# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1861 data_4 _publ_contact_author_name 'Makoto Fujita' _publ_contact_author_address ; Department of Applied Chemistry Graduate School of Engineering, Nagoya University Chikusaku, Nagoya 464-8603, Japan Tel +81-52-789-4668; Fax +81-52-789-3199 E-mail mfujita@apchem.nagoya-u.ac.jp ; _publ_requested_journal ; Chemical Communications ; _publ_section_title ; Selective formation of rectangular grid coordination polymers with grid dimensions 10x15, 10x20 and 15x20 A ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H56 N6 Ni O6' _chemical_formula_weight 1039.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.1225(19) _cell_length_b 11.3408(13) _cell_length_c 31.106(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.190(2) _cell_angle_gamma 90.00 _cell_volume 5514.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9228 _exptl_absorpt_correction_T_max 0.9603 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17529 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.97 _reflns_number_total 6477 _reflns_number_gt 4029 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+5.1985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6477 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1654 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.002 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 0.5000 0.52264(5) 0.7500 0.02320(16) Uani 1 2 d S . . N1 N 0.30236(18) 0.5240(3) 0.74579(10) 0.0435(7) Uani 1 1 d . . . O1 O 0.2943(2) 0.4633(3) 0.77511(12) 0.0908(12) Uani 1 1 d . . . O2 O 0.36453(13) 0.52025(19) 0.72808(6) 0.0318(5) Uani 1 1 d . . . O3 O 0.2556(4) 0.6012(7) 0.7375(3) 0.266(5) Uani 1 1 d . . . N11A N 0.50512(15) 0.5235(2) 0.81766(7) 0.0253(5) Uani 1 1 d . . . C11A C 0.4575(2) 0.5966(3) 0.83553(9) 0.0309(7) Uani 1 1 d . . . H11A H 0.4218 0.6518 0.8166 0.037 Uiso 1 1 calc R . . C12A C 0.4577(2) 0.5961(3) 0.87991(10) 0.0320(7) Uani 1 1 d . . . H12A H 0.4223 0.6495 0.8908 0.038 Uiso 1 1 calc R . . C13A C 0.5098(2) 0.5169(3) 0.90861(9) 0.0290(6) Uani 1 1 d . . . C14A C 0.5604(2) 0.4432(3) 0.89011(10) 0.0343(7) Uani 1 1 d . . . H14A H 0.5977 0.3883 0.9083 0.041 Uiso 1 1 calc R . . C15A C 0.5569(2) 0.4490(3) 0.84553(9) 0.0301(7) Uani 1 1 d . . . H15A H 0.5927 0.3979 0.8339 0.036 Uiso 1 1 calc R . . C21A C 0.4801(2) 0.6049(3) 0.97729(10) 0.0357(8) Uani 1 1 d . . . H21A H 0.4667 0.6776 0.9620 0.043 Uiso 1 1 calc R . . C22A C 0.5073(2) 0.5099(3) 0.95586(9) 0.0286(7) Uani 1 1 d . . . C23A C 0.5275(2) 0.4052(3) 0.97944(10) 0.0353(8) Uani 1 1 d . . . H23A H 0.5469 0.3396 0.9656 0.042 Uiso 1 1 calc R . . N11B N 0.5000 1.3361(3) 0.7500 0.0269(8) Uani 1 2 d S . . C11B C 0.5643(2) 1.2742(3) 0.74055(11) 0.0334(7) Uani 1 1 d . . . H11B H 0.6101 1.3161 0.7334 0.040 Uiso 1 1 calc R . . C12B C 0.5669(2) 1.1532(3) 0.74078(11) 0.0361(8) Uani 1 1 d . . . H12B H 0.6144 1.1131 0.7346 0.043 Uiso 1 1 calc R . . C13B C 0.5000 1.0898(4) 0.7500 0.0294(10) Uani 1 2 d S . . N21B N 0.5000 0.7101(3) 0.7500 0.0261(8) Uani 1 2 d S . . C21B C 0.5718(2) 0.7725(3) 0.76609(11) 0.0344(7) Uani 1 1 d . . . H21B H 0.6233 0.7306 0.7780 0.041 Uiso 1 1 calc R . . C22B C 0.5749(2) 0.8942(3) 0.76627(11) 0.0364(7) Uani 1 1 d . . . H22B H 0.6276 0.9341 0.7774 0.044 Uiso 1 1 calc R . . C23B C 0.5000 0.9576(4) 0.7500 0.0293(10) Uani 1 2 d S . . C101 C 0.7464(3) 0.6684(4) 0.8770(2) 0.0747(14) Uani 1 1 d . . . H101 H 0.7244 0.6015 0.8596 0.090 Uiso 1 1 calc R . . C102 C 0.7561(4) 0.6655(5) 0.9220(2) 0.0877(17) Uani 1 1 d . . . H102 H 0.7403 0.5976 0.9360 0.105 Uiso 1 1 calc R . . C103 C 0.7902(4) 0.7663(7) 0.94714(19) 0.0884(17) Uani 1 1 d . . . H103 H 0.7994 0.7664 0.9785 0.106 Uiso 1 1 calc R . . C104 C 0.8094(3) 0.8631(5) 0.9254(2) 0.0828(16) Uani 1 1 d . . . H104 H 0.8305 0.9321 0.9417 0.099 Uiso 1 1 calc R . . C105 C 0.7988(3) 0.8622(5) 0.8814(2) 0.0818(16) Uani 1 1 d . . . H105 H 0.8131 0.9302 0.8668 0.098 Uiso 1 1 calc R . . C106 C 0.7680(3) 0.7655(5) 0.85737(17) 0.0728(14) Uani 1 1 d . . . H106 H 0.7615 0.7660 0.8262 0.087 Uiso 1 1 calc R . . C201 C 0.5746(4) -0.0391(6) 0.9538(3) 0.107(2) Uani 1 1 d . . . H201 H 0.6079 -0.0663 0.9816 0.128 Uiso 1 1 calc R . . C202 C 0.5716(4) -0.1024(6) 0.9169(4) 0.124(3) Uani 1 1 d . . . H202 H 0.6017 -0.1748 0.9185 0.149 Uiso 1 1 calc R . . C203 C 0.5250(8) -0.0617(10) 0.8776(3) 0.148(4) Uani 1 1 d . . . H203 H 0.5225 -0.1051 0.8512 0.178 Uiso 1 1 calc R . . C204 C 0.4822(5) 0.0412(8) 0.8760(2) 0.118(3) Uani 1 1 d . . . H204 H 0.4494 0.0696 0.8483 0.141 Uiso 1 1 calc R . . C205 C 0.4855(3) 0.1036(5) 0.9129(2) 0.0784(15) Uani 1 1 d . . . H205 H 0.4559 0.1765 0.9114 0.094 Uiso 1 1 calc R . . C206 C 0.5307(4) 0.0623(5) 0.95158(18) 0.0792(15) Uani 1 1 d . . . H206 H 0.5320 0.1052 0.9780 0.095 Uiso 1 1 calc R . . C301 C 0.2434(6) 0.7456(10) 0.8451(3) 0.148(4) Uani 1 1 d . . . H301 H 0.2299 0.7341 0.8139 0.178 Uiso 1 1 calc R . . C302 C 0.2944(4) 0.8359(6) 0.8650(3) 0.108(2) Uani 1 1 d . . . H302 H 0.3168 0.8892 0.8471 0.129 Uiso 1 1 calc R . . C303 C 0.3136(4) 0.8513(5) 0.9087(3) 0.098(2) Uani 1 1 d . . . H303 H 0.3493 0.9150 0.9216 0.117 Uiso 1 1 calc R . . C304 C 0.2828(5) 0.7777(8) 0.9346(3) 0.127(3) Uani 1 1 d . . . H304 H 0.2964 0.7896 0.9658 0.153 Uiso 1 1 calc R . . C305 C 0.2292(8) 0.6802(12) 0.9153(6) 0.204(9) Uani 1 1 d . . . H305 H 0.2067 0.6246 0.9323 0.245 Uiso 1 1 calc R . . C306 C 0.2143(7) 0.6758(10) 0.8714(7) 0.198(10) Uani 1 1 d . . . H306 H 0.1777 0.6140 0.8573 0.237 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0324(3) 0.0210(3) 0.0175(2) 0.000 0.0086(2) 0.000 N1 0.0330(15) 0.0462(16) 0.0572(18) 0.0195(15) 0.0220(14) 0.0154(15) O1 0.102(3) 0.091(2) 0.105(3) 0.043(2) 0.075(2) 0.024(2) O2 0.0291(11) 0.0333(11) 0.0350(11) 0.0001(10) 0.0118(9) -0.0004(10) O3 0.187(6) 0.321(8) 0.375(10) 0.267(8) 0.232(7) 0.199(6) N11A 0.0284(13) 0.0266(12) 0.0219(11) 0.0016(10) 0.0078(10) 0.0039(12) C11A 0.0393(19) 0.0299(17) 0.0238(15) 0.0041(12) 0.0082(13) 0.0079(14) C12A 0.0416(19) 0.0293(17) 0.0275(15) -0.0004(12) 0.0129(14) 0.0109(14) C13A 0.0349(17) 0.0306(15) 0.0220(13) 0.0007(12) 0.0080(12) 0.0010(14) C14A 0.0388(19) 0.0374(18) 0.0272(15) 0.0080(13) 0.0090(14) 0.0140(14) C15A 0.0361(18) 0.0305(18) 0.0266(15) 0.0009(12) 0.0129(13) 0.0076(13) C21A 0.052(2) 0.0333(18) 0.0224(15) 0.0051(12) 0.0099(14) 0.0081(16) C22A 0.0351(17) 0.0308(17) 0.0204(13) -0.0013(12) 0.0079(12) 0.0030(13) C23A 0.055(2) 0.0276(17) 0.0255(15) -0.0001(12) 0.0143(15) 0.0118(15) N11B 0.036(2) 0.0224(19) 0.0237(17) 0.000 0.0104(15) 0.000 C11B 0.0342(18) 0.0282(17) 0.0419(18) -0.0044(14) 0.0170(15) -0.0040(14) C12B 0.0364(19) 0.0300(17) 0.0455(19) -0.0097(15) 0.0167(15) -0.0020(14) C13B 0.030(2) 0.026(2) 0.032(2) 0.000 0.0054(19) 0.000 N21B 0.030(2) 0.0269(19) 0.0227(17) 0.000 0.0082(15) 0.000 C21B 0.0317(17) 0.0290(17) 0.0381(17) -0.0035(14) 0.0003(14) 0.0063(14) C22B 0.0307(18) 0.0279(16) 0.049(2) -0.0077(15) 0.0065(15) -0.0022(15) C23B 0.032(2) 0.020(2) 0.038(2) 0.000 0.0119(19) 0.000 C101 0.061(3) 0.056(3) 0.100(4) -0.009(3) 0.006(3) -0.004(2) C102 0.074(4) 0.069(4) 0.122(5) 0.039(4) 0.028(4) 0.011(3) C103 0.063(3) 0.130(6) 0.070(3) 0.002(4) 0.012(3) 0.025(4) C104 0.050(3) 0.082(4) 0.108(5) -0.027(4) 0.004(3) -0.006(3) C105 0.051(3) 0.062(3) 0.124(5) 0.016(3) 0.005(3) -0.006(2) C106 0.049(3) 0.082(4) 0.077(3) 0.010(3) -0.004(2) -0.001(3) C201 0.093(5) 0.078(5) 0.124(6) 0.031(4) -0.024(4) -0.008(4) C202 0.070(4) 0.066(4) 0.252(11) -0.019(6) 0.070(6) 0.001(3) C203 0.203(11) 0.151(9) 0.138(7) -0.069(6) 0.130(8) -0.070(8) C204 0.147(7) 0.143(7) 0.053(3) 0.026(4) 0.004(4) -0.043(6) C205 0.061(3) 0.069(3) 0.102(4) 0.019(3) 0.015(3) 0.001(3) C206 0.098(4) 0.070(3) 0.069(3) -0.006(3) 0.019(3) -0.011(3) C301 0.079(6) 0.134(8) 0.192(9) -0.071(8) -0.042(6) 0.063(5) C302 0.075(4) 0.077(4) 0.159(7) 0.010(5) 0.004(4) 0.030(4) C303 0.068(4) 0.053(3) 0.160(7) -0.013(4) 0.005(4) 0.011(3) C304 0.086(5) 0.114(6) 0.192(8) 0.039(6) 0.053(5) 0.046(5) C305 0.091(8) 0.123(9) 0.43(2) 0.141(15) 0.125(13) 0.052(7) C306 0.067(6) 0.060(6) 0.44(3) -0.010(11) 0.011(12) 0.007(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 N11A 2.086(2) 2_656 ? Ni1 N11A 2.086(2) . ? Ni1 N11B 2.115(3) 1_545 ? Ni1 O2 2.123(2) . ? Ni1 O2 2.123(2) 2_656 ? Ni1 N21B 2.126(4) . ? N1 O3 1.143(5) . ? N1 O1 1.175(4) . ? N1 O2 1.257(3) . ? N11A C11A 1.339(4) . ? N11A C15A 1.345(4) . ? C11A C12A 1.380(4) . ? C12A C13A 1.394(4) . ? C13A C14A 1.388(4) . ? C13A C22A 1.483(4) . ? C14A C15A 1.375(4) . ? C21A C23A 1.386(4) 5_667 ? C21A C22A 1.392(4) . ? C22A C23A 1.391(4) . ? C23A C21A 1.386(4) 5_667 ? N11B C11B 1.342(4) . ? N11B C11B 1.342(4) 2_656 ? N11B Ni1 2.115(3) 1_565 ? C11B C12B 1.374(4) . ? C12B C13B 1.383(4) . ? C13B C12B 1.383(4) 2_656 ? C13B C23B 1.500(5) . ? N21B C21B 1.344(4) 2_656 ? N21B C21B 1.344(4) . ? C21B C22B 1.381(4) . ? C22B C23B 1.389(4) . ? C23B C22B 1.389(4) 2_656 ? C101 C106 1.346(7) . ? C101 C102 1.368(7) . ? C102 C103 1.418(8) . ? C103 C104 1.365(8) . ? C104 C105 1.338(8) . ? C105 C106 1.351(7) . ? C201 C206 1.344(8) . ? C201 C202 1.343(10) . ? C202 C203 1.350(11) . ? C203 C204 1.350(12) . ? C204 C205 1.338(9) . ? C205 C206 1.331(7) . ? C301 C306 1.305(16) . ? C301 C302 1.363(11) . ? C302 C303 1.330(9) . ? C303 C304 1.337(9) . ? C304 C305 1.441(16) . ? C305 C306 1.33(2) . ? 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 N11A Ni1 N11A 179.45(14) 2_656 . ? N11A Ni1 N11B 90.27(7) 2_656 1_545 ? N11A Ni1 N11B 90.27(7) . 1_545 ? N11A Ni1 O2 83.85(8) 2_656 . ? N11A Ni1 O2 96.16(8) . . ? N11B Ni1 O2 89.27(6) 1_545 . ? N11A Ni1 O2 96.16(8) 2_656 2_656 ? N11A Ni1 O2 83.85(8) . 2_656 ? N11B Ni1 O2 89.27(6) 1_545 2_656 ? O2 Ni1 O2 178.54(12) . 