# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name E.C.Constable C.E.Housecroft J.A.Zampese G.Zhang _publ_contact_author_name 'Catherine Housecroft' _publ_contact_author_email Catherine.Housecroft@unibas.ch data_gq265 _database_code_depnum_ccdc_archive 'CCDC 841380' #TrackingRef 'GQ265.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C38 H38 Cl2 N6 Ni), C60, 27(H2 O)' _chemical_formula_sum 'C174 H168 Cl6 N18 Ni3 O27' _chemical_formula_weight 3332.14 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' 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 Rhombohedral _symmetry_space_group_name_H-M R-3m _symmetry_space_group_name_Hall -R32" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 25.712(4) _cell_length_b 25.712(4) _cell_length_c 36.372(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20825(6) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6393 _cell_measurement_theta_min 4.18 _cell_measurement_theta_max 41.21 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5058 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8882 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; The C60 fullerene is disordered. The solvent was too disordered to identify. All electron density peaks that could be identified in the void were modelled as partial occupancy water molecules, even though close contacts make this model unrealistic. No other sensible solution was visible, as the solvent is obviously very disordered. Even after all the significant peaks in the difference map were assigned, a large void still remains, which is almost certainly also filled with disordered solvent. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 160201 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4403 _reflns_number_gt 4298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1998P)^2^+35.0127P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4403 _refine_ls_number_parameters 308 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.1143 _refine_ls_wR_factor_ref 0.3381 _refine_ls_wR_factor_gt 0.3369 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.264 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.1667 0.3333 0.3333 0.0629(5) Uani 1 4 d S . . Cl1 Cl 0.20316(4) 0.40633(7) 0.38398(4) 0.0670(5) Uani 1 2 d S . . N1 N 0.08256(19) 0.28296(17) 0.36021(9) 0.0658(10) Uani 1 1 d . . . C1A C 0.0559(4) 0.2236(4) 0.3583(2) 0.062(2) Uani 0.50 1 d P A 1 H1AA H 0.0752 0.2048 0.3465 0.075 Uiso 0.50 1 calc PR A 1 C2A C -0.0005(4) 0.1895(4) 0.3739(2) 0.0573(19) Uani 0.50 1 d P A 1 H2AA H -0.0209 0.1472 0.3709 0.069 Uiso 0.50 1 calc PR A 1 C1B C 0.0275(5) 0.2503(6) 0.3409(2) 0.090(3) Uani 0.50 1 d P A 2 H1BA H 0.0287 0.2526 0.3148 0.107 Uiso 0.50 1 calc PR A 2 C2B C -0.0286(5) 0.2146(6) 0.3577(3) 0.088(3) Uani 0.50 1 d P A 2 H2BA H -0.0641 0.1909 0.3438 0.105 Uiso 0.50 1 calc PR A 2 C3 C -0.0291(2) 0.21595(19) 0.39435(11) 0.0583(10) Uani 1 1 d . . . C4A C 0.0067(4) 0.2790(4) 0.3961(2) 0.062(2) Uani 0.50 1 d P A 1 H4AA H -0.0079 0.3009 0.4093 0.074 Uiso 0.50 1 calc PR A 1 C5A C 0.0633(4) 0.3108(4) 0.3789(2) 0.063(2) Uani 0.50 1 d P A 1 H5AA H 0.0867 0.3532 0.3815 0.076 Uiso 0.50 1 calc PR A 1 C4B C 0.0185(4) 0.2482(4) 0.4150(2) 0.062(2) Uani 0.50 1 d P A 2 H4BA H 0.0160 0.2486 0.4410 0.075 Uiso 0.50 1 calc PR A 2 C5B C 0.0733(4) 0.2820(4) 0.3962(2) 0.064(2) Uani 0.50 1 d P A 2 H5BA H 0.1074 0.3068 0.4109 0.076 Uiso 0.50 1 calc PR A 2 N2 N -0.12497(11) 0.12497(11) 0.39595(13) 0.0582(11) Uani 1 2 d S . . C6 C -0.08851(19) 0.17820(19) 0.41233(10) 0.0562(9) Uani 1 1 d . A . C7 C -0.1042(2) 0.1959(2) 0.44483(12) 0.0610(10) Uani 1 1 d . . . H7A H -0.0770 0.2336 0.4555 0.073 Uiso 1 1 calc R A . C8 C -0.15900(13) 0.15900(13) 0.46162(17) 0.0598(14) Uani 1 2 d S A . C9 C -0.17699(15) 0.17699(15) 0.4974(2) 0.0735(18) Uani 1 2 d S . . C10 C -0.1334(5) 0.2319(6) 0.5131(3) 0.084(3) Uani 0.50 1 d P A . H10A H -0.1493 0.2392 0.5358 0.125 Uiso 0.50 1 calc PR . . H10B H -0.1235 0.2647 0.4958 0.125 Uiso 0.50 1 calc PR . . H10C H -0.0971 0.2300 0.5187 0.125 Uiso 0.50 1 calc PR . . C11 C -0.1984(7) 0.1215(6) 0.5262(3) 0.091(3) Uani 0.50 1 d P A . H11A H -0.1653 0.1136 0.5305 0.137 Uiso 0.50 1 calc PR . . H11B H -0.2329 0.0855 0.5160 0.137 Uiso 0.50 1 calc PR . . H11C H -0.2099 0.1320 0.5496 0.137 Uiso 0.50 1 calc PR . . C12 C -0.2393(6) 0.1768(8) 0.4889(4) 0.120(5) Uani 0.50 1 d P A . H12A H -0.2547 0.1843 0.5117 0.180 Uiso 0.50 1 calc PR . . H12B H -0.2690 0.1376 0.4789 0.180 Uiso 0.50 1 calc PR . . H12C H -0.2316 0.2083 0.4710 0.180 Uiso 0.50 1 calc PR . . C101 C 0.0000 0.0000 0.5967(4) 0.095(5) Uani 0.90 6 d SP . . C102 C -0.1053(8) -0.0526(4) 0.5712(5) 0.169(7) Uani 1 2 d S . . C103 C -0.0535(4) 0.0535(4) 0.5712(5) 0.165(7) Uani 1 2 d S . . C104 C -0.1155(10) 0.0220(15) 0.5324(5) 0.221(11) Uani 0.95 1 d P . . C105 C -0.0685(4) 0.0685(4) 0.5485(5) 0.19(2) Uani 0.50 2 d SP . . C106 C -0.0538(8) 0.0021(9) 0.5877(3) 0.179(7) Uani 0.80 1 d PU . . C107 C -0.1370(5) -0.0336(14) 0.5368(9) 0.204(17) Uani 0.59 1 d P . . C108 C -0.1553(5) -0.0776(2) 0.5161(5) 0.238(16) Uani 1 2 d S . . C109 C -0.1022(11) 0.0520(13) 0.5068(9) 0.115(11) Uani 0.35 1 d P . . C110 C -0.1061(14) -0.1032(14) 0.5608(9) 0.100(8) Uani 0.26 1 d P . . C111 C -0.132(2) 0.0000 0.5000 0.142(17) Uiso 0.30 2 d SP . . O200 O -0.0518(5) 0.0518(5) 0.3162(6) 0.209(16) Uani 0.50 2 d SP B 1 O201 O 0.0227(11) 0.045(2) 0.3129(5) 0.31(3) Uani 0.50 2 d SP . 2 O202 O 0.0102(19) 0.0864(12) 0.3129(9) 0.169(13) Uani 0.25 1 d P . 3 O203 O 0.0085(9) 0.3861(9) 0.4772(7) 0.219(8) Uani 0.50 1 d P . 3 O204 O 0.015(3) 0.4190(17) 0.4309(15) 0.28(3) Uani 0.25 1 d P C 2 O205 O -0.0402(19) 0.209(3) 0.254(3) 0.40(5) Uani 0.25 1 d P D 1 O206 O -0.0886(13) 0.384(2) 0.4350(13) 0.25(2) Uani 0.25 1 d P E 1 O207 O -0.089(2) 0.218(3) 0.2945(11) 0.32(4) Uani 0.25 1 d P F 1 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 0.0761(6) 0.0694(7) 0.0409(6) 0.0193(4) 0.0097(2) 0.0347(4) Cl1 0.0828(8) 0.0689(9) 0.0448(8) 0.0150(6) 0.0075(3) 0.0344(5) N1 0.079(2) 0.070(2) 0.0449(18) 0.0162(15) 0.0080(17) 0.0347(19) C1A 0.079(5) 0.066(5) 0.048(4) 0.014(3) 0.013(4) 0.040(4) C2A 0.078(5) 0.059(4) 0.042(4) 0.017(3) 0.017(3) 0.040(4) C1B 0.067(5) 0.141(10) 0.038(4) 0.014(5) -0.002(4) 0.034(6) C2B 0.062(5) 0.133(9) 0.050(5) 0.002(5) 0.002(4) 0.036(6) C3 0.069(2) 0.065(2) 0.045(2) 0.0095(17) 0.0019(17) 0.036(2) C4A 0.062(5) 0.064(5) 0.063(5) 0.005(4) 0.012(4) 0.033(4) C5A 0.082(6) 0.050(4) 0.056(4) 0.013(4) 0.018(4) 0.032(4) C4B 0.077(5) 0.062(5) 0.042(4) 0.006(3) 0.010(4) 0.031(4) C5B 0.077(6) 0.067(5) 0.039(4) 0.010(4) 0.005(4) 0.030(4) N2 0.068(2) 0.068(2) 0.043(2) 0.0024(10) -0.0024(10) 0.037(2) C6 0.069(2) 0.066(2) 0.0441(19) 0.0064(17) 0.0007(17) 0.041(2) C7 0.072(3) 0.068(2) 0.048(2) -0.0020(18) -0.0002(19) 0.039(2) C8 0.069(3) 0.069(3) 0.053(3) -0.0019(12) 0.0019(12) 0.043(3) C9 0.088(4) 0.088(4) 0.063(4) -0.0084(15) 0.0084(15) 0.058(4) C10 0.091(7) 0.092(8) 0.067(6) -0.015(6) 0.003(5) 0.045(6) C11 0.115(9) 0.097(8) 0.061(6) -0.004(5) 0.031(6) 0.052(7) C12 0.107(9) 0.175(14) 0.118(10) -0.050(10) -0.012(8) 0.102(10) C101 0.118(8) 0.118(8) 0.048(7) 0.000 0.000 0.059(4) C102 0.111(12) 0.24(2) 0.118(12) 0.043(6) 0.085(11) 0.056(6) C103 0.234(19) 0.234(19) 0.102(11) -0.038(5) 0.038(5) 0.18(2) C104 0.208(17) 0.47(4) 0.132(13) -0.10(2) -0.028(13) 0.28(2) C105 0.38(5) 0.38(5) 0.027(8) -0.003(3) 0.003(3) 0.36(5) C106 0.198(13) 0.230(15) 0.098(7) -0.009(8) 0.077(8) 0.099(12) C107 0.037(5) 0.26(3) 0.25(3) -0.16(3) 0.024(9) 0.027(9) C108 0.042(5) 0.44(4) 0.097(10) 0.002(3) 0.004(6) 0.021(3) C109 0.15(2) 0.21(3) 0.091(14) 0.056(16) 0.051(14) 0.16(2) C110 0.10(2) 0.070(15) 0.085(16) 0.044(15) 0.042(15) 0.009(13) O200 0.34(4) 0.34(4) 0.102(12) 0.005(5) -0.005(5) 0.29(4) O201 0.37(4) 0.58(10) 0.053(8) -0.023(19) -0.011(9) 0.29(5) O202 0.27(4) 0.106(15) 0.16(2) 0.044(15) -0.03(2) 0.12(2) O203 0.173(14) 0.194(16) 0.25(2) 0.032(15) 0.026(15) 0.061(13) O204 0.39(8) 0.13(3) 0.28(5) 0.05(3) 0.16(5) 0.11(4) O205 0.13(3) 0.21(4) 0.69(15) -0.23(7) -0.02(5) -0.03(3) O206 0.124(19) 0.31(4) 0.33(5) 0.21(4) 0.09(3) 0.11(3) O207 0.16(3) 0.45(8) 0.14(3) 0.00(4) 0.02(2) -0.02(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.123(4) 17 ? Ni1 N1 2.123(4) 23 ? Ni1 N1 2.123(4) . ? Ni1 N1 2.124(4) 31 ? Ni1 Cl1 2.4567(16) . ? Ni1 Cl1 2.4568(16) 31 ? N1 C5A 1.256(9) . ? N1 C1A 1.325(9) . ? N1 C5B 1.328(9) . ? N1 C1B 1.419(11) . ? C1A C2A 1.386(12) . ? C1A H1AA 0.9500 . ? C2A C3 1.434(9) . ? C2A H2AA 0.9500 . ? C1B C2B 1.406(14) . ? C1B H1BA 0.9500 . ? C2B C3 1.333(10) . ? C2B H2BA 0.9500 . ? C3 C4B 1.316(10) . ? C3 C4A 1.410(10) . ? C3 C6 1.490(6) . ? C4A C5A 1.408(12) . ? C4A H4AA 0.9500 . ? C5A H5AA 0.9500 . ? C4B C5B 1.409(13) . ? C4B H4BA 0.9500 . ? C5B H5BA 0.9500 . ? N2 C6 1.351(5) 22 ? N2 C6 1.351(5) . ? C6 C7 1.397(6) . ? C7 C8 1.387(6) . ? C7 H7A 0.9500 . ? C8 C7 1.387(6) 22 ? C8 C9 1.527(9) . ? C9 C10 1.413(12) . ? C9 C10 1.413(12) 22 ? C9 C12 1.628(14) . ? C9 C12 1.628(14) 22 ? C9 C11 1.629(14) 22 ? C9 C11 1.629(14) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C101 C106 1.448(18) 24 ? C101 C106 1.448(18) 2 ? C101 C106 1.448(18) . ? C101 C106 1.448(18) 23 ? C101 C106 1.448(18) 22 ? C101 C106 1.448(19) 3 ? C102 C110 1.35(4) 24 ? C102 C110 1.35(4) . ? C102 C106 1.49(2) . ? C102 C106 1.49(2) 24 ? C102 C107 1.69(4) . ? C102 C107 1.69(4) 24 ? C103 C105 1.06(3) . ? C103 C106 1.45(2) 22 ? C103 C106 1.45(2) . ? C103 C110 1.45(4) 24 ? C103 C110 1.45(4) 3 ? C103 C104 1.98(2) . ? C103 C104 1.98(2) 22 ? C104 C109 1.15(3) . ? C104 C107 1.26(4) . ? C104 C111 1.281(17) . ? C104 C110 1.30(4) 24 ? C104 C105 1.34(3) . ? C105 C104 1.34(3) 22 ? C105 C110 1.65(4) 24 ? C105 C110 1.65(4) 3 ? C105 C109 1.69(3) . ? C105 C109 1.69(3) 22 ? C106 C106 1.33(4) 22 ? C106 C106 1.49(4) 24 ? C106 C110 1.62(4) 24 ? C107 C110 1.18(4) 24 ? C107 C108 1.24(2) . ? C107 C111 1.56(5) . ? C107 C109 1.65(4) 5_556 ? C107 C107 1.80(7) 24 ? C108 C109 1.054(19) 5_556 ? C108 C109 1.054(19) 21_556 ? C108 C107 1.24(2) 24 ? C108 C111 1.865(14) . ? C108 C111 1.865(14) 21_556 ? C109 C108 1.054(19) 20_556 ? C109 C111 1.19(3) . ? C109 C109 1.29(6) 22 ? C109 C107 1.65(4) 5_556 ? C110 C107 1.18(4) 24 ? C110 C104 1.30(4) 24 ? C110 C103 1.45(4) 2 ? C110 C106 1.62(4) 24 ? C110 C105 1.65(4) 2 ? C111 C109 1.19(3) 5_556 ? C111 C104 1.281(17) 5_556 ? C111 C107 1.56(5) 5_556 ? C111 C108 1.865(14) 20_556 ? O201 O201 1.75(9) 2 ? O201 O201 1.75(8) 3 ? O202 O202 1.70(8) 23 ? O203 O203 1.70(5) 6_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 179.996(1) 17 23 ? N1 Ni1 N1 89.0(2) 17 . ? N1 Ni1 N1 91.0(2) 23 . ? N1 Ni1 N1 91.0(2) 17 31 ? N1 Ni1 N1 89.0(2) 23 31 ? N1 Ni1 N1 179.997(1) . 