# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _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_safin69 _database_code_depnum_ccdc_archive 'CCDC 805254' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H44 N4 Ni O8 P2 S4, C H2 Cl2' _chemical_formula_sum 'C31 H46 Cl2 N4 Ni O8 P2 S4' _chemical_formula_weight 922.51 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.3129(4) _cell_length_b 13.0620(5) _cell_length_c 18.7085(7) _cell_angle_alpha 79.439(2) _cell_angle_beta 84.354(2) _cell_angle_gamma 69.584(2) _cell_volume 2095.25(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7835 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 56997 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 32.62 _reflns_number_total 15238 _reflns_number_gt 11502 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0423P)^2^+0.7850P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15238 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.590720(19) 0.436555(12) 0.261210(9) 0.01820(4) Uani 1 1 d . . . P1 P 0.39286(4) 0.38491(3) 0.146500(18) 0.01986(7) Uani 1 1 d . . . S1 S 0.61231(4) 0.34868(3) 0.167680(19) 0.02514(7) Uani 1 1 d . . . S2 S 0.40587(4) 0.59006(3) 0.221569(19) 0.02676(8) Uani 1 1 d . . . N1 N 0.30310(14) 0.51271(9) 0.11539(6) 0.0232(2) Uani 1 1 d . . . N2 N 0.22602(15) 0.70068(9) 0.11879(7) 0.0250(2) Uani 1 1 d . . . H2 H 0.234(2) 0.7460(16) 0.1406(11) 0.037(5) Uiso 1 1 d . . . O1 O 0.29350(12) 0.35148(8) 0.21259(5) 0.0268(2) Uani 1 1 d . . . O2 O 0.38250(12) 0.31374(8) 0.08979(5) 0.02321(19) Uani 1 1 d . . . O3 O 0.12379(14) 0.89698(9) 0.16231(7) 0.0380(3) Uani 1 1 d . . . O4 O -0.11982(15) 0.99320(10) 0.13754(7) 0.0439(3) Uani 1 1 d . . . C1 C 0.30811(15) 0.59379(10) 0.14541(7) 0.0210(2) Uani 1 1 d . . . C2 C 0.32887(19) 0.23644(11) 0.24962(8) 0.0276(3) Uani 1 1 d . . . H2A H 0.4304 0.1895 0.2310 0.033 Uiso 1 1 calc R . . C3 C 0.3360(3) 0.23774(17) 0.32923(9) 0.0454(5) Uani 1 1 d . . . H3A H 0.4172 0.2659 0.3367 0.068 Uiso 1 1 calc R . . H3B H 0.3582 0.1624 0.3561 0.068 Uiso 1 1 calc R . . H3C H 0.2373 0.2857 0.3469 0.068 Uiso 1 1 calc R . . C4 C 0.2051(3) 0.19644(16) 0.23273(11) 0.0461(5) Uani 1 1 d . . . H4A H 0.1050 0.2462 0.2475 0.069 Uiso 1 1 calc R . . H4B H 0.2215 0.1216 0.2594 0.069 Uiso 1 1 calc R . . H4C H 0.2080 0.1954 0.1804 0.069 Uiso 1 1 calc R . . C5 C 0.47218(18) 0.30621(12) 0.02059(7) 0.0257(3) Uani 1 1 d . . . H5 H 0.5448 0.3482 0.0176 0.031 Uiso 1 1 calc R . . C6 C 0.5605(2) 0.18550(14) 0.02064(10) 0.0433(4) Uani 