2_656 ? N11A Ni1 N21B 89.73(7) 2_656 . ? N11A Ni1 N21B 89.73(7) . . ? N11B Ni1 N21B 179.998(2) 1_545 . ? O2 Ni1 N21B 90.73(6) . . ? O2 Ni1 N21B 90.73(6) 2_656 . ? O3 N1 O1 115.6(4) . . ? O3 N1 O2 118.6(3) . . ? O1 N1 O2 124.9(3) . . ? N1 O2 Ni1 136.6(2) . . ? C11A N11A C15A 116.7(2) . . ? C11A N11A Ni1 122.5(2) . . ? C15A N11A Ni1 120.83(18) . . ? N11A C11A C12A 123.5(3) . . ? C11A C12A C13A 119.8(3) . . ? C14A C13A C12A 116.5(3) . . ? C14A C13A C22A 122.7(3) . . ? C12A C13A C22A 120.7(3) . . ? C15A C14A C13A 120.4(3) . . ? N11A C15A C14A 123.1(3) . . ? C23A C21A C22A 120.9(3) 5_667 . ? C21A C22A C23A 117.9(3) . . ? C21A C22A C13A 121.4(3) . . ? C23A C22A C13A 120.6(3) . . ? C21A C23A C22A 121.2(3) 5_667 . ? C11B N11B C11B 116.9(4) . 2_656 ? C11B N11B Ni1 121.53(19) . 1_565 ? C11B N11B Ni1 121.53(18) 2_656 1_565 ? N11B C11B C12B 123.1(3) . . ? C11B C12B C13B 119.7(3) . . ? C12B C13B C12B 117.4(4) 2_656 . ? C12B C13B C23B 121.3(2) 2_656 . ? C12B C13B C23B 121.3(2) . . ? C21B N21B C21B 116.4(4) 2_656 . ? C21B N21B Ni1 121.79(19) 2_656 . ? C21B N21B Ni1 121.79(18) . . ? N21B C21B C22B 123.7(3) . . ? C21B C22B C23B 119.2(3) . . ? C22B C23B C22B 117.7(4) . 2_656 ? C22B C23B C13B 121.2(2) . . ? C22B C23B C13B 121.2(2) 2_656 . ? C106 C101 C102 120.4(5) . . ? C101 C102 C103 118.5(5) . . ? C104 C103 C102 118.6(5) . . ? C105 C104 C103 120.9(6) . . ? C104 C105 C106 120.6(5) . . ? C101 C106 C105 120.9(5) . . ? C206 C201 C202 120.3(6) . . ? C201 C202 C203 119.1(7) . . ? C204 C203 C202 119.6(7) . . ? C205 C204 C203 121.0(7) . . ? C206 C205 C204 119.1(6) . . ? C205 C206 C201 120.9(6) . . ? C306 C301 C302 116.2(12) . . ? C303 C302 C301 121.7(9) . . ? C302 C303 C304 120.4(8) . . ? C303 C304 C305 120.1(10) . . ? C306 C305 C304 113.4(12) . . ? C301 C306 C305 128.2(15) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.036 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.071 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H72 N6 Ni O6' _chemical_formula_weight 1272.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 39.824(3) _cell_length_b 15.5840(9) _cell_length_c 11.2915(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7007.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.334 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9362 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42836 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.91 _reflns_number_total 8301 _reflns_number_gt 6222 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+10.3716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8301 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1864 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.432 _refine_ls_shift/su_mean 0.023 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 0.2500 0.5000 0.47291(3) 0.01740(13) Uani 1 2 d S . . N1A N 0.25781(6) 0.69734(14) 0.48950(19) 0.0256(5) Uani 1 1 d . . . O1A O 0.25117(7) 0.74770(16) 0.5703(2) 0.0554(7) Uani 1 1 d . . . O2A O 0.28206(6) 0.71110(15) 0.4241(2) 0.0462(6) Uani 1 1 d . . . O3A O 0.23917(5) 0.63212(12) 0.47404(15) 0.0246(4) Uani 1 1 d . . . C101 C 0.10904(19) 0.2500 0.7500 0.0762(19) Uani 1 2 d S . . H101 H 0.0852 0.2500 0.7500 0.091 Uiso 1 2 calc SR . . C102 C 0.12679(15) 0.2909(3) 0.8400(4) 0.0760(14) Uani 1 1 d . . . H102 H 0.1151 0.3193 0.9019 0.091 Uiso 1 1 calc R . . C103 C 0.16085(13) 0.2898(3) 0.8389(4) 0.0673(12) Uani 1 1 d . . . H103 H 0.1730 0.3171 0.9008 0.081 Uiso 1 1 calc R . . C104 C 0.17762(17) 0.2500 0.7500 0.0637(16) Uani 1 2 d S . . H104 H 0.2015 0.2500 0.7500 0.076 Uiso 1 2 calc SR . . C111 C 0.1908(2) 0.7500 0.2500 0.076(2) Uani 1 2 d S . . H111 H 0.2147 0.7500 0.2500 0.092 Uiso 1 2 calc SR . . C112 C 0.17420(16) 0.7104(3) 0.1610(4) 0.0787(14) Uani 1 1 d . . . H112 H 0.1865 0.6834 0.0993 0.094 Uiso 1 1 calc R . . C113 C 0.14018(17) 0.7091(3) 0.1592(4) 0.0797(15) Uani 1 1 d . . . H113 H 0.1287 0.6807 0.0968 0.096 Uiso 1 1 calc R . . C114 C 0.1219(2) 0.7500 0.2500 0.084(2) Uani 1 2 d S . . H114 H 0.0980 0.7500 0.2500 0.101 Uiso 1 2 calc SR . . C121 C 0.08374(19) 0.2500 0.2500 0.100(3) Uani 1 2 d S . . H121 H 0.0599 0.2500 0.2500 0.120 Uiso 1 2 calc SR . . C122 C 0.10304(15) 0.2817(3) 0.3491(4) 0.0771(14) Uani 1 1 d . . . H122 H 0.0921 0.3036 0.4174 0.093 Uiso 1 1 calc R . . C123 C 0.13665(13) 0.2796(3) 0.3433(4) 0.0731(13) Uani 1 1 d . . . H123 H 0.1492 0.3002 0.4089 0.088 Uiso 1 1 calc R . . C124 C 0.15301(19) 0.2500 0.2500 0.0681(17) Uani 1 2 d S . . H124 H 0.1769 0.2500 0.2500 0.082 Uiso 1 2 calc SR . . C131 C 0.10545(18) 0.4594(3) 1.0973(4) 0.159(4) Uani 1 1 d G . . H131 H 0.0960 0.4306 1.1634 0.191 Uiso 1 1 calc R . . C132 C 0.14007(16) 0.4605(2) 1.0818(3) 0.115(3) Uani 1 1 d G . . H132 H 0.1542 0.4325 1.1373 0.138 Uiso 1 1 calc R . . C133 C 0.15396(9) 0.5027(2) 0.9850(4) 0.0881(17) Uani 1 1 d G . . H133 H 0.1776 0.5035 0.9744 0.106 Uiso 1 1 calc R . . C134 C 0.13323(13) 0.5437(3) 0.9037(3) 0.0914(17) Uani 1 1 d G . . H134 H 0.1427 0.5725 0.8376 0.110 Uiso 1 1 calc R . . C135 C 0.09861(12) 0.5426(3) 0.9193(5) 0.163(4) Uani 1 1 d G . . H135 H 0.0844 0.5706 0.8637 0.196 Uiso 1 1 calc R . . C136 C 0.08472(10) 0.5004(4) 1.0160(7) 0.236(8) Uani 1 1 d G . . H136 H 0.0611 0.4996 1.0267 0.284 Uiso 1 1 calc R . . C141 C 0.10925(13) 0.7500 0.7500 0.0583(15) Uani 1 2 d S . . H141 H 0.0854 0.7500 0.7500 0.070 Uiso 1 2 calc SR . . C142 C 