# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Hailong Wang' _publ_contact_author_email XIAOLONGZ@126.COM _publ_section_title ; Diverse Ni(II) MOFs Constructed from Asymmetric Semi-Rigid V-Shaped Multicarboxylate Ligands: Structures and Magnetic Properties ; loop_ _publ_author_name 'Hailong Wang.' 'Yuting Chen.' 'Jianzhuang Jiang.' 'Zhonghai Ni.' ; Daofeng Sun ; 'Laijin Tian.' 'Kang Wang.' 'Daopeng Zhang.' data_709626 _database_code_depnum_ccdc_archive 'CCDC 709626' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H60 N8 Ni3 O21 ' _chemical_formula_weight 1525.27 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 _symmetry_space_group_name_Hall '-C 2yc ' 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 17.0025(14) _cell_length_b 36.907(3) _cell_length_c 11.2149(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.907(2) _cell_angle_gamma 90.00 _cell_volume 7011.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3560 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 22.83 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8446 _exptl_absorpt_correction_T_max 0.9024 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 17392 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6156 _reflns_number_gt 4613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0743P)^2^+3.4393P] 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 6156 _refine_ls_number_parameters 480 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.072 _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 C1 C 1.2844(2) 0.46054(10) 0.1309(3) 0.0343(8) Uani 1 1 d . . . C2 C 1.33053(19) 0.43096(8) 0.3784(3) 0.0273(7) Uani 1 1 d . . . C3 C 1.2782(2) 0.42091(10) 0.1582(3) 0.0343(8) Uani 1 1 d . . . C4 C 1.2521(2) 0.39703(11) 0.0665(3) 0.0473(10) Uani 1 1 d . . . H4 H 1.2384 0.4059 -0.0101 0.057 Uiso 1 1 calc R . . C5 C 1.2463(3) 0.36061(11) 0.0884(4) 0.0563(12) Uani 1 1 d . . . H5 H 1.2298 0.3449 0.0263 0.068 Uiso 1 1 calc R . . C6 C 1.2647(3) 0.34727(11) 0.2011(4) 0.0551(11) Uani 1 1 d . . . H6 H 1.2607 0.3226 0.2158 0.066 Uiso 1 1 calc R . . C7 C 1.2894(2) 0.37083(9) 0.2936(3) 0.0377(8) Uani 1 1 d . . . C8 C 1.29827(18) 0.40772(9) 0.2745(3) 0.0300(7) Uani 1 1 d . . . C9 C 1.2565(2) 0.33710(10) 0.4626(3) 0.0420(9) Uani 1 1 d . . . C10 C 1.2828(2) 0.30771(10) 0.5263(3) 0.0459(9) Uani 1 1 d . . . H10 H 1.3358 0.3012 0.5296 0.055 Uiso 1 1 calc R . . C11 C 1.2296(2) 0.28710(10) 0.5873(3) 0.0462(9) Uani 1 1 d . . . H11 H 1.2475 0.2670 0.6316 0.055 Uiso 1 1 calc R . . C12 C 1.1512(2) 0.29651(10) 0.5819(3) 0.0443(9) Uani 1 1 d . . . C13 C 1.1267(3) 0.32718(13) 0.5185(4) 0.0637(13) Uani 1 1 d . . . H13 H 1.0739 0.3340 0.5147 0.076 Uiso 1 1 calc R . . C14 C 1.1797(3) 0.34806(13) 0.4604(4) 0.0666(13) Uani 1 1 d . . . H14 H 1.1631 0.3692 0.4206 0.080 Uiso 1 1 calc R . . C15 C 1.0935(2) 0.27433(10) 0.6436(3) 0.0428(9) Uani 1 1 d . . . C16 C 1.0192(2) 0.17049(11) 0.6138(3) 0.0460(10) Uani 1 1 d . . . H16 H 1.0626 0.1672 0.6689 0.055 Uiso 1 1 calc R . . C17 C 0.9997(2) 0.14302(10) 0.5335(3) 0.0465(10) Uani 1 1 d . . . H17 H 1.0285 0.1216 0.5364 0.056 Uiso 1 1 calc R . . C18 C 0.9366(2) 0.14778(9) 0.4487(3) 0.0367(8) Uani 1 1 d . . . C19 C 0.8967(2) 0.18073(10) 0.4488(3) 0.0484(10) Uani 1 1 d . . . H19 H 0.8550 0.1853 0.3917 0.058 Uiso 1 1 calc R . . C20 C 0.9192(2) 0.20646(10) 0.5334(3) 0.0465(10) Uani 1 1 d . . . H20 H 0.8914 0.2282 0.5325 0.056 Uiso 1 1 calc R . . C21 C 0.8896(2) 0.05647(10) 0.3122(3) 0.0384(8) Uani 1 1 d . . . H21 H 0.8947 0.0322 0.3343 0.046 Uiso 1 1 calc R . . C22 C 0.9185(2) 0.08217(10) 0.3922(3) 0.0414(9) Uani 1 1 d . . . H22 H 0.9431 0.0753 0.4661 0.050 Uiso 1 1 calc R . . C23 C 0.9108(2) 0.11875(10) 0.3621(3) 0.0371(8) Uani 1 1 d . . . C24 C 0.8758(3) 0.12664(10) 0.2498(3) 0.0543(11) Uani 1 1 d . . . H24 H 0.8704 0.1506 0.2249 0.065 Uiso 1 1 calc R . . C25 C 0.8490(3) 0.09912(10) 0.1746(3) 0.0511(10) Uani 1 1 d . . . H25 H 0.8258 0.1053 0.0992 0.061 Uiso 1 1 calc R . . C26 C 0.6795(2) 0.03227(12) 0.2641(3) 0.0493(11) Uani 1 1 d . . . H26 H 0.7229 0.0282 0.3187 0.059 Uiso 1 1 calc R . . C27 C 0.6067(2) 0.03438(13) 0.3062(3) 0.0582(12) Uani 1 1 d . . . H27 H 0.6016 0.0314 0.3875 0.070 Uiso 1 1 calc R . . C28 C 0.5405(2) 0.04095(15) 0.2290(3) 0.0646(14) Uani 1 1 d . . . C29 C 0.5535(2) 0.04651(18) 0.1090(4) 0.087(2) Uani 1 1 d . . . H29 H 0.5115 0.0519 0.0533 0.104 Uiso 1 1 calc R . . C30 C 0.6288(2) 0.04390(16) 0.0740(4) 0.0736(16) Uani 1 1 d . . . H30 H 0.6362 0.0480 -0.0061 0.088 Uiso 1 1 calc R . . C31 C 1.0489(7) 0.4163(5) 0.1852(13) 0.119(5) Uani 0.386(12) 1 d PD A 1 H31 H 1.0831 0.4290 0.1400 0.143 Uiso 0.386(12) 1 calc PR A 1 C32 C 1.0509(8) 0.3787(5) 0.1826(13) 0.157(7) Uani 0.386(12) 1 d PD A 1 H32 H 1.0857 0.3667 0.1365 0.188 Uiso 0.386(12) 1 calc PR A 1 C33 C 1.0000 0.3591(5) 0.2500 0.095(5) Uani 0.386(12) 2 d SPD . 1 C34 C 1.0000 0.3187(5) 0.2500 0.117(7) Uani 0.386(12) 2 d SPD . 1 C35 C 1.0681(4) 0.2986(6) 0.2293(18) 0.172(6) Uani 0.386(12) 1 d PDU A 1 H35 H 1.1146 0.3105 0.2151 0.206 Uiso 0.386(12) 1 calc PR A 1 C36 C 1.0652(4) 0.2612(6) 0.2302(17) 0.201(7) Uani 0.386(12) 1 d PDU A 1 H36 H 1.1108 0.2485 0.2163 0.242 Uiso 0.386(12) 1 calc PR A 1 N4 N 1.0000 0.4354(6) 0.2500 0.172(7) Uani 0.386(12) 2 d SPD . 1 N5 N 1.0000 0.2420(6) 0.2500 0.259(10) Uani 0.386(12) 2 d SPDU . 1 C31' C 1.0623(4) 0.4374(4) 0.2173(11) 0.119(5) Uani 0.614(12) 1 d PD A 2 H31' H 1.1055 0.4503 0.1946 0.143 Uiso 0.614(12) 1 calc PR A 2 C32' C 1.0651(4) 0.3995(4) 0.2159(11) 0.157(7) Uani 0.614(12) 1 d PD A 2 H32' H 1.1093 0.3875 0.1926 0.188 Uiso 0.614(12) 1 calc PR A 2 C33' C 1.0000 0.3800(4) 0.2500 0.095(5) Uani 0.614(12) 2 d SPD . 2 C34' C 1.0000 0.3393(4) 0.2500 0.117(7) Uani 0.614(12) 2 d SPD . 2 C35' C 1.0506(6) 0.3192(4) 0.1817(10) 0.172(6) Uani 0.614(12) 1 d PD A 2 H35' H 1.0852 0.3311 0.1350 0.206 Uiso 0.614(12) 1 calc PR A 2 C36' C 1.0487(6) 0.2815(4) 0.1843(9) 0.201(7) Uani 0.614(12) 1 d PD A 2 H36' H 1.0826 0.2688 0.1385 0.242 Uiso 0.614(12) 1 calc PR A 2 N4' N 1.0000 0.4557(4) 0.2500 0.172(7) Uani 0.614(12) 2 d SPD . 2 N5' N 1.0000 0.2621(5) 0.2500 0.259(10) Uani 0.614(12) 2 d SPD . 2 N1 N 0.97927(17) 0.20162(8) 0.6169(3) 0.0376(7) Uani 1 1 d . . . N2 N 0.85422(15) 0.06421(8) 0.2034(2) 0.0321(6) Uani 1 1 d . . . N3 N 0.69199(16) 0.03578(9) 0.1482(3) 0.0431(8) Uani 1 1 d . . . O1 O 1.31608(14) 0.48133(6) 0.21052(19) 0.0343(5) Uani 1 1 d . . . O2 O 1.25801(15) 0.47261(7) 0.0304(2) 0.0422(6) Uani 1 1 d . . . O3 O 1.40388(12) 0.43420(6) 0.3948(2) 0.0338(5) Uani 1 1 d . . . O4 O 1.28017(12) 0.44344(6) 0.44478(18) 0.0307(5) Uani 1 1 d . . . O5 O 1.31182(15) 0.35769(7) 0.4083(2) 0.0465(7) Uani 1 1 d . . . O6 O 1.02021(16) 0.28007(7) 0.6235(2) 0.0515(7) Uani 1 1 d . . . O7 O 1.11727(15) 0.24984(7) 0.7171(2) 0.0430(6) Uani 1 1 d . . . O8 O 0.91230(13) 0.00829(7) 0.0386(2) 0.0377(6) Uani 1 1 d D . . H8B H 0.9444 0.0038 0.0986 0.056 Uiso 1 1 d RD . . H8A H 0.9254 0.0276 0.0044 0.056 Uiso 1 1 d RD . . Ni1 Ni 1.0000 0.239267(16) 0.7500 0.03307(18) Uani 1 2 d S . . Ni2 Ni 0.80290(2) 0.024739(11) 0.09149(3) 0.02775(15) Uani 1 1 d . . . O9 O 1.0000 -0.02129(10) 0.2500 0.0445(9) Uani 1 2 d SD . . H9A H 1.0106 -0.0013 0.2171 0.067 Uiso 0.50 1 d PRD . . H9B H 1.0280 -0.0381 0.2245 0.067 Uiso 0.50 1 d PRD . . O10 O 0.7382(4) 0.2329(2) 0.3939(5) 0.253(5) Uani 1 1 d . . . O11 O 1.0837(11) 0.3378(6) -0.1203(18) 0.69(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0348(19) 0.043(2) 0.0260(18) -0.0025(16) 0.0076(15) -0.0070(16) C2 0.0338(19) 0.0265(17) 0.0220(16) 0.0055(13) 0.0050(14) -0.0011(14) C3 0.0356(19) 0.041(2) 0.0272(17) -0.0071(15) 0.0102(14) -0.0103(15) C4 0.052(2) 0.058(3) 0.033(2) -0.0109(18) 0.0085(17) -0.018(2) C5 0.073(3) 0.051(3) 0.048(2) -0.022(2) 0.019(2) -0.024(2) C6 0.067(3) 0.038(2) 0.063(3) -0.011(2) 0.022(2) -0.016(2) C7 0.037(2) 0.034(2) 0.044(2) -0.0005(16) 0.0159(16) -0.0058(15) C8 0.0278(17) 0.0325(19) 0.0312(18) -0.0040(14) 0.0119(14) -0.0042(14) C9 0.047(2) 0.035(2) 0.046(2) 0.0042(17) 0.0194(18) -0.0056(17) C10 0.042(2) 0.041(2) 0.056(2) 0.0088(19) 0.0120(19) -0.0009(17) C11 0.055(2) 0.033(2) 0.052(2) 0.0104(18) 0.0122(19) 0.0010(18) C12 0.049(2) 0.041(2) 0.045(2) 0.0098(18) 0.0158(18) -0.0025(18) C13 0.048(3) 0.070(3) 0.076(3) 0.029(3) 0.017(2) 0.005(2) C14 0.060(3) 0.058(3) 0.084(3) 0.035(3) 0.022(3) 0.009(2) C15 0.051(2) 