# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_Ni-BMTMP

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H26 K2 Ni O13 S4'
_chemical_formula_weight         667.50

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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   7.3428(2)
_cell_length_b                   13.2262(3)
_cell_length_c                   13.8832(3)
_cell_angle_alpha                89.8360(10)
_cell_angle_beta                 83.4980(10)
_cell_angle_gamma                77.4130(10)
_cell_volume                     1307.10(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9273
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      28.22

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6406
_exptl_absorpt_correction_T_max  0.8464
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 Breeze CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21574
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.50
_reflns_number_total             5398
_reflns_number_gt                4584
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0445P)²+2.3914P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5398
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.52364(5) 0.99360(3) 0.75161(2) 0.01428(10) Uani 1 1 d . . .
K1 K 1.07086(8) 0.92350(5) 0.88538(5) 0.02090(15) Uani 1 1 d . . .
K2 K 1.02399(8) 0.94322(5) 0.36042(5) 0.02523(16) Uani 1 1 d . . .
S1 S 0.60412(12) 1.34573(6) 0.87983(7) 0.0333(2) Uani 1 1 d . . .
S2 S 0.21149(11) 1.33027(6) 0.96285(6) 0.03042(19) Uani 1 1 d . . .
S3 S 0.48012(15) 0.63464(7) 0.61958(9) 0.0493(3) Uani 1 1 d . . .
S4 S 0.85461(12) 0.67700(7) 0.53728(7) 0.0368(2) Uani 1 1 d . . .
O1 O 0.8277(3) 1.12087(15) 0.93125(14) 0.0205(4) Uani 1 1 d . . .
O2 O 0.7299(2) 1.05019(14) 0.80717(13) 0.0165(4) Uani 1 1 d . . .
O3 O 0.2672(3) 1.10511(16) 1.02067(13) 0.0207(4) Uani 1 1 d . . .
O4 O 0.3478(3) 1.03057(15) 0.87482(13) 0.0188(4) Uani 1 1 d . . .
O5 O 0.2116(3) 0.84553(16) 0.59114(15) 0.0236(4) Uani 1 1 d . . .
O6 O 0.3145(2) 0.93621(14) 0.69912(13) 0.0167(4) Uani 1 1 d . . .
O7 O 0.7168(3) 0.91550(16) 0.46991(14) 0.0230(4) Uani 1 1 d . . .
O8 O 0.6979(3) 0.95737(15) 0.62568(13) 0.0194(4) Uani 1 1 d . . .
O9 O 0.6239(3) 0.84972(15) 0.80850(14) 0.0204(4) Uani 1 1 d . . .
H9B H 0.7321 0.8295 0.7790 0.024 Uiso 1 1 d R . .
H9C H 0.6227 0.8293 0.8659 0.024 Uiso 1 1 d R . .
O10 O 0.4234(3) 1.13672(15) 0.68800(14) 0.0190(4) Uani 1 1 d . . .
H10B H 0.3783 1.1267 0.6321 0.023 Uiso 1 1 d R . .
H10C H 0.5123 1.1671 0.6754 0.023 Uiso 1 1 d R . .
O11 O 1.2953(3) 0.77518(18) 0.40326(17) 0.0349(5) Uani 1 1 d . . .
H11D H 1.2568 0.8088 0.3554 0.042 Uiso 1 1 d R . .
O12 O 1.0000(3) 0.77792(17) 0.74848(16) 0.0316(5) Uani 1 1 d . . .
H12D H 1.0569 0.7853 0.6938 0.038 Uiso 1 1 d R . .
O14 O 0.9586(3) 0.79377(19) 0.23736(18) 0.0384(6) Uani 1 1 d . . .
H14B H 0.8246 0.8188 0.2346 0.046 Uiso 1 1 d R . .
H14C H 0.9879 0.8088 0.1797 0.046 Uiso 1 1 d R . .
C1 C 0.7025(4) 1.1075(2) 0.88287(19) 0.0153(5) Uani 1 1 d . . .
C2 C 0.5004(4) 1.1630(2) 0.91557(19) 0.0158(5) Uani 1 1 d . . .
C3 C 0.3611(3) 1.0944(2) 0.93983(19) 0.0145(5) Uani 1 1 d . . .
C4 C 0.4448(4) 1.2662(2) 0.9180(2) 0.0202(6) Uani 1 1 d . . .