0.12676(10) 0.7144(2) 0.6553(3) 0.0545(9) Uani 1 1 d . . . H142 H 0.1149 0.6899 0.5905 0.065 Uiso 1 1 calc R . . C143 C 0.16121(9) 0.7148(2) 0.6557(3) 0.0455(8) Uani 1 1 d . . . H143 H 0.1732 0.6908 0.5910 0.055 Uiso 1 1 calc R . . C144 C 0.17847(12) 0.7500 0.7500 0.0399(10) Uani 1 2 d S . . H144 H 0.2023 0.7500 0.7500 0.048 Uiso 1 2 calc SR . . N11A N 0.19767(5) 0.48995(13) 0.47656(17) 0.0206(4) Uani 1 1 d . . . C11A C 0.18057(6) 0.44549(17) 0.5587(2) 0.0250(5) Uani 1 1 d . . . H11A H 0.1929 0.4116 0.6133 0.030 Uiso 1 1 calc R . . C12A C 0.14597(7) 0.44634(19) 0.5681(2) 0.0312(6) Uani 1 1 d . . . H12A H 0.1352 0.4138 0.6283 0.037 Uiso 1 1 calc R . . C13A C 0.12689(7) 0.49493(18) 0.4893(2) 0.0288(5) Uani 1 1 d . . . C14A C 0.14465(6) 0.54099(19) 0.4042(2) 0.0290(6) Uani 1 1 d . . . H14A H 0.1329 0.5751 0.3482 0.035 Uiso 1 1 calc R . . C15A C 0.17912(6) 0.53726(18) 0.4009(2) 0.0257(5) Uani 1 1 d . . . H15A H 0.1905 0.5698 0.3422 0.031 Uiso 1 1 calc R . . C21A C 0.08965(7) 0.4973(2) 0.4942(3) 0.0367(7) Uani 1 1 d . . . C22A C 0.07220(10) 0.4713(6) 0.5895(5) 0.161(4) Uani 1 1 d . . . H22A H 0.0841 0.4516 0.6572 0.193 Uiso 1 1 calc R . . C23A C 0.03727(10) 0.4724(7) 0.5923(6) 0.191(5) Uani 1 1 d . . . H23A H 0.0261 0.4536 0.6619 0.229 Uiso 1 1 calc R . . C24A C 0.01871(8) 0.4995(3) 0.4988(4) 0.0577(11) Uani 1 1 d . . . C25A C 0.03609(8) 0.5240(3) 0.4018(3) 0.0567(11) Uani 1 1 d . . . H25A H 0.0241 0.5426 0.3336 0.068 Uiso 1 1 calc R . . C26A C 0.07086(8) 0.5228(3) 0.3991(3) 0.0583(11) Uani 1 1 d . . . H26A H 0.0820 0.5402 0.3288 0.070 Uiso 1 1 calc R . . N11B N 0.2500 0.5000 0.6600(2) 0.0206(6) Uani 1 2 d S . . C11B C 0.23631(7) 0.56457(16) 0.7219(2) 0.0236(5) Uani 1 1 d . . . H11B H 0.2262 0.6104 0.6795 0.028 Uiso 1 1 calc R . . C12B C 0.23624(7) 0.56773(17) 0.8443(2) 0.0260(5) Uani 1 1 d . . . H12B H 0.2269 0.6157 0.8845 0.031 Uiso 1 1 calc R . . C13B C 0.2500 0.5000 0.9079(3) 0.0236(7) Uani 1 2 d S . . N21B N 0.2500 0.5000 0.2870(2) 0.0199(5) Uani 1 2 d S . . C21B C 0.23952(6) 0.43141(16) 0.2254(2) 0.0220(5) Uani 1 1 d . . . H21B H 0.2318 0.3827 0.2678 0.026 Uiso 1 1 calc R . . C22B C 0.23950(7) 0.42832(17) 0.1026(2) 0.0248(5) Uani 1 1 d . . . H22B H 0.2324 0.3780 0.0622 0.030 Uiso 1 1 calc R . . C23B C 0.2500 0.5000 0.0396(3) 0.0244(7) Uani 1 2 d S . . C151 C 0.0239(3) 0.310(2) 0.9539(17) 0.311(15) Uani 1 1 d . . . C154 C -0.0368(4) 0.2750(15) 0.9949(15) 0.208(7) Uani 1 1 d . . . C152 C 0.0092(5) 0.3596(16) 1.0506(17) 0.156(8) Uani 0.50 1 d P . . C153 C -0.0151(6) 0.3097(17) 1.095(2) 0.165(8) Uani 0.50 1 d P . . C155 C -0.0234(6) 0.2662(14) 0.881(3) 0.174(11) Uani 0.50 1 d P . . C156 C 0.0052(5) 0.3154(15) 0.854(2) 0.129(6) Uani 0.50 1 d P . . C157 C 0.0093(5) 0.2254(12) 1.0363(18) 0.134(6) Uani 0.50 1 d P . . C158 C 0.0086(8) 0.3653(17) 0.922(3) 0.145(11) Uani 0.50 1 d P . . C159 C -0.0252(6) 0.2353(17) 1.056(2) 0.128(7) Uani 0.50 1 d P . . C160 C -0.0274(6) 0.3516(16) 0.9256(17) 0.140(6) Uani 0.50 1 d P . . 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 0.0161(2) 0.0245(2) 0.0116(2) 0.000 0.000 0.00063(17) N1A 0.0315(12) 0.0242(11) 0.0212(10) 0.0013(8) 0.0024(8) 0.0035(8) O1A 0.0805(19) 0.0381(13) 0.0477(14) -0.0202(11) 0.0214(13) -0.0094(12) O2A 0.0426(13) 0.0477(13) 0.0483(13) -0.0106(11) 0.0176(11) -0.0153(10) O3A 0.0248(8) 0.0250(9) 0.0240(9) 0.0013(7) -0.0011(7) 0.0007(7) C101 0.074(4) 0.090(5) 0.065(4) 0.028(4) 0.000 0.000 C102 0.107(4) 0.081(3) 0.040(2) 0.006(2) 0.011(2) 0.018(3) C103 0.091(3) 0.062(3) 0.049(2) 0.007(2) -0.016(2) -0.001(2) C104 0.073(4) 0.054(3) 0.064(4) 0.020(3) 0.000 0.000 C111 0.102(6) 0.053(4) 0.074(5) 0.027(3) 0.000 0.000 C112 0.117(5) 0.060(3) 0.059(3) 0.013(2) 0.014(3) 0.009(3) C113 0.128(5) 0.054(3) 0.057(3) 0.011(2) -0.014(3) -0.004(3) C114 0.086(5) 0.061(4) 0.106(6) 0.042(4) 0.000 0.000 C121 0.061(4) 0.068(5) 0.170(9) 0.035(5) 0.000 0.000 C122 0.104(4) 0.069(3) 0.059(3) -0.009(2) 0.018(3) 0.017(3) C123 0.084(3) 0.078(3) 0.058(3) -0.005(2) -0.006(2) 0.012(3) C124 0.088(5) 0.058(4) 0.058(4) 0.000(3) 0.000 0.000 C131 0.222(11) 0.084(5) 0.172(8) 0.011(5) 0.115(8) -0.030(6) C132 0.223(9) 0.059(3) 0.062(3) -0.001(3) -0.030(4) 0.019(4) C133 0.069(3) 0.069(3) 0.126(5) -0.009(3) -0.004(3) 0.000(2) C134 0.127(5) 0.069(3) 0.079(4) 0.021(3) 0.009(3) -0.015(3) C135 0.108(6) 0.153(7) 0.228(11) 0.078(7) -0.070(7) -0.011(6) C136 0.083(6) 0.177(11) 0.45(2) 0.114(13) 0.041(9) -0.018(5) C141 0.037(3) 0.063(4) 0.075(4) 0.015(3) 0.000 0.000 C142 0.060(2) 0.054(2) 0.049(2) 0.0005(17) -0.0168(18) -0.0017(18) C143 0.058(2) 0.0429(19) 0.0360(17) -0.0009(14) -0.0003(15) 0.0074(16) C144 0.041(2) 0.037(2) 0.042(2) 0.0020(19) 0.000 0.000 N11A 0.0198(9) 0.0238(11) 0.0183(9) 0.0009(8) 0.0006(8) -0.0001(8) C11A 0.0209(12) 0.0319(14) 0.0224(12) 0.0053(10) 0.0002(9) 0.0002(10) C12A 0.0222(13) 0.0412(16) 0.0302(14) 0.0104(12) 0.0038(11) -0.0039(11) C13A 0.0188(11) 0.0380(15) 0.0295(13) 0.0015(12) 0.0002(10) 0.0008(11) C14A 0.0214(12) 0.0372(15) 0.0284(13) 0.0081(12) -0.0040(10) 0.0030(11) C15A 