0.038(2) 0.041(2) 0.0001(18) 0.0137(18) -0.0024(18) C16 0.041(2) 0.050(2) 0.045(2) -0.0115(19) -0.0060(17) 0.0124(18) C17 0.044(2) 0.040(2) 0.053(2) -0.0139(19) -0.0055(18) 0.0140(17) C18 0.039(2) 0.036(2) 0.0351(19) -0.0043(16) 0.0032(16) 0.0017(16) C19 0.056(2) 0.047(2) 0.040(2) -0.0024(18) -0.0118(18) 0.0120(19) C20 0.062(3) 0.034(2) 0.042(2) -0.0050(17) -0.0048(19) 0.0149(18) C21 0.042(2) 0.037(2) 0.0350(19) -0.0014(16) -0.0051(16) 0.0045(16) C22 0.046(2) 0.042(2) 0.0342(19) -0.0008(17) -0.0122(16) 0.0097(17) C23 0.037(2) 0.041(2) 0.0333(19) -0.0066(16) 0.0042(15) 0.0025(16) C24 0.089(3) 0.034(2) 0.038(2) 0.0032(18) -0.008(2) 0.003(2) C25 0.079(3) 0.043(2) 0.0292(19) 0.0023(18) -0.0093(19) 0.004(2) C26 0.029(2) 0.093(3) 0.0260(19) 0.003(2) 0.0032(15) 0.0027(19) C27 0.034(2) 0.115(4) 0.0264(19) 0.002(2) 0.0088(16) -0.001(2) C28 0.030(2) 0.132(4) 0.033(2) 0.000(2) 0.0081(17) 0.000(2) C29 0.030(2) 0.195(6) 0.036(2) 0.012(3) 0.0028(19) 0.011(3) C30 0.035(2) 0.153(5) 0.033(2) 0.013(3) 0.0064(18) 0.008(3) C31 0.053(5) 0.115(12) 0.191(11) 0.052(10) 0.019(6) 0.000(7) C32 0.068(7) 0.23(2) 0.176(13) 0.083(14) 0.019(7) 0.013(9) C33 0.070(7) 0.116(17) 0.098(8) 0.000 0.004(6) 0.000 C34 0.110(10) 0.15(2) 0.094(8) 0.000 0.006(7) 0.000 C35 0.154(8) 0.189(11) 0.174(10) -0.016(8) 0.018(7) -0.019(8) C36 0.214(10) 0.173(11) 0.213(11) -0.047(8) -0.005(8) 0.005(8) N4 0.098(8) 0.110(16) 0.311(18) 0.000 0.035(10) 0.000 N5 0.279(13) 0.245(14) 0.256(12) 0.000 0.038(9) 0.000 C31' 0.053(5) 0.115(12) 0.191(11) 0.052(10) 0.019(6) 0.000(7) C32' 0.068(7) 0.23(2) 0.176(13) 0.083(14) 0.019(7) 0.013(9) C33' 0.070(7) 0.116(17) 0.098(8) 0.000 0.004(6) 0.000 C34' 0.110(10) 0.15(2) 0.094(8) 0.000 0.006(7) 0.000 C35' 0.154(8) 0.189(11) 0.174(10) -0.016(8) 0.018(7) -0.019(8) C36' 0.214(10) 0.173(11) 0.213(11) -0.047(8) -0.005(8) 0.005(8) N4' 0.098(8) 0.110(16) 0.311(18) 0.000 0.035(10) 0.000 N5' 0.279(13) 0.245(14) 0.256(12) 0.000 0.038(9) 0.000 N1 0.0442(18) 0.0354(17) 0.0333(16) -0.0049(13) 0.0036(13) 0.0030(14) N2 0.0303(15) 0.0382(17) 0.0280(15) -0.0003(12) 0.0040(12) 0.0029(12) N3 0.0267(15) 0.077(2) 0.0264(15) 0.0029(15) 0.0052(12) 0.0009(15) O1 0.0415(14) 0.0352(13) 0.0251(12) -0.0004(10) -0.0027(10) -0.0059(10) O2 0.0482(15) 0.0533(16) 0.0239(12) 0.0051(11) -0.0040(11) -0.0097(12) O3 0.0252(12) 0.0407(14) 0.0358(13) 0.0001(11) 0.0048(10) 0.0031(10) O4 0.0272(12) 0.0424(14) 0.0232(11) -0.0040(10) 0.0058(9) -0.0019(10) O5 0.0482(16) 0.0402(15) 0.0522(16) 0.0137(13) 0.0107(13) -0.0080(12) O6 0.0474(17) 0.0517(17) 0.0573(17) 0.0160(14) 0.0161(14) 0.0008(13) O7 0.0455(15) 0.0391(14) 0.0449(15) 0.0100(12) 0.0074(12) -0.0040(12) O8 0.0322(13) 0.0445(14) 0.0367(13) 0.0031(11) 0.0056(10) 0.0046(11) Ni1 0.0384(4) 0.0302(4) 0.0314(3) 0.000 0.0076(3) 0.000 Ni2 0.0244(2) 0.0368(3) 0.0223(2) 0.00179(18) 0.00377(16) -0.00129(18) O9 0.036(2) 0.049(2) 0.049(2) 0.000 0.0110(17) 0.000 O10 0.245(8) 0.374(11) 0.123(4) -0.086(6) -0.081(5) 0.232(8) O11 0.53(2) 0.84(4) 0.75(3) -0.61(3) 0.38(2) -0.52(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.258(4) . ? C1 O1 1.263(4) . ? C1 C3 1.500(5) . ? C1 Ni2 2.436(4) 3 ? C2 O3 1.251(4) . ? C2 O4 1.269(4) . ? C2 C8 1.511(4) . ? C3 C4 1.398(5) . ? C3 C8 1.407(5) . ? C4 C5 1.372(6) . ? C4 H4 0.9300 . ? C5 C6 1.367(6) . ? C5 H5 0.9300 . ? C6 C7 1.391(5) . ? C6 H6 0.9300 . ? C7 C8 1.388(5) . ? C7 O5 1.397(4) . ? C9 C10 1.353(5) . ? C9 C14 1.366(6) . ? C9 O5 1.389(4) . ? C10 C11 1.404(5) . ? C10 H10 0.9300 . ? C11 C12 1.373(5) . ? C11 H11 0.9300 . ? C12 C13 1.382(5) . ? C12 C15 1.493(5) . ? C13 C14 1.390(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.265(4) . ? C15 O7 1.266(4) . ? C15 Ni1 2.439(4) . ? C16 N1 1.336(5) . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 C18 1.383(5) . ? C17 H17 0.9300 . ? C18 C19 1.392(5) . ? C18 C23 1.487(5) . ? C19 C20 1.373(5) . ? C19 H19 0.9300 . ? C20 N1 1.338(5) . ? C20 H20 0.9300 . ? C21 N2 1.344(4) . ? C21 C22 1.368(5) . ? C21 H21 0.9300 . ? C22 C23 1.395(5) . ? C22 H22 0.9300 . ? C23 C24 1.377(5) . ? C24 C25 1.373(5) . ? C24 H24 0.9300 . ? C25 N2 1.329(5) . ? C25 H25 0.9300 . ? C26 N3 1.340(4) . ? C26 C27 1.365(5) . ? C26 H26 0.9300 . ? C27 C28 1.382(5) . ? C27 H27 0.9300 . ? C28 C29 1.397(6) . ? C28 C28 1.494(7) 2_655 ? C29 C30 1.374(6) . ? C29 H29 0.9300 . ? C30 N3 1.336(5) . ? C30 H30 0.9300 . ? C31 N4 1.348(7) . ? C31 C32 1.387(9) . ? C31 H31 0.9300 . ? C32 C33 1.400(7) . ? C32 H32 0.9300 . ? C33 C32 1.400(7) 2_755 ? C33 C34 1.491(10) . ? C34 C35 1.410(7) 2_755 ? C34 C35 1.410(7) . ? C35 C36 1.383(9) . ? C35 H35 0.9300 . ? C36 N5 1.349(7) . ? C36 H36 0.9300 . ? N4 C31 1.348(7) 2_755 ? N5 C36 1.349(7) 2_755 ? C31' N4' 1.333(6) . ? C31' C32' 1.402(8) . ? C31' H31' 0.9300 . ? C32' C33' 1.400(6) . ? C32' H32' 0.9300 . ? C33' C32' 1.400(6) 2_755 ? C33' C34' 1.501(9) . ? C34' C35' 1.411(6) 2_755 ? C34' C35' 1.411(6) . ? C35' C36' 1.393(8) . ? C35' H35' 0.9300 . ? C36' N5' 1.358(7) . ? C36' H36' 0.9300 . ? N4' C31' 1.333(6) 2_755 ? N5' C36' 1.358(7) 2_755 ? N1 Ni1 2.047(3) . ? N2 Ni2 2.067(3) . ? N3 Ni2 2.081(3) . ? O1 Ni2 2.085(2) 3 ? O2 Ni2 2.160(2) 3 ? O4 Ni2 2.032(2) 8_556 ? O6 Ni1 2.117(3) . ? O7 Ni1 2.095(2) . ? O8 Ni2 2.090(2) . ? O8 H8B 0.8457 . ? O8 H8A 0.8474 . ? Ni1 N1 2.047(3) 2_756 ? Ni1 O7 2.095(2) 2_756 ? Ni1 O6 2.117(3) 2_756 ? Ni1 C15 2.439(4) 2_756 ? Ni2 O4 2.032(2) 8_455 ? Ni2 O1 2.085(2) 3_445 ? Ni2 O2 2.160(2) 3_445 ? Ni2 C1 2.436(4) 3_445 ? O9 H9A 0.8505 . ? O9 H9B 0.8470 . ? 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 O2 C1 O1 121.1(3) . . ? O2 C1 C3 120.2(3) . . ? O1 C1 C3 118.7(3) . . ? O2 C1 Ni2 62.27(18) . 3 ? O1 C1 Ni2 58.88(17) . 3 ? C3 C1 Ni2 176.4(3) . 3 ? O3 C2 O4 126.4(3) . . ? O3 C2 C8 117.3(3) . . ? O4 C2 C8 116.1(3) . . ? C4 C3 C8 120.1(3) . . ? C4 C3 C1 119.2(3) . . ? C8 C3 C1 120.8(3) . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 119.7(4) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C7 C6 121.9(3) . . ? C8 C7 O5 117.2(3) . . ? C6 C7 O5 120.8(3) . . ? C7 C8 C3 117.5(3) . . ? C7 C8 C2 118.4(3) . . ? C3 C8 C2 124.1(3) . . ? C10 C9 C14 121.2(3) . . ? C10 C9 O5 117.7(3) . . ? C14 C9 O5 120.8(3) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 118.6(3) . . ? C11 C12 C15 121.0(3) . . ? C13 C12 C15 120.4(4) . . ? C12 C13 C14 121.1(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C9 C14 C13 119.0(4) . . ? C9 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? O6 C15 O7 119.4(3) . . ? O6 C15 C12 120.2(3) . . ? O7 C15 C12 120.5(4) . . ? O6 C15 Ni1 60.18(19) . . ? O7 C15 Ni1 59.20(18) . . ? C12 C15 Ni1 178.2(3) . . ? N1 C16 C17 123.8(3) . . ? N1 C16 H16 118.1 . . ? C17 C16 H16 118.1 . . ? C16 C17 C18 119.0(3) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C19 117.3(3) . . ? C17 C18 C23 121.7(3) . . ? C19 C18 C23 120.9(3) . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? N1 C20 C19 122.8(3) . . ? N1 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N2 C21 C22 123.8(3) . . ? N2 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 119.4(3) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 116.8(3) . . ? C24 C23 C18 121.7(3) . . ? C22 C23 C18 121.5(3) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? N2 C25 C24 123.8(3) . . ? N2 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? N3 C26 C27 123.6(3) . . ? N3 C26 H26 118.2 . . ? C27 C26 H26 118.2 . . ? C26 C27 C28 120.5(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 116.3(3) . . ? C27 C28 C28 121.7(4) . 2_655 ? C29 C28 C28 122.0(4) . 2_655 ? C30 C29 C28 119.5(4) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N3 C30 C29 123.9(4) . . ? N3 C30 H30 118.1 . . ? C29 C30 H30 118.1 . . ? N4 C31 C32 123.4(6) . . ? N4 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C31 C32 C33 119.3(6) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C32 C33 C32 117.6(9) 2_755 . ? C32 C33 C34 121.2(4) 2_755 . ? C32 C33 C34 121.2(4) . . ? C35 C34 C35 116.6(9) 2_755 . ? C35 C34 C33 121.7(4) 2_755 . ? C35 C34 C33 121.7(4) . . ? C36 C35 C34 119.6(6) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? N5 C36 C35 123.7(6) . . ? N5 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C31 N4 C31 117.1(9) 2_755 . ? C36 N5 C36 116.8(10) . 2_755 ? N4' C31' C32' 122.6(5) . . ? N4' C31' H31' 118.7 . . ? C32' C31' H31' 118.7 . . ? C33' C32' C31' 118.8(5) . . ? C33' C32' H32' 120.6 . . ? C31' C32' H32' 120.6 . . ? C32' C33' C32' 118.1(8) . 