Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Maria Carla Aragoni' _publ_contact_author_address ; Dipartimento di Chimica Inorganica ed Analitica Universita degli Studi di Cagliari Cittadella Universitaria Monserrato SS 554 - bivio Sestu Cagliari 09042 ITALY ; _publ_contact_author_email ARAGONI@UNICA.IT _publ_section_title ; Investigation on the reactivity of the coordinatively unsaturated phosphonodithioato [Ni(MeOpdt)2] towards 2,4,6-tris-2-pyridyl- 1,3,5-triazine: goals and achievements ; loop_ _publ_author_name 'Maria Carla Aragoni' 'Massimiliano Arca' 'F. A. Devillanova' 'M Hursthouse' 'Susanne L. Huth' ; F.Isaia ; 'Vito Lippolis' 'Annalisa Mancini' 'Serena Soddu' 'Gaetano Verani' #===END data_04slh011 _database_code_depnum_ccdc_archive 'CCDC 278294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H36 N6 Ni O5 P2 S4' _chemical_formula_weight 869.59 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 8.967(2) _cell_length_b 14.267(4) _cell_length_c 15.313(4) _cell_angle_alpha 96.09(2) _cell_angle_beta 97.72(2) _cell_angle_gamma 94.94(3) _cell_volume 1920.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14980 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description blade _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8611 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _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 ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26901 _diffrn_reflns_av_R_equivalents 0.0861 _diffrn_reflns_av_sigmaI/netI 0.1475 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8736 _reflns_number_gt 5178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)' _computing_structure_solution ? _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^)+(0.0432P)^2^+0.2353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8736 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.3565(4) 0.2875(3) -0.0922(2) 0.0193(9) Uani 1 1 d . . . C2 C 0.2420(4) 0.2296(3) -0.1497(3) 0.0227(9) Uani 1 1 d . . . H2 H 0.2599 0.1674 -0.1718 0.027 Uiso 1 1 calc R . . C3 C 0.1054(4) 0.2615(3) -0.1742(3) 0.0255(10) Uani 1 1 d . . . H3 H 0.0290 0.2216 -0.2134 0.031 Uiso 1 1 calc R . . C4 C 0.0774(4) 0.3520(3) -0.1423(3) 0.0210(9) Uani 1 1 d . . . C5 C 0.1888(4) 0.4109(3) -0.0859(3) 0.0227(9) Uani 1 1 d . . . H5 H 0.1703 0.4730 -0.0642 0.027 Uiso 1 1 calc R . . C6 C 0.3286(4) 0.3778(3) -0.0614(3) 0.0236(10) Uani 1 1 d . . . H6 H 0.4056 0.4180 -0.0230 0.028 Uiso 1 1 calc R . . C7 C -0.1003(4) 0.4678(3) -0.1380(3) 0.0287(10) Uani 1 1 d . . . H7A H -0.2040 0.4755 -0.1637 0.043 Uiso 1 1 calc R . . H7B H -0.0304 0.5170 -0.1549 0.043 Uiso 1 1 calc R . . H7C H -0.0927 0.4734 -0.0732 0.043 Uiso 1 1 calc R . . C8 C 0.7044(4) 0.1837(3) -0.1886(3) 0.0259(10) Uani 1 1 d . . . H8A H 0.7093 0.1823 -0.2523 0.039 Uiso 1 1 calc R . . H8B H 0.6962 0.1188 -0.1730 0.039 Uiso 1 1 calc R . . H8C H 0.7964 0.2192 -0.1549 0.039 Uiso 1 1 calc R . . C11 C 0.6437(4) 0.4329(3) 0.3350(3) 0.0220(9) Uani 1 1 d . . . C12 C 0.6491(5) 0.5050(3) 0.2804(3) 0.0350(11) Uani 1 1 d . . . H12 H 0.7275 0.5099 0.2446 0.042 Uiso 1 1 calc R . . C13 C 0.5420(5) 0.5695(3) 0.2776(3) 0.0383(12) Uani 1 1 d . . . H13 H 0.5462 0.6181 0.2398 0.046 Uiso 1 1 calc R . . C14 C 0.4283(4) 0.5623(3) 0.3308(3) 0.0278(10) Uani 1 1 d . . . C15 C 0.4218(4) 0.4912(3) 0.3847(3) 0.0295(11) Uani 1 1 d . . . H15 H 0.3437 0.4860 0.4206 0.035 Uiso 1 1 calc R . . C16 C 0.5289(4) 0.4276(3) 0.3864(3) 0.0264(10) Uani 1 1 d . . . H16 H 0.5237 0.3788 0.4239 0.032 Uiso 1 1 calc R . . C17 C 0.1996(5) 0.6205(3) 0.3687(3) 0.0424(12) Uani 1 1 d . . . H17A H 0.1381 0.6728 0.3579 0.064 Uiso 1 1 calc R . . H17B H 0.2332 0.6226 0.4326 0.064 Uiso 1 1 calc R . . H17C H 0.1392 0.5600 0.3467 0.064 Uiso 1 1 calc R . . C18 C 1.0533(4) 0.3878(3) 0.4403(3) 0.0324(11) Uani 1 1 d . . . H18A H 1.1209 0.4386 0.4775 0.049 Uiso 1 1 calc R . . H18B H 1.1037 0.3622 0.3913 0.049 Uiso 1 1 calc R . . H18C H 1.0283 0.3373 0.4761 0.049 Uiso 1 1 calc R . . C21 C 0.5683(4) 0.1014(3) 0.2382(2) 0.0173(9) Uani 1 1 d . . . C22 C 0.6758(4) -0.0189(3) 0.2959(3) 0.0210(9) Uani 1 1 d . . . C23 C 0.7897(4) 0.0588(3) 0.1977(3) 0.0182(9) Uani 1 1 d . . . C24 C 0.9097(4) 0.0784(3) 0.1423(2) 0.0171(9) Uani 1 1 d . . . C25 C 1.0345(4) 0.0275(3) 0.1431(3) 0.0221(9) Uani 1 1 d . . . H25 H 1.0474 -0.0219 0.1797 0.026 Uiso 1 1 calc R . . C26 C 1.1403(4) 0.0514(3) 0.0884(3) 0.0221(9) Uani 1 1 d . . . H26 H 1.2269 0.0177 0.0862 0.027 Uiso 1 1 calc R . . C27 C 1.1182(4) 0.1239(3) 0.0378(3) 0.0223(9) Uani 1 1 d . . . H27 H 1.1897 0.1416 0.0005 0.027 Uiso 1 1 calc R . . C28 C 0.9907(4) 0.1709(3) 0.0417(2) 0.0211(9) Uani 1 1 d . . . H28 H 0.9772 0.2215 0.0068 0.025 Uiso 1 1 calc R . . C29 C 0.4561(4) 0.1698(3) 0.2287(2) 0.0187(9) Uani 1 1 d . . . C30 C 0.3300(4) 0.1677(3) 0.2723(3) 0.0237(9) Uani 1 1 d . . . H30 H 0.3120 0.1201 0.3097 0.028 Uiso 1 1 calc R . . C31 C 0.2316(4) 0.2356(3) 0.2605(3) 0.0260(10) Uani 1 1 d . . . H31 H 0.1431 0.2349 0.2883 0.031 Uiso 1 1 calc R . . C32 C 0.2636(4) 0.3046(3) 0.2076(3) 0.0280(10) Uani 1 1 d . . . H32 H 0.1981 0.3528 0.1993 0.034 Uiso 1 1 calc R . . C33 C 0.3925(4) 0.3033(3) 0.1665(3) 0.0238(10) Uani 1 1 d . . . H33 H 0.4135 0.3512 0.1300 0.029 Uiso 1 1 calc R . . C34 C 0.6749(4) -0.0941(3) 0.3557(3) 0.0234(9) Uani 1 1 d . . . C35 C 0.5472(4) -0.1198(3) 0.3923(3) 0.0317(11) Uani 1 1 d . . . H35 H 0.4583 -0.0889 0.3805 0.038 Uiso 1 1 calc R . . C36 C 0.5509(5) -0.1909(3) 0.4460(3) 0.0430(13) Uani 1 1 d . . . H36 H 0.4645 -0.2104 0.4719 0.052 Uiso 1 1 calc R . . C37 C 0.6812(5) -0.2331(3) 0.4616(3) 0.0474(14) Uani 1 1 d . . . H37 H 0.6880 -0.2819 0.4992 0.057 Uiso 1 1 calc R . . C38 C 0.8030(5) -0.2035(3) 0.4215(3) 0.0516(14) Uani 1 1 d . . . H38 H 0.8927 -0.2341 0.4318 0.062 Uiso 1 1 calc R . . N1 N 0.6790(3) 0.1142(2) 0.1888(2) 0.0172(7) Uani 1 1 d . . . N2 N 0.5582(3) 0.0330(2) 0.2894(2) 0.0204(8) Uani 1 1 d . . . N3 N 0.7969(3) -0.0075(2) 0.2523(2) 0.0195(7) Uani 1 1 d . . . N4 N 0.8859(3) 0.1492(2) 0.0919(2) 0.0185(7) Uani 1 1 d . . . N5 N 0.4882(3) 0.2367(2) 0.1765(2) 0.0195(7) Uani 1 1 d . . . N6 N 0.8022(4) -0.1350(2) 0.3697(2) 0.0353(9) Uani 1 1 d . . . O1 O 0.5742(3) 0.22924(18) -0.16757(17) 0.0238(6) Uani 1 1 d . . . O2 O -0.0622(3) 0.37687(19) -0.17025(18) 0.0287(7) Uani 1 1 d . . . O3 O 0.9186(3) 0.42453(18) 0.40543(18) 0.0258(7) Uani 1 1 d . . . O4 O 0.3286(3) 0.6293(2) 0.3235(2) 0.0356(8) Uani 1 1 d . . . P1 P 0.53641(11) 0.24218(7) -0.06890(7) 0.0200(3) Uani 1 1 d . . . P2 P 0.78865(11) 0.35302(7) 0.34168(7) 0.0211(3) Uani 1 1 d . . . S1 S 0.68460(10) 0.33471(7) 0.01392(7) 0.0236(3) Uani 1 1 d . . . S2 S 0.52327(10) 0.11894(7) -0.01859(7) 0.0224(2) Uani 1 1 d . . . S3 S 0.86235(10) 0.32961(7) 0.22379(7) 0.0222(2) Uani 1 1 d . . . S4 S 0.73608(12) 0.24094(7) 0.39933(7) 0.0289(3) Uani 1 1 d . . . Ni1 Ni 0.68673(5) 0.21890(3) 0.11534(3) 0.01932(15) Uani 1 1 d . . . C1S C 0.1614(6) 0.9643(6) 0.4231(4) 0.102(3) Uani 1 1 d . . . H1S1 H 0.2658 0.9922 0.4255 0.154 Uiso 1 1 calc R . . H1S2 H 0.1591 0.9152 0.4632 0.154 Uiso 1 1 calc R . . H1S3 H 0.0986 1.0136 0.4414 0.154 Uiso 1 1 calc R . . O1S O 0.1080(4) 0.9258(3) 0.3405(3) 0.0618(12) Uani 1 1 d . . . H1O1 H 0.024(5) 0.913(4) 0.339(4) 0.06(2) Uiso 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 0.023(2) 0.021(2) 0.015(2) 0.0064(18) 0.0038(17) 0.0001(17) C2 0.025(2) 0.019(2) 0.026(3) 0.0048(19) 0.0056(18) 0.0072(17) C3 0.027(2) 0.021(2) 0.026(3) -0.0021(19) -0.0008(18) 0.0012(18) C4 0.022(2) 0.024(2) 0.019(2) 0.0067(19) 0.0053(17) 0.0044(18) C5 0.027(2) 0.016(2) 0.026(3) 0.0018(19) 0.0074(19) 0.0029(18) C6 0.024(2) 0.023(2) 0.024(3) 0.0031(19) 0.0027(18) -0.0005(17) C7 0.027(2) 0.026(3) 0.036(3) 0.007(2) 0.0075(19) 0.0095(18) C8 0.022(2) 0.037(3) 0.020(2) 0.001(2) 0.0070(18) 0.0060(18) C11 0.024(2) 0.022(2) 0.020(2) 0.0003(19) 0.0036(18) 0.0025(17) C12 0.037(3) 0.042(3) 0.033(3) 0.014(2) 0.016(2) 0.009(2) C13 0.043(3) 0.036(3) 0.046(3) 0.021(2) 0.021(2) 0.018(2) C14 0.027(2) 0.027(3) 0.029(3) -0.001(2) 0.0030(19) 0.0096(19) C15 0.020(2) 0.041(3) 0.028(3) 0.003(2) 0.0108(19) 0.000(2) C16 0.024(2) 0.036(3) 0.021(3) 0.007(2) 0.0066(18) 0.0032(19) C17 0.041(3) 0.060(3) 0.032(3) 0.008(3) 0.011(2) 0.026(2) C18 0.030(2) 0.034(3) 0.031(3) 0.001(2) -0.002(2) 0.004(2) C21 0.017(2) 0.018(2) 0.014(2) -0.0026(18) -0.0008(16) -0.0021(16) C22 0.023(2) 0.021(2) 0.017(2) -0.0009(18) 0.0022(17) -0.0014(17) C23 0.025(2) 0.010(2) 0.018(2) -0.0010(17) 0.0015(17) 0.0014(16) C24 0.0137(19) 0.020(2) 0.017(2) -0.0008(18) 0.0038(16) -0.0001(16) C25 0.021(2) 0.021(2) 0.025(3) 0.0039(19) 0.0027(18) 0.0036(17) C26 