Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Kaikarainen, Anssi' 'Mutikainen, Ilpo' 'Pajunen, Aarne' 'Pietikainen, Pekka' 'Sipila, Jussi' _publ_contact_author_name ; Anssi Haikarainen ; _publ_contact_author_address ; Deparment of Chemistry, Laboratory of Inorganic Chemistry P.O. Box 55, 00014 University of Helsinki, Finland ; _publ_contact_author_email ; Anssi.Haikarainen@helsinki.fi ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Characterization of Bulky Salen complexes of Co, Cu, Fe, Mn and Ni with Amphiphilic Solubility Properties ; data_2 _database_code_CSD 158146 _audit_creation_method SHELXL97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; C62 H62 Cu N2 O2 P2 2+, (Cl 1-)2, 2(C2 H3 N), 1.5(C6 H14 O) ; _chemical_formula_sum 'C75 H89 Cl2 Cu N4 O3.5 P2' _chemical_formula_weight 1298.88 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 14.941(8) _cell_length_b 19.023(8) _cell_length_c 13.869(6) _cell_angle_alpha 95.42(5) _cell_angle_beta 116.06(5) _cell_angle_gamma 88.96(5) _cell_volume 3524(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.33 _cell_measurement_theta_max 10.36 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S diffractometer' _diffrn_measurement_method 2\q/\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.1 _diffrn_reflns_number 9310 _diffrn_reflns_av_R_equivalents 0.086 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8953 _reflns_number_gt 6634 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993a ; _computing_cell_refinement ? ; MSC/AFC Diffarctometer Control Software (Molecular Structure Corporation, 1993a ; _computing_data_reduction ? ; TEXSAN PROCESS (Molecular Structure Corporation 1993b) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^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 calculated _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8953 _refine_ls_number_parameters 757 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1335 _refine_ls_r-factor_obs 0.1100 _refine_ls_R_factor_gt 0.1100 _refine_ls_r_factor_obs 0.1100 _refine_ls_wR_factor_ref 0.3347 _refine_ls_wR_factor_all 0.3347 _refine_ls_wr_factor_obs 0.3080 _refine_ls_wR_factor_gt 0.3080 _refine_ls_goodness_of_fit_ref 1.336 _refine_ls_goodness_of_fit_all 1.336 _refine_ls_restrained_S_all 1.366 _refine_ls_shift/su_max 0.166 _refine_ls_shift/su_mean 0.005 _diffrn_measured_fraction_theta_max 0.810 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.810 _refine_diff_density_max 1.692 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.116 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.79408(7) 0.43732(5) -0.02256(8) 0.0537(4) Uani 1 d . . . P1 P 1.08585(16) 0.81153(11) 0.15581(18) 0.0531(6) Uani 1 d . . . P2 P 0.45083(16) 0.14835(12) 0.03258(19) 0.0566(6) Uani 1 d . . . Cl1 Cl 0.3708(2) 0.10998(18) 0.6809(2) 0.0948(9) Uani 1 d . . . Cl2 Cl 0.6799(3) 0.2925(2) 0.6062(3) 0.1119(11) Uani 1 d . . . O1 O 0.8912(4) 0.4899(3) 0.1019(4) 0.0508(13) Uani 1 d . . . O2 O 0.7951(4) 0.3636(3) 0.0595(5) 0.0634(16) Uani 1 d . . . N1 N 0.6746(5) 0.4011(4) -0.1455(5) 0.0546(17) Uani 1 d . . . N2 N 0.8053(5) 0.4986(4) -0.1202(6) 0.0544(18) Uani 1 d . . . C1 C 0.7335(6) 0.3085(4) 0.0311(7) 0.054(2) Uani 1 d . . . C2 C 0.7568(6) 0.2568(4) 0.1066(7) 0.055(2) Uani 1 d . . . C3 C 0.6881(6) 0.2008(4) 0.0785(7) 0.056(2) Uani 1 d . . . H3A H 0.7026 0.1652 0.1276 0.068 Uiso 1 d R . . C4 C 0.5998(6) 0.1947(4) -0.0163(8) 0.057(2) Uani 1 d . . . C5 C 0.5815(6) 0.2430(4) -0.0904(7) 0.057(2) Uani 1 d . . . H5A H 0.5222 0.2373 -0.1581 0.069 Uiso 1 d R . . C6 C 0.6479(6) 0.2998(4) -0.0683(7) 0.056(2) Uani 1 d . . . C7 C 0.6238(6) 0.3465(5) -0.1514(7) 0.057(2) Uani 1 d . . . H7A H 0.5638 0.3358 -0.2172 0.068 Uiso 1 d R . . C8 C 0.6443(6) 0.4457(5) -0.2354(7) 0.067(2) Uani 1 d . . . H8A H 0.6024 0.4827 -0.2285 0.100 Uiso 1 d R . . H8B H 0.6077 0.4178 -0.3031 0.100 Uiso 1 d R . . C9 C 0.7369(7) 0.4763(5) -0.2337(7) 0.062(2) Uani 1 d . . . H9A H 0.7685 0.4416 -0.2624 0.093 Uiso 1 d R . . H9B H 0.7217 0.5161 -0.2756 0.093 Uiso 1 d R . . C10 C 0.8690(6) 0.5479(4) -0.0948(7) 0.052(2) Uani 1 d . . . H10A H 0.8726 0.5692 -0.1530 0.063 Uiso 1 d R . . C11 C 0.9384(6) 0.5733(4) 0.0138(7) 0.052(2) Uani 1 d . . . C12 C 1.0009(6) 0.6321(4) 0.0267(7) 0.053(2) Uani 1 d . . . H12A H 0.9987 0.6507 -0.0362 0.063 Uiso 1 d R . . C13 C 1.0634(6) 0.6633(4) 0.1255(7) 0.053(2) Uani 1 d . . . C14 C 1.0646(6) 0.6352(4) 0.2168(7) 0.057(2) Uani 1 d . . . H14A H 1.1090 0.6576 0.2868 0.068 Uiso 1 d R . . C15 C 1.0076(6) 0.5784(4) 0.2123(7) 0.054(2) Uani 1 d . . . C16 C 0.9440(6) 0.5446(4) 0.1082(7) 0.054(2) Uani 1 d . . . C17 C 0.8511(6) 0.2632(5) 0.2137(7) 0.056(2) Uani 1 d . . . C18 C 0.9438(6) 0.2712(5) 0.1920(7) 0.060(2) Uani 1 d . . . H18A H 0.9367 0.3120 0.1536 0.090 Uiso 1 d R . . H18B H 1.0031 0.2768 0.2596 0.090 Uiso 1 d R . . H18C H 0.9488 0.2299 0.1494 0.090 Uiso 1 d R . . C19 C 0.8449(7) 0.3255(5) 0.2847(8) 0.069(2) Uani 1 d . . . H19A H 0.7873 0.3194 0.2971 0.103 Uiso 1 d R . . H19B H 0.9041 0.3287 0.3524 0.103 Uiso 1 d R . . H19C H 0.8391 0.3681 0.2504 0.103 Uiso 1 d R . . C20 C 0.8667(7) 0.1974(5) 0.2736(8) 0.070(3) Uani 1 d . . . H20A H 0.8107 0.1907 0.2883 0.105 Uiso 1 d R . . H20B H 0.8724 0.1567 0.2302 0.105 Uiso 1 d R . . H20C H 0.9268 0.2036 0.3404 0.105 Uiso 1 d R . . C21 C 0.5264(6) 0.1348(4) -0.0402(7) 0.052(2) Uani 1 d . . . H21A H 0.4824 0.1300 -0.1163 0.077 Uiso 1 d R . . H21B H 0.5614 0.0914 -0.0223 0.077 Uiso 1 d R . . C22 C 1.1319(6) 0.7235(4) 0.1408(7) 0.054(2) Uani 1 d . . . H22A H 1.1931 0.7181 0.2045 0.081 Uiso 1 d R . . H22B H 1.1476 0.7210 0.0805 0.081 Uiso 1 d