# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       damir.safin@ksu.ru
_publ_contact_author_name        'Damir Safin'
_publ_author_name                'Damir Safin'

data_safinHL
_database_code_depnum_ccdc_archive 'CCDC 848847'
#TrackingRef '- HL.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H35 N2 O7 P S2'
_chemical_formula_sum            'C21 H35 N2 O7 P S2'
_chemical_formula_weight         522.60

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'
P P 0.1023 0.0942 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   7.7391(3)
_cell_length_b                   9.1558(11)
_cell_length_c                   20.7496(17)
_cell_angle_alpha                83.459(8)
_cell_angle_beta                 85.820(5)
_cell_angle_gamma                69.189(7)
_cell_volume                     1364.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7538
_cell_measurement_theta_min      1.9730
_cell_measurement_theta_max      25.1910

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    0.294
_exptl_absorpt_correction_T_min  0.98023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
Two datasets on the same crystal were measured to
increase the data coverage.
Each dataset was integrated with crysalispro, with
absorption correction, the resulting files were
merged by xprep to give the final hkl file for
refining.
Rint set1: 0.063 150frames \D\F 2.5\%'
Rint set2: 0.045 30frames \D\F 2.5\%

Rint for the merged dataset 0.0478
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '150 images, \D\F 2.5\%'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4731
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         25.26
_reflns_number_total             4731
_reflns_number_gt                4000
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       MAR
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0623P)^2^+0.8203P] where P=(Fo^2^+2Fc^2^)/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         4731
_refine_ls_number_parameters     302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1424
_refine_ls_wR_factor_gt          0.1352
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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
P1 P 0.97504(10) 0.25523(9) 0.14639(3) 0.0511(2) Uani 1 1 d . . .
S2 S 1.17858(13) 0.12880(13) 0.09516(4) 0.0851(3) Uani 1 1 d . . .
N3 N 0.9978(3) 0.1815(3) 0.22378(10) 0.0505(5) Uani 1 1 d . . .
H3 H 1.1036 0.1108 0.2324 0.061 Uiso 1 1 calc R . .
C4 C 0.8741(3) 0.2157(3) 0.27661(11) 0.0427(6) Uani 1 1 d . . .
S5 S 0.68706(12) 0.37577(9) 0.27711(4) 0.0688(3) Uani 1 1 d . . .
N6 N 0.9255(3) 0.1015(2) 0.32604(9) 0.0468(5) Uani 1 1 d . . .
H6 H 1.0175 0.0188 0.3176 0.056 Uiso 1 1 calc R . .
O7 O 0.7804(3) 0.2710(3) 0.12438(10) 0.0632(5) Uani 1 1 d . . .
C8 C 0.7414(7) 0.1353(6) 0.1047(2) 0.1000(13) Uani 1 1 d . . .
H8 H 0.8595 0.0543 0.0939 0.120 Uiso 1 1 calc R . .
C9 C 0.6511(9) 0.0698(7) 0.1590(3) 0.138(2) Uani 1 1 d . . .
H9A H 0.7385 0.0191 0.1923 0.207 Uiso 1 1 calc R . .
H9B H 0.6064 -0.0053 0.1441 0.207 Uiso 1 1 calc R . .
H9C H 0.5493 0.1528 0.1763 0.207 Uiso 1 1 calc R . .
C10 C 0.6342(10) 0.1900(9) 0.0454(2) 0.163(3) Uani 1 1 d . . .
H10A H 0.5946 0.1084 0.0340 0.245 Uiso 1 1 calc R . .
H10B H 0.7100 0.2160 0.0106 0.245 Uiso 1 1 calc R . .
H10C H 0.5279 0.2812 0.0530 0.245 Uiso 1 1 calc R . .
O11 O 0.9561(4) 0.4298(3) 0.14889(9) 0.0725(6) Uani 1 1 d . . .
C12 C 0.9062(8) 0.5443(5) 0.09083(16) 0.0969(14) Uani 1 1 d . . .
H12 H 0.9151 0.4880 0.0526 0.116 Uiso 1 1 calc R . .
C13 C 0.7079(10) 0.6503(7) 0.1016(3) 0.164(3) Uani 1 1 d . . .
H13A H 0.6984 0.7044 0.1395 0.246 Uiso 1 1 calc R . .
H13B H 0.6295 0.5884 0.1077 0.246 Uiso 1 1 calc R . .
H13C H 0.6699 0.7255 0.0645 0.246 Uiso 1 1 calc R . .
C14 C 1.0419(10) 0.6256(7) 0.0832(2) 0.145(2) Uani 1 1 d . . .
H14A H 1.0219 0.6924 0.1175 0.218 Uiso 1 1 calc R . .
H14B H 1.0271 0.6877 0.0421 0.218 Uiso 1 1 calc R . .
H14C H 1.1649 0.5494 0.0850 0.218 Uiso 1 1 calc R . .
C15 C 0.8474(3) 0.1000(3) 0.39037(11) 0.0404(5) Uani 1 1 d . . .
C16 C 0.7955(3) 0.2312(3) 0.42502(11) 0.0441(6) Uani 1 1 d . . .
H16 H 0.8040 0.3250 0.4053 0.053 Uiso 1 1 calc R . .
C17 C 0.7310(3) 0.2222(3) 0.48884(11) 0.0417(5) Uani 1 1 d . . .
C18 C 0.7117(3) 0.0830(3) 0.51785(11) 0.0411(5) Uani 1 1 d . . .
C19 C 0.7674(4) -0.0466(3) 0.48346(12) 0.0491(6) Uani 1 1 d . . .
H19 H 0.7579 -0.1403 0.5028 0.059 Uiso 1 1 calc R . .
C20 C 0.8383(4) -0.0394(3) 0.41957(12) 0.0470(6) Uani 1 1 d . . .
H20 H 0.8789 -0.1285 0.3971 0.056 Uiso 1 1 calc R . .
O21 O 0.6824(3) 0.3425(2) 0.52765(9) 0.0552(5) Uani 1 1 d . . .
