Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Evamarie Hey-Hawkins' _publ_contact_author_address ; Faculty of Chemistry and Mineralogy, Universitat Leipzig Department of Inorganic Chemistry Johannisallee 29 Leipzig 04103 Germany ; _publ_contact_author_email HEY@RZ.UNI-LEIPZIG.DE _publ_section_title ; Oligodentate P,N Ligands: N,N,N',N'-Tetrakis(diphenylphosphanyl)- 1,3-diaminobenzene Complexes of Rhodium, Nickel and PalladiumFelicite ; loop_ _publ_author_name 'Peter Lonnecke' 'Elena V.Novikova' 'Gennadii P.Belov' 'Evamarie Hey-Hawkins' data_c1231fin_squeeze _database_code_depnum_ccdc_archive 'CCDC 274893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H52 Cl12 N2 P4 Pd2' _chemical_formula_weight 1539.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' P P 0.1023 0.0942 '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' 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' _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 17.592(2) _cell_length_b 22.333(3) _cell_length_c 16.920(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.097(2) _cell_angle_gamma 90.00 _cell_volume 6610.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 1018 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.37 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_absorpt_coefficient_mu 1.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_crystal_preparation ; To avoid loss of CH2Cl2 the crystal was encapsulated with epoxy resin and mounted on a glass needle ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'ccd area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42507 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 29.31 _reflns_number_total 16184 _reflns_number_gt 11258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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. 3 solvent molecules removed from the data with SQUEEZE ; _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^)+(0.0671P)^2^+5.2071P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16184 _refine_ls_number_parameters 617 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.049 _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 Pd1 Pd 0.322474(16) 0.138074(12) 0.525480(18) 0.04374(9) Uani 1 1 d . A . Pd2 Pd 0.242329(16) -0.266594(11) 0.757425(15) 0.03778(8) Uani 1 1 d . . . Cl1 Cl 0.25345(8) 0.16796(7) 0.40531(9) 0.0866(4) Uani 1 1 d . . . Cl2 Cl 0.43605(6) 0.18529(5) 0.50133(9) 0.0713(3) Uani 1 1 d . . . Cl3 Cl 0.14926(7) -0.33784(5) 0.78476(6) 0.0573(3) Uani 1 1 d . . . Cl4 Cl 0.33530(7) -0.33661(5) 0.72872(6) 0.0573(3) Uani 1 1 d . . . P1 P 0.23044(5) 0.09038(4) 0.57838(5) 0.03639(19) Uani 1 1 d . A . P2 P 0.37357(5) 0.09685(4) 0.63748(6) 0.0410(2) Uani 1 1 d . . . P3 P 0.17714(5) -0.18712(4) 0.78919(5) 0.03776(19) Uani 1 1 d . . . P4 P 0.30716(5) -0.18633(4) 0.72786(5) 0.03507(18) Uani 1 1 d . . . N1 N 0.29096(16) 0.06097(12) 0.65339(16) 0.0364(6) Uani 1 1 d . A . N2 N 0.24301(16) -0.13740(12) 0.76237(16) 0.0367(6) Uani 1 1 d . A . C1 C 0.17673(19) 0.03198(16) 0.5256(2) 0.0396(7) Uani 1 1 d D . . C2 C 0.1214(2) -0.00038(17) 0.5608(3) 0.0494(9) Uani 1 1 d D A . H2 H 0.1124 0.0076 0.6135 0.059 Uiso 1 1 calc R . . C3 C 0.0799(2) -0.04448(19) 0.5176(3) 0.0619(11) Uani 1 1 d D . . H3 H 0.0426 -0.0665 0.5411 0.074 Uiso 1 1 calc R A . C4 C 0.0932(3) -0.0560(2) 0.4404(3) 0.0679(13) Uani 1 1 d D A . H4 H 0.0644 -0.0857 0.4114 0.081 Uiso 1 1 calc R . . C5 C 0.1470(3) -0.0254(2) 0.4055(3) 0.0680(13) Uani 1 1 d D . . H5 H 0.1558 -0.0343 0.3529 0.082 Uiso 1 1 calc R A . C6 C 0.1896(2) 0.01955(19) 0.4477(2) 0.0550(10) Uani 1 1 d D A . H6 H 0.2266 0.0412 0.4235 0.066 Uiso 1 1 calc R . . C7 C 0.1625(2) 0.13887(17) 0.6193(2) 0.0473(9) Uani 1 1 d . . . C8 C 0.0899(3) 0.1478(2) 0.5796(3) 0.0641(12) Uani 1 1 d . A . H8 H 0.0738 0.1255 0.5338 0.077 Uiso 1 1 calc R . . C9 C 0.0415(3) 0.1899(2) 0.6080(4) 0.0872(18) Uani 1 1 d . . . H9 H -0.0079 0.1954 0.5819 0.105 Uiso 1 1 calc R A . C10 C 0.0650(4) 0.2234(3) 0.6735(4) 0.103(2) Uani 1 1 d . A . H10 H 0.0310 0.2509 0.6928 0.124 Uiso 1 1 calc R . . C11 C 0.1378(4) 0.2175(3) 0.7121(4) 0.0945(19) Uani 1 1 d . . . H11 H 0.1539 0.2418 0.7560 0.113 Uiso 1 1 calc R A . C12 C 0.1869(3) 0.1753(2) 0.6851(3) 0.0681(13) Uani 1 1 d . A . H12 H 0.2366 0.1710 0.7109 0.082 Uiso 1 1 calc R . . C13 C 0.4487(2) 0.04419(18) 0.6290(2) 0.0437(8) Uani 1 1 d . A . C14 C 0.4339(2) -0.01061(17) 0.5918(2) 0.0439(8) Uani 1 1 d . . . H14 H 0.3834 -0.0217 0.5737 0.053 Uiso 1 1 calc R A . C15 C 0.4944(3) -0.0490(2) 0.5813(3) 0.0596(11) Uani 1 1 d . A . H15 H 0.4850 -0.0865 0.5570 0.072 Uiso 1 1 calc R . . C16 C 0.5677(3) -0.0319(3) 0.6065(3) 0.0694(13) Uani 1 1 d . . . H16 H 0.6082 -0.0584 0.6006 0.083 Uiso 1 1 calc R A . C17 C 0.5829(3) 0.0226(3) 0.6400(3) 0.0747(14) Uani 1 1 d . A . H17 H 0.6338 0.0341 0.6551 0.090 Uiso 1 1 calc R . . C18 C 0.5241(2) 0.0610(2) 0.6520(3) 0.0621(11) Uani 1 1 d . . . H18 H 0.5348 0.0986 0.6756 0.075 Uiso 1 1 calc R A . C19 C 0.4076(4) 0.1357(3) 0.7294(4) 