R . . C23 C 1.0140(7) 0.5505(5) 0.3155(7) 0.065(2) Uani 1 d . . . C24 C 1.0855(10) 0.5939(6) 0.4163(8) 0.097(4) Uani 1 d . . . H24A H 1.1513 0.5931 0.4204 0.145 Uiso 1 d R . . H24B H 1.0632 0.6417 0.4133 0.145 Uiso 1 d R . . H24C H 1.0870 0.5755 0.4791 0.145 Uiso 1 d R . . C25 C 0.9095(8) 0.5533(6) 0.3135(8) 0.083(3) Uani 1 d . . . H25A H 0.8627 0.5252 0.2502 0.125 Uiso 1 d R . . H25B H 0.9123 0.5351 0.3770 0.125 Uiso 1 d R . . H25C H 0.8885 0.6013 0.3112 0.125 Uiso 1 d R . . C26 C 1.0513(8) 0.4754(5) 0.3252(8) 0.071(3) Uani 1 d . . . H26A H 1.1163 0.4742 0.3271 0.106 Uiso 1 d R . . H26B H 1.0552 0.4590 0.3903 0.106 Uiso 1 d R . . H26C H 1.0055 0.4455 0.2638 0.106 Uiso 1 d R . . C27 C 0.5288(7) 0.1488(5) 0.1745(7) 0.061(2) Uani 1 d . . . C28 C 0.5507(7) 0.0852(5) 0.2220(8) 0.071(3) Uani 1 d . . . H28A H 0.5203 0.0421 0.1782 0.085 Uiso 1 d R . . C29 C 0.6129(8) 0.0831(7) 0.3290(10) 0.085(3) Uani 1 d . . . H29A H 0.6278 0.0393 0.3615 0.102 Uiso 1 d R . . C30 C 0.6550(8) 0.1462(8) 0.3908(10) 0.092(4) Uani 1 d . . . H30A H 0.6994 0.1455 0.4663 0.111 Uiso 1 d R . . C31 C 0.6350(8) 0.2088(6) 0.3450(9) 0.081(3) Uani 1 d . . . H31A H 0.6639 0.2521 0.3893 0.097 Uiso 1 d R . . C32 C 0.5731(7) 0.2110(5) 0.2371(8) 0.068(3) Uani 1 d . . . H32A H 0.5604 0.2546 0.2041 0.082 Uiso 1 d R . . C33 C 0.3586(6) 0.0779(4) -0.0112(7) 0.057(2) Uani 1 d . . . C34 C 0.3293(7) 0.0421(5) -0.1081(8) 0.064(2) Uani 1 d . . . H34A H 0.3628 0.0503 -0.1513 0.077 Uiso 1 d R . . C35 C 0.2492(7) -0.0072(5) -0.1469(8) 0.069(2) Uani 1 d . . . H35A H 0.2264 -0.0322 -0.2175 0.083 Uiso 1 d R . . C36 C 0.2036(8) -0.0180(6) -0.0816(10) 0.080(3) Uani 1 d . . . H36A H 0.1498 -0.0523 -0.1060 0.096 Uiso 1 d R . . C37 C 0.2360(7) 0.0192(5) 0.0206(9) 0.074(3) Uani 1 d . . . H37A H 0.2033 0.0107 0.0645 0.089 Uiso 1 d R . . C38 C 0.3107(7) 0.0661(5) 0.0550(8) 0.069(3) Uani 1 d . . . H38A H 0.3328 0.0918 0.1250 0.083 Uiso 1 d R . . C39 C 0.3833(6) 0.2290(4) 0.0006(8) 0.061(2) Uani 1 d . . . C40 C 0.3497(7) 0.2496(5) -0.1007(8) 0.071(3) Uani 1 d . . . H40A H 0.3663 0.2222 -0.1520 0.085 Uiso 1 d R . . C41 C 0.2912(8) 0.3070(6) -0.1297(10) 0.090(3) Uani 1 d . . . H41A H 0.2697 0.3225 -0.2003 0.109 Uiso 1 d R . . C42 C 0.2643(9) 0.3430(6) -0.0584(11) 0.098(4) Uani 1 d . . . H42A H 0.2197 0.3816 -0.0813 0.118 Uiso 1 d R . . C43 C 0.2984(8) 0.3244(6) 0.0462(10) 0.088(3) Uani 1 d . . . H43A H 0.2823 0.3528 0.0970 0.106 Uiso 1 d R . . C44 C 0.3573(7) 0.2669(5) 0.0760(9) 0.074(3) Uani 1 d . . . H44A H 0.3796 0.2515 0.1469 0.088 Uiso 1 d R . . C45 C 1.1899(6) 0.8740(4) 0.2107(7) 0.058(2) Uani 1 d . . . C46 C 1.1881(7) 0.9325(5) 0.2721(8) 0.071(3) Uani 1 d . . . H46A H 1.1320 0.9410 0.2875 0.086 Uiso 1 d R . . C47 C 1.2690(8) 0.9803(6) 0.3147(9) 0.081(3) Uani 1 d . . . H47A H 1.2683 1.0230 0.3570 0.097 Uiso 1 d R . . C48 C 1.3490(7) 0.9656(6) 0.2942(9) 0.079(3) Uani 1 d . . . H48A H 1.4052 0.9982 0.3238 0.095 Uiso 1 d R . . C49 C 1.3508(7) 0.9066(6) 0.2332(10) 0.083(3) Uani 1 d . . . H49A H 1.4089 0.8982 0.2214 0.099 Uiso 1 d R . . C50 C 1.2731(7) 0.8598(6) 0.1901(8) 0.073(3) Uani 1 d . . . H50A H 1.2746 0.8177 0.1469 0.087 Uiso 1 d R . . C51 C 1.0318(6) 0.8166(4) 0.2483(7) 0.055(2) Uani 1 d . . . C52 C 1.0922(7) 0.7982(5) 0.3523(7) 0.070(3) Uani 1 d . . . H52A H 1.1587 0.7822 0.3711 0.084 Uiso 1 d R . . C53 C 1.0548(9) 0.8029(5) 0.4280(8) 0.081(3) Uani 1 d . . . H53A H 1.0963 0.7914 0.5004 0.098 Uiso 1 d R . . C54 C 0.9597(9) 0.8241(6) 0.4014(9) 0.085(3) Uani 1 d . . . H54A H 0.9343 0.8255 0.4541 0.102 Uiso 1 d R . . C55 C 0.9004(8) 0.8432(6) 0.3000(9) 0.079(3) Uani 1 d . . . H55A H 0.8344 0.8597 0.2828 0.095 Uiso 1 d R . . C56 C 0.9354(7) 0.8391(5) 0.2215(8) 0.066(2) Uani 1 d . . . H56A H 0.8932 0.8506 0.1493 0.079 Uiso 1 d R . . C57 C 0.9967(6) 0.8355(5) 0.0276(7) 0.058(2) Uani 1 d . . . C58 C 1.0155(6) 0.8926(5) -0.0170(8) 0.062(2) Uani 1 d . . . H58A H 1.0737 0.9226 0.0244 0.074 Uiso 1 d R . . C59 C 0.9511(7) 0.9065(5) -0.1201(8) 0.068(3) Uani 1 d . . . H59A H 0.9656 0.9439 -0.1532 0.082 Uiso 1 d R . . C60 C 0.8657(8) 0.8649(6) -0.1776(8) 0.077(3) Uani 1 d . . . H60A H 0.8188 0.8758 -0.2485 0.092 Uiso 1 d R . . C61 C 0.8441(7) 0.8091(5) -0.1344(8) 0.068(2) Uani 1 d . . . H61A H 0.7843 0.7807 -0.1755 0.081 Uiso 1 d R . . C62 C 0.9099(7) 0.7945(5) -0.0305(8) 0.066(3) Uani 1 d . . . H62A H 0.8966 0.7549 -0.0001 0.080 Uiso 1 d R . . N3 N 0.3814(7) 0.1641(6) 0.3146(9) 0.100(3) Uani 1 d . . . C63 C 0.4311(9) 0.1575(6) 0.4014(12) 0.090(3) Uani 1 d . . . C64 C 0.4977(11) 0.1473(10) 0.5155(12) 0.140(6) Uani 1 d . . . N4 N 0.0174(11) 0.0400(8) 0.3490(11) 0.133(5) Uani 1 d . . . C65 C 0.0739(11) 0.0259(7) 0.4256(14) 0.106(4) Uani 1 d . . . C66 C 0.1462(11) 0.0017(8) 0.5337(13) 0.124(5) Uani 1 d . . . O3A O 0.6552(15) 0.7348(11) 0.3745(16) 0.133(4) Uiso 0.50 d PD . . C67A C 0.762(2) 0.7355(16) 0.442(2) 0.133(4) Uiso 0.50 d PD . . C68A C 0.797(2) 0.6681(15) 0.475(2) 0.133(4) Uiso 0.50 d PD . . C69A C 0.790(2) 0.7833(15) 0.542(2) 0.133(4) Uiso 0.50 d PD . . C70A C 0.554(2) 0.7362(17) 0.372(3) 0.133(4) Uiso 0.50 d PD . . C71A C 0.553(2) 0.6745(17) 0.438(3) 0.133(4) Uiso 0.50 d PD . . O3B O 0.506(2) 0.6157(16) -0.377(2) 0.204(7) Uiso 0.50 d PD . . C67B C 0.419(3) 0.603(2) -0.343(4) 0.204(7) Uiso 0.50 d PD . . C68B C 0.399(3) 0.542(2) -0.460(3) 0.204(7) Uiso 0.50 d PD . . C69B C 0.452(4) 0.559(3) -0.263(4) 0.204(7) Uiso 0.50 d PD . . C70B C 0.616(4) 0.639(3) -0.366(4) 0.204(7) Uiso 0.50 d PD . . C71B C 0.562(3) 0.665(3) -0.473(3) 0.204(7) Uiso 0.50 d PD . . C72B C 0.697(3) 0.654(3) -0.300(4) 0.204(7) Uiso 0.50 d PD . . O3C O 0.483(4) 0.496(3) 0.035(4) 0.301(13) Uiso 0.50 d PD . . C67C C 0.595(5) 0.470(4) 0.109(6) 0.301(13) Uiso 0.50 d PD . . C68C C 0.607(5) 0.509(4) 0.213(5) 0.301(13) Uiso 0.50 d PD . . C69C C 0.562(7) 0.398(3) 0.128(7) 0.301(13) Uiso 0.50 d PD . . C70C C 0.461(6) 0.510(4) -0.077(5) 0.301(13) Uiso 0.50 d PD . . C71C C 0.416(6) 0.456(4) -0.154(5) 0.301(13) Uiso 0.50 d PD . . C72C C 0.428(8) 0.580(4) -0.099(7) 0.301(13) Uiso 0.50 d PD . . 