2_755 ? C32' C33' C34' 120.9(4) . . ? C32' C33' C34' 120.9(4) 2_755 . ? C35' C34' C35' 116.5(8) 2_755 . ? C35' C34' C33' 121.7(4) 2_755 . ? C35' C34' C33' 121.7(4) . . ? C36' C35' C34' 119.8(5) . . ? C36' C35' H35' 120.1 . . ? C34' C35' H35' 120.1 . . ? N5' C36' C35' 123.7(6) . . ? N5' C36' H36' 118.2 . . ? C35' C36' H36' 118.2 . . ? C31' N4' C31' 119.1(8) 2_755 . ? C36' N5' C36' 116.4(9) . 2_755 ? C16 N1 C20 117.1(3) . . ? C16 N1 Ni1 123.1(2) . . ? C20 N1 Ni1 119.6(2) . . ? C25 N2 C21 116.2(3) . . ? C25 N2 Ni2 121.3(2) . . ? C21 N2 Ni2 122.3(2) . . ? C30 N3 C26 116.1(3) . . ? C30 N3 Ni2 123.7(2) . . ? C26 N3 Ni2 120.0(2) . . ? C1 O1 Ni2 89.9(2) . 3 ? C1 O2 Ni2 86.7(2) . 3 ? C2 O4 Ni2 126.5(2) . 8_556 ? C9 O5 C7 116.9(3) . . ? C15 O6 Ni1 88.6(2) . . ? C15 O7 Ni1 89.5(2) . . ? Ni2 O8 H8B 111.2 . . ? Ni2 O8 H8A 99.2 . . ? H8B O8 H8A 110.4 . . ? N1 Ni1 N1 94.53(16) . 2_756 ? N1 Ni1 O7 96.02(11) . . ? N1 Ni1 O7 98.50(11) 2_756 . ? N1 Ni1 O7 98.50(11) . 2_756 ? N1 Ni1 O7 96.02(11) 2_756 2_756 ? O7 Ni1 O7 158.54(14) . 2_756 ? N1 Ni1 O6 91.26(11) . . ? N1 Ni1 O6 160.64(11) 2_756 . ? O7 Ni1 O6 62.48(10) . . ? O7 Ni1 O6 101.37(10) 2_756 . ? N1 Ni1 O6 160.64(11) . 2_756 ? N1 Ni1 O6 91.26(11) 2_756 2_756 ? O7 Ni1 O6 101.37(10) . 2_756 ? O7 Ni1 O6 62.48(10) 2_756 2_756 ? O6 Ni1 O6 89.31(15) . 2_756 ? N1 Ni1 C15 129.63(13) . 2_756 ? N1 Ni1 C15 94.72(12) 2_756 2_756 ? O7 Ni1 C15 131.09(12) . 2_756 ? O7 Ni1 C15 31.26(11) 2_756 2_756 ? O6 Ni1 C15 95.75(11) . 2_756 ? O6 Ni1 C15 31.23(11) 2_756 2_756 ? N1 Ni1 C15 94.72(12) . . ? N1 Ni1 C15 129.63(13) 2_756 . ? O7 Ni1 C15 31.26(11) . . ? O7 Ni1 C15 131.09(12) 2_756 . ? O6 Ni1 C15 31.23(11) . . ? O6 Ni1 C15 95.75(11) 2_756 . ? C15 Ni1 C15 115.91(18) 2_756 . ? O4 Ni2 N2 97.22(10) 8_455 . ? O4 Ni2 N3 91.13(10) 8_455 . ? N2 Ni2 N3 91.30(11) . . ? O4 Ni2 O1 164.85(9) 8_455 3_445 ? N2 Ni2 O1 97.82(10) . 3_445 ? N3 Ni2 O1 90.31(11) . 3_445 ? O4 Ni2 O8 92.90(9) 8_455 . ? N2 Ni2 O8 92.14(10) . . ? N3 Ni2 O8 174.33(11) . . ? O1 Ni2 O8 84.77(9) 3_445 . ? O4 Ni2 O2 102.74(9) 8_455 3_445 ? N2 Ni2 O2 160.04(10) . 3_445 ? N3 Ni2 O2 88.08(12) . 3_445 ? O1 Ni2 O2 62.24(9) 3_445 3_445 ? O8 Ni2 O2 87.15(10) . 3_445 ? O4 Ni2 C1 133.67(10) 8_455 3_445 ? N2 Ni2 C1 129.05(11) . 3_445 ? N3 Ni2 C1 90.03(12) . 3_445 ? O1 Ni2 C1 31.24(10) 3_445 3_445 ? O8 Ni2 C1 84.30(10) . 3_445 ? O2 Ni2 C1 31.03(10) 3_445 3_445 ? H9A O9 H9B 110.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.533 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.070 #===END data_73992019 _database_code_depnum_ccdc_archive 'CCDC 739919' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H50 N6 Ni3 O20' _chemical_formula_weight 1351.17 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 'C c' _symmetry_space_group_name_Hall 'C -2yc' 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' _cell_length_a 11.336(3) _cell_length_b 19.518(6) _cell_length_c 27.059(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.092(5) _cell_angle_gamma 90.00 _cell_volume 5928(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2889 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.04 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8212 _exptl_absorpt_correction_T_max 0.9225 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 14329 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7325 _reflns_number_gt 6131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.1533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(3) _refine_ls_number_reflns 7325 _refine_ls_number_parameters 803 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2094 _refine_ls_wR_factor_gt 0.1986 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3387(9) 1.0911(6) 0.3357(4) 0.033(3) Uani 1 1 d . . . C2 C 0.2280(10) 0.9561(5) 0.3031(4) 0.031(2) Uani 1 1 d . . . C3 C 0.3171(8) 1.0718(5) 0.2822(4) 0.024(2) Uani 1 1 d . . . C4 C 0.3459(11) 1.1177(6) 0.2451(4) 0.038(3) Uani 1 1 d . . . H4 H 0.3812 1.1595 0.2547 0.045 Uiso 1 1 calc R . . C5 C 0.3235(13) 1.1021(6) 0.1976(4) 0.045(3) Uani 1 1 d . . . H5 H 0.3438 1.1334 0.1743 0.054 Uiso 1 1 calc R . . C6 C 0.2709(12) 1.0408(6) 0.1810(4) 0.042(3) Uani 1 1 d . . . H6 H 0.2562 1.0304 0.1471 0.050 Uiso 1 1 calc R . . C7 C 0.2409(10) 0.9957(5) 0.2165(4) 0.032(2) Uani 1 1 d . . . C8 C 0.2644(8) 1.0092(5) 0.2672(4) 0.022(2) Uani 1 1 d . . . C9 C 0.0963(9) 0.9302(5) 0.1626(4) 0.031(2) Uani 1 1 d . . . C10 C -0.0167(14) 0.9405(7) 0.1737(6) 0.057(4) Uani 1 1 d . . . H10 H -0.0294 0.9508 0.2061 0.069 Uiso 1 1 calc R . . C11 C -0.1111(14) 0.9353(8) 0.1356(6) 0.060(4) Uani 1 1 d U . . H11 H -0.1883 0.9414 0.1428 0.072 Uiso 1 1 calc R . . C12 C -0.0941(13) 0.9216(8) 0.0888(7) 0.065(4) Uani 1 1 d . . . H12 H -0.1587 0.9173 0.0636 0.078 Uiso 1 1 calc R . . C13 C 0.0246(10) 0.9137(6) 0.0779(5) 0.040(3) Uani 1 1 d . . . H13 H 0.0381 0.9068 0.0452 0.048 Uiso 1 1 calc R . . C14 C 0.1187(11) 0.9164(6) 0.1155(4) 0.035(3) Uani 1 1 d . . . C15 C 0.2426(9) 0.9071(5) 0.1019(4) 0.029(2) Uani 1 1 d . . . C16 C 0.4648(11) 0.7049(5) 0.0180(4) 0.031(2) Uani 1 1 d . . . C17 C 0.4221(11) 0.6453(6) -0.0074(4) 0.038(3) Uani 1 1 d . . . C18 C 0.4755(16) 0.5823(7) 0.0088(6) 0.064(5) Uani 1 1 d . . . H18 H 0.4486 0.5419 -0.0074 0.077 Uiso 1 1 calc R . . C19 C 0.5626(16) 0.5800(6) 0.0462(5) 0.064(5) Uani 1 1 d . . . H19 H 0.5968 0.5377 0.0554 0.077 Uiso 1 1 calc R . . C20 C 0.6053(12) 0.6368(6) 0.0724(5) 0.042(3) Uani 1 1 d . . . H20 H 0.6673 0.6342 0.0988 0.050 Uiso 1 1 calc R . . C21 C 0.5505(9) 0.6990(5) 0.0574(4) 0.028(2) Uani 1 1 d . . . C22 C 0.4114(9) 0.7758(5) 0.0013(4) 0.027(2) Uani 1 1 d . . . C23 C 0.3227(13) 0.6446(6) -0.0513(4) 0.042(3) Uani 1 1 d . . . C24 C 0.7062(9) 0.7623(5) 0.1109(4) 0.028(2) Uani 1 1 d . . . C25 C 0.7956(11) 0.7502(7) 0.0821(5) 0.046(3) Uani 1 1 d . . . H25 H 0.7771 0.7407 0.0482 0.055 Uiso 1 1 calc R . . C26 C 0.9128(10) 0.7526(6) 0.1045(6) 0.049(3) Uani 1 1 d . . . H26 H 0.9744 0.7451 0.0858 0.059 Uiso 1 1 calc R . . C27 C 0.9377(9) 0.7662(6) 0.1549(5) 0.040(3) Uani 1 1 d . . . H27 H 1.0162 0.7666 0.1705 0.048 Uiso 1 1 calc R . . C28 C 0.8474(9) 0.7791(5) 0.1814(4) 0.032(2) Uani 1 1 d . . . H28 H 0.8658 0.7902 0.2150 0.038 Uiso 1 1 calc R . . C29 C 0.7289(8) 0.7765(5) 0.1605(4) 0.025(2) Uani 1 1 d . . . C30 C 0.6380(8) 0.7900(4) 0.1936(4) 0.022(2) Uani 1 1 d . . . C31 C 0.1147(11) 1.0649(6) 0.4150(5) 0.040(3) Uani 1 1 d . . . H31 H 0.1538 1.0250 0.4079 0.048 Uiso 1 1 calc R . . C32 C -0.0038(10) 1.0616(6) 0.4157(5) 0.036(3) Uani 1 1 d . . . H32 H -0.0435 1.0202 0.4087 0.044 Uiso 1 1 calc R . . C33 C -0.0678(9) 1.1192(6) 0.4266(4) 0.031(2) Uani 1 1 d . . . C34 C -0.0020(11) 1.1769(6) 0.4360(6) 0.048(3) Uani 1 1 d . . . H34 H -0.0402 1.2171 0.4434 0.058 Uiso 1 1 calc R . . C35 C 0.1219(10) 1.1784(6) 0.4350(5) 0.037(3) Uani 1 1 d . . . H35 H 0.1636 1.2191 0.4420 0.045 Uiso 1 1 calc R . . C36 C -0.3871(11) 1.1767(6) 0.4240(5) 0.042(3) Uani 1 1 d . . . H36 H -0.4296 1.2176 0.4216 0.051 Uiso 1 1 calc R . . C37 C -0.2615(12) 1.1786(6) 0.4250(6) 0.054(4) Uani 1 1 d . . . H37 H -0.2229 1.2205 0.4238 0.065 Uiso 1 1 calc R . . C38 C -0.1971(9) 1.1189(6) 0.4277(4) 0.032(2) Uani 1 1 d . . . C39 C -0.2623(10) 1.0569(6) 0.4287(4) 0.036(3) Uani 1 1 d . . . H39 H -0.2246 1.0146 0.4293 0.044 Uiso 1 1 calc R . . C40 C -0.3814(10) 1.0619(6) 0.4287(5) 0.040(3) Uani 1 1 d . . . H40 H -0.4229 1.0211 0.4305 0.048 Uiso 1 1 calc R . . C41 C 0.5437(10) 0.6758(6) 0.2889(5) 0.040(3) Uani 1 1 d . . . H41 H 0.6236 0.6754 0.2846 0.049 Uiso 1 1 calc R . . C42 C 0.4847(10) 0.6138(5) 0.2872(5) 0.038(3) Uani 1 1 d . . . H42 H 0.5245 0.5734 0.2817 0.046 Uiso 1 1 calc R . . C43 C 0.3675(10) 0.6121(5) 0.2935(4) 0.033(2) Uani 1 1 d . . . C44 C 0.3117(10) 0.6752(5) 0.3013(5) 0.041(3) Uani 1 1 d . . . H44 H 0.2310 0.6773 0.3042 0.049 Uiso 1 1 calc R . . C45 C 0.3826(11) 0.7348(6) 0.3044(5) 0.042(3) Uani 1 1 d U . . H45 H 0.3482 0.7758 0.3125 0.051 Uiso 1 1 calc R . . C46 C 0.7946(11) 0.9247(6) 0.2939(4) 0.038(3) Uani 1 1 d . . . H46 H 0.8360 0.8838 0.2926 0.045 Uiso 1 1 calc R . . C47 C 0.8574(9) 0.9865(5) 0.2926(5) 0.034(3) Uani 1 1 d . . . H47 H 0.9388 0.9859 0.2912 0.041 Uiso 1 1 calc R . . C48 C 0.7994(10) 1.0467(5) 0.2935(4) 0.028(2) Uani 1 1 d . . . C49 C 0.6780(10) 1.0459(6) 0.2954(5) 0.042(3) Uani 1 1 d . . . H49 