Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Paul Beer' 'Andrew G. Cheetham' 'Michael G. B. Drew' 'O. D. Fox' 'Elizabeth J. Hayes' 'T. D. Rolls' _publ_contact_author_name 'Prof Paul Beer' _publ_contact_author_address ; Inorganic Chemistry Laboratory, Department of Chemistry University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email PAUL.BEER@CHEM.OX.AC.UK _publ_section_title ; Pyrrole-Based Metallo-Macrocycles and Cryptands ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_2-Ni _database_code_CSD 195408 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H26 N2 Ni S4' _chemical_formula_weight 577.46 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.294(10) _cell_length_b 10.323(14) _cell_length_c 10.909(17) _cell_angle_alpha 100.747(10) _cell_angle_beta 93.284(10) _cell_angle_gamma 106.730(10) _cell_volume 662.2(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 300 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.313 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2120 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.04 _reflns_number_total 2120 _reflns_number_gt 1240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.1798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2120 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.2688 _refine_ls_wR_factor_gt 0.2298 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.0000 0.0599(5) Uani 1 d S . . S1 S 0.1287(3) -0.02695(19) -0.18404(19) 0.0642(6) Uani 1 d . . . S2 S 0.3375(3) 0.1495(2) 0.04741(19) 0.0669(6) Uani 1 d . . . C3 C 0.3719(11) 0.0978(7) -0.1083(7) 0.0539(17) Uani 1 d . . . N4 C 0.5509(10) 0.1443(6) -0.1592(6) 0.0457(14) Uani 1 d . . . C41 C 0.7531(13) 0.2434(8) -0.0824(8) 0.071(2) Uani 1 d . . . H41A H 0.8563 0.1935 -0.0645 0.085 Uiso 1 calc R . . H41B H 0.7117 0.2828 -0.0030 0.085 Uiso 1 calc R . . C42 C 0.8719(12) 0.3600(7) -0.1433(7) 0.0581(18) Uani 1 d . . . C43 C 1.0685(12) 0.3646(8) -0.1912(8) 0.070(2) Uani 1 d . . . H43 H 1.1305 0.2931 -0.1902 0.084 Uiso 1 calc R . . C44 C 1.1711(17) 0.4720(11) -0.2394(12) 0.095(3) Uani 1 d . . . H44 H 1.3086 0.4780 -0.2690 0.114 Uiso 1 calc R . . C45 C 1.073(3) 0.5737(15) -0.2453(16) 0.139(6) Uani 1 d . . . H45 H 1.1454 0.6473 -0.2809 0.166 Uiso 1 calc R . . C46 C 0.882(3) 0.5710(14) -0.2026(15) 0.128(5) Uani 1 d . . . H46 H 0.8133 0.6386 -0.2093 0.153 Uiso 1 calc R . . C47 C 0.7930(17) 0.4679(10) -0.1503(9) 0.082(3) Uani 1 d . . . H47 H 0.6629 0.4682 -0.1142 0.099 Uiso 1 calc R . . C51 C 0.5689(13) 0.0865(8) -0.2935(8) 0.070(2) Uani 1 d . . . H51A H 0.7227 0.0884 -0.3005 0.084 Uiso 1 calc R . . H51B H 0.4778 -0.0098 -0.3145 0.084 Uiso 1 calc R . . C52 C 0.5019(12) 0.1573(8) -0.3879(7) 0.0597(18) Uani 1 d . . . C53 C 0.637(2) 0.2541(10) -0.4408(11) 0.104(4) Uani 1 d . . . H53 H 0.7924 0.2859 -0.4241 0.124 Uiso 1 calc R . . C54 C 0.497(5) 0.3048(16) -0.5336(14) 0.201(11) Uani 1 d . . . H54 H 0.5425 0.3688 -0.5840 0.242 Uiso 1 calc R . . C55 C 0.266(3) 0.2198(14) -0.5175(11) 0.109(4) Uani 1 d . . . H55 H 0.1330 0.2224 -0.5574 0.131 Uiso 1 calc R . . N56 N 0.2831(15) 0.1390(11) -0.4357(8) 0.100(3) Uani 1 d . . . H56 H 0.1693 0.0816 -0.4151 0.120 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0563(8) 0.0631(9) 0.0620(9) 0.0156(6) 0.0065(6) 0.0193(6) S1 0.0604(11) 0.0598(11) 0.0663(12) 0.0095(9) 0.0073(8) 0.0111(8) S2 0.0617(11) 0.0742(12) 0.0587(11) 0.0098(10) 0.0072(8) 0.0139(8) C3 0.049(4) 0.055(4) 0.059(4) 0.015(3) -0.007(3) 0.019(3) N4 0.044(3) 0.048(3) 0.046(3) 0.008(3) -0.002(3) 0.017(3) C41 0.061(4) 0.078(5) 0.072(5) 0.033(4) 0.005(4) 0.009(3) C42 0.057(4) 0.059(4) 0.058(4) 0.007(4) 0.007(3) 0.019(3) C43 0.060(4) 0.065(4) 0.087(6) 0.016(4) 0.016(4) 0.021(4) C44 0.070(5) 0.088(6) 0.119(8) 0.028(6) 0.011(5) 0.007(5) C45 0.138(13) 0.110(10) 0.152(13) -0.017(10) -0.020(10) 0.049(9) C46 0.158(13) 0.088(8) 0.136(12) -0.005(9) -0.003(10) 0.057(9) C47 0.107(7) 0.074(6) 0.075(6) 0.008(5) 0.016(5) 0.046(5) C51 0.069(5) 0.066(4) 0.083(5) 0.016(4) 0.022(4) 0.032(4) C52 0.062(4) 0.064(4) 0.048(4) 0.003(4) 0.004(3) 0.017(3) C53 0.139(10) 0.067(6) 0.093(8) 0.012(6) 0.025(6) 0.014(6) C54 0.45(4) 0.098(10) 0.082(9) 0.025(8) 0.087(15) 0.103(18) C55 0.164(12) 0.118(9) 0.068(7) 0.019(7) -0.002(6) 0.081(9) N56 0.105(6) 0.127(7) 0.079(5) 0.026(6) 0.018(4) 0.050(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S2 2.202(3) 2 ? Ni1 S2 2.202(3) . ? Ni1 S1 2.207(4) . ? Ni1 S1 2.207(4) 2 ? S1 C3 1.734(7) . ? S2 C3 1.728(8) . ? C3 N4 1.292(11) . ? N4 C41 1.475(10) . ? N4 C51 1.499(11) . ? C41 C42 1.512(12) . ? C42 C47 1.357(13) . ? C42 C43 1.362(10) . ? C43 C44 1.329(14) . ? C44 C45 1.371(17) . ? C45 C46 1.31(2) . ? C46 C47 1.299(19) . ? C51 C52 1.477(12) . ? C52 C53 1.356(14) . ? C52 N56 1.391(11) . ? C53 C54 1.56(2) . ? C54 C55 1.51(2) . ? C55 N56 1.349(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni1 S2 180.0 2 . ? S2 Ni1 S1 100.52(9) 2 . ? S2 Ni1 S1 79.48(9) . . ? S2 Ni1 S1 79.48(9) 2 2 ? S2 Ni1 S1 100.52(10) . 2 ? S1 Ni1 S1 180.0 . 2 ? C3 S1 Ni1 85.6(3) . . ? C3 S2 Ni1 85.9(2) . . ? N4 C3 S2 125.2(5) . . ? N4 C3 S1 125.8(6) . . ? S2 C3 S1 109.0(4) . . ? C3 N4 C41 120.6(7) . . ? C3 N4 C51 121.1(6) . . ? C41 N4 C51 117.9(7) . . ? N4 C41 C42 114.3(7) . . ? C47 C42 C43 116.1(9) . . ? C47 C42 C41 122.2(8) . . ? C43 C42 C41 121.7(7) . . ? C44 C43 C42 119.5(8) . . ? C43 C44 C45 119.7(12) . . ? C46 C45 C44 122.3(18) . . ? C47 C46 C45 115.9(14) . . ? C46 C47 C42 126.4(12) . . ? C52 C51 N4 116.4(6) . . ? C53 C52 N56 107.4(10) . . ? C53 C52 C51 127.3(9) . . ? N56 C52 C51 125.3(9) . . ? C52 C53 C54 110.5(13) . . ? C55 C54 C53 99.4(12) . . ? N56 C55 C54 108.8(12) . . ? C55 N56 C52 113.8(11) . . ? _refine_diff_density_max 0.490 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.102 #===END data_7-Zn-pyr _database_code_CSD 195409 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H80 N12 S8 Zn2' _chemical_formula_weight 1572.76 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.696(15) _cell_length_b 11.949(15) _cell_length_c 16.07(2) _cell_angle_alpha 85.959(10) _cell_angle_beta 73.810(10) _cell_angle_gamma 79.748(10) _cell_volume 1941(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour white _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.884 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.409 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6942 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1401 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.06 _reflns_number_total 6942 _reflns_number_gt 3222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6942 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1931 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1185 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.176 _refine_ls_shift/su_mean 0.011 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.11126(7) -0.35305(5) 0.05441(5) 0.0610(3) Uani 1 d . . . S11 S 0.07690(18) -0.27725(13) -0.09165(11) 0.0681(5) Uani 1 d . . . S12 S 0.19862(15) -0.18152(12) 0.02488(10) 0.0558(4) Uani 1 d . . . C13 C 0.1353(5) -0.1639(4) -0.0648(3) 0.0462(14) Uani 1 d . . . N14 N 0.1312(4) -0.0648(4) -0.1091(3) 0.0476(12) Uani 1 d . . . C151 C 0.0592(6) -0.0416(5) -0.1765(4) 0.0659(18) Uani 1 d . . . H15A H -0.0180 0.0158 -0.1560 0.079 Uiso 1 calc R . . H15B H 0.0291 -0.1105 -0.1857 0.079 Uiso 1 calc R . . C152 C 0.1425(4) -0.0012(4) -0.2623(2) 0.0550(16) Uani 1 d G . . C153 C 0.1202(4) 0.1125(3) -0.2881(3) 0.0648(18) Uani 1 d G . . H153 H 0.0532 0.1633 -0.2533 0.078 Uiso 1 calc R . . C154 C 0.1982(6) 0.1501(3) -0.3658(3) 0.091(2) Uani 1 d G . . H154 H 0.1833 0.2262 -0.3830 0.110 Uiso 1 calc R . . C155 C 0.2983(5) 0.0742(5) -0.4179(3) 0.107(3) Uani 1 d G . . H155 H 0.3504 0.0994 -0.4699 0.128 Uiso 1 calc R . . C156 C 0.3206(4) -0.0395(5) -0.3921(3) 0.108(3) Uani 1 d G . . H156 H 0.3876 -0.0903 -0.4269 0.129 Uiso 1 calc R . . C157 C 0.2427(5) -0.0771(3) -0.3144(3) 0.078(2) Uani 1 d G . . H157 H 0.2575 -0.1532 -0.2972 0.094 Uiso 1 calc R . . C15 C 0.1780(5) 0.0352(4) -0.0836(4) 0.0523(16) Uani 1 d . . . H15C H 0.1577 0.0355 -0.0209 0.063 Uiso 1 calc R . . H15D H 0.1289 0.1043 -0.1019 0.063 Uiso 1 calc R . . C16 C 0.3238(6) 0.0381(4) -0.1207(3) 0.0417(14) Uani 1 d . . . N17 N 0.3750(4) 0.0940(3) -0.1976(3) 0.0466(12) Uani 1 d . . . H17 H 0.3295 0.1238 -0.2325 0.056 Uiso 1 calc R . . C18 C 0.5063(6) 0.0962(4) -0.2116(4) 0.0478(15) Uani 1 d . . . C19 C 0.5410(6) 0.0372(5) -0.1433(4) 0.0606(17) Uani 1 d . . . H19 H 0.6251 0.0236 -0.1349 0.073 Uiso 1 calc R . . C20 C 0.4262(6) -0.0003(5) -0.0866(4) 0.0540(16) Uani 1 d . . . H20 H 0.4227 -0.0432 -0.0357 0.065 Uiso 1 calc R . . C21 C 0.5890(6) 0.1492(5) -0.2908(4) 0.0584(16) Uani 1 d . . . C211 C 0.6500(6) 0.0579(5) -0.3612(4) 0.077(2) Uani 1 d . . . H21A H 0.7103 -0.0001 -0.3414 0.093 Uiso 1 calc R . . H21B H 0.6964 0.0928 -0.4137 0.093 Uiso 1 calc R . . H21C H 0.5810 0.0245 -0.3721 0.093 Uiso 1 calc R . . C212 C 0.7009(6) 0.1936(6) -0.2665(5) 0.090(2) Uani 1 d . . . H21D H 0.7509 0.2316 -0.3160 0.108 Uiso 1 calc R . . H21E H 0.7577 0.1309 -0.2485 0.108 Uiso 1 calc R . . H21F H 0.6636 0.2461 -0.2200 0.108 Uiso 1 calc R . . C22 C 0.5108(6) 0.2477(5) -0.3278(4) 0.0508(15) Uani 1 d . . . N23 N 0.4117(4) 0.3235(4) -0.2777(3) 0.0514(12) Uani 1 d . . . H23 H 0.3834 0.3178 -0.2222 0.062 Uiso 1 calc R . . C24 C 0.3627(7) 0.4104(5) -0.3276(4) 0.0615(17) Uani 1 d . . . C25 C 0.4356(7) 0.3879(5) -0.4111(5) 0.079(2) Uani 1 d . . . H25 H 0.4260 0.4324 -0.4595 0.095 Uiso 1 calc R . . C26 C 0.5265(7) 0.2882(6) -0.4129(4) 0.080(2) Uani 1 d . . . H26 H 0.5866 0.2547 -0.4619 0.096 Uiso 1 calc R . . C27 C 0.2515(6) 0.5007(5) -0.2908(4) 0.0610(17) Uani 1 d . . . H27A H 0.2633 0.5705 -0.3244 0.073 Uiso 1 calc R . . H27B H 0.2510 0.5144 -0.2319 0.073 Uiso 1 calc R . . N28 N 0.1213(5) 0.4695(4) -0.2904(3) 0.0586(14) Uani 1 d . . . C29 C 0.0481(5) 0.4241(4) -0.2206(4) 0.0485(15) Uani 1 d . . . S31 S -0.10598(17) 0.39294(13) -0.21990(11) 0.0670(5) Uani 1 d . . . S30 S 0.10085(16) 0.38958(12) -0.12900(10) 0.0568(4) Uani 1 d . . . N100 N 0.2439(5) -0.4997(4) 0.0170(4) 0.0585(14) Uani 1 d . . . C101 C 0.3551(8) -0.4951(5) -0.0469(5) 0.074(2) Uani 1 d . . . H101 H 0.3700 -0.4258 -0.0747 0.088 Uiso 1 calc R . . C102 C 0.4479(7) -0.5917(7) -0.0720(5) 0.087(2) Uani 1 d . . . H102 H 0.5262 -0.5864 -0.1144 0.104 Uiso 1 calc R . . C103 C 0.4249(9) -0.6946(7) -0.0347(6) 0.088(2) Uani 1 d . . . H103 H 0.4848 -0.7605 -0.0530 0.106 Uiso 1 calc R . . C104 C 0.3119(10) -0.6987(6) 0.0300(6) 0.102(3) Uani 1 d . . . H104 H 0.2953 -0.7674 0.0582 0.123 Uiso 1 calc R . . C105 C 0.2224(7) -0.6001(6) 0.0533(4) 0.076(2) Uani 1 d . . . H105 H 0.1442 -0.6042 0.0961 0.091 Uiso 1 calc R . . C32 C 0.0862(7) 0.4944(5) -0.3724(4) 0.077(2) Uani 1 d . . . H32A H 0.0096 0.4602 -0.3703 0.092 Uiso 1 calc R . . H32B H 0.1586 0.4600 -0.4192 0.092 Uiso 1 calc R . . C33 C 0.0559(6) 0.6206(6) -0.3914(4) 0.0602(17) Uani 1 d . . . C34 C 0.0735(7) 0.6543(7) -0.4790(5) 0.094(2) Uani 1 d . . . H34 H 0.1083 0.6012 -0.5226 0.112 Uiso 1 calc R . . C35 C 0.0372(10) 0.7704(10) -0.4995(8) 0.140(4) Uani 1 d . . . H35 H 0.0507 0.7955 -0.5569 0.168 Uiso 1 calc R . . C36 C -0.0175(10) 0.8440(10) -0.4342(10) 0.146(5) Uani 1 d . . . H36 H -0.0394 0.9206 -0.4479 0.175 Uiso 1 calc R . . C37 C -0.0417(9) 0.8111(8) -0.3493(7) 0.116(3) Uani 1 d . . . H37 H -0.0807 0.8639 -0.3058 0.139 Uiso 1 calc R . . C38 C -0.0073(8) 0.6976(7) -0.3288(6) 0.102(3) Uani 1 d . . . H38 H -0.0278 0.6734 -0.2710 0.122 Uiso 1 calc R . . N200 N 0.6131(15) 0.5588(10) -0.3085(12) 0.185(4) Uani 1 d . . . C201 C 0.6734(12) 0.6256(15) -0.3690(9) 0.160(5) Uani 1 d . . . H201 H 0.7352 0.5993 -0.4199 0.192 Uiso 1 calc R . . C202 C 0.5541(16) 0.7782(12) -0.2709(12) 0.171(5) Uani 1 d . . . H202 H 0.5340 0.8552 -0.2584 0.205 Uiso 1 calc R . . C203 C 0.636(2) 0.7370(16) -0.3492(10) 0.231(8) Uani 1 d . . . H203 H 0.6669 0.7899 -0.3916 0.277 Uiso 1 calc R . . C204 C 0.5126(14) 0.7083(12) -0.2216(9) 0.182(6) Uani 1 d . . . H204 H 0.4633 0.7324 -0.1666 0.218 Uiso 1 calc R . . C205 C 0.5284(16) 0.5990(15) -0.2358(10) 0.202(7) Uani 1 d . . . H205 H 0.4813 0.5511 -0.1957 0.243 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0600(5) 0.0504(5) 0.0700(6) 0.0016(3) -0.0108(4) -0.0142(3) S11 0.0833(13) 0.0636(11) 0.0656(12) -0.0014(8) -0.0222(10) -0.0302(9) S12 0.0625(11) 0.0509(9) 0.0584(11) 0.0033(7) -0.0187(9) -0.0190(7) C13 0.044(4) 0.045(3) 0.045(4) 0.005(3) -0.005(3) -0.009(3) N14 0.046(3) 0.051(3) 0.046(3) -0.001(2) -0.006(2) -0.016(2) C151 0.058(4) 0.077(4) 0.065(5) 0.005(3) -0.015(4) -0.023(3) C152 0.060(4) 0.062(4) 0.052(4) -0.006(3) -0.024(4) -0.020(3) C153 0.081(5) 0.066(4) 0.051(4) 0.004(3) -0.025(4) -0.015(3) C154 0.104(7) 0.090(6) 0.094(7) 0.021(5) -0.047(5) -0.030(5) C155 0.135(8) 0.134(8) 0.063(6) 0.022(5) -0.030(6) -0.057(6) C156 0.110(7) 0.140(8) 0.076(7) -0.026(5) -0.013(5) -0.036(6) C157 0.088(6) 0.081(5) 0.060(5) -0.003(4) -0.006(4) -0.024(4) C15 0.060(4) 0.043(4) 0.052(4) -0.003(3) -0.009(3) -0.014(3) C16 0.053(4) 0.036(3) 0.037(4) 0.002(2) -0.010(3) -0.013(3) N17 0.046(3) 0.050(3) 0.045(3) 0.005(2) -0.013(3) -0.011(2) C18 0.042(4) 0.046(3) 0.055(4) -0.004(3) -0.010(3) -0.009(3) C19 0.044(4) 0.074(4) 0.068(5) 0.006(3) -0.022(4) -0.012(3) C20 0.061(4) 0.063(4) 0.041(4) 0.008(3) -0.014(3) -0.019(3) C21 0.059(4) 0.062(4) 0.050(4) -0.004(3) -0.005(3) -0.012(3) C211 0.078(5) 0.075(5) 0.063(5) -0.007(3) 0.000(4) 0.000(4) C212 0.070(5) 0.110(6) 0.094(6) 0.011(4) -0.017(4) -0.038(4) C22 0.051(4) 0.054(4) 0.045(4) -0.004(3) -0.004(3) -0.016(3) N23 0.058(3) 0.059(3) 0.041(3) 0.005(2) -0.014(3) -0.021(3) C24 0.079(5) 0.060(4) 0.049(4) 0.009(3) -0.015(4) -0.027(3) C25 0.101(6) 0.073(5) 0.057(5) 0.022(4) -0.013(4) -0.021(4) C26 0.091(6) 0.084(5) 0.056(5) -0.012(4) 0.001(4) -0.023(4) C27 0.072(5) 0.055(4) 0.059(4) 0.010(3) -0.019(4) -0.021(3) N28 0.071(4) 0.050(3) 0.057(4) 0.005(2) -0.020(3) -0.015(3) C29 0.050(4) 0.049(3) 0.046(4) -0.001(3) -0.011(3) -0.011(3) S31 0.0672(12) 0.0720(11) 0.0715(13) 0.0005(9) -0.0303(10) -0.0189(9) S30 0.0559(11) 0.0634(10) 0.0542(11) 0.0090(7) -0.0194(9) -0.0149(7) N100 0.065(4) 0.047(3) 0.072(4) -0.006(3) -0.029(3) -0.014(3) C101 0.084(6) 0.063(5) 0.080(6) -0.014(4) -0.026(5) -0.018(4) C102 0.077(6) 0.096(6) 0.092(6) -0.018(5) -0.026(5) -0.013(5) C103 0.095(7) 0.084(6) 0.088(7) -0.024(5) -0.034(5) 0.003(5) C104 0.148(9) 0.054(5) 0.107(7) -0.008(4) -0.044(7) -0.007(5) C105 0.078(5) 0.064(5) 0.086(6) -0.007(4) -0.021(4) -0.016(4) C32 0.094(6) 0.083(5) 0.064(5) 0.008(4) -0.037(4) -0.023(4) C33 0.066(5) 0.079(5) 0.039(4) 0.009(4) -0.023(4) -0.010(3) C34 0.076(6) 0.108(7) 0.083(6) 0.012(5) -0.012(5) 0.000(4) C35 0.084(8) 0.158(11) 0.142(11) 0.063(8) 0.002(7) -0.003(7) C36 0.098(8) 0.123(9) 0.199(14) 0.075(9) -0.034(9) -0.013(6) C37 0.134(8) 0.105(7) 0.125(9) 0.017(6) -0.069(7) -0.014(6) C38 0.118(7) 0.102(7) 0.102(7) 0.017(6) -0.065(6) -0.013(5) N200 0.169(11) 0.174(11) 0.210(14) -0.024(10) -0.033(10) -0.048(9) C201 0.128(10) 0.179(14) 0.162(13) -0.028(11) -0.003(9) -0.042(10) C202 0.229(16) 0.127(12) 0.178(16) -0.020(11) -0.073(13) -0.053(10) C203 0.42(3) 0.146(14) 0.120(13) 0.006(9) -0.046(14) -0.064(13) C204 0.241(15) 0.073(10) 0.186(14) -0.001(8) 