31 ? N1 Ni1 Cl1 89.76(11) 17 . ? N1 Ni1 Cl1 90.24(11) 23 . ? N1 Ni1 Cl1 90.24(11) . . ? N1 Ni1 Cl1 89.76(11) 31 . ? N1 Ni1 Cl1 90.24(11) 17 31 ? N1 Ni1 Cl1 89.75(11) 23 31 ? N1 Ni1 Cl1 89.76(11) . 31 ? N1 Ni1 Cl1 90.24(11) 31 31 ? Cl1 Ni1 Cl1 180.0 . 31 ? C5A N1 C1A 124.1(6) . . ? C5A N1 C5B 50.1(6) . . ? C1A N1 C5B 92.6(6) . . ? C5A N1 C1B 92.6(8) . . ? C1A N1 C1B 60.2(7) . . ? C5B N1 C1B 111.1(6) . . ? C5A N1 Ni1 118.3(5) . . ? C1A N1 Ni1 117.5(4) . . ? C5B N1 Ni1 125.7(5) . . ? C1B N1 Ni1 122.9(4) . . ? N1 C1A C2A 118.9(7) . . ? N1 C1A H1AA 120.6 . . ? C2A C1A H1AA 120.6 . . ? C1A C2A C3 122.3(7) . . ? C1A C2A H2AA 118.9 . . ? C3 C2A H2AA 118.9 . . ? C2B C1B N1 124.5(8) . . ? C2B C1B H1BA 117.8 . . ? N1 C1B H1BA 117.8 . . ? C3 C2B C1B 115.9(9) . . ? C3 C2B H2BA 122.0 . . ? C1B C2B H2BA 122.0 . . ? C4B C3 C2B 124.7(7) . . ? C4B C3 C4A 52.0(5) . . ? C2B C3 C4A 93.8(7) . . ? C4B C3 C2A 93.4(6) . . ? C2B C3 C2A 57.0(7) . . ? C4A C3 C2A 111.9(6) . . ? C4B C3 C6 119.1(5) . . ? C2B C3 C6 116.2(6) . . ? C4A C3 C6 126.6(5) . . ? C2A C3 C6 121.4(5) . . ? C5A C4A C3 122.6(7) . . ? C5A C4A H4AA 118.7 . . ? C3 C4A H4AA 118.7 . . ? N1 C5A C4A 119.7(7) . . ? N1 C5A H5AA 120.1 . . ? C4A C5A H5AA 120.1 . . ? C3 C4B C5B 116.1(7) . . ? C3 C4B H4BA 121.9 . . ? C5B C4B H4BA 121.9 . . ? N1 C5B C4B 127.1(8) . . ? N1 C5B H5BA 116.4 . . ? C4B C5B H5BA 116.4 . . ? C6 N2 C6 117.3(5) 22 . ? N2 C6 C7 122.5(4) . . ? N2 C6 C3 115.6(4) . . ? C7 C6 C3 121.9(4) . . ? C8 C7 C6 120.6(4) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C7 116.6(5) 22 . ? C7 C8 C9 121.7(3) 22 . ? C7 C8 C9 121.7(3) . . ? C10 C9 C10 127.4(10) . 22 ? C10 C9 C8 116.0(5) . . ? C10 C9 C8 116.0(5) 22 . ? C10 C9 C12 111.6(9) . . ? C10 C9 C12 58.9(9) 22 . ? C8 C9 C12 106.5(7) . . ? C10 C9 C12 58.9(9) . 22 ? C10 C9 C12 111.6(9) 22 22 ? C8 C9 C12 106.5(7) . 22 ? C12 C9 C12 59.1(13) . 22 ? C10 C9 C11 111.5(9) 22 22 ? C8 C9 C11 107.7(5) . 22 ? C12 C9 C11 144.8(8) . 22 ? C12 C9 C11 102.6(9) 22 22 ? C10 C9 C11 111.5(9) . . ? C8 C9 C11 107.7(5) . . ? C12 C9 C11 102.6(9) . . ? C12 C9 C11 144.8(8) 22 . ? C11 C9 C11 74.7(12) 22 . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C106 C101 C106 54.7(16) 24 2 ? C106 C101 C106 61.9(16) 24 . ? C106 C101 C106 115.0(5) 2 . ? C106 C101 C106 115.0(5) 24 23 ? C106 C101 C106 61.9(16) 2 23 ? C106 C101 C106 153.4(14) . 23 ? C106 C101 C106 115.0(5) 24 22 ? C106 C101 C106 153.4(14) 2 22 ? C106 C101 C106 54.7(16) . 22 ? C106 C101 C106 115.0(5) 23 22 ? C106 C101 C106 153.4(14) 24 3 ? C106 C101 C106 115.0(5) 2 3 ? C106 C101 C106 115.0(5) . 3 ? C106 C101 C106 54.7(16) 23 3 ? C106 C101 C106 61.9(16) 22 3 ? C110 C102 C110 147(3) 24 . ? C110 C102 C106 69.2(18) 24 . ? C110 C102 C106 127(2) . . ? C110 C102 C106 127(2) 24 24 ? C110 C102 C106 69.2(18) . 24 ? C106 C102 C106 59.8(18) . 24 ? C110 C102 C107 107(3) . . ? C106 C102 C107 110.6(12) . . ? C106 C102 C107 151.7(9) 24 . ? C110 C102 C107 107(3) 24 24 ? C106 C102 C107 151.7(9) . 24 ? C106 C102 C107 110.6(12) 24 24 ? C107 C102 C107 64.0(19) . 24 ? C105 C103 C106 144.6(11) . 22 ? C105 C103 C106 144.6(11) . . ? C106 C103 C106 54.7(17) 22 . ? C105 C103 C110 80.3(19) . 24 ? C106 C103 C110 120(2) 22 24 ? C106 C103 C110 67.7(17) . 24 ? C105 C103 C110 80.3(19) . 3 ? C106 C103 C110 67.7(17) 22 3 ? C106 C103 C110 120(2) . 3 ? C110 C103 C110 149(3) 24 3 ? C106 C103 C104 147.6(9) 22 . ? C106 C103 C104 106.6(12) . . ? C110 C103 C104 115(2) 3 . ? C106 C103 C104 106.6(12) 22 22 ? C106 C103 C104 147.6(9) . 22 ? C110 C103 C104 115(2) 24 22 ? C104 C103 C104 75(2) . 22 ? C109 C104 C107 133(3) . . ? C109 C104 C111 58.3(18) . . ? C107 C104 C111 76(2) . . ? C109 C104 C110 155(3) . 24 ? C107 C104 C110 55(3) . 24 ? C111 C104 C110 128(3) . 24 ? C109 C104 C105 85(3) . . ? C107 C104 C105 130(2) . . ? C111 C104 C105 138(3) . . ? C110 C104 C105 78(2) 24 . ? C109 C104 C103 113(3) . . ? C107 C104 C103 100(2) . . ? C111 C104 C103 149(3) . . ? C110 C104 C103 47(2) 24 . ? C103 C105 C104 110.2(14) . . ? C103 C105 C104 110.2(14) . 22 ? C104 C105 C104 128(2) . 22 ? C103 C105 C110 60.2(15) . 24 ? C104 C105 C110 50.2(17) . 24 ? C104 C105 C110 152.1(14) 22 24 ? C103 C105 C110 60.2(15) . 3 ? C104 C105 C110 152.1(14) . 3 ? C104 C105 C110 50.2(17) 22 3 ? C110 C105 C110 116(3) 24 3 ? C103 C105 C109 147.0(13) . . ? C104 C105 C109 87.0(16) 22 . ? C110 C105 C109 91.3(16) 24 . ? C110 C105 C109 132.0(16) 3 . ? C103 C105 C109 147.0(13) . 22 ? C104 C105 C109 87.0(16) . 22 ? C110 C105 C109 132.0(16) 24 22 ? C110 C105 C109 91.3(16) 3 22 ? C106 C106 C103 62.7(8) 22 . ? C106 C106 C101 62.7(8) 22 . ? C103 C106 C101 124.0(14) . . ? C106 C106 C106 120.000(7) 22 24 ? C103 C106 C106 155.7(7) . 24 ? C101 C106 C106 59.1(8) . 24 ? C106 C106 C102 156.2(6) 22 . ? C103 C106 C102 107.0(11) . . ? C101 C106 C102 118.1(14) . . ? C106 C106 C102 60.1(9) 24 . ? C106 C106 C110 117.1(19) 22 24 ? C103 C106 C110 56.3(17) . 24 ? C101 C106 C110 155.2(12) . 24 ? C106 C106 C110 109.8(18) 24 24 ? C102 C106 C110 51.1(16) . 24 ? C110 C107 C108 152(4) 24 . ? C110 C107 C104 64(2) 24 . ? C108 C107 C104 135(4) . . ? C110 C107 C111 115(4) 24 . ? C108 C107 C111 82.6(19) . . ? C104 C107 C111 53(2) . . ? C110 C107 C109 154(3) 24 5_556 ? C104 C107 C109 96(3) . 5_556 ? C110 C107 C102 52(3) 24 . ? C108 C107 C102 102(3) . . ? C104 C107 C102 115.0(17) . . ? C111 C107 C102 151(2) . . ? C109 C107 C102 136.4(19) 5_556 . ? C110 C107 C107 109(3) 24 24 ? C104 C107 C107 156.4(10) . 24 ? C111 C107 C107 120.5(14) . 24 ? C109 C107 C107 81.2(15) 5_556 24 ? C102 C107 C107 58.0(10) . 24 ? C109 C108 C109 75(4) 5_556 21_556 ? C109 C108 C107 92(3) 5_556 . ? C109 C108 C107 156.3(18) 21_556 . ? C109 C108 C107 156.3(18) 5_556 24 ? C109 C108 C107 92(3) 21_556 24 ? C107 C108 C107 93(4) . 24 ? C109 C108 C111 107.5(16) 21_556 . ? C107 C108 C111 56(2) . . ? C107 C108 C111 139(2) 24 . ? C109 C108 C111 107.5(16) 5_556 21_556 ? C107 C108 C111 139(2) . 21_556 ? C107 C108 C111 56(2) 24 21_556 ? C111 C108 C111 130(3) . 21_556 ? C108 C109 C104 161.2(18) 20_556 . ? C108 C109 C111 113(3) 20_556 . ? C104 C109 C111 66.6(19) . . ? C108 C109 C109 52.3(18) 20_556 22 ? C104 C109 C109 119(2) . 22 ? C111 C109 C109 152(3) . 22 ? C108 C109 C107 48.7(19) 20_556 5_556 ? C104 C109 C107 129(3) . 5_556 ? C111 C109 C107 64.2(18) . 5_556 ? C109 C109 C107 98.8(16) 22 5_556 ? C108 C109 C105 119(2) 20_556 . ? C104 C109 C105 52(2) . . ? C111 C109 C105 115.3(18) . . ? C109 C109 C105 67.6(9) 22 . ? C107 C109 C105 150.1(13) 5_556 . ? C107 C110 C104 61(3) 24 24 ? C107 C110 C102 84(4) 24 . ? C104 C110 C102 142(3) 24 . ? C107 C110 C103 147(4) 24 2 ? C104 C110 C103 92(3) 24 2 ? C102 C110 C103 115(3) . 2 ? C107 C110 C106 139(4) 24 24 ? C104 C110 C106 143(3) 24 24 ? C102 C110 C106 59.7(19) . 24 ? C103 C110 C106 56.0(16) 2 24 ? C107 C110 C105 112(4) 24 2 ? C104 C110 C105 52(2) 24 2 ? C102 C110 C105 149(2) . 2 ? C106 C110 C105 94(2) 24 2 ? C109 C111 C109 172(6) 5_556 . ? C109 C111 C104 123.9(17) 5_556 . ? C109 C111 C104 55.1(14) . . ? C109 C111 C104 55.1(14) 5_556 5_556 ? C109 C111 C104 123.9(17) . 5_556 ? C104 C111 C104 168(5) . 5_556 ? C109 C111 C107 72.5(13) 5_556 . ? C109 C111 C107 105.9(17) . . ? C104 C111 C107 51.4(13) . . ? C104 C111 C107 125.9(18) 5_556 . ? C109 C111 C107 105.9(17) 5_556 5_556 ? C109 C111 C107 72.5(13) . 5_556 ? C104 C111 C107 125.9(18) . 5_556 ? C104 C111 C107 51.4(13) 5_556 5_556 ? C107 C111 C107 159(5) . 5_556 ? C109 C111 C108 145(3) . . ? C104 C111 C108 92.6(16) . . ? C104 C111 C108 85.0(15) 5_556 . ? C107 C111 C108 132(2) 5_556 . ? C109 C111 C108 145(3) 5_556 20_556 ? C104 C111 C108 85.0(16) . 20_556 ? C104 C111 C108 92.6(16) 5_556 20_556 ? C107 C111 C108 132(2) . 20_556 ? C108 C111 C108 156(4) . 20_556 ? O201 O201 O201 60.000(6) 2 3 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.619 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.137 # start Validation Reply Form _vrf_PLAT234_I ; PROBLEM: Large Hirshfeld Difference C103 -- C105 .. 0.37 Ang. RESPONSE: Relates to disordered C60 fullerene ; _vrf_PLAT430_I ; PROBLEM: Short Inter D...A Contact O200 .. O201 .. 2.00 Ang. RESPONSE: Electron density peaks resulting from heavily disordered solvent were all assigned as partial occupancy water molecules. The distances to neighbouring atoms are not sensible and these peaks could not be identified as more complex solvent molecules. ; _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 6439 A**3 RESPONSE: Even with all significant electron density peaks labelled as partial water molecules, there is still a large void space where the disorder is so great that no solvent could be located at all. ; # end Validation Reply Form # Attachment '- GQ271.CIF' data_gq271 _database_code_depnum_ccdc_archive 'CCDC 841381' #TrackingRef '- GQ271.