Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_1 _database_code_CSD 190498 _journal_coden_Cambridge 186 _journal_volume ? _journal_year ? _journal_page_first ? _publ_contact_author 'Igor O.Fritsky' _publ_contact_author_address ; Prof Jolanta Swiatek-Kozlowska Department of Basic Medical Sciences Wroclaw Medical University Kochanowskiego 14 WROCLAW 51-601 POLAND ; _publ_contact_author_email 'ifritsky@yahoo.com' loop_ _publ_author_name 'J.Swiatek-Kozlowska' 'E.Gumienna-Kontecka' 'A.Dobosz' 'I.A.Golenya' 'I.O.Fritsky' _journal_name_full 'J.Chem.Soc., Dalton Trans.' _publ_section_title ; 2,6-pyridine-dihydroxamic acid a powerful dihydroxamate ligand for Ni2+ and Cu2+ ions ; _publ_contact_author 'Igor O.Fritsky' _publ_contact_author_email 'ifritsky@yahoo.com' _journal_name_full 'J.Chem.Soc., Dalton Trans.' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Di-tetraphenylphosphonium [bis(pyridyl-2,6-dihydroxamate(2-)) nickelate(II)] heptahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H64 N6 Ni O15 P2' _chemical_formula_weight 1253.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 14.200(3) _cell_length_b 14.412(3) _cell_length_c 15.629(3) _cell_angle_alpha 108.05(3) _cell_angle_beta 98.06(3) _cell_angle_gamma 98.03(3) _cell_volume 2953.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'dark-red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.457 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'KUMA CCD area detector diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20399 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 28.38 _reflns_number_total 12968 _reflns_number_gt 10495 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OPTEP,1964' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.0094P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12968 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.002 _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 0.808817(15) 0.485577(16) 0.267121(14) 0.01265(7) Uani 1 1 d . . . P2 P 0.31324(3) 0.68637(3) 0.32652(3) 0.01310(10) Uani 1 1 d . . . P1 P 1.25506(3) 0.02671(3) 0.14307(3) 0.01274(10) Uani 1 1 d . . . O1 O 0.74525(10) 0.29965(10) 0.32800(9) 0.0217(3) Uani 1 1 d . . . H1O1 H 0.6883(16) 0.2518(16) 0.3149(14) 0.026 Uiso 1 1 d . . . O2 O 0.56083(9) 0.27542(9) 0.24515(9) 0.0189(3) Uani 1 1 d . . . O3 O 0.76292(10) 0.70452(9) 0.15509(9) 0.0215(3) Uani 1 1 d . . . O4 O 0.92432(9) 0.66088(10) 0.21961(9) 0.0231(3) Uani 1 1 d . . . H1O4 H 0.9067(16) 0.7097(17) 0.2033(15) 0.028 Uiso 1 1 d . . . O5 O 0.87736(10) 0.31967(10) 0.11001(8) 0.0210(3) Uani 1 1 d . . . H1O5 H 0.9289(16) 0.2992(16) 0.1134(15) 0.025 Uiso 1 1 d . . . O6 O 1.04419(9) 0.34464(10) 0.21445(8) 0.0192(3) Uani 1 1 d . . . O7 O 0.85377(10) 0.71686(9) 0.51826(8) 0.0213(3) Uani 1 1 d . . . O8 O 0.69920(9) 0.63706(10) 0.39245(9) 0.0208(3) Uani 1 1 d . . . H1O8 H 0.7181(16) 0.6832(17) 0.4431(15) 0.025 Uiso 1 1 d . . . O1W O 0.87556(11) 0.88760(12) 0.46918(10) 0.0265(3) Uani 1 1 d . . . H1W1 