# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Maria Carla Aragoni' _publ_contact_author_email ARAGONI@UNICA.IT _publ_section_title ; Investigation on the reactivity of coordinatively unsaturated phosphonodithioato/dithiophosphato NiII complexes towards 2,4,6-tris-2-pyridyl-1,3,5-triazine: developments and new perspectives. ; loop_ _publ_author_name 'Maria Carla Aragoni' 'Massimiliano Arca' 'Miriam Crespo' 'F A Devillanova' 'Mike Hursthouse' ; S.L.Huth ; 'Francesco Isaia' 'Vito Lippolis' 'Gaetano Verani' # Attachment '_4.tptz_03mma002.cif' data_03mma002 _database_code_depnum_ccdc_archive 'CCDC 278292' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 N6 Ni O4 P2 S4' _chemical_formula_weight 893.65 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 '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 12.0483(15) _cell_length_b 25.569(3) _cell_length_c 26.479(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8157.1(15) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5941 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut block' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7823 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; The crystals were found to be of poor quality and particularly weakly diffracting with no observed diffraction above 22 degrees in theta, hence the low values of theta_max and data completeness. As a further consequence the merging of the data yielded a high Rint and the data to parameter ratio is lower than 10. However, despite these bad statistics the connectivity of the compound could be establish unambigiously. Searches for better crystals were not successful. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39380 _diffrn_reflns_av_R_equivalents 0.1640 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 21.81 _reflns_number_total 4411 _reflns_number_gt 2772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hoof, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0413P)^2^+46.1118P] 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 4411 _refine_ls_number_parameters 496 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1527 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.079 _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 C1 C 0.3839(8) 0.0874(3) 0.5657(3) 0.028(2) Uani 1 1 d . . . C2 C 0.4581(8) 0.1006(3) 0.5283(4) 0.034(3) Uani 1 1 d . . . H2 H 0.5128 0.1264 0.5353 0.041 Uiso 1 1 calc R . . C3 C 0.4561(8) 0.0778(4) 0.4810(3) 0.035(3) Uani 1 1 d . . . H3 H 0.5080 0.0878 0.4558 0.042 Uiso 1 1 calc R . . C4 C 0.3769(10) 0.0400(4) 0.4714(3) 0.039(3) Uani 1 1 d . . . C5 C 0.3019(9) 0.0255(4) 0.5074(4) 0.046(3) Uani 1 1 d . . . H5 H 0.2477 -0.0005 0.5002 0.055 Uiso 1 1 calc R . . C6 C 0.3058(9) 0.0489(4) 0.5542(4) 0.053(3) Uani 1 1 d . . . H6 H 0.2539 0.0386 0.5793 0.063 Uiso 1 1 calc R . . C7 C 0.4440(9) 0.0282(4) 0.3862(3) 0.048(3) Uani 1 1 d . . . H7A H 0.4266 0.0084 0.3555 0.072 Uiso 1 1 calc R . . H7B H 0.5189 0.0191 0.3977 0.072 Uiso 1 1 calc R . . H7C H 0.4404 0.0657 0.3790 0.072 Uiso 1 1 calc R . . C8 C 0.4144(10) 0.0703(4) 0.7164(3) 0.043(3) Uani 1 1 d . . . H8 H 0.3640 0.0993 0.7272 0.052 Uiso 1 1 calc R . . C9 C 0.5289(9) 0.0795(4) 0.7372(4) 0.046(3) Uani 1 1 d . . . H9A H 0.5546 0.1144 0.7271 0.069 Uiso 1 1 calc R . . H9B H 0.5798 0.0530 0.7239 0.069 Uiso 1 1 calc R . . H9C H 0.5269 0.0772 0.7741 0.069 Uiso 1 1 calc R . . C10 C 0.3637(9) 0.0184(4) 0.7304(4) 0.052(3) Uani 1 1 d . . . H10A H 0.2888 0.0160 0.7162 0.077 Uiso 1 1 calc R . . H10B H 0.3598 0.0155 0.7673 0.077 Uiso 1 1 calc R . . H10C H 0.4096 -0.0100 0.7169 0.077 Uiso 1 1 calc R . . C11 C 0.3637(9) 0.3695(3) 0.5374(3) 0.027(2) Uani 1 1 d . . . C12 C 0.2716(9) 0.3869(3) 0.5121(4) 0.034(3) Uani 1 1 d . . . H12 H 0.2078 0.3959 0.5313 0.040 Uiso 1 1 calc R . . C13 C 0.2667(9) 0.3919(4) 0.4599(4) 0.037(3) Uani 1 1 d . . . H13 H 0.2014 0.4043 0.4437 0.045 Uiso 1 1 calc R . . C14 C 0.3585(9) 0.3784(3) 0.4326(3) 0.028(3) Uani 1 1 d . . . C15 C 0.4527(9) 0.3600(3) 0.4560(4) 0.036(3) Uani 1 1 d . . . H15 H 0.5160 0.3504 0.4367 0.043 Uiso 1 1 calc R . . C16 C 0.4537(9) 0.3556(3) 0.5082(4) 0.037(3) Uani 1 1 d . . . H16 H 0.5184 0.3425 0.5244 0.044 Uiso 1 1 calc R . . C17 C 0.2726(9) 0.4049(4) 0.3550(3) 0.049(3) Uani 1 1 d . . . H17A H 0.2874 0.4067 0.3186 0.074 Uiso 1 1 calc R . . H17B H 0.2576 0.4401 0.3679 0.074 Uiso 1 1 calc R . . H17C H 0.2079 0.3825 0.3610 0.074 Uiso 1 1 calc R . . C18 C 0.4560(9) 0.4686(3) 0.5972(4) 0.044(3) Uani 1 1 d . . . H18 H 0.3873 0.4711 0.5762 0.052 Uiso 1 1 calc R . . C19 C 0.5560(10) 0.4813(4) 0.5649(4) 0.063(4) Uani 1 1 d . . . H19A H 0.5570 0.4582 0.5354 0.095 Uiso 1 1 calc R . . H19B H 0.6238 0.4760 0.5847 0.095 Uiso 1 1 calc R . . H19C H 0.5519 0.5178 0.5538 0.095 Uiso 1 1 calc R . . C20 C 0.4437(9) 0.5028(4) 0.6430(4) 0.059(3) Uani 1 1 d U . . H20A H 0.3760 0.4932 0.6612 0.089 Uiso 1 1 calc R . . H20B H 0.4392 0.5395 0.6325 0.089 Uiso 1 1 calc R . . H20C H 0.5081 0.4980 0.6651 0.089 Uiso 1 1 calc R . . C21 C 0.1131(9) 0.2804(3) 0.6113(3) 0.026(2) Uani 1 1 d U . . C22 C -0.0109(9) 0.3168(3) 0.6634(4) 0.029(3) Uani 1 1 d U . . C23 C 0.1423(8) 0.2781(3) 0.6963(3) 0.021(2) Uani 1 1 d U . . C24 C 0.2160(9) 0.2568(3) 0.7366(3) 0.024(2) Uani 1 1 d U . . C25 C 0.1836(8) 0.2570(3) 0.7866(3) 0.027(2) Uani 1 1 d U . . H25 H 0.1161 0.2730 0.7968 0.032 Uiso 1 1 calc R . . C26 C 0.2526(9) 0.2331(3) 0.8214(4) 0.032(3) Uani 1 1 d . . . H26 H 0.2320 0.2311 0.8560 0.039 Uiso 1 1 calc R . . C27 C 0.3525(9) 0.2123(3) 0.8048(3) 0.031(3) Uani 1 1 d . . . H27 H 0.4024 0.1966 0.8281 0.037 Uiso 1 1 calc R . . C28 C 0.3786(9) 0.2146(3) 0.7541(4) 0.033(3) Uani 1 1 d . . . H28 H 0.4477 0.2007 0.7432 0.039 Uiso 1 1 calc R . . C29 C 0.1604(8) 0.2635(3) 0.5616(3) 0.026(2) Uani 1 1 d . . . C30 C 0.1047(8) 0.2710(3) 0.5164(3) 0.030(2) Uani 1 1 d . . . H30 H 0.0350 0.2884 0.5154 0.036 Uiso 1 1 calc R . . C31 C 0.1547(9) 0.2521(4) 0.4723(3) 0.032(3) Uani 1 1 d . . . H31 H 0.1194 0.2570 0.4405 0.039 Uiso 1 1 calc R . . C32 C 0.2530(9) 0.2271(3) 0.4750(4) 0.034(3) Uani 1 1 d . . . H32 H 0.2870 0.2132 0.4455 0.041 Uiso 1 1 calc R . . C33 C 0.3034(8) 0.2219(3) 0.5219(3) 0.030(3) Uani 1 1 d . . . H33 H 0.3737 0.2052 0.5231 0.036 Uiso 1 1 calc R . . C34 C -0.1136(8) 0.3450(3) 0.6728(4) 0.026(2) Uani 1 1 d . . . C35 C -0.1390(8) 0.3658(3) 0.7201(3) 0.030(3) Uani 1 1 d . . . H35 H -0.0881 0.3628 0.7473 0.036 Uiso 1 1 calc R . . C36 C -0.2405(10) 0.3912(4) 0.7266(4) 0.041(3) Uani 1 1 d . . . H36 H -0.2603 0.4056 0.7584 0.049 Uiso 1 1 calc R . . C37 C -0.3107(9) 0.3948(3) 0.6863(4) 0.038(3) Uani 1 1 d . . . H37 H -0.3800 0.4122 0.6895 0.046 Uiso 1 1 calc R . . C38 C -0.2795(9) 0.3729(3) 0.6410(4) 0.038(3) Uani 1 1 d . . . H38 H -0.3298 0.3755 0.6135 0.045 Uiso 1 1 calc R . . N1 N 0.1785(6) 0.2665(2) 0.6497(3) 0.0223(18) Uani 1 1 d . . . N2 N 0.0176(7) 0.3041(3) 0.6153(2) 0.0232(19) Uani 1 1 d . . . N3 N 0.0489(7) 0.3040(3) 0.7053(3) 0.028(2) Uani 1 1 d . . . N4 N 0.3108(7) 0.2356(3) 0.7196(3) 0.0248(19) Uani 1 1 d . . . N5 N -0.1835(7) 0.3481(3) 0.6329(3) 0.032(2) Uani 1 1 d . . . N6 N 0.2606(7) 0.2388(3) 0.5649(2) 0.0247(19) Uani 1 1 d . . . S1 S 0.4861(2) 0.17845(8) 0.62970(9) 0.0307(7) Uani 1 1 d . . . S2 S 0.2294(2) 0.14170(9) 0.64542(9) 0.0357(7) Uani 1 1 d . . . S3 S 0.4443(2) 0.30725(8) 0.63314(9) 0.0312(6) Uani 1 1 d . . . S4 S 0.2290(2) 0.39570(9) 0.63333(10) 0.0392(7) Uani 1 1 d . . . P1 P 0.3805(2) 0.11775(9) 0.62667(9) 0.0310(7) Uani 1 1 d . . . P2 P 0.3698(2) 0.37209(9) 0.60571(9) 0.0301(7) Uani 1 1 d . . . O1 O 0.4220(5) 0.0692(2) 0.6604(2) 0.0375(18) Uani 1 1 d . . . O2 O 0.3648(6) 0.0153(2) 0.4251(2) 0.0444(19) Uani 1 1 d . . . O3 O 0.4692(5) 0.4141(2) 0.6155(2) 0.0317(17) Uani 1 1 d . . . O4 O 0.3685(6) 0.3832(2) 0.3806(2) 0.0406(18) Uani 1 1 d . . . Ni1 Ni 0.32259(10) 0.23138(4) 0.63897(4) 0.0260(4) 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 C1 0.025(7) 0.033(6) 0.027(6) 0.001(4) 0.000(5) -0.006(5) C2 0.023(8) 0.038(6) 0.042(7) -0.006(5) -0.001(6) -0.001(5) C3 0.022(8) 0.047(7) 0.035(6) -0.002(5) 0.013(5) 0.005(5) C4 0.061(9) 0.034(6) 0.023(6) -0.002(5) 0.001(6) -0.001(6) C5 0.039(9) 0.064(7) 0.035(7) -0.004(6) 0.013(6) -0.022(6) C6 0.060(10) 0.066(8) 0.032(7) -0.004(5) 0.025(6) -0.029(7) C7 0.063(9) 0.047(7) 0.034(6) -0.008(5) 0.007(6) 0.011(6) C8 0.067(10) 0.033(6) 0.029(6) 0.004(5) -0.006(6) 0.005(6) C9 0.036(9) 0.055(7) 0.048(7) 0.001(5) -0.020(6) -0.010(6) C10 0.060(9) 0.059(7) 0.036(6) 0.006(5) 0.003(6) -0.017(6) C11 0.030(8) 0.021(5) 0.029(6) -0.002(4) -0.009(6) 0.000(5) C12 0.025(8) 0.045(6) 0.030(7) 0.005(5) 0.007(6) -0.002(5) C13 0.024(8) 0.049(7) 0.039(7) 0.000(5) 0.003(6) 0.002(5) C14 0.028(9) 0.029(6) 0.027(7) -0.002(4) -0.002(6) -0.005(5) C15 0.020(8) 0.048(7) 0.040(7) -0.008(5) 0.003(6) 0.007(5) C16 0.023(8) 0.045(6) 0.043(7) -0.002(5) -0.005(6) 0.012(5) C17 0.069(10) 0.054(7) 0.026(6) 0.005(5) -0.007(6) 0.001(6) C18 0.051(9) 0.027(6) 0.053(7) -0.007(5) -0.019(6) -0.002(5) C19 0.092(11) 0.044(7) 0.054(8) 0.007(5) -0.001(8) -0.018(7) C20 0.060(7) 0.054(6) 0.063(6) -0.006(5) -0.014(6) 0.009(5) C21 0.034(7) 0.027(5) 0.019(5) 0.003(4) -0.007(5) -0.007(5) C22 0.029(7) 0.027(5) 0.032(5) -0.001(4) 0.003(5) -0.002(4) C23 0.007(6) 0.030(5) 0.025(5) 0.003(4) -0.006(5) -0.008(4) C24 0.032(7) 0.022(5) 0.019(5) 0.001(4) -0.006(5) -0.003(4) C25 0.026(6) 0.034(5) 0.021(5) -0.003(4) 0.007(5) -0.002(4) C26 0.026(8) 0.041(6) 0.030(6) 0.000(5) 0.006(6) -0.006(5) C27 0.032(9) 0.035(6) 0.025(6) 0.011(4) 0.006(5) -0.009(5) C28 0.035(8) 0.033(6) 0.031(6) 0.005(5) -0.006(6) -0.004(5) C29 0.020(8) 0.029(6) 0.028(6) -0.006(4) 0.000(5) -0.004(5) C30 0.013(7) 0.055(6) 0.021(6) 0.006(5) -0.006(5) 0.004(5) C31 0.031(9) 0.053(7) 0.013(6) -0.001(4) -0.003(5) -0.007(6) C32 0.028(8) 0.040(6) 0.034(7) -0.007(5) -0.004(6) 0.007(6) C33 0.024(8) 0.041(6) 0.024(6) 0.002(4) -0.010(6) 0.003(5) C34 0.016(7) 0.033(6) 0.029(6) -0.001(4) -0.009(6) -0.003(5) C35 0.021(8) 0.039(6) 0.030(6) 0.000(5) -0.004(5) 0.002(5) C36 0.041(9) 0.041(6) 0.039(7) -0.005(5) -0.008(7) 0.004(6) C37 0.035(8) 0.034(6) 0.046(7) -0.001(5) -0.006(7) 0.002(5) C38 0.040(9) 0.034(6) 0.040(7) -0.001(5) -0.004(6) -0.001(5) N1 0.008(5) 0.027(4) 0.032(5) 0.003(3) 0.007(4) -0.006(4) N2 0.009(6) 0.038(5) 0.023(5) 0.002(3) -0.004(4) 0.003(4) N3 0.016(6) 0.035(5) 0.034(5) -0.001(4) -0.004(4) 0.001(4) N4 0.013(6) 0.031(4) 0.031(5) -0.004(4) 0.002(4) -0.001(4) N5 0.022(6) 0.031(4) 0.042(5) -0.001(4) 0.002(5) 0.004(4) N6 0.021(6) 0.033(5) 0.020(5) -0.006(3) 0.005(4) 0.002(4) S1 0.0248(19) 0.0351(13) 0.0323(14) -0.0020(11) -0.0018(13) 0.0006(11) S2 0.031(2) 0.0360(14) 0.0405(16) -0.0014(12) 0.0023(14) -0.0037(12) S3 0.0254(18) 0.0358(14) 0.0324(14) 0.0040(11) -0.0008(14) -0.0002(11) S4 0.032(2) 0.0488(16) 0.0373(16) -0.0003(13) 0.0002(14) 0.0025(12) P1 0.032(2) 0.0321(14) 0.0285(15) 0.0003(11) -0.0010(14) -0.0009(13) P2 0.024(2) 0.0338(15) 0.0326(15) -0.0010(11) -0.0023(14) 0.0003(13) O1 0.049(6) 0.036(4) 0.027(4) 0.001(3) -0.005(3) 0.010(3) O2 0.042(5) 0.058(5) 0.033(4) -0.006(3) 0.007(4) -0.011(4) O3 0.024(5) 0.030(4) 0.041(4) -0.002(3) -0.013(3) 0.004(3) O4 0.040(5) 0.054(4) 0.027(4) -0.003(3) -0.006(4) -0.003(4) Ni1 0.0216(9) 0.0333(7) 0.0231(7) 0.0006(5) -0.0001(6) 0.0003(6) _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 C1 C2 1.376(12) . ? C1 C6 1.396(12) . ? C1 P1 1.791(9) . ? C2 C3 1.383(12) . ? C2 H2 0.9500 . ? C3 C4 1.381(13) . ? C3 H3 0.9500 . ? C4 C5 1.366(13) . ? C4 O2 1.385(10) . ? C5 C6 1.379(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O2 1.443(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.485(10) . ? C8 C10 1.506(12) . ? C8 C9 1.504(13) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.370(12) . ? C11 C16 1.379(12) . ? C11 P2 1.811(9) . ? C12 C13 1.390(12) . ? C12 H12 0.9500 . ? C13 C14 1.366(13) . ? C13 H13 0.9500 . ? C14 C15 1.376(12) . ? C14 O4 1.386(10) . ? C15 C16 1.388(12) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O4 1.451(11) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O3 1.484(10) . ? C18 C20 1.501(13) . ? C18 C19 1.512(14) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N2 1.306(11) . ? C21 N1 1.334(11) . ? C21 C29 1.498(12) . ? C22 N2 1.359(10) . ? C22 N3 1.361(11) . ? C22 C34 1.456(12) . ? C23 N3 1.328(10) . ? C23 N1 1.343(10) . ? C23 C24 1.491(12) . ? C24 N4 1.341(11) . ? C24 C25 1.382(11) . ? C25 C26 1.382(12) . ? C25 H25 0.9500 . ? C26 C27 1.387(12) . ? C26 H26 0.9500 . ? C27 C28 1.382(12) . ? C27 H27 0.9500 . ? C28 N4 1.338(11) . ? C28 H28 0.9500 . ? C29 N6 1.366(11) . ? C29 C30 1.384(12) . ? C30 C31 1.402(12) . ? C30 H30 0.9500 . ? C31 C32 1.349(12) . ? C31 H31 0.9500 . ? C32 C33 1.388(12) . ? C32 H32 0.9500 . ? C33 N6 1.324(10) . ? C33 H33 0.9500 . ? C34 N5 1.353(11) . ? C34 C35 1.393(12) . ? C35 C36 1.395(13) . ? C35 H35 0.9500 . ? C36 C37 1.365(12) . ? C36 H36 0.9500 . ? C37 C38 1.377(12) . ? C37 H37 0.9500 . ? C38 N5 1.335(11) . ? C38 H38 0.9500 . ? N1 Ni1 1.975(7) . ? N4 Ni1 2.142(7) . ? N6 Ni1 2.106(7) . ? S1 P1 2.009(3) . ? S1 Ni1 2.403(3) . ? S2 P1 1.984(4) . ? S2 Ni1 2.559(3) . ? S3 P2 2.020(3) . ? S3 Ni1 2.436(3) . ? S4 P2 1.943(4) . ? P1 O1 1.610(6) . ? P2 O3 1.630(6) . ? 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 C2 C1 C6 117.0(8) . . ? C2 C1 P1 123.9(7) . . ? C6 C1 P1 119.2(7) . . ? C3 C2 C1 122.6(9) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C2 C3 C4 118.3(9) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 121.3(9) . . ? C5 C4 O2 115.0(9) . . ? C3 C4 O2 123.7(9) . . ? C4 C5 C6 119.1(9) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C1 121.8(9) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C10 104.8(7) . . ? O1 C8 C9 108.2(8) . . ? C10 C8 C9 114.9(8) . . ? O1 C8 H8 109.6 . . ? C10 C8 H8 109.6 . . ? C9 C8 H8 109.6 . . ? 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 C11 C16 116.5(8) . . ? C12 C11 P2 120.7(8) . . ? C16 C11 P2 122.5(8) . . ? C11 C12 C13 123.4(9) . . ? C11 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? C14 C13 C12 118.0(10) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? C13 C14 C15 121.0(9) . . ? C13 C14 O4 125.0(9) . . ? C15 C14 O4 113.9(9) . . ? C14 C15 C16 119.0(9) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C11 C16 C15 122.1(9) . . ? C11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 C20 107.1(8) . . ? O3 C18 C19 107.5(8) . . ? C20 C18 C19 114.2(9) . . ? O3 C18 H18 109.3 . . ? C20 C18 H18 109.3 . . ? C19 C18 H18 109.