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 Cu 0.0529(7) 0.0572(7) 0.0697(7) 0.0350(5) 0.0389(5) 0.0141(5) P1 0.0555(13) 0.0560(13) 0.0706(14) 0.0315(11) 0.0443(11) 0.0171(10) P2 0.0541(13) 0.0634(14) 0.0775(15) 0.0312(11) 0.0476(12) 0.0166(10) Cl1 0.0806(18) 0.133(2) 0.0909(18) 0.0465(17) 0.0495(15) 0.0059(16) Cl2 0.095(2) 0.130(3) 0.094(2) 0.0133(19) 0.0276(17) 0.0421(19) O1 0.052(3) 0.055(3) 0.054(3) 0.020(2) 0.029(3) -0.004(2) O2 0.061(4) 0.076(4) 0.070(4) 0.045(3) 0.038(3) 0.017(3) N1 0.046(4) 0.059(4) 0.063(4) 0.028(3) 0.023(3) 0.005(3) N2 0.061(4) 0.056(4) 0.068(4) 0.038(3) 0.043(4) 0.022(4) C1 0.054(5) 0.058(5) 0.081(6) 0.036(4) 0.052(5) 0.016(4) C2 0.056(5) 0.061(5) 0.074(5) 0.034(4) 0.048(4) 0.020(4) C3 0.053(5) 0.060(5) 0.086(6) 0.042(4) 0.053(5) 0.028(4) C4 0.053(5) 0.055(5) 0.092(6) 0.033(4) 0.054(5) 0.019(4) C5 0.048(5) 0.071(6) 0.072(5) 0.038(4) 0.038(4) 0.018(4) C6 0.048(5) 0.065(5) 0.074(6) 0.033(4) 0.039(5) 0.013(4) C7 0.040(4) 0.066(5) 0.067(5) 0.029(4) 0.023(4) 0.013(4) C8 0.055(5) 0.080(6) 0.070(6) 0.043(5) 0.024(5) 0.016(4) C9 0.066(5) 0.067(6) 0.069(6) 0.034(5) 0.038(5) 0.012(4) C10 0.060(5) 0.056(5) 0.071(6) 0.040(4) 0.050(5) 0.024(4) C11 0.056(5) 0.062(5) 0.063(5) 0.037(4) 0.044(4) 0.027(4) C12 0.063(5) 0.058(5) 0.072(6) 0.042(4) 0.056(5) 0.027(4) C13 0.065(5) 0.053(5) 0.063(5) 0.032(4) 0.045(5) 0.021(4) C14 0.068(5) 0.063(5) 0.058(5) 0.025(4) 0.042(4) 0.025(4) C15 0.073(6) 0.056(5) 0.061(5) 0.030(4) 0.051(5) 0.017(4) C16 0.058(5) 0.055(5) 0.081(6) 0.038(5) 0.054(5) 0.023(4) C17 0.052(5) 0.072(6) 0.065(5) 0.040(4) 0.039(4) 0.017(4) C18 0.050(5) 0.077(6) 0.072(5) 0.030(5) 0.038(4) 0.008(4) C19 0.068(6) 0.080(6) 0.077(6) 0.023(5) 0.047(5) 0.013(5) C20 0.061(5) 0.080(6) 0.088(6) 0.049(5) 0.043(5) 0.009(5) C21 0.045(4) 0.061(5) 0.069(5) 0.021(4) 0.041(4) 0.007(4) C22 0.051(5) 0.054(5) 0.076(5) 0.030(4) 0.042(4) 0.011(4) C23 0.088(7) 0.069(6) 0.064(6) 0.030(5) 0.053(5) 0.011(5) C24 0.156(11) 0.088(8) 0.060(6) 0.026(6) 0.056(7) -0.014(7) C25 0.109(8) 0.103(8) 0.081(7) 0.045(6) 0.075(7) 0.035(6) C26 0.099(7) 0.065(6) 0.076(6) 0.042(5) 0.058(6) 0.026(5) C27 0.065(5) 0.074(6) 0.077(6) 0.029(5) 0.057(5) 0.022(5) C28 0.068(6) 0.080(7) 0.077(6) 0.029(5) 0.042(5) 0.020(5) C29 0.075(7) 0.112(9) 0.093(8) 0.053(7) 0.053(6) 0.042(7) C30 0.060(6) 0.141(12) 0.093(8) 0.037(8) 0.045(6) 0.020(7) C31 0.073(7) 0.100(8) 0.089(8) 0.016(6) 0.051(6) 0.002(6) C32 0.079(6) 0.071(6) 0.081(7) 0.022(5) 0.058(6) 0.015(5) C33 0.052(5) 0.065(5) 0.080(6) 0.033(5) 0.049(5) 0.020(4) C34 0.069(6) 0.072(6) 0.079(6) 0.029(5) 0.054(5) 0.007(5) C35 0.067(6) 0.081(7) 0.077(6) 0.024(5) 0.045(5) 0.006(5) C36 0.082(7) 0.082(7) 0.108(8) 0.033(6) 0.065(7) 0.009(5) C37 0.077(6) 0.079(7) 0.100(8) 0.022(6) 0.068(6) -0.008(5) C38 0.070(6) 0.084(7) 0.083(6) 0.034(5) 0.055(5) 0.014(5) C39 0.058(5) 0.057(5) 0.087(6) 0.029(5) 0.046(5) 0.012(4) C40 0.056(5) 0.089(7) 0.089(7) 0.043(6) 0.045(5) 0.027(5) C41 0.084(7) 0.099(8) 0.113(9) 0.050(7) 0.060(7) 0.037(6) C42 0.086(8) 0.097(8) 0.146(11) 0.063(8) 0.074(8) 0.045(6) C43 0.088(7) 0.078(7) 0.129(10) 0.024(7) 0.074(7) 0.032(6) C44 0.069(6) 0.072(6) 0.109(8) 0.029(5) 0.062(6) 0.022(5) C45 0.066(5) 0.058(5) 0.073(5) 0.032(4) 0.048(5) 0.026(4) C46 0.056(6) 0.082(7) 0.098(7) 0.039(6) 0.049(5) 0.018(5) C47 0.077(7) 0.079(7) 0.108(8) 0.022(6) 0.057(6) 0.018(6) C48 0.063(6) 0.095(8) 0.094(7) 0.032(6) 0.043(6) 0.014(5) C49 0.060(6) 0.099(8) 0.129(9) 0.048(7) 0.071(7) 0.024(6) C50 0.056(6) 0.093(7) 0.097(7) 0.043(6) 0.053(5) 0.019(5) C51 0.054(5) 0.060(5) 0.068(5) 0.021(4) 0.042(4) 0.008(4) C52 0.073(6) 0.091(7) 0.062(5) 0.032(5) 0.041(5) 0.017(5) C53 0.113(9) 0.084(7) 0.074(6) 0.026(5) 0.063(6) 0.022(6) C54 0.106(9) 0.091(7) 0.092(8) 0.018(6) 0.072(7) 0.005(6) C55 0.084(7) 0.094(7) 0.091(7) 0.024(6) 0.065(6) 0.024(6) C56 0.071(6) 0.072(6) 0.075(6) 0.022(5) 0.048(5) 0.016(5) C57 0.056(5) 0.071(5) 0.076(6) 0.040(5) 0.051(5) 0.030(4) C58 0.055(5) 0.064(5) 0.088(6) 0.037(5) 0.046(5) 0.015(4) C59 0.061(6) 0.088(7) 0.081(6) 0.050(5) 0.046(5) 0.019(5) C60 0.070(7) 0.109(8) 0.069(6) 0.042(6) 0.040(5) 0.031(6) C61 0.052(5) 0.082(6) 0.079(6) 0.033(5) 0.034(5) 0.022(5) C62 0.056(6) 0.077(6) 0.094(7) 0.043(5) 0.053(5) 0.028(5) N3 0.071(6) 0.138(9) 0.097(7) 0.032(7) 0.038(6) 0.023(6) C63 0.075(7) 0.103(9) 0.124(10) 0.042(8) 0.067(8) 0.017(6) C64 0.114(11) 0.231(19) 0.100(10) 0.082(11) 0.058(9) 0.030(11) N4 0.134(11) 0.169(12) 0.105(9) 0.049(9) 0.056(8) 0.053(9) C65 0.099(10) 0.105(10) 0.132(12) 0.018(9) 0.066(10) 0.028(8) C66 0.092(9) 0.127(12) 0.133(11) 0.030(9) 0.028(9) 0.013(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 Cu O2 1.883(5) . ? Cu O1 1.900(6) . ? Cu N1 1.928(7) . ? Cu N2 1.930(6) . ? P1 C51 1.786(7) . ? P1 C57 1.787(9) . ? P1 C45 1.807(10) . ? P1 C22 1.827(8) . ? P2 C27 1.792(10) . ? P2 C33 1.801(9) . ? P2 C39 1.801(8) . ? P2 C21 1.816(7) . ? O1 C16 1.290(9) . ? O2 C1 1.320(10) . ? N1 C7 1.274(10) . ? N1 C8 1.473(9) . ? N2 C10 1.260(10) . ? N2 C9 1.475(12) . ? C1 C6 1.407(12) . ? C1 C2 1.431(10) . ? C2 C3 1.396(12) . ? C2 C17 1.529(12) . ? C3 C4 1.391(12) . ? C4 C5 1.378(11) . ? C4 C21 1.506(11) . ? C5 C6 1.399(12) . ? C6 C7 1.436(11) . ? C8 C9 1.500(12) . ? C10 C11 