0.0216(12) 0.0347(14) 0.0209(12) 0.0076(11) 0.0004(10) -0.0013(11) C21A 0.0179(12) 0.0541(18) 0.0381(15) 0.0070(14) 0.0017(11) 0.0033(12) C22A 0.0190(18) 0.380(12) 0.083(4) 0.132(6) 0.006(2) 0.015(4) C23A 0.0199(19) 0.451(15) 0.101(4) 0.164(7) 0.013(2) 0.021(4) C24A 0.0195(15) 0.101(3) 0.053(2) 0.030(2) 0.0035(14) 0.0047(17) C25A 0.0234(15) 0.098(3) 0.049(2) 0.028(2) -0.0022(14) 0.0024(17) C26A 0.0218(14) 0.104(3) 0.048(2) 0.031(2) 0.0023(14) 0.0010(17) N11B 0.0212(13) 0.0263(14) 0.0143(12) 0.000 0.000 -0.0003(12) C11B 0.0303(13) 0.0251(12) 0.0155(11) 0.0022(9) 0.0011(9) 0.0056(10) C12B 0.0375(14) 0.0239(13) 0.0165(11) -0.0027(10) 0.0026(10) 0.0051(11) C13B 0.0334(18) 0.0249(17) 0.0126(14) 0.000 0.000 -0.0033(15) N21B 0.0198(13) 0.0265(14) 0.0134(12) 0.000 0.000 0.0003(12) C21B 0.0256(12) 0.0251(12) 0.0153(11) 0.0025(9) -0.0004(9) -0.0023(10) C22B 0.0337(13) 0.0236(13) 0.0172(11) -0.0026(9) -0.0028(10) -0.0012(10) C23B 0.0342(18) 0.0272(17) 0.0117(14) 0.000 0.000 0.0015(15) C151 0.101(9) 0.65(5) 0.182(17) -0.13(2) 0.024(10) -0.066(18) C154 0.158(14) 0.28(2) 0.188(15) -0.006(15) 0.040(11) -0.089(14) C152 0.130(14) 0.22(2) 0.117(13) 0.011(15) -0.018(12) -0.057(15) C153 0.124(15) 0.16(2) 0.21(2) -0.014(17) 0.027(15) -0.024(14) C155 0.116(14) 0.127(14) 0.28(3) -0.077(18) -0.086(17) 0.047(12) C156 0.118(13) 0.112(14) 0.156(17) 0.023(12) -0.021(12) 0.010(11) C157 0.106(11) 0.126(13) 0.170(16) -0.046(12) 0.004(11) -0.002(10) C158 0.19(3) 0.127(16) 0.119(17) 0.056(13) -0.016(19) -0.015(18) C159 0.097(13) 0.145(17) 0.143(18) 0.001(14) 0.006(12) 0.016(12) C160 0.114(13) 0.178(19) 0.128(14) 0.019(14) -0.003(11) 0.045(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N11A 2.090(2) . ? Ni1 N11A 2.091(2) 2_565 ? Ni1 N21B 2.099(3) . ? Ni1 O3A 2.1037(18) . ? Ni1 O3A 2.1038(18) 2_565 ? Ni1 N11B 2.113(3) . ? N1A O1A 1.232(3) . ? N1A O2A 1.234(3) . ? N1A O3A 1.271(3) . ? C101 C102 1.392(6) . ? C101 C102 1.392(6) 4_556 ? C102 C103 1.357(7) . ? C103 C104 1.356(6) . ? C104 C103 1.356(6) 4_556 ? C111 C112 1.352(7) 4_565 ? C111 C112 1.352(7) . ? C112 C113 1.355(8) . ? C113 C114 1.410(7) . ? C114 C113 1.410(7) 4_565 ? C121 C122 1.445(6) 4 ? C121 C122 1.445(6) . ? C122 C123 1.340(7) . ? C123 C124 1.322(6) . ? C124 C123 1.322(6) 4 ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C135 C136 1.3900 . ? C141 C142 1.392(5) 4_566 ? C141 C142 1.393(5) . ? C142 C143 1.372(5) . ? C143 C144 1.381(4) . ? C144 C143 1.381(4) 4_566 ? N11A C11A 1.343(3) . ? N11A C15A 1.348(3) . ? C11A C12A 1.382(4) . ? C12A C13A 1.394(4) . ? C13A C14A 1.393(4) . ? C13A C21A 1.484(4) . ? C14A C15A 1.375(4) . ? C21A C22A 1.344(5) . ? C21A C26A 1.368(4) . ? C22A C23A 1.392(5) . ? C23A C24A 1.356(6) . ? C24A C25A 1.351(5) . ? C24A C24A 1.490(6) 5_566 ? C25A C26A 1.385(4) . ? N11B C11B 1.341(3) . ? N11B C11B 1.341(3) 2_565 ? C11B C12B 1.383(3) . ? C12B C13B 1.389(3) . ? C13B C12B 1.389(3) 2_565 ? C13B C23B 1.487(4) 1_556 ? N21B C21B 1.342(3) . ? N21B C21B 1.342(3) 2_565 ? C21B C22B 1.387(3) . ? C22B C23B 1.389(3) . ? C23B C22B 1.389(3) 2_565 ? C23B C13B 1.487(4) 1_554 ? C151 C158 1.11(3) . ? C151 C156 1.36(3) . ? C151 C152 1.46(3) . ? C151 C157 1.72(3) . ? C154 C159 1.04(2) . ? C154 C155 1.39(3) . ? C154 C160 1.48(3) . ? C154 C153 1.52(3) . ? C152 C153 1.34(3) . ? C152 C158 1.46(3) . ? C152 C160 2.03(3) . ? C153 C159 1.30(3) . ? C153 C157 1.76(3) . ? C155 C156 1.41(3) . ? C155 C160 1.43(3) . ? C155 C159 2.03(4) . ? C156 C158 1.10(3) . ? C156 C160 1.63(3) . ? C157 C159 1.40(3) . ? C158 C160 1.45(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11A Ni1 N11A 177.74(11) . 2_565 ? N11A Ni1 N21B 91.13(5) . . ? N11A Ni1 N21B 91.13(5) 2_565 . ? N11A Ni1 O3A 82.46(7) . . ? N11A Ni1 O3A 97.53(7) 2_565 . ? N21B Ni1 O3A 90.35(5) . . ? N11A Ni1 O3A 97.53(7) . 2_565 ? N11A Ni1 O3A 82.46(7) 2_565 2_565 ? N21B Ni1 O3A 90.35(5) . 2_565 ? O3A Ni1 O3A 179.30(9) . 2_565 ? N11A Ni1 N11B 88.87(5) . . ? N11A Ni1 N11B 88.87(5) 2_565 . ? N21B Ni1 N11B 180.000(1) . . ? O3A Ni1 N11B 89.65(5) . . ? O3A Ni1 N11B 89.65(5) 2_565 . ? O1A N1A O2A 120.0(2) . . ? O1A N1A O3A 119.0(2) . . ? O2A N1A O3A 120.9(2) . . ? N1A O3A Ni1 131.59(16) . . ? C102 C101 C102 119.0(7) . 4_556 ? C103 C102 C101 119.7(5) . . ? C104 C103 C102 120.3(5) . . ? C103 C104 C103 121.0(7) . 4_556 ? C112 C111 C112 121.4(8) 4_565 . ? C111 C112 C113 120.5(6) . . ? C112 C113 C114 119.9(5) . . ? C113 C114 C113 117.8(8) . 4_565 ? C122 C121 C122 115.7(7) 4 . ? C123 C122 C121 119.0(5) . . ? C124 C123 C122 122.7(5) . . ? C123 C124 C123 120.9(8) 4 . ? C132 C131 C136 120.0 . . ? C131 C132 C133 120.0 . . ? C132 C133 C134 120.0 . . ? C135 C134 C133 120.0 . . ? C134 C135 C136 120.0 . . ? C135 C136 C131 120.0 . . ? C142 C141 C142 119.9(5) 4_566 . ? C143 C142 C141 119.8(4) . . ? C142 C143 C144 120.1(4) . . ? C143 C144 C143 120.3(5) 4_566 . ? C11A N11A C15A 116.2(2) . . ? C11A N11A Ni1 123.89(16) . . ? C15A N11A Ni1 119.51(16) . . ? N11A C11A C12A 123.6(2) . . ? C11A C12A C13A 120.0(2) . . ? C14A C13A C12A 116.3(2) . . ? C14A C13A C21A 121.3(2) . . ? C12A C13A C21A 122.3(2) . . ? C15A C14A C13A 120.3(2) . . ? N11A C15A C14A 123.6(2) . . ? C22A C21A C26A 115.7(3) . . ? C22A C21A C13A 122.6(3) . . ? C26A C21A C13A 121.6(3) . . ? C21A C22A C23A 122.1(4) . . ? C24A C23A C22A 122.1(4) . . ? C25A C24A C23A 116.1(3) . . ? C25A C24A C24A 121.6(4) . 