data_mn1701 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Et4N)2[Ni(DMF)2{Ni(PhPepS)}2] _chemical_melting_point ? _chemical_formula_moiety 'C46 H38 N6 Ni3 O6 S4, 2(C8 H20 N)' _chemical_formula_sum 'C62 H78 N8 Ni3 O6 S4' _chemical_formula_weight 1335.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.2141(15) _cell_length_b 15.5332(17) _cell_length_c 16.2978(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.638(3) _cell_angle_gamma 90.00 _cell_volume 3064.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 876 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 20.0 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28697 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 1.68 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5605 _reflns_number_gt 3681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.054 (Bruker, 2002)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT 6.45A (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL-97 _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. There are two sets of positions for the atoms of the Et4N group, and the occupancy of the major part is 0.550(7). The DMF group is also disordered, with a common O and N atom but split positions for the remainder. The major part (part "b") has a refined occupancy of 0.515(10). Some distance restraints were included to set the geometry of the disordered groups. ; _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^)+(0.0171P)^2^+17.8364P] 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 5605 _refine_ls_number_parameters 366 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.001 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 0.21432(6) 0.14066(5) 0.03816(5) 0.0336(2) Uani 1 1 d . . . Ni2 Ni 0.0000 0.0000 0.0000 0.0436(4) Uani 1 2 d S . . S1 S 0.19433(12) 0.00278(10) 0.05928(10) 0.0380(4) Uani 1 1 d . . . S2 S 0.06746(12) 0.13599(11) -0.05123(10) 0.0390(4) Uani 1 1 d . . . O1 O 0.4796(5) 0.1111(4) 0.2199(3) 0.081(2) Uani 1 1 d . . . O2 O 0.1965(4) 0.4030(3) 0.0196(4) 0.0626(15) Uani 1 1 d . . . N1 N 0.3511(4) 0.1452(3) 0.1085(3) 0.0359(12) Uani 1 1 d . . . N2 N 0.2386(4) 0.2593(3) 0.0203(3) 0.0353(12) Uani 1 1 d . . . C1 C 0.2174(5) 0.0000(4) 0.1689(4) 0.0452(17) Uani 1 1 d . . . C2 C 0.1491(6) -0.0512(5) 0.2111(5) 0.054(2) Uani 1 1 d . . . H2 H 0.0912 -0.0833 0.1806 0.064 Uiso 1 1 calc R . . C3 C 0.1646(8) -0.0557(6) 0.2967(5) 0.078(3) Uani 1 1 d . . . H3 H 0.1160 -0.0893 0.3246 0.094 Uiso 1 1 calc R . . C4 C 0.2503(9) -0.0116(7) 0.3414(5) 0.099(4) Uani 1 1 d . . . H4 H 0.2618 -0.0148 0.4001 0.119 Uiso 1 1 calc R . . C5 C 0.3192(8) 0.0372(7) 0.2998(5) 0.091(4) Uani 1 1 d . . . H5 H 0.3792 0.0664 0.3309 0.109 Uiso 1 1 calc R . . C6 C 0.3042(6) 0.0454(5) 0.2140(4) 0.059(2) Uani 1 1 d . . . C7 C 0.3863(6) 0.1030(5) 0.1785(4) 0.054(2) Uani 1 1 d . . . C8 C 0.4162(5) 0.2116(4) 0.0797(4) 0.0327(14) Uani 1 1 d . . . C9 C 0.5313(5) 0.2190(4) 0.0941(4) 0.0402(15) Uani 1 1 d . . . H9 H 0.5739 0.1766 