Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'F. A. Cotton' _publ_contact_author_address ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry Texas A&M University, PO Box 30012 College Station, TX 77842-3012, USA ; _publ_contact_author_email cotton@tamu.edu _publ_contact_author_fax '(979) 845 9351' _publ_contact_author_phone '(979) 845 4432' # TITLE AND AUTHOR LIST _publ_section_title ; Making connections with molecular wires: extending tri-nickel chains with axial cyanide, dicyanamide, and phenylacetylide ligands ; loop_ _publ_author_name _publ_author_address 'John F. Berry' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; 'F. Albert Cotton' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; 'Carlos A. Murillo' ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry, PO Box 30012 College Station, TX 77842-3012, USA ; data_Compound_3 _database_code_CSD 207897 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(dpa)4(CN)2,CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety Ni3(C10H8N3)4(CN)2,CH2Cl2 _chemical_formula_sum 'C43 H34 Cl2 N14 Ni3' _chemical_formula_weight 993.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnn2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 13.0161(12) _cell_length_b 14.0693(13) _cell_length_c 11.4942(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2104.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5059 _cell_measurement_theta_min 4.6 _cell_measurement_theta_max 55 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5256 _exptl_absorpt_correction_T_max 0.5911 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12152 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.59 _reflns_number_total 4178 _reflns_number_gt 4041 _reflns_threshold_expression I>2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+0.5055P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(12) _refine_ls_number_reflns 4178 _refine_ls_number_parameters 285 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 1.162515(15) 0.588162(14) -2.00202(3) 0.01996(6) Uani 1 1 d . . . Ni2 Ni 1.0000 0.5000 -1.99950(4) 0.01753(7) Uani 1 2 d S . . N1 N 1.22069(13) 0.46191(12) -2.06678(15) 0.0223(3) Uani 1 1 d . . . N2 N 1.05423(15) 0.41771(13) -2.11582(18) 0.0213(4) Uani 1 1 d . . . N3 N 0.88854(12) 0.37909(12) -2.17028(15) 0.0229(3) Uani 1 1 d . . . N4 N 1.17492(13) 0.52866(12) -1.83351(16) 0.0236(3) Uani 1 1 d . . . N5 N 1.05104(16) 0.41729(12) -1.88221(18) 0.0220(4) Uani 1 1 d . . . N6 N 0.93063(13) 0.30434(12) -1.93635(17) 0.0268(4) Uani 1 1 d . . . N7 N 1.36797(16) 0.70688(16) -2.0182(2) 0.0474(6) Uani 1 1 d . . . C1 C 1.29411(14) 0.66336(13) -2.0080(3) 0.0287(4) Uani 1 1 d . . . C11 C 1.15793(14) 0.39668(15) -2.11591(19) 0.0225(4) Uani 1 1 d . . . C12 C 1.19958(17) 0.31020(15) -2.1574(2) 0.0340(5) Uani 1 1 d . . . H12A H 1.1568 0.2642 -2.1894 0.041 Uiso 1 1 calc R . . C13 C 1.30370(18) 0.29459(17) -2.1501(2) 0.0394(6) Uani 1 1 d . . . H13A H 1.3314 0.2384 -2.1790 0.047 Uiso 1 1 calc R . . C14 C 1.36782(18) 0.36216(18) -2.0998(2) 0.0378(5) Uani 1 1 d . . . H14A H 1.4384 0.3527 -2.0943 0.045 Uiso 1 1 calc R . . C15 C 1.32199(16) 0.44377(16) -2.0586(2) 0.0301(5) Uani 1 1 d . . . H15A H 1.3635 0.4890 -2.0230 0.036 Uiso 1 1 calc R . . C31 C 0.98931(15) 0.38523(15) -2.20061(18) 0.0241(4) Uani 1 1 d . . . C32 C 1.02032(17) 0.36406(18) -2.3156(2) 0.0341(5) Uani 1 1 d . . . H32A H 1.0891 0.3689 -2.3365 0.041 Uiso 1 1 calc R . . C33 C 0.94846(19) 0.3363(2) -2.3964(2) 0.0414(6) Uani 1 1 d . . . H33A H 0.9687 0.3204 -2.4715 0.050 Uiso 1 1 calc R . . C34 C 0.84514(19) 0.3322(2) -2.3651(2) 0.0416(6) Uani 1 1 d . . . H34A H 0.7951 0.3150 -2.4188 0.050 Uiso 1 1 calc R . . C35 C 0.81968(17) 0.35446(18) -2.2524(2) 0.0320(5) Uani 1 1 d . . . H35A H 0.7507 0.3524 -2.2315 0.038 Uiso 1 1 calc R . . C41 C 1.11717(15) 0.45330(14) -1.79972(18) 0.0243(4) Uani 1 1 d . . . C42 C 1.12265(19) 0.41911(17) -1.6848(2) 0.0349(5) Uani 1 1 d . . . H42A H 1.0810 0.3690 -1.6611 0.042 Uiso 1 1 calc R . . C43 C 1.1905(2) 0.4606(2) -1.6076(2) 0.0433(6) Uani 1 1 d . . . H43A H 1.1954 0.4379 -1.5318 0.052 Uiso 1 1 calc R . . C44 C 1.2511(2) 0.5358(2) -1.6430(2) 0.0417(6) Uani 1 1 d . . . H44A H 1.2977 0.5641 -1.5923 0.050 Uiso 1 1 calc R . . C45 C 1.24033(17) 0.56765(16) -1.7554(2) 0.0309(4) Uani 1 1 d . . . H45A H 1.2803 0.6189 -1.7792 0.037 Uiso 1 1 calc R . . C61 C 1.02097(16) 0.32365(15) -1.88253(19) 0.0263(4) Uani 1 1 d . . . C62 C 1.08113(18) 0.24906(16) -1.8376(3) 0.0383(6) Uani 1 1 d . . . H62A H 1.1430 0.2623 -1.8005 0.046 Uiso 1 1 calc R . . C63 C 1.0482(2) 0.15664(18) -1.8486(3) 0.0574(9) Uani 1 1 d . . . H63A H 1.0873 0.1071 -1.8184 0.069 Uiso 1 1 calc R . . C64 C 0.9564(2) 0.13766(18) -1.9048(4) 0.0640(10) Uani 1 1 d . . . H64A H 0.9326 0.0756 -1.9126 0.077 Uiso 1 1 calc R . . C65 C 0.90147(19) 0.21258(16) -1.9488(3) 0.0439(6) Uani 1 1 d . . . H65A H 0.8411 0.1997 -1.9891 0.053 Uiso 1 1 calc R . . C1S C 0.48466(14) 0.44402(14) -1.80365(18) 0.1101(8) Uani 0.50 1 d PD . 1 H1SA H 0.5318 0.4117 -1.8557 0.132 Uiso 0.50 1 calc PR . 1 H1SB H 0.4167 0.4387 -1.8377 0.132 Uiso 0.50 1 calc PR . 1 Cl2S Cl 0.48343(14) 0.38081(14) -1.67211(16) 0.0653(4) Uani 0.50 1 d PD A 1 Cl1S Cl 0.48466(14) 0.44402(14) -1.80365(18) 0.1101(8) Uani 0.50 1 d P . 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 0.01434(10) 0.02113(10) 0.02443(11) -0.00174(13) -0.00022(13) -0.00095(7) Ni2 0.01366(13) 0.01817(13) 0.02076(14) 0.000 0.000 0.00091(9) N1 0.0168(8) 0.0249(8) 0.0252(8) -0.0031(7) 0.0001(6) 0.0019(6) N2 0.0164(10) 0.0232(9) 0.0242(9) -0.0032(7) 0.0009(8) -0.0002(7) N3 0.0161(8) 0.0269(7) 0.0258(8) -0.0030(7) -0.0005(6) -0.0015(6) N4 0.0194(8) 0.0257(8) 0.0258(9) -0.0036(7) -0.0014(7) 0.0023(6) N5 0.0172(10) 0.0214(8) 0.0273(10) 0.0029(7) -0.0013(8) 0.0025(6) N6 0.0220(9) 0.0230(8) 0.0353(10) 0.0033(7) -0.0024(7) -0.0010(6) N7 0.0285(9) 0.0526(11) 0.0612(17) -0.0016(12) -0.0013(11) -0.0158(8) C1 0.0222(8) 0.0316(9) 0.0324(10) -0.0036(11) -0.0019(12) -0.0012(7) C11 0.0174(10) 0.0268(9) 0.0232(9) -0.0006(8) 0.0015(7) 0.0015(7) C12 0.0248(11) 0.0290(10) 0.0482(13) -0.0130(11) -0.0015(10) 0.0013(8) C13 0.0258(11) 0.0345(11) 0.0579(16) -0.0167(12) -0.0010(11) 0.0104(9) C14 0.0194(10) 0.0434(13) 0.0507(15) -0.0115(11) -0.0029(10) 0.0084(9) C15 0.0190(10) 0.0346(11) 0.0368(12) -0.0075(10) -0.0052(9) 0.0005(8) C31 0.0193(9) 0.0248(9) 0.0280(10) -0.0016(8) -0.0001(8) -0.0017(7) C32 0.0218(10) 0.0519(14) 0.0285(10) -0.0076(10) 0.0049(9) -0.0027(9) C33 0.0331(13) 0.0641(17) 0.0269(11) -0.0114(11) 0.0007(9) -0.0030(11) C34 0.0290(12) 0.0645(17) 0.0312(12) -0.0113(12) -0.0047(9) -0.0069(11) C35 0.0208(10) 0.0413(12) 0.0340(11) -0.0070(10) -0.0014(9) -0.0045(9) C41 0.0190(10) 0.0258(9) 0.0281(10) 0.0011(8) 0.0003(8) 0.0057(7) C42 0.0361(13) 0.0418(12) 0.0268(11) 0.0056(9) -0.0035(10) -0.0011(9) C43 0.0490(15) 0.0552(15) 0.0257(11) 0.0033(11) -0.0072(11) 0.0029(12) C44 0.0413(14) 0.0515(14) 0.0323(12) -0.0092(11) -0.0130(11) -0.0006(11) C45 0.0266(11) 0.0327(10) 0.0336(11) -0.0070(9) -0.0035(9) 0.0011(9) C61 0.0209(9) 0.0257(9) 0.0324(10) 0.0039(9) 0.0009(8) 0.0023(8) C62 0.0263(12) 0.0289(11) 0.0596(16) 0.0075(11) -0.0130(11) 0.0030(9) C63 0.0384(15) 0.0275(11) 0.106(3) 0.0194(14) -0.0245(16) 0.0027(10) C64 0.0433(16) 0.0220(11) 0.127(3) 0.0120(15) -0.0284(18) -0.0066(10) C65 0.0296(12) 0.0238(10) 0.0784(18) 0.0060(12) -0.0133(12) -0.0054(9) C1S 0.0742(11) 0.1493(17) 0.1069(15) -0.0650(13) -0.0354(11) 0.0494(12) Cl2S 0.0561(9) 0.0781(11) 0.0617(9) 0.0112(9) 0.0062(8) 0.0081(8) Cl1S 0.0742(11) 0.1493(17) 0.1069(15) -0.0650(13) -0.0354(11) 0.0494(12) _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 C1 2.0144(19) . ? Ni1 N1 2.0695(17) . ? Ni1 N6 2.0801(17) 2_765 ? Ni1 N3 2.0962(18) 2_765 ? Ni1 N4 2.1163(19) . ? Ni1 Ni2 2.4523(3) . ? Ni2 N5 1.9007(19) 2_765 ? Ni2 N5 1.9007(19) . ? Ni2 N2 1.904(2) 2_765 ? Ni2 N2 1.904(2) . ? Ni2 Ni1 2.4523(3) 2_765 ? N1 C15 1.346(3) . ? N1 C11 1.352(3) . ? N2 C31 1.368(3) . ? N2 C11 1.382(3) . ? N3 C35 1.347(3) . ? N3 C31 1.360(2) . ? N3 Ni1 2.0962(18) 2_765 ? N4 C45 1.353(3) . ? N4 C41 1.356(3) . ? N5 C61 1.374(3) . ? N5 C41 1.377(3) . ? N6 C65 1.353(3) . ? N6 C61 1.356(3) . ? N6 Ni1 2.0800(17) 2_765 ? N7 C1 1.146(3) . ? C11 C12 1.415(3) . ? C12 C13 1.375(3) . ? C13 C14 1.391(3) . ? C14 C15 1.378(3) . ? C31 C32 1.414(3) . ? C32 C33 1.375(3) . ? C33 C34 1.393(3) . ? C34 C35 1.373(3) . ? C41 C42 1.407(3) . ? C42 C43 1.382(4) . ? C43 C44 1.381(4) . ? C44 C45 1.375(4) . ? C61 C62 1.408(3) . ? C62 C63 1.375(3) . ? C63 C64 1.384(4) . ? C64 C65 1.370(4) . ? C1S C1S 1.625(4) 2_665 ? C1S Cl2S 1.754(3) . ? 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 C1 Ni1 N1 97.32(8) . . ? C1 Ni1 N6 97.25(8) . 2_765 ? N1 Ni1 N6 165.43(7) . 2_765 ? C1 Ni1 N3 97.05(9) . 2_765 ? N1 Ni1 N3 88.44(7) . 