C22 C 0.7600(5) 0.4622(3) 0.51171(14) 0.0575(7) Uani 1 1 d . . .
H22A H 0.6882 0.5401 0.4790 0.069 Uiso 1 1 calc R . .
H22B H 0.8862 0.4177 0.4949 0.069 Uiso 1 1 calc R . .
C23 C 0.7560(5) 0.5357(3) 0.57305(15) 0.0617(8) Uani 1 1 d . . .
H23A H 0.7836 0.6314 0.5632 0.074 Uiso 1 1 calc R . .
H23B H 0.6339 0.5621 0.5940 0.074 Uiso 1 1 calc R . .
O24 O 0.8879(3) 0.4289(2) 0.61449(10) 0.0698(6) Uani 1 1 d . . .
C25 C 0.8756(5) 0.4775(4) 0.67781(16) 0.0736(9) Uani 1 1 d . . .
H25A H 0.7469 0.5220 0.6920 0.088 Uiso 1 1 calc R . .
H25B H 0.9314 0.5571 0.6775 0.088 Uiso 1 1 calc R . .
C26 C 0.9743(5) 0.3385(4) 0.72302(18) 0.0777(10) Uani 1 1 d . . .
H26A H 1.1026 0.2958 0.7082 0.093 Uiso 1 1 calc R . .
H26B H 0.9721 0.3728 0.7657 0.093 Uiso 1 1 calc R . .
O27 O 0.8983(3) 0.2179(3) 0.72852(12) 0.0753(6) Uani 1 1 d . . .
C28 C 0.7209(5) 0.2510(4) 0.76075(16) 0.0680(8) Uani 1 1 d . . .
H28A H 0.6688 0.3615 0.7676 0.082 Uiso 1 1 calc R . .
H28B H 0.7337 0.1907 0.8028 0.082 Uiso 1 1 calc R . .
C29 C 0.5945(4) 0.2102(3) 0.72097(15) 0.0627(8) Uani 1 1 d . . .
H29A H 0.4704 0.2434 0.7404 0.075 Uiso 1 1 calc R . .
H29B H 0.5897 0.2628 0.6775 0.075 Uiso 1 1 calc R . .
O30 O 0.6644(3) 0.0438(2) 0.71853(8) 0.0530(5) Uani 1 1 d . . .
C31 C 0.5567(4) -0.0138(3) 0.68198(12) 0.0531(7) Uani 1 1 d . . .
H31A H 0.4336 0.0644 0.6777 0.064 Uiso 1 1 calc R . .
H31B H 0.5445 -0.1076 0.7056 0.064 Uiso 1 1 calc R . .
C32 C 0.6391(4) -0.0518(3) 0.61573(12) 0.0460(6) Uani 1 1 d . . .
H32A H 0.7649 -0.1257 0.6189 0.055 Uiso 1 1 calc R . .
H32B H 0.5673 -0.0985 0.5941 0.055 Uiso 1 1 calc R . .
O33 O 0.6375(3) 0.0905(2) 0.58018(8) 0.0523(5) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0557(4) 0.0643(5) 0.0334(3) 0.0023(3) -0.0013(3) -0.0234(3)
S2 0.0702(6) 0.1218(8) 0.0475(5) -0.0060(5) 0.0152(4) -0.0182(5)
N3 0.0435(12) 0.0589(13) 0.0372(11) 0.0039(9) 0.0008(9) -0.0062(10)
C4 0.0450(14) 0.0465(14) 0.0331(12) -0.0008(10) -0.0026(10) -0.0123(11)
S5 0.0674(5) 0.0593(5) 0.0477(4) 0.0045(3) 0.0010(3) 0.0135(4)
N6 0.0457(12) 0.0458(12) 0.0339(10) 0.0002(9) 0.0035(8) 0.0003(9)
O7 0.0580(12) 0.0753(14) 0.0544(11) 0.0009(10) -0.0117(9) -0.0211(10)
C8 0.095(3) 0.136(4) 0.093(3) -0.031(3) -0.007(2) -0.062(3)
C9 0.182(6) 0.169(5) 0.109(4) 0.018(4) -0.026(4) -0.124(5)
C10 0.201(7) 0.303(9) 0.067(3) -0.013(4) -0.009(3) -0.188(7)
O11 0.1177(19) 0.0740(14) 0.0370(10) 0.0078(9) -0.0087(11) -0.0500(13)
C12 0.176(5) 0.083(3) 0.0409(17) 0.0088(16) -0.011(2) -0.059(3)
C13 0.198(7) 0.101(4) 0.146(5) 0.031(4) -0.037(5) -0.002(4)
C14 0.258(8) 0.138(4) 0.083(3) 0.023(3) 0.000(4) -0.134(5)
C15 0.0375(13) 0.0456(13) 0.0314(11) -0.0001(10) -0.0028(9) -0.0071(10)
C16 0.0495(15) 0.0398(13) 0.0406(13) 0.0015(10) 0.0009(11) -0.0149(11)
C17 0.0448(14) 0.0415(13) 0.0387(12) -0.0050(10) -0.0004(10) -0.0148(10)
C18 0.0469(14) 0.0445(13) 0.0316(11) -0.0020(10) -0.0020(10) -0.0160(11)
C19 0.0661(17) 0.0393(13) 0.0398(13) 0.0014(10) -0.0014(12) -0.0178(12)
C20 0.0584(16) 0.0404(13) 0.0364(13) -0.0054(10) -0.0028(11) -0.0095(11)
O21 0.0764(13) 0.0479(10) 0.0495(10) -0.0150(8) 0.0173(9) -0.0324(9)
C22 0.078(2) 0.0426(14) 0.0547(16) -0.0018(12) 0.0062(14) -0.0272(14)
C23 0.082(2) 0.0374(14) 0.0666(18) -0.0100(13) 0.0045(16) -0.0217(14)
O24 0.0809(15) 0.0610(13) 0.0629(13) -0.0212(10) -0.0038(11) -0.0144(11)
C25 0.091(2) 0.066(2) 0.074(2) -0.0249(17) -0.0039(18) -0.0339(18)
C26 0.072(2) 0.091(3) 0.074(2) -0.0239(19) -0.0134(18) -0.0259(19)
O27 0.0718(15) 0.0605(13) 0.0868(16) -0.0158(11) 0.0078(12) -0.0142(11)
C28 0.076(2) 0.0547(17) 0.0644(19) -0.0197(15) 0.0065(16) -0.0103(15)
C29 0.0617(18) 0.0499(16) 0.0616(18) -0.0102(13) -0.0036(14) 0.0003(13)
O30 0.0592(12) 0.0468(10) 0.0430(10) -0.0053(8) -0.0071(8) -0.0051(8)
C31 0.0557(17) 0.0588(16) 0.0427(14) 0.0015(12) 0.0043(12) -0.0204(13)
C32 0.0526(15) 0.0441(14) 0.0423(13) 0.0002(11) -0.0008(11) -0.0198(11)
O33 0.0750(13) 0.0441(10) 0.0378(9) -0.0044(7) 0.0089(8) -0.0230(9)

_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
P1 O7 1.558(2) . ?