0.020(2) 0.024(2) 0.021(2) -0.0018(19) -0.0001(17) 0.0039(17) C27 0.019(2) 0.028(2) 0.018(2) -0.0032(19) 0.0056(17) -0.0044(17) C28 0.026(2) 0.022(2) 0.015(2) 0.0010(18) 0.0034(17) -0.0015(17) C29 0.016(2) 0.022(2) 0.016(2) -0.0026(18) -0.0001(16) 0.0018(16) C30 0.019(2) 0.030(2) 0.022(2) 0.0029(19) 0.0023(17) 0.0042(18) C31 0.019(2) 0.029(3) 0.029(3) -0.002(2) 0.0059(18) 0.0016(18) C32 0.023(2) 0.023(2) 0.035(3) -0.009(2) 0.0015(19) 0.0067(18) C33 0.025(2) 0.024(2) 0.021(2) 0.0003(19) 0.0020(18) 0.0030(18) C34 0.034(2) 0.018(2) 0.017(2) 0.0023(18) 0.0036(18) 0.0001(18) C35 0.031(2) 0.037(3) 0.030(3) 0.012(2) 0.008(2) 0.000(2) C36 0.049(3) 0.042(3) 0.045(3) 0.026(3) 0.017(2) 0.001(2) C37 0.055(3) 0.048(3) 0.049(4) 0.033(3) 0.018(3) 0.011(3) C38 0.051(3) 0.054(3) 0.065(4) 0.039(3) 0.022(3) 0.028(3) N1 0.0181(16) 0.0142(17) 0.020(2) 0.0025(14) 0.0038(14) 0.0045(13) N2 0.0233(18) 0.0191(19) 0.019(2) 0.0026(15) 0.0027(14) 0.0008(14) N3 0.0204(17) 0.0189(19) 0.0193(19) -0.0006(15) 0.0059(14) 0.0013(14) N4 0.0206(17) 0.0170(18) 0.019(2) 0.0045(15) 0.0036(14) 0.0034(13) N5 0.0166(16) 0.0209(19) 0.021(2) 0.0039(16) 0.0011(14) 0.0046(14) N6 0.038(2) 0.034(2) 0.043(3) 0.024(2) 0.0157(18) 0.0159(17) O1 0.0249(14) 0.0293(16) 0.0200(16) 0.0049(13) 0.0075(12) 0.0089(12) O2 0.0247(15) 0.0273(17) 0.0333(19) 0.0004(14) 0.0000(13) 0.0083(12) O3 0.0261(15) 0.0261(16) 0.0243(17) 0.0012(13) 0.0008(12) 0.0036(12) O4 0.0363(17) 0.0366(19) 0.038(2) 0.0061(15) 0.0114(14) 0.0167(14) P1 0.0214(5) 0.0193(6) 0.0205(6) 0.0055(5) 0.0043(4) 0.0027(4) P2 0.0232(5) 0.0207(6) 0.0190(6) 0.0020(5) 0.0032(4) 0.0007(4) S1 0.0250(5) 0.0211(6) 0.0238(6) 0.0054(5) 0.0000(4) -0.0015(4) S2 0.0240(5) 0.0176(6) 0.0256(6) 0.0043(5) 0.0028(4) 0.0022(4) S3 0.0206(5) 0.0257(6) 0.0208(6) 0.0017(5) 0.0055(4) 0.0023(4) S4 0.0406(6) 0.0240(6) 0.0224(7) 0.0041(5) 0.0070(5) -0.0002(5) Ni1 0.0193(3) 0.0200(3) 0.0202(3) 0.0046(2) 0.0051(2) 0.0042(2) C1S 0.053(4) 0.180(8) 0.063(5) -0.037(5) 0.022(3) -0.012(4) O1S 0.040(2) 0.110(4) 0.038(3) 0.013(2) 0.0098(19) 0.012(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 C6 1.379(5) . ? C1 C2 1.404(5) . ? C1 P1 1.795(4) . ? C2 C3 1.363(5) . ? C2 H2 0.9500 . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 O2 1.357(4) . ? C4 C5 1.385(5) . ? C5 C6 1.396(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O2 1.424(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 O1 1.441(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C16 1.379(5) . ? C11 C12 1.394(5) . ? C11 P2 1.801(4) . ? C12 C13 1.387(6) . ? C12 H12 0.9500 . ? C13 C14 1.392(5) . ? C13 H13 0.9500 . ? C14 O4 1.366(5) . ? C14 C15 1.377(6) . ? C15 C16 1.376(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 O4 1.429(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O3 1.419(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 N2 1.320(5) . ? C21 N1 1.339(4) . ? C21 C29 1.464(5) . ? C22 N2 1.339(4) . ? C22 N3 1.356(4) . ? C22 C34 1.483(5) . ? C23 N1 1.322(4) . ? C23 N3 1.327(5) . ? C23 C24 1.484(5) . ? C24 N4 1.348(5) . ? C24 C25 1.385(5) . ? C25 C26 1.392(5) . ? C25 H25 0.9500 . ? C26 C27 1.369(5) . ? C26 H26 0.9500 . ? C27 C28 1.379(5) . ? C27 H27 0.9500 . ? C28 N4 1.329(4) . ? C28 H28 0.9500 . ? C29 N5 1.346(5) . ? C29 C30 1.388(5) . ? C30 C31 1.376(5) . ? C30 H30 0.9500 . ? C31 C32 1.374(5) . ? C31 H31 0.9500 . ? C32 C33 1.389(5) . ? C32 H32 0.9500 . ? C33 N5 1.341(5) . ? C33 H33 0.9500 . ? C34 N6 1.329(5) . ? C34 C35 1.380(5) . ? C35 C36 1.373(6) . ? C35 H35 0.9500 . ? C36 C37 1.364(6) . ? C36 H36 0.9500 . ? C37 C38 1.379(6) . ? C37 H37 0.9500 . ? C38 N6 1.323(5) . ? C38 H38 0.9500 . ? N1 Ni1 1.965(3) . ? N4 Ni1 2.170(3) . ? N5 Ni1 2.141(3) . ? O1 P1 1.588(3) . ? O3 P2 1.622(3) . ? P1 S2 1.9939(15) . ? P1 S1 2.0017(15) . ? P2 S4 1.9597(15) . ? P2 S3 2.0094(15) . ? S1 Ni1 2.3842(13) . ? S2 Ni1 2.5691(14) . ? S3 Ni1 2.4586(14) . ? C1S O1S 1.333(7) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O1S H1O1 0.76(5) . ? 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 118.7(3) . . ? C6 C1 P1 123.6(3) . . ? C2 C1 P1 117.6(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? O2 C4 C5 124.1(3) . . ? O2 C4 C3 115.8(3) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 C6 119.2(4) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 120.9(4) . . ? C1 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? 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 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C16 C11 C12 118.2(4) . . ? C16 C11 P2 121.3(3) . . ? C12 C11 P2 120.4(3) . . ? C13 C12 C11 121.0(4) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 119.2(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? O4 C14 C15 125.1(3) . . ? O4 C14 C13 114.8(4) . . ? C15 C14 C13 120.2(4) . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 121.7(4) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? 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 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C21 N1 123.8(3) . . ? N2 C21 C29 122.7(3) . . ? N1 C21 C29 113.5(3) . . ? N2 C22 N3 124.9(3) . . ? N2 C22 C34 117.8(3) . . ? N3 C22 C34 117.2(3) . . ? N1 C23 N3 124.0(3) . . ? N1 C23 C24 114.0(3) . . ? N3 C23 C24 121.9(3) . . ? N4 C24 C25 123.8(3) . . ? N4 C24 C23 114.1(3) . . ? C25 C24 C23 122.1(3) . . ? C24 C25 C26 117.5(4) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? C27 C26 C25 119.3(3) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? N4 C28 C27 123.5(4) . . ? N4 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? N5 C29 C30 122.9(3) . . ? N5 C29 C21 114.3(3) . . ? C30 C29 C21 122.8(3) . . ? C31 C30 C29 118.8(4) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C32 C31 C30 118.9(4) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? N5 C33 C32 122.3(4) . . ? N5 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? N6 C34 C35 123.2(4) . . ? N6 C34 C22 115.9(3) . . ? C35 C34 C22 120.9(4) . . ? C36 C35 C34 118.9(4) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C37 C36 C35 118.6(4) . . ? C37 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? C36 C37 C38 118.7(4) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? N6 C38 C37 123.8(4) . . ? N6 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? C23 N1 C21 117.1(3) . . ? C23 N1 Ni1 121.4(2) . . ? C21 N1 Ni1 121.2(2) . . ? C21 N2 C22 115.1(3) . . ? C23 N3 C22 114.7(3) . . ? C28 N4 C24 116.9(3) . . ? C28 N4 Ni1 129.6(3) . . ? C24 N4 Ni1 113.2(2) . . ? C33 N5 C29 117.6(3) . . ? C33 N5 Ni1 128.2(3) . . ? C29 N5 Ni1 114.2(2) . . ? C38 N6 C34 116.9(3) . . ? C8 O1 P1 121.1(2) . . ? C4 O2 C7 118.8(3) . . ? C18 O3 P2 118.4(2) . . ? C14 O4 C17 118.0(3) . . ? O1 P1 C1 97.77(16) . . ? O1 P1 S2 111.41(11) . . ? C1 P1 S2 113.36(12) . . ? O1 P1 S1 113.73(11) . . ? C1 P1 S1 111.74(13) . . ? S2 P1 S1 108.63(7) . . ? O3 P2 C11 97.34(16) . . ? O3 P2 S4 110.70(11) . . ? C11 P2 S4 113.52(13) . . ? O3 P2 S3 106.61(10) . . ? C11 P2 S3 110.19(14) . . ? S4 P2 S3 116.58(7) . . ? P1 S1 Ni1 86.69(5) . . ? P1 S2 Ni1 81.95(5) . . ? P2 S3 Ni1 113.04(5) . . ? N1 Ni1 N5 76.76(12) . . ? N1 Ni1 N4 76.81(11) . . ? N5 Ni1 N4 153.57(12) . . ? N1 Ni1 S1 174.24(9) . . ? N5 Ni1 S1 104.02(9) . . ? N4 Ni1 S1 102.35(9) . . ? N1 Ni1 S3 96.38(9) . . ? N5 Ni1 S3 97.00(9) . . ? N4 Ni1 S3 85.16(9) . . ? S1 Ni1 S3 89.20(4) . . ? N1 Ni1 S2 92.54(9) . . ? N5 Ni1 S2 89.68(9) . . ? N4 Ni1 S2 92.25(9) . . ? S1 Ni1 S2 81.78(4) . . ? S3 Ni1 S2 169.88(4) . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S O1S H1O1 107(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.509 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.102 #===END data_mma003 _database_code_depnum_ccdc_archive 'CCDC 278295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 N12 Ni O8 P2 S4' _chemical_formula_weight 1221.95 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 16.8179(3) _cell_length_b 17.2357(3) _cell_length_c 19.2582(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.8920(10) _cell_angle_gamma 90.00 _cell_volume 5575.23(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 26549 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 0.