Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Robert Paine' _publ_contact_author_address ; Dept. of Chemistry University of New Mexico MSC03 2060 Albuquerque New Mexico 87131-0001 UNITED STATES OF AMERICA ; _publ_contact_author_email RTPAINE@UNM.EDU loop_ _publ_author_name 'Xin Min Gan' ' Eileen N. Duesler' ' Sahrah Parveen' 'Robert T. Paine' _publ_section_title ; Synthesis of Trifunctional Ligands Containing Thiophosphoryl and Pyridine or Pyridine N-Oxide Donor Groups ; data_rtp018a _database_code_CSD 215637 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H27 N3 Ni O6 P2 S2' _chemical_formula_weight 722.33 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 Pbca 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 15.431(2) _cell_length_b 18.055(3) _cell_length_c 22.931(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6388.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 13.32 _exptl_crystal_description prism _exptl_crystal_colour apple-green _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.184 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type 'gaussian face-indexed' _exptl_absorpt_correction_T_min 0.79345 _exptl_absorpt_correction_T_max 0.84732 _exptl_absorpt_process_details ? _exptl_special_details ; Note that standard reflection intensities gradually increased 28% over the course of data collection [~120 hours]. Bruker engineers think it is due to worn gears but most likely due to the x-ray tube behavior. octants -h,k,+/-l collected for 2-theta between 3 and 50 degrees. ; _diffrn_ambient_temperature 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 25 _diffrn_reflns_number 11094 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5623 _reflns_number_gt 3412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0334P)^2^+0.0000P] 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 ; all hydrogen atoms allowed to vary in position with fixed isotropic U=1.25U[equiv] of parent atom ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5623 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Ni Ni 0.18561(3) 0.04910(3) 0.63899(2) 0.03344(16) Uani 1 1 d . . . S1 S 0.20031(7) 0.13906(6) 0.72021(5) 0.0420(3) Uani 1 1 d . . . S2 S 0.23714(8) 0.14409(8) 0.57434(5) 0.0508(4) Uani 1 1 d . . . P1 P 0.10117(7) 0.11142(6) 0.77048(4) 0.0312(3) Uani 1 1 d . . . P2 P 0.13705(8) 0.16155(7) 0.52204(5) 0.0364(3) Uani 1 1 d . . . N1 N 0.0502(2) 0.06339(16) 0.63327(13) 0.0295(8) Uani 1 1 d . . . N2 N 0.2946(3) -0.0307(2) 0.69275(15) 0.0454(10) Uani 1 1 d . . . N3 N 0.1531(3) -0.0906(3) 0.57485(16) 0.0503(11) Uani 