0.018(11) -0.027(8) C205 0.251(17) 0.139(14) 0.153(13) 0.017(9) 0.051(11) -0.041(10) _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 Zn1 N100 2.057(5) . ? Zn1 S30 2.353(3) 2 ? Zn1 S12 2.366(3) . ? Zn1 S11 2.555(4) . ? Zn1 S31 2.656(4) 2 ? S11 C13 1.716(5) . ? S12 C13 1.741(6) . ? C13 N14 1.338(6) . ? N14 C151 1.481(7) . ? N14 C15 1.498(6) . ? C151 C152 1.518(7) . ? C152 C153 1.3900 . ? C152 C157 1.3900 . ? C153 C154 1.3900 . ? C154 C155 1.3900 . ? C155 C156 1.3900 . ? C156 C157 1.3900 . ? C15 C16 1.512(7) . ? C16 C20 1.353(7) . ? C16 N17 1.382(6) . ? N17 C18 1.364(6) . ? C18 C19 1.365(7) . ? C18 C21 1.505(7) . ? C19 C20 1.433(7) . ? C21 C22 1.506(8) . ? C21 C212 1.543(8) . ? C21 C211 1.551(7) . ? C22 N23 1.370(7) . ? C22 C26 1.392(8) . ? N23 C24 1.385(7) . ? C24 C25 1.370(8) . ? C24 C27 1.473(8) . ? C25 C26 1.393(9) . ? C27 N28 1.503(7) . ? N28 C29 1.321(6) . ? N28 C32 1.464(7) . ? C29 S30 1.717(6) . ? C29 S31 1.750(6) . ? S31 Zn1 2.656(4) 2 ? S30 Zn1 2.353(3) 2 ? N100 C105 1.325(7) . ? N100 C101 1.345(8) . ? C101 C102 1.384(9) . ? C102 C103 1.361(9) . ? C103 C104 1.363(10) . ? C104 C105 1.381(9) . ? C32 C33 1.513(8) . ? C33 C38 1.358(9) . ? C33 C34 1.407(9) . ? C34 C35 1.414(11) . ? C35 C36 1.350(13) . ? C36 C37 1.360(13) . ? C37 C38 1.382(10) . ? N200 C201 1.312(13) . ? N200 C205 1.324(13) . ? C201 C203 1.354(16) . ? C202 C204 1.169(13) . ? C202 C203 1.381(17) . ? C204 C205 1.314(14) . ? 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 N100 Zn1 S30 112.49(17) . 2 ? N100 Zn1 S12 115.92(18) . . ? S30 Zn1 S12 131.43(6) 2 . ? N100 Zn1 S11 100.63(16) . . ? S30 Zn1 S11 101.53(9) 2 . ? S12 Zn1 S11 73.56(6) . . ? N100 Zn1 S31 92.02(15) . 2 ? S30 Zn1 S31 72.32(8) 2 2 ? S12 Zn1 S31 101.86(6) . 2 ? S11 Zn1 S31 167.31(6) . 2 ? C13 S11 Zn1 81.43(19) . . ? C13 S12 Zn1 86.80(18) . . ? N14 C13 S11 122.4(4) . . ? N14 C13 S12 120.4(4) . . ? S11 C13 S12 117.1(3) . . ? C13 N14 C151 121.3(4) . . ? C13 N14 C15 122.2(5) . . ? C151 N14 C15 115.7(4) . . ? N14 C151 C152 113.2(5) . . ? C153 C152 C157 120.0 . . ? C153 C152 C151 119.9(4) . . ? C157 C152 C151 120.1(4) . . ? C152 C153 C154 120.0 . . ? C155 C154 C153 120.0 . . ? C156 C155 C154 120.0 . . ? C157 C156 C155 120.0 . . ? C156 C157 C152 120.0 . . ? N14 C15 C16 115.0(4) . . ? C20 C16 N17 106.4(5) . . ? C20 C16 C15 130.2(5) . . ? N17 C16 C15 123.2(5) . . ? C18 N17 C16 111.8(5) . . ? N17 C18 C19 105.6(5) . . ? N17 C18 C21 123.7(5) . . ? C19 C18 C21 130.5(6) . . ? C18 C19 C20 108.6(5) . . ? C16 C20 C19 107.5(5) . . ? C18 C21 C22 112.7(5) . . ? C18 C21 C212 109.0(5) . . ? C22 C21 C212 108.0(5) . . ? C18 C21 C211 109.1(5) . . ? C22 C21 C211 108.7(5) . . ? C212 C21 C211 109.3(5) . . ? N23 C22 C26 105.9(5) . . ? N23 C22 C21 123.3(5) . . ? C26 C22 C21 130.5(6) . . ? C22 N23 C24 111.6(5) . . ? C25 C24 N23 105.2(6) . . ? C25 C24 C27 131.8(6) . . ? N23 C24 C27 123.0(6) . . ? C24 C25 C26 109.8(6) . . ? C22 C26 C25 107.6(6) . . ? C24 C27 N28 111.8(5) . . ? C29 N28 C32 124.9(5) . . ? C29 N28 C27 120.8(5) . . ? C32 N28 C27 114.2(5) . . ? N28 C29 S30 122.1(5) . . ? N28 C29 S31 120.3(4) . . ? S30 C29 S31 117.6(3) . . ? C29 S31 Zn1 79.46(19) . 2 ? C29 S30 Zn1 89.5(2) . 2 ? C105 N100 C101 118.4(5) . . ? C105 N100 Zn1 121.9(5) . . ? C101 N100 Zn1 119.7(4) . . ? N100 C101 C102 121.0(6) . . ? C103 C102 C101 120.2(8) . . ? C102 C103 C104 118.4(7) . . ? C105 C104 C103 119.4(7) . . ? N100 C105 C104 122.5(7) . . ? N28 C32 C33 112.8(5) . . ? C38 C33 C34 119.3(7) . . ? C38 C33 C32 123.0(6) . . ? C34 C33 C32 116.7(6) . . ? C33 C34 C35 118.7(8) . . ? C36 C35 C34 118.8(10) . . ? C37 C36 C35 122.8(11) . . ? C36 C37 C38 118.6(10) . . ? C33 C38 C37 121.3(8) . . ? C201 N200 C205 122.1(14) . . ? N200 C201 C203 112.5(14) . . ? C204 C202 C203 114.4(17) . . ? C201 C203 C202 125.1(15) . . ? C202 C204 C205 126.8(16) . . ? C204 C205 N200 118.3(12) . . ? _refine_diff_density_max 0.415 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.063 #===END data_7-Ni _database_code_CSD 195410 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H68 N8 Ni2 O4 S8' _chemical_formula_weight 1315.10 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.996(17) _cell_length_b 16.75(2) _cell_length_c 17.05(2) _cell_angle_alpha 68.672(10) _cell_angle_beta 83.409(10) _cell_angle_gamma 80.283(10) _cell_volume 3404(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelopiped _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.623 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11522 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1471 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 26.41 _reflns_number_total 11522 _reflns_number_gt 5036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.1440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11522 _refine_ls_number_parameters 691 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1638 _refine_ls_R_factor_gt 0.0991 _refine_ls_wR_factor_ref 0.2628 _refine_ls_wR_factor_gt 0.2479 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.054 _refine_ls_shift/su_mean 0.011 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.20244(7) 0.07177(5) 0.04066(5) 0.0477(3) Uani 1 d . . . S11 S 0.14193(17) 0.15582(13) -0.08217(12) 0.0610(5) Uani 1 d . . . S12 S 0.03593(15) 0.06567(11) 0.06669(11) 0.0543(5) Uani 1 d . . . C13 C 0.0195(6) 0.1387(4) -0.0344(4) 0.0505(18) Uani 1 d . . . N14 N -0.0679(5) 0.1746(3) -0.0673(3) 0.0504(15) Uani 1 d . . . C141 C -0.0749(8) 0.2464(5) -0.1521(5) 0.073(2) Uani 1 d . . . H14A H -0.0095 0.2704 -0.1675 0.088 Uiso 1 calc R . . H14B H -0.1300 0.2922 -0.1488 0.088 Uiso 1 calc R . . C142 C -0.0983(6) 0.2124(5) -0.2211(5) 0.061(2) Uani 1 d . . . C143 C -0.0455(6) 0.1371(5) -0.2278(5) 0.0575(19) Uani 1 d . . . H143 H 0.0036 0.1038 -0.1891 0.069 Uiso 1 calc R . . C144 C -0.0655(8) 0.1088(6) -0.2946(5) 0.078(3) Uani 1 d . . . H144 H -0.0321 0.0563 -0.2977 0.094 Uiso 1 calc R . . C145 C -0.1346(7) 0.1607(6) -0.3530(6) 0.074(2) Uani 1 d . . . H145 H -0.1451 0.1448 -0.3980 0.089 Uiso 1 calc R . . C146 C -0.1743(6) 0.2712(5) -0.2795(4) 0.0527(18) Uani 1 d . . . H146 H -0.2087 0.3231 -0.2756 0.063 Uiso 1 calc R . . C147 C -0.1897(9) 0.2370(8) -0.3463(6) 0.112(4) Uani 1 d . . . H147 H -0.2389 0.2685 -0.3857 0.134 Uiso 1 calc R . . C15 C -0.1639(7) 0.1454(5) -0.0213(5) 0.072(2) Uani 1 d . . . H15A H -0.1566 0.1297 0.0386 0.087 Uiso 1 calc R . . H15B H -0.1754 0.0942 -0.0312 0.087 Uiso 1 calc R . . C16 C -0.2566(6) 0.2134(4) -0.0474(4) 0.0476(16) Uani 1 d . . . C17 C -0.3070(7) 0.2750(5) -0.0157(5) 0.073(2) Uani 1 d . . . H17 H -0.2826 0.2879 0.0268 0.087 Uiso 1 calc R . . C18 C -0.4010(8) 0.3163(5) -0.0561(5) 0.073(2) Uani 1 d . . . H18 H -0.4499 0.3596 -0.0464 0.088 Uiso 1 calc R . . C19 C -0.4012(6) 0.2746(4) -0.1158(4) 0.0496(17) Uani 1 d . . . N20 N -0.3245(5) 0.2120(4) -0.1029(4) 0.0510(14) Uani 1 d . . . H20 H -0.3168 0.1737 -0.1265 0.061 Uiso 1 calc R . . C21 C -0.4850(6) 0.2935(4) -0.1787(4) 0.0507(17) Uani 1 d . . . C211 C -0.5041(8) 0.2132(6) -0.1924(6) 0.089(3) Uani 1 d . . . H21A H -0.5233 0.1711 -0.1394 0.106 Uiso 1 calc R . . H21B H -0.4415 0.1897 -0.2167 0.106 Uiso 1 calc R . . H21C H -0.5596 0.2278 -0.2299 0.106 Uiso 1 calc R . . C212 C -0.5911(7) 0.3321(5) -0.1444(6) 0.071(2) Uani 1 d . . . H21D H -0.6060 0.2961 -0.0872 0.086 Uiso 1 calc R . . H21E H -0.6461 0.3346 -0.1785 0.086 Uiso 1 calc R . . H21F H -0.5861 0.3894 -0.1464 0.086 Uiso 1 calc R . . C22 C -0.4529(5) 0.3628(5) -0.2620(5) 0.0523(18) Uani 1 d . . . N23 N -0.3982(5) 0.4245(4) -0.2646(4) 0.0533(15) Uani 1 d . . . H23 H -0.3777 0.4311 -0.2214 0.064 Uiso 1 calc R . . C24 C -0.3797(7) 0.4766(6) -0.3481(5) 