0.0403(16) Uiso 0.580(11) 1 d PD A 1 C20 C 0.4361(4) 0.1049(4) 0.7977(5) 0.065(2) Uiso 0.580(11) 1 d PD A 1 H20 H 0.4405 0.0630 0.7966 0.079 Uiso 0.580(11) 1 calc PR A 1 C21 C 0.4582(6) 0.1361(5) 0.8680(6) 0.098(4) Uiso 0.580(11) 1 d PD A 1 H21 H 0.4788 0.1173 0.9152 0.118 Uiso 0.580(11) 1 calc PR A 1 C22 C 0.4472(8) 0.1969(6) 0.8618(8) 0.106(5) Uiso 0.580(11) 1 d PD A 1 H22 H 0.4594 0.2179 0.9096 0.127 Uiso 0.580(11) 1 calc PR A 1 C23 C 0.4229(8) 0.2306(5) 0.8016(7) 0.094(4) Uiso 0.580(11) 1 d PD A 1 H23 H 0.4205 0.2725 0.8045 0.113 Uiso 0.580(11) 1 calc PR A 1 C24 C 0.3999(5) 0.1973(4) 0.7299(5) 0.063(2) Uiso 0.580(11) 1 d PD A 1 H24 H 0.3798 0.2175 0.6836 0.075 Uiso 0.580(11) 1 calc PR A 1 C19F C 0.3943(6) 0.1549(5) 0.7061(6) 0.049(3) Uiso 0.420(11) 1 d PD A 2 C20F C 0.4298(8) 0.1390(7) 0.7795(8) 0.092(5) Uiso 0.420(11) 1 d PD A 2 H20F H 0.4479 0.0994 0.7853 0.110 Uiso 0.420(11) 1 calc PR A 2 C21F C 0.4419(13) 0.1769(10) 0.8479(12) 0.169(13) Uiso 0.420(11) 1 d PD A 2 H21F H 0.4662 0.1654 0.8977 0.203 Uiso 0.420(11) 1 calc PR A 2 C22F C 0.4128(12) 0.2320(9) 0.8297(11) 0.114(7) Uiso 0.420(11) 1 d PD A 2 H22F H 0.4151 0.2588 0.8727 0.136 Uiso 0.420(11) 1 calc PR A 2 C23F C 0.3821(10) 0.2538(7) 0.7623(9) 0.111(6) Uiso 0.420(11) 1 d PD A 2 H23F H 0.3702 0.2947 0.7571 0.133 Uiso 0.420(11) 1 calc PR A 2 C24F C 0.3667(8) 0.2134(5) 0.6957(8) 0.081(4) Uiso 0.420(11) 1 d PD A 2 H24F H 0.3395 0.2259 0.6477 0.097 Uiso 0.420(11) 1 calc PR A 2 C25 C 0.2733(2) 0.02371(15) 0.7194(2) 0.0383(7) Uani 1 1 d . . . C26 C 0.26588(18) -0.03750(15) 0.70905(19) 0.0349(7) Uani 1 1 d . A . H26 H 0.2728 -0.0547 0.6596 0.042 Uiso 1 1 calc R . . C27 C 0.2482(2) -0.07370(15) 0.7715(2) 0.0397(7) Uani 1 1 d . . . C28 C 0.2366(3) -0.04772(19) 0.8437(2) 0.0726(15) Uani 1 1 d . A . H28 H 0.2247 -0.0718 0.8862 0.087 Uiso 1 1 calc R . . C29 C 0.2425(4) 0.0136(2) 0.8531(3) 0.101(2) Uani 1 1 d . . . H29 H 0.2336 0.0311 0.9018 0.121 Uiso 1 1 calc R A . C30 C 0.2615(3) 0.04969(19) 0.7914(2) 0.0724(15) Uani 1 1 d . A . H30 H 0.2664 0.0913 0.7985 0.087 Uiso 1 1 calc R . . C31 C 0.0864(2) -0.16893(18) 0.7359(2) 0.0472(9) Uani 1 1 d . . . C32 C 0.0504(3) -0.1150(3) 0.7482(4) 0.0910(18) Uani 1 1 d . . . H32 H 0.0732 -0.0872 0.7851 0.109 Uiso 1 1 calc R . . C33 C -0.0202(4) -0.1026(3) 0.7051(5) 0.114(2) Uani 1 1 d . . . H33 H -0.0447 -0.0660 0.7132 0.137 Uiso 1 1 calc R . . C34 C -0.0537(3) -0.1424(3) 0.6519(4) 0.0891(19) Uani 1 1 d . . . H34 H -0.1014 -0.1338 0.6237 0.107 Uiso 1 1 calc R . . C35 C -0.0181(3) -0.1944(3) 0.6398(3) 0.0810(16) Uani 1 1 d . . . H35 H -0.0411 -0.2217 0.6024 0.097 Uiso 1 1 calc R . . C36 C 0.0518(3) -0.2084(2) 0.6814(3) 0.0635(11) Uani 1 1 d . . . H36 H 0.0755 -0.2451 0.6723 0.076 Uiso 1 1 calc R . . C37 C 0.1686(2) -0.18020(17) 0.8945(2) 0.0478(9) Uani 1 1 d . . . C38 C 0.2353(3) -0.1825(2) 0.9465(2) 0.0612(12) Uani 1 1 d . . . H38 H 0.2830 -0.1867 0.9268 0.073 Uiso 1 1 calc R . . C39 C 0.2311(4) -0.1787(2) 1.0276(2) 0.0718(14) Uani 1 1 d . . . H39 H 0.2761 -0.1799 1.0630 0.086 Uiso 1 1 calc R . . C40 C 0.1625(4) -0.1732(3) 1.0562(3) 0.0856(18) Uani 1 1 d . . . H40 H 0.1603 -0.1685 1.1112 0.103 Uiso 1 1 calc R . . C41 C 0.0975(4) -0.1743(4) 1.0066(4) 0.109(2) Uani 1 1 d . . . H41 H 0.0501 -0.1732 1.0275 0.131 Uiso 1 1 calc R . . C42 C 0.0995(3) -0.1770(3) 0.9235(3) 0.0801(16) Uani 1 1 d . . . H42 H 0.0540 -0.1766 0.8890 0.096 Uiso 1 1 calc R . . C43 C 0.30754(19) -0.17517(15) 0.62236(19) 0.0354(7) Uani 1 1 d . . . C44 C 0.2399(2) -0.16169(17) 0.5764(2) 0.0445(8) Uani 1 1 d . . . H44 H 0.1952 -0.1550 0.6011 0.053 Uiso 1 1 calc R . . C45 C 0.2374(3) -0.15802(18) 0.4950(2) 0.0521(9) Uani 1 1 d . . . H45 H 0.1909 -0.1499 0.4640 0.063 Uiso 1 1 calc R . . C46 C 0.3030(3) -0.1663(2) 0.4592(2) 0.0616(12) Uani 1 1 d . . . H46 H 0.3018 -0.1625 0.4037 0.074 Uiso 1 1 calc R . . C47 C 0.3693(3) -0.1799(3) 0.5033(3) 0.0769(16) Uani 1 1 d . . . H47 H 0.4138 -0.1862 0.4782 0.092 Uiso 1 1 calc R . . C48 C 0.3723(2) -0.1846(2) 0.5849(2) 0.0598(11) Uani 1 1 d . . . H48 H 0.4186 -0.1944 0.6150 0.072 Uiso 1 1 calc R . . C49 C 0.4003(2) -0.16899(17) 0.7764(2) 0.0442(8) Uani 1 1 d . . . C50 C 0.4331(3) -0.2048(2) 0.8369(3) 0.0629(12) Uani 1 1 d . . . H50 H 0.4089 -0.2402 0.8506 0.076 Uiso 1 1 calc R . . C51 C 0.5027(4) -0.1877(3) 0.8776(4) 0.0954(19) Uani 1 1 d . . . H51 H 0.5249 -0.2114 0.9199 0.114 Uiso 1 1 calc R . . C52 C 0.5395(3) -0.1365(3) 0.8566(4) 0.0923(19) Uani 1 1 d . . . H52 H 0.5867 -0.1254 0.8841 0.111 Uiso 1 1 calc R . . C53 C 0.5071(3) -0.1021(3) 0.7958(3) 0.0772(14) Uani 1 1 d . . . H53 H 0.5322 -0.0672 0.7814 0.093 Uiso 1 1 calc R . . C54 C 0.4380(2) -0.1177(2) 0.7549(3) 0.0553(10) Uani 1 1 d . . . H54 H 0.4163 -0.0938 0.7127 0.066 Uiso 1 1 calc R . . Cl5 Cl 0.1904(6) -0.0082(3) 0.0799(5) 0.479(6) Uani 1 1 d D . . Cl6 Cl 0.2413(2) 0.03944(18) 0.23257(19) 0.1992(14) Uani 1 1 d D . . C55 C 0.2323(10) -0.0246(4) 0.1743(6) 0.240(8) Uani 1 1 d D . . H55A H 0.2829 -0.0422 0.1710 0.288 Uiso 1 1 calc R . . H55B H 0.2010 -0.0541 0.1989 0.288 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 Pd1 0.03911(15) 0.03135(13) 0.06382(19) 0.00785(12) 0.01972(13) 0.00052(11) Pd2 0.04693(16) 0.03402(14) 0.03262(13) 0.00554(10) 0.00519(11) 0.00212(11) Cl1 0.0687(8) 0.0926(10) 0.0968(9) 0.0504(8) 0.0016(7) -0.0096(7) Cl2 0.0514(6) 0.0476(6) 0.1206(10) 0.0107(6) 0.0367(6) -0.0089(5) Cl3 0.0699(7) 0.0528(5) 0.0492(5) 0.0128(4) 0.0068(5) -0.0163(5) Cl4 0.0688(7) 0.0494(5) 0.0537(5) 0.0011(4) 0.0055(5) 0.0206(5) P1 0.0329(4) 0.0330(4) 0.0447(5) 0.0039(3) 0.0106(4) 0.0013(3) P2 0.0364(5) 0.0383(5) 0.0493(5) -0.0143(4) 0.0097(4) -0.0049(4) P3 0.0434(5) 0.0402(5) 0.0308(4) 0.0047(3) 0.0090(4) 0.0017(4) P4 0.0375(4) 0.0347(4) 0.0332(4) 0.0047(3) 0.0046(3) 0.0034(3) N1 0.0360(15) 0.0324(14) 0.0415(15) -0.0007(11) 0.0073(12) -0.0003(11) N2 0.0422(16) 0.0358(14) 0.0327(13) 0.0017(11) 0.0072(12) 0.0028(12) C1 0.0308(16) 0.0423(18) 0.0460(19) 0.0041(15) 0.0046(14) 0.0019(14) C2 0.042(2) 0.046(2) 0.061(2) 0.0001(17) 0.0067(18) -0.0035(16) C3 0.043(2) 0.051(2) 0.092(3) 0.003(2) 0.005(2) -0.0088(18) C4 0.059(3) 0.049(2) 0.091(4) -0.009(2) -0.016(3) -0.002(2) C5 0.086(3) 0.061(3) 0.054(3) -0.011(2) -0.004(2) 0.004(3) C6 0.057(2) 0.055(2) 0.052(2) -0.0045(19) 0.0033(19) 0.0002(19) C7 0.044(2) 0.0424(19) 0.058(2) 0.0061(17) 0.0185(18) 0.0073(16) C8 0.049(2) 0.054(3) 0.089(3) 0.000(2) 0.008(2) 0.0073(19) C9 0.047(3) 0.070(3) 0.143(5) -0.005(4) 0.003(3) 0.025(2) C10 0.088(4) 0.108(5) 0.117(5) -0.019(4) 0.027(4) 0.052(4) C11 0.107(5) 0.093(4) 0.085(4) -0.021(3) 0.017(3) 0.042(4) C12 0.075(3) 0.064(3) 0.066(3) -0.009(2) 0.010(2) 0.023(2) C13 0.0354(18) 0.058(2) 0.0379(18) -0.0039(16) 0.0029(15) 0.0028(16) C14 0.045(2) 0.049(2) 0.0395(18) 0.0008(15) 0.0124(16) 0.0044(16) C15 0.071(3) 0.053(2) 0.060(2) 0.0075(19) 0.029(2) 0.015(2) C16 0.049(3) 0.089(4) 0.074(3) 0.013(3) 0.020(2) 0.024(2) C17 0.039(2) 0.110(4) 0.074(3) 0.003(3) 0.003(2) 0.011(3) C18 0.041(2) 0.083(3) 0.061(3) -0.013(2) 0.0016(19) -0.002(2) C25 0.0436(19) 0.0358(17) 0.0358(16) -0.0012(13) 0.0066(14) 0.0019(14) C26 0.0355(16) 0.0367(17) 0.0328(16) -0.0007(13) 0.0056(13) 0.0035(13) C27 0.049(2) 0.0345(17) 0.0356(17) -0.0005(13) 0.0036(15) 0.0049(14) C28 0.138(5) 0.046(2) 0.038(2) 0.0036(17) 0.025(3) 0.003(3) C29 0.212(8) 0.054(3) 0.042(2) -0.007(2) 0.042(3) 0.002(4) C30 0.138(5) 0.036(2) 0.045(2) -0.0056(17) 0.020(3) 0.000(2) C31 0.042(2) 0.057(2) 0.0439(19) 0.0098(17) 0.0118(16) 0.0046(17) C32 0.066(3) 0.091(4) 0.112(5) -0.019(3) -0.011(3) 0.033(3) C33 0.072(4) 0.116(5) 0.148(6) -0.015(5) -0.017(4) 0.050(4) C34 0.044(3) 0.125(5) 0.096(4) 0.034(4) -0.002(3) 0.005(3) C35 0.064(3) 0.102(4) 0.072(3) 0.018(3) -0.018(3) -0.018(3) C36 0.060(3) 0.069(3) 0.058(3) 0.011(2) -0.006(2) 0.000(2) C37 0.068(3) 0.0423(19) 0.0342(18) 0.0018(14) 0.0134(18) -0.0043(18) C38 0.083(3) 0.065(3) 0.0357(19) 0.0099(18) 0.006(2) 0.020(2) C39 0.120(4) 0.059(3) 0.036(2) 0.0087(18) 0.003(2) 0.013(3) C40 0.132(5) 0.090(4) 0.038(2) -0.004(2) 0.025(3) -0.013(4) C41 0.112(5) 0.164(7) 0.061(3) -0.018(4) 0.050(4) -0.027(5) C42 0.068(3) 0.128(5) 0.048(2) -0.017(3) 0.026(2) -0.022(3) C43 0.0378(17) 0.0360(16) 0.0327(16) -0.0012(13) 0.0057(14) 0.0002(13) C44 0.049(2) 0.049(2) 0.0364(18) 0.0036(15) 0.0089(16) 0.0096(17) C45 0.062(3) 0.055(2) 0.0384(19) -0.0003(17) 0.0008(18) 0.0076(19) C46 0.072(3) 0.077(3) 0.037(2) -0.0114(19) 0.014(2) -0.023(2) C47 0.048(3) 0.137(5) 0.048(2) -0.033(3) 0.019(2) -0.018(3) C48 0.0330(19) 0.095(3) 0.051(2) -0.019(2) 0.0027(17) -0.002(2) C49 0.0403(19) 0.050(2) 0.0404(18) 0.0011(16) -0.0036(15) 0.0054(16) C50 0.063(3) 0.058(3) 0.063(3) 0.014(2) -0.014(2) 0.011(2) C51 0.092(4) 0.088(4) 0.095(4) 0.020(3) -0.044(3) 0.016(3) C52 0.066(3) 0.091(4) 0.109(5) -0.002(4) -0.038(3) -0.001(3) C53 0.061(3) 0.077(3) 0.090(4) 0.004(3) -0.014(3) -0.012(3) C54 0.047(2) 0.058(2) 0.058(2) 0.0077(19) -0.0054(19) -0.0031(19) Cl5 0.765(17) 0.288(7) 0.353(9) 0.082(6) -0.089(10) -0.058(9) Cl6 0.231(3) 0.205(3) 0.159(2) 0.035(2) 0.006(2) 0.049(3) C55 0.47(2) 0.093(7) 0.148(9) 0.029(7) -0.033(12) 0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2056(9) . ? Pd1 P2 2.2103(11) . ? Pd1 Cl2 2.3333(10) . ? Pd1 Cl1 2.3515(14) . ? Pd2 P3 2.2102(10) . ? Pd2 P4 2.2104(9) . ? Pd2 Cl4 2.3504(10) . ? Pd2 Cl3 2.3637(10) . ? P1 N1 1.700(3) . ? P1 C1 1.792(4) . ? P1 C7 1.804(4) . ? P1 P2 2.6128(13) . ? P2 N1 1.706(3) . ? P2 C19F 1.752(9) . ? P2 C13 1.786(4) . ? P2 C19 1.825(6) . ? P3 N2 1.701(3) . ? P3 C31 1.794(4) . ? P3 C37 1.810(4) . ? P3 P4 2.6102(13) . ? P4 N2 1.717(3) . ? P4 C49 1.796(4) . ? P4 C43 1.803(3) . ? N1 C25 1.452(4) . ? N2 C27 1.433(4) . ? C1 C6 1.389(5) . ? C1 C2 1.395(5) . ? C2 C3 1.388(6) . ? C3 C4 1.375(7) . ? C4 C5 1.353(7) . ? C5 C6 1.402(6) . ? C7 C8 1.393(6) . ? C7 C12 1.408(6) . ? C8 C9 1.388(7) . ? C9 C10 1.364(9) . ? C10 C11 1.380(9) . ? C11 C12 1.388(7) . ? C13 C14 1.389(5) . ? C13 C18 1.394(5) . ? C14 C15 1.394(5) . ? C15 C16 1.368(7) . ? C16 C17 1.356(8) . ? C17 C18 1.376(7) . ? C19 C24 