0.1260 0.048 Uiso 1 1 calc R . . C10 C 0.5832(5) 0.2885(5) 0.0617(4) 0.0478(18) Uani 1 1 d . . . H10 H 0.6614 0.2933 0.0711 0.057 Uiso 1 1 calc R . . C11 C 0.5211(5) 0.3507(5) 0.0157(4) 0.0453(17) Uani 1 1 d . . . H11 H 0.5570 0.3978 -0.0066 0.054 Uiso 1 1 calc R . . C12 C 0.4075(5) 0.3447(4) 0.0020(4) 0.0398(15) Uani 1 1 d . . . H12 H 0.3655 0.3882 -0.0287 0.048 Uiso 1 1 calc R . . C13 C 0.3544(5) 0.2752(4) 0.0332(4) 0.0333(14) Uani 1 1 d . . . C14 C 0.1666(5) 0.3261(4) 0.0121(4) 0.0397(16) Uani 1 1 d . . . C15 C 0.0444(5) 0.3092(4) -0.0061(4) 0.0376(15) Uani 1 1 d . . . C16 C -0.0230(5) 0.3802(4) 0.0030(4) 0.0440(17) Uani 1 1 d . . . H16 H 0.0102 0.4322 0.0245 0.053 Uiso 1 1 calc R . . C17 C -0.1364(5) 0.3776(4) -0.0180(4) 0.0446(17) Uani 1 1 d . . . H17 H -0.1801 0.4270 -0.0110 0.054 Uiso 1 1 calc R . . C18 C -0.1853(5) 0.3020(4) -0.0495(4) 0.0416(16) Uani 1 1 d . . . H18 H -0.2629 0.2997 -0.0660 0.050 Uiso 1 1 calc R . . C19 C -0.1213(5) 0.2306(4) -0.0569(3) 0.0337(14) Uani 1 1 d . . . H19 H -0.1562 0.1788 -0.0776 0.040 Uiso 1 1 calc R . . C20 C -0.0068(5) 0.2311(4) -0.0351(4) 0.0345(14) Uani 1 1 d . . . O3 O -0.0533(5) 0.0518(4) 0.1043(4) 0.097(3) Uani 1 1 d . . . N3 N -0.0825(5) 0.1471(4) 0.2020(3) 0.0512(16) Uani 1 1 d . . . C21 C -0.0304(12) 0.1125(8) 0.1392(7) 0.030(3) Uiso 0.485(10) 1 d P A 1 H21 H 0.0310 0.1435 0.1242 0.036 Uiso 0.485(10) 1 calc PR A 1 C22 C -0.1936(13) 0.1622(11) 0.1949(10) 0.059(5) Uiso 0.485(10) 1 d P A 1 H22A H -0.2121 0.1864 0.2469 0.088 Uiso 0.485(10) 1 calc PR A 1 H22B H -0.2337 0.1080 0.1830 0.088 Uiso 0.485(10) 1 calc PR A 1 H22C H -0.2147 0.2031 0.1497 0.088 Uiso 0.485(10) 1 calc PR A 1 C23 C -0.0101(15) 0.1926(12) 0.2651(11) 0.076(6) Uiso 0.485(10) 1 d P A 1 H23A H -0.0533 0.2152 0.3069 0.113 Uiso 0.485(10) 1 calc PR A 1 H23B H 0.0256 0.2404 0.2397 0.113 Uiso 0.485(10) 1 calc PR A 1 H23C H 0.0464 0.1530 0.2915 0.113 Uiso 0.485(10) 1 calc PR A 1 C21B C -0.0896(12) 0.1077(8) 0.1290(8) 0.035(3) Uiso 0.515(10) 1 d P A 2 H21B H -0.1394 0.1363 0.0881 0.043 Uiso 0.515(10) 1 calc PR A 2 C22B C -0.1310(15) 0.2276(12) 0.2180(11) 0.079(6) Uiso 0.515(10) 1 d P A 2 H22D H -0.1124 0.2421 0.2767 0.118 Uiso 0.515(10) 1 calc PR A 2 H22E H -0.2114 0.2237 0.2041 0.118 Uiso 0.515(10) 1 calc PR A 2 H22F H -0.1025 0.2723 0.1841 0.118 Uiso 0.515(10) 1 calc PR A 2 C23B C -0.0439(10) 0.0946(8) 0.2825(7) 0.037(3) Uiso 0.515(10) 1 d P A 2 H23D H -0.0425 0.1323 0.3308 0.056 Uiso 0.515(10) 1 calc PR A 2 H23E H 0.0303 0.0715 0.2801 0.056 Uiso 0.515(10) 1 calc PR A 2 H23F H -0.0954 0.0470 0.2872 0.056 Uiso 0.515(10) 1 calc PR A 2 N4 N 0.6416(7) 0.8635(6) 0.2205(5) 0.035(2) Uiso 0.550(7) 1 d PD B 1 C24 C 0.6899(9) 0.7741(7) 0.2461(7) 0.041(3) Uiso 0.550(7) 1 d PD B 1 H24A H 0.7113 0.7749 0.3069 0.049 Uiso 0.550(7) 1 calc PR B 1 H24B H 0.6294 0.7316 0.2345 0.049 Uiso 0.550(7) 1 calc PR B 1 C25 C 0.7866(9) 0.7409(8) 0.2081(8) 0.046(3) Uiso 0.550(7) 1 d PD B 1 H25A H 0.8077 0.6841 0.2311 0.069 Uiso 0.550(7) 1 calc