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8358 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _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 56708 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.46 _reflns_number_total 12649 _reflns_number_gt 8765 _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. ; _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^)+(0.0524P)^2^+3.4581P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12649 _refine_ls_number_parameters 740 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.710130(19) 0.067045(19) 0.189930(16) 0.01887(9) Uani 1 1 d . . . N1 N 0.66031(12) 0.10428(12) 0.10072(11) 0.0198(5) Uani 1 1 d . . . N2 N 0.58536(12) 0.20085(12) 0.04154(11) 0.0207(5) Uani 1 1 d . . . N3 N 0.59546(12) 0.07330(12) -0.00662(11) 0.0207(5) Uani 1 1 d . . . N4 N 0.68996(12) 0.18725(12) 0.20938(11) 0.0207(5) Uani 1 1 d . . . N5 N 0.70355(12) -0.03529(12) 0.12821(11) 0.0204(5) Uani 1 1 d . . . N6 N 0.49986(13) 0.24770(13) -0.07359(11) 0.0254(5) Uani 1 1 d . . . N7 N 0.74536(12) 0.03278(12) 0.28443(11) 0.0186(4) Uani 1 1 d . . . N8 N 0.84880(12) 0.00492(12) 0.36701(11) 0.0198(5) Uani 1 1 d . . . N9 N 0.71193(12) -0.00935(12) 0.39520(10) 0.0196(5) Uani 1 1 d . . . N10 N 0.83704(12) 0.07328(12) 0.18880(11) 0.0197(5) Uani 1 1 d . . . N11 N 0.59959(12) 0.04486(12) 0.23808(11) 0.0209(5) Uani 1 1 d . . . N12 N 0.76121(14) -0.04508(15) 0.52712(12) 0.0316(6) Uani 1 1 d . . . C1 C 0.62985(14) 0.17567(14) 0.09547(13) 0.0182(5) Uani 1 1 d . . . C2 C 0.57187(14) 0.14842(15) -0.00915(13) 0.0195(5) Uani 1 1 d . . . C3 C 0.63957(14) 0.05403(15) 0.05002(13) 0.0189(5) Uani 1 1 d . . . C4 C 0.64868(15) 0.22468(15) 0.15732(13) 0.0207(5) Uani 1 1 d . . . C5 C 0.62465(16) 0.30088(16) 0.16233(14) 0.0259(6) Uani 1 1 d . . . H5 H 0.5965 0.3259 0.1246 0.031 Uiso 1 1 calc R . . C6 C 0.64290(17) 0.34002(17) 0.22417(15) 0.0308(7) Uani 1 1 d . . . H6 H 0.6270 0.3925 0.2295 0.037 Uiso 1 1 calc R . . C7 C 0.68421(17) 0.30227(17) 0.27780(15) 0.0295(6) Uani 1 1 d . . . H7 H 0.6967 0.3281 0.3205 0.035 Uiso 1 1 calc R . . C8 C 0.70729(16) 0.22564(16) 0.26824(14) 0.0243(6) Uani 1 1 d . . . H8 H 0.7364 0.1998 0.3050 0.029 Uiso 1 1 calc R . . C9 C 0.66767(14) -0.02579(15) 0.06372(13) 0.0189(5) Uani 1 1 d . . . C10 C 0.65779(16) -0.08561(16) 0.01640(14) 0.0248(6) Uani 1 1 d . . . H10 H 0.6325 -0.0768 -0.0281 0.030 Uiso 1 1 calc R . . C11 C 0.68559(17) -0.15884(16) 0.03527(15) 0.0297(6) Uani 1 1 d . . . H11 H 0.6794 -0.2011 0.0038 0.036 Uiso 1 1 calc R . . C12 C 0.72252(17) -0.16955(17) 0.10061(15) 0.0307(7) Uani 1 1 d . . . H12 H 0.7422 -0.2191 0.1145 0.037 Uiso 1 1 calc R . . C13 C 0.73025(16) -0.10633(16) 0.14538(15) 0.0269(6) Uani 1 1 d . . . H13 H 0.7556 -0.1139 0.1901 0.032 Uiso 1 1 calc R . . C14 C 0.52639(15) 0.17392(15) -0.07307(13) 0.0217(6) Uani 1 1 d . . . C15 C 0.51310(16) 0.12380(17) -0.12867(14) 0.0273(6) Uani 1 1 d . . . H15 H 0.5323 0.0720 -0.1264 0.033 Uiso 1 1 calc R . . C16 C 0.47135(17) 0.15057(18) -0.18765(14) 0.0303(7) Uani 1 1 d . . . H16 H 0.4619 0.1175 -0.2267 0.036 Uiso 1 1 calc R . . C17 C 0.44366(17) 0.22561(17) -0.18906(15) 0.0320(7) Uani 1 1 d . . . H17 H 0.4149 0.2455 -0.2289 0.038 Uiso 1 1 calc R . . C18 C 0.45880(18) 0.27128(17) -0.13118(15) 0.0315(7) Uani 1 1 d . . . H18 H 0.4388 0.3228 -0.1322 0.038 Uiso 1 1 calc R . . C19 C 0.82241(15) 0.02976(14) 0.30477(13) 0.0181(5) Uani 1 1 d . . . C20 C 0.79112(15) -0.01487(14) 0.40964(13) 0.0194(5) Uani 1 1 d . . . C21 C 0.69246(15) 0.01403(14) 0.33112(12) 0.0179(5) Uani 1 1 d . . . C22 C 0.87562(15) 0.05526(14) 0.25026(13) 0.0190(5) Uani 1 1 d . . . C23 C 0.95682(15) 0.06006(15) 0.26171(14) 0.0230(6) Uani 1 1 d . . . H23 H 0.9814 0.0471 0.3057 0.028 Uiso 1 1 calc R . . C24 C 1.00199(16) 0.08442(16) 0.20729(14) 0.0257(6) Uani 1 1 d . . . H24 H 1.0582 0.0892 0.2136 0.031 Uiso 1 1 calc R . . C25 C 0.96387(16) 0.10150(16) 0.14399(14) 0.0259(6) Uani 1 1 d . . . H25 H 0.9936 0.1175 0.1059 0.031 Uiso 1 1 calc R . . C26 C 0.88152(16) 0.09501(15) 0.13656(14) 0.0230(6) Uani 1 1 d . . . H26 H 0.8558 0.1065 0.0927 0.028 Uiso 1 1 calc R . . C27 C 0.60883(15) 0.02231(14) 0.30552(13) 0.0192(5) Uani 1 1 d . . . C28 C 0.54542(15) 0.00985(15) 0.34712(13) 0.0224(6) Uani 1 1 d . . . H28 H 0.5540 -0.0054 0.3943 0.027 Uiso 1 1 calc R . . C29 C 0.46887(16) 0.02021(16) 0.31821(14) 0.0256(6) Uani 1 1 d . . . H29 H 0.4240 0.0117 0.3453 0.031 Uiso 1 1 calc R . . C30 C 0.45875(16) 0.04295(17) 0.24995(15) 0.0278(6) Uani 1 1 d . . . H30 H 0.4068 0.0501 0.2292 0.033 Uiso 1 1 calc R . . C31 C 0.52553(15) 0.05538(16) 0.21174(14) 0.0241(6) Uani 1 1 d . . . H31 H 0.5181 0.0721 0.1649 0.029 Uiso 1 1 calc R . . C32 C 0.81566(15) -0.04763(15) 0.47871(13) 0.0218(6) Uani 1 1 d . . . C33 C 0.88932(16) -0.08189(16) 0.49027(14) 0.0255(6) Uani 1 1 d . . . H33 H 0.9267 -0.0822 0.4549 0.031 Uiso 1 1 calc R . . C34 C 0.90800(18) -0.11603(17) 0.55466(15) 0.0313(7) Uani 1 1 d . . . H34 H 0.9578 -0.1411 0.5636 0.038 Uiso 1 1 calc R . . C35 C 0.85298(18) -0.11261(18) 0.60475(15) 0.0343(7) Uani 1 1 d . . . H35 H 0.8642 -0.1344 0.6495 0.041 Uiso 1 1 calc R . . C36 C 0.78089(18) -0.0768(2) 0.58887(15) 0.0386(8) Uani 1 1 d . . . H36 H 0.7431 -0.0747 0.6239 0.046 Uiso 1 1 calc R . . C37 C 0.86026(15) 0.31059(15) 0.03062(13) 0.0204(5) Uani 1 1 d . . . C38 C 0.83390(16) 0.28089(16) 0.09263(14) 0.0264(6) Uani 1 1 d . . . H38 H 0.8030 0.2347 0.0913 0.032 Uiso 1 1 calc R . . C39 C 0.85106(17) 0.31628(17) 0.15614(15) 0.0287(6) Uani 1 1 d . . . H39 H 0.8326 0.2943 0.1976 0.034 Uiso 1 1 calc R . . C40 C 0.89530(15) 0.38377(15) 0.15869(14) 0.0240(6) Uani 1 1 d . . . C41 C 0.92382(17) 0.41424(17) 0.09764(15) 0.0302(7) Uani 1 1 d . . . H41 H 0.9555 0.4599 0.0994 0.036 Uiso 1 1 calc R . . C42 C 0.90626(16) 0.37830(16) 0.03454(15) 0.0274(6) Uani 1 1 d . . . H42 H 0.9257 0.3998 -0.0067 0.033 Uiso 1 1 calc R . . C43 C 0.86840(18) 0.40977(19) 0.27702(15) 0.0337(7) Uani 1 1 d . . . H43A H 0.8119 0.4176 0.2641 0.051 Uiso 1 1 calc R . . H43B H 0.8846 0.4454 0.3148 0.051 Uiso 1 1 calc R . . H43C H 0.8770 0.3561 0.2926 0.051 Uiso 1 1 calc R . . C44 C 0.68854(17) 0.33894(18) -0.03791(16) 0.0328(7) Uani 1 1 d . . . H44A H 0.6667 0.2870 -0.0308 0.049 Uiso 1 1 calc R . . H44B H 0.6485 0.3712 -0.0629 0.049 Uiso 1 1 calc R . . H44C H 0.7030 0.3625 0.0073 0.049 Uiso 1 1 calc R . . S1 S 0.90857(4) 0.28546(4) -0.12339(4) 0.02488(15) Uani 1 1 d . . . S2 S 0.78136(4) 0.16645(4) -0.04204(4) 0.02481(15) Uani 1 1 d . . . P1 P 0.82798(4) 0.27118(4) -0.05369(3) 0.01943(15) Uani 1 1 d . . . O1 O 0.75818(10) 0.33319(10) -0.07796(9) 0.0218(4) Uani 1 1 d . . . O2 O 0.91479(12) 0.42465(12) 0.21805(10) 0.0320(5) Uani 1 1 d . . . C45 C 0.17120(16) 0.17193(16) 0.11422(14) 0.0244(6) Uani 1 1 d . . . C46 C 0.17758(16) 0.09173(16) 0.10464(14) 0.0261(6) Uani 1 1 d . . . H46 H 0.2028 0.0609 0.1403 0.031 Uiso 1 1 calc R . . C47 C 0.14795(17) 0.05660(16) 0.04451(15) 0.0289(6) Uani 1 1 d . . . H47 H 0.1529 0.0021 0.0387 0.035 Uiso 1 1 calc R . . C48 C 0.11059(17) 0.10165(16) -0.00788(15) 0.0277(6) Uani 1 1 d . . . C49 C 0.10193(18) 0.18065(17) 0.00087(15) 0.0304(7) Uani 1 1 d . . . H49 H 0.0748 0.2110 -0.0341 0.036 Uiso 1 1 calc R . . C50 C 0.13334(18) 0.21538(16) 0.06147(14) 0.0293(6) Uani 1 1 d . . . H50 H 0.1288 0.2700 0.0669 0.035 Uiso 1 1 calc R . . C51 C 0.0503(2) 0.1081(2) -0.12202(18) 0.0528(10) Uani 1 1 d . . . H51A H 0.0012 0.1321 -0.1070 0.079 Uiso 1 1 calc R . . H51B H 0.0380 0.0748 -0.1624 0.079 Uiso 1 1 calc R . . H51C H 0.0877 0.1487 -0.1347 0.079 Uiso 1 1 calc R . . C52 C 0.06374(19) 0.2767(2) 0.21908(18) 0.0440(8) Uani 1 1 d . . . H52A H 0.0827 0.3302 0.2154 0.066 Uiso 1 1 calc R . . H52B H 0.0223 0.2742 0.2530 0.066 Uiso 1 1 calc R . . H52C H 0.0418 0.2592 0.1736 0.066 Uiso 1 1 calc R . . S3 S 0.24532(5) 0.32420(4) 0.17215(4) 0.0381(2) Uani 1 1 d . . . S4 S 0.27856(4) 0.14844(5) 0.24782(4) 0.03254(18) Uani 1 1 d . . . P2 P 0.20781(4) 0.21906(4) 0.19405(4) 0.02560(16) Uani 1 1 d . . . O3 O 0.12977(11) 0.22675(12) 0.24169(10) 0.0327(5) Uani 1 1 d . . . O4 O 0.08531(13) 0.06259(12) -0.06663(11) 0.0381(5) Uani 1 1 d . . . O5 O 0.59865(12) 0.51222(13) 0.03249(11) 0.0342(5) Uani 1 1 d D . . H5C H 0.6471(8) 0.5160(19) 0.0247(17) 0.041 Uiso 1 1 d D . . H5D H 0.5831(19) 0.4661(8) 0.0289(18) 0.041 Uiso 1 1 d D . . O6 O 0.50485(13) 0.37709(12) 0.02074(11) 0.0344(5) Uani 1 1 d D . . H6C H 0.511(2) 0.3356(12) -0.0016(15) 0.041 Uiso 1 1 d D . . H6D H 0.4710(15) 0.4076(16) 0.0023(16) 0.041 Uiso 1 1 d D . . O7 O 0.43292(16) 0.32030(16) 0.13944(14) 0.0565(7) Uani 1 1 d D . . H7C H 0.3756(7) 0.324(2) 0.141(2) 0.068 Uiso 1 1 d D . . H7D H 0.446(2) 0.337(2) 0.0933(10) 0.068 Uiso 1 1 d D . . O8 O 0.41602(15) 0.16030(15) 0.12186(12) 0.0498(6) Uani 1 1 d D . . H8C H 0.432(2) 0.2143(9) 0.117(2) 0.060 Uiso 1 1 d D . . H8D H 0.3719(15) 0.171(2) 0.1503(16) 0.060 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01919(17) 0.02333(18) 0.01398(16) 0.00336(14) -0.00041(12) 0.00249(13) N1 0.0204(11) 0.0230(11) 0.0160(11) 0.0017(9) -0.0002(9) -0.0010(9) N2 0.0205(11) 0.0232(11) 0.0182(11) 