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C76 H76 Cl4 N12 Ni2), 13(C6 H4 Cl2), 30(H2 O)' _chemical_formula_sum 'C382 H416 Cl42 N48 Ni8 O30' _chemical_formula_weight 8118.19 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.817(5) _cell_length_b 25.609(5) _cell_length_c 16.634(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.25(3) _cell_angle_gamma 90.00 _cell_volume 10571(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3223 _cell_measurement_theta_min 5.63 _cell_measurement_theta_max 67.61 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4162 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9053 _exptl_absorpt_correction_T_max 0.9734 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; The solvent residues in the large voids could be mostly identified, however all are at least partially disordered and very difficult to model. To stabilise the refinement, heavy restraints had to be used. In one region of the void the disorder was so great that no individual solvent molecules could be identified from the peaks in the difference map, so the electron density was modelled as partially disordered water molecules. Every attempt was made to identify the solvent molecules in this structure and avoid using squeeze. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 138545 _diffrn_reflns_av_R_equivalents 0.1838 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.05 _reflns_number_total 18709 _reflns_number_gt 14137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0925P)^2^+31.1592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18709 _refine_ls_number_parameters 1280 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2166 _refine_ls_wR_factor_gt 0.1981 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.008 _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 0.98608(3) 0.23626(3) 0.73876(5) 0.01820(18) Uani 1 1 d . . . Cl1 Cl 1.04058(6) 0.17976(6) 0.65237(10) 0.0245(3) Uani 1 1 d . . . Cl2 Cl 0.92520(7) 0.28855(6) 0.82446(10) 0.0264(4) Uani 1 1 d . . . Ni2 Ni 1.48295(3) 0.22857(3) 0.75005(5) 0.01955(19) Uani 1 1 d . . . Cl3 Cl 1.42493(7) 0.17490(6) 0.66428(10) 0.0257(3) Uani 1 1 d . . . Cl4 Cl 1.54469(7) 0.27849(7) 0.83745(10) 0.0274(4) Uani 1 1 d . . . N1 N 0.9201(2) 0.2208(2) 0.6634(3) 0.0230(12) Uani 1 1 d . . . N2 N 0.7333(2) 0.1935(2) 0.5622(3) 0.0263(12) Uani 1 1 d . . . N3 N 0.5480(2) 0.2133(2) 0.6725(3) 0.0255(12) Uani 1 1 d . . . C1 C 0.9223(3) 0.2202(3) 0.5819(4) 0.0266(15) Uani 1 1 d . . . H1A H 0.9560 0.2266 0.5570 0.032 Uiso 1 1 calc R . . C2 C 0.8790(3) 0.2109(3) 0.5339(4) 0.0292(16) Uani 1 1 d . . . H2A H 0.8826 0.2126 0.4772 0.035 Uiso 1 1 calc R . . C3 C 0.8289(3) 0.1989(3) 0.5680(4) 0.0254(15) Uani 1 1 d . . . C4 C 0.8269(3) 0.1974(3) 0.6514(4) 0.0307(16) Uani 1 1 d . . . H4A H 0.7941 0.1890 0.6775 0.037 Uiso 1 1 calc R . . C5 C 0.8723(3) 0.2082(3) 0.6961(4) 0.0291(16) Uani 1 1 d . . . H5A H 0.8698 0.2066 0.7531 0.035 Uiso 1 1 calc R . . C6 C 0.7790(3) 0.1907(3) 0.5193(4) 0.0250(15) Uani 1 1 d . . . C7 C 0.7792(3) 0.1821(3) 0.4376(4) 0.0288(16) Uani 1 1 d . . . H7A H 0.8125 0.1799 0.4098 0.035 Uiso 1 1 calc R . . C8 C 0.7304(3) 0.1767(3) 0.3950(4) 0.0297(15) Uani 1 1 d . . . C9 C 0.6842(3) 0.1804(3) 0.4397(4) 0.0302(16) Uani 1 1 d . . . H9A H 0.6501 0.1771 0.4140 0.036 Uiso 1 1 calc R . . C10 C 0.6869(3) 0.1889(3) 0.5223(4) 0.0281(16) Uani 1 1 d . . . C11 C 0.5970(3) 0.2022(3) 0.7032(4) 0.0328(17) Uani 1 1 d . . . H11A H 0.6008 0.2007 0.7600 0.039 Uiso 1 1 calc R . . C12 C 0.6416(3) 0.1928(3) 0.6570(4) 0.0337(17) Uani 1 1 d . . . H12A H 0.6751 0.1844 0.6819 0.040 Uiso 1 1 calc R . . C13 C 0.6378(3) 0.1957(3) 0.5729(4) 0.0258(15) Uani 1 1 d . . . C14 C 0.5868(3) 0.2058(3) 0.5411(4) 0.0285(16) Uani 1 1 d . . . H14A H 0.5814 0.2061 0.4845 0.034 Uiso 1 1 calc R . . C15 C 0.5439(3) 0.2153(3) 0.5921(4) 0.0269(15) Uani 1 1 d . . . H15A H 0.5099 0.2236 0.5690 0.032 Uiso 1 1 calc R . . C16 C 0.7308(3) 0.1700(4) 0.3038(4) 0.0396(19) Uani 1 1 d U . . C17 C 0.7454(8) 0.2218(6) 0.2671(7) 0.113(5) Uani 1 1 d U . . H17A H 0.7777 0.2356 0.2936 0.169 Uiso 1 1 calc R . . H17B H 0.7155 0.2463 0.2741 0.169 Uiso 1 1 calc R . . H17C H 0.7525 0.2171 0.2096 0.169 Uiso 1 1 calc R . . C18 C 0.7716(6) 0.1316(8) 0.2795(7) 0.125(7) Uani 1 1 d U . . H18A H 0.8067 0.1415 0.3021 0.187 Uiso 1 1 calc R . . H18B H 0.7739 0.1307 0.2207 0.187 Uiso 1 1 calc R . . H18C H 0.7614 0.0970 0.2995 0.187 Uiso 1 1 calc R . . C19 C 0.6766(4) 0.1517(6) 0.2738(6) 0.088(5) Uani 1 1 d . . . H19A H 0.6712 0.1151 0.2891 0.132 Uiso 1 1 calc R . . H19B H 0.6751 0.1548 0.2151 0.132 Uiso 1 1 calc R . . H19C H 0.6482 0.1732 0.2976 0.132 Uiso 1 1 calc R . . N4 N 0.9659(2) 0.1705(2) 0.8092(3) 0.0225(12) Uani 1 1 d . . . N5 N 0.9478(3) -0.0119(2) 0.9129(4) 0.0319(14) Uani 1 1 d . . . N6 N 0.9888(2) -0.1960(2) 0.8290(3) 0.0238(12) Uani 1 1 d . . . C20 C 0.9587(3) 0.1230(3) 0.7747(4) 0.0269(15) Uani 1 1 d . . . H20A H 0.9611 0.1204 0.7178 0.032 Uiso 1 1 calc R . . C21 C 0.9479(3) 0.0780(3) 0.8184(4) 0.0311(16) Uani 1 1 d . . . H21A H 0.9429 0.0456 0.7916 0.037 Uiso 1 1 calc R . . C22 C 0.9444(3) 0.0809(3) 0.9011(4) 0.0291(16) Uani 1 1 d . . . C23 C 0.9507(3) 0.1295(3) 0.9371(4) 0.0312(16) Uani 1 1 d . . . H23A H 0.9475 0.1333 0.9937 0.037 Uiso 1 1 calc R . . C24 C 0.9618(3) 0.1725(3) 0.8891(4) 0.0241(14) Uani 1 1 d . . . H24A H 0.9668 0.2053 0.9147 0.029 Uiso 1 1 calc R . . C25 C 0.9331(3) 0.0326(3) 0.9487(4) 0.0307(16) Uani 1 1 d . . . C26 C 0.9098(3) 0.0344(3) 1.0246(5) 0.0320(17) Uani 1 1 d . . . H26A H 0.9001 0.0671 1.0475 0.038 Uiso 1 1 calc R . . C27 C 0.9007(3) -0.0110(3) 1.0662(5) 0.0361(18) Uani 1 1 d . . . C28 C 0.9153(3) -0.0577(3) 1.0299(5) 0.0338(17) Uani 1 1 d . . . H28A H 0.9100 -0.0899 1.0571 0.041 Uiso 1 1 calc R . . C29 C 0.9377(3) -0.0570(3) 0.9538(4) 0.0298(16) Uani 1 1 d . . . C30 C 1.0111(4) -0.1491(3) 0.8143(5) 0.041(2) Uani 1 1 d . . . H30A H 1.0398 -0.1470 0.7769 0.049 Uiso 1 1 calc R . . C31 C 0.9938(4) -0.1037(3) 0.8519(5) 0.0393(19) Uani 1 1 d . . . H31A H 1.0090 -0.0711 0.8368 0.047 Uiso 1 1 calc R . . C32 C 0.9549(3) -0.1052(3) 0.9107(4) 0.0303(16) Uani 1 1 d . . . C33 C 0.9330(4) -0.1539(3) 0.9276(6) 0.044(2) Uani 1 1 d . . . H33A H 0.9062 -0.1574 0.9678 0.053 Uiso 1 1 calc R . . C34 C 0.9509(3) -0.1977(3) 0.8847(5) 0.040(2) Uani 1 1 d . . . H34A H 0.9349 -0.2305 0.8964 0.048 Uiso 1 1 calc R . . C35 C 0.8726(4) -0.0128(3) 1.1496(5) 0.045(2) Uani 1 1 d . . . C36 C 0.8204(4) -0.0442(5) 1.1389(7) 0.064(3) Uani 1 1 d . . . H36A H 0.7996 -0.0430 1.1888 0.095 Uiso 1 1 calc R . . H36B H 0.8292 -0.0805 1.1260 0.095 Uiso 1 1 calc R . . H36C H 0.7990 -0.0290 1.0950 0.095 Uiso 1 1 calc R . . C37 C 0.8591(6) 0.0414(4) 1.1791(7) 0.086(5) Uani 1 1 d . . . H37A H 0.8423 0.0391 1.2321 0.129 Uiso 1 1 calc R . . H37B H 0.8342 0.0581 1.1412 0.129 Uiso 1 1 calc R . . H37C H 0.8922 0.0621 1.1830 0.129 Uiso 1 1 calc R . . C38 C 0.9094(4) -0.0395(4) 1.2095(5) 0.051(2) Uani 1 1 d . . . H38A H 0.9425 -0.0190 1.2158 0.076 Uiso 1 1 calc R . . H38B H 0.9184 -0.0745 1.1900 0.076 Uiso 1 1 calc R . . H38C H 0.8912 -0.0422 1.2615 0.076 Uiso 1 1 calc R . . N7 N 1.0514(2) 0.2494(2) 0.8210(3) 0.0226(12) Uani 1 1 d . . . N8 N 1.2348(2) 0.2642(2) 0.9374(3) 0.0275(12) Uani 1 1 d . . . N9 N 1.4193(2) 0.2442(2) 0.8317(3) 0.0256(12) Uani 1 1 d . . . C39 C 1.0923(3) 0.2160(3) 0.8254(4) 0.0273(15) Uani 1 1 d . . . H39A H 1.0906 0.1851 0.7939 0.033 Uiso 1 1 calc R . . C40 C 1.1372(3) 0.2240(3) 0.8737(4) 0.0316(16) Uani 1 1 d . . . H40A H 1.1660 0.1996 0.8733 0.038 Uiso 1 1 calc R . . C41 C 1.1399(3) 0.2681(3) 0.9230(4) 0.0268(15) Uani 1 1 d . . . C42 C 1.0957(3) 0.3019(3) 0.9213(5) 0.0374(19) Uani 1 1 d . . . H42A H 1.0950 0.3318 0.9550 0.045 Uiso 1 1 calc R . . C43 C 1.0527(3) 0.2912(3) 0.8697(5) 0.0369(18) Uani 1 1 d . . . H43A H 1.0229 0.3145 0.8689 0.044 Uiso 1 1 calc R . . C44 C 1.1884(3) 0.2805(3) 0.9706(4) 0.0287(16) Uani 1 1 d . . . C45 C 1.1860(3) 0.3095(3) 1.0412(4) 0.0298(16) Uani 1 1 d . . . H45A H 1.1521 0.3197 1.0625 0.036 Uiso 1 1 calc R . . C46 C 1.2339(3) 0.3237(3) 1.0808(4) 0.0319(16) Uani 1 1 d . . . C47 C 1.2821(3) 0.3086(3) 1.0439(5) 0.0358(18) Uani 1 1 d . . . H47A H 1.3157 0.3183 1.0671 0.043 Uiso 1 1 calc R . . C48 C 1.2810(3) 0.2795(3) 0.9737(4) 0.0290(16) Uani 1 1 d . . . C49 C 1.3784(3) 0.2100(3) 0.8397(4) 0.0262(15) Uani 1 1 d . . . H49A H 1.3803 0.1780 0.8111 0.031 Uiso 1 1 calc R . . C50 C 1.3345(3) 0.2191(3) 0.8867(4) 0.0291(16) Uani 1 1 d . . . H50A H 1.3065 0.1939 0.8897 0.035 Uiso 1 1 calc R . . C51 C 1.3307(3) 0.2654(3) 0.9301(4) 0.0260(15) Uani 1 1 d . . . C52 C 1.3747(3) 0.2989(3) 0.9262(5) 0.0385(19) Uani 1 1 d . . . H52A H 1.3755 0.3297 0.9581 0.046 Uiso 1 1 calc R . . C53 C 1.4168(3) 0.2873(3) 0.8762(5) 0.0322(17) Uani 1 1 d . . . H53A H 1.4458 0.3114 0.8731 0.039 Uiso 1 1 calc R . . C54 C 1.2338(3) 0.3565(3) 1.1570(5) 0.0380(18) Uani 1 1 d . . . C55 C 1.1780(4) 0.3583(5) 1.1934(6) 0.066(3) Uani 1 1 d . . . H55A H 1.1643 0.3227 1.1999 0.099 Uiso 1 1 calc R . . H55B H 1.1538 0.3779 1.1578 0.099 Uiso 1 1 calc R . . H55C H 1.1797 0.3755 1.2460 0.099 Uiso 1 1 calc R . . C56 C 1.2564(6) 0.4097(4) 1.1382(6) 0.069(3) Uani 1 1 d . . . H56A H 1.2663 0.4274 1.1884 0.103 Uiso 1 1 calc R . . H56B H 1.2292 0.4304 1.1095 0.103 Uiso 1 1 calc R . . H56C H 1.2884 0.4059 1.1045 0.103 Uiso 1 1 calc R . . C57 C 1.2709(5) 0.3301(5) 1.2208(6) 0.064(3) Uani 1 1 d . . . H57A H 1.2556 0.2963 1.2360 0.096 Uiso 1 1 calc R . . H57B H 1.2735 0.3525 1.2684 0.096 Uiso 1 1 calc R . . H57C H 1.3068 0.3249 1.1981 0.096 Uiso 1 1 calc R . . N10 N 1.5028(2) 0.1616(2) 0.8173(3) 0.0260(13) Uani 1 1 d . . . N11 N 1.5543(3) -0.0178(2) 0.9106(4) 0.0333(14) Uani 1 1 d . . . N12 N 1.5380(2) -0.2028(2) 0.8173(3) 0.0257(12) Uani 1 1 d . . . C58 C 1.5134(3) 0.1159(3) 0.7809(4) 0.0355(17) Uani 1 1 d . . . H58A H 1.5075 0.1132 0.7246 0.043 Uiso 1 1 calc R . . C59 C 1.5324(3) 0.0724(3) 0.8221(5) 0.0350(17) Uani 1 1 d . . . H59A H 1.5396 0.0410 0.7936 0.042 Uiso 1 1 calc R . . C60 C 1.5409(3) 0.0744(3) 0.9043(4) 0.0296(16) Uani 1 1 d . . . C61 C 1.5291(3) 