5_566 ? C23A C24A C24A 122.3(4) . 5_566 ? C24A C25A C26A 121.8(3) . . ? C21A C26A C25A 122.2(3) . . ? C11B N11B C11B 117.2(3) . 2_565 ? C11B N11B Ni1 121.39(14) . . ? C11B N11B Ni1 121.39(14) 2_565 . ? N11B C11B C12B 123.2(2) . . ? C11B C12B C13B 119.2(2) . . ? C12B C13B C12B 117.8(3) 2_565 . ? C12B C13B C23B 121.11(15) 2_565 1_556 ? C12B C13B C23B 121.11(15) . 1_556 ? C21B N21B C21B 117.5(3) . 2_565 ? C21B N21B Ni1 121.24(14) . . ? C21B N21B Ni1 121.24(14) 2_565 . ? N21B C21B C22B 123.1(2) . . ? C21B C22B C23B 118.9(2) . . ? C22B C23B C22B 118.4(3) . 2_565 ? C22B C23B C13B 120.82(15) . 1_554 ? C22B C23B C13B 120.82(15) 2_565 1_554 ? C158 C151 C156 52.0(19) . . ? C158 C151 C152 68(3) . . ? C156 C151 C152 112(2) . . ? C158 C151 C157 126(2) . . ? C156 C151 C157 108.0(18) . . ? C152 C151 C157 82.2(14) . . ? C159 C154 C155 112(3) . . ? C159 C154 C160 136(3) . . ? C155 C154 C160 59.6(13) . . ? C159 C154 C153 58(2) . . ? C155 C154 C153 119.8(15) . . ? C160 C154 C153 87.7(17) . . ? C153 C152 C158 113(2) . . ? C153 C152 C151 105(2) . . ? C158 C152 C151 44.9(16) . . ? C153 C152 C160 72.8(15) . . ? C158 C152 C160 45.4(14) . . ? C151 C152 C160 74.6(11) . . ? C159 C153 C152 128(2) . . ? C159 C153 C154 42.2(13) . . ? C152 C153 C154 110.0(19) . . ? C159 C153 C157 51.7(14) . . ? C152 C153 C157 83.9(17) . . ? C154 C153 C157 76.8(16) . . ? C156 C155 C154 117.5(18) . . ? C156 C155 C160 70.1(18) . . ? C154 C155 C160 63.0(15) . . ? C156 C155 C159 111.9(16) . . ? C154 C155 C159 28.2(15) . . ? C160 C155 C159 83.1(18) . . ? C158 C156 C151 53(2) . . ? C158 C156 C155 109(3) . . ? C151 C156 C155 103(2) . . ? C158 C156 C160 60(2) . . ? C151 C156 C160 92.4(17) . . ? C155 C156 C160 55.6(14) . . ? C159 C157 C151 109.4(16) . . ? C159 C157 C153 46.9(14) . . ? C151 C157 C153 79.3(13) . . ? C156 C158 C151 75(3) . . ? C156 C158 C152 131(2) . . ? C151 C158 C152 67.6(19) . . ? C156 C158 C160 78(2) . . ? C151 C158 C160 115(3) . . ? C152 C158 C160 89(2) . . ? C154 C159 C153 80(2) . . ? C154 C159 C157 114(3) . . ? C153 C159 C157 81(2) . . ? C154 C159 C155 39.5(18) . . ? C153 C159 C155 96.0(19) . . ? C157 C159 C155 80.7(15) . . ? C155 C160 C154 57.3(17) . . ? C155 C160 C158 91.1(18) . . ? C154 C160 C158 112.8(15) . . ? C155 C160 C156 54.3(15) . . ? C154 C160 C156 100.8(15) . . ? C158 C160 C156 41.5(14) . . ? C155 C160 C152 102.7(14) . . ? C154 C160 C152 82.2(12) . . ? C158 C160 C152 45.8(14) . . ? C156 C160 C152 78.3(14) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.863 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.069 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H44 N6 Ni O7' _chemical_formula_weight 995.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.7742(12) _cell_length_b 19.9751(15) _cell_length_c 16.2065(13) _cell_angle_alpha 90.00 _cell_angle_beta 106.398(2) _cell_angle_gamma 90.00 _cell_volume 4898.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9345 _exptl_absorpt_correction_T_max 0.9556 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15750 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.93 _reflns_number_total 5732 _reflns_number_gt 3642 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+10.8720P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5732 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1923 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.007 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 0.5000 0.95153(3) 0.7500 0.0204(2) Uani 1 2 d S . . N1A N 0.5333(5) 0.9765(4) 0.5663(5) 0.0410(19) Uani 0.50 1 d P . . O1A O 0.5720(8) 1.0302(5) 0.5732(6) 0.096(4) Uani 0.50 1 d P . . O2A O 0.5018(6) 0.9535(4) 0.4935(5) 0.065(2) Uani 0.50 1 d P . . O3A O 0.53115(19) 0.94653(15) 0.63271(18) 0.0327(7) Uani 1 1 d . . . N1B N -0.1790(6) 0.6337(4) 0.4433(6) 0.043(2) Uani 0.50 1 d P . . O1B O -0.1909(9) 0.5744(6) 0.4482(10) 0.131(5) Uani 0.50 1 d P . . O2B O -0.1218(9) 0.6510(5) 0.4216(12) 0.160(7) Uani 0.50 1 d P . . O3B O -0.2063(5) 0.6714(5) 0.4821(6) 0.071(2) Uani 0.50 1 d P . . N11B N 0.3622(2) 0.95374(17) 0.6829(2) 0.0265(7) Uani 1 1 d . . . N11A N 0.5000 1.0579(2) 0.7500 0.0272(11) Uani 1 2 d S . . C11A C 0.4537(3) 1.0925(2) 0.6825(3) 0.0326(10) Uani 1 1 d . . . H11A H 0.4204 1.0683 0.6336 0.039 Uiso 1 1 calc R . . C12A C 0.4509(3) 1.1616(2) 0.6792(3) 0.0363(11) Uani 1 1 d . . . H12A H 0.4161 1.1838 0.6294 0.044 Uiso 1 1 calc R . . C13A C 0.5000 1.1985(3) 0.7500 0.0324(14) Uani 1 2 d S . . C21A C 0.5000 1.2721(3) 0.7500 0.0339(14) Uani 1 2 d S . . C22A C 0.4231(3) 1.3083(2) 0.7125(3) 0.0375(11) Uani 1 1 d . . . H22A H 0.3699 1.2850 0.6860 0.045 Uiso 1 1 calc R . . C23A C 0.4230(3) 1.3777(2) 0.7132(3) 0.0361(10) Uani 1 1 d . . . H23A H 0.3694 