H 0.9025(18) 0.9272(18) 0.5147(16) 0.032 Uiso 1 1 d . . . H1W2 H 0.8662(17) 0.8335(18) 0.4810(16) 0.032 Uiso 1 1 d . . . O2W O -0.14142(12) 0.16354(12) 0.22537(12) 0.0359(4) Uani 1 1 d . . . H2W1 H -0.1691(19) 0.2112(19) 0.2663(17) 0.043 Uiso 1 1 d . . . H2W2 H -0.085(2) 0.1740(19) 0.2551(18) 0.043 Uiso 1 1 d . . . O3W O 0.05680(11) 0.20564(10) 0.30142(10) 0.0237(3) Uani 1 1 d . . . H3W1 H 0.0856(16) 0.2398(16) 0.3591(16) 0.028 Uiso 1 1 d . . . H3W2 H 0.0596(17) 0.2494(17) 0.2792(16) 0.028 Uiso 1 1 d . . . O4W O 0.61055(11) 0.11474(11) 0.29187(10) 0.0293(3) Uani 1 1 d . . . H4W1 H 0.5856(17) 0.1570(18) 0.2642(16) 0.035 Uiso 1 1 d . . . H4W2 H 0.6443(17) 0.0701(18) 0.2517(16) 0.035 Uiso 1 1 d . . . O5W O 0.83604(10) 0.88963(11) 0.29093(10) 0.0246(3) Uani 1 1 d . . . H5W1 H 0.8405(17) 0.8876(17) 0.3427(17) 0.030 Uiso 1 1 d . . . H5W2 H 0.8173(16) 0.8297(18) 0.2520(16) 0.030 Uiso 1 1 d . . . O6W O 1.02814(11) 1.01418(12) 0.34298(10) 0.0268(3) Uani 1 1 d . . . H6W1 H 0.9778(19) 0.9812(18) 0.3205(16) 0.032 Uiso 1 1 d . . . H6W2 H 1.0279(18) 1.0585(19) 0.3264(16) 0.032 Uiso 1 1 d . . . O7W O 0.72899(11) 0.99524(11) 0.19879(10) 0.0260(3) Uani 1 1 d . . . H7W1 H 0.7613(17) 0.9663(18) 0.2264(16) 0.031 Uiso 1 1 d . . . H7W2 H 0.7779(17) 1.0480(18) 0.2115(15) 0.031 Uiso 1 1 d . . . N1 N 0.71830(11) 0.36612(10) 0.28280(9) 0.0144(3) Uani 1 1 d . . . N2 N 0.67896(10) 0.47962(10) 0.19344(9) 0.0134(3) Uani 1 1 d . . . N3 N 0.83671(10) 0.59400(11) 0.20630(10) 0.0157(3) Uani 1 1 d . . . N4 N 0.89689(11) 0.39348(11) 0.19802(9) 0.0150(3) Uani 1 1 d . . . N5 N 0.93352(10) 0.52288(10) 0.35801(9) 0.0135(3) Uani 1 1 d . . . N6 N 0.78186(11) 0.59332(11) 0.38232(10) 0.0161(3) Uani 1 1 d . . . C54 C 0.12044(14) 0.86675(14) 0.49345(13) 0.0220(4) Uani 1 1 d . . . H54 H 0.0808 0.9023 0.5280 0.026 Uiso 1 1 calc R . . C53 C 0.21581(14) 0.87221(14) 0.53352(13) 0.0211(4) Uani 1 1 d . . . H53 H 0.2397 0.9109 0.5947 0.025 Uiso 1 1 calc R . . C41 C 0.36118(13) 0.52853(14) 0.49920(12) 0.0193(4) Uani 1 1 d . . . H41 H 0.3614 0.5365 0.5606 0.023 Uiso 1 1 calc R . . C55 C 0.08406(14) 0.80906(14) 0.40296(13) 0.0206(4) Uani 1 1 d . . . H55 H 0.0205 0.8069 0.3767 0.025 Uiso 1 1 calc R . . C42 C 0.38092(14) 0.44202(14) 0.44169(13) 0.0217(4) Uani 1 1 d . . . H42 H 0.3940 0.3919 0.4647 0.026 Uiso 1 1 calc R . . C40 C 0.34113(12) 0.60317(13) 0.46541(11) 0.0158(3) Uani 1 1 d . . . H40 H 0.3291 0.6618 0.5043 0.019 Uiso 1 1 calc R . . C52 C 0.27513(13) 0.81973(13) 0.48188(12) 0.0183(4) Uani 1 1 d . . . H52 H 0.3394 0.8244 0.5079 0.022 Uiso 1 1 calc R . . C56 C 0.14186(13) 0.75424(13) 0.35089(12) 0.0178(4) Uani 1 1 d . . . H56 H 0.1168 0.7143 0.2903 0.021 Uiso 1 1 calc R . . C51 C 0.23790(12) 0.75962(12) 0.39035(11) 0.0143(3) Uani 1 1 d . . . C43 C 0.38140(15) 0.42942(14) 0.35000(13) 0.0231(4) Uani 1 1 d . . . H43 H 0.3966 0.3719 0.3122 0.028 Uiso 1 1 calc R . . C39 C 0.33899(12) 0.59042(13) 0.37241(11) 0.0136(3) Uani 1 1 d . . . C44 C 0.35916(14) 0.50296(13) 0.31506(12) 0.0195(4) Uani 