# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wen-Hua Sun' _publ_contact_author_email WHSUN@ICCAS.AC.CN _publ_section_title ; Synthesis, Characterization and Ethylene Oligomerization of Nickel Complexes Bearing N-(2-(1H-benzo[d]imidazol-2-yl)quinolin-8-yl)benzamide Derivatives ; loop_ _publ_author_name 'Wen-Hua Sun' 'Miao Shen' 'Kefeng Wang' # Attachment 'CIF.CIF' data_12 _database_code_depnum_ccdc_archive 'CCDC 713150' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 N4 O' _chemical_formula_weight 392.45 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 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 22.362(4) _cell_length_b 22.568(4) _cell_length_c 33.477(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.23(3) _cell_angle_gamma 90.00 _cell_volume 16137(5) _cell_formula_units_Z 32 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 759 _cell_measurement_theta_min 1.27 _cell_measurement_theta_max 25.01 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6591 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9720 _exptl_absorpt_correction_T_max 0.9799 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 27140 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.1178 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.01 _reflns_number_total 14198 _reflns_number_gt 6856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0938P)^2^+0.6264P] 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 14198 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2316 _refine_ls_R_factor_gt 0.1183 _refine_ls_wR_factor_ref 0.2655 _refine_ls_wR_factor_gt 0.2180 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 O1B O 0.4961(2) 0.25492(18) 0.18819(14) 0.0656(14) Uani 1 1 d . . . O1D O 0.2457(2) 0.00568(18) 0.18859(15) 0.0680(14) Uani 1 1 d . . . O1 O 0.2019(2) 0.4644(2) 0.18704(15) 0.0684(14) Uani 1 1 d . . . O1A O 0.04427(19) 0.20768(19) 0.31348(14) 0.0582(13) Uani 1 1 d . . . N1B N 0.4561(2) 0.38962(19) 0.07981(14) 0.0369(11) Uani 1 1 d . . . N1C N 0.2015(2) 0.13795(18) 0.07880(15) 0.0398(12) Uani 1 1 d . . . N1 N 0.0203(2) 0.45770(19) 0.07753(15) 0.0400(12) Uani 1 1 d . . . N1A N 0.2298(2) 0.20337(19) 0.42114(15) 0.0379(12) Uani 1 1 d . . . C1 C -0.0031(3) 0.4758(2) 0.10888(18) 0.0380(14) Uani 1 1 d . . . C1A C 0.2532(3) 0.2184(2) 0.38935(18) 0.0397(15) Uani 1 1 d . . . C1B C 0.4536(3) 0.4261(2) 0.11182(19) 0.0413(15) Uani 1 1 d . . . C1C C 0.1981(2) 0.1758(2) 0.10939(17) 0.0346(13) Uani 1 1 d . . . N2B N 0.4568(2) 0.33821(19) 0.15453(14) 0.0412(12) Uani 1 1 d . . . N2C N 0.2013(2) 0.08688(19) 0.15426(14) 0.0428(13) Uani 1 1 d . . . N2 N 0.1047(2) 0.4920(2) 0.15206(14) 0.0427(12) Uani 1 1 d . . . N2A N 0.1437(2) 0.2325(2) 0.34570(14) 0.0382(11) Uani 1 1 d . . . C2A C 0.2094(3) 0.2329(2) 0.34971(19) 0.0414(15) Uani 1 1 d . . . C2B C 0.4552(3) 0.4015(2) 0.15088(19) 0.0420(15) Uani 1 1 d . . . C2C C 0.1976(2) 0.1506(2) 0.14869(18) 0.0392(14) Uani 1 1 d . . . C2 C 0.0391(3) 0.4922(2) 0.14768(17) 0.0380(14) Uani 1 1 d . . . N3B N 0.4592(2) 0.3915(2) -0.02720(16) 0.0452(13) Uani 1 1 d . . . N3C N 0.2062(2) 0.1400(2) -0.02815(17) 0.0493(14) Uani 1 1 d . . . N3 N -0.0282(2) 0.4055(2) -0.02919(16) 0.0453(13) Uani 1 1 d . . . N3A N 0.2830(2) 0.1553(2) 0.52912(16) 0.0476(14) Uani 1 1 d . . . C3B C 0.4528(3) 0.4371(3) 0.1832(2) 0.0496(16) Uani 1 1 d . . . H3BB H 0.4526 0.4207 0.2086 0.060 Uiso 1 1 calc R . . C3 C 0.0163(3) 0.5083(3) 0.1798(2) 0.0550(18) Uani 1 1 d . . . H3B H 0.0436 0.5194 0.2055 0.066 Uiso 1 1 calc R . . C3C C 0.1951(3) 0.1867(3) 0.1809(2) 0.0542(18) Uani 1 1 d . . . H3CB H 0.1945 0.1697 0.2061 0.065 Uiso 1 1 calc R . . C3A C 0.2301(3) 0.2472(3) 0.3167(2) 0.0502(16) Uani 1 1 d . . . H3AB H 0.2011 0.2563 0.2912 0.060 Uiso 1 1 calc R . . N4B N 0.4623(2) 0.3121(2) 0.01289(15) 0.0447(13) Uani 1 1 d . . . N4C N 0.2090(2) 0.0608(2) 0.01209(16) 0.0457(13) Uani 1 1 d . . . N4 N 0.0699(2) 0.4178(2) 0.01194(16) 0.0470(13) Uani 1 1 d . . . N4A N 0.1841(2) 0.1699(2) 0.48982(15) 0.0453(13) Uani 1 1 d . . . C4 C -0.0481(3) 0.5080(3) 0.1736(2) 0.060(2) Uani 1 1 d . . . H4A H -0.0626 0.5184 0.1960 0.072 Uiso 1 1 calc R . . C4A C 0.2942(3) 0.2487(3) 0.3200(2) 0.0574(19) Uani 1 1 d . . . H4AA H 0.3075 0.2586 0.2970 0.069 Uiso 1 1 calc R . . C4B C 0.4506(3) 0.4985(3) 0.1778(2) 0.059(2) Uani 1 1 d . . . H4BA H 0.4505 0.5225 0.2003 0.071 Uiso 1 1 calc R . . C4C C 0.1934(3) 0.2489(3) 0.1770(2) 0.061(2) Uani 1 1 d . . . H4CA H 0.1926 0.2728 0.1995 0.073 Uiso 1 1 calc R . . C5 C -0.0897(3) 0.4938(3) 0.1377(2) 0.0624(19) Uani 1 1 d . . . H5A H -0.1323 0.4949 0.1351 0.075 Uiso 1 1 calc R . . C5A C 0.3365(3) 0.2355(3) 0.3576(2) 0.0604(19) Uani 1 1 d . . . H5AA H 0.3790 0.2361 0.3600 0.072 Uiso 1 1 calc R . . C5B C 0.4485(3) 0.5242(3) 0.1411(2) 0.0560(19) Uani 1 1 d . . . H5BA H 0.4458 0.5652 0.1383 0.067 Uiso 1 1 calc R . . C5C C 0.1930(3) 0.2733(3) 0.1396(2) 0.060(2) Uani 1 1 d . . . H5CA H 0.1912 0.3143 0.1367 0.072 Uiso 1 1 calc R . . C6B C 0.4504(3) 0.4887(3) 0.10711(19) 0.0417(15) Uani 1 1 d . . . C6C C 0.1953(3) 0.2379(3) 0.1049(2) 0.0536(19) Uani 1 1 d . . . C6 C -0.0688(3) 0.4767(3) 0.1033(2) 0.0465(16) Uani 1 1 d . . . C6A C 0.3172(3) 0.2208(3) 0.3930(2) 0.0484(17) Uani 1 1 d . . . C7B C 0.4485(3) 0.5114(3) 0.0668(2) 0.0554(18) Uani 1 1 d . . . H7BA H 0.4466 0.5521 0.0622 0.066 Uiso 1 1 calc R . . C7C C 0.1961(3) 0.2598(3) 0.0664(2) 0.0582(19) Uani 1 1 d . . . H7CA H 0.1951 0.3006 0.0620 0.070 Uiso 1 1 calc R . . C7 C -0.1085(3) 0.4602(3) 0.0636(2) 0.0567(18) Uani 1 1 d . . . H7A H -0.1517 0.4610 0.0586 0.068 Uiso 1 1 calc R . . C7A C 0.3583(3) 0.2066(3) 0.4323(2) 0.0561(18) Uani 1 1 d . . . H7AA H 0.4012 0.2070 0.4363 0.067 Uiso 1 1 calc R . . C8B C 0.4493(3) 0.4746(3) 0.0358(2) 0.0542(18) Uani 1 1 d . . . H8BA H 0.4468 0.4893 0.0095 0.065 Uiso 1 1 calc R . . C8 C -0.0845(3) 0.4433(3) 0.0327(2) 0.0545(18) Uani 1 1 d . . . H8A H -0.1107 0.4327 0.0065 0.065 Uiso 1 1 calc R . . C8A C 0.3361(3) 0.1921(3) 0.4649(2) 0.0480(16) Uani 1 1 d . . . H8AA H 0.3635 0.1835 0.4911 0.058 Uiso 1 1 calc R . . C8C C 0.1984(3) 0.2226(3) 0.0350(2) 0.0534(17) Uani 1 1 d . . . H8CA H 0.1981 0.2375 0.0090 0.064 Uiso 1 1 calc R . . C9B C 0.4541(3) 0.4126(3) 0.04361(18) 0.0406(15) Uani 1 1 d . . . C9 C -0.0191(3) 0.4423(2) 0.0411(2) 0.0415(15) Uani 1 1 d . . . C9A C 0.2714(3) 0.1904(2) 0.45801(17) 0.0378(14) Uani 1 1 d . . . C9C C 0.2014(3) 0.1609(2) 0.04259(19) 0.0402(15) Uani 1 1 d . . . C10B C 0.4582(2) 0.3730(2) 0.00957(19) 0.0375(14) Uani 1 1 d . . . C10 C 0.0077(3) 0.4226(2) 0.00804(19) 0.0391(14) Uani 1 1 d . . . C10A C 0.2470(3) 0.1728(2) 0.49204(19) 0.0415(15) Uani 1 1 d . . . C10C C 0.2044(3) 0.1216(2) 0.00872(19) 0.0408(14) Uani 1 1 d . . . C11C C 0.2140(3) 0.0396(3) -0.0258(2) 0.0476(16) Uani 1 1 d . . . C11A C 0.1815(3) 0.1488(2) 0.52802(19) 0.0436(15) Uani 1 1 d . . . C11B C 0.4643(3) 0.3406(3) -0.04912(19) 0.0447(15) Uani 1 1 d . . . C11 C 0.0130(3) 0.3896(2) -0.05090(19) 0.0444(16) Uani 1 1 d . . . C12 C 0.0025(4) 0.3674(3) -0.0918(2) 0.0568(19) Uani 1 1 d . . . H12A H -0.0380 0.3615 -0.1092 0.068 Uiso 1 1 calc R . . C12B C 0.4674(3) 0.3341(3) -0.0907(2) 0.0586(19) Uani 1 1 d . . . H12B H 0.4656 0.3666 -0.1081 0.070 Uiso 1 1 calc R . . C12C C 0.2201(3) -0.0167(3) -0.0398(2) 0.067(2) Uani 1 1 d . . . H12C H 0.2223 -0.0496 -0.0227 0.081 Uiso 1 1 calc R . . C12A C 0.1315(4) 0.1374(3) 0.5430(3) 0.071(2) Uani 1 1 d . . . H12D H 0.0904 0.1434 0.5267 0.085 Uiso 1 1 calc R . . C13 C 0.0527(4) 0.3546(3) -0.1052(2) 0.065(2) Uani 1 1 d . . . H13A H 0.0461 0.3413 -0.1325 0.078 Uiso 1 1 calc R . . C13B C 0.4734(3) 0.2772(3) -0.1038(2) 0.0609(19) Uani 1 1 d . . . H13B H 0.4751 0.2713 -0.1309 0.073 Uiso 1 1 calc R . . C13C C 0.2228(4) -0.0222(4) -0.0800(3) 0.076(2) Uani 1 1 d . . . H13C H 0.2263 -0.0597 -0.0906 0.091 Uiso 1 1 calc R . . C13A C 0.1455(5) 0.1165(3) 0.5836(3) 0.086(3) Uani 1 1 d . . . H13D H 0.1131 0.1080 0.5950 0.103 Uiso 1 1 calc R . . C14C C 0.2204(3) 0.0277(4) -0.1054(2) 0.070(2) Uani 1 1 d . . . H14A H 0.2221 0.0227 -0.1326 0.084 Uiso 1 1 calc R . . C14A C 0.2071(4) 0.1079(3) 0.6076(2) 0.076(2) Uani 1 1 d . . . H14B H 0.2150 0.0938 0.6348 0.091 Uiso 1 1 calc R . . C14B C 0.4770(3) 0.2291(4) -0.0784(2) 0.068(2) Uani 1 1 d . . . H14C H 0.4824 0.1916 -0.0884 0.082 Uiso 1 1 calc R . . C14 C 0.1136(4) 0.3609(3) -0.0793(2) 0.070(2) Uani 1 1 d . . . H14D H 0.1469 0.3510 -0.0893 0.084 Uiso 1 1 calc R . . C15C C 0.2154(3) 0.0839(4) -0.0908(2) 0.064(2) Uani 1 1 d . . . H15A H 0.2149 0.1170 -0.1075 0.076 Uiso 1 1 calc R . . C15A C 0.2563(4) 0.1193(3) 0.5929(2) 0.0589(19) Uani 1 1 d . . . H15B H 0.2973 0.1131 0.6095 0.071 Uiso 1 1 calc R . . C15B C 0.4729(3) 0.2344(3) -0.0388(2) 0.067(2) Uani 1 1 d . . . H15C H 0.4745 0.2014 -0.0220 0.080 Uiso 1 1 calc R . . C15 C 0.1255(3) 0.3818(3) -0.0387(2) 0.0614(19) Uani 1 1 d . . . H15D H 0.1661 0.3861 -0.0211 0.074 Uiso 1 1 calc R . . C16 C 0.0746(3) 0.3958(2) -0.0257(2) 0.0451(15) Uani 1 1 d . . . C16B C 0.4663(3) 0.2915(3) -0.0245(2) 0.0455(16) Uani 1 1 d . . . C16C C 0.2113(3) 0.0896(3) -0.0506(2) 0.0472(16) Uani 1 1 d . . . C16A C 0.2433(3) 0.1406(2) 0.55169(19) 0.0477(16) Uani 1 1 d . . . C17B C 0.5035(3) 0.3077(2) 0.18152(18) 0.0412(15) Uani 1 1 d . . . C17C C 0.2490(3) 0.0587(3) 0.18262(18) 0.0410(15) Uani 1 1 d . . . C17 C 0.1454(3) 0.4575(3) 