P1 O11 1.559(2) . ?
P1 N3 1.666(2) . ?
P1 S2 1.9213(12) . ?
N3 C4 1.389(3) . ?
N3 H3 0.8600 . ?
C4 N6 1.350(3) . ?
C4 S5 1.654(3) . ?
N6 C15 1.425(3) . ?
N6 H6 0.8600 . ?
O7 C8 1.485(5) . ?
C8 C9 1.466(6) . ?
C8 C10 1.471(6) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
O11 C12 1.480(4) . ?
C12 C14 1.479(6) . ?
C12 C13 1.513(8) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C20 1.372(3) . ?
C15 C16 1.391(3) . ?
C16 C17 1.384(3) . ?
C16 H16 0.9300 . ?
C17 O21 1.366(3) . ?
C17 C18 1.399(3) . ?
C18 C19 1.374(3) . ?
C18 O33 1.375(3) . ?
C19 C20 1.401(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
O21 C22 1.424(3) . ?
C22 C23 1.499(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 O24 1.401(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
O24 C25 1.420(4) . ?
C25 C26 1.491(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 O27 1.414(4) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
O27 C28 1.429(4) . ?
C28 C29 1.492(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 O30 1.430(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
O30 C31 1.429(3) . ?
C31 C32 1.497(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 O33 1.419(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 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
O7 P1 O11 102.30(13) . . ?
O7 P1 N3 109.05(11) . . ?
O11 P1 N3 103.67(11) . . ?
O7 P1 S2 114.62(9) . . ?
O11 P1 S2 117.10(10) . . ?
N3 P1 S2 109.29(9) . . ?
C4 N3 P1 130.56(18) . . ?
C4 N3 H3 114.7 . . ?
P1 N3 H3 114.7 . . ?
N6 C4 N3 111.3(2) . . ?
N6 C4 S5 125.31(18) . . ?
N3 C4 S5 123.34(18) . . ?
C4 N6 C15 128.5(2) . . ?
C4 N6 H6 115.7 . . ?
C15 N6 H6 115.7 . . ?
C8 O7 P1 121.9(2) . . ?
C9 C8 C10 115.0(4) . . ?
C9 C8 O7 109.6(4) . . ?
C10 C8 O7 107.2(4) . . ?
C9 C8 H8 108.3 . . ?
C10 C8 H8 108.3 . . ?
O7 C8 H8 108.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 O11 P1 121.1(2) . . ?
C14 C12 O11 107.2(4) . . ?
C14 C12 C13 114.6(5) . . ?
O11 C12 C13 107.1(4) . . ?
C14 C12 H12 109.3 . . ?
O11 C12 H12 109.3 . . ?
C13 C12 H12 109.3 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C20 C15 C16 120.2(2) . . ?
C20 C15 N6 117.9(2) . . ?
C16 C15 N6 121.7(2) . . ?
C17 C16 C15 119.9(2) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
O21 C17 C16 124.5(2) . . ?
O21 C17 C18 115.3(2) . . ?
C16 C17 C18 120.2(2) . . ?
C19 C18 O33 126.0(2) . . ?
C19 C18 C17 119.1(2) . . ?
O33 C18 C17 114.9(2) . . ?
C18 C19 C20 120.8(2) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C15 C20 C19 119.6(2) . . ?
C15 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C17 O21 C22 117.8(2) . . ?
O21 C22 C23 106.9(2) . . ?
O21 C22 H22A 110.4 . . ?
C23 C22 H22A 110.4 . . ?
O21 C22 H22B 110.4 . . ?
C23 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
O24 C23 C22 108.8(2) . . ?
O24 C23 H23A 109.9 . . ?
C22 C23 H23A 109.9 . . ?
O24 C23 H23B 109.9 . . ?
C22 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C23 O24 C25 113.1(2) . . ?
O24 C25 C26 108.8(3) . . ?
O24 C25 H25A 109.9 . . ?
C26 C25 H25A 109.9 . . ?
O24 C25 H25B 109.9 . . ?
C26 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
O27 C26 C25 114.1(3) . . ?
O27 C26 H26A 108.7 . . ?
C25 C26 H26A 108.7 . . ?
O27 C26 H26B 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C26 O27 C28 116.6(3) . . ?
O27 C28 C29 110.1(3) . . ?
O27 C28 H28A 109.6 . . ?
C29 C28 H28A 109.6 . . ?
O27 C28 H28B 109.6 . . ?
C29 C28 H28B 109.6 . . ?
H28A C28 H28B 108.2 . . ?
O30 C29 C28 107.9(2) . . ?
O30 C29 H29A 110.1 . . ?
C28 C29 H29A 110.1 . . ?
O30 C29 H29B 110.1 . . ?
C28 C29 H29B 110.1 . . ?
H29A C29 H29B 108.4 . . ?
C29 O30 C31 114.5(2) . . ?