1 1 d . . . H44 H 0.3577 0.4939 0.2533 0.023 Uiso 1 1 calc R . . C62 C 0.17387(13) 0.55096(13) 0.18445(12) 0.0186(4) Uani 1 1 d . . . H62 H 0.1529 0.5280 0.2293 0.022 Uiso 1 1 calc R . . C61 C 0.12559(14) 0.50797(14) 0.09327(13) 0.0227(4) Uani 1 1 d . . . H61 H 0.0721 0.4565 0.0773 0.027 Uiso 1 1 calc R . . C57 C 0.25384(13) 0.62857(13) 0.20812(11) 0.0153(3) Uani 1 1 d . . . C45 C 0.42430(12) 0.76523(13) 0.33122(11) 0.0151(3) Uani 1 1 d . . . C46 C 0.42899(14) 0.86712(14) 0.34999(13) 0.0211(4) Uani 1 1 d . . . H46 H 0.3756 0.8950 0.3647 0.025 Uiso 1 1 calc R . . C50 C 0.50461(13) 0.72350(13) 0.30927(12) 0.0178(4) Uani 1 1 d . . . H50 H 0.5022 0.6558 0.2976 0.021 Uiso 1 1 calc R . . C1 C 0.62588(12) 0.34498(12) 0.24430(11) 0.0142(3) Uani 1 1 d . . . C9 C 0.85588(13) 0.64057(13) 0.44993(11) 0.0155(3) Uani 1 1 d . . . C60 C 0.15721(15) 0.54187(15) 0.02636(13) 0.0243(4) Uani 1 1 d . . . H60 H 0.1247 0.5130 -0.0343 0.029 Uiso 1 1 calc R . . C58 C 0.28568(14) 0.66224(14) 0.13997(12) 0.0200(4) Uani 1 1 d . . . H58 H 0.3392 0.7136 0.1552 0.024 Uiso 1 1 calc R . . C47 C 0.51249(14) 0.92651(14) 0.34683(13) 0.0238(4) Uani 1 1 d . . . H47 H 0.5159 0.9945 0.3600 0.029 Uiso 1 1 calc R . . C29 C 1.30469(14) 0.07881(15) 0.41886(12) 0.0223(4) Uani 1 1 d . . . H29 H 1.2773 0.0559 0.4610 0.027 Uiso 1 1 calc R . . C13 C 1.03138(13) 0.62822(13) 0.50052(12) 0.0169(4) Uani 1 1 d . . . H13 H 1.0390 0.6808 0.5551 0.020 Uiso 1 1 calc R . . C4 C 0.50949(13) 0.41829(13) 0.15450(12) 0.0176(4) Uani 1 1 d . . . H4 H 0.4562 0.3721 0.1534 0.021 Uiso 1 1 calc R . . C14 C 0.94419(13) 0.59735(12) 0.43774(11) 0.0147(3) Uani 1 1 d . . . C3 C 0.60212(12) 0.41532(12) 0.19459(11) 0.0133(3) Uani 1 1 d . . . C59 C 0.23658(15) 0.61813(15) 0.04925(13) 0.0251(4) Uani 1 1 d . . . H59 H 0.2574 0.6402 0.0039 0.030 Uiso 1 1 calc R . . C49 C 0.58785(13) 0.78337(14) 0.30495(12) 0.0204(4) Uani 1 1 d . . . H49 H 0.6411 0.7558 0.2894 0.024 Uiso 1 1 calc R . . C30 C 1.38790(14) 0.15155(15) 0.44827(13) 0.0237(4) Uani 1 1 d . . . H30 H 1.4167 0.1766 0.5102 0.028 Uiso 1 1 calc R . . C48 C 0.59146(14) 0.88428(15) 0.32384(13) 0.0236(4) Uani 1 1 d . . . H48 H 0.6475 0.9243 0.3211 0.028 Uiso 1 1 calc R . . C12 C 1.10661(13) 0.57904(13) 0.48012(12) 0.0182(4) Uani 1 1 d . . . H12 H 1.1648 0.5970 0.5222 0.022 Uiso 1 1 calc R . . C28 C 1.26179(13) 0.03980(14) 0.32615(12) 0.0174(4) Uani 1 1 d . . . H28 H 1.2059 -0.0093 0.3059 0.021 Uiso 1 1 calc R . . C18 C 0.95374(15) -0.15784(16) 0.10053(13) 0.0279(5) Uani 1 1 d . . . H18 H 0.8927 -0.1954 0.0942 0.033 Uiso 1 1 calc R . . C17 C 1.03539(15) -0.20039(15) 0.10670(14) 0.0293(5) Uani 1 1 d . . . H17 H 1.0289 -0.2666 0.1034 0.035 Uiso 1 1 calc R . . C5 C 0.49832(13) 0.49194(14) 0.11610(12) 0.0189(4) Uani 1 1 d . . . H5 H 0.4371 0.4945 0.0878 0.023 Uiso 1 1 calc R . . C11 C 1.09546(13) 0.50270(13) 0.39662(12) 0.0172(4) Uani 1 1 d . . . H11 H 1.1460 0.4700 0.3817 0.021 Uiso 1 1 calc R . . C19 C 0.96283(14) -0.06041(16) 0.10369(13) 0.0250(4) Uani 1 1 