0.073(2) Uani 1 d . . . C25 C -0.4299(7) 0.4488(6) -0.3957(6) 0.080(3) Uani 1 d . . . H25 H -0.4357 0.4748 -0.4537 0.096 Uiso 1 calc R . . C26 C -0.4714(6) 0.3753(5) -0.3443(5) 0.063(2) Uani 1 d . . . H26 H -0.5054 0.3405 -0.3617 0.076 Uiso 1 calc R . . C27 C -0.3272(7) 0.5495(5) -0.3688(5) 0.066(2) Uani 1 d . . . H27A H -0.3461 0.5764 -0.3265 0.079 Uiso 1 calc R . . H27B H -0.3485 0.5915 -0.4228 0.079 Uiso 1 calc R . . N28 N -0.2075(5) 0.5227(3) -0.3733(3) 0.0492(14) Uani 1 d . . . C29 C -0.1495(6) 0.5102(4) -0.3111(5) 0.057(2) Uani 1 d . . . C281 C -0.1664(6) 0.4997(5) -0.4493(5) 0.061(2) Uani 1 d . . . H28A H -0.0954 0.4702 -0.4408 0.074 Uiso 1 calc R . . H28B H -0.2087 0.4600 -0.4553 0.074 Uiso 1 calc R . . C282 C -0.1670(6) 0.5756(5) -0.5274(4) 0.059(2) Uani 1 d . . . C283 C -0.0950(7) 0.6356(5) -0.5351(5) 0.066(2) Uani 1 d . . . H283 H -0.0524 0.6272 -0.4918 0.080 Uiso 1 calc R . . C284 C -0.0921(9) 0.7048(6) -0.6082(6) 0.091(3) Uani 1 d . . . H284 H -0.0407 0.7400 -0.6165 0.109 Uiso 1 calc R . . C285 C -0.1613(10) 0.7259(7) -0.6711(7) 0.104(4) Uani 1 d . . . H285 H -0.1682 0.7794 -0.7145 0.125 Uiso 1 calc R . . C286 C -0.2220(9) 0.6586(8) -0.6643(7) 0.109(4) Uani 1 d . . . H286 H -0.2578 0.6631 -0.7103 0.130 Uiso 1 calc R . . C287 C -0.2282(9) 0.5858(8) -0.5891(6) 0.097(3) Uani 1 d . . . H287 H -0.2736 0.5462 -0.5829 0.116 Uiso 1 calc R . . S31 S -0.20475(17) 0.52070(13) -0.21590(12) 0.0602(5) Uani 1 d . . . S30 S -0.02196(18) 0.47385(14) -0.30621(13) 0.0667(6) Uani 1 d . . . Ni2 Ni -0.04933(8) 0.45743(6) -0.17036(6) 0.0536(3) Uani 1 d . . . S41 S -0.08238(16) 0.42757(13) -0.03336(13) 0.0603(5) Uani 1 d . . . S42 S 0.10613(17) 0.39295(13) -0.12475(13) 0.0617(5) Uani 1 d . . . C43 C 0.0450(7) 0.3843(5) -0.0260(5) 0.063(2) Uani 1 d . . . N44 N 0.0952(5) 0.3408(4) 0.0485(4) 0.0617(17) Uani 1 d . . . C45 C 0.0374(7) 0.3457(5) 0.1278(5) 0.067(2) Uani 1 d . . . H45A H -0.0362 0.3643 0.1177 0.081 Uiso 1 calc R . . H45B H 0.0629 0.3888 0.1434 0.081 Uiso 1 calc R . . C46 C 0.0496(7) 0.2585(5) 0.2017(5) 0.063(2) Uani 1 d . . . C47 C 0.0128(8) 0.1824(6) 0.2303(6) 0.085(3) Uani 1 d . . . H47 H -0.0323 0.1655 0.2026 0.102 Uiso 1 calc R . . C48 C 0.0500(9) 0.1363(6) 0.3023(6) 0.092(3) Uani 1 d . . . H48 H 0.0314 0.0824 0.3355 0.111 Uiso 1 calc R . . C49 C 0.1193(9) 0.1753(7) 0.3243(6) 0.085(3) Uani 1 d . . . N50 N 0.1177(6) 0.2512(4) 0.2605(4) 0.0709(19) Uani 1 d . . . H50 H 0.1547 0.2905 0.2568 0.085 Uiso 1 calc R . . C51 C 0.1865(10) 0.1421(7) 0.3997(7) 0.103(4) Uani 1 d . . . C512 C 0.114(3) 0.0954(18) 0.4906(15) 0.331(18) Uani 1 d . . . H51A H 0.0408 0.1068 0.4789 0.398 Uiso 1 d . . . H51B H 0.1225 0.1211 0.5317 0.398 Uiso 1 d . . . H51C H 0.1355 0.0349 0.5129 0.398 Uiso 1 d . . . C511 C 0.1915(14) 0.2201(10) 0.4221(10) 0.163(7) Uani 1 d . . . H51D H 0.1269 0.2320 0.4523 0.196 Uiso 1 d . . . H51E H 0.2009 0.2682 0.3721 0.196 Uiso 1 d . . . H51F H 0.2484 0.2078 0.4577 0.196 Uiso 1 d . . . C52 C 0.2988(10) 0.1054(7) 0.3750(5) 0.087(3) Uani 1 d . . . C53 C 0.3921(14) 0.0998(9) 0.4043(8) 0.129(5) Uani 1 d . . . H53 H 0.4064 0.1207 0.4450 0.155 Uiso 1 calc R . . C54 C 0.4559(11) 0.0607(9) 0.3654(8) 0.116(4) Uani 1 d . . . H54 H 0.5276 0.0518 0.3711 0.140 Uiso 1 calc R . . C55 C 0.4086(7) 0.0310(6) 0.3112(5) 0.074(2) Uani 1 d . . . N56 N 0.3083(6) 0.0611(4) 0.3195(4) 0.0647(17) Uani 1 d . . . H56 H 0.2581 0.0543 0.2948 0.078 Uiso 1 calc R . . C57 C 0.4562(7) -0.0216(5) 0.2564(5) 0.065(2) Uani 1 d . . . H57A H 0.5286 -0.0432 0.2697 0.078 Uiso 1 calc R . . H57B H 0.4194 -0.0712 0.2700 0.078 Uiso 1 calc R . . N58 N 0.4525(5) 0.0262(4) 0.1684(4) 0.0618(17) Uani 1 d . . . C581 C 0.5404(9) 0.0678(10) 0.1191(8) 0.127(5) Uani 1 d . . . H58A H 0.5158 0.1281 0.0884 0.152 Uiso 1 calc R . . H58B H 0.5672 0.0406 0.0781 0.152 Uiso 1 calc R . . C582 C 0.6292(5) 0.0630(5) 0.1727(4) 0.073(2) Uani 1 d G . . C583 C 0.6407(6) 0.1336(4) 0.1938(5) 0.089(3) Uani 1 d G . . H583 H 0.5934 0.1841 0.1760 0.107 Uiso 1 calc R . . C584 C 0.7228(8) 0.1288(7) 0.2416(7) 0.197(9) Uani 1 d G . . H584 H 0.7305 0.1760 0.2557 0.237 Uiso 1 calc R . . C585 C 0.7935(7) 0.0534(9) 0.2682(7) 0.191(9) Uani 1 d G . . H585 H 0.8484 0.0501 0.3002 0.229 Uiso 1 calc R . . C586 C 0.7819(7) -0.0172(7) 0.2472(7) 0.183(8) Uani 1 d G . . H586 H 0.8292 -0.0677 0.2650 0.220 Uiso 1 calc R . . C587 C 0.6998(7) -0.0124(4) 0.1994(6) 0.123(5) Uani 1 d G . . H587 H 0.6921 -0.0597 0.1853 0.147 Uiso 1 calc R . . C59 C 0.3769(7) 0.0361(5) 0.1220(5) 0.066(2) Uani 1 d . . . S60 S 0.36617(19) 0.08789(15) 0.01656(13) 0.0700(6) Uani 1 d . . . S61 S 0.26143(16) -0.00745(13) 0.16678(13) 0.0595(5) Uani 1 d . . . C441 C 0.1990(5) 0.2894(4) 0.0510(5) 0.0531(18) Uani 1 d . . . H44A H 0.2173 0.2820 -0.0030 0.064 Uiso 1 calc R . . H44B H 0.1970 0.2325 0.0939 0.064 Uiso 1 calc R . . C442 C 0.2801(6) 0.3317(5) 0.0695(5) 0.061(2) Uani 1 d . . . C443 C 0.2913(7) 0.4210(6) 0.0200(6) 0.073(2) Uani 1 d . . . H443 H 0.2506 0.4526 -0.0256 0.088 Uiso 1 calc R . . C444 C 0.3638(7) 0.4564(6) 0.0429(6) 0.073(2) Uani 1 d . . . H444 H 0.3723 0.5139 0.0133 0.088 Uiso 1 calc R . . C445 C 0.4280(10) 0.4060(7) 0.1125(8) 0.108(4) Uani 1 d . . . H445 H 0.4755 0.4334 0.1269 0.129 Uiso 1 calc R . . C446 C 0.4235(9) 0.3218(8) 0.1581(7) 0.097(3) Uani 1 d . . . H446 H 0.4706 0.2898 0.1991 0.116 Uiso 1 calc R . . C447 C 0.3393(7) 0.2832(6) 0.1390(6) 0.074(2) Uani 1 d . . . H447 H 0.3261 0.2278 0.1727 0.089 Uiso 1 calc R . . O100 O -0.2411(7) 0.1528(5) -0.5534(6) 0.129(3) Uiso 1 d . . . O200 O -0.1632(9) 0.3532(7) -0.5803(7) 0.169(4) Uiso 1 d . . . O300 O 0.2806(9) -0.3871(7) -0.1880(7) 0.170(4) Uiso 1 d . . . O400 O -0.5524(5) 0.2199(4) -0.4445(4) 0.0807(17) Uiso 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 0.0523(6) 0.0473(5) 0.0428(5) -0.0146(4) -0.0058(4) -0.0057(4) S11 0.0606(13) 0.0682(12) 0.0466(11) -0.0094(9) -0.0049(9) -0.0116(10) S12 0.0601(12) 0.0540(10) 0.0421(10) -0.0072(8) -0.0074(9) -0.0092(9) C13 0.083(6) 0.035(3) 0.036(4) -0.013(3) -0.011(4) -0.008(3) N14 0.069(4) 0.043(3) 0.036(3) -0.004(2) -0.011(3) -0.019(3) C141 0.110(7) 0.060(5) 0.048(5) -0.008(4) -0.027(5) -0.016(5) C142 0.057(5) 0.074(5) 0.049(4) -0.014(4) -0.005(4) -0.018(4) C143 0.057(5) 0.063(5) 0.045(4) -0.012(3) -0.011(4) 0.000(4) C144 0.103(8) 0.075(6) 0.061(6) -0.026(4) -0.007(5) -0.014(5) C145 0.063(6) 0.100(7) 0.075(6) -0.044(5) -0.005(5) -0.021(5) C146 0.051(5) 0.057(4) 0.046(4) -0.010(3) -0.002(3) -0.017(3) C147 0.108(9) 0.158(11) 0.054(6) -0.028(6) -0.022(6) 0.015(8) C15 0.084(7) 0.065(5) 0.059(5) -0.009(4) -0.005(5) -0.012(4) C16 0.050(4) 0.052(4) 0.039(4) -0.011(3) 0.003(3) -0.014(3) C17 0.095(7) 0.064(5) 0.059(5) -0.023(4) -0.021(5) 0.003(5) C18 0.094(7) 0.062(5) 0.070(6) -0.030(4) -0.020(5) 0.002(4) C19 0.048(5) 0.052(4) 0.045(4) -0.012(3) -0.003(3) -0.009(3) N20 0.057(4) 0.048(3) 0.049(4) -0.017(3) -0.005(3) -0.010(3) C21 0.044(4) 0.056(4) 0.049(4) -0.010(3) -0.008(3) -0.015(3) C211 0.107(8) 0.083(6) 0.082(7) -0.032(5) -0.015(6) -0.016(5) C212 0.070(6) 0.065(5) 0.069(6) -0.017(4) -0.005(4) 0.003(4) C22 0.034(4) 0.069(5) 0.052(4) -0.020(4) -0.002(3) -0.005(3) N23 0.058(4) 0.052(3) 0.046(3) -0.010(3) -0.012(3) -0.005(3) C24 0.069(6) 0.081(6) 0.053(5) -0.006(4) -0.012(4) -0.002(5) C25 0.081(7) 0.103(7) 0.055(5) -0.017(5) -0.019(5) -0.022(5) C26 0.060(5) 0.080(5) 0.060(5) -0.028(4) -0.005(4) -0.027(4) C27 0.085(6) 0.054(4) 0.047(4) -0.001(3) -0.007(4) -0.015(4) N28 0.052(4) 0.050(3) 0.041(3) -0.015(3) -0.004(3) 0.003(3) C29 0.075(6) 0.046(4) 0.050(4) -0.023(3) -0.013(4) 0.014(4) C281 0.051(5) 0.079(5) 0.062(5) -0.035(4) -0.005(4) -0.007(4) C282 