1.4010 0.6882 0.043 Uiso 1 1 calc R . . C24A C 0.5000 1.4137(3) 0.7500 0.0291(13) Uani 1 2 d S . . C31A C 0.5000 1.4879(3) 0.7500 0.0313(14) Uani 1 2 d S . . C32A C 0.4424(3) 1.5242(2) 0.6838(3) 0.0341(10) Uani 1 1 d . . . H32A H 0.4024 1.5009 0.6379 0.041 Uiso 1 1 calc R . . C33A C 0.4424(3) 1.5936(2) 0.6839(3) 0.0315(10) Uani 1 1 d . . . H33A H 0.4026 1.6172 0.6381 0.038 Uiso 1 1 calc R . . C34A C 0.5000 1.6292(3) 0.7500 0.0287(13) Uani 1 2 d S . . N41A N 0.5000 1.8455(2) 0.7500 0.0257(10) Uani 1 2 d S . . C41A C 0.4853(3) 1.8093(2) 0.6765(3) 0.0306(9) Uani 1 1 d . . . H41A H 0.4750 1.8328 0.6236 0.037 Uiso 1 1 calc R . . C42A C 0.4845(3) 1.7402(2) 0.6742(3) 0.0325(10) Uani 1 1 d . . . H42A H 0.4733 1.7176 0.6207 0.039 Uiso 1 1 calc R . . C43A C 0.5000 1.7036(3) 0.7500 0.0298(13) Uani 1 2 d S . . C11B C 0.3033(3) 0.9750(3) 0.7225(3) 0.0414(11) Uani 1 1 d . . . H11B H 0.3231 0.9828 0.7827 0.050 Uiso 1 1 calc R . . C12B C 0.2156(3) 0.9863(3) 0.6808(3) 0.0450(12) Uani 1 1 d . . . H12B H 0.1768 1.0022 0.7119 0.054 Uiso 1 1 calc R . . C13B C 0.1840(3) 0.9743(2) 0.5933(3) 0.0341(10) Uani 1 1 d . . . C14B C 0.2434(3) 0.9516(2) 0.5523(3) 0.0388(11) Uani 1 1 d . . . H14B H 0.2246 0.9422 0.4924 0.047 Uiso 1 1 calc R . . C15B C 0.3309(3) 0.9422(2) 0.5985(3) 0.0342(10) Uani 1 1 d . . . H15B H 0.3709 0.9268 0.5686 0.041 Uiso 1 1 calc R . . C21B C 0.0286(3) 0.9343(2) 0.5268(3) 0.0334(10) Uani 1 1 d . . . C22B C -0.0623(3) 0.9460(2) 0.4805(3) 0.0330(10) Uani 1 1 d . . . C23B C -0.1218(3) 0.8916(2) 0.4653(3) 0.0406(11) Uani 1 1 d . . . H23B H -0.1825 0.8993 0.4370 0.049 Uiso 1 1 calc R . . C24B C -0.0940(3) 0.8285(3) 0.4903(3) 0.0450(12) Uani 1 1 d . . . H24B H -0.1347 0.7924 0.4775 0.054 Uiso 1 1 calc R . . C25B C -0.0046(3) 0.8165(3) 0.5353(3) 0.0418(11) Uani 1 1 d . . . H25B H 0.0144 0.7722 0.5526 0.050 Uiso 1 1 calc R . . C26B C 0.0539(3) 0.8676(2) 0.5539(3) 0.0371(11) Uani 1 1 d . . . H26B H 0.1133 0.8588 0.5858 0.045 Uiso 1 1 calc R . . C27B C 0.0887(3) 0.9877(2) 0.5455(3) 0.0331(10) Uani 1 1 d . . . C101 C -0.3108(8) 0.8546(6) 0.1608(13) 0.140(5) Uani 1 1 d . . . H101 H -0.3419 0.8959 0.1516 0.168 Uiso 1 1 calc R . . C102 C -0.2666(9) 0.8404(8) 0.2352(9) 0.126(4) Uani 1 1 d . . . H102 H -0.2606 0.8719 0.2804 0.152 Uiso 1 1 calc R . . C103 C -0.2284(7) 0.7814(8) 0.2508(7) 0.116(4) Uani 1 1 d . . . H103 H -0.1978 0.7708 0.3087 0.139 Uiso 1 1 calc R . . C104 C -0.2300(6) 0.7357(5) 0.1906(8) 0.094(3) Uani 1 1 d . . . H104 H -0.2023 0.6936 0.2067 0.113 Uiso 1 1 calc R . . C105 C -0.2692(8) 0.7480(6) 0.1100(8) 0.122(4) Uani 1 1 d . . . H105 H -0.2670 0.7168 0.0664 0.146 Uiso 1 1 calc R . . C106 C -0.3173(8) 0.8123(8) 0.0886(7) 0.159(6) Uani 1 1 d . . . H106 H -0.3497 0.8242 0.0316 0.190 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0199(4) 0.0149(3) 0.0232(4) 0.000 0.0008(3) 0.000 N1A 0.046(5) 0.033(4) 0.036(5) -0.001(3) -0.001(4) -0.006(4) O1A 0.127(9) 0.092(7) 0.060(6) 0.013(5) 0.009(6) -0.055(7) O2A 0.106(7) 0.050(4) 0.032(4) 0.000(4) 0.007(4) 0.011(4) O3A 0.0350(16) 0.0347(16) 0.0269(16) 0.0062(13) 0.0061(12) -0.0025(13) N1B 0.044(5) 0.034(5) 0.062(6) -0.011(4) 0.035(4) -0.011(4) O1B 0.140(11) 0.090(8) 0.212(15) 0.010(9) 0.127(11) -0.005(8) O2B 0.133(10) 0.060(6) 0.35(2) 0.093(10) 0.165(14) 0.036(7) O3B 0.050(5) 0.072(6) 0.101(7) -0.012(5) 0.035(5) -0.009(4) N11B 0.0207(16) 0.0249(16) 0.0312(18) 0.0002(15) 0.0031(13) -0.0009(14) N11A 0.028(2) 0.019(2) 0.033(3) 0.000 0.006(2) 0.000 C11A 0.037(2) 0.023(2) 0.033(2) -0.0013(17) 0.0037(19) -0.0012(17) C12A 0.046(3) 0.023(2) 0.034(2) 0.0037(17) 0.002(2) 0.0028(18) C13A 0.037(3) 0.019(3) 0.039(4) 0.000 0.008(3) 0.000 C21A 0.045(4) 0.019(3) 0.038(4) 0.000 0.013(3) 0.000 C22A 0.041(3) 0.022(2) 0.048(3) -0.0019(19) 0.009(2) -0.0043(18) C23A 0.041(3) 0.022(2) 0.044(3) -0.0005(19) 0.010(2) 0.0052(18) C24A 0.043(3) 0.014(3) 0.034(3) 0.000 0.015(3) 0.000 C31A 0.044(4) 0.022(3) 0.031(3) 0.000 0.016(3) 0.000 C32A 0.046(3) 0.0195(19) 0.034(2) -0.0031(17) 0.005(2) -0.0019(18) C33A 0.043(3) 0.021(2) 0.028(2) 0.0028(16) 0.0060(19) 0.0016(17) C34A 0.042(3) 0.018(3) 0.028(3) 0.000 0.013(3) 0.000 N41A 0.027(2) 0.020(2) 0.027(3) 0.000 0.001(2) 0.000 C41A 0.040(2) 0.025(2) 0.024(2) 0.0019(16) 0.0056(18) -0.0005(17) C42A 0.046(3) 0.021(2) 0.028(2) -0.0024(16) 0.0064(19) 0.0007(17) C43A 0.036(3) 0.022(3) 0.031(3) 0.000 0.010(3) 0.000 C11B 0.030(2) 0.062(3) 0.028(2) -0.002(2) 0.0021(19) 0.005(2) C12B 0.029(2) 0.071(4) 0.034(3) 0.001(2) 0.008(2) 0.009(2) C13B 0.023(2) 0.037(2) 0.038(3) 0.0041(19) 0.0003(18) 0.0012(17) C14B 0.027(2) 0.051(3) 0.032(2) -0.008(2) -0.0009(18) 0.002(2) C15B 0.027(2) 0.038(3) 0.036(2) -0.0057(19) 0.0044(18) 0.0030(18) C21B 0.026(2) 0.043(3) 0.029(2) 0.0017(18) 0.0045(18) 0.0022(17) C22B 0.023(2) 0.043(3) 0.031(2) 0.0026(19) 0.0046(17) 0.0010(18) C23B 0.027(2) 0.048(3) 0.041(3) 0.008(2) 0.001(2) -0.002(2) C24B 0.037(3) 0.048(3) 0.045(3) 0.004(2) 0.004(2) -0.010(2) C25B 0.040(3) 0.043(3) 0.041(3) 0.004(2) 0.010(2) 0.001(2) C26B 0.030(2) 0.040(3) 0.039(3) 