1.443(12) . ? C11 C12 1.417(12) . ? C11 C16 1.434(10) . ? C12 C13 1.358(12) . ? C13 C14 1.413(10) . ? C13 C22 1.487(11) . ? C14 C15 1.368(12) . ? C15 C16 1.430(12) . ? C15 C23 1.537(10) . ? C17 C19 1.496(13) . ? C17 C20 1.527(10) . ? C17 C18 1.553(10) . ? C23 C24 1.510(14) . ? C23 C26 1.520(12) . ? C23 C25 1.549(13) . ? C27 C32 1.387(13) . ? C27 C28 1.397(12) . ? C28 C29 1.365(14) . ? C29 C30 1.391(17) . ? C30 C31 1.368(16) . ? C31 C32 1.375(14) . ? C33 C34 1.335(13) . ? C33 C38 1.423(11) . ? C34 C35 1.406(13) . ? C35 C36 1.382(12) . ? C36 C37 1.402(14) . ? C37 C38 1.325(14) . ? C39 C40 1.363(12) . ? C39 C44 1.404(13) . ? C40 C41 1.362(13) . ? C41 C42 1.349(16) . ? C42 C43 1.390(16) . ? C43 C44 1.368(13) . ? C45 C46 1.344(13) . ? C45 C50 1.409(12) . ? C46 C47 1.395(15) . ? C47 C48 1.364(14) . ? C48 C49 1.348(15) . ? C49 C50 1.351(15) . ? C51 C56 1.390(12) . ? C51 C52 1.400(12) . ? C52 C53 1.384(12) . ? C53 C54 1.366(15) . ? C54 C55 1.373(15) . ? C55 C56 1.396(12) . ? C57 C62 1.393(13) . ? C57 C58 1.391(11) . ? C58 C59 1.375(12) . ? C59 C60 1.383(15) . ? C60 C61 1.375(13) . ? C61 C62 1.394(13) . ? N3 C63 1.121(14) . ? C63 C64 1.48(2) . ? N4 C65 1.083(16) . ? C65 C66 1.52(2) . ? O3A C67A 1.45(3) . ? O3A C70A 1.50(3) . ? C67A C68A 1.41(3) . ? C67A C69A 1.47(3) . ? C70A C71A 1.56(3) . ? C71A C71B 1.21(4) 1_556 ? O3B C67B 1.60(4) . ? O3B C70B 1.64(5) . ? C67B C69B 1.36(4) . ? C67B C68B 1.82(3) . ? C69B C68C 1.92(8) 2_665 ? C70B C72B 1.17(4) . ? C70B C71B 1.48(4) . ? C71B C71A 1.21(4) 1_554 ? O3C C70C 0.79(8) 2_665 ? O3C O3C 1.30(11) 2_665 ? O3C C70C 1.49(4) . ? O3C C67C 1.63(5) . ? O3C C71C 1.85(11) 2_665 ? O3C C67C 1.99(11) 2_665 ? C67C C70C 0.86(9) 2_665 ? C67C C72C 0.99(11) 2_665 ? C67C C71C 1.53(11) 2_665 ? C67C C68C 1.49(5) . ? C67C C69C 1.54(5) . ? C67C O3C 1.99(11) 2_665 ? C68C C71C 1.04(9) 2_665 ? C68C C70C 1.71(10) 2_665 ? C68C C69B 1.92(8) 2_665 ? C69C C72C 0.67(12) 2_665 ? C69C C70C 1.92(11) 2_665 ? C70C O3C 0.79(8) 2_665 ? C70C C67C 0.86(9) 2_665 ? C70C C71C 1.36(5) . ? C70C C72C 1.42(4) . ? C70C C68C 1.71(10) 2_665 ? C70C C69C 1.92(11) 2_665 ? C70C C70C 2.00(12) 2_665 ? C71C C68C 1.04(9) 2_665 ? C71C C67C 1.53(11) 2_665 ? C71C O3C 1.85(11) 2_665 ? C72C C69C 0.67(12) 2_665 ? C72C C67C 0.99(11) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu O1 91.1(2) . . ? O2 Cu N1 93.2(3) . . ? O1 Cu N1 166.3(3) . . ? O2 Cu N2 168.0(3) . . ? O1 Cu N2 93.5(3) . . ? N1 Cu N2 84.9(3) . . ? C51 P1 C57 109.9(4) . . ? C51 P1 C45 106.9(4) . . ? C57 P1 C45 109.4(4) . . ? C51 P1 C22 111.9(4) . . ? C57 P1 C22 110.0(4) . . ? C45 P1 C22 108.6(4) . . ? C27 P2 C33 109.7(4) . . ? C27 P2 C39 111.6(4) . . ? C33 P2 C39 106.4(4) . . ? C27 P2 C21 109.6(4) . . ? C33 P2 C21 109.1(4) . . ? C39 P2 C21 110.4(4) . . ? C16 O1 Cu 129.1(5) . . ? C1 O2 Cu 128.7(5) . . ? C7 N1 C8 121.8(7) . . ? C7 N1 Cu 126.2(6) . . ? C8 N1 Cu 112.0(5) . . ? C10 N2 C9 121.8(6) . . ? C10 N2 Cu 125.7(6) . . ? C9 N2 Cu 112.1(5) . . ? O2 C1 C6 122.6(7) . . ? O2 C1 C2 117.0(8) . . ? C6 C1 C2 120.4(8) . . ? C3 C2 C1 116.6(8) . . ? C3 C2 C17 121.7(6) . . ? C1 C2 C17 121.7(8) . . ? C4 C3 C2 123.2(7) . . ? C5 C4 C3 119.1(8) . . ? C5 C4 C21 120.0(8) . . ? C3 C4 C21 120.9(7) . . ? C4 C5 C6 120.6(8) . . ? C5 C6 C1 119.8(7) . . ? C5 C6 C7 116.6(8) . . ? C1 C6 C7 123.5(8) . . ? N1 C7 C6 125.6(8) . . ? N1 C8 C9 108.0(7) . . ? N2 C9 C8 107.5(7) . . ? N2 C10 C11 125.6(6) . . ? C12 C11 C16 118.8(8) . . ? C12 C11 C10 117.4(6) . . ? C16 C11 C10 123.8(8) . . ? C13 C12 C11 122.1(7) . . ? C12 C13 C14 117.7(8) . . ? C12 C13 C22 122.8(7) . . ? C14 C13 C22 119.5(8) . . ? C15 C14 C13 124.4(9) . . ? C14 C15 C16 117.6(7) . . ? C14 C15 C23 121.3(8) . . ? C16 C15 C23 121.1(7) . . ? O1 C16 C15 118.8(6) . . ? O1 C16 C11 121.8(9) . . ? C15 C16 C11 119.4(7) . . ? C19 C17 C2 109.9(7) . . ? C19 C17 C20 108.5(7) . . ? C2 C17 C20 112.0(7) . . ? C19 C17 C18 110.3(8) . . ? C2 C17 C18 109.6(6) . . ? C20 C17 C18 106.4(6) . . ? C4 C21 P2 112.9(6) . . ? C13 C22 P1 115.9(5) . . ? C24 C23 C26 106.3(8) . . ? C24 C23 C15 112.4(7) . . ? C26 C23 C15 111.1(7) . . ? C24 C23 C25 107.9(8) . . ? C26 C23 C25 110.2(8) . . ? C15 C23 C25 108.9(7) . . ? C32 C27 C28 119.0(9) . . ? C32 C27 P2 121.0(7) . . ? C28 C27 P2 119.9(8) . . ? C29 C28 C27 121.7(11) . . ? C30 C29 C28 118.3(10) . . ? C29 C30 C31 120.6(11) . . ? C30 C31 C32 121.1(12) . . ? C27 C32 C31 119.2(9) . . ? C34 C33 C38 120.7(9) . . ? C34 C33 P2 120.5(6) . . ? C38 C33 P2 118.5(8) . . ? C33 C34 C35 120.2(7) . . ? C36 C35 C34 118.3(10) . . ? C35 C36 C37 121.0(10) . . ? C38 C37 C36 119.7(8) . . ? C37 C38 C33 120.1(10) . . ? C40 C39 C44 119.9(8) . . ? C40 C39 P2 119.5(7) . . ? C44 C39 P2 120.3(7) . . ? C41 C40 C39 120.7(10) . . ? C42 C41 C40 119.9(10) . . ? C41 C42 C43 121.1(9) . . ? C44 C43 C42 119.3(10) . . ? C43 C44 C39 119.1(10) . . ? C46 C45 C50 120.8(9) . . ? C46 C45 P1 119.9(6) . . ? C50 C45 P1 119.3(8) . . ? C45 C46 C47 119.6(8) . . ? C48 C47 C46 118.9(11) . . ? C49 C48 C47 121.3(11) . . ? C48 C49 C50 121.0(9) . . ? C49 C50 C45 118.4(10) . . ? C56 C51 C52 120.2(7) . . ? C56 C51 P1 122.9(6) . . ? C52 C51 P1 116.8(6) . . ? C53 C52 C51 119.2(9) . . ? C54 C53 C52 120.6(9) . . ? C53 C54 C55 120.6(9) . . ? C54 C55 C56 120.4(9) . . ? C51 C56 C55 118.9(9) . . ? C62 C57 C58 119.7(8) . . ? C62 C57 P1 119.7(6) . . ? C58 C57 P1 120.6(7) . . ? C59 C58 C57 120.1(9) . . ? C58 C59 C60 119.7(8) . . ? C61 C60 C59 121.4(9) . . ? C60 C61 C62 119.0(10) . . ? C57 C62 C61 120.0(8) . . ? N3 C63 C64 178.6(15) . . ? N4 C65 C66 174.8(18) . . ? C67A O3A C70A 146(2) . . ? C68A C67A C69A 107(2) . . ? C68A C67A O3A 113(3) . . ? C69A C67A O3A 112(2) . . ? C71A C70A O3A 105(2) . . ? C71B C71A C70A 140(4) 1_556 . ? C67B O3B C70B 159(3) . . ? C69B C67B O3B 108(3) . . ? C69B C67B C68B 101(4) . . ? O3B C67B C68B 71.7(18) . . ? C67B C69B C68C 136(4) . 