0.062(5) 0.072(5) 0.039(4) -0.016(3) -0.012(4) 0.001(4) C283 0.072(6) 0.078(6) 0.053(5) -0.022(4) 0.014(4) -0.033(5) C284 0.120(9) 0.081(6) 0.072(7) -0.020(5) -0.003(6) -0.034(6) C285 0.144(11) 0.084(7) 0.069(7) -0.005(5) 0.019(7) -0.044(7) C286 0.093(9) 0.143(10) 0.073(7) -0.027(7) -0.013(6) 0.006(8) C287 0.092(8) 0.128(9) 0.067(7) -0.034(6) 0.004(6) -0.013(6) S31 0.0654(13) 0.0647(12) 0.0476(11) -0.0190(9) -0.0034(9) -0.0028(9) S30 0.0657(14) 0.0782(13) 0.0570(12) -0.0264(10) -0.0048(10) -0.0047(10) Ni2 0.0592(7) 0.0534(6) 0.0484(6) -0.0190(4) -0.0058(5) -0.0038(4) S41 0.0561(13) 0.0679(12) 0.0545(12) -0.0209(9) -0.0038(9) -0.0035(9) S42 0.0648(14) 0.0652(12) 0.0535(12) -0.0197(9) -0.0039(10) -0.0070(10) C43 0.079(6) 0.052(4) 0.061(5) -0.024(4) -0.008(4) -0.008(4) N44 0.070(5) 0.057(4) 0.057(4) -0.019(3) -0.016(3) -0.002(3) C45 0.081(6) 0.066(5) 0.051(5) -0.018(4) 0.000(4) -0.010(4) C46 0.065(5) 0.066(5) 0.055(5) -0.022(4) -0.003(4) -0.004(4) C47 0.101(8) 0.090(7) 0.078(7) -0.038(6) -0.008(6) -0.030(6) C48 0.127(10) 0.076(6) 0.062(6) -0.008(5) 0.014(6) -0.032(6) C49 0.117(9) 0.083(6) 0.053(5) -0.022(5) -0.013(5) -0.007(6) N50 0.095(6) 0.070(4) 0.051(4) -0.017(3) -0.015(4) -0.022(4) C51 0.138(11) 0.090(7) 0.069(7) -0.018(5) -0.012(7) -0.002(7) C512 0.53(5) 0.28(3) 0.124(19) -0.009(18) -0.12(3) 0.03(3) C511 0.222(18) 0.140(12) 0.143(13) -0.081(10) -0.084(12) 0.056(11) C52 0.123(9) 0.091(7) 0.040(5) -0.018(4) 0.000(5) -0.011(6) C53 0.191(16) 0.144(12) 0.082(8) -0.062(8) -0.028(9) -0.040(10) C54 0.110(10) 0.178(13) 0.091(8) -0.057(9) -0.002(7) -0.078(9) C55 0.067(6) 0.101(7) 0.061(5) -0.030(5) -0.011(5) -0.021(5) N56 0.074(5) 0.071(4) 0.046(4) -0.019(3) -0.009(3) -0.001(3) C57 0.061(5) 0.077(5) 0.059(5) -0.024(4) -0.006(4) -0.009(4) N58 0.067(5) 0.081(4) 0.042(4) -0.023(3) 0.000(3) -0.022(4) C581 0.092(9) 0.208(14) 0.086(8) -0.048(9) 0.004(7) -0.048(9) C582 0.057(6) 0.108(7) 0.061(5) -0.035(5) 0.006(4) -0.022(5) C583 0.092(8) 0.047(5) 0.129(9) -0.034(5) 0.003(6) -0.013(4) C584 0.130(14) 0.37(3) 0.163(17) -0.15(2) 0.024(12) -0.109(17) C585 0.181(19) 0.22(2) 0.20(2) -0.095(17) -0.106(16) 0.021(15) C586 0.088(11) 0.23(2) 0.183(18) -0.040(15) -0.035(11) 0.039(12) C587 0.096(9) 0.101(9) 0.190(15) -0.081(9) 0.012(9) -0.008(7) C59 0.075(6) 0.082(5) 0.035(4) -0.020(4) 0.025(4) -0.014(4) S60 0.0733(15) 0.0803(14) 0.0510(12) -0.0167(10) -0.0040(10) -0.0102(11) S61 0.0568(13) 0.0635(11) 0.0540(11) -0.0119(9) -0.0088(10) -0.0132(9) C441 0.051(5) 0.048(4) 0.063(5) -0.025(3) -0.013(4) 0.005(3) C442 0.058(5) 0.059(5) 0.070(5) -0.028(4) -0.007(4) 0.001(4) C443 0.075(6) 0.082(6) 0.068(6) -0.041(5) -0.006(5) 0.011(5) C444 0.071(6) 0.076(6) 0.085(7) -0.043(5) 0.009(5) -0.020(5) C445 0.122(10) 0.089(8) 0.144(11) -0.066(8) -0.018(8) -0.039(7) C446 0.100(8) 0.115(9) 0.095(8) -0.052(7) -0.011(6) -0.028(7) C447 0.069(6) 0.080(6) 0.071(6) -0.033(5) -0.002(5) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S60 2.164(4) . ? Ni1 S12 2.171(4) . ? Ni1 S11 2.202(3) . ? Ni1 S61 2.221(3) . ? S11 C13 1.721(9) . ? S12 C13 1.725(7) . ? C13 N14 1.281(9) . ? N14 C15 1.453(11) . ? N14 C141 1.508(9) . ? C141 C142 1.558(10) . ? C142 C143 1.367(11) . ? C142 C146 1.456(10) . ? C143 C144 1.447(11) . ? C144 C145 1.366(12) . ? C145 C147 1.392(14) . ? C146 C147 1.494(13) . ? C15 C16 1.495(11) . ? C16 C17 1.371(10) . ? C16 N20 1.376(9) . ? C17 C18 1.417(12) . ? C18 C19 1.430(10) . ? C19 N20 1.293(8) . ? C19 C21 1.529(9) . ? C21 C211 1.511(10) . ? C21 C22 1.539(10) . ? C21 C212 1.565(11) . ? C22 N23 1.335(9) . ? C22 C26 1.385(10) . ? N23 C24 1.391(10) . ? C24 C25 1.342(12) . ? C24 C27 1.413(12) . ? C25 C26 1.382(12) . ? C27 N28 1.546(10) . ? N28 C29 1.304(9) . ? N28 C281 1.501(9) . ? C29 S30 1.667(8) . ? C29 S31 1.756(8) . ? C281 C282 1.469(11) . ? C282 C287 1.337(12) . ? C282 C283 1.447(11) . ? C283 C284 1.361(12) . ? C284 C285 1.387(14) . ? C285 C286 1.446(15) . ? C286 C287 1.418(15) . ? S31 Ni2 2.201(3) . ? S30 Ni2 2.225(4) . ? Ni2 S42 2.206(3) . ? Ni2 S41 2.211(4) . ? S41 C43 1.691(9) . ? S42 C43 1.744(9) . ? C43 N44 1.389(9) . ? N44 C441 1.469(9) . ? N44 C45 1.492(10) . ? C45 C46 1.541(11) . ? C46 C47 1.339(12) . ? C46 N50 1.371(10) . ? C47 C48 1.288(13) . ? C48 C49 1.353(14) . ? C49 N50 1.338(11) . ? C49 C51 1.517(14) . ? C51 C511 1.502(16) . ? C51 C52 1.558(15) . ? C51 C512 1.71(3) . ? C52 C53 1.340(16) . ? C52 N56 1.384(11) . ? C53 C54 1.251(18) . ? C54 C55 1.432(13) . ? C55 N56 1.327(11) . ? C55 C57 1.521(12) . ? C57 N58 1.423(10) . ? N58 C59 1.284(10) . ? N58 C581 1.456(13) . ? C581 C582 1.526(12) . ? C582 C583 1.3900 . ? C582 C587 1.3900 . ? C583 C584 1.3900 . ? C584 C585 1.3900 . ? C585 C586 1.3900 . ? C586 C587 1.3900 . ? C59 S60 1.699(8) . ? C59 S61 1.752(9) . ? C441 C442 1.484(10) . ? C442 C447 1.398(11) . ? C442 C443 1.449(12) . ? C443 C444 1.354(12) . ? C444 C445 1.442(14) . ? C445 C446 1.348(14) . ? C446 C447 1.481(13) . ? 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 S60 Ni1 S12 175.26(9) . . ? S60 Ni1 S11 100.31(10) . . ? S12 Ni1 S11 78.99(9) . . ? S60 Ni1 S61 79.87(9) . . ? S12 Ni1 S61 100.60(9) . . ? S11 Ni1 S61 177.14(9) . . ? C13 S11 Ni1 86.1(2) . . ? C13 S12 Ni1 87.0(3) . . ? N14 C13 S12 126.1(6) . . ? N14 C13 S11 126.3(5) . . ? S12 C13 S11 107.6(4) . . ? C13 N14 C15 118.9(6) . . ? C13 N14 C141 122.3(7) . . ? C15 N14 C141 118.8(6) . . ? N14 C141 C142 111.0(6) . . ? C143 C142 C146 124.6(7) . . ? C143 C142 C141 121.7(7) . . ? C146 C142 C141 113.6(7) . . ? C142 C143 C144 120.6(7) . . ? C145 C144 C143 118.6(8) . . ? C144 C145 C147 121.3(8) . . ? C142 C146 C147 111.1(7) . . ? C145 C147 C146 123.7(8) . . ? N14 C15 C16 112.1(6) . . ? C17 C16 N20 103.9(6) . . ? C17 C16 C15 133.2(7) . . ? N20 C16 C15 121.7(7) . . ? C16 C17 C18 111.4(7) . . ? C17 C18 C19 102.1(7) . . ? N20 C19 C18 109.1(6) . . ? N20 C19 C21 124.6(6) . . ? C18 C19 C21 126.0(7) . . ? C19 N20 C16 112.6(6) . . ? C211 C21 C19 112.6(6) . . ? C211 C21 C22 111.4(7) . . ? C19 C21 C22 108.8(6) . . ? C211 C21 C212 107.2(7) . . ? C19 C21 C212 109.5(6) . . ? C22 C21 C212 107.2(6) . . ? N23 C22 C26 107.4(7) . . ? N23 C22 C21 122.4(6) . . ? C26 C22 C21 130.2(7) . . ? C22 N23 C24 109.4(7) . . ? C25 C24 N23 107.1(8) . . ? C25 C24 C27 131.4(8) . . ? N23 C24 C27 121.2(8) . . ? C24 C25 C26 108.5(8) . . ? C22 C26 C25 107.3(7) . . ? C24 C27 N28 110.5(6) . . ? C29 N28 C281 122.7(6) . . ? C29 N28 C27 122.7(6) . . ? C281 N28 C27 114.1(5) . . ? N28 C29 S30 126.6(6) . . ? N28 C29 S31 121.3(6) . . ? S30 C29 S31 111.8(4) . . ? C282 C281 N28 112.8(6) . . ? C287 C282 C283 122.4(9) . . ? C287 C282 C281 120.8(9) . . ? C283 C282 C281 116.7(7) . . ? C284 C283 C282 117.5(8) . . ? C283 C284 C285 123.8(10) . . ? C284 C285 C286 115.1(9) . . ? C287 C286 C285 121.5(10) . . ? C282 C287 C286 118.1(11) . . ? C29 S31 Ni2 83.3(3) . . ? C29 S30 Ni2 84.6(3) . . ? S31 Ni2 S42 179.50(9) . . ? S31 Ni2 S41 100.00(10) . . ? S42 Ni2 S41 80.05(9) . . ? S31 Ni2 S30 79.69(9) . . ? S42 Ni2 S30 100.20(10) . . ? S41 Ni2 S30 173.76(9) . . ? C43 S41 Ni2 84.7(3) . . ? C43 S42 Ni2 83.6(3) . . ? N44 C43 S41 125.6(7) . . ? N44 C43 S42 122.7(6) . . ? S41 C43 S42 111.6(4) . . ? C43 N44 C441 122.3(7) . . ? C43 N44 C45 117.0(7) . . ? C441 N44 C45 120.6(6) . . ? N44 C45 C46 112.7(6) . . ? C47 C46 N50 104.2(8) . . ? C47 C46 C45 140.1(8) . . ? N50 C46 C45 115.8(8) . . ? C48 C47 C46 109.1(9) . . ? C47 C48 C49 112.3(9) . . ? N50 C49 C48 102.7(8) . . ? N50 C49 C51 127.4(10) . . ? C48 C49 C51 129.9(10) . . ? C49 N50 C46 111.6(8) . . ? C511 C51 C49 105.0(9) . . ? C511 C51 C52 109.5(12) . . ? C49 C51 C52 110.3(9) . . ? C511 C51 C512 92.3(13) . . ? C49 C51 C512 