0.0029(9) 0.0001(9) -0.0005(9) N3 0.0211(11) 0.0241(12) 0.0167(11) 0.0023(9) -0.0009(9) -0.0016(9) N4 0.0214(11) 0.0253(12) 0.0154(11) 0.0020(9) -0.0002(9) 0.0013(9) N5 0.0210(11) 0.0220(11) 0.0182(11) 0.0045(9) 0.0007(9) 0.0018(9) N6 0.0290(13) 0.0241(12) 0.0224(12) 0.0026(10) -0.0069(10) 0.0003(10) N7 0.0185(11) 0.0209(11) 0.0163(11) 0.0021(9) 0.0011(8) 0.0018(8) N8 0.0218(11) 0.0200(11) 0.0175(11) 0.0015(9) -0.0001(9) 0.0000(9) N9 0.0220(11) 0.0205(11) 0.0163(11) 0.0007(9) -0.0001(9) 0.0020(9) N10 0.0226(11) 0.0208(11) 0.0156(11) 0.0020(9) 0.0012(9) 0.0022(9) N11 0.0206(11) 0.0239(11) 0.0181(11) -0.0001(9) -0.0003(9) 0.0026(9) N12 0.0280(13) 0.0472(15) 0.0194(12) 0.0099(11) 0.0011(10) 0.0039(11) C1 0.0186(13) 0.0198(13) 0.0163(13) 0.0037(10) 0.0013(10) -0.0008(10) C2 0.0174(13) 0.0228(13) 0.0185(13) 0.0031(11) 0.0008(10) -0.0033(10) C3 0.0179(13) 0.0244(13) 0.0146(12) 0.0025(11) 0.0022(10) -0.0009(10) C4 0.0198(13) 0.0252(14) 0.0169(13) 0.0020(11) -0.0010(10) 0.0001(11) C5 0.0246(14) 0.0281(15) 0.0246(14) 0.0012(12) -0.0040(11) 0.0040(11) C6 0.0354(16) 0.0257(15) 0.0309(16) -0.0068(13) -0.0034(13) 0.0075(12) C7 0.0319(16) 0.0349(16) 0.0214(14) -0.0062(13) -0.0013(12) 0.0001(13) C8 0.0261(14) 0.0291(15) 0.0172(13) 0.0013(11) -0.0033(11) 0.0001(11) C9 0.0178(13) 0.0220(13) 0.0170(13) 0.0024(11) 0.0026(10) -0.0011(10) C10 0.0255(14) 0.0287(15) 0.0200(14) 0.0005(12) 0.0004(11) 0.0004(11) C11 0.0355(16) 0.0239(14) 0.0298(16) -0.0039(12) 0.0026(13) 0.0013(12) C12 0.0348(16) 0.0245(14) 0.0329(16) 0.0038(13) 0.0032(13) 0.0054(12) C13 0.0270(15) 0.0278(15) 0.0261(15) 0.0061(12) 0.0021(12) 0.0031(12) C14 0.0210(13) 0.0253(14) 0.0185(13) 0.0019(11) -0.0016(10) -0.0024(11) C15 0.0292(15) 0.0286(15) 0.0233(14) 0.0006(12) -0.0060(12) 0.0029(12) C16 0.0319(16) 0.0383(17) 0.0199(14) -0.0039(13) -0.0077(12) 0.0008(13) C17 0.0325(16) 0.0359(17) 0.0265(16) 0.0065(13) -0.0090(13) 0.0024(13) C18 0.0358(17) 0.0263(15) 0.0310(16) 0.0053(13) -0.0112(13) 0.0018(12) C19 0.0206(13) 0.0168(12) 0.0171(13) 0.0001(10) 0.0015(10) 0.0034(10) C20 0.0240(14) 0.0192(12) 0.0151(12) -0.0001(10) 0.0006(10) 0.0008(10) C21 0.0216(13) 0.0173(12) 0.0148(12) 0.0004(10) 0.0005(10) 0.0011(10) C22 0.0205(13) 0.0193(13) 0.0171(13) -0.0004(10) 0.0000(10) 0.0021(10) C23 0.0218(14) 0.0236(13) 0.0234(14) 0.0011(11) 0.0008(11) 0.0016(11) C24 0.0201(14) 0.0277(15) 0.0298(15) 0.0008(12) 0.0058(11) -0.0009(11) C25 0.0274(15) 0.0276(15) 0.0233(14) 0.0030(12) 0.0081(12) -0.0020(11) C26 0.0288(15) 0.0241(13) 0.0166(13) 0.0028(11) 0.0045(11) 0.0016(11) C27 0.0195(13) 0.0207(13) 0.0174(13) -0.0010(11) 0.0004(10) -0.0021(10) C28 0.0233(14) 0.0270(14) 0.0170(13) 0.0003(11) 0.0020(11) -0.0012(11) C29 0.0206(14) 0.0321(15) 0.0244(14) -0.0048(12) 0.0048(11) -0.0019(11) C30 0.0206(14) 0.0357(16) 0.0267(15) -0.0052(13) -0.0026(11) 0.0024(12) C31 0.0228(14) 0.0308(15) 0.0182(13) -0.0006(12) -0.0022(11) 0.0012(11) C32 0.0231(14) 0.0250(14) 0.0171(13) 0.0026(11) -0.0023(11) -0.0004(11) C33 0.0276(15) 0.0273(14) 0.0218(14) 0.0039(12) 0.0021(11) 0.0025(11) C34 0.0315(16) 0.0321(16) 0.0298(16) 0.0051(13) -0.0051(13) 0.0040(12) C35 0.0370(17) 0.0432(18) 0.0221(15) 0.0116(14) -0.0053(13) -0.0001(14) C36 0.0325(17) 0.060(2) 0.0237(15) 0.0168(15) 0.0026(13) 0.0023(15) C37 0.0197(13) 0.0205(13) 0.0207(13) -0.0001(11) -0.0013(10) -0.0001(10) C38 0.0278(15) 0.0250(14) 0.0265(15) -0.0003(12) 0.0018(12) -0.0048(11) C39 0.0322(16) 0.0315(15) 0.0225(14) 0.0005(12) 0.0023(12) -0.0034(12) C40 0.0230(14) 0.0259(14) 0.0227(14) -0.0032(12) -0.0006(11) -0.0012(11) C41 0.0310(16) 0.0284(15) 0.0311(16) -0.0030(13) 0.0013(13) -0.0085(12) C42 0.0289(15) 0.0288(15) 0.0247(15) 0.0002(12) 0.0039(12) -0.0027(12) C43 0.0377(17) 0.0395(17) 0.0238(15) -0.0059(13) 0.0014(13) -0.0009(14) C44 0.0229(15) 0.0384(17) 0.0380(17) 0.0120(14) 0.0090(13) 0.0055(12) S1 0.0236(3) 0.0288(4) 0.0226(3) -0.0030(3) 0.0042(3) -0.0018(3) S2 0.0306(4) 0.0199(3) 0.0236(4) 0.0005(3) -0.0015(3) -0.0039(3) P1 0.0203(3) 0.0200(3) 0.0180(3) -0.0006(3) -0.0002(3) -0.0009(3) O1 0.0222(9) 0.0217(9) 0.0214(9) 0.0034(8) 0.0010(7) 0.0025(7) O2 0.0375(12) 0.0363(11) 0.0221(10) -0.0079(9) 0.0020(9) -0.0099(9) C45 0.0266(14) 0.0245(14) 0.0222(14) 0.0004(12) 0.0023(11) -0.0021(11) C46 0.0287(15) 0.0265(14) 0.0232(14) 0.0040(12) 0.0019(12) 0.0008(12) C47 0.0302(15) 0.0217(14) 0.0349(17) -0.0044(13) 0.0031(13) -0.0001(12) C48 0.0298(15) 0.0281(15) 0.0248(15) -0.0068(12) -0.0011(12) 0.0028(12) C49 0.0392(17) 0.0277(15) 0.0234(15) 0.0014(12) -0.0051(13) 0.0057(13) C50 0.0413(17) 0.0211(14) 0.0251(15) -0.0012(12) -0.0020(13) 0.0016(12) C51 0.070(3) 0.049(2) 0.037(2) -0.0165(17) -0.0256(18) 0.0178(19) C52 0.0368(18) 0.052(2) 0.043(2) -0.0098(17) 0.0005(15) 0.0170(16) S3 0.0548(5) 0.0275(4) 0.0315(4) 0.0008(3) -0.0028(4) -0.0115(4) S4 0.0310(4) 0.0378(4) 0.0283(4) 0.0045(3) -0.0041(3) 0.0042(3) P2 0.0316(4) 0.0244(4) 0.0207(4) 0.0006(3) 0.0000(3) -0.0017(3) O3 0.0260(11) 0.0411(12) 0.0313(11) 0.0045(9) 0.0055(8) 0.0049(9) O4 0.0476(13) 0.0322(11) 0.0331(12) -0.0129(10) -0.0129(10) 0.0066(10) O5 0.0235(11) 0.0479(13) 0.0319(11) -0.0063(11) 0.0063(9) -0.0043(10) O6 0.0381(13) 0.0291(12) 0.0364(13) -0.0050(10) 0.0047(10) 0.0022(9) O7 0.0512(16) 0.0634(17) 0.0553(16) 0.0049(14) 0.0050(13) -0.0023(13) O8 0.0509(15) 0.0615(16) 0.0372(13) -0.0009(13) 0.0022(11) 0.0116(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N7 1.976(2) . ? Ni1 N1 1.980(2) . ? Ni1 N5 2.127(2) . ? Ni1 N4 2.136(2) . ? Ni1 N10 2.138(2) . ? Ni1 N11 2.153(2) . ? N1 C1 1.335(3) . ? N1 C3 1.338(3) . ? N2 C1 1.322(3) . ? N2 C2 1.341(3) . ? N3 C3 1.330(3) . ? N3 C2 1.354(3) . ? N4 C8 1.332(3) . ? N4 C4 1.354(3) . ? N5 C13 1.340(3) . ? N5 C9 1.363(3) . ? N6 C18 1.340(3) . ? N6 C14 1.347(3) . ? N7 C19 1.336(3) . ? N7 C21 1.336(3) . ? N8 C19 1.328(3) . ? N8 C20 1.346(3) . ? N9 C21 1.323(3) . ? N9 C20 1.350(3) . ? N10 C26 1.337(3) . ? N10 C22 1.357(3) . ? N11 C31 1.333(3) . ? N11 C27 1.357(3) . ? N12 C36 1.336(4) . ? N12 C32 1.340(3) . ? C1 C4 1.481(4) . ? C2 C14 1.483(4) . ? C3 C9 1.474(4) . ? C4 C5 1.379(4) . ? C5 C6 1.389(4) . ? C5 H5 0.9500 . ? C6 C7 1.379(4) . ? C6 H6 0.9500 . ? C7 C8 1.392(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.381(4) . ? C10 C11 1.388(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C12 C13 1.391(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.385(4) . ? C15 C16 1.384(4) . ? C15 H15 0.9500 . ? C16 C17 1.374(4) . ? C16 H16 0.9500 . ? C17 C18 1.378(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C22 1.480(3) . ? C20 C32 1.484(4) . ? C21 C27 1.474(3) . ? C22 C23 1.375(4) . ? C23 C24 1.390(4) . ? C23 H23 0.9500 . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.390(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.382(3) . ? C28 C29 1.388(4) . ? C28 H28 0.9500 . ? C29 C30 1.374(4) . ? C29 H29 0.9500 . ? C30 C31 1.390(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.380(4) . ? C33 C34 1.394(4) . ? C33 H33 0.9500 . ? C34 C35 1.371(4) . ? C34 H34 0.9500 . ? C35 C36 1.381(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.392(4) . ? C37 C42 1.400(4) . ? C37 P1 1.818(3) . ? C38 C39 1.384(4) . ? C38 H38 0.9500 . ? C39 C40 1.380(4) . ? C39 H39 0.9500 . ? C40 O2 1.369(3) . ? C40 C41 1.395(4) . ? C41 C42 1.382(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O2 1.433(3) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 O1 1.438(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? S1 P1 1.9706(9) . ? S2 P1 1.9852(9) . ? P1 O1 1.6380(18) . ? C45 C50 1.390(4) . ? C45 C46 1.399(4) . ? C45 P2 1.818(3) . ? C46 C47 1.377(4) . ? C46 H46 0.9500 . ? C47 C48 1.397(4) . ? C47 H47 0.9500 . ? C48 O4 1.366(3) . ? C48 C49 1.381(4) . ? C49 C50 1.392(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 O4 1.427(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O3 1.454(4) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? S3 P2 1.9714(10) . ? S4 P2 1.9610(10) . ? P2 O3 1.644(2) . ? O5 H5C 0.838(10) . ? O5 H5D 0.839(10) . ? O6 H6C 0.843(10) . ? O6 H6D 0.840(10) . ? O7 H7C 0.968(10) . ? O7 H7D 0.973(10) . ? O8 H8C 0.976(10) . ? O8 H8D 0.961(10) . ? 