H 0.6343 1.0863 0.2950 0.050 Uiso 1 1 calc R . . C50 C 0.6216(10) 0.9795(6) 0.2982(5) 0.040(3) Uani 1 1 d U . . H50 H 0.5407 0.9782 0.3009 0.049 Uiso 1 1 calc R . . C51 C 0.3630(12) 0.6773(6) 0.1476(5) 0.042(3) Uani 1 1 d . . . H51 H 0.4271 0.6850 0.1725 0.050 Uiso 1 1 calc R . . C52 C 0.3006(13) 0.6175(7) 0.1501(5) 0.053(4) Uani 1 1 d . . . H52 H 0.3231 0.5859 0.1754 0.064 Uiso 1 1 calc R . . C53 C 0.2043(11) 0.6055(6) 0.1144(4) 0.037(3) Uani 1 1 d . . . C54 C 0.1787(10) 0.6553(5) 0.0776(5) 0.035(3) Uani 1 1 d . . . H54 H 0.1161 0.6485 0.0520 0.042 Uiso 1 1 calc R . . C55 C 0.2433(10) 0.7129(6) 0.0787(4) 0.036(3) Uani 1 1 d . . . H55 H 0.2211 0.7464 0.0548 0.043 Uiso 1 1 calc R . . C56 C 0.0479(11) 0.4477(5) 0.1500(4) 0.036(3) Uani 1 1 d . . . H56 H 0.0185 0.4307 0.1780 0.043 Uiso 1 1 calc R . . C57 C 0.0970(10) 0.5125(5) 0.1522(5) 0.038(3) Uani 1 1 d . . . H57 H 0.1002 0.5382 0.1813 0.045 Uiso 1 1 calc R . . C58 C 0.1415(11) 0.5393(6) 0.1115(5) 0.040(3) Uani 1 1 d . . . C59 C 0.1285(10) 0.5005(5) 0.0685(4) 0.031(2) Uani 1 1 d . . . H59 H 0.1539 0.5174 0.0396 0.037 Uiso 1 1 calc R . . C60 C 0.0768(9) 0.4354(5) 0.0688(4) 0.031(2) Uani 1 1 d . . . H60 H 0.0671 0.4099 0.0395 0.037 Uiso 1 1 calc R . . N1 N 0.1802(7) 1.1224(5) 0.4241(4) 0.031(2) Uani 1 1 d . . . N2 N -0.4444(8) 1.1187(5) 0.4264(4) 0.031(2) Uani 1 1 d U . . N3 N 0.4941(8) 0.7361(4) 0.2965(4) 0.035(2) Uani 1 1 d . . . N4 N 0.6779(8) 0.9220(4) 0.2970(4) 0.032(2) Uani 1 1 d . . . N5 N 0.3400(8) 0.7243(4) 0.1134(4) 0.032(2) Uani 1 1 d . . . N6 N 0.0409(8) 0.4085(5) 0.1092(3) 0.031(2) Uani 1 1 d . . . O1 O 0.3471(7) 1.1539(4) 0.3483(3) 0.0347(17) Uani 1 1 d . . . O2 O 0.3495(6) 1.0466(4) 0.3688(2) 0.0283(16) Uani 1 1 d . . . O3 O 0.1316(7) 0.9658(4) 0.3193(3) 0.044(2) Uani 1 1 d . . . O4 O 0.2969(8) 0.9052(4) 0.3134(3) 0.050(2) Uani 1 1 d . . . O5 O 0.1898(8) 0.9320(4) 0.2031(3) 0.0407(19) Uani 1 1 d . . . O6 O 0.3050(6) 0.8639(4) 0.1285(3) 0.0319(17) Uani 1 1 d . . . O7 O 0.2687(8) 0.9378(4) 0.0661(4) 0.050(2) Uani 1 1 d . . . O8 O 0.3488(9) 0.6276(4) -0.0923(3) 0.053(2) Uani 1 1 d . . . O9 O 0.2211(9) 0.6598(6) -0.0424(4) 0.062(3) Uani 1 1 d . . . O10 O 0.3883(6) 0.7853(4) -0.0445(3) 0.0309(16) Uani 1 1 d . . . O11 O 0.4003(6) 0.8184(3) 0.0335(3) 0.0232(15) Uani 1 1 d U . . O12 O 0.5874(6) 0.7583(4) 0.0860(3) 0.0314(17) Uani 1 1 d . . . O13 O 0.5258(6) 0.7959(4) 0.1772(3) 0.0292(16) Uani 1 1 d . . . O14 O 0.6757(6) 0.7959(4) 0.2400(3) 0.0288(16) Uani 1 1 d . . . O15 O 0.3782(7) 1.0526(4) 0.4820(3) 0.0385(19) Uani 1 1 d D . . H15A H 0.4077 1.0347 0.5097 0.058 Uiso 1 1 d RD . . H15B H 0.3225 1.0265 0.4687 0.058 Uiso 1 1 d RD . . O16 O 0.7384(8) 0.7863(4) 0.3415(3) 0.050(2) Uani 1 1 d D . . H16A H 0.6977 0.7924 0.3653 0.075 Uiso 1 1 d RD . . H16B H 0.7773 0.7492 0.3473 0.075 Uiso 1 1 d RD . . O17 O 0.5373(13) 0.8540(6) 0.3650(4) 0.085(4) Uani 1 1 d D . . H17A H 0.4721 0.8724 0.3519 0.127 Uiso 1 1 d RD . . H17B H 0.5669 0.8766 0.3904 0.127 Uiso 1 1 d RD . . O18 O 0.4479(7) 0.8721(3) 0.2540(3) 0.0364(18) Uani 1 1 d D . . H18A H 0.4016 0.8726 0.2767 0.055 Uiso 1 1 d RD . . H18C H 0.4432 0.8356 0.2388 0.055 Uiso 1 1 d RD . . O19 O 0.5726(15) 0.6370(7) -0.1159(6) 0.105(5) Uani 1 1 d D . . H19A H 0.5325 0.6373 -0.1454 0.158 Uiso 1 1 d RD . . H19B H 0.5999 0.5967 -0.1096 0.158 Uiso 1 1 d RD . . Ni1 Ni 0.36610(10) 1.12136(6) 0.42468(5) 0.0249(3) Uani 1 1 d . . . Ni2 Ni 0.44457(10) 0.81504(6) 0.10804(5) 0.0241(3) Uani 1 1 d . . . Ni3 Ni 0.59157(11) 0.82728(6) 0.29743(5) 0.0301(3) Uani 1 1 d . . . O20 O 0.0377(19) 0.7550(13) 0.3104(9) 0.169(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.011(5) 0.053(7) 0.037(6) 0.005(5) 0.005(4) 0.005(4) C2 0.031(6) 0.025(5) 0.035(6) -0.006(4) 0.004(4) -0.005(4) C3 0.017(5) 0.018(5) 0.036(6) -0.006(4) 0.006(4) -0.002(4) C4 0.048(7) 0.027(6) 0.039(7) 0.005(5) 0.011(5) -0.007(5) C5 0.071(9) 0.034(6) 0.032(7) 0.004(5) 0.013(6) 0.004(6) C6 0.053(8) 0.044(7) 0.029(6) 0.008(5) 0.008(5) -0.001(6) C7 0.032(6) 0.025(5) 0.039(6) -0.002(4) 0.008(4) 0.006(4) C8 0.011(4) 0.024(5) 0.031(5) 0.002(4) 0.006(4) -0.001(4) C9 0.027(6) 0.022(5) 0.046(7) -0.001(4) 0.008(5) -0.001(4) C10 0.060(9) 0.051(8) 0.069(10) 0.001(7) 0.037(8) 0.008(7) C11 0.050(5) 0.061(5) 0.071(6) 0.004(4) 0.011(4) 0.003(4) C12 0.031(7) 0.064(9) 0.097(13) 0.025(8) -0.002(7) 0.000(7) C13 0.034(7) 0.034(6) 0.051(7) 0.000(5) -0.001(5) 0.008(5) C14 0.047(7) 0.031(6) 0.026(6) -0.008(4) 0.006(5) -0.014(5) C15 0.023(5) 0.023(5) 0.043(7) -0.002(5) 0.013(5) 0.008(4) C16 0.042(6) 0.021(5) 0.032(6) 0.002(4) 0.011(5) 0.002(5) C17 0.043(7) 0.038(6) 0.032(6) -0.001(5) 0.004(5) 0.006(5) C18 0.094(12) 0.027(7) 0.062(9) -0.020(6) -0.020(8) 0.011(7) C19 0.113(14) 0.021(6) 0.047(8) 0.006(5) -0.025(8) 0.016(7) C20 0.049(8) 0.031(6) 0.039(7) 0.004(5) -0.016(6) 0.011(5) C21 0.028(6) 0.027(5) 0.030(6) -0.002(4) 0.010(4) 0.000(4) C22 0.019(5) 0.029(6) 0.035(6) 0.005(4) 0.006(4) -0.010(4) C23 0.055(9) 0.035(6) 0.031(7) -0.008(5) -0.009(6) -0.002(6) C24 0.012(5) 0.021(5) 0.049(7) -0.006(4) -0.001(4) 0.000(4) C25 0.027(7) 0.056(8) 0.058(8) -0.005(6) 0.013(5) 0.011(5) C26 0.015(6) 0.048(7) 0.089(11) 0.011(7) 0.021(6) 0.006(5) C27 0.010(5) 0.042(7) 0.069(9) 0.001(6) 0.005(5) 0.001(4) C28 0.028(6) 0.018(5) 0.049(7) -0.002(4) -0.002(5) -0.001(4) C29 0.014(5) 0.024(5) 0.037(6) -0.001(4) 0.002(4) 0.005(4) C30 0.018(5) 0.004(4) 0.045(6) 0.003(4) 0.003(4) 0.000(3) C31 0.036(7) 0.039(7) 0.049(7) -0.007(5) 0.021(5) -0.006(5) C32 0.027(6) 0.031(6) 0.052(7) -0.007(5) 0.012(5) -0.007(5) C33 0.016(5) 0.039(6) 0.037(6) 0.001(5) 0.001(4) 0.003(4) C34 0.023(6) 0.031(6) 0.092(11) -0.008(6) 0.012(6) 0.004(5) C35 0.021(6) 0.025(6) 0.067(8) -0.011(5) 0.012(5) -0.002(4) C36 0.036(7) 0.019(5) 0.074(9) 0.004(5) 0.018(6) -0.004(5) C37 0.027(6) 0.037(7) 0.105(12) -0.009(7) 0.029(7) -0.010(5) C38 0.020(6) 0.038(6) 0.039(7) 0.004(5) 0.009(5) 0.005(4) C39 0.030(6) 0.030(6) 0.048(7) -0.001(5) 0.003(5) -0.001(5) C40 0.021(6) 0.037(7) 0.061(8) 0.001(5) 0.006(5) -0.005(5) C41 0.022(6) 0.035(6) 0.064(8) 0.002(5) 0.008(5) -0.011(5) C42 0.023(6) 0.019(5) 0.071(8) 0.009(5) 0.002(5) -0.002(4) C43 0.032(6) 0.020(5) 0.045(7) -0.011(4) 0.002(5) -0.017(4) C44 0.027(6) 0.016(5) 0.083(9) -0.003(5) 0.021(6) -0.003(4) C45 0.039(5) 0.035(4) 0.055(5) -0.005(4) 0.014(4) -0.004(4) C46 0.046(7) 0.022(5) 0.047(7) 0.004(5) 0.007(5) 0.001(5) C47 0.009(5) 0.031(6) 0.064(8) -0.002(5) 0.009(4) -0.006(4) C48 0.034(6) 0.018(5) 0.034(6) 0.000(4) 0.010(4) -0.007(4) C49 0.023(6) 0.029(6) 0.075(9) -0.007(5) 0.010(5) -0.001(4) C50 0.029(4) 0.040(4) 0.053(5) -0.002(4) 0.010(4) -0.002(4) C51 0.043(7) 0.033(6) 0.045(7) 0.005(5) -0.007(5) -0.016(5) C52 0.056(9) 0.045(8) 0.058(9) 0.012(6) 0.002(7) -0.019(6) C53 0.042(7) 0.028(6) 0.041(7) -0.001(5) 0.010(5) -0.010(5) C54 0.025(6) 0.023(5) 0.053(7) 0.002(5) -0.005(5) -0.001(4) C55 0.032(6) 0.032(6) 0.043(7) 0.006(5) 0.006(5) 0.004(5) C56 0.047(7) 0.024(5) 0.040(6) -0.003(5) 0.013(5) -0.009(5) C57 0.038(6) 0.015(5) 0.064(8) -0.011(5) 0.018(6) -0.008(4) C58 0.037(7) 0.044(7) 0.040(7) 0.015(5) 0.006(5) -0.006(5) C59 0.033(6) 0.021(5) 0.040(6) 0.003(4) 0.007(4) -0.009(4) C60 0.028(6) 0.031(6) 0.034(6) -0.006(4) 0.001(4) -0.012(4) N1 0.014(4) 0.032(5) 0.048(6) -0.005(4) 0.010(4) -0.009(4) N2 0.018(4) 0.039(4) 0.036(4) -0.003(3) 0.006(3) 0.003(3) N3 0.027(5) 0.023(5) 0.054(6) -0.001(4) 0.003(4) -0.003(4) N4 0.028(5) 0.015(4) 0.054(6) 0.002(4) 0.006(4) -0.003(3) N5 0.025(5) 0.026(5) 0.044(5) -0.005(4) 0.003(4) -0.004(4) N6 0.020(5) 0.028(5) 0.043(6) 0.000(4) 0.003(4) -0.007(4) O1 0.032(4) 0.037(4) 0.035(4) -0.010(3) 0.004(3) 0.007(3) O2 0.019(4) 0.038(4) 0.028(4) -0.001(3) 0.006(3) 0.001(3) O3 0.030(5) 0.051(5) 0.052(5) 0.001(4) 0.013(4) -0.005(4) O4 0.056(6) 0.032(5) 0.068(6) 0.013(4) 0.028(5) 0.017(4) O5 0.065(6) 0.023(4) 0.034(4) -0.006(3) 0.005(4) -0.005(4) O6 0.024(4) 0.026(4) 0.046(5) 0.000(3) 0.005(3) 0.005(3) O7 0.053(6) 0.041(5) 0.063(6) 0.019(4) 0.032(5) 0.013(4) O8 0.067(7) 0.040(5) 0.048(6) -0.011(4) -0.006(5) 0.017(4) O9 0.043(6) 0.069(7) 0.074(7) -0.003(5) 0.005(5) -0.011(5) O10 0.023(4) 0.030(4) 0.036(4) 0.005(3) -0.004(3) 0.002(3) O11 0.025(3) 0.011(3) 0.033(3) -0.002(2) 0.006(3) -0.006(2) O12 0.009(3) 0.034(4) 0.050(5) -0.006(3) -0.001(3) 0.005(3) O13 0.019(4) 0.029(4) 0.039(4) 0.001(3) 0.004(3) -0.010(3) O14 0.014(3) 0.030(4) 