1 1 d . . . O1 O 0.2131(2) -0.04004(16) 0.69865(13) 0.0471(8) Uani 1 1 d . . . O2 O 0.31695(19) 0.02135(17) 0.65857(13) 0.0468(8) Uani 1 1 d . . . O3 O 0.3477(2) -0.0680(2) 0.71794(15) 0.0749(11) Uani 1 1 d . . . O4 O 0.1981(2) -0.03191(18) 0.57625(13) 0.0541(9) Uani 1 1 d . . . O5 O 0.0804(3) -0.0911(2) 0.5934(2) 0.0920(14) Uani 1 1 d . . . O6 O 0.1810(3) -0.1458(2) 0.55061(17) 0.0981(15) Uani 1 1 d . . . C1 C 0.0002(3) 0.0586(2) 0.68133(17) 0.0318(10) Uani 1 1 d . . . C2 C -0.0867(3) 0.0756(2) 0.68113(18) 0.0422(12) Uani 1 1 d . . . H2 H -0.1190 0.0719 0.7153 0.053 Uiso 1 1 calc R . . C3 C -0.1254(3) 0.0978(3) 0.6303(2) 0.0499(13) Uani 1 1 d . . . H3 H -0.1838 0.1106 0.6295 0.062 Uiso 1 1 calc R . . C4 C -0.0764(3) 0.1009(2) 0.5808(2) 0.0457(12) Uani 1 1 d . . . H4 H -0.1018 0.1147 0.5456 0.057 Uiso 1 1 calc R . . C5 C 0.0111(3) 0.0835(2) 0.58274(17) 0.0334(10) Uani 1 1 d . . . C6 C 0.0412(3) 0.0349(2) 0.73769(16) 0.0336(10) Uani 1 1 d . . . H6A H 0.0802 -0.0062 0.7305 0.042 Uiso 1 1 calc R . . H6B H -0.0034 0.0182 0.7644 0.042 Uiso 1 1 calc R . . C7 C 0.0618(3) 0.0848(2) 0.52655(17) 0.0384(11) Uani 1 1 d . . . H7A H 0.0216 0.0878 0.4941 0.048 Uiso 1 1 calc R . . H7B H 0.0937 0.0388 0.5229 0.048 Uiso 1 1 calc R . . C8 C 0.1325(3) 0.0807(2) 0.84242(17) 0.0309(10) Uani 1 1 d . . . C9 C 0.1622(3) 0.0088(2) 0.84922(18) 0.0404(12) Uani 1 1 d . . . H9 H 0.1633 -0.0234 0.8176 0.051 Uiso 1 1 calc R . . C10 C 0.1905(3) -0.0148(3) 0.90360(19) 0.0504(13) Uani 1 1 d . . . H10 H 0.2100 -0.0631 0.9085 0.063 Uiso 1 1 calc R . . C11 C 0.1897(3) 0.0334(3) 0.95055(18) 0.0500(13) Uani 1 1 d . . . H11 H 0.2076 0.0172 0.9871 0.063 Uiso 1 1 calc R . . C12 C 0.1626(3) 0.1048(3) 0.94311(18) 0.0447(12) Uani 1 1 d . . . H12 H 0.1637 0.1377 0.9743 0.056 Uiso 1 1 calc R . . C13 C 0.1335(3) 0.1283(2) 0.88922(17) 0.0392(11) Uani 1 1 d . . . H13 H 0.1144 0.1768 0.8845 0.049 Uiso 1 1 calc R . . C14 C 0.0238(3) 0.1855(2) 0.77878(17) 0.0341(10) Uani 1 1 d . . . C15 C 0.0271(3) 0.2448(3) 0.74152(19) 0.0521(13) Uani 1 1 d . . . H15 H 0.0703 0.2473 0.7134 0.065 Uiso 1 1 calc R . . C16 C -0.0336(4) 0.3008(3) 0.7456(2) 0.0662(16) Uani 1 1 d . . . H16 H -0.0315 0.3405 0.7199 0.083 Uiso 1 1 calc R . . C17 C -0.0973(3) 0.2980(3) 0.7876(2) 0.0610(15) Uani 1 1 d . . . H17 H -0.1373 0.3363 0.7910 0.076 Uiso 1 1 calc R . . C18 C -0.1010(3) 0.2384(3) 0.8241(2) 0.0582(14) Uani 1 1 d . . . H18 H -0.1442 0.2360 0.8523 0.073 Uiso 1 1 calc R . . C19 C -0.0413(3) 0.1815(3) 0.8197(2) 0.0491(12) Uani 1 1 d . . . H19 H -0.0451 0.1407 0.8444 0.061 Uiso 1 1 calc R . . C20 C 