0.18062(19) 0.0430(15) Uani 1 1 d . . . C17A C 0.0999(3) 0.1991(3) 0.31895(17) 0.0407(15) Uani 1 1 d . . . C18B C 0.5642(3) 0.3369(2) 0.20400(18) 0.0352(14) Uani 1 1 d . . . C18C C 0.3049(3) 0.0943(2) 0.20523(18) 0.0369(14) Uani 1 1 d . . . C18 C 0.1220(3) 0.4129(2) 0.20421(19) 0.0415(15) Uani 1 1 d . . . C18A C 0.1203(3) 0.1498(3) 0.29520(18) 0.0384(14) Uani 1 1 d . . . C19B C 0.5939(3) 0.3776(2) 0.1858(2) 0.0452(16) Uani 1 1 d . . . H19A H 0.5749 0.3900 0.1585 0.054 Uiso 1 1 calc R . . C19C C 0.3248(3) 0.0927(3) 0.2482(2) 0.0550(18) Uani 1 1 d . . . H19B H 0.3029 0.0704 0.2625 0.066 Uiso 1 1 calc R . . C19 C 0.0807(3) 0.3700(3) 0.1852(2) 0.0539(18) Uani 1 1 d . . . H19C H 0.0653 0.3693 0.1562 0.065 Uiso 1 1 calc R . . C19A C 0.1692(3) 0.1100(3) 0.3128(2) 0.0504(17) Uani 1 1 d . . . H19D H 0.1934 0.1149 0.3404 0.060 Uiso 1 1 calc R . . C20B C 0.6511(3) 0.3998(3) 0.2074(2) 0.057(2) Uani 1 1 d . . . H20A H 0.6705 0.4272 0.1946 0.069 Uiso 1 1 calc R . . C20C C 0.3765(3) 0.1236(3) 0.2699(2) 0.070(2) Uani 1 1 d . . . H20B H 0.3891 0.1230 0.2990 0.083 Uiso 1 1 calc R . . C20 C 0.0612(3) 0.3278(3) 0.2080(2) 0.062(2) Uani 1 1 d . . . H20C H 0.0336 0.2985 0.1941 0.075 Uiso 1 1 calc R . . C20A C 0.1817(3) 0.0639(3) 0.2898(3) 0.062(2) Uani 1 1 d . . . H20D H 0.2143 0.0378 0.3018 0.075 Uiso 1 1 calc R . . C21B C 0.6803(3) 0.3826(3) 0.2478(2) 0.065(2) Uani 1 1 d . . . H21A H 0.7196 0.3974 0.2622 0.078 Uiso 1 1 calc R . . C21C C 0.4103(3) 0.1557(3) 0.2491(2) 0.0552(19) Uani 1 1 d . . . H21B H 0.4462 0.1758 0.2641 0.066 Uiso 1 1 calc R . . C21 C 0.0817(3) 0.3281(3) 0.2506(3) 0.069(2) Uani 1 1 d . . . H21C H 0.0675 0.2999 0.2659 0.083 Uiso 1 1 calc R . . C21A C 0.1454(4) 0.0564(3) 0.2483(3) 0.072(2) Uani 1 1 d . . . H21D H 0.1533 0.0251 0.2325 0.087 Uiso 1 1 calc R . . C22B C 0.6505(3) 0.3431(4) 0.2664(2) 0.073(2) Uani 1 1 d . . . H22A H 0.6691 0.3322 0.2941 0.088 Uiso 1 1 calc R . . C22 C 0.1242(3) 0.3710(3) 0.2705(2) 0.071(2) Uani 1 1 d . . . H22B H 0.1396 0.3717 0.2996 0.085 Uiso 1 1 calc R . . C22A C 0.0977(4) 0.0957(3) 0.2310(2) 0.067(2) Uani 1 1 d . . . H22C H 0.0736 0.0908 0.2034 0.080 Uiso 1 1 calc R . . C22C C 0.3912(3) 0.1580(3) 0.2065(2) 0.063(2) Uani 1 1 d . . . H22D H 0.4133 0.1807 0.1924 0.076 Uiso 1 1 calc R . . C23B C 0.5931(3) 0.3192(3) 0.24474(19) 0.0469(16) Uani 1 1 d . . . H23A H 0.5741 0.2913 0.2575 0.056 Uiso 1 1 calc R . . C23C C 0.3382(3) 0.1260(3) 0.1840(2) 0.0574(19) Uani 1 1 d . . . H23B H 0.3257 0.1263 0.1550 0.069 Uiso 1 1 calc R . . C23 C 0.1434(3) 0.4127(3) 0.2472(2) 0.0525(18) Uani 1 1 d . . . H23C H 0.1717 0.4416 0.2608 0.063 Uiso 1 1 calc R . . C23A C 0.0852(3) 0.1419(3) 0.25392(18) 0.0436(15) Uani 1 1 d . . . H23D H 0.0529 0.1682 0.2416 0.052 Uiso 1 1 calc R . . C24B C 0.4590(4) 0.2734(3) 0.0470(2) 0.075(2) Uani 1 1 d . . . H24A H 0.4629 0.2329 0.0393 0.112 Uiso 1 1 calc R . . H24B H 0.4195 0.2789 0.0524 0.112 Uiso 1 1 calc R . . H24C H 0.4924 0.2830 0.0717 0.112 Uiso 1 1 calc R . . C24C C 0.2077(4) 0.0217(3) 0.0466(2) 0.075(2) Uani 1 1 d . . . H24D H 0.2044 0.0451 0.0698 0.113 Uiso 1 1 calc R . . H24E H 0.2455 -0.0012 0.0550 0.113 Uiso 1 1 calc R . . H24F H 0.1723 -0.0044 0.0378 0.113 Uiso 1 1 calc R . . C24 C 0.1244(3) 0.4330(4) 0.0474(2) 0.081(3) Uani 1 1 d . . . H24G H 0.1105 0.4477 0.0700 0.122 Uiso 1 1 calc R . . H24H H 0.1487 0.4630 0.0389 0.122 Uiso 1 1 calc R . . H24I H 0.1497 0.3984 0.0563 0.122 Uiso 1 1 calc R . . C24A C 0.1295(3) 0.1861(3) 0.4562(2) 0.069(2) Uani 1 1 d . . . H24J H 0.1420 0.1994 0.4326 0.103 Uiso 1 1 calc R . . H24K H 0.1075 0.2174 0.4653 0.103 Uiso 1 1 calc R . . H24L H 0.1024 0.1523 0.4482 0.103 Uiso 1 1 calc R . . C25A C 0.1211(3) 0.2782(3) 0.3690(2) 0.0528(18) Uani 1 1 d . . . H25A H 0.0768 0.2736 0.3640 0.079 Uiso 1 1 calc R . . H25B H 0.1295 0.3167 0.3597 0.079 Uiso 1 1 calc R . . H25C H 0.1421 0.2740 0.3983 0.079 Uiso 1 1 calc R . . C25 C 0.1295(3) 0.5353(3) 0.12920(19) 0.0481(16) Uani 1 1 d . . . H25D H 0.1738 0.5294 0.1350 0.072 Uiso 1 1 calc R . . H25E H 0.1218 0.5745 0.1377 0.072 Uiso 1 1 calc R . . H25F H 0.1094 0.5307 0.0998 0.072 Uiso 1 1 calc R . . C25B C 0.4000(3) 0.3055(3) 0.1331(2) 0.0560(19) Uani 1 1 d . . . H25G H 0.4072 0.2638 0.1381 0.084 Uiso 1 1 calc R . . H25H H 0.3891 0.3131 0.1036 0.084 Uiso 1 1 calc R . . H25I H 0.3664 0.3180 0.1436 0.084 Uiso 1 1 calc R . . C25C C 0.1470(3) 0.0521(3) 0.13148(18) 0.0494(17) Uani 1 1 d . . . H25J H 0.1555 0.0108 0.1372 0.074 Uiso 1 1 calc R . . H25K H 0.1383 0.0591 0.1020 0.074 Uiso 1 1 calc R . . H25L H 0.1115 0.0635 0.1402 0.074 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 O1B 0.063(3) 0.049(3) 0.069(3) 0.021(2) -0.004(2) -0.014(2) O1D 0.067(3) 0.045(3) 0.078(4) 0.014(2) 0.001(3) -0.010(2) O1 0.035(3) 0.089(3) 0.075(4) 0.022(3) 0.008(2) -0.005(2) O1A 0.030(3) 0.081(3) 0.057(3) -0.023(2) 0.001(2) 0.006(2) N1B 0.037(3) 0.041(3) 0.031(3) 0.001(2) 0.009(2) 0.003(2) N1C 0.038(3) 0.032(3) 0.049(3) 0.009(2) 0.013(2) 0.000(2) N1 0.035(3) 0.039(3) 0.043(3) 0.004(2) 0.006(2) 0.001(2) N1A 0.039(3) 0.036(3) 0.041(3) -0.002(2) 0.015(2) 0.001(2) C1 0.039(4) 0.034(3) 0.044(4) 0.002(3) 0.016(3) 0.000(3) C1A 0.044(4) 0.035(3) 0.041(4) 0.003(3) 0.014(3) 0.000(3) C1B 0.036(3) 0.035(3) 0.055(4) 0.007(3) 0.016(3) -0.001(3) C1C 0.029(3) 0.036(3) 0.037(3) -0.004(3) 0.007(3) -0.003(2) N2B 0.054(3) 0.034(3) 0.035(3) 0.005(2) 0.012(2) -0.004(2) N2C 0.048(3) 0.037(3) 0.039(3) 0.003(2) 0.006(2) -0.002(2) N2 0.034(3) 0.053(3) 0.036(3) 0.009(2) 0.002(2) -0.001(2) N2A 0.035(3) 0.050(3) 0.028(3) -0.003(2) 0.006(2) 0.000(2) C2A 0.039(4) 0.038(3) 0.047(4) 0.001(3) 0.012(3) -0.002(3) C2B 0.038(4) 0.039(3) 0.047(4) 0.001(3) 0.009(3) 0.004(3) C2C 0.032(3) 0.038(3) 0.042(4) -0.002(3) 0.004(3) -0.001(3) C2 0.043(4) 0.040(3) 0.031(3) 0.003(3) 0.012(3) -0.004(3) N3B 0.043(3) 0.053(3) 0.038(3) 0.014(3) 0.010(2) 0.007(3) N3C 0.048(3) 0.056(3) 0.047(4) 0.012(3) 0.019(3) 0.004(3) N3 0.047(3) 0.042(3) 0.044(3) 0.000(2) 0.008(3) 0.004(2) N3A 0.055(3) 0.041(3) 0.042(3) 0.010(2) 0.007(3) 0.002(3) C3B 0.055(4) 0.050(4) 0.044(4) -0.002(3) 0.016(3) -0.001(3) C3 0.054(4) 0.062(4) 0.044(4) -0.001(3) 0.008(3) 0.009(3) C3C 0.062(5) 0.055(4) 0.045(4) -0.003(3) 0.014(3) 0.001(3) C3A 0.049(4) 0.055(4) 0.047(4) 0.005(3) 0.016(3) -0.005(3) N4B 0.050(3) 0.046(3) 0.043(3) 0.006(2) 0.022(3) 0.002(2) N4C 0.051(3) 0.042(3) 0.047(3) 0.005(2) 0.019(3) 0.005(2) N4 0.035(3) 0.057(3) 0.049(3) -0.013(3) 0.012(2) -0.002(2) N4A 0.047(3) 0.054(3) 0.035(3) 0.010(2) 0.012(2) 0.003(3) C4 0.053(5) 0.079(5) 0.053(5) 0.006(4) 0.021(4) 0.011(4) C4A 0.058(5) 0.077(5) 0.046(4) 0.017(4) 0.029(4) -0.001(4) C4B 0.062(5) 0.046(4) 0.064(5) -0.005(4) 0.012(4) 0.007(3) C4C 0.075(5) 0.055(4) 0.059(5) -0.016(4) 0.031(4) 0.003(4) C5 0.048(4) 0.075(5) 0.071(5) 0.000(4) 0.029(4) 0.004(4) C5A 0.040(4) 0.077(5) 0.068(5) 0.006(4) 0.022(4) -0.006(4) C5B 0.058(4) 0.032(3) 0.079(5) 0.002(4) 0.021(4) 0.003(3) C5C 0.080(5) 0.035(3) 0.064(5) -0.010(3) 0.019(4) 0.000(3) C6B 0.043(4) 0.041(3) 0.041(4) -0.001(3) 0.013(3) 0.000(3) C6C 0.038(4) 0.038(3) 0.085(6) 0.000(4) 0.018(4) -0.002(3) C6 0.048(4) 0.040(3) 0.055(4) 0.000(3) 0.021(3) 0.003(3) C6A 0.029(4) 0.053(4) 0.063(5) 0.004(3) 0.014(3) -0.002(3) C7B 0.061(5) 0.031(3) 0.079(5) 0.015(4) 0.029(4) 0.007(3) C7C 0.077(5) 0.037(4) 0.067(5) 0.020(4) 0.031(4) 0.006(3) C7 0.031(4) 0.066(4) 0.069(5) -0.010(4) 0.007(3) -0.009(3) C7A 0.031(4) 0.075(5) 0.065(5) 0.010(4) 0.019(3) 0.002(3) C8B 0.065(5) 0.041(4) 0.065(5) 0.019(3) 0.033(4) 0.012(3) C8 0.040(4) 0.061(4) 0.058(5) -0.014(4) 0.007(3) -0.004(3) C8A 0.029(4) 0.063(4) 0.044(4) -0.001(3) 0.000(3) 0.001(3) C8C 0.066(5) 0.058(4) 0.038(4) 0.004(3) 0.019(3) 0.000(4) C9B 0.031(3) 0.051(4) 0.042(4) 0.008(3) 0.014(3) -0.005(3) C9 0.038(4) 0.027(3) 0.055(4) 0.005(3) 0.007(3) 0.004(3) C9A 0.042(4) 0.038(3) 0.034(3) 0.009(3) 0.013(3) 0.007(3) C9C 0.037(3) 0.030(3) 0.050(4) 0.005(3) 0.007(3) 0.002(3) C10B 0.027(3) 0.035(3) 0.048(4) 0.008(3) 0.007(3) 0.003(2) C10 0.036(4) 0.032(3) 0.046(4) -0.002(3) 0.007(3) 0.001(3) C10A 0.045(4) 0.036(3) 0.044(4) 0.000(3) 0.014(3) 0.005(3) C10C 0.035(3) 0.042(3) 0.046(4) 0.005(3) 0.015(3) -0.003(3) C11C 0.039(4) 0.056(4) 0.045(4) 0.001(3) 0.009(3) 0.004(3) C11A 0.048(4) 0.041(3) 0.043(4) -0.001(3) 0.014(3) -0.003(3) C11B 0.030(3) 0.064(4) 0.040(4) 0.004(3) 0.011(3) 0.000(3) C11 0.054(4) 0.035(3) 0.043(4) 0.003(3) 0.013(3) 0.003(3) C12 0.081(5) 0.046(4) 0.038(4) 0.009(3) 0.008(4) 0.004(4) C12B 0.041(4) 0.089(5) 0.048(4) 0.019(4) 0.016(3) 0.011(4) C12C 0.081(6) 0.056(4) 0.072(5) -0.009(4) 0.034(4) -0.003(4) C12A 0.061(5) 0.079(5) 0.077(6) 0.011(4) 0.027(4) -0.001(4) C13 0.095(6) 0.058(4) 0.047(4) -0.002(4) 0.029(4) 0.014(4) C13B 0.048(4) 0.089(5) 0.047(4) -0.020(4) 0.016(3) 0.003(4) C13C 0.074(6) 0.076(5) 0.077(6) -0.027(5) 0.022(5) 0.013(4) C13A 0.107(8) 0.082(6) 0.086(7) 0.008(5) 0.056(6) -0.013(5) C14C 0.055(5) 0.108(6) 0.049(5) -0.013(5) 0.015(4) 0.003(5) C14A 0.124(8) 0.062(5) 0.048(5) 0.002(4) 0.035(5) -0.015(5) C14B 0.061(5) 0.075(5) 0.068(5) -0.023(4) 0.018(4) -0.001(4) C14 0.085(6) 0.082(5) 0.055(5) 0.013(4) 0.039(4) 0.013(5) C15C 0.051(4) 0.093(6) 0.045(4) -0.005(4) 0.011(3) -0.007(4) C15A 0.077(5) 0.052(4) 0.047(4) 0.002(3) 0.016(4) -0.012(4) C15B 0.066(5) 0.067(5) 0.071(5) -0.003(4) 0.027(4) -0.001(4) C15 0.063(5) 0.077(5) 0.053(5) -0.001(4) 