0.1215(3) 0.9422(4) 0.0298(16) Uani 1 1 d . . . H61A H 1.5337 0.1249 0.9987 0.036 Uiso 1 1 calc R . . C62 C 1.5107(3) 0.1636(3) 0.8973(4) 0.0260(15) Uani 1 1 d . . . H62A H 1.5032 0.1954 0.9244 0.031 Uiso 1 1 calc R . . C63 C 1.5618(3) 0.0285(3) 0.9486(5) 0.0345(17) Uani 1 1 d . . . C64 C 1.5872(4) 0.0323(3) 1.0228(5) 0.0380(19) Uani 1 1 d . . . H64A H 1.5919 0.0656 1.0472 0.046 Uiso 1 1 calc R . . C65 C 1.6058(4) -0.0124(3) 1.0621(6) 0.045(2) Uani 1 1 d . . . C66 C 1.5978(3) -0.0596(3) 1.0226(5) 0.0386(19) Uani 1 1 d . . . H66A H 1.6100 -0.0911 1.0467 0.046 Uiso 1 1 calc R . . C67 C 1.5721(3) -0.0610(3) 0.9476(5) 0.0312(16) Uani 1 1 d . . . C68 C 1.5771(3) -0.2006(3) 0.8718(6) 0.046(2) Uani 1 1 d . . . H68A H 1.5980 -0.2312 0.8804 0.055 Uiso 1 1 calc R . . C69 C 1.5895(4) -0.1567(3) 0.9173(6) 0.052(3) Uani 1 1 d . . . H69A H 1.6170 -0.1583 0.9571 0.063 Uiso 1 1 calc R . . C70 C 1.5618(3) -0.1109(3) 0.9043(4) 0.0293(16) Uani 1 1 d . . . C71 C 1.5215(4) -0.1129(3) 0.8478(5) 0.048(2) Uani 1 1 d . . . H71A H 1.5013 -0.0822 0.8365 0.058 Uiso 1 1 calc R . . C72 C 1.5097(4) -0.1580(3) 0.8071(5) 0.043(2) Uani 1 1 d . . . H72A H 1.4804 -0.1579 0.7701 0.051 Uiso 1 1 calc R . . C73 C 1.6336(4) -0.0079(4) 1.1439(7) 0.060(3) Uani 1 1 d . . . C74 C 1.5979(5) 0.0233(4) 1.2024(7) 0.072(3) Uani 1 1 d . . . H74A H 1.6148 0.0238 1.2557 0.107 Uiso 1 1 calc R . . H74B H 1.5623 0.0069 1.2058 0.107 Uiso 1 1 calc R . . H74C H 1.5939 0.0592 1.1827 0.107 Uiso 1 1 calc R . . C75 C 1.6860(5) 0.0232(5) 1.1325(9) 0.085(4) Uani 1 1 d . . . H75A H 1.6775 0.0578 1.1107 0.128 Uiso 1 1 calc R . . H75B H 1.7095 0.0046 1.0951 0.128 Uiso 1 1 calc R . . H75C H 1.7043 0.0271 1.1844 0.128 Uiso 1 1 calc R . . C76 C 1.6462(9) -0.0616(4) 1.1790(10) 0.133(8) Uani 1 1 d . . . H76A H 1.6642 -0.0830 1.1383 0.200 Uiso 1 1 calc R . . H76B H 1.6126 -0.0787 1.1952 0.200 Uiso 1 1 calc R . . H76C H 1.6698 -0.0577 1.2259 0.200 Uiso 1 1 calc R . . Cl10 Cl 1.58885(17) 0.06106(13) 1.6099(2) 0.0946(11) Uani 1 1 d . . . Cl11 Cl 1.6334(2) 0.0224(2) 1.4435(2) 0.1178(15) Uani 1 1 d . . . C100 C 1.5686(6) 0.0017(4) 1.5707(7) 0.073(4) Uani 1 1 d . . . C101 C 1.5883(6) -0.0163(4) 1.4986(6) 0.072(3) Uani 1 1 d . . . C102 C 1.5742(7) -0.0616(6) 1.4671(9) 0.091(5) Uani 1 1 d . . . H10D H 1.5898 -0.0731 1.4181 0.109 Uiso 1 1 calc R . . C103 C 1.5370(7) -0.0918(5) 1.5055(10) 0.089(5) Uani 1 1 d . . . H10A H 1.5254 -0.1233 1.4809 0.107 Uiso 1 1 calc R . . C104 C 1.5153(7) -0.0776(5) 1.5805(10) 0.097(5) Uani 1 1 d . . . H10B H 1.4900 -0.0994 1.6072 0.116 Uiso 1 1 calc R . . C105 C 1.5325(6) -0.0296(5) 1.6145(8) 0.086(4) Uani 1 1 d . . . H10C H 1.5199 -0.0187 1.6657 0.104 Uiso 1 1 calc R . . Cl20 Cl 0.88168(18) -0.05689(15) 1.4903(3) 0.0787(12) Uani 0.75 1 d P A 1 Cl21 Cl 0.8554(2) 0.06193(18) 1.4530(3) 0.126(2) Uani 0.75 1 d P A 1 C200 C 0.9293(2) -0.01612(19) 1.4372(4) 0.063(4) Uani 0.75 1 d PR A 1 C201 C 0.9216(2) 0.03655(18) 1.4204(3) 0.091(5) Uani 0.75 1 d PRU A 1 C202 C 0.9622(3) 0.0651(2) 1.3836(6) 0.108(6) Uani 0.75 1 d PRU A 1 H20B H 0.9569 0.1011 1.3721 0.130 Uiso 0.75 1 calc PR A 1 C203 C 1.0105(3) 0.0410(2) 1.3634(6) 0.093(7) Uani 0.75 1 d PR A 1 H20C H 1.0379 0.0604 1.3373 0.111 Uiso 0.75 1 calc PR A 1 C204 C 1.0185(2) -0.0113(2) 1.3813(4) 0.110(8) Uani 0.75 1 d PR A 1 H20D H 1.0520 -0.0275 1.3691 0.132 Uiso 0.75 1 calc PR A 1 C205 C 0.9776(2) -0.04020(19) 1.4171(4) 0.069(4) Uani 0.75 1 d PR A 1 H20E H 0.9826 -0.0763 1.4277 0.083 Uiso 0.75 1 calc PR A 1 Cl30 Cl 1.2481(5) -0.0550(5) 1.3659(8) 0.166(5) Uani 0.50 1 d PD B 2 Cl31 Cl 1.2714(9) 0.0545(12) 1.4246(8) 0.309(14) Uani 0.50 1 d PD B 2 C300 C 1.2118(13) 0.0012(11) 1.346(2) 0.144(13) Uani 0.50 1 d PDU B 2 C301 C 1.2220(11) 0.0548(13) 1.3647(19) 0.135(10) Uani 0.50 1 d PDU B 2 C302 C 1.1994(11) 0.0977(13) 1.3324(17) 0.125(11) Uani 0.50 1 d PDU B 2 H30B H 1.2119 0.1303 1.3525 0.150 Uiso 0.50 1 calc PR B 2 C303 C 1.1574(11) 0.1001(17) 1.2690(19) 0.112(9) Uani 0.50 1 d PDU B 2 H30C H 1.1431 0.1316 1.2476 0.134 Uiso 0.50 1 calc PR B 2 C304 C 1.1403(10) 0.0473(13) 1.2431(17) 0.097(8) Uani 0.50 1 d PDU B 2 H30D H 1.1122 0.0402 1.2056 0.116 Uiso 0.50 1 calc PR B 2 C305 C 1.1722(12) 0.0083(16) 1.283(2) 0.139(10) Uani 0.50 1 d PDU B 2 H30E H 1.1646 -0.0247 1.2593 0.167 Uiso 0.50 1 calc PR B 2 Cl40 Cl 0.6655(3) 0.1691(3) 1.0299(5) 0.084(2) Uani 0.50 1 d P C 1 Cl41 Cl 0.6613(2) 0.1170(2) 0.8550(4) 0.143(4) Uani 0.50 1 d PU C 1 C400 C 0.7134(2) 0.1584(2) 0.9645(4) 0.081(8) Uani 0.50 1 d PR C 1 C401 C 0.7083(2) 0.1345(2) 0.8899(4) 0.133(15) Uani 0.50 1 d PRU C 1 C402 C 0.7541(2) 0.1223(4) 0.8457(4) 0.18(2) Uani 0.50 1 d PRU C 1 H40B H 0.7506 0.1059 0.7947 0.219 Uiso 0.50 1 calc PR C 1 C403 C 0.8049(2) 0.1341(4) 0.8762(4) 0.32(2) Uani 0.50 1 d PRU C 1 H40C H 0.8361 0.1258 0.8460 0.378 Uiso 0.50 1 calc PR C 1 C404 C 0.8100(2) 0.1581(4) 0.9508(4) 0.162(17) Uani 0.50 1 d PRU C 1 H40D H 0.8447 0.1662 0.9715 0.195 Uiso 0.50 1 calc PR C 1 C405 C 0.7642(2) 0.1702(2) 0.9950(4) 0.21(3) Uani 0.50 1 d PR C 1 H40E H 0.7677 0.1865 1.0460 0.246 Uiso 0.50 1 calc PR C 1 Cl50 Cl 0.8079(2) 0.1615(2) 1.0398(3) 0.093(2) Uani 0.50 1 d PRU C 2 Cl51 Cl 0.8157(2) 0.1292(4) 0.8709(4) 0.279(11) Uani 0.50 1 d PRU C 2 C500 C 0.7543(2) 0.1522(2) 0.9754(4) 0.130(14) Uani 0.50 1 d PRU C 2 C501 C 0.7484(2) 0.1353(4) 0.8964(4) 0.23(4) Uani 0.50 1 d PR C 2 C502 C 0.6992(3) 0.1416(4) 0.8573(5) 0.196(17) Uani 0.50 1 d PRU C 2 H50B H 0.6949 0.1308 0.8030 0.235 Uiso 0.50 1 calc PR C 2 C503 C 0.6560(3) 0.1639(2) 0.8985(6) 0.160(17) Uani 0.50 1 d PRU C 2 H50C H 0.6223 0.1682 0.8719 0.192 Uiso 0.50 1 calc PR C 2 C504 C 0.6616(2) 0.1795(2) 0.9766(5) 0.110(12) Uani 0.50 1 d PRU C 2 H50D H 0.6315 0.1931 1.0048 0.132 Uiso 0.50 1 calc PR C 2 C505 C 0.7107(2) 0.1755(2) 1.0143(5) 0.130(19) Uani 0.50 1 d PR C 2 H50E H 0.7152 0.1887 1.0673 0.156 Uiso 0.50 1 calc PR C 2 O100 O 0.7606(8) -0.1294(8) 0.9694(9) 0.190(8) Uani 1 1 d . D 1 O101 O 1.2517(14) 0.1860(6) 1.1397(11) 0.271(14) Uani 1 1 d . E 2 O102 O 0.7884(10) -0.0198(9) 0.9041(13) 0.108(7) Uani 0.50 1 d P F 3 O103 O 0.7647(14) -0.0796(11) 0.9431(15) 0.162(14) Uani 0.50 1 d P G 4 O104 O 0.7214(15) -0.0164(10) 0.903(2) 0.202(19) Uani 0.50 1 d P H 5 O105 O 1.1683(12) -0.0557(8) 1.3172(15) 0.131(9) Uani 0.50 1 d P I 6 O106 O 1.6649(12) -0.0399(15) 0.7790(19) 0.266(14) Uani 0.75 1 d PU J 7 O107 O 1.1068(12) -0.0495(14) 1.3845(16) 0.161(12) Uani 0.50 1 d P K 8 O108 O 1.6759(11) -0.132(2) 0.7574(14) 0.41(4) Uani 0.75 1 d P L 9 O109 O 0.8771(15) 0.0092(14) 1.440(2) 0.184(13) Uani 0.50 1 d PU M 10 O110 O 0.7221(13) -0.0977(18) 0.867(2) 0.218(16) Uani 0.50 1 d PU N 1 O111 O 1.0441(10) 0.0375(14) 1.3513(16) 0.137(11) Uani 0.50 1 d P O 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 0.0158(4) 0.0226(4) 0.0161(4) -0.0004(3) -0.0004(3) 0.0002(3) Cl1 0.0210(8) 0.0274(8) 0.0250(8) -0.0041(6) 0.0004(7) 0.0016(6) Cl2 0.0239(8) 0.0322(9) 0.0230(8) -0.0010(6) 0.0057(7) 0.0053(7) Ni2 0.0167(4) 0.0265(4) 0.0154(4) -0.0009(3) 0.0009(3) 0.0003(3) Cl3 0.0252(8) 0.0284(8) 0.0235(8) -0.0052(6) -0.0011(7) -0.0011(7) Cl4 0.0245(8) 0.0364(9) 0.0213(8) -0.0014(7) -0.0064(7) -0.0043(7) N1 0.017(3) 0.037(3) 0.016(3) -0.002(2) 0.003(2) 0.003(2) N2 0.019(3) 0.042(3) 0.019(3) 0.000(2) 0.001(2) 0.002(3) N3 0.019(3) 0.038(3) 0.019(3) 0.000(2) 0.000(2) -0.004(2) C1 0.016(3) 0.043(4) 0.021(3) 0.002(3) -0.004(3) -0.002(3) C2 0.021(4) 0.054(5) 0.013(3) 0.003(3) 0.000(3) -0.001(3) C3 0.017(3) 0.040(4) 0.019(3) -0.002(3) -0.001(3) -0.006(3) C4 0.018(3) 0.054(5) 0.020(3) -0.002(3) 0.001(3) -0.005(3) C5 0.021(4) 0.056(5) 0.010(3) 0.001(3) 0.004(3) -0.010(3) C6 0.010(3) 0.040(4) 0.025(3) -0.004(3) 0.001(3) -0.002(3) C7 0.016(3) 0.050(4) 0.020(3) -0.007(3) 0.006(3) 0.002(3) C8 0.024(4) 0.042(4) 0.022(3) -0.006(3) 0.002(3) 0.001(3) C9 0.017(3) 0.054(5) 0.019(3) -0.010(3) 0.002(3) -0.002(3) C10 0.016(3) 0.047(4) 0.021(3) -0.010(3) 0.003(3) 0.002(3) C11 0.020(4) 0.059(5) 0.019(3) -0.001(3) 0.000(3) 0.004(3) C12 0.017(3) 0.062(5) 0.022(4) -0.002(3) -0.003(3) 0.006(3) C13 0.018(3) 0.041(4) 0.018(3) -0.007(3) 0.005(3) -0.003(3) C14 0.023(4) 0.046(4) 0.017(3) 0.006(3) -0.003(3) -0.001(3) C15 0.015(3) 0.044(4) 0.021(3) 0.001(3) 0.000(3) 0.005(3) C16 0.033(4) 0.069(5) 0.017(3) -0.016(3) 0.000(3) -0.001(4) C17 0.166(13) 0.130(11) 0.041(6) 0.014(7) -0.014(8) -0.043(10) C18 0.088(9) 0.232(17) 0.055(7) -0.078(9) -0.021(7) 0.089(11) C19 0.048(6) 0.186(15) 0.031(5) -0.044(7) 0.007(5) -0.031(7) N4 0.023(3) 0.024(3) 0.020(3) 0.000(2) -0.003(2) -0.002(2) N5 0.042(4) 0.020(3) 0.034(3) 0.000(2) 0.006(3) 0.004(3) N6 0.023(3) 0.023(3) 0.025(3) 0.003(2) 0.002(3) -0.001(2) C20 0.036(4) 0.026(3) 0.020(3) -0.004(3) 0.000(3) -0.009(3) C21 0.039(4) 0.023(3) 0.032(4) -0.008(3) 0.002(3) -0.004(3) C22 0.031(4) 0.028(4) 0.029(4) 0.002(3) 0.008(3) 0.000(3) C23 0.043(4) 0.031(4) 0.019(3) -0.004(3) 0.001(3) 0.002(3) C24 0.030(4) 0.020(3) 0.023(3) -0.003(3) -0.002(3) -0.003(3) C25 0.035(4) 0.030(4) 0.028(4) 0.005(3) 0.006(3) 0.001(3) C26 0.037(4) 0.022(4) 0.037(4) 0.004(3) 0.015(3) 0.005(3) C27 0.048(5) 0.027(4) 0.034(4) 0.001(3) 0.013(4) 0.006(3) C28 0.034(4) 0.033(4) 0.035(4) 0.003(3) 0.009(3) -0.002(3) C29 0.034(4) 0.027(4) 0.028(4) 0.005(3) 0.003(3) 0.000(3) C30 0.054(5) 0.039(4) 0.030(4) 0.000(3) 0.015(4) -0.018(4) C31 0.053(5) 0.026(4) 0.039(4) 0.000(3) 0.022(4) -0.009(3) C32 0.040(4) 0.024(4) 0.027(4) -0.003(3) 0.004(3) 0.005(3) C33 0.051(5) 0.025(4) 0.057(5) 0.004(4) 0.031(4) -0.003(4) C34 0.044(5) 0.021(4) 0.056(5) 0.000(3) 0.027(4) -0.003(3) C35 0.059(6) 0.041(5) 0.035(5) 0.010(4) 0.025(4) 0.003(4) C36 0.046(6) 0.082(7) 0.063(7) 0.027(6) 0.020(5) 0.010(5) C37 0.126(11) 0.057(6) 0.075(8) 0.011(6) 0.075(8) 0.023(7) C38 0.053(6) 0.058(6) 0.041(5) -0.001(4) 0.015(4) -0.002(4) N7 0.020(3) 0.024(3) 0.024(3) -0.003(2) -0.002(2) 0.001(2) N8 0.018(3) 0.040(3) 0.024(3) -0.009(3) -0.002(3) 