0.041(5) 0.002(3) 0.001(3) 0.004(3) O15 0.035(5) 0.043(5) 0.037(4) 0.007(3) 0.005(3) 0.010(4) O16 0.052(6) 0.041(5) 0.054(6) -0.005(4) -0.006(4) -0.004(4) O17 0.125(11) 0.062(7) 0.076(8) -0.029(6) 0.047(7) -0.045(7) O18 0.030(4) 0.018(4) 0.065(5) 0.000(3) 0.018(4) 0.000(3) O19 0.130(13) 0.080(9) 0.107(11) -0.016(7) 0.022(9) 0.019(8) Ni1 0.0143(6) 0.0271(7) 0.0338(7) -0.0046(5) 0.0051(5) -0.0026(5) Ni2 0.0211(7) 0.0163(6) 0.0348(7) 0.0001(5) 0.0035(5) -0.0042(5) Ni3 0.0309(8) 0.0186(6) 0.0416(8) -0.0005(5) 0.0083(6) -0.0089(5) O20 0.107(15) 0.21(2) 0.19(2) -0.027(16) 0.024(14) 0.017(14) _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 C1 O2 1.240(13) . ? C1 O1 1.273(14) . ? C1 C3 1.482(15) . ? C1 Ni1 2.456(11) . ? C2 O3 1.248(14) . ? C2 O4 1.269(13) . ? C2 C8 1.516(14) . ? C3 C8 1.395(13) . ? C3 C4 1.418(15) . ? C4 C5 1.311(17) . ? C4 H4 0.9300 . ? C5 C6 1.385(17) . ? C5 H5 0.9300 . ? C6 C7 1.380(16) . ? C6 H6 0.9300 . ? C7 C8 1.386(15) . ? C7 O5 1.397(13) . ? C9 C14 1.360(16) . ? C9 C10 1.372(18) . ? C9 O5 1.413(14) . ? C10 C11 1.38(2) . ? C10 H10 0.9300 . ? C11 C12 1.34(2) . ? C11 H11 0.9300 . ? C12 C13 1.43(2) . ? C12 H12 0.9300 . ? C13 C14 1.368(17) . ? C13 H13 0.9300 . ? C14 C15 1.513(16) . ? C15 O7 1.210(13) . ? C15 O6 1.258(13) . ? C16 C21 1.342(15) . ? C16 C17 1.401(16) . ? C16 C22 1.552(14) . ? C17 C18 1.414(18) . ? C17 C23 1.518(17) . ? C18 C19 1.31(2) . ? C18 H18 0.9300 . ? C19 C20 1.368(18) . ? C19 H19 0.9300 . ? C20 C21 1.397(15) . ? C20 H20 0.9300 . ? C21 O12 1.423(13) . ? C22 O11 1.223(12) . ? C22 O10 1.246(12) . ? C23 O8 1.235(16) . ? C23 O9 1.244(17) . ? C24 C29 1.358(15) . ? C24 C25 1.383(16) . ? C24 O12 1.420(12) . ? C25 C26 1.382(18) . ? C25 H25 0.9300 . ? C26 C27 1.377(19) . ? C26 H26 0.9300 . ? C27 C28 1.354(16) . ? C27 H27 0.9300 . ? C28 C29 1.383(14) . ? C28 H28 0.9300 . ? C29 C30 1.481(14) . ? C30 O14 1.276(12) . ? C30 O13 1.292(12) . ? C31 N1 1.350(14) . ? C31 C32 1.347(17) . ? C31 H31 0.9300 . ? C32 C33 1.392(16) . ? C32 H32 0.9300 . ? C33 C34 1.356(16) . ? C33 C38 1.470(13) . ? C34 C35 1.410(17) . ? C34 H34 0.9300 . ? C35 N1 1.332(14) . ? C35 H35 0.9300 . ? C36 N2 1.310(14) . ? C36 C37 1.420(18) . ? C36 H36 0.9300 . ? C37 C38 1.372(17) . ? C37 H37 0.9300 . ? C38 C39 1.419(15) . ? C39 C40 1.355(17) . ? C39 H39 0.9300 . ? C40 N2 1.315(15) . ? C40 H40 0.9300 . ? C41 N3 1.333(15) . ? C41 C42 1.381(15) . ? C41 H41 0.9300 . ? C42 C43 1.363(16) . ? C42 H42 0.9300 . ? C43 C44 1.413(15) . ? C43 C48 1.491(13) 3_445 ? C44 C45 1.410(15) . ? C44 H44 0.9300 . ? C45 N3 1.311(15) . ? C45 H45 0.9300 . ? C46 N4 1.338(16) . ? C46 C47 1.402(15) . ? C46 H46 0.9300 . ? C47 C48 1.349(15) . ? C47 H47 0.9300 . ? C48 C49 1.385(16) . ? C48 C43 1.491(13) 3 ? C49 C50 1.453(16) . ? C49 H49 0.9300 . ? C50 N4 1.293(15) . ? C50 H50 0.9300 . ? C51 N5 1.304(15) . ? C51 C52 1.370(16) . ? C51 H51 0.9300 . ? C52 C53 1.373(19) . ? C52 H52 0.9300 . ? C53 C54 1.393(16) . ? C53 C58 1.471(16) . ? C54 C55 1.340(16) . ? C54 H54 0.9300 . ? C55 N5 1.357(15) . ? C55 H55 0.9300 . ? C56 N6 1.337(14) . ? C56 C57 1.380(14) . ? C56 H56 0.9300 . ? C57 C58 1.377(16) . ? C57 H57 0.9300 . ? C58 C59 1.379(17) . ? C59 C60 1.401(14) . ? C59 H59 0.9300 . ? C60 N6 1.327(14) . ? C60 H60 0.9300 . ? N1 Ni1 2.105(8) . ? N2 Ni1 2.143(9) 1_455 ? N3 Ni3 2.093(9) . ? N4 Ni3 2.094(8) . ? N5 Ni2 2.148(9) . ? N6 Ni2 2.123(9) 3_445 ? O1 Ni1 2.144(8) . ? O2 Ni1 2.090(7) . ? O6 Ni2 1.991(7) . ? O10 Ni1 2.004(7) 2_574 ? O11 Ni2 2.010(7) . ? O12 Ni2 2.115(7) . ? O13 Ni2 2.000(7) . ? O14 Ni3 2.028(7) . ? O15 Ni1 2.042(8) . ? O15 H15A 0.8500 . ? O15 H15B 0.8500 . ? O16 Ni3 2.067(9) . ? O16 H16A 0.8502 . ? O16 H16B 0.8499 . ? O17 Ni3 2.077(11) . ? O17 H17A 0.8528 . ? O17 H17B 0.8455 . ? O18 Ni3 2.064(8) . ? O18 H18A 0.8632 . ? O18 H18C 0.8208 . ? O19 H19A 0.8610 . ? O19 H19B 0.8529 . ? Ni1 O10 2.004(7) 2_575 ? Ni1 N2 2.143(9) 1_655 ? Ni2 N6 2.123(9) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 119.0(10) . . ? O2 C1 C3 120.9(10) . . ? O1 C1 C3 120.1(10) . . ? O2 C1 Ni1 58.3(6) . . ? O1 C1 Ni1 60.8(6) . . ? C3 C1 Ni1 177.6(7) . . ? O3 C2 O4 125.7(10) . . ? O3 C2 C8 116.9(9) . . ? O4 C2 C8 117.4(9) . . ? C8 C3 C4 118.6(9) . . ? C8 C3 C1 120.8(9) . . ? C4 C3 C1 120.5(9) . . ? C5 C4 C3 121.1(11) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 122.3(11) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C7 C6 C5 117.5(11) . . ? C7 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? C6 C7 C8 122.5(10) . . ? C6 C7 O5 121.4(10) . . ? C8 C7 O5 116.1(9) . . ? C7 C8 C3 118.0(9) . . ? C7 C8 C2 118.2(9) . . ? C3 C8 C2 123.8(9) . . ? C14 C9 C10 122.5(12) . . ? C14 C9 O5 120.9(10) . . ? C10 C9 O5 116.6(11) . . ? C11 C10 C9 118.3(14) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C12 C11 C10 121.6(15) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 118.9(14) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.2(13) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C9 C14 C13 118.4(12) . . ? C9 C14 C15 123.7(10) . . ? C13 C14 C15 117.9(10) . . ? O7 C15 O6 127.4(10) . . ? O7 C15 C14 118.4(10) . . ? O6 C15 C14 114.0(9) . . ? C21 C16 C17 118.7(10) . . ? C21 C16 C22 121.1(9) . . ? C17 C16 C22 120.2(10) . . ? C16 C17 C18 117.9(11) . . ? C16 C17 C23 124.0(10) . . ? C18 C17 C23 118.1(11) . . ? C19 C18 C17 120.7(12) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 123.1(11) . . ? C18 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C19 C20 C21 116.3(10) . . ? C19 C20 H20 121.8 . . ? C21 C20 H20 121.8 . . ? C16 C21 C20 123.2(10) . . ? C16 C21 O12 119.1(9) . . ? C20 C21 O12 117.7(9) . . ? O11 C22 O10 125.4(10) . . ? O11 C22 C16 118.4(9) . . ? O10 C22 C16 116.2(9) . . ? O8 C23 O9 125.7(12) . . ? O8 C23 C17 117.5(13) . . ? O9 C23 C17 116.8(11) . . ? C29 C24 C25 122.6(10) . . ? C29 C24 O12 121.0(9) . . ? C25 C24 O12 116.4(10) . . ? C24 C25 C26 118.8(12) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C27 C26 C25 119.4(11) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C28 C27 C26 119.7(10) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 122.7(11) . . ? C27 C28 H28 118.7 . . ? C29 C28 H28 118.7 . . ? C24 C29 C28 116.7(9) . . ? C24 C29 C30 125.6(9) . . ? C28 C29 C30 117.7(9) . . ? O14 C30 O13 120.5(9) . . ? O14 C30 C29 116.5(8) . . ? O13 C30 C29 123.0(9) . . ? N1 C31 C32 124.2(11) . . ? N1 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C31 C32 C33 121.0(11) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 115.0(10) . . ? C34 C33 C38 121.5(10) . . ? C32 C33 C38 123.5(10) . . ? C33 C34 C35 122.5(11) . . ? C33 C34 H34 118.7 . . ? C35 C34 H34 118.7 . . ? N1 C35 C34 120.9(10) . . ? N1 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? N2 C36 C37 121.6(11) . . ? N2 C36 H36 119.2 . . ? C37 C36 H36 119.2 . . ? C38 C37 C36 120.2(11) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 116.8(10) . . ? C37 C38 C33 121.3(10) . . ? C39 C38 C33 121.8(10) . . ? C40 C39 C38 117.4(11) . . ? C40 C39 H39 121.3 . . ? C38 C39 H39 121.3 . . ? N2 C40 C39 126.5(11) . . ? N2 C40 H40 116.7 . . ? C39 C40 H40 116.7 . . ? N3 C41 C42 124.5(11) . . ? N3 C41 H41 117.7 . . ? C42 C41 H41 117.7 . . ? C43 C42 C41 119.5(10) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 117.5(9) . . ? C42 C43 C48 122.2(10) . 3_445 ? C44 C43 C48 120.2(10) . 3_445 ? C45 C44 C43 117.7(10) . . ? C45 C44 H44 121.2 . . ? C43 C44 H44 121.2 . . ? N3 C45 C44 124.1(11) . . ? N3 C45 H45 117.9 . . ? C44 C45 H45 117.9 . . ? N4 C46 C47 123.0(10) . . ? N4 C46 H46 118.5 . . ? C47 C46 H46 118.5 . . ? C48 C47 C46 119.9(10) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 118.7(9) . . ? C47 C48 C43 119.5(10) . 3 ? C49 C48 C43 121.8(10) . 3 ? C48 C49 C50 117.4(10) . . ? C48 C49 H49 121.3 . . ? C50 C49 H49 121.3 . . ? N4 C50 C49 123.4(10) . . ? N4 C50 H50 118.3 . . ? C49 C50 H50 118.3 . . ? N5 C51 C52 125.5(11) . . ? N5 C51 H51 117.3 . . ? C52 C51 H51 117.3 . . ? C53 C52 C51 118.5(12) . . ? C53 C52 H52 120.8 . . ? C51 C52 H52 120.8 . . ? C52 C53 C54 116.6(10) . . ? C52 C53 C58 121.3(11) . . ? C54 C53 C58 121.6(10) . . ? C55 C54 C53 120.8(11) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C54 C55 N5 122.5(10) . . ? C54 C55 H55 118.7 . . ? N5 C55 H55 118.7 . . ? N6 C56 C57 122.5(11) . . ? N6 C56 H56 118.7 . . ? C57 C56 H56 118.7 . . ? C58 C57 C56 120.3(11) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 117.3(11) . . ? C57 C58 C53 121.3(11) . . ? C59 C58 C53 121.4(10) . . ? C58 C59 C60 119.2(10) . . ? C58 C59 H59 120.4 . . ? C60 C59 H59 120.4 . . ? N6 C60 C59 122.8(10) . . ? N6 C60 H60 118.6 . . ? C59 C60 H60 118.6 . . ? C35 N1 C31 116.5(9) . . ? C35 N1 Ni1 122.3(7) . . ? C31 N1 Ni1 121.2(8) . . ? C36 N2 C40 117.4(10) . . ? C36 N2 Ni1 118.8(8) . 