PR B 1 H25B H 0.8489 0.7807 0.2202 0.069 Uiso 0.550(7) 1 calc PR B 1 H25C H 0.7666 0.7361 0.1480 0.069 Uiso 0.550(7) 1 calc PR B 1 C26 C 0.5259(8) 0.8686(8) 0.2463(7) 0.032(3) Uiso 0.550(7) 1 d PD B 1 H26A H 0.5312 0.8531 0.3056 0.038 Uiso 0.550(7) 1 calc PR B 1 H26B H 0.5006 0.9291 0.2408 0.038 Uiso 0.550(7) 1 calc PR B 1 C27 C 0.4378(13) 0.8118(11) 0.1981(10) 0.032(4) Uiso 0.550(7) 1 d PD B 1 H27A H 0.3669 0.8212 0.2185 0.047 Uiso 0.550(7) 1 calc PR B 1 H27B H 0.4592 0.7512 0.2056 0.047 Uiso 0.550(7) 1 calc PR B 1 H27C H 0.4309 0.8265 0.1391 0.047 Uiso 0.550(7) 1 calc PR B 1 C28 C 0.6418(15) 0.8678(11) 0.1299(9) 0.053(5) Uiso 0.550(7) 1 d PD B 1 H28A H 0.6013 0.8174 0.1039 0.063 Uiso 0.550(7) 1 calc PR B 1 H28B H 0.7190 0.8642 0.1178 0.063 Uiso 0.550(7) 1 calc PR B 1 C29 C 0.5876(12) 0.9525(9) 0.0895(9) 0.046(4) Uiso 0.550(7) 1 d PD B 1 H29A H 0.5897 0.9512 0.0297 0.069 Uiso 0.550(7) 1 calc PR B 1 H29B H 0.6287 1.0027 0.1135 0.069 Uiso 0.550(7) 1 calc PR B 1 H29C H 0.5107 0.9562 0.1004 0.069 Uiso 0.550(7) 1 calc PR B 1 C30 C 0.7041(9) 0.9353(8) 0.2714(8) 0.046(3) Uiso 0.550(7) 1 d PD B 1 H30A H 0.6932 0.9273 0.3300 0.056 Uiso 0.550(7) 1 calc PR B 1 H30B H 0.6696 0.9909 0.2529 0.056 Uiso 0.550(7) 1 calc PR B 1 C31 C 0.8286(10) 0.9424(10) 0.2675(9) 0.068(4) Uiso 0.550(7) 1 d PD B 1 H31A H 0.8589 0.9911 0.3014 0.102 Uiso 0.550(7) 1 calc PR B 1 H31B H 0.8414 0.9513 0.2100 0.102 Uiso 0.550(7) 1 calc PR B 1 H31C H 0.8652 0.8892 0.2887 0.102 Uiso 0.550(7) 1 calc PR B 1 N4B N 0.6129(8) 0.9054(7) 0.2172(6) 0.026(3) Uiso 0.450(7) 1 d P B 2 C24B C 0.6562(13) 0.9924(10) 0.2461(10) 0.049(4) Uiso 0.450(7) 1 d P B 2 H24C H 0.6149 1.0368 0.2110 0.059 Uiso 0.450(7) 1 calc PR B 2 H24D H 0.7345 0.9963 0.2368 0.059 Uiso 0.450(7) 1 calc PR B 2 C25B C 0.6491(13) 1.0143(10) 0.3368(9) 0.048(4) Uiso 0.450(7) 1 d P B 2 H25D H 0.6796 1.0719 0.3492 0.072 Uiso 0.450(7) 1 calc PR B 2 H25E H 0.6914 0.9719 0.3726 0.072 Uiso 0.450(7) 1 calc PR B 2 H25F H 0.5716 1.0130 0.3466 0.072 Uiso 0.450(7) 1 calc PR B 2 C26B C 0.627(2) 0.8922(15) 0.1292(13) 0.057(6) Uiso 0.450(7) 1 d P B 2 H26C H 0.6139 0.8309 0.1147 0.068 Uiso 0.450(7) 1 calc PR B 2 H26D H 0.7043 0.9060 0.1215 0.068 Uiso 0.450(7) 1 calc PR B 2 C27B C 0.5489(17) 0.9478(13) 0.0710(12) 0.056(5) Uiso 0.450(7) 1 d P B 2 H27D H 0.5613 0.9372 0.0137 0.083 Uiso 0.450(7) 1 calc PR B 2 H27E H 0.5626 1.0087 0.0845 0.083 Uiso 0.450(7) 1 calc PR B 2 H27F H 0.4724 0.9334 0.0774 0.083 Uiso 0.450(7) 1 calc PR B 2 C28B C 0.4935(14) 0.8957(11) 0.2302(10) 0.043(4) Uiso 0.450(7) 1 d P B 2 H28C H 0.4548 0.9502 0.2134 0.052 Uiso 0.450(7) 1 calc PR B 2 H28D H 0.4907 0.8881 0.2902 0.052 Uiso 0.450(7) 1 calc PR B 2 C29B C 0.430(3) 0.822(2) 0.185(2) 0.111(15) Uiso 0.450(7) 1 d P B 2 H29D H 0.3530 0.8237 0.1961 0.166 Uiso 0.450(7) 1 calc PR B 2 H29E H 0.4636 0.7675 0.2033 0.166 Uiso 0.450(7) 1 calc PR B 2 H29F H 0.4313 0.8289 0.1249 0.166 Uiso 0.450(7) 1 calc PR B 2 C30B C 0.6805(12) 0.8324(10) 0.2707(10) 0.046(4) Uiso 