110.7(14) . . ? C52 C51 C512 125.8(12) . . ? C53 C52 N56 110.1(10) . . ? C53 C52 C51 131.9(11) . . ? N56 C52 C51 117.6(10) . . ? C54 C53 C52 105.4(10) . . ? C53 C54 C55 114.0(12) . . ? N56 C55 C54 102.4(9) . . ? N56 C55 C57 126.7(7) . . ? C54 C55 C57 130.9(10) . . ? C55 N56 C52 107.9(8) . . ? N58 C57 C55 113.6(7) . . ? C59 N58 C57 126.6(7) . . ? C59 N58 C581 111.5(7) . . ? C57 N58 C581 121.9(8) . . ? N58 C581 C582 113.3(9) . . ? C583 C582 C587 120.0 . . ? C583 C582 C581 120.6(8) . . ? C587 C582 C581 119.4(8) . . ? C584 C583 C582 120.0 . . ? C585 C584 C583 120.0 . . ? C584 C585 C586 120.0 . . ? C587 C586 C585 120.0 . . ? C586 C587 C582 120.0 . . ? N58 C59 S60 130.5(7) . . ? N58 C59 S61 120.2(6) . . ? S60 C59 S61 109.3(5) . . ? C59 S60 Ni1 86.2(3) . . ? C59 S61 Ni1 83.2(3) . . ? N44 C441 C442 111.5(6) . . ? C447 C442 C443 122.5(8) . . ? C447 C442 C441 117.0(8) . . ? C443 C442 C441 120.4(7) . . ? C444 C443 C442 117.1(8) . . ? C443 C444 C445 120.9(9) . . ? C446 C445 C444 124.2(9) . . ? C445 C446 C447 116.1(10) . . ? C442 C447 C446 118.8(9) . . ? _refine_diff_density_max 0.626 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.121 #===END data_7-Pd _database_code_CSD 195411 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H73 Cl0 N8 O4.50 Pd2 S8' _chemical_formula_weight 1447.54 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' Pd Pd -0.9988 1.0072 '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' Cl Cl 0.1484 0.1585 '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 13.160(17) _cell_length_b 16.82(2) _cell_length_c 17.26(2) _cell_angle_alpha 68.390(10) _cell_angle_beta 81.782(10) _cell_angle_gamma 78.999(10) _cell_volume 3475(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1490 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.375 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11783 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.02 _reflns_number_total 11783 _reflns_number_gt 6514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.1821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11783 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1433 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2632 _refine_ls_wR_factor_gt 0.2244 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.634 _refine_ls_shift/su_mean 0.038 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.20384(5) 0.07237(3) 0.04129(4) 0.0660(2) Uani 1 d . . . S11 S 0.13820(18) 0.15739(14) -0.08578(13) 0.0792(6) Uani 1 d . . . S12 S 0.02577(17) 0.06802(12) 0.06431(12) 0.0726(5) Uani 1 d . . . C13 C 0.0172(6) 0.1392(4) -0.0351(5) 0.0619(17) Uani 1 d . . . N14 N -0.0729(5) 0.1757(4) -0.0707(4) 0.0659(15) Uani 1 d . . . C141 C -0.0764(6) 0.2422(5) -0.1553(4) 0.0693(19) Uani 1 d . . . H14A H -0.0101 0.2633 -0.1714 0.083 Uiso 1 calc R . . H14B H -0.1291 0.2905 -0.1534 0.083 Uiso 1 calc R . . C142 C -0.0995(6) 0.2105(5) -0.2214(4) 0.0662(19) Uani 1 d . . . C143 C -0.0498(7) 0.1336(5) -0.2284(5) 0.078(2) Uani 1 d . . . H143 H -0.0027 0.0987 -0.1898 0.094 Uiso 1 calc R . . C144 C -0.0675(8) 0.1067(6) -0.2909(6) 0.095(3) Uani 1 d . . . H144 H -0.0347 0.0532 -0.2928 0.114 Uiso 1 calc R . . C145 C -0.1341(9) 0.1594(8) -0.3508(6) 0.108(3) Uani 1 d . . . H145 H -0.1431 0.1428 -0.3948 0.130 Uiso 1 calc R . . C146 C -0.1672(7) 0.2645(6) -0.2819(5) 0.086(2) Uani 1 d . . . H146 H -0.1988 0.3184 -0.2804 0.103 Uiso 1 calc R . . C147 C -0.1869(8) 0.2360(8) -0.3457(6) 0.103(3) Uani 1 d . . . H147 H -0.2355 0.2692 -0.3837 0.124 Uiso 1 calc R . . C15 C -0.1712(7) 0.1474(5) -0.0233(6) 0.081(2) Uani 1 d . . . H15A H -0.1801 0.0948 -0.0307 0.097 Uiso 1 calc R . . H15B H -0.1651 0.1338 0.0357 0.097 Uiso 1 calc R . . C16 C -0.2650(6) 0.2119(5) -0.0483(5) 0.071(2) Uani 1 d . . . C17 C -0.3100(7) 0.2781(5) -0.0220(5) 0.082(2) Uani 1 d . . . H17 H -0.2858 0.2945 0.0171 0.099 Uiso 1 calc R . . C18 C -0.4001(7) 0.3172(5) -0.0646(5) 0.080(2) Uani 1 d . . . H18 H -0.4458 0.3643 -0.0583 0.096 Uiso 1 calc R . . C19 C -0.4100(6) 0.2754(5) -0.1166(5) 0.0636(17) Uani 1 d . . . N20 N -0.3258(5) 0.2096(4) -0.1054(4) 0.0698(16) Uani 1 d . . . H20 H -0.3137 0.1727 -0.1305 0.084 Uiso 1 calc R . . C21 C -0.4880(6) 0.2922(5) -0.1788(5) 0.074(2) Uani 1 d . . . C211 C -0.4994(8) 0.2086(6) -0.1944(6) 0.094(3) Uani 1 d . . . H21A H -0.5300 0.1694 -0.1445 0.113 Uiso 1 calc R . . H21B H -0.4322 0.1813 -0.2089 0.113 Uiso 1 calc R . . H21C H -0.5430 0.2236 -0.2393 0.113 Uiso 1 calc R . . C212 C -0.5940(7) 0.3281(7) -0.1449(6) 0.096(3) Uani 1 d . . . H21D H -0.6156 0.2859 -0.0931 0.116 Uiso 1 calc R . . H21E H -0.6442 0.3409 -0.1847 0.116 Uiso 1 calc R . . H21F H -0.5884 0.3800 -0.1356 0.116 Uiso 1 calc R . . C22 C -0.4557(6) 0.3574(6) -0.2621(5) 0.077(2) Uani 1 d . . . N23 N -0.4023(5) 0.4234(4) -0.2666(4) 0.0706(16) Uani 1 d . . . H23 H -0.3818 0.4296 -0.2243 0.085 Uiso 1 calc R . . C24 C -0.3870(6) 0.4782(6) -0.3498(5) 0.081(2) Uani 1 d . . . C25 C -0.4312(8) 0.4455(7) -0.3957(6) 0.104(3) Uani 1 d . . . H25 H -0.4334 0.4687 -0.4535 0.125 Uiso 1 calc R . . C26 C -0.4739(8) 0.3702(7) -0.3421(6) 0.102(3) Uani 1 d . . . H26 H -0.5080 0.3361 -0.3586 0.122 Uiso 1 calc R . . C27 C -0.3251(7) 0.5506(5) -0.3739(5) 0.077(2) Uani 1 d . . . H27A H -0.3439 0.5920 -0.4281 0.092 Uiso 1 calc R . . H27B H -0.3436 0.5799 -0.3338 0.092 Uiso 1 calc R . . N28 N -0.2131(5) 0.5234(4) -0.3781(4) 0.0678(16) Uani 1 d . . . C29 C -0.1579(6) 0.5104(5) -0.3137(5) 0.071(2) Uani 1 d . . . C281 C -0.1683(7) 0.5007(5) -0.4518(5) 0.077(2) Uani 1 d . . . H28A H -0.2093 0.4624 -0.4596 0.093 Uiso 1 calc R . . H28B H -0.0983 0.4701 -0.4425 0.093 Uiso 1 calc R . . C282 C -0.1660(6) 0.5801(6) -0.5291(5) 0.073(2) Uani 1 d . . . C283 C -0.1053(7) 0.6417(6) -0.5374(5) 0.087(2) Uani 1 d . . . H283 H -0.0684 0.6340 -0.4924 0.105 Uiso 1 calc R . . C284 C -0.0958(10) 0.7131(7) -0.6075(7) 0.111(3) Uani 1 d . . . H284 H -0.0495 0.7504 -0.6122 0.133 Uiso 1 calc R . . C285 C -0.1550(11) 0.7272(8) -0.6683(9) 0.124(4) Uani 1 d . . . H285 H -0.1530 0.7775 -0.7149 0.149 Uiso 1 calc R . . C286 C -0.2187(10) 0.6713(11) -0.6657(7) 0.136(5) Uani 1 d . . . H286 H -0.2567 0.6829 -0.7111 0.164 Uiso 1 calc R . . C287 C -0.2282(8) 0.5948(8) -0.5941(6) 0.110(3) Uani 1 d . . . H287 H -0.2730 0.5569 -0.5908 0.132 Uiso 1 calc R . . S31 S -0.21398(18) 0.52091(15) -0.22056(14) 0.0797(6) Uani 1 d . . . S30 S -0.02761(17) 0.47752(16) -0.31299(14) 0.0828(6) Uani 1 d . . . Pd2 Pd -0.05123(5) 0.45756(4) -0.17120(4) 0.0690(2) Uani 1 d . . . S41 S -0.07756(17) 0.42519(14) -0.02755(14) 0.0766(6) Uani 1 d . . . S42 S 0.11002(17) 0.39075(15) -0.12133(14) 0.0787(6) Uani 1 d . . . C43 C 0.0497(6) 0.3770(5) -0.0232(6) 0.077(2) Uani 1 d . . . N44 N 0.0962(5) 0.3359(4) 0.0486(4) 0.0739(17) Uani 1 d . . . C45 C 0.0404(8) 0.3383(7) 0.1283(6) 0.096(3) Uani 1 d . . . H45A H 0.0603 0.3851 0.1401 0.115 Uiso 1 calc R . . H45B H -0.0333 0.3525 0.1208 0.115 Uiso 1 calc R . . C46 C 0.0567(8) 0.2591(6) 0.2024(5) 0.082(2) Uani 1 d . . . C47 C 0.0191(10) 0.1844(7) 0.2283(7) 0.114(4) Uani 1 d . . . H47 H -0.0266 0.1706 0.2005 0.136 Uiso 1 calc R . . C48 C 0.0599(13) 0.1296(7) 0.3047(8) 0.143(5) Uani 1 d . . . H48 H 0.0470 0.0735 0.3351 0.172 Uiso 1 calc R . . C49 C 0.1226(10) 0.1746(6) 0.3260(6) 0.112(4) Uani 1 d . . . N50 N 0.1206(6) 0.2535(5) 0.2603(4) 0.088(2) Uani 1 d . . . H50 H 0.1552 0.2934 0.2567 0.105 Uiso 1 calc R . . C51 C 0.1923(12) 0.1508(7) 0.3964(7) 0.130(5) Uani 1 d . . . C512 C 0.1419(13) 0.0839(13) 0.4720(8) 0.239(12) Uani 1 d . . . H51A H 0.0780 0.1115 0.4916 0.287 Uiso 1 calc R . . H51B H 0.1882 0.0599 0.5158 0.287 Uiso 1 calc R . . H51C H 0.1279 0.0386 