0.1713(3) 0.1702(2) 0.44721(17) 0.0362(11) Uani 1 1 d . . . C21 C 0.2491(3) 0.2066(2) 0.43578(19) 0.0482(12) Uani 1 1 d . . . H21 H 0.2821 0.2250 0.4665 0.060 Uiso 1 1 calc R . . C22 C 0.2775(4) 0.2155(3) 0.3788(2) 0.0600(15) Uani 1 1 d . . . H22 H 0.3291 0.2403 0.3711 0.075 Uiso 1 1 calc R . . C23 C 0.2286(4) 0.1873(3) 0.3338(2) 0.0640(16) Uani 1 1 d . . . H23 H 0.2477 0.1927 0.2955 0.080 Uiso 1 1 calc R . . C24 C 0.1532(4) 0.1519(3) 0.3446(2) 0.0645(16) Uani 1 1 d . . . H24 H 0.1207 0.1333 0.3137 0.081 Uiso 1 1 calc R . . C25 C 0.1241(3) 0.1432(3) 0.40111(19) 0.0566(14) Uani 1 1 d . . . H25 H 0.0720 0.1187 0.4080 0.071 Uiso 1 1 calc R . . C26 C 0.0775(3) 0.2450(2) 0.53757(18) 0.0407(11) Uani 1 1 d . . . C27 C 0.0075(3) 0.2644(3) 0.5028(2) 0.0548(13) Uani 1 1 d . . . H27 H -0.0119 0.2323 0.4739 0.069 Uiso 1 1 calc R . . C28 C -0.0332(4) 0.3318(3) 0.5114(3) 0.0724(17) Uani 1 1 d . . . H28 H -0.0793 0.3454 0.4875 0.091 Uiso 1 1 calc R . . C29 C -0.0067(4) 0.3784(3) 0.5543(3) 0.086(2) Uani 1 1 d . . . H29 H -0.0346 0.4235 0.5597 0.108 Uiso 1 1 calc R . . C30 C 0.0608(4) 0.3590(3) 0.5895(3) 0.0800(19) Uani 1 1 d . . . H30 H 0.0781 0.3908 0.6192 0.100 Uiso 1 1 calc R . . C31 C 0.1041(4) 0.2925(3) 0.5815(2) 0.0612(14) Uani 1 1 d . . . H31 H 0.1506 0.2800 0.6054 0.077 Uiso 1 1 calc 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 Ni 0.0272(3) 0.0435(3) 0.0296(3) 0.0021(3) 0.0002(3) -0.0014(3) S1 0.0374(7) 0.0492(7) 0.0395(6) -0.0068(5) 0.0087(5) -0.0106(6) S2 0.0387(7) 0.0709(9) 0.0428(7) 0.0200(6) -0.0095(6) -0.0153(7) P1 0.0288(6) 0.0357(6) 0.0290(6) -0.0008(5) 0.0011(5) 0.0003(5) P2 0.0328(7) 0.0468(7) 0.0297(6) 0.0047(5) -0.0014(5) -0.0062(6) N1 0.0285(19) 0.0299(19) 0.0301(18) -0.0012(16) -0.0015(16) -0.0013(16) N2 0.047(3) 0.054(3) 0.036(2) -0.0019(19) -0.007(2) 0.011(2) N3 0.061(3) 0.054(3) 0.036(2) 0.000(2) -0.007(2) -0.004(3) O1 0.039(2) 0.052(2) 0.0502(19) 0.0068(16) 0.0033(16) -0.0006(17) O2 0.0342(18) 0.054(2) 0.0516(19) 0.0013(16) 0.0032(16) -0.0018(17) O3 0.068(3) 0.088(3) 0.068(2) 0.018(2) -0.020(2) 0.032(2) O4 0.060(2) 0.058(2) 0.0444(19) -0.0124(16) 0.0087(17) -0.0104(19) O5 0.045(3) 0.073(3) 0.158(4) 0.000(3) 0.009(3) -0.011(2) O6 0.150(4) 0.056(3) 0.089(3) -0.016(2) 0.024(3) 0.005(3) C1 0.030(2) 0.031(2) 0.035(2) 0.000(2) -0.002(2) -0.009(2) C2 0.029(3) 0.060(3) 0.038(3) 0.001(2) 0.005(2) -0.012(2) C3 0.025(3) 0.067(3) 0.058(3) 0.002(3) -0.005(2) 0.002(2) C4 0.037(3) 0.053(3) 0.047(3) 0.007(2) -0.014(2) -0.008(2) C5 0.030(3) 0.039(2) 0.031(2) 0.004(2) -0.004(2) -0.009(2) C6 0.034(3) 0.035(2) 0.031(2) -0.0004(19) 