1.382(9) . ? C19 C20 1.392(10) . ? C20 C21 1.398(11) . ? C21 C22 1.372(15) . ? C22 C23 1.302(14) . ? C23 C24 1.443(12) . ? C19F C20F 1.377(13) . ? C19F C24F 1.399(13) . ? C20F C21F 1.431(15) . ? C21F C22F 1.355(17) . ? C22F C23F 1.305(16) . ? C23F C24F 1.446(14) . ? C25 C26 1.383(5) . ? C25 C30 1.386(5) . ? C26 C27 1.392(5) . ? C27 C28 1.386(5) . ? C28 C29 1.382(6) . ? C29 C30 1.386(6) . ? C31 C36 1.371(6) . ? C31 C32 1.385(7) . ? C32 C33 1.401(8) . ? C33 C34 1.355(9) . ? C34 C35 1.345(9) . ? C35 C36 1.387(7) . ? C37 C42 1.361(6) . ? C37 C38 1.392(6) . ? C38 C39 1.385(6) . ? C39 C40 1.352(8) . ? C40 C41 1.346(9) . ? C41 C42 1.411(7) . ? C43 C48 1.377(5) . ? C43 C44 1.384(5) . ? C44 C45 1.376(5) . ? C45 C46 1.372(6) . ? C46 C47 1.351(7) . ? C47 C48 1.380(6) . ? C49 C50 1.376(5) . ? C49 C54 1.390(6) . ? C50 C51 1.392(7) . ? C51 C52 1.381(9) . ? C52 C53 1.360(8) . ? C53 C54 1.379(6) . ? Cl5 C55 1.726(10) . ? Cl6 C55 1.736(9) . ? 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 P1 Pd1 P2 72.55(4) . . ? P1 Pd1 Cl2 165.57(5) . . ? P2 Pd1 Cl2 93.47(4) . . ? P1 Pd1 Cl1 98.86(4) . . ? P2 Pd1 Cl1 170.14(4) . . ? Cl2 Pd1 Cl1 95.36(5) . . ? P3 Pd2 P4 72.38(3) . . ? P3 Pd2 Cl4 167.13(4) . . ? P4 Pd2 Cl4 96.06(4) . . ? P3 Pd2 Cl3 96.02(4) . . ? P4 Pd2 Cl3 167.16(4) . . ? Cl4 Pd2 Cl3 95.99(4) . . ? N1 P1 C1 110.24(15) . . ? N1 P1 C7 109.44(16) . . ? C1 P1 C7 107.01(18) . . ? N1 P1 Pd1 93.50(10) . . ? C1 P1 Pd1 121.35(12) . . ? C7 P1 Pd1 114.24(13) . . ? N1 P1 P2 39.98(9) . . ? C1 P1 P2 131.80(12) . . ? C7 P1 P2 118.05(14) . . ? Pd1 P1 P2 53.81(3) . . ? N1 P2 C19F 111.3(3) . . ? N1 P2 C13 110.69(16) . . ? C19F P2 C13 115.9(4) . . ? N1 P2 C19 107.3(2) . . ? C19F P2 C19 19.5(3) . . ? C13 P2 C19 101.7(3) . . ? N1 P2 Pd1 93.16(10) . . ? C19F P2 Pd1 107.3(4) . . ? C13 P2 Pd1 116.26(12) . . ? C19 P2 Pd1 126.8(2) . . ? N1 P2 P1 39.81(10) . . ? C19F P2 P1 114.8(4) . . ? C13 P2 P1 128.61(13) . . ? C19 P2 P1 124.6(2) . . ? Pd1 P2 P1 53.64(3) . . ? N2 P3 C31 108.24(16) . . ? N2 P3 C37 109.69(16) . . ? C31 P3 C37 108.21(19) . . ? N2 P3 Pd2 94.22(10) . . ? C31 P3 Pd2 121.11(14) . . ? C37 P3 Pd2 114.04(13) . . ? N2 P3 P4 40.44(10) . . ? C31 P3 P4 124.69(12) . . ? C37 P3 P4 123.95(15) . . ? Pd2 P3 P4 53.81(3) . . ? N2 P4 C49 107.95(16) . . ? N2 P4 C43 108.69(14) . . ? C49 P4 C43 108.89(17) . . ? N2 P4 Pd2 93.76(10) . . ? C49 P4 Pd2 122.62(13) . . ? C43 P4 Pd2 113.11(11) . . ? N2 P4 P3 39.99(10) . . ? C49 P4 P3 127.98(13) . . ? C43 P4 P3 119.35(12) . . ? Pd2 P4 P3 53.81(3) . . ? C25 N1 P1 128.9(2) . . ? C25 N1 P2 130.2(2) . . ? P1 N1 P2 100.21(15) . . ? C27 N2 P3 131.0(2) . . ? C27 N2 P4 129.2(2) . . ? P3 N2 P4 99.57(15) . . ? C6 C1 C2 119.5(4) . . ? C6 C1 P1 119.2(3) . . ? C2 C1 P1 121.3(3) . . ? C3 C2 C1 119.7(4) . . ? C4 C3 C2 120.0(4) . . ? C5 C4 C3 121.2(4) . . ? C4 C5 C6 120.0(4) . . ? C1 C6 C5 119.7(4) . . ? C8 C7 C12 119.0(4) . . ? C8 C7 P1 120.8(3) . . ? C12 C7 P1 119.5(3) . . ? C9 C8 C7 119.7(5) . . ? C10 C9 C8 120.6(5) . . ? C9 C10 C11 121.2(5) . . ? C10 C11 C12 119.3(6) . . ? C11 C12 C7 120.2(5) . . ? C14 C13 C18 119.4(4) . . ? C14 C13 P2 120.8(3) . . ? C18 C13 P2 119.3(3) . . ? C13 C14 C15 119.4(4) . . ? C16 C15 C14 119.7(4) . . ? C17 C16 C15 121.3(4) . . ? C16 C17 C18 120.2(5) . . ? C17 C18 C13 119.9(5) . . ? C24 C19 C20 120.9(7) . . ? C24 C19 P2 117.1(6) . . ? C20 C19 P2 121.9(5) . . ? C19 C20 C21 120.2(8) . . ? C22 C21 C20 113.8(11) . . ? C23 C22 C21 131.6(14) . . ? C22 C23 C24 113.5(12) . . ? C19 C24 C23 119.9(8) . . ? C20F C19F C24F 118.2(10) . . ? C20F C19F P2 116.7(9) . . ? C24F C19F P2 124.2(9) . . ? C19F C20F C21F 126.2(14) . . ? C22F C21F C20F 109.5(17) . . ? C23F C22F C21F 130.4(18) . . ? C22F C23F C24F 118.3(15) . . ? C19F C24F C23F 116.8(12) . . ? C26 C25 C30 120.3(3) . . ? C26 C25 N1 119.6(3) . . ? C30 C25 N1 120.1(3) . . ? C25 C26 C27 120.3(3) . . ? C28 C27 C26 119.4(3) . . ? C28 C27 N2 119.8(3) . . ? C26 C27 N2 120.7(3) . . ? C29 C28 C27 120.0(4) . . ? C28 C29 C30 120.7(4) . . ? C25 C30 C29 119.3(4) . . ? C36 C31 C32 118.8(4) . . ? C36 C31 P3 120.0(3) . . ? C32 C31 P3 121.2(4) . . ? C31 C32 C33 119.3(6) . . ? C34 C33 C32 121.0(6) . . ? C35 C34 C33 119.5(5) . . ? C34 C35 C36 121.3(6) . . ? C31 C36 C35 120.2(5) . . ? C42 C37 C38 119.9(4) . . ? C42 C37 P3 122.1(3) . . ? C38 C37 P3 117.9(3) . . ? C39 C38 C37 119.6(5) . . ? C40 C39 C38 120.3(5) . . ? C41 C40 C39 120.4(5) . . ? C40 C41 C42 120.8(6) . . ? C37 C42 C41 118.7(5) . . ? C48 C43 C44 118.6(3) . . ? C48 C43 P4 121.7(3) . . ? C44 C43 P4 119.5(3) . . ? C45 C44 C43 120.7(4) . . ? C46 C45 C44 119.7(4) . . ? C47 C46 C45 120.2(4) . . ? C46 C47 C48 120.6(4) . . ? C43 C48 C47 120.2(4) . . ? C50 C49 C54 119.9(4) . . ? C50 C49 P4 120.4(3) . . ? C54 C49 P4 119.6(3) . . ? C49 C50 C51 119.1(5) . . ? C52 C51 C50 120.7(5) . . ? C53 C52 C51 119.5(5) . . ? C52 C53 C54 120.9(5) . . ? C53 C54 C49 119.8(4) . . ? Cl5 C55 Cl6 110.8(6) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 29.31 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.763 _refine_diff_density_min -1.293 _refine_diff_density_rms 0.089 #------------------------------------------------------------------------------# # NEXT STRUCTURE # #------------------------------------------------------------------------------# data_c1458fin _database_code_depnum_ccdc_archive 'CCDC 274894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58.50 H53 Br4 Cl9 N2 Ni2 P4' _chemical_formula_weight 1664.