0.450(7) 1 d P B 2 H30C H 0.6621 0.8354 0.3280 0.055 Uiso 0.450(7) 1 calc PR B 2 H30D H 0.6555 0.7756 0.2478 0.055 Uiso 0.450(7) 1 calc PR B 2 C31B C 0.8018(13) 0.8373(11) 0.2739(11) 0.058(5) Uiso 0.450(7) 1 d P B 2 H31D H 0.8362 0.7901 0.3080 0.087 Uiso 0.450(7) 1 calc PR B 2 H31E H 0.8282 0.8925 0.2980 0.087 Uiso 0.450(7) 1 calc PR B 2 H31F H 0.8216 0.8325 0.2177 0.087 Uiso 0.450(7) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0275(4) 0.0338(4) 0.0406(5) -0.0212(4) 0.0092(3) -0.0031(3) Ni2 0.0311(6) 0.0455(7) 0.0565(8) -0.0397(6) 0.0142(6) -0.0076(5) S1 0.0334(8) 0.0359(9) 0.0464(10) -0.0201(7) 0.0121(7) -0.0057(7) S2 0.0290(8) 0.0409(9) 0.0478(10) -0.0272(8) 0.0082(7) -0.0009(7) O1 0.070(4) 0.125(5) 0.041(3) 0.027(3) -0.015(3) -0.062(4) O2 0.042(3) 0.034(3) 0.113(5) -0.018(3) 0.018(3) -0.004(2) N1 0.034(3) 0.042(3) 0.034(3) -0.015(2) 0.012(2) -0.012(2) N2 0.028(3) 0.034(3) 0.045(3) -0.020(2) 0.010(2) -0.002(2) C1 0.045(4) 0.046(4) 0.048(4) -0.018(3) 0.016(3) -0.010(3) C2 0.057(5) 0.056(5) 0.054(5) -0.020(4) 0.028(4) -0.022(4) C3 0.091(7) 0.090(7) 0.060(6) -0.018(5) 0.037(5) -0.053(5) C4 0.127(9) 0.130(9) 0.043(5) -0.008(5) 0.024(5) -0.086(7) C5 0.111(8) 0.127(9) 0.035(5) -0.007(5) 0.010(5) -0.084(7) C6 0.064(5) 0.080(6) 0.035(4) -0.004(4) 0.011(4) -0.037(4) C7 0.055(5) 0.072(5) 0.035(4) 0.002(4) 0.007(4) -0.029(4) C8 0.034(3) 0.041(4) 0.025(3) -0.008(3) 0.008(3) -0.007(3) C9 0.032(3) 0.059(4) 0.030(3) 0.001(3) 0.005(3) -0.006(3) C10 0.033(4) 0.072(5) 0.041(4) 0.011(4) 0.013(3) -0.005(3) C11 0.042(4) 0.057(4) 0.041(4) 0.008(3) 0.018(3) -0.008(3) C12 0.043(4) 0.038(4) 0.040(4) -0.004(3) 0.012(3) -0.001(3) C13 0.028(3) 0.041(4) 0.032(3) -0.014(3) 0.010(3) 0.000(3) C14 0.032(3) 0.036(4) 0.052(4) -0.015(3) 0.011(3) -0.004(3) C15 0.031(3) 0.044(4) 0.040(4) -0.013(3) 0.012(3) 0.004(3) C16 0.046(4) 0.044(4) 0.043(4) -0.025(3) 0.011(3) 0.004(3) C17 0.037(4) 0.055(4) 0.042(4) -0.018(3) 0.008(3) 0.020(3) C18 0.029(3) 0.058(4) 0.039(4) -0.017(3) 0.012(3) 0.002(3) C19 0.032(3) 0.042(4) 0.028(3) -0.010(3) 0.007(3) -0.005(3) C20 0.032(3) 0.041(4) 0.032(3) -0.010(3) 0.012(3) -0.001(3) O3 0.086(4) 0.091(4) 0.128(5) -0.099(4) 0.072(4) -0.045(4) N3 0.068(4) 0.043(3) 0.042(3) -0.027(3) 0.006(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.895(5) . ? Ni1 N1 1.898(5) . ? Ni1 S2 2.1565(18) . ? Ni1 S1 2.1880(18) . ? Ni2 O3 2.063(5) 3 ? Ni2 O3 2.063(5) . ? Ni2 S1 2.4412(16) 3 ? Ni2 S1 2.4412(16) . ? Ni2 S2 2.4537(18) . ? Ni2 S2 2.4538(18) 3 ? S1 C1 1.772(7) . ? S2 C20 1.771(6) . ? O1 C7 1.251(8) . ? O2 C14 1.250(7) . ? N1 C7 1.336(9) . ? N1 C8 1.421(7) . ? N2 C14 1.355(8) . ? N2 C13 1.424(7) . ? C1 C2 1.396(9) . ? C1 C6 1.398(9) . ? C2 C3 1.385(10) . ? C2 H2 0.9500 . ? C3 C4 1.375(11) . ? C3 H3 0.9500 . ? C4 C5 1.375(10) . ? C4 H4 0.9500 . ? C5 C6 1.393(10) . ? C5 H5 0.9500 . ? C6 C7 1.515(9) . ? C8 C9 1.399(8) . ? C8 C13 1.402(9) . ? C9 C10 1.391(9) . ? C9 H9 0.9500 . ? C10 C11 1.386(9) . ? C10 H10 0.9500 . ? C11 C12 1.378(9) . ? C11 