0.001(3) N9 0.020(3) 0.035(3) 0.022(3) -0.001(2) 0.003(2) 0.003(2) C39 0.021(3) 0.034(4) 0.026(4) -0.013(3) -0.007(3) 0.000(3) C40 0.022(4) 0.040(4) 0.033(4) -0.015(3) -0.003(3) 0.006(3) C41 0.017(3) 0.038(4) 0.025(3) -0.008(3) -0.005(3) 0.000(3) C42 0.027(4) 0.043(4) 0.042(4) -0.020(4) -0.005(3) 0.006(3) C43 0.031(4) 0.039(4) 0.040(4) -0.015(4) -0.010(3) -0.002(3) C44 0.018(3) 0.041(4) 0.027(4) -0.008(3) 0.002(3) 0.000(3) C45 0.022(4) 0.041(4) 0.026(4) -0.007(3) 0.001(3) 0.003(3) C46 0.023(3) 0.052(4) 0.021(3) -0.011(3) -0.002(3) 0.001(3) C47 0.022(4) 0.056(5) 0.029(4) -0.014(4) 0.000(3) -0.008(3) C48 0.024(4) 0.038(4) 0.025(4) -0.009(3) 0.002(3) 0.002(3) C49 0.026(4) 0.030(4) 0.022(3) -0.004(3) 0.003(3) 0.000(3) C50 0.021(3) 0.036(4) 0.030(4) -0.004(3) 0.005(3) -0.006(3) C51 0.017(3) 0.037(4) 0.023(3) -0.008(3) 0.001(3) -0.003(3) C52 0.020(4) 0.045(5) 0.051(5) -0.021(4) 0.003(4) -0.002(3) C53 0.024(4) 0.030(4) 0.042(4) -0.011(3) 0.008(3) -0.009(3) C54 0.026(4) 0.058(5) 0.030(4) -0.017(4) 0.003(3) 0.001(4) C55 0.041(5) 0.112(9) 0.046(5) -0.049(6) 0.005(4) -0.006(5) C56 0.110(10) 0.061(6) 0.035(5) -0.020(4) 0.012(6) -0.022(6) C57 0.067(7) 0.088(8) 0.037(5) -0.022(5) -0.016(5) 0.014(6) N10 0.029(3) 0.028(3) 0.021(3) -0.002(2) 0.003(2) 0.001(2) N11 0.042(4) 0.023(3) 0.035(3) -0.003(3) 0.000(3) 0.000(3) N12 0.024(3) 0.031(3) 0.022(3) -0.001(2) -0.002(2) -0.002(2) C58 0.036(4) 0.043(4) 0.027(4) -0.001(3) 0.002(3) 0.020(4) C59 0.045(5) 0.029(4) 0.031(4) -0.004(3) -0.003(3) 0.008(3) C60 0.032(4) 0.026(4) 0.030(4) 0.000(3) -0.006(3) 0.002(3) C61 0.035(4) 0.036(4) 0.019(3) -0.003(3) -0.002(3) 0.008(3) C62 0.036(4) 0.024(3) 0.018(3) 0.000(3) 0.003(3) 0.007(3) C63 0.037(4) 0.027(4) 0.039(4) 0.004(3) -0.006(4) 0.005(3) C64 0.052(5) 0.024(4) 0.037(4) -0.002(3) -0.017(4) 0.007(3) C65 0.043(5) 0.027(4) 0.064(6) 0.001(4) -0.023(4) -0.004(3) C66 0.042(5) 0.029(4) 0.044(5) 0.002(3) -0.021(4) 0.010(3) C67 0.029(4) 0.031(4) 0.033(4) 0.002(3) -0.007(3) 0.000(3) C68 0.039(5) 0.026(4) 0.073(6) -0.007(4) -0.033(5) 0.009(3) C69 0.053(6) 0.037(5) 0.067(6) -0.008(4) -0.043(5) 0.000(4) C70 0.029(4) 0.028(4) 0.031(4) 0.006(3) -0.001(3) 0.000(3) C71 0.060(6) 0.033(4) 0.050(5) -0.016(4) -0.029(5) 0.020(4) C72 0.043(5) 0.044(5) 0.041(4) -0.012(4) -0.023(4) 0.017(4) C73 0.069(7) 0.035(5) 0.076(7) -0.012(5) -0.045(6) 0.014(4) C74 0.087(8) 0.065(7) 0.063(7) 0.002(5) -0.040(6) 0.006(6) C75 0.050(7) 0.096(9) 0.110(11) -0.033(8) -0.039(7) 0.001(6) C76 0.24(2) 0.043(6) 0.116(12) -0.019(7) -0.129(14) 0.043(9) Cl10 0.117(3) 0.071(2) 0.096(2) -0.0391(18) 0.012(2) -0.0053(19) Cl11 0.137(4) 0.146(4) 0.071(2) 0.004(2) 0.018(2) 0.009(3) C100 0.125(11) 0.044(6) 0.052(6) -0.023(5) -0.011(7) 0.021(6) C101 0.109(10) 0.060(7) 0.046(6) -0.009(5) -0.013(6) 0.030(6) C102 0.112(12) 0.072(9) 0.089(10) -0.037(8) -0.045(9) 0.034(8) C103 0.104(11) 0.064(8) 0.099(11) -0.044(8) -0.045(9) 0.024(8) C104 0.099(11) 0.068(8) 0.122(13) 0.013(8) -0.033(10) 0.004(8) C105 0.114(11) 0.080(9) 0.065(8) -0.018(7) -0.001(8) -0.003(8) Cl20 0.083(3) 0.054(2) 0.100(3) 0.008(2) -0.020(2) -0.0166(19) Cl21 0.122(5) 0.096(4) 0.159(6) 0.021(4) 0.014(4) 0.044(3) C200 0.073(10) 0.059(8) 0.057(9) 0.005(7) -0.013(8) -0.003(7) C201 0.126(15) 0.065(10) 0.082(11) 0.006(8) -0.041(11) -0.005(10) C202 0.173(18) 0.073(11) 0.078(11) 0.029(9) -0.033(12) -0.040(11) C203 0.101(17) 0.120(18) 0.057(11) 0.011(11) 0.002(12) -0.035(15) C204 0.16(2) 0.103(15) 0.064(11) -0.027(10) 0.067(13) -0.018(14) C205 0.093(12) 0.065(9) 0.049(8) -0.010(7) -0.013(8) 0.006(8) Cl30 0.164(11) 0.166(10) 0.168(10) 0.053(8) -0.029(9) -0.046(8) Cl31 0.214(18) 0.62(5) 0.094(9) 0.001(16) 0.026(10) 0.07(2) C300 0.16(3) 0.14(2) 0.14(2) 0.00(2) 0.09(2) -0.02(2) C301 0.13(2) 0.14(2) 0.14(2) 0.016(18) 0.073(19) 0.010(18) C302 0.13(2) 0.098(19) 0.15(2) 0.011(17) 0.108(19) 0.020(16) C303 0.053(13) 0.18(3) 0.099(17) 0.044(18) -0.005(13) -0.009(15) C304 0.048(11) 0.17(2) 0.073(14) 0.045(15) -0.020(10) -0.013(12) C305 0.077(16) 0.20(3) 0.14(2) 0.04(2) 0.028(16) -0.005(17) Cl40 0.089(5) 0.062(4) 0.102(5) -0.008(4) 0.048(5) -0.003(3) Cl41 0.074(5) 0.208(12) 0.147(9) 0.069(8) -0.005(6) 0.014(6) C400 0.062(16) 0.09(2) 0.09(2) 0.038(17) 0.008(15) -0.004(14) C401 0.11(2) 0.15(2) 0.14(2) 0.020(17) 0.022(17) 0.001(17) C402 0.19(3) 0.13(2) 0.22(3) 0.09(2) 0.05(3) 0.02(2) C403 0.19(4) 0.45(4) 0.30(4) 0.10(4) 0.08(4) -0.01(4) C404 0.09(2) 0.19(4) 0.21(4) 0.08(3) 0.05(3) 0.05(2) C405 0.07(2) 0.11(3) 0.44(10) 0.15(4) 0.10(4) 0.02(2) Cl50 0.109(6) 0.083(4) 0.086(5) -0.016(4) -0.022(4) 0.010(4) Cl51 0.136(12) 0.43(3) 0.28(2) 0.11(2) 0.080(14) 0.001(15) C500 0.09(2) 0.12(2) 0.18(3) 0.07(2) -0.04(2) 0.020(18) C501 0.42(12) 0.14(4) 0.12(4) 0.07(3) -0.16(6) -0.09(6) C502 0.13(2) 0.24(3) 0.21(3) 0.07(2) -0.03(2) -0.02(2) C503 0.10(3) 0.21(4) 0.17(4) -0.01(3) -0.04(3) 0.02(3) C504 0.09(2) 0.065(16) 0.17(3) -0.015(19) 0.02(2) 0.018(14) C505 0.23(6) 0.054(17) 0.11(3) 0.006(18) -0.07(4) 0.02(3) O100 0.207(16) 0.230(18) 0.132(11) 0.097(12) -0.078(11) -0.076(15) O101 0.56(5) 0.097(10) 0.151(13) 0.017(9) 0.01(2) -0.013(18) O102 0.125(18) 0.106(16) 0.092(14) 0.000(12) -0.051(13) 0.007(13) O103 0.25(3) 0.131(19) 0.101(16) -0.076(16) -0.12(2) 0.09(2) O104 0.25(4) 0.107(18) 0.25(3) -0.06(2) 0.19(3) -0.08(2) O105 0.20(3) 0.079(13) 0.114(17) -0.028(13) 0.006(18) -0.034(15) O106 0.20(2) 0.38(3) 0.22(2) 0.04(2) 0.145(18) -0.02(2) O107 0.15(2) 0.23(3) 0.102(18) -0.05(2) -0.043(18) 0.01(2) O108 0.19(2) 0.90(9) 0.144(18) -0.25(4) 0.111(18) -0.35(4) O109 0.19(2) 0.18(2) 0.19(2) -0.011(19) 0.06(2) 0.080(19) O110 0.14(2) 0.35(4) 0.17(2) 0.00(3) 0.08(2) -0.08(2) O111 0.089(17) 0.22(3) 0.102(18) 0.037(18) 0.018(15) 0.041(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.094(6) . ? Ni1 N4 2.114(5) . ? Ni1 N7 2.144(6) . ? Ni1 N6 2.163(6) 2_756 ? Ni1 Cl1 2.4507(18) . ? Ni1 Cl2 2.4753(18) . ? Ni2 N10 2.104(6) . ? Ni2 N3 2.107(6) 1_655 ? Ni2 N9 2.126(6) . ? Ni2 N12 2.147(6) 2_856 ? Ni2 Cl3 2.4452(18) . ? Ni2 Cl4 2.4650(19) . ? N1 C5 1.347(9) . ? N1 C1 1.358(9) . ? N2 C10 1.333(9) . ? N2 C6 1.344(9) . ? N3 C15 1.342(9) . ? N3 C11 1.346(9) . ? N3 Ni2 2.107(6) 1_455 ? C1 C2 1.357(10) . ? C1 H1A 0.9500 . ? C2 C3 1.401(10) . ? C2 H2A 0.9500 . ? C3 C4 1.389(10) . ? C3 C6 1.492(9) . ? C4 C5 1.376(10) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.378(10) . ? C7 C8 1.407(10) . ? C7 H7A 0.9500 . ? C8 C9 1.373(10) . ? C8 C16 1.527(9) . ? C9 C10 1.392(10) . ? C9 H9A 0.9500 . ? C10 C13 1.493(9) . ? C11 C12 1.373(10) . ? C11 H11A 0.9500 . ? C12 C13 1.404(10) . ? C12 H12A 0.9500 . ? C13 C14 1.396(10) . ? C14 C15 1.385(10) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C18 1.470(14) . ? C16 C17 1.504(16) . ? C16 C19 1.509(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N4 C24 1.335(9) . ? N4 C20 1.356(8) . ? N5 C25 1.335(9) . ? N5 C29 1.364(9) . ? N6 C34 1.324(9) . ? N6 C30 1.343(9) . ? N6 Ni1 2.163(6) 2_746 ? C20 C21 1.389(10) . ? C20 H20A 0.9500 . ? C21 C22 1.382(10) . ? C21 H21A 0.9500 . ? C22 C23 1.391(10) . ? C22 C25 1.495(10) . ? C23 C24 1.387(10) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.392(10) . ? C26 C27 1.374(10) . ? C26 H26A 0.9500 . ? C27 C28 1.387(11) . ? C27 C35 1.557(10) . ? C28 C29 1.385(10) . ? C28 H28A 0.9500 . ? C29 C32 1.492(10) . ? C30 C31 1.389(11) . ? C30 H30A 0.9500 . ? C31 C32 1.377(11) . ? C31 H31A 0.9500 . ? C32 C33 1.388(11) . ? C33 C34 1.403(11) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C37 1.510(13) . ? C35 C38 1.512(14) . ? C35 C36 1.533(15) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? N7 C39 1.328(9) . ? N7 C43 1.340(9) . ? N8 C44 1.346(9) . ? N8 C48 1.352(9) . ? N9 C53 1.331(9) . ? N9 C49 1.346(9) . ? C39 C40 1.387(10) . ? C39 H39A 0.9500 . ? C40 C41 1.397(10) . ? C40 H40A 0.9500 . ? C41 C42 1.398(10) . ? C41 C44 1.472(10) . ? C42 C43 1.396(11) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 C45 1.391(10) . ? C45 C46 1.406(10) . ? C45 H45A 0.9500 . ? C46 C47 1.401(11) . ? C46 C54 1.521(9) . ? C47 C48 1.385(10) . ? C47 H47A 0.9500 . ? C48 C51 1.478(9) . ? C49 C50 1.364(10) . ? C49 H49A 0.9500 . ? C50 C51 1.392(10) . ? C50 H50A 0.9500 . ? C51 C52 1.389(10) . ? C52 C53 1.372(11) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? C54 C56 1.506(13) . ? C54 C55 1.515(12) . ? C54 C57 1.556(13) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? N10 C58 1.344(9) . ? N10 C62 1.346(9) . ? N11 C67 1.340(10) . ? N11 C63 1.356(10) . ? N12 C68 1.327(10) . ? N12 C72 1.355(10) . ? N12 Ni2 2.147(6) 2_846 ? C58 C59 1.390(10) . ? C58 H58A 0.9500 . ? C59 C60 1.384(11) . ? C59 H59A 0.9500 . ? C60 C61 1.395(10) . ? C60 C63 1.478(10) . ? C61 C62 1.387(10) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 C64 1.387(11) . ? C64 C65 1.395(11) . ? C64 H64A 0.9500 . ? C65 C66 1.389(11) . ? C65 C73 1.528(13) . ? C66 C67 1.399(11) . ? C66 H66A 0.9500 . ? C67 C70 1.488(10) . ? C68 C69 1.389(12) . ? C68 H68A 0.9500 . ? C69 C70 1.376(11) . ? C69 H69A 0.9500 . ? C70 C71 1.371(11) . ? C71 C72 1.371(11) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? C73 C76 1.527(14) . ? C73 C75 1.537(16) . ? C73 C74 1.541(17) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? Cl10 C100 1.729(11) . ? Cl11 C101 1.756(15) . ? C100 C101 1.376(15) . ? C100 C105 1.407(19) . ? C101 C102 1.320(17) . ? C102 C103 1.36(2) . ? C102 H10D 0.9500 . ? C103 C104 1.41(2) . ? C103 H10A 0.9500 . ? C104 C105 1.419(19) . ? C104 H10B 0.9500 . ? C105 H10C 0.9500 . ? Cl20 C200 1.809(7) . ? Cl21 C201 1.8490 . ? C200 C205 1.3896 . ? C200 C201 1.3904 . ? C201 C202 1.3902 . ? C202 C203 1.3899 . ? C202 H20B 0.9500 . ? C203 C204 1.3880 . ? C203 H20C 0.9500 . ? C204 C205 1.3927(12) . ? C204 H20D 0.9500 . ? C205 H20E 0.9500 . ? Cl30 C300 1.729(19) . ? Cl31 C301 1.577(19) . ? C300 C301 1.431(19) . ? C300 C305 1.445(19) . ? C301 C302 1.34(4) . ? C302 C303 1.482(19) . ? C302 H30B 0.9500 . ? C303 C304 1.48(5) . ? C303 H30C 0.9500 . ? C304 C305 1.434(19) . ? C304 H30D 0.9500 . ? C305 H30E 0.9500 . ? Cl40 C400 1.637(9) . ? Cl41 C401 1.3766 . ? C400 C405 1.3900 . ? C400 C401 1.3900 . ? C401 C402 1.3903 . ? C402 C403 1.3901 . ? C402 H40B 0.9500 . ? C403 C404 1.389(3) . ? C403 H40C 0.9500 . ? C404 C405 1.391(2) . ? C404 H40D 0.9500 . ? C405 H40E 0.9500 . ? Cl50 C500 1.7210 . ? Cl51 C501 1.7327 . ? C500 C501 1.3909(13) . ? C500 C505 1.396(3) . ? C501 C502 1.3901 . ? C502 C503 1.397(4) . ? C502 H50B 0.9500 . ? C503 C504 1.3661(19) . ? C503 H50C 0.9500 . ? C504 C505 1.3737 . ? C504 H50D 0.9500 . ? C505 H50E 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 89.7(2) . . ? N1 Ni1 N7 176.8(2) . . ? N4 Ni1 N7 87.3(2) . . ? N1 Ni1 N6 93.8(2) . 