0.030(4) -0.001(4) C16 0.049(4) 0.037(3) 0.052(4) -0.001(3) 0.018(3) -0.002(3) C16B 0.043(4) 0.046(4) 0.052(4) -0.006(3) 0.020(3) -0.003(3) C16C 0.033(4) 0.061(4) 0.043(4) -0.002(3) 0.006(3) 0.005(3) C16A 0.068(5) 0.036(3) 0.037(4) -0.002(3) 0.013(3) -0.009(3) C17B 0.055(4) 0.031(3) 0.040(4) 0.006(3) 0.019(3) -0.001(3) C17C 0.049(4) 0.042(3) 0.035(4) 0.003(3) 0.017(3) -0.004(3) C17 0.037(4) 0.048(4) 0.045(4) -0.001(3) 0.014(3) -0.010(3) C17A 0.036(4) 0.051(4) 0.029(3) 0.005(3) -0.001(3) -0.003(3) C18B 0.048(4) 0.025(3) 0.037(4) -0.006(3) 0.019(3) -0.003(3) C18C 0.032(3) 0.042(3) 0.035(4) 0.011(3) 0.008(3) 0.010(3) C18 0.035(3) 0.043(3) 0.041(4) -0.010(3) 0.003(3) -0.006(3) C18A 0.028(3) 0.049(3) 0.038(4) -0.003(3) 0.011(3) -0.004(3) C19B 0.052(4) 0.040(3) 0.048(4) 0.006(3) 0.021(3) 0.004(3) C19C 0.054(4) 0.054(4) 0.052(4) 0.012(3) 0.007(3) -0.005(3) C19 0.074(5) 0.045(4) 0.045(4) 0.000(3) 0.022(4) 0.000(4) C19A 0.040(4) 0.050(4) 0.055(4) 0.003(3) 0.006(3) 0.008(3) C20B 0.042(4) 0.052(4) 0.088(6) -0.015(4) 0.033(4) -0.013(3) C20C 0.079(6) 0.074(5) 0.045(4) -0.002(4) 0.002(4) -0.015(4) C20 0.065(5) 0.042(4) 0.072(6) 0.000(4) 0.010(4) -0.005(3) C20A 0.065(5) 0.038(4) 0.097(6) -0.002(4) 0.045(5) 0.012(3) C21B 0.038(4) 0.076(5) 0.075(6) -0.032(4) 0.008(4) 0.000(4) C21C 0.028(3) 0.049(4) 0.077(5) -0.003(4) -0.002(3) -0.006(3) C21 0.059(5) 0.066(5) 0.085(6) 0.043(4) 0.025(4) 0.008(4) C21A 0.090(6) 0.058(5) 0.083(6) -0.030(4) 0.049(5) -0.015(4) C22B 0.059(5) 0.099(6) 0.058(5) -0.009(4) 0.013(4) -0.017(5) C22 0.079(6) 0.079(5) 0.047(5) 0.018(4) 0.005(4) -0.017(5) C22A 0.072(5) 0.082(5) 0.054(5) -0.009(4) 0.032(4) -0.011(5) C22C 0.047(4) 0.067(5) 0.074(6) 0.011(4) 0.017(4) -0.008(4) C23B 0.050(4) 0.053(4) 0.038(4) 0.011(3) 0.015(3) 0.004(3) C23C 0.051(4) 0.070(5) 0.057(5) 0.006(4) 0.024(4) -0.001(4) C23 0.048(4) 0.052(4) 0.049(4) 0.002(3) 0.000(3) 0.003(3) C23A 0.037(3) 0.064(4) 0.033(3) -0.008(3) 0.015(3) -0.006(3) C24B 0.135(7) 0.039(4) 0.061(5) -0.006(3) 0.048(5) 0.009(4) C24C 0.134(7) 0.035(4) 0.069(5) 0.007(4) 0.050(5) 0.011(4) C24 0.037(4) 0.130(7) 0.072(6) -0.038(5) 0.008(4) 0.009(4) C24A 0.039(4) 0.110(6) 0.058(5) 0.025(4) 0.016(3) 0.006(4) C25A 0.047(4) 0.045(4) 0.058(5) -0.005(3) 0.003(3) 0.010(3) C25 0.053(4) 0.056(4) 0.038(4) 0.008(3) 0.018(3) -0.005(3) C25B 0.047(4) 0.048(4) 0.067(5) 0.011(3) 0.008(3) -0.006(3) C25C 0.051(4) 0.057(4) 0.034(4) -0.002(3) 0.004(3) -0.006(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 O1B C17B 1.232(6) . ? O1D C17C 1.220(6) . ? O1 C17 1.227(7) . ? O1A C17A 1.217(7) . ? N1B C9B 1.307(7) . ? N1B C1B 1.366(7) . ? N1C C9C 1.318(7) . ? N1C C1C 1.352(7) . ? N1 C9 1.322(7) . ? N1 C1 1.367(7) . ? N1A C9A 1.339(7) . ? N1A C1A 1.360(7) . ? C1 C2 1.410(8) . ? C1 C6 1.425(8) . ? C1A C6A 1.401(8) . ? C1A C2A 1.433(8) . ? C1B C2B 1.411(8) . ? C1B C6B 1.420(8) . ? C1C C6C 1.411(8) . ? C1C C2C 1.436(8) . ? N2B C17B 1.350(7) . ? N2B C2B 1.433(7) . ? N2B C25B 1.460(7) . ? N2C C17C 1.357(7) . ? N2C C2C 1.450(7) . ? N2C C25C 1.458(7) . ? N2 C17 1.353(7) . ? N2 C2 1.432(7) . ? N2 C25 1.449(7) . ? N2A C17A 1.346(7) . ? N2A C2A 1.436(7) . ? N2A C25A 1.469(7) . ? C2A C3A 1.359(8) . ? C2B C3B 1.361(8) . ? C2C C3C 1.364(8) . ? C2 C3 1.368(8) . ? N3B C10B 1.307(7) . ? N3B C11B 1.387(8) . ? N3C C10C 1.315(7) . ? N3C C16C 1.387(8) . ? N3 C10 1.324(7) . ? N3 C11 1.380(8) . ? N3A C10A 1.324(7) . ? N3A C16A 1.367(8) . ? C3B C4B 1.396(8) . ? C3B H3BB 0.9300 . ? C3 C4 1.393(9) . ? C3 H3B 0.9300 . ? C3C C4C 1.409(9) . ? C3C H3CB 0.9300 . ? C3A C4A 1.405(8) . ? C3A H3AB 0.9300 . ? N4B C16B 1.364(7) . ? N4B C10B 1.379(7) . ? N4B C24B 1.456(8) . ? N4C C10C 1.379(7) . ? N4C C11C 1.392(8) . ? N4C C24C 1.461(8) . ? N4 C10 1.362(7) . ? N4 C16 1.389(7) . ? N4 C24 1.467(7) . ? N4A C10A 1.388(7) . ? N4A C11A 1.382(7) . ? N4A C24A 1.442(7) . ? C4 C5 1.323(9) . ? C4 H4A 0.9300 . ? C4A C5A 1.365(9) . ? C4A H4AA 0.9300 . ? C4B C5B 1.347(9) . ? C4B H4BA 0.9300 . ? C4C C5C 1.367(9) . ? C4C H4CA 0.9300 . ? C5 C6 1.419(9) . ? C5 H5A 0.9300 . ? C5A C6A 1.417(9) . ? C5A H5AA 0.9300 . ? C5B C6B 1.401(9) . ? C5B H5BA 0.9300 . ? C5C C6C 1.424(9) . ? C5C H5CA 0.9300 . ? C6B C7B 1.431(8) . ? C6C C7C 1.384(9) . ? C6 C7 1.414(9) . ? C6A C7A 1.402(9) . ? C7B C8B 1.334(9) . ? C7B H7BA 0.9300 . ? C7C C8C 1.358(9) . ? C7C H7CA 0.9300 . ? C7 C8 1.353(9) . ? C7 H7A 0.9300 . ? C7A C8A 1.363(9) . ? C7A H7AA 0.9300 . ? C8B C9B 1.421(8) . ? C8B H8BA 0.9300 . ? C8 C9 1.405(8) . ? C8 H8A 0.9300 . ? C8A C9A 1.396(8) . ? C8A H8AA 0.9300 . ? C8C C9C 1.414(8) . ? C8C H8CA 0.9300 . ? C9B C10B 1.473(8) . ? C9 C10 1.476(8) . ? C9A C10A 1.456(8) . ? C9C C10C 1.457(8) . ? C11C C12C 1.374(9) . ? C11C C16C 1.392(8) . ? C11A C12A 1.379(9) . ? C11A C16A 1.386(8) . ? C11B C16B 1.373(8) . ? C11B C12B 1.421(9) . ? C11 C16 1.393(8) . ? C11 C12 1.409(8) . ? C12 C13 1.358(9) . ? C12 H12A 0.9300 . ? C12B C13B 1.376(9) . ? C12B H12B 0.9300 . ? C12C C13C 1.370(10) . ? C12C H12C 0.9300 . ? C12A C13A 1.383(10) . ? C12A H12D 0.9300 . ? C13 C14 1.387(9) . ? C13 H13A 0.9300 . ? C13B C14B 1.368(10) . ? C13B H13B 0.9300 . ? C13C C14C 1.402(10) . ? C13C H13C 0.9300 . ? C13A C14A 1.389(11) . ? C13A H13D 0.9300 . ? C14C C15C 1.374(10) . ? C14C H14A 0.9300 . ? C14A C15A 1.357(10) . ? C14A H14B 0.9300 . ? C14B C15B 1.359(10) . ? C14B H14C 0.9300 . ? C14 C15 1.388(9) . ? C14 H14D 0.9300 . ? C15C C16C 1.383(9) . ? C15C H15A 0.9300 . ? C15A C16A 1.408(9) . ? C15A H15B 0.9300 . ? C15B C16B 1.397(9) . ? C15B H15C 0.9300 . ? C15 C16 1.369(9) . ? C15 H15D 0.9300 . ? C17B C18B 1.497(8) . ? C17C C18C 1.491(8) . ? C17 C18 1.469(8) . ? C17A C18A 1.515(8) . ? C18B C19B 1.375(8) . ? C18B C23B 1.384(8) . ? C18C C23C 1.372(8) . ? C18C C19C 1.374(8) . ? C18 C19 1.358(8) . ? C18 C23 1.375(8) . ? C18A C19A 1.402(8) . ? C18A C23A 1.384(8) . ? C19B C20B 1.364(8) . ? C19B H19A 0.9300 . ? C19C C20C 1.361(8) . ? C19C H19B 0.9300 . ? C19 C20 1.369(9) . ? C19 H19C 0.9300 . ? C19A C20A 1.370(9) . ? C19A H19D 0.9300 . ? C20B C21B 1.373(10) . ? C20B H20A 0.9300 . ? C20C C21C 1.376(9) . ? C20C H20B 0.9300 . ? C20 C21 1.363(10) . ? C20 H20C 0.9300 . ? C20A C21A 1.396(10) . ? C20A H20D 0.9300 . ? C21B C22B 1.369(10) . ? C21B H21A 0.9300 . ? C21C C22C 1.364(10) . ? C21C H21B 0.9300 . ? C21 C22 1.383(9) . ? C21 H21C 0.9300 . ? C21A C22A 1.375(10) . ? C21A H21D 0.9300 . ? C22B C23B 1.383(9) . ? C22B H22A 0.9300 . ? C22 C23 1.370(9) . ? C22 H22B 0.9300 . ? C22A C23A 1.372(9) . ? C22A H22C 0.9300 . ? C22C C23C 1.401(9) . ? C22C H22D 0.9300 . ? C23B H23A 0.9300 . ? C23C H23B 0.9300 . ? C23 H23C 0.9300 . ? C23A H23D 0.9300 . ? C24B H24A 0.9600 . ? C24B H24B 0.9600 . ? C24B H24C 0.9600 . ? C24C H24D 0.9600 . ? C24C H24E 0.9600 . ? C24C H24F 0.9600 . ? C24 H24G 0.9600 . ? C24 H24H 0.9600 . ? C24 H24I 0.9600 . ? C24A H24J 0.9600 . ? C24A H24K 0.9600 . ? C24A H24L 0.9600 . ? C25A H25A 0.9600 . ? C25A H25B 0.9600 . ? C25A H25C 0.9600 . ? C25 H25D 0.9600 . ? C25 H25E 0.9600 . ? C25 H25F 0.9600 . ? C25B H25G 0.9600 . ? C25B H25H 0.9600 . ? C25B H25I 0.9600 . ? C25C H25J 0.9600 . ? C25C H25K 0.9600 . ? C25C H25L 0.9600 . ? 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 C9B N1B C1B 119.3(5) . . ? C9C N1C C1C 117.6(5) . . ? C9 N1 C1 119.0(5) . . ? C9A N1A C1A 116.9(5) . . ? N1 C1 C2 118.8(5) . . ? N1 C1 C6 121.3(5) . . ? C2 C1 C6 119.9(6) . . ? N1A C1A C6A 124.0(6) . . ? N1A C1A C2A 117.8(5) . . ? C6A C1A C2A 118.1(6) . . ? N1B C1B C2B 119.5(5) . . ? N1B C1B C6B 121.7(5) . . ? C2B C1B C6B 118.8(6) . . ? N1C C1C C6C 123.9(6) . . ? N1C C1C C2C 117.5(5) . . ? C6C C1C C2C 118.6(6) . . ? C17B N2B C2B 124.0(5) . . ? C17B N2B C25B 117.3(5) . . ? C2B N2B C25B 117.8(5) . . ? C17C N2C C2C 123.9(5) . . ? C17C N2C C25C 118.3(5) . . ? C2C N2C C25C 117.4(4) . . ? C17 N2 C2 121.9(5) . . ? C17 N2 C25 118.6(5) . . ? C2 N2 C25 119.0(4) . . ? C17A N2A C2A 126.1(5) . . ? C17A N2A C25A 116.7(5) . . ? C2A N2A C25A 116.7(5) . . ? C3A C2A N2A 120.8(5) . . ? C3A C2A C1A 120.3(6) . . ? N2A C2A C1A 118.9(5) . . ? C3B C2B N2B 121.7(6) . . ? C3B C2B C1B 120.5(5) . . ? N2B C2B C1B 117.7(5) . . ? C3C C2C N2C 120.3(6) . . ? C3C C2C C1C 120.1(5) . . ? N2C C2C C1C 119.6(5) . . ? C3 C2 C1 119.4(6) . . ? C3 C2 N2 121.9(5) . . ? C1 C2 N2 118.6(5) . . ? C10B N3B C11B 105.1(5) . . ? C10C N3C C16C 106.2(5) . . ? C10 N3 C11 104.9(5) . . ? C10A N3A C16A 106.1(5) . . ? C2B C3B C4B 119.4(6) . . ? C2B C3B H3BB 120.3 . . ? C4B C3B H3BB 120.3 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3B 120.3 . . ? C4 C3 H3B 120.3 . . ? C2C C3C C4C 121.9(6) . . ? C2C C3C H3CB 119.1 . . ? C4C C3C H3CB 119.1 . . ? C2A C3A C4A 121.8(6) . . ? C2A C3A H3AB 119.1 . . ? C4A C3A H3AB 119.1 . . ? C16B N4B C10B 106.7(5) . . ? C16B N4B C24B 123.2(5) . . ? C10B N4B C24B 130.0(5) . . ? C10C N4C C11C 107.0(5) . . ? C10C N4C C24C 130.3(5) . . ? C11C N4C C24C 122.7(5) . . ? C10 N4 C16 106.9(5) . . ? C10 N4 C24 129.7(5) . . ? C16 N4 C24 123.3(5) . . ? C10A N4A C11A 106.7(5) . . ? C10A N4A C24A 129.9(5) . . ? C11A N4A C24A 123.4(5) . . ? C5 C4 C3 123.8(7) . . ? C5 C4 H4A 118.1 . . ? C3 C4 H4A 118.1 . . ? C5A C4A C3A 118.7(6) . . ? C5A C4A H4AA 120.7 . . ? C3A C4A H4AA 120.7 . . ? C5B C4B C3B 122.5(7) . . ? C5B C4B H4BA 118.8 . . ? C3B C4B H4BA 118.8 . . ? C5C C4C C3C 118.6(6) . . ? C5C C4C H4CA 120.7 . . ? C3C C4C H4CA 120.7 . . ? C4 C5 C6 