1 1 d . . . H6A H 0.6309 0.1577 0.0609 0.065 Uiso 1 1 calc R . . H6B H 0.6192 0.1758 -0.0255 0.065 Uiso 1 1 calc R . . H6C H 0.4890 0.1442 0.0266 0.065 Uiso 1 1 calc R . . C7 C 0.3601(2) 0.35693(16) -0.03948(9) 0.0427(4) Uani 1 1 d . . . H7A H 0.2864 0.3175 -0.0349 0.064 Uiso 1 1 calc R . . H7B H 0.4155 0.3513 -0.0867 0.064 Uiso 1 1 calc R . . H7C H 0.3052 0.4350 -0.0359 0.064 Uiso 1 1 calc R . . C11 C 0.11341(16) 0.74459(10) 0.06659(7) 0.0221(2) Uani 1 1 d . . . C12 C 0.00649(16) 0.85144(10) 0.07012(8) 0.0237(3) Uani 1 1 d . . . C13 C -0.10590(19) 0.89825(12) 0.01807(9) 0.0319(3) Uani 1 1 d . . . H13 H -0.1785 0.9699 0.0203 0.038 Uiso 1 1 calc R . . C14 C -0.1133(2) 0.84258(13) -0.03621(9) 0.0374(4) Uani 1 1 d . . . H14 H -0.1896 0.8758 -0.0715 0.045 Uiso 1 1 calc R . . C15 C -0.0080(2) 0.73712(13) -0.03911(9) 0.0365(4) Uani 1 1 d . . . H15 H -0.0134 0.6982 -0.0764 0.044 Uiso 1 1 calc R . . C16 C 0.10441(19) 0.68823(12) 0.01171(8) 0.0295(3) Uani 1 1 d . . . H16 H 0.1755 0.6162 0.0092 0.035 Uiso 1 1 calc R . . C17 C 0.01213(18) 0.91475(11) 0.12727(8) 0.0280(3) Uani 1 1 d . . . C18 C -0.1262(3) 1.05550(16) 0.19544(12) 0.0558(6) Uani 1 1 d . . . H18A H -0.0981 1.0044 0.2412 0.084 Uiso 1 1 calc R . . H18B H -0.2304 1.1077 0.2007 0.084 Uiso 1 1 calc R . . H18C H -0.0543 1.0964 0.1834 0.084 Uiso 1 1 calc R . . P1' P 0.79079(4) 0.48721(2) 0.377887(18) 0.01746(6) Uani 1 1 d . . . S1' S 0.57337(4) 0.52875(3) 0.351074(18) 0.02112(7) Uani 1 1 d . . . S2' S 0.76796(5) 0.28145(3) 0.30481(2) 0.03037(9) Uani 1 1 d . . . N1' N 0.87731(13) 0.35906(9) 0.40920(6) 0.0215(2) Uani 1 1 d . . . N2' N 0.96329(14) 0.17204(9) 0.40139(7) 0.0238(2) Uani 1 1 d . . . H2' H 0.956(2) 0.1259(17) 0.3782(11) 0.039(5) Uiso 1 1 d . . . O1' O 0.89783(11) 0.51906(8) 0.31515(5) 0.0242(2) Uani 1 1 d . . . O2' O 0.79197(11) 0.55688(7) 0.43750(5) 0.02010(18) Uani 1 1 d . . . O3' O 1.06266(16) -0.02120(9) 0.35517(7) 0.0407(3) Uani 1 1 d . . . O4' O 1.22602(14) -0.16244(8) 0.42434(7) 0.0352(3) Uani 1 1 d . . . C1' C 0.87309(15) 0.27822(10) 0.37827(7) 0.0204(2) Uani 1 1 d . . . C2' C 0.85363(19) 0.61959(13) 0.26086(9) 0.0334(3) Uani 1 1 d . . . H2'1 H 0.7409 0.6597 0.2659 0.040 Uiso 1 1 calc R . . C3' C 0.8917(3) 0.5818(2) 0.18781(10) 0.0598(6) Uani 1 1 d . . . H3'1 H 1.0015 0.5400 0.1839 0.090 Uiso 1 1 calc R . . H3'2 H 0.8654 0.6464 0.1492 0.090 Uiso 1 1 calc R . . H3'3 H 0.8329 0.5344 0.1828 0.090 Uiso 1 1 calc R . . C4' C 0.9408(3) 0.69130(16) 0.27482(13) 0.0511(5) Uani 1 1 d . . . H4'1 