0.002(2) 0.006(2) 0.0045(19) C27B 0.021(2) 0.047(3) 0.029(2) 0.0024(19) 0.0031(17) 0.0023(18) C101 0.084(7) 0.099(8) 0.233(16) -0.018(10) 0.038(9) -0.016(6) C102 0.110(10) 0.171(13) 0.100(9) -0.031(9) 0.033(7) -0.028(9) C103 0.068(6) 0.191(12) 0.084(7) 0.010(8) 0.015(5) -0.040(7) C104 0.079(6) 0.094(7) 0.125(8) 0.017(6) 0.053(6) -0.003(5) C105 0.168(10) 0.119(8) 0.101(8) -0.049(6) 0.076(7) -0.097(8) C106 0.156(11) 0.196(13) 0.082(7) 0.058(8) -0.034(7) -0.103(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3A 2.096(3) 2_656 ? Ni1 O3A 2.096(3) . ? Ni1 N41A 2.117(5) 1_545 ? Ni1 N11A 2.124(4) . ? Ni1 N11B 2.138(3) . ? Ni1 N11B 2.138(3) 2_656 ? N1A O1A 1.226(11) . ? N1A O2A 1.231(10) . ? N1A O3A 1.240(9) . ? N1A O2A 1.703(11) 5_676 ? O1A O2A 1.386(13) 5_676 ? O2A O1A 1.386(13) 5_676 ? O2A N1A 1.703(11) 5_676 ? N1B O2B 1.114(12) . ? N1B O3B 1.141(11) . ? N1B O1B 1.205(13) . ? N11B C15B 1.336(5) . ? N11B C11B 1.339(6) . ? N11A C11A 1.325(5) . ? N11A C11A 1.325(5) 2_656 ? C11A C12A 1.381(6) . ? C12A C13A 1.399(5) . ? C13A C12A 1.399(5) 2_656 ? C13A C21A 1.470(8) . ? C21A C22A 1.395(5) . ? C21A C22A 1.395(5) 2_656 ? C22A C23A 1.385(6) . ? C23A C24A 1.393(5) . ? C24A C23A 1.393(5) 2_656 ? C24A C31A 1.481(7) . ? C31A C32A 1.397(5) . ? C31A C32A 1.397(5) 2_656 ? C32A C33A 1.387(6) . ? C33A C34A 1.389(5) . ? C34A C33A 1.389(5) 2_656 ? C34A C43A 1.486(8) . ? N41A C41A 1.357(5) . ? N41A C41A 1.357(5) 2_656 ? N41A Ni1 2.117(5) 1_565 ? C41A C42A 1.381(6) . ? C42A C43A 1.390(5) . ? C43A C42A 1.390(5) 2_656 ? C11B C12B 1.376(6) . ? C12B C13B 1.385(6) . ? C13B C14B 1.369(7) . ? C13B C27B 1.508(6) . ? C14B C15B 1.385(6) . ? C21B C27B 1.403(6) . ? C21B C26B 1.423(6) . ? C21B C22B 1.438(6) . ? C22B C23B 1.410(6) . ? C22B C27B 1.416(6) 5_576 ? C23B C24B 1.358(7) . ? C24B C25B 1.413(7) . ? C25B C26B 1.353(7) . ? C27B C22B 1.416(6) 5_576 ? C101 C102 1.243(17) . ? C101 C106 1.423(18) . ? C102 C103 1.315(16) . ? C103 C104 1.331(14) . ? C104 C105 1.301(14) . ? C105 C106 1.483(17) . ? 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 O3A Ni1 O3A 174.54(16) 2_656 . ? O3A Ni1 N41A 87.27(8) 2_656 1_545 ? O3A Ni1 N41A 87.27(8) . 1_545 ? O3A Ni1 N11A 92.73(8) 2_656 . ? O3A Ni1 N11A 92.73(8) . . ? N41A Ni1 N11A 179.999(2) 1_545 . ? O3A Ni1 N11B 89.85(12) 2_656 . ? O3A Ni1 N11B 90.27(12) . . ? N41A Ni1 N11B 91.19(9) 1_545 . ? N11A Ni1 N11B 88.81(9) . . ? O3A Ni1 N11B 90.26(12) 2_656 2_656 ? O3A Ni1 N11B 89.85(12) . 2_656 ? N41A Ni1 N11B 91.18(9) 1_545 2_656 ? N11A Ni1 N11B 88.81(9) . 2_656 ? N11B Ni1 N11B 177.63(18) . 2_656 ? O1A N1A O2A 118.0(9) . . ? O1A N1A O3A 118.6(8) . . ? O2A N1A O3A 123.3(8) . . ? O1A N1A O2A 53.5(7) . 5_676 ? O2A N1A O2A 77.4(6) . 5_676 ? O3A N1A O2A 143.7(7) . 5_676 ? N1A O1A O2A 81.2(8) . 5_676 ? N1A O2A O1A 133.0(9) . 5_676 ? N1A O2A N1A 102.6(6) . 5_676 ? O1A O2A N1A 45.3(5) 5_676 5_676 ? N1A O3A Ni1 146.6(4) . . ? O2B N1B O3B 115.7(11) . . ? O2B N1B O1B 118.9(11) . . ? O3B N1B O1B 121.6(10) . . ? C15B N11B C11B 116.0(4) . . ? C15B N11B Ni1 123.1(3) . . ? C11B N11B Ni1 120.4(3) . . ? C11A N11A C11A 117.1(5) . 2_656 ? C11A N11A Ni1 121.4(2) . . ? C11A N11A Ni1 121.4(2) 2_656 . ? N11A C11A C12A 123.8(4) . . ? C11A C12A C13A 119.4(4) . . ? C12A C13A C12A 116.3(5) . 2_656 ? C12A C13A C21A 121.8(3) . . ? C12A C13A C21A 121.8(3) 2_656 . ? C22A C21A C22A 117.6(5) . 2_656 ? C22A C21A C13A 121.2(3) . . ? C22A C21A C13A 121.2(3) 2_656 . ? C23A C22A C21A 121.2(4) . . ? C22A C23A C24A 121.1(4) . . ? C23A C24A C23A 117.8(5) . 2_656 ? C23A C24A C31A 121.1(3) . . ? C23A C24A C31A 121.1(3) 2_656 . ? C32A C31A C32A 117.4(5) . 2_656 ? C32A C31A C24A 121.3(3) . . ? C32A C31A C24A 121.3(3) 2_656 . ? C33A C32A C31A 121.3(4) . . ? C32A C33A C34A 120.8(4) . . ? C33A C34A C33A 118.4(5) . 2_656 ? C33A C34A C43A 120.8(3) . . ? C33A C34A C43A 120.8(3) 2_656 . ? C41A N41A C41A 115.6(5) . 2_656 ? C41A N41A Ni1 122.2(2) . 1_565 ? C41A N41A Ni1 122.2(2) 2_656 1_565 ? N41A C41A C42A 123.6(4) . . ? C41A C42A C43A 120.3(4) . . ? C42A C43A C42A 116.6(5) . 2_656 ? C42A C43A C34A 121.7(3) . . ? C42A C43A C34A 121.7(3) 2_656 . ? N11B C11B C12B 123.7(4) . . ? C11B C12B C13B 119.7(5) . . ? C14B C13B C12B 117.2(4) . . ? C14B C13B C27B 121.9(4) . . ? C12B C13B C27B 120.8(4) . . ? C13B C14B C15B 119.7(4) . . ? N11B C15B C14B 123.7(4) . . ? C27B C21B C26B 122.1(4) . . ? C27B C21B C22B 120.2(4) . . ? C26B C21B C22B 117.7(4) . . ? C23B C22B C27B 122.9(4) . 5_576 ? C23B C22B C21B 118.8(4) . . ? C27B C22B C21B 118.3(4) 5_576 . ? C24B C23B C22B 121.3(4) . . ? C23B C24B C25B 120.2(5) . . ? C26B C25B C24B 120.3(5) . . ? C25B C26B C21B 121.6(4) . . ? C21B C27B C22B 121.5(4) . 5_576 ? C21B C27B C13B 119.3(4) . . ? C22B C27B C13B 119.1(4) 5_576 . ? C102 C101 C106 123.6(13) . . ? C101 C102 C103 119.5(13) . . ? C102 C103 C104 124.1(11) . . ? C105 C104 C103 120.8(10) . . ? C104 C105 C106 117.7(9) . . ? C101 C106 C105 114.1(10) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.929 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.096 #===END