119.3(7) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C4A C5A C6A 121.6(6) . . ? C4A C5A H5AA 119.2 . . ? C6A C5A H5AA 119.2 . . ? C4B C5B C6B 119.5(6) . . ? C4B C5B H5BA 120.3 . . ? C6B C5B H5BA 120.3 . . ? C4C C5C C6C 122.0(6) . . ? C4C C5C H5CA 119.0 . . ? C6C C5C H5CA 119.0 . . ? C5B C6B C1B 119.4(6) . . ? C5B C6B C7B 124.1(6) . . ? C1B C6B C7B 116.5(6) . . ? C7C C6C C1C 116.3(6) . . ? C7C C6C C5C 124.9(6) . . ? C1C C6C C5C 118.8(7) . . ? C1 C6 C5 118.3(6) . . ? C1 C6 C7 117.0(6) . . ? C5 C6 C7 124.8(6) . . ? C1A C6A C7A 116.2(6) . . ? C1A C6A C5A 119.5(6) . . ? C7A C6A C5A 124.2(6) . . ? C8B C7B C6B 120.5(6) . . ? C8B C7B H7BA 119.8 . . ? C6B C7B H7BA 119.8 . . ? C8C C7C C6C 120.9(6) . . ? C8C C7C H7CA 119.6 . . ? C6C C7C H7CA 119.6 . . ? C8 C7 C6 120.9(6) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C8A C7A C6A 120.8(6) . . ? C8A C7A H7AA 119.6 . . ? C6A C7A H7AA 119.6 . . ? C7B C8B C9B 119.2(6) . . ? C7B C8B H8BA 120.4 . . ? C9B C8B H8BA 120.4 . . ? C7 C8 C9 118.4(6) . . ? C7 C8 H8A 120.8 . . ? C9 C8 H8A 120.8 . . ? C7A C8A C9A 118.7(6) . . ? C7A C8A H8AA 120.7 . . ? C9A C8A H8AA 120.7 . . ? C7C C8C C9C 118.8(6) . . ? C7C C8C H8CA 120.6 . . ? C9C C8C H8CA 120.6 . . ? N1B C9B C8B 122.7(6) . . ? N1B C9B C10B 118.9(5) . . ? C8B C9B C10B 118.3(6) . . ? N1 C9 C8 123.4(6) . . ? N1 C9 C10 117.6(5) . . ? C8 C9 C10 119.1(6) . . ? N1A C9A C8A 123.3(6) . . ? N1A C9A C10A 117.5(5) . . ? C8A C9A C10A 119.2(5) . . ? N1C C9C C8C 122.6(6) . . ? N1C C9C C10C 119.2(5) . . ? C8C C9C C10C 118.1(6) . . ? N3B C10B N4B 112.1(5) . . ? N3B C10B C9B 123.9(5) . . ? N4B C10B C9B 124.1(5) . . ? N3 C10 N4 112.7(5) . . ? N3 C10 C9 121.7(5) . . ? N4 C10 C9 125.6(5) . . ? N3A C10A N4A 111.1(5) . . ? N3A C10A C9A 123.4(6) . . ? N4A C10A C9A 125.4(5) . . ? N3C C10C N4C 111.7(6) . . ? N3C C10C C9C 124.0(5) . . ? N4C C10C C9C 124.2(5) . . ? C12C C11C C16C 122.5(7) . . ? C12C C11C N4C 132.2(6) . . ? C16C C11C N4C 105.3(5) . . ? C12A C11A C16A 123.0(6) . . ? C12A C11A N4A 131.6(6) . . ? C16A C11A N4A 105.5(5) . . ? N3B C11B C16B 110.2(5) . . ? N3B C11B C12B 129.7(6) . . ? C16B C11B C12B 120.1(6) . . ? N3 C11 C16 110.5(5) . . ? N3 C11 C12 131.2(6) . . ? C16 C11 C12 118.3(6) . . ? C13 C12 C11 118.7(7) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? C13B C12B C11B 116.5(6) . . ? C13B C12B H12B 121.8 . . ? C11B C12B H12B 121.8 . . ? C11C C12C C13C 117.1(7) . . ? C11C C12C H12C 121.4 . . ? C13C C12C H12C 121.4 . . ? C11A C12A C13A 116.8(7) . . ? C11A C12A H12D 121.6 . . ? C13A C12A H12D 121.6 . . ? C12 C13 C14 121.7(7) . . ? C12 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C12B C13B C14B 122.4(7) . . ? C12B C13B H13B 118.8 . . ? C14B C13B H13B 118.8 . . ? C14C C13C C12C 121.1(7) . . ? C14C C13C H13C 119.4 . . ? C12C C13C H13C 119.4 . . ? C14A C13A C12A 120.8(8) . . ? C14A C13A H13D 119.6 . . ? C12A C13A H13D 119.6 . . ? C15C C14C C13C 121.2(7) . . ? C15C C14C H14A 119.4 . . ? C13C C14C H14A 119.4 . . ? C13A C14A C15A 122.5(7) . . ? C13A C14A H14B 118.8 . . ? C15A C14A H14B 118.8 . . ? C15B C14B C13B 121.8(7) . . ? C15B C14B H14C 119.1 . . ? C13B C14B H14C 119.1 . . ? C15 C14 C13 120.9(7) . . ? C15 C14 H14D 119.5 . . ? C13 C14 H14D 119.5 . . ? C14C C15C C16C 117.8(7) . . ? C14C C15C H15A 121.1 . . ? C16C C15C H15A 121.1 . . ? C14A C15A C16A 117.7(7) . . ? C14A C15A H15B 121.1 . . ? C16A C15A H15B 121.1 . . ? C14B C15B C16B 117.4(7) . . ? C14B C15B H15C 121.3 . . ? C16B C15B H15C 121.3 . . ? C16 C15 C14 117.0(7) . . ? C16 C15 H15D 121.5 . . ? C14 C15 H15D 121.5 . . ? N4 C16 C11 104.9(5) . . ? N4 C16 C15 131.6(6) . . ? C11 C16 C15 123.4(6) . . ? N4B C16B C11B 106.0(5) . . ? N4B C16B C15B 132.2(6) . . ? C11B C16B C15B 121.8(6) . . ? N3C C16C C11C 109.8(6) . . ? N3C C16C C15C 130.1(6) . . ? C11C C16C C15C 120.1(6) . . ? N3A C16A C11A 110.6(5) . . ? N3A C16A C15A 130.1(6) . . ? C11A C16A C15A 119.2(7) . . ? O1B C17B N2B 119.7(5) . . ? O1B C17B C18B 119.1(5) . . ? N2B C17B C18B 121.2(5) . . ? O1D C17C N2C 120.1(5) . . ? O1D C17C C18C 121.9(5) . . ? N2C C17C C18C 118.0(5) . . ? O1 C17 N2 119.5(6) . . ? O1 C17 C18 120.3(6) . . ? N2 C17 C18 120.2(5) . . ? O1A C17A N2A 121.4(6) . . ? O1A C17A C18A 119.5(5) . . ? N2A C17A C18A 119.2(5) . . ? C19B C18B C23B 118.9(6) . . ? C19B C18B C17B 123.8(6) . . ? C23B C18B C17B 117.2(5) . . ? C23C C18C C19C 119.8(6) . . ? C23C C18C C17C 121.4(6) . . ? C19C C18C C17C 118.7(6) . . ? C19 C18 C23 117.7(6) . . ? C19 C18 C17 122.6(6) . . ? C23 C18 C17 119.7(5) . . ? C19A C18A C23A 118.5(6) . . ? C19A C18A C17A 124.7(5) . . ? C23A C18A C17A 116.6(5) . . ? C20B C19B C18B 120.7(6) . . ? C20B C19B H19A 119.7 . . ? C18B C19B H19A 119.7 . . ? C18C C19C C20C 120.5(7) . . ? C18C C19C H19B 119.8 . . ? C20C C19C H19B 119.8 . . ? C18 C19 C20 121.3(7) . . ? C18 C19 H19C 119.3 . . ? C20 C19 H19C 119.3 . . ? C18A C19A C20A 120.9(6) . . ? C18A C19A H19D 119.5 . . ? C20A C19A H19D 119.5 . . ? C21B C20B C19B 121.1(7) . . ? C21B C20B H20A 119.5 . . ? C19B C20B H20A 119.5 . . ? C21C C20C C19C 120.3(7) . . ? C21C C20C H20B 119.8 . . ? C19C C20C H20B 119.8 . . ? C21 C20 C19 121.0(7) . . ? C21 C20 H20C 119.5 . . ? C19 C20 H20C 119.5 . . ? C21A C20A C19A 119.7(7) . . ? C21A C20A H20D 120.1 . . ? C19A C20A H20D 120.1 . . ? C20B C21B C22B 118.6(7) . . ? C20B C21B H21A 120.7 . . ? C22B C21B H21A 120.7 . . ? C20C C21C C22C 120.2(6) . . ? C20C C21C H21B 119.9 . . ? C22C C21C H21B 119.9 . . ? C20 C21 C22 118.6(7) . . ? C20 C21 H21C 120.7 . . ? C22 C21 H21C 120.7 . . ? C22A C21A C20A 119.3(7) . . ? C22A C21A H21D 120.4 . . ? C20A C21A H21D 120.4 . . ? C23B C22B C21B 121.1(7) . . ? C23B C22B H22A 119.5 . . ? C21B C22B H22A 119.5 . . ? C23 C22 C21 119.4(7) . . ? C23 C22 H22B 120.3 . . ? C21 C22 H22B 120.3 . . ? C21A C22A C23A 121.1(7) . . ? C21A C22A H22C 119.4 . . ? C23A C22A H22C 119.4 . . ? C21C C22C C23C 119.6(7) . . ? C21C C22C H22D 120.2 . . ? C23C C22C H22D 120.2 . . ? C22B C23B C18B 119.6(6) . . ? C22B C23B H23A 120.2 . . ? C18B C23B H23A 120.2 . . ? C18C C23C C22C 119.6(7) . . ? C18C C23C H23B 120.2 . . ? C22C C23C H23B 120.2 . . ? C18 C23 C22 121.9(6) . . ? C18 C23 H23C 119.0 . . ? C22 C23 H23C 119.0 . . ? C22A C23A C18A 120.4(6) . . ? C22A C23A H23D 119.8 . . ? C18A C23A H23D 119.8 . . ? N4B C24B H24A 109.5 . . ? N4B C24B H24B 109.5 . . ? H24A C24B H24B 109.5 . . ? N4B C24B H24C 109.5 . . ? H24A C24B H24C 109.5 . . ? H24B C24B H24C 109.5 . . ? N4C C24C H24D 109.5 . . ? N4C C24C H24E 109.5 . . ? H24D C24C H24E 109.5 . . ? N4C C24C H24F 109.5 . . ? H24D C24C H24F 109.5 . . ? H24E C24C H24F 109.5 . . ? N4 C24 H24G 109.5 . . ? N4 C24 H24H 109.5 . . ? H24G C24 H24H 109.5 . . ? N4 C24 H24I 109.5 . . ? H24G C24 H24I 109.5 . . ? H24H C24 H24I 109.5 . . ? N4A C24A H24J 109.5 . . ? N4A C24A H24K 109.5 . . ? H24J C24A H24K 109.5 . . ? N4A C24A H24L 109.5 . . ? H24J C24A H24L 109.5 . . ? H24K C24A H24L 109.5 . . ? N2A C25A H25A 109.5 . . ? N2A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? N2A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? N2 C25 H25D 109.5 . . ? N2 C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? N2 C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? N2B C25B H25G 109.5 . . ? N2B C25B H25H 109.5 . . ? H25G C25B H25H 109.5 . . ? N2B C25B H25I 109.5 . . ? H25G C25B H25I 109.5 . . ? H25H C25B H25I 109.5 . . ? N2C C25C H25J 109.5 . . ? N2C C25C H25K 109.5 . . ? H25J C25C H25K 109.5 . . ? N2C C25C H25L 109.5 . . ? H25J C25C H25L 109.5 . . ? H25K C25C H25L 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.337 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.084 #===END data_5a _database_code_depnum_ccdc_archive 'CCDC 713151' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H34 N8 Ni O3' _chemical_formula_weight 817.53 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.456(3) _cell_length_b 13.234(3) _cell_length_c 19.459(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.32(3) _cell_angle_gamma 90.00 _cell_volume 3891.