O30 C31 C32 113.1(2) . . ?
O30 C31 H31A 109.0 . . ?
C32 C31 H31A 109.0 . . ?
O30 C31 H31B 109.0 . . ?
C32 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
O33 C32 C31 107.6(2) . . ?
O33 C32 H32A 110.2 . . ?
C31 C32 H32A 110.2 . . ?
O33 C32 H32B 110.2 . . ?
C31 C32 H32B 110.2 . . ?
H32A C32 H32B 108.5 . . ?
C18 O33 C32 117.69(19) . . ?

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
O7 P1 N3 C4 -42.6(3) . . . . ?
O11 P1 N3 C4 65.8(3) . . . . ?
S2 P1 N3 C4 -168.6(2) . . . . ?
P1 N3 C4 N6 162.7(2) . . . . ?
P1 N3 C4 S5 -16.6(4) . . . . ?
N3 C4 N6 C15 172.8(2) . . . . ?
S5 C4 N6 C15 -8.0(4) . . . . ?
O11 P1 O7 C8 169.8(3) . . . . ?
N3 P1 O7 C8 -80.9(3) . . . . ?
S2 P1 O7 C8 42.0(3) . . . . ?
P1 O7 C8 C9 98.8(4) . . . . ?
P1 O7 C8 C10 -135.7(4) . . . . ?
O7 P1 O11 C12 -57.8(3) . . . . ?
N3 P1 O11 C12 -171.2(3) . . . . ?
S2 P1 O11 C12 68.4(3) . . . . ?
P1 O11 C12 C14 -130.1(4) . . . . ?
P1 O11 C12 C13 106.5(4) . . . . ?
C4 N6 C15 C20 143.1(3) . . . . ?
C4 N6 C15 C16 -42.1(4) . . . . ?
C20 C15 C16 C17 -1.2(4) . . . . ?
N6 C15 C16 C17 -175.9(2) . . . . ?
C15 C16 C17 O21 177.7(2) . . . . ?
C15 C16 C17 C18 -2.3(4) . . . . ?
O21 C17 C18 C19 -176.3(2) . . . . ?
C16 C17 C18 C19 3.7(4) . . . . ?
O21 C17 C18 O33 3.2(3) . . . . ?
C16 C17 C18 O33 -176.7(2) . . . . ?
O33 C18 C19 C20 178.9(2) . . . . ?
C17 C18 C19 C20 -1.6(4) . . . . ?
C16 C15 C20 C19 3.3(4) . . . . ?
N6 C15 C20 C19 178.2(2) . . . . ?
C18 C19 C20 C15 -1.8(4) . . . . ?
C16 C17 O21 C22 -23.1(4) . . . . ?
C18 C17 O21 C22 157.0(2) . . . . ?
C17 O21 C22 C23 -155.9(2) . . . . ?
O21 C22 C23 O24 71.2(3) . . . . ?
C22 C23 O24 C25 -170.8(3) . . . . ?
C23 O24 C25 C26 161.7(3) . . . . ?
O24 C25 C26 O27 -61.8(4) . . . . ?
C25 C26 O27 C28 -69.3(4) . . . . ?
C26 O27 C28 C29 130.7(3) . . . . ?
O27 C28 C29 O30 66.1(3) . . . . ?
C28 C29 O30 C31 179.8(2) . . . . ?
C29 O30 C31 C32 101.9(3) . . . . ?
O30 C31 C32 O33 -64.6(3) . . . . ?
C19 C18 O33 C32 8.5(4) . . . . ?
C17 C18 O33 C32 -171.0(2) . . . . ?
C31 C32 O33 C18 178.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        25.26
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.051

# Attachment '- NiL2.cif'

data_safinNiL2
_database_code_depnum_ccdc_archive 'CCDC 848848'
#TrackingRef '- NiL2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H68 N4 Ni O14 P2 S4, 2(H2 O)'
_chemical_formula_sum            'C42 H72 N4 Ni O16 P2 S4'
_chemical_formula_weight         1137.93

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   23.4963(6)
_cell_length_b                   8.2208(3)
_cell_length_c                   29.2604(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5651.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    13318
_cell_measurement_theta_min      1.6364
_cell_measurement_theta_max      25.2455

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2408
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_min  0.96830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '150 images, \D\F 1.2\%'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35470
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         25.30
_reflns_number_total             5101
_reflns_number_gt                4279
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0424P)^2^+5.1185P] where P=(Fo^2^+2Fc^2^)/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         5101
_refine_ls_number_parameters     347
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.1026
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.126
_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
O51 O 0.91766(9) 0.8557(3) 0.34273(7) 0.0507(6) Uani 1 1 d . . .
Ni1 Ni 1.0000 1.0000 0.0000 0.02772(14) Uani 1 2 d S . .
S2 S 0.90617(3) 1.01691(11) 0.00673(2) 0.0446(2) Uani 1 1 d . . .
P3 P 0.89008(3) 0.91946(8) 0.06776(2) 0.02964(17) Uani 1 1 d . A .
N4 N 0.92116(10) 0.9985(3) 0.11045(7) 0.0344(5) Uani 1 1 d . . .
C5 C 0.97040(11) 1.0742(3) 0.11199(8) 0.0276(5) Uani 1 1 d . . .
S6 S 1.02244(3) 1.08574(9) 0.06933(2) 0.03625(18) Uani 1 1 d . . .
O7 O 0.89558(10) 0.7308(3) 0.06813(9) 0.0571(6) Uani 1 1 d D . .