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 N7 Ni1 N1 172.03(8) . . ? N7 Ni1 N5 105.76(8) . . ? N1 Ni1 N5 77.06(8) . . ? N7 Ni1 N4 99.87(8) . . ? N1 Ni1 N4 76.92(8) . . ? N5 Ni1 N4 153.95(8) . . ? N7 Ni1 N10 76.77(8) . . ? N1 Ni1 N10 110.72(8) . . ? N5 Ni1 N10 93.43(8) . . ? N4 Ni1 N10 96.92(8) . . ? N7 Ni1 N11 77.03(8) . . ? N1 Ni1 N11 95.43(8) . . ? N5 Ni1 N11 94.11(8) . . ? N4 Ni1 N11 87.05(8) . . ? N10 Ni1 N11 153.80(8) . . ? C1 N1 C3 117.2(2) . . ? C1 N1 Ni1 120.56(17) . . ? C3 N1 Ni1 120.44(17) . . ? C1 N2 C2 114.8(2) . . ? C3 N3 C2 114.7(2) . . ? C8 N4 C4 118.4(2) . . ? C8 N4 Ni1 126.96(18) . . ? C4 N4 Ni1 114.36(17) . . ? C13 N5 C9 117.5(2) . . ? C13 N5 Ni1 127.78(18) . . ? C9 N5 Ni1 114.70(16) . . ? C18 N6 C14 116.7(2) . . ? C19 N7 C21 117.5(2) . . ? C19 N7 Ni1 121.56(16) . . ? C21 N7 Ni1 120.89(17) . . ? C19 N8 C20 114.4(2) . . ? C21 N9 C20 114.1(2) . . ? C26 N10 C22 117.3(2) . . ? C26 N10 Ni1 128.19(18) . . ? C22 N10 Ni1 114.41(16) . . ? C31 N11 C27 117.6(2) . . ? C31 N11 Ni1 128.48(17) . . ? C27 N11 Ni1 113.79(16) . . ? C36 N12 C32 117.3(2) . . ? N2 C1 N1 124.2(2) . . ? N2 C1 C4 122.3(2) . . ? N1 C1 C4 113.5(2) . . ? N2 C2 N3 125.4(2) . . ? N2 C2 C14 117.8(2) . . ? N3 C2 C14 116.8(2) . . ? N3 C3 N1 123.4(2) . . ? N3 C3 C9 122.7(2) . . ? N1 C3 C9 113.8(2) . . ? N4 C4 C5 122.9(2) . . ? N4 C4 C1 113.9(2) . . ? C5 C4 C1 123.2(2) . . ? C4 C5 C6 118.0(3) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 118.8(3) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? N4 C8 C7 122.2(2) . . ? N4 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? N5 C9 C10 123.0(2) . . ? N5 C9 C3 113.5(2) . . ? C10 C9 C3 123.5(2) . . ? C9 C10 C11 118.6(3) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 118.8(3) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? N5 C13 C12 122.9(3) . . ? N5 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? N6 C14 C15 122.8(2) . . ? N6 C14 C2 116.3(2) . . ? C15 C14 C2 120.9(2) . . ? C16 C15 C14 118.8(3) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 119.2(3) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 118.2(3) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? N6 C18 C17 124.3(3) . . ? N6 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? N8 C19 N7 123.5(2) . . ? N8 C19 C22 123.3(2) . . ? N7 C19 C22 113.1(2) . . ? N8 C20 N9 126.2(2) . . ? N8 C20 C32 117.8(2) . . ? N9 C20 C32 116.0(2) . . ? N9 C21 N7 124.0(2) . . ? N9 C21 C27 121.9(2) . . ? N7 C21 C27 114.1(2) . . ? N10 C22 C23 123.6(2) . . ? N10 C22 C19 114.0(2) . . ? C23 C22 C19 122.4(2) . . ? C22 C23 C24 118.3(2) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C25 C24 C23 118.9(2) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 119.3(2) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? N10 C26 C25 122.5(2) . . ? N10 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? N11 C27 C28 123.0(2) . . ? N11 C27 C21 114.2(2) . . ? C28 C27 C21 122.8(2) . . ? C27 C28 C29 118.3(2) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C30 C29 C28 119.2(2) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C31 119.1(3) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? N11 C31 C30 122.8(2) . . ? N11 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? N12 C32 C33 122.8(2) . . ? N12 C32 C20 116.2(2) . . ? C33 C32 C20 120.9(2) . . ? C32 C33 C34 119.0(3) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C35 C34 C33 118.5(3) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? C34 C35 C36 118.7(3) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? N12 C36 C35 123.8(3) . . ? N12 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? C38 C37 C42 117.3(2) . . ? C38 C37 P1 122.3(2) . . ? C42 C37 P1 119.9(2) . . ? C39 C38 C37 122.3(3) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C40 C39 C38 119.4(3) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? O2 C40 C39 124.7(2) . . ? O2 C40 C41 115.6(2) . . ? C39 C40 C41 119.7(3) . . ? C42 C41 C40 120.3(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C37 120.9(3) . . ? C41 C42 H42 119.5 . . ? C37 C42 H42 119.5 . . ? O2 C43 H43A 109.5 . . ? O2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O1 C44 H44A 109.5 . . ? O1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O1 P1 C37 100.87(11) . . ? O1 P1 S1 103.40(7) . . ? C37 P1 S1 112.15(9) . . ? O1 P1 S2 110.13(7) . . ? C37 P1 S2 109.92(9) . . ? S1 P1 S2 118.67(4) . . ? C44 O1 P1 118.90(16) . . ? C40 O2 C43 116.9(2) . . ? C50 C45 C46 118.1(3) . . ? C50 C45 P2 120.0(2) . . ? C46 C45 P2 121.9(2) . . ? C47 C46 C45 121.2(3) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C48 119.6(3) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? O4 C48 C49 123.8(3) . . ? O4 C48 C47 115.7(2) . . ? C49 C48 C47 120.4(3) . . ? C48 C49 C50 119.2(3) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? C45 C50 C49 121.4(3) . . ? C45 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? O4 C51 H51A 109.5 . . ? O4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O3 C52 H52A 109.5 . . ? O3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O3 P2 C45 105.19(12) . . ? O3 P2 S4 103.62(8) . . ? C45 P2 S4 109.86(10) . . ? O3 P2 S3 108.56(8) . . ? C45 P2 S3 109.15(9) . . ? S4 P2 S3 119.43(5) . . ? C52 O3 P2 119.98(19) . . ? C48 O4 C51 116.6(2) . . ? H5C O5 H5D 111(3) . . ? H6C O6 H6D 115(3) . . ? H7C O7 H7D 106(3) . . ? H8C O8 H8D 96(3) . . ? 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 H5C N12 0.838(10) 1.982(13) 2.799(3) 165(3) 4_565 O5 H5D O6 0.839(10) 2.022(16) 2.816(3) 158(3) . O6 H6C N6 0.843(10) 2.056(14) 2.875(3) 164(3) . O6 H6D O5 0.840(10) 1.911(12) 2.746(3) 172(3) 3_665 O7 H7C S3 0.968(10) 2.303(14) 3.249(3) 166(3) . O7 H7D O6 0.973(10) 1.879(17) 2.815(3) 161(4) . O8 H8C O7 0.976(10) 1.879(19) 2.791(4) 154(3) . O8 H8D S4 0.961(10) 2.537(18) 3.441(3) 157(3) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.104 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.075 data_03mbh055 _database_code_depnum_ccdc_archive 'CCDC 635250' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 Ni O4 P2 S4' _chemical_formula_weight 525.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.8112(7) _cell_length_b 10.7778(4) _cell_length_c 7.2354(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.160(2) _cell_angle_gamma 90.00 _cell_volume 1063.29(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2159 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7568 _exptl_absorpt_correction_T_max 0.7568 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _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 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8029 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2377 _reflns_number_gt 2017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1999)' _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^)+(0.0237P)^2^+0.5770P] 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 0.0067(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2377 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.79131(15) 0.07280(19) 0.2023(3) 0.0293(4) Uani 1 1 d . . . C2 C 0.87491(17) 0.00426(19) 0.2678(3) 0.0336(5) Uani 1 1 d . . . H2 H 0.8692 -0.0680 0.3356 0.040 Uiso 1 1 calc R . . C3 C 0.96676(16) 0.0412(2) 0.2342(3) 0.0343(5) Uani 1 1 d . . . H3 H 1.0221 -0.0056 0.2792 0.041 Uiso 1 1 calc R . . C4 C 0.97503(16) 0.1489(2) 0.1327(3) 0.0327(5) Uani 1 1 d . . . C5 C 0.89164(17) 0.2157(2) 0.0622(3) 0.0404(5) Uani 1 1 d . . . H5 H 0.8970 0.2864 -0.0091 0.048 Uiso 1 1 calc R . . C6 C 0.80089(17) 0.1786(2) 0.0967(3) 0.0382(5) Uani 1 1 d . . . H6 H 0.7455 0.2246 0.0490 0.046 Uiso 1 1 calc R . . C7 C 1.15001(18) 0.1399(3) 0.1809(4) 0.0515(6) Uani 1 1 d . . . H7A H 1.1548 0.1457 0.3144 0.077 Uiso 1 1 calc R . . H7B H 1.2047 0.1818 0.1419 0.077 Uiso 1 1 calc R . . H7C H 1.1505 0.0542 0.1449 0.077 Uiso 1 1 calc R . . C8 C 0.6336(2) -0.0101(3) 0.6011(4) 0.0581(8) Uani 1 1 d . . . H8A H 0.5855 0.0550 0.5894 0.087 Uiso 1 1 calc R . . H8B H 0.6652 -0.0157 0.7290 0.087 Uiso 1 1 calc R . . H8C H 0.6021 -0.0875 0.5636 0.087 Uiso 1 1 calc R . . O1 O 0.70648(11) 0.01733(15) 0.4819(2) 0.0418(4) Uani 1 1 d . . . O2 O 1.06090(11) 0.19620(15) 0.0938(2) 0.0448(4) Uani 1 1 d . . . P1 P 0.67523(4) 0.02950(5) 0.26193(8) 0.03155(15) Uani 1 1 d . . . S1 S 0.61741(5) -0.12626(5) 0.14084(9) 0.04526(18) Uani 1 1 d . . . S2 S 0.56880(4) 0.15296(5) 0.18368(8) 0.03817(16) Uani 1 1 d . . . Ni1 Ni 0.5000 0.0000 0.0000 0.02978(13) Uani 1 2 d S . . 