C5 C 0.6685(6) 1.3761(3) 0.9967(3) 0.0568(12) Uani 1 1 d . . .
H5A H 0.7583 1.4212 0.9880 0.068 Uiso 1 1 calc R . .
H5B H 0.7260 1.3119 1.0272 0.068 Uiso 1 1 calc R . .
H5C H 0.5559 1.4115 1.0383 0.068 Uiso 1 1 calc R . .
C6 C 0.1509(5) 1.4225(3) 0.8697(3) 0.0410(9) Uani 1 1 d . . .
H6A H 0.0229 1.4632 0.8870 0.049 Uiso 1 1 calc R . .
H6B H 0.1580 1.3856 0.8078 0.049 Uiso 1 1 calc R . .
H6C H 0.2389 1.4688 0.8637 0.049 Uiso 1 1 calc R . .
C7 C 0.3414(4) 0.8730(2) 0.6283(2) 0.0173(6) Uani 1 1 d . . .
C8 C 0.5416(4) 0.8285(2) 0.5848(2) 0.0177(6) Uani 1 1 d . . .
C9 C 0.6617(4) 0.9061(2) 0.55638(19) 0.0162(5) Uani 1 1 d . . .
C10 C 0.6139(4) 0.7267(2) 0.5788(2) 0.0280(7) Uani 1 1 d . . .
C11 C 0.6133(8) 0.5808(4) 0.7198(4) 0.0770(16) Uani 1 1 d . . .
H11A H 0.5556 0.5275 0.7519 0.092 Uiso 1 1 calc R . .
H11B H 0.6118 0.6363 0.7667 0.092 Uiso 1 1 calc R . .
H11C H 0.7434 0.5499 0.6941 0.092 Uiso 1 1 calc R . .
C12 C 0.8304(6) 0.6027(3) 0.4324(3) 0.0528(11) Uani 1 1 d . . .
H12A H 0.9552 0.5687 0.4013 0.063 Uiso 1 1 calc R . .
H12B H 0.7638 0.6490 0.3863 0.063 Uiso 1 1 calc R . .
H12C H 0.7591 0.5501 0.4525 0.063 Uiso 1 1 calc R . .
C14 C 1.0573(6) 0.6737(3) 0.7758(3) 0.0466(10) Uani 1 1 d . . .
H14A H 1.1897 0.6598 0.7871 0.056 Uiso 1 1 calc R . .
H14D H 1.0414 0.6275 0.7238 0.056 Uiso 1 1 calc R . .
H14E H 0.9804 0.6617 0.8354 0.056 Uiso 1 1 calc R . .
C13 C 1.3003(7) 0.6714(3) 0.3852(3) 0.0586(12) Uani 1 1 d . . .
H13A H 1.4276 0.6363 0.3584 0.070 Uiso 1 1 calc R . .
H13B H 1.2121 0.6657 0.3385 0.070 Uiso 1 1 calc R . .
H13C H 1.2646 0.6388 0.4458 0.070 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 O4 2.0153(18) . ?
Ni1 O8 2.0381(19) . ?
Ni1 O2 2.0522(18) . ?
Ni1 O6 2.0569(18) . ?
Ni1 K2 3.7660(7) 2_776 ?
Ni1 K1 3.9112(7) 1_455 ?
K1 O4 2.7108(19) 1_655 ?
K1 O1 2.759(2) 2_777 ?
K1 O3 2.771(2) 2_677 ?
K1 O1 2.851(2) . ?
K1 O6 2.9993(19) 1_655 ?
K1 O2 3.005(2) . ?
K1 C1 3.223(3) . ?
K1 K1 3.6981(12) 2_777 ?
K1 K2 3.8995(9) 2_776 ?
K1 Ni1 3.9112(7) 1_655 ?
K2 O7 2.667(2) . ?
K2 O8 2.6829(19) 2_776 ?
K2 O2 2.7932(19) 2_776 ?
K2 O6 2.852(2) 2_676 ?
K2 O5 2.982(2) 2_676 ?
K2 C7 3.193(3) 2_676 ?
K2 Ni1 3.7660(7) 2_776 ?
K2 K1 3.8995(9) 2_776 ?
K2 K2 4.1102(13) 2_776 ?
K2 H11D 2.1765 . ?
S1 C4 1.774(3) . ?
S1 C5 1.810(4) . ?
S2 C4 1.780(3) . ?
S2 C6 1.800(4) . ?
S3 C10 1.777(3) . ?