d . . . H19 H 0.9078 -0.0328 0.0986 0.030 Uiso 1 1 calc R . . C10 C 1.00692(12) 0.47673(13) 0.33639(11) 0.0140(3) Uani 1 1 d . . . C31 C 1.42896(14) 0.18758(14) 0.38662(12) 0.0206(4) Uani 1 1 d . . . H31 H 1.4848 0.2368 0.4073 0.025 Uiso 1 1 calc R . . C16 C 1.12615(14) -0.14420(14) 0.11766(14) 0.0246(4) Uani 1 1 d . . . H16 H 1.1809 -0.1723 0.1223 0.030 Uiso 1 1 calc R . . C6 C 0.57802(13) 0.56176(13) 0.11975(12) 0.0174(4) Uani 1 1 d . . . H6 H 0.5708 0.6127 0.0961 0.021 Uiso 1 1 calc R . . C7 C 0.66865(13) 0.55348(13) 0.15957(11) 0.0146(3) Uani 1 1 d . . . C27 C 1.30391(12) 0.07553(13) 0.26401(11) 0.0139(3) Uani 1 1 d . . . C20 C 1.05350(13) -0.00312(14) 0.11442(12) 0.0194(4) Uani 1 1 d . . . H20 H 1.0595 0.0627 0.1167 0.023 Uiso 1 1 calc R . . C8 C 0.98363(12) 0.39851(13) 0.24379(12) 0.0144(3) Uani 1 1 d . . . C15 C 1.13554(13) -0.04530(13) 0.12174(11) 0.0166(4) Uani 1 1 d . . . C32 C 1.38702(13) 0.15041(13) 0.29430(12) 0.0165(4) Uani 1 1 d . . . H32 H 1.4139 0.1750 0.2528 0.020 Uiso 1 1 calc R . . C2 C 0.76098(13) 0.62418(13) 0.17300(11) 0.0152(3) Uani 1 1 d . . . C38 C 1.42358(13) -0.04815(14) 0.12421(12) 0.0193(4) Uani 1 1 d . . . H38 H 1.4481 -0.0080 0.1848 0.023 Uiso 1 1 calc R . . C22 C 1.22062(13) 0.21257(13) 0.15369(12) 0.0177(4) Uani 1 1 d . . . H22 H 1.1959 0.2116 0.2055 0.021 Uiso 1 1 calc R . . C33 C 1.32896(13) -0.05237(13) 0.08393(12) 0.0147(3) Uani 1 1 d . . . C21 C 1.25629(12) 0.13114(13) 0.10401(11) 0.0139(3) Uani 1 1 d . . . C37 C 1.48180(14) -0.10431(15) 0.07346(13) 0.0255(4) Uani 1 1 d . . . H37 H 1.5453 -0.1019 0.1000 0.031 Uiso 1 1 calc R . . C34 C 1.29100(13) -0.11335(13) -0.00697(12) 0.0196(4) Uani 1 1 d . . . H34 H 1.2273 -0.1165 -0.0336 0.024 Uiso 1 1 calc R . . C23 C 1.22219(13) 0.29487(14) 0.12540(12) 0.0185(4) Uani 1 1 d . . . H23 H 1.1973 0.3488 0.1576 0.022 Uiso 1 1 calc R . . C36 C 1.44458(15) -0.16385(15) -0.01687(14) 0.0275(5) Uani 1 1 d . . . H36 H 1.4837 -0.2007 -0.0510 0.033 Uiso 1 1 calc R . . C35 C 1.34965(14) -0.16898(15) -0.05667(13) 0.0261(4) Uani 1 1 d . . . H35 H 1.3251 -0.2100 -0.1170 0.031 Uiso 1 1 calc R . . C26 C 1.29437(12) 0.13291(13) 0.02643(11) 0.0153(3) Uani 1 1 d . . . H26 H 1.3178 0.0785 -0.0070 0.018 Uiso 1 1 calc R . . C24 C 1.26090(13) 0.29682(13) 0.04895(12) 0.0175(4) Uani 1 1 d . . . H24 H 1.2627 0.3525 0.0306 0.021 Uiso 1 1 calc R . . C25 C 1.29691(13) 0.21622(13) -0.00016(12) 0.0176(4) Uani 1 1 d . . . H25 H 1.3229 0.2181 -0.0511 0.021 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 0.01212(12) 0.01350(12) 0.01209(11) 0.00495(9) 0.00118(8) 0.00138(8) P2 0.0130(2) 0.0137(2) 0.0126(2) 0.00430(17) 0.00284(17) 0.00249(16) P1 0.0116(2) 0.0139(2) 0.0123(2) 0.00377(17) 0.00285(16) 0.00168(16) O1 0.0257(7) 0.0179(7) 0.0221(7) 0.0109(6) -0.0003(6) 0.0014(5) O2 0.0162(6) 0.0179(6) 0.0226(7) 0.0078(5) 0.0052(5) -0.0002(5) O3 0.0238(7) 0.0195(7) 0.0241(7) 0.0136(6) 0.0015(6) 0.0020(5) O4 0.0158(7) 0.0237(7) 0.0324(8) 0.0164(6) 0.0027(6) -0.0022(5) O5 0.0231(7) 0.0211(7) 