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 N1 125.6(8) . . ? N2 C21 C29 122.7(9) . . ? N1 C21 C29 111.6(9) . . ? N2 C22 N3 125.0(9) . . ? N2 C22 C34 119.5(9) . . ? N3 C22 C34 115.5(8) . . ? N3 C23 N1 123.4(8) . . ? N3 C23 C24 124.0(9) . . ? N1 C23 C24 112.6(8) . . ? N4 C24 C25 124.3(8) . . ? N4 C24 C23 114.5(8) . . ? C25 C24 C23 121.1(9) . . ? C24 C25 C26 117.9(9) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? C25 C26 C27 118.7(9) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 119.3(9) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? N4 C28 C27 122.8(10) . . ? N4 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? N6 C29 C30 123.4(8) . . ? N6 C29 C21 114.3(8) . . ? C30 C29 C21 122.3(9) . . ? C29 C30 C31 117.6(9) . . ? C29 C30 H30 121.2 . . ? C31 C30 H30 121.2 . . ? C32 C31 C30 119.8(9) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 118.5(9) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? N6 C33 C32 124.7(9) . . ? N6 C33 H33 117.7 . . ? C32 C33 H33 117.7 . . ? N5 C34 C35 122.8(9) . . ? N5 C34 C22 115.2(8) . . ? C35 C34 C22 122.0(9) . . ? C36 C35 C34 118.8(9) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C37 C36 C35 118.5(10) . . ? C37 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? C36 C37 C38 119.0(10) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? N5 C38 C37 124.7(10) . . ? N5 C38 H38 117.6 . . ? C37 C38 H38 117.6 . . ? C21 N1 C23 116.8(8) . . ? C21 N1 Ni1 122.0(6) . . ? C23 N1 Ni1 121.2(6) . . ? C21 N2 C22 114.2(8) . . ? C23 N3 C22 114.9(8) . . ? C24 N4 C28 116.9(8) . . ? C24 N4 Ni1 114.3(6) . . ? C28 N4 Ni1 128.3(7) . . ? C38 N5 C34 116.2(8) . . ? C33 N6 C29 116.0(8) . . ? C33 N6 Ni1 129.4(7) . . ? C29 N6 Ni1 114.6(6) . . ? P1 S1 Ni1 85.39(12) . . ? P1 S2 Ni1 81.79(11) . . ? P2 S3 Ni1 114.14(14) . . ? O1 P1 C1 99.1(4) . . ? O1 P1 S2 112.6(3) . . ? C1 P1 S2 112.3(4) . . ? O1 P1 S1 112.2(3) . . ? C1 P1 S1 110.9(3) . . ? S2 P1 S1 109.45(14) . . ? O3 P2 C11 102.3(4) . . ? O3 P2 S4 112.1(2) . . ? C11 P2 S4 110.6(4) . . ? O3 P2 S3 99.1(2) . . ? C11 P2 S3 110.3(3) . . ? S4 P2 S3 120.48(16) . . ? C8 O1 P1 121.3(5) . . ? C4 O2 C7 117.2(8) . . ? C18 O3 P2 119.2(6) . . ? C14 O4 C17 115.4(8) . . ? N1 Ni1 N6 77.3(3) . . ? N1 Ni1 N4 77.0(3) . . ? N6 Ni1 N4 154.1(3) . . ? N1 Ni1 S1 172.5(2) . . ? N6 Ni1 S1 104.3(2) . . ? N4 Ni1 S1 100.6(2) . . ? N1 Ni1 S3 100.1(2) . . ? N6 Ni1 S3 94.8(2) . . ? N4 Ni1 S3 93.6(2) . . ? S1 Ni1 S3 87.05(9) . . ? N1 Ni1 S2 90.71(19) . . ? N6 Ni1 S2 89.2(2) . . ? N4 Ni1 S2 87.10(19) . . ? S1 Ni1 S2 82.07(9) . . ? S3 Ni1 S2 169.03(10) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 21.81 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.518 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.087 # Attachment '_2.tptz_03mma004.cif' data_03mma004 _database_code_depnum_ccdc_archive 'CCDC 278293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 03mma004/39 ; _chemical_name_common 03mma004/39 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 N6 Ni O4 P2 S4' _chemical_formula_weight 865.60 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3304(3) _cell_length_b 13.1931(3) _cell_length_c 14.5372(2) _cell_angle_alpha 105.4840(10) _cell_angle_beta 101.2430(10) _cell_angle_gamma 98.8710(10) _cell_volume 2004.50(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27523 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour 'deep green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7913 _exptl_absorpt_correction_T_max 0.8802 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40210 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9162 _reflns_number_gt 7171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The ethoxy group O1-C8-C9 is disorder over two positions with a ratio of 65%:35%. The slightly enlarged ellipsoids of this group indicate further disorder, but moddelling of more than 2 positions did not improve the fit significantly. The PLATON module SQUEEZE was used to remove unresolvable disordered solvent from the model and to correct the intensities for this. There remains one spurious peak close to the disordered ethoxy group. Attempts to model this residual electron density as solvent did not improve the model, but led to a worse fit. ; _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^)+(0.0728P)^2^+1.1866P] 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 9162 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1388 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 C1 C 0.8950(3) 0.2704(3) 0.5506(2) 0.0486(7) Uani 1 1 d . A . C2 C 0.9345(3) 0.3793(3) 0.5997(2) 0.0493(7) Uani 1 1 d . . . H2 H 0.9708 0.4244 0.5687 0.059 Uiso 1 1 calc R . . C3 C 0.9212(3) 0.4235(3) 0.6947(2) 0.0501(7) Uani 1 1 d . . . H3 H 0.9480 0.4972 0.7263 0.060 Uiso 1 1 calc R . . C4 C 0.8677(3) 0.3566(3) 0.7420(2) 0.0544(8) Uani 1 1 d . . . C5 C 0.8287(4) 0.2472(4) 0.6934(3) 0.0664(10) Uani 1 1 d . . . H5 H 0.7932 0.2020 0.7247 0.080 Uiso 1 1 calc R . . C6 C 0.8418(4) 0.2039(3) 0.5995(3) 0.0623(9) Uani 1 1 d . . . H6 H 0.8152 0.1301 0.5682 0.075 Uiso 1 1 calc R . . C7 C 0.8839(3) 0.5013(3) 0.8859(3) 0.0642(10) Uani 1 1 d . . . H7A H 0.9721 0.5228 0.9003 0.096 Uiso 1 1 calc R . . H7B H 0.8582 0.5145 0.9464 0.096 Uiso 1 1 calc R . . H7C H 0.8471 0.5420 0.8470 0.096 Uiso 1 1 calc R . . C8 C 1.1140(5) 0.1697(5) 0.4809(5) 0.0555(17) Uani 0.650(11) 1 d P A 1 H8A H 1.1624 0.1963 0.4407 0.067 Uiso 0.650(11) 1 calc PR A 1 H8B H 1.1178 0.2291 0.5384 0.067 Uiso 0.650(11) 1 calc PR A 1 C9 C 1.1614(8) 0.0854(7) 0.5104(7) 0.090(3) Uani 0.650(11) 1 d P A 1 H9A H 1.1089 0.0557 0.5455 0.134 Uiso 0.650(11) 1 calc PR A 1 H9B H 1.2431 0.1143 0.5524 0.134 Uiso 0.650(11) 1 calc PR A 1 H9C H 1.1639 0.0299 0.4531 0.134 Uiso 0.650(11) 1 calc PR A 1 C8' C 1.0998(13) 0.1231(12) 0.4103(11) 0.075(4) Uani 0.350(11) 1 d P A 2 H8'1 H 1.0545 0.0536 0.3647 0.089 Uiso 0.350(11) 1 calc PR A 2 H8'2 H 1.1145 0.1703 0.3708 0.089 Uiso 0.350(11) 1 calc PR A 2 C9' C 1.2077(15) 0.1095(13) 0.4507(18) 0.119(8) Uani 0.350(11) 1 d P A 2 H9'1 H 1.2702 0.1713 0.4583 0.178 Uiso 0.350(11) 1 calc PR A 2 H9'2 H 1.2249 0.0464 0.4092 0.178 Uiso 0.350(11) 1 calc PR A 2 H9'3 H 1.2072 0.1007 0.5140 0.178 Uiso 0.350(11) 1 calc PR A 2 C11 C 0.4453(2) 0.2521(2) 0.02773(19) 0.0345(5) Uani 1 1 d . . . C12 C 0.4533(2) 0.1500(2) -0.0272(2) 0.0366(6) Uani 1 1 d . . . H12 H 0.4445 0.0930 -0.0010 0.044 Uiso 1 1 calc R . . C13 C 0.4741(3) 0.1326(2) -0.1202(2) 0.0386(6) Uani 1 1 d . . . H13 H 0.4773 0.0640 -0.1569 0.046 Uiso 1 1 calc R . . C14 C 0.4903(3) 0.2183(2) -0.15855(19) 0.0384(6) Uani 1 1 d . . . C15 C 0.4867(3) 0.3214(2) -0.1041(2) 0.0384(6) Uani 1 1 d . . . H15 H 0.5002 0.3790 -0.1290 0.046 Uiso 1 1 calc R . . C16 C 0.4624(2) 0.3369(2) -0.01161(19) 0.0375(6) Uani 1 1 d . . . H16 H 0.4576 0.4053 0.0245 0.045 Uiso 1 1 calc R . . C17 C 0.5221(3) 0.2783(3) -0.2945(2) 0.0518(8) Uani 1 1 d . . . H17A H 0.4490 0.3069 -0.2983 0.078 Uiso 1 1 calc R . . H17B H 0.5336 0.2509 -0.3596 0.078 Uiso 1 1 calc R . . H17C H 0.5921 0.3343 -0.2548 0.078 Uiso 1 1 calc R . . C18 C 0.2027(3) 0.2156(3) 0.1919(2) 0.0569(9) Uani 1 1 d . . . H18A H 0.2505 0.1977 0.2460 0.068 Uiso 1 1 calc R . . H18B H 0.1914 0.2884 0.2169 0.068 Uiso 1 1 calc R . . C19 C 0.0840(4) 0.1414(4) 0.1533(3) 0.0843(15) Uani 1 1 d . . . H19A H 0.0346 0.1624 0.1029 0.126 Uiso 1 1 calc R . . H19B H 0.0431 0.1428 0.2054 0.126 Uiso 1 1 calc R . . H19C H 0.0952 0.0699 0.1259 0.126 Uiso 1 1 calc R . . C21 C 0.7322(2) 0.4907(2) 0.30218(19) 0.0356(6) Uani 1 1 d . . . C22 C 0.7897(2) 0.5753(2) 0.1974(2) 0.0368(6) Uani 1 1 d . . . C23 C 0.7645(2) 0.3955(2) 0.15716(19) 0.0342(5) Uani 1 1 d . . . C24 C 0.7679(2) 0.2863(2) 0.09623(19) 0.0334(5) Uani 1 1 d . . . C25 C 0.7842(2) 0.2645(2) 0.0019(2) 0.0384(6) Uani 1 1 d . . . H25 H 0.7962 0.3189 -0.0271 0.046 Uiso 1 1 calc R . . C26 C 0.7822(3) 0.1578(2) -0.0487(2) 0.0414(6) Uani 1 1 d . . . H26 H 0.7924 0.1400 -0.1126 0.050 Uiso 1 1 calc R . . C27 C 0.7652(3) 0.0794(2) -0.0035(2) 0.0407(6) Uani 1 1 d . . . H27 H 0.7627 0.0080 -0.0365 0.049 Uiso 1 1 calc R . . C28 C 0.7518(2) 0.1088(2) 0.0922(2) 0.0375(6) Uani 1 1 d . . . H28 H 0.7419 0.0558 0.1231 0.045 Uiso 1 1 calc R . . C29 C 0.7014(2) 0.4832(2) 0.39442(19) 0.0376(6) Uani 1 1 d . . . C30 C 0.6868(3) 0.5717(2) 0.4652(2) 0.0434(6) Uani 1 1 d . . . H30 H 0.6974 0.6397 0.4569 0.052 Uiso 1 1 calc R . . C31 C 0.6559(3) 0.5551(3) 0.5486(2) 0.0474(7) Uani 1 1 d . . . H31 H 0.6458 0.6124 0.5978 0.057 Uiso 1 1 calc R . . C32 C 0.6404(3) 0.4530(3) 0.5581(2) 0.0454(7) Uani 1 1 d . . . H32 H 0.6194 0.4407 0.6135 0.054 Uiso 1 1 calc R . . C33 C 0.6563(3) 0.3687(2) 0.4840(2) 0.0409(6) Uani 1 1 d . . . H33 H 0.6453 0.2999 0.4906 0.049 Uiso 1 1 calc R . . C34 C 0.8285(2) 0.6779(2) 0.1765(2) 0.0416(6) Uani 1 1 d . . . C35 C 0.8187(3) 0.7740(3) 0.2357(3) 0.0605(9) Uani 1 1 d . . . H35 H 0.7861 0.7766 0.2900 0.073 Uiso 1 1 calc R . . C36 C 0.8579(4) 0.8681(3) 0.2140(3) 0.0698(11) Uani 1 1 d . . . H36 H 0.8535 0.9347 0.2540 0.084 Uiso 1 1 calc R . . C37 C 0.9028(3) 0.8603(3) 0.1329(3) 0.0637(10) Uani 1 1 d . . . H37 H 0.9286 0.9216 0.1157 0.076 Uiso 1 1 calc R . . C38 C 0.9094(3) 0.7609(3) 0.0768(3) 0.0609(9) Uani 1 1 d . . . H38 H 0.9413 0.7569 0.0219 0.073 Uiso 1 1 calc R . . N1 N 0.7364(2) 0.39594(17) 0.24175(16) 0.0344(5) Uani 1 1 d . A . N2 N 0.7582(2) 0.58342(18) 0.28321(17) 0.0376(5) Uani 1 1 d . . . N3 N 0.7921(2) 0.48280(18) 0.13062(16) 0.0359(5) Uani 1 1 d . . . N4 N 0.7526(2) 0.21007(17) 0.14182(16) 0.0344(5) Uani 1 1 d . A . N5 N 0.6870(2) 0.38331(19) 0.40350(16) 0.0374(5) Uani 1 1 d . A . N6 N 0.8729(3) 0.6698(2) 0.0961(2) 0.0504(6) Uani 1 1 d . . . O1 O 0.9820(5) 0.1228(4) 0.4227(4) 0.0464(12) Uani 0.650(11) 1 d P A 1 O1' O 1.0234(14) 0.1618(15) 0.4637(13) 0.091(5) Uani 0.350(11) 1 d P A 2 O2 O 0.8459(2) 0.3894(2) 0.83256(16) 0.0612(6) Uani 1 1 d . . . O3 O 0.26900(18) 0.21016(16) 0.11525(14) 0.0423(5) Uani 1 1 d . . . O4 O 0.5098(2) 0.19331(16) -0.25129(14) 0.0464(5) Uani 1 1 d . . . P1 P 0.90051(8) 0.21078(7) 0.42520(6) 0.0495(2) Uani 1 1 d . . . P2 P 0.41183(6) 0.27325(5) 0.14711(5) 0.03503(16) Uani 1 1 d . . . S1 S 0.73641(8) 0.11683(6) 0.34711(6) 0.04876(19) Uani 1 1 d . A . S2 S 0.95401(7) 0.32237(7) 0.36437(5) 0.04651(19) Uani 1 1 d . A . S3 S 0.50088(7) 0.18448(6) 0.21940(5) 0.03988(17) Uani 1 1 d . A . S4 S 0.43272(7) 0.42665(5) 0.21608(5) 0.03969(17) Uani 1 1 d . . . Ni1 Ni 0.71784(3) 0.26571(3) 0.28390(2) 0.03637(11) 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 C1 0.0419(16) 0.067(2) 0.0411(16) 0.0228(15) 0.0108(12) 0.0115(14) C2 0.0351(15) 0.075(2) 0.0400(16) 0.0244(15) 0.0081(12) 0.0092(14) C3 0.0387(16) 0.072(2) 0.0368(15) 0.0169(15) 0.0066(12) 0.0079(14) C4 0.0432(17) 0.084(3) 0.0361(16) 0.0219(16) 0.0082(13) 0.0101(16) C5 0.071(2) 0.084(3) 0.0463(19) 0.0267(19) 0.0197(17) 0.003(2) C6 0.067(2) 0.074(2) 0.0496(19) 0.0252(18) 0.0195(16) 0.0069(18) C7 0.056(2) 0.093(3) 0.0420(18) 0.0168(18) 0.0138(15) 0.0172(19) C8 0.034(3) 0.065(3) 0.053(4) -0.004(3) 0.010(2) 0.010(2) C9 0.067(5) 0.081(5) 0.099(6) 0.007(4) -0.009(4) 0.028(4) C8' 0.086(10) 0.076(8) 0.075(10) 0.025(8) 0.032(7) 0.036(7) C9' 0.084(11) 0.069(9) 0.18(2) -0.027(10) 0.064(12) 0.015(8) C11 0.0305(13) 0.0359(13) 0.0319(13) 0.0044(10) 0.0086(10) 0.0016(10) C12 0.0356(14) 0.0322(13) 0.0384(14) 0.0066(11) 0.0107(11) 0.0018(10) C13 0.0391(14) 0.0325(13) 0.0388(14) 0.0019(11) 0.0123(11) 0.0047(11) C14 0.0389(14) 0.0414(14) 0.0319(13) 0.0058(11) 0.0117(11) 0.0057(11) C15 0.0429(15) 0.0384(14) 0.0349(14) 0.0108(11) 0.0125(11) 0.0089(11) C16 0.0388(14) 0.0355(13) 0.0346(13) 0.0041(11) 0.0109(11) 0.0068(11) C17 0.068(2) 0.0563(19) 0.0365(15) 0.0154(14) 0.0228(14) 0.0148(16) C18 0.0445(17) 0.072(2) 0.0488(18) 0.0080(16) 0.0232(14) 0.0001(15) C19 0.066(2) 0.089(3) 0.074(3) -0.012(2) 0.042(2) -0.021(2) C21 0.0332(13) 0.0345(13) 0.0352(13) 0.0052(11) 0.0106(10) 0.0032(10) C22 0.0312(13) 0.0344(13) 0.0436(15) 0.0105(11) 0.0104(11) 0.0047(10) C23 0.0330(13) 0.0361(13) 0.0324(13) 0.0091(10) 0.0105(10) 0.0042(10) C24 0.0307(13) 0.0349(13) 0.0327(13) 0.0062(10) 0.0109(10) 0.0048(10) C25 0.0377(14) 0.0427(15) 0.0343(13) 0.0113(11) 0.0119(11) 0.0049(11) C26 0.0421(15) 0.0467(16) 0.0323(13) 0.0044(12) 0.0135(11) 0.0091(12) C27 0.0409(15) 0.0359(14) 0.0401(15) 0.0009(11) 0.0138(12) 0.0074(11) C28 0.0345(14) 0.0348(13) 0.0407(14) 0.0074(11) 0.0122(11) 0.0042(11) C29 0.0365(14) 0.0387(14) 0.0332(13) 0.0043(11) 0.0111(11) 0.0041(11) C30 0.0464(16) 0.0374(14) 0.0394(15) 0.0011(12) 0.0144(12) 0.0031(12) C31 0.0468(16) 0.0518(17) 0.0347(15) -0.0021(13) 0.0131(12) 0.0082(13) C32 0.0429(16) 0.0605(18) 0.0334(14) 0.0109(13) 0.0152(12) 0.0120(14) C33 0.0409(15) 0.0491(16) 0.0337(14) 0.0113(12) 0.0130(11) 0.0106(12) C34 0.0317(14) 0.0369(14) 0.0549(17) 0.0155(13) 0.0096(12) 0.0032(11) C35 0.065(2) 0.0399(17) 0.083(3) 0.0160(17) 0.0371(19) 0.0101(15) C36 0.073(3) 0.0380(17) 0.101(3) 0.0163(19) 0.033(2) 0.0131(16) C37 0.057(2) 0.0490(19) 0.094(3) 0.037(2) 0.0221(19) 0.0074(16) C38 0.063(2) 0.061(2) 0.067(2) 0.0337(18) 0.0205(17) 0.0059(17) N1 0.0363(12) 0.0336(11) 0.0305(11) 0.0051(9) 0.0120(9) 0.0033(9) N2 0.0333(12) 0.0337(11) 0.0421(12) 0.0062(9) 0.0117(9) 0.0032(9) N3 0.0348(12) 0.0369(11) 0.0371(12) 0.0125(9) 0.0117(9) 0.0054(9) N4 0.0362(12) 0.0328(11) 0.0338(11) 0.0082(9) 0.0118(9) 0.0056(9) N5 0.0393(12) 0.0399(12) 0.0316(11) 0.0067(9) 0.0127(9) 0.0071(10) N6 0.0538(16) 0.0475(14) 0.0536(15) 0.0230(12) 0.0163(12) 0.0048(12) O1 0.034(2) 0.056(2) 0.042(2) 0.0079(18) 0.0023(16) 0.0098(17) O1' 0.079(11) 0.141(14) 0.121(12) 0.099(11) 0.061(9) 0.072(10) O2 0.0606(14) 0.0859(18) 0.0373(12) 0.0185(12) 0.0174(10) 0.0108(13) O3 0.0375(10) 0.0456(11) 0.0404(10) 0.0065(9) 0.0171(8) 0.0011(8) O4 0.0617(13) 0.0430(11) 0.0346(10) 0.0061(8) 0.0208(9) 0.0104(10) P1 0.0539(5) 0.0610(5) 0.0459(4) 0.0239(4) 0.0224(4) 0.0219(4) P2 0.0354(4) 0.0341(3) 0.0324(3) 0.0047(3) 0.0127(3) 0.0025(3) S1 0.0695(5) 0.0406(4) 0.0409(4) 0.0146(3) 0.0202(3) 0.0137(3) S2 0.0466(4) 0.0562(4) 0.0391(4) 0.0152(3) 0.0169(3) 0.0089(3) S3 0.0450(4) 0.0367(3) 0.0374(3) 0.0112(3) 0.0141(3) 0.0028(3) S4 0.0438(4) 0.0360(3) 0.0354(3) 0.0031(3) 0.0140(3) 0.0063(3) Ni1 0.0453(2) 0.03377(19) 0.03138(19) 0.00830(14) 0.01613(14) 0.00696(14) _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 C1 C2 1.380(5) . ? C1 C6 1.406(5) . ? C1 P1 1.799(3) . ? C2 C3 1.396(4) . ? C2 H2 0.9300 . ? C3 C4 1.393(5) . ? C3 H3 0.9300 . ? C4 O2 1.355(4) . ? C4 C5 1.385(6) . ? C5 C6 1.379(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O2 1.424(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.435(10) . ? C8 O1 1.509(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C8' C9' 1.31(2) . ? C8' O1' 1.342(19) . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C11 C16 1.392(4) . ? C11 C12 1.397(4) . ? C11 P2 1.807(3) . ? C12 C13 1.382(4) . ? C12 H12 0.9300 . ? C13 C14 1.390(4) . ? C13 H13 0.9300 . ? C14 O4 1.370(3) . ? C14 C15 1.391(4) . ? C15 C16 1.392(4) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O4 1.426(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.446(5) . ? C18 O3 1.453(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 N2 1.327(4) . ? C21 N1 1.336(3) . ? C21 C29 1.474(4) . ? C22 N2 1.345(4) . ? C22 N3 1.350(4) . ? C22 C34 1.485(4) . ? C23 N3 1.322(3) . ? C23 N1 1.328(3) . ? C23 C24 1.487(4) . ? C24 N4 1.352(3) . ? C24 C25 1.380(4) . ? C25 C26 1.397(4) . ? C25 H25 0.9300 . ? C26 C27 1.375(4) . ? C26 H26 0.9300 . ? C27 C28 1.386(4) . ? C27 H27 0.9300 . ? C28 N4 1.336(3) . ? C28 H28 0.9300 . ? C29 N5 1.347(4) . ? C29 C30 1.391(4) . ? C30 C31 1.387(4) . ? C30 H30 0.9300 . ? C31 C32 1.378(5) . ? C31 H31 0.9300 . ? C32 C33 1.388(4) . ? C32 H32 0.9300 . ? C33 N5 1.336(3) . ? C33 H33 0.9300 . ? C34 N6 1.346(4) . ? C34 C35 1.363(4) . ? C35 C36 1.390(5) . ? C35 H35 0.9300 . ? C36 C37 1.357(6) . ? C36 H36 0.9300 . ? C37 C38 1.369(5) . ? C37 H37 0.9300 . ? C38 N6 1.329(4) . ? C38 H38 0.9300 . ? N1 Ni1 1.968(2) . ? N4 Ni1 2.135(2) . ? N5 Ni1 2.125(2) . ? O1 P1 1.588(6) . ? O1' P1 1.683(12) . ? O3 P2 1.616(2) . ? P1 S2 1.9863(11) . ? P1 S1 1.9993(13) . ? P2 S4 1.9579(10) . ? P2 S3 2.0254(10) . ? S1 Ni1 2.4004(8) . ? S2 Ni1 2.6045(9) . ? S3 Ni1 2.4130(8) . ? 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 C2 C1 C6 118.1(3) . . ? C2 C1 P1 123.3(2) . . ? C6 C1 P1 118.5(3) . . ? C1 C2 C3 121.6(3) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? O2 C4 C5 115.3(3) . . ? O2 C4 C3 125.6(4) . . ? C5 C4 C3 119.0(3) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 O1 107.5(6) . . ? C9 C8 H8A 110.2 . . ? O1 C8 H8A 110.2 . . ? C9 C8 H8B 110.2 . . ? O1 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C9' C8' O1' 122.5(16) . . ? C9' C8' H8'1 106.7 . . ? O1' C8' H8'1 106.7 . . ? C9' C8' H8'2 106.7 . . ? O1' C8' H8'2 106.7 . . ? H8'1 C8' H8'2 106.6 . . ? C8' C9' H9'1 109.5 . . ? C8' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C8' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C16 C11 C12 118.8(2) . . ? C16 C11 P2 120.6(2) . . ? C12 C11 P2 120.6(2) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.7(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? O4 C14 C13 115.5(2) . . ? O4 C14 C15 123.8(3) . . ? C13 C14 C15 120.7(2) . . ? C14 C15 C16 118.9(3) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 121.2(3) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 O3 110.3(3) . . ? C19 C18 H18A 109.6 . . ? O3 C18 H18A 109.6 . . ? C19 C18 H18B 109.6 . . ? O3 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C21 N1 123.4(2) . . ? N2 C21 C29 123.0(2) . . ? N1 C21 C29 113.5(2) . . ? N2 C22 N3 125.7(2) . . ? N2 C22 C34 116.6(2) . . ? N3 C22 C34 117.7(2) . . ? N3 C23 N1 124.2(2) . . ? N3 C23 C24 122.7(2) . . ? N1 C23 C24 113.0(2) . . ? N4 C24 C25 123.1(2) . . ? N4 C24 C23 113.6(2) . . ? C25 C24 C23 123.3(2) . . ? C24 C25 C26 117.7(3) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 118.8(3) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? N4 C28 C27 122.6(3) . . ? N4 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? N5 C29 C30 123.1(3) . . ? N5 C29 C21 114.3(2) . . ? C30 C29 C21 122.6(3) . . ? C31 C30 C29 117.8(3) . . ? C31 C30 H30 121.1 . . ? C29 C30 H30 121.1 . . ? C32 C31 C30 119.4(3) . . ? C32 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C31 C32 C33 119.3(3) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? N5 C33 C32 122.1(3) . . ? N5 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? N6 C34 C35 122.5(3) . . ? N6 C34 C22 116.0(3) . . ? C35 C34 C22 121.4(3) . . ? C34 C35 C36 119.3(3) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C37 C36 C35 118.3(3) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C36 C37 C38 119.0(3) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? N6 C38 C37 123.8(3) . . ? N6 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? C23 N1 C21 117.5(2) . . ? C23 N1 Ni1 121.81(18) . . ? C21 N1 Ni1 120.43(18) . . ? C21 N2 C22 114.7(2) . . ? C23 N3 C22 114.3(2) . . ? C28 N4 C24 118.1(2) . . ? C28 N4 Ni1 127.09(18) . . ? C24 N4 Ni1 114.63(17) . . ? C33 N5 C29 118.3(2) . . ? C33 N5 Ni1 127.6(2) . . ? C29 N5 Ni1 114.10(17) . . ? C38 N6 C34 116.9(3) . . ? C8 O1 P1 113.0(4) . . ? C8' O1' P1 126.9(13) . . ? C4 O2 C7 117.7(3) . . ? C18 O3 P2 117.97(18) . . ? C14 O4 C17 117.1(2) . . ? O1 P1 O1' 24.6(7) . . ? O1 P1 C1 108.7(2) . . ? O1' P1 C1 90.8(6) . . ? O1 P1 S2 114.6(2) . . ? O1' P1 S2 108.4(5) . . ? C1 P1 S2 111.45(12) . . ? O1 P1 S1 100.25(17) . . ? O1' P1 S1 123.2(7) . . ? C1 P1 S1 109.91(11) . . ? S2 P1 S1 111.30(5) . . ? O3 P2 C11 100.49(11) . . ? O3 P2 S4 112.00(8) . . ? C11 P2 S4 111.66(9) . . ? O3 P2 S3 104.07(8) . . ? C11 P2 S3 109.18(10) . . ? S4 P2 S3 117.81(4) . . ? P1 S1 Ni1 83.23(4) . . ? P1 S2 Ni1 78.29(4) . . ? P2 S3 Ni1 111.51(4) . . ? N1 Ni1 N5 77.39(9) . . ? N1 Ni1 N4 76.71(9) . . ? N5 Ni1 N4 154.06(9) . . ? N1 Ni1 S1 169.25(7) . . ? N5 Ni1 S1 103.11(7) . . ? N4 Ni1 S1 102.61(6) . . ? N1 Ni1 S3 103.36(7) . . ? N5 Ni1 S3 92.79(6) . . ? N4 Ni1 S3 91.69(6) . . ? S1 Ni1 S3 87.36(3) . . ? N1 Ni1 S2 87.16(7) . . ? N5 Ni1 S2 89.99(6) . . ? N4 Ni1 S2 90.24(6) . . ? S1 Ni1 S2 82.11(3) . . ? S3 Ni1 S2 169.46(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.664 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.071 # Attachment '_3.tptz_04slh043.cif' data_04slh043 _database_code_depnum_ccdc_archive 'CCDC 707533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 04lsh043/95 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 N6 Ni O4 P2 S4' _chemical_formula_weight 893.65 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5691(7) _cell_length_b 13.3601(7) _cell_length_c 13.8241(8) _cell_angle_alpha 76.563(2) _cell_angle_beta 81.865(2) _cell_angle_gamma 72.466(3) _cell_volume 2146.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9226 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.1 _exptl_crystal_description 'cut sheet' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.767 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8618 _exptl_absorpt_correction_T_max 0.9924 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; The values for minimum and maximum transmission are based on the cell dimensions only and were generated using the size command in SHELX. SADABS estimates the minimum and maximum transmission as 0.6413 and 0.7455, respectively. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\F & \wscans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65715 _diffrn_reflns_av_R_equivalents 0.1665 _diffrn_reflns_av_sigmaI/netI 0.1468 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7530 _reflns_number_gt 4862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The crystals were found to be of poor quality and weakly diffracting at higher angles, hence merging of the data resulted in a high Rint. The crystal morphologies were that of stacked plates and some twinning effects were observed, but no twin law could be identified. The high R-factor (R1) also reflects this. However, despite these bad statistics the connectivity of the compound could be establish unambigiously. Searches for better crystals were not successful. The PLATON module SQUEEZE was used to remove unresolvable disordered solvent from the model and to correct the intensities for this. ; _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^)+(0.0711P)^2^+8.2171P] 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 7530 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.1124 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 C1 C 0.6190(7) 0.4519(6) -0.2133(6) 0.034(2) Uani 1 1 d . . . C2 C 0.5092(6) 0.4696(6) -0.1705(6) 0.0317(19) Uani 1 1 d . . . H2 H 0.4951 0.4632 -0.1003 0.038 Uiso 1 1 calc R . . C3 C 0.4207(7) 0.4963(6) -0.2294(6) 0.0348(19) Uani 1 1 d . . . H3 H 0.3468 0.5041 -0.1990 0.042 Uiso 1 1 calc R . . C4 C 0.4385(7) 0.5119(6) -0.3322(7) 0.038(2) Uani 1 1 d . . . C5 C 0.5467(7) 0.4988(6) -0.3748(7) 0.041(2) Uani 1 1 d . . . H5 H 0.5596 0.5115 -0.4454 0.049 Uiso 1 1 calc R . . C6 C 0.6369(7) 0.4675(6) -0.3167(7) 0.043(2) Uani 1 1 d . . . H6 H 0.7109 0.4567 -0.3475 0.052 Uiso 1 1 calc R . . C7 C 0.2460(7) 0.5409(7) -0.3579(7) 0.049(2) Uani 1 1 d . . . H7A H 0.2461 0.4718 -0.3140 0.074 Uiso 1 1 calc R . . H7B H 0.1992 0.5537 -0.4129 0.074 Uiso 1 1 calc R . . H7C H 0.2160 0.5982 -0.3199 0.074 Uiso 1 1 calc R . . C8 C 0.9304(7) 0.4335(7) -0.1627(8) 0.053(3) Uani 1 1 d . . . H8A H 0.9840 0.3858 -0.2036 0.064 Uiso 1 1 calc R . . H8B H 0.9304 0.3943 -0.0925 0.064 Uiso 1 1 calc R . . C9 C 0.9660(8) 0.5307(8) -0.1706(9) 0.069(3) Uani 1 1 d . . . H9A H 0.9079 0.5818 -0.1360 0.083 Uiso 1 1 calc R . . H9B H 0.9738 0.5655 -0.2417 0.083 Uiso 1 1 calc R . . C10 C 1.0790(8) 0.5043(8) -0.1240(8) 0.065(3) Uani 1 1 d . . . H10A H 1.0712 0.4709 -0.0533 0.098 Uiso 1 1 calc R . . H10B H 1.1002 0.5706 -0.1303 0.098 Uiso 1 1 calc R . . H10C H 1.1370 0.4549 -0.1590 0.098 Uiso 1 1 calc R . . C11 C 0.6175(6) -0.0246(6) 0.2206(6) 0.0283(18) Uani 1 1 d . . . C12 C 0.5332(6) -0.0181(6) 0.1614(6) 0.0320(19) Uani 1 1 d . . . H12 H 0.5528 -0.0297 0.0951 0.038 Uiso 1 1 calc R . . C13 C 0.4226(7) 0.0045(6) 0.1971(6) 0.036(2) Uani 1 1 d . . . H13 H 0.3663 0.0071 0.1567 0.043 Uiso 1 1 calc R . . C14 C 0.3949(6) 0.0234(6) 0.2929(6) 0.0313(19) Uani 1 1 d . . . C15 C 0.4762(7) 0.0168(6) 0.3525(6) 0.036(2) Uani 1 1 d . . . H15 H 0.4563 0.0286 0.4186 0.043 Uiso 1 1 calc R . . C16 C 0.5877(6) -0.0070(6) 0.3158(6) 0.0325(19) Uani 1 1 d . . . H16 H 0.6438 -0.0113 0.3571 0.039 Uiso 1 1 calc R . . C17 C 0.2493(7) 0.0611(8) 0.4225(6) 0.052(2) Uani 1 1 d . . . H17A H 0.2852 -0.0035 0.4696 0.078 Uiso 1 1 calc R . . H17B H 0.1678 0.0759 0.4343 0.078 Uiso 1 1 calc R . . H17C H 0.2720 0.1220 0.4319 0.078 Uiso 1 1 calc R . . C18 C 0.9400(6) -0.0752(7) 0.2598(6) 0.036(2) Uani 1 1 d . . . H18A H 0.9800 -0.0264 0.2153 0.043 Uiso 1 1 calc R . . H18B H 0.9675 -0.1461 0.2408 0.043 Uiso 1 1 calc R . . C19 C 0.9603(7) -0.0853(7) 0.3667(6) 0.047(2) Uani 1 1 d . . . H19A H 0.9227 -0.1368 0.4099 0.056 Uiso 1 1 calc R . . H19B H 0.9268 -0.0149 0.3861 0.056 Uiso 1 1 calc R . . C20 C 1.0847(7) -0.1230(9) 0.3840(7) 0.061(3) Uani 1 1 d . . . H20A H 1.1192 -0.1906 0.3612 0.091 Uiso 1 1 calc R . . H20B H 1.0937 -0.1338 0.4553 0.091 Uiso 1 1 calc R . . H20C H 1.1210 -0.0687 0.3465 0.091 Uiso 1 1 calc R . . C21 C 0.5633(6) 0.2430(6) 0.2016(6) 0.0304(18) Uani 1 1 d . . . C22 C 0.5911(7) 0.2392(6) 0.3598(6) 0.036(2) Uani 1 1 d . . . C23 C 0.7390(6) 0.2139(6) 0.2455(6) 0.0322(19) Uani 1 1 d . . . C24 C 0.8578(6) 0.2004(6) 0.2075(6) 0.0333(19) Uani 1 1 d . . . C25 C 0.9397(6) 0.1988(6) 0.2646(6) 0.0333(19) Uani 1 1 d . . . H25 H 0.9224 0.2070 0.3320 0.040 Uiso 1 1 calc R . . C26 C 1.0489(7) 0.1848(6) 0.2210(7) 0.040(2) Uani 1 1 d . . . H26 H 1.1075 0.1829 0.2584 0.048 Uiso 1 1 calc R . . C27 C 1.0711(7) 0.1736(6) 0.1221(7) 0.042(2) Uani 1 1 d . . . H27 H 1.1450 0.1630 0.0912 0.050 Uiso 1 1 calc R . . C28 C 0.9824(6) 0.1784(6) 0.0691(6) 0.037(2) Uani 1 1 d . . . H28 H 0.9974 0.1710 0.0014 0.044 Uiso 1 1 calc R . . C29 C 0.4955(6) 0.2510(6) 0.1193(6) 0.0316(19) Uani 1 1 d . . . C30 C 0.3793(6) 0.2776(6) 0.1278(7) 0.039(2) Uani 1 1 d . . . H30 H 0.3373 0.2932 0.1879 0.047 Uiso 1 1 calc R . . C31 C 0.3270(7) 0.2805(6) 0.0442(7) 0.041(2) Uani 1 1 d . . . H31 H 0.2476 0.2994 0.0461 0.050 Uiso 1 1 calc R . . C32 C 0.3907(7) 0.2557(7) -0.0409(7) 0.045(2) Uani 1 1 d . . . H32 H 0.3558 0.2551 -0.0973 0.054 Uiso 1 1 calc R . . C33 C 0.5065(7) 0.2317(6) -0.0439(6) 0.039(2) Uani 1 1 d . . . H33 H 0.5500 0.2154 -0.1032 0.047 Uiso 1 1 calc R . . C34 C 0.5465(7) 0.2421(6) 0.4639(6) 0.039(2) Uani 1 1 d . . . C35 C 0.6154(8) 0.2358(6) 0.5357(6) 0.045(2) Uani 1 1 d . . . H35 H 0.6934 0.2269 0.5204 0.054 Uiso 1 1 calc R . . C36 C 0.5651(9) 0.2431(7) 0.6333(7) 0.052(3) Uani 1 1 d . . . H36 H 0.6093 0.2388 0.6852 0.063 Uiso 1 1 calc R . . C37 C 0.4524(9) 0.2565(7) 0.6520(7) 0.053(3) Uani 1 1 d . . . H37 H 0.4174 0.2619 0.7169 0.063 Uiso 1 1 calc R . . C38 C 0.3907(9) 0.2620(7) 0.5759(7) 0.053(3) Uani 1 1 d . . . H38 H 0.3127 0.2703 0.5905 0.064 Uiso 1 1 calc R . . N1 N 0.6724(5) 0.2190(5) 0.1776(4) 0.0248(14) Uani 1 1 d . . . N2 N 0.7030(5) 0.2200(5) 0.3401(5) 0.0334(16) Uani 1 1 d . . . N3 N 0.5168(5) 0.2546(5) 0.2918(5) 0.0348(16) Uani 1 1 d . . . N4 N 0.5584(5) 0.2308(5) 0.0343(5) 0.0323(16) Uani 1 1 d . . . N5 N 0.8774(5) 0.1930(5) 0.1098(5) 0.0284(15) Uani 1 1 d . . . N6 N 0.4330(6) 0.2563(5) 0.4824(6) 0.0478(19) Uani 1 1 d . . . O1 O 0.8188(4) 0.4611(4) -0.1968(4) 0.0443(15) Uani 1 1 d . . . O2 O 0.3575(4) 0.5396(4) -0.3970(4) 0.0420(14) Uani 1 1 d . . . O3 O 0.8198(4) -0.0324(4) 0.2506(4) 0.0344(13) Uani 1 1 d . . . O4 O 0.2825(4) 0.0449(5) 0.3231(4) 0.0454(15) Uani 1 1 d . . . P1 P 0.73478(17) 0.39334(17) -0.13727(16) 0.0332(5) Uani 1 1 d . . . P2 P 0.76240(16) -0.06661(16) 0.17136(16) 0.0308(5) Uani 1 1 d . . . S1 S 0.79705(17) 0.23636(16) -0.13695(16) 0.0362(5) Uani 1 1 d . . . S2 S 0.69743(17) 0.41347(16) 0.00281(16) 0.0363(5) Uani 1 1 d . . . S3 S 0.78318(16) 0.02034(16) 0.03395(15) 0.0345(5) Uani 1 1 d . . . S4 S 0.81384(16) -0.22240(16) 0.17750(16) 0.0363(5) Uani 1 1 d . . . Ni1 Ni 0.73326(8) 0.20907(8) 0.03811(7) 0.0291(3) 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 C1 0.042(5) 0.024(4) 0.038(5) -0.005(4) 0.002(4) -0.014(4) C2 0.026(4) 0.030(4) 0.036(5) -0.008(4) 0.005(4) -0.005(4) C3 0.038(5) 0.040(5) 0.029(5) -0.008(4) -0.002(4) -0.013(4) C4 0.037(5) 0.025(4) 0.052(6) -0.004(4) -0.006(4) -0.012(4) C5 0.049(6) 0.041(5) 0.038(5) -0.012(4) -0.004(4) -0.018(4) C6 0.043(5) 0.040(5) 0.051(6) -0.015(4) 0.008(5) -0.020(4) C7 0.041(6) 0.060(6) 0.054(6) -0.019(5) -0.003(5) -0.021(5) C8 0.027(5) 0.043(6) 0.087(8) -0.007(5) 0.004(5) -0.014(4) C9 0.055(7) 0.048(6) 0.101(9) -0.009(6) -0.024(6) -0.008(5) C10 0.055(7) 0.071(7) 0.079(8) -0.019(6) -0.008(6) -0.027(6) C11 0.022(4) 0.030(4) 0.036(5) -0.008(4) 0.002(4) -0.013(3) C12 0.035(5) 0.033(5) 0.032(5) -0.001(4) -0.007(4) -0.018(4) C13 0.033(5) 0.039(5) 0.041(5) -0.009(4) -0.001(4) -0.017(4) C14 0.018(4) 0.027(4) 0.042(5) 0.000(4) 