H11 0.9500 . ? C12 C13 1.390(8) . ? C12 H12 0.9500 . ? C14 C15 1.505(8) . ? C15 C16 1.396(8) . ? C15 C20 1.418(8) . ? C16 C17 1.382(9) . ? C16 H16 0.9500 . ? C17 C18 1.385(9) . ? C17 H17 0.9500 . ? C18 C19 1.372(8) . ? C18 H18 0.9500 . ? C19 C20 1.397(8) . ? C19 H19 0.9500 . ? O3 C21B 1.078(13) . ? O3 C21 1.118(13) . ? N3 C21B 1.331(13) . ? N3 C22 1.367(16) . ? N3 C21 1.383(13) . ? N3 C22B 1.422(18) . ? N3 C23 1.448(18) . ? N3 C23B 1.564(13) . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C21B H21B 0.9500 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? N4 C28 1.479(14) . ? N4 C26 1.529(12) . ? N4 C30 1.532(12) . ? N4 C24 1.544(12) . ? C24 C25 1.498(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.525(14) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.576(15) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.535(14) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N4B C26B 1.48(2) . ? N4B C24B 1.503(18) . ? N4B C28B 1.509(18) . ? N4B C30B 1.593(18) . ? C24B C25B 1.53(2) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26B C27B 1.52(3) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28B C29B 1.52(4) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B C31B 1.48(2) . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? 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 Ni1 N1 85.1(2) . . ? N2 Ni1 S2 93.56(16) . . ? N1 Ni1 S2 174.77(16) . . ? N2 Ni1 S1 177.42(15) . . ? N1 Ni1 S1 92.79(17) . . ? S2 Ni1 S1 88.46(7) . . ? O3 Ni2 O3 180.00(18) 3 . ? O3 Ni2 S1 93.65(18) 3 3 ? O3 Ni2 S1 86.35(18) . 3 ? O3 Ni2 S1 86.35(18) 3 . ? O3 Ni2 S1 93.65(18) . . ? S1 Ni2 S1 180.0 3 . ? O3 Ni2 S2 84.15(18) 3 . ? O3 Ni2 S2 95.85(18) . . ? S1 Ni2 S2 103.50(5) 3 . ? S1 Ni2 S2 76.50(5) . . ? O3 Ni2 S2 95.85(18) 3 3 ? O3 Ni2 S2 84.15(18) . 3 ? S1 Ni2 S2 76.50(5) 3 3 ? S1 Ni2 S2 103.50(5) . 3 ? S2 Ni2 S2 180.0 . 3 ? C1 S1 Ni1 100.2(2) . . ? C1 S1 Ni2 114.5(2) . . ? Ni1 S1 Ni2 94.47(7) . . ? C20 S2 Ni1 105.5(2) . . ? C20 S2 Ni2 117.8(2) . . ? Ni1 S2 Ni2 94.93(7) . . ? C7 N1 C8 120.5(5) . . ? C7 N1 Ni1 131.0(4) . . ? C8 N1 Ni1 108.3(4) . . ? C14 N2 C13 120.1(5) . . ? C14 N2 Ni1 130.3(4) . . ? C13 N2 Ni1 108.6(4) . . ? C2 C1 C6 119.3(6) . . ? C2 C1 S1 119.0(5) . . ? C6 C1 S1 121.6(5) . . ? C3 C2 C1 120.9(7) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 120.0(7) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 119.1(8) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 122.5(8) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 118.1(7) . . ? C5 C6 C7 115.6(6) . . ? C1 C6 C7 126.3(6) . . ? O1 C7 N1 125.3(6) . . ? O1 C7 C6 117.1(6) . . ? N1 C7 C6 117.5(6) . . ? C9 C8 C13 119.3(6) . . ? C9 C8 N1 126.7(6) . . ? C13 C8 N1 113.9(5) . . ? C10 C9 C8 119.9(6) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.1(6) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.5(6) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.1(6) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 120.0(6) . . ? C12 