S3 C11 1.844(5) . ?
S4 C10 1.776(3) . ?
S4 C12 1.806(4) . ?
O1 C1 1.240(3) . ?
O1 K1 2.759(2) 2_777 ?
O2 C1 1.269(3) . ?
O2 K2 2.7931(19) 2_776 ?
O3 C3 1.240(3) . ?
O3 K1 2.7709(19) 2_677 ?
O4 C3 1.264(3) . ?
O4 K1 2.7108(19) 1_455 ?
O5 C7 1.253(3) . ?
O5 K2 2.982(2) 2_676 ?
O6 C7 1.262(3) . ?
O6 K2 2.8518(19) 2_676 ?
O6 K1 2.9993(19) 1_455 ?
O7 C9 1.238(3) . ?
O8 C9 1.264(3) . ?
O8 K2 2.6829(19) 2_776 ?
O9 H9B 0.8401 . ?
O9 H9C 0.8398 . ?
O10 H10B 0.8990 . ?
O10 H10C 0.8398 . ?
O11 C13 1.389(5) . ?
O11 H11D 0.8400 . ?
O12 C14 1.414(4) . ?
O12 H12D 0.8402 . ?
O14 H14B 0.9723 . ?
O14 H14C 0.8401 . ?
C1 C2 1.524(4) . ?
C2 C4 1.337(4) . ?
C2 C3 1.519(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.516(4) . ?
C7 K2 3.193(3) 2_676 ?
C8 C10 1.335(4) . ?
C8 C9 1.516(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14D 0.9800 . ?
C14 H14E 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

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
O4 Ni1 O8 179.03(8) . . ?
O4 Ni1 O2 91.86(7) . . ?
O8 Ni1 O2 88.79(7) . . ?
O4 Ni1 O6 86.96(7) . . ?
O8 Ni1 O6 92.40(7) . . ?
O2 Ni1 O6 178.68(7) . . ?
O4 Ni1 K2 136.98(5) . 2_776 ?
O8 Ni1 K2 43.48(5) . 2_776 ?
O2 Ni1 K2 46.74(5) . 2_776 ?
O6 Ni1 K2 134.54(5) . 2_776 ?
O4 Ni1 K1 40.37(5) . 1_455 ?
O8 Ni1 K1 139.24(5) . 1_455 ?
O2 Ni1 K1 129.59(5) . 1_455 ?
O6 Ni1 K1 49.11(5) . 1_455 ?
K2 Ni1 K1 175.824(17) 2_776 1_455 ?
O4 K1 O1 83.36(6) 1_655 2_777 ?
O4 K1 O3 147.87(6) 1_655 2_677 ?
O1 K1 O3 79.91(6) 2_777 2_677 ?
O4 K1 O1 84.38(6) 1_655 . ?
O1 K1 O1 97.53(6) 2_777 . ?
O3 K1 O1 70.97(6) 2_677 . ?
O4 K1 O6 58.52(5) 1_655 1_655 ?
O1 K1 O6 129.36(6) 2_777 1_655 ?
O3 K1 O6 148.95(6) 2_677 1_655 ?
O1 K1 O6 109.23(6) . 1_655 ?
O4 K1 O2 110.12(6) 1_655 . ?
O1 K1 O2 134.58(6) 2_777 . ?
O3 K1 O2 65.85(6) 2_677 . ?
O1 K1 O2 44.51(5) . . ?
O6 K1 O2 92.08(5) 1_655 . ?
O4 K1 C1 101.68(6) 1_655 . ?
O1 K1 C1 113.56(7) 2_777 . ?
O3 K1 C1 61.42(6) 2_677 . ?
O1 K1 C1 22.51(6) . . ?
O6 K1 C1 106.35(6) 1_655 . ?
O2 K1 C1 23.16(6) . . ?
O4 K1 K1 80.70(4) 1_655 2_777 ?
O1 K1 K1 49.84(4) 2_777 2_777 ?
O3 K1 K1 67.54(4) 2_677 2_777 ?
O1 K1 K1 47.69(4) . 2_777 ?
O6 K1 K1 136.64(4) 1_655 2_777 ?
O2 K1 K1 88.50(4) . 2_777 ?
C1 K1 K1 65.54(5) . 2_777 ?
O4 K1 K2 82.62(4) 1_655 2_776 ?
O1 K1 K2 163.89(5) 2_777 2_776 ?
O3 K1 K2 108.45(5) 2_677 2_776 ?