0.006(4) -0.006(3) C15 0.041(5) 0.038(5) 0.030(5) -0.004(4) -0.004(4) -0.014(4) C16 0.022(4) 0.036(5) 0.041(5) -0.010(4) 0.000(4) -0.011(4) C17 0.044(6) 0.075(7) 0.036(6) -0.016(5) 0.014(4) -0.019(5) C18 0.026(4) 0.044(5) 0.041(5) -0.014(4) -0.006(4) -0.010(4) C19 0.040(5) 0.058(6) 0.045(6) -0.018(5) 0.000(4) -0.014(5) C20 0.044(6) 0.098(8) 0.050(6) -0.020(6) -0.018(5) -0.023(6) C21 0.028(5) 0.021(4) 0.042(5) -0.007(4) -0.002(4) -0.007(3) C22 0.039(5) 0.030(5) 0.039(5) -0.014(4) 0.016(4) -0.013(4) C23 0.031(5) 0.022(4) 0.043(5) -0.006(4) 0.000(4) -0.008(4) C24 0.033(5) 0.030(5) 0.040(5) -0.008(4) -0.008(4) -0.010(4) C25 0.030(5) 0.031(5) 0.038(5) -0.008(4) -0.008(4) -0.003(4) C26 0.031(5) 0.041(5) 0.050(6) -0.007(4) -0.015(4) -0.012(4) C27 0.026(5) 0.036(5) 0.064(7) -0.008(4) 0.004(4) -0.014(4) C28 0.024(5) 0.040(5) 0.048(5) -0.020(4) 0.010(4) -0.008(4) C29 0.037(5) 0.024(4) 0.037(5) -0.010(4) 0.003(4) -0.013(4) C30 0.021(4) 0.038(5) 0.051(6) -0.003(4) -0.002(4) -0.004(4) C31 0.029(5) 0.037(5) 0.061(6) -0.001(4) -0.018(5) -0.013(4) C32 0.039(5) 0.040(5) 0.060(6) -0.009(5) -0.012(5) -0.015(4) C33 0.045(5) 0.037(5) 0.043(5) -0.012(4) -0.008(4) -0.017(4) C34 0.041(5) 0.036(5) 0.037(5) -0.003(4) 0.005(4) -0.011(4) C35 0.053(6) 0.038(5) 0.040(6) -0.006(4) 0.003(5) -0.012(4) C36 0.088(8) 0.033(5) 0.045(6) -0.007(4) -0.008(5) -0.030(5) C37 0.078(8) 0.032(5) 0.045(6) -0.017(4) 0.027(6) -0.018(5) C38 0.070(7) 0.043(6) 0.043(6) -0.012(5) 0.012(5) -0.016(5) N1 0.016(3) 0.033(4) 0.028(4) -0.009(3) 0.000(3) -0.008(3) N2 0.036(4) 0.032(4) 0.031(4) -0.011(3) 0.002(3) -0.007(3) N3 0.033(4) 0.032(4) 0.041(4) -0.013(3) 0.004(3) -0.010(3) N4 0.029(4) 0.028(4) 0.044(4) -0.007(3) -0.008(3) -0.010(3) N5 0.022(3) 0.030(4) 0.036(4) -0.009(3) -0.001(3) -0.010(3) N6 0.053(5) 0.034(4) 0.054(5) -0.013(4) 0.020(4) -0.017(4) O1 0.035(3) 0.041(3) 0.056(4) -0.008(3) 0.007(3) -0.014(3) O2 0.037(3) 0.050(4) 0.044(4) -0.014(3) -0.006(3) -0.013(3) O3 0.022(3) 0.044(3) 0.040(3) -0.012(3) 0.000(2) -0.012(3) O4 0.029(3) 0.058(4) 0.041(4) -0.004(3) -0.001(3) -0.007(3) P1 0.0284(12) 0.0344(12) 0.0370(13) -0.0099(10) 0.0043(10) -0.0100(10) P2 0.0243(11) 0.0328(12) 0.0389(13) -0.0107(10) -0.0028(9) -0.0103(9) S1 0.0347(12) 0.0357(12) 0.0375(13) -0.0110(10) 0.0052(10) -0.0094(10) S2 0.0317(12) 0.0378(12) 0.0417(13) -0.0116(10) -0.0026(10) -0.0105(10) S3 0.0324(12) 0.0379(12) 0.0365(12) -0.0141(10) 0.0047(9) -0.0129(10) S4 0.0296(11) 0.0340(12) 0.0495(14) -0.0129(10) -0.0028(10) -0.0118(9) Ni1 0.0238(6) 0.0350(6) 0.0315(6) -0.0096(5) 0.0005(4) -0.0116(5) _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 C1 C6 1.392(11) . ? C1 C2 1.396(10) . ? C1 P1 1.788(8) . ? C2 C3 1.382(10) . ? C2 H2 0.9500 . ? C3 C4 1.383(11) . ? C3 H3 0.9500 . ? C4 O2 1.361(9) . ? C4 C5 1.380(11) . ? C5 C6 1.386(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O2 1.426(9) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.456(10) . ? C8 C9 1.474(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.551(12) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.371(10) . ? C11 C12 1.399(10) . ? C11 P2 1.818(7) . ? C12 C13 1.375(10) . ? C12 H12 0.9500 . ? C13 C14 1.382(11) . ? C13 H13 0.9500 . ? C14 C15 1.371(10) . ? C14 O4 1.378(8) . ? C15 C16 1.388(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O4 1.425(9) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O3 1.458(8) . ? C18 C19 1.504(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.526(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N3 1.322(9) . ? C21 N1 1.323(9) . ? C21 C29 1.482(11) . ? C22 N2 1.351(10) . ? C22 N3 1.356(10) . ? C22 C34 1.475(11) . ? C23 N1 1.322(9) . ? C23 N2 1.335(9) . ? C23 C24 1.482(10) . ? C24 N5 1.359(9) . ? C24 C25 1.376(10) . ? C25 C26 1.395(11) . ? C25 H25 0.9500 . ? C26 C27 1.389(11) . ? C26 H26 0.9500 . ? C27 C28 1.396(11) . ? C27 H27 0.9500 . ? C28 N5 1.336(9) . ? C28 H28 0.9500 . ? C29 N4 1.354(9) . ? C29 C30 1.390(10) . ? C30 C31 1.396(11) . ? C30 H30 0.9500 . ? C31 C32 1.374(12) . ? C31 H31 0.9500 . ? C32 C33 1.390(11) . ? C32 H32 0.9500 . ? C33 N4 1.336(10) . ? C33 H33 0.9500 . ? C34 N6 1.375(10) . ? C34 C35 1.379(12) . ? C35 C36 1.418(12) . ? C35 H35 0.9500 . ? C36 C37 1.367(13) . ? C36 H36 0.9500 . ? C37 C38 1.369(13) . ? C37 H37 0.9500 . ? C38 N6 1.336(11) . ? C38 H38 0.9500 . ? N1 Ni1 1.990(6) . ? N4 Ni1 2.134(6) . ? N5 Ni1 2.118(6) . ? O1 P1 1.611(5) . ? O3 P2 1.608(5) . ? P1 S2 1.988(3) . ? P1 S1 2.005(3) . ? P2 S4 1.970(3) . ? P2 S3 2.011(3) . ? S1 Ni1 2.419(2) . ? S2 Ni1 2.569(2) . ? S3 Ni1 2.421(2) . ? 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 C6 C1 C2 118.6(8) . . ? C6 C1 P1 120.1(6) . . ? C2 C1 P1 120.8(6) . . ? C3 C2 C1 120.6(8) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.7(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? O2 C4 C5 115.8(8) . . ? O2 C4 C3 125.5(7) . . ? C5 C4 C3 118.7(8) . . ? C4 C5 C6 121.3(8) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 120.0(8) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C9 110.6(7) . . ? O1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 111.5(8) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.5(7) . . ? C16 C11 P2 122.9(6) . . ? C12 C11 P2 118.4(6) . . ? C13 C12 C11 121.4(7) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 118.8(7) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 O4 124.0(7) . . ? C15 C14 C13 120.9(7) . . ? O4 C14 C13 115.1(7) . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.7(7) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C18 C19 107.7(6) . . ? O3 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? O3 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C18 C19 C20 112.3(7) . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 N1 124.1(7) . . ? N3 C21 C29 121.7(7) . . ? N1 C21 C29 114.1(7) . . ? N2 C22 N3 125.3(7) . . ? N2 C22 C34 117.2(8) . . ? N3 C22 C34 117.5(7) . . ? N1 C23 N2 123.2(7) . . ? N1 C23 C24 114.0(7) . . ? N2 C23 C24 122.8(7) . . ? N5 C24 C25 123.2(7) . . ? N5 C24 C23 113.4(7) . . ? C25 C24 C23 123.3(7) . . ? C24 C25 C26 118.2(8) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C27 C26 C25 119.3(7) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 118.6(7) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? N5 C28 C27 122.6(8) . . ? N5 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? N4 C29 C30 123.4(7) . . ? N4 C29 C21 113.0(7) . . ? C30 C29 C21 123.6(7) . . ? C29 C30 C31 117.1(8) . . ? C29 C30 H30 121.4 . . ? C31 C30 H30 121.4 . . ? C32 C31 C30 119.7(8) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 119.6(8) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? N4 C33 C32 121.8(8) . . ? N4 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? N6 C34 C35 123.3(8) . . ? N6 C34 C22 115.8(8) . . ? C35 C34 C22 120.9(8) . . ? C34 C35 C36 117.3(8) . . ? C34 C35 H35 121.3 . . ? C36 C35 H35 121.3 . . ? C37 C36 C35 119.4(9) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 119.1(9) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? N6 C38 C37 124.3(9) . . ? N6 C38 H38 117.9 . . ? C37 C38 H38 117.9 . . ? C23 N1 C21 118.2(6) . . ? C23 N1 Ni1 120.5(5) . . ? C21 N1 Ni1 120.8(5) . . ? C23 N2 C22 114.5(7) . . ? C21 N3 C22 114.2(6) . . ? C33 N4 C29 118.3(7) . . ? C33 N4 Ni1 126.5(5) . . ? C29 N4 Ni1 115.1(5) . . ? C28 N5 C24 118.0(7) . . ? C28 N5 Ni1 127.1(5) . . ? C24 N5 Ni1 114.8(5) . . ? C38 N6 C34 116.6(8) . . ? C8 O1 P1 118.0(5) . . ? C4 O2 C7 118.7(6) . . ? C18 O3 P2 119.8(4) . . ? C14 O4 C17 117.6(6) . . ? O1 P1 C1 99.4(3) . . ? O1 P1 S2 111.8(2) . . ? C1 P1 S2 113.4(3) . . ? O1 P1 S1 112.2(2) . . ? C1 P1 S1 111.0(3) . . ? S2 P1 S1 108.92(13) . . ? O3 P2 C11 98.6(3) . . ? O3 P2 S4 111.6(2) . . ? C11 P2 S4 111.5(2) . . ? O3 P2 S3 110.5(2) . . ? C11 P2 S3 110.1(3) . . ? S4 P2 S3 113.46(13) . . ? P1 S1 Ni1 85.93(10) . . ? P1 S2 Ni1 82.28(9) . . ? P2 S3 Ni1 110.54(10) . . ? N1 Ni1 N5 77.1(2) . . ? N1 Ni1 N4 76.4(2) . . ? N5 Ni1 N4 153.5(2) . . ? N1 Ni1 S1 168.31(18) . . ? N5 Ni1 S1 103.33(17) . . ? N4 Ni1 S1 102.55(19) . . ? N1 Ni1 S3 105.34(17) . . ? N5 Ni1 S3 93.37(17) . . ? N4 Ni1 S3 93.83(17) . . ? S1 Ni1 S3 86.33(7) . . ? N1 Ni1 S2 87.11(17) . . ? N5 Ni1 S2 88.95(16) . . ? N4 Ni1 S2 89.47(17) . . ? S1 Ni1 S2 81.23(7) . . ? S3 Ni1 S2 167.55(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.657 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.095 # Attachment '_5.tptz_04slh042.cif' data_04slh042 _database_code_depnum_ccdc_archive 'CCDC 707534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 04slh042/93 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H44 N6 Ni O4 P2 S4' _chemical_formula_weight 921.70 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.294(2) _cell_length_b 20.6419(18) _cell_length_c 12.5615(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.260(8) _cell_angle_gamma 90.00 _cell_volume 4223.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9538 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'chunky needle' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8346 _exptl_absorpt_correction_T_max 0.9120 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; The values for minimum and maximum transmission are based on the cell dimensions only and were generated using the size command in SHELX. SADABS estimates the ratio of minimum to maximum transmission as 0.606808. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32213 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9665 _reflns_number_gt 6694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The structure contains a significant amount of disorder leading to elevated ratios of max to min ADP values. Appropriate constraints were applied. ; _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^)+(0.0000P)^2^+19.3288P] 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 SHELXL _refine_ls_extinction_coef 0.0024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9665 _refine_ls_number_parameters 641 _refine_ls_number_restraints 204 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.1880 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.146 _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 C1A C 0.4174(4) 0.7385(4) 0.0834(6) 0.045(2) Uani 0.547(5) 1 d PGU A 1 C2A C 0.4249(5) 0.7625(4) 0.1865(6) 0.046(3) Uani 0.547(5) 1 d PGU A 1 H2A H 0.3788 0.7626 0.2315 0.056 Uiso 0.547(5) 1 calc PR A 1 C3A C 0.4999(6) 0.7865(6) 0.2237(6) 0.059(5) Uani 0.547(5) 1 d PGU A 1 H3A H 0.5051 0.8029 0.2942 0.071 Uiso 0.547(5) 1 calc PR A 1 C4A C 0.5674(5) 0.7865(7) 0.1579(8) 0.055(5) Uani 0.547(5) 1 d PGU A 1 C5A C 0.5598(4) 0.7624(5) 0.0548(7) 0.054(3) Uani 0.547(5) 1 d PGU A 1 H5A H 0.6059 0.7624 0.0097 0.064 Uiso 0.547(5) 1 calc PR A 1 C6A C 0.4848(5) 0.7385(4) 0.0175(5) 0.049(3) Uani 0.547(5) 1 d PGU A 1 H6A H 0.4797 0.7220 -0.0530 0.058 Uiso 0.547(5) 1 calc PR A 1 C7A C 0.6640(11) 0.8074(8) 0.3034(17) 0.097(7) Uani 0.547(5) 1 d P A 1 H7A1 H 0.6321 0.8401 0.3409 0.145 Uiso 0.547(5) 1 calc PR A 1 H7A2 H 0.7227 0.8158 0.3149 0.145 Uiso 0.547(5) 1 calc PR A 1 H7A3 H 0.6505 0.7643 0.3307 0.145 Uiso 0.547(5) 1 calc PR A 1 C8A C 0.1732(11) 0.7569(10) 0.0898(15) 0.068(6) Uani 0.547(5) 1 d PDU A 1 H8A1 H 0.1551 0.7244 0.0363 0.082 Uiso 0.547(5) 1 calc PR A 1 H8A2 H 0.1522 0.7999 0.0670 0.082 Uiso 0.547(5) 1 calc PR A 1 C9A C 0.1382(7) 0.7389(7) 0.2029(12) 0.065(4) Uani 0.547(5) 1 d PDU A 1 H9A1 H 0.1570 0.6950 0.2239 0.078 Uiso 0.547(5) 1 calc PR A 1 H9A2 H 0.1589 0.7701 0.2570 0.078 Uiso 0.547(5) 1 calc PR A 1 C10A C 0.0497(10) 0.7407(9) 0.1979(12) 0.054(4) Uani 0.547(5) 1 d PDU A 1 H10A H 0.0290 0.7075 0.1470 0.065 Uiso 0.547(5) 1 calc PR A 1 H10B H 0.0310 0.7837 0.1722 0.065 Uiso 0.547(5) 1 calc PR A 1 C11A C 0.0153(9) 0.7277(8) 0.3076(14) 0.081(4) Uani 0.547(5) 1 d PDU A 1 H11A H 0.0306 0.6839 0.3307 0.122 Uiso 0.547(5) 1 calc PR A 1 H11B H -0.0446 0.7316 0.3043 0.122 Uiso 0.547(5) 1 calc PR A 1 H11C H 0.0379 0.7594 0.3585 0.122 Uiso 0.547(5) 1 calc PR A 1 O1A O 0.2616(5) 0.7583(5) 0.0975(7) 0.065(3) Uani 0.547(5) 1 d P A 1 O2A O 0.6439(6) 0.8103(5) 0.1895(10) 0.081(4) Uani 0.547(5) 1 d P A 1 C1B C 0.2169(5) 0.7187(5) 0.1220(8) 0.045(2) Uani 0.453(5) 1 d PGU A 2 C2B C 0.1888(6) 0.6950(4) 0.2181(7) 0.051(4) Uani 0.453(5) 1 d PGU A 2 H2B H 0.2215 0.6656 0.2588 0.061 Uiso 0.453(5) 1 calc PR A 2 C3B C 0.1127(7) 0.7143(5) 0.2547(7) 0.058(4) Uani 0.453(5) 1 d PGU A 2 H3B H 0.0935 0.6981 0.3204 0.070 Uiso 0.453(5) 1 calc PR A 2 C4B C 0.0648(6) 0.7574(6) 0.1952(9) 0.073(9) Uani 0.453(5) 1 d PGU A 2 C5B C 0.0930(7) 0.7811(5) 0.0991(9) 0.058(4) Uani 0.453(5) 1 d PGU A 2 H5B H 0.0602 0.8105 0.0584 0.069 Uiso 0.453(5) 1 calc PR A 2 C6B C 0.1690(7) 0.7617(5) 0.0625(7) 0.060(7) Uani 0.453(5) 1 d PGU A 2 H6B H 0.1883 0.7779 -0.0032 0.072 Uiso 0.453(5) 1 calc PR A 2 C7B C -0.0484(12) 0.7472(10) 0.3164(16) 0.084(6) Uani 0.453(5) 1 d P A 2 H7B1 H -0.0508 0.6999 0.3094 0.126 Uiso 0.453(5) 1 calc PR A 2 H7B2 H -0.1040 0.7643 0.3250 0.126 Uiso 0.453(5) 1 calc PR A 2 H7B3 H -0.0144 0.7586 0.3788 0.126 Uiso 0.453(5) 1 calc PR A 2 C8B C 0.4510(10) 0.7526(9) 0.0918(13) 0.064(5) Uani 0.453(5) 1 d PDU A 2 H8B1 H 0.4533 0.7874 0.0377 0.077 Uiso 0.453(5) 1 calc PR A 2 H8B2 H 0.4748 0.7128 0.0612 0.077 Uiso 0.453(5) 1 calc PR A 2 C9B C 0.5014(9) 0.7734(12) 0.1958(16) 0.070(6) Uani 0.453(5) 1 d PDU A 2 H9B1 H 0.4798 0.8149 0.2229 0.084 Uiso 0.453(5) 1 calc PR A 2 H9B2 H 0.4949 0.7401 0.2518 0.084 Uiso 0.453(5) 1 calc PR A 2 C10B C 0.5871(13) 0.7805(14) 0.1723(17) 0.092(9) Uani 0.453(5) 1 d PDU A 2 H10C H 0.5947 0.8184 0.1252 0.110 Uiso 0.453(5) 1 calc PR A 2 H10D H 0.6067 0.7415 0.1348 0.110 Uiso 0.453(5) 1 calc PR A 2 C11B C 0.6364(11) 0.7899(11) 0.276(2) 0.081(4) Uani 0.453(5) 1 d PDU A 2 H11D H 0.6007 0.8079 0.3303 0.122 Uiso 0.453(5) 1 calc PR A 2 H11E H 0.6820 0.8198 0.2637 0.122 Uiso 0.453(5) 1 calc PR A 2 H11F H 0.6581 0.7480 0.3001 0.122 Uiso 0.453(5) 1 calc PR A 2 O1B O 0.3715(8) 0.7417(7) 0.1193(9) 0.092(5) Uani 0.453(5) 1 d P A 2 O2B O -0.0143(7) 0.7738(6) 0.2248(10) 0.071(4) Uani 0.453(5) 1 d P A 2 C12 C 0.3165(3) 0.3990(2) -0.2171(5) 0.0342(12) Uani 1 1 d . . . C13 C 0.3974(3) 0.3922(3) -0.1775(5) 0.0363(13) Uani 1 1 d . . . H13 H 0.4070 0.3909 -0.1026 0.044 Uiso 1 1 calc R . . C14 C 0.4628(3) 0.3873(3) -0.2442(5) 0.0379(13) Uani 1 1 d . . . H14 H 0.5169 0.3826 -0.2154 0.045 Uiso 1 1 calc R . . C15 C 0.4498(3) 0.3894(3) -0.3538(5) 0.0357(12) Uani 1 1 d . . . C16 C 0.3701(3) 0.3959(3) -0.3950(5) 0.0425(14) Uani 1 1 d . . . H16 H 0.3609 0.3977 -0.4699 0.051 Uiso 1 1 