0.0053(19) -0.003(2) C7 0.035(3) 0.049(3) 0.031(2) 0.003(2) -0.008(2) -0.009(2) C8 0.027(2) 0.033(2) 0.033(2) 0.0005(19) -0.0006(19) 0.002(2) C9 0.048(3) 0.038(3) 0.035(3) -0.004(2) -0.006(2) 0.008(2) C10 0.057(3) 0.038(3) 0.056(3) 0.009(2) -0.011(3) 0.009(3) C11 0.048(3) 0.072(4) 0.030(2) 0.013(2) -0.003(2) -0.003(3) C12 0.047(3) 0.055(3) 0.032(2) -0.009(2) 0.002(2) 0.006(3) C13 0.038(3) 0.041(3) 0.038(3) -0.004(2) -0.001(2) 0.005(2) C14 0.030(3) 0.041(3) 0.031(2) 0.002(2) -0.003(2) 0.003(2) C15 0.052(3) 0.056(3) 0.048(3) 0.007(3) 0.004(3) 0.012(3) C16 0.078(4) 0.047(3) 0.073(4) 0.017(3) -0.003(4) 0.015(3) C17 0.053(4) 0.054(3) 0.077(4) -0.006(3) -0.014(3) 0.018(3) C18 0.037(3) 0.073(4) 0.065(4) -0.009(3) 0.008(3) 0.007(3) C19 0.041(3) 0.048(3) 0.058(3) 0.007(3) 0.002(3) 0.002(3) C20 0.040(3) 0.038(3) 0.031(2) 0.004(2) 0.001(2) 0.007(2) C21 0.052(3) 0.046(3) 0.046(3) 0.002(2) 0.005(3) 0.003(3) C22 0.062(4) 0.056(3) 0.063(4) 0.014(3) 0.021(3) 0.002(3) C23 0.077(4) 0.076(4) 0.039(3) 0.017(3) 0.022(3) 0.019(3) C24 0.066(4) 0.096(5) 0.032(3) 0.001(3) 0.000(3) 0.006(4) C25 0.047(3) 0.083(4) 0.039(3) 0.001(3) 0.000(2) 0.000(3) C26 0.038(3) 0.044(3) 0.040(3) 0.004(2) 0.008(2) -0.010(2) C27 0.034(3) 0.061(3) 0.069(3) 0.002(3) 0.002(3) -0.003(3) C28 0.036(3) 0.076(4) 0.106(5) 0.013(4) 0.011(3) 0.011(3) C29 0.071(5) 0.066(4) 0.122(6) -0.020(4) 0.034(4) 0.020(4) C30 0.083(5) 0.077(5) 0.081(5) -0.037(4) 0.017(4) 0.001(4) C31 0.066(4) 0.070(4) 0.048(3) -0.005(3) 0.011(3) 0.000(3) _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 Ni O4 2.061(3) . ? Ni N1 2.110(3) . ? Ni O2 2.136(3) . ? Ni O1 2.154(3) . ? Ni S2 2.4024(13) . ? Ni S1 2.4814(12) . ? S1 P1 1.9795(15) . ? S2 P2 1.9807(16) . ? P1 C14 1.802(4) . ? P1 C8 1.806(4) . ? P1 C6 1.825(4) . ? P2 C26 1.801(5) . ? P2 C20 1.802(4) . ? P2 C7 1.811(4) . ? N1 C1 1.347(5) . ? N1 C5 1.356(5) . ? N2 O3 1.208(4) . ? N2 O2 1.271(4) . ? N2 O1 1.276(4) . ? N3 O5 1.199(5) . ? N3 O6 1.220(5) . ? N3 O4 1.268(5) . ? C1 C2 1.377(5) . ? C1 C6 1.501(5) . ? C2 C3 1.370(6) . ? C2 H2 0.9300 . ? C3 C4 1.365(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(6) . ? C4 H4 0.9300 . ? C5 C7 1.507(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.375(5) . ? C8 C9 1.386(5) . ? C9 C10 1.388(6) . ? C9 H9 0.9300 . ? C10 C11 1.384(6) . ? C10 H10 0.9300 . ? C11 C12 1.367(6) . ? C11 H11 0.9300 . ? C12 C13 1.381(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.371(6) . ? C14 C19 1.377(6) . ? C15 C16 1.382(6) . ? C15 H15 0.9300 . ? C16 C17 1.375(7) . ? C16 H16 0.9300 . ? C17 C18 1.365(7) . ? C17 H17 0.9300 . ? C18 