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br Br -0.2901 2.4595 '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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/4' '-x, -y, z+1/2' '-x+1/2, y+1/2, -z+3/4' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' '-y, -x, -z+1/2' _cell_length_a 15.488(2) _cell_length_b 15.488(2) _cell_length_c 58.128(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13944(4) _cell_formula_units_Z 8 _cell_measurement_temperature 208(2) _cell_measurement_reflns_used 974 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 25.56 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6616 _exptl_absorpt_coefficient_mu 3.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 208(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75395 _diffrn_reflns_av_R_equivalents 0.1528 _diffrn_reflns_av_sigmaI/netI 0.1131 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 72 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 26.41 _reflns_number_total 14296 _reflns_number_gt 9624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.1007P)^2^+136.7325P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 14296 _refine_ls_number_parameters 679 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1541 _refine_ls_R_factor_gt 0.1071 _refine_ls_wR_factor_ref 0.2641 _refine_ls_wR_factor_gt 0.2411 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.06406(14) 0.30329(12) 0.23357(3) 0.0554(5) Uani 1 1 d . . . Br2 Br 1.00341(12) 0.10193(11) 0.21079(3) 0.0520(4) Uani 1 1 d . . . Br3 Br 0.87648(12) 0.87424(10) 0.12861(3) 0.0524(4) Uani 1 1 d . . . Br4 Br 0.90118(11) 0.83979(10) 0.06793(3) 0.0469(4) Uani 1 1 d . . . Ni1 Ni 1.01067(12) 0.24569(12) 0.19955(3) 0.0339(4) Uani 1 1 d . . . Ni2 Ni 0.89325(12) 0.76200(11) 0.10216(3) 0.0317(4) Uani 1 1 d . . . P1 P 1.0108(2) 0.3659(2) 0.18235(6) 0.0317(8) Uani 1 1 d . . . P2 P 0.9587(2) 0.2204(2) 0.16656(6) 0.0318(8) Uani 1 1 d . . . P3 P 0.8948(2) 0.6671(2) 0.12837(6) 0.0288(7) Uani 1 1 d . . . P4 P 0.9002(2) 0.6417(2) 0.08480(6) 0.0300(7) Uani 1 1 d . . . N1 N 0.9596(7) 0.3280(7) 0.1581(2) 0.031(3) Uani 1 1 d . . . N2 N 0.9059(7) 0.5822(7) 0.10987(18) 0.026(2) Uani 1 1 d . . . C1 C 1.1157(9) 0.4098(9) 0.1748(2) 0.033(3) Uani 1 1 d . . . C2 C 1.1479(10) 0.3983(9) 0.1530(3) 0.040(3) Uani 1 1 d . . . H2 H 1.1126 0.3731 0.1417 0.048 Uiso 1 1 calc R . . C3 C 1.2317(10) 0.4232(9) 0.1473(3) 0.045(4) Uani 1 1 d . . . H3 H 1.2557 0.4125 0.1327 0.054 Uiso 1 1 calc R . . C4 C 1.2778(10) 0.4655(12) 0.1648(3) 0.054(5) Uani 1 1 d . . . H4 H 1.3321 0.4891 0.1612 0.064 Uiso 1 1 calc R . . C5 C 1.2497(11) 0.4738(10) 0.1856(3) 0.052(5) Uani 1 1 d . . . H5 H 1.2857 0.4974 0.1970 0.062 Uiso 1 1 calc R . . C6 C 1.1643(9) 0.4474(9) 0.1913(3) 0.038(3) Uani 1 1 d . . . H6 H 1.1421 0.4559 0.2061 0.045 Uiso 1 1 calc R . . C7 C 0.9434(10) 0.4461(10) 0.1970(3) 0.042(4) Uani 1 1 d . . . C8 C 0.9708(10) 0.5275(11) 0.2013(3) 0.046(4) Uani 1 1 d . . . H8 H 1.0224 0.5473 0.1947 0.056 Uiso 1 1 calc R . . C9 C 0.9235(15) 0.5821(13) 0.2156(4) 0.074(7) Uani 1 1 d . . . H9 H 0.9408 0.6391 0.2187 0.088 Uiso 1 1 calc R . . C10 C 0.8473(16) 0.546(2) 0.2252(3) 0.092(9) Uani 1 1 d . . . H10 H 0.8133 0.5803 0.2350 0.111 Uiso 1 1 calc R . . C11 C 0.8236(16) 0.4688(15) 0.2210(3) 0.069(6) Uani 1 1 d . . . H11 H 0.7713 0.4481 0.2270 0.083 Uiso 1 1 calc R . . C12 C 0.8722(14) 0.4170(13) 0.2080(4) 0.073(6) Uani 1 1 d . . . H12 H 0.8564 0.3587 0.2064 0.088 Uiso 1 1 calc R . . C13 C 1.0266(8) 0.1577(8) 0.1479(2) 0.027(3) Uani 1 1 d . . . C14 C 0.9968(10) 0.0962(10) 0.1329(3) 0.048(4) Uani 1 1 d . . . H14 H 0.9372 0.0853 0.1319 0.057 Uiso 1 1 calc R . . C15 C 1.0548(12) 0.0487(9) 0.1188(3) 0.048(4) Uani 1 1 d . . . H15 H 1.0340 0.0076 0.1082 0.058 Uiso 1 1 calc R . . C16 C 1.1388(12) 0.0637(11) 0.1208(3) 0.050(4) Uani 1 1 d . . . H16 H 1.1777 0.0311 0.1119 0.060 Uiso 1 1 calc R . . C17 C 1.1710(11) 0.1261(10) 0.1355(3) 0.046(4) Uani 1 1 d . . . H17 H 1.2306 0.1376 0.1358 0.055 Uiso 1 1 calc R . . C18 C 1.1160(9) 0.1718(10) 0.1500(2) 0.036(3) Uani 1 1 d . . . H18 H 1.1380 0.2111 0.1609 0.043 Uiso 1 1 calc R . . C19 C 0.8482(11) 0.1828(10) 0.1638(3) 0.043(4) Uani 1 1 d . . . C20 C 0.7827(10) 0.2400(11) 0.1598(3) 0.045(4) Uani 1 1 d . . . H20 H 0.7943 0.2988 0.1573 0.054 Uiso 1 1 calc R . . C21 C 0.6965(14) 0.2082(18) 0.1597(4) 0.084(8) Uani 1 1 d . . . H21 H 0.6501 0.2468 0.1580 0.101 Uiso 1 1 calc R . . C22 C 0.6811(12) 0.1223(15) 0.1620(4) 0.082(8) Uani 1 1 d . . . H22 H 0.6244 0.1012 0.1606 0.099 Uiso 1 1 calc R . . C23 C 0.7469(14) 0.0667(13) 0.1663(3) 0.068(6) Uani 1 1 d . . . H23 H 0.7354 0.0079 0.1689 0.081 Uiso 1 1 calc R . . C24 C 0.8312(11) 0.0968(10) 0.1670(3) 0.044(4) Uani 1 1 d . . . H24 H 0.8769 0.0581 0.1696 0.052 Uiso 1 1 calc R . . C25 C 0.9426(9) 0.3652(10) 0.1362(2) 0.035(3) Uani 1 1 d . . . C26 C 0.9304(8) 0.4544(9) 0.1350(2) 0.028(3) Uani 1 1 d . . . H26 H 0.9323 0.4892 0.1483 0.033 Uiso 1 1 calc R . . C27 C 0.9146(8) 0.4909(8) 0.1125(2) 0.023(3) Uani 1 1 d . . . C28 C 0.9068(10) 0.4375(9) 0.0932(2) 0.032(3) Uani 1 1 d . . . H28 H 0.8958 0.4610 0.0785 0.039 Uiso 1 1 calc R . . C29 C 0.9156(10) 0.3489(9) 0.0961(2) 0.039(4) Uani 1 1 d . . . H29 H 0.9091 0.3123 0.0833 0.046 Uiso 1 1 calc R . . C30 C 0.9333(11) 0.3140(9) 0.1170(2) 0.045(4) Uani 1 1 d . . . H30 H 0.9393 0.2539 0.1184 0.053 Uiso 1 1 calc R . . C31 C 0.7959(9) 0.6522(9) 0.1441(3) 0.033(3) Uani 1 1 d . . . C32 C 0.7206(8) 0.6753(10) 0.1340(3) 0.039(4) Uani 1 1 d . . . H32 H 0.7235 0.7037 0.1198 0.046 Uiso 1 1 calc R . . C33 C 0.6393(11) 0.6598(10) 0.1433(3) 0.047(4) Uani 1 1 d . . . H33 H 0.5887 0.6717 0.1350 0.057 Uiso 1 1 calc R . . C34 C 0.6359(11) 0.6278(12) 0.1644(3) 0.058(5) Uani 1 1 d . . . H34 H 0.5821 0.6237 0.1718 0.070 Uiso 1 1 calc R . . C35 C 0.7117(11) 0.5992(12) 0.1764(3) 0.052(4) Uani 1 1 d . . . H35 H 0.7076 0.5725 0.1908 0.062 Uiso 1 1 calc R . . C36 C 0.7939(10) 0.6126(11) 0.1656(3) 0.047(4) Uani 1 1 d . . . H36 H 0.8452 0.5950 0.1729 0.057 Uiso 1 1 calc R . . C37 C 0.9835(8) 0.6671(9) 0.1477(2) 0.029(3) Uani 1 1 d . . . C38 C 1.0619(10) 0.6304(9) 0.1403(2) 0.035(3) Uani 1 1 d . . . H38 H 1.0632 0.5973 0.1267 0.042 Uiso 1 1 calc R . . C39 C 1.1377(10) 0.6425(9) 0.1529(3) 0.040(4) Uani 1 1 d . . . H39 H 1.1898 0.6171 0.1481 0.047 Uiso 1 1 calc R . . C40 C 1.1348(10) 0.6936(10) 0.1731(3) 0.047(4) Uani 1 1 d . . . H40 H 1.1853 0.7026 0.1818 0.056 Uiso 1 1 calc R . . C41 C 1.0590(11) 0.7297(11) 0.1800(3) 0.050(4) Uani 1 1 d . . . H41 H 1.0563 0.7616 0.1938 0.060 Uiso 1 1 calc R . . C42 C 0.9853(11) 0.7190(10) 0.1664(3) 0.045(4) Uani 1 1 d . . . H42 H 0.9348 0.7491 0.1705 0.054 Uiso 1 1 calc R . . C43 C 0.8052(9) 0.6125(9) 0.0695(2) 0.031(3) Uani 1 1 d . . . C44 C 0.7390(9) 0.5644(9) 0.0802(2) 0.033(3) Uani 1 1 d . . . H44 H 0.7475 0.5420 0.0951 0.040 Uiso 1 1 calc R . . C45 C 0.6589(9) 0.5496(10) 0.0685(3) 0.040(4) Uani 1 1 d . . . H45 H 0.6127 0.5218 0.0759 0.048 Uiso 1 1 calc R . . C46 C 0.6512(10) 0.5774(9) 0.0459(3) 0.042(4) Uani 1 1 d . . . H46 H 0.6018 0.5631 0.0373 0.050 Uiso 1 1 calc R . . C47 C 0.7148(11) 0.6252(13) 0.0360(3) 0.056(5) Uani 1 1 d . . . H47 H 0.7058 0.6481 0.0213 0.067 Uiso 1 1 calc R . . C48 C 0.7928(10) 0.6416(10) 0.0471(2) 0.041(4) Uani 1 1 d . . . H48 H 0.8368 0.6721 0.0394 0.049 Uiso 1 1 calc R . . C49 C 0.9933(10) 0.6171(9) 0.0675(3) 0.037(3) Uani 1 1 d . . . C50 C 1.0712(11) 0.6517(12) 0.0742(3) 0.049(4) Uani 1 1 d . . . H50 H 1.0733 0.6889 0.0870 0.059 Uiso 1 1 calc R . . C51 C 1.1437(12) 0.6334(13) 0.0629(3) 0.059(5) Uani 1 1 d . . . H51 H 1.1969 0.6553 0.0681 0.071 Uiso 1 1 calc R . . C52 C 1.1401(13) 0.5820(12) 0.0437(3) 0.064(6) Uani 1 1 d . . . H52 H 1.1910 0.5734 0.0352 0.077 Uiso 1 1 calc R . . C53 C 1.0668(13) 0.5434(14) 0.0364(4) 0.073(6) Uani 1 1 d . . . H53 H 1.0669 0.5059 0.0237 0.088 Uiso 1 1 calc R . . C54 C 0.9909(12) 0.5614(12) 0.0485(3) 0.055(5) Uani 1 1 d . . . H54 H 0.9384 0.5363 0.0438 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.8825(4) 0.8884(4) 0.19945(10) 0.0816(16) Uani 1 1 d D . . Cl2 Cl 0.9703(4) 0.8268(4) 0.24031(9) 0.0861(18) Uani 1 1 d D . . C55 C 0.8990(11) 0.9021(12) 0.2291(3) 0.063(5) Uani 1 1 d D . . H55A H 0.9216 0.9602 0.2320 0.075 Uiso 1 1 calc R . . H55B H 0.8435 0.8971 0.2371 0.075 Uiso 1 1 calc R . . Cl3 Cl 0.2667(4) 0.2533(4) 0.19534(9) 0.0759(15) Uani 1 1 d D . . Cl4 Cl 0.3417(4) 0.1089(4) 0.21870(10) 0.0849(17) Uani 1 1 d D . . C56 C 0.2452(11) 0.1604(12) 0.2114(4) 0.081(7) Uani 1 1 d D . . H56A H 0.2138 0.1761 0.2255 0.097 Uiso 1 1 calc R . . H56B H 0.2088 0.1211 0.2025 0.097 Uiso 1 1 calc R . . Cl5 Cl 0.282(3) 0.293(3) 0.2682(7) 0.55(2) Uiso 1 1 d D . . Cl6 Cl 0.389(3) 0.429(3) 0.2581(7) 0.56(3) Uiso 1 1 d D . . C57 C 0.282(3) 0.396(3) 0.2559(12) 0.33(4) Uiso 1 1 d D . . H57A H 0.2638 0.3938 0.2397 0.394 Uiso 1 1 calc R . . H57B H 0.2439 0.4352 0.2643 0.394 Uiso 1 1 calc R . . Cl7 Cl 0.508(2) 0.379(2) 0.1846(6) 0.463(19) Uiso 1 1 d D . . Cl8 Cl 0.555(4) 0.324(4) 0.2261(7) 0.68(4) Uiso 1 1 d D . . C58 C 0.538(5) 0.421(3) 0.2115(9) 0.35(4) Uiso 1 1 d D . . H58A H 0.5908 0.4559 0.2105 0.417 Uiso 1 1 calc R . . H58B H 0.4917 0.4554 0.2185 0.417 Uiso 1 1 calc R . . Cl9 Cl 0.7518(9) 0.1938(8) 0.2269(2) 0.180(4) Uiso 1 1 d . . . C59 C 0.8215(18) 0.1785(18) 0.2500 0.102(12) Uiso 1 2 d S . . H59A H 0.8149 0.1191 0.2555 0.122 Uiso 0.50 1 calc PR . . H59B H 0.8809 0.1851 0.2445 0.122 Uiso 0.50 1 calc PR . . 