2_756 ? N4 Ni1 N6 176.5(2) . 2_756 ? N7 Ni1 N6 89.3(2) . 2_756 ? N1 Ni1 Cl1 88.27(15) . . ? N4 Ni1 Cl1 89.27(16) . . ? N7 Ni1 Cl1 92.83(15) . . ? N6 Ni1 Cl1 90.40(15) 2_756 . ? N1 Ni1 Cl2 88.23(15) . . ? N4 Ni1 Cl2 88.00(16) . . ? N7 Ni1 Cl2 90.53(16) . . ? N6 Ni1 Cl2 92.54(15) 2_756 . ? Cl1 Ni1 Cl2 175.57(7) . . ? N10 Ni2 N3 89.8(2) . 1_655 ? N10 Ni2 N9 89.2(2) . . ? N3 Ni2 N9 178.0(2) 1_655 . ? N10 Ni2 N12 179.2(2) . 2_856 ? N3 Ni2 N12 91.0(2) 1_655 2_856 ? N9 Ni2 N12 90.0(2) . 2_856 ? N10 Ni2 Cl3 89.33(17) . . ? N3 Ni2 Cl3 89.41(16) 1_655 . ? N9 Ni2 Cl3 92.36(16) . . ? N12 Ni2 Cl3 90.87(16) 2_856 . ? N10 Ni2 Cl4 88.02(17) . . ? N3 Ni2 Cl4 88.91(16) 1_655 . ? N9 Ni2 Cl4 89.27(16) . . ? N12 Ni2 Cl4 91.80(16) 2_856 . ? Cl3 Ni2 Cl4 176.87(7) . . ? C5 N1 C1 116.1(6) . . ? C5 N1 Ni1 119.4(4) . . ? C1 N1 Ni1 124.4(4) . . ? C10 N2 C6 117.3(5) . . ? C15 N3 C11 116.7(6) . . ? C15 N3 Ni2 123.2(5) . 1_455 ? C11 N3 Ni2 120.0(4) . 1_455 ? C2 C1 N1 123.7(6) . . ? C2 C1 H1A 118.2 . . ? N1 C1 H1A 118.2 . . ? C1 C2 C3 120.2(6) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 116.4(6) . . ? C4 C3 C6 120.3(6) . . ? C2 C3 C6 123.2(6) . . ? C5 C4 C3 120.2(6) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C5 C4 123.4(6) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? N2 C6 C7 122.7(6) . . ? N2 C6 C3 113.9(6) . . ? C7 C6 C3 123.3(6) . . ? C6 C7 C8 120.3(6) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 116.1(6) . . ? C9 C8 C16 123.7(7) . . ? C7 C8 C16 120.1(7) . . ? C8 C9 C10 120.6(7) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? N2 C10 C9 122.9(6) . . ? N2 C10 C13 114.4(6) . . ? C9 C10 C13 122.6(6) . . ? N3 C11 C12 123.7(6) . . ? N3 C11 H11A 118.1 . . ? C12 C11 H11A 118.1 . . ? C11 C12 C13 119.8(7) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 116.4(6) . . ? C14 C13 C10 123.3(6) . . ? C12 C13 C10 120.3(6) . . ? C15 C14 C13 119.9(6) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? N3 C15 C14 123.3(6) . . ? N3 C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? C18 C16 C17 108.1(12) . . ? C18 C16 C19 108.4(10) . . ? C17 C16 C19 110.8(11) . . ? C18 C16 C8 110.8(8) . . ? C17 C16 C8 107.9(8) . . ? C19 C16 C8 110.7(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C24 N4 C20 116.5(6) . . ? C24 N4 Ni1 122.7(4) . . ? C20 N4 Ni1 120.7(4) . . ? C25 N5 C29 116.6(6) . . ? C34 N6 C30 116.8(6) . . ? C34 N6 Ni1 123.0(5) . 2_746 ? C30 N6 Ni1 120.1(5) . 2_746 ? N4 C20 C21 123.2(6) . . ? N4 C20 H20A 118.4 . . ? C21 C20 H20A 118.4 . . ? C22 C21 C20 119.4(6) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C23 117.9(7) . . ? C21 C22 C25 119.7(7) . . ? C23 C22 C25 122.3(7) . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? N4 C24 C23 123.9(6) . . ? N4 C24 H24A 118.0 . . ? C23 C24 H24A 118.0 . . ? N5 C25 C26 123.3(7) . . ? N5 C25 C22 114.6(6) . . ? C26 C25 C22 122.0(7) . . ? C27 C26 C25 119.8(7) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 117.8(7) . . ? C26 C27 C35 123.3(7) . . ? C28 C27 C35 118.7(7) . . ? C29 C28 C27 119.5(7) . . ? C29 C28 H28A 120.2 . . ? C27 C28 H28A 120.2 . . ? N5 C29 C28 122.9(7) . . ? N5 C29 C32 114.1(6) . . ? C28 C29 C32 123.0(7) . . ? N6 C30 C31 122.5(7) . . ? N6 C30 H30A 118.7 . . ? C31 C30 H30A 118.7 . . ? C32 C31 C30 121.0(7) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 C33 116.4(7) . . ? C31 C32 C29 121.4(7) . . ? C33 C32 C29 122.2(7) . . ? C32 C33 C34 119.3(7) . . ? C32 C33 H33A 120.3 . . ? C34 C33 H33A 120.3 . . ? N6 C34 C33 123.8(7) . . ? N6 C34 H34A 118.1 . . ? C33 C34 H34A 118.1 . . ? C37 C35 C38 109.6(9) . . ? C37 C35 C36 109.3(9) . . ? C38 C35 C36 110.4(7) . . ? C37 C35 C27 111.2(7) . . ? C38 C35 C27 109.1(7) . . ? C36 C35 C27 107.1(8) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C39 N7 C43 117.7(6) . . ? C39 N7 Ni1 120.6(4) . . ? C43 N7 Ni1 121.8(5) . . ? C44 N8 C48 116.9(6) . . ? C53 N9 C49 116.6(6) . . ? C53 N9 Ni2 123.2(5) . . ? C49 N9 Ni2 120.2(5) . . ? N7 C39 C40 123.3(6) . . ? N7 C39 H39A 118.4 . . ? C40 C39 H39A 118.4 . . ? C39 C40 C41 119.8(7) . . ? C39 C40 H40A 120.1 . . ? C41 C40 H40A 120.1 . . ? C40 C41 C42 116.9(6) . . ? C40 C41 C44 121.9(6) . . ? C42 C41 C44 121.1(6) . . ? C43 C42 C41 119.3(7) . . ? C43 C42 H42A 120.3 . . ? C41 C42 H42A 120.3 . . ? N7 C43 C42 123.0(7) . . ? N7 C43 H43A 118.5 . . ? C42 C43 H43A 118.5 . . ? N8 C44 C45 123.5(6) . . ? N8 C44 C41 114.2(6) . . ? C45 C44 C41 122.1(6) . . ? C44 C45 C46 119.6(7) . . ? C44 C45 H45A 120.2 . . ? C46 C45 H45A 120.2 . . ? C47 C46 C45 116.4(6) . . ? C47 C46 C54 121.6(7) . . ? C45 C46 C54 121.9(7) . . ? C48 C47 C46 120.4(7) . . ? C48 C47 H47A 119.8 . . ? C46 C47 H47A 119.8 . . ? N8 C48 C47 123.1(6) . . ? N8 C48 C51 114.7(6) . . ? C47 C48 C51 122.1(6) . . ? N9 C49 C50 123.4(6) . . ? N9 C49 H49A 118.3 . . ? C50 C49 H49A 118.3 . . ? C49 C50 C51 119.9(7) . . ? C49 C50 H50A 120.1 . . ? C51 C50 H50A 120.1 . . ? C52 C51 C50 116.6(6) . . ? C52 C51 C48 121.9(6) . . ? C50 C51 C48 121.4(6) . . ? C53 C52 C51 119.7(7) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? N9 C53 C52 123.6(7) . . ? N9 C53 H53A 118.2 . . ? C52 C53 H53A 118.2 . . ? C56 C54 C55 113.4(9) . . ? C56 C54 C46 108.9(7) . . ? C55 C54 C46 110.8(7) . . ? C56 C54 C57 108.4(8) . . ? C55 C54 C57 106.2(8) . . ? C46 C54 C57 109.0(7) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C58 N10 C62 116.8(6) . . ? C58 N10 Ni2 121.1(5) . . ? C62 N10 Ni2 121.9(5) . . ? C67 N11 C63 117.7(7) . . ? C68 N12 C72 115.3(6) . . ? C68 N12 Ni2 124.5(5) . 2_846 ? C72 N12 Ni2 120.2(5) . 2_846 ? N10 C58 C59 122.9(7) . . ? N10 C58 H58A 118.5 . . ? C59 C58 H58A 118.5 . . ? C60 C59 C58 120.5(7) . . ? C60 C59 H59A 119.8 . . ? C58 C59 H59A 119.8 . . ? C59 C60 C61 116.6(7) . . ? C59 C60 C63 121.0(7) . . ? C61 C60 C63 122.4(7) . . ? C62 C61 C60 119.8(6) . . ? C62 C61 H61A 120.1 . . ? C60 C61 H61A 120.1 . . ? N10 C62 C61 123.4(6) . . ? N10 C62 H62A 118.3 . . ? C61 C62 H62A 118.3 . . ? N11 C63 C64 122.4(7) . . ? N11 C63 C60 114.6(7) . . ? C64 C63 C60 123.0(7) . . ? C63 C64 C65 120.5(7) . . ? C63 C64 H64A 119.8 . . ? C65 C64 H64A 119.8 . . ? C66 C65 C64 116.6(8) . . ? C66 C65 C73 123.3(7) . . ? C64 C65 C73 120.1(7) . . ? C65 C66 C67 120.5(7) . . ? C65 C66 H66A 119.8 . . ? C67 C66 H66A 119.8 . . ? N11 C67 C66 122.4(7) . . ? N11 C67 C70 115.6(6) . . ? C66 C67 C70 122.1(7) . . ? N12 C68 C69 124.5(7) . . ? N12 C68 H68A 117.8 . . ? C69 C68 H68A 117.8 . . ? C70 C69 C68 119.7(8) . . ? C70 C69 H69A 120.2 . . ? C68 C69 H69A 120.2 . . ? C71 C70 C69 116.0(7) . . ? C71 C70 C67 119.1(7) . . ? C69 C70 C67 124.8(7) . . ? C72 C71 C70 121.6(7) . . ? C72 C71 H71A 119.2 . . ? C70 C71 H71A 119.2 . . ? N12 C72 C71 122.8(7) . . ? N12 C72 H72A 118.6 . . ? C71 C72 H72A 118.6 . . ? C76 C73 C65 111.3(8) . . ? C76 C73 C75 110.0(11) . . ? C65 C73 C75 107.9(10) . . ? C76 C73 C74 110.1(12) . . ? C65 C73 C74 110.1(8) . . ? C75 C73 C74 107.3(9) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C101 C100 C105 119.4(11) . . ? C101 C100 Cl10 121.2(11) . . ? C105 C100 Cl10 119.3(9) . . ? C102 C101 C100 123.0(15) . . ? C102 C101 Cl11 117.2(12) . . ? C100 C101 Cl11 119.8(10) . . ? C101 C102 C103 119.4(15) . . ? C101 C102 H10D 120.3 . . ? C103 C102 H10D 120.3 . . ? C102 C103 C104 122.1(13) . . ? C102 C103 H10A 119.0 . . ? C104 C103 H10A 119.0 . . ? C103 C104 C105 117.4(15) . . ? C103 C104 H10B 121.3 . . ? C105 C104 H10B 121.3 . . ? C100 C105 C104 118.5(13) . . ? C100 C105 H10C 120.7 . . ? C104 C105 H10C 120.7 . . ? C205 C200 C201 120.0 . . ? C205 C200 Cl20 115.3(2) . . ? C201 C200 Cl20 124.6(2) . . ? C202 C201 C200 120.0 . . ? C202 C201 Cl21 126.2 . . ? C200 C201 Cl21 113.8 . . ? C203 C202 C201 120.0 . . ? C203 C202 H20B 120.0 . . ? C201 C202 H20B 120.0 . . ? C204 C203 C202 120.0 . . ? C204 C203 H20C 120.0 . . ? C202 C203 H20C 120.0 . . ? C203 C204 C205 120.0 . . ? C203 C204 H20D 120.0 . . ? C205 C204 H20D 120.0 . . ? C200 C205 C204 119.9 . . ? C200 C205 H20E 120.0 . . ? C204 C205 H20E 120.0 . . ? C301 C300 C305 99(3) . . ? C301 C300 Cl30 132(3) . . ? C305 C300 Cl30 127(2) . . ? C302 C301 C300 129(3) . . ? C302 C301 Cl31 125(3) . . ? C300 C301 Cl31 106(3) . . ? C301 C302 C303 128(3) . . ? C301 C302 H30B 116.2 . . ? C303 C302 H30B 116.2 . . ? C304 C303 C302 112(3) . . ? C304 C303 H30C 124.2 . . ? C302 C303 H30C 124.2 . . ? C305 C304 C303 110(3) . . ? C305 C304 H30D 124.9 . . ? C303 C304 H30D 124.9 . . ? C304 C305 C300 143(4) . . ? C304 C305 H30E 108.7 . . ? C300 C305 H30E 108.7 . . ? C405 C400 C401 120.0 . . ? C405 C400 Cl40 112.4(4) . . ? C401 C400 Cl40 127.1(4) . . ? Cl41 C401 C400 126.4 . . ? Cl41 C401 C402 113.4 . . ? C400 C401 C402 120.0 . . ? C403 C402 C401 120.0 . . ? C403 C402 H40B 120.0 . . ? C401 C402 H40B 120.0 . . ? C404 C403 C402 120.04(7) . . ? C404 C403 H40C 120.0 . . ? C402 C403 H40C 120.0 . . ? C403 C404 C405 120.0 . . ? C403 C404 H40D 120.0 . . ? C405 C404 H40D 120.0 . . ? C400 C405 C404 120.0 . . ? C400 C405 H40E 120.0 . . ? C404 C405 H40E 120.0 . . ? C501 C500 C505 119.55(18) . . ? C501 C500 Cl50 135.15(9) . . ? C505 C500 Cl50 104.5 . . ? C502 C501 C500 119.61(11) . . ? C502 C501 Cl51 137.9(4) . . ? C500 C501 Cl51 99.31(12) . . ? C501 C502 C503 119.5(3) . . ? C501 C502 H50B 120.2 . . ? C503 C502 H50B 120.2 . . ? C504 C503 C502 120.7 . . ? C504 C503 H50C 119.6 . . ? C502 C503 H50C 119.6 . . ? C503 C504 C505 120.0 . . ? C503 C504 H50D 120.0 . . ? C505 C504 H50D 120.0 . . ? C504 C505 C500 120.5 . . ? C504 C505 H50E 119.8 . . ? C500 C505 H50E 119.