C8 C 0.9347(7) 0.6386(16) 0.0951(6) 0.085(6) Uani 0.398(17) 1 d PDU A 1
H8 H 0.9539 0.7106 0.1169 0.102 Uiso 0.398(17) 1 calc PR A 1
C9 C 0.8971(10) 0.526(3) 0.1199(7) 0.148(8) Uani 0.398(17) 1 d PDU A 1
H9A H 0.8870 0.4371 0.1003 0.222 Uiso 0.398(17) 1 calc PR A 1
H9B H 0.8633 0.5826 0.1293 0.222 Uiso 0.398(17) 1 calc PR A 1
H9C H 0.9166 0.4852 0.1464 0.222 Uiso 0.398(17) 1 calc PR A 1
C10 C 0.9772(8) 0.561(3) 0.0653(9) 0.148(8) Uani 0.398(17) 1 d PDU A 1
H10A H 0.9597 0.4735 0.0488 0.222 Uiso 0.398(17) 1 calc PR A 1
H10B H 1.0079 0.5198 0.0835 0.222 Uiso 0.398(17) 1 calc PR A 1
H10C H 0.9916 0.6400 0.0440 0.222 Uiso 0.398(17) 1 calc PR A 1
C8B C 0.9447(4) 0.6423(8) 0.0825(3) 0.058(3) Uani 0.602(17) 1 d PDU A 2
H8B H 0.9766 0.7190 0.0830 0.070 Uiso 0.602(17) 1 calc PR A 2
C9B C 0.9390(7) 0.5761(13) 0.1290(3) 0.125(5) Uani 0.602(17) 1 d PDU A 2
H9D H 0.9082 0.6299 0.1444 0.188 Uiso 0.602(17) 1 calc PR A 2
H9E H 0.9737 0.5935 0.1455 0.188 Uiso 0.602(17) 1 calc PR A 2
H9F H 0.9312 0.4616 0.1273 0.188 Uiso 0.602(17) 1 calc PR A 2
C10B C 0.9569(7) 0.5218(14) 0.0467(3) 0.145(5) Uani 0.602(17) 1 d PDU A 2
H10D H 0.9234 0.4578 0.0410 0.218 Uiso 0.602(17) 1 calc PR A 2
H10E H 0.9873 0.4521 0.0565 0.218 Uiso 0.602(17) 1 calc PR A 2
H10F H 0.9679 0.5769 0.0191 0.218 Uiso 0.602(17) 1 calc PR A 2
O11 O 0.82420(8) 0.9320(2) 0.07655(7) 0.0380(5) Uani 1 1 d . . .
C12 C 0.79548(14) 1.0898(4) 0.07785(11) 0.0495(8) Uani 1 1 d . A .
H12 H 0.8235 1.1758 0.0722 0.059 Uiso 1 1 calc R . .
C13 C 0.7526(2) 1.0903(6) 0.04030(16) 0.0983(17) Uani 1 1 d . . .
H13A H 0.7713 1.0708 0.0116 0.147 Uiso 1 1 calc R A .
H13B H 0.7338 1.1940 0.0394 0.147 Uiso 1 1 calc R . .
H13C H 0.7250 1.0064 0.0457 0.147 Uiso 1 1 calc R . .
C14 C 0.7712(2) 1.1115(6) 0.12465(14) 0.0932(16) Uani 1 1 d . . .
H14A H 0.7473 1.0204 0.1319 0.140 Uiso 1 1 calc R A .
H14B H 0.7491 1.2097 0.1256 0.140 Uiso 1 1 calc R . .
H14C H 0.8016 1.1183 0.1465 0.140 Uiso 1 1 calc R . .
N15 N 0.98632(9) 1.1489(3) 0.15106(7) 0.0301(5) Uani 1 1 d . . .
H15 H 1.0194 1.1935 0.1506 0.036 Uiso 1 1 calc R . .
C16 C 0.95581(11) 1.1639(3) 0.19289(8) 0.0301(6) Uani 1 1 d . . .
C17 C 0.91148(12) 1.0599(3) 0.20553(9) 0.0332(6) Uani 1 1 d . . .
H17 H 0.9004 0.9765 0.1860 0.040 Uiso 1 1 calc R . .
C18 C 0.88391(11) 1.0801(3) 0.24704(9) 0.0322(6) Uani 1 1 d . . .
C19 C 0.90059(12) 1.2045(3) 0.27677(9) 0.0345(6) Uani 1 1 d . . .
C20 C 0.94467(13) 1.3053(4) 0.26396(10) 0.0443(8) Uani 1 1 d . . .
H20 H 0.9562 1.3880 0.2836 0.053 Uiso 1 1 calc R . .
C21 C 0.97231(13) 1.2858(4) 0.22222(10) 0.0411(7) Uani 1 1 d . . .
H21 H 1.0019 1.3552 0.2142 0.049 Uiso 1 1 calc R . .
O22 O 0.83975(9) 0.9842(2) 0.26135(6) 0.0428(5) Uani 1 1 d . . .
C23 C 0.83268(16) 0.8307(4) 0.23939(11) 0.0549(9) Uani 1 1 d . . .
H23A H 0.8688 0.7742 0.2375 0.066 Uiso 1 1 calc R . .
H23B H 0.8180 0.8455 0.2087 0.066 Uiso 1 1 calc R . .
C24 C 0.79103(16) 0.7342(4) 0.26792(12) 0.0592(10) Uani 1 1 d . . .
H24A H 0.7564 0.7962 0.2724 0.071 Uiso 1 1 calc R . .
H24B H 0.7813 0.6334 0.2525 0.071 Uiso 1 1 calc R . .
O25 O 0.81659(10) 0.7006(3) 0.31019(8) 0.0583(6) Uani 1 1 d . . .
C26 C 0.77993(16) 0.6274(4) 0.34304(12) 0.0605(10) Uani 1 1 d . . .
H26A H 0.7752 0.5127 0.3363 0.073 Uiso 1 1 calc R . .
H26B H 0.7428 0.6787 0.3421 0.073 Uiso 1 1 calc R . .
C27 C 0.80589(17) 0.6482(4) 0.38930(13) 0.0611(10) Uani 1 1 d . . .
H27A H 0.7862 0.5802 0.4113 0.073 Uiso 1 1 calc R . .
H27B H 0.8455 0.6153 0.3885 0.073 Uiso 1 1 calc R . .
O28 O 0.80186(10) 0.8133(3) 0.40265(8) 0.0578(6) Uani 1 1 d . . .