2_765 ? N6 Ni1 N3 89.44(7) 2_765 2_765 ? C1 Ni1 N4 100.02(10) . . ? N1 Ni1 N4 87.81(7) . . ? N6 Ni1 N4 90.00(7) 2_765 . ? N3 Ni1 N4 162.85(6) 2_765 . ? C1 Ni1 Ni2 178.17(7) . . ? N1 Ni1 Ni2 83.44(5) . . ? N6 Ni1 Ni2 81.99(5) 2_765 . ? N3 Ni1 Ni2 81.30(5) 2_765 . ? N4 Ni1 Ni2 81.66(5) . . ? N5 Ni2 N5 89.65(12) 2_765 . ? N5 Ni2 N2 89.78(6) 2_765 2_765 ? N5 Ni2 N2 178.70(11) . 2_765 ? N5 Ni2 N2 178.70(11) 2_765 . ? N5 Ni2 N2 89.78(6) . . ? N2 Ni2 N2 90.81(12) 2_765 . ? N5 Ni2 Ni1 90.01(6) 2_765 . ? N5 Ni2 Ni1 90.95(6) . . ? N2 Ni2 Ni1 90.23(6) 2_765 . ? N2 Ni2 Ni1 88.83(6) . . ? N5 Ni2 Ni1 90.95(6) 2_765 2_765 ? N5 Ni2 Ni1 90.01(6) . 2_765 ? N2 Ni2 Ni1 88.83(6) 2_765 2_765 ? N2 Ni2 Ni1 90.22(6) . 2_765 ? Ni1 Ni2 Ni1 178.65(2) . 2_765 ? C15 N1 C11 119.48(17) . . ? C15 N1 Ni1 119.73(14) . . ? C11 N1 Ni1 120.78(13) . . ? C31 N2 C11 122.08(19) . . ? C31 N2 Ni2 118.31(15) . . ? C11 N2 Ni2 119.52(15) . . ? C35 N3 C31 118.57(19) . . ? C35 N3 Ni1 119.49(14) . 2_765 ? C31 N3 Ni1 121.89(13) . 2_765 ? C45 N4 C41 118.40(19) . . ? C45 N4 Ni1 119.65(15) . . ? C41 N4 Ni1 121.94(14) . . ? C61 N5 C41 122.17(19) . . ? C61 N5 Ni2 119.04(15) . . ? C41 N5 Ni2 118.79(14) . . ? C65 N6 C61 118.84(19) . . ? C65 N6 Ni1 119.47(15) . 2_765 ? C61 N6 Ni1 121.69(14) . 2_765 ? N7 C1 Ni1 176.0(3) . . ? N1 C11 N2 116.39(18) . . ? N1 C11 C12 119.53(18) . . ? N2 C11 C12 123.96(19) . . ? C13 C12 C11 119.6(2) . . ? C12 C13 C14 120.5(2) . . ? C15 C14 C13 116.9(2) . . ? N1 C15 C14 123.9(2) . . ? N3 C31 N2 115.73(18) . . ? N3 C31 C32 120.11(19) . . ? N2 C31 C32 124.05(19) . . ? C33 C32 C31 119.8(2) . . ? C32 C33 C34 119.6(2) . . ? C35 C34 C33 117.8(2) . . ? N3 C35 C34 124.0(2) . . ? N4 C41 N5 115.90(18) . . ? N4 C41 C42 120.51(19) . . ? N5 C41 C42 123.5(2) . . ? C43 C42 C41 119.4(2) . . ? C44 C43 C42 120.0(2) . . ? C45 C44 C43 117.9(2) . . ? N4 C45 C44 123.8(2) . . ? N6 C61 N5 116.11(18) . . ? N6 C61 C62 120.03(19) . . ? N5 C61 C62 123.7(2) . . ? C63 C62 C61 119.8(2) . . ? C62 C63 C64 119.6(2) . . ? C65 C64 C63 118.3(2) . . ? N6 C65 C64 123.3(2) . . ? C1S C1S Cl2S 119.58(10) 2_665 . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.396 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.071 #===END of Compound 3.CH2Cl2 ================ data_Compound_4 _database_code_CSD 207898 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(dpa)4(NCNCN)2,(CH2Cl2)2.5 _chemical_melting_point 'not measured' _chemical_formula_moiety 'Ni3(C10H8N3)4(N3C2)2 (CH2Cl2)2.5' _chemical_formula_sum 'C46.50 H37 Cl5 N18 Ni3' _chemical_formula_weight 1201.32 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3181(8) _cell_length_b 11.9122(9) _cell_length_c 20.7918(15) _cell_angle_alpha 102.8300(10) _cell_angle_beta 91.261(2) _cell_angle_gamma 111.5660(10) _cell_volume 2525.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5247 _cell_measurement_theta_min 5 _cell_measurement_theta_max 55 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1222 _exptl_absorpt_coefficient_mu 1.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6742 _exptl_absorpt_correction_T_max 0.9067 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17215 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.56 _reflns_number_total 11074 _reflns_number_gt 7551 _reflns_threshold_expression I>2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0448P)^2^+6.6699P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11074 _refine_ls_number_parameters 661 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.22656(5) 0.71220(5) 0.17815(3) 0.02427(14) Uani 1 1 d . . . Ni2 Ni 0.10012(5) 0.71420(5) 0.26950(3) 0.01944(12) Uani 1 1 d . . . Ni3 Ni -0.02418(5) 0.71814(5) 0.36190(3) 0.02194(13) Uani 1 1 d . . . N1 N 0.1525(4) 0.5209(3) 0.17216(17) 0.0273(8) Uani 1 1 d . . . N2 N -0.0104(3) 0.5492(3) 0.22953(17) 0.0246(8) Uani 1 1 d . . . N3 N -0.1697(3) 0.5790(3) 0.29043(18) 0.0257(8) Uani 1 1 d . . . N4 N 0.0591(4) 0.6965(3) 0.12502(17) 0.0271(8) Uani 1 1 d . . . N5 N -0.0037(3) 0.7722(3) 0.22498(17) 0.0237(8) Uani 1 1 d . . . N6 N -0.0564(3) 0.8560(3) 0.32586(17) 0.0240(8) Uani 1 1 d . . . N7 N 0.2752(3) 0.9037(3) 0.20575(17) 0.0264(8) Uani 1 1 d . . . N8 N 0.2110(3) 0.8795(3) 0.30809(16) 0.0227(7) Uani 1 1 d . . . N9 N 0.1473(3) 0.8555(3) 0.41092(17) 0.0240(8) Uani 1 1 d . . . N10 N 0.3658(3) 0.7317(3) 0.25189(18) 0.0264(8) Uani 1 1 d . . . N11 N 0.2029(3) 0.6555(3) 0.31452(17) 0.0236(8) Uani 1 1 d . . . N12 N 0.0397(3) 0.5830(3) 0.37785(17) 0.0238(8) Uani 1 1 d . . . N13 N 0.3296(4) 0.7028(4) 0.1015(2) 0.0403(10) Uani 1 1 d . A . N14 N 0.4002(16) 0.6415(15) -0.0073(9) 0.050 Uiso 0.330(13) 1 d P A 1 N14A N 0.4406(16) 0.6263(13) 0.0137(8) 0.050 Uiso 0.421(13) 1 d P A 2 N14B N 0.501(2) 0.667(2) 0.0402(11) 0.050 Uiso 0.249(11) 1 d P A 3 N15 N 0.6022(7) 0.7439(8) -0.0463(3) 0.102(3) Uani 1 1 d . A . N16 N -0.1344(4) 0.7216(3) 0.43896(19) 0.0294(8) Uani 1 1 d . B . N17 N -0.276(5) 0.752(5) 0.519(3) 0.050 Uiso 0.126(14) 1 d P B 1 N17A N -0.342(2) 0.658(4) 0.4819(12) 0.050 Uiso 0.33(4) 1 d P B 2 N17B N -0.3247(17) 0.703(3) 0.4927(10) 0.050 Uiso 0.55(4) 1 d P B 3 N18 N -0.3936(5) 0.6364(6) 0.5941(3) 0.0663(15) Uani 1 1 d . B . C1 C 0.3851(7) 0.6793(6) 0.0595(3) 0.0607(18) Uani 1 1 d . . . C2 C 0.5267(7) 0.7001(7) -0.0170(3) 0.0633(18) Uani 1 1 d . . . C3 C -0.2196(5) 0.7061(5) 0.4665(3) 0.0407(12) Uani 1 1 d . . . C4 C -0.3572(5) 0.6614(6) 0.5457(3) 0.0469(14) Uani 1 1 d . . . C11 C 0.0410(4) 0.4675(4) 0.1966(2) 0.0256(9) Uani 1 1 d . . . C12 C -0.0093(5) 0.3395(4) 0.1926(3) 0.0392(12) Uani 1 1 d . . . H12A H -0.0869 0.3032 0.2085 0.047 Uiso 1 1 calc R . . C13 C 0.0566(6) 0.2682(5) 0.1653(3) 0.0457(13) Uani 1 1 d . . . H13A H 0.0233 0.1828 0.1618 0.055 Uiso 1 1 calc R . . C14 C 0.1734(5) 0.3239(5) 0.1428(2) 0.0407(12) Uani 1 1 d . . . H14A H 0.2205 0.2772 0.1251 0.049 Uiso 1 1 calc R . . C15 C 0.2175(5) 0.4487(4) 0.1473(2) 0.0319(10) Uani 1 1 d . . . H15A H 0.2960 0.4861 0.1326 0.038 Uiso 1 1 calc R . . C31 C -0.1392(4) 0.5148(4) 0.2356(2) 0.0263(9) Uani 1 1 d . . . C32 C -0.2357(5) 0.4277(4) 0.1857(2) 0.0379(11) Uani 1 1 d . . . H32A H -0.2146 0.3837 0.1480 0.046 Uiso 1 1 calc R . . C33 C -0.3615(5) 0.4083(5) 0.1935(3) 0.0490(14) Uani 1 1 d . . . H33A H -0.4260 0.3508 0.1610 0.059 Uiso 1 1 calc R . . C34 C -0.3920(5) 0.4738(5) 0.2493(3) 0.0459(13) Uani 1 1 d . . . H34A H -0.4767 0.4616 0.2552 0.055 Uiso 1 1 calc R . . C35 C -0.2939(4) 0.5575(4) 0.2958(3) 0.0342(11) Uani 1 1 d . . . H35A H -0.3144 0.6023 0.3335 0.041 Uiso 1 1 calc R . . C41 C -0.0298(4) 0.7300(4) 0.1568(2) 0.0269(9) Uani 1 1 d . . . C42 C -0.1451(5) 0.7133(5) 0.1217(2) 0.0378(12) Uani 1 1 d . . . H42A H -0.2069 0.7347 0.1442 0.045 Uiso 1 1 calc R . . C43 C -0.1663(6) 0.6653(5) 0.0543(3) 0.0521(16) Uani 1 1 d . . . H43A H -0.2420 0.6543 0.0305 0.062 Uiso 1 1 calc R . . C44 C -0.0727(6) 0.6333(5) 0.0220(3) 0.0505(15) Uani 1 1 d . . . H44A H -0.0842 0.6012 -0.0237 0.061 Uiso 1 1 calc R . . C45 C 0.0364(5) 0.6499(5) 0.0588(2) 0.0381(12) Uani 1 1 d . . . H45A H 0.0985 0.6279 0.0369 0.046 Uiso 1 1 calc R . . C61 C -0.0446(4) 0.8586(4) 0.2614(2) 0.0239(9) Uani 1 1 d . . . C62 C -0.0614(4) 0.9544(4) 0.2377(2) 0.0305(10) Uani 1 1 d . . . H62A H -0.0564 0.9547 0.1931 0.037 Uiso 1 1 calc R . . C63 C -0.0854(5) 1.0471(4) 0.2807(2) 0.0342(11) Uani 1 1 d . . . H63A H -0.0965 1.1107 0.2654 0.041 Uiso 1 1 calc R . . C64 C -0.0929(5) 1.0456(4) 0.3469(2) 0.0335(11) Uani 1 1 d . . . H64A H -0.1077 1.1083 0.3769 0.040 Uiso 1 1 calc R . . C65 C -0.0779(4) 0.9493(4) 0.3670(2) 0.0267(9) Uani 1 1 d . . . H65A H -0.0829 0.9483 0.4115 0.032 Uiso 1 1 calc R . . C71 C 0.2611(4) 0.9586(4) 0.2676(2) 0.0248(9) Uani 1 1 d . . . C72 C 0.2863(4) 1.0867(4) 0.2853(2) 0.0320(10) Uani 1 1 d . . . H72A H 0.2762 1.1243 0.3279 0.038 Uiso 1 1 calc R . . C73 C 0.3255(5) 1.1562(5) 0.2399(3) 0.0416(13) Uani 1 1 d . . . H73A H 0.3425 1.2411 0.2516 0.050 Uiso 1 1 calc R . . C74 C 0.3398(5) 1.0991(5) 0.1763(3) 0.0412(12) Uani 1 1 d . . . H74A H 0.3668 1.1446 0.1447 0.049 Uiso 1 1 calc R . . C75 C 0.3129(5) 0.9740(5) 0.1616(2) 0.0361(11) Uani 1 1 d . . . H75A H 0.3210 0.9352 0.1188 0.043 Uiso 1 1 calc R . . C91 C 0.2381(4) 0.9183(4) 0.3763(2) 0.0233(9) Uani 1 1 d . . . C92 C 0.3546(4) 1.0103(4) 0.4092(2) 0.0309(10) Uani 1 1 d . . . H92A H 0.4169 1.0524 0.3852 0.037 Uiso 1 1 calc R . . C93 C 0.3759(5) 1.0376(4) 0.4770(2) 0.0351(11) Uani 1 1 d . . . H93A H 0.4517 1.1000 0.4994 0.042 Uiso 1 1 calc R . . C94 C 0.2839(5) 0.9717(4) 0.5124(2) 0.0341(11) Uani 1 1 d . . . H94A H 0.2974 0.9879 0.5583 0.041 Uiso 1 1 calc R . . C95 C 0.1728(4) 0.8823(4) 0.4775(2) 0.0306(10) Uani 1 1 d . . . H95A H 0.1115 0.8374 0.5010 0.037 Uiso 1 1 calc R . . C101 C 0.3314(4) 0.6948(4) 0.3076(2) 0.0246(9) Uani 1 1 d . . . C102 C 0.4254(4) 0.7080(4) 0.3576(2) 0.0295(10) Uani 1 1 d . . . H10A H 0.4015 0.6819 0.3960 0.035 Uiso 1 1 calc R . . C103 C 0.5521(4) 0.7596(4) 0.3490(2) 0.0352(11) Uani 1 1 d . . . H10B H 0.6149 0.7685 0.3815 0.042 Uiso 1 1 calc R . . C104 C 0.5862(5) 0.7983(5) 0.2917(3) 0.0394(12) Uani 1 1 