O1 K1 K2 73.23(4) . 2_776 ?
O6 K1 K2 46.61(4) 1_655 2_776 ?
O2 K1 K2 45.47(4) . 2_776 ?
C1 K1 K2 61.96(5) . 2_776 ?
K1 K1 K2 119.62(3) 2_777 2_776 ?
O4 K1 Ni1 28.79(4) 1_655 1_655 ?
O1 K1 Ni1 102.09(4) 2_777 1_655 ?
O3 K1 Ni1 174.20(5) 2_677 1_655 ?
O1 K1 Ni1 103.30(4) . 1_655 ?
O6 K1 Ni1 31.23(3) 1_655 1_655 ?
O2 K1 Ni1 109.58(4) . 1_655 ?
C1 K1 Ni1 112.92(5) . 1_655 ?
K1 K1 Ni1 109.48(2) 2_777 1_655 ?
K2 K1 Ni1 68.311(14) 2_776 1_655 ?
O7 K2 O8 137.75(6) . 2_776 ?
O7 K2 O2 158.34(6) . 2_776 ?
O8 K2 O2 62.97(6) 2_776 2_776 ?
O7 K2 O6 67.01(6) . 2_676 ?
O8 K2 O6 116.29(6) 2_776 2_676 ?
O2 K2 O6 99.93(6) 2_776 2_676 ?
O7 K2 O5 73.89(6) . 2_676 ?
O8 K2 O5 81.81(6) 2_776 2_676 ?
O2 K2 O5 109.68(6) 2_776 2_676 ?
O6 K2 O5 44.61(5) 2_676 2_676 ?
O7 K2 C7 62.55(7) . 2_676 ?
O8 K2 C7 103.24(7) 2_776 2_676 ?
O2 K2 C7 112.20(6) 2_776 2_676 ?
O6 K2 C7 23.22(6) 2_676 2_676 ?
O5 K2 C7 23.09(6) 2_676 2_676 ?
O7 K2 Ni1 169.15(5) . 2_776 ?
O8 K2 Ni1 31.52(4) 2_776 2_776 ?
O2 K2 Ni1 32.35(4) 2_776 2_776 ?
O6 K2 Ni1 116.65(4) 2_676 2_776 ?
O5 K2 Ni1 101.32(4) 2_676 2_776 ?
C7 K2 Ni1 116.32(5) 2_676 2_776 ?
O7 K2 K1 114.48(5) . 2_776 ?
O8 K2 K1 89.97(5) 2_776 2_776 ?
O2 K2 K1 50.09(4) 2_776 2_776 ?
O6 K2 K1 49.84(4) 2_676 2_776 ?
O5 K2 K1 73.32(4) 2_676 2_776 ?
C7 K2 K1 65.20(5) 2_676 2_776 ?
Ni1 K2 K1 72.406(15) 2_776 2_776 ?
O7 K2 K2 66.47(5) . 2_776 ?
O8 K2 K2 71.63(4) 2_776 2_776 ?
O2 K2 K2 134.60(5) 2_776 2_776 ?
O6 K2 K2 99.39(4) 2_676 2_776 ?
O5 K2 K2 61.34(4) 2_676 2_776 ?
C7 K2 K2 76.88(5) 2_676 2_776 ?
Ni1 K2 K2 102.68(2) 2_776 2_776 ?
K1 K2 K2 132.66(3) 2_776 2_776 ?
O7 K2 H11D 113.0 . . ?
O8 K2 H11D 81.5 2_776 . ?
O2 K2 H11D 71.0 2_776 . ?
O6 K2 H11D 154.6 2_676 . ?
O5 K2 H11D 160.6 2_676 . ?
C7 K2 H11D 175.0 2_676 . ?
Ni1 K2 H11D 68.5 2_776 . ?
K1 K2 H11D 116.6 2_776 . ?
K2 K2 H11D 103.7 2_776 . ?
C4 S1 C5 99.25(17) . . ?
C4 S2 C6 102.09(16) . . ?
C10 S3 C11 98.6(2) . . ?
C10 S4 C12 99.77(18) . . ?
C1 O1 K1 137.53(17) . 2_777 ?
C1 O1 K1 95.88(16) . . ?
K1 O1 K1 82.47(6) 2_777 . ?
C1 O2 Ni1 124.04(16) . . ?
C1 O2 K2 128.06(15) . 2_776 ?