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1639 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8559 _exptl_absorpt_correction_T_max 0.9467 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _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 ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 12578 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6813 _reflns_number_gt 4986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.1000P)^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 6813 _refine_ls_number_parameters 521 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1796 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Ni1 Ni 0.34098(4) -0.55158(5) -0.37075(3) 0.0287(2) Uani 1 1 d . . . O1 O 0.6052(3) -0.6670(4) -0.2834(2) 0.0636(14) Uani 1 1 d . . . O1A O 0.3799(3) -0.8634(3) -0.3118(2) 0.0473(10) Uani 1 1 d . . . O3 O 0.7608(3) -0.2078(4) -0.1817(2) 0.0743(16) Uani 1 1 d D . . H47 H 0.8161 -0.2043 -0.1843 0.089 Uiso 1 1 d RD . . N2 N 0.4854(3) -0.5587(4) -0.3256(2) 0.0408(11) Uani 1 1 d . . . N1 N 0.3752(3) -0.4847(3) -0.2703(2) 0.0312(10) Uani 1 1 d . . . N3 N 0.2160(3) -0.5310(3) -0.3629(2) 0.0320(10) Uani 1 1 d . . . N4 N 0.14864(13) -0.47447(15) -0.29073(10) 0.0370(11) Uani 1 1 d D . . H100 H 0.1438 -0.4349 -0.2556 0.044 Uiso 1 1 d RD . . N2A N 0.32519(13) -0.71173(15) -0.36922(10) 0.0322(10) Uani 1 1 d R . . N1A N 0.29440(13) -0.58454(15) -0.47987(10) 0.0295(10) Uani 1 1 d R . . N3A N 0.33598(13) -0.40410(15) -0.42322(10) 0.0373(11) Uani 1 1 d R . . N4A N 0.29924(13) -0.32304(15) -0.53176(10) 0.0376(11) Uani 1 1 d RD . . H200 H 0.2758 -0.3165 -0.5815 0.045 Uiso 1 1 d RD . . C23 C 0.4810(4) -0.6262(6) -0.4723(3) 0.0565(18) Uani 1 1 d . . . H23A H 0.4818 -0.5561 -0.4689 0.068 Uiso 1 1 calc R . . C22 C 0.4580(5) -0.6721(8) -0.5411(4) 0.079(3) Uani 1 1 d . . . H22A H 0.4442 -0.6331 -0.5840 0.095 Uiso 1 1 calc R . . C21 C 0.4557(5) -0.7750(10) -0.5460(5) 0.091(3) Uani 1 1 d . . . H21A H 0.4407 -0.8060 -0.5923 0.109 Uiso 1 1 calc R . . C20 C 0.4758(6) -0.8336(7) -0.4820(6) 0.084(3) Uani 1 1 d . . . H20A H 0.4717 -0.9037 -0.4858 0.101 Uiso 1 1 calc R . . C19 C 0.5017(5) -0.7878(6) -0.4134(4) 0.0638(19) Uani 1 1 d . . . H19A H 0.5186 -0.8271 -0.3703 0.077 Uiso 1 1 calc R . . C18 C 0.5029(4) -0.6845(5) -0.4078(3) 0.0451(15) Uani 1 1 d . . . C17 C 0.5347(4) -0.6343(5) -0.3331(3) 0.0438(15) Uani 1 1 d . . . C2 C 0.5218(4) -0.4989(4) -0.2607(3) 0.0375(13) Uani 1 1 d . . . C3 C 0.6084(4) -0.4673(5) -0.2250(4) 0.0583(18) Uani 1 1 d . . . H3A H 0.6504 -0.4883 -0.2428 0.070 Uiso 1 1 calc R . . C4 C 0.6340(5) -0.4037(5) -0.1620(4) 0.062(2) Uani 1 1 d . . . H4B H 0.6931 -0.3845 -0.1392 0.075 Uiso 1 1 calc R . . C5 C 0.5767(5) -0.3689(5) -0.1327(4) 0.0592(18) Uani 1 1 d . . . H5A H 0.5964 -0.3282 -0.0903 0.071 Uiso 1 1 calc R . . C6 C 0.4876(4) -0.3959(4) -0.1681(3) 0.0445(15) Uani 1 1 d . . . C7 C 0.4195(5) -0.3617(5) -0.1462(3) 0.0520(17) Uani 1 1 d . . . H7A H 0.4336 -0.3203 -0.1044 0.062 Uiso 1 1 calc R . . C8 C 0.3337(4) -0.3891(4) -0.1859(3) 0.0414(14) Uani 1 1 d . . . H8A H 0.2895 -0.3678 -0.1708 0.050 Uiso 1 1 calc R . . C9 C 0.3128(4) -0.4498(4) -0.2498(3) 0.0351(12) Uani 1 1 d . . . C1 C 0.4612(4) -0.4606(4) -0.2317(3) 0.0378(13) Uani 1 1 d . . . C10 C 0.2243(3) -0.4819(4) -0.3013(3) 0.0318(12) Uani 1 1 d . . . C11 C 0.0846(4) -0.5234(4) -0.3498(3) 0.0369(13) Uani 1 1 d . . . C12 C -0.0045(4) -0.5388(5) -0.3676(4) 0.0510(16) Uani 1 1 d . . . H12A H -0.0323 -0.5135 -0.3378 0.061 Uiso 1 1 calc R . . C13 C -0.0499(4) -0.5933(5) -0.4313(4) 0.0526(16) Uani 1 1 d . . . H13A H -0.1097 -0.6065 -0.4441 0.063 Uiso 1 1 calc R . . C14 C -0.0094(4) -0.6301(5) -0.4780(3) 0.0482(15) Uani 1 1 d . . . H14A H -0.0426 -0.6658 -0.5212 0.058 Uiso 1 1 calc R . . C15 C 0.0792(4) -0.6132(4) -0.4599(3) 0.0378(13) Uani 1 1 d . . . H15A H 0.1063 -0.6373 -0.4904 0.045 Uiso 1 1 calc R . . C16 C 0.1274(3) -0.5598(4) -0.3952(3) 0.0324(12) Uani 1 1 d . . . C23A C 0.3159(4) -0.6923(4) -0.2150(3) 0.0410(14) Uani 1 1 d . . . H23B H 0.2577 -0.6969 -0.2496 0.049 Uiso 1 1 calc R . . C22A C 0.3336(4) -0.6535(5) -0.1444(3) 0.0509(16) Uani 1 1 d . . . H22B H 0.2873 -0.6346 -0.1312 0.061 Uiso 1 1 calc R . . C21A C 0.4198(5) -0.6430(5) -0.0937(4) 0.062(2) Uani 1 1 d . . . H21B H 0.4320 -0.6141 -0.0470 0.074 Uiso 1 1 calc R . . C20A C 0.4878(5) -0.6757(6) -0.1127(3) 0.0609(19) Uani 1 1 d . . . H20B H 0.5461 -0.6702 -0.0784 0.073 Uiso 1 1 calc R . . C19A C 0.4691(4) -0.7164(5) -0.1826(3) 0.0529(16) Uani 1 1 d . . . H19B H 0.5152 -0.7391 -0.1948 0.063 Uiso 1 1 calc R . . C18A C 0.3837(4) -0.7241(4) -0.2345(3) 0.0361(13) Uani 1 1 d . . . C17A C 0.3628(3) -0.7711(4) -0.3105(3) 0.0331(12) Uani 1 1 d . . . C2A C 0.2901(3) -0.7534(4) -0.4421(3) 0.0324(12) Uani 1 1 d . . . C3A C 0.2651(4) -0.8511(5) -0.4630(3) 0.0450(15) Uani 1 1 d . . . H3AA H 0.2734 -0.8997 -0.4263 0.054 Uiso 1 1 calc R . . C4A C 0.2274(4) -0.8798(5) -0.5386(4) 0.0521(16) Uani 1 1 d . . . H4AB H 0.2124 -0.9472 -0.5506 0.062 Uiso 1 1 calc R . . C5A C 0.2121(4) -0.8118(5) -0.5951(3) 0.0567(18) Uani 1 1 d . . . H5AA H 0.1869 -0.8331 -0.6447 0.068 Uiso 1 1 calc R . . C6A C 0.2345(4) -0.7095(5) -0.5782(3) 0.0418(14) Uani 1 1 d . . . C7A C 0.2207(4) -0.6317(5) -0.6293(3) 0.0518(17) Uani 1 1 d . . . H7AA H 0.1955 -0.6466 -0.6801 0.062 Uiso 1 1 calc R . . C8A C 0.2429(4) -0.5335(5) -0.6076(3) 0.0476(16) Uani 1 1 d . . . H8AA H 0.2341 -0.4824 -0.6426 0.057 Uiso 1 1 calc R . . C9A C 0.2797(3) -0.5130(4) -0.5303(3) 0.0331(12) Uani 1 1 d . . . C1A C 0.2728(3) -0.6814(4) -0.5001(3) 0.0325(12) Uani 1 1 d . . . C10A C 0.3047(3) -0.4135(4) -0.4970(3) 0.0321(12) Uani 1 1 d . . . C11A C 0.3294(4) -0.2505(4) -0.4774(3) 0.0385(13) Uani 1 1 d . . . C12A C 0.3397(4) -0.1470(5) -0.4806(4) 0.0497(16) Uani 1 1 d . . . H12B H 0.3236 -0.1137 -0.5262 0.060 Uiso 1 1 calc R . . C13A C 0.3743(4) -0.0957(5) -0.4147(4) 0.0570(18) Uani 1 1 d . . . H13B H 0.3817 -0.0261 -0.4153 0.068 Uiso 1 1 calc R . . C14A C 0.3987(4) -0.1453(5) -0.3465(4) 0.0542(17) Uani 1 1 d . . . H14B H 0.4229 -0.1079 -0.3025 0.065 Uiso 1 1 calc R . . C15A C 0.3883(4) -0.2472(5) -0.3420(3) 0.0479(16) Uani 1 1 d . . . H15B H 0.4045 -0.2793 -0.2960 0.057 Uiso 1 1 calc R . . C16A C 0.3525(4) -0.3015(4) -0.4086(3) 0.0381(13) Uani 1 1 d . . . C47 C 0.6839(7) -0.1916(9) -0.2457(5) 0.124(4) Uani 1 1 d . . . H47A H 0.6346 -0.1827 -0.2317 0.149 Uiso 1 1 calc R . . H47B H 0.6732 -0.2488 -0.2785 0.149 Uiso 1 1 calc R . . H47C H 0.6909 -0.1321 -0.2711 0.149 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 0.0320(4) 0.0275(4) 0.0258(3) -0.0005(3) 0.0106(3) 0.0005(3) O1 0.057(3) 0.087(4) 0.042(2) 0.009(2) 0.015(2) 0.034(3) O1A 0.071(3) 0.036(2) 0.043(2) 0.0056(19) 0.032(2) 0.002(2) O3 0.054(3) 0.127(5) 0.039(2) -0.014(3) 0.015(2) -0.026(3) N2 0.036(3) 0.044(3) 0.041(3) 0.004(2) 0.014(2) 0.000(2) N1 0.041(3) 0.023(2) 0.026(2) -0.0003(18) 0.0094(19) -0.003(2) N3 0.040(3) 0.026(2) 0.030(2) -0.0014(18) 0.0135(19) 0.0003(19) N4 0.047(3) 0.034(3) 0.034(2) -0.007(2) 0.021(2) 0.002(2) N2A 0.035(3) 0.032(2) 0.034(2) 0.003(2) 0.018(2) 0.003(2) N1A 0.029(2) 0.035(3) 0.022(2) 0.0008(18) 0.0072(17) 0.0035(19) N3A 0.036(3) 0.035(3) 0.040(3) 0.005(2) 0.014(2) 0.004(2) N4A 0.037(3) 0.040(3) 0.033(2) 0.012(2) 0.011(2) 0.007(2) C23 0.046(4) 0.086(5) 0.043(4) 0.002(3) 0.024(3) 0.008(4) C22 0.051(5) 0.141(9) 0.045(4) 0.007(5) 0.020(3) 0.030(5) C21 0.047(5) 0.160(11) 0.073(6) -0.045(7) 0.030(4) 0.009(6) C20 0.078(6) 0.083(6) 0.111(7) -0.039(6) 0.058(5) -0.011(5) C19 0.059(5) 0.069(5) 0.077(5) -0.006(4) 0.042(4) 0.006(4) C18 0.042(4) 0.050(4) 0.052(4) 0.004(3) 0.029(3) 0.004(3) C17 0.042(4) 0.065(4) 0.030(3) 0.012(3) 0.019(3) 0.007(3) C2 0.034(3) 0.035(3) 0.036(3) 0.007(3) 0.006(2) -0.002(3) C3 0.040(4) 0.058(5) 0.065(4) 0.004(3) 0.009(3) -0.006(3) C4 0.045(4) 0.053(4) 0.063(4) 0.000(4) -0.006(3) -0.014(3) C5 0.059(5) 0.050(4) 0.048(4) -0.007(3) 0.000(3) -0.010(4) C6 0.046(4) 0.034(3) 0.035(3) 0.001(3) -0.003(3) -0.003(3) C7 0.076(5) 0.036(3) 0.034(3) -0.007(3) 0.011(3) 0.003(3) C8 0.052(4) 0.037(3) 0.029(3) -0.011(2) 0.009(3) -0.001(3) C9 0.045(3) 0.031(3) 0.031(3) -0.002(2) 0.016(2) 0.002(3) C1 0.039(3) 0.030(3) 0.035(3) 0.001(2) 0.006(2) -0.005(3) C10 0.039(3) 0.030(3) 0.028(3) -0.002(2) 0.014(2) 0.004(2) C11 0.043(3) 0.030(3) 0.038(3) -0.001(2) 0.017(3) 0.001(2) C12 0.045(4) 0.054(4) 0.060(4) 0.002(3) 0.028(3) 0.005(3) C13 0.032(3) 0.051(4) 0.072(4) -0.001(3) 0.017(3) -0.003(3) C14 0.044(4) 0.040(4) 0.047(3) 0.000(3) 0.005(3) 0.002(3) C15 0.043(3) 0.035(3) 0.034(3) -0.005(2) 0.013(3) 0.005(3) C16 0.037(3) 0.027(3) 0.031(3) -0.002(2) 0.011(2) 0.003(2) C23A 0.046(4) 0.038(3) 0.040(3) 0.008(3) 0.018(3) 0.006(3) C22A 0.061(4) 0.057(4) 0.044(3) 0.006(3) 0.031(3) 0.001(3) C21A 0.092(6) 0.056(4) 0.038(3) 0.000(3) 0.027(4) -0.007(4) C20A 0.058(5) 0.072(5) 0.042(4) 0.002(3) 0.009(3) -0.004(4) C19A 0.050(4) 0.059(4) 0.052(4) 0.008(3) 0.023(3) -0.001(3) C18A 0.040(3) 0.030(3) 0.042(3) 0.008(2) 0.019(3) 0.001(3) C17A 0.035(3) 0.032(3) 0.041(3) 0.000(2) 0.024(2) -0.007(2) C2A 0.027(3) 0.034(3) 0.035(3) -0.010(2) 0.012(2) 0.000(2) C3A 0.047(4) 0.040(4) 0.046(3) -0.002(3) 0.016(3) 0.003(3) C4A 0.054(4) 0.039(4) 0.060(4) -0.016(3) 0.019(3) -0.006(3) C5A 0.051(4) 0.063(5) 0.045(4) -0.027(3) 0.006(3) 0.001(3) C6A 0.038(3) 0.047(4) 0.039(3) -0.010(3) 0.014(3) 0.006(3) C7A 0.055(4) 0.066(5) 0.027(3) -0.006(3) 0.007(3) 0.008(3) C8A 0.055(4) 0.051(4) 0.032(3) 0.008(3) 0.013(3) 0.010(3) C9A 0.035(3) 0.039(3) 0.025(3) 0.001(2) 0.012(2) 0.005(2) C1A 0.025(3) 0.039(3) 0.033(3) -0.011(2) 0.010(2) 0.002(2) C10A 0.032(3) 0.039(3) 0.024(3) 0.008(2) 0.009(2) 0.004(2) C11A 0.033(3) 0.038(3) 0.043(3) 0.008(3) 0.013(2) 0.005(3) C12A 0.045(4) 0.036(4) 0.061(4) 0.020(3) 0.015(3) 0.009(3) C13A 0.054(4) 0.031(3) 0.087(5) 0.014(4) 0.028(4) 0.006(3) C14A 0.057(4) 0.034(4) 0.070(4) -0.007(3) 0.024(3) 0.004(3) C15A 0.065(4) 0.047(4) 0.032(3) -0.003(3) 0.020(3) 0.001(3) C16A 0.041(3) 0.032(3) 0.046(3) 0.007(3) 0.022(3) 0.005(3) C47 0.125(9) 0.158(11) 0.087(7) -0.026(7) 0.041(7) -0.031(8) _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 N1A 1.999(2) . ? Ni1 N1 2.014(4) . ? Ni1 N2A 2.137(2) . ? Ni1 N3 2.139(4) . ? Ni1 N2 2.185(5) . ? Ni1 N3A 2.189(2) . ? O1 C17 1.257(7) . ? O1A C17A 1.257(6) . ? O3 C47 1.398(10) . ? O3 H47 0.9317 . ? N2 C17 1.332(7) . ? N2 C2 1.407(7) . ? N1 C9 1.323(7) . ? N1 C1 1.351(7) . ? N3 C10 1.323(6) . ? N3 C16 1.393(7) . ? N4 C10 1.343(6) . ? N4 C11 1.375(6) . ? N4 H100 0.8892 . ? N2A C17A 1.321(6) . ? N2A C2A 1.414(5) . ? N1A C9A 1.315(5) . ? N1A C1A 1.347(6) . ? N3A C10A 1.326(5) . ? N3A C16A 1.392(6) . ? N4A C10A 1.360(5) . ? N4A C11A 1.367(6) . ? N4A H200 0.8937 . ? C23 C22 1.380(10) . ? C23 