d . . . H10C H 0.6716 0.8336 0.2850 0.047 Uiso 1 1 calc R . . C105 C 0.4909(4) 0.7834(4) 0.2452(2) 0.0349(11) Uani 1 1 d . . . H10D H 0.5137 0.8104 0.2069 0.042 Uiso 1 1 calc R . . C121 C 0.1448(4) 0.5721(4) 0.35174(19) 0.0229(9) Uani 1 1 d . . . C122 C 0.1821(5) 0.4744(4) 0.3582(2) 0.0330(10) Uani 1 1 d . . . H12B H 0.2545 0.4675 0.3405 0.040 Uiso 1 1 calc R . . C123 C 0.1100(5) 0.3897(4) 0.3910(3) 0.0376(12) Uani 1 1 d . . . H12C H 0.1330 0.3240 0.3951 0.045 Uiso 1 1 calc R . . C124 C 0.0032(5) 0.4009(4) 0.4181(2) 0.0370(11) Uani 1 1 d . . . H12D H -0.0460 0.3445 0.4409 0.044 Uiso 1 1 calc R . . C125 C -0.0273(5) 0.4986(4) 0.4100(2) 0.0314(10) Uani 1 1 d . . . H12E H -0.0990 0.5067 0.4281 0.038 Uiso 1 1 calc R . . C1S C -0.3614(6) 1.2984(6) 0.3687(3) 0.068(2) Uani 1 1 d D . . H1SA H -0.4477 1.2947 0.3606 0.082 Uiso 1 1 calc R . . H1SB H -0.3028 1.3729 0.3578 0.082 Uiso 1 1 calc R . . Cl1 Cl -0.3467(2) 1.1667(3) 0.31752(15) 0.1162(9) Uani 1 1 d D . . Cl2 Cl -0.32762(17) 1.3067(2) 0.45303(11) 0.0880(7) Uani 1 1 d D . . C2S C -0.0887(8) 0.9370(19) 0.0039(8) 0.149(11) Uani 0.50 1 d PD . . H2SA H -0.1532 0.9558 0.0291 0.179 Uiso 0.50 1 calc PR . . H2SB H -0.1227 0.8485 -0.0172 0.179 Uiso 0.50 1 calc PR . . Cl3 Cl 0.0523(2) 0.97627(19) 0.05838(10) 0.0859(6) Uani 1 1 d D . . C3S C -0.3842(16) 1.0417(18) 0.0784(9) 0.147(8) Uiso 0.57 1 d PD C 1 H3SA H -0.4420 0.9689 0.0458 0.177 Uiso 0.57 1 calc PR C 1 H3SB H -0.4353 1.0806 0.1043 0.177 Uiso 0.57 1 calc PR C 1 Cl4 Cl -0.2960(4) 0.9929(4) 0.1327(2) 0.0897(13) Uiso 0.57 1 d PD C 1 Cl5 Cl -0.2809(4) 1.1494(3) 0.03607(19) 0.0771(10) Uiso 0.57 1 d PD C 1 C3SA C -0.2785(19) 1.0285(17) 0.0596(7) 0.087(6) Uiso 0.43 1 d PD D 2 H3SC H -0.1866 1.0594 0.0583 0.104 Uiso 0.43 1 calc PR D 2 H3SD H -0.3186 0.9465 0.0295 0.104 Uiso 0.43 1 calc PR D 2 Cl4A Cl -0.3221(6) 1.0311(6) 0.1434(3) 0.0990(19) Uiso 0.43 1 d PD D 2 Cl5A Cl -0.3453(7) 1.1340(6) 0.0441(3) 0.110(2) Uiso 0.43 1 d PD D 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 0.0297(3) 0.0263(3) 0.0180(3) 0.0058(2) 0.0039(2) 0.0119(2) Ni2 0.0220(3) 0.0184(3) 0.0174(3) 0.0034(2) 0.00003(19) 0.0079(2) Ni3 0.0247(3) 0.0213(3) 0.0203(3) 0.0057(2) 0.0028(2) 0.0090(2) N1 0.034(2) 0.028(2) 0.0217(19) 0.0064(15) -0.0006(15) 0.0149(17) N2 0.0268(19) 0.0186(18) 0.0258(19) 0.0016(15) -0.0001(15) 0.0081(15) N3 0.0253(19) 0.0213(18) 0.029(2) 0.0066(15) 0.0016(15) 0.0069(15) N4 0.037(2) 0.0257(19) 0.0208(18) 0.0046(15) 0.0009(15) 0.0149(17) N5 0.0283(19) 0.0213(18) 0.0214(18) 0.0036(14) -0.0012(14) 0.0105(15) N6 0.0260(19) 0.0212(18) 0.0245(19) 0.0050(15) 0.0003(14) 0.0093(15) N7 0.030(2) 0.029(2) 0.0202(18) 0.0060(15) 0.0011(15) 0.0118(16) N8 0.0244(18) 0.0228(18) 0.0177(17) 0.0034(14) -0.0011(14) 0.0064(15) N9 0.0252(18) 0.0229(18) 0.0244(19) 0.0074(15) 0.0022(14) 0.0088(15) N10 0.030(2) 0.0245(19) 0.0246(19) 0.0040(15) 0.0021(15) 0.0119(16) N11 0.0251(18) 0.0246(19) 0.0246(19) 0.0055(15) 0.0015(14) 0.0137(15) N12 0.0285(19) 0.0220(18) 0.0192(18) 0.0042(14) 0.0007(14) 0.0082(15) N13 0.055(3) 0.047(3) 0.024(2) 0.0149(19) 0.0112(19) 0.021(2) N15 0.080(5) 0.172(8) 0.061(4) 0.043(5) 0.038(4) 0.048(5) N16 0.029(2) 0.031(2) 0.033(2) 0.0179(17) 0.0070(17) 0.0112(17) N18 0.066(4) 0.100(5) 0.053(3) 0.025(3) 0.022(3) 0.050(3) C1 0.087(5) 0.055(4) 0.049(4) 0.019(3) 0.044(4) 0.031(4) C2 0.067(4) 0.105(6) 0.037(3) 0.032(4) 0.026(3) 0.045(4) C3 0.045(3) 0.049(3) 0.041(3) 0.021(3) 0.017(2) 0.027(3) C4 0.041(3) 0.061(4) 0.049(3) 0.018(3) 0.015(3) 0.028(3) C11 0.034(2) 0.025(2) 0.019(2) 0.0041(17) 0.0015(17) 0.0141(19) C12 0.048(3) 0.027(3) 0.041(3) 0.007(2) 0.009(2) 0.013(2) C13 0.071(4) 0.024(2) 0.046(3) 0.007(2) 0.017(3) 0.022(3) C14 0.059(3) 0.036(3) 0.036(3) 0.010(2) 0.013(2) 0.029(3) C15 0.043(3) 0.037(3) 0.021(2) 0.0062(19) 0.0031(19) 0.022(2) C31 0.027(2) 0.021(2) 0.029(2) 0.0065(18) -0.0005(18) 0.0062(18) C32 0.038(3) 0.031(3) 0.033(3) -0.001(2) -0.002(2) 0.006(2) C33 0.033(3) 0.039(3) 0.054(4) -0.001(3) -0.013(2) -0.002(2) C34 0.024(2) 0.044(3) 0.060(4) 0.007(3) -0.002(2) 0.007(2) C35 0.030(2) 0.031(3) 0.043(3) 0.011(2) 0.006(2) 0.012(2) C41 0.038(3) 0.021(2) 0.022(2) 0.0057(18) -0.0012(18) 0.0125(19) C42 0.041(3) 0.038(3) 0.034(3) 0.002(2) -0.011(2) 0.020(2) C43 0.066(4) 0.048(3) 0.041(3) -0.003(3) -0.023(3) 0.031(3) C44 0.082(4) 0.049(3) 0.025(3) -0.006(2) -0.014(3) 0.039(3) C45 0.058(3) 0.038(3) 0.022(2) 0.003(2) -0.001(2) 0.026(3) C61 0.022(2) 0.020(2) 0.027(2) 0.0039(17) -0.0017(17) 0.0073(17) C62 0.042(3) 0.027(2) 0.028(2) 0.0112(19) 0.007(2) 0.016(2) C63 0.043(3) 0.026(2) 0.041(3) 0.014(2) 0.008(2) 0.018(2) C64 0.039(3) 0.025(2) 0.039(3) 0.006(2) 0.010(2) 0.015(2) C65 0.031(2) 0.023(2) 0.024(2) 0.0026(18) 0.0054(18) 0.0097(18) C71 0.022(2) 0.024(2) 0.025(2) 0.0065(18) -0.0032(17) 0.0051(17) C72 0.036(3) 0.025(2) 0.032(3) 0.006(2) 0.002(2) 0.010(2) C73 0.045(3) 0.029(3) 0.048(3) 0.015(2) -0.001(2) 0.008(2) C74 0.049(3) 0.038(3) 0.039(3) 0.023(2) 0.007(2) 0.011(2) C75 0.041(3) 0.038(3) 0.029(3) 0.016(2) 0.006(2) 0.012(2) C91 0.028(2) 0.020(2) 0.022(2) 0.0044(17) 0.0006(17) 0.0099(17) C92 0.026(2) 0.030(2) 0.027(2) 0.0025(19) 0.0000(18) 0.0014(19) C93 0.032(3) 0.032(3) 0.032(3) -0.001(2) -0.007(2) 0.008(2) C94 0.043(3) 0.038(3) 0.018(2) 0.002(2) -0.002(2) 0.015(2) C95 0.034(2) 0.034(3) 0.023(2) 0.0087(19) 0.0034(19) 0.012(2) C101 0.025(2) 0.023(2) 0.026(2) 0.0014(17) -0.0005(17) 0.0119(18) C102 0.034(2) 0.030(2) 0.024(2) 0.0041(19) -0.0013(18) 0.015(2) C103 0.031(3) 0.034(3) 0.039(3) -0.001(2) -0.007(2) 0.016(2) C104 0.025(2) 0.042(3) 0.049(3) 0.008(2) 0.004(2) 0.011(2) C105 0.032(3) 0.036(3) 0.037(3) 0.008(2) 0.008(2) 0.014(2) C121 0.028(2) 0.025(2) 0.0145(19) 0.0034(16) -0.0029(16) 0.0099(18) C122 0.037(3) 0.032(2) 0.034(3) 0.009(2) 0.002(2) 0.016(2) C123 0.044(3) 0.029(3) 0.047(3) 0.016(2) 0.003(2) 0.019(2) C124 0.041(3) 0.033(3) 0.040(3) 0.019(2) 0.009(2) 0.011(2) C125 0.035(3) 0.031(2) 0.027(2) 0.009(2) 0.0047(19) 0.010(2) C1S 0.047(4) 0.073(5) 0.097(6) 0.044(4) 0.009(3) 0.025(3) Cl1 0.0875(16) 0.127(2) 0.147(2) 0.0142(18) 0.0304(15) 0.0672(16) Cl2 0.0554(10) 0.1232(18) 0.0964(15) 0.0664(14) 0.0192(10) 0.0234(11) C2S 0.149(19) 0.16(2) 0.075(13) 0.064(13) -0.038(12) -0.034(15) Cl3 0.1165(17) 0.0678(12) 0.0754(13) 0.0142(10) 0.0186(12) 0.0392(12) _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 N13 2.003(4) . ? Ni1 N7 2.078(4) . ? Ni1 N10 2.087(3) . ? Ni1 N1 2.092(4) . ? Ni1 N4 2.099(4) . ? Ni1 Ni2 2.4044(8) . ? Ni2 N8 1.879(3) . ? Ni2 N2 1.882(3) . ? Ni2 N5 1.883(3) . ? Ni2 N11 1.887(3) . ? Ni2 Ni3 2.4082(8) . ? Ni3 N16 2.054(4) . ? Ni3 N12 2.075(3) . ? Ni3 N9 2.079(3) . ? Ni3 N6 2.090(3) . ? Ni3 N3 2.112(4) . ? N1 C15 1.353(6) . ? N1 C11 1.355(6) . ? N2 C11 1.375(5) . ? N2 C31 1.378(5) . ? N3 C35 1.346(6) . ? N3 C31 1.352(6) . ? N4 C45 1.346(6) . ? N4 C41 1.348(6) . ? N5 C61 1.367(5) . ? N5 C41 1.380(5) . ? N6 C65 1.346(5) . ? N6 C61 1.355(5) . ? N7 C71 1.349(5) . ? N7 C75 1.350(5) . ? N8 C71 1.379(5) . ? N8 C91 1.381(5) . ? N9 C95 1.349(5) . ? N9 C91 1.356(5) . ? N10 C101 1.343(5) . ? N10 C105 1.345(6) . ? N11 C101 1.377(5) . ? N11 C121 1.379(5) . ? N12 C125 1.340(5) . ? N12 C121 1.355(5) . ? N13 C1 1.131(7) . ? N14 C2 1.385(17) . ? N14 C1 1.396(17) . ? N14A C1 1.324(14) . ? N14A C2 1.332(14) . ? N14B C2 1.34(2) . ? N14B C1 1.44(2) . ? N15 C2 1.100(8) . ? N16 C3 1.110(6) . ? N17 C4 1.36(4) . ? N17 C3 1.39(4) . ? N17A C4 1.34(2) . ? N17A C3 1.37(2) . ? N17B C3 1.312(13) . ? N17B C4 1.315(13) . ? N18 C4 1.153(7) . ? C11 C12 1.400(6) . ? C12 C13 1.367(7) . ? C13 C14 1.388(7) . ? C14 C15 1.364(7) . ? C31 C32 1.409(6) . ? C32 C33 1.375(7) . ? C33 C34 1.373(8) . ? C34 C35 1.369(7) . ? C41 C42 1.407(6) . ? C42 C43 1.370(7) . ? C43 C44 1.390(8) . ? C44 C45 1.363(7) . ? C61 C62 1.410(6) . ? C62 C63 1.373(6) . ? C63 C64 1.385(7) . ? C64 C65 1.368(6) . ? C71 C72 1.404(6) . ? C72 C73 1.366(6) . ? C73 C74 1.388(7) . ? C74 C75 1.367(7) . ? C91 C92 1.405(6) . ? C92 C93 1.369(6) . ? C93 C94 1.388(7) . ? C94 C95 1.369(6) . ? C101 C102 1.412(6) . ? C102 C103 1.371(7) . ? C103 C104 1.383(7) . ? C104 C105 1.367(7) . ? C121 C122 1.407(6) . ? C122 C123 1.369(7) . ? C123 C124 1.382(7) . ? C124 C125 1.371(6) . ? C1S Cl1 1.755(6) . ? C1S Cl2 1.761(6) . ? C2S Cl3 1.785(5) . ? C2S Cl3 1.794(5) 2_575 ? Cl3 C2S 1.794(5) 2_575 ? C3S Cl5 1.797(12) . ? C3S Cl4 1.810(12) . ? C3SA Cl5A 1.766(12) . ? C3SA Cl4A 1.818(12) . ? 