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.926 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.103 # start Validation Reply Form _vrf_PLAT306_I ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O101 RESPONSE: Data quality did not allow location of hydrogen atoms from the difference map ; _vrf_PLAT430_I ; PROBLEM: Short Inter D...A Contact O100 .. O101 .. 2.34 Ang. RESPONSE: Disordered solvent that could not be identified was modelled as water molecules ; # Attachment 'SQUEEZE_265_revised.CIF' data_ry_2 _database_code_depnum_ccdc_archive 'CCDC 841382' #TrackingRef 'SQUEEZE_265_revised.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C38 H38 Cl2 N6 Ni), C60' _chemical_formula_sum 'C174 H114 Cl6 N18 Ni3' _chemical_formula_weight 2845.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Rhombohedral _symmetry_space_group_name_H-M R-3m _symmetry_space_group_name_Hall -R32" loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 25.712(5) _cell_length_b 25.712(5) _cell_length_c 36.372(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20825(6) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6393 _cell_measurement_theta_min 4.18 _cell_measurement_theta_max 41.21 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4410 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8925 _exptl_absorpt_correction_T_max 0.9576 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; The C60 fullerene is disordered, and is modelled as best as possible considering it is really just a spherical ball of electron density. The ellipsoids of one atom was restrained in modelling this disorder with the command: isor 0.03 c111 SQUEEZE was used as the solvent in the large voids is too disordered to locate from the difference map. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 145225 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4389 _reflns_number_gt 4217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0961P)^2^+18.0572P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4389 _refine_ls_number_parameters 245 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1807 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.161 _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 0.1667 0.3333 0.3333 0.0640(2) Uani 1 4 d S . . Cl1 Cl 0.20313(2) 0.40626(4) 0.38398(2) 0.0675(3) Uani 1 2 d S . . N1 N 0.08254(10) 0.28279(10) 0.36014(5) 0.0656(5) Uani 1 1 d . . . C1A C 0.0559(2) 0.2238(2) 0.35835(12) 0.0630(12) Uani 0.50 1 d P A 1 H1AA H 0.0751 0.2051 0.3465 0.076 Uiso 0.50 1 calc PR A 1 C2A C -0.0003(2) 0.1895(2) 0.37385(12) 0.0611(11) Uani 0.50 1 d P A 1 H2AA H -0.0206 0.1471 0.3709 0.073 Uiso 0.50 1 calc PR A 1 C1B C 0.0276(3) 0.2510(3) 0.34151(14) 0.092(2) Uani 0.50 1 d P A 2 H1BA H 0.0289 0.2545 0.3155 0.110 Uiso 0.50 1 calc PR A 2 C2B C -0.0284(3) 0.2149(3) 0.35725(14) 0.0868(18) Uani 0.50 1 d P A 2 H2BA H -0.0635 0.1913 0.3430 0.104 Uiso 0.50 1 calc PR A 2 C3 C -0.02920(11) 0.21586(11) 0.39438(6) 0.0590(6) Uani 1 1 d . . . C4A C 0.0073(2) 0.2791(2) 0.39631(13) 0.0633(11) Uani 0.50 1 d P A 1 H4AA H -0.0068 0.3010 0.4100 0.076 Uiso 0.50 1 calc PR A 1 C5A C 0.0627(2) 0.3103(2) 0.37922(14) 0.0645(12) Uani 0.50 1 d P A 1 H5AA H 0.0861 0.3527 0.3818 0.077 Uiso 0.50 1 calc PR A 1 C4B C 0.0187(2) 0.2483(2) 0.41480(12) 0.0639(12) Uani 0.50 1 d P A 2 H4BA H 0.0163 0.2489 0.4409 0.077 Uiso 0.50 1 calc PR A 2 C5B C 0.0726(2) 0.2815(2) 0.39647(12) 0.0648(12) Uani 0.50 1 d P A 2 H5BA H 0.1065 0.3063 0.4113 0.078 Uiso 0.50 1 calc PR A 2 N2 N -0.12495(6) 0.12495(6) 0.39599(7) 0.0593(7) Uani 1 2 d S . . C6 C -0.08863(11) 0.17804(10) 0.41234(6) 0.0567(5) Uani 1 1 d . A . C7 C -0.10436(12) 0.19578(11) 0.44479(6) 0.0615(6) Uani 1 1 d . . . H7A H -0.0773 0.2336 0.4554 0.074 Uiso 1 1 calc R A . C8 C -0.15886(7) 0.15886(7) 0.46157(9) 0.0608(8) Uani 1 2 d S A . C9 C -0.17712(9) 0.17712(9) 0.49740(11) 0.0766(10) Uani 1 2 d S . . C10 C -0.1331(3) 0.2319(3) 0.51310(18) 0.0865(17) Uani 0.50 1 d P A . H10A H -0.1497 0.2407 0.5349 0.130 Uiso 0.50 1 calc PR . . H10B H -0.1210 0.2643 0.4951 0.130 Uiso 0.50 1 calc PR . . H10C H -0.0981 0.2287 0.5202 0.130 Uiso 0.50 1 calc PR . . C11 C -0.1987(3) 0.1221(3) 0.52578(17) 0.0909(19) Uani 0.50 1 d P A . H11A H -0.1657 0.1141 0.5301 0.136 Uiso 0.50 1 calc PR . . H11B H -0.2331 0.0862 0.5154 0.136 Uiso 0.50 1 calc PR . . H11C H -0.2104 0.1325 0.5491 0.136 Uiso 0.50 1 calc PR . . C12 C -0.2382(3) 0.1768(4) 0.4893(2) 0.116(3) Uani 0.50 1 d P A . H12A H -0.2528 0.1855 0.5120 0.174 Uiso 0.50 1 calc PR . . H12B H -0.2682 0.1372 0.4800 0.174 Uiso 0.50 1 calc PR . . H12C H -0.2310 0.2074 0.4708 0.174 Uiso 0.50 1 calc PR . . C101 C 0.0000 0.0000 0.5963(2) 0.099(3) Uani 0.90 6 d SP . . C102 C -0.1071(5) -0.0535(3) 0.5700(3) 0.175(5) Uani 1 2 d S . . C103 C -0.0529(3) 0.0529(3) 0.5718(3) 0.166(4) Uani 1 2 d S . . C104 C -0.1139(6) 0.0236(8) 0.5334(3) 0.219(6) Uani 0.95 1 d P . . C105 C -0.0688(2) 0.0688(2) 0.5488(3) 0.160(11) Uani 0.50 2 d SP . . C106 C -0.0558(6) 0.0008(7) 0.58655(19) 0.217(6) Uani 0.80 1 d P . . C107 C -0.1365(3) -0.0342(9) 0.5389(5) 0.189(8) Uani 0.59 1 d P . . C108 C -0.1549(3) -0.07744(14) 0.5164(3) 0.215(7) Uani 1 2 d S . . C109 C -0.0986(6) 0.0557(7) 0.5076(5) 0.110(6) Uani 0.35 1 d P . . C110 C -0.1048(9) -0.0013(12) 0.5618(5) 0.095(5) Uani 0.26 1 d P . . C111 C -0.1347(6) 0.0000 0.5000 0.161(11) Uani 0.30 2 d SPU . . 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 0.0772(4) 0.0705(4) 0.0421(3) 0.0193(3) 0.00964(13) 0.0352(2) Cl1 0.0832(5) 0.0684(5) 0.0460(4) 0.0149(3) 0.00746(17) 0.0342(3) N1 0.0802(14) 0.0694(13) 0.0458(10) 0.0174(9) 0.0102(10) 0.0363(11) C1A 0.077(3) 0.071(3) 0.047(2) 0.017(2) 0.014(2) 0.041(3) C2A 0.080(3) 0.063(3) 0.047(2) 0.019(2) 0.020(2) 0.041(2) C1B 0.072(3) 0.144(6) 0.040(2) 0.013(3) -0.002(2) 0.039(4) C2B 0.071(3) 0.133(5) 0.046(2) 0.004(3) 0.003(2) 0.044(4) C3 0.0726(15) 0.0660(14) 0.0427(11) 0.0093(10) 0.0024(10) 0.0380(12) C4A 0.067(3) 0.062(3) 0.063(3) 0.005(2) 0.011(2) 0.034(2) C5A 0.079(3) 0.055(3) 0.060(3) 0.011(2) 0.013(2) 0.034(2) C4B 0.079(3) 0.065(3) 0.042(2) 0.007(2) 0.009(2) 0.032(3) C5B 0.081(3) 0.067(3) 0.038(2) 0.011(2) 0.003(2) 0.030(3) N2 0.0689(12) 0.0689(12) 0.0440(13) 0.0020(6) -0.0020(6) 0.0375(14) C6 0.0680(14) 0.0640(13) 0.0449(11) 0.0051(10) -0.0017(10) 0.0381(11) C7 0.0708(15) 0.0693(14) 0.0505(12) -0.0034(10) -0.0009(11) 0.0396(12) C8 0.0690(16) 0.0690(16) 0.0556(18) -0.0022(7) 0.0022(7) 0.0427(18) C9 0.090(2) 0.090(2) 0.065(2) -0.0098(9) 0.0098(9) 0.056(2) C10 0.100(5) 0.090(4) 0.070(4) -0.016(3) 0.002(3) 0.048(4) C11 0.104(5) 0.100(5) 0.062(3) -0.007(3) 0.028(3) 0.046(4) C12 0.098(5) 0.160(7) 0.118(6) -0.039(5) -0.001(4) 0.087(5) C101 0.123(5) 0.123(5) 0.051(4) 0.000 0.000 0.062(2) C102 0.099(7) 0.263(16) 0.110(7) 0.034(3) 0.068(6) 0.050(3) C103 0.240(12) 0.240(12) 0.092(6) -0.035(3) 0.035(3) 0.175(14) C104 0.194(11) 0.42(2) 0.166(11) -0.105(14) -0.019(9) 0.249(14) C105 0.31(3) 0.31(3) 0.037(5) -0.005(2) 0.005(2) 0.29(3) C106 0.292(15) 0.309(16) 0.093(4) 0.023(6) 0.104(6) 0.183(15) C107 0.044(3) 0.268(16) 0.200(13) -0.136(14) 0.018(5) 0.038(6) C108 0.051(3) 0.382(18) 0.101(6) 0.005(2) 0.010(4) 0.0255(17) C109 0.127(11) 0.167(14) 0.107(10) 0.051(9) 0.048(8) 0.128(12) C110 0.112(13) 0.140(14) 0.071(8) 0.002(12) 0.030(9) 0.092(13) C111 0.074(7) 0.23(2) 0.23(3) -0.04(2) -0.021(11) 0.115(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 N1 2.123(2) 17 ? Ni1 N1 2.123(2) 23 ? Ni1 N1 2.123(2) . ? Ni1 N1 2.123(2) 31 ? Ni1 Cl1 2.4558(9) . ? Ni1 Cl1 2.4559(9) 31 ? N1 C5A 1.266(5) . ? N1 C1A 1.316(5) . ? N1 C5B 1.343(5) . ? N1 C1B 1.403(6) . ? C1A C2A 1.382(7) . ? C1A H1AA 0.9500 . ? C2A C3 1.439(5) . ? C2A H2AA 0.9500 . ? C1B C2B 1.388(8) . ? C1B H1BA 0.9500 . ? C2B C3 1.351(5) . ? C2B H2BA 0.9500 . ? C3 C4B 1.318(6) . ? C3 C4A 1.415(6) . ? C3 C6 1.490(3) . ? C4A C5A 1.384(7) . ? C4A H4AA 0.9500 . ? C5A H5AA 0.9500 . ? C4B C5B 1.382(7) . ? C4B H4BA 0.9500 . ? C5B H5BA 0.9500 . ? N2 C6 1.347(3) . ? N2 C6 1.347(3) 22 ? C6 C7 1.396(3) . ? C7 C8 1.381(3) . ? C7 H7A 0.9500 . ? C8 C7 1.381(3) 22 ? C8 C9 1.536(5) . ? C9 C10 1.413(7) . ? C9 C10 1.413(7) 22 ? C9 C12 1.593(8) . ? C9 C12 1.593(8) 22 ? C9 C11 1.609(8) 22 ? C9 C11 1.609(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C101 C106 1.488(11) 23 ? C101 C106 1.488(11) 2 ? C101 C106 1.488(11) 24 ? C101 C106 1.488(11) 3 ? C101 C106 1.488(11) . ? C101 C106 1.488(11) 22 ? C102 C110 1.35(2) 24 ? C102 C110 1.35(2) . ? C102 C106 1.487(13) 24 ? C102 C106 1.487(14) . ? C102 C107 1.57(2) 24 ? C102 C107 1.57(2) . ? C103 C105 1.094(16) . ? C103 C106 1.411(12) 22 ? C103 C106 1.411(12) . ? C103 C110 1.41(3) . ? C103 C110 1.41(3) 22 ? C103 C104 1.946(14) . ? C103 C104 1.946(14) 22 ? C104 C109 1.182(17) . ? C104 C105 1.290(16) . ? C104 C110 1.29(2) . ? C104 C107 1.31(2) . ? C104 C111 1.344(12) . ? C104 C109 1.99(2) 22 ? C105 C104 1.290(16) 22 ? C105 C110 1.63(3) 22 ? C105 C110 1.63(3) . ? C105 C109 1.64(2) . ? C105 C109 1.64(2) 22 ? C106 C106 1.41(3) 22 ? C106 C106 1.48(3) 24 ? C106 C110 1.53(2) . ? C107 C110 1.18(3) . ? C107 C108 1.267(12) . ? C107 C111 1.65(3) . ? C107 C107 1.75(4) 24 ? C107 C109 1.77(3) 5_556 ? C108 C109 1.031(11) 21_556 ? C108 C109 1.031(11) 5_556 ? C108 C107 1.267(12) 24 ? C108 C111 1.885(5) 21_556 ? C108 C111 1.885(5) . ? C109 C108 1.031(11) 20_556 ? C109 C109 1.10(3) 22 ? C109 C111 1.288(19) . ? C109 C107 1.77(3) 5_556 ? C109 C104 1.99(2) 22 ? C111 C109 1.288(19) 5_556 ? C111 C104 1.344(12) 5_556 ? C111 C107 1.65(3) 5_556 ? C111 C108 1.885(5) 20_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.0 17 23 ? N1 Ni1 N1 89.08(11) 17 . ? N1 Ni1 N1 90.93(11) 23 . ? N1 Ni1 N1 90.93(11) 17 31 ? N1 Ni1 N1 89.07(11) 23 31 ? N1 Ni1 N1 180.0 . 