Ni1 O2 K2 100.91(7) . 2_776 ?
C1 O2 K1 88.12(15) . . ?
Ni1 O2 K1 126.10(8) . . ?
K2 O2 K1 84.44(5) 2_776 . ?
C3 O3 K1 141.36(17) . 2_677 ?
C3 O4 Ni1 125.97(16) . . ?
C3 O4 K1 123.19(16) . 1_455 ?
Ni1 O4 K1 110.84(8) . 1_455 ?
C7 O5 K2 87.94(16) . 2_676 ?
C7 O6 Ni1 124.03(17) . . ?
C7 O6 K2 93.74(16) . 2_676 ?
Ni1 O6 K2 125.83(8) . 2_676 ?
C7 O6 K1 125.25(16) . 1_455 ?
Ni1 O6 K1 99.66(7) . 1_455 ?
K2 O6 K1 83.55(5) 2_676 1_455 ?
C9 O7 K2 139.19(18) . . ?
C9 O8 Ni1 123.57(16) . . ?
C9 O8 K2 131.14(16) . 2_776 ?
Ni1 O8 K2 105.00(7) . 2_776 ?
H9B O9 H9C 109.5 . . ?
H10B O10 H10C 108.0 . . ?
C13 O11 H11D 107.9 . . ?
C14 O12 H12D 108.5 . . ?
H14B O14 H14C 93.9 . . ?
O1 C1 O2 124.7(2) . . ?
O1 C1 C2 118.6(2) . . ?
O2 C1 C2 116.8(2) . . ?
O1 C1 K1 61.62(14) . . ?
O2 C1 K1 68.71(14) . . ?
C2 C1 K1 154.51(17) . . ?
C4 C2 C3 121.2(2) . . ?
C4 C2 C1 122.4(2) . . ?
C3 C2 C1 116.3(2) . . ?
O3 C3 O4 124.4(2) . . ?
O3 C3 C2 118.6(2) . . ?
O4 C3 C2 117.0(2) . . ?
C2 C4 S1 121.0(2) . . ?
C2 C4 S2 122.0(2) . . ?
S1 C4 S2 117.00(16) . . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S2 C6 H6A 109.5 . . ?
S2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
S2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O5 C7 O6 123.7(2) . . ?
O5 C7 C8 117.9(2) . . ?
O6 C7 C8 118.4(2) . . ?
O5 C7 K2 68.96(15) . 2_676 ?
O6 C7 K2 63.03(14) . 2_676 ?
C8 C7 K2 148.87(18) . 2_676 ?
C10 C8 C7 122.2(3) . . ?
C10 C8 C9 121.3(3) . . ?
C7 C8 C9 116.3(2) . . ?
O7 C9 O8 124.7(2) . . ?
O7 C9 C8 119.8(2) . . ?
O8 C9 C8 115.5(2) . . ?
C8 C10 S4 121.2(2) . . ?
C8 C10 S3 122.1(2) . . ?
S4 C10 S3 116.59(18) . . ?
S3 C11 H11A 109.5 . . ?
S3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
S3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
S4 C12 H12A 109.5 . . ?
S4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O12 C14 H14A 109.5 . . ?
O12 C14 H14D 109.5 . . ?
H14A C14 H14D 109.5 . . ?
O12 C14 H14E 109.5 . . ?
H14A C14 H14E 109.5 . . ?
H14D C14 H14E 109.5 . . ?
O11 C13 H13A 109.5 . . ?
O11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 998428'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_nth

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 Ag8 Ni2 O31 S12'
_chemical_formula_weight         2341.84

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-3

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

_cell_length_a                   15.8928(3)
_cell_length_b                   15.8928(3)
_cell_length_c                   7.91160(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1730.60(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2124
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      23.19

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    3.181
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4918
_exptl_absorpt_correction_T_max  0.7014
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Breeze CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30522
_diffrn_reflns_av_R_equivalents  0.0995
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2658
_reflns_number_gt                1650
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1453P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2658
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0715
_refine_ls_wR_factor_ref         0.2386
_refine_ls_wR_factor_gt          0.2221
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_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
Ag1 Ag 0.56705(6) 0.56358(6) 0.67389(11) 0.0367(3) Uani 1 1 d . . .
Ag2 Ag 0.3183(4) 0.5593(4) 0.4041(6) 0.0937(14) Uani 0.33 1 d P . .
Ni1 Ni 0.3333 0.6667 0.9316(3) 0.0279(5) Uani 1 3 d S . .