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 Br1 0.0814(13) 0.0491(10) 0.0357(8) 0.0015(7) -0.0101(9) -0.0020(9) Br2 0.0649(11) 0.0378(8) 0.0533(10) 0.0116(8) -0.0051(8) 0.0009(8) Br3 0.0698(12) 0.0280(8) 0.0595(10) -0.0074(7) -0.0085(9) 0.0038(7) Br4 0.0477(9) 0.0375(8) 0.0556(10) 0.0145(7) -0.0024(8) 0.0029(7) Ni1 0.0387(11) 0.0322(10) 0.0309(9) 0.0072(8) -0.0016(8) 0.0013(8) Ni2 0.0332(10) 0.0207(8) 0.0412(10) 0.0023(7) -0.0045(8) 0.0024(7) P1 0.040(2) 0.0273(18) 0.0280(17) -0.0001(14) -0.0020(16) -0.0015(16) P2 0.036(2) 0.0284(19) 0.0307(19) 0.0034(15) -0.0033(16) -0.0018(15) P3 0.0293(18) 0.0240(16) 0.0331(18) 0.0003(14) -0.0023(15) 0.0034(15) P4 0.0320(19) 0.0269(18) 0.0311(18) 0.0032(15) -0.0016(16) 0.0004(15) N1 0.035(6) 0.021(6) 0.038(7) 0.005(5) 0.003(5) 0.002(5) N2 0.025(6) 0.024(6) 0.031(6) 0.001(4) 0.000(5) 0.001(4) C1 0.040(8) 0.025(7) 0.035(8) 0.005(6) 0.006(6) -0.002(6) C2 0.043(9) 0.023(7) 0.055(9) -0.001(7) 0.003(7) -0.003(6) C3 0.036(8) 0.024(8) 0.074(11) 0.010(7) 0.015(8) -0.008(6) C4 0.030(9) 0.064(12) 0.067(12) 0.016(9) 0.019(8) -0.014(8) C5 0.047(10) 0.046(10) 0.063(11) 0.016(8) -0.020(9) -0.022(8) C6 0.028(7) 0.030(8) 0.055(9) 0.002(7) -0.010(7) 0.008(6) C7 0.038(9) 0.044(9) 0.043(9) -0.006(7) -0.001(7) -0.002(7) C8 0.038(9) 0.056(10) 0.045(9) -0.028(8) 0.002(7) -0.015(7) C9 0.093(17) 0.053(12) 0.075(14) -0.027(10) -0.042(13) 0.018(11) C10 0.078(17) 0.17(3) 0.033(10) 0.006(14) 0.011(10) 0.049(18) C11 0.087(16) 0.064(14) 0.058(13) -0.003(11) 0.012(11) -0.011(12) C12 0.080(15) 0.051(12) 0.088(15) -0.003(10) 0.035(12) 0.017(10) C13 0.031(7) 0.025(7) 0.026(7) -0.005(6) 0.001(6) -0.001(5) C14 0.031(8) 0.037(8) 0.074(11) 0.007(8) -0.007(8) 0.000(7) C15 0.069(12) 0.025(8) 0.050(10) -0.025(7) 0.011(9) 0.008(8) C16 0.067(12) 0.042(9) 0.040(9) 0.015(8) 0.017(8) 0.008(8) C17 0.038(8) 0.030(8) 0.069(11) 0.002(8) 0.007(8) 0.010(7) C18 0.034(8) 0.039(8) 0.033(8) 0.007(6) 0.010(6) 0.003(6) C19 0.053(10) 0.045(9) 0.031(8) 0.009(7) 0.008(7) -0.002(8) C20 0.036(9) 0.049(10) 0.050(9) 0.022(8) 0.006(7) 0.016(7) C21 0.051(12) 0.14(2) 0.064(14) 0.029(14) -0.002(10) -0.020(13) C22 0.027(10) 0.075(15) 0.14(2) 0.039(15) -0.019(11) -0.024(10) C23 0.067(14) 0.060(12) 0.076(14) -0.013(10) 0.007(11) -0.031(11) C24 0.049(9) 0.042(9) 0.039(8) -0.003(7) -0.006(7) -0.013(8) C25 0.032(8) 0.038(8) 0.036(8) -0.009(6) -0.001(6) -0.009(6) C26 0.022(7) 0.028(7) 0.033(7) 0.000(6) -0.004(6) 0.002(5) C27 0.025(6) 0.018(6) 0.025(6) 0.008(5) 0.006(5) 0.019(5) C28 0.055(9) 0.028(7) 0.013(6) 0.001(5) -0.006(6) 0.016(7) C29 0.047(9) 0.035(8) 0.034(8) -0.011(6) -0.001(7) 0.012(7) C30 0.079(12) 0.015(7) 0.039(8) -0.008(6) -0.018(8) 0.025(7) C31 0.026(7) 0.033(8) 0.041(8) -0.012(7) -0.006(6) 0.003(6) C32 0.020(7) 0.045(9) 0.050(9) -0.013(7) -0.002(6) 0.009(6) C33 0.058(11) 0.036(9) 0.048(10) -0.001(7) -0.005(8) 0.029(8) C34 0.045(10) 0.052(11) 0.078(13) -0.041(10) 0.001(9) 0.007(8) C35 0.042(9) 0.065(11) 0.048(10) 0.008(9) 0.015(7) -0.002(8) C36 0.034(8) 0.058(11) 0.049(10) -0.019(8) 0.003(7) -0.012(8) C37 0.026(7) 0.027(7) 0.034(7) -0.004(6) 0.001(6) 0.000(6) C38 0.047(9) 0.033(8) 0.025(7) -0.003(6) 0.003(6) -0.002(7) C39 0.045(9) 0.027(8) 0.047(9) 0.008(7) -0.004(7) -0.005(6) C40 0.030(8) 0.032(8) 0.079(12) 0.010(8) -0.010(8) -0.013(7) C41 0.054(11) 0.044(9) 0.053(10) 0.003(8) -0.026(8) -0.016(8) C42 0.047(10) 0.035(8) 0.053(10) 0.004(7) 0.002(8) 0.003(7) C43 0.038(8) 0.029(7) 0.027(7) -0.010(6) -0.004(6) 0.004(6) C44 0.038(8) 0.026(7) 0.035(8) 0.000(6) 0.003(6) 0.004(6) C45 0.025(7) 0.037(8) 0.057(10) -0.006(7) -0.010(7) -0.001(6) C46 0.037(9) 0.030(8) 0.059(10) 0.007(7) -0.019(7) -0.004(6) C47 0.045(10) 0.082(13) 0.041(9) -0.003(9) -0.032(8) -0.014(9) C48 0.044(9) 0.047(9) 0.031(8) 0.012(7) -0.006(7) -0.004(7) C49 0.044(9) 0.024(7) 0.043(8) -0.006(6) 0.006(7) 0.009(6) C50 0.045(10) 0.058(11) 0.043(9) -0.004(8) -0.004(8) -0.001(8) C51 0.045(11) 0.078(14) 0.054(11) -0.001(10) -0.007(8) 0.004(9) C52 0.065(13) 0.058(12) 0.070(13) -0.008(10) 0.015(10) 0.032(10) C53 0.053(12) 0.089(15) 0.077(14) -0.040(12) 0.002(10) -0.042(11) C54 0.053(11) 0.062(11) 0.051(10) -0.002(9) 0.008(9) -0.019(9) Cl1 0.070(3) 0.086(4) 0.089(4) -0.021(3) -0.010(3) 0.009(3) Cl2 0.097(4) 0.109(5) 0.052(3) 0.005(3) 0.006(3) 0.023(4) C55 0.043(10) 0.060(11) 0.085(14) 0.015(10) 0.019(9) 0.014(9) Cl3 0.076(3) 0.075(3) 0.077(3) 0.024(3) 0.005(3) 0.017(3) Cl4 0.086(4) 0.096(4) 0.073(3) 0.002(3) -0.008(3) 0.039(3) C56 0.055(12) 0.051(11) 0.14(2) 0.031(13) 0.033(13) 0.010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ni1 2.322(2) . ? Br2 Ni1 2.323(2) . ? Br3 Ni2 2.335(2) . ? Br4 Ni2 2.329(2) . ? Ni1 P1 2.114(4) . ? Ni1 P2 2.116(4) . ? Ni2 P3 2.117(4) . ? Ni2 P4 2.121(4) . ? P1 N1 1.719(12) . ? P1 C1 1.817(15) . ? P1 C7 1.831(16) . ? P1 P2 2.563(5) . ? P2 N1 1.737(11) . ? P2 C13 1.794(13) . ? P2 C19 1.815(17) . ? P3 N2 1.707(11) . ? P3 C37 1.773(14) . ? P3 C31 1.800(15) . ? P3 P4 2.564(5) . ? P4 N2 1.726(11) . ? P4 C43 1.778(14) . ? P4 C49 1.800(15) . ? N1 C25 1.425(18) . ? N2 C27 1.430(15) . ? C1 C6 1.35(2) . ? C1 C2 1.37(2) . ? C2 C3 1.39(2) . ? C3 C4 1.41(2) . ? C4 C5 1.29(2) . ? C5 C6 1.42(2) . ? C7 C12 1.35(2) . ? C7 C8 