2_665 ? C72B C70B C71B 128(5) . . ? C72B C70B O3B 141(5) . . ? C71B C70B O3B 87(3) . . ? C71A C71B C70B 153(5) 1_554 . ? C70C O3C O3C 87(10) 2_665 2_665 ? C70C O3C C70C 119(9) 2_665 . ? O3C O3C C70C 32(4) 2_665 . ? C70C O3C C67C 11(9) 2_665 . ? O3C O3C C67C 85(6) 2_665 . ? C70C O3C C67C 117(5) . . ? C70C O3C C71C 41(8) 2_665 2_665 ? O3C O3C C71C 98(6) 2_665 2_665 ? C70C O3C C71C 122(4) . 2_665 ? C67C O3C C71C 52(4) . 2_665 ? C70C O3C C67C 141(10) 2_665 2_665 ? O3C O3C C67C 54(4) 2_665 2_665 ? C70C O3C C67C 23(4) . 2_665 ? C67C O3C C67C 140(4) . 2_665 ? C71C O3C C67C 127(5) 2_665 2_665 ? C70C C67C C72C 101(10) 2_665 2_665 ? C70C C67C C71C 62(7) 2_665 2_665 ? C72C C67C C71C 144(10) 2_665 2_665 ? C70C C67C C68C 89(9) 2_665 . ? C72C C67C C68C 114(10) 2_665 . ? C71C C67C C68C 40(4) 2_665 . ? C70C C67C C69C 102(9) 2_665 . ? C72C C67C C69C 17(9) 2_665 . ? C71C C67C C69C 129(6) 2_665 . ? C68C C67C C69C 97(4) . . ? C70C C67C O3C 10(8) 2_665 . ? C72C C67C O3C 92(9) 2_665 . ? C71C C67C O3C 72(5) 2_665 . ? C68C C67C O3C 97(4) . . ? C69C C67C O3C 96(4) . . ? C70C C67C O3C 43(8) 2_665 2_665 ? C72C C67C O3C 104(9) 2_665 2_665 ? C71C C67C O3C 86(4) 2_665 2_665 ? C68C C67C O3C 124(5) . 2_665 ? C69C C67C O3C 117(5) . 2_665 ? O3C C67C O3C 40(4) . 2_665 ? C71C C68C C67C 72(6) 2_665 . ? C71C C68C C70C 53(5) 2_665 2_665 ? C67C C68C C70C 30(4) . 2_665 ? C71C C68C C69B 138(9) 2_665 2_665 ? C67C C68C C69B 100(4) . 2_665 ? C70C C68C C69B 100(5) 2_665 2_665 ? C72C C69C C67C 26(10) 2_665 . ? C72C C69C C70C 35(10) 2_665 2_665 ? C67C C69C C70C 26(4) . 2_665 ? O3C C70C C67C 160(10) 2_665 2_665 ? O3C C70C C71C 117(10) 2_665 . ? C67C C70C C71C 84(9) 2_665 . ? O3C C70C C72C 119(10) 2_665 . ? C67C C70C C72C 43(8) 2_665 . ? C71C C70C C72C 119(5) . . ? O3C C70C O3C 61(9) 2_665 . ? C67C C70C O3C 113(10) 2_665 . ? C71C C70C O3C 116(5) . . ? C72C C70C O3C 113(4) . . ? O3C C70C C68C 135(10) 2_665 2_665 ? C67C C70C C68C 61(7) 2_665 2_665 ? C71C C70C C68C 37(4) . 2_665 ? C72C C70C C68C 84(5) . 2_665 ? O3C C70C C68C 150(7) . 2_665 ? O3C C70C C69C 114(10) 2_665 2_665 ? C67C C70C C69C 52(7) 2_665 2_665 ? C71C C70C C69C 115(5) . 2_665 ? C72C C70C C69C 16(6) . 2_665 ? O3C C70C C69C 124(6) . 2_665 ? C68C C70C C69C 77(4) 2_665 2_665 ? O3C C70C C70C 40(6) 2_665 2_665 ? C67C C70C C70C 132(10) 2_665 2_665 ? C71C C70C C70C 120(7) . 2_665 ? C72C C70C C70C 119(6) . 2_665 ? O3C C70C C70C 20(3) . 2_665 ? C68C C70C C70C 157(8) 2_665 2_665 ? C69C C70C C70C 125(7) 2_665 2_665 ? C68C C71C C70C 90(7) 2_665 . ? C68C C71C C67C 68(6) 2_665 2_665 ? C70C C71C C67C 34(4) . 2_665 ? C68C C71C O3C 104(8) 2_665 2_665 ? C70C C71C O3C 22(4) . 2_665 ? C67C C71C O3C 57(4) 2_665 2_665 ? C69C C72C C67C 137(10) 2_665 2_665 ? C69C C72C C70C 129(10) 2_665 . ? C67C C72C C70C 37(5) 2_665 . ? #=========================================== #===END #=========================================== data_5 _database_code_CSD 158147 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; C62 H62 N2 Ni O2 P2 2+, (Cl-)2, 6(C D Cl3) ; _chemical_formula_sum 'C68 H62 Cl20 D6 N2 Ni O2 P2' _chemical_formula_weight 1780.93 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' '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' 'D' 'D' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 13.410(8) _cell_length_b 13.047(8) _cell_length_c 45.995(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.39(4) _cell_angle_gamma 90.00 _cell_volume 8033(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.40 _cell_measurement_theta_max 13.75 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3616 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rikagu AFC7S diffractometer' _diffrn_measurement_method 2\q/\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9014 _diffrn_reflns_av_R_equivalents 0.1167 _diffrn_reflns_av_sigmaI/netI 0.4972 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 21.00 _reflns_number_total 8439 _reflns_number_gt 2036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993a) ; _computing_cell_refinement ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993a) ; _computing_data_reduction ; TEXSAN PROCESS (Molecular Structure Corporation 1993b) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0806P)^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 calculated _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8439 _refine_ls_number_parameters 526 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.4126 _refine_ls_R_factor_gt 0.1524 _refine_ls_R_factor_obs 0.1524 _refine_ls_wR_factor_ref 0.3423 _refine_ls_wR_factor_all 0.3423 _refine_ls_wR_factor_obs 0.2567 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_goodness_of_fit_all 0.876 _refine_ls_restrained_S_all 0.875 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.002 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.690 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.125 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni -0.0526(3) 0.0953(3) -0.03284(7) 0.0431(10) Uani 1 d . . . Cl1 Cl -0.3625(5) -0.4189(5) -0.15592(16) 0.065(2) Uani 1 d . . . Cl2 Cl -0.1854(5) 0.1049(5) 0.13227(14) 0.055(2) Uani 1 d . . . Cl3 Cl -0.3536(8) -0.0922(8) -0.30646(19) 0.122(4) Uani 1 d . . . Cl4 Cl -0.4944(8) -0.0436(7) -0.2635(2) 0.120(4) Uani 1 d . . . Cl5 Cl -0.3830(8) 0.1154(8) -0.2893(2) 0.125(4) Uani 1 d . . . Cl6 Cl -0.3272(8) 0.2918(8) -0.1920(2) 0.132(4) Uani 1 d . . . Cl7 Cl -0.4492(8) 0.2840(8) -0.1435(2) 