0.0143(6) 0.0004(5) 0.0007(5) 0.0056(6) O6 0.0160(6) 0.0240(7) 0.0190(6) 0.0064(5) 0.0059(5) 0.0071(5) O7 0.0292(7) 0.0166(6) 0.0153(6) 0.0014(5) 0.0025(5) 0.0066(5) O8 0.0181(7) 0.0233(7) 0.0216(7) 0.0056(6) 0.0046(5) 0.0091(5) O1W 0.0346(9) 0.0231(8) 0.0237(7) 0.0098(6) 0.0069(6) 0.0061(6) O2W 0.0263(8) 0.0281(8) 0.0508(10) 0.0141(8) 0.0004(7) 0.0018(7) O3W 0.0311(8) 0.0216(7) 0.0167(7) 0.0055(6) 0.0012(6) 0.0048(6) O4W 0.0281(8) 0.0284(8) 0.0373(9) 0.0171(7) 0.0082(7) 0.0085(6) O5W 0.0274(8) 0.0227(7) 0.0238(7) 0.0096(6) 0.0040(6) 0.0018(6) O6W 0.0247(8) 0.0260(8) 0.0276(8) 0.0112(6) 0.0006(6) -0.0023(6) O7W 0.0239(8) 0.0248(8) 0.0292(8) 0.0105(6) 0.0017(6) 0.0044(6) N1 0.0181(8) 0.0122(7) 0.0129(7) 0.0054(6) 0.0008(6) 0.0021(6) N2 0.0146(7) 0.0142(7) 0.0103(7) 0.0028(6) 0.0027(5) 0.0021(6) N3 0.0122(7) 0.0173(7) 0.0169(7) 0.0072(6) 0.0020(6) -0.0012(6) N4 0.0167(8) 0.0157(7) 0.0096(7) 0.0023(6) 0.0005(6) 0.0003(6) N5 0.0151(7) 0.0141(7) 0.0123(7) 0.0068(6) 0.0028(6) 0.0005(6) N6 0.0150(8) 0.0168(7) 0.0184(7) 0.0077(6) 0.0042(6) 0.0047(6) C54 0.0253(10) 0.0168(9) 0.0264(10) 0.0060(8) 0.0124(8) 0.0075(8) C53 0.0260(10) 0.0178(9) 0.0175(9) 0.0024(7) 0.0065(8) 0.0042(7) C41 0.0177(9) 0.0251(10) 0.0165(9) 0.0092(8) 0.0034(7) 0.0031(7) C55 0.0170(9) 0.0216(10) 0.0248(10) 0.0080(8) 0.0052(8) 0.0073(7) C42 0.0248(10) 0.0204(10) 0.0228(9) 0.0117(8) 0.0039(8) 0.0049(8) C40 0.0148(9) 0.0172(9) 0.0142(8) 0.0031(7) 0.0040(7) 0.0030(7) C52 0.0170(9) 0.0166(9) 0.0192(9) 0.0037(7) 0.0025(7) 0.0027(7) C56 0.0182(9) 0.0193(9) 0.0168(9) 0.0066(7) 0.0028(7) 0.0053(7) C51 0.0151(9) 0.0130(8) 0.0156(8) 0.0054(7) 0.0046(7) 0.0029(6) C43 0.0306(11) 0.0181(9) 0.0218(9) 0.0055(8) 0.0075(8) 0.0083(8) C39 0.0111(8) 0.0157(8) 0.0147(8) 0.0064(7) 0.0027(6) 0.0017(6) C44 0.0244(10) 0.0206(9) 0.0147(8) 0.0062(7) 0.0054(7) 0.0057(8) C62 0.0201(9) 0.0199(9) 0.0163(9) 0.0066(7) 0.0030(7) 0.0046(7) C61 0.0224(10) 0.0199(10) 0.0202(9) 0.0020(8) -0.0021(8) 0.0029(7) C57 0.0165(9) 0.0158(9) 0.0145(8) 0.0052(7) 0.0024(7) 0.0062(7) C45 0.0152(9) 0.0165(9) 0.0140(8) 0.0066(7) 0.0024(7) 0.0012(7) C46 0.0203(10) 0.0208(10) 0.0251(10) 0.0109(8) 0.0050(8) 0.0058(7) C50 0.0185(9) 0.0164(9) 0.0156(8) 0.0021(7) 0.0031(7) 0.0015(7) C1 0.0161(9) 0.0129(8) 0.0124(8) 0.0021(7) 0.0052(7) 0.0015(6) C9 0.0199(9) 0.0140(8) 0.0131(8) 0.0061(7) 0.0035(7) 0.0016(7) C60 0.0272(11) 0.0284(11) 0.0141(9) 0.0035(8) -0.0014(8) 0.0092(8) C58 0.0208(10) 0.0212(9) 0.0199(9) 0.0088(8) 0.0043(7) 0.0055(7) C47 0.0268(11) 0.0168(9) 0.0294(10) 0.0108(8) 0.0054(8) 0.0021(8) C29 0.0239(10) 0.0323(11) 0.0173(9) 0.0126(8) 0.0094(8) 0.0113(8) C13 0.0204(9) 0.0151(9) 0.0130(8) 0.0043(7) 0.0027(7) -0.0018(7) C4 0.0154(9) 0.0182(9) 0.0155(8) 0.0013(7) 0.0035(7) 0.0012(7) C14 0.0184(9) 0.0134(8) 0.0132(8) 0.0065(7) 0.0039(7) 0.0006(7) C3 0.0136(8) 0.0135(8) 0.0102(8) 0.0005(6) 0.0031(6) 0.0013(6) C59 0.0319(11) 0.0328(11) 0.0156(9) 0.0123(8) 0.0072(8) 0.0107(9) C49 0.0165(9) 0.0246(10) 0.0184(9) 0.0044(8) 0.0065(7) 