C29 C 0.83758(17) 0.8520(5) 0.44000(11) 0.0616(10) Uani 1 1 d . . .
H29A H 0.8749 0.8045 0.4354 0.074 Uiso 1 1 calc R . .
H29B H 0.8217 0.8080 0.4680 0.074 Uiso 1 1 calc R . .
C30 C 0.84247(17) 1.0324(5) 0.44362(11) 0.0579(9) Uani 1 1 d . . .
H30A H 0.8049 1.0814 0.4435 0.069 Uiso 1 1 calc R . .
H30B H 0.8613 1.0617 0.4720 0.069 Uiso 1 1 calc R . .
O31 O 0.87457(11) 1.0897(3) 0.40572(7) 0.0569(6) Uani 1 1 d . . .
C32 C 0.86819(14) 1.2573(4) 0.39692(10) 0.0470(8) Uani 1 1 d . . .
H32A H 0.8837 1.3201 0.4221 0.056 Uiso 1 1 calc R . .
H32B H 0.8282 1.2841 0.3938 0.056 Uiso 1 1 calc R . .
C33 C 0.89921(14) 1.2973(4) 0.35366(10) 0.0450(8) Uani 1 1 d . . .
H33A H 0.8990 1.4139 0.3485 0.054 Uiso 1 1 calc R . .
H33B H 0.9384 1.2613 0.3557 0.054 Uiso 1 1 calc R . .
O34 O 0.87112(9) 1.2162(3) 0.31717(6) 0.0434(5) Uani 1 1 d . . .
H51A H 0.9045 0.9252 0.3608 0.052 Uiso 1 1 d R . .
H51B H 0.8884 0.8137 0.3311 0.052 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O51 0.0378(12) 0.0686(14) 0.0456(12) 0.0009(11) 0.0064(10) 0.0170(11)
Ni1 0.0269(3) 0.0391(3) 0.0171(2) -0.00116(19) 0.00043(18) 0.0005(2)
S2 0.0302(4) 0.0829(6) 0.0207(3) 0.0013(3) -0.0010(3) 0.0056(4)
P3 0.0269(4) 0.0353(4) 0.0267(3) -0.0039(3) -0.0034(3) 0.0004(3)
N4 0.0354(13) 0.0476(14) 0.0202(11) -0.0008(10) 0.0025(9) -0.0121(11)
C5 0.0301(14) 0.0315(13) 0.0211(13) 0.0028(10) 0.0006(11) 0.0005(11)
S6 0.0294(4) 0.0586(5) 0.0207(3) -0.0081(3) 0.0034(3) -0.0067(3)
O7 0.0551(14) 0.0392(12) 0.0769(17) -0.0072(11) -0.0313(12) 0.0068(10)
C8 0.095(9) 0.078(8) 0.083(8) -0.011(6) -0.023(6) 0.003(6)
C9 0.144(11) 0.146(10) 0.154(11) 0.056(8) -0.011(8) -0.006(8)
C10 0.128(10) 0.149(11) 0.168(11) -0.020(9) 0.003(8) 0.029(8)
C8B 0.046(4) 0.039(4) 0.089(6) 0.005(3) -0.018(4) 0.022(3)
C9B 0.143(9) 0.117(7) 0.117(6) 0.056(5) -0.033(6) 0.005(6)
C10B 0.158(9) 0.116(7) 0.162(8) -0.052(6) -0.018(7) 0.078(6)
O11 0.0263(10) 0.0439(11) 0.0439(12) 0.0013(9) 0.0019(8) -0.0019(8)
C12 0.0441(19) 0.0505(19) 0.054(2) -0.0035(15) 0.0030(15) 0.0152(15)
C13 0.084(3) 0.122(4) 0.090(3) -0.024(3) -0.032(3) 0.058(3)
C14 0.105(4) 0.111(4) 0.063(3) -0.011(3) 0.020(3) 0.047(3)
N15 0.0296(12) 0.0422(13) 0.0185(10) -0.0047(9) 0.0028(9) -0.0108(10)
C16 0.0327(15) 0.0386(15) 0.0191(12) -0.0010(11) 0.0016(10) -0.0053(11)
C17 0.0405(16) 0.0385(15) 0.0207(13) -0.0064(11) 0.0030(11) -0.0111(12)
C18 0.0326(15) 0.0396(15) 0.0245(13) 0.0007(11) 0.0018(11) -0.0086(12)
C19 0.0351(16) 0.0443(16) 0.0240(13) -0.0051(11) 0.0064(11) -0.0049(12)
C20 0.0521(19) 0.0511(18) 0.0297(15) -0.0182(13) 0.0082(13) -0.0197(15)
C21 0.0411(17) 0.0493(17) 0.0330(15) -0.0074(13) 0.0114(13) -0.0172(14)
O22 0.0445(12) 0.0509(12) 0.0331(11) -0.0068(9) 0.0107(9) -0.0211(10)
C23 0.068(2) 0.059(2) 0.0377(17) -0.0125(15) 0.0115(16) -0.0301(18)
C24 0.064(2) 0.061(2) 0.053(2) -0.0062(16) 0.0110(18) -0.0312(18)
O25 0.0540(15) 0.0652(15) 0.0557(15) 0.0093(12) 0.0166(12) -0.0145(12)
C26 0.064(2) 0.051(2) 0.067(2) 0.0124(17) 0.0245(19) -0.0072(17)
C27 0.065(2) 0.051(2) 0.067(2) 0.0181(17) 0.0265(19) 0.0056(17)
O28 0.0602(15) 0.0561(14) 0.0572(15) 0.0057(11) 0.0083(12) 0.0176(11)
C29 0.065(2) 0.080(3) 0.0404(19) 0.0152(17) 0.0176(17) 0.022(2)
C30 0.062(2) 0.079(3) 0.0321(17) 0.0017(16) 0.0134(15) 0.0093(19)
O31 0.0635(16) 0.0693(16) 0.0378(12) 0.0007(11) 0.0203(11) 0.0112(12)
C32 0.053(2) 0.057(2) 0.0303(16) -0.0154(14) 0.0077(14) -0.0084(16)
C33 0.0469(18) 0.0565(19) 0.0317(16) -0.0175(14) 0.0063(13) -0.0107(14)
O34 0.0430(12) 0.0590(13) 0.0282(10) -0.0151(9) 0.0112(9) -0.0143(10)

_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
O51 H51A 0.8386 . ?