0.137(4) Uani 1 d . . . Cl8 Cl -0.2395(7) 0.2598(8) -0.1351(2) 0.120(4) Uani 1 d . . . Cl9 Cl -0.0912(6) 0.2778(6) 0.19403(17) 0.080(3) Uani 1 d . . . Cl10 Cl -0.2362(6) 0.1669(6) 0.22541(17) 0.081(3) Uani 1 d . . . Cl11 Cl -0.0502(8) 0.0771(7) 0.2156(2) 0.131(4) Uani 1 d . . . Cl12 Cl -0.5856(8) 0.3639(9) 0.0688(2) 0.157(5) Uani 1 d . . . Cl13 Cl -0.6557(8) 0.5675(8) 0.0735(2) 0.143(4) Uani 1 d . . . Cl14 Cl -0.7931(7) 0.4018(8) 0.0717(3) 0.148(5) Uani 1 d . . . Cl15 Cl 0.3973(9) 0.2274(8) -0.0323(3) 0.185(6) Uani 1 d . . . Cl16 Cl 0.4294(10) 0.4367(10) -0.0281(3) 0.198(6) Uani 1 d . . . Cl17 Cl 0.2520(10) 0.3585(10) -0.0135(4) 0.247(9) Uani 1 d . . . Cl18 Cl 0.2979(7) 0.1732(7) -0.1167(2) 0.120(4) Uani 1 d . . . Cl19 Cl 0.0898(6) 0.2140(6) -0.12472(17) 0.078(3) Uani 1 d . . . Cl20 Cl 0.2084(9) 0.1881(7) -0.1736(2) 0.143(5) Uani 1 d . . . P1 P -0.2721(6) -0.1280(5) -0.18765(15) 0.047(2) Uani 1 d . . . P2 P -0.0757(5) 0.4418(5) 0.11286(15) 0.043(2) Uani 1 d . . . O1 O -0.1320(10) 0.1486(11) -0.0061(3) 0.036(4) Uiso 1 d . . . O2 O -0.1660(12) 0.0594(13) -0.0520(3) 0.055(5) Uiso 1 d . . . N1 N 0.0596(13) 0.1266(13) -0.0120(4) 0.029(5) Uiso 1 d . . . N2 N 0.0227(14) 0.0468(14) -0.0606(4) 0.039(6) Uiso 1 d . . . C1 C 0.0661(18) 0.1646(18) 0.0155(5) 0.045(7) Uiso 1 d . . . H1 H 0.1316(18) 0.1673(18) 0.0252(5) 0.054 Uiso 1 d R . . C2 C -0.0113(16) 0.1985(15) 0.0312(4) 0.017(6) Uiso 1 d . . . C3 C 0.0037(19) 0.2382(18) 0.0578(5) 0.049(8) Uiso 1 d . . . H3 H 0.0714(19) 0.2540(18) 0.0643(5) 0.058 Uiso 1 d R . . C4 C -0.0671(17) 0.2659(17) 0.0762(5) 0.033(7) Uiso 1 d . . . C5 C -0.1636(17) 0.2601(16) 0.0650(5) 0.032(7) Uiso 1 d . . . H5 H -0.2158(17) 0.2809(16) 0.0772(5) 0.038 Uiso 1 d R . . C6 C -0.1904(18) 0.2275(19) 0.0372(5) 0.046(8) Uiso 1 d . . . C7 C -0.1112(17) 0.1850(17) 0.0212(5) 0.032(7) Uiso 1 d . . . C8 C 0.0047(17) -0.0033(17) -0.0852(5) 0.036(7) Uiso 1 d . . . H8 H 0.0585(17) -0.0275(17) -0.0962(5) 0.043 Uiso 1 d R . . C9 C -0.0975(16) -0.0244(16) -0.0937(5) 0.027(6) Uiso 1 d . . . C10 C -0.1035(16) -0.0838(16) -0.1195(4) 0.028(6) Uiso 1 d . . . H10 H -0.0457(16) -0.0976(16) -0.1303(4) 0.033 Uiso 1 d R . . C11 C -0.1945(18) -0.1186(19) -0.1286(5) 0.043(7) Uiso 1 d . . . C12 C -0.2770(18) -0.0912(18) -0.1142(5) 0.040(7) Uiso 1 d . . . H12 H -0.3417(18) -0.1159(18) -0.1209(5) 0.048 Uiso 1 d R . . C13 C -0.2652(19) -0.0324(19) -0.0896(5) 0.046(8) Uiso 1 d . . . C14 C -0.1748(18) 0.0010(18) -0.0765(5) 0.036(7) Uiso 1 d . . . C15 C -0.364(2) -0.012(2) -0.0734(6) 0.059(9) Uiso 1 d . . . C16 C -0.4609(18) -0.052(2) -0.0879(5) 0.071(9) Uiso 1 d . . . H16A H -0.5153(18) -0.038(2) -0.0758(5) 0.106 Uiso 1 d R . . H16B H -0.4726(18) -0.017(2) -0.1062(5) 0.106 Uiso 1 d R . . H16C H -0.4559(18) -0.124(2) -0.0913(5) 0.106 Uiso 1 d R . . C17 C -0.3775(18) 0.0982(18) -0.0678(5) 0.054(8) Uiso 1 d . . . H17A H -0.3167(18) 0.1234(18) -0.0583(5) 0.081 Uiso 1 d R . . H17B H -0.3895(18) 0.1325(18) -0.0861(5) 0.081 Uiso 1 d R . . H17C H -0.4321(18) 0.1110(18) -0.0557(5) 0.081 Uiso 1 d R . . C18 C -0.3529(18) -0.060(2) -0.0435(5) 0.065(9) Uiso 1 d . . . H18A H -0.2922(18) -0.037(2) -0.0336(5) 0.098 Uiso 1 d R . . H18B H -0.4088(18) -0.041(2) -0.0326(5) 0.098 Uiso 1 d R . . H18C H -0.3510(18) -0.134(2) -0.0454(5) 0.098 Uiso 1 d R . . C19 C -0.2126(19) -0.1813(19) -0.1558(5) 0.057(8) Uiso 1 d . . . H19A H -0.1473(19) -0.2021(19) -0.1609(5) 0.068 Uiso 1 d R . . H19B H -0.2482(19) -0.2421(19) -0.1508(5) 0.068 Uiso 1 d R . . C20 C -0.2080(19) -0.027(2) -0.2018(6) 0.054(8) Uiso 1 d . . . C21 C -0.1541(17) 0.0432(18) -0.1824(5) 0.042(7) Uiso 1 d . . . H21 H -0.1534(17) 0.0301(18) -0.1619(5) 0.051 Uiso 1 d R . . C22 C -0.1078(19) 0.134(2) -0.1930(6) 0.064(9) Uiso 1 d . . . H22 H -0.0870(19) 0.189(2) -0.1801(6) 0.077 Uiso 1 d R . . C23 C -0.098(2) 0.140(2) -0.2233(6) 0.081(10) Uiso 1 d . . . H23 H -0.049(2) 0.185(2) -0.2310(6) 0.097 Uiso 1 d R . . C24 C -0.1505(19) 0.076(2) -0.2426(6) 0.063(9) Uiso 1 d . . . H24 H -0.1552(19) 0.087(2) -0.2632(6) 0.076 Uiso 1 d R . . C25 C -0.2038(18) -0.014(2) -0.2299(6) 0.052(8) Uiso 1 d . . . H25 H -0.2392(18) -0.063(2) -0.2423(6) 0.063 Uiso 1 d R . . C26 C -0.3942(18) -0.092(2) -0.1816(5) 0.046(7) Uiso 1 d . . . C27 C -0.421(2) 0.016(2) -0.1827(6) 0.065(9) Uiso 1 d . . . H27 H -0.372(2) 0.067(2) -0.1865(6) 0.078 Uiso 1 d R . . C28 C -0.5193(17) 0.0387(18) -0.1797(5) 0.033(7) Uiso 1 d . . . H28 H -0.5465(17) 0.1036(18) -0.1860(5) 0.040 Uiso 1 d R . . C29 C -0.584(2) -0.031(2) -0.1670(5) 0.056(8) Uiso 1 d . . . H29 H -0.648(2) -0.009(2) -0.1606(5) 0.067 Uiso 1 d R . . C30 C -0.5561(18) -0.1361(19) -0.1640(5) 0.044(7) Uiso 1 d . . . H30 H -0.6023(18) -0.1863(19) -0.1576(5) 0.052 Uiso 1 d R . . C31 C -0.4617(19) -0.158(2) -0.1703(5) 0.059(9) Uiso 1 d . . . H31 H -0.4390(19) -0.226(2) -0.1657(5) 0.071 Uiso 1 d R . . C32 C -0.271(2) -0.224(2) -0.2147(6) 0.064(9) Uiso 1 d . . . C33 C -0.1857(19) -0.2638(19) -0.2224(5) 0.051(8) Uiso 1 d . . . H33 H -0.1235(19) -0.2350(19) -0.2150(5) 0.061 Uiso 1 d R . . C34 C -0.191(2) -0.344(2) -0.2438(6) 0.072(9) Uiso 1 d . . . H34 H -0.132(2) -0.382(2) -0.2473(6) 0.086 Uiso 1 d R . . C35 C -0.2761(17) -0.3702(17) -0.2576(5) 0.034(7) Uiso 1 d . . . H35 H -0.2754(17) -0.4197(17) -0.2730(5) 0.040 Uiso 1 d R . . C36 C -0.366(2) -0.328(2) -0.2529(6) 0.076(10) Uiso 1 d . . . H36 H -0.426(2) -0.348(2) -0.2637(6) 0.091 Uiso 1 d R . . C37 C -0.3692(19) -0.2535(18) -0.2297(5) 0.048(8) Uiso 1 d . . . H37 H -0.4294(19) -0.2199(18) -0.2245(5) 0.058 Uiso 1 d R . . C38 C -0.3006(17) 0.2203(18) 0.0251(5) 0.035(7) Uiso 1 d . . . C39 C -0.3668(18) 0.271(2) 0.0474(5) 