1_455 ? C40 N2 Ni1 123.8(8) . 1_455 ? C45 N3 C41 116.4(9) . . ? C45 N3 Ni3 122.3(8) . . ? C41 N3 Ni3 121.3(7) . . ? C50 N4 C46 117.6(9) . . ? C50 N4 Ni3 122.2(8) . . ? C46 N4 Ni3 120.1(7) . . ? C51 N5 C55 116.0(10) . . ? C51 N5 Ni2 124.8(8) . . ? C55 N5 Ni2 119.2(7) . . ? C60 N6 C56 117.6(9) . . ? C60 N6 Ni2 123.0(7) . 3_445 ? C56 N6 Ni2 118.4(7) . 3_445 ? C1 O1 Ni1 88.0(6) . . ? C1 O2 Ni1 91.4(7) . . ? C7 O5 C9 117.5(8) . . ? C15 O6 Ni2 124.5(7) . . ? C22 O10 Ni1 123.1(7) . 2_574 ? C22 O11 Ni2 131.0(7) . . ? C21 O12 C24 119.3(7) . . ? C21 O12 Ni2 113.7(6) . . ? C24 O12 Ni2 123.3(6) . . ? C30 O13 Ni2 129.7(7) . . ? C30 O14 Ni3 130.8(6) . . ? Ni1 O15 H15A 156.1 . . ? Ni1 O15 H15B 96.1 . . ? H15A O15 H15B 107.7 . . ? Ni3 O16 H16A 84.5 . . ? Ni3 O16 H16B 142.2 . . ? H16A O16 H16B 107.7 . . ? Ni3 O17 H17A 94.9 . . ? Ni3 O17 H17B 135.6 . . ? H17A O17 H17B 110.0 . . ? Ni3 O18 H18A 96.3 . . ? Ni3 O18 H18C 84.7 . . ? H18A O18 H18C 111.3 . . ? H19A O19 H19B 108.8 . . ? O10 Ni1 O15 106.9(3) 2_575 . ? O10 Ni1 O2 158.2(3) 2_575 . ? O15 Ni1 O2 94.6(3) . . ? O10 Ni1 N1 93.5(3) 2_575 . ? O15 Ni1 N1 88.4(4) . . ? O2 Ni1 N1 90.8(3) . . ? O10 Ni1 N2 86.9(3) 2_575 1_655 ? O15 Ni1 N2 90.5(3) . 1_655 ? O2 Ni1 N2 89.3(3) . 1_655 ? N1 Ni1 N2 178.8(4) . 1_655 ? O10 Ni1 O1 97.0(3) 2_575 . ? O15 Ni1 O1 156.1(3) . . ? O2 Ni1 O1 61.5(3) . . ? N1 Ni1 O1 91.5(4) . . ? N2 Ni1 O1 89.6(3) 1_655 . ? O10 Ni1 C1 128.2(4) 2_575 . ? O15 Ni1 C1 124.9(4) . . ? O2 Ni1 C1 30.3(3) . . ? N1 Ni1 C1 90.4(4) . . ? N2 Ni1 C1 90.2(3) 1_655 . ? O1 Ni1 C1 31.2(3) . . ? O6 Ni2 O13 96.3(3) . . ? O6 Ni2 O11 99.6(3) . . ? O13 Ni2 O11 164.1(3) . . ? O6 Ni2 O12 177.0(3) . . ? O13 Ni2 O12 84.0(3) . . ? O11 Ni2 O12 80.0(3) . . ? O6 Ni2 N6 90.7(3) . 3 ? O13 Ni2 N6 88.8(3) . 3 ? O11 Ni2 N6 92.4(3) . 3 ? O12 Ni2 N6 92.4(3) . 3 ? O6 Ni2 N5 84.7(3) . . ? O13 Ni2 N5 88.2(3) . . ? O11 Ni2 N5 91.9(3) . . ? O12 Ni2 N5 92.3(3) . . ? N6 Ni2 N5 174.2(4) 3 . ? O14 Ni3 O18 96.3(3) . . ? O14 Ni3 O16 84.1(3) . . ? O18 Ni3 O16 177.7(3) . . ? O14 Ni3 O17 168.5(5) . . ? O18 Ni3 O17 95.0(5) . . ? O16 Ni3 O17 84.5(5) . . ? O14 Ni3 N3 92.2(3) . . ? O18 Ni3 N3 88.9(3) . . ? O16 Ni3 N3 93.4(4) . . ? O17 Ni3 N3 90.2(4) . . ? O14 Ni3 N4 89.5(3) . . ? O18 Ni3 N4 87.4(3) . . ? O16 Ni3 N4 90.4(3) . . ? O17 Ni3 N4 88.9(4) . . ? N3 Ni3 N4 176.0(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.885 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.153 #===END data_739920 _database_code_depnum_ccdc_archive 'CCDC 739920' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H54 N8 Ni3 O18, 2(H2 O)' _chemical_formula_sum 'C70 H58 N8 Ni3 O20 ' _chemical_formula_weight 1507.31 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.990(3) _cell_length_b 22.497(7) _cell_length_c 14.764(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.521(5) _cell_angle_gamma 90.00 _cell_volume 3262.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4904 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 26.80 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1556 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8488 _exptl_absorpt_correction_T_max 0.9285 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 18651 _diffrn_reflns_av_R_equivalents 0.1187 _diffrn_reflns_av_sigmaI/netI 0.1234 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.66 _reflns_number_total 7414 _reflns_number_gt 5097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.0652P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7414 _refine_ls_number_parameters 457 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2193(3) 0.56325(16) 0.6318(2) 0.0315(7) Uani 1 1 d . . . C2 C 0.4887(3) 0.62692(14) 0.63755(19) 0.0270(6) Uani 1 1 d . . . C3 C 0.3311(3) 0.56200(15) 0.7164(2) 0.0306(7) Uani 1 1 d . . . C4 C 0.3105(3) 0.53008(17) 0.7930(2) 0.0413(8) Uani 1 1 d . . . H4 H 0.2317 0.5075 0.7899 0.050 Uiso 1 1 calc R . . C5 C 0.4045(4) 0.53128(19) 0.8731(2) 0.0461(9) Uani 1 1 d . . . H5 H 0.3889 0.5097 0.9239 0.055 Uiso 1 1 calc R . . C6 C 0.5215(3) 0.56417(17) 0.8788(2) 0.0403(8) Uani 1 1 d . . . H6 H 0.5853 0.5651 0.9332 0.048 Uiso 1 1 calc R . . C7 C 0.5431(3) 0.59566(15) 0.8029(2) 0.0298(7) Uani 1 1 d . . . C8 C 0.4506(3) 0.59503(14) 0.72043(19) 0.0266(6) Uani 1 1 d . . . C9 C 0.7763(3) 0.61581(16) 0.8605(2) 0.0326(7) Uani 1 1 d . . . C10 C 0.8415(4) 0.5647(2) 0.8405(3) 0.0506(10) Uani 1 1 d . . . H10 H 0.7996 0.5392 0.7943 0.061 Uiso 1 1 calc R . . C11 C 0.9692(4) 0.5518(2) 0.8896(3) 0.0644(12) Uani 1 1 d . . . H11 H 1.0126 0.5167 0.8782 0.077 Uiso 1 1 calc R . . C12 C 1.0324(4) 0.5909(2) 0.9553(3) 0.0663(13) Uani 1 1 d . . . H12 H 1.1200 0.5829 0.9867 0.080 Uiso 1 1 calc R . . C13 C 0.9668(3) 0.6419(2) 0.9751(3) 0.0483(10) Uani 1 1 d . . . H13 H 1.0105 0.6680 1.0197 0.058 Uiso 1 1 calc R . . C14 C 0.8352(3) 0.65460(16) 0.9286(2) 0.0317(7) Uani 1 1 d . . . C15 C 0.7630(3) 0.70876(16) 0.95380(19) 0.0304(7) Uani 1 1 d . . . C16 C -0.0665(3) 0.45035(16) 0.6764(2) 0.0358(8) Uani 1 1 d . . . H15 H 0.0279 0.4492 0.6925 0.043 Uiso 1 1 calc R . . C17 C -0.1412(3) 0.42433(16) 0.7348(2) 0.0350(7) Uani 1 1 d . . . H16 H -0.0978 0.4067 0.7893 0.042 Uiso 1 1 calc R . . C18 C -0.2820(3) 0.42462(15) 0.7118(2) 0.0296(7) Uani 1 1 d . . . C19 C -0.3394(3) 0.45416(19) 0.6326(2) 0.0454(9) Uani 1 1 d . . . H18 H -0.4336 0.4565 0.6154 0.055 Uiso 1 1 calc R . . C20 C -0.2567(3) 0.48029(19) 0.5791(2) 0.0424(9) Uani 1 1 d . . . H19 H -0.2975 0.5013 0.5271 0.051 Uiso 1 1 calc R . . C21 C -0.4334(3) 0.35944(15) 0.9053(2) 0.0344(7) Uani 1 1 d . . . H21 H -0.4380 0.3676 0.9664 0.041 Uiso 1 1 calc R . . C22 C -0.3662(3) 0.39944(16) 0.8583(2) 0.0382(8) Uani 1 1 d . . . H22 H -0.3243 0.4330 0.8876 0.046 Uiso 1 1 calc R . . C23 C -0.3630(3) 0.38820(14) 0.76587(19) 0.0282(6) Uani 1 1 d . . . C24 C -0.4296(3) 0.33919(15) 0.7268(2) 0.0331(7) Uani 1 1 d . . . H24 H -0.4341 0.3316 0.6644 0.040 Uiso 1 1 calc R . . C25 C -0.4901(3) 0.30097(15) 0.7792(2) 0.0319(7) Uani 1 1 d . . . H25 H -0.5320 0.2670 0.7515 0.038 Uiso 1 1 calc R . . C26 C -0.2623(3) 0.22281(17) 1.0265(2) 0.0351(8) Uani 1 1 d . . . H26 H -0.2671 0.2002 0.9732 0.042 Uiso 1 1 calc R . . C27 C -0.1404(3) 0.22576(18) 1.0871(2) 0.0395(8) Uani 1 1 d . . . H27 H -0.0648 0.2054 1.0745 0.047 Uiso 1 1 calc R . . C28 C -0.1303(3) 0.25923(15) 1.1674(2) 0.0290(7) Uani 1 1 d . . . C29 C -0.2452(3) 0.28911(16) 1.1811(2) 0.0342(7) Uani 1 1 d . . . H29 H -0.2427 0.3124 1.2334 0.041 Uiso 1 1 calc R . . C30 C -0.3632(3) 0.28442(16) 1.1175(2) 0.0323(7) Uani 1 1 d . . . H30 H -0.4393 0.3053 1.1278 0.039 Uiso 1 1 calc R . . C31 C -0.7999(3) 0.28677(16) 0.8126(2) 0.0341(7) Uani 1 1 d . . . H31 H -0.7500 0.3216 0.8254 0.041 Uiso 1 1 calc R . . C32 C -0.9222(3) 0.28941(16) 0.7519(2) 0.0376(8) Uani 1 1 d . . . H32 H -0.9516 0.3251 0.7232 0.045 Uiso 1 1 calc R . . C33 C -0.0008(3) 0.26113(15) 1.2341(2) 0.0295(7) Uani 1 1 d . . . C34 C 0.0491(3) 0.31213(16) 1.2793(2) 0.0340(7) Uani 1 1 d . . . H34 H -0.0018 0.3470 1.2715 0.041 Uiso 1 1 calc R . . C35 C -0.8252(3) 0.18851(16) 0.8364(2) 0.0331(7) Uani 1 1 d . . . H35 H -0.7917 0.1530 0.8639 0.040 Uiso 1 1 calc R . . N1 N -0.1211(2) 0.47711(13) 0.59786(17) 0.0313(6) Uani 1 1 d . . . N2 N -0.4915(2) 0.31026(12) 0.86825(15) 0.0258(5) Uani 1 1 d . . . N3 N -0.3742(2) 0.25109(12) 1.04105(16) 0.0268(6) Uani 1 1 d . . . N4 N -0.7496(2) 0.23690(12) 0.85401(16) 0.0271(6) Uani 1 1 d . . . O1 O 0.1629(2) 0.51390(10) 0.60705(14) 0.0318(5) Uani 1 1 d . . . O2 O 0.1875(2) 0.61191(12) 0.59557(17) 0.0495(7) Uani 1 1 d . . . O3 O 0.5326(3) 0.59453(11) 0.58147(16) 0.0461(6) Uani 1 1 d . . . O4 O 0.4788(2) 0.68236(9) 0.63585(13) 0.0286(5) Uani 1 1 d . . . O5 O 0.6545(2) 0.63226(11) 0.80551(14) 0.0362(5) Uani 1 1 d . . . O6 O 0.65149(19) 0.69813(11) 0.98032(14) 0.0327(5) Uani 1 1 d . . . O7 O 0.8178(2) 0.75780(12) 0.95059(18) 0.0463(6) Uani 1 1 d . . . O8 O -0.6112(2) 0.17314(10) 1.02821(14) 0.0349(5) Uani 1 1 d D . . H8A H -0.6040 0.1437 0.9941 0.052 Uiso 1 1 d RD . . H8B H -0.6927 