S1 S 0.43174(18) 0.42458(19) 0.8170(3) 0.0272(6) Uani 1 1 d . . .
S2 S 0.2994(2) 0.4117(2) 0.5244(3) 0.0331(6) Uani 1 1 d . . .
O1 O 0.1229(5) 0.4036(5) 0.7358(9) 0.0332(17) Uani 1 1 d . . .
O2 O 0.2208(5) 0.5615(5) 0.7914(9) 0.0337(16) Uani 1 1 d . . .
O3 O 0.3296(5) 0.5583(5) 1.0826(8) 0.0325(16) Uani 1 1 d . . .
O4 O 0.2971(5) 0.4084(5) 1.1247(8) 0.0314(16) Uani 1 1 d . . .
O5 O 0.0000 0.0000 1.0000 0.029(4) Uani 1 6 d S . .
O6 O 0.131(3) 0.081(4) 0.829(5) 0.113(15) Uani 0.33 1 d P . .
H6D H 0.0895 0.0705 0.7577 0.136 Uiso 0.33 1 d PR . .
H6E H 0.1468 0.1327 0.8767 0.136 Uiso 0.33 1 d PR . .
O7 O 0.2309(16) 0.2190(14) 1.068(2) 0.102(6) Uani 0.67 1 d P . .
H7A H 0.2816 0.2713 1.0742 0.122 Uiso 0.67 1 d PR . .
H7B H 0.1879 0.2275 1.0291 0.122 Uiso 0.67 1 d PR . .
C1 C 0.2024(7) 0.4747(8) 0.7844(11) 0.027(2) Uani 1 1 d . . .
C2 C 0.2791(7) 0.4543(7) 0.8473(11) 0.024(2) Uani 1 1 d . . .
C3 C 0.3050(7) 0.4749(7) 1.0353(11) 0.0227(19) Uani 1 1 d . . .
C4 C 0.3264(7) 0.4255(7) 0.7448(11) 0.025(2) Uani 1 1 d . . .
C5 C 0.4188(8) 0.3153(8) 0.7317(15) 0.040(3) Uani 1 1 d . . .
H5A H 0.4734 0.3087 0.7648 0.048 Uiso 1 1 calc R . .
H5B H 0.4161 0.3172 0.6106 0.048 Uiso 1 1 calc R . .
H5C H 0.3601 0.2609 0.7735 0.048 Uiso 1 1 calc R . .
C6 C 0.2083(9) 0.2869(9) 0.5101(17) 0.050(3) Uani 1 1 d . . .
H6A H 0.1879 0.2710 0.3946 0.060 Uiso 1 1 calc R . .
H6B H 0.1537 0.2752 0.5787 0.060 Uiso 1 1 calc R . .
H6C H 0.2343 0.2473 0.5492 0.060 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
Ag1 O1 2.329(7) 2_665 ?
Ag1 S1 2.457(3) . ?
Ag1 S2 2.507(3) 4_666 ?
Ag1 O4 2.537(7) 4_667 ?
Ag1 Ag2 3.328(5) 4_666 ?
Ag2 S2 2.407(6) . ?
Ag2 O3 2.551(8) 1_554 ?
Ag2 Ag2 2.772(9) 3_565 ?
Ag2 Ag2 2.772(9) 2_665 ?
Ag2 Ag1 3.328(5) 4_666 ?
Ni1 O2 2.057(7) . ?
Ni1 O2 2.057(7) 3_565 ?
Ni1 O2 2.057(7) 2_665 ?
Ni1 O3 2.073(7) 3_565 ?
Ni1 O3 2.073(7) 2_665 ?
Ni1 O3 2.073(7) . ?
S1 C4 1.776(10) . ?
S1 C5 1.778(12) . ?
S2 C6 1.780(13) . ?
S2 C4 1.783(9) . ?
S2 Ag1 2.507(3) 4_666 ?
O1 C1 1.263(12) . ?
O1 Ag1 2.329(7) 3_565 ?
O2 C1 1.260(13) . ?
O3 C3 1.237(12) . ?
O3 Ag2 2.551(8) 1_556 ?
O4 C3 1.225(11) . ?
O4 Ag1 2.537(7) 4_667 ?
O6 H6D 0.8200 . ?
O6 H6E 0.8200 . ?
O7 H7A 0.8200 . ?
O7 H7B 0.8201 . ?