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 N13 Ni1 N7 99.10(16) . . ? N13 Ni1 N10 97.27(16) . . ? N7 Ni1 N10 89.16(14) . . ? N13 Ni1 N1 95.72(16) . . ? N7 Ni1 N1 165.14(15) . . ? N10 Ni1 N1 87.84(14) . . ? N13 Ni1 N4 97.66(16) . . ? N7 Ni1 N4 88.09(14) . . ? N10 Ni1 N4 165.07(15) . . ? N1 Ni1 N4 91.08(14) . . ? N13 Ni1 Ni2 177.59(13) . . ? N7 Ni1 Ni2 83.31(10) . . ? N10 Ni1 Ni2 82.59(10) . . ? N1 Ni1 Ni2 81.87(11) . . ? N4 Ni1 Ni2 82.51(10) . . ? N8 Ni2 N2 179.10(16) . . ? N8 Ni2 N5 89.98(15) . . ? N2 Ni2 N5 89.57(15) . . ? N8 Ni2 N11 90.25(15) . . ? N2 Ni2 N11 90.20(15) . . ? N5 Ni2 N11 179.50(17) . . ? N8 Ni2 Ni1 89.20(11) . . ? N2 Ni2 Ni1 90.02(11) . . ? N5 Ni2 Ni1 90.59(11) . . ? N11 Ni2 Ni1 89.86(11) . . ? N8 Ni2 Ni3 90.16(11) . . ? N2 Ni2 Ni3 90.62(11) . . ? N5 Ni2 Ni3 89.75(11) . . ? N11 Ni2 Ni3 89.81(11) . . ? Ni1 Ni2 Ni3 179.28(3) . . ? N16 Ni3 N12 98.53(14) . . ? N16 Ni3 N9 98.51(15) . . ? N12 Ni3 N9 89.55(13) . . ? N16 Ni3 N6 96.76(14) . . ? N12 Ni3 N6 164.69(14) . . ? N9 Ni3 N6 87.31(13) . . ? N16 Ni3 N3 96.74(15) . . ? N12 Ni3 N3 88.99(13) . . ? N9 Ni3 N3 164.73(14) . . ? N6 Ni3 N3 90.11(13) . . ? N16 Ni3 Ni2 178.34(11) . . ? N12 Ni3 Ni2 82.67(10) . . ? N9 Ni3 Ni2 82.63(10) . . ? N6 Ni3 Ni2 82.07(10) . . ? N3 Ni3 Ni2 82.11(10) . . ? C15 N1 C11 118.3(4) . . ? C15 N1 Ni1 121.2(3) . . ? C11 N1 Ni1 120.5(3) . . ? C11 N2 C31 122.9(4) . . ? C11 N2 Ni2 118.6(3) . . ? C31 N2 Ni2 118.5(3) . . ? C35 N3 C31 118.3(4) . . ? C35 N3 Ni3 121.3(3) . . ? C31 N3 Ni3 120.2(3) . . ? C45 N4 C41 118.5(4) . . ? C45 N4 Ni1 120.9(3) . . ? C41 N4 Ni1 120.6(3) . . ? C61 N5 C41 123.0(3) . . ? C61 N5 Ni2 118.3(3) . . ? C41 N5 Ni2 118.6(3) . . ? C65 N6 C61 118.9(4) . . ? C65 N6 Ni3 120.9(3) . . ? C61 N6 Ni3 120.0(3) . . ? C71 N7 C75 118.7(4) . . ? C71 N7 Ni1 119.9(3) . . ? C75 N7 Ni1 121.2(3) . . ? C71 N8 C91 122.0(4) . . ? C71 N8 Ni2 119.1(3) . . ? C91 N8 Ni2 118.8(3) . . ? C95 N9 C91 118.3(4) . . ? C95 N9 Ni3 121.1(3) . . ? C91 N9 Ni3 120.6(3) . . ? C101 N10 C105 119.0(4) . . ? C101 N10 Ni1 120.2(3) . . ? C105 N10 Ni1 120.8(3) . . ? C101 N11 C121 122.8(3) . . ? C101 N11 Ni2 119.0(3) . . ? C121 N11 Ni2 118.2(3) . . ? C125 N12 C121 118.3(4) . . ? C125 N12 Ni3 120.7(3) . . ? C121 N12 Ni3 120.8(3) . . ? C1 N13 Ni1 169.2(5) . . ? C2 N14 C1 109.4(12) . . ? C1 N14A C2 117.4(11) . . ? C2 N14B C1 109.7(15) . . ? C3 N16 Ni3 160.7(4) . . ? C4 N17 C3 114(3) . . ? C4 N17A C3 117.1(18) . . ? C3 N17B C4 122.7(10) . . ? N13 C1 N14A 166.6(9) . . ? N13 C1 N14 153.8(11) . . ? N14A C1 N14 30.6(7) . . ? N13 C1 N14B 147.2(12) . . ? N14A C1 N14B 33.2(9) . . ? N14 C1 N14B 59.0(12) . . ? N15 C2 N14A 168.2(10) . . ? N15 C2 N14B 145.5(13) . . ? N14A C2 N14B 34.6(9) . . ? N15 C2 N14 153.0(11) . . ? N14A C2 N14 30.7(7) . . ? N14B C2 N14 61.6(12) . . ? N16 C3 N17B 168.3(8) . . ? N16 C3 N17A 161.5(16) . . ? N17B C3 N17A 21.3(9) . . ? N16 C3 N17 148(2) . . ? N17B C3 N17 31.7(19) . . ? N17A C3 N17 50(2) . . ? N18 C4 N17B 170.5(11) . . ? N18 C4 N17A 163.3(18) . . ? N17B C4 N17A 21.6(10) . . ? N18 C4 N17 145(2) . . ? N17B C4 N17 32.0(19) . . ? N17A C4 N17 52(3) . . ? N1 C11 N2 115.1(4) . . ? N1 C11 C12 120.8(4) . . ? N2 C11 C12 123.9(4) . . ? C13 C12 C11 119.6(5) . . ? C12 C13 C14 119.6(5) . . ? C15 C14 C13 118.4(5) . . ? N1 C15 C14 123.3(5) . . ? N3 C31 N2 115.8(4) . . ? N3 C31 C32 120.4(4) . . ? N2 C31 C32 123.5(4) . . ? C33 C32 C31 119.3(5) . . ? C34 C33 C32 120.1(5) . . ? C35 C34 C33 117.9(5) . . ? N3 C35 C34 124.0(5) . . ? N4 C41 N5 115.8(4) . . ? N4 C41 C42 120.6(4) . . ? N5 C41 C42 123.5(4) . . ? C43 C42 C41 119.9(5) . . ? C42 C43 C44 118.8(5) . . ? C45 C44 C43 118.7(5) . . ? N4 C45 C44 123.5(5) . . ? N6 C61 N5 115.8(4) . . ? N6 C61 C62 120.1(4) . . ? N5 C61 C62 123.9(4) . . ? C63 C62 C61 119.6(4) . . ? C62 C63 C64 119.7(4) . . ? C65 C64 C63 118.2(4) . . ? N6 C65 C64 123.5(4) . . ? N7 C71 N8 115.6(4) . . ? N7 C71 C72 120.2(4) . . ? N8 C71 C72 124.0(4) . . ? C73 C72 C71 120.1(5) . . ? C72 C73 C74 119.5(5) . . ? C75 C74 C73 118.0(4) . . ? N7 C75 C74 123.5(5) . . ? N9 C91 N8 115.5(4) . . ? N9 C91 C92 120.7(4) . . ? N8 C91 C92 123.6(4) . . ? C93 C92 C91 119.5(4) . . ? C92 C93 C94 119.8(4) . . ? C95 C94 C93 118.0(4) . . ? N9 C95 C94 123.7(4) . . ? N10 C101 N11 116.0(4) . . ? N10 C101 C102 120.4(4) . . ? N11 C101 C102 123.4(4) . . ? C103 C102 C101 119.3(4) . . ? C102 C103 C104 119.7(4) . . ? C105 C104 C103 118.3(4) . . ? N10 C105 C104 123.4(5) . . ? N12 C121 N11 115.2(3) . . ? N12 C121 C122 120.7(4) . . ? N11 C121 C122 123.8(4) . . ? C123 C122 C121 119.0(5) . . ? C122 C123 C124 120.5(4) . . ? C125 C124 C123 117.4(4) . . ? N12 C125 C124 124.2(5) . . ? Cl1 C1S Cl2 110.9(4) . . ? Cl3 C2S Cl3 110.0(4) . 2_575 ? C2S Cl3 C2S 70.0(4) . 2_575 ? Cl5 C3S Cl4 112.3(9) . . ? Cl5A C3SA Cl4A 96.6(8) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.829 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.095 #===END of Compound 4.2.5CH2Cl2 ================ data_Compound_5 _database_code_CSD 207899 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni3(dpa)4(CCPh)2,0.3methanol _chemical_melting_point ? _chemical_formula_moiety Ni3(C10H8N3)4(C8H5)2,(CH3OH)0.3 _chemical_formula_sum 'C56.30 H43.20 N12 Ni3 O0.30' _chemical_formula_weight 1068.76 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' 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 37.149(3) _cell_length_b 15.8661(12) _cell_length_c 17.1491(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.435(2) _cell_angle_gamma 90.00 _cell_volume 10098.8(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4713 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 55 _exptl_crystal_description plate _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4411 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7381 _exptl_absorpt_correction_T_max 0.8621 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16101 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11952 _reflns_number_gt 9267 _reflns_threshold_expression I>2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.612(17) _refine_ls_number_reflns 11952 _refine_ls_number_parameters 1266 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.77337(2) 0.36513(6) 0.41538(4) 0.0307(2) Uani 1 1 d . . . Ni2 Ni 0.74928(2) 0.36639(6) 0.27844(4) 0.02807(19) Uani 1 1 d . A . Ni3 Ni 0.72443(2) 0.36824(7) 0.14233(5) 0.0400(2) Uani 1 1 d . . . Ni4 Ni 0.52037(2) 0.13222(6) 0.63997(4) 0.0349(2) Uani 1 1 d . . . Ni5 Ni 0.5000 0.13396(8) 0.5000 0.0279(3) Uani 1 2 d S . . Ni6 Ni 0.5000 0.62170(8) 0.0000 0.0291(3) Uani 1 2 d S . . Ni7 Ni 0.47845(2) 0.62025(7) 0.13285(4) 0.0372(2) Uani 1 1 d . . . N1 N 0.74001(15) 0.2585(4) 0.4192(3) 0.0340(14) Uani 1 1 d . . . N2 N 0.73942(16) 0.2505(4) 0.2848(3) 0.0343(14) Uani 1 1 d . . . N3 N 0.73825(17) 0.2401(4) 0.1504(3) 0.0425(16) Uani 1 1 d . A . N4 N 0.81263(15) 0.2910(3) 0.3659(3) 0.0267(13) Uani 1 1 d . . . N5 N 0.79599(15) 0.3427(3) 0.2429(3) 0.0303(14) Uani 1 1 d . . . N6 N 0.77855(15) 0.3933(4) 0.1211(3) 0.0333(14) Uani 1 1 d . A . N7 N 0.80209(15) 0.4694(4) 0.3734(3) 0.0329(14) Uani 1 1 d . . . N8 N 0.75977(16) 0.4826(3) 0.2723(3) 0.0314(13) Uani 1 1 d . . . N9 N 0.71856(16) 0.4977(4) 0.1687(3) 0.0411(16) Uani 1 1 d . A . N10 N 0.72853(15) 0.4428(4) 0.4311(3) 0.0353(14) Uani 1 1 d . . . N11 N 0.70300(15) 0.3916(4) 0.3143(3) 0.0353(14) Uani 1 1 d . . . N12 N 0.67658(16) 0.3424(4) 0.1989(4) 0.0411(16) Uani 1 1 d . A . N13 N 0.43418(15) 0.1886(4) 0.4086(3) 0.0328(14) Uani 1 1 d . . . N14 N 0.45130(15) 0.1343(4) 0.5289(3) 0.0350(14) Uani 1 1 d . . . N15 N 0.46794(16) 0.0845(4) 0.6516(3) 0.0372(15) Uani 1 1 d . B . N16 N 0.53841(16) 0.0114(4) 0.6104(3) 0.0381(15) Uani 1 1 d . B . N17 N 0.5000 0.0143(5) 0.5000 0.0311(19) Uani 1 2 d S . . N18 N 0.49793(16) 0.2533(4) 0.6351(3) 0.0343(14) Uani 1 1 d . B . N19 N 0.5000 0.2528(5) 0.5000 0.0279(19) Uani 1 2 d S . . N21 N 0.53186(15) 0.5798(4) 0.1568(3) 0.0352(14) Uani 1 1 d . . . N22 N 0.53413(15) 0.5377(3) 0.0299(3) 0.0318(14) Uani 1 1 d . . . N23 N 0.56901(17) 0.6633(4) -0.0719(3) 0.0392(15) Uani 1 1 d . . . N24 N 0.49678(18) 0.7460(4) 0.1271(3) 0.0421(16) Uani 1 1 d . . . N25 N 0.53339(16) 0.7062(3) 0.0292(3) 0.0307(14) Uani 1 1 d . . . N26 N 0.53746(16) 0.4978(4) -0.1003(3) 0.0409(15) Uani 1 1 d . . . C7 C 0.4623(2) 0.6175(6) 0.2417(4) 0.0473(19) Uani 1 1 d . . . C8 C 0.4556(2) 0.6019(6) 0.3077(4) 0.056(2) Uani 1 1 d . . . C11 C 0.72904(18) 0.2162(5) 0.3548(4) 0.0356(17) Uani 1 1 d . A . C12 C 0.70616(19) 0.1460(5) 0.3597(4) 0.0445(19) Uani 1 1 d . . . H12A H 0.6978 0.1184 0.3146 0.053 Uiso 1 1 calc R A . C13 C 0.6962(2) 0.1185(5) 0.4321(4) 0.0512(19) Uani 1 1 d . A . H13A H 0.6820 0.0706 0.4361 0.061 Uiso 1 1 calc R . . C14 C 0.7074(2) 0.1630(6) 0.4995(5) 0.052(2) Uani 1 1 d . . . H14A H 0.7007 0.1464 0.5488 0.062 Uiso 1 1 calc R A . C15 C 0.7286(2) 0.2315(5) 0.4891(4) 0.044(2) Uani 1 1 d . A . H15A H 0.7359 0.2621 0.5332 0.052 Uiso 1 1 calc R . . C31 C 0.74329(19) 0.2005(5) 0.2197(4) 0.0362(18) Uani 1 1 d . A . C32 C 0.7552(2) 0.1163(5) 0.2233(4) 0.0455(19) Uani 1 1 d . . . H32A H 0.7591 0.0895 0.2711 0.055 Uiso 1 1 calc R A . C33 C 0.7608(2) 0.0746(6) 0.1553(5) 0.063(2) Uani 1 1 d . A . H33A H 0.7682 0.0186 0.1571 0.075 Uiso 1 1 calc R . . C34 C 0.7559(3) 0.1141(6) 0.0839(5) 0.068(3) Uani 1 1 d . . . H34A H 0.7599 0.0858 0.0375 0.082 Uiso 1 1 calc R A . C35 C 0.7450(2) 0.1962(6) 0.0838(4) 0.053(2) Uani 1 1 d . A . H35A H 0.7420 0.2239 0.0362 0.064 Uiso 1 1 calc R . . C41 