calc R . . C17 C 0.3048(3) 0.3997(3) -0.3278(5) 0.0394(13) Uani 1 1 d . . . H17 H 0.2507 0.4028 -0.3570 0.047 Uiso 1 1 calc R . . C18 C 0.5931(3) 0.3776(3) -0.3875(5) 0.0492(16) Uani 1 1 d . . . H18A H 0.6082 0.4112 -0.3356 0.074 Uiso 1 1 calc R . . H18B H 0.6310 0.3790 -0.4470 0.074 Uiso 1 1 calc R . . H18C H 0.5964 0.3350 -0.3532 0.074 Uiso 1 1 calc R . . C19A C 0.2066(6) 0.2830(4) -0.1098(8) 0.062(3) Uani 0.746(9) 1 d PDU B 1 H19A H 0.2548 0.2637 -0.1445 0.075 Uiso 0.746(9) 1 calc PR B 1 H19B H 0.1667 0.2944 -0.1672 0.075 Uiso 0.746(9) 1 calc PR B 1 C20A C 0.1700(7) 0.2330(4) -0.0471(8) 0.056(2) Uani 0.746(9) 1 d PDU B 1 H20A H 0.1161 0.2494 -0.0239 0.067 Uiso 0.746(9) 1 calc PR B 1 H20B H 0.2047 0.2274 0.0179 0.067 Uiso 0.746(9) 1 calc PR B 1 C21A C 0.1565(8) 0.1690(6) -0.0931(9) 0.075(3) Uani 0.746(9) 1 d PDU B 1 H21A H 0.2104 0.1482 -0.1036 0.090 Uiso 0.746(9) 1 calc PR B 1 H21B H 0.1296 0.1741 -0.1641 0.090 Uiso 0.746(9) 1 calc PR B 1 C22A C 0.1041(8) 0.1244(6) -0.0259(12) 0.068(4) Uani 0.746(9) 1 d PDU B 1 H22A H 0.1283 0.1211 0.0460 0.101 Uiso 0.746(9) 1 calc PR B 1 H22B H 0.1018 0.0813 -0.0585 0.101 Uiso 0.746(9) 1 calc PR B 1 H22C H 0.0484 0.1421 -0.0219 0.101 Uiso 0.746(9) 1 calc PR B 1 C19B C 0.1894(15) 0.3072(9) 0.005(2) 0.073(8) Uani 0.254(9) 1 d PDU B 2 H19C H 0.1304 0.3137 -0.0123 0.088 Uiso 0.254(9) 1 calc PR B 2 H19D H 0.2000 0.3266 0.0765 0.088 Uiso 0.254(9) 1 calc PR B 2 C20B C 0.2043(13) 0.2390(9) 0.013(3) 0.081(8) Uani 0.254(9) 1 d PDU B 2 H20C H 0.2422 0.2322 0.0748 0.097 Uiso 0.254(9) 1 calc PR B 2 H20D H 0.2344 0.2262 -0.0512 0.097 Uiso 0.254(9) 1 calc PR B 2 C21B C 0.1368(16) 0.1936(10) 0.024(2) 0.075(8) Uani 0.254(9) 1 d PDU B 2 H21C H 0.0845 0.2171 0.0114 0.090 Uiso 0.254(9) 1 calc PR B 2 H21D H 0.1371 0.1773 0.0981 0.090 Uiso 0.254(9) 1 calc PR B 2 C22B C 0.140(2) 0.1359(14) -0.052(3) 0.080(12) Uani 0.254(9) 1 d PDU B 2 H22D H 0.1879 0.1396 -0.0965 0.120 Uiso 0.254(9) 1 calc PR B 2 H22E H 0.0898 0.1354 -0.0967 0.120 Uiso 0.254(9) 1 calc PR B 2 H22F H 0.1430 0.0957 -0.0102 0.120 Uiso 0.254(9) 1 calc PR B 2 C23 C 0.1722(3) 0.5736(3) -0.2680(4) 0.0334(12) Uani 1 1 d . . . C24 C 0.2113(3) 0.5546(2) -0.4362(4) 0.0335(12) Uani 1 1 d . . . C25 C 0.3069(3) 0.5589(2) -0.3047(4) 0.0307(11) Uani 1 1 d . . . C26 C 0.3918(3) 0.5555(2) -0.2590(4) 0.0315(11) Uani 1 1 d . . . C27 C 0.4595(3) 0.5475(2) -0.3213(5) 0.0345(12) Uani 1 1 d . . . H27 H 0.4543 0.5445 -0.3966 0.041 Uiso 1 1 calc R . . C28 C 0.5358(3) 0.5440(3) -0.2701(5) 0.0409(14) Uani 1 1 d . . . H28 H 0.5840 0.5382 -0.3102 0.049 Uiso 1 1 calc R . . C29 C 0.5411(3) 0.5488(3) -0.1612(5) 0.0425(15) Uani 1 1 d . . . H29 H 0.5929 0.5460 -0.1252 0.051 Uiso 1 1 calc R . . C30 C 0.4700(3) 0.5578(3) -0.1044(5) 0.0415(14) Uani 1 1 d . . . H30 H 0.4742 0.5616 -0.0291 0.050 Uiso 1 1 calc R . . C31 C 0.1138(3) 0.5858(3) -0.1829(4) 0.0359(12) Uani 1 1 d . . . C32 C 0.0297(3) 0.5901(3) -0.2009(5) 0.0441(14) Uani 1 1 d . . . H32 H 0.0068 0.5873 -0.2709 0.053 Uiso 1 1 calc R . . C33 C -0.0194(4) 0.5985(3) -0.1150(6) 0.0524(16) Uani 1 1 d . . . H33 H -0.0773 0.6009 -0.1250 0.063 Uiso 1 1 calc R . . C34 C 0.0148(4) 0.6036(3) -0.0138(6) 0.0496(16) Uani 1 1 d . . . H34 H -0.0190 0.6094 0.0462 0.060 Uiso 1 1 calc R . . C35 C 0.0994(4) 0.6001(3) -0.0018(5) 0.0441(14) Uani 1 1 d . . . H35 H 0.1232 0.6040 0.0677 0.053 Uiso 1 1 calc R . . C36 C 0.1885(3) 0.5417(3) -0.5496(4) 0.0348(12) Uani 1 1 d . . . C37 C 0.1107(4) 0.5572(3) -0.5882(5) 0.0454(15) Uani 1 1 d . . . H37 H 0.0714 0.5767 -0.5434 0.054 Uiso 1 1 calc R . . C38 C 0.0915(4) 0.5435(3) -0.6944(5) 0.0494(16) Uani 1 1 d . . . H38 H 0.0390 0.5542 -0.7238 0.059 Uiso 1 1 calc R . . C39 C 0.1492(4) 0.5145(3) -0.7559(5) 0.0446(14) Uani 1 1 d . . . H39 H 0.1377 0.5049 -0.8286 0.053 Uiso 1 1 calc R . . C40 C 0.2247(4) 0.4995(3) -0.7100(5) 0.0461(15) Uani 1 1 d . . . H40 H 0.2641 0.4786 -0.7529 0.055 Uiso 1 1 calc R . . N1 N 0.2503(2) 0.5690(2) -0.2329(3) 0.0319(10) Uani 1 1 d . . . N2 N 0.1495(3) 0.5670(2) -0.3694(4) 0.0357(10) Uani 1 1 d . . . N3 N 0.2916(2) 0.5515(2) -0.4079(3) 0.0321(10) Uani 1 1 d . . . N4 N 0.3956(3) 0.5615(2) -0.1519(4) 0.0348(10) Uani 1 1 d . . . N5 N 0.1484(3) 0.5917(2) -0.0834(4) 0.0371(11) Uani 1 1 d . . . N6 N 0.2456(3) 0.5126(2) -0.6085(4) 0.0411(11) Uani 1 1 d . . . O3 O 0.2317(3) 0.3391(2) -0.0632(4) 0.0698(15) Uani 1 1 d D . . O4 O 0.5107(2) 0.3885(2) -0.4266(3) 0.0440(10) Uani 1 1 d . . . P1 P 0.31573(11) 0.69889(10) 0.05053(17) 0.0633(6) Uani 1 1 d . . . P2 P 0.23202(9) 0.40682(7) -0.12716(13) 0.0388(4) Uani 1 1 d . B . S1 S 0.31831(14) 0.60786(11) 0.10089(14) 0.0767(7) Uani 1 1 d . A . S2 S 0.30348(10) 0.70005(8) -0.10575(14) 0.0518(4) Uani 1 1 d . A . S3 S 0.26278(8) 0.46971(7) -0.01078(12) 0.0381(3) Uani 1 1 d . . . S4 S 0.12899(8) 0.42136(8) -0.20783(13) 0.0435(4) Uani 1 1 d . . . Ni1 Ni 0.27927(4) 0.57927(4) -0.07934(6) 0.0373(2) Uani 1 1 d . A . 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 C1A 0.068(7) 0.031(4) 0.034(5) 0.010(4) -0.001(5) -0.035(5) C2A 0.041(6) 0.038(6) 0.060(8) -0.018(5) 0.000(5) -0.001(5) C3A 0.065(11) 0.028(8) 0.085(12) -0.006(7) 0.005(8) -0.006(7) C4A 0.073(11) 0.038(9) 0.054(10) 0.007(7) -0.012(8) -0.002(8) C5A 0.045(6) 0.049(7) 0.066(8) 0.029(6) -0.008(6) -0.008(5) C6A 0.055(7) 0.045(6) 0.045(7) 0.017(5) -0.005(6) -0.003(5) C7A 0.083(12) 0.063(11) 0.141(18) 0.000(11) -0.072(12) -0.003(9) C8A 0.086(15) 0.061(12) 0.057(9) -0.010(8) -0.006(9) -0.011(11) C9A 0.056(8) 0.055(8) 0.082(11) -0.014(7) -0.029(8) -0.007(7) C10A 0.051(8) 0.052(9) 0.058(10) -0.027(7) -0.014(7) 0.001(8) C11A 0.058(8) 0.063(8) 0.123(13) -0.021(8) -0.009(8) -0.002(6) O1A 0.049(5) 0.078(7) 0.069(6) -0.017(5) -0.006(4) 0.008(5) O2A 0.054(6) 0.064(6) 0.123(10) 0.024(6) -0.033(6) -0.036(5) C1B 0.068(7) 0.031(4) 0.034(5) 0.010(4) -0.001(5) -0.035(5) C2B 0.072(9) 0.049(8) 0.031(7) -0.003(6) 0.000(7) -0.009(7) C3B 0.070(11) 0.055(10) 0.051(10) 0.004(7) -0.002(8) -0.022(8) C4B 0.10(2) 0.040(11) 0.077(15) -0.023(9) -0.004(13) -0.011(11) C5B 0.083(11) 0.042(8) 0.049(9) -0.006(6) 0.030(8) -0.017(7) C6B 0.070(14) 0.042(11) 0.071(14) -0.013(10) 0.032(11) -0.010(10) C7B 0.086(14) 0.075(13) 0.093(15) -0.020(11) 0.036(12) -0.022(11) C8B 0.076(12) 0.059(10) 0.058(11) 0.000(8) 0.025(9) -0.049(9) C9B 0.037(11) 0.047(11) 0.124(16) 0.005(12) -0.008(11) 0.004(8) C10B 0.105(16) 0.054(14) 0.12(2) 0.020(14) -0.013(16) -0.011(14) C11B 0.058(8) 0.063(8) 0.123(13) -0.021(8) -0.009(8) -0.002(6) O1B 0.095(9) 0.137(12) 0.046(7) 0.001(7) 0.001(6) -0.091(9) O2B 0.065(7) 0.067(7) 0.083(9) -0.014(6) 0.026(6) 0.005(6) C12 0.031(3) 0.026(2) 0.045(3) -0.001(2) -0.007(2) 0.000(2) C13 0.035(3) 0.034(3) 0.039(3) -0.001(2) -0.013(2) 0.004(2) C14 0.029(3) 0.035(3) 0.049(4) -0.007(3) -0.008(2) 0.003(2) C15 0.033(3) 0.032(3) 0.043(3) -0.009(2) 0.002(2) 0.001(2) C16 0.039(3) 0.042(3) 0.046(4) -0.010(3) -0.011(3) 0.000(3) C17 0.031(3) 0.039(3) 0.048(4) -0.003(3) -0.013(3) -0.001(2) C18 0.027(3) 0.057(4) 0.063(4) 0.002(3) 0.003(3) -0.002(3) C19A 0.068(6) 0.042(5) 0.076(7) 0.006(5) -0.011(5) -0.001(4) C20A 0.080(7) 0.047(5) 0.040(5) 0.013(4) -0.008(5) 0.005(5) C21A 0.087(8) 0.080(8) 0.058(7) 0.013(6) -0.005(6) -0.019(7) C22A 0.079(9) 0.046(6) 0.078(8) 0.013(6) 0.010(7) -0.018(6) C19B 0.061(14) 0.048(13) 0.111(18) 0.043(14) 0.022(14) -0.002(12) C20B 0.098(17) 0.041(13) 0.102(19) 0.049(14) -0.040(16) -0.007(13) C21B 0.071(15) 0.069(15) 0.085(17) 0.025(14) 0.009(14) 0.015(13) C22B 0.07(3) 0.06(2) 0.11(3) 0.02(2) -0.02(2) -0.01(2) C23 0.027(2) 0.034(3) 0.039(3) 0.006(2) -0.007(2) -0.004(2) C24 0.033(3) 0.032(3) 0.035(3) 0.002(2) -0.006(2) 0.000(2) C25 0.030(3) 0.032(3) 0.029(3) 0.001(2) -0.008(2) -0.002(2) C26 0.030(3) 0.031(3) 0.033(3) 0.003(2) -0.009(2) -0.004(2) C27 0.033(3) 0.033(3) 0.037(3) 0.005(2) -0.002(2) -0.002(2) C28 0.029(3) 0.037(3) 0.056(4) 0.007(3) -0.007(3) -0.001(2) C29 0.029(3) 0.039(3) 0.058(4) 0.011(3) -0.016(3) -0.006(2) C30 0.040(3) 0.041(3) 0.043(4) 0.009(3) -0.021(3) -0.007(3) C31 0.036(3) 0.038(3) 0.034(3) -0.004(2) -0.002(2) -0.003(2) C32 0.036(3) 0.044(3) 0.052(4) -0.002(3) 0.001(3) -0.002(3) C33 0.036(3) 0.053(4) 0.068(5) -0.001(3) 0.006(3) -0.003(3) C34 0.051(4) 0.040(3) 0.058(4) 0.004(3) 0.025(3) 0.002(3) C35 0.057(4) 0.036(3) 0.040(4) 0.000(3) 0.006(3) -0.003(3) C36 0.034(3) 0.034(3) 0.035(3) 0.001(2) -0.011(2) -0.004(2) C37 0.042(3) 0.051(4) 0.043(4) -0.002(3) -0.014(3) 0.009(3) C38 0.046(3) 0.048(4) 0.053(4) 0.004(3) -0.022(3) 0.007(3) C39 0.053(4) 0.044(3) 0.036(3) 0.004(3) -0.008(3) -0.007(3) C40 0.044(3) 0.060(4) 0.034(3) 0.005(3) -0.001(3) -0.010(3) N1 0.028(2) 0.037(2) 0.031(2) 0.0033(19) -0.0040(18) -0.0027(18) N2 0.031(2) 0.039(2) 0.037(3) 0.001(2) -0.009(2) 0.001(2) N3 0.028(2) 0.036(2) 0.031(3) 0.0057(19) -0.0059(18) -0.0022(19) N4 0.031(2) 0.040(2) 0.033(3) 0.006(2) -0.0095(19) -0.0106(19) N5 0.038(2) 0.036(2) 0.037(3) -0.001(2) 0.001(2) -0.004(2) N6 0.040(3) 0.054(3) 0.029(3) -0.001(2) -0.004(2) -0.004(2) O3 0.077(3) 0.049(3) 0.082(4) 0.025(3) -0.035(3) -0.025(2) O4 0.035(2) 0.052(2) 0.045(2) -0.006(2) -0.0007(18) 0.0017(18) P1 0.0527(10) 0.0742(13) 0.0619(13) -0.0254(10) -0.0227(9) 0.0011(9) P2 0.0312(7) 0.0386(8) 0.0462(9) 0.0061(7) -0.0070(6) -0.0059(6) S1 0.1021(15) 0.0980(15) 0.0298(9) -0.0002(9) -0.0046(9) -0.0622(13) S2 0.0553(9) 0.0419(8) 0.0581(11) -0.0014(8) -0.0042(8) -0.0076(7) S3 0.0317(7) 0.0467(8) 0.0356(8) 0.0061(6) -0.0044(6) -0.0045(6) S4 0.0261(6) 0.0527(9) 0.0516(10) -0.0014(7) -0.0060(6) -0.0045(6) Ni1 0.0345(4) 0.0456(4) 0.0315(4) 0.0020(3) -0.0051(3) -0.0092(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 C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C1A P1 1.885(6) . ? C2A C3A 1.3900 . ? C2A H2A 0.9500 . ? C3A C4A 1.3900 . ? C3A H3A 0.9500 . ? C4A C5A 1.3900 . ? C4A O2A 1.390(10) . ? C5A C6A 1.3900 . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A O2A 1.46(2) . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A O1A 1.442(18) . ? C8A C9A 1.586(19) . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9A C10A 1.442(17) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A C11A 1.523(19) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? O1A P1 1.628(9) . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C1B P1 1.904(8) . ? C2B C3B 1.3900 . ? C2B H2B 0.9500 . ? C3B C4B 1.3900 . ? C3B H3B 0.9500 . ? C4B C5B 1.3900 . ? C4B O2B 1.391(13) . ? C5B C6B 1.3900 . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B O2B 1.40(2) . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B O1B 1.367(18) . ? C8B C9B 1.587(19) . ? C8B H8B1 0.9900 . ? C8B H8B2 0.9900 . ? C9B C10B 1.441(17) . ? C9B H9B1 0.9900 . ? C9B H9B2 0.9900 . ? C10B C11B 1.53(2) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? O1B P1 1.523(11) . ? C12 C17 1.399(8) . ? C12 C13 1.404(7) . ? C12 P2 1.808(6) . ? C13 C14 1.375(8) . ? C13 H13 0.9500 . ? C14 C15 1.389(8) . ? C14 H14 0.9500 . ? C15 O4 1.364(6) . ? C15 C16 1.393(7) . ? C16 C17 1.375(8) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 O4 1.438(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19A O3 1.357(9) . ? C19A C20A 1.435(11) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A C21A 1.456(13) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A C22A 1.525(14) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C19B O3 1.295(16) . ? C19B C20B 1.433(12) . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? C20B C21B 1.453(14) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B C22B 1.524(14) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23 N2 1.326(7) . ? C23 N1 1.341(6) . ? C23 C31 1.468(8) . ? C24 N2 1.349(7) . ? C24 N3 1.349(6) . ? C24 C36 1.488(7) . ? C25 N1 1.321(7) . ? C25 N3 1.324(6) . ? C25 C26 1.487(7) . ? C26 N4 1.351(7) . ? C26 C27 1.377(7) . ? C27 C28 1.388(7) . ? C27 H27 0.9500 . ? C28 C29 1.373(8) . ? C28 H28 0.9500 . ? C29 C30 1.386(8) . ? C29 H29 0.9500 . ? C30 N4 1.343(6) . ? C30 H30 0.9500 . ? C31 N5 1.366(7) . ? C31 C32 1.387(7) . ? C32 C33 1.368(9) . ? C32 H32 0.9500 . ? C33 C34 1.380(9) . ? C33 H33 0.9500 . ? C34 C35 1.386(8) . ? C34 H34 0.9500 . ? C35 N5 1.325(7) . ? C35 H35 0.9500 . ? C36 N6 1.342(7) . ? C36 C37 1.386(7) . ? C37 C38 1.393(8) . ? C37 H37 0.9500 . ? C38 C39 1.368(9) . ? C38 H38 0.9500 . ? C39 C40 1.381(8) . ? C39 H39 0.9500 . ? C40 N6 1.340(7) . ? C40 H40 0.9500 . ? N1 Ni1 1.987(4) . ? N4 Ni1 2.152(5) . ? N5 Ni1 2.147(4) . ? O3 P2 1.613(5) . ? P1 S2 1.969(3) . ? P1 S1 1.983(3) . ? P2 S4 1.965(2) . ? P2 S3 2.010(2) . ? S1 Ni1 2.4115(18) . ? S2 Ni1 2.5471(18) . ? S3 Ni1 2.4369(16) . ? 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 C2A C1A C6A 120.0 . . ? C2A C1A P1 114.7(4) . . ? C6A C1A P1 124.9(4) . . ? C3A C2A C1A 120.0 . . ? C3A C2A H2A 120.0 . . ? C1A C2A H2A 120.0 . . ? C4A C3A C2A 120.0 . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C3A C4A C5A 120.0 . . ? C3A C4A O2A 123.1(8) . . ? C5A C4A O2A 116.9(8) . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A H6A 120.0 . . ? C1A C6A H6A 120.0 . . ? O1A C8A C9A 108.8(13) . . ? O1A C8A H8A1 109.9 . . ? C9A C8A H8A1 109.9 . . ? O1A C8A H8A2 109.9 . . ? C9A C8A H8A2 109.9 . . ? H8A1 C8A H8A2 108.3 . . ? C10A C9A C8A 109.5(12) . . ? C10A C9A H9A1 109.8 . . ? C8A C9A H9A1 109.8 . . ? C10A C9A H9A2 109.8 . . ? C8A C9A H9A2 109.8 . . ? H9A1 C9A H9A2 108.2 . . ? C9A C10A C11A 110.1(12) . . ? C9A C10A H10A 109.6 . . ? C11A C10A H10A 109.6 . . ? C9A C10A H10B 109.6 . . ? C11A C10A H10B 109.6 . . ? H10A C10A H10B 108.2 . . ? C8A O1A P1 120.6(11) . . ? C4A O2A C7A 116.4(12) . . ? C2B C1B C6B 120.0 . . ? C2B C1B P1 129.2(5) . . ? C6B C1B P1 110.7(5) . . ? C3B C2B C1B 120.0 . . ? C3B C2B H2B 120.0 . . ? C1B C2B H2B 120.0 . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3B 120.0 . . ? C4B C3B H3B 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B O2B 118.2(9) . . ? C3B C4B O2B 121.6(9) . . ? C4B C5B C6B 120.0 . . ? C4B C5B H5B 120.0 . . ? C6B C5B H5B 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B H6B 120.0 . . ? C1B C6B H6B 120.0 . . ? O2B C7B H7B1 109.5 . . ? O2B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? O2B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? O1B C8B C9B 108.2(12) . . ? O1B C8B H8B1 110.1 . . ? C9B C8B H8B1 110.1 . . ? O1B C8B H8B2 110.1 . . ? C9B C8B H8B2 110.1 . . ? H8B1 C8B H8B2 108.4 . . ? C10B C9B C8B 110.1(13) . . ? C10B C9B H9B1 109.6 . . ? C8B C9B H9B1 109.6 . . ? C10B C9B H9B2 109.6 . . ? C8B C9B H9B2 109.6 . . ? H9B1 C9B H9B2 108.1 . . ? C9B C10B C11B 109.4(13) . . ? C9B C10B H10C 109.8 . . ? C11B C10B H10C 109.8 . . ? C9B C10B H10D 109.8 . . ? C11B C10B H10D 109.8 . . ? H10C C10B H10D 108.2 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C8B O1B P1 120.6(11) . . ? C4B O2B C7B 120.7(14) . . ? C17 C12 C13 117.3(5) . . ? C17 C12 P2 122.1(4) . . ? C13 C12 P2 120.6(4) . . ? C14 C13 C12 121.7(5) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? O4 C15 C14 124.5(5) . . ? O4 C15 C16 116.0(5) . . ? C14 C15 C16 119.4(5) . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 121.3(5) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? 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 . . ? O3 C19A C20A 120.2(9) . . ? O3 C19A H19A 107.3 . . ? C20A C19A H19A 107.3 . . ? O3 C19A H19B 107.3 . . ? C20A C19A H19B 107.3 . . ? H19A C19A H19B 106.9 . . ? C19A C20A C21A 119.7(9) . . ? C19A C20A H20A 107.4 . . ? C21A C20A H20A 107.4 . . ? C19A C20A H20B 107.4 . . ? C21A C20A H20B 107.4 . . ? H20A C20A H20B 106.9 . . ? C20A C21A C22A 114.2(11) . . ? C20A C21A H21A 108.7 . . ? C22A C21A H21A 108.7 . . ? C20A C21A H21B 108.7 . . ? C22A C21A H21B 108.7 . . ? H21A C21A H21B 107.6 . . ? O3 C19B C20B 116.8(19) . . ? O3 C19B H19C 108.1 . . ? C20B C19B H19C 108.1 . . ? O3 C19B H19D 108.1 . . ? C20B C19B H19D 108.1 . . ? H19C C19B H19D 107.3 . . ? C19B C20B C21B 120.8(13) . . ? C19B C20B H20C 107.1 . . ? C21B C20B H20C 107.1 . . ? C19B C20B H20D 107.1 . . ? C21B C20B H20D 107.1 . . ? H20C C20B H20D 106.8 . . ? C20B C21B C22B 114.3(13) . . ? C20B C21B H21C 108.7 . . ? C22B C21B H21C 108.7 . . ? C20B C21B H21D 108.7 . . ? C22B C21B H21D 108.7 . . ? H21C C21B H21D 107.6 . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N2 C23 N1 123.4(5) . . ? N2 C23 C31 123.1(4) . . ? N1 C23 C31 113.5(5) . . ? N2 C24 N3 125.3(5) . . ? N2 C24 C36 117.1(4) . . ? N3 C24 C36 117.6(5) . . ? N1 C25 N3 124.6(4) . . ? N1 C25 C26 113.7(5) . . ? N3 C25 C26 121.7(5) . . ? N4 C26 C27 123.9(5) . . ? N4 C26 C25 113.7(5) . . ? C27 C26 C25 122.4(5) . . ? C26 C27 C28 117.6(5) . . ? C26 C27 H27 121.2 . . ? C28 C27 H27 121.2 . . ? C29 C28 C27 119.6(6) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 119.2(5) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? N4 C30 C29 122.4(6) . . ? N4 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N5 C31 C32 122.0(5) . . ? N5 C31 C23 114.8(5) . . ? C32 C31 C23 123.2(5) . . ? C33 C32 C31 118.2(6) . . ? C33 C32 H32 120.9 . . ? C31 C32 H32 120.9 . . ? C32 C33 C34 120.3(6) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 118.5(6) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? N5 C35 C34 122.5(6) . . ? N5 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? N6 C36 C37 123.4(5) . . ? N6 C36 C24 116.5(4) . . ? C37 C36 C24 120.0(5) . . ? C36 C37 C38 118.2(6) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C39 C38 C37 119.1(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 118.7(6) . . ? C38 C39 H39 120.7 . . ? C40 C39 H39 120.7 . . ? N6 C40 C39 123.8(6) . . ? N6 C40 H40 118.1 . . ? C39 C40 H40 118.1 . . ? C25 N1 C23 117.3(5) . . ? C25 N1 Ni1 121.7(3) . . ? C23 N1 Ni1 121.0(4) . . ? C23 N2 C24 114.9(4) . . ? C25 N3 C24 114.4(5) . . ? C30 N4 C26 117.3(5) . . ? C30 N4 Ni1 128.1(4) . . ? C26 N4 Ni1 114.6(3) . . ? C35 N5 C31 118.4(5) . . ? C35 N5 Ni1 127.8(4) . . ? C31 N5 Ni1 113.7(4) . . ? C40 N6 C36 116.8(5) . . ? C19B O3 C19A 72.2(14) . . ? C19B O3 P2 141.1(10) . . ? C19A O3 P2 122.0(5) . . ? C15 O4 C18 117.4(5) . . ? O1B P1 O1A 71.3(7) . . ? O1B P1 C1A 27.5(6) . . ? O1A P1 C1A 94.3(4) . . ? O1B P1 C1B 96.2(6) . . ? O1A P1 C1B 36.6(4) . . ? C1A P1 C1B 123.5(4) . . ? O1B P1 S2 127.2(5) . . ? O1A P1 S2 108.0(3) . . ? C1A P1 S2 106.4(3) . . ? C1B P1 S2 113.5(3) . . ? O1B P1 S1 111.2(6) . . ? O1A P1 S1 127.3(4) . . ? C1A P1 S1 109.2(3) . . ? C1B P1 S1 93.7(3) . . ? S2 P1 S1 109.31(11) . . ? O3 P2 C12 104.1(3) . . ? O3 P2 S4 112.18(18) . . ? C12 P2 S4 110.22(19) . . ? O3 P2 S3 101.6(2) . . ? C12 P2 S3 109.33(18) . . ? S4 P2 S3 118.23(10) . . ? P1 S1 Ni1 85.93(9) . . ? P1 S2 Ni1 82.58(9) . . ? P2 S3 Ni1 111.71(8) . . ? N1 Ni1 N5 76.99(17) . . ? N1 Ni1 N4 76.31(16) . . ? N5 Ni1 N4 153.30(17) . . ? N1 Ni1 S1 171.75(14) . . ? N5 Ni1 S1 103.57(14) . . ? N4 Ni1 S1 102.87(13) . . ? N1 Ni1 S3 102.59(13) . . ? N5 Ni1 S3 90.10(12) . . ? N4 Ni1 S3 95.54(12) . . ? S1 Ni1 S3 85.65(7) . . ? N1 Ni1 S2 90.72(13) . . ? N5 Ni1 S2 92.12(13) . . ? N4 Ni1 S2 88.35(12) . . ? S1 Ni1 S2 81.04(7) . . ? S3 Ni1 S2 166.66(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.143 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.090 # Attachment '_6.tptz_04slh048_88.cif' data_04slh048 _database_code_depnum_ccdc_archive 'CCDC 707535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 04slh048/88 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 N6 Ni O4 P2 S4' _chemical_formula_weight 741.47 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.770(2) _cell_length_b 13.0216(19) _cell_length_c 29.654(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.64(2) _cell_angle_gamma 90.00 _cell_volume 3379.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7142 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cut lath' _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7008 _exptl_absorpt_correction_T_max 0.9811 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; The values for minimum and maximum transmission are based on the cell dimensions only and were generated using the size command in SHELX. SADABS reports the ratio of minimum to maximum transmission as 0.489983. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27618 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7649 _reflns_number_gt 5272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0954P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7649 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _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 C1 C 0.7071(5) 0.7187(3) 0.89069(13) 0.0236(9) Uani 1 1 d . . . H1A H 0.6909 0.6465 0.8811 0.028 Uiso 1 1 calc R . . H1B H 0.7796 0.7192 0.9177 0.028 Uiso 1 1 calc R . . C2 C 0.7721(6) 0.7785(4) 0.85355(16) 0.0365(12) Uani 1 1 d . . . H2A H 0.7004 0.7773 0.8268 0.055 Uiso 1 1 calc R . . H2B H 0.8694 0.7478 0.8461 0.055 Uiso 1 1 calc R . . H2C H 0.7893 0.8496 0.8634 0.055 Uiso 1 1 calc R . . C3 C 0.2948(5) 0.8988(3) 0.93221(15) 0.0259(10) Uani 1 1 d . . . H3A H 0.3043 0.9085 0.8994 0.031 Uiso 1 1 calc R . . H3B H 0.3590 0.9507 0.9488 0.031 Uiso 1 1 calc R . . C4 C 0.1307(6) 0.9089(4) 0.9436(2) 0.0478(15) Uani 1 1 d . . . H4A H 0.0688 0.8570 0.9270 0.072 Uiso 1 1 calc R . . H4B H 0.0930 0.9775 0.9351 0.072 Uiso 1 1 calc R . . H4C H 0.1233 0.8988 0.9761 0.072 Uiso 1 1 calc R . . C5 C 0.7612(5) 0.6483(3) 1.21675(13) 0.0274(10) Uani 1 1 d . . . H5A H 0.6668 0.6078 1.2198 0.033 Uiso 1 1 calc R . . H5B H 0.7641 0.7040 1.2395 0.033 Uiso 1 1 calc R . . C6 C 0.8987(6) 0.5804(4) 1.22454(16) 0.0358(11) Uani 1 1 d . . . H6A H 0.8976 0.5275 1.2010 0.054 Uiso 1 1 calc R . . H6B H 0.8965 0.5477 1.2542 0.054 Uiso 1 1 calc R . . H6C H 0.9917 0.6218 1.2234 0.054 Uiso 1 1 calc R . . C7 C 0.5379(5) 0.9436(3) 1.16712(14) 0.0220(9) Uani 1 1 d . . . H7A H 0.5088 0.9533 1.1346 0.026 Uiso 1 1 calc R . . H7B H 0.6204 0.9929 1.1760 0.026 Uiso 1 1 calc R . . C8 C 0.4007(5) 0.9629(3) 1.19476(15) 0.0301(10) Uani 1 1 d . . . H8A H 0.3230 0.9101 1.1878 0.045 Uiso 1 1 calc R . . H8B H 0.3578 1.0308 1.1873 0.045 Uiso 1 1 calc R . . H8C H 0.4326 0.9602 1.2270 0.045 Uiso 1 1 calc R . . C9 C 0.5434(4) 0.5769(3) 1.11156(12) 0.0143(8) Uani 1 1 d . . . C10 C 0.6689(5) 0.4356(3) 1.13820(12) 0.0162(8) Uani 1 1 d . . . C11 C 0.7778(4) 0.5354(3) 1.08742(12) 0.0146(8) Uani 1 1 d . . . C12 C 0.9034(4) 0.5706(3) 1.05970(12) 0.0148(8) Uani 1 1 d . . . C13 C 1.0445(4) 0.5232(3) 1.06107(12) 0.0175(8) Uani 1 1 d . . . H13 H 1.0656 0.4650 1.0798 0.021 Uiso 1 1 calc R . . C14 C 1.1550(5) 0.5630(3) 1.03429(13) 0.0190(8) Uani 1 1 d . . . H14 H 1.2532 0.5322 1.0341 0.023 Uiso 1 1 calc R . . C15 C 1.1194(5) 0.6481(3) 1.00805(12) 0.0182(8) Uani 1 1 d . . . H15 H 1.1928 0.6765 0.9894 0.022 Uiso 1 1 calc R . . C16 C 0.9750(5) 0.6921(3) 1.00917(12) 0.0170(8) Uani 1 1 d . . . H16 H 0.9520 0.7511 0.9912 0.020 Uiso 1 1 calc R . . C17 C 0.4209(4) 0.6548(3) 1.10925(12) 0.0145(8) Uani 1 1 d . . . C18 C 0.2988(4) 0.6510(3) 1.13596(13) 0.0180(8) Uani 1 1 d . . . H18 H 0.2875 0.5959 1.1565 0.022 Uiso 1 1 calc R . . C20 C 0.2133(5) 0.8090(3) 1.10152(13) 0.0224(9) Uani 1 1 d . . . H20 H 0.1418 0.8638 1.0983 0.027 Uiso 1 1 calc R . . C21 C 0.3387(5) 0.8071(3) 1.07592(13) 0.0183(8) Uani 1 1 d . . . H21 H 0.3517 0.8610 1.0549 0.022 Uiso 1 1 calc R . . C22 C 0.6792(4) 0.3444(3) 1.16828(12) 0.0166(8) Uani 1 1 d . . . C23 C 0.7898(5) 0.2706(3) 1.16293(14) 0.0246(9) Uani 1 1 d . . . H23 H 0.8597 0.2771 1.1399 0.030 Uiso 1 1 calc R . . C24 C 0.7966(5) 0.1869(3) 1.19180(15) 0.0303(10) Uani 1 1 d . . . H24 H 0.8698 0.1342 1.1885 0.036 Uiso 1 1 calc R . . C25 C 0.6961(5) 0.1813(3) 1.22523(14) 0.0253(10) Uani 1 1 d . . . H25 H 0.6995 0.1253 1.2458 0.030 Uiso 1 1 calc R . . C26 C 0.5896(5) 0.2588(3) 1.22835(14) 0.0270(10) Uani 1 1 d . . . H26 H 0.5208 0.2546 1.2518 0.032 Uiso 1 1 calc R . . C190 C 0.1919(5) 0.7302(3) 1.13216(14) 0.0240(9) Uani 1 1 d . . . H190 H 0.1060 0.7303 1.1501 0.029 Uiso 1 1 calc R . . N1 N 0.6564(4) 0.5974(2) 1.08474(10) 0.0140(7) Uani 1 1 d . . . N2 N 0.5441(4) 0.4962(2) 1.13906(10) 0.0173(7) Uani 1 1 d . . . N3 N 0.7906(4) 0.4531(2) 1.11347(10) 0.0165(7) Uani 1 1 d . . . N4 N 0.8678(4) 0.6546(2) 1.03454(10) 0.0148(7) Uani 1 1 d . . . N5 N 0.4429(4) 0.7321(2) 1.07946(10) 0.0153(7) Uani 1 1 d . . . N6 N 0.5777(4) 0.3394(2) 1.20040(11) 0.0215(8) Uani 1 1 d . . . O1 O 0.5636(3) 0.7635(2) 0.90176(9) 0.0188(6) Uani 1 1 d . . . O2 O 0.3417(3) 0.79494(19) 0.94597(9) 0.0184(6) Uani 1 1 d . . . O3 O 0.7614(3) 0.6919(2) 1.17138(8) 0.0211(6) Uani 1 1 d . . . O4 O 0.5912(3) 0.8392(2) 1.17519(9) 0.0196(6) Uani 1 1 d . . . P1 P 0.51531(12) 0.76160(7) 0.95271(3) 0.0154(2) Uani 1 1 d . . . P2 P 0.76319(12) 0.81294(8) 1.16379(3) 0.0169(2) Uani 1 1 d . . . S1 S 0.52114(11) 0.62262(7) 0.97972(3) 0.0166(2) Uani 1 1 d . . . S2 S 0.64034(12) 0.85893(7) 0.99144(3) 0.0191(2) Uani 1 1 d . . . S3 S 0.79094(12) 0.83568(7) 1.09839(3) 0.0177(2) Uani 1 1 d . . . S4 S 0.91175(13) 0.88457(9) 1.20447(4) 0.0275(3) Uani 1 1 d . . . Ni1 Ni 0.65081(6) 0.72103(3) 1.046360(15) 0.01364(14) 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 C1 0.020(2) 0.031(2) 0.0196(19) 0.0007(17) 0.0052(17) 0.0087(19) C2 0.025(3) 0.052(3) 0.033(2) 0.010(2) 0.007(2) -0.002(2) C3 0.024(2) 0.020(2) 0.033(2) 0.0102(18) -0.0003(19) 0.0026(18) C4 0.025(3) 0.028(3) 0.092(4) 0.026(3) 0.014(3) 0.006(2) C5 0.039(3) 0.025(2) 0.0175(19) 0.0070(17) -0.0009(19) 0.004(2) C6 0.038(3) 0.037(3) 0.031(2) 0.005(2) -0.009(2) 0.008(2) C7 0.023(2) 0.0159(19) 0.026(2) -0.0018(16) 0.0012(18) 0.0060(17) C8 0.029(3) 0.030(2) 0.032(2) -0.0012(19) 0.008(2) 0.009(2) C9 0.0113(19) 0.0185(18) 0.0131(17) -0.0030(14) 0.0000(15) -0.0016(16) C10 0.017(2) 0.0167(18) 0.0146(17) -0.0023(14) 0.0000(16) 0.0005(16) C11 0.013(2) 0.0150(18) 0.0150(17) -0.0032(14) -0.0027(15) 0.0018(15) C12 0.014(2) 0.0164(18) 0.0132(17) -0.0035(14) -0.0016(15) -0.0014(16) C13 0.016(2) 0.0175(19) 0.0184(18) -0.0038(15) -0.0048(16) 0.0058(16) C14 0.013(2) 0.024(2) 0.0213(19) -0.0079(16) 0.0037(16) -0.0007(17) C15 0.016(2) 0.023(2) 0.0166(18) -0.0036(15) 0.0033(16) -0.0038(17) C16 0.016(2) 0.0138(18) 0.0209(19) 0.0005(15) 0.0001(16) -0.0061(16) C17 0.0110(19) 0.0166(18) 0.0157(17) -0.0043(14) -0.0013(15) 0.0003(15) C18 0.014(2) 0.0211(19) 0.0192(19) -0.0008(15) 0.0021(16) 0.0000(16) C20 0.019(2) 0.023(2) 0.025(2) -0.0053(17) -0.0021(18) 0.0088(18) C21 0.017(2) 0.0169(19) 0.0211(19) -0.0006(15) 0.0005(17) 0.0046(16) C22 0.015(2) 0.0171(19) 0.0177(18) -0.0005(15) -0.0035(16) -0.0022(16) C23 0.026(2) 0.021(2) 0.026(2) 0.0039(17) 0.0005(19) 0.0021(18) C24 0.030(3) 0.025(2) 0.035(2) 0.0088(19) -0.004(2) 0.007(2) C25 0.032(3) 0.018(2) 0.025(2) 0.0060(17) -0.0049(19) -0.0054(19) C26 0.032(3) 0.025(2) 0.024(2) 0.0055(17) 0.0044(19) -0.003(2) C190 0.018(2) 0.027(2) 0.027(2) -0.0056(17) 0.0040(18) 0.0037(18) N1 0.0140(17) 0.0132(15) 0.0148(14) -0.0013(12) 0.0006(13) 0.0013(13) N2 0.0198(19) 0.0173(16) 0.0146(15) 0.0021(13) -0.0002(14) -0.0030(14) N3 0.0175(18) 0.0146(16) 0.0174(15) -0.0005(12) 0.0008(14) -0.0023(13) N4 0.0160(17) 0.0154(15) 0.0128(14) -0.0026(12) -0.0014(13) -0.0014(13) N5 0.0110(16) 0.0182(16) 0.0166(15) -0.0019(12) -0.0003(13) 0.0010(13) N6 0.025(2) 0.0217(17) 0.0188(16) 0.0049(14) 0.0053(15) -0.0004(15) O1 0.0164(15) 0.0242(14) 0.0159(13) 0.0028(11) 0.0020(11) 0.0026(12) O2 0.0157(15) 0.0155(13) 0.0238(14) 0.0057(11) -0.0009(12) 0.0000(11) O3 0.0281(17) 0.0188(14) 0.0160(13) 0.0006(11) -0.0035(12) 0.0034(13) O4 0.0173(15) 0.0208(14) 0.0211(14) -0.0009(11) 0.0049(12) 0.0027(12) P1 0.0162(5) 0.0150(5) 0.0148(5) 0.0021(4) -0.0006(4) 0.0002(4) P2 0.0174(6) 0.0170(5) 0.0160(5) -0.0026(4) -0.0007(4) 0.0007(4) S1 0.0181(5) 0.0133(4) 0.0180(4) 0.0003(3) -0.0008(4) 0.0005(4) S2 0.0232(6) 0.0153(5) 0.0183(5) 0.0020(4) -0.0030(4) -0.0036(4) S3 0.0195(5) 0.0173(5) 0.0164(4) -0.0018(4) 0.0014(4) -0.0023(4) S4 0.0233(6) 0.0340(6) 0.0246(5) -0.0135(5) -0.0031(5) -0.0027(5) Ni1 0.0135(3) 0.0135(2) 0.0139(2) 0.00091(18) 0.00070(19) 0.0006(2) _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 C1 O1 1.443(5) . ? C1 C2 1.491(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O2 1.465(5) . ? C3 C4 1.505(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O3 1.461(5) . ? C5 C6 1.501(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O4 1.452(4) . ? C7 C8 1.519(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N2 1.330(5) . ? C9 N1 1.337(5) . ? C9 C17 1.476(5) . ? C10 N2 1.351(5) . ? C10 N3 1.352(5) . ? C10 C22 1.485(5) . ? C11 N3 1.322(5) . ? C11 N1 1.334(5) . ? C11 C12 1.488(5) . ? C12 N4 1.350(5) . ? C12 C13 1.382(5) . ? C13 C14 1.392(6) . ? C13 H13 0.9500 . ? C14 C15 1.378(6) . ? C14 H14 0.9500 . ? C15 C16 1.393(6) . ? C15 H15 0.9500 . ? C16 N4 1.334(5) . ? C16 H16 0.9500 . ? C17 N5 1.362(5) . ? C17 C18 1.373(5) . ? C18 C190 1.394(6) . ? C18 H18 0.9500 . ? C20 C21 1.376(6) . ? C20 C190 1.392(6) . ? C20 H20 0.9500 . ? C21 N5 1.337(5) . ? C21 H21 0.9500 . ? C22 N6 1.346(5) . ? C22 C23 1.382(6) . ? C23 C24 1.384(6) . ? C23 H23 0.9500 . ? C24 C25 1.370(7) . ? C24 H24 0.9500 . ? C25 C26 1.382(6) . ? C25 H25 0.9500 . ? C26 N6 1.337(5) . ? C26 H26 0.9500 . ? C190 H190 0.9500 . ? N1 Ni1 1.970(3) . ? N4 Ni1 2.139(3) . ? N5 Ni1 2.130(3) . ? O1 P1 1.595(3) . ? O2 P1 1.583(3) . ? O3 P2 1.592(3) . ? O4 P2 1.603(3) . ? P1 S1 1.9785(13) . ? P1 S2 1.9919(14) . ? P2 S4 1.9553(15) . ? P2 S3 1.9920(14) . ? S1 Ni1 2.5602(11) . ? S2 Ni1 2.4219(11) . ? S3 Ni1 2.4246(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 109.7(4) . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C4 105.9(3) . . ? O2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 108.8(4) . . ? O3 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? O3 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? 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 . . ? O4 C7 C8 108.9(3) . . ? O4 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 N1 123.2(3) . . ? N2 C9 C17 123.1(3) . . ? N1 C9 C17 113.6(3) . . ? N2 C10 N3 125.5(3) . . ? N2 C10 C22 118.3(3) . . ? N3 C10 C22 116.2(3) . . ? N3 C11 N1 124.3(4) . . ? N3 C11 C12 122.2(3) . . ? N1 C11 C12 113.4(3) . . ? N4 C12 C13 123.6(4) . . ? N4 C12 C11 113.6(3) . . ? C13 C12 C11 122.7(3) . . ? C12 C13 C14 118.1(4) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C15 C14 C13 118.8(4) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? N4 C16 C15 122.5(4) . . ? N4 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? N5 C17 C18 123.3(3) . . ? N5 C17 C9 113.9(3) . . ? C18 C17 C9 122.7(3) . . ? C17 C18 C190 118.2(4) . . ? C17 C18 H18 120.9 . . ? C190 C18 H18 120.9 . . ? C21 C20 C190 119.5(4) . . ? C21 C20 H20 120.3 . . ? C190 C20 H20 120.3 . . ? N5 C21 C20 122.5(4) . . ? N5 C21 H21 118.7 . . ? C20 C21 H21 118.7 . . ? N6 C22 C23 123.2(4) . . ? N6 C22 C10 116.5(3) . . ? C23 C22 C10 120.3(4) . . ? C22 C23 C24 118.6(4) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? C25 C24 C23 119.0(4) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 118.5(4) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? N6 C26 C25 123.9(4) . . ? N6 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? C20 C190 C18 118.7(4) . . ? C20 C190 H190 120.6 . . ? C18 C190 H190 120.6 . . ? C11 N1 C9 117.6(3) . . ? C11 N1 Ni1 121.3(3) . . ? C9 N1 Ni1 121.0(3) . . ? C9 N2 C10 114.9(3) . . ? C11 N3 C10 114.4(3) . . ? C16 N4 C12 117.5(3) . . ? C16 N4 Ni1 127.6(3) . . ? C12 N4 Ni1 114.5(3) . . ? C21 N5 C17 117.8(3) . . ? C21 N5 Ni1 127.9(3) . . ? C17 N5 Ni1 114.2(2) . . ? C26 N6 C22 116.6(4) . . ? C1 O1 P1 119.8(2) . . ? C3 O2 P1 122.6(2) . . ? C5 O3 P2 121.1(2) . . ? C7 O4 P2 117.5(2) . . ? O2 P1 O1 100.80(15) . . ? O2 P1 S1 107.56(11) . . ? O1 P1 S1 113.32(11) . . ? O2 P1 S2 112.83(11) . . ? O1 P1 S2 111.52(12) . . ? S1 P1 S2 110.45(6) . . ? O3 P2 O4 99.41(16) . . ? O3 P2 S4 113.40(11) . . ? O4 P2 S4 111.53(11) . . ? O3 P2 S3 106.72(11) . . ? O4 P2 S3 110.38(11) . . ? S4 P2 S3 114.32(7) . . ? P1 S1 Ni1 81.57(4) . . ? P1 S2 Ni1 84.95(5) . . ? P2 S3 Ni1 116.08(6) . . ? N1 Ni1 N5 77.29(13) . . ? N1 Ni1 N4 76.95(13) . . ? N5 Ni1 N4 154.06(12) . . ? N1 Ni1 S2 173.04(9) . . ? N5 Ni1 S2 105.22(9) . . ? N4 Ni1 S2 100.71(9) . . ? N1 Ni1 S3 98.19(9) . . ? N5 Ni1 S3 94.53(9) . . ? N4 Ni1 S3 86.17(9) . . ? S2 Ni1 S3 88.13(4) . . ? N1 Ni1 S1 91.74(9) . . ? N5 Ni1 S1 92.20(9) . . ? N4 Ni1 S1 91.56(8) . . ? S2 Ni1 S1 81.73(4) . . ? S3 Ni1 S1 169.02(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.847 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.172 # Attachment '_7_04slh037.cif' data_04slh037 _database_code_depnum_ccdc_archive 'CCDC 707536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 04slh037/100 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H26 N7 Ni O6 P S2' _chemical_formula_weight 698.35 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.578(3) _cell_length_b 11.808(4) _cell_length_c 13.972(7) _cell_angle_alpha 113.89(4) _cell_angle_beta 104.80(3) _cell_angle_gamma 96.21(2) _cell_volume 1498.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6289 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.10 _exptl_crystal_description 'cut needle' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8274 _exptl_absorpt_correction_T_max 0.9911 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; The values for minimum and maximum transmission are based on the cell dimensions only and were generated using the size command in SHELX. SADABS reports the ratio of minimum to maximum transmission as 0.392855. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26049 _diffrn_reflns_av_R_equivalents 0.2524 _diffrn_reflns_av_sigmaI/netI 0.1868 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5259 _reflns_number_gt 3160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The crystals were of poor quality and very small. The diffraction was very weak at high angles, hence merging of the data resulted in an abnormally high Rint. However, the connectivity of the compound could be establish unambigiously. Searches for better crystals were not successful. ; _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^)+(0.0657P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0064(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5259 _refine_ls_number_parameters 400 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1419 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.939 _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 C1 C -0.1606(5) 0.0627(6) 0.2541(4) 0.0214(13) Uani 1 1 d . . . C2 C -0.2245(5) -0.0508(6) 0.1610(5) 0.0265(14) Uani 1 1 d . . . H2 H -0.2506 -0.0513 0.0906 0.032 Uiso 1 1 calc R . . C3 C -0.2521(5) -0.1649(6) 0.1672(5) 0.0268(14) Uani 1 1 d . . . H3 H -0.2966 -0.2423 0.1018 0.032 Uiso 1 1 calc R . . C4 C -0.2136(5) -0.1646(6) 0.2703(5) 0.0269(14) Uani 1 1 d . . . C5 C -0.1471(6) -0.0491(6) 0.3661(5) 0.0283(15) Uani 1 1 d . . . H5 H -0.1211 -0.0483 0.4367 0.034 Uiso 1 1 calc R . . C6 C -0.1194(5) 0.0627(6) 0.3579(5) 0.0261(14) Uani 1 1 d . . . H6 H -0.0724 0.1400 0.4227 0.031 Uiso 1 1 calc R . . C7 C -0.3220(7) -0.3815(7) 0.1940(6) 0.0430(17) Uani 1 1 d . . . H7A H -0.4067 -0.3629 0.1630 0.065 Uiso 1 1 calc R . . H7B H -0.3408 -0.4481 0.2168 0.065 Uiso 1 1 calc R . . H7C H -0.2778 -0.4112 0.1377 0.065 Uiso 1 1 calc R . . C8 C -0.3079(5) 0.2964(6) 0.1382(5) 0.0306(14) Uani 1 1 d . . . H8A H -0.2542 0.3019 0.0910 0.037 Uiso 1 1 calc R . . H8B H -0.2814 0.3795 0.2053 0.037 Uiso 1 1 calc R . . C9 C -0.4555(5) 0.2667(7) 0.0757(5) 0.0347(16) Uani 1 1 d . . . H9A H -0.4831 0.1805 0.0141 0.052 Uiso 1 1 calc R . . H9B H -0.4723 0.3285 0.0467 0.052 Uiso 1 1 calc R . . H9C H -0.5074 0.2717 0.1256 0.052 Uiso 1 1 calc R . . C10 C 0.2502(5) 0.6562(6) 0.4526(4) 0.0176(12) Uani 1 1 d . . . C11 C 0.4144(5) 0.7471(5) 0.6186(4) 0.0189(12) Uani 1 1 d . . . C12 C 0.3396(5) 0.5341(6) 0.5313(4) 0.0188(12) Uani 1 1 d . . . C13 C 0.3376(5) 0.4016(5) 0.5142(4) 0.0176(12) Uani 1 1 d . . . C14 C 0.4256(5) 0.3726(6) 0.5885(4) 0.0227(13) Uani 1 1 d . . . H14 H 0.4906 0.4384 0.6541 0.027 Uiso 1 1 calc R . . C15 C 0.4167(5) 0.2462(5) 0.5653(5) 0.0204(12) Uani 1 1 d . . . H15 H 0.4760 0.2236 0.6146 0.024 Uiso 1 1 calc R . . C16 C 0.3213(5) 0.1537(6) 0.4702(5) 0.0247(13) Uani 1 1 d . . . H16 H 0.3130 0.0663 0.4534 0.030 Uiso 1 1 calc R . . C17 C 0.2361(5) 0.1890(6) 0.3980(4) 0.0230(13) Uani 1 1 d . . . H17 H 0.1698 0.1243 0.3325 0.028 Uiso 1 1 calc R . . C18 C 0.1578(5) 0.6548(6) 0.3519(4) 0.0193(12) Uani 1 1 d . . . C19 C 0.1487(5) 0.7652(6) 0.3414(4) 0.0218(12) Uani 1 1 d . . . H19 H 0.1963 0.8465 0.4009 0.026 Uiso 1 1 calc R . . C20 C 0.0675(5) 0.7535(6) 0.2409(5) 0.0286(14) Uani 1 1 d . . . H20 H 0.0581 0.8271 0.2303 0.034 Uiso 1 1 calc R . . C21 C 0.0010(5) 0.6335(6) 0.1568(5) 0.0254(13) Uani 1 1 d . . . H21 H -0.0539 0.6234 0.0871 0.030 Uiso 1 1 calc R . . C22 C 0.0146(5) 0.5278(6) 0.1745(4) 0.0201(12) Uani 1 1 d . . . H22 H -0.0329 0.4457 0.1161 0.024 Uiso 1 1 calc R . . C23 C 0.5118(5) 0.8637(6) 0.7105(4) 0.0197(12) Uani 1 1 d . . . C24 C 0.4989(5) 0.9838(6) 0.7214(5) 0.0236(13) Uani 1 1 d . . . H24 H 0.4226 0.9923 0.6737 0.028 Uiso 1 1 calc R . . C25 C 0.5975(5) 1.0910(6) 0.8019(5) 0.0303(14) Uani 1 1 d . . . H25 H 0.5908 1.1740 0.8106 0.036 Uiso 1 1 calc R . . C26 C 0.7066(5) 1.0727(6) 0.8693(5) 0.0281(14) Uani 1 1 d . . . H26 H 0.7774 1.1435 0.9245 0.034 Uiso 1 1 calc R . . C27 C 0.7112(5) 0.9504(6) 0.8555(4) 0.0225(13) Uani 1 1 d . . . H27 H 0.7860 0.9400 0.9031 0.027 Uiso 1 1 calc R . . N1 N 0.2502(4) 0.5399(4) 0.4467(3) 0.0181(10) Uani 1 1 d . . . N2 N 0.3302(4) 0.7633(5) 0.5371(3) 0.0178(10) Uani 1 1 d . . . N3 N 0.4230(4) 0.6341(5) 0.6193(3) 0.0200(10) Uani 1 1 d . . . N4 N 0.2451(4) 0.3103(4) 0.4181(3) 0.0179(10) Uani 1 1 d . . . N5 N 0.0924(4) 0.5364(5) 0.2712(4) 0.0216(11) Uani 1 1 d . . . N6 N 0.6160(4) 0.8462(4) 0.7786(4) 0.0185(10) Uani 1 1 d . . . O1 O -0.2826(3) 0.1957(4) 0.1697(3) 0.0216(9) Uani 1 1 d . . . O2 O -0.2360(4) -0.2689(4) 0.2876(3) 0.0362(11) Uani 1 1 d . . . O3 O 0.2932(3) 0.3804(4) 0.2488(3) 0.0200(8) Uani 1 1 d D . . H3A H 0.3134 0.3063 0.2361 0.030 Uiso 1 1 d D . . H3B H 0.2888 0.4013 0.1925 0.030 Uiso 1 1 d D . . P1 P -0.13124(13) 0.20642(15) 0.23819(11) 0.0203(3) Uani 1 1 d . . . S1 S -0.00709(13) 0.19822(15) 0.14942(11) 0.0227(3) Uani 1 1 d . . . S2 S -0.05747(13) 0.36484(15) 0.38063(11) 0.0237(3) Uani 1 1 d . . . Ni1 Ni 0.13618(6) 0.38478(7) 0.31197(5) 0.0178(2) Uani 1 1 d . . . N7 N 0.2934(4) 0.5508(5) 0.1058(4) 0.0219(11) Uani 1 1 d . . . O4 O 0.3541(4) 0.6223(4) 0.2059(3) 0.0296(9) Uani 1 1 d . . . O5 O 0.2593(4) 0.4322(4) 0.0718(3) 0.0288(9) Uani 1 1 d . . . O6 O 0.2646(4) 0.5961(4) 0.0379(3) 0.0368(11) 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 C1 0.010(3) 0.032(4) 0.021(3) 0.013(3) 0.005(2) 0.002(2) C2 0.025(3) 0.033(4) 0.020(3) 0.013(3) 0.003(3) 0.009(3) C3 0.024(3) 0.029(4) 0.027(3) 0.014(3) 0.004(3) 0.005(3) C4 0.025(3) 0.030(4) 0.037(4) 0.019(3) 0.021(3) 0.013(3) C5 0.033(3) 0.035(4) 0.035(4) 0.027(3) 0.018(3) 0.018(3) C6 0.020(3) 0.040(4) 0.017(3) 0.012(3) 0.006(2) 0.010(3) C7 0.059(4) 0.025(4) 0.056(5) 0.020(4) 0.034(4) 0.013(4) C8 0.027(3) 0.029(4) 0.035(4) 0.019(3) 0.002(3) 0.006(3) C9 0.023(3) 0.044(5) 0.039(4) 0.025(4) 0.003(3) 0.004(3) C10 0.010(2) 0.023(4) 0.018(3) 0.008(3) 0.002(2) 0.003(2) C11 0.015(3) 0.023(4) 0.023(3) 0.012(3) 0.008(2) 0.006(2) C12 0.020(3) 0.026(4) 0.016(3) 0.013(3) 0.009(3) 0.006(2) C13 0.015(3) 0.023(3) 0.016(3) 0.008(3) 0.009(2) 0.004(2) C14 0.023(3) 0.031(4) 0.017(3) 0.013(3) 0.007(2) 0.008(3) C15 0.022(3) 0.016(3) 0.028(3) 0.013(3) 0.009(3) 0.007(2) C16 0.028(3) 0.025(4) 0.030(3) 0.017(3) 0.014(3) 0.010(3) C17 0.021(3) 0.028(4) 0.020(3) 0.008(3) 0.010(2) 0.003(3) C18 0.012(3) 0.025(4) 0.023(3) 0.012(3) 0.006(2) 0.006(2) C19 0.019(3) 0.021(4) 0.020(3) 0.005(3) 0.005(2) 0.004(2) C20 0.023(3) 0.036(4) 0.035(4) 0.023(3) 0.009(3) 0.012(3) C21 0.016(3) 0.034(4) 0.021(3) 0.013(3) 0.001(3) 0.001(3) C22 0.014(3) 0.023(4) 0.020(3) 0.011(3) -0.001(2) 0.000(2) C23 0.013(3) 0.025(4) 0.021(3) 0.009(3) 0.006(2) 0.003(2) C24 0.020(3) 0.025(4) 0.026(3) 0.012(3) 0.008(3) 0.008(3) C25 0.028(3) 0.029(4) 0.029(4) 0.011(3) 0.004(3) 0.005(3) C26 0.023(3) 0.032(4) 0.027(3) 0.011(3) 0.008(3) 0.003(3) C27 0.015(3) 0.032(4) 0.017(3) 0.009(3) 0.003(2) 0.005(3) N1 0.015(2) 0.022(3) 0.020(3) 0.012(2) 0.005(2) 0.006(2) N2 0.015(2) 0.022(3) 0.016(2) 0.008(2) 0.005(2) 0.006(2) N3 0.016(2) 0.027(3) 0.013(2) 0.009(2) 0.000(2) 0.005(2) N4 0.018(2) 0.017(3) 0.015(2) 0.004(2) 0.005(2) 0.003(2) N5 0.014(2) 0.029(3) 0.022(3) 0.011(2) 0.006(2) 0.004(2) N6 0.017(2) 0.019(3) 0.019(3) 0.008(2) 0.005(2) 0.005(2) O1 0.0148(18) 0.026(2) 0.026(2) 0.016(2) 0.0013(16) 0.0041(16) O2 0.054(3) 0.026(3) 0.038(3) 0.018(2) 0.023(2) 0.012(2) O3 0.0200(18) 0.023(2) 0.023(2) 0.0145(19) 0.0079(16) 0.0074(17) P1 0.0155(7) 0.0236(9) 0.0194(8) 0.0094(7) 0.0038(6) 0.0017(6) S1 0.0187(7) 0.0265(9) 0.0185(7) 0.0074(7) 0.0050(6) 0.0023(6) S2 0.0205(7) 0.0243(9) 0.0209(8) 0.0055(7) 0.0076(6) 0.0006(6) Ni1 0.0152(4) 0.0203(5) 0.0157(4) 0.0078(3) 0.0031(3) 0.0017(3) N7 0.019(2) 0.024(3) 0.023(3) 0.013(3) 0.005(2) 0.005(2) O4 0.032(2) 0.029(3) 0.017(2) 0.008(2) -0.0012(19) 0.0009(19) O5 0.037(2) 0.024(3) 0.019(2) 0.009(2) 0.0019(18) 0.0031(19) O6 0.049(3) 0.037(3) 0.024(2) 0.021(2) 0.003(2) 0.004(2) _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 C1 C2 1.374(8) . ? C1 C6 1.404(7) . ? C1 P1 1.804(6) . ? C2 C3 1.389(8) . ? C2 H2 0.9500 . ? C3 C4 1.391(7) . ? C3 H3 0.9500 . ? C4 O2 1.356(7) . ? C4 C5 1.406(9) . ? C5 C6 1.377(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O2 1.425(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.453(6) . ? C8 C9 1.503(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N2 1.326(7) . ? C10 N1 1.342(7) . ? C10 C18 1.487(7) . ? C11 N2 1.350(6) . ? C11 N3 1.350(7) . ? C11 C23 1.481(8) . ? C12 N3 1.315(7) . ? C12 N1 1.343(6) . ? C12 C13 1.481(8) . ? C13 N4 1.360(7) . ? C13 C14 1.388(6) . ? C14 C15 1.380(8) . ? C14 H14 0.9500 . ? C15 C16 1.371(8) . ? C15 H15 0.9500 . ? C16 C17 1.401(7) . ? C16 H16 0.9500 . ? C17 N4 1.331(7) . ? C17 H17 0.9500 . ? C18 N5 1.349(8) . ? C18 C19 1.381(7) . ? C19 C20 1.389(7) . ? C19 H19 0.9500 . ? C20 C21 1.377(9) . ? C20 H20 0.9500 . ? C21 C22 1.382(7) . ? C21 H21 0.9500 . ? C22 N5 1.348(6) . ? C22 H22 0.9500 . ? C23 N6 1.354(6) . ? C23 C24 1.389(7) . ? C24 C25 1.385(9) . ? C24 H24 0.9500 . ? C25 C26 1.389(7) . ? C25 H25 0.9500 . ? C26 C27 1.385(8) . ? C26 H26 0.9500 . ? C27 N6 1.339(7) . ? C27 H27 0.9500 . ? N1 Ni1 1.981(5) . ? N4 Ni1 2.169(4) . ? N5 Ni1 2.148(4) . ? O1 P1 1.603(3) . ? O3 Ni1 2.067(3) . ? O3 H3A 0.8813 . ? O3 H3B 0.9077 . ? P1 S2 1.986(3) . ? P1 S1 2.0087(17) . ? S1 Ni1 2.403(2) . ? S2 Ni1 2.5009(15) . ? N7 O4 1.244(6) . ? N7 O6 1.255(5) . ? N7 O5 1.257(6) . ? 