O51 H51B 0.8409 . ?
Ni1 S6 2.2113(6) . ?
Ni1 S6 2.2113(6) 5_775 ?
Ni1 S2 2.2179(7) . ?
Ni1 S2 2.2179(7) 5_775 ?
S2 P3 1.9934(10) . ?
P3 O7 1.556(2) . ?
P3 O11 1.573(2) . ?
P3 N4 1.586(2) . ?
N4 C5 1.315(3) . ?
C5 N15 1.350(3) . ?
C5 S6 1.750(3) . ?
O7 C8B 1.428(6) . ?
O7 C8 1.430(13) . ?
C8 C10 1.4700(11) . ?
C8 C9 1.4701(11) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C8B C9B 1.4702(11) . ?
C8B C10B 1.4702(10) . ?
C8B H8B 0.9800 . ?
C9B H9D 0.9600 . ?
C9B H9E 0.9600 . ?
C9B H9F 0.9600 . ?
C10B H10D 0.9600 . ?
C10B H10E 0.9600 . ?
C10B H10F 0.9600 . ?
O11 C12 1.463(4) . ?
C12 C13 1.492(5) . ?
C12 C14 1.494(5) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
N15 C16 1.424(3) . ?
N15 H15 0.8600 . ?
C16 C21 1.375(4) . ?
C16 C17 1.398(4) . ?
C17 C18 1.387(4) . ?
C17 H17 0.9300 . ?
C18 O22 1.369(3) . ?
C18 C19 1.399(4) . ?
C19 O34 1.373(3) . ?
C19 C20 1.378(4) . ?
C20 C21 1.393(4) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
O22 C23 1.426(4) . ?
C23 C24 1.511(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 O25 1.403(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
O25 C26 1.424(4) . ?
C26 C27 1.495(5) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 O28 1.415(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
O28 C29 1.414(4) . ?
C29 C30 1.491(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 O31 1.422(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
O31 C32 1.410(4) . ?
C32 C33 1.497(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 O34 1.421(3) . ?
C33 H33A 0.9700 . ?
C33 H33B 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
H51A O51 H51B 103.6 . . ?
S6 Ni1 S6 179.999(13) . 5_775 ?
S6 Ni1 S2 97.80(3) . . ?
S6 Ni1 S2 82.20(3) 5_775 . ?
S6 Ni1 S2 82.20(3) . 5_775 ?
S6 Ni1 S2 97.80(3) 5_775 5_775 ?
S2 Ni1 S2 180.0 . 5_775 ?
P3 S2 Ni1 104.05(4) . . ?
O7 P3 O11 98.38(12) . . ?
O7 P3 N4 111.37(13) . . ?
O11 P3 N4 107.31(12) . . ?
O7 P3 S2 113.02(11) . . ?
O11 P3 S2 107.87(8) . . ?
N4 P3 S2 116.98(9) . . ?
C5 N4 P3 128.77(18) . . ?
N4 C5 N15 119.2(2) . . ?
N4 C5 S6 128.02(19) . . ?
N15 C5 S6 112.70(19) . . ?
C5 S6 Ni1 118.08(9) . . ?
C8B O7 P3 125.2(4) . . ?
C8 O7 P3 125.8(6) . . ?
O7 C8 C10 109.7(16) . . ?
O7 C8 C9 102.7(12) . . ?
C10 C8 C9 115.36(18) . . ?
O7 C8 H8 109.6 . . ?
C10 C8 H8 109.6 . . ?
C9 C8 H8 109.6 . . ?
O7 C8B C9B 112.8(7) . . ?
O7 C8B C10B 106.9(7) . . ?
C9B C8B C10B 115.30(17) . . ?
O7 C8B H8B 107.2 . . ?
C9B C8B H8B 107.2 . . ?
C10B C8B H8B 107.2 . . ?
C8B C9B H9D 109.5 . . ?
C8B C9B H9E 109.5 . . ?
H9D C9B H9E 109.5 . . ?
C8B C9B H9F 109.5 . . ?
H9D C9B H9F 109.5 . . ?
H9E C9B H9F 109.5 . . ?
C8B C10B H10D 109.5 . . ?
C8B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C12 O11 P3 121.10(19) . . ?
O11 C12 C13 107.2(3) . . ?
O11 C12 C14 107.8(3) . . ?
C13 C12 C14 114.6(4) . . ?
O11 C12 H12 109.0 . . ?
C13 C12 H12 109.0 . . ?
C14 C12 H12 109.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C5 N15 C16 128.9(2) . . ?
C5 N15 H15 115.6 . . ?
C16 N15 H15 115.6 . . ?
C21 C16 C17 119.4(2) . . ?
C21 C16 N15 117.2(2) . . ?
C17 C16 N15 123.3(2) . . ?
C18 C17 C16 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
O22 C18 C17 123.6(2) . . ?
O22 C18 C19 116.3(2) . . ?
C17 C18 C19 120.1(2) . . ?
O34 C19 C20 124.8(2) . . ?
O34 C19 C18 116.4(2) . . ?
C20 C19 C18 118.7(2) . . ?
C19 C20 C21 121.3(3) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C16 C21 C20 120.0(3) . . ?
C16 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C18 O22 C23 117.4(2) . . ?
O22 C23 C24 106.9(3) . . ?
O22 C23 H23A 110.3 . . ?
C24 C23 H23A 110.3 . . ?
O22 C23 H23B 110.3 . . ?
C24 C23 H23B 110.3 . . ?
H23A C23 H23B 108.6 . . ?
O25 C24 C23 108.2(3) . . ?