C 0.81905(19) 0.2939(4) 0.2885(4) 0.0328(17) Uani 1 1 d . A . C42 C 0.84749(19) 0.2461(5) 0.2588(4) 0.0379(18) Uani 1 1 d . . . H42A H 0.8520 0.2477 0.2059 0.045 Uiso 1 1 calc R A . C43 C 0.8686(2) 0.1968(5) 0.3093(4) 0.0434(19) Uani 1 1 d . A . H43A H 0.8876 0.1655 0.2906 0.052 Uiso 1 1 calc R . . C44 C 0.8613(2) 0.1944(5) 0.3876(4) 0.0373(17) Uani 1 1 d . . . H44A H 0.8751 0.1613 0.4221 0.045 Uiso 1 1 calc R A . C45 C 0.83347(19) 0.2415(4) 0.4133(4) 0.0331(17) Uani 1 1 d . A . H45A H 0.8286 0.2394 0.4660 0.040 Uiso 1 1 calc R . . C61 C 0.80581(19) 0.3775(4) 0.1746(3) 0.0342(16) Uani 1 1 d . A . C62 C 0.8408(2) 0.4032(5) 0.1600(4) 0.0405(18) Uani 1 1 d . . . H62A H 0.8591 0.3941 0.1977 0.049 Uiso 1 1 calc R A . C63 C 0.8487(2) 0.4415(5) 0.0917(4) 0.052(2) Uani 1 1 d . A . H63A H 0.8723 0.4570 0.0823 0.063 Uiso 1 1 calc R . . C64 C 0.8214(2) 0.4568(6) 0.0366(4) 0.056(2) Uani 1 1 d . . . H64A H 0.8261 0.4822 -0.0107 0.067 Uiso 1 1 calc R A . C65 C 0.7865(3) 0.4330(5) 0.0539(4) 0.054(2) Uani 1 1 d . A . H65A H 0.7679 0.4449 0.0178 0.064 Uiso 1 1 calc R . . C71 C 0.79082(19) 0.5112(4) 0.3099(4) 0.0341(16) Uani 1 1 d . A . C72 C 0.8122(2) 0.5756(5) 0.2784(4) 0.047(2) Uani 1 1 d . . . H72A H 0.8042 0.6049 0.2339 0.056 Uiso 1 1 calc R A . C73 C 0.8449(2) 0.5941(5) 0.3148(4) 0.055(2) Uani 1 1 d . A . H73A H 0.8596 0.6352 0.2942 0.066 Uiso 1 1 calc R . . C74 C 0.8559(2) 0.5523(5) 0.3809(5) 0.051(2) Uani 1 1 d . . . H74A H 0.8775 0.5661 0.4075 0.061 Uiso 1 1 calc R A . C75 C 0.8341(2) 0.4888(5) 0.4072(4) 0.0387(18) Uani 1 1 d . A . H75A H 0.8421 0.4580 0.4507 0.046 Uiso 1 1 calc R . . C80 C 0.4443(2) 0.5808(5) 0.3842(4) 0.044(2) Uani 1 1 d . . . C81 C 0.4548(2) 0.6278(7) 0.4505(4) 0.057(2) Uani 1 1 d . . . H81A H 0.4706 0.6729 0.4463 0.068 Uiso 1 1 calc R . . C82 C 0.4416(2) 0.6066(6) 0.5229(4) 0.056(2) Uani 1 1 d . . . H82A H 0.4495 0.6359 0.5673 0.067 Uiso 1 1 calc R . . C83 C 0.4170(2) 0.5428(6) 0.5289(5) 0.060(3) Uani 1 1 d . . . H83A H 0.4074 0.5317 0.5770 0.072 Uiso 1 1 calc R . . C84 C 0.4060(3) 0.4947(6) 0.4652(5) 0.063(2) Uani 1 1 d . . . H84A H 0.3894 0.4515 0.4702 0.076 Uiso 1 1 calc R . . C85 C 0.4205(2) 0.5124(6) 0.3929(4) 0.054(2) Uani 1 1 d . . . H85A H 0.4143 0.4786 0.3501 0.064 Uiso 1 1 calc R . . C91 C 0.7374(2) 0.5347(5) 0.2283(4) 0.0388(18) Uani 1 1 d . A . C92 C 0.7319(2) 0.6194(6) 0.2461(4) 0.057(2) Uani 1 1 d . . . H92A H 0.7442 0.6437 0.2888 0.069 Uiso 1 1 calc R A . C93 C 0.7085(3) 0.6666(6) 0.2009(6) 0.084(3) Uani 1 1 d . A . H93A H 0.7057 0.7238 0.2109 0.101 Uiso 1 1 calc R . . C94 C 0.6888(3) 0.6282(7) 0.1396(6) 0.084(3) Uani 1 1 d . . . H94A H 0.6722 0.6589 0.1090 0.101 Uiso 1 1 calc R A . C95 C 0.6944(2) 0.5443(6) 0.1255(5) 0.060(2) Uani 1 1 d . A . H95A H 0.6811 0.5183 0.0849 0.072 Uiso 1 1 calc R . . C101 C 0.7010(2) 0.4453(5) 0.3782(4) 0.0392(18) Uani 1 1 d . A . C102 C 0.6733(2) 0.5047(6) 0.3863(5) 0.060(2) Uani 1 1 d . . . H10A H 0.6542 0.5075 0.3496 0.072 Uiso 1 1 calc R A . C103 C 0.6747(3) 0.5584(6) 0.4490(5) 0.073(3) Uani 1 1 d . A . H10B H 0.6567 0.5982 0.4551 0.088 Uiso 1 1 calc R . . C104 C 0.7033(3) 0.5527(6) 0.5028(5) 0.064(3) Uani 1 1 d . . . H10C H 0.7046 0.5882 0.5460 0.077 Uiso 1 1 calc R A . C105 C 0.7293(2) 0.4947(5) 0.4919(4) 0.050(2) Uani 1 1 d . A . H10D H 0.7485 0.4911 0.5284 0.060 Uiso 1 1 calc R . . C121 C 0.67271(18) 0.3593(5) 0.2757(4) 0.0368(16) Uani 1 1 d . A . C122 C 0.6409(2) 0.3413(6) 0.3110(5) 0.057(2) Uani 1 1 d . . . H12B H 0.6386 0.3546 0.3634 0.068 Uiso 1 1 calc R A . C123 C 0.6130(2) 0.3045(7) 0.2702(6) 0.073(3) Uani 1 1 d . A . H12C H 0.5915 0.2926 0.2940 0.087 Uiso 1 1 calc R . . C124 C 0.6174(3) 0.2847(7) 0.1911(6) 0.078(3) Uani 1 1 d . . . H12D H 0.5990 0.2584 0.1618 0.094 Uiso 1 1 calc R A . C125 C 0.6489(2) 0.3048(6) 0.1582(5) 0.059(2) Uani 1 1 d . A . H12E H 0.6516 0.2923 0.1058 0.071 Uiso 1 1 calc R . . C131 C 0.4271(2) 0.1802(4) 0.4841(4) 0.0334(17) Uani 1 1 d . B . C132 C 0.3970(2) 0.2214(5) 0.5141(5) 0.051(2) Uani 1 1 d . . . H13B H 0.3916 0.2148 0.5662 0.061 Uiso 1 1 calc R B . C133 C 0.3760(2) 0.2705(6) 0.4665(6) 0.063(2) Uani 1 1 d . B . H13C H 0.3560 0.2972 0.4860 0.075 Uiso 1 1 calc R . . C134 C 0.3839(2) 0.2813(5) 0.3902(5) 0.056(2) Uani 1 1 d . . . H13D H 0.3698 0.3160 0.3575 0.067 Uiso 1 1 calc R B . C135 C 0.4132(2) 0.2395(5) 0.3628(5) 0.047(2) Uani 1 1 d . B . H13E H 0.4188 0.2465 0.3109 0.057 Uiso 1 1 calc R . . C151 C 0.4418(2) 0.0939(4) 0.5962(4) 0.0370(18) Uani 1 1 d . B . C152 C 0.4072(2) 0.0604(5) 0.6060(5) 0.052(2) Uani 1 1 d . . . H15B H 0.3894 0.0649 0.5664 0.063 Uiso 1 1 calc R B . C153 C 0.4000(3) 0.0206(6) 0.6753(5) 0.070(3) Uani 1 1 d . B . H15C H 0.3772 -0.0007 0.6835 0.084 Uiso 1 1 calc R . . C154 C 0.4270(3) 0.0129(6) 0.7317(5) 0.074(3) Uani 1 1 d . . . H15D H 0.4226 -0.0132 0.7790 0.088 Uiso 1 1 calc R B . C155 C 0.4607(3) 0.0442(5) 0.7177(4) 0.057(2) Uani 1 1 d . B . H15E H 0.4791 0.0370 0.7555 0.068 Uiso 1 1 calc R . . C161 C 0.5256(2) -0.0285(5) 0.5452(4) 0.0367(17) Uani 1 1 d . B . C162 C 0.5393(2) -0.1075(5) 0.5265(5) 0.056(2) Uani 1 1 d . . . H16A H 0.5310 -0.1342 0.4809 0.067 Uiso 1 1 calc R B . C163 C 0.5645(2) -0.1459(5) 0.5738(5) 0.068(3) Uani 1 1 d . B . H16B H 0.5733 -0.1989 0.5612 0.082 Uiso 1 1 calc R . . C164 C 0.5769(2) -0.1058(5) 0.6404(5) 0.061(2) Uani 1 1 d . . . H16C H 0.5938 -0.1312 0.6744 0.073 Uiso 1 1 calc R B . C165 C 0.5638(2) -0.0281(5) 0.6554(4) 0.048(2) Uani 1 1 d . B . H16D H 0.5729 -0.0001 0.6996 0.058 Uiso 1 1 calc R . . C181 C 0.49219(18) 0.2965(4) 0.5677(4) 0.0312(16) Uani 1 1 d . B . C182 C 0.4775(2) 0.3776(5) 0.5700(4) 0.047(2) Uani 1 1 d . . . H18A H 0.4721 0.4062 0.5236 0.056 Uiso 1 1 calc R B . C183 C 0.4709(2) 0.4151(5) 0.6396(4) 0.053(2) Uani 1 1 d . B . H18B H 0.4621 0.4699 0.6410 0.064 Uiso 1 1 calc R . . C184 C 0.4774(2) 0.3706(6) 0.7078(4) 0.058(2) Uani 1 1 d . . . H18C H 0.4735 0.3951 0.7560 0.069 Uiso 1 1 calc R B . C185 C 0.4899(2) 0.2893(5) 0.7028(4) 0.0417(19) Uani 1 1 d . B . H18D H 0.4929 0.2580 0.7485 0.050 Uiso 1 1 calc R . . C211 C 0.5504(2) 0.5426(4) 0.1009(4) 0.0379(17) Uani 1 1 d . . . C212 C 0.5872(2) 0.5187(5) 0.1183(4) 0.047(2) Uani 1 1 d . . . H21B H 0.6004 0.4927 0.0803 0.056 Uiso 1 1 calc R . . C213 C 0.6026(2) 0.5339(6) 0.1897(5) 0.061(2) Uani 1 1 d . . . H21C H 0.6263 0.5175 0.2007 0.073 Uiso 1 1 calc R . . C214 C 0.5830(2) 0.5747(6) 0.2476(4) 0.055(2) Uani 1 1 d . . . H21D H 0.5932 0.5870 0.2967 0.066 Uiso 1 1 calc R . . C215 C 0.5480(2) 0.5951(5) 0.2268(4) 0.047(2) Uani 1 1 d . . . H21E H 0.5344 0.6214 0.2641 0.057 Uiso 1 1 calc R . . C231 C 0.5663(2) 0.7080(4) -0.0027(4) 0.0379(18) Uani 1 1 d . . . C232 C 0.5976(2) 0.7459(5) 0.0311(4) 0.046(2) Uani 1 1 d . . . H23B H 0.5964 0.7787 0.0759 0.055 Uiso 1 1 calc R . . C233 C 0.6305(2) 0.7335(6) -0.0038(5) 0.054(2) Uani 1 1 d . . . H23C H 0.6511 0.7597 0.0172 0.065 Uiso 1 1 calc R . . C234 C 0.6329(2) 0.6836(6) -0.0684(4) 0.056(2) Uani 1 1 d . . . H23D H 0.6550 0.6719 -0.0895 0.067 Uiso 1 1 calc R . . C235 C 0.6013(2) 0.6513(5) -0.1008(4) 0.046(2) Uani 1 1 d . . . H23E H 0.6027 0.6190 -0.1458 0.055 Uiso 1 1 calc R . . C241 C 0.5219(2) 0.7702(5) 0.0779(4) 0.0368(18) Uani 1 1 d . . . C242 C 0.5316(2) 0.8554(5) 0.0707(4) 0.050(2) Uani 1 1 d . . . H24B H 0.5492 0.8715 0.0368 0.060 Uiso 1 1 calc R . . C243 C 0.5147(3) 0.9140(5) 0.1145(5) 0.065(3) Uani 1 1 d . . . H24C H 0.5212 0.9704 0.1111 0.078 Uiso 1 1 calc R . . C244 C 0.4884(3) 0.8908(6) 0.1633(5) 0.078(3) Uani 1 1 d . . . H24D H 0.4766 0.9307 0.1926 0.094 Uiso 1 1 calc R . . C245 C 0.4800(3) 0.8070(6) 0.1678(4) 0.057(2) Uani 1 1 d . . . H24E H 0.4618 0.7909 0.2005 0.068 Uiso 1 1 calc R . . C261 C 0.5425(2) 0.4774(5) -0.0237(4) 0.0401(18) Uani 1 1 d . . . C262 C 0.5544(2) 0.3963(6) -0.0019(5) 0.060(2) Uani 1 1 d . . . H26A H 0.5579 0.3827 0.0507 0.072 Uiso 1 1 calc R . . C263 C 0.5609(3) 0.3375(6) -0.0577(6) 0.077(3) Uani 1 1 d . . . H26B H 0.5686 0.2836 -0.0435 0.093 Uiso 1 1 calc R . . C264 C 0.5558(3) 0.3587(7) -0.1351(6) 0.077(3) Uani 1 1 d . . . H26C H 0.5607 0.3200 -0.1740 0.092 Uiso 1 1 calc R . . C265 C 0.5436(2) 0.4372(6) -0.1537(5) 0.057(2) Uani 1 1 d . . . H26D H 0.5392 0.4500 -0.2061 0.068 Uiso 1 1 calc R . . C1 C 0.79305(16) 0.3659(5) 0.5255(3) 0.0321(15) Uani 1 1 d D . . C2 C 0.8053(2) 0.3671(5) 0.5911(4) 0.0475(19) Uani 1 1 d D . . C20 C 0.82036(19) 0.3687(6) 0.6708(4) 0.0431(18) Uani 1 1 d D . . C21 C 0.8048(3) 0.4193(6) 0.7277(4) 0.059(2) Uani 1 1 d D . . H21A H 0.7841 0.4498 0.7145 0.071 Uiso 1 1 calc R . . C22 C 0.8196(3) 0.4247(7) 0.8020(5) 0.073(3) Uani 1 1 d D . . H22A H 0.8092 0.4596 0.8382 0.087 Uiso 1 1 calc R . . C23 C 0.8501(3) 0.3784(6) 0.8235(4) 0.067(3) Uani 1 1 d D . . H23A H 0.8601 0.3818 0.8741 0.080 Uiso 1 1 calc R . . C24 C 0.8654(2) 0.3279(6) 0.7700(5) 0.069(3) Uani 1 1 d D . . H24A H 0.8860 0.2972 0.7837 0.082 Uiso 1 1 calc R . . C25 C 0.8500(2) 0.3223(6) 0.6939(5) 0.061(2) Uani 1 1 d D . . H25A H 0.8601 