0.4557 0.287 Uiso 1 calc R . . C511 C 0.1989(17) 0.2307(11) 0.4161(12) 0.264(14) Uani 1 d . . . H51D H 0.1543 0.2794 0.3821 0.316 Uiso 1 calc R . . H51E H 0.2692 0.2423 0.4047 0.316 Uiso 1 calc R . . H51F H 0.1775 0.2206 0.4741 0.316 Uiso 1 calc R . . C52 C 0.2993(11) 0.1073(7) 0.3742(6) 0.110(3) Uani 1 d . . . C53 C 0.3926(14) 0.1016(11) 0.4005(9) 0.163(6) Uani 1 d . . . H53 H 0.4054 0.1257 0.4380 0.196 Uiso 1 calc R . . C54 C 0.4665(11) 0.0542(11) 0.3627(8) 0.144(5) Uani 1 d . . . H54 H 0.5371 0.0417 0.3703 0.173 Uiso 1 calc R . . C55 C 0.4184(8) 0.0288(7) 0.3123(6) 0.095(3) Uani 1 d . . . N56 N 0.3155(7) 0.0637(4) 0.3200(4) 0.089(2) Uani 1 d . . . H56 H 0.2676 0.0586 0.2938 0.107 Uiso 1 calc R . . C57 C 0.4592(7) -0.0234(6) 0.2599(5) 0.087(3) Uani 1 d . . . H57A H 0.4163 -0.0683 0.2729 0.105 Uiso 1 calc R . . H57B H 0.5285 -0.0518 0.2752 0.105 Uiso 1 calc R . . N58 N 0.4644(6) 0.0234(5) 0.1684(5) 0.090(2) Uani 1 d . . . C581 C 0.5616(10) 0.0578(13) 0.1196(8) 0.192(9) Uani 1 d . . . H58A H 0.5935 0.0216 0.0874 0.230 Uiso 1 calc R . . H58B H 0.5417 0.1156 0.0803 0.230 Uiso 1 calc R . . C582 C 0.6385(6) 0.0613(6) 0.1706(5) 0.091(3) Uani 1 d G . . C583 C 0.6425(7) 0.1351(5) 0.1879(6) 0.133(4) Uani 1 d G . . H583 H 0.5945 0.1845 0.1669 0.159 Uiso 1 calc R . . C584 C 0.7182(10) 0.1349(8) 0.2365(7) 0.222(12) Uani 1 d G . . H584 H 0.7208 0.1842 0.2481 0.267 Uiso 1 calc R . . C585 C 0.7899(8) 0.0609(11) 0.2679(7) 0.236(14) Uani 1 d G . . H585 H 0.8405 0.0608 0.3004 0.283 Uiso 1 calc R . . C586 C 0.7859(7) -0.0128(8) 0.2506(8) 0.248(13) Uani 1 d G . . H586 H 0.8339 -0.0623 0.2715 0.298 Uiso 1 calc R . . C587 C 0.7102(8) -0.0126(5) 0.2019(7) 0.174(7) Uani 1 d G . . H587 H 0.7076 -0.0620 0.1903 0.209 Uiso 1 calc R . . C59 C 0.3831(6) 0.0337(5) 0.1237(5) 0.072(2) Uani 1 d . . . S60 S 0.37962(19) 0.08684(16) 0.02057(14) 0.0862(6) Uani 1 d . . . S61 S 0.26911(16) -0.00724(13) 0.17109(13) 0.0723(5) Uani 1 d . . . C441 C 0.2014(6) 0.2886(5) 0.0499(6) 0.081(2) Uani 1 d . . . H44A H 0.2230 0.2837 -0.0045 0.097 Uiso 1 calc R . . H44B H 0.2016 0.2306 0.0907 0.097 Uiso 1 calc R . . C442 C 0.2794(6) 0.3325(5) 0.0715(5) 0.073(2) Uani 1 d . . . C443 C 0.2910(7) 0.4173(6) 0.0249(6) 0.081(2) Uani 1 d . . . H443 H 0.2487 0.4479 -0.0186 0.098 Uiso 1 calc R . . C444 C 0.3619(8) 0.4579(7) 0.0400(7) 0.097(3) Uani 1 d . . . H444 H 0.3670 0.5153 0.0076 0.116 Uiso 1 calc R . . C445 C 0.4243(9) 0.4148(10) 0.1020(10) 0.125(4) Uani 1 d . . . H445 H 0.4728 0.4429 0.1120 0.150 Uiso 1 calc R . . C446 C 0.4183(8) 0.3287(9) 0.1521(7) 0.109(4) Uani 1 d . . . H446 H 0.4617 0.2992 0.1950 0.131 Uiso 1 calc R . . C447 C 0.3434(7) 0.2877(7) 0.1350(6) 0.093(3) Uani 1 d . . . H447 H 0.3376 0.2303 0.1669 0.112 Uiso 1 calc R . . O300 O 0.7672(7) 0.1476(5) 0.4506(5) 0.133(3) Uiso 1 d . A 2 O100 O 0.4368(8) 0.2207(6) 0.5596(6) 0.081(3) Uiso 0.67 d P B 2 O101 O 0.4770(15) 0.2229(10) 0.5349(11) 0.063(4) Uiso 0.33 d P B 2 O200 O 1.1463(11) -0.3406(9) 0.5744(9) 0.100(4) Uiso 0.50 d P C 2 C400 C 0.576(3) 0.218(2) 0.512(2) 0.176(12) Uiso 0.50 d P D 3 H40A H 0.5136 0.1948 0.5394 0.211 Uiso 0.50 calc PR D 3 H40B H 0.5581 0.2709 0.4662 0.211 Uiso 0.50 calc PR D 3 H40C H 0.6104 0.2299 0.5511 0.211 Uiso 0.50 calc PR D 3 O401 O 0.645(3) 0.155(2) 0.4801(18) 0.223(11) Uiso 0.50 d P D 3 H401 H 0.6569 0.1089 0.5187 0.267 Uiso 0.50 calc PR D 3 O501 O 0.2763(16) 0.6091(14) 0.8117(13) 0.139(6) Uiso 0.50 d P E 3 H501 H 0.2286 0.5910 0.8007 0.167 Uiso 0.50 calc PR E 3 C500 C 0.347(2) 0.618(2) 0.753(2) 0.160(10) Uiso 0.50 d P E 3 H50A H 0.3655 0.6746 0.7357 0.192 Uiso 0.50 calc PR E 3 H50B H 0.3233 0.6094 0.7073 0.192 Uiso 0.50 calc PR E 3 H50C H 0.4069 0.5754 0.7729 0.192 Uiso 0.50 calc PR E 3 O601 O 0.179(3) 0.623(3) 0.685(3) 0.267(15) Uiso 0.50 d P F 4 H601 H 0.2041 0.6474 0.6376 0.320 Uiso 0.50 calc PR F 4 C600 C 0.251(4) 0.587(3) 0.734(3) 0.217(17) Uiso 0.50 d P F 4 H60A H 0.2657 0.5260 0.7429 0.260 Uiso 0.50 calc PR F 4 H60B H 0.2303 0.5947 0.7866 0.260 Uiso 0.50 calc PR F 4 H60C H 0.3130 0.6124 0.7096 0.260 Uiso 0.50 calc PR F 4 C700 C 0.327(3) 0.579(3) 0.653(3) 0.215(17) Uiso 0.50 d P G 5 H70A H 0.3387 0.6216 0.6744 0.259 Uiso 0.50 calc PR G 5 H70B H 0.3879 0.5649 0.6201 0.259 Uiso 0.50 calc PR G 5 H70C H 0.3120 0.5280 0.6989 0.259 Uiso 0.50 calc PR G 5 O701 O 0.2224(16) 0.6205(13) 0.5913(12) 0.146(6) Uiso 0.50 d P G 5 H701 H 0.1883 0.6622 0.6016 0.175 Uiso 0.50 calc PR G 5 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 Pd1 0.0769(4) 0.0552(4) 0.0671(4) -0.0217(3) -0.0154(3) -0.0052(3) S11 0.0820(15) 0.0790(13) 0.0687(12) -0.0136(10) -0.0143(10) -0.0125(10) S12 0.0839(14) 0.0655(11) 0.0625(11) -0.0106(8) -0.0196(10) -0.0111(9) C13 0.072(5) 0.048(4) 0.067(4) -0.019(3) -0.002(4) -0.018(3) N14 0.076(4) 0.054(3) 0.064(4) -0.015(3) -0.013(3) -0.007(3) C141 0.072(5) 0.061(4) 0.063(4) -0.006(3) -0.015(4) -0.009(3) C142 0.072(5) 0.060(4) 0.058(4) -0.006(3) -0.014(4) -0.014(3) C143 0.087(6) 0.057(4) 0.089(6) -0.018(4) -0.028(5) -0.006(4) C144 0.119(8) 0.079(6) 0.095(7) -0.036(5) -0.006(6) -0.025(5) C145 0.130(9) 0.125(9) 0.082(7) -0.037(6) -0.021(6) -0.035(7) C146 0.083(6) 0.082(6) 0.076(6) -0.008(4) -0.019(5) -0.006(4) C147 0.084(7) 0.139(9) 0.069(6) -0.017(6) -0.019(5) -0.005(6) C15 0.080(6) 0.061(5) 0.086(6) -0.007(4) -0.018(5) -0.005(4) C16 0.077(5) 0.069(5) 0.064(5) -0.012(4) -0.017(4) -0.015(4) C17 0.099(7) 0.082(6) 0.074(5) -0.035(4) -0.022(5) -0.005(5) C18 0.094(6) 0.078(5) 0.079(5) -0.043(4) -0.013(5) -0.001(4) C19 0.057(5) 0.063(4) 0.065(4) -0.018(3) -0.001(3) -0.005(3) N20 0.070(4) 0.066(4) 0.073(4) -0.029(3) -0.010(3) 0.001(3) C21 0.062(5) 0.075(5) 0.083(5) -0.029(4) 0.004(4) -0.009(4) C211 0.090(7) 0.091(6) 0.105(7) -0.031(5) -0.019(5) -0.020(5) C212 0.069(6) 0.110(7) 0.096(7) -0.025(5) -0.010(5) 0.000(5) C22 0.049(4) 0.108(6) 0.068(5) -0.022(4) -0.008(4) -0.013(4) N23 0.077(4) 0.067(4) 0.065(4) -0.021(3) -0.017(3) 0.000(3) C24 0.065(5) 0.110(7) 0.061(5) -0.021(4) -0.015(4) -0.003(4) C25 0.099(7) 0.139(9) 0.065(5) -0.009(6) -0.025(5) -0.033(6) C26 0.089(7) 0.135(9) 0.091(7) -0.037(6) -0.010(5) -0.043(6) C27 0.086(6) 0.064(5) 0.063(5) -0.005(4) -0.007(4) -0.002(4) N28 0.064(4) 0.067(4) 0.056(4) -0.008(3) -0.007(3) 0.001(3) C29 0.075(5) 0.054(4) 0.069(5) -0.012(3) 0.009(4) -0.006(3) C281 0.086(6) 0.078(5) 0.066(5) -0.028(4) 0.001(4) -0.010(4) C282 0.065(5) 0.091(5) 0.059(4) -0.024(4) 0.001(4) -0.011(4) C283 0.082(6) 0.109(7) 0.069(5) -0.030(5) 0.006(4) -0.019(5) C284 0.120(9) 0.105(8) 0.085(7) -0.014(6) -0.005(7) -0.009(6) C285 0.105(10) 0.106(9) 0.135(12) -0.021(8) 0.015(8) -0.016(7) C286 0.098(9) 0.195(14) 0.065(6) -0.005(8) -0.015(6) 0.022(9) C287 0.076(7) 0.166(10) 0.086(7) -0.037(7) -0.005(5) -0.027(6) S31 0.0771(14) 0.0862(14) 0.0725(13) -0.0314(10) -0.0025(10) 0.0001(10) S30 0.0690(14) 0.1023(16) 0.0802(14) -0.0402(12) -0.0009(11) -0.0073(11) Pd2 0.0714(4) 0.0637(4) 0.0752(4) -0.0295(3) -0.0056(3) -0.0076(3) S41 0.0690(13) 0.0824(14) 0.0819(14) -0.0376(11) -0.0069(10) -0.0014(10) S42 0.0686(13) 0.0890(15) 0.0787(14) -0.0342(11) -0.0021(10) -0.0050(10) C43 0.071(5) 0.063(5) 0.098(6) -0.039(4) 0.019(5) -0.009(4) N44 0.066(4) 0.085(4) 0.076(4) -0.041(4) -0.005(3) 0.001(3) C45 0.081(6) 0.103(7) 0.108(7) -0.052(6) -0.019(5) 0.013(5) C46 0.102(7) 0.068(5) 0.079(6) -0.031(4) -0.004(5) -0.015(4) C47 0.144(10) 0.106(8) 0.112(8) -0.048(7) -0.006(7) -0.052(7) C48 0.250(17) 0.080(7) 0.117(10) -0.048(7) 0.035(10) -0.078(9) C49 0.177(12) 0.075(6) 0.074(6) -0.024(5) -0.017(7) 0.000(6) N50 0.119(6) 0.070(4) 0.078(5) -0.031(4) -0.019(4) -0.008(4) C51 0.204(14) 0.092(7) 0.084(7) -0.035(6) -0.044(8) 