0.069(9) Uiso 1 d . . . H39A H -0.4362(18) 0.267(2) 0.0410(5) 0.104 Uiso 1 d R . . H39B H -0.3565(18) 0.235(2) 0.0656(5) 0.104 Uiso 1 d R . . H39C H -0.3473(18) 0.341(2) 0.0500(5) 0.104 Uiso 1 d R . . C40 C -0.309(2) 0.287(2) -0.0012(6) 0.086(11) Uiso 1 d . . . H40A H -0.375(2) 0.286(2) -0.0105(6) 0.130 Uiso 1 d R . . H40B H -0.292(2) 0.355(2) 0.0046(6) 0.130 Uiso 1 d R . . H40C H -0.262(2) 0.262(2) -0.0146(6) 0.130 Uiso 1 d R . . C41 C -0.337(2) 0.119(2) 0.0192(6) 0.088(11) Uiso 1 d . . . H41A H -0.405(2) 0.115(2) 0.0116(6) 0.132 Uiso 1 d R . . H41B H -0.295(2) 0.085(2) 0.0062(6) 0.132 Uiso 1 d R . . H41C H -0.331(2) 0.087(2) 0.0380(6) 0.132 Uiso 1 d R . . C42 C -0.0473(14) 0.3133(14) 0.1068(4) 0.016(6) Uiso 1 d . . . H42A H -0.0826(14) 0.2726(14) 0.1202(4) 0.019 Uiso 1 d R . . H42B H 0.0227(14) 0.3042(14) 0.1118(4) 0.019 Uiso 1 d R . . C43 C -0.0176(16) 0.4764(16) 0.1471(5) 0.024(6) Uiso 1 d . . . C44 C 0.0831(18) 0.4625(19) 0.1560(5) 0.048(8) Uiso 1 d . . . H44 H 0.1241(18) 0.4246(19) 0.1434(5) 0.057 Uiso 1 d R . . C45 C 0.122(2) 0.495(2) 0.1796(6) 0.062(9) Uiso 1 d . . . H45 H 0.191(2) 0.481(2) 0.1847(6) 0.074 Uiso 1 d R . . C46 C 0.073(2) 0.5440(19) 0.1987(6) 0.057(8) Uiso 1 d . . . H46 H 0.108(2) 0.5671(19) 0.2162(6) 0.068 Uiso 1 d R . . C47 C -0.0297(17) 0.5644(17) 0.1938(5) 0.037(7) Uiso 1 d . . . H47 H -0.0678(17) 0.5964(17) 0.2083(5) 0.044 Uiso 1 d R . . C48 C -0.078(2) 0.5307(19) 0.1661(5) 0.059(9) Uiso 1 d . . . H48 H -0.145(2) 0.5504(19) 0.1600(5) 0.071 Uiso 1 d R . . C49 C -0.2053(15) 0.4535(16) 0.1120(4) 0.023(6) Uiso 1 d . . . C50 C -0.2629(19) 0.380(2) 0.1268(5) 0.057(8) Uiso 1 d . . . H50 H -0.2309(19) 0.322(2) 0.1360(5) 0.068 Uiso 1 d R . . C51 C -0.3676(18) 0.4004(19) 0.1285(5) 0.046(7) Uiso 1 d . . . H51 H -0.4103(18) 0.3478(19) 0.1354(5) 0.055 Uiso 1 d R . . C52 C -0.4071(19) 0.4936(19) 0.1191(5) 0.053(8) Uiso 1 d . . . H52 H -0.4743(19) 0.5114(19) 0.1231(5) 0.063 Uiso 1 d R . . C53 C -0.3505(18) 0.5653(19) 0.1045(5) 0.048(8) Uiso 1 d . . . H53 H -0.3791(18) 0.6216(19) 0.0934(5) 0.058 Uiso 1 d R . . C54 C -0.2531(19) 0.5430(19) 0.1058(5) 0.049(8) Uiso 1 d . . . H54 H -0.2094(19) 0.6003(19) 0.1035(5) 0.058 Uiso 1 d R . . C55 C -0.0298(18) 0.5182(18) 0.0841(5) 0.040(7) Uiso 1 d . . . C56 C -0.063(2) 0.505(2) 0.0572(6) 0.065(9) Uiso 1 d . . . H56 H -0.105(2) 0.448(2) 0.0524(6) 0.078 Uiso 1 d R . . C57 C -0.029(2) 0.571(2) 0.0353(6) 0.075(10) Uiso 1 d . . . H57 H -0.063(2) 0.569(2) 0.0163(6) 0.090 Uiso 1 d R . . C58 C 0.0394(18) 0.6366(19) 0.0406(5) 0.049(8) Uiso 1 d . . . H58 H 0.0663(18) 0.6739(19) 0.0249(5) 0.058 Uiso 1 d R . . C59 C 0.0797(16) 0.6560(17) 0.0698(5) 0.034(7) Uiso 1 d . . . H59 H 0.1253(16) 0.7109(17) 0.0747(5) 0.040 Uiso 1 d R . . C60 C 0.0417(18) 0.5921(19) 0.0909(6) 0.055(8) Uiso 1 d . . . H60 H 0.0717(18) 0.5949(19) 0.1103(6) 0.066 Uiso 1 d R . . C61 C 0.1499(18) 0.095(2) -0.0228(5) 0.056(8) Uiso 1 d . . . H61A H 0.1722(18) 0.032(2) -0.0139(5) 0.067 Uiso 1 d R . . H61B H 0.1992(18) 0.147(2) -0.0182(5) 0.067 Uiso 1 d R . . C62 C 0.1320(19) 0.081(2) -0.0551(6) 0.073(9) Uiso 1 d . . . H62A H 0.1409(19) 0.145(2) -0.0650(6) 0.087 Uiso 1 d R . . H62B H 0.1774(19) 0.032(2) -0.0620(6) 0.087 Uiso 1 d R . . C63 C -0.439(2) -0.006(2) -0.2954(7) 0.087(11) Uani 1 d U . . D63 D -0.4897 0.0008 -0.3108 0.104 Uiso 1 d R . . C64 C -0.337(2) 0.315(2) -0.1560(6) 0.073(10) Uani 1 d U . . D64 D -0.3302 0.3876 -0.1533 0.087 Uiso 1 d R . . C65 C -0.140(2) 0.156(2) 0.2022(7) 0.091(11) Uani 1 d U . . D65 D -0.1680 0.1270 0.1843 0.110 Uiso 1 d R . . C66 C -0.6719(18) 0.4283(18) 0.0844(5) 0.049(8) Uani 1 d U . . D66 D -0.6647 0.4208 0.1052 0.059 Uiso 1 d R . . C67 C 0.367(2) 0.333(3) -0.0130(7) 0.095(11) Uani 1 d U . . D67 D 0.3912 0.3245 0.0069 0.114 Uiso 1 d R . . C68 C 0.189(2) 0.155(2) -0.1373(6) 0.065(9) Uani 1 d U . . D68 D 0.1755 0.0827 -0.1368 0.078 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.044(2) 0.040(2) 0.046(2) -0.002(2) 0.0144(18) 0.005(2) Cl1 0.079(6) 0.021(4) 0.096(6) 0.005(4) 0.011(5) 0.004(4) Cl2 0.081(6) 0.028(4) 0.061(5) 0.008(4) 0.037(4) 0.003(4) Cl3 0.166(10) 0.121(9) 0.082(7) -0.005(7) 0.018(7) 0.038(8) Cl4 0.138(9) 0.083(7) 0.142(9) -0.001(7) 0.031(8) 0.015(7) Cl5 0.127(9) 0.107(8) 0.140(9) 0.003(7) -0.014(7) -0.008(7) Cl6 0.178(11) 0.106(8) 0.112(9) 0.016(7) 0.004(8) -0.004(8) Cl7 0.133(10) 0.096(8) 0.186(11) -0.031(8) 0.035(8) -0.009(7) Cl8 0.099(8) 0.140(9) 0.119(8) -0.036(8) 0.001(7) 0.008(7) Cl9 0.123(8) 0.039(5) 0.080(6) -0.009(5) 0.014(5) -0.005(5) Cl10 0.080(6) 0.083(6) 0.082(6) 0.001(5) 0.019(5) -0.003(5) Cl11 0.126(9) 0.091(8) 0.181(11) 0.051(8) 0.053(8) 0.049(7) Cl12 0.117(9) 0.181(12) 0.173(11) -0.089(10) 0.016(8) 0.048(8) Cl13 0.136(10) 0.105(9) 0.185(12) 0.021(8) -0.011(8) -0.023(8) Cl14 0.081(8) 0.123(9) 0.243(14) -0.032(10) 0.032(8) -0.012(7) Cl15 0.140(10) 0.088(8) 0.337(18) -0.051(11) 0.104(11) 0.011(8) Cl16 0.203(14) 0.133(11) 0.257(16) -0.016(11) 0.010(12) -0.059(11) Cl17 0.153(13) 0.145(12) 0.46(3) 0.005(15) 0.136(15) 0.022(10) Cl18 0.100(8) 0.081(7) 0.185(11) -0.014(7) 0.049(8) -0.007(6) Cl19 0.111(7) 0.048(5) 0.080(6) 0.004(5) 0.044(5) 0.000(5) Cl20 0.246(13) 0.087(8) 0.106(8) 0.012(6) 0.102(9) 0.051(8) P1 0.068(6) 0.036(5) 0.038(5) -0.007(4) 0.019(4) -0.004(4) P2 0.045(5) 0.044(5) 0.042(5) 0.009(4) 0.013(4) -0.006(4) C63 0.094(14) 0.082(14) 0.085(14) 0.006(9) 0.001(9) -0.002(9) C64 0.075(12) 0.064(12) 0.081(13) -0.010(9) 0.011(9) 0.000(9) C65 0.093(14) 0.093(14) 0.089(14) 0.000(9) 0.009(9) 0.006(9) C66 0.051(11) 0.052(11) 0.044(11) 0.011(9) -0.001(8) 0.017(9) C67 0.093(14) 0.093(14) 0.099(14) 0.003(9) 0.005(9) 0.006(10) C68 