1.35(2) . ? C8 C9 1.39(3) . ? C9 C10 1.42(3) . ? C10 C11 1.28(3) . ? C11 C12 1.33(3) . ? C13 C14 1.37(2) . ? C13 C18 1.407(19) . ? C14 C15 1.42(2) . ? C15 C16 1.33(2) . ? C16 C17 1.38(2) . ? C17 C18 1.39(2) . ? C19 C20 1.37(2) . ? C19 C24 1.37(2) . ? C20 C21 1.42(3) . ? C21 C22 1.36(3) . ? C22 C23 1.36(3) . ? C23 C24 1.39(2) . ? C25 C30 1.376(19) . ? C25 C26 1.40(2) . ? C26 C27 1.445(17) . ? C27 C28 1.403(18) . ? C28 C29 1.389(19) . ? C29 C30 1.357(19) . ? C31 C32 1.353(19) . ? C31 C36 1.39(2) . ? C32 C33 1.39(2) . ? C33 C34 1.32(2) . ? C34 C35 1.43(2) . ? C35 C36 1.43(2) . ? C37 C42 1.36(2) . ? C37 C38 1.407(19) . ? C38 C39 1.40(2) . ? C39 C40 1.42(2) . ? C40 C41 1.36(2) . ? C41 C42 1.40(2) . ? C43 C48 1.391(19) . ? C43 C44 1.41(2) . ? C44 C45 1.43(2) . ? C45 C46 1.39(2) . ? C46 C47 1.36(2) . ? C47 C48 1.39(2) . ? C49 C50 1.38(2) . ? C49 C54 1.40(2) . ? C50 C51 1.33(2) . ? C51 C52 1.37(3) . ? C52 C53 1.35(3) . ? C53 C54 1.40(3) . ? Cl1 C55 1.758(16) . ? Cl2 C55 1.732(15) . ? Cl3 C56 1.748(15) . ? Cl4 C56 1.747(16) . ? Cl5 C57 1.76(2) . ? Cl6 C57 1.73(2) . ? Cl7 C58 1.76(2) . ? Cl8 C58 1.75(2) . ? Cl9 C59 1.74(2) . ? C59 Cl9 1.74(2) 8_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 P1 Ni1 P2 74.62(15) . . ? P1 Ni1 Br1 93.66(13) . . ? P2 Ni1 Br1 168.06(14) . . ? P1 Ni1 Br2 167.84(14) . . ? P2 Ni1 Br2 93.41(13) . . ? Br1 Ni1 Br2 98.38(9) . . ? P3 Ni2 P4 74.45(15) . . ? P3 Ni2 Br4 166.71(14) . . ? P4 Ni2 Br4 92.61(12) . . ? P3 Ni2 Br3 92.54(12) . . ? P4 Ni2 Br3 166.52(14) . . ? Br4 Ni2 Br3 100.56(9) . . ? N1 P1 C1 110.0(6) . . ? N1 P1 C7 110.4(6) . . ? C1 P1 C7 111.7(7) . . ? N1 P1 Ni1 94.9(4) . . ? C1 P1 Ni1 116.4(5) . . ? C7 P1 Ni1 112.2(5) . . ? N1 P1 P2 42.4(4) . . ? C1 P1 P2 121.5(5) . . ? C7 P1 P2 125.7(5) . . ? Ni1 P1 P2 52.74(12) . . ? N1 P2 C13 110.2(6) . . ? N1 P2 C19 106.9(7) . . ? C13 P2 C19 108.9(7) . . ? N1 P2 Ni1 94.3(4) . . ? C13 P2 Ni1 115.1(5) . . ? C19 P2 Ni1 119.9(5) . . ? N1 P2 P1 41.8(4) . . ? C13 P2 P1 120.5(5) . . ? C19 P2 P1 127.7(6) . . ? Ni1 P2 P1 52.65(12) . . ? N2 P3 C37 108.7(6) . . ? N2 P3 C31 107.9(6) . . ? C37 P3 C31 109.8(6) . . ? N2 P3 Ni2 94.7(4) . . ? C37 P3 Ni2 117.6(5) . . ? C31 P3 Ni2 116.5(5) . . ? N2 P3 P4 42.0(4) . . ? C37 P3 P4 126.8(5) . . ? C31 P3 P4 120.7(5) . . ? Ni2 P3 P4 52.84(12) . . ? N2 P4 C43 109.3(6) . . ? N2 P4 C49 108.5(6) . . ? C43 P4 C49 109.2(7) . . ? N2 P4 Ni2 94.0(4) . . ? C43 P4 Ni2 114.8(5) . . ? C49 P4 Ni2 119.5(5) . . ? N2 P4 P3 41.4(4) . . ? C43 P4 P3 120.5(5) . . ? C49 P4 P3 127.6(5) . . ? Ni2 P4 P3 52.71(12) . . ? C25 N1 P1 132.9(9) . . ? C25 N1 P2 129.7(10) . . ? P1 N1 P2 95.8(6) . . ? C27 N2 P3 134.7(9) . . ? C27 N2 P4 128.6(9) . . ? P3 N2 P4 96.6(5) . . ? C6 C1 C2 120.6(14) . . ? C6 C1 P1 119.1(11) . . ? C2 C1 P1 120.1(11) . . ? C1 C2 C3 121.5(15) . . ? C2 C3 C4 115.4(15) . . ? C5 C4 C3 123.6(15) . . ? C4 C5 C6 120.0(16) . . ? C1 C6 C5 118.6(15) . . ? C12 C7 C8 118.5(16) . . ? C12 C7 P1 117.3(13) . . ? C8 C7 P1 122.6(12) . . ? C7 C8 C9 120.8(17) . . ? C8 C9 C10 116(2) . . ? C11 C10 C9 122(2) . . ? C10 C11 C12 121(2) . . ? C11 C12 C7 122(2) . . ? C14 C13 C18 119.5(13) . . ? C14 C13 P2 124.2(11) . . ? C18 C13 P2 116.2(10) . . ? C13 C14 C15 120.9(14) . . ? C16 C15 C14 118.6(15) . . ? C15 C16 C17 121.9(16) . . ? C16 C17 C18 120.7(16) . . ? C17 C18 C13 118.2(14) . . ? C20 C19 C24 120.7(16) . . ? C20 C19 P2 120.4(13) . . ? C24 C19 P2 118.8(13) . . ? C19 C20 C21 118.2(18) . . ? C22 C21 C20 120(2) . . ? C23 C22 C21 120.5(18) . . ? C22 C23 C24 119.9(18) . . ? C19 C24 C23 120.3(18) . . ? C30 C25 C26 121.1(14) . . ? C30 C25 N1 120.8(13) . . ? C26 C25 N1 117.9(12) . . ? C25 C26 C27 116.9(12) . . ? C28 C27 N2 119.2(11) . . ? C28 C27 C26 120.7(11) . . ? N2 C27 C26 120.1(11) . . ? C29 C28 C27 118.3(12) . . ? C30 C29 C28 121.6(13) . . ? C29 C30 C25 121.1(13) . . ? C32 C31 C36 119.0(14) . . ? C32 C31 P3 118.7(12) . . ? C36 C31 P3 122.2(11) . . ? C31 C32 C33 124.6(16) . . ? C34 C33 C32 117.3(16) . . ? C33 C34 C35 122.1(17) . . ? C34 C35 C36 118.1(16) . . ? C31 C36 C35 118.4(15) . . ? C42 C37 C38 118.0(13) . . ? C42 C37 P3 121.6(11) . . ? C38 C37 P3 118.3(10) . . ? C39 C38 C37 120.6(13) . . ? C38 C39 C40 118.9(15) . . ? C41 C40 C39 120.1(15) . . ? C40 C41 C42 119.3(16) . . ? C37 C42 C41 122.7(16) . . ? C48 C43 C44 118.9(13) . . ? C48 C43 P4 120.1(11) . . ? C44 C43 P4 120.9(11) . . ? C43 C44 C45 120.1(13) . . ? C46 C45 C44 118.3(14) . . ? C47 C46 C45 120.3(14) . . ? C46 C47 C48 122.4(15) . . ? C47 C48 C43 119.5(15) . . ? C50 C49 C54 119.0(15) . . ? C50 C49 P4 117.5(11) . . ? C54 C49 P4 123.3(13) . . ? C51 C50 C49 121.1(16) . . ? C50 C51 C52 119.4(18) . . ? C53 C52 C51 123.0(18) . . ? C52 C53 C54 117.5(17) . . ? C53 C54 C49 119.7(16) . . ? Cl2 C55 Cl1 112.3(9) . . ? Cl4 C56 Cl3 110.0(9) . . ? Cl6 C57 Cl5 104(2) . . ? Cl8 C58 Cl7 98.7(19) . . ? Cl9 C59 Cl9 115(2) 8_665 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.377 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.171 #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#