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 0.0283(11) 0.0307(10) 0.0276(10) -0.0023(9) 0.0004(8) -0.0028(8) C2 0.0369(13) 0.0288(10) 0.0347(12) 0.0025(9) 0.0041(9) -0.0001(9) C3 0.0308(12) 0.0350(11) 0.0362(11) 0.0009(10) 0.0023(9) 0.0063(9) C4 0.0316(12) 0.0371(11) 0.0296(10) -0.0006(9) 0.0054(9) -0.0024(9) C5 0.0380(13) 0.0413(12) 0.0413(12) 0.0150(10) 0.0043(10) 0.0001(10) C6 0.0307(12) 0.0422(12) 0.0396(12) 0.0092(10) -0.0010(9) 0.0029(10) C7 0.0313(14) 0.0637(17) 0.0589(16) 0.0003(14) 0.0053(12) -0.0011(12) C8 0.0411(16) 0.086(2) 0.0500(15) 0.0205(14) 0.0167(13) 0.0029(14) O1 0.0291(9) 0.0629(11) 0.0326(8) 0.0070(7) 0.0025(7) -0.0046(7) O2 0.0312(9) 0.0526(10) 0.0514(10) 0.0094(8) 0.0088(7) -0.0032(7) P1 0.0256(3) 0.0331(3) 0.0337(3) 0.0012(2) -0.0021(2) -0.0029(2) S1 0.0349(3) 0.0288(3) 0.0655(4) 0.0005(3) -0.0122(3) -0.0011(2) S2 0.0299(3) 0.0331(3) 0.0485(3) -0.0046(2) -0.0031(2) 0.0012(2) Ni1 0.0225(2) 0.0295(2) 0.0356(2) 0.00013(16) -0.00090(16) -0.00148(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 1.389(3) . ? C1 C6 1.391(3) . ? C1 P1 1.787(2) . ? C2 C3 1.387(3) . ? C2 H2 0.9300 . ? C3 C4 1.388(3) . ? C3 H3 0.9300 . ? C4 O2 1.361(3) . ? C4 C5 1.385(3) . ? C5 C6 1.376(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O2 1.426(3) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O1 1.456(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? O1 P1 1.5868(16) . ? P1 S2 1.9967(8) . ? P1 S1 2.0002(8) . ? S1 Ni1 2.2347(6) . ? S2 Ni1 2.2327(5) . ? Ni1 S2 2.2327(5) 3_655 ? Ni1 S1 2.2347(6) 3_655 ? Ni1 P1 2.8442(5) 3_655 ? 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 118.5(2) . . ? C2 C1 P1 120.52(16) . . ? C6 C1 P1 120.95(16) . . ? C3 C2 C1 121.4(2) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 119.2(2) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? O2 C4 C5 115.48(19) . . ? O2 C4 C3 124.8(2) . . ? C5 C4 C3 119.7(2) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 120.5(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? 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 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C8 O1 P1 120.51(15) . . ? C4 O2 C7 117.93(18) . . ? O1 P1 C1 98.76(9) . . ? O1 P1 S2 114.20(7) . . ? C1 P1 S2 113.94(7) . . ? O1 P1 S1 113.32(7) . . ? C1 P1 S1 115.11(7) . . ? S2 P1 S1 102.16(3) . . ? P1 S1 Ni1 84.19(3) . . ? P1 S2 Ni1 84.32(3) . . ? S2 Ni1 S2 180.00(3) . 3_655 ? S2 Ni1 S1 91.77(2) . 3_655 ? S2 Ni1 S1 88.23(2) 3_655 3_655 ? S2 Ni1 S1 88.23(2) . . ? S2 Ni1 S1 91.77(2) 3_655 . ? S1 Ni1 S1 180.00(3) 3_655 . ? S2 Ni1 P1 135.688(18) . 3_655 ? S2 Ni1 P1 44.312(18) 3_655 3_655 ? S1 Ni1 P1 44.399(18) 3_655 3_655 ? S1 Ni1 P1 135.601(18) . 3_655 ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.226 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.056 #===END data_04slh008 _database_code_depnum_ccdc_archive 'CCDC 635251' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 I6 N12 Ni' _chemical_formula_weight 1444.78 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.7548(13) _cell_length_b 15.3966(19) _cell_length_c 25.220(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.758(9) _cell_angle_gamma 90.00 _cell_volume 4174.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 32062 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 4.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1912 _exptl_absorpt_correction_T_max 0.9076 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _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 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 33937 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9354 _reflns_number_gt 7156 _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. ; _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^)+(0.0348P)^2^+22.1652P] 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 9354 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.58996(7) 0.24687(5) 0.19280(3) 0.02084(16) Uani 1 1 d . . . N1 N 0.4453(5) 0.2648(3) 0.14353(19) 0.0231(11) Uani 1 1 d . . . N2 N 0.3486(5) 0.3407(3) 0.07224(19) 0.0238(11) Uani 1 1 d . . . N3 N 0.2350(5) 0.2370(3) 0.12333(19) 0.0234(11) Uani 1 1 d . . . N4 N 0.6508(5) 0.3465(3) 0.13906(19) 0.0232(10) Uani 1 1 d . . . N5 N 0.4588(4) 0.1522(3) 0.21873(18) 0.0210(10) Uani 1 1 d . . . N6 N 0.1285(5) 0.3772(3) 0.0171(2) 0.0290(12) Uani 1 1 d . . . N7 N 0.7320(4) 0.2380(3) 0.24462(18) 0.0206(10) Uani 1 1 d . . . N8 N 0.9275(5) 0.1783(3) 0.2683(2) 0.0247(11) Uani 1 1 d . . . N9 N 0.8294(4) 0.2836(3) 0.32398(19) 0.0234(11) Uani 1 1 d . . . N10 N 0.7077(5) 0.1524(3) 0.15850(19) 0.0231(10) Uani 1 1 d . . . N11 N 0.5361(5) 0.3294(3) 0.25727(19) 0.0236(11) Uani 1 1 d . . . N12 N 1.1290(5) 0.1782(4) 0.3377(2) 0.0357(13) Uani 1 1 d . . . C1 C 0.4453(6) 0.3232(4) 0.1047(2) 0.0216(12) Uani 1 1 d . . . C2 C 0.2446(5) 0.2956(4) 0.0838(2) 0.0230(12) Uani 1 1 d . . . C3 C 0.3403(5) 0.2230(4) 0.1511(2) 0.0226(12) Uani 1 1 d . . . C4 C 0.5664(5) 0.3689(4) 0.1005(2) 0.0215(12) Uani 1 1 d . . . C5 C 0.5912(6) 0.4278(4) 0.0615(2) 0.0275(14) Uani 1 1 d . . . H5 H 0.5295 0.4416 0.0351 0.033 Uiso 1 1 calc R . . C6 C 0.7068(7) 0.4671(4) 0.0609(3) 0.0351(16) Uani 1 1 d . . . H6 H 0.7261 0.5084 0.0344 0.042 Uiso 1 1 calc R . . C7 C 0.7934(6) 0.4441(4) 0.1003(3) 0.0326(15) Uani 1 1 d . . . H7 H 0.8737 0.4699 0.1010 0.039 Uiso 1 1 calc R . . C8 C 0.7636(6) 0.3842(4) 0.1384(2) 0.0262(13) Uani 1 1 d . . . H8 H 0.8244 0.3690 0.1649 0.031 Uiso 1 1 calc R . . C9 C 0.3454(5) 0.1592(4) 0.1950(2) 0.0233(12) Uani 1 1 d . . . C10 C 0.2446(6) 0.1106(5) 0.2097(3) 0.0332(15) Uani 1 1 d . . . H10 H 0.1659 0.1170 0.1919 0.040 Uiso 1 1 calc R . . C11 C 0.2608(6) 0.0518(5) 0.2513(3) 0.0363(16) Uani 1 1 d . . . H11 H 0.1931 0.0180 0.2631 0.044 Uiso 1 1 calc R . . C12 C 0.3761(6) 0.0439(4) 0.2745(3) 0.0319(15) Uani 1 1 d . . . H12 H 0.3899 0.0031 0.3023 0.038 Uiso 1 1 calc R . . C13 C 0.4732(6) 0.0950(4) 0.2580(2) 0.0275(13) Uani 1 1 d . . . H13 H 0.5527 0.0891 0.2751 0.033 Uiso 1 1 calc R . . C14 C 0.1306(6) 0.3093(4) 0.0505(2) 0.0256(13) Uani 1 1 d . . . C15 C 0.0334(6) 0.2514(5) 0.0543(3) 0.0377(17) Uani 1 1 d . . . H15 H 0.0397 0.2040 0.0783 0.045 Uiso 1 1 calc R . . C16 C -0.0737(6) 0.2625(5) 0.0228(3) 0.0422(18) Uani 1 1 d . . . H16 H -0.1419 0.2235 0.0247 0.051 Uiso 1 1 calc R . . C17 C -0.0771(7) 0.3331(5) -0.0115(3) 0.0402(17) Uani 1 1 d . . . H17 H -0.1483 0.3436 -0.0338 0.048 Uiso 1 1 calc R . . C18 C 0.0241(6) 0.3875(4) -0.0128(3) 0.0329(15) Uani 1 1 d . . . H18 H 0.0199 0.4355 -0.0365 0.040 Uiso 1 1 calc R . . C19 C 0.8270(5) 0.1842(4) 0.2361(2) 0.0205(12) Uani 1 1 d . . . C20 C 0.9239(6) 0.2306(4) 0.3114(2) 0.0245(13) Uani 1 1 d . . . C21 C 0.7351(5) 0.2840(4) 0.2892(2) 0.0212(12) Uani 1 1 d . . . C22 C 0.6217(5) 0.3350(4) 0.2980(2) 0.0231(12) Uani 1 1 d . . . C23 C 0.6004(6) 0.3791(4) 0.3441(2) 0.0304(14) Uani 1 1 d . . . H23 H 0.6624 0.3815 0.3717 0.036 Uiso 1 1 calc R . . C24 C 0.4880(6) 0.4197(5) 0.3496(3) 0.0346(16) Uani 1 1 d . . . H24 H 0.4716 0.4520 0.3807 0.042 Uiso 1 1 calc R . . C25 C 0.3988(6) 0.4130(4) 0.3091(2) 0.0317(15) Uani 1 1 d . . . H25 H 0.3189 0.4381 0.3129 0.038 Uiso 1 1 calc R . . C26 C 0.4270(6) 0.3696(4) 0.2632(3) 0.0285(14) Uani 1 1 d . . . H26 H 0.3669 0.3681 0.2348 0.034 Uiso 1 1 calc R . . C27 C 0.8126(5) 0.1332(4) 0.1874(2) 0.0236(13) Uani 1 1 d . . . C28 C 0.8941(5) 0.0691(4) 0.1731(3) 0.0285(14) Uani 1 1 d . . . H28 H 0.9649 0.0556 0.1950 0.034 Uiso 1 1 calc R . . C29 C 0.8711(6) 0.0250(5) 0.1265(3) 0.0340(16) Uani 1 1 d . . . H29 H 0.9258 -0.0196 0.1158 0.041 Uiso 1 1 calc R . . C30 C 0.7680(7) 0.0462(5) 0.0955(3) 0.0360(16) Uani 1 1 d . . . H30 H 0.7524 0.0179 0.0625 0.043 Uiso 1 1 calc R . . C31 C 0.6880(6) 0.1089(4) 0.1130(2) 0.0303(14) Uani 1 1 d . . . H31 H 0.6157 0.1220 0.0919 0.036 Uiso 1 1 calc R . . C32 C 1.0367(6) 0.2329(4) 0.3477(2) 0.0248(13) Uani 1 1 d . . . C33 C 1.0388(6) 0.2912(4) 0.3893(3) 0.0333(15) Uani 1 1 d . . . H33 H 0.9693 0.3274 0.3955 0.040 Uiso 1 1 calc R . . C34 C 1.1442(6) 0.2955(4) 0.4214(3) 0.0349(16) Uani 1 1 d . . . H34 H 1.1491 0.3354 0.4501 0.042 Uiso 1 1 calc R . . C35 C 1.2421(6) 0.2414(5) 0.4116(3) 0.0357(16) Uani 1 1 d . . . H35 H 1.3160 0.2436 0.4332 0.043 Uiso 1 1 calc R . . C36 C 1.2315(7) 0.1838(5) 0.3698(3) 0.0421(18) Uani 1 1 d . . . H36 H 1.2994 0.1462 0.3633 0.051 Uiso 1 1 calc R . . I1 I 0.06454(4) 0.38150(3) 0.22802(2) 0.04258(13) Uani 1 1 d . . . I2 I 0.21748(4) 0.49923(3) 0.163041(16) 0.02850(10) Uani 1 1 d . . . I3 I 0.37462(4) 0.61120(3) 0.103910(17) 0.03496(12) Uani 1 1 d . . . I4 I 0.57613(4) 0.20477(3) -0.015579(16) 0.03116(11) Uani 1 1 d . . . I5 I 0.37691(4) 0.09875(3) 0.024307(15) 0.02517(10) Uani 1 1 d . . . I6 I 0.16287(4) 0.00221(3) 0.05975(2) 0.03967(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0164(4) 0.0273(4) 0.0184(4) 0.0001(3) -0.0063(3) -0.0014(3) N1 0.019(3) 0.025(3) 0.025(3) 0.001(2) -0.008(2) -0.006(2) N2 0.023(3) 0.026(3) 0.022(2) -0.005(2) -0.008(2) -0.001(2) N3 0.019(3) 0.029(3) 0.021(2) -0.001(2) -0.005(2) -0.003(2) N4 0.020(3) 0.027(3) 0.022(2) -0.001(2) -0.005(2) -0.001(2) N5 0.019(3) 0.025(3) 0.019(2) -0.0023(19) -0.0028(19) 0.0027(19) N6 0.028(3) 0.032(3) 0.026(3) 0.001(2) -0.011(2) 0.003(2) N7 0.017(2) 0.026(3) 