D 113.8 . . ?
H11C C11B H11D 111.1 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
O6 S1 O5 113.32(18) . . ?
O6 S1 O7 112.05(16) . . ?
O5 S1 O7 112.34(16) . . ?
O6 S1 C13 105.71(16) . . ?
O5 S1 C13 106.87(16) . . ?
O7 S1 C13 105.89(18) . . ?
C22 C13 C14 120.1(4) . . ?
C22 C13 S1 120.2(3) . . ?
C14 C13 S1 119.7(3) . . ?
C15 C14 C13 120.1(4) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 121.5(5) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C21 120.3(5) . . ?
C15 C16 C17 121.9(6) . . ?
C21 C16 C17 117.8(6) . . ?
C18 C17 C16 120.7(7) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.3(7) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 121.5(8) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C21 C20 C19 119.4(7) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C16 120.3(5) . . ?
C20 C21 C22 121.6(5) . . ?
C16 C21 C22 118.1(4) . . ?
C13 C22 C21 119.7(4) . . ?
C13 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?

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
O1 H1A O5 0.817(10) 1.940(11) 2.755(4) 175(4) 3_566
O1 H1B O6 0.817(10) 2.011(18) 2.796(4) 161(4) .
O2 H2B O7 0.818(10) 2.025(14) 2.829(4) 167(4) 3_566
O2 H2A O7 0.824(10) 1.974(11) 2.798(4) 177(4) 2_556

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.075
_exptl_crystal_recrystallization_method 'Vapour deposition'