C19 1.384(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.374(6) . ? C20 C21 1.392(6) . ? C21 C22 1.388(6) . ? C21 H21 0.9300 . ? C22 C23 1.376(7) . ? C22 H22 0.9300 . ? C23 C24 1.351(7) . ? C23 H23 0.9300 . ? C24 C25 1.381(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C31 1.386(6) . ? C26 C27 1.388(6) . ? C27 C28 1.385(7) . ? C27 H27 0.9300 . ? C28 C29 1.357(8) . ? C28 H28 0.9300 . ? C29 C30 1.364(8) . ? C29 H29 0.9300 . ? C30 C31 1.386(7) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? 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 Ni N1 97.84(13) . . ? O4 Ni O2 83.75(12) . . ? N1 Ni O2 169.07(12) . . ? O4 Ni O1 83.95(12) . . ? N1 Ni O1 109.03(12) . . ? O2 Ni O1 60.27(11) . . ? O4 Ni S2 92.57(10) . . ? N1 Ni S2 101.67(9) . . ? O2 Ni S2 89.03(9) . . ? O1 Ni S2 149.30(9) . . ? O4 Ni S1 168.50(10) . . ? N1 Ni S1 93.28(9) . . ? O2 Ni S1 84.78(8) . . ? O1 Ni S1 89.68(9) . . ? S2 Ni S1 88.03(5) . . ? P1 S1 Ni 101.62(6) . . ? P2 S2 Ni 103.25(6) . . ? C14 P1 C8 107.98(18) . . ? C14 P1 C6 105.63(19) . . ? C8 P1 C6 106.23(18) . . ? C14 P1 S1 112.73(15) . . ? C8 P1 S1 113.72(14) . . ? C6 P1 S1 110.04(14) . . ? C26 P2 C20 105.37(19) . . ? C26 P2 C7 107.6(2) . . ? C20 P2 C7 108.0(2) . . ? C26 P2 S2 114.29(16) . . ? C20 P2 S2 111.18(15) . . ? C7 P2 S2 110.11(15) . . ? C1 N1 C5 117.5(3) . . ? C1 N1 Ni 120.5(3) . . ? C5 N1 Ni 121.8(3) . . ? O3 N2 O2 121.5(4) . . ? O3 N2 O1 123.0(4) . . ? O2 N2 O1 115.5(4) . . ? O5 N3 O6 119.0(5) . . ? O5 N3 O4 120.7(5) . . ? O6 N3 O4 120.1(5) . . ? N2 O1 Ni 91.6(2) . . ? N2 O2 Ni 92.6(2) . . ? N3 O4 Ni 124.0(3) . . ? N1 C1 C2 122.7(4) . . ? N1 C1 C6 118.8(4) . . ? C2 C1 C6 118.5(4) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 118.6(4) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C7 120.2(4) . . ? C4 C5 C7 118.3(4) . . ? C1 C6 P1 110.6(3) . . ? C1 C6 H6A 109.5 . . ? P1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C5 C7 P2 113.2(3) . . ? C5 C7 H7A 108.9 . . ? P2 C7 H7A 108.9 . . ? C5 C7 H7B 108.9 . . ? P2 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? C13 C8 C9 119.6(4) . . ? C13 C8 P1 121.6(3) . . ? C9 C8 P1 118.6(3) . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.2(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 120.7(4) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C19 119.5(4) . . ? C15 C14 P1 119.3(3) . . ? C19 C14 P1 121.1(3) . . ? C14 C15 C16 120.3(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.3(5) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 120.8(5) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 