0.1823 1.0281 0.052 Uiso 1 1 d RD . . O9 O 0.0614(2) 0.41227(11) 0.49263(15) 0.0370(5) Uani 1 1 d D . . H9A H 0.1071 0.3959 0.5397 0.055 Uiso 1 1 d RD . . H9B H -0.0189 0.3984 0.4815 0.055 Uiso 1 1 d RD . . O10 O 0.2432(3) 0.39751(14) 0.66252(19) 0.0644(8) Uani 1 1 d D . . H10A H 0.2527 0.4335 0.6468 0.097 Uiso 1 1 d RD . . H10B H 0.3091 0.3768 0.6490 0.097 Uiso 1 1 d RD . . Ni1 Ni 0.0000 0.5000 0.5000 0.02584(15) Uani 1 2 d S . . Ni2 Ni -0.55900(3) 0.241960(18) 0.94658(2) 0.02314(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0243(14) 0.0372(19) 0.0327(16) 0.0019(15) 0.0043(12) -0.0047(15) C2 0.0216(13) 0.0300(17) 0.0275(15) -0.0018(13) -0.0007(11) -0.0030(14) C3 0.0302(15) 0.0309(17) 0.0297(15) -0.0013(13) 0.0028(12) -0.0035(15) C4 0.0367(17) 0.050(2) 0.0374(18) 0.0041(16) 0.0066(14) -0.0133(18) C5 0.050(2) 0.058(3) 0.0294(17) 0.0132(17) 0.0043(15) -0.009(2) C6 0.0434(18) 0.050(2) 0.0242(16) 0.0038(15) -0.0026(13) -0.0021(18) C7 0.0262(14) 0.0320(17) 0.0299(15) -0.0049(13) 0.0015(12) -0.0009(14) C8 0.0272(14) 0.0260(16) 0.0255(14) 0.0005(12) 0.0017(11) 0.0027(13) C9 0.0263(14) 0.0373(19) 0.0324(16) -0.0014(14) 0.0009(12) -0.0007(15) C10 0.047(2) 0.049(2) 0.055(2) -0.0160(19) 0.0070(17) 0.001(2) C11 0.051(2) 0.060(3) 0.082(3) -0.018(3) 0.011(2) 0.017(2) C12 0.037(2) 0.072(3) 0.082(3) -0.009(3) -0.009(2) 0.019(2) C13 0.0298(16) 0.060(3) 0.049(2) -0.0157(19) -0.0084(14) 0.0054(19) C14 0.0228(14) 0.043(2) 0.0296(15) -0.0004(14) 0.0054(12) 0.0017(15) C15 0.0259(15) 0.041(2) 0.0241(14) -0.0041(14) 0.0031(11) -0.0002(15) C16 0.0277(15) 0.045(2) 0.0357(17) 0.0058(15) 0.0079(13) -0.0052(16) C17 0.0346(16) 0.041(2) 0.0290(16) 0.0077(14) 0.0051(13) -0.0010(16) C18 0.0303(15) 0.0305(17) 0.0295(15) 0.0010(13) 0.0094(12) -0.0025(14) C19 0.0259(15) 0.066(3) 0.047(2) 0.0175(19) 0.0133(14) 0.0033(18) C20 0.0301(16) 0.060(2) 0.0383(18) 0.0198(17) 0.0093(14) 0.0000(18) C21 0.0454(18) 0.0362(18) 0.0233(15) -0.0050(14) 0.0110(13) -0.0104(17) C22 0.0476(19) 0.0379(19) 0.0299(16) -0.0046(14) 0.0090(14) -0.0149(18) C23 0.0265(14) 0.0324(17) 0.0261(14) 0.0046(13) 0.0058(11) 0.0006(14) C24 0.0377(16) 0.0394(19) 0.0228(15) 0.0007(13) 0.0069(12) -0.0041(16) C25 0.0370(16) 0.0304(17) 0.0273(15) -0.0022(13) 0.0031(12) -0.0082(15) C26 0.0267(15) 0.046(2) 0.0303(16) -0.0110(15) -0.0007(12) 0.0042(16) C27 0.0246(15) 0.056(2) 0.0353(17) -0.0143(16) -0.0008(13) 0.0073(17) C28 0.0226(14) 0.0331(17) 0.0291(15) -0.0036(13) -0.0010(11) -0.0008(14) C29 0.0307(15) 0.041(2) 0.0292(16) -0.0085(14) -0.0005(12) 0.0036(16) C30 0.0233(14) 0.0389(19) 0.0329(16) -0.0045(14) 0.0003(12) 0.0037(15) C31 0.0250(14) 0.0341(18) 0.0398(17) 0.0067(15) -0.0030(13) -0.0032(15) C32 0.0251(14) 0.0373(19) 0.0463(19) 0.0114(16) -0.0048(13) 0.0020(16) C33 0.0216(13) 0.0390(18) 0.0260(15) -0.0047(13) -0.0009(11) -0.0007(14) C34 0.0268(15) 0.0341(18) 0.0377(17) -0.0031(14) -0.0027(13) 0.0074(15) C35 0.0273(15) 0.0328(18) 0.0350(17) 0.0069(14) -0.0055(12) 0.0044(15) N1 0.0293(13) 0.0357(15) 0.0312(13) 0.0030(12) 0.0113(10) -0.0047(13) N2 0.0221(11) 0.0302(14) 0.0255(12) 0.0024(11) 0.0056(9) -0.0028(11) N3 0.0207(11) 0.0350(15) 0.0234(12) -0.0008(11) 0.0005(9) -0.0024(12) N4 0.0198(11) 0.0363(15) 0.0239(12) 0.0024(11) 0.0003(9) 0.0000(12) O1 0.0293(10) 0.0347(13) 0.0300(11) -0.0001(10) 0.0018(8) -0.0080(11) O2 0.0419(13) 0.0347(14) 0.0618(16) 0.0118(12) -0.0176(11) -0.0116(13) O3 0.0679(16) 0.0336(13) 0.0419(13) -0.0044(11) 0.0235(12) 0.0022(14) O4 0.0268(10) 0.0275(12) 0.0312(11) 0.0003(9) 0.0047(8) -0.0022(10) O5 0.0309(11) 0.0380(13) 0.0344(12) 0.0036(10) -0.0082(9) -0.0065(11) O6 0.0211(10) 0.0434(14) 0.0339(11) -0.0061(10) 0.0061(8) -0.0013(10) O7 0.0372(13) 0.0441(15) 0.0633(16) -0.0044(13) 0.0244(12) -0.0067(13) O8 0.0328(11) 0.0384(13) 0.0332(11) 0.0070(10) 0.0053(9) 0.0015(11) O9 0.0319(11) 0.0367(13) 0.0406(12) 0.0029(10) 0.0022(9) 0.0013(11) O10 0.0689(18) 0.0537(18) 0.0718(19) 0.0069(15) 0.0156(15) 0.0178(17) Ni1 0.0231(3) 0.0287(3) 0.0261(3) 0.0019(2) 0.0054(2) -0.0054(2) Ni2 0.01834(19) 0.0282(2) 0.0220(2) 0.00193(15) 0.00119(13) -0.00117(16) _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 C1 O2 1.234(4) . ? C1 O1 1.268(4) . ? C1 C3 1.516(4) . ? C2 O3 1.241(4) . ? C2 O4 1.251(4) . ? C2 C8 1.526(4) . ? C3 C4 1.387(4) . ? C3 C8 1.397(4) . ? C4 C5 1.369(5) . ? C4 H4 0.9300 . ? C5 C6 1.374(5) . ? C5 H5 0.9300 . ? C6 C7 1.376(4) . ? C6 H6 0.9300 . ? C7 O5 1.379(4) . ? C7 C8 1.387(4) . ? C9 C14 1.379(4) . ? C9 C10 1.380(5) . ? C9 O5 1.384(4) . ? C10 C11 1.379(6) . ? C10 H10 0.9300 . ? C11 C12 1.375(6) . ? C11 H11 0.9300 . ? C12 C13 1.378(6) . ? C12 H12 0.9300 . ? C13 C14 1.397(4) . ? C13 H13 0.9300 . ? C14 C15 1.497(5) . ? C15 O7 1.236(4) . ? C15 O6 1.269(3) . ? C16 N1 1.331(4) . ? C16 C17 1.371(4) . ? C16 H15 0.9300 . ? C17 C18 1.386(4) . ? C17 H16 0.9300 . ? C18 C19 1.375(5) . ? C18 C23 1.483(4) . ? C19 C20 1.375(4) . ? C19 H18 0.9300 . ? C20 N1 1.334(4) . ? C20 H19 0.9300 . ? C21 N2 1.320(4) . ? C21 C22 1.382(4) . ? C21 H21 0.9300 . ? C22 C23 1.395(4) . ? C22 H22 0.9300 . ? C23 C24 1.361(5) . ? C24 C25 1.368(4) . ? C24 H24 0.9300 . ? C25 N2 1.334(4) . ? C25 H25 0.9300 . ? C26 N3 1.337(4) . ? C26 C27 1.375(4) . ? C26 H26 0.9300 . ? C27 C28 1.392(4) . ? C27 H27 0.9300 . ? C28 C29 1.377(4) . ? C28 C33 1.476(4) . ? C29 C30 1.371(4) . ? C29 H29 0.9300 . ? C30 N3 1.342(4) . ? C30 H30 0.9300 . ? C31 N4 1.331(4) . ? C31 C32 1.378(4) . ? C31 H31 0.9300 . ? C32 C33 1.379(5) 4_465 ? C32 H32 0.9300 . ? C33 C34 1.374(5) . ? C33 C32 1.379(5) 4_666 ? C34 C35 1.379(4) 4_666 ? C34 H34 0.9300 . ? C35 N4 1.323(4) . ? C35 C34 1.379(4) 4_465 ? C35 H35 0.9300 . ? N1 Ni1 2.111(2) . ? N2 Ni2 2.107(2) . ? N3 Ni2 2.111(2) . ? N4 Ni2 2.134(2) . ? O1 Ni1 2.075(2) . ? O4 Ni2 2.068(2) 2_556 ? O6 Ni2 2.049(2) 3_567 ? O8 Ni2 2.086(2) . ? O8 H8A 0.8440 . ? O8 H8B 0.8391 . ? O9 Ni1 2.075(2) . ? O9 H9A 0.8437 . ? O9 H9B 0.8480 . ? O10 H10A 0.8529 . ? O10 H10B 0.8593 . ? Ni1 O1 2.075(2) 3_566 ? Ni1 O9 2.075(2) 3_566 ? Ni1 N1 2.111(2) 3_566 ? Ni2 O6 2.049(2) 3_567 ? Ni2 O4 2.068(2) 2_546 ? 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 O2 C1 O1 125.9(3) . . ? O2 C1 C3 117.8(3) . . ? O1 C1 C3 116.3(3) . . ? O3 C2 O4 127.4(3) . . ? O3 C2 C8 115.4(3) . . ? O4 C2 C8 117.0(3) . . ? C4 C3 C8 119.6(3) . . ? C4 C3 C1 119.0(3) . . ? C8 C3 C1 121.4(3) . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 119.0(3) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 O5 122.0(3) . . ? C6 C7 C8 122.1(3) . . ? O5 C7 C8 115.8(3) . . ? C7 C8 C3 118.0(3) . . ? C7 C8 C2 118.3(3) . . ? C3 C8 C2 123.5(2) . . ? C14 C9 C10 121.9(3) . . ? C14 C9 O5 118.1(3) . . ? C10 C9 O5 119.7(3) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 119.9(4) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 117.8(3) . . ? C9 C14 C15 122.3(3) . . ? C13 C14 C15 119.8(3) . . ? O7 C15 O6 126.8(3) . . ? O7 C15 C14 118.7(3) . . ? O6 C15 C14 114.4(3) . . ? N1 C16 C17 123.9(3) . . ? N1 C16 H15 118.1 . . ? C17 C16 H15 118.1 . . ? C16 C17 C18 119.3(3) . . ? C16 C17 H16 120.4 . . ? C18 C17 H16 120.4 . . ? C19 C18 C17 117.2(3) . . ? C19 C18 C23 122.7(3) . . ? C17 C18 C23 119.7(3) . . ? C20 C19 C18 119.6(3) . . ? C20 C19 H18 120.2 . . ? C18 C19 H18 120.2 . . ? N1 C20 C19 123.5(3) . . ? N1 C20 H19 118.3 . . ? C19 C20 H19 118.3 . . ? N2 C21 C22 123.7(3) . . ? N2 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 118.2(3) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C24 C23 C22 117.7(3) . . ? C24 C23 C18 119.5(3) . . ? C22 C23 C18 122.6(3) . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? N2 C25 C24 122.9(3) . . ? N2 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? N3 C26 C27 122.7(3) . . ? N3 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C28 119.9(3) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 117.2(3) . . ? C29 C28 C33 122.7(3) . . ? C27 C28 C33 120.1(3) . . ? C30 C29 C28 119.8(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? N3 C30 C29 123.2(3) . . ? N3 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N4 C31 C32 123.4(3) . . ? N4 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C31 C32 C33 119.7(3) . 4_465 ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 4_465 . ? C34 C33 C32 116.9(3) . 4_666 ? C34 C33 C28 123.0(3) . . ? C32 C33 C28 120.1(3) 4_666 . ? C33 C34 C35 119.8(3) . 