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 C2 C1 C6 119.0(5) . . ? C2 C1 P1 118.7(4) . . ? C6 C1 P1 122.3(5) . . ? C1 C2 C3 121.8(5) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? O2 C4 C3 125.0(6) . . ? O2 C4 C5 115.5(5) . . ? C3 C4 C5 119.5(5) . . ? C6 C5 C4 120.3(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 120.1(6) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1 C8 C9 108.7(5) . . ? O1 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? O1 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 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 . . ? N2 C10 N1 123.9(4) . . ? N2 C10 C18 122.0(5) . . ? N1 C10 C18 113.9(5) . . ? N2 C11 N3 125.8(5) . . ? N2 C11 C23 116.0(5) . . ? N3 C11 C23 118.0(4) . . ? N3 C12 N1 124.4(5) . . ? N3 C12 C13 122.8(4) . . ? N1 C12 C13 112.8(5) . . ? N4 C13 C14 122.6(5) . . ? N4 C13 C12 114.6(4) . . ? C14 C13 C12 122.8(5) . . ? C15 C14 C13 118.7(6) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N4 C17 C16 122.1(6) . . ? N4 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? N5 C18 C19 124.2(5) . . ? N5 C18 C10 113.6(5) . . ? C19 C18 C10 122.0(6) . . ? C18 C19 C20 117.8(6) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 119.5(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? N5 C22 C21 122.7(6) . . ? N5 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? N6 C23 C24 122.6(5) . . ? N6 C23 C11 116.6(5) . . ? C24 C23 C11 120.8(4) . . ? C25 C24 C23 119.9(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 117.5(6) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? C27 C26 C25 119.5(6) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? N6 C27 C26 123.5(5) . . ? N6 C27 H27 118.3 . . ? C26 C27 H27 118.3 . . ? C12 N1 C10 116.7(5) . . ? C12 N1 Ni1 122.2(4) . . ? C10 N1 Ni1 120.7(3) . . ? C10 N2 C11 114.6(5) . . ? C12 N3 C11 114.6(4) . . ? C17 N4 C13 117.9(4) . . ? C17 N4 Ni1 128.1(4) . . ? C13 N4 Ni1 113.9(3) . . ? C22 N5 C18 116.7(5) . . ? C22 N5 Ni1 128.4(4) . . ? C18 N5 Ni1 114.8(3) . . ? C27 N6 C23 117.0(5) . . ? C8 O1 P1 118.0(3) . . ? C4 O2 C7 115.7(5) . . ? Ni1 O3 H3A 106.7 . . ? Ni1 O3 H3B 120.6 . . ? H3A O3 H3B 113.3 . . ? O1 P1 C1 98.6(2) . . ? O1 P1 S2 112.63(16) . . ? C1 P1 S2 113.97(19) . . ? O1 P1 S1 111.66(14) . . ? C1 P1 S1 110.99(16) . . ? S2 P1 S1 108.79(9) . . ? P1 S1 Ni1 84.97(8) . . ? P1 S2 Ni1 82.85(7) . . ? N1 Ni1 O3 88.71(15) . . ? N1 Ni1 N5 76.93(17) . . ? O3 Ni1 N5 88.93(13) . . ? N1 Ni1 N4 76.29(17) . . ? O3 Ni1 N4 87.92(13) . . ? N5 Ni1 N4 153.10(19) . . ? N1 Ni1 S1 178.56(11) . . ? O3 Ni1 S1 92.60(12) . . ? N5 Ni1 S1 102.49(14) . . ? N4 Ni1 S1 104.34(14) . . ? N1 Ni1 S2 95.81(12) . . ? O3 Ni1 S2 173.89(11) . . ? N5 Ni1 S2 96.09(11) . . ? N4 Ni1 S2 89.15(11) . . ? S1 Ni1 S2 82.93(6) . . ? O4 N7 O6 120.5(5) . . ? O4 N7 O5 120.2(4) . . ? O6 N7 O5 119.3(5) . . ? 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 O3 H3A N6 0.88 1.98 2.854(5) 172.1 2_666 O3 H3B O5 0.91 1.82 2.728(5) 173.2 . O3 H3B N7 0.91 2.52 3.361(5) 155.2 . O3 H3B O4 0.91 2.54 3.181(5) 127.7 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.675 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.135 # Attachment '_8_04slh035.cif' data_04slh035 _database_code_depnum_ccdc_archive 'CCDC 707537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 04lsh035/104 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 N12 Ni2 O16 S2' _chemical_formula_weight 1078.34 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5672(11) _cell_length_b 11.0578(15) _cell_length_c 11.8063(14) _cell_angle_alpha 71.926(6) _cell_angle_beta 77.024(7) _cell_angle_gamma 77.929(7) _cell_volume 1024.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4438 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9568 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; The values for minimum and maximum transmission are based on the cell dimensions only and were generated using the size command in SHELX. SADABS estimates the minimum and maximum transmission as 0.3040 and 0.4305, respectively. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16334 _diffrn_reflns_av_R_equivalents 0.1652 _diffrn_reflns_av_sigmaI/netI 0.1450 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3584 _reflns_number_gt 2290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. The crystals were found to be of poor quality and weakly diffracting at higher angles, hence merging of the data resulted in a high Rint. However, the connectivity of the compound could be establish unambigiously. Searches for better crystals were not successful. The water molecule containing atom O8 is disordered over two positions with a refined ratio of 52%:48%. ; _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^)+(0.0232P)^2^+3.3391P] 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 3584 _refine_ls_number_parameters 317 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1470 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1261 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _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 C1 C -0.0261(8) -0.1179(7) 0.6428(6) 0.0217(16) Uani 1 1 d . . . C2 C 0.1411(8) -0.2780(7) 0.5747(6) 0.0242(16) Uani 1 1 d . . . C3 C 0.2183(8) -0.1983(6) 0.7055(6) 0.0210(16) Uani 1 1 d . . . C4 C -0.1759(8) -0.0257(6) 0.6524(5) 0.0196(15) Uani 1 1 d . . . C5 C -0.2997(8) -0.0154(7) 0.5921(6) 0.0261(17) Uani 1 1 d . . . H5 H -0.2924 -0.0670 0.5395 0.031 Uiso 1 1 calc R . . C6 C -0.4370(8) 0.0742(7) 0.6116(6) 0.0277(17) Uani 1 1 d . . . H6 H -0.5267 0.0830 0.5733 0.033 Uiso 1 1 calc R . . C7 C -0.4427(8) 0.1496(7) 0.6856(6) 0.0282(17) Uani 1 1 d . . . H7 H -0.5354 0.2112 0.6987 0.034 Uiso 1 1 calc R . . C8 C -0.3112(8) 0.1343(7) 0.7408(6) 0.0266(17) Uani 1 1 d . . . H8 H -0.3151 0.1869 0.7918 0.032 Uiso 1 1 calc R . . C9 C 0.3260(8) -0.1860(7) 0.7819(6) 0.0228(16) Uani 1 1 d . . . C10 C 0.4770(9) -0.2617(7) 0.7905(6) 0.0288(17) Uani 1 1 d . . . H10 H 0.5139 -0.3252 0.7477 0.035 Uiso 1 1 calc R . . C11 C 0.5731(9) -0.2433(7) 0.8624(6) 0.0298(18) Uani 1 1 d . . . H11 H 0.6774 -0.2925 0.8692 0.036 Uiso 1 1 calc R . . C12 C 0.5120(8) -0.1511(7) 0.9234(6) 0.0253(17) Uani 1 1 d . . . H12 H 0.5750 -0.1355 0.9727 0.030 Uiso 1 1 calc R . . C13 C 0.3597(8) -0.0812(7) 0.9134(6) 0.0272(17) Uani 1 1 d . . . H13 H 0.3198 -0.0198 0.9582 0.033 Uiso 1 1 calc R . . C14 C 0.1728(8) -0.3736(7) 0.5050(6) 0.0253(17) Uani 1 1 d . . . C15 C 0.2886(8) -0.4813(7) 0.5282(6) 0.0270(17) Uani 1 1 d . . . H15 H 0.3524 -0.4958 0.5887 0.032 Uiso 1 1 calc R . . C16 C 0.3090(9) -0.5677(7) 0.4603(6) 0.0302(18) Uani 1 1 d . . . H16 H 0.3862 -0.6437 0.4746 0.036 Uiso 1 1 calc R . . C17 C 0.2161(8) -0.5418(7) 0.3721(6) 0.0262(17) Uani 1 1 d . . . H17 H 0.2278 -0.5995 0.3246 0.031 Uiso 1 1 calc R . . C18 C 0.1055(8) -0.4302(7) 0.3541(6) 0.0261(17) Uani 1 1 d . . . H18 H 0.0422 -0.4128 0.2927 0.031 Uiso 1 1 calc R . . N1 N 0.0796(7) -0.1166(5) 0.7097(5) 0.0233(14) Uani 1 1 d . . . N2 N -0.0020(7) -0.1978(6) 0.5738(5) 0.0243(14) Uani 1 1 d . . . N3 N 0.2562(7) -0.2812(5) 0.6389(5) 0.0251(14) Uani 1 1 d . . . N4 N -0.1780(7) 0.0483(5) 0.7254(5) 0.0228(13) Uani 1 1 d . . . N5 N 0.2656(6) -0.0959(5) 0.8434(5) 0.0244(14) Uani 1 1 d . . . N6 N 0.0824(6) -0.3451(5) 0.4180(5) 0.0223(13) Uani 1 1 d . . . O1 O -0.1011(5) -0.1224(4) 0.9463(4) 0.0247(11) Uani 1 1 d . . . O2 O 0.0558(6) -0.3265(4) 1.0339(4) 0.0292(12) Uani 1 1 d . . . O3 O -0.1886(6) -0.2413(5) 1.1520(4) 0.0304(12) Uani 1 1 d . . . O4 O 0.0520(5) -0.1407(4) 1.1027(4) 0.0236(11) Uani 1 1 d . . . O5 O 0.1538(5) 0.1418(4) 0.6698(4) 0.0264(12) Uani 1 1 d D . . H5A H 0.0774 0.1845 0.6336 0.040 Uiso 1 1 d D . . H5B H 0.1744 0.1819 0.7130 0.040 Uiso 1 1 d D . . S1 S -0.0455(2) -0.20880(18) 1.05842(15) 0.0246(4) Uani 1 1 d . . . Ni1 Ni 0.02916(11) 0.00474(9) 0.81015(8) 0.0224(3) Uani 1 1 d . . . O6 O 0.3747(6) -0.4559(5) 1.0842(5) 0.0556(17) Uani 1 1 d D . . H6A H 0.4288 -0.4039 1.0907 0.083 Uiso 1 1 d D . . H6B H 0.2936 -0.4077 1.0564 0.083 Uiso 1 1 d D . . O7 O -0.0139(8) -0.4052(5) 0.8431(5) 0.0613(19) Uani 1 1 d D . . H7A H 0.0387 -0.4073 0.8957 0.092 Uiso 1 1 d D . . H7B H -0.0278 -0.4816 0.8561 0.092 Uiso 1 1 d D . . O8 O -0.364(3) -0.4284(16) 1.182(2) 0.063(8) Uani 0.52(4) 1 d PD A 1 H8A H -0.4412 -0.4366 1.1523 0.094 Uiso 0.52 1 d PD A 1 H8B H -0.3083 -0.3689 1.1722 0.094 Uiso 0.52 1 d PD A 1 O8' O -0.448(2) -0.392(2) 1.2232(13) 0.051(6) Uani 0.48(4) 1 d PD A 2 H8A' H -0.3700 -0.3478 1.1932 0.077 Uiso 0.48 1 d PD A 2 H8B' H -0.5059 -0.3671 1.1693 0.077 Uiso 0.48 1 d PD A 2 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 C1 0.018(4) 0.023(4) 0.022(4) -0.003(3) -0.006(3) -0.003(3) C2 0.024(4) 0.027(4) 0.025(4) -0.010(3) -0.008(3) -0.005(3) C3 0.020(4) 0.024(4) 0.019(4) -0.006(3) -0.001(3) -0.006(3) C4 0.018(4) 0.027(4) 0.016(3) -0.010(3) 0.001(3) -0.004(3) C5 0.018(4) 0.034(5) 0.026(4) -0.013(4) -0.002(3) 0.001(3) C6 0.016(4) 0.046(5) 0.027(4) -0.015(4) -0.005(3) -0.009(3) C7 0.019(4) 0.033(5) 0.032(4) -0.011(4) -0.005(3) 0.000(3) C8 0.025(4) 0.025(4) 0.030(4) -0.009(3) -0.002(3) -0.003(3) C9 0.014(4) 0.026(4) 0.027(4) -0.012(3) 0.004(3) 0.000(3) C10 0.029(4) 0.027(4) 0.030(4) -0.011(3) -0.006(3) 0.001(3) C11 0.026(4) 0.033(5) 0.033(4) -0.009(4) -0.011(4) -0.002(3) C12 0.019(4) 0.037(5) 0.023(4) -0.011(3) -0.003(3) -0.008(3) C13 0.027(4) 0.027(4) 0.030(4) -0.008(3) -0.008(3) -0.006(3) C14 0.021(4) 0.030(5) 0.022(4) -0.004(3) 0.002(3) -0.009(3) C15 0.025(4) 0.033(5) 0.025(4) -0.008(3) -0.011(3) -0.001(3) C16 0.028(4) 0.030(5) 0.031(4) -0.011(4) -0.004(3) 0.002(3) C17 0.029(4) 0.029(4) 0.022(4) -0.012(3) -0.001(3) -0.002(3) C18 0.025(4) 0.032(4) 0.021(4) -0.003(3) -0.004(3) -0.008(3) N1 0.018(3) 0.031(4) 0.023(3) -0.009(3) -0.003(3) -0.006(3) N2 0.020(3) 0.035(4) 0.021(3) -0.012(3) -0.004(3) -0.002(3) N3 0.025(3) 0.028(4) 0.024(3) -0.010(3) -0.006(3) -0.001(3) N4 0.018(3) 0.030(4) 0.020(3) -0.006(3) -0.003(3) -0.006(3) N5 0.018(3) 0.033(4) 0.026(3) -0.009(3) -0.007(3) -0.004(3) N6 0.015(3) 0.034(4) 0.019(3) -0.010(3) 0.003(2) -0.008(3) O1 0.024(3) 0.031(3) 0.021(2) -0.006(2) -0.005(2) -0.008(2) O2 0.032(3) 0.022(3) 0.035(3) -0.009(2) -0.011(2) 0.001(2) O3 0.032(3) 0.038(3) 0.023(3) -0.008(2) -0.001(2) -0.014(2) O4 0.021(3) 0.027(3) 0.026(3) -0.009(2) -0.007(2) -0.006(2) O5 0.016(3) 0.039(3) 0.026(3) -0.013(2) -0.007(2) 0.003(2) S1 0.0240(10) 0.0288(11) 0.0230(9) -0.0091(8) -0.0036(8) -0.0057(8) Ni1 0.0178(5) 0.0288(6) 0.0224(5) -0.0105(4) -0.0040(4) -0.0020(4) O6 0.045(4) 0.060(4) 0.064(4) -0.013(3) -0.019(3) -0.009(3) O7 0.112(6) 0.049(4) 0.033(3) -0.009(3) -0.013(3) -0.036(4) O8 0.072(17) 0.051(10) 0.074(12) 0.003(8) -0.037(12) -0.032(9) O8' 0.054(12) 0.054(11) 0.051(9) -0.015(8) -0.015(8) -0.011(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 C1 N1 1.333(8) . ? C1 N2 1.335(8) . ? C1 C4 1.469(9) . ? C2 N2 1.355(9) . ? C2 N3 1.361(8) . ? C2 C14 1.480(9) . ? C3 N3 1.332(8) . ? C3 N1 1.335(8) . ? C3 C9 1.479(9) . ? C4 N4 1.355(8) . ? C4 C5 1.372(9) . ? C5 C6 1.396(9) . ? C5 H5 0.9500 . ? C6 C7 1.370(9) . ? C6 H6 0.9500 . ? C7 C8 1.380(9) . ? C7 H7 0.9500 . ? C8 N4 1.342(9) . ? C8 H8 0.9500 . ? C9 N5 1.361(8) . ? C9 C10 1.392(9) . ? C10 C11 1.390(9) . ? C10 H10 0.9500 . ? C11 C12 1.376(9) . ? C11 H11 0.9500 . ? C12 C13 1.379(9) . ? C12 H12 0.9500 . ? C13 N5 1.340(8) . ? C13 H13 0.9500 . ? C14 N6 1.344(8) . ? C14 C15 1.379(10) . ? C15 C16 1.389(9) . ? C15 H15 0.9500 . ? C16 C17 1.375(9) . ? C16 H16 0.9500 . ? C17 C18 1.380(10) . ? C17 H17 0.9500 . ? C18 N6 1.338(8) . ? C18 H18 0.9500 . ? N1 Ni1 1.977(6) . ? N4 Ni1 2.127(5) . ? N5 Ni1 2.154(5) . ? O1 S1 1.484(4) . ? O1 Ni1 2.062(5) . ? O2 S1 1.476(5) . ? O3 S1 1.477(5) . ? O4 S1 1.497(4) . ? O4 Ni1 2.001(4) 2_557 ? O5 Ni1 2.123(5) . ? O5 H5A 0.8400 . ? O5 H5B 0.8374 . ? Ni1 O4 2.001(4) 2_557 ? O6 H6A 0.8402 . ? O6 H6B 0.8446 . ? O7 H7A 0.8373 . ? O7 H7B 0.8393 . ? O8 H8A 0.8476 . ? O8 H8B 0.8552 . ? O8 H8A' 0.9317 . ? O8 H8B' 1.2807 . ? O8' H8A 1.0821 . ? O8' H8B 1.2490 . ? O8' H8A' 0.8533 . ? O8' H8B' 0.8407 . ? 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 N1 C1 N2 123.6(6) . . ? N1 C1 C4 114.9(6) . . ? N2 C1 C4 121.5(6) . . ? N2 C2 N3 125.1(6) . . ? N2 C2 C14 117.9(6) . . ? N3 C2 C14 117.0(6) . . ? N3 C3 N1 123.7(6) . . ? N3 C3 C9 123.6(6) . . ? N1 C3 C9 112.8(6) . . ? N4 C4 C5 123.8(6) . . ? N4 C4 C1 113.2(6) . . ? C5 C4 C1 123.0(6) . . ? C4 C5 C6 117.0(6) . . ? C4 C5 H5 121.5 . . ? C6 C5 H5 121.5 . . ? C7 C6 C5 120.3(6) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 118.7(7) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? N4 C8 C7 122.8(7) . . ? N4 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? N5 C9 C10 122.9(6) . . ? N5 C9 C3 114.9(6) . . ? C10 C9 C3 122.3(6) . . ? C11 C10 C9 119.2(7) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 117.7(7) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? C11 C12 C13 120.4(6) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? N5 C13 C12 123.1(7) . . ? N5 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? N6 C14 C15 124.0(7) . . ? N6 C14 C2 114.6(6) . . ? C15 C14 C2 121.4(6) . . ? C14 C15 C16 117.9(6) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C17 C16 C15 119.2(7) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 118.6(7) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N6 C18 C17 123.8(6) . . ? N6 C18 H18 118.1 . . ? C17 C18 H18 118.1 . . ? C1 N1 C3 118.0(6) . . ? C1 N1 Ni1 119.9(5) . . ? C3 N1 Ni1 122.1(4) . . ? C1 N2 C2 114.9(6) . . ? C3 N3 C2 114.8(6) . . ? C8 N4 C4 117.3(6) . . ? C8 N4 Ni1 127.8(5) . . ? C4 N4 Ni1 114.8(4) . . ? C13 N5 C9 116.8(6) . . ? C13 N5 Ni1 129.6(5) . . ? C9 N5 Ni1 113.6(4) . . ? C18 N6 C14 116.4(6) . . ? S1 O1 Ni1 126.3(3) . . ? S1 O4 Ni1 127.9(3) . 2_557 ? Ni1 O5 H5A 100.4 . . ? Ni1 O5 H5B 97.7 . . ? H5A O5 H5B 110.3 . . ? O2 S1 O3 110.6(3) . . ? O2 S1 O1 110.0(3) . . ? O3 S1 O1 108.9(3) . . ? O2 S1 O4 109.3(3) . . ? O3 S1 O4 108.7(3) . . ? O1 S1 O4 109.4(3) . . ? N1 Ni1 O4 170.7(2) . 2_557 ? N1 Ni1 O1 90.2(2) . . ? O4 Ni1 O1 90.52(18) 2_557 . ? N1 Ni1 O5 91.1(2) . . ? O4 Ni1 O5 87.81(18) 2_557 . ? O1 Ni1 O5 177.45(19) . . ? N1 Ni1 N4 77.2(2) . . ? O4 Ni1 N4 93.6(2) 2_557 . ? O1 Ni1 N4 84.88(19) . . ? O5 Ni1 N4 93.29(18) . . ? N1 Ni1 N5 76.7(2) . . ? O4 Ni1 N5 112.41(19) 2_557 . ? O1 Ni1 N5 96.4(2) . . ? O5 Ni1 N5 86.04(19) . . ? N4 Ni1 N5 153.9(2) . . ? H6A O6 H6B 103.4 . . ? H7A O7 H7B 105.1 . . ? H8A O8 H8B 136.3 . . ? H8A O8 H8A' 114.7 . . ? H8B O8 H8A' 36.7 . . ? H8A O8 H8B' 44.4 . . ? H8B O8 H8B' 103.4 . . ? H8A' O8 H8B' 72.0 . . ? H8A O8' H8B 85.1 . . ? H8A O8' H8A' 100.8 . . ? H8B O8' H8A' 22.7 . . ? H8A O8' H8B' 53.9 . . ? H8B O8' H8B' 107.0 . . ? H8A' O8' H8B' 103.5 . . ? 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 O5 H5A N6 0.84 2.02 2.795(7) 153.0 2_556 O5 H5A N2 0.84 2.62 3.253(6) 132.9 2_556 O5 H5B O3 0.84 1.94 2.754(6) 164.2 2_557 O5 H5B S1 0.84 2.76 3.400(4) 134.5 2_557 O6 H6A O8' 0.84 2.12 2.793(12) 136.2 1_655 O6 H6A O8 0.84 2.21 2.846(9) 133.1 1_655 O6 H6B O2 0.84 2.09 2.904(7) 162.3 . O7 H7A O2 0.84 2.13 2.868(6) 146.4 . O7 H7B O2 0.84 2.15 2.928(7) 154.8 2_547 O8 H8A O6 0.85 2.00 2.846(9) 179.5 1_455 O8 H8B O3 0.86 1.84 2.696(9) 179.8 . O8 H8B S1 0.86 2.97 3.774(14) 156.6 . O8' H8A' O3 0.85 2.03 2.872(10) 170.0 . O8' H8B' O6 0.84 2.12 2.793(12) 136.3 1_455 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.489 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.108