C18 1.393(8) . ? C23 H23A 0.9300 . ? C22 C21 1.364(13) . ? C22 H22A 0.9300 . ? C21 C20 1.391(13) . ? C21 H21A 0.9300 . ? C20 C19 1.372(10) . ? C20 H20A 0.9300 . ? C19 C18 1.372(9) . ? C19 H19A 0.9300 . ? C18 C17 1.492(8) . ? C2 C3 1.381(8) . ? C2 C1 1.419(8) . ? C3 C4 1.407(9) . ? C3 H3A 0.9300 . ? C4 C5 1.360(10) . ? C4 H4B 0.9300 . ? C5 C6 1.398(9) . ? C5 H5A 0.9300 . ? C6 C7 1.421(9) . ? C6 C1 1.424(8) . ? C7 C8 1.364(8) . ? C7 H7A 0.9300 . ? C8 C9 1.403(7) . ? C8 H8A 0.9300 . ? C9 C10 1.466(7) . ? C11 C12 1.382(8) . ? C11 C16 1.415(7) . ? C12 C13 1.372(9) . ? C12 H12A 0.9300 . ? C13 C14 1.411(9) . ? C13 H13A 0.9300 . ? C14 C15 1.375(8) . ? C14 H14A 0.9300 . ? C15 C16 1.387(7) . ? C15 H15A 0.9300 . ? C23A C18A 1.379(8) . ? C23A C22A 1.386(8) . ? C23A H23B 0.9300 . ? C22A C21A 1.377(9) . ? C22A H22B 0.9300 . ? C21A C20A 1.380(10) . ? C21A H21B 0.9300 . ? C20A C19A 1.381(9) . ? C20A H20B 0.9300 . ? C19A C18A 1.371(8) . ? C19A H19B 0.9300 . ? C18A C17A 1.513(7) . ? C2A C3A 1.369(8) . ? C2A C1A 1.418(7) . ? C3A C4A 1.404(8) . ? C3A H3AA 0.9300 . ? C4A C5A 1.364(9) . ? C4A H4AB 0.9300 . ? C5A C6A 1.407(9) . ? C5A H5AA 0.9300 . ? C6A C7A 1.386(8) . ? C6A C1A 1.445(7) . ? C7A C8A 1.370(9) . ? C7A H7AA 0.9300 . ? C8A C9A 1.408(7) . ? C8A H8AA 0.9300 . ? C9A C10A 1.453(7) . ? C11A C12A 1.384(8) . ? C11A C16A 1.411(7) . ? C12A C13A 1.361(9) . ? C12A H12B 0.9300 . ? C13A C14A 1.389(9) . ? C13A H13B 0.9300 . ? C14A C15A 1.367(8) . ? C14A H14B 0.9300 . ? C15A C16A 1.392(8) . ? C15A H15B 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? 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 N1A Ni1 N1 165.85(13) . . ? N1A Ni1 N2A 78.51(7) . . ? N1 Ni1 N2A 114.30(13) . . ? N1A Ni1 N3 97.36(12) . . ? N1 Ni1 N3 77.40(17) . . ? N2A Ni1 N3 90.00(12) . . ? N1A Ni1 N2 108.46(14) . . ? N1 Ni1 N2 77.68(18) . . ? N2A Ni1 N2 94.03(14) . . ? N3 Ni1 N2 154.16(16) . . ? N1A Ni1 N3A 76.79(7) . . ? N1 Ni1 N3A 90.30(13) . . ? N2A Ni1 N3A 155.30(10) . . ? N3 Ni1 N3A 93.42(12) . . ? N2 Ni1 N3A 93.46(14) . . ? C47 O3 H47 120.2 . . ? C17 N2 C2 117.3(5) . . ? C17 N2 Ni1 127.0(4) . . ? C2 N2 Ni1 110.2(4) . . ? C9 N1 C1 121.2(5) . . ? C9 N1 Ni1 119.6(3) . . ? C1 N1 Ni1 118.1(4) . . ? C10 N3 C16 104.9(4) . . ? C10 N3 Ni1 111.7(3) . . ? C16 N3 Ni1 142.9(3) . . ? C10 N4 C11 106.8(3) . . ? C10 N4 H100 122.1 . . ? C11 N4 H100 130.3 . . ? C17A N2A C2A 120.1(4) . . ? C17A N2A Ni1 125.7(3) . . ? C2A N2A Ni1 112.1(2) . . ? C9A N1A C1A 121.1(3) . . ? C9A N1A Ni1 121.0(3) . . ? C1A N1A Ni1 117.7(2) . . ? C10A N3A C16A 105.9(3) . . ? C10A N3A Ni1 110.4(3) . . ? C16A N3A Ni1 143.8(3) . . ? C10A N4A C11A 107.6(3) . . ? C10A N4A H200 122.6 . . ? C11A N4A H200 129.7 . . ? C22 C23 C18 120.2(8) . . ? C22 C23 H23A 119.9 . . ? C18 C23 H23A 119.9 . . ? C21 C22 C23 119.8(8) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C21 C20 120.3(8) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C19 C20 C21 119.8(9) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C18 C19 C20 120.4(8) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C18 C23 119.4(6) . . ? C19 C18 C17 120.6(6) . . ? C23 C18 C17 119.8(6) . . ? O1 C17 N2 126.3(5) . . ? O1 C17 C18 117.2(6) . . ? N2 C17 C18 116.6(5) . . ? C3 C2 N2 127.6(6) . . ? C3 C2 C1 116.0(6) . . ? N2 C2 C1 116.2(5) . . ? C2 C3 C4 120.9(7) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 123.3(6) . . ? C5 C4 H4B 118.4 . . ? C3 C4 H4B 118.4 . . ? C4 C5 C6 118.3(6) . . ? C4 C5 H5A 120.9 . . ? C6 C5 H5A 120.9 . . ? C5 C6 C7 124.7(6) . . ? C5 C6 C1 118.8(6) . . ? C7 C6 C1 116.5(5) . . ? C8 C7 C6 120.5(5) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 119.4(6) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? N1 C9 C8 121.2(5) . . ? N1 C9 C10 111.9(4) . . ? C8 C9 C10 126.9(5) . . ? N1 C1 C2 116.2(5) . . ? N1 C1 C6 121.1(5) . . ? C2 C1 C6 122.6(5) . . ? N3 C10 N4 113.9(4) . . ? N3 C10 C9 118.7(5) . . ? N4 C10 C9 127.2(4) . . ? N4 C11 C12 131.7(5) . . ? N4 C11 C16 106.0(4) . . ? C12 C11 C16 122.3(5) . . ? C13 C12 C11 116.6(6) . . ? C13 C12 H12A 121.7 . . ? C11 C12 H12A 121.7 . . ? C12 C13 C14 122.5(6) . . ? C12 C13 H13A 118.8 . . ? C14 C13 H13A 118.8 . . ? C15 C14 C13 120.1(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 118.9(5) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C15 C16 N3 132.0(5) . . ? C15 C16 C11 119.5(5) . . ? N3 C16 C11 108.5(4) . . ? C18A C23A C22A 120.7(5) . . ? C18A C23A H23B 119.6 . . ? C22A C23A H23B 119.6 . . ? C21A C22A C23A 120.0(6) . . ? C21A C22A H22B 120.0 . . ? C23A C22A H22B 120.0 . . ? C22A C21A C20A 119.4(6) . . ? C22A C21A H21B 120.3 . . ? C20A C21A H21B 120.3 . . ? C21A C20A C19A 119.9(6) . . ? C21A C20A H20B 120.1 . . ? C19A C20A H20B 120.1 . . ? C18A C19A C20A 121.2(6) . . ? C18A C19A H19B 119.4 . . ? C20A C19A H19B 119.4 . . ? C19A C18A C23A 118.6(5) . . ? C19A C18A C17A 121.4(5) . . ? C23A C18A C17A 119.9(5) . . ? O1A C17A N2A 126.3(5) . . ? O1A C17A C18A 117.0(5) . . ? N2A C17A C18A 116.7(4) . . ? C3A C2A N2A 128.5(5) . . ? C3A C2A C1A 117.1(5) . . ? N2A C2A C1A 114.2(4) . . ? C2A C3A C4A 121.5(6) . . ? C2A C3A H3AA 119.2 . . ? C4A C3A H3AA 119.2 . . ? C5A C4A C3A 122.0(6) . . ? C5A C4A H4AB 119.0 . . ? C3A C4A H4AB 119.0 . . ? C4A C5A C6A 119.9(6) . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C7A C6A C5A 126.5(6) . . ? C7A C6A C1A 116.2(5) . . ? C5A C6A C1A 117.3(6) . . ? C8A C7A C6A 122.4(5) . . ? C8A C7A H7AA 118.8 . . ? C6A C7A H7AA 118.8 . . ? C7A C8A C9A 117.5(5) . . ? C7A C8A H8AA 121.3 . . ? C9A C8A H8AA 121.3 . . ? N1A C9A C8A 122.2(5) . . ? N1A C9A C10A 112.6(4) . . ? C8A C9A C10A 125.2(5) . . ? N1A C1A C2A 117.4(4) . . ? N1A C1A C6A 120.5(5) . . ? C2A C1A C6A 122.1(5) . . ? N3A C10A N4A 112.1(4) . . ? N3A C10A C9A 119.2(4) . . ? N4A C10A C9A 128.7(4) . . ? N4A C11A C12A 132.3(5) . . ? N4A C11A C16A 106.1(5) . . ? C12A C11A C16A 121.6(6) . . ? C13A C12A C11A 117.7(6) . . ? C13A C12A H12B 121.2 . . ? C11A C12A H12B 121.2 . . ? C12A C13A C14A 121.3(6) . . ? C12A C13A H13B 119.3 . . ? C14A C13A H13B 119.3 . . ? C15A C14A C13A 122.1(6) . . ? C15A C14A H14B 119.0 . . ? C13A C14A H14B 119.0 . . ? C14A C15A C16A 117.8(6) . . ? C14A C15A H15B 121.1 . . ? C16A C15A H15B 121.1 . . ? C15A C16A N3A 132.0(5) . . ? C15A C16A C11A 119.5(5) . . ? N3A C16A C11A 108.4(5) . . ? O3 C47 H47A 109.5 . . ? O3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? O3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Ni1 N2 C17 -51.0(5) . . . . ? N1 Ni1 N2 C17 142.2(5) . . . . ? N2A Ni1 N2 C17 28.2(4) . . . . ? N3 Ni1 N2 C17 126.5(5) . . . . ? N3A Ni1 N2 C17 -128.3(4) . . . . ? N1A Ni1 N2 C2 156.1(3) . . . . ? N1 Ni1 N2 C2 -10.6(3) . . . . ? N2A Ni1 N2 C2 -124.6(3) . . . . ? N3 Ni1 N2 C2 -26.3(6) . . . . ? N3A Ni1 N2 C2 78.9(3) . . . . ? N1A Ni1 N1 C9 61.9(8) . . . . ? N2A Ni1 N1 C9 -91.8(4) . . . . ? N3 Ni1 N1 C9 -7.6(4) . . . . ? N2 Ni1 N1 C9 179.3(4) . . . . ? N3A Ni1 N1 C9 85.8(4) . . . . ? N1A Ni1 N1 C1 -106.4(6) . . . . ? N2A Ni1 N1 C1 99.9(4) . . . . ? N3 Ni1 N1 C1 -175.9(4) . . . . ? N2 Ni1 N1 C1 11.0(4) . . . . ? N3A Ni1 N1 C1 -82.5(4) . . . . ? N1A Ni1 N3 C10 -163.0(3) . . . . ? N1 Ni1 N3 C10 3.6(3) . . . . ? N2A Ni1 N3 C10 118.5(3) . . . . ? N2 Ni1 N3 C10 19.3(6) . . . . ? N3A Ni1 N3 C10 -85.9(3) . . . . ? N1A Ni1 N3 C16 27.0(6) . . . . ? N1 Ni1 N3 C16 -166.3(6) . . . . ? N2A Ni1 N3 C16 -51.4(5) . . . . ? N2 Ni1 N3 C16 -150.7(5) . . . . ? N3A Ni1 N3 C16 104.1(5) . . . . ? N1A Ni1 N2A C17A 161.9(3) . . . . ? N1 Ni1 N2A C17A -24.4(3) . . . . ? N3 Ni1 N2A C17A -100.6(3) . . . . ? N2 Ni1 N2A C17A 53.9(3) . . . . ? N3A Ni1 N2A C17A 161.2(3) . . . . ? N1A Ni1 N2A C2A -1.4(3) . . . . ? N1 Ni1 N2A C2A 172.2(3) . . . . ? N3 Ni1 N2A C2A 96.1(3) . . . . ? N2 Ni1 N2A C2A -109.5(3) . . . . ? N3A Ni1 N2A C2A -2.1(4) . . . . ? N1 Ni1 N1A C9A 22.6(7) . . . . ? N2A Ni1 N1A C9A 178.3(3) . . . . ? N3 Ni1 N1A C9A 89.8(3) . . . . ? N2 Ni1 N1A C9A -91.3(3) . . . . ? N3A Ni1 N1A C9A -2.0(3) . . . . ? N1 Ni1 N1A C1A -152.8(6) . . . . ? N2A Ni1 N1A C1A 2.9(3) . . . . ? N3 Ni1 N1A C1A -85.6(3) . . . . ? N2 Ni1 N1A C1A 93.3(3) . . . . ? N3A Ni1 N1A C1A -177.4(3) . . . . ? N1A Ni1 N3A C10A 0.8(3) . . . . ? N1 Ni1 N3A C10A -173.3(3) . . . . ? N2A Ni1 N3A C10A 1.5(4) . . . . ? N3 Ni1 N3A C10A -95.9(3) . . . . ? N2 Ni1 N3A C10A 109.0(3) . . . . ? N1A Ni1 N3A C16A 179.9(4) . . . . ? N1 Ni1 N3A C16A 5.7(5) . . . . ? N2A Ni1 N3A C16A -179.5(4) . . . . ? N3 Ni1 N3A C16A 83.1(4) . . . . ? N2 Ni1 N3A C16A -72.0(4) . . . . ? C18 C23 C22 C21 0.9(11) . . . . ? C23 C22 C21 C20 0.4(12) . . . . ? C22 C21 C20 C19 -2.8(12) . . . . ? C21 C20 C19 C18 3.9(11) . . . . ? C20 C19 C18 C23 -2.5(10) . . . . ? C20 C19 C18 C17 -177.4(6) . . . . ? C22 C23 C18 C19 0.1(9) . . . . ? C22 C23 C18 C17 175.0(6) . . . . ? C2 N2 C17 O1 11.0(9) . . . . ? Ni1 N2 C17 O1 -140.1(5) . . . . ? C2 N2 C17 C18 -168.9(5) . . . . ? Ni1 N2 C17 C18 40.0(7) . . . . ? C19 C18 C17 O1 45.6(8) . . . . ? C23 C18 C17 O1 -129.2(6) . . . . ? C19 C18 C17 N2 -134.4(6) . . . . ? C23 C18 C17 N2 50.7(8) . . . . ? C17 N2 C2 C3 38.6(8) . . . . ? Ni1 N2 C2 C3 -165.7(5) . . . . ? C17 N2 C2 C1 -146.3(5) . . . . ? Ni1 N2 C2 C1 9.4(6) . . . . ? N2 C2 C3 C4 177.2(6) . . . . ? C1 C2 C3 C4 2.1(9) . . . . ? C2 C3 C4 C5 -0.5(11) . . . . ? C3 C4 C5 C6 -1.5(10) . . . . ? C4 C5 C6 C7 -177.0(6) . . . . ? C4 C5 C6 C1 1.7(9) . . . . ? C5 C6 