C13 N2 125.7(6) . . ? C8 C13 N2 114.3(5) . . ? O2 C14 N2 122.9(6) . . ? O2 C14 C15 117.0(6) . . ? N2 C14 C15 120.0(5) . . ? C16 C15 C20 118.1(6) . . ? C16 C15 C14 115.2(6) . . ? C20 C15 C14 126.6(5) . . ? C17 C16 C15 122.5(6) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 119.1(6) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 119.7(6) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 122.4(6) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C15 118.2(6) . . ? C19 C20 S2 118.2(5) . . ? C15 C20 S2 123.5(4) . . ? C21B O3 C21 38.5(7) . . ? C21B O3 Ni2 144.3(9) . . ? C21 O3 Ni2 131.6(8) . . ? C21B N3 C22 93.3(10) . . ? C21B N3 C21 30.9(6) . . ? C22 N3 C21 123.6(10) . . ? C21B N3 C22B 126.0(11) . . ? C22 N3 C22B 55.4(9) . . ? C21 N3 C22B 136.1(10) . . ? C21B N3 C23 145.1(11) . . ? C22 N3 C23 118.8(11) . . ? C21 N3 C23 114.7(11) . . ? C22B N3 C23 70.8(10) . . ? C21B N3 C23B 119.2(8) . . ? C22 N3 C23B 110.2(9) . . ? C21 N3 C23B 107.5(8) . . ? C22B N3 C23B 113.1(9) . . ? C23 N3 C23B 64.6(9) . . ? O3 C21 N3 126.6(12) . . ? O3 C21 H21 116.7 . . ? N3 C21 H21 116.7 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C21B N3 136.3(14) . . ? O3 C21B H21B 111.9 . . ? N3 C21B H21B 111.9 . . ? N3 C22B H22D 109.5 . . ? N3 C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? N3 C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N3 C23B H23D 109.5 . . ? N3 C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? N3 C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C28 N4 C26 113.3(10) . . ? C28 N4 C30 116.2(10) . . ? C26 N4 C30 103.1(8) . . ? C28 N4 C24 105.1(9) . . ? C26 N4 C24 107.8(8) . . ? C30 N4 C24 111.3(9) . . ? C25 C24 N4 119.5(9) . . ? C25 C24 H24A 107.5 . . ? N4 C24 H24A 107.5 . . ? C25 C24 H24B 107.5 . . ? N4 C24 H24B 107.5 . . ? H24A C24 H24B 107.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N4 116.3(10) . . ? C27 C26 H26A 108.2 . . ? N4 C26 H26A 108.2 . . ? C27 C26 H26B 108.2 . . ? N4 C26 H26B 108.2 . . ? H26A C26 H26B 107.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C29 113.5(12) . . ? N4 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? N4 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 C31 117.0(10) . . ? N4 C30 H30A 108.0 . . ? C31 C30 H30A 108.0 . . ? N4 C30 H30B 108.0 . . ? C31 C30 H30B 108.0 . . ? H30A C30 H30B 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26B N4B C24B 110.2(13) . . ? C26B N4B C28B 111.2(13) . . ? C24B N4B C28B 110.6(11) . . ? C26B N4B C30B 108.2(13) . . ? C24B N4B C30B 109.5(10) . . ? C28B N4B C30B 107.0(10) . . ? N4B C24B C25B 116.0(12) . . ? N4B C24B H24C 108.3 . . ? C25B C24B H24C 108.3 . . ? N4B C24B H24D 108.3 . . ? C25B C24B H24D 108.3 . . ? H24C C24B H24D 107.4 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? N4B C26B C27B 112.3(17) . . ? N4B C26B H26C 109.2 . . ? C27B C26B H26C 109.2 . . ? N4B C26B H26D 109.2 . . ? C27B C26B H26D 109.2 . . ? H26C C26B H26D 107.9 . . ? C26B C27B H27D 109.5 . . ? C26B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? N4B