119.8(4) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C25 C20 C21 118.7(4) . . ? C25 C20 P2 123.1(4) . . ? C21 C20 P2 118.2(3) . . ? C22 C21 C20 120.3(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.5(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C20 C25 C24 120.6(5) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C31 C26 C27 119.6(5) . . ? C31 C26 P2 120.7(4) . . ? C27 C26 P2 119.6(4) . . ? C28 C27 C26 119.5(5) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C27 120.8(6) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.1(6) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C31 120.8(6) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C26 C31 C30 119.3(5) . . ? C26 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ni S1 P1 -121.8(5) . . . . ? N1 Ni S1 P1 43.44(10) . . . . ? O2 Ni S1 P1 -125.77(10) . . . . ? O1 Ni S1 P1 -65.60(10) . . . . ? S2 Ni S1 P1 145.02(6) . . . . ? O4 Ni S2 P2 75.30(11) . . . . ? N1 Ni S2 P2 -23.25(11) . . . . ? O2 Ni S2 P2 159.00(10) . . . . ? O1 Ni S2 P2 157.75(16) . . . . ? S1 Ni S2 P2 -116.19(7) . . . . ? Ni S1 P1 C14 -118.16(15) . . . . ? Ni S1 P1 C8 118.50(15) . . . . ? Ni S1 P1 C6 -0.53(15) . . . . ? Ni S2 P2 C26 103.85(16) . . . . ? Ni S2 P2 C20 -137.02(16) . . . . ? Ni S2 P2 C7 -17.34(16) . . . . ? O4 Ni N1 C1 126.7(3) . . . . ? O2 Ni N1 C1 29.0(8) . . . . ? O1 Ni N1 C1 40.4(3) . . . . ? S2 Ni N1 C1 -139.0(3) . . . . ? S1 Ni N1 C1 -50.4(3) . . . . ? O4 Ni N1 C5 -58.8(3) . . . . ? O2 Ni N1 C5 -156.5(6) . . . . ? O1 Ni N1 C5 -145.1(3) . . . . ? S2 Ni N1 C5 35.5(3) . . . . ? S1 Ni N1 C5 124.1(3) . . . . ? O3 N2 O1 Ni 180.0(4) . . . . ? O2 N2 O1 Ni 0.4(3) . . . . ? O4 Ni O1 N2 86.0(2) . . . . ? N1 Ni O1 N2 -177.8(2) . . . . ? O2 Ni O1 N2 -0.3(2) . . . . ? S2 Ni O1 N2 1.2(3) . . . . ? S1 Ni O1 N2 -84.4(2) . . . . ? O3 N2 O2 Ni -180.0(4) . . . . ? O1 N2 O2 Ni -0.4(4) . . . . ? O4 Ni O2 N2 -86.3(2) . . . . ? N1 Ni O2 N2 12.7(7) . . . . ? O1 Ni O2 N2 0.3(2) . . . . ? S2 Ni O2 N2 -179.0(2) . . . . ? S1 Ni O2 N2 92.9(2) . . . . ? O5 N3 O4 Ni 30.3(6) . . . . ? O6 N3 O4 Ni -155.2(3) . . . . ? N1 Ni O4 N3 -50.8(4) . . . . ? O2 Ni O4 N3 118.3(4) . . . . ? O1 Ni O4 N3 57.6(3) . . . . ? S2 Ni O4 N3 -153.0(3) . . . . ? S1 Ni O4 N3 114.3(5) . . . . ? C5 N1 C1 C2 -2.2(6) . . . . ? Ni N1 C1 C2 172.5(3) . . . . ? C5 N1 C1 C6 178.7(3) . . . . ? Ni N1 C1 C6 -6.5(5) . . . . ? N1 C1 C2 C3 0.5(6) . . . . ? C6 C1 C2 C3 179.6(4) . . . . ? C1 C2 C3 C4 1.4(7) . . . . ? C2 C3 C4 C5 -1.6(7) . . . . ? C1 N1 C5 C4 2.0(6) . . . . ? Ni N1 C5 C4 -172.6(3) . . . . ? C1 N1 C5 C7 -175.7(3) . . . . ? Ni N1 C5 C7 