0.2861 0.6583 0.074 Uiso 1 1 calc R . . C3 C 0.7044(5) 0.3785(8) 0.0341(6) 0.024(3) Uiso 0.57 1 d PD A 1 C4 C 0.6923(5) 0.3777(14) -0.0329(7) 0.047(6) Uiso 0.57 1 d PD A 1 C40 C 0.6832(5) 0.3915(12) -0.1152(7) 0.052(5) Uiso 0.57 1 d PD A 1 C401 C 0.6544(6) 0.4486(14) -0.1349(10) 0.088(7) Uiso 0.57 1 d PD A 1 H40A H 0.6407 0.4716 -0.0960 0.106 Uiso 0.57 1 calc PR A 1 C402 C 0.6472(5) 0.4688(13) -0.2119(9) 0.075(6) Uiso 0.57 1 d PD A 1 H40B H 0.6276 0.5031 -0.2252 0.090 Uiso 0.57 1 calc PR A 1 C403 C 0.6688(5) 0.4390(12) -0.2707(9) 0.071(5) Uiso 0.57 1 d PD A 1 H40C H 0.6650 0.4595 -0.3212 0.085 Uiso 0.57 1 calc PR A 1 C404 C 0.6952(6) 0.3812(16) -0.2570(10) 0.103(8) Uiso 0.57 1 d PD A 1 H40D H 0.7081 0.3577 -0.2970 0.124 Uiso 0.57 1 calc PR A 1 C405 C 0.7022(7) 0.358(2) -0.1745(10) 0.129(11) Uiso 0.57 1 d PD A 1 H40E H 0.7203 0.3193 -0.1622 0.155 Uiso 0.57 1 calc PR A 1 C3' C 0.7056(10) 0.360(2) 0.0299(11) 0.058 Uiso 0.43 1 d PD A 2 C4' C 0.7008(7) 0.372(2) -0.0398(9) 0.052(8) Uiso 0.43 1 d PD A 2 C40' C 0.6931(6) 0.3823(16) -0.1221(8) 0.050(7) Uiso 0.43 1 d PD A 2 C41' C 0.6626(6) 0.4290(15) -0.1519(10) 0.055(6) Uiso 0.43 1 d PD A 2 H41A H 0.6456 0.4478 -0.1178 0.066 Uiso 0.43 1 calc PR A 2 C42' C 0.6582(7) 0.4466(19) -0.2305(11) 0.088(9) Uiso 0.43 1 d PD A 2 H42B H 0.6385 0.4780 -0.2492 0.106 Uiso 0.43 1 calc PR A 2 C43' C 0.6837(6) 0.4165(14) -0.2823(10) 0.061(6) Uiso 0.43 1 d PD A 2 H43B H 0.6836 0.4366 -0.3332 0.073 Uiso 0.43 1 calc PR A 2 C44' C 0.7086(5) 0.3578(13) -0.2577(8) 0.050 Uiso 0.43 1 d PD A 2 H44B H 0.7217 0.3277 -0.2933 0.060 Uiso 0.43 1 calc PR A 2 C45' C 0.7140(6) 0.3438(14) -0.1748(8) 0.050 Uiso 0.43 1 d PD A 2 H45B H 0.7322 0.3076 -0.1570 0.060 Uiso 0.43 1 calc PR A 2 C5 C 0.5414(3) 0.1316(9) 0.7495(6) 0.031(3) Uiso 0.69 1 d P B 1 C6 C 0.5598(3) 0.1276(8) 0.8080(5) 0.043(2) Uiso 0.69 1 d P B 1 C60 C 0.5824(3) 0.1248(9) 0.8845(6) 0.053(3) Uiso 0.69 1 d P B 1 C601 C 0.6159(3) 0.1693(8) 0.8853(7) 0.063(3) Uiso 0.69 1 d P B 1 H60A H 0.6233 0.1970 0.8409 0.075 Uiso 0.69 1 calc PR B 1 C602 C 0.6370(4) 0.1700(9) 0.9541(7) 0.075(4) Uiso 0.69 1 d P B 1 H60B H 0.6591 0.1977 0.9573 0.090 Uiso 0.69 1 calc PR B 1 C603 C 0.6231(4) 0.1252(10) 1.0216(7) 0.076(4) Uiso 0.69 1 d P B 1 H60C H 0.6364 0.1265 1.0688 0.091 Uiso 0.69 1 calc PR B 1 C604 C 0.5926(5) 0.0834(11) 1.0177(8) 0.077(4) Uiso 0.69 1 d P B 1 H60D H 0.5864 0.0555 1.0629 0.092 Uiso 0.69 1 calc PR B 1 C605 C 0.5667(5) 0.0754(11) 0.9493(8) 0.069(5) Uiso 0.69 1 d P B 1 H60E H 0.5451 0.0456 0.9473 0.083 Uiso 0.69 1 calc PR B 1 C5' C 0.5291(8) 0.130(2) 0.7577(16) 0.050 Uiso 0.31 1 d P B -2 C6' C 0.5352(8) 0.131(2) 0.8243(16) 0.067(8) Uiso 0.31 1 d P B -2 C60' C 0.5407(5) 0.1314(12) 0.9135(6) 0.053 Uiso 0.31 1 d PG B -2 C61' C 0.5725(4) 0.0985(13) 0.9464(9) 0.029(7) Uiso 0.31 1 d PG B -2 H61A H 0.5897 0.0762 0.9145 0.034 Uiso 0.31 1 calc PR B -2 C62' C 0.5786(4) 0.0990(15) 1.0269(9) 0.093(14) Uiso 0.31 1 d PG B -2 H62B H 0.5999 0.0770 1.0489 0.111 Uiso 0.31 1 calc PR B -2 C63' C 0.5528(5) 0.1323(13) 1.0746(6) 0.063 Uiso 0.31 1 d PG B -2 H63B H 0.5568 0.1326 1.1285 0.076 Uiso 0.31 1 calc PR B -2 C64' C 0.5209(4) 0.1652(11) 1.0417(8) 0.046 Uiso 0.31 1 d PG B -2 H64B H 0.5037 0.1875 1.0736 0.055 Uiso 0.31 1 calc PR B -2 C65' C 0.5149(4) 0.1647(12) 0.9612(8) 0.067 Uiso 0.31 1 d PG B -2 H65B H 0.4936 0.1867 0.9392 0.080 Uiso 0.31 1 calc PR B -2 C1S C 0.4619(5) 0.8099(11) 0.6728(8) 0.081(6) Uani 0.60 1 d P . . H1SA H 0.4565 0.7929 0.7248 0.097 Uiso 0.60 1 calc PR . . H1SB H 0.4398 0.8182 0.6427 0.097 Uiso 0.60 1 calc PR . . H1SC H 0.4753 0.8617 0.6748 0.097 Uiso 0.60 1 calc PR . . O1S O 0.4813(3) 0.7501(6) 0.6394(5) 0.054(2) Uani 0.60 1 d P . . H1SD H 0.5008 0.7454 0.6633 0.065 Uiso 0.60 1 calc PR . . 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 0.0326(5) 0.0296(5) 0.0299(4) 0.0013(4) 0.0005(3) 0.0027(5) Ni2 0.0292(4) 0.0226(4) 0.0323(4) 0.0020(4) -0.0013(3) 0.0003(4) Ni3 0.0421(5) 0.0408(6) 0.0360(5) 0.0048(5) -0.0094(4) -0.0025(5) Ni4 0.0467(6) 0.0280(5) 0.0291(4) 0.0005(4) -0.0078(4) 0.0001(5) Ni5 0.0323(7) 0.0211(7) 0.0300(6) 0.000 -0.0034(4) 0.000 Ni6 0.0418(7) 0.0217(6) 0.0237(5) 0.000 0.0016(4) 0.000 Ni7 0.0450(5) 0.0413(6) 0.0254(4) 0.0047(4) 0.0029(3) 0.0057(5) N1 0.031(3) 0.040(4) 0.031(3) 0.003(3) -0.001(2) 0.006(3) N2 0.033(4) 0.029(3) 0.041(3) 0.007(3) 0.002(3) -0.001(3) N3 0.043(4) 0.041(4) 0.043(4) -0.008(3) -0.005(3) -0.007(3) N4 0.033(3) 0.019(3) 0.028(3) -0.001(2) 0.001(2) 0.003(2) N5 0.034(3) 0.029(3) 0.028(3) -0.001(2) -0.003(2) 0.004(3) N6 0.042(4) 0.030(3) 0.028(3) 0.001(2) -0.002(2) 0.000(3) N7 0.034(4) 0.031(3) 0.033(3) -0.008(3) -0.002(2) -0.001(3) N8 0.039(4) 0.022(3) 0.034(3) 0.003(2) 0.004(2) 0.000(3) N9 0.038(4) 0.036(4) 0.049(4) 0.016(3) -0.001(3) 0.002(3) N10 0.037(4) 0.035(4) 0.034(3) 0.004(3) -0.001(3) 0.003(3) N11 0.028(3) 0.039(4) 0.038(3) 0.004(3) -0.002(2) 0.005(3) N12 0.034(4) 0.030(4) 0.058(4) 0.003(3) -0.011(3) -0.003(3) N13 0.031(3) 0.023(3) 0.044(3) 0.004(3) -0.013(3) -0.005(3) N14 0.039(3) 0.034(4) 0.032(3) -0.002(3) -0.002(2) -0.005(3) N15 0.048(4) 0.030(3) 0.034(3) 0.002(3) -0.001(3) 0.002(3) N16 0.042(4) 0.026(3) 0.044(3) 0.002(3) -0.008(3) -0.006(3) N17 0.042(5) 0.023(5) 0.028(4) 0.000 -0.001(4) 0.000 N18 0.042(4) 0.026(3) 0.034(3) -0.005(3) -0.006(3) 0.001(3) N19 0.031(5) 0.021(4) 0.031(4) 0.000 -0.013(3) 0.000 N21 0.034(4) 0.040(4) 0.032(3) 0.011(3) 0.005(2) 0.002(3) N22 0.032(4) 0.022(3) 0.042(3) -0.001(3) 0.004(3) 0.002(3) N23 0.049(4) 0.040(4) 0.028(3) 0.001(3) -0.002(3) -0.008(3) N24 0.061(4) 0.038(4) 0.026(3) -0.007(3) -0.009(3) 0.004(3) N25 0.041(4) 0.027(3) 0.023(3) 0.003(2) -0.002(2) -0.004(3) N26 0.044(4) 0.040(4) 0.039(3) -0.016(3) 0.010(3) -0.003(3) C7 0.049(5) 0.057(5) 0.035(4) 0.006(4) -0.002(3) 0.003(5) C8 0.046(5) 0.083(7) 0.038(4) 0.014(4) -0.005(3) 0.022(5) C11 0.029(4) 0.030(4) 0.047(4) 0.008(3) 0.005(3) 0.006(3) C12 0.038(4) 0.041(5) 0.054(4) 0.003(4) 0.004(3) -0.005(4) C13 0.045(5) 0.034(4) 0.075(5) 0.017(4) 0.000(4) -0.004(4) C14 0.042(5) 0.062(6) 0.052(5) 0.017(4) 0.010(4) -0.006(4) C15 0.047(5) 0.042(5) 0.043(4) 0.000(4) 0.009(4) -0.002(4) C31 0.032(4) 0.030(4) 0.046(4) 0.000(3) -0.008(3) -0.007(3) C32 0.059(5) 0.032(4) 0.046(4) -0.011(4) 0.004(3) 0.006(4) C33 0.071(7) 0.037(5) 0.081(7) -0.014(5) 0.007(5) 0.005(5) C34 0.088(7) 0.054(6) 0.065(5) -0.024(5) 0.012(5) -0.007(6) C35 0.068(6) 0.056(6) 0.035(4) -0.011(4) 0.003(4) -0.012(5) C41 0.040(4) 0.022(4) 0.035(4) -0.008(3) -0.007(3) -0.006(3) C42 0.040(5) 0.042(5) 0.032(4) -0.007(3) 0.007(3) 0.008(4) C43 0.034(4) 0.044(5) 0.052(5) -0.009(4) 0.004(3) 0.007(4) C44 0.040(5) 0.031(4) 0.040(4) 0.007(3) -0.006(3) 0.006(4) C45 0.040(5) 0.031(4) 0.028(4) 0.006(3) 0.000(3) -0.003(3) C61 0.050(5) 0.025(4) 0.027(3) -0.002(3) -0.002(3) 0.005(4) C62 0.039(5) 0.045(5) 0.038(4) -0.004(3) 0.001(3) -0.008(4) C63 0.051(5) 0.050(5) 0.057(5) 0.007(4) 0.016(4) -0.012(4) C64 0.072(7) 0.061(6) 0.035(4) 0.013(4) 0.009(4) -0.016(5) C65 0.076(7) 0.048(5) 0.036(4) 0.000(4) -0.010(4) -0.002(5) C71 0.037(4) 0.027(4) 0.038(4) -0.007(3) 0.002(3) -0.004(3) C72 0.060(5) 0.037(5) 0.043(4) 0.002(3) -0.003(4) -0.017(4) C73 0.057(6) 0.053(6) 0.056(5) -0.004(4) 0.016(4) -0.025(4) C74 0.041(5) 0.057(6) 0.055(5) -0.024(4) 0.008(4) -0.006(4) C75 0.041(5) 0.037(4) 0.038(4) -0.014(3) 0.006(3) 0.000(4) C80 0.038(5) 0.060(5) 0.035(4) 0.010(4) 0.006(3) 0.012(4) C81 0.046(5) 0.076(6) 0.048(4) 0.007(5) -0.005(3) 0.004(5) C82 0.066(6) 0.065(7) 0.035(4) -0.004(4) -0.007(4) -0.006(5) C83 0.066(6) 0.078(7) 0.038(5) 0.013(4) 0.006(4) 0.019(6) C84 0.076(7) 0.051(6) 0.064(6) 0.020(5) 0.011(5) -0.001(5) C85 0.054(6) 0.062(6) 0.044(5) -0.004(4) 0.002(4) 0.005(5) C91 0.040(5) 0.028(4) 0.049(4) 0.010(3) 0.001(3) -0.001(4) C92 0.066(6) 0.032(4) 0.072(5) 0.006(4) -0.007(4) 0.005(5) C93 0.093(8) 0.040(6) 0.118(9) 0.017(6) -0.006(7) 0.024(6) C94 0.072(7) 0.063(7) 0.116(8) 0.026(7) -0.026(6) 0.025(6) C95 0.057(6) 0.060(6) 0.063(5) 0.021(5) -0.009(4) 0.011(5) C101 0.043(5) 0.033(4) 0.043(4) 0.004(3) 0.010(3) 0.005(4) C102 0.047(5) 0.072(7) 0.060(5) -0.003(5) 0.003(4) 0.017(5) C103 0.068(7) 0.070(7) 0.082(7) -0.023(5) -0.002(5) 0.035(6) C104 0.073(7) 0.060(6) 0.058(5) -0.022(4) -0.005(5) 0.022(5) C105 0.049(5) 0.050(5) 0.050(5) -0.012(4) -0.002(4) 0.012(4) C121 0.032(4) 0.033(4) 0.045(4) 0.004(4) 0.000(3) 0.011(4) C122 0.038(5) 0.061(6) 0.070(5) 0.003(4) -0.008(4) -0.008(4) C123 0.035(5) 0.092(8) 0.092(7) 0.015(6) 0.004(5) -0.011(5) C124 0.048(6) 0.095(9) 0.091(8) -0.003(6) -0.019(5) -0.018(6) C125 0.044(5) 0.059(6) 0.073(6) -0.004(5) -0.014(4) -0.006(5) C131 0.042(5) 0.014(4) 0.043(4) -0.008(3) -0.003(3) -0.005(3) C132 0.048(5) 0.041(5) 0.062(5) -0.005(4) -0.006(4) 0.002(4) C133 0.051(6) 0.049(6) 0.088(7) -0.005(5) -0.007(5) 0.015(5) C134 0.057(6) 0.027(4) 0.082(6) 0.007(4) -0.020(5) 0.002(4) C135 0.049(5) 0.034(5) 0.058(5) 0.005(4) -0.019(4) -0.006(4) C151 0.050(5) 0.023(4) 