O25 C24 H24A 110.0 . . ?
C23 C24 H24A 110.0 . . ?
O25 C24 H24B 110.0 . . ?
C23 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
C24 O25 C26 114.8(3) . . ?
O25 C26 C27 108.4(3) . . ?
O25 C26 H26A 110.0 . . ?
C27 C26 H26A 110.0 . . ?
O25 C26 H26B 110.0 . . ?
C27 C26 H26B 110.0 . . ?
H26A C26 H26B 108.4 . . ?
O28 C27 C26 109.4(3) . . ?
O28 C27 H27A 109.8 . . ?
C26 C27 H27A 109.8 . . ?
O28 C27 H27B 109.8 . . ?
C26 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
C29 O28 C27 112.9(3) . . ?
O28 C29 C30 108.9(3) . . ?
O28 C29 H29A 109.9 . . ?
C30 C29 H29A 109.9 . . ?
O28 C29 H29B 109.9 . . ?
C30 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
O31 C30 C29 108.3(3) . . ?
O31 C30 H30A 110.0 . . ?
C29 C30 H30A 110.0 . . ?
O31 C30 H30B 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
C32 O31 C30 114.2(2) . . ?
O31 C32 C33 108.5(2) . . ?
O31 C32 H32A 110.0 . . ?
C33 C32 H32A 110.0 . . ?
O31 C32 H32B 110.0 . . ?
C33 C32 H32B 110.0 . . ?
H32A C32 H32B 108.4 . . ?
O34 C33 C32 107.8(2) . . ?
O34 C33 H33A 110.1 . . ?
C32 C33 H33A 110.1 . . ?
O34 C33 H33B 110.1 . . ?
C32 C33 H33B 110.1 . . ?
H33A C33 H33B 108.5 . . ?
C19 O34 C33 116.4(2) . . ?

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
S6 Ni1 S2 P3 -44.85(4) . . . . ?
S6 Ni1 S2 P3 135.15(4) 5_775 . . . ?
Ni1 S2 P3 O7 -74.45(10) . . . . ?
Ni1 S2 P3 O11 177.88(8) . . . . ?
Ni1 S2 P3 N4 56.89(11) . . . . ?
O7 P3 N4 C5 103.6(3) . . . . ?
O11 P3 N4 C5 -149.8(2) . . . . ?
S2 P3 N4 C5 -28.5(3) . . . . ?
P3 N4 C5 N15 172.6(2) . . . . ?
P3 N4 C5 S6 -10.6(4) . . . . ?
N4 C5 S6 Ni1 11.0(3) . . . . ?
N15 C5 S6 Ni1 -171.93(15) . . . . ?
S2 Ni1 S6 C5 20.60(10) . . . . ?
S2 Ni1 S6 C5 -159.40(10) 5_775 . . . ?
O11 P3 O7 C8B -149.6(5) . . . . ?
N4 P3 O7 C8B -37.2(5) . . . . ?
S2 P3 O7 C8B 96.9(5) . . . . ?
O11 P3 O7 C8 -127.8(9) . . . . ?
N4 P3 O7 C8 -15.5(9) . . . . ?
S2 P3 O7 C8 118.6(9) . . . . ?
C8B O7 C8 C10 -18(2) . . . . ?
P3 O7 C8 C10 -112.0(10) . . . . ?
C8B O7 C8 C9 -141(3) . . . . ?
P3 O7 C8 C9 124.9(10) . . . . ?
C8 O7 C8B C9B 3(3) . . . . ?
P3 O7 C8B C9B 101.1(7) . . . . ?
C8 O7 C8B C10B 130(3) . . . . ?
P3 O7 C8B C10B -131.2(6) . . . . ?
O7 P3 O11 C12 -177.8(2) . . . . ?
N4 P3 O11 C12 66.6(2) . . . . ?
S2 P3 O11 C12 -60.3(2) . . . . ?
P3 O11 C12 C13 118.7(3) . . . . ?
P3 O11 C12 C14 -117.4(3) . . . . ?
N4 C5 N15 C16 -2.3(4) . . . . ?
S6 C5 N15 C16 -179.6(2) . . . . ?
C5 N15 C16 C21 -160.0(3) . . . . ?
C5 N15 C16 C17 21.4(4) . . . . ?
C21 C16 C17 C18 0.6(4) . . . . ?
N15 C16 C17 C18 179.3(3) . . . . ?
C16 C17 C18 O22 179.1(3) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
O22 C18 C19 O34 0.4(4) . . . . ?
C17 C18 C19 O34 180.0(3) . . . . ?
O22 C18 C19 C20 -179.7(3) . . . . ?
C17 C18 C19 C20 -0.1(4) . . . . ?
O34 C19 C20 C21 -179.7(3) . . . . ?
C18 C19 C20 C21 0.4(5) . . . . ?
C17 C16 C21 C20 -0.4(5) . . . . ?
N15 C16 C21 C20 -179.1(3) . . . . ?
C19 C20 C21 C16 -0.1(5) . . . . ?
C17 C18 O22 C23 18.6(4) . . . . ?
C19 C18 O22 C23 -161.8(3) . . . . ?
C18 O22 C23 C24 167.2(3) . . . . ?
O22 C23 C24 O25 -66.4(4) . . . . ?
C23 C24 O25 C26 172.6(3) . . . . ?
C24 O25 C26 C27 -161.9(3) . . . . ?
O25 C26 C27 O28 71.5(4) . . . . ?
C26 C27 O28 C29 -164.8(3) . . . . ?
C27 O28 C29 C30 165.0(3) . . . . ?
O28 C29 C30 O31 -69.4(4) . . . . ?
C29 C30 O31 C32 161.7(3) . . . . ?
C30 O31 C32 C33 -174.2(3) . . . . ?
O31 C32 C33 O34 65.9(3) . . . . ?
C20 C19 O34 C33 -22.2(4) . . . . ?
C18 C19 O34 C33 157.7(3) . . . . ?
C32 C33 O34 C19 -164.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.30
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.057