H 0.9193 0.7060 0.3250 0.077 Uiso 1 1 calc R . . H4'2 H 0.9088 0.7614 0.2411 0.077 Uiso 1 1 calc R . . H4'3 H 1.0509 0.6532 0.2674 0.077 Uiso 1 1 calc R . . C5' C 0.70067(15) 0.55019(10) 0.50649(7) 0.0200(2) Uani 1 1 d . . . H5' H 0.6535 0.4916 0.5086 0.024 Uiso 1 1 calc R . . C6' C 0.57568(18) 0.66064(12) 0.50714(8) 0.0289(3) Uani 1 1 d . . . H6'1 H 0.6216 0.7176 0.5075 0.043 Uiso 1 1 calc R . . H6'2 H 0.5089 0.6569 0.5507 0.043 Uiso 1 1 calc R . . H6'3 H 0.5152 0.6792 0.4636 0.043 Uiso 1 1 calc R . . C7' C 0.81073(18) 0.51788(12) 0.56719(8) 0.0281(3) Uani 1 1 d . . . H7'1 H 0.8914 0.4473 0.5617 0.042 Uiso 1 1 calc R . . H7'2 H 0.7554 0.5100 0.6141 0.042 Uiso 1 1 calc R . . H7'3 H 0.8570 0.5752 0.5653 0.042 Uiso 1 1 calc R . . C11' C 1.07666(15) 0.12707(10) 0.45297(7) 0.0203(2) Uani 1 1 d . . . C12' C 1.16575(16) 0.01353(10) 0.45708(8) 0.0229(3) Uani 1 1 d . . . C13' C 1.27745(19) -0.03517(12) 0.50946(9) 0.0324(3) Uani 1 1 d . . . H13' H 1.3367 -0.1115 0.5125 0.039 Uiso 1 1 calc R . . C14' C 1.3029(2) 0.02571(13) 0.55659(10) 0.0373(4) Uani 1 1 d . . . H14' H 1.3790 -0.0082 0.5920 0.045 Uiso 1 1 calc R . . C15' C 1.21606(19) 0.13710(12) 0.55182(9) 0.0310(3) Uani 1 1 d . . . H15' H 1.2339 0.1794 0.5840 0.037 Uiso 1 1 calc R . . C16' C 1.10396(17) 0.18766(11) 0.50096(7) 0.0245(3) Uani 1 1 d . . . H16' H 1.0454 0.2640 0.4988 0.029 Uiso 1 1 calc R . . C17' C 1.14446(17) -0.05536(11) 0.40663(8) 0.0266(3) Uani 1 1 d . . . C18' C 1.2115(2) -0.23427(13) 0.37717(11) 0.0421(4) Uani 1 1 d . . . H18D H 1.1038 -0.2283 0.3766 0.063 Uiso 1 1 calc R . . H18E H 1.2733 -0.3110 0.3952 0.063 Uiso 1 1 calc R . . H18F H 1.2477 -0.2122 0.3277 0.063 Uiso 1 1 calc R . . C1L C 0.5565(3) 0.12296(19) 0.77437(13) 0.0564(6) Uani 1 1 d . . . H1L1 H 0.6682 0.0825 0.7771 0.068 Uiso 1 1 calc R . . H1L2 H 0.5398 0.2027 0.7715 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.46497(16) 0.07854(11) 0.85228(5) 0.1280(4) Uani 1 1 d . . . Cl2 Cl 0.49085(8) 0.10239(6) 0.69569(4) 0.07107(18) 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 Ni1 0.01667(8) 0.01776(7) 0.01838(8) -0.00386(5) -0.00464(6) -0.00206(6) P1 0.02099(16) 0.01859(13) 0.01777(14) -0.00264(11) -0.00336(12) -0.00334(12) S1 0.02075(16) 0.02634(15) 0.02509(16) -0.01054(12) -0.00658(12) 0.00080(12) S2 0.02968(19) 0.02077(13) 0.02397(16) -0.00580(11) -0.01151(13) 0.00268(12) N1 0.0225(6) 0.0201(5) 0.0240(5) -0.0009(4) -0.0071(4) -0.0033(4) N2 0.0273(6) 0.0183(5) 0.0255(6) -0.0030(4) -0.0110(5) -0.0004(4) O1 0.0300(5) 