C7 C8 177.5(6) . . . . ? C1 C6 C7 C8 -1.2(8) . . . . ? C6 C7 C8 C9 -1.4(9) . . . . ? C1 N1 C9 C8 -2.0(8) . . . . ? Ni1 N1 C9 C8 -169.9(4) . . . . ? C1 N1 C9 C10 177.6(4) . . . . ? Ni1 N1 C9 C10 9.6(6) . . . . ? C7 C8 C9 N1 3.1(8) . . . . ? C7 C8 C9 C10 -176.4(5) . . . . ? C9 N1 C1 C2 -177.4(5) . . . . ? Ni1 N1 C1 C2 -9.3(6) . . . . ? C9 N1 C1 C6 -0.7(8) . . . . ? Ni1 N1 C1 C6 167.4(4) . . . . ? C3 C2 C1 N1 174.7(5) . . . . ? N2 C2 C1 N1 -0.9(7) . . . . ? C3 C2 C1 C6 -1.9(8) . . . . ? N2 C2 C1 C6 -177.6(5) . . . . ? C5 C6 C1 N1 -176.4(5) . . . . ? C7 C6 C1 N1 2.3(8) . . . . ? C5 C6 C1 C2 0.0(8) . . . . ? C7 C6 C1 C2 178.8(5) . . . . ? C16 N3 C10 N4 -1.0(5) . . . . ? Ni1 N3 C10 N4 -174.7(3) . . . . ? C16 N3 C10 C9 173.9(5) . . . . ? Ni1 N3 C10 C9 0.2(6) . . . . ? C11 N4 C10 N3 0.6(5) . . . . ? C11 N4 C10 C9 -173.8(5) . . . . ? N1 C9 C10 N3 -6.1(7) . . . . ? C8 C9 C10 N3 173.4(5) . . . . ? N1 C9 C10 N4 168.0(4) . . . . ? C8 C9 C10 N4 -12.5(9) . . . . ? C10 N4 C11 C12 -179.7(6) . . . . ? C10 N4 C11 C16 0.1(5) . . . . ? N4 C11 C12 C13 -179.0(5) . . . . ? C16 C11 C12 C13 1.3(9) . . . . ? C11 C12 C13 C14 -1.7(9) . . . . ? C12 C13 C14 C15 1.1(10) . . . . ? C13 C14 C15 C16 -0.1(8) . . . . ? C14 C15 C16 N3 -179.6(5) . . . . ? C14 C15 C16 C11 -0.3(8) . . . . ? C10 N3 C16 C15 -179.7(6) . . . . ? Ni1 N3 C16 C15 -9.3(10) . . . . ? C10 N3 C16 C11 1.0(6) . . . . ? Ni1 N3 C16 C11 171.3(4) . . . . ? N4 C11 C16 C15 179.9(4) . . . . ? C12 C11 C16 C15 -0.3(8) . . . . ? N4 C11 C16 N3 -0.6(5) . . . . ? C12 C11 C16 N3 179.2(5) . . . . ? C18A C23A C22A C21A 2.4(9) . . . . ? C23A C22A C21A C20A -3.0(10) . . . . ? C22A C21A C20A C19A 1.4(10) . . . . ? C21A C20A C19A C18A 0.9(10) . . . . ? C20A C19A C18A C23A -1.5(9) . . . . ? C20A C19A C18A C17A -178.5(6) . . . . ? C22A C23A C18A C19A -0.1(8) . . . . ? C22A C23A C18A C17A 176.9(5) . . . . ? C2A N2A C17A O1A 7.9(7) . . . . ? Ni1 N2A C17A O1A -154.2(4) . . . . ? C2A N2A C17A C18A -169.3(4) . . . . ? Ni1 N2A C17A C18A 28.5(5) . . . . ? C19A C18A C17A O1A 65.0(7) . . . . ? C23A C18A C17A O1A -111.9(6) . . . . ? C19A C18A C17A N2A -117.5(6) . . . . ? C23A C18A C17A N2A 65.6(6) . . . . ? C17A N2A C2A C3A 20.9(7) . . . . ? Ni1 N2A C2A C3A -174.7(5) . . . . ? C17A N2A C2A C1A -164.5(4) . . . . ? Ni1 N2A C2A C1A -0.1(5) . . . . ? N2A C2A C3A C4A 177.1(5) . . . . ? C1A C2A C3A C4A 2.6(8) . . . . ? C2A C3A C4A C5A -1.2(10) . . . . ? C3A C4A C5A C6A 0.1(10) . . . . ? C4A C5A C6A C7A -178.1(6) . . . . ? C4A C5A C6A C1A -0.5(9) . . . . ? C5A C6A C7A C8A 178.5(6) . . . . ? C1A C6A C7A C8A 0.8(9) . . . . ? C6A C7A C8A C9A -1.0(9) . . . . ? C1A N1A C9A C8A -1.6(7) . . . . ? Ni1 N1A C9A C8A -176.9(4) . . . . ? C1A N1A C9A C10A 177.9(4) . . . . ? Ni1 N1A C9A C10A 2.7(5) . . . . ? C7A C8A C9A N1A 1.4(9) . . . . ? C7A C8A C9A C10A -178.1(5) . . . . ? C9A N1A C1A C2A -179.3(4) . . . . ? Ni1 N1A C1A C2A -3.9(5) . . . . ? C9A N1A C1A C6A 1.4(6) . . . . ? Ni1 N1A C1A C6A 176.8(4) . . . . ? C3A C2A C1A N1A 177.8(4) . . . . ? N2A C2A C1A N1A 2.5(6) . . . . ? C3A C2A C1A C6A -3.0(8) . . . . ? N2A C2A C1A C6A -178.2(4) . . . . ? C7A C6A C1A N1A -1.0(7) . . . . ? C5A C6A C1A N1A -178.9(5) . . . . ? C7A C6A C1A C2A 179.8(5) . . . . ? C5A C6A C1A C2A 1.9(8) . . . . ? C16A N3A C10A N4A -0.4(5) . . . . ? Ni1 N3A C10A N4A 179.0(2) . . . . ? C16A N3A C10A C9A -179.2(4) . . . . ? Ni1 N3A C10A C9A 0.2(5) . . . . ? C11A N4A C10A N3A 0.6(5) . . . . ? C11A N4A C10A C9A 179.2(5) . . . . ? N1A C9A C10A N3A -1.8(6) . . . . ? C8A C9A C10A N3A 177.7(5) . . . . ? N1A C9A C10A N4A 179.7(4) . . . . ? C8A C9A C10A N4A -0.8(9) . . . . ? C10A N4A C11A C12A 178.9(6) . . . . ? C10A N4A C11A C16A -0.5(5) . . . . ? N4A C11A C12A C13A -178.4(5) . . . . ? C16A C11A C12A C13A 0.9(9) . . . . ? C11A C12A C13A C14A 0.2(10) . . . . ? C12A C13A C14A C15A -0.9(10) . . . . ? C13A C14A C15A C16A 0.5(10) . . . . ? C14A C15A C16A N3A 177.9(5) . . . . ? C14A C15A C16A C11A 0.6(9) . . . . ? C10A N3A C16A C15A -177.5(6) . . . . ? Ni1 N3A C16A C15A 3.5(9) . . . . ? C10A N3A C16A C11A 0.1(5) . . . . ? Ni1 N3A C16A C11A -178.9(3) . . . . ? N4A C11A C16A C15A 178.2(5) . . . . ? C12A C11A C16A C15A -1.3(8) . . . . ? N4A C11A C16A N3A 0.2(5) . . . . ? C12A C11A C16A N3A -179.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.426 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.068 #===END data_14a _database_code_depnum_ccdc_archive 'CCDC 713152' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 Cl4 N12 Ni2 O4' _chemical_formula_weight 1128.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.186(7) _cell_length_b 11.301(10) _cell_length_c 13.024(10) _cell_angle_alpha 97.40(8) _cell_angle_beta 101.03(6) _cell_angle_gamma 116.31(4) _cell_volume 1279.7(18) _cell_formula_units_Z 1 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used 3787 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 27.45 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8563 _exptl_absorpt_correction_T_max 0.9360 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 Multi-scan _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8480 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.1596 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4412 _reflns_number_gt 2358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1500P)^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 4412 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1874 _refine_ls_R_factor_gt 0.1167 _refine_ls_wR_factor_ref 0.3251 _refine_ls_wR_factor_gt 0.2696 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Ni1 Ni 0.82794(14) 0.83346(12) 0.44253(11) 0.0363(5) Uani 1 1 d . . . Cl1 Cl 0.9143(3) 1.0543(2) 0.4104(2) 0.0378(7) Uani 1 1 d . . . Cl2 Cl 0.6063(3) 0.7239(2) 0.2924(2) 0.0389(7) Uani 1 1 d . . . N1 N 0.7874(9) 0.6580(8) 0.4862(7) 0.035(2) Uani 1 1 d . . . N2 N 0.9503(9) 0.7658(8) 0.3496(7) 0.038(2) Uani 1 1 d . . . H2 H 1.0513 0.8169 0.3912 0.046 Uiso 1 1 calc R . . N3 N 0.7093(9) 0.8339(8) 0.5582(7) 0.037(2) Uani 1 1 d . . . N4 N 0.6086(10) 0.7347(9) 0.6816(7) 0.043(2) Uani 1 1 d . . . C1 C 0.8311(11) 0.5752(10) 0.4313(10) 0.042(3) Uani 1 1 d . . . C2 C 0.9125(11) 0.6259(11) 0.3571(8) 0.035(2) Uani 1 1 d . . . C3 C 0.9508(12) 0.5440(11) 0.2983(9) 0.043(3) Uani 1 1 d . . . H3 H 1.0057 0.5767 0.2477 0.052 Uiso 1 1 calc R . . C4 C 0.9095(12) 0.4083(11) 0.3115(10) 0.049(3) Uani 1 1 d . . . H4 H 0.9337 0.3509 0.2680 0.059 Uiso 1 1 calc R . . C5 C 0.8349(11) 0.3622(10) 0.3871(9) 0.040(3) Uani 1 1 d . . . H5 H 0.8135 0.2750 0.3988 0.048 Uiso 1 1 calc R . . C6 C 0.7898(12) 0.4431(10) 0.4476(9) 0.041(3) Uani 1 1 d . . . C7 C 0.7122(12) 0.4074(11) 0.5268(9) 0.045(3) Uani 1 1 d . . . H7 H 0.6870 0.3217 0.5431 0.054 Uiso 1 1 calc R . . C8 C 0.6721(12) 0.4922(10) 0.5809(9) 0.039(3) Uani 1 1 d . . . H8 H 0.6160 0.4636 0.6316 0.046 Uiso 1 1 calc R . . C9 C 0.7142(11) 0.6227(10) 0.5612(9) 0.036(2) Uani 1 1 d . . . C10 C 0.6770(10) 0.7300(9) 0.6040(9) 0.034(2) Uani 1 1 d . . . C11 C 0.5886(11) 0.8490(9) 0.6863(8) 0.033(2) Uani 1 1 d . . . C12 C 0.5205(12) 0.9026(11) 0.7493(10) 0.047(3) Uani 1 1 d . . . H12 H 0.4755 0.8595 0.8009 0.056 Uiso 1 1 calc R . . C13 C 0.5226(11) 1.0205(11) 0.7319(9) 0.042(3) Uani 1 1 d . . . H13 H 0.4782 1.0598 0.7733 0.051 Uiso 1 1 calc R . . C14 C 0.5871(12) 1.0853(11) 0.6562(10) 0.047(3) Uani 1 1 d . . . H14 H 0.5843 1.1662 0.6469 0.056 Uiso 1 1 calc R . . C15 C 0.6556(11) 1.0332(10) 0.5939(9) 0.040(3) Uani 1 1 d . . . H15 H 0.6982 1.0769 0.5417 0.047 Uiso 1 1 calc R . . C16 C 0.6599(11) 0.9134(10) 0.6107(9) 0.039(3) Uani 1 1 d . . . C17 C 0.5550(12) 0.6356(10) 0.7502(8) 0.043(3) Uani 1 1 d . . . H17A H 0.5809 0.5631 0.7324 0.064 Uiso 1 1 calc R . . H17B H 0.4443 0.5960 0.7367 0.064 Uiso 1 1 calc R . . H17C H 0.6051 0.6830 0.8265 0.064 Uiso 1 1 calc R . . C18 C 0.9572(13) 0.7926(11) 0.2430(9) 0.049(3) Uani 1 1 d . . . H18A H 1.0175 0.7562 0.2142 0.074 Uiso 1 1 calc R . . H18B H 1.0050 0.8910 0.2494 0.074 Uiso 1 1 calc R . . H18C H 0.8537 0.7486 0.1942 0.074 Uiso 1 1 calc R . . O1 O 0.9278(10) 0.7540(9) 0.8502(8) 0.071(3) Uani 1 1 d . . . O2 O 0.3594(12) 0.7253(14) -0.0828(10) 0.127(5) Uani 1 1 d . . . N5 N 1.1441(11) 0.9545(10) 0.9361(8) 0.053(3) Uani 1 1 d . . . N6 N 0.2623(13) 0.5917(14) 0.0247(9) 0.079(4) Uani 1 1 d . . . C19 C 1.0403(14) 0.8597(12) 0.8495(10) 0.053(3) Uani 1 1 d . . . H19 H 1.0535 0.8743 0.7811 0.063 Uiso 1 1 calc R . . C20 C 1.2742(15) 1.0728(15) 0.9269(13) 0.085(5) Uani 1 1 d . . . H20A H 1.2714 1.0674 0.8507 0.127 Uiso 1 1 calc R . . H20B H 1.3684 1.0761 0.9664 0.127 Uiso 1 1 calc R . . H20C H 1.2712 1.1552 0.9574 0.127 Uiso 1 1 calc R . . C21 C 1.1272(14) 0.9402(13) 1.0413(10) 0.062(4) Uani 1 1 d . . . H21A H 1.0358 0.8546 1.0347 0.092 Uiso 1 1 calc R . . H21B H 1.1174 1.0166 1.0767 0.092 Uiso 1 1 calc R . . H21C H 1.2170 0.9397 1.0843 0.092 Uiso 1 1 calc R . . C22 C 0.2773(18) 0.6994(17) -0.0225(13) 0.081(5) Uani 1 1 d . . . H22 H 0.2263 0.7500 -0.0085 0.097 Uiso 1 1 calc R . . C23 C 0.3564(19) 0.5323(18) 0.0058(13) 0.110(7) Uani 1 1 d . . . H23A H 0.3946 0.5585 -0.0557 0.164 Uiso 1 1 calc R . . H23B H 0.2964 0.4330 -0.0098 0.164 Uiso 1 1 calc R . . H23C H 0.4426 0.5648 0.0701 0.164 Uiso 1 1 calc R . . C24 C 0.1886(17) 0.5738(16) 0.1070(12) 0.088(5) Uani 1 1 d . . . H24A H 0.1294 0.6226 0.1035 0.132 Uiso 1 1 calc R . . H24B