0.0022(7) C30 0.0272(11) 0.0297(11) 0.0132(9) 0.0037(8) 0.0016(8) 0.0122(8) C48 0.0221(10) 0.0261(10) 0.0220(9) 0.0098(8) 0.0063(8) -0.0035(8) C12 0.0135(9) 0.0235(9) 0.0162(9) 0.0086(7) -0.0002(7) -0.0025(7) C28 0.0148(9) 0.0211(9) 0.0191(9) 0.0093(7) 0.0053(7) 0.0051(7) C18 0.0167(10) 0.0414(12) 0.0203(10) 0.0102(9) 0.0011(8) -0.0083(8) C17 0.0292(12) 0.0221(10) 0.0326(11) 0.0076(9) 0.0081(9) -0.0069(8) C5 0.0137(9) 0.0232(10) 0.0169(9) 0.0032(7) 0.0007(7) 0.0051(7) C11 0.0134(9) 0.0217(9) 0.0175(9) 0.0091(7) 0.0029(7) 0.0011(7) C19 0.0131(9) 0.0407(12) 0.0196(9) 0.0105(9) 0.0009(7) 0.0017(8) C10 0.0143(9) 0.0165(9) 0.0132(8) 0.0085(7) 0.0031(7) 0.0010(7) C31 0.0182(9) 0.0194(9) 0.0189(9) 0.0012(7) -0.0015(7) 0.0036(7) C16 0.0195(10) 0.0204(10) 0.0344(11) 0.0095(8) 0.0078(8) 0.0019(8) C6 0.0202(9) 0.0190(9) 0.0132(8) 0.0053(7) 0.0017(7) 0.0061(7) C7 0.0180(9) 0.0156(8) 0.0100(8) 0.0034(7) 0.0034(7) 0.0045(7) C27 0.0129(8) 0.0148(8) 0.0149(8) 0.0047(7) 0.0043(7) 0.0047(6) C20 0.0165(9) 0.0253(10) 0.0167(9) 0.0080(8) 0.0025(7) 0.0039(7) C8 0.0149(9) 0.0152(8) 0.0157(8) 0.0080(7) 0.0057(7) 0.0020(6) C15 0.0137(9) 0.0204(9) 0.0129(8) 0.0037(7) 0.0017(7) -0.0006(7) C32 0.0162(9) 0.0150(9) 0.0174(8) 0.0037(7) 0.0044(7) 0.0035(7) C2 0.0192(9) 0.0155(9) 0.0107(8) 0.0045(7) 0.0033(7) 0.0026(7) C38 0.0163(9) 0.0216(9) 0.0161(9) 0.0017(7) 0.0016(7) 0.0038(7) C22 0.0166(9) 0.0204(9) 0.0161(8) 0.0048(7) 0.0055(7) 0.0047(7) C33 0.0145(9) 0.0144(8) 0.0152(8) 0.0048(7) 0.0036(7) 0.0022(6) C21 0.0110(8) 0.0150(8) 0.0148(8) 0.0046(7) 0.0015(6) 0.0014(6) C37 0.0147(9) 0.0297(11) 0.0268(10) 0.0013(9) 0.0026(8) 0.0080(8) C34 0.0146(9) 0.0201(9) 0.0198(9) 0.0020(7) 0.0009(7) 0.0024(7) C23 0.0175(9) 0.0169(9) 0.0191(9) 0.0032(7) 0.0026(7) 0.0047(7) C36 0.0235(10) 0.0277(11) 0.0255(10) -0.0027(9) 0.0083(8) 0.0097(8) C35 0.0234(10) 0.0254(10) 0.0198(9) -0.0055(8) 0.0029(8) 0.0049(8) C26 0.0129(8) 0.0190(9) 0.0135(8) 0.0043(7) 0.0030(7) 0.0038(7) C24 0.0145(9) 0.0174(9) 0.0206(9) 0.0088(7) -0.0005(7) 0.0019(7) C25 0.0150(9) 0.0240(10) 0.0166(9) 0.0096(7) 0.0046(7) 0.0052(7) _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 N5 1.9994(16) . ? Ni1 N2 2.0082(16) . ? Ni1 N3 2.0869(15) . ? Ni1 N1 2.0995(16) . ? Ni1 N6 2.1038(16) . ? Ni1 N4 2.1087(16) . ? P2 C45 1.7886(19) . ? P2 C51 1.7934(18) . ? P2 C57 1.8001(19) . ? P2 C39 1.8007(18) . ? P1 C21 1.7898(18) . ? P1 C15 1.7898(19) . ? P1 C33 1.7910(18) . ? P1 C27 1.7946(18) . ? O1 N1 1.4175(18) . ? O2 C1 1.269(2) . ? O3 C2 1.270(2) . ? O4 N3 1.4100(19) . ? O5 N4 1.4158(19) . ? O6 C8 1.276(2) . ? O7 C9 1.281(2) . ? O8 N6 1.4132(19) . ? N1 C1 1.315(2) . ? N2 C3 1.335(2) . ? N2 C7 1.344(2) . ? N3 C2 1.316(2) . ? N4 C8 1.315(2) . ? N5 C10 1.340(2) . ? N5 C14 1.342(2) . ? N6 C9 1.314(2) . ? C54 C55 1.380(3) . ? C54 C53 1.391(3) . ? C53 C52 1.387(3) . ? C41 C40 1.383(2) . ? C41 C42 1.384(3) . ? C55 C56 1.389(2) . ? C42 C43 1.389(3) . ? C40 C39 1.403(2) . ? C52 C51 1.403(2) . ? C56 C51 1.397(2) . ? C43 C44 