0.0221(4) 0.0233(5) -0.0027(4) 0.0036(4) -0.0043(4) O2 0.0262(5) 0.0254(4) 0.0200(4) -0.0057(3) -0.0015(4) -0.0099(4) O3 0.0363(7) 0.0288(5) 0.0470(7) -0.0123(5) -0.0199(5) -0.0007(5) O4 0.0392(7) 0.0340(6) 0.0502(7) -0.0197(5) -0.0187(6) 0.0091(5) C1 0.0190(6) 0.0208(5) 0.0191(6) -0.0007(4) -0.0034(5) -0.0023(4) C2 0.0344(8) 0.0234(6) 0.0222(6) -0.0010(5) 0.0005(6) -0.0082(5) C3 0.0677(14) 0.0541(10) 0.0226(7) 0.0010(7) -0.0072(8) -0.0327(10) C4 0.0611(13) 0.0467(10) 0.0406(10) -0.0039(8) -0.0070(9) -0.0308(9) C5 0.0282(7) 0.0306(6) 0.0201(6) -0.0060(5) -0.0001(5) -0.0114(5) C6 0.0477(11) 0.0360(8) 0.0380(9) -0.0128(7) 0.0053(8) -0.0023(7) C7 0.0466(11) 0.0532(10) 0.0242(8) 0.0002(7) -0.0094(7) -0.0130(8) C11 0.0222(6) 0.0202(5) 0.0212(6) 0.0007(4) -0.0059(5) -0.0043(5) C12 0.0230(7) 0.0198(5) 0.0255(6) -0.0003(5) -0.0071(5) -0.0039(5) C13 0.0294(8) 0.0261(6) 0.0343(8) -0.0019(6) -0.0141(6) 0.0001(6) C14 0.0380(9) 0.0346(7) 0.0340(8) -0.0027(6) -0.0203(7) -0.0016(7) C15 0.0424(10) 0.0345(7) 0.0292(8) -0.0071(6) -0.0159(7) -0.0041(7) C16 0.0330(8) 0.0249(6) 0.0258(7) -0.0047(5) -0.0086(6) -0.0016(5) C17 0.0314(8) 0.0181(5) 0.0314(7) -0.0017(5) -0.0104(6) -0.0034(5) C18 0.0571(13) 0.0410(9) 0.0604(13) -0.0298(9) -0.0226(10) 0.0109(9) P1' 0.01616(15) 0.01718(13) 0.01773(14) -0.00233(10) -0.00299(11) -0.00360(11) S1' 0.01623(15) 0.02330(13) 0.02271(15) -0.00783(11) -0.00403(11) -0.00235(11) S2' 0.0335(2) 0.02064(14) 0.03245(18) -0.00890(13) -0.01857(15) 0.00336(13) N1' 0.0220(6) 0.0180(4) 0.0226(5) -0.0013(4) -0.0070(4) -0.0038(4) N2' 0.0278(6) 0.0168(4) 0.0247(6) -0.0028(4) -0.0104(5) -0.0026(4) O1' 0.0200(5) 0.0259(4) 0.0216(4) 0.0007(3) 0.0002(4) -0.0040(4) O2' 0.0205(5) 0.0207(4) 0.0205(4) -0.0041(3) -0.0019(3) -0.0080(3) O3' 0.0572(8) 0.0230(5) 0.0385(6) -0.0068(4) -0.0216(6) -0.0031(5) O4' 0.0318(6) 0.0202(4) 0.0496(7) -0.0080(4) -0.0077(5) -0.0007(4) C1' 0.0197(6) 0.0187(5) 0.0206(6) -0.0017(4) -0.0040(5) -0.0036(4) C2' 0.0258(8) 0.0353(7) 0.0314(8) 0.0116(6) -0.0027(6) -0.0088(6) C3' 0.0669(15) 0.1031(19) 0.0230(8) 0.0046(10) -0.0066(9) -0.0519(14) C4' 0.0604(14) 0.0385(9) 0.0588(13) -0.0033(8) 0.0088(10) -0.0272(9) C5' 0.0205(6) 0.0213(5) 0.0191(6) -0.0033(4) -0.0015(5) -0.0080(5) C6' 0.0256(7) 0.0269(6) 0.0299(7) -0.0074(5) -0.0018(6) -0.0019(5) C7' 0.0297(8) 0.0316(7) 0.0229(6) -0.0023(5) -0.0073(6) -0.0097(6) C11' 0.0202(6) 0.0185(5) 0.0196(6) 0.0005(4) -0.0035(5) -0.0043(4) C12' 0.0213(6) 0.0201(5) 0.0245(6) -0.0014(4) -0.0034(5) -0.0037(5) C13' 