C28B C29B 116.7(19) . . ? N4B C28B H28C 108.1 . . ? C29B C28B H28C 108.1 . . ? N4B C28B H28D 108.1 . . ? C29B C28B H28D 108.1 . . ? H28C C28B H28D 107.3 . . ? C28B C29B H29D 109.5 . . ? C28B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C28B C29B H29F 109.4 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C31B C30B N4B 115.3(13) . . ? C31B C30B H30C 108.5 . . ? N4B C30B H30C 108.5 . . ? C31B C30B H30D 108.5 . . ? N4B C30B H30D 108.5 . . ? H30C C30B H30D 107.5 . . ? C30B C31B H31D 109.5 . . ? C30B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 S1 C1 84(4) . . . . ? N1 Ni1 S1 C1 50.4(3) . . . . ? S2 Ni1 S1 C1 -134.6(2) . . . . ? N2 Ni1 S1 Ni2 -160(4) . . . . ? N1 Ni1 S1 Ni2 166.30(15) . . . . ? S2 Ni1 S1 Ni2 -18.78(6) . . . . ? O3 Ni2 S1 C1 -154.9(3) 3 . . . ? O3 Ni2 S1 C1 25.1(3) . . . . ? S1 Ni2 S1 C1 -33(3) 3 . . . ? S2 Ni2 S1 C1 120.2(3) . . . . ? S2 Ni2 S1 C1 -59.8(3) 3 . . . ? O3 Ni2 S1 Ni1 101.8(2) 3 . . . ? O3 Ni2 S1 Ni1 -78.2(2) . . . . ? S1 Ni2 S1 Ni1 -136(3) 3 . . . ? S2 Ni2 S1 Ni1 16.91(5) . . . . ? S2 Ni2 S1 Ni1 -163.09(5) 3 . . . ? N2 Ni1 S2 C20 -42.3(3) . . . . ? N1 Ni1 S2 C20 -116.8(18) . . . . ? S1 Ni1 S2 C20 139.3(2) . . . . ? N2 Ni1 S2 Ni2 -162.91(14) . . . . ? N1 Ni1 S2 Ni2 122.6(18) . . . . ? S1 Ni1 S2 Ni2 18.69(6) . . . . ? O3 Ni2 S2 C20 144.7(3) 3 . . . ? O3 Ni2 S2 C20 -35.3(3) . . . . ? S1 Ni2 S2 C20 52.4(2) 3 . . . ? S1 Ni2 S2 C20 -127.6(2) . . . . ? S2 Ni2 S2 C20 -13(3) 3 . . . ? O3 Ni2 S2 Ni1 -104.8(2) 3 . . . ? O3 Ni2 S2 Ni1 75.2(2) . . . . ? S1 Ni2 S2 Ni1 162.82(5) 3 . . . ? S1 Ni2 S2 Ni1 -17.18(5) . . . . ? S2 Ni2 S2 Ni1 97(3) 3 . . . ? N2 Ni1 N1 C7 146.2(6) . . . . ? S2 Ni1 N1 C7 -138.9(16) . . . . ? S1 Ni1 N1 C7 -35.2(6) . . . . ? N2 Ni1 N1 C8 -27.9(4) . . . . ? S2 Ni1 N1 C8 47(2) . . . . ? S1 Ni1 N1 C8 150.7(3) . . . . ? N1 Ni1 N2 C14 -141.5(6) . . . . ? S2 Ni1 N2 C14 43.5(6) . . . . ? S1 Ni1 N2 C14 -175(3) . . . . ? N1 Ni1 N2 C13 26.4(4) . . . . ? S2 Ni1 N2 C13 -148.5(3) . . . . ? S1 Ni1 N2 C13 -7(4) . . . . ? Ni1 S1 C1 C2 137.5(6) . . . . ? Ni2 S1 C1 C2 37.8(7) . . . . ? Ni1 S1 C1 C6 -44.6(7) . . . . ? Ni2 S1 C1 C6 -144.3(6) . . . . ? C6 C1 C2 C3 1.7(12) . . . . ? S1 C1 C2 C3 179.6(7) . . . . ? C1 C2 C3 C4 -2.1(15) . . . . ? C2 C3 C4 C5 0.5(17) . . . . ? C3 C4 C5 C6 1.4(19) . . . . ? C4 C5 C6 C1 -1.8(16) . . . . ? C4 C5 C6 C7 178.8(10) . . . . ? C2 C1 C6 C5 0.2(13) . . . . ? S1 C1 C6 C5 -177.6(7) . . . . ? C2 C1 C6 C7 179.5(8) . . . . ? S1 C1 C6 C7 1.7(12) . . . . ? C8 N1 C7 O1 -6.8(12) . . . . ? Ni1 N1 C7 O1 179.7(6) . . . . ? C8 N1 C7 C6 168.6(6) . . . . ? Ni1 N1 C7 C6 -4.9(10) . . . . ? C5 C6 C7 O1 26.6(12) . . . . ? C1 C6 C7 O1 -152.7(9) . . . . ? C5 C6 C7 N1 -149.2(8) . . . . ? C1 C6 C7 N1 31.5(13) . . . . ? C7 N1 C8 C9 28.0(9) . . . . ? Ni1 N1 C8 C9 -157.1(5) . . . . ? C7 N1 C8 C13 -151.2(6) . . . . ? Ni1 N1 C8 C13 23.7(6) . . . . ? C13 C8 C9 C10 -0.6(9) . . . . ? N1 C8 C9 C10 -179.8(6) . . . . ? C8 C9 C10 C11 0.5(10) . . . . ? C9 C10 C11 