0.018(2) -0.0004(19) -0.0063(19) 0.0007(19) N8 0.019(3) 0.026(3) 0.029(3) -0.004(2) -0.004(2) -0.002(2) N9 0.014(2) 0.031(3) 0.025(3) -0.003(2) -0.003(2) -0.002(2) N10 0.022(3) 0.027(3) 0.020(2) 0.002(2) -0.003(2) -0.008(2) N11 0.020(3) 0.031(3) 0.019(2) 0.000(2) -0.003(2) -0.001(2) N12 0.022(3) 0.044(4) 0.041(3) -0.012(3) -0.007(2) 0.005(2) C1 0.024(3) 0.025(3) 0.016(3) -0.002(2) -0.001(2) 0.000(2) C2 0.019(3) 0.031(3) 0.019(3) -0.004(2) -0.004(2) 0.001(2) C3 0.021(3) 0.026(3) 0.020(3) -0.002(2) -0.005(2) -0.001(2) C4 0.022(3) 0.026(3) 0.016(3) -0.005(2) -0.002(2) 0.003(2) C5 0.029(3) 0.030(3) 0.023(3) 0.006(2) -0.008(3) 0.003(3) C6 0.034(4) 0.030(4) 0.041(4) 0.005(3) -0.001(3) -0.007(3) C7 0.027(4) 0.035(4) 0.036(4) -0.001(3) 0.001(3) -0.009(3) C8 0.018(3) 0.036(4) 0.025(3) -0.004(2) -0.004(2) -0.004(2) C9 0.013(3) 0.033(3) 0.023(3) 0.001(2) -0.004(2) -0.004(2) C10 0.021(3) 0.050(4) 0.027(3) 0.005(3) -0.008(3) -0.004(3) C11 0.027(4) 0.049(4) 0.032(4) 0.013(3) -0.006(3) -0.010(3) C12 0.038(4) 0.028(4) 0.030(3) 0.008(3) 0.001(3) -0.003(3) C13 0.029(3) 0.031(3) 0.022(3) 0.001(2) -0.007(3) 0.000(3) C14 0.021(3) 0.029(3) 0.027(3) -0.002(2) -0.009(3) 0.002(2) C15 0.028(4) 0.046(4) 0.038(4) 0.003(3) -0.019(3) 0.000(3) C16 0.018(3) 0.057(5) 0.051(5) 0.007(4) -0.008(3) -0.004(3) C17 0.028(4) 0.051(5) 0.040(4) -0.002(3) -0.019(3) 0.003(3) C18 0.030(4) 0.033(4) 0.035(4) 0.005(3) -0.010(3) 0.006(3) C19 0.017(3) 0.022(3) 0.021(3) 0.002(2) -0.006(2) -0.005(2) C20 0.021(3) 0.024(3) 0.028(3) 0.002(2) -0.003(3) -0.005(2) C21 0.019(3) 0.025(3) 0.019(3) 0.004(2) -0.003(2) -0.004(2) C22 0.016(3) 0.034(3) 0.019(3) 0.005(2) -0.003(2) 0.004(2) C23 0.034(4) 0.036(4) 0.021(3) -0.004(3) -0.006(3) 0.003(3) C24 0.034(4) 0.042(4) 0.027(3) -0.011(3) -0.003(3) 0.012(3) C25 0.031(4) 0.039(4) 0.025(3) 0.001(3) 0.000(3) 0.016(3) C26 0.022(3) 0.035(4) 0.028(3) 0.002(3) -0.009(3) 0.002(3) C27 0.016(3) 0.032(3) 0.023(3) -0.003(2) -0.004(2) -0.008(2) C28 0.010(3) 0.038(4) 0.037(4) -0.008(3) 0.005(3) -0.004(2) C29 0.019(3) 0.041(4) 0.042(4) -0.021(3) 0.011(3) -0.006(3) C30 0.036(4) 0.042(4) 0.031(4) -0.014(3) 0.009(3) -0.011(3) C31 0.032(4) 0.040(4) 0.019(3) 0.004(3) -0.005(3) -0.011(3) C32 0.021(3) 0.036(4) 0.017(3) -0.001(2) -0.008(2) -0.001(2) C33 0.031(4) 0.031(4) 0.037(4) -0.009(3) -0.012(3) 0.003(3) C34 0.030(4) 0.034(4) 0.040(4) -0.011(3) -0.016(3) -0.004(3) C35 0.027(4) 0.045(4) 0.034(4) -0.007(3) -0.018(3) -0.007(3) C36 0.025(4) 0.054(5) 0.047(4) -0.007(3) -0.016(3) 0.012(3) I1 0.0255(2) 0.0552(3) 0.0465(3) 0.0077(2) -0.0076(2) -0.0117(2) I2 0.0247(2) 0.0329(2) 0.0275(2) -0.00229(16) -0.00679(16) 0.00433(16) I3 0.0326(2) 0.0431(3) 0.0288(2) 0.00660(18) -0.00547(18) 0.00221(18) I4 0.0247(2) 0.0401(2) 0.0284(2) 0.00185(17) -0.00284(17) -0.00437(17) I5 0.0211(2) 0.0313(2) 0.02270(19) -0.00146(15) -0.00534(15) 0.00053(15) I6 0.0275(2) 0.0460(3) 0.0456(3) 0.0066(2) 0.0037(2) -0.00486(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.981(5) . ? Ni1 N7 1.985(5) . ? Ni1 N10 2.129(5) . ? Ni1 N5 2.145(5) . ? Ni1 N11 2.157(5) . ? Ni1 N4 2.162(5) . ? N1 C3 1.318(8) . ? N1 C1 1.330(7) . ? N2 C1 1.331(7) . ? N2 C2 1.356(8) . ? N3 C3 1.330(8) . ? N3 C2 1.350(8) . ? N4 C8 1.345(8) . ? N4 C4 1.355(7) . ? N5 C13 1.331(8) . ? N5 C9 1.346(7) . ? N6 C18 1.342(8) . ? N6 C14 1.342(8) . ? N7 C21 1.328(7) . ? N7 C19 1.338(7) . ? N8 C19 1.334(7) . ? N8 C20 1.354(8) . ? N9 C21 1.320(7) . ? N9 C20 1.350(8) . ? N11 C26 1.339(8) . ? N11 C22 1.360(7) . ? N10 C31 1.340(8) . ? N10 C27 1.357(8) . ? N12 C32 1.332(8) . ? N12 C36 1.350(9) . ? C1 C4 1.487(8) . ? C2 C14 1.481(8) . ? C3 C9 1.481(8) . ? C4 C5 1.369(8) . ? C5 C6 1.382(9) . ? C5 H5 0.9500 . ? C6 C7 1.386(10) . ? C6 H6 0.9500 . ? C7 C8 1.377(9) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.379(9) . ? C10 C11 1.392(9) . ? C10 H10 0.9500 . ? C11 C12 1.360(9) . ? C11 H11 0.9500 . ? C12 C13 1.382(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.380(9) . ? C15 C16 1.389(9) . ? C15 H15 0.9500 . ? C16 C17 1.388(11) . ? C16 H16 0.9500 . ? C17 C18 1.375(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C27 1.462(8) . ? C20 C32 1.498(8) . ? C21 C22 1.473(8) . ? C22 C23 1.372(9) . ? C23 C24 1.372(9) . ? C23 H23 0.9500 . ? C24 C25 1.383(9) . ? C24 H24 0.9500 . ? C25 C26 1.379(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.376(9) . ? C28 C29 1.372(9) . ? C28 H28 0.9500 . ? C29 C30 1.377(10) . ? C29 H29 0.9500 . ? C30 C31 1.375(10) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.379(9) . ? C33 C34 1.375(9) . ? C33 H33 0.9500 . ? C34 C35 1.371(10) . ? C34 H34 0.9500 . ? C35 C36 1.379(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? I1 I2 2.9735(7) . ? I2 I3 2.8648(7) . ? I4 I5 2.8982(6) . ? I5 I6 2.9041(7) . ? 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 Ni1 N7 175.5(2) . . ? N1 Ni1 N10 107.8(2) . . ? N7 Ni1 N10 76.41(19) . . ? N1 Ni1 N5 76.96(19) . . ? N7 Ni1 N5 104.64(19) . . ? N10 Ni1 N5 93.71(18) . . ? N1 Ni1 N11 99.6(2) . . ? N7 Ni1 N11 76.31(19) . . ? N10 Ni1 N11 152.31(19) . . ? N5 Ni1 N11 88.63(18) . . ? N1 Ni1 N4 75.82(19) . . ? N7 Ni1 N4 102.70(19) . . ? N10 Ni1 N4 91.99(19) . . ? N5 Ni1 N4 152.64(18) . . ? N11 Ni1 N4 98.51(19) . . ? C3 N1 C1 117.1(5) . . ? C3 N1 Ni1 120.1(4) . . ? C1 N1 Ni1 122.6(4) . . ? C1 N2 C2 113.5(5) . . ? C3 N3 C2 114.4(5) . . ? C8 N4 C4 117.7(5) . . ? C8 N4 Ni1 127.2(4) . . ? C4 N4 Ni1 114.9(4) . . ? C13 N5 C9 117.9(5) . . ? C13 N5 Ni1 127.9(4) . . ? C9 N5 Ni1 113.9(4) . . ? C18 N6 C14 116.2(6) . . ? C21 N7 C19 117.8(5) . . ? C21 N7 Ni1 121.3(4) . . ? C19 N7 Ni1 120.9(4) . . ? C19 N8 C20 113.9(5) . . ? C21 N9 C20 114.5(5) . . ? C26 N11 C22 117.6(5) . . ? C26 N11 Ni1 127.8(4) . . ? C22 N11 Ni1 114.5(4) . . ? C31 N10 C27 117.3(6) . . ? C31 N10 Ni1 127.5(4) . . ? C27 N10 Ni1 115.2(4) . . ? C32 N12 C36 116.5(6) . . ? N1 C1 N2 124.8(5) . . ? N1 C1 C4 113.1(5) . . ? N2 C1 C4 122.0(5) . . ? N3 C2 N2 125.7(5) . . ? N3 C2 C14 115.7(5) . . ? N2 C2 C14 118.6(5) . . ? N1 C3 N3 124.4(6) . . ? N1 C3 C9 114.8(5) . . ? N3 C3 C9 120.8(5) . . ? N4 C4 C5 122.9(6) . . ? N4 C4 C1 113.4(5) . . ? C5 C4 C1 123.7(5) . . ? C4 C5 C6 119.5(6) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 117.7(6) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C8 C7 C6 120.3(6) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? N4 C8 C7 121.9(6) . . ? N4 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? N5 C9 C10 123.1(6) . . ? N5 C9 C3 113.5(5) . . ? C10 C9 C3 123.4(5) . . ? C9 C10 C11 118.3(6) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 118.3(6) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C11 C12 C13 120.5(6) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? N5 C13 C12 121.9(6) . . ? N5 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? N6 C14 C15 123.3(6) . . ? N6 C14 C2 117.7(5) . . ? C15 C14 C2 118.9(6) . . ? C14 C15 C16 119.8(7) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 117.2(7) . . ? C17 C16 H16 121.4 . . ? C15 C16 H16 121.4 . . ? C18 C17 C16 119.1(6) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N6 C18 C17 124.3(6) . . ? N6 C18 H18 117.8 . . ? C17 C18 H18 117.8 . . ? N8 C19 N7 123.6(5) . . ? N8 C19 C27 122.5(5) . . ? N7 C19 C27 113.9(5) . . ? N9 C20 N8 126.1(5) . . ? N9 C20 C32 116.3(5) . . ? N8 C20 C32 117.6(5) . . ? N9 C21 N7 124.0(5) . . ? N9 C21 C22 121.7(5) . . ? N7 C21 C22 114.3(5) . . ? N11 C22 C23 122.9(6) . . ? N11 C22 C21 113.5(5) . . ? C23 C22 C21 123.5(5) . . ? C24 C23 C22 118.8(6) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 118.9(6) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 119.4(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? N11 C26 C25 122.2(6) . . ? N11 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? N10 C27 C28 122.8(6) . . ? N10 C27 C19 113.5(5) . . ? C28 C27 C19 123.6(6) . . ? C29 C28 C27 118.6(6) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? C28 C29 C30 119.4(6) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 119.0(6) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? N10 C31 C30 122.8(6) . . ? N10 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? N12 C32 C33 124.1(6) . . ? N12 C32 C20 117.6(5) . . ? C33 C32 C20 118.3(6) . . ? C34 C33 C32 118.3(6) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C35 C34 C33 119.2(6) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 118.9(6) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? N12 C36 C35 123.1(7) . . ? N12 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? I3 I2 I1 177.27(2) . . ? I4 I5 I6 175.23(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.451 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.193 #===END data_04slh012 _database_code_depnum_ccdc_archive 'CCDC 635252' __audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 Br4 N12 Ni2' _chemical_formula_weight 1061.73 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.215(5) _cell_length_b 8.5211(17) _cell_length_c 17.543(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.96(3) _cell_angle_gamma 90.00 _cell_volume 4062.