0.0274(8) 0.0246(6) 0.0384(8) -0.0021(6) -0.0114(6) 0.0010(5) C14' 0.0323(9) 0.0342(7) 0.0401(9) -0.0026(6) -0.0197(7) -0.0015(6) C15' 0.0319(8) 0.0309(7) 0.0304(7) -0.0049(6) -0.0109(6) -0.0080(6) C16' 0.0275(7) 0.0218(5) 0.0226(6) -0.0022(5) -0.0056(5) -0.0058(5) C17' 0.0264(7) 0.0203(5) 0.0302(7) -0.0049(5) -0.0017(6) -0.0036(5) C18' 0.0394(10) 0.0266(7) 0.0603(12) -0.0183(7) -0.0004(8) -0.0057(6) C1L 0.0619(14) 0.0558(12) 0.0613(14) -0.0076(10) -0.0185(11) -0.0287(11) Cl1 0.1815(12) 0.1750(11) 0.0645(5) -0.0110(6) 0.0153(6) -0.1158(10) Cl2 0.0634(4) 0.0867(4) 0.0671(4) -0.0236(3) -0.0221(3) -0.0194(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 Ni1 S2' 2.1956(4) . ? Ni1 S2 2.1981(4) . ? Ni1 S1' 2.2035(4) . ? Ni1 S1 2.2194(4) . ? P1 O1 1.5603(11) . ? P1 O2 1.5632(10) . ? P1 N1 1.6094(11) . ? P1 S1 1.9934(5) . ? S2 C1 1.7493(14) . ? N1 C1 1.3026(17) . ? N2 C1 1.3628(16) . ? N2 C11 1.3997(17) . ? N2 H2 0.81(2) . ? O1 C2 1.4711(16) . ? O2 C5 1.4696(17) . ? O3 C17 1.2145(18) . ? O4 C17 1.3207(18) . ? O4 C18 1.455(2) . ? C2 C4 1.501(2) . ? C2 C3 1.501(2) . ? C2 H2A 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.503(2) . ? C5 C7 1.506(2) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C11 C16 1.393(2) . ? C11 C12 1.4124(18) . ? C12 C13 1.3976(19) . ? C12 C17 1.482(2) . ? C13 C14 1.373(2) . ? C13 H13 0.9500 . ? C14 C15 1.392(2) . ? C14 H14 0.9500 . ? C15 C16 1.384(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? P1' O1' 1.5570(10) . ? P1' O2' 1.5664(10) . ? P1' N1' 1.6083(11) . ? P1' S1' 1.9949(5) . ? S2' C1' 1.7504(13) . ? N1' C1' 1.3072(16) . ? N2' C1' 1.3619(16) . ? N2' C11' 1.3968(17) . ? N2' H2' 0.83(2) . ? O1' C2' 1.4634(17) . ? O2' C5' 1.4801(16) . ? O3' C17' 1.2067(18) . ? O4' C17' 1.3347(16) . ? O4' C18' 1.447(2) . ? C2' C4' 1.505(3) . ? C2' C3' 1.506(3) . ? C2' H2'1 1.0000 . ? C3' H3'1 0.9800 . ? C3' H3'2 0.9800 . ? C3' H3'3 0.9800 . ? C4' H4'1 0.9800 . ? C4' H4'2 0.9800 . ? C4' H4'3 0.9800 . ? C5' C6' 1.5061(18) . ? C5' C7' 1.5066(19) . ? C5' H5' 1.0000 . ? C6' H6'1 0.9800 . ? C6' H6'2 0.9800 . ? C6' H6'3 0.9800 . ? C7' H7'1 0.9800 . ? C7' H7'2 0.9800 . ? C7' H7'3 0.9800 . ? C11' C16' 1.3940(19) . ? C11' C12' 1.4163(17) . ? C12' C13' 1.399(2) . ? C12' C17' 1.487(2) . ? C13' C14' 1.377(2) . ? C13' H13' 0.9500 . ? C14' C15' 1.387(2) . ? C14' H14' 0.9500 . ? C15' C16' 1.384(2) . ? C15' H15' 0.9500 . ? C16' H16' 0.9500 . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? C1L Cl1 1.726(3) . ? C1L Cl2 1.746(2) . ? C1L H1L1 0.9900 . ? C1L H1L2 0.9900 . ? 