C12 0.4(10) . . . . ? C10 C11 C12 C13 -1.1(10) . . . . ? C11 C12 C13 C8 1.0(9) . . . . ? C11 C12 C13 N2 -176.9(6) . . . . ? C9 C8 C13 C12 -0.1(9) . . . . ? N1 C8 C13 C12 179.2(5) . . . . ? C9 C8 C13 N2 178.0(5) . . . . ? N1 C8 C13 N2 -2.7(7) . . . . ? C14 N2 C13 C12 -32.2(9) . . . . ? Ni1 N2 C13 C12 158.4(5) . . . . ? C14 N2 C13 C8 149.8(6) . . . . ? Ni1 N2 C13 C8 -19.6(6) . . . . ? C13 N2 C14 O2 -3.9(10) . . . . ? Ni1 N2 C14 O2 162.9(5) . . . . ? C13 N2 C14 C15 176.7(5) . . . . ? Ni1 N2 C14 C15 -16.5(9) . . . . ? O2 C14 C15 C16 -11.8(9) . . . . ? N2 C14 C15 C16 167.7(6) . . . . ? O2 C14 C15 C20 164.8(7) . . . . ? N2 C14 C15 C20 -15.7(10) . . . . ? C20 C15 C16 C17 -2.5(10) . . . . ? C14 C15 C16 C17 174.4(6) . . . . ? C15 C16 C17 C18 -0.1(10) . . . . ? C16 C17 C18 C19 2.0(10) . . . . ? C17 C18 C19 C20 -1.3(10) . . . . ? C18 C19 C20 C15 -1.4(9) . . . . ? C18 C19 C20 S2 -177.5(5) . . . . ? C16 C15 C20 C19 3.2(9) . . . . ? C14 C15 C20 C19 -173.3(6) . . . . ? C16 C15 C20 S2 179.1(5) . . . . ? C14 C15 C20 S2 2.6(10) . . . . ? Ni1 S2 C20 C19 -153.6(4) . . . . ? Ni2 S2 C20 C19 -49.3(5) . . . . ? Ni1 S2 C20 C15 30.5(6) . . . . ? Ni2 S2 C20 C15 134.8(5) . . . . ? O3 Ni2 O3 C21B -110.8(15) 3 . . . ? S1 Ni2 O3 C21B -68.5(15) 3 . . . ? S1 Ni2 O3 C21B 111.5(15) . . . . ? S2 Ni2 O3 C21B 34.7(15) . . . . ? S2 Ni2 O3 C21B -145.3(15) 3 . . . ? O3 Ni2 O3 C21 -166.7(11) 3 . . . ? S1 Ni2 O3 C21 -124.5(12) 3 . . . ? S1 Ni2 O3 C21 55.5(12) . . . . ? S2 Ni2 O3 C21 -21.3(12) . . . . ? S2 Ni2 O3 C21 158.7(12) 3 . . . ? C21B O3 C21 N3 41.4(15) . . . . ? Ni2 O3 C21 N3 170.3(7) . . . . ? C21B N3 C21 O3 -40.4(15) . . . . ? C22 N3 C21 O3 -52.7(18) . . . . ? C22B N3 C21 O3 -125.5(16) . . . . ? C23 N3 C21 O3 147.0(15) . . . . ? C23B N3 C21 O3 77.5(15) . . . . ? C21 O3 C21B N3 -52.9(18) . . . . ? Ni2 O3 C21B N3 -147.3(11) . . . . ? C22 N3 C21B O3 -138.8(18) . . . . ? C21 N3 C21B O3 51.4(18) . . . . ? C22B N3 C21B O3 172.7(16) . . . . ? C23 N3 C21B O3 63(3) . . . . ? C23B N3 C21B O3 -23(2) . . . . ? C28 N4 C24 C25 41.3(14) . . . . ? C26 N4 C24 C25 162.4(10) . . . . ? C30 N4 C24 C25 -85.2(13) . . . . ? C28 N4 C26 C27 46.3(16) . . . . ? C30 N4 C26 C27 172.6(12) . . . . ? C24 N4 C26 C27 -69.6(14) . . . . ? C26 N4 C28 C29 58.6(16) . . . . ? C30 N4 C28 C29 -60.5(16) . . . . ? C24 N4 C28 C29 176.1(12) . . . . ? C28 N4 C30 C31 -61.8(16) . . . . ? C26 N4 C30 C31 173.6(11) . . . . ? C24 N4 C30 C31 58.4(14) . . . . ? C26B N4B C24B C25B -178.8(14) . . . . ? C28B N4B C24B C25B 57.8(16) . . . . ? C30B N4B C24B C25B -59.9(16) . . . . ? C24B N4B C26B C27B -71(2) . . . . ? C28B N4B C26B C27B 52(2) . . . . ? C30B N4B C26B C27B 169.2(16) . . . . ? C26B N4B C28B C29B 42(2) . . . . ? C24B N4B C28B C29B 164.5(19) . . . . ? C30B N4B C28B C29B -76(2) . . . . ? C26B N4B C30B C31B 66.8(18) . . . . ? C24B N4B C30B C31B -53.3(16) . . . . ? C28B N4B C30B C31B -173.3(13) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.695 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.101