4_666 ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 4_666 . ? N4 C35 C34 123.5(3) . 4_465 ? N4 C35 H35 118.2 . . ? C34 C35 H35 118.2 4_465 . ? C16 N1 C20 116.4(3) . . ? C16 N1 Ni1 120.7(2) . . ? C20 N1 Ni1 122.2(2) . . ? C21 N2 C25 117.1(3) . . ? C21 N2 Ni2 122.99(19) . . ? C25 N2 Ni2 119.3(2) . . ? C26 N3 C30 117.3(2) . . ? C26 N3 Ni2 120.24(19) . . ? C30 N3 Ni2 122.5(2) . . ? C35 N4 C31 116.7(3) . . ? C35 N4 Ni2 125.4(2) . . ? C31 N4 Ni2 117.8(2) . . ? C1 O1 Ni1 126.6(2) . . ? C2 O4 Ni2 128.35(19) . 2_556 ? C7 O5 C9 118.4(2) . . ? C15 O6 Ni2 123.0(2) . 3_567 ? Ni2 O8 H8A 100.4 . . ? Ni2 O8 H8B 99.4 . . ? H8A O8 H8B 112.4 . . ? Ni1 O9 H9A 119.6 . . ? Ni1 O9 H9B 94.7 . . ? H9A O9 H9B 110.4 . . ? H10A O10 H10B 108.8 . . ? O1 Ni1 O1 180.0 3_566 . ? O1 Ni1 O9 89.15(9) 3_566 3_566 ? O1 Ni1 O9 90.85(9) . 3_566 ? O1 Ni1 O9 90.85(9) 3_566 . ? O1 Ni1 O9 89.15(9) . . ? O9 Ni1 O9 180.0 3_566 . ? O1 Ni1 N1 89.04(9) 3_566 3_566 ? O1 Ni1 N1 90.96(9) . 3_566 ? O9 Ni1 N1 90.90(10) 3_566 3_566 ? O9 Ni1 N1 89.10(10) . 3_566 ? O1 Ni1 N1 90.96(9) 3_566 . ? O1 Ni1 N1 89.04(9) . . ? O9 Ni1 N1 89.10(10) 3_566 . ? O9 Ni1 N1 90.90(10) . . ? N1 Ni1 N1 180.000(1) 3_566 . ? O6 Ni2 O4 175.38(8) 3_567 2_546 ? O6 Ni2 O8 89.96(9) 3_567 . ? O4 Ni2 O8 91.35(9) 2_546 . ? O6 Ni2 N2 91.71(10) 3_567 . ? O4 Ni2 N2 87.28(9) 2_546 . ? O8 Ni2 N2 175.88(9) . . ? O6 Ni2 N3 90.69(9) 3_567 . ? O4 Ni2 N3 93.78(9) 2_546 . ? O8 Ni2 N3 88.36(9) . . ? N2 Ni2 N3 87.86(9) . . ? O6 Ni2 N4 86.39(9) 3_567 . ? O4 Ni2 N4 89.13(9) 2_546 . ? O8 Ni2 N4 92.42(9) . . ? N2 Ni2 N4 91.44(9) . . ? N3 Ni2 N4 176.97(10) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.041 _refine_diff_density_min -1.009 _refine_diff_density_rms 0.106 #===END # Attachment 'new compound.cif' data_qq _database_code_depnum_ccdc_archive 'CCDC 745620' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H10 O7' _chemical_formula_sum 'C15 H10 O7' _chemical_formula_weight 302.23 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' 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 25.342(16) _cell_length_b 8.645(5) _cell_length_c 14.204(11) _cell_angle_alpha 90.00 _cell_angle_beta 120.412(19) _cell_angle_gamma 90.00 _cell_volume 2684(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1069 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 27.22 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9704 _exptl_absorpt_correction_T_max 0.9928 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 6238 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2305 _reflns_number_gt 1444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_reduction SAINT-Plus _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material XP _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^)+(0.1931P)^2^+3.6209P] 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 2305 _refine_ls_number_parameters 199 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1347 _refine_ls_R_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.3021 _refine_ls_wR_factor_gt 0.2792 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6170(2) 0.4151(5) 0.4392(4) 0.0459(12) Uani 1 1 d . . . C2 C 0.7401(2) 0.5505(6) 0.5473(4) 0.0524(13) Uani 1 1 d . . . C3 C 0.6709(2) 0.3336(5) 0.5310(4) 0.0431(11) Uani 1 1 d . . . C4 C 0.7304(2) 0.3931(6) 0.5778(4) 0.0480(12) Uani 1 1 d . . . C5 C 0.7788(2) 0.3110(7) 0.6547(4) 0.0595(14) Uani 1 1 d . . . H5 H 0.8181 0.3505 0.6835 0.071 Uiso 1 1 calc R . . C6 C 0.7705(2) 0.1702(7) 0.6906(5) 0.0622(15) Uani 1 1 d . . . H6 H 0.8041 0.1161 0.7440 0.075 Uiso 1 1 calc R . . C7 C 0.7124(2) 0.1092(6) 0.6476(4) 0.0530(13) Uani 1 1 d . . . H7 H 0.7065 0.0142 0.6715 0.064 Uiso 1 1 calc R . . C8 C 0.6635(2) 0.1919(5) 0.5686(4) 0.0445(12) Uani 1 1 d . . . C9 C 0.5833(2) 0.2485(6) 0.6894(4) 0.0510(13) Uani 1 1 d . . . C10 C 0.5780(2) 0.0845(6) 0.6568(4) 0.0449(12) Uani 1 1 d . . . C11 C 0.5879(2) 0.0335(5) 0.5732(4) 0.0425(11) Uani 1 1 d . . . C12 C 0.5799(3) -0.1191(6) 0.5418(5) 0.0589(14) Uani 1 1 d . . . H12 H 0.5881 -0.1519 0.4881 0.071 Uiso 1 1 calc R . . C13 C 0.5599(3) -0.2227(6) 0.5899(5) 0.0656(16) Uani 1 1 d . . . H13 H 0.5530 -0.3251 0.5666 0.079 Uiso 1 1 calc R . . C14 C 0.5497(2) -0.1768(6) 0.6728(5) 0.0620(16) Uani 1 1 d . . . H14 H 0.5367 -0.2478 0.7058 0.074 Uiso 1 1 calc R . . C15 C 0.5592(2) -0.0270(7) 0.7050(5) 0.0587(14) Uani 1 1 d . . . H15 H 0.5529 0.0029 0.7615 0.070 Uiso 1 1 calc R . . O1 O 0.61506(18) 0.4457(4) 0.3550(3) 0.0633(11) Uani 1 1 d . . . O2 O 0.57080(18) 0.4475(5) 0.4519(4) 0.0723(12) Uani 1 1 d D . . H2 H 0.5799 0.4294 0.5151 0.108 Uiso 1 1 d RD . . O3 O 0.70043(19) 0.6494(4) 0.5187(4) 0.0723(13) Uani 1 1 d D . . H3 H 0.7069 0.7189 0.4866 0.108 Uiso 1 1 d RD . . O4 O 0.79333(18) 0.5750(5) 0.5592(4) 0.0746(13) Uani 1 1 d . . . O5 O 0.60401(14) 0.1351(4) 0.5160(3) 0.0478(9) Uani 1 1 d . . . O6 O 0.5888(2) 0.3575(4) 0.6414(4) 0.0771(13) Uani 1 1 d . . . O7 O 0.5806(2) 0.2681(5) 0.7783(3) 0.0813(14) Uani 1 1 d . . . H7A H 0.5838 0.3604 0.7934 0.122 Uiso 1 1 d 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 C1 0.049(3) 0.043(2) 0.044(3) -0.004(2) 0.022(2) -0.011(2) C2 0.054(3) 0.052(3) 0.055(3) -0.012(2) 0.030(3) -0.016(3) C3 0.045(3) 0.044(3) 0.040(3) -0.007(2) 0.022(2) -0.012(2) C4 0.046(3) 0.056(3) 0.042(3) -0.008(2) 0.022(2) -0.011(2) C5 0.047(3) 0.069(3) 0.057(3) -0.005(3) 0.022(3) -0.012(3) C6 0.050(3) 0.070(4) 0.058(3) 0.005(3) 0.021(3) 0.001(3) C7 0.045(3) 0.057(3) 0.053(3) 0.009(3) 0.022(2) 0.001(2) C8 0.043(3) 0.047(3) 0.044(3) -0.008(2) 0.022(2) -0.008(2) C9 0.054(3) 0.058(3) 0.040(3) 0.000(2) 0.023(2) -0.005(2) C10 0.031(2) 0.052(3) 0.045(3) 0.006(2) 0.015(2) -0.003(2) C11 0.036(2) 0.045(3) 0.040(2) 0.006(2) 0.0138(19) -0.0034(19) C12 0.059(3) 0.047(3) 0.070(4) -0.003(3) 0.032(3) -0.001(2) C13 0.055(3) 0.042(3) 0.078(4) 0.000(3) 0.018(3) -0.013(2) C14 0.045(3) 0.057(3) 0.065(4) 0.016(3) 0.015(3) -0.009(2) C15 0.045(3) 0.067(4) 0.063(3) 0.013(3) 0.027(3) 0.000(3) O1 0.076(3) 0.064(2) 0.048(2) 0.0067(18) 0.030(2) 0.0018(19) O2 0.061(2) 0.073(3) 0.086(3) 0.021(2) 0.040(2) 0.009(2) O3 0.067(3) 0.057(2) 0.102(3) 0.000(2) 0.050(2) -0.015(2) O4 0.058(2) 0.071(3) 0.100(3) -0.002(2) 0.043(2) -0.023(2) O5 0.048(2) 0.0502(19) 0.0438(19) 0.0028(15) 0.0218(16) -0.0079(15) O6 0.120(4) 0.052(2) 0.086(3) -0.006(2) 0.071(3) -0.007(2) O7 0.124(4) 0.073(3) 0.062(3) -0.006(2) 0.058(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.202(6) . ? C1 O2 1.302(6) . ? C1 C3 1.504(7) . ? C2 O3 1.221(6) . ? C2 O4 1.291(6) . ? C2 C4 1.485(7) . ? C3 C8 1.387(6) . ? C3 C4 1.401(7) . ? C4 C5 1.358(8) . ? C5 C6 1.377(8) . ? C5 H5 0.9300 . ? C6 C7 1.380(7) . ? C6 H6 0.9300 . ? C7 C8 1.378(7) . ? C7 H7 0.9300 . ? C8 O5 1.390(5) . ? C9 O6 1.211(6) . ? C9 O7 1.309(6) . ? C9 C10 1.476(7) . ? C10 C15 1.398(7) . ? C10 C11 1.404(7) . ? C11 C12 1.374(7) . ? C11 O5 1.391(5) . ? C12 C13 1.371(8) . ? C12 H12 0.9300 . ? C13 C14 1.384(8) . ? C13 H13 0.9300 . ? C14 C15 1.354(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? O2 H2 0.8200 . ? O3 H3 0.8200 . ? O7 H7A 0.8200 . ? 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 O1 C1 O2 120.3(5) . . ? O1 C1 C3 121.8(5) . . ? O2 C1 C3 117.8(4) . . ? O3 C2 O4 123.9(5) . . ? O3 C2 C4 120.6(4) . . ? O4 C2 C4 115.4(5) . . ? C8 C3 C4 117.7(4) . . ? C8 C3 C1 120.5(4) . . ? C4 C3 C1 121.8(4) . . ? C5 C4 C3 120.4(5) . . ? C5 C4 C2 119.8(5) . . ? C3 C4 C2 119.7(5) . . ? C4 C5 C6 121.0(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 120.2(5) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 118.7(5) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C3 122.1(4) . . ? C7 C8 O5 122.6(4) . . ? C3 C8 O5 115.2(4) . . ? O6 C9 O7 121.3(5) . . ? O6 C9 C10 126.1(5) . . ? O7 C9 C10 112.6(4) . . ? C15 C10 C11 116.6(5) . . ? C15 C10 C9 120.6(5) . . ? C11 C10 C9 122.7(4) . . ? C12 C11 O5 117.1(4) . . ? C12 C11 C10 121.1(5) . . ? O5 C11 C10 121.8(4) . . ? C13 C12 C11 119.7(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.8(5) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.0(5) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C10 122.7(5) . . ? C14 C15 H15 118.7 . . ? C10 C15 H15 118.7 . . ? C1 O2 H2 109.6 . . ? C2 O3 H3 109.6 . . ? C8 O5 C11 118.0(4) . . ? C9 O7 H7A 109.4 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.491 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.103