0.038(4) -0.005(3) 0.004(3) -0.005(3) C152 0.051(5) 0.052(6) 0.054(5) -0.008(4) 0.007(4) -0.010(4) C153 0.074(7) 0.077(7) 0.062(6) 0.001(5) 0.023(5) -0.031(6) C154 0.104(9) 0.074(7) 0.045(5) 0.021(5) 0.013(5) -0.020(6) C155 0.078(7) 0.052(6) 0.041(5) 0.010(4) 0.000(4) -0.011(5) C161 0.040(5) 0.028(4) 0.042(4) 0.000(3) -0.005(3) 0.002(4) C162 0.058(6) 0.040(5) 0.068(5) -0.019(4) -0.015(4) 0.003(4) C163 0.079(7) 0.031(5) 0.091(6) -0.005(5) -0.032(5) 0.024(5) C164 0.059(6) 0.035(5) 0.086(6) 0.010(4) -0.026(5) 0.007(4) C165 0.052(5) 0.038(5) 0.052(5) 0.005(4) -0.023(4) 0.004(4) C181 0.028(4) 0.023(4) 0.042(4) -0.001(3) -0.005(3) -0.001(3) C182 0.060(5) 0.039(5) 0.042(4) 0.006(4) -0.001(3) 0.014(4) C183 0.077(7) 0.029(5) 0.054(5) -0.014(4) 0.003(4) 0.013(4) C184 0.061(5) 0.070(6) 0.041(4) -0.017(5) -0.001(3) 0.010(6) C185 0.049(5) 0.038(5) 0.037(4) -0.003(3) -0.007(3) 0.006(4) C211 0.053(5) 0.025(4) 0.036(4) 0.006(3) 0.009(3) -0.001(4) C212 0.050(5) 0.048(5) 0.043(4) 0.007(4) 0.012(4) 0.007(4) C213 0.042(5) 0.088(7) 0.052(5) 0.023(5) -0.003(4) 0.007(5) C214 0.048(5) 0.076(6) 0.041(4) 0.011(4) 0.001(4) -0.001(5) C215 0.055(5) 0.054(5) 0.033(4) 0.014(3) -0.001(3) 0.001(4) C231 0.061(5) 0.028(4) 0.023(3) 0.012(3) -0.008(3) -0.011(4) C232 0.062(6) 0.039(5) 0.035(4) 0.008(3) -0.014(4) -0.014(4) C233 0.046(5) 0.065(6) 0.050(5) 0.024(4) -0.017(4) -0.018(5) C234 0.049(5) 0.082(7) 0.035(4) 0.024(4) -0.001(4) -0.007(5) C235 0.039(4) 0.073(6) 0.027(3) 0.007(3) 0.007(3) -0.001(4) C241 0.056(5) 0.032(4) 0.022(3) -0.002(3) -0.008(3) -0.002(4) C242 0.075(6) 0.031(5) 0.044(4) -0.010(4) -0.010(4) -0.008(4) C243 0.104(9) 0.030(5) 0.058(6) -0.011(4) -0.016(5) -0.002(5) C244 0.112(9) 0.054(7) 0.068(6) -0.034(5) -0.006(6) 0.021(6) C245 0.068(6) 0.062(6) 0.041(5) -0.025(4) -0.008(4) 0.014(5) C261 0.045(5) 0.023(4) 0.052(5) -0.003(3) 0.006(3) -0.002(4) C262 0.065(6) 0.049(6) 0.067(5) -0.002(4) -0.001(4) 0.016(5) C263 0.088(8) 0.053(6) 0.089(7) -0.024(5) -0.011(6) 0.029(6) C264 0.077(7) 0.057(7) 0.096(7) -0.049(6) 0.000(5) 0.006(6) C265 0.051(6) 0.060(6) 0.058(5) -0.020(5) 0.002(4) 0.004(5) C1 0.032(4) 0.043(4) 0.020(3) -0.004(3) -0.011(2) 0.005(4) C2 0.050(5) 0.035(4) 0.057(5) -0.003(4) 0.005(4) 0.003(4) C20 0.044(4) 0.043(5) 0.042(4) 0.010(4) -0.011(3) 0.003(4) C21 0.074(7) 0.058(6) 0.044(5) -0.007(4) -0.010(4) 0.004(5) C22 0.098(8) 0.083(7) 0.037(5) -0.001(5) -0.006(5) 0.017(6) C23 0.090(7) 0.071(7) 0.038(4) -0.002(5) -0.014(4) 0.009(6) C24 0.062(6) 0.073(7) 0.069(6) 0.019(5) -0.013(5) 0.009(5) C25 0.062(6) 0.062(6) 0.059(5) 0.006(4) -0.013(4) 0.008(5) C1S 0.125(17) 0.077(13) 0.039(9) 0.002(8) -0.007(9) -0.001(12) O1S 0.058(7) 0.062(7) 0.041(5) -0.011(5) -0.005(4) 0.004(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 C1 1.995(5) . ? Ni1 N4 2.082(5) . ? Ni1 N10 2.099(6) . ? Ni1 N1 2.100(6) . ? Ni1 N7 2.112(6) . ? Ni1 Ni2 2.4774(10) . ? Ni2 N2 1.879(6) . ? Ni2 N8 1.888(6) . ? Ni2 N11 1.894(6) . ? Ni2 N5 1.901(6) . ? Ni2 Ni3 2.4735(11) . ? Ni3 C3 1.977(11) . ? Ni3 C3' 2.027(19) . ? Ni3 N6 2.096(6) . ? Ni3 N3 2.100(7) . ? Ni3 N12 2.101(7) . ? Ni3 N9 2.117(6) . ? Ni4 C5 2.003(10) . ? Ni4 C5' 2.03(3) . ? Ni4 N18 2.094(6) . ? Ni4 N16 2.100(6) . ? Ni4 N15 2.107(6) . ? Ni4 N13 2.113(6) 2_656 ? Ni4 Ni5 2.4861(7) . ? Ni5 N19 1.886(8) . ? Ni5 N14 1.896(6) 2_656 ? Ni5 N14 1.896(6) . ? Ni5 N17 1.899(8) . ? Ni5 Ni4 2.4861(7) 2_656 ? Ni6 N25 1.880(6) 2_655 ? Ni6 N25 1.880(6) . ? Ni6 N22 1.894(6) 2_655 ? Ni6 N22 1.894(6) . ? Ni6 Ni7 2.4467(8) 2_655 ? Ni6 Ni7 2.4468(8) . ? Ni7 C7 1.985(7) . ? Ni7 N26 2.099(6) 2_655 ? Ni7 N21 2.109(6) . ? Ni7 N24 2.112(6) . ? Ni7 N23 2.124(6) 2_655 ? N1 C11 1.342(9) . ? N1 C15 1.357(9) . ? N2 C31 1.382(9) . ? N2 C11 1.387(9) . ? N3 C31 1.350(9) . ? N3 C35 1.369(9) . ? N4 C45 1.351(8) . ? N4 C41 1.359(8) . ? N5 C61 1.357(8) . ? N5 C41 1.374(8) . ? N6 C65 1.357(9) . ? N6 C61 1.361(8) . ? N7 C71 1.327(8) . ? N7 C75 1.337(9) . ? N8 C71 1.375(8) . ? N8 C91 1.375(8) . ? N9 C91 1.348(9) . ? N9 C95 1.359(9) . ? N10 C105 1.327(9) . ? N10 C101 1.338(9) . ? N11 C121 1.381(8) . ? N11 C101 1.392(9) . ? N12 C125 1.356(9) . ? N12 C121 1.357(9) . ? N13 C131 1.339(8) . ? N13 C135 1.351(9) . ? N13 Ni4 2.113(6) 2_656 ? N14 C131 1.367(9) . ? N14 C151 1.378(8) . ? N15 C151 1.336(8) . ? N15 C155 1.338(9) . ? N16 C165 1.348(9) . ? N16 C161 1.352(8) . ? N17 C161 1.379(8) 2_656 ? N17 C161 1.380(8) . ? N18 C185 1.338(8) . ? N18 C181 1.354(8) . ? N19 C181 1.394(8) 2_656 ? N19 C181 1.394(8) . ? N21 C215 1.340(8) . ? N21 C211 1.342(9) . ? N22 C211 1.339(9) . ? N22 C261 1.372(9) . ? N23 C235 1.332(9) . ? N23 C231 1.389(9) . ? N23 Ni7 2.124(6) 2_655 ? N24 C241 1.340(9) . ? N24 C245 1.360(10) . ? N25 C231 1.361(9) . ? N25 C241 1.393(9) . ? N26 C265 1.352(9) . ? N26 C261 1.358(9) . ? N26 Ni7 2.100(6) 2_655 ? C7 C8 1.196(9) . ? C8 C80 1.433(10) . ? C11 C12 1.406(10) . ? C12 C13 1.382(9) . ? C13 C14 1.403(11) . ? C14 C15 1.358(11) . ? C31 C32 1.408(10) . ? C32 C33 1.364(10) . ? C33 C34 1.381(12) . ? C34 C35 1.365(13) . ? C41 C42 1.413(10) . ? C42 C43 1.386(10) . ? C43 C44 1.382(9) . ? C44 C45 1.364(10) . ? C61 C62 1.395(10) . ? C62 C63 1.363(10) . ? C63 C64 1.378(11) . ? C64 C65 1.392(11) . ? C71 C72 1.415(10) . ? C72 C73 1.376(10) . ? C73 C74 1.360(11) . ? C74 C75 1.381(11) . ? C80 C81 1.401(11) . ? C80 C85 1.414(11) . ? C81 C82 1.396(10) . ? C82 C83 1.370(12) . ? C83 C84 1.379(12) . ? C84 C85 1.400(11) . ? C91 C92 1.395(11) . ? C92 C93 1.363(11) . ? C93 C94 1.396(13) . ? C94 C95 1.371(14) . ? C101 C102 1.407(10) . ? C102 C103 1.370(11) . ? C103 C104 1.379(12) . ? C104 C105 1.353(11) . ? C121 C122 1.379(10) . ? C122 C123 1.359(11) . ? C123 C124 1.409(13) . ? C124 C125 1.360(13) . ? C131 C132 1.412(10) . ? C132 C133 1.351(11) . ? C133 C134 1.365(12) . ? C134 C135 1.374(11) . ? C151 C152 1.409(10) . ? C152 C153 1.381(11) . ? C153 C154 1.368(13) . ? C154 C155 1.379(13) . ? C161 C162 1.396(10) . ? C162 C163 1.358(10) . ? C163 C164 1.370(11) . ? C164 C165 1.354(11) . ? C181 C182 1.399(10) . ? C182 C183 1.365(10) . ? C183 C184 1.377(11) . ? C184 C185 1.375(11) . ? C211 C212 1.437(10) . ? C212 C213 1.351(10) . ? C213 C214 1.414(12) . ? C214 C215 1.374(11) . ? C231 C232 1.412(10) . ? C232 C233 1.396(11) . ? C233 C234 1.367(11) . ? C234 C235 1.374(10) . ? C241 C242 1.406(10) . ? C242 C243 1.365(12) . ? C243 C244 1.363(14) . ? C244 C245 1.370(13) . ? C261 C262 1.407(10) . ? C262 C263 1.366(11) . ? C263 C264 1.374(12) . ? C264 C265 1.359(13) . ? C1 C2 1.195(7) . ? C2 C20 1.456(8) . ? C20 C25 1.367(10) . ? C20 C21 1.406(10) . ? C21 C22 1.368(10) . ? C22 C23 1.387(12) . ? C23 C24 1.360(11) . ? C24 C25 1.405(10) . ? C3 C4 1.216(11) . ? C4 C40 1.455(12) . ? C40 C405 1.369(16) . ? C40 C401 1.432(16) . ? C401 C402 1.375(14) . ? C402 C403 1.398(18) . ? C403 C404 1.356(17) . ? C404 C405 1.473(15) . ? C3' C4' 1.217(14) . ? C4' C40' 1.437(13) . ? C40' C45' 1.362(17) . ? C40' C41' 1.429(16) . ? C41' C42' 1.380(16) . ? C42' C43' 1.410(19) . ? C43' C44' 1.365(18) . ? C44' C45' 1.444(14) . ? C5 C6 1.191(13) . ? C6 C60 1.529(14) . ? C60 C601 1.428(17) . ? C60 C605 1.50(2) . ? C601 C602 1.390(17) . ? C602 C603 1.471(18) . ? C603 C604 1.311(19) . ? C604 C605 1.491(19) . ? C5' C6' 1.15(4) . ? C6' C60' 1.54(3) . ? C60' C61' 1.3900 . ? C60' C65' 1.3900 . ? C61' C62' 1.3900 . ? C62' C63' 1.3900 . ? C63' C64' 1.3900 . ? C64' C65' 1.3900 . ? C1S O1S 1.337(18) . ? 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 C1 Ni1 N4 98.9(2) . . ? C1 Ni1 N10 97.8(2) . . ? N4 Ni1 N10 163.3(2) . . ? C1 Ni1 N1 99.7(3) . . ? N4 Ni1 N1 89.0(2) . . ? N10 Ni1 N1 89.8(2) . . ? C1 Ni1 N7 98.5(3) . . ? N4 Ni1 N7 86.0(2) . . ? N10 Ni1 N7 89.9(2) . . ? N1 Ni1 N7 161.7(2) . . ? C1 Ni1 Ni2 179.1(2) . . ? N4 Ni1 Ni2 81.33(14) . . ? N10 Ni1 Ni2 81.98(15) . . ? N1 Ni1 Ni2 81.18(14) . . ? N7 Ni1 Ni2 80.67(14) . . ? N2 Ni2 N8 179.3(3) . . ? N2 Ni2 N11 90.4(3) . . ? N8 Ni2 N11 90.2(3) . . ? N2 Ni2 N5 90.5(3) . . ? N8 Ni2 N5 89.0(2) . . ? N11 Ni2 N5 179.1(3) . . ? N2 Ni2 Ni3 90.01(17) . . ? N8 Ni2 Ni3 90.32(16) . . ? N11 Ni2 Ni3 89.81(16) . . ? N5 Ni2 Ni3 90.50(15) . . ? N2 Ni2 Ni1 90.04(17) . . ? N8 Ni2 Ni1 89.63(16) . . ? N11 Ni2 Ni1 89.41(16) . . ? N5 Ni2 Ni1 90.27(15) . . ? Ni3 Ni2 Ni1 179.23(5) . . ? C3 Ni3 C3' 8.8(11) . . ? C3 Ni3 N6 98.4(6) . . ? C3' Ni3 N6 98.2(10) . . ? C3 Ni3 N3 102.9(4) . . ? C3' Ni3 N3 94.1(9) . . ? N6 Ni3 N3 87.8(2) . . ? C3 Ni3 N12 99.1(6) . . ? C3' Ni3 N12 99.3(10) . . ? N6 Ni3 N12 162.5(2) . . ? N3 Ni3 N12 89.4(2) . . ? C3 Ni3 N9 94.7(4) . . ? C3' Ni3 N9 103.6(9) . . ? N6 Ni3 N9 87.8(2) . . ? N3 Ni3 N9 162.3(2) . . ? N12 Ni3 N9 89.6(2) . . ? C3 Ni3 Ni2 175.9(4) . . ? C3' Ni3 Ni2 175.1(9) . . ? N6 Ni3 Ni2 81.01(14) . . ? N3 Ni3 Ni2 81.15(16) . . ? N12 Ni3 Ni2 81.44(16) . . ? N9 Ni3 Ni2 81.22(15) . . ? C5 Ni4 C5' 13.7(9) . . ? C5 Ni4 N18 100.4(4) . . ? C5' Ni4 N18 95.8(11) . . ? C5 Ni4 N16 96.1(4) . . ? C5' Ni4 N16 100.7(11) . . ? N18 Ni4 N16 163.4(2) . . ? C5 Ni4 N15 103.6(3) . . ? C5' Ni4 N15 90.6(9) . . ? N18 Ni4 N15 88.0(2) . . ? N16 Ni4 N15 90.0(2) . . ? C5 Ni4 N13 94.9(3) . 