1.388(3) . ? C39 C44 1.395(2) . ? C62 C61 1.395(3) . ? C62 C57 1.396(3) . ? C61 C60 1.386(3) . ? C57 C58 1.403(2) . ? C45 C46 1.395(3) . ? C45 C50 1.398(2) . ? C46 C47 1.378(3) . ? C50 C49 1.385(3) . ? C1 C3 1.502(2) . ? C9 C14 1.486(2) . ? C60 C59 1.380(3) . ? C58 C59 1.393(3) . ? C47 C48 1.388(3) . ? C29 C30 1.382(3) . ? C29 C28 1.392(3) . ? C13 C12 1.383(3) . ? C13 C14 1.389(2) . ? C4 C3 1.388(2) . ? C4 C5 1.388(3) . ? C49 C48 1.383(3) . ? C30 C31 1.386(3) . ? C12 C11 1.394(3) . ? C28 C27 1.397(2) . ? C18 C19 1.377(3) . ? C18 C17 1.390(3) . ? C17 C16 1.381(3) . ? C5 C6 1.387(3) . ? C11 C10 1.387(2) . ? C19 C20 1.387(3) . ? C10 C8 1.492(2) . ? C31 C32 1.384(2) . ? C16 C15 1.393(3) . ? C6 C7 1.386(2) . ? C7 C2 1.489(2) . ? C27 C32 1.397(2) . ? C20 C15 1.394(2) . ? C38 C33 1.386(2) . ? C38 C37 1.393(3) . ? C22 C23 1.387(3) . ? C22 C21 1.396(2) . ? C33 C34 1.400(2) . ? C21 C26 1.401(2) . ? C37 C36 1.386(3) . ? C34 C35 1.386(3) . ? C23 C24 1.390(3) . ? C36 C35 1.385(3) . ? C26 C25 1.385(2) . ? C24 C25 1.387(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 N5 Ni1 N2 166.52(6) . . ? N5 Ni1 N3 98.23(6) . . ? N2 Ni1 N3 76.37(6) . . ? N5 Ni1 N1 109.76(6) . . ? N2 Ni1 N1 75.93(6) . . ? N3 Ni1 N1 151.96(6) . . ? N5 Ni1 N6 76.18(7) . . ? N2 Ni1 N6 91.35(7) . . ? N3 Ni1 N6 90.06(6) . . ? N1 Ni1 N6 94.85(6) . . ? N5 Ni1 N4 76.50(6) . . ? N2 Ni1 N4 115.98(6) . . ? N3 Ni1 N4 95.13(6) . . ? N1 Ni1 N4 93.07(6) . . ? N6 Ni1 N4 152.64(6) . . ? C45 P2 C51 109.33(8) . . ? C45 P2 C57 108.22(9) . . ? C51 P2 C57 110.30(8) . . ? C45 P2 C39 109.58(8) . . ? C51 P2 C39 110.80(8) . . ? C57 P2 C39 108.57(8) . . ? C21 P1 C15 112.27(8) . . ? C21 P1 C33 108.99(8) . . ? C15 P1 C33 108.07(9) . . ? C21 P1 C27 106.72(8) . . ? C15 P1 C27 110.17(9) . . ? C33 P1 C27 110.64(8) . . ? C1 N1 O1 113.53(14) . . ? C1 N1 Ni1 118.84(12) . . ? O1 N1 Ni1 127.56(11) . . ? C3 N2 C7 121.28(15) . . ? C3 N2 Ni1 119.42(12) . . ? C7 N2 Ni1 117.98(12) . . ? C2 N3 O4 112.44(14) . . ? C2 N3 Ni1 116.49(12) . . ? O4 N3 Ni1 128.05(11) . . ? C8 N4 O5 111.58(14) . . ? C8 N4 Ni1 117.18(12) . . ? O5 N4 Ni1 131.10(11) . . ? C10 N5 C14 120.95(15) . . ? C10 N5 Ni1 119.51(11) . . ? C14 N5 Ni1 119.45(12) . . ? C9 N6 O8 112.38(14) . . ? C9 N6 Ni1 117.32(12) . . ? O8 N6 Ni1 129.19(11) . . ? C55 C54 C53 120.63(17) . . ? C52 C53 C54 119.70(17) . . ? C40 C41 C42 120.03(17) . . ? C54 C55 C56 120.39(17) . . ? C41 C42 C43 120.58(18) . . ? C41 C40 C39 119.99(16) . . ? C53 C52 C51 119.82(17) . . ? C55 C56 C51 119.41(17) . . ? C56 C51 C52 120.02(16) . . ? C56 C51 P2 120.61(14) . . ? C52 C51 P2 119.33(13) . . ? C44 C43 C42 119.74(17) . . ? C44 C39 C40 119.50(16) . . ? C44 C39 P2 119.51(13) . . ? C40 C39 P2 120.98(13) . . ? C43 C44 C39 120.12(16) . . ? C61 C62 C57 119.75(17) . . ? C60 C61 C62 120.11(18) . . ? C62 C57 C58 119.83(16) . . ? C62 C57 P2 119.44(14) . . ? C58 C57 P2 120.72(14) . . ? C46 C45 C50 119.80(16) . . ? C46 C45 P2 120.30(14) . . ? C50 C45 P2 119.73(13) . . ? C47 C46 C45 120.17(18) . . ? C49 C50 C45 