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 S2' Ni1 S2 177.343(19) . . ? S2' Ni1 S1' 98.459(14) . . ? S2 Ni1 S1' 80.603(13) . . ? S2' Ni1 S1 82.487(14) . . ? S2 Ni1 S1 98.550(14) . . ? S1' Ni1 S1 177.569(16) . . ? O1 P1 O2 102.85(6) . . ? O1 P1 N1 106.44(6) . . ? O2 P1 N1 107.86(6) . . ? O1 P1 S1 114.29(4) . . ? O2 P1 S1 109.05(4) . . ? N1 P1 S1 115.46(5) . . ? P1 S1 Ni1 101.291(18) . . ? C1 S2 Ni1 118.47(4) . . ? C1 N1 P1 122.62(10) . . ? C1 N2 C11 130.86(12) . . ? C1 N2 H2 114.8(14) . . ? C11 N2 H2 113.7(14) . . ? C2 O1 P1 122.22(9) . . ? C5 O2 P1 123.91(9) . . ? C17 O4 C18 116.08(13) . . ? N1 C1 N2 120.69(12) . . ? N1 C1 S2 129.68(10) . . ? N2 C1 S2 109.60(10) . . ? O1 C2 C4 107.46(13) . . ? O1 C2 C3 106.85(12) . . ? C4 C2 C3 113.25(15) . . ? O1 C2 H2A 109.7 . . ? C4 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 C6 106.38(12) . . ? O2 C5 C7 107.08(13) . . ? C6 C5 C7 113.62(14) . . ? O2 C5 H5 109.9 . . ? C6 C5 H5 109.9 . . ? C7 C5 H5 109.9 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C16 C11 N2 122.89(12) . . ? C16 C11 C12 119.49(12) . . ? N2 C11 C12 117.62(12) . . ? C13 C12 C11 118.97(13) . . ? C13 C12 C17 119.64(12) . . ? C11 C12 C17 121.38(12) . . ? C14 C13 C12 121.22(14) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.48(14) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.77(15) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 120.07(13) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? O3 C17 O4 122.56(14) . . ? O3 C17 C12 124.77(13) . . ? O4 C17 C12 112.67(13) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1' P1' O2' 104.34(5) . . ? O1' P1' N1' 105.68(6) . . ? O2' P1' N1' 107.73(5) . . ? O1' P1' S1' 114.32(4) . . ? O2' P1' S1' 107.20(4) . . ? N1' P1' S1' 116.73(5) . . ? P1' S1' Ni1 103.343(17) . . ? C1' S2' Ni1 119.48(4) . . ? C1' N1' P1' 122.80(9) . . ? C1' N2' C11' 131.83(12) . . ? C1' N2' H2' 114.8(14) . . ? C11' N2' H2' 113.1(14) . . ? C2' O1' P1' 125.18(9) . . ? C5' O2' P1' 120.76(8) . . ? C17' O4' C18' 115.58(13) . . ? N1' C1' N2' 120.54(12) . . ? N1' C1' S2' 130.03(10) . . ? N2' C1' S2' 109.40(9) . . ? O1' C2' C4' 107.57(14) . . ? O1' C2' C3' 106.07(15) . . ? C4' C2' C3' 113.78(16) . . ? O1' C2' H2'1 109.8 . . ? C4' C2' H2'1 109.8 . . ? C3' C2' H2'1 109.8 . . ? C2' C3' H3'1 109.5 . . ? C2' C3' H3'2 109.5 . . ? H3'1 C3' H3'2 109.5 . . ? C2' C3' H3'3 109.5 . . ? H3'1 C3' H3'3 109.5 . . ? H3'2 C3' H3'3 109.5 . . ? C2' C4' H4'1 109.5 . . ? C2' C4' H4'2 