H 0.2650 0.6097 0.1773 0.132 Uiso 1 1 calc R . . H24C H 0.1201 0.4767 0.0976 0.132 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 0.0429(9) 0.0207(7) 0.0433(9) 0.0094(6) 0.0144(7) 0.0122(6) Cl1 0.0409(14) 0.0256(13) 0.0458(16) 0.0137(12) 0.0154(13) 0.0123(11) Cl2 0.0403(15) 0.0257(13) 0.0426(16) 0.0086(12) 0.0090(12) 0.0099(11) N1 0.028(4) 0.035(5) 0.047(6) 0.017(4) 0.014(4) 0.017(4) N2 0.027(4) 0.026(5) 0.042(6) 0.000(4) -0.003(4) 0.005(4) N3 0.033(5) 0.027(5) 0.049(6) 0.010(4) 0.014(4) 0.012(4) N4 0.045(5) 0.033(5) 0.047(6) 0.018(4) 0.014(5) 0.014(4) C1 0.035(6) 0.032(6) 0.067(8) 0.013(6) 0.019(6) 0.021(5) C2 0.030(5) 0.039(6) 0.043(6) 0.011(5) 0.009(5) 0.022(5) C3 0.048(7) 0.043(7) 0.051(7) 0.015(6) 0.019(6) 0.029(6) C4 0.052(7) 0.030(6) 0.062(8) 0.003(6) 0.014(6) 0.020(5) C5 0.038(6) 0.024(5) 0.062(8) 0.014(5) 0.020(6) 0.014(5) C6 0.037(6) 0.029(6) 0.051(7) 0.005(5) 0.001(5) 0.017(5) C7 0.048(7) 0.031(6) 0.058(8) 0.014(6) 0.023(6) 0.017(5) C8 0.044(6) 0.030(6) 0.049(7) 0.023(5) 0.017(5) 0.019(5) C9 0.035(6) 0.029(6) 0.043(7) 0.006(5) 0.013(5) 0.014(5) C10 0.028(5) 0.021(5) 0.048(7) 0.002(5) 0.013(5) 0.007(4) C11 0.044(6) 0.023(5) 0.032(6) 0.011(4) 0.020(5) 0.012(5) C12 0.040(6) 0.041(7) 0.052(8) 0.017(6) 0.012(6) 0.013(5) C13 0.033(6) 0.042(7) 0.041(7) 0.001(5) 0.001(5) 0.015(5) C14 0.056(7) 0.029(6) 0.072(8) 0.022(6) 0.026(7) 0.028(5) C15 0.041(6) 0.021(5) 0.047(7) 0.008(5) 0.009(5) 0.008(5) C16 0.030(6) 0.028(6) 0.055(7) 0.009(5) 0.007(5) 0.012(5) C17 0.051(7) 0.030(6) 0.043(7) 0.012(5) 0.019(6) 0.014(5) C18 0.050(7) 0.031(6) 0.051(8) 0.003(5) 0.013(6) 0.009(5) O1 0.058(5) 0.040(5) 0.086(7) 0.001(5) 0.004(5) 0.009(4) O2 0.070(7) 0.140(12) 0.083(9) 0.000(8) 0.017(7) -0.016(7) N5 0.053(6) 0.046(6) 0.059(7) 0.014(5) 0.020(5) 0.019(5) N6 0.059(7) 0.104(11) 0.058(8) 0.032(8) 0.014(6) 0.023(7) C19 0.072(8) 0.036(7) 0.037(7) 0.005(6) 0.005(6) 0.020(7) C20 0.061(9) 0.076(11) 0.104(13) 0.034(10) 0.030(9) 0.016(8) C21 0.052(7) 0.049(8) 0.062(9) 0.009(7) -0.006(7) 0.015(6) C22 0.086(11) 0.083(12) 0.068(11) 0.034(9) 0.016(9) 0.035(9) C23 0.086(12) 0.123(17) 0.097(14) -0.036(12) -0.024(10) 0.067(12) C24 0.071(9) 0.086(12) 0.078(11) 0.020(10) 0.024(9) 0.012(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.019(8) . ? Ni1 N3 2.105(8) . ? Ni1 N2 2.188(9) . ? Ni1 Cl1 2.375(3) . ? Ni1 Cl2 2.379(4) . ? Ni1 Cl1 2.582(4) 2_776 ? Cl1 Ni1 2.582(4) 2_776 ? N1 C9 1.337(12) . ? N1 C1 1.380(12) . ? N2 C18 1.466(13) . ? N2 C2 1.474(12) . ? N2 H2 0.9300 . ? N3 C10 1.326(12) . ? N3 C16 1.379(13) . ? N4 C10 1.341(12) . ? N4 C11 1.389(13) . ? N4 C17 1.502(12) . ? C1 C2 1.406(14) . ? C1 C6 1.418(14) . ? C2 C3 1.359(14) . ? C3 C4 1.444(15) . ? C3 H3 0.9500 . ? C4 C5 1.372(15) . ? C4 H4 0.9500 . ? C5 C6 1.412(14) . ? C5 H5 0.9500 . ? C6 C7 1.410(15) . ? C7 C8 1.365(14) . ? C7 H7 0.9500 . ? C8 C9 1.415(13) . ? C8 H8 0.9500 . ? C9 C10 1.496(13) . ? C11 C12 1.408(14) . ? C11 C16 1.421(14) . ? C12 C13 1.372(15) . ? C12 H12 0.9500 . ? C13 C14 1.395(14) . ? C13 H13 0.9500 . ? C14 C15 1.397(14) . ? C14 H14 0.9500 . ? C15 C16 1.417(13) . ? C15 H15 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1 C19 1.239(14) . ? O2 C22 1.223(17) . ? N5 C19 1.329(14) . ? N5 C21 1.433(15) . ? N5 C20 1.446(15) . ? N6 C22 1.395(18) . ? N6 C24 1.409(16) . ? N6 C23 1.431(18) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N3 77.5(3) . . ? N1 Ni1 N2 79.8(3) . . ? N3 Ni1 N2 156.9(3) . . ? N1 Ni1 Cl1 171.0(2) . . ? N3 Ni1 Cl1 103.6(2) . . ? N2 Ni1 Cl1 98.1(2) . . ? N1 Ni1 Cl2 93.0(3) . . ? N3 Ni1 Cl2 95.1(3) . . ? N2 Ni1 Cl2 90.3(2) . . ? Cl1 Ni1 Cl2 95.79(13) . . ? N1 Ni1 Cl1 86.8(2) . 2_776 ? N3 Ni1 Cl1 91.8(2) . 2_776 ? N2 Ni1 Cl1 82.8(2) . 2_776 ? Cl1 Ni1 Cl1 84.22(12) . 2_776 ? Cl2 Ni1 Cl1 172.94(10) . 2_776 ? Ni1 Cl1 Ni1 95.78(12) . 2_776 ? C9 N1 C1 122.5(9) . . ? C9 N1 Ni1 120.4(7) . . ? C1 N1 Ni1 117.1(7) . . ? C18 N2 C2 115.5(9) . . ? C18 N2 Ni1 120.9(7) . . ? C2 N2 Ni1 108.1(6) . . ? C18 N2 H2 103.3 . . ? C2 N2 H2 103.3 . . ? Ni1 N2 H2 103.2 . . ? C10 N3 C16 105.1(8) . . ? C10 N3 Ni1 113.7(7) . . ? C16 N3 Ni1 140.9(7) . . ? C10 N4 C11 107.4(8) . . ? C10 N4 C17 128.6(9) . . ? C11 N4 C17 124.0(9) . . ? N1 C1 C2 117.2(9) . . ? N1 C1 C6 120.5(10) . . ? C2 C1 C6 122.3(10) . . ? C3 C2 C1 118.5(10) . . ? C3 C2 N2 124.8(9) . . ? C1 C2 N2 116.7(9) . . ? C2 C3 C4 121.0(10) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.8(10) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 126.2(10) . . ? C7 C6 C1 116.1(10) . . ? C5 C6 C1 117.6(10) . . ? C8 C7 C6 122.1(10) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C9 119.9(10) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? N1 C9 C8 118.8(9) . . ? N1 C9 C10 110.6(9) . . ? C8 C9 C10 130.3(9) . . ? N3 C10 N4 113.4(9) . . ? N3 C10 C9 117.6(9) . . ? N4 C10 C9 129.0(9) . . ? N4 C11 C12 132.6(9) . . ? N4 C11 C16 104.4(8) . . ? C12 C11 C16 122.9(9) . . ? C13 C12 C11 116.2(10) . . ? C13 C12 H12 121.9 . . ? C11 C12 H12 121.9 . . ? C12 C13 C14 123.0(11) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C15 121.2(10) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 118.1(10) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? N3 C16 C15 131.6(10) . . ? N3 C16 C11 109.4(9) . . ? C15 C16 C11 118.6(10) . . ? N4 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 N5 C21 119.7(10) . . ? C19 N5 C20 121.5(11) . . ? C21 N5 C20 118.9(11) . . ? C22 N6 C24 117.4(15) . . ? C22 N6 C23 116.3(14) . . ? C24 N6 C23 124.1(14) . . ? O1 C19 N5 125.6(12) . . ? O1 C19 H19 117.2 . . ? N5 C19 H19 117.2 . . ? N5 C20 H20A 109.5 . . ? N5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 H21A 109.5 . . ? N5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C22 N6 116.6(17) . . ? O2 C22 H22 121.7 . . ? N6 C22 H22 121.7 . . ? N6 C23 H23A 109.5 . . ? N6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 Cl1 Ni1 -5.9(16) . . . 2_776 ? N3 Ni1 Cl1 Ni1 90.4(3) . . . 2_776 ? N2 Ni1 Cl1 Ni1 -81.8(2) . . . 2_776 ? Cl2 Ni1 Cl1 Ni1 -172.91(10) . . . 2_776 ? Cl1 Ni1 Cl1 Ni1 0.0 2_776 . . 2_776 ? N3 Ni1 N1 C9 -0.9(8) . . . . ? N2 Ni1 N1 C9 174.9(8) . . . . ? Cl1 Ni1 N1 C9 97.6(16) . . . . ? Cl2 Ni1 N1 C9 -95.4(8) . . . . ? Cl1 Ni1 N1 C9 91.6(8) 2_776 . . . ? N3 Ni1 N1 C1 175.7(8) . . . . ? N2 Ni1 N1 C1 -8.5(7) . . . . ? Cl1 Ni1 N1 C1 -85.8(18) . . . . ? Cl2 Ni1 N1 C1 81.2(7) . . . . ? Cl1 Ni1 N1 C1 -91.7(7) 2_776 . . . ? N1 Ni1 N2 C18 145.8(8) . . . . ? N3 Ni1 N2 C18 156.3(8) . . . . ? Cl1 Ni1 N2 C18 -43.1(7) . . . . ? Cl2 Ni1 N2 C18 52.8(7) . . . . ? Cl1 Ni1 N2 C18 -126.2(7) 2_776 . . . ? N1 Ni1 N2 C2 9.3(6) . . . . ? N3 Ni1 N2 C2 19.9(11) . . . . ? Cl1 Ni1 N2 C2 -179.6(6) . . . . ? Cl2 Ni1 N2 C2 -83.7(6) . . . . ? Cl1 Ni1 N2 C2 97.3(6) 2_776 . . . ? N1 Ni1 N3 C10 3.6(7) . . . . ? N2 Ni1 N3 C10 -7.1(13) . . . . ? Cl1 Ni1 N3 C10 -167.2(7) . . . . ? Cl2 Ni1 N3 C10 95.6(7) . . . . ? Cl1 Ni1 N3 C10 -82.7(7) 2_776 . . . ? N1 Ni1 N3 C16 177.3(12) . . . . ? N2 Ni1 N3 C16 166.7(10) . . . . ? Cl1 Ni1 N3 C16 6.5(12) . . . . ? Cl2 Ni1 N3 C16 -90.7(11) . . . . ? Cl1 Ni1 N3 C16 91.0(11) 2_776 . . . ? C9 N1 C1 C2 -177.7(9) . . . . ? Ni1 N1 C1 C2 5.7(13) . . . . ? C9 N1 C1 C6 4.5(16) . . . . ? Ni1 N1 C1 C6 -172.1(8) . . . . ? N1 C1 C2 C3 -177.0(9) . . . . ? C6 C1 C2 C3 0.8(17) . . . . ? N1 C1 C2 N2 3.2(14) . . . . ? C6 C1 C2 N2 -179.0(9) . . . . ? C18 N2 C2 C3 31.7(14) . . . . ? Ni1 N2 C2 C3 170.8(9) . . . . ? C18 N2 C2 C1 -148.5(10) . . . . ? Ni1 N2 C2 C1 -9.4(11) . . . . ? C1 C2 C3 C4 -0.1(16) . . . . ? N2 C2 C3 C4 179.7(9) . . . . ? C2 C3 C4 C5 -2.3(17) . . . . ? C3 C4 C5 C6 3.9(17) . . . . ? C4 C5 C6 C7 179.6(11) . . . . ? C4 C5 C6 C1 -3.1(16) . . . . ? N1 C1 C6 C7 -4.0(16) . . . . ? C2 C1 C6 C7 178.3(10) . . . . ? N1 C1 C6 C5 178.5(10) . . . . ? C2 C1 C6 C5 0.7(16) . . . . ? C5 C6 C7 C8 -179.5(11) . . . . ? C1 C6 C7 C8 3.2(16) . . . . ? C6 C7 C8 C9 -2.7(17) . . . . ? C1 N1 C9 C8 -3.7(15) . . . . ? Ni1 N1 C9 C8 172.7(7) . . . . ? C1 N1 C9 C10 -178.1(9) . . . . ? Ni1 N1 C9 C10 -1.6(12) . . . . ? C7 C8 C9 N1 2.8(16) . . . . ? C7 C8 C9 C10 175.9(11) . . . . ? C16 N3 C10 N4 0.8(12) . . . . ? Ni1 N3 C10 N4 176.7(7) . . . . ? C16 N3 C10 C9 178.4(9) . . . . ? Ni1 N3 C10 C9 -5.7(12) . . . . ? C11 N4 C10 N3 2.0(12) . . . . ? C17 N4 C10 N3 179.7(9) . . . . ? C11 N4 C10 C9 -175.3(10) . . . . ? C17 N4 C10 C9 2.4(18) . . . . ? N1 C9 C10 N3 4.9(14) . . . . ? C8 C9 C10 N3 -168.6(10) . . . . ? N1 C9 C10 N4 -177.9(10) . . . . ? C8 C9 C10 N4 8.6(19) . . . . ? C10 N4 C11 C12 178.0(11) . . . . ? C17 N4 C11 C12 0.2(19) . . . . ? C10 N4 C11 C16 -3.8(12) . . . . ? C17 N4 C11 C16 178.4(9) . . . . ? N4 C11 C12 C13 179.6(11) . . . . ? C16 C11 C12 C13 1.7(16) . . . . ? C11 C12 C13 C14 0.4(17) . . . . ? C12 C13 C14 C15 -0.8(18) . . . . ? C13 C14 C15 C16 -0.9(16) . . . . ? C10 N3 C16 C15 -176.0(11) . . . . ? Ni1 N3 C16 C15 10(2) . . . . ? C10 N3 C16 C11 -3.2(11) . . . . ? Ni1 N3 C16 C11 -177.3(8) . . . . ? C14 C15 C16 N3 175.1(11) . . . . ? C14 C15 C16 C11 2.8(16) . . . . ? N4 C11 C16 N3 4.4(12) . . . . ? C12 C11 C16 N3 -177.2(10) . . . . ? N4 C11 C16 C15 178.3(9) . . . . ? C12 C11 C16 C15 -3.3(16) . . . . ? C21 N5 C19 O1 -2(2) . . . . ? C20 N5 C19 O1 178.2(13) . . . . ? C24 N6 C22 O2 170.1(13) . . . . ? C23 N6 C22 O2 6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.632 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.197 #===END