119.75(17) . . ? O2 C1 N1 127.88(16) . . ? O2 C1 C3 120.83(15) . . ? N1 C1 C3 111.29(15) . . ? O7 C9 N6 124.30(17) . . ? O7 C9 C14 123.07(16) . . ? N6 C9 C14 112.62(15) . . ? C59 C60 C61 120.40(18) . . ? C59 C58 C57 119.52(18) . . ? C46 C47 C48 119.66(18) . . ? C30 C29 C28 120.04(18) . . ? C12 C13 C14 118.57(16) . . ? C3 C4 C5 118.38(17) . . ? N5 C14 C13 120.93(17) . . ? N5 C14 C9 113.71(15) . . ? C13 C14 C9 125.37(16) . . ? N2 C3 C4 120.75(16) . . ? N2 C3 C1 114.18(15) . . ? C4 C3 C1 125.04(16) . . ? C60 C59 C58 120.39(18) . . ? C48 C49 C50 119.79(18) . . ? C29 C30 C31 120.79(17) . . ? C49 C48 C47 120.82(18) . . ? C13 C12 C11 120.16(17) . . ? C29 C28 C27 119.05(17) . . ? C19 C18 C17 120.28(18) . . ? C16 C17 C18 119.88(19) . . ? C6 C5 C4 120.37(17) . . ? C10 C11 C12 118.22(17) . . ? C18 C19 C20 120.49(19) . . ? N5 C10 C11 121.12(16) . . ? N5 C10 C8 113.81(15) . . ? C11 C10 C8 125.07(16) . . ? C32 C31 C30 120.09(18) . . ? C17 C16 C15 119.89(19) . . ? C7 C6 C5 118.20(17) . . ? N2 C7 C6 120.85(16) . . ? N2 C7 C2 113.78(15) . . ? C6 C7 C2 125.32(16) . . ? C32 C27 C28 120.70(16) . . ? C32 C27 P1 117.51(14) . . ? C28 C27 P1 121.79(13) . . ? C19 C20 C15 119.30(18) . . ? O6 C8 N4 125.51(16) . . ? O6 C8 C10 121.64(16) . . ? N4 C8 C10 112.84(15) . . ? C16 C15 C20 120.15(17) . . ? C16 C15 P1 118.24(14) . . ? C20 C15 P1 121.51(14) . . ? C31 C32 C27 119.32(17) . . ? O3 C2 N3 125.74(17) . . ? O3 C2 C7 122.08(16) . . ? N3 C2 C7 112.16(15) . . ? C33 C38 C37 119.69(17) . . ? C23 C22 C21 119.70(17) . . ? C38 C33 C34 120.64(17) . . ? C38 C33 P1 121.17(14) . . ? C34 C33 P1 118.01(14) . . ? C22 C21 C26 120.16(16) . . ? C22 C21 P1 118.75(13) . . ? C26 C21 P1 121.07(13) . . ? C36 C37 C38 119.69(18) . . ? C35 C34 C33 119.09(17) . . ? C22 C23 C24 120.00(17) . . ? C35 C36 C37 120.56(18) . . ? C36 C35 C34 120.31(18) . . ? C25 C26 C21 119.50(16) . . ? C25 C24 C23 120.36(17) . . ? C26 C25 C24 120.26(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O1 O4W 0.94(2) 2.02(2) 2.902(2) 155.2(19) . O1 H1O1 O2 0.94(2) 2.10(2) 2.678(2) 118.0(17) . O4 H1O4 O3 0.87(2) 2.06(2) 2.610(2) 120.2(19) . O5 H1O5 O6 0.83(2) 1.98(2) 2.592(2) 130(2) . O8 H1O8 O7 0.84(2) 2.02(2) 2.586(2) 124.2(19) . O1W H1W1 O6W 0.77(2) 2.15(2) 2.872(2) 157(2) 2_776 O1W H1W2 O7 0.85(2) 1.94(3) 2.786(2) 175(2) . O2W H2W1 O1 0.95(3) 2.01(3) 2.944(2) 166(2) 1_455 O2W H2W2 O3W 0.84(3) 1.97(3) 2.800(2) 167(3) . O3W H3W1 O7 0.89(2) 1.86(2) 2.730(2) 167(2) 2_666 O3W H3W2 O6 0.81(2) 1.96(2) 2.759(2) 170(2) 1_455 O4W H4W1 O2 0.93(2) 1.89(3) 2.785(2) 160(2) . O4W H4W2 O7W 0.98(2) 1.84(2) 2.802(2) 167(2) 1_545 O5W H5W2 O3 0.87(2) 1.93(2) 2.793(2) 171(2) . O5W H5W1 O1W 0.81(2) 1.97(2) 2.774(2) 170(2) . O6W H6W1 O5W 0.77(3) 2.15(3) 2.903(2) 166(2) . O6W H6W2 O3W 0.76(2) 2.27(3) 3.012(2) 167(2) 1_665 O7W H7W1 O5W 0.82(2) 2.02(2) 2.845(2) 177(2) . O7W H7W2 O2W 0.91(2) 1.82(3) 2.712(2) 169(2) 1_665 _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 0.387 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.063