109.5 . . ? H4'1 C4' H4'2 109.5 . . ? C2' C4' H4'3 109.5 . . ? H4'1 C4' H4'3 109.5 . . ? H4'2 C4' H4'3 109.5 . . ? O2' C5' C6' 107.74(10) . . ? O2' C5' C7' 106.74(11) . . ? C6' C5' C7' 114.21(12) . . ? O2' C5' H5' 109.3 . . ? C6' C5' H5' 109.3 . . ? C7' C5' H5' 109.3 . . ? C5' C6' H6'1 109.5 . . ? C5' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C5' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C5' C7' H7'1 109.5 . . ? C5' C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? C5' C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? C16' C11' N2' 123.34(11) . . ? C16' C11' C12' 118.89(12) . . ? N2' C11' C12' 117.76(12) . . ? C13' C12' C11' 119.38(13) . . ? C13' C12' C17' 118.99(12) . . ? C11' C12' C17' 121.63(12) . . ? C14' C13' C12' 121.05(13) . . ? C14' C13' H13' 119.5 . . ? C12' C13' H13' 119.5 . . ? C13' C14' C15' 119.24(14) . . ? C13' C14' H14' 120.4 . . ? C15' C14' H14' 120.4 . . ? C16' C15' C14' 121.18(14) . . ? C16' C15' H15' 119.4 . . ? C14' C15' H15' 119.4 . . ? C15' C16' C11' 120.25(12) . . ? C15' C16' H16' 119.9 . . ? C11' C16' H16' 119.9 . . ? O3' C17' O4' 122.05(13) . . ? O3' C17' C12' 125.32(12) . . ? O4' C17' C12' 112.63(12) . . ? O4' C18' H18D 109.5 . . ? O4' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? O4' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Cl1 C1L Cl2 112.30(13) . . ? Cl1 C1L H1L1 109.1 . . ? Cl2 C1L H1L1 109.1 . . ? Cl1 C1L H1L2 109.1 . . ? Cl2 C1L H1L2 109.1 . . ? H1L1 C1L H1L2 107.9 . . ? 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 O1 P1 S1 Ni1 -56.16(5) . . . . ? O2 P1 S1 Ni1 -170.62(4) . . . . ? N1 P1 S1 Ni1 67.80(5) . . . . ? S2' Ni1 S1 P1 136.00(2) . . . . ? S2 Ni1 S1 P1 -41.53(2) . . . . ? S1' Ni1 S2 C1 -171.04(6) . . . . ? S1 Ni1 S2 C1 11.27(6) . . . . ? O1 P1 N1 C1 79.49(13) . . . . ? O2 P1 N1 C1 -170.71(12) . . . . ? S1 P1 N1 C1 -48.49(13) . . . . ? O2 P1 O1 C2 58.90(12) . . . . ? N1 P1 O1 C2 172.18(11) . . . . ? S1 P1 O1 C2 -59.16(11) . . . . ? O1 P1 O2 C5 -172.78(10) . . . . ? N1 P1 O2 C5 74.99(11) . . . . ? S1 P1 O2 C5 -51.09(10) . . . . ? P1 N1 C1 N2 -177.68(11) . . . . ? P1 N1 C1 S2 0.5(2) . . . . ? C11 N2 C1 N1 9.4(2) . . . . ? C11 N2 C1 S2 -169.04(13) . . . . ? Ni1 S2 C1 N1 16.35(16) . . . . ? Ni1 S2 C1 N2 -165.34(8) . . . . ? P1 O1 C2 C4 -110.73(14) . . . . ? P1 O1 C2 C3 127.42(13) . . . . ? P1 O2 C5 C6 123.16(13) . . . . ? P1 O2 C5 C7 -115.03(13) . . . . ? C1 N2 C11 C16 -25.8(2) . . . . ? C1 N2 C11 C12 155.03(15) . . . . ? C16 C11 C12 C13 -0.2(2) . . . . ? N2 C11 