2_656 ? C5' Ni4 N13 107.5(9) . 2_656 ? N18 Ni4 N13 85.4(2) . 2_656 ? N16 Ni4 N13 91.3(2) . 2_656 ? N15 Ni4 N13 161.2(2) . 2_656 ? C5 Ni4 Ni5 174.7(3) . . ? C5' Ni4 Ni5 171.5(9) . . ? N18 Ni4 Ni5 81.22(15) . . ? N16 Ni4 Ni5 82.17(15) . . ? N15 Ni4 Ni5 81.41(14) . . ? N13 Ni4 Ni5 80.22(14) 2_656 . ? N19 Ni5 N14 89.8(2) . 2_656 ? N19 Ni5 N14 89.8(2) . . ? N14 Ni5 N14 179.7(4) 2_656 . ? N19 Ni5 N17 180.000(1) . . ? N14 Ni5 N17 90.2(2) 2_656 . ? N14 Ni5 N17 90.2(2) . . ? N19 Ni5 Ni4 90.63(4) . 2_656 ? N14 Ni5 Ni4 90.11(14) 2_656 2_656 ? N14 Ni5 Ni4 89.89(14) . 2_656 ? N17 Ni5 Ni4 89.37(4) . 2_656 ? N19 Ni5 Ni4 90.64(4) . . ? N14 Ni5 Ni4 89.89(14) 2_656 . ? N14 Ni5 Ni4 90.11(14) . . ? N17 Ni5 Ni4 89.36(4) . . ? Ni4 Ni5 Ni4 178.73(7) 2_656 . ? N25 Ni6 N25 89.0(3) 2_655 . ? N25 Ni6 N22 90.2(2) 2_655 2_655 ? N25 Ni6 N22 179.2(3) . 2_655 ? N25 Ni6 N22 179.2(3) 2_655 . ? N25 Ni6 N22 90.2(2) . . ? N22 Ni6 N22 90.7(3) 2_655 . ? N25 Ni6 Ni7 89.83(17) 2_655 2_655 ? N25 Ni6 Ni7 90.94(17) . 2_655 ? N22 Ni6 Ni7 89.02(17) 2_655 2_655 ? N22 Ni6 Ni7 90.23(17) . 2_655 ? N25 Ni6 Ni7 90.94(17) 2_655 . ? N25 Ni6 Ni7 89.83(17) . . ? N22 Ni6 Ni7 90.22(17) 2_655 . ? N22 Ni6 Ni7 89.02(17) . . ? Ni7 Ni6 Ni7 178.92(7) 2_655 . ? C7 Ni7 N26 97.9(3) . 2_655 ? C7 Ni7 N21 97.4(3) . . ? N26 Ni7 N21 91.3(2) 2_655 . ? C7 Ni7 N24 100.1(3) . . ? N26 Ni7 N24 161.7(2) 2_655 . ? N21 Ni7 N24 89.7(2) . . ? C7 Ni7 N23 101.1(3) . 2_655 ? N26 Ni7 N23 87.0(2) 2_655 2_655 ? N21 Ni7 N23 161.5(2) . 2_655 ? N24 Ni7 N23 86.3(2) . 2_655 ? C7 Ni7 Ni6 178.3(2) . . ? N26 Ni7 Ni6 82.01(15) 2_655 . ? N21 Ni7 Ni6 80.92(14) . . ? N24 Ni7 Ni6 80.13(16) . . ? N23 Ni7 Ni6 80.58(16) 2_655 . ? C11 N1 C15 118.3(6) . . ? C11 N1 Ni1 122.4(5) . . ? C15 N1 Ni1 119.3(5) . . ? C31 N2 C11 121.0(6) . . ? C31 N2 Ni2 119.2(5) . . ? C11 N2 Ni2 119.7(5) . . ? C31 N3 C35 118.3(7) . . ? C31 N3 Ni3 122.2(5) . . ? C35 N3 Ni3 119.3(5) . . ? C45 N4 C41 119.2(6) . . ? C45 N4 Ni1 118.5(4) . . ? C41 N4 Ni1 122.3(4) . . ? C61 N5 C41 122.4(6) . . ? C61 N5 Ni2 118.6(4) . . ? C41 N5 Ni2 118.9(5) . . ? C65 N6 C61 118.4(7) . . ? C65 N6 Ni3 118.8(5) . . ? C61 N6 Ni3 122.7(4) . . ? C71 N7 C75 119.0(6) . . ? C71 N7 Ni1 121.7(4) . . ? C75 N7 Ni1 119.0(5) . . ? C71 N8 C91 122.3(6) . . ? C71 N8 Ni2 117.9(5) . . ? C91 N8 Ni2 119.8(5) . . ? C91 N9 C95 119.2(7) . . ? C91 N9 Ni3 122.0(5) . . ? C95 N9 Ni3 118.8(6) . . ? C105 N10 C101 120.3(6) . . ? C105 N10 Ni1 118.4(5) . . ? C101 N10 Ni1 121.2(5) . . ? C121 N11 C101 122.4(6) . . ? C121 N11 Ni2 119.9(5) . . ? C101 N11 Ni2 117.7(5) . . ? C125 N12 C121 118.5(7) . . ? C125 N12 Ni3 119.1(6) . . ? C121 N12 Ni3 122.4(4) . . ? C131 N13 C135 119.3(7) . . ? C131 N13 Ni4 122.1(5) . 2_656 ? C135 N13 Ni4 118.4(5) . 2_656 ? C131 N14 C151 122.3(6) . . ? C131 N14 Ni5 117.8(5) . . ? C151 N14 Ni5 119.8(5) . . ? C151 N15 C155 119.3(7) . . ? C151 N15 Ni4 122.6(5) . . ? C155 N15 Ni4 118.1(5) . . ? C165 N16 C161 118.0(6) . . ? C165 N16 Ni4 120.6(5) . . ? C161 N16 Ni4 121.5(4) . . ? C161 N17 C161 121.2(8) 2_656 . ? C161 N17 Ni5 119.4(4) 2_656 . ? C161 N17 Ni5 119.4(4) . . ? C185 N18 C181 119.4(6) . . ? C185 N18 Ni4 117.4(5) . . ? C181 N18 Ni4 123.1(4) . . ? C181 N19 C181 120.3(8) 2_656 . ? C181 N19 Ni5 119.8(4) 2_656 . ? C181 N19 Ni5 119.8(4) . . ? C215 N21 C211 119.8(6) . . ? C215 N21 Ni7 120.0(5) . . ? C211 N21 Ni7 120.1(5) . . ? C211 N22 C261 122.9(6) . . ? C211 N22 Ni6 118.5(5) . . ? C261 N22 Ni6 118.5(5) . . ? C235 N23 C231 119.3(6) . . ? C235 N23 Ni7 120.9(5) . 2_655 ? C231 N23 Ni7 119.7(5) . 2_655 ? C241 N24 C245 117.9(7) . . ? C241 N24 Ni7 122.3(5) . . ? C245 N24 Ni7 119.4(6) . . ? C231 N25 C241 122.0(6) . . ? C231 N25 Ni6 120.1(5) . . ? C241 N25 Ni6 117.6(5) . . ? C265 N26 C261 117.7(7) . . ? C265 N26 Ni7 122.1(6) . 2_655 ? C261 N26 Ni7 120.1(4) . 2_655 ? C8 C7 Ni7 168.1(8) . . ? C7 C8 C80 174.8(8) . . ? N1 C11 N2 115.5(6) . . ? N1 C11 C12 120.7(6) . . ? N2 C11 C12 123.6(6) . . ? C13 C12 C11 119.4(7) . . ? C12 C13 C14 120.0(8) . . ? C15 C14 C13 116.7(7) . . ? N1 C15 C14 124.9(7) . . ? N3 C31 N2 115.4(6) . . ? N3 C31 C32 120.7(7) . . ? N2 C31 C32 123.6(6) . . ? C33 C32 C31 118.8(7) . . ? C32 C33 C34 121.2(8) . . ? C35 C34 C33 117.5(8) . . ? C34 C35 N3 123.3(8) . . ? N4 C41 N5 116.4(6) . . ? N4 C41 C42 119.9(6) . . ? N5 C41 C42 123.7(6) . . ? C43 C42 C41 119.4(6) . . ? C44 C43 C42 119.5(7) . . ? C45 C44 C43 118.9(6) . . ? N4 C45 C44 123.1(6) . . ? N5 C61 N6 115.9(6) . . ? N5 C61 C62 124.1(6) . . ? N6 C61 C62 119.8(6) . . ? C63 C62 C61 121.5(7) . . ? C62 C63 C64 119.2(8) . . ? C63 C64 C65 118.1(7) . . ? N6 C65 C64 123.1(7) . . ? N7 C71 N8 116.7(6) . . ? N7 C71 C72 120.8(6) . . ? N8 C71 C72 122.2(6) . . ? C73 C72 C71 118.6(7) . . ? C74 C73 C72 120.2(7) . . ? C73 C74 C75 117.9(7) . . ? N7 C75 C74 123.4(7) . . ? C81 C80 C85 118.5(7) . . ? C81 C80 C8 122.5(8) . . ? C85 C80 C8 119.0(7) . . ? C82 C81 C80 119.8(9) . . ? C83 C82 C81 120.4(8) . . ? C82 C83 C84 121.6(8) . . ? C83 C84 C85 118.6(9) . . ? C84 C85 C80 120.9(8) . . ? N9 C91 N8 115.9(6) . . ? N9 C91 C92 120.6(7) . . ? N8 C91 C92 123.3(7) . . ? C93 C92 C91 120.0(8) . . ? C92 C93 C94 119.4(9) . . ? C95 C94 C93 118.5(8) . . ? N9 C95 C94 122.2(9) . . ? N10 C101 N11 116.8(6) . . ? N10 C101 C102 119.6(7) . . ? N11 C101 C102 123.4(7) . . ? C103 C102 C101 119.3(7) . . ? C102 C103 C104 119.1(8) . . ? C105 C104 C103 119.0(8) . . ? N10 C105 C104 122.6(7) . . ? N12 C121 C122 120.9(7) . . ? N12 C121 N11 114.9(6) . . ? C122 C121 N11 124.1(7) . . ? C123 C122 C121 120.8(9) . . ? C122 C123 C124 118.3(9) . . ? C125 C124 C123 118.9(8) . . ? N12 C125 C124 122.5(9) . . ? N13 C131 N14 116.5(6) . . ? N13 C131 C132 119.8(7) . . ? N14 C131 C132 123.6(7) . . ? C133 C132 C131 119.6(8) . . ? C132 C133 C134 120.6(9) . . ? C133 C134 C135 118.2(7) . . ? N13 C135 C134 122.4(8) . . ? N15 C151 N14 116.3(7) . . ? N15 C151 C152 120.8(7) . . ? N14 C151 C152 122.8(6) . . ? C153 C152 C151 119.0(8) . . ? C154 C153 C152 119.2(9) . . ? C153 C154 C155 119.2(8) . . ? N15 C155 C154 122.5(8) . . ? N16 C161 N17 116.4(6) . . ? N16 C161 C162 119.4(6) . . ? N17 C161 C162 124.1(6) . . ? C163 C162 C161 121.0(7) . . ? C162 C163 C164 119.2(8) . . ? C165 C164 C163 118.0(7) . . ? N16 C165 C164 124.3(7) . . ? N18 C181 N19 115.4(6) . . ? N18 C181 C182 119.3(6) . . ? N19 C181 C182 125.2(6) . . ? C183 C182 C181 120.6(7) . . ? C182 C183 C184 119.2(7) . . ? C185 C184 C183 118.4(7) . . ? N18 C185 C184 122.9(7) . . ? N22 C211 N21 116.7(7) . . ? N22 C211 C212 124.3(7) . . ? N21 C211 C212 118.7(6) . . ? C213 C212 C211 120.3(7) . . ? C212 C213 C214 120.4(8) . . ? C215 C214 C213 115.9(7) . . ? N21 C215 C214 124.9(8) . . ? N25 C231 N23 115.6(6) . . ? N25 C231 C232 125.6(7) . . ? N23 C231 C232 118.7(7) . . ? C233 C232 C231 118.9(8) . . ? C234 C233 C232 121.2(8) . . ? C233 C234 C235 117.4(8) . . ? N23 C235 C234 124.3(7) . . ? N24 C241 N25 114.1(6) . . ? N24 C241 C242 121.1(7) . . ? N25 C241 C242 124.2(7) . . ? C243 C242 C241 118.8(8) . . ? C244 C243 C242 120.8(9) . . ? C243 C244 C245 117.9(9) . . ? N24 C245 C244 123.4(10) . . ? N26 C261 N22 117.2(6) . . ? N26 C261 C262 120.2(7) . . ? N22 C261 C262 122.5(7) . . ? C263 C262 C261 120.1(8) . . ? C262 C263 C264 119.2(9) . . ? C265 C264 C263 118.8(8) . . ? N26 C265 C264 123.8(8) . . ? C2 C1 Ni1 179.0(7) . . ? C1 C2 C20 179.7(10) . . ? C25 C20 C21 117.1(6) . . ? C25 C20 C2 122.3(7) . . ? C21 C20 C2 120.6(7) . . ? C22 C21 C20 121.4(8) . . ? C21 C22 C23 120.4(9) . . ? C24 C23 C22 119.4(7) . . ? C23 C24 C25 119.9(8) . . ? C20 C25 C24 121.7(8) . . ? C4 C3 Ni3 174.6(15) . . ? C3 C4 C40 168(2) . . ? C405 C40 C401 118.3(13) . . ? C405 C40 C4 123.9(15) . . ? C401 C40 C4 117.6(14) . . ? C402 C401 C40 119.0(15) . . ? C401 C402 C403 121.4(15) . . ? C404 C403 C402 122.5(15) . . ? C403 C404 C405 115.5(16) . . ? C40 C405 C404 122.8(16) . . ? C4' C3' Ni3 162(3) . . ? C3' C4' C40' 176(3) . . ? C45' C40' C41' 117.4(13) . . ? C45' C40' C4' 120.3(16) . . ? C41' C40' C4' 122.2(16) . . ? C42' C41' C40' 121.0(17) . . ? C41' C42' C43' 119.4(18) . . ? C44' C43' C42' 120.1(16) . . ? C43' C44' C45' 118.3(15) . . ? C40' C45' C44' 121.6(15) . . ? C6 C5 Ni4 167.7(9) . . ? C5 C6 C60 178.0(14) . . ? C601 C60 C605 128.1(11) . . ? C601 C60 C6 116.2(10) . . ? C605 C60 C6 115.7(11) . . ? C602 C601 C60 118.2(12) . . ? C601 C602 C603 117.4(14) . . ? C604 C603 C602 122.4(13) . . ? C603 C604 C605 127.6(15) . . ? C604 C605 C60 106.2(15) . . ? C6' C5' Ni4 178(3) . . ? C5' C6' C60' 176(3) . . ? C61' C60' C65' 120.0 . . ? C61' C60' C6' 118.4(15) . . ? C65' C60' C6' 121.6(16) . . ? C60' C61' C62' 120.0 . . ? C63' C62' C61' 120.0 . . ? C64' C63' C62' 120.0 . . ? C63' C64' C65' 120.0 . . ? C64' C65' C60' 120.0 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.730 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.074 #===END of Compound 5.0.3Methanol================