31 ? N1 Ni1 Cl1 89.66(6) 17 . ? N1 Ni1 Cl1 90.35(6) 23 . ? N1 Ni1 Cl1 90.35(6) . . ? N1 Ni1 Cl1 89.66(6) 31 . ? N1 Ni1 Cl1 90.35(6) 17 31 ? N1 Ni1 Cl1 89.65(6) 23 31 ? N1 Ni1 Cl1 89.66(6) . 31 ? N1 Ni1 Cl1 90.34(6) 31 31 ? Cl1 Ni1 Cl1 180.0 . 31 ? C5A N1 C1A 123.2(3) . . ? C5A N1 C5B 49.4(3) . . ? C1A N1 C5B 92.1(3) . . ? C5A N1 C1B 91.2(4) . . ? C1A N1 C1B 60.8(4) . . ? C5B N1 C1B 109.7(4) . . ? C5A N1 Ni1 118.7(3) . . ? C1A N1 Ni1 117.8(2) . . ? C5B N1 Ni1 126.2(3) . . ? C1B N1 Ni1 123.8(2) . . ? N1 C1A C2A 119.5(4) . . ? N1 C1A H1AA 120.3 . . ? C2A C1A H1AA 120.3 . . ? C1A C2A C3 122.1(4) . . ? C1A C2A H2AA 119.0 . . ? C3 C2A H2AA 119.0 . . ? C2B C1B N1 126.6(4) . . ? C2B C1B H1BA 116.7 . . ? N1 C1B H1BA 116.7 . . ? C3 C2B C1B 114.8(5) . . ? C3 C2B H2BA 122.6 . . ? C1B C2B H2BA 122.6 . . ? C4B C3 C2B 123.9(4) . . ? C4B C3 C4A 51.0(3) . . ? C2B C3 C4A 93.6(4) . . ? C4B C3 C2A 93.0(3) . . ? C2B C3 C2A 57.1(4) . . ? C4A C3 C2A 111.3(3) . . ? C4B C3 C6 119.7(3) . . ? C2B C3 C6 116.5(3) . . ? C4A C3 C6 127.1(3) . . ? C2A C3 C6 121.5(3) . . ? C5A C4A C3 123.0(4) . . ? C5A C4A H4AA 118.5 . . ? C3 C4A H4AA 118.5 . . ? N1 C5A C4A 120.4(4) . . ? N1 C5A H5AA 119.8 . . ? C4A C5A H5AA 119.8 . . ? C3 C4B C5B 116.7(4) . . ? C3 C4B H4BA 121.6 . . ? C5B C4B H4BA 121.6 . . ? N1 C5B C4B 127.5(5) . . ? N1 C5B H5BA 116.2 . . ? C4B C5B H5BA 116.2 . . ? C6 N2 C6 117.2(3) . 22 ? N2 C6 C7 122.5(2) . . ? N2 C6 C3 115.7(2) . . ? C7 C6 C3 121.8(2) . . ? C8 C7 C6 120.6(2) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C7 116.7(3) 22 . ? C7 C8 C9 121.67(15) 22 . ? C7 C8 C9 121.67(15) . . ? C10 C9 C10 128.0(6) . 22 ? C10 C9 C8 115.7(3) . . ? C10 C9 C8 115.7(3) 22 . ? C10 C9 C12 112.1(5) . . ? C10 C9 C12 59.0(4) 22 . ? C8 C9 C12 106.9(4) . . ? C10 C9 C12 59.0(4) . 22 ? C10 C9 C12 112.1(5) 22 22 ? C8 C9 C12 106.9(4) . 22 ? C12 C9 C12 59.4(7) . 22 ? C10 C9 C11 111.7(5) 22 22 ? C8 C9 C11 107.4(3) . 22 ? C12 C9 C11 144.6(4) . 22 ? C12 C9 C11 102.0(5) 22 22 ? C10 C9 C11 111.7(5) . . ? C8 C9 C11 107.4(3) . . ? C12 C9 C11 102.0(5) . . ? C12 C9 C11 144.6(4) 22 . ? C11 C9 C11 75.4(6) 22 . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C106 C101 C106 59.5(12) 23 2 ? C106 C101 C106 114.5(3) 23 24 ? C106 C101 C106 56.8(12) 2 24 ? C106 C101 C106 56.8(12) 23 3 ? C106 C101 C106 114.5(3) 2 3 ? C106 C101 C106 152.5(8) 24 3 ? C106 C101 C106 152.5(8) 23 . ? C106 C101 C106 114.5(3) 2 . ? C106 C101 C106 59.5(12) 24 . ? C106 C101 C106 114.5(3) 3 . ? C106 C101 C106 114.5(3) 23 22 ? C106 C101 C106 152.5(8) 2 22 ? C106 C101 C106 114.5(3) 24 22 ? C106 C101 C106 59.5(12) 3 22 ? C106 C101 C106 56.8(12) . 22 ? C110 C102 C110 154.1(17) 24 . ? C110 C102 C106 65.0(11) 24 24 ? C110 C102 C106 123.0(17) . 24 ? C110 C102 C106 123.0(17) 24 . ? C110 C102 C106 65.0(11) . . ? C106 C102 C106 59.5(12) 24 . ? C110 C102 C107 46.7(11) 24 24 ? C110 C102 C107 113.5(17) . 24 ? C106 C102 C107 109.6(7) 24 24 ? C106 C102 C107 152.6(6) . 24 ? C110 C102 C107 113.5(17) 24 . ? C110 C102 C107 46.7(11) . . ? C106 C102 C107 152.6(6) 24 . ? C106 C102 C107 109.6(7) . . ? C107 C102 C107 67.7(13) 24 . ? C105 C103 C106 142.6(8) . 22 ? C105 C103 C106 142.6(8) . . ? C106 C103 C106 60.2(14) 22 . ? C105 C103 C110 80.1(11) . . ? C106 C103 C110 123.6(14) 22 . ? C106 C103 C110 65.5(9) . . ? C105 C103 C110 80.1(11) . 22 ? C106 C103 C110 65.5(9) 22 22 ? C106 C103 C110 123.6(14) . 22 ? C110 C103 C110 149.8(16) . 22 ? C106 C103 C104 148.6(5) 22 . ? C106 C103 C104 104.8(8) . . ? C110 C103 C104 113.9(13) 22 . ? C106 C103 C104 104.8(8) 22 22 ? C106 C103 C104 148.6(5) . 22 ? C110 C103 C104 113.9(13) . 22 ? C104 C103 C104 73.3(12) . 22 ? C109 C104 C105 83(2) . . ? C109 C104 C110 154.1(17) . . ? C105 C104 C110 78.3(13) . . ? C109 C104 C107 135.7(19) . . ? C105 C104 C107 130.2(16) . . ? C110 C104 C107 53.6(16) . . ? C109 C104 C111 60.9(11) . . ? C105 C104 C111 140.8(15) . . ? C110 C104 C111 128.8(18) . . ? C107 C104 C111 77.0(13) . . ? C109 C104 C103 112.1(18) . . ? C110 C104 C103 46.5(13) . . ? C107 C104 C103 98.3(12) . . ? C111 C104 C103 152.1(8) . . ? C105 C104 C109 55.2(11) . 22 ? C110 C104 C109 128.4(15) . 22 ? C107 C104 C109 149.5(7) . 22 ? C111 C104 C109 86.9(7) . 22 ? C103 C104 C109 83.9(9) . 22 ? C103 C105 C104 109.2(9) . . ? C103 C105 C104 109.2(9) . 22 ? C104 C105 C104 128.4(16) . 22 ? C103 C105 C110 58.5(9) . 22 ? C104 C105 C110 151.2(9) . 22 ? C104 C105 C110 51.0(9) 22 22 ? C103 C105 C110 58.5(9) . . ? C104 C105 C110 51.0(9) . . ? C104 C105 C110 151.2(9) 22 . ? C110 C105 C110 113.5(17) 22 . ? C103 C105 C109 147.4(8) . . ? C104 C105 C109 45.6(10) . . ? C104 C105 C109 84.6(10) 22 . ? C110 C105 C109 130.5(9) 22 . ? C110 C105 C109 95.0(10) . . ? C103 C105 C109 147.4(8) . 22 ? C104 C105 C109 84.6(10) . 22 ? C104 C105 C109 45.6(10) 22 22 ? C110 C105 C109 95.0(10) 22 22 ? C110 C105 C109 130.5(9) . 22 ? C103 C106 C106 59.9(7) . 22 ? C103 C106 C106 157.4(5) . 24 ? C106 C106 C106 120.000(6) 22 24 ? C103 C106 C102 109.8(7) . . ? C106 C106 C102 155.9(5) 22 . ? C106 C106 C102 60.3(6) 24 . ? C103 C106 C101 120.7(12) . . ? C106 C106 C101 61.6(6) 22 . ? C106 C106 C101 60.3(6) 24 . ? C102 C106 C101 119.4(10) . . ? C103 C106 C110 57.3(11) . . ? C106 C106 C110 115.4(14) 22 . ? C106 C106 C110 112.2(13) 24 . ? C102 C106 C110 53.1(11) . . ? C101 C106 C110 157.4(7) . . ? C110 C107 C108 155(2) . . ? C110 C107 C104 62.4(15) . . ? C108 C107 C104 131(2) . . ? C110 C107 C102 56.6(16) . . ? C108 C107 C102 102.3(18) . . ? C104 C107 C102 117.2(10) . . ? C110 C107 C111 113(2) . . ? C108 C107 C111 79.2(11) . . ? C104 C107 C111 52.4(13) . . ? C102 C107 C111 153.2(8) . . ? C110 C107 C107 111.9(19) . 24 ? C108 C107 C107 46.3(13) . 24 ? C104 C107 C107 155.7(6) . 24 ? C102 C107 C107 56.2(7) . 24 ? C111 C107 C107 121.1(6) . 24 ? C110 C107 C109 151.7(18) . 5_556 ? C104 C107 C109 96.2(17) . 5_556 ? C102 C107 C109 132.8(13) . 5_556 ? C107 C107 C109 79.4(9) 24 5_556 ? C109 C108 C109 65(2) 21_556 5_556 ? C109 C108 C107 99.9(18) 21_556 24 ? C109 C108 C107 155.7(11) 5_556 24 ? C109 C108 C107 155.7(12) 21_556 . ? C109 C108 C107 99.9(18) 5_556 . ? C107 C108 C107 87(3) 24 . ? C109 C108 C111 102.8(11) 5_556 21_556 ? C107 C108 C111 59.5(12) 24 21_556 ? C107 C108 C111 139.6(12) . 21_556 ? C109 C108 C111 102.8(11) 21_556 . ? C107 C108 C111 139.6(12) 24 . ? C107 C108 C111 59.5(12) . . ? C111 C108 C111 133.3(8) 21_556 . ? C108 C109 C109 57.7(11) 20_556 22 ? C108 C109 C104 162.3(12) 20_556 . ? C109 C109 C104 121.1(14) 22 . ? C108 C109 C111 108.3(17) 20_556 . ? C109 C109 C111 156.3(8) 22 . ? C104 C109 C111 65.8(11) . . ? C108 C109 C105 126.6(14) 20_556 . ? C109 C109 C105 70.4(5) 22 . ? C104 C109 C105 51.2(13) . . ? C111 C109 C105 115.3(9) . . ? C108 C109 C107 45.0(12) 20_556 5_556 ? C109 C109 C107 100.6(9) 22 5_556 ? C104 C109 C107 126.6(16) . 5_556 ? C111 C109 C107 63.3(10) . 5_556 ? C105 C109 C107 152.4(8) . 5_556 ? C108 C109 C104 86.6(11) 20_556 22 ? C104 C109 C104 90.5(18) . 22 ? C111 C109 C104 145.7(10) . 22 ? C107 C109 C104 124.6(13) 5_556 22 ? C107 C110 C104 63.9(17) . . ? C107 C110 C102 77(2) . . ? C104 C110 C102 138(2) . . ? C107 C110 C103 150(2) . . ? C104 C110 C103 92(2) . . ? C102 C110 C103 118.4(17) . . ? C107 C110 C106 135(2) . . ? C104 C110 C106 143(2) . . ? C102 C110 C106 61.9(11) . . ? C103 C110 C106 57.2(11) . . ? C107 C110 C105 113(2) . . ? C104 C110 C105 50.7(12) . . ? C102 C110 C105 152.1(14) . . ? C106 C110 C105 97.5(18) . . ? C109 C111 C109 161.1(17) 5_556 . ? C109 C111 C104 53.3(8) 5_556 5_556 ? C109 C111 C104 122.8(8) . 5_556 ? C109 C111 C104 122.8(8) 5_556 . ? C109 C111 C104 53.3(8) . . ? C104 C111 C104 160.3(14) 5_556 . ? C109 C111 C107 102.8(9) 5_556 5_556 ? C109 C111 C107 72.6(8) . 5_556 ? C104 C111 C107 50.6(7) 5_556 5_556 ? C104 C111 C107 123.6(8) . 5_556 ? C109 C111 C107 72.6(8) 5_556 . ? C109 C111 C107 102.8(9) . . ? C104 C111 C107 123.6(8) 5_556 . ? C104 C111 C107 50.6(7) . . ? C107 C111 C107 152.6(13) 5_556 . ? C109 C111 C108 140.5(9) 5_556 20_556 ? C104 C111 C108 91.6(8) 5_556 20_556 ? C104 C111 C108 83.4(8) . 20_556 ? C107 C111 C108 129.2(6) . 20_556 ? C109 C111 C108 140.5(9) . . ? C104 C111 C108 83.4(8) 5_556 . ? C104 C111 C108 91.6(8) . . ? C107 C111 C108 129.2(6) 5_556 . ? C108 C111 C108 150.8(10) 20_556 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.279 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.046 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.017 -0.011 -0.002 11569 1995 ' ' 2 0.000 0.000 0.500 22 9 ' ' 3 0.333 0.667 0.167 20 8 ' ' 4 0.667 0.333 0.833 20 8 ' ' _platon_squeeze_details ; Before applying SQUEEZE, the solvent voids were so large that little solvent could be located. Electron density peaks that could be located were assigned as disordered water molecules as individual solvent molecules could not be identified. The details from the original unsqueezed version which differ from this squeezed version are given here: _chemical_formula_moiety '3(C38 H38 Cl2 N6 Ni), C60, 27(H2 O)' _chemical_formula_sum 'C174 H168 Cl6 N18 Ni3 O27' _chemical_formula_weight 3332.14 _exptl_crystal_density_diffrn 0.784 _exptl_crystal_F_000 5058 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_T_min 0.8882 _exptl_absorpt_correction_T_max 0.9559 _diffrn_reflns_number 160201 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4403 _reflns_number_gt 4298 _refine_ls_number_reflns 4403 _refine_ls_number_parameters 308 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.1143 _refine_ls_wR_factor_ref 0.3381 _refine_ls_wR_factor_gt 0.3369 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.264 ;