C12 C13 179.02(14) . . . . ? C16 C11 C12 C17 -179.66(14) . . . . ? N2 C11 C12 C17 -0.5(2) . . . . ? C11 C12 C13 C14 -0.4(3) . . . . ? C17 C12 C13 C14 179.13(16) . . . . ? C12 C13 C14 C15 0.7(3) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C14 C15 C16 C11 -0.1(3) . . . . ? N2 C11 C16 C15 -178.77(16) . . . . ? C12 C11 C16 C15 0.4(2) . . . . ? C18 O4 C17 O3 -2.1(3) . . . . ? C18 O4 C17 C12 176.93(16) . . . . ? C13 C12 C17 O3 -159.57(17) . . . . ? C11 C12 C17 O3 19.9(2) . . . . ? C13 C12 C17 O4 21.4(2) . . . . ? C11 C12 C17 O4 -159.08(15) . . . . ? O1' P1' S1' Ni1 60.21(5) . . . . ? O2' P1' S1' Ni1 175.32(4) . . . . ? N1' P1' S1' Ni1 -63.83(5) . . . . ? S2' Ni1 S1' P1' 39.93(2) . . . . ? S2 Ni1 S1' P1' -142.59(2) . . . . ? S1' Ni1 S2' C1' -13.82(6) . . . . ? S1 Ni1 S2' C1' 163.92(6) . . . . ? O1' P1' N1' C1' -81.04(13) . . . . ? O2' P1' N1' C1' 167.88(11) . . . . ? S1' P1' N1' C1' 47.30(13) . . . . ? O2' P1' O1' C2' -80.10(12) . . . . ? N1' P1' O1' C2' 166.44(12) . . . . ? S1' P1' O1' C2' 36.68(13) . . . . ? O1' P1' O2' C5' 179.30(9) . . . . ? N1' P1' O2' C5' -68.70(10) . . . . ? S1' P1' O2' C5' 57.69(9) . . . . ? P1' N1' C1' N2' 171.77(11) . . . . ? P1' N1' C1' S2' -6.1(2) . . . . ? C11' N2' C1' N1' -4.8(2) . . . . ? C11' N2' C1' S2' 173.50(13) . . . . ? Ni1 S2' C1' N1' -8.74(16) . . . . ? Ni1 S2' C1' N2' 173.16(8) . . . . ? P1' O1' C2' C4' 111.80(14) . . . . ? P1' O1' C2' C3' -126.09(14) . . . . ? P1' O2' C5' C6' -112.90(11) . . . . ? P1' O2' C5' C7' 124.03(10) . . . . ? C1' N2' C11' C16' 10.1(2) . . . . ? C1' N2' C11' C12' -171.06(14) . . . . ? C16' C11' C12' C13' 0.6(2) . . . . ? N2' C11' C12' C13' -178.21(14) . . . . ? C16' C11' C12' C17' -178.87(13) . . . . ? N2' C11' C12' C17' 2.3(2) . . . . ? C11' C12' C13' C14' -0.5(2) . . . . ? C17' C12' C13' C14' 179.01(16) . . . . ? C12' C13' C14' C15' 0.0(3) . . . . ? C13' C14' C15' C16' 0.5(3) . . . . ? C14' C15' C16' C11' -0.3(3) . . . . ? N2' C11' C16' C15' 178.56(14) . . . . ? C12' C11' C16' C15' -0.2(2) . . . . ? C18' O4' C17' O3' 0.9(2) . . . . ? C18' O4' C17' C12' -179.60(14) . . . . ? C13' C12' C17' O3' -172.77(17) . . . . ? C11' C12' C17' O3' 6.7(2) . . . . ? C13' C12' C17' O4' 7.7(2) . . . . ? C11' C12' C17' O4' -172.75(13) . . . . ? 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 N2 H2 O3 0.81(2) 1.98(2) 2.6558(16) 141.7(19) . N2' H2' O3' 0.83(2) 1.94(2) 2.6435(15) 143(2) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.955 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.063