9.6(5) . . . . ? C3 C4 C5 N1 -0.2(7) . . . . ? C3 C4 C5 C7 177.6(4) . . . . ? N1 C1 C6 P1 77.9(4) . . . . ? C2 C1 C6 P1 -101.2(4) . . . . ? C14 P1 C6 C1 56.7(3) . . . . ? C8 P1 C6 C1 171.3(3) . . . . ? S1 P1 C6 C1 -65.2(3) . . . . ? N1 C5 C7 P2 -73.2(4) . . . . ? C4 C5 C7 P2 109.0(4) . . . . ? C26 P2 C7 C5 -52.0(4) . . . . ? C20 P2 C7 C5 -165.3(3) . . . . ? S2 P2 C7 C5 73.1(3) . . . . ? C14 P1 C8 C13 -30.2(4) . . . . ? C6 P1 C8 C13 -143.1(4) . . . . ? S1 P1 C8 C13 95.7(4) . . . . ? C14 P1 C8 C9 154.6(3) . . . . ? C6 P1 C8 C9 41.7(4) . . . . ? S1 P1 C8 C9 -79.5(4) . . . . ? C13 C8 C9 C10 1.7(7) . . . . ? P1 C8 C9 C10 177.0(4) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C9 C10 C11 C12 -1.2(8) . . . . ? C10 C11 C12 C13 2.0(7) . . . . ? C9 C8 C13 C12 -1.0(7) . . . . ? P1 C8 C13 C12 -176.1(3) . . . . ? C11 C12 C13 C8 -0.9(7) . . . . ? C8 P1 C14 C15 141.4(4) . . . . ? C6 P1 C14 C15 -105.3(4) . . . . ? S1 P1 C14 C15 14.9(4) . . . . ? C8 P1 C14 C19 -42.2(4) . . . . ? C6 P1 C14 C19 71.1(4) . . . . ? S1 P1 C14 C19 -168.7(3) . . . . ? C19 C14 C15 C16 1.1(7) . . . . ? P1 C14 C15 C16 177.5(4) . . . . ? C14 C15 C16 C17 0.8(8) . . . . ? C15 C16 C17 C18 -1.6(8) . . . . ? C16 C17 C18 C19 0.6(8) . . . . ? C15 C14 C19 C18 -2.1(7) . . . . ? P1 C14 C19 C18 -178.4(4) . . . . ? C17 C18 C19 C14 1.2(7) . . . . ? C26 P2 C20 C25 -92.4(4) . . . . ? C7 P2 C20 C25 22.3(4) . . . . ? S2 P2 C20 C25 143.2(4) . . . . ? C26 P2 C20 C21 87.1(4) . . . . ? C7 P2 C20 C21 -158.2(3) . . . . ? S2 P2 C20 C21 -37.2(4) . . . . ? C25 C20 C21 C22 0.5(7) . . . . ? P2 C20 C21 C22 -179.1(4) . . . . ? C20 C21 C22 C23 -0.8(7) . . . . ? C21 C22 C23 C24 0.7(8) . . . . ? C22 C23 C24 C25 -0.3(8) . . . . ? C21 C20 C25 C24 0.0(7) . . . . ? P2 C20 C25 C24 179.5(4) . . . . ? C23 C24 C25 C20 0.0(8) . . . . ? C20 P2 C26 C31 -120.1(4) . . . . ? C7 P2 C26 C31 124.8(4) . . . . ? S2 P2 C26 C31 2.2(4) . . . . ? C20 P2 C26 C27 55.8(4) . . . . ? C7 P2 C26 C27 -59.3(4) . . . . ? S2 P2 C26 C27 178.1(3) . . . . ? C31 C26 C27 C28 1.8(7) . . . . ? P2 C26 C27 C28 -174.1(4) . . . . ? C26 C27 C28 C29 -1.5(8) . . . . ? C27 C28 C29 C30 0.1(9) . . . . ? C28 C29 C30 C31 1.0(10) . . . . ? C27 C26 C31 C30 -0.7(7) . . . . ? P2 C26 C31 C30 175.2(4) . . . . ? C29 C30 C31 C26 -0.7(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17 O1 0.93 2.53 3.442(6) 165.9 3_556 C24 H24 O3 0.93 2.54 3.275(6) 136.2 2_554 C25 H25 O5 0.93 2.41 3.295(6) 160.2 5_556 C4 H4 O6 0.93 2.58 3.512(6) 175.8 5_556 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.341 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.067 #===END