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 26537 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description slab _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 4.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4405 _exptl_absorpt_correction_T_max 0.7574 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _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 17625 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4647 _reflns_number_gt 3902 _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. ; _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^)+(0.0409P)^2^+17.1620P] 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 4647 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 0.39597(13) 0.6253(4) -0.0085(2) 0.0205(7) Uani 1 1 d . . . C2 C 0.46474(14) 0.7574(4) 0.0274(2) 0.0226(7) Uani 1 1 d . . . C3 C 0.39657(13) 0.7962(4) 0.0916(2) 0.0200(7) Uani 1 1 d . . . C4 C 0.36539(14) 0.8746(4) 0.1462(2) 0.0206(7) Uani 1 1 d . . . C5 C 0.38314(14) 0.9870(4) 0.1975(2) 0.0240(8) Uani 1 1 d . . . H5 H 0.4170 1.0148 0.2001 0.029 Uiso 1 1 calc R . . C6 C 0.35045(16) 1.0584(4) 0.2451(2) 0.0268(8) Uani 1 1 d . . . H6 H 0.3613 1.1371 0.2804 0.032 Uiso 1 1 calc R . . C7 C 0.30171(15) 1.0119(4) 0.2396(2) 0.0247(8) Uani 1 1 d . . . H7 H 0.2786 1.0583 0.2715 0.030 Uiso 1 1 calc R . . C8 C 0.28684(14) 0.8976(4) 0.1876(2) 0.0213(7) Uani 1 1 d . . . H8 H 0.2533 0.8664 0.1847 0.026 Uiso 1 1 calc R . . C9 C 0.36499(14) 0.5184(4) -0.0563(2) 0.0208(7) Uani 1 1 d . . . C10 C 0.38093(15) 0.4465(4) -0.1209(2) 0.0272(8) Uani 1 1 d . . . H10 H 0.4131 0.4654 -0.1376 0.033 Uiso 1 1 calc R . . C11 C 0.34878(16) 0.3454(5) -0.1611(2) 0.0297(9) Uani 1 1 d . . . H11 H 0.3582 0.2961 -0.2067 0.036 Uiso 1 1 calc R . . C12 C 0.30298(15) 0.3184(5) -0.1334(2) 0.0270(8) Uani 1 1 d . . . H12 H 0.2810 0.2460 -0.1583 0.032 Uiso 1 1 calc R . . C13 C 0.28932(14) 0.3976(4) -0.0689(2) 0.0235(8) Uani 1 1 d . . . H13 H 0.2575 0.3797 -0.0509 0.028 Uiso 1 1 calc R . . C14 C 0.51747(14) 0.7935(4) 0.0161(2) 0.0259(8) Uani 1 1 d . . . C15 C 0.53888(14) 0.7276(4) -0.0447(2) 0.0250(8) Uani 1 1 d . . . H15 H 0.5208 0.6597 -0.0787 0.030 Uiso 1 1 calc R . . C16 C 0.58703(16) 0.7618(5) -0.0553(3) 0.0354(10) Uani 1 1 d . . . H16 H 0.6026 0.7186 -0.0978 0.042 Uiso 1 1 calc R . . C17 C 0.61311(15) 0.8579(5) -0.0054(3) 0.0329(9) Uani 1 1 d . . . H17 H 0.6468 0.8803 -0.0126 0.039 Uiso 1 1 calc R . . C18 C 0.58998(15) 0.9216(5) 0.0554(3) 0.0323(9) Uani 1 1 d . . . H18 H 0.6079 0.9895 0.0896 0.039 Uiso 1 1 calc R . . N1 N 0.37266(11) 0.6906(4) 0.04815(17) 0.0201(6) Uani 1 1 d . . . N2 N 0.44257(12) 0.6561(4) -0.02167(18) 0.0235(7) Uani 1 1 d . . . N3 N 0.44364(11) 0.8319(4) 0.08438(18) 0.0230(6) Uani 1 1 d . . . N4 N 0.31760(11) 0.8297(4) 0.14149(17) 0.0201(6) Uani 1 1 d . . . N5 N 0.31912(11) 0.4978(3) -0.03126(17) 0.0201(6) Uani 1 1 d . . . N6 N 0.54202(14) 0.8893(4) 0.0672(2) 0.0376(9) Uani 1 1 d . . . Ni1 Ni 0.301891(16) 0.65032(5) 0.05823(3) 0.01892(12) Uani 1 1 d . . . Br1 Br 0.314471(14) 0.44098(4) 0.15888(2) 0.02578(11) Uani 1 1 d . . . Br2 Br 0.211275(13) 0.63240(4) 0.05333(2) 0.02149(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 0.0165(18) 0.0228(18) 0.0223(18) 0.0015(14) 0.0020(14) 0.0018(14) C2 0.0159(17) 0.0240(18) 0.0281(19) 0.0051(15) 0.0026(14) 0.0007(14) C3 0.0171(17) 0.0226(18) 0.0202(17) 0.0021(14) 0.0007(13) -0.0009(14) C4 0.0186(18) 0.0222(17) 0.0210(17) 0.0029(13) 0.0004(14) -0.0003(14) C5 0.0201(19) 0.0278(19) 0.0241(18) -0.0007(15) 0.0020(15) -0.0024(15) C6 0.035(2) 0.0240(19) 0.0216(18) -0.0008(15) 0.0001(16) 0.0003(16) C7 0.028(2) 0.0241(18) 0.0223(18) 0.0022(14) 0.0069(15) 0.0040(16) C8 0.0188(18) 0.0265(18) 0.0188(17) 0.0025(14) 0.0041(14) 0.0017(14) C9 0.0200(18) 0.0197(17) 0.0231(18) 0.0025(14) 0.0030(14) -0.0008(14) C10 0.025(2) 0.028(2) 0.029(2) -0.0014(16) 0.0048(16) 0.0014(16) C11 0.034(2) 0.031(2) 0.0246(19) -0.0076(16) 0.0046(17) 0.0003(17) C12 0.027(2) 0.0259(19) 0.0269(19) -0.0057(15) -0.0068(16) -0.0005(16) C13 0.0202(19) 0.0252(18) 0.0247(18) 0.0034(15) -0.0015(15) -0.0018(15) C14 0.0178(19) 0.0250(19) 0.035(2) 0.0019(16) 0.0010(15) -0.0020(15) C15 0.0157(18) 0.0255(19) 0.034(2) 0.0002(16) 0.0062(15) -0.0019(15) C16 0.030(2) 0.033(2) 0.044(2) 0.0028(19) 0.0099(19) 0.0035(18) C17 0.018(2) 0.034(2) 0.047(3) 0.0126(19) 0.0040(18) -0.0028(16) C18 0.021(2) 0.034(2) 0.042(2) 0.0050(18) -0.0048(18) -0.0053(17) N1 0.0155(15) 0.0241(15) 0.0206(15) -0.0004(12) -0.0002(12) -0.0009(12) N2 0.0185(16) 0.0241(16) 0.0280(16) -0.0029(13) 0.0032(13) -0.0013(12) N3 0.0151(15) 0.0266(16) 0.0273(16) -0.0019(13) 0.0015(13) -0.0008(12) N4 0.0163(15) 0.0217(15) 0.0222(15) 0.0023(12) -0.0003(12) -0.0005(12) N5 0.0180(15) 0.0211(15) 0.0211(15) -0.0004(12) 0.0017(12) -0.0009(12) N6 0.0264(19) 0.042(2) 0.045(2) 0.0056(17) 0.0031(17) -0.0025(16) Ni1 0.0130(2) 0.0232(2) 0.0207(2) -0.00069(17) 0.00193(18) -0.00144(17) Br1 0.0214(2) 0.0294(2) 0.0269(2) 0.00555(15) 0.00437(15) 0.00242(15) Br2 0.01444(18) 0.0259(2) 0.02414(19) 0.00325(13) 0.00150(13) -0.00273(13) _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 N2 1.327(5) . ? C1 N1 1.328(5) . ? C1 C9 1.474(5) . ? C2 N2 1.340(5) . ? C2 N3 1.339(5) . ? C2 C14 1.490(5) . ? C3 N1 1.328(5) . ? C3 N3 1.329(5) . ? C3 C4 1.472(5) . ? C4 N4 1.354(5) . ? C4 C5 1.384(5) . ? C5 C6 1.391(5) . ? C5 H5 0.9500 . ? C6 C7 1.383(6) . ? C6 H6 0.9500 . ? C7 C8 1.381(5) . ? C7 H7 0.9500 . ? C8 N4 1.326(5) . ? C8 H8 0.9500 . ? C9 N5 1.356(5) . ? C9 C10 1.378(5) . ? C10 C11 1.393(6) . ? C10 H10 0.9500 . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 C13 1.384(5) . ? C12 H12 0.9500 . ? C13 N5 1.330(5) . ? C13 H13 0.9500 . ? C14 N6 1.362(5) . ? C14 C15 1.362(6) . ? C15 C16 1.365(6) . ? C15 H15 0.9500 . ? C16 C17 1.370(6) . ? C16 H16 0.9500 . ? C17 C18 1.377(6) . ? C17 H17 0.9500 . ? C18 N6 1.361(6) . ? C18 H18 0.9500 . ? N1 Ni1 1.973(3) . ? N4 Ni1 2.142(3) . ? N5 Ni1 2.109(3) . ? Ni1 Br2 2.4679(8) . ? Ni1 Br1 2.5208(7) . ? Ni1 Br2 2.7045(7) 7_565 ? Br2 Ni1 2.7045(7) 7_565 ? 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 N2 C1 N1 123.0(3) . . ? N2 C1 C9 123.2(3) . . ? N1 C1 C9 113.8(3) . . ? N2 C2 N3 126.1(3) . . ? N2 C2 C14 116.9(3) . . ? N3 C2 C14 117.0(3) . . ? N1 C3 N3 123.1(3) . . ? N1 C3 C4 113.5(3) . . ? N3 C3 C4 123.3(3) . . ? N4 C4 C5 122.5(3) . . ? N4 C4 C3 114.6(3) . . ? C5 C4 C3 122.9(3) . . ? C4 C5 C6 118.7(4) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 118.3(4) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C8 C7 C6 119.7(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? N4 C8 C7 122.5(4) . . ? N4 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? N5 C9 C10 122.9(3) . . ? N5 C9 C1 113.9(3) . . ? C10 C9 C1 123.2(3) . . ? C9 C10 C11 118.4(4) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 119.5(4) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? N5 C13 C12 122.4(4) . . ? N5 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? N6 C14 C15 123.2(4) . . ? N6 C14 C2 118.7(4) . . ? C15 C14 C2 118.2(3) . . ? C14 C15 C16 118.2(4) . . ? C14 C15 H15 120.9 . . ? C16 C15 H15 120.9 . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 119.2(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? N6 C18 C17 121.3(4) . . ? N6 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C1 N1 C3 118.3(3) . . ? C1 N1 Ni1 120.0(2) . . ? C3 N1 Ni1 121.2(2) . . ? C1 N2 C2 114.7(3) . . ? C3 N3 C2 114.6(3) . . ? C8 N4 C4 118.3(3) . . ? C8 N4 Ni1 128.1(3) . . ? C4 N4 Ni1 113.6(2) . . ? C13 N5 C9 118.1(3) . . ? C13 N5 Ni1 127.7(3) . . ? C9 N5 Ni1 113.9(2) . . ? C18 N6 C14 117.6(4) . . ? N1 Ni1 N5 77.59(12) . . ? N1 Ni1 N4 77.03(12) . . ? N5 Ni1 N4 154.55(12) . . ? N1 Ni1 Br2 170.35(9) . . ? N5 Ni1 Br2 101.30(9) . . ? N4 Ni1 Br2 103.41(9) . . ? N1 Ni1 Br1 95.04(9) . . ? N5 Ni1 Br1 93.32(8) . . ? N4 Ni1 Br1 90.70(8) . . ? Br2 Ni1 Br1 94.59(3) . . ? N1 Ni1 Br2 84.81(9) . 7_565 ? N5 Ni1 Br2 84.81(8) . 7_565 ? N4 Ni1 Br2 91.10(8) . 7_565 ? Br2 Ni1 Br2 85.54(3) . 7_565 ? Br1 Ni1 Br2 178.11(2) . 7_565 ? Ni1 Br2 Ni1 94.46(3) . 7_565 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.937 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.125