0.035(8) C512 0.218(18) 0.27(2) 0.083(9) 0.023(11) 0.061(10) 0.077(16) C511 0.39(3) 0.222(19) 0.25(2) -0.178(17) -0.24(2) 0.148(19) C52 0.148(11) 0.111(8) 0.064(6) -0.016(5) -0.013(6) -0.028(7) C53 0.210(17) 0.224(17) 0.119(10) -0.101(11) -0.006(11) -0.106(14) C54 0.133(11) 0.226(15) 0.122(10) -0.098(11) -0.015(8) -0.059(10) C55 0.087(7) 0.125(8) 0.087(6) -0.044(6) -0.010(5) -0.036(6) N56 0.133(7) 0.080(5) 0.063(4) -0.029(3) -0.026(4) -0.015(4) C57 0.072(6) 0.116(7) 0.076(6) -0.031(5) -0.020(4) -0.013(5) N58 0.072(5) 0.115(6) 0.088(5) -0.039(4) -0.005(4) -0.021(4) C581 0.115(11) 0.39(3) 0.095(9) -0.077(12) 0.019(7) -0.144(14) C582 0.080(6) 0.110(7) 0.101(7) -0.054(6) 0.001(5) -0.027(5) C583 0.121(10) 0.119(9) 0.151(12) -0.044(8) 0.020(8) -0.028(7) C584 0.22(2) 0.32(3) 0.25(2) -0.21(2) 0.042(17) -0.15(2) C585 0.156(18) 0.39(4) 0.178(17) -0.05(2) -0.029(14) -0.16(2) C586 0.076(10) 0.26(2) 0.32(3) 0.03(2) -0.073(14) -0.035(12) C587 0.089(10) 0.187(15) 0.28(2) -0.135(15) 0.056(11) -0.030(9) C59 0.068(5) 0.070(5) 0.081(5) -0.031(4) -0.013(4) -0.006(4) S60 0.0799(15) 0.1042(17) 0.0722(13) -0.0255(12) -0.0056(11) -0.0199(12) S61 0.0681(13) 0.0719(12) 0.0741(12) -0.0176(9) -0.0161(10) -0.0125(9) C441 0.085(6) 0.063(5) 0.099(6) -0.039(4) -0.010(5) 0.004(4) C442 0.073(5) 0.064(5) 0.086(5) -0.037(4) -0.006(4) 0.004(4) C443 0.077(6) 0.086(6) 0.084(6) -0.038(5) 0.002(4) -0.009(4) C444 0.091(7) 0.102(7) 0.098(7) -0.039(6) -0.008(6) -0.006(6) C445 0.085(8) 0.149(11) 0.181(13) -0.108(11) 0.034(8) -0.046(8) C446 0.071(6) 0.164(11) 0.115(8) -0.081(8) -0.023(6) 0.010(6) C447 0.073(6) 0.108(7) 0.098(7) -0.046(5) -0.021(5) 0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S11 2.315(3) . ? Pd1 S12 2.331(4) . ? Pd1 S61 2.335(3) . ? Pd1 S60 2.335(4) . ? S11 C13 1.728(8) . ? S12 C13 1.697(8) . ? C13 N14 1.346(9) . ? N14 C141 1.477(9) . ? N14 C15 1.489(11) . ? C141 C142 1.513(10) . ? C142 C143 1.372(10) . ? C142 C146 1.403(10) . ? C143 C144 1.376(11) . ? C144 C145 1.382(13) . ? C145 C147 1.369(14) . ? C146 C147 1.424(13) . ? C15 C16 1.476(11) . ? C16 C17 1.357(11) . ? C16 N20 1.371(9) . ? C17 C18 1.405(11) . ? C18 C19 1.359(10) . ? C19 N20 1.388(9) . ? C19 C21 1.506(10) . ? C21 C22 1.514(12) . ? C21 C212 1.536(12) . ? C21 C211 1.564(11) . ? C22 C26 1.366(12) . ? C22 N23 1.397(10) . ? N23 C24 1.402(10) . ? C24 C25 1.357(12) . ? C24 C27 1.493(12) . ? C25 C26 1.426(14) . ? C27 N28 1.458(10) . ? N28 C29 1.343(10) . ? N28 C281 1.473(10) . ? C29 S30 1.698(9) . ? C29 S31 1.726(8) . ? C281 C282 1.504(11) . ? C282 C283 1.380(12) . ? C282 C287 1.404(12) . ? C283 C284 1.366(13) . ? C284 C285 1.321(15) . ? C285 C286 1.360(18) . ? C286 C287 1.428(17) . ? S31 Pd2 2.330(3) . ? S30 Pd2 2.327(4) . ? Pd2 S41 2.323(4) . ? Pd2 S42 2.325(3) . ? S41 C43 1.714(9) . ? S42 C43 1.718(9) . ? C43 N44 1.346(10) . ? N44 C441 1.458(10) . ? N44 C45 1.475(11) . ? C45 C46 1.473(13) . ? C46 C47 1.335(13) . ? C46 N50 1.362(10) . ? C47 C48 1.411(16) . ? C48 C49 1.385(16) . ? C49 N50 1.390(12) . ? C49 C51 1.516(15) . ? C51 C511 1.522(17) . ? C51 C52 1.524(17) . ? C51 C512 1.538(19) . ? C52 C53 1.344(18) . ? C52 N56 1.359(12) . ? C53 C54 1.38(2) . ? C54 C55 1.369(13) . ? C55 N56 1.378(12) . ? C55 C57 1.464(13) . ? C57 N58 1.480(11) . ? N58 C59 1.356(10) . ? N58 C581 1.516(14) . ? C581 C582 1.456(12) . ? C582 C583 1.3900 . ? C582 C587 1.3900 . ? C583 C584 1.3900 . ? C584 C585 1.3900 . ? C585 C586 1.3900 . ? C586 C587 1.3900 . ? C59 S60 1.674(9) . ? C59 S61 1.738(9) . ? C441 C442 1.529(11) . ? C442 C447 1.375(11) . ? C442 C443 1.381(12) . ? C443 C444 1.359(13) . ? C444 C445 1.342(16) . ? C445 C446 1.397(16) . ? C446 C447 1.424(14) . ? C400 O401 1.48(4) . ? O501 C500 1.26(3) . ? O601 C600 1.28(4) . ? C700 O701 1.74(4) . ? 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 S11 Pd1 S12 75.24(9) . . ? S11 Pd1 S61 177.18(8) . . ? S12 Pd1 S61 104.86(9) . . ? S11 Pd1 S60 104.36(10) . . ? S12 Pd1 S60 175.47(8) . . ? S61 Pd1 S60 75.31(9) . . ? C13 S11 Pd1 86.2(3) . . ? C13 S12 Pd1 86.4(3) . . ? N14 C13 S12 124.1(6) . . ? N14 C13 S11 124.0(6) . . ? S12 C13 S11 111.8(4) . . ? C13 N14 C141 121.9(6) . . ? C13 N14 C15 118.7(6) . . ? C141 N14 C15 119.4(6) . . ? N14 C141 C142 114.0(6) . . ? C143 C142 C146 118.7(7) . . ? C143 C142 C141 122.1(6) . . ? C146 C142 C141 119.0(7) . . ? C142 C143 C144 122.0(8) . . ? C143 C144 C145 119.7(9) . . ? C147 C145 C144 120.5(9) . . ? C142 C146 C147 119.3(8) . . ? C145 C147 C146 119.7(8) . . ? C16 C15 N14 114.5(6) . . ? C17 C16 N20 107.5(7) . . ? C17 C16 C15 131.2(7) . . ? N20 C16 C15 121.3(8) . . ? C16 C17 C18 107.3(7) . . ? C19 C18 C17 109.4(7) . . ? C18 C19 N20 105.6(7) . . ? C18 C19 C21 131.8(7) . . ? N20 C19 C21 122.5(6) . . ? C16 N20 C19 110.1(6) . . ? C19 C21 C22 110.3(7) . . ? C19 C21 C212 108.4(7) . . ? C22 C21 C212 109.6(7) . . ? C19 C21 C211 112.6(7) . . ? C22 C21 C211 107.5(7) . . ? C212 C21 C211 108.5(7) . . ? C26 C22 N23 106.8(8) . . ? C26 C22 C21 131.9(9) . . ? N23 C22 C21 121.2(7) . . ? C22 N23 C24 110.3(6) . . ? C25 C24 N23 105.6(8) . . ? C25 C24 C27 132.3(8) . . ? N23 C24 C27 122.0(7) . . ? C24 C25 C26 109.9(8) . . ? C22 C26 C25 107.4(8) . . ? N28 C27 C24 114.1(7) . . ? C29 N28 C27 121.2(6) . . ? C29 N28 C281 122.8(6) . . ? C27 N28 C281 115.5(6) . . ? N28 C29 S30 124.1(6) . . ? N28 C29 S31 122.9(6) . . ? S30 C29 S31 112.9(5) . . ? N28 C281 C282 111.1(7) . . ? C283 C282 C287 118.2(9) . . ? C283 C282 C281 121.2(7) . . ? C287 C282 C281 120.6(9) . . ? C284 C283 C282 124.2(10) . . ? C285 C284 C283 117.4(12) . . ? C284 C285 C286 122.8(12) . . ? C285 C286 C287 121.0(11) . . ? C282 C287 C286 116.3(11) . . ? C29 S31 Pd2 85.0(3) . . ? C29 S30 Pd2 85.7(3) . . ? S41 Pd2 S42 75.25(9) . . ? S41 Pd2 S30 174.86(8) . . ? S42 Pd2 S30 104.34(9) . . ? S41 Pd2 S31 104.68(9) . . ? S42 Pd2 S31 178.48(8) . . ? S30 Pd2 S31 75.60(9) . . ? C43 S41 Pd2 86.6(3) . . ? C43 S42 Pd2 86.4(3) . . ? N44 C43 S41 123.6(6) . . ? N44 C43 S42 124.9(6) . . ? S41 C43 S42 111.5(5) . . ? C43 N44 C441 121.6(7) . . ? C43 N44 C45 119.8(6) . . ? C441 N44 C45 118.6(7) . . ? C46 C45 N44 117.1(7) . . ? C47 C46 N50 107.2(9) . . ? C47 C46 C45 132.4(10) . . ? N50 C46 C45 120.4(8) . . ? C46 C47 C48 109.2(9) . . ? C49 C48 C47 107.5(9) . . ? C48 C49 N50 105.0(9) . . ? C48 C49 C51 133.5(11) . . ? N50 C49 C51 121.2(11) . . ? C46 N50 C49 111.0(8) . . ? C49 C51 C511 110.2(9) . . ? C49 C51 C52 110.5(9) . . ? C511 C51 C52 111.7(14) . . ? C49 C51 C512 106.0(14) . . ? C511 C51 C512 110.6(14) . . ? C52 C51 C512 107.7(9) . . ? C53 C52 N56 106.1(12) . . ? C53 C52 C51 131.0(12) . . ? N56 C52 C51 122.9(11) . . ? C52 C53 C54 109.2(10) . . ? C55 C54 C53 108.7(12) . . ? C54 C55 N56 104.7(10) . . ? C54 C55 C57 131.4(11) . . ? N56 C55 C57 124.0(8) . . ? C52 N56 C55 111.4(9) . . ? C55 C57 N58 116.4(8) . . ? C59 N58 C57 121.0(8) . . ? C59 N58 C581 116.7(8) . . ? C57 N58 C581 122.2(8) . . ? C582 C581 N58 114.7(9) . . ? C583 C582 C587 120.0 . . ? C583 C582 C581 122.5(11) . . ? C587 C582 C581 117.5(11) . . ? C582 C583 C584 120.0 . . ? C585 C584 C583 120.0 . . ? C584 C585 C586 120.0 . . ? C587 C586 C585 120.0 . . ? C586 C587 C582 120.0 . . ? N58 C59 S60 125.1(7) . . ? N58 C59 S61 121.5(7) . . ? S60 C59 S61 113.4(4) . . ? C59 S60 Pd1 85.9(3) . . ? C59 S61 Pd1 84.5(3) . . ? N44 C441 C442 112.6(6) . . ? C447 C442 C443 118.1(8) . . ? C447 C442 C441 121.1(8) . . ? C443 C442 C441 120.7(8) . . ? C444 C443 C442 122.7(9) . . ? C445 C444 C443 119.6(11) . . ? C444 C445 C446 121.6(10) . . ? C445 C446 C447 117.7(10) . . ? C442 C447 C446 120.3(10) . . ? _refine_diff_density_max 1.111 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.113 #===END