C1 C2 1.496(13) . ?
C2 C4 1.333(13) . ?
C2 C3 1.533(12) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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 Ag1 S1 118.61(18) 2_665 . ?
O1 Ag1 S2 105.10(18) 2_665 4_666 ?
S1 Ag1 S2 136.15(10) . 4_666 ?
O1 Ag1 O4 88.9(3) 2_665 4_667 ?
S1 Ag1 O4 98.84(17) . 4_667 ?
S2 Ag1 O4 77.65(16) 4_666 4_667 ?
O1 Ag1 Ag2 141.7(2) 2_665 4_666 ?
S1 Ag1 Ag2 92.74(11) . 4_666 ?
S2 Ag1 Ag2 46.12(10) 4_666 4_666 ?
O4 Ag1 Ag2 63.37(18) 4_667 4_666 ?
S2 Ag2 O3 111.3(3) . 1_554 ?
S2 Ag2 Ag2 143.2(3) . 3_565 ?
O3 Ag2 Ag2 93.6(2) 1_554 3_565 ?
S2 Ag2 Ag2 142.2(3) . 2_665 ?
O3 Ag2 Ag2 89.8(2) 1_554 2_665 ?
Ag2 Ag2 Ag2 60.001(1) 3_565 2_665 ?
S2 Ag2 Ag1 48.66(11) . 4_666 ?
O3 Ag2 Ag1 75.5(2) 1_554 4_666 ?
Ag2 Ag2 Ag1 167.60(14) 3_565 4_666 ?
Ag2 Ag2 Ag1 113.2(3) 2_665 4_666 ?
O2 Ni1 O2 93.7(3) . 3_565 ?
O2 Ni1 O2 93.7(3) . 2_665 ?
O2 Ni1 O2 93.7(3) 3_565 2_665 ?
O2 Ni1 O3 87.1(3) . 3_565 ?
O2 Ni1 O3 89.1(3) 3_565 3_565 ?
O2 Ni1 O3 177.1(3) 2_665 3_565 ?
O2 Ni1 O3 177.1(3) . 2_665 ?
O2 Ni1 O3 87.1(3) 3_565 2_665 ?
O2 Ni1 O3 89.1(3) 2_665 2_665 ?
O3 Ni1 O3 90.1(3) 3_565 2_665 ?
O2 Ni1 O3 89.1(3) . . ?
O2 Ni1 O3 177.1(3) 3_565 . ?
O2 Ni1 O3 87.1(3) 2_665 . ?
O3 Ni1 O3 90.1(3) 3_565 . ?
O3 Ni1 O3 90.1(3) 2_665 . ?
C4 S1 C5 103.7(5) . . ?
C4 S1 Ag1 104.5(3) . . ?
C5 S1 Ag1 109.0(4) . . ?
C6 S2 C4 102.2(6) . . ?
C6 S2 Ag2 134.1(5) . . ?
C4 S2 Ag2 111.2(4) . . ?
C6 S2 Ag1 106.7(4) . 4_666 ?
C4 S2 Ag1 117.4(3) . 4_666 ?
Ag2 S2 Ag1 85.22(15) . 4_666 ?
C1 O1 Ag1 117.5(6) . 3_565 ?
C1 O2 Ni1 123.0(6) . . ?
C3 O3 Ni1 125.3(6) . . ?
C3 O3 Ag2 108.8(6) . 1_556 ?
Ni1 O3 Ag2 122.8(3) . 1_556 ?
C3 O4 Ag1 120.1(6) . 4_667 ?
H6D O6 H6E 109.5 . . ?
H7A O7 H7B 109.5 . . ?
O2 C1 O1 125.1(9) . . ?
O2 C1 C2 117.0(9) . . ?
O1 C1 C2 117.8(9) . . ?
C4 C2 C1 122.2(8) . . ?
C4 C2 C3 121.8(8) . . ?
C1 C2 C3 115.9(8) . . ?
O4 C3 O3 126.2(8) . . ?
O4 C3 C2 118.4(8) . . ?
O3 C3 C2 115.4(8) . . ?
C2 C4 S1 120.2(7) . . ?
C2 C4 S2 119.7(7) . . ?
S1 C4 S2 118.9(5) . . ?
S1 C5 H5A 109.5 . . ?
S1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
S1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S2 C6 H6A 109.5 . . ?
S2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
S2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.147
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.271
_database_code_depnum_ccdc_archive 'CCDC 998429'