0.063(12) 0.059(12) 0.074(12) 0.014(9) 0.014(9) 0.005(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 Ni O2 1.774(16) . ? Ni N1 1.784(17) . ? Ni N2 1.789(19) . ? Ni O1 1.813(14) . ? Cl3 C63 1.70(3) . ? Cl4 C63 1.76(3) . ? Cl5 C63 1.76(3) . ? Cl6 C64 1.70(3) . ? Cl7 C64 1.68(3) . ? Cl8 C64 1.74(3) . ? Cl9 C65 1.77(3) . ? Cl10 C65 1.72(3) . ? Cl11 C65 1.68(3) . ? Cl12 C66 1.63(2) . ? Cl13 C66 1.90(3) . ? Cl14 C66 1.73(2) . ? Cl15 C67 1.71(3) . ? Cl16 C67 1.75(3) . ? Cl17 C67 1.57(3) . ? Cl18 C68 1.71(3) . ? Cl19 C68 1.67(3) . ? Cl20 C68 1.76(3) . ? P1 C20 1.73(3) . ? P1 C26 1.74(2) . ? P1 C19 1.77(2) . ? P1 C32 1.77(3) . ? P2 C42 1.746(19) . ? P2 C49 1.74(2) . ? P2 C43 1.78(2) . ? P2 C55 1.79(2) . ? O1 C7 1.36(2) . ? O2 C14 1.36(2) . ? N1 C1 1.36(2) . ? N1 C61 1.40(3) . ? N2 C8 1.32(2) . ? N2 C62 1.54(3) . ? C1 C2 1.37(3) . ? C2 C3 1.33(3) . ? C2 C7 1.40(3) . ? C3 C4 1.36(3) . ? C4 C5 1.37(3) . ? C4 C42 1.55(3) . ? C5 C6 1.37(3) . ? C6 C7 1.44(3) . ? C6 C38 1.55(3) . ? C8 C9 1.43(3) . ? C9 C14 1.38(3) . ? C9 C10 1.42(3) . ? C10 C11 1.35(3) . ? C11 C12 1.37(3) . ? C11 C19 1.50(3) . ? C12 C13 1.37(3) . ? C13 C14 1.39(3) . ? C13 C15 1.58(3) . ? C15 C17 1.47(3) . ? C15 C16 1.52(3) . ? C15 C18 1.52(3) . ? C20 C25 1.30(3) . ? C20 C21 1.44(3) . ? C21 C22 1.44(3) . ? C22 C23 1.41(3) . ? C23 C24 1.38(3) . ? C24 C25 1.51(3) . ? C26 C31 1.38(3) . ? C26 C27 1.46(3) . ? C27 C28 1.36(3) . ? C28 C29 1.41(3) . ? C29 C30 1.43(3) . ? C30 C31 1.35(3) . ? C32 C33 1.32(3) . ? C32 C37 1.50(3) . ? C33 C34 1.43(3) . ? C34 C35 1.31(3) . ? C35 C36 1.35(3) . ? C36 C37 1.44(3) . ? C38 C41 1.43(3) . ? C38 C40 1.49(3) . ? C38 C39 1.54(3) . ? C43 C48 1.41(3) . ? C43 C44 1.40(3) . ? C44 C45 1.25(3) . ? C45 C46 1.30(3) . ? C46 C47 1.40(3) . ? C47 C48 1.46(3) . ? C49 C54 1.35(3) . ? C49 C50 1.43(3) . ? C50 C51 1.44(3) . ? C51 C52 1.39(3) . ? C52 C53 1.40(3) . ? C53 C54 1.34(3) . ? C55 C56 1.30(3) . ? C55 C60 1.38(3) . ? C56 C57 1.42(3) . ? C57 C58 1.27(3) . ? C58 C59 1.44(3) . ? C59 C60 1.40(3) . ? C61 C62 1.50(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni N1 176.7(8) . . ? O2 Ni N2 93.2(8) . . ? N1 Ni N2 88.3(8) . . ? O2 Ni O1 85.3(7) . . ? N1 Ni O1 93.3(7) . . ? N2 Ni O1 177.2(8) . . ? C20 P1 C26 110.3(13) . . ? C20 P1 C19 113.9(13) . . ? C26 P1 C19 110.8(12) . . ? C20 P1 C32 104.6(13) . . ? C26 P1 C32 110.7(13) . . ? C19 P1 C32 106.2(12) . . ? C42 P2 C49 107.9(10) . . ? C42 P2 C43 107.3(10) . . ? C49 P2 C43 112.5(10) . . ? C42 P2 C55 109.2(11) . . ? C49 P2 C55 108.7(11) . . ? C43 P2 C55 111.2(11) . . ? C7 O1 Ni 131.8(14) . . ? C14 O2 Ni 126.2(15) . . ? C1 N1 C61 115.5(19) . . ? C1 N1 Ni 126.2(16) . . ? C61 N1 Ni 117.5(15) . . ? C8 N2 C62 114(2) . . ? C8 N2 Ni 134.9(18) . . ? C62 N2 Ni 110.6(15) . . ? N1 C1 C2 127(2) . . ? C3 C2 C1 122(2) . . ? C3 C2 C7 116(2) . . ? C1 C2 C7 122(2) . . ? C2 C3 C4 127(3) . . ? C3 C4 C5 116(2) . . ? C3 C4 C42 126(2) . . ? C5 C4 C42 118(2) . . ? C4 C5 C6 124(2) . . ? C5 C6 C7 116(2) . . ? C5 C6 C38 123(2) . . ? C7 C6 C38 121(2) . . ? O1 C7 C2 119(2) . . ? O1 C7 C6 119(2) . . ? C2 C7 C6 120(2) . . ? N2 C8 C9 117(2) . . ? C14 C9 C10 127(2) . . ? C14 C9 C8 123(2) . . ? C10 C9 C8 110(2) . . ? C11 C10 C9 117(2) . . ? C10 C11 C12 120(2) . . ? C10 C11 C19 123(2) . . ? C12 C11 C19 117(2) . . ? C13 C12 C11 119(2) . . ? C12 C13 C14 126(2) . . ? C12 C13 C15 115(2) . . ? C14 C13 C15 118(2) . . ? O2 C14 C9 125(2) . . ? O2 C14 C13 124(2) . . ? C9 C14 C13 110(2) . . ? C17 C15 C16 108(2) . . ? C17 C15 C18 105(2) . . ? C16 C15 C18 107(2) . . ? C17 C15 C13 111(2) . . ? C16 C15 C13 117(2) . . ? C18 C15 C13 108(2) . . ? C11 C19 P1 121.2(18) . . ? C25 C20 C21 119(3) . . ? C25 C20 P1 121(2) . . ? C21 C20 P1 120(2) . . ? C22 C21 C20 122(2) . . ? C23 C22 C21 117(3) . . ? C24 C23 C22 121(3) . . ? C23 C24 C25 117(3) . . ? C20 C25 C24 122(3) . . ? C31 C26 C27 117(3) . . ? C31 C26 P1 122(2) . . ? C27 C26 P1 119(2) . . ? C28 C27 C26 117(3) . . ? C27 C28 C29 122(2) . . ? C28 C29 C30 120(3) . . ? C31 C30 C29 116(3) . . ? C30 C31 C26 126(3) . . ? C33 C32 C37 122(3) . . ? C33 C32 P1 121(2) . . ? C37 C32 P1 117(2) . . ? C32 C33 C34 117(3) . . ? C35 C34 C33 122(3) . . ? C34 C35 C36 125(3) . . ? C35 C36 C37 117(3) . . ? C36 C37 C32 116(2) . . ? C41 C38 C40 112(2) . . ? C41 C38 C6 116(2) . . ? C40 C38 C6 106(2) . . ? C41 C38 C39 108(2) . . ? C40 C38 C39 106(2) . . ? C6 C38 C39 108(2) . . ? C4 C42 P2 120.2(14) . . ? C48 C43 C44 118(2) . . ? C48 C43 P2 116.0(18) . . ? C44 C43 P2 126.2(19) . . ? C45 C44 C43 124(3) . . ? C44 C45 C46 124(3) . . ? C45 C46 C47 121(3) . . ? C46 C47 C48 117(2) . . ? C43 C48 C47 117(2) . . ? C54 C49 C50 115(2) . . ? C54 C49 P2 122.6(18) . . ? C50 C49 P2 119.8(18) . . ? C51 C50 C49 117(2) . . ? C52 C51 C50 120(2) . . ? C51 C52 C53 122(3) . . ? C54 C53 C52 113(3) . . ? C53 C54 C49 130(3) . . ? C56 C55 C60 120(3) . . ? C56 C55 P2 121(2) . . ? C60 C55 P2 119(2) . . ? C55 C56 C57 119(3) . . ? C58 C57 C56 122(3) . . ? C57 C58 C59 122(3) . . ? C60 C59 C58 114(2) . . ? C55 C60 C59 123(2) . . ? N1 C61 C62 107(2) . . ? C61 C62 N2 107(2) . . ? Cl3 C63 Cl5 111.0(18) . . ? Cl3 C63 Cl4 113.0(18) . . ? Cl5 C63 Cl4 108.3(17) . . ? Cl7 C64 Cl8 111.8(17) . . ? Cl7 C64 Cl6 114.5(17) . . ? Cl8 C64 Cl6 111.2(17) . . ? Cl11 C65 Cl10 111.9(18) . . ? Cl11 C65 Cl9 110.9(17) . . ? Cl10 C65 Cl9 110.8(17) . . ? Cl12 C66 Cl14 115.2(16) . . ? Cl12 C66 Cl13 106.4(14) . . ? Cl14 C66 Cl13 102.9(13) . . ? Cl17 C67 Cl15 115(2) . . ? Cl17 C67 Cl16 109(2) . . ? Cl15 C67 Cl16 106.4(19) . . ? Cl18 C68 Cl19 114.5(17) . . ? Cl18 C68 Cl20 108.9(16) . . ? Cl19 C68 Cl20 112.4(16) . . ? #===END OF CIF #=====================