# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1432 data_global #============================================================================ # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Yifan Zheng Inorganic Chemistry Laboratory University of Oxford South Park Road Oxford OX1 3QR U.K. ; _publ_contact_author_phone '01865 272619' _publ_contact_author_fax '01865 272690' _publ_contact_author_email yifan.zheng@chem.ox.ac.uk _publ_requested_journal 'J. Chem. Soc. Dalton Trans' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Binuclear Complexes with Ligands Based on the 2,6-Diphenylphosphinoaryl Framework. The Syntheses and X-ray Crystal Structures of and Xrya Crystal Structures of [Ir2Cl2..........] [Ni2.......] and [Rh2Cl2(CO)2.....] ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Jonathan R. Dilworth' ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UK ; 'Yifan Zheng' ; Inorganic Chemistry Laboratory University of Oxford South Park Road Oxford OX1 3QR UK ; 'D. Vaughan Griffiths' ; Department of Chemistry Queen Mary & Westfield College(University of London) Mile End Road London E1 4NS UK ; data_(1) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33.50 H29 Cl3 Ir O0.50 P2 S' _chemical_formula_weight 832.12 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Ir' 'Ir' -1.4442 7.9887 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.060(7) _cell_length_b 13.434(3) _cell_length_c 19.625(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.95(4) _cell_angle_gamma 90.00 _cell_volume 6383(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 15 _exptl_crystal_description brick _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method ? _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 4.625 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enral-Nonius_CAD4' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 25 _diffrn_reflns_number 6071 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5926 _reflns_number_observed 3864 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD-4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 (Enraf-Nonius, 1989)' _computing_data_reduction 'Molen (Enraf-Nonius, 1990)' _computing_structure_solution 'SHELXS-92 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1859P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5926 _refine_ls_number_parameters 371 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1436 _refine_ls_R_factor_obs 0.0850 _refine_ls_wR_factor_all 0.2294 _refine_ls_wR_factor_obs 0.2062 _refine_ls_goodness_of_fit_all 0.962 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 0.961 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ir1 Ir 0.06118(2) 0.10175(4) 0.24661(2) 0.0268(2) Uani 1 d . . S1 S -0.01886(15) 0.0218(3) 0.16825(17) 0.0330(8) Uani 1 d . . P1 P 0.13576(15) 0.1522(3) 0.33476(18) 0.0331(8) Uani 1 d . . P2 P 0.08974(15) 0.1678(3) 0.15411(18) 0.0341(8) Uani 1 d . . Cl Cl 0.11337(18) -0.0614(3) 0.2427(2) 0.0465(9) Uani 1 d . . C C 0.0000 0.2011(14) 0.2500 0.031(4) Uani 1 d SU . O O 0.0000 0.2903(9) 0.2500 0.039(3) Uani 1 d S . C1 C -0.0438(6) 0.0810(11) 0.0827(7) 0.036(3) Uani 1 d . . C2 C -0.0053(7) 0.1092(11) 0.0468(7) 0.040(4) Uani 1 d . . C3 C -0.0271(7) 0.1501(13) -0.0215(7) 0.051(4) Uani 1 d . . H3 H -0.0026 0.1715 -0.0468 0.061 Uiso 1 calc R . C4 C -0.0817(8) 0.1592(14) -0.0514(8) 0.056(5) Uani 1 d . . H4 H -0.0943 0.1850 -0.0967 0.067 Uiso 1 calc R . C5 C -0.1186(7) 0.1295(13) -0.0136(8) 0.051(4) Uani 1 d . . H5 H -0.1563 0.1377 -0.0332 0.062 Uiso 1 calc R . C6 C -0.1002(6) 0.0874(11) 0.0532(7) 0.036(3) Uani 1 d . . C11 C 0.1383(6) 0.2702(11) 0.3847(7) 0.038(3) Uani 1 d . . C12 C 0.0936(8) 0.3234(14) 0.3824(9) 0.060(5) Uani 1 d . . H12 H 0.0602 0.3055 0.3514 0.072 Uiso 1 calc R . C13 C 0.0960(9) 0.4059(18) 0.4256(13) 0.089(8) Uani 1 d . . H13 H 0.0641 0.4424 0.4239 0.106 Uiso 1 calc R . C14 C 0.1458(10) 0.4344(17) 0.4717(11) 0.084(7) Uani 1 d . . H14 H 0.1475 0.4903 0.5001 0.100 Uiso 1 calc R . C15 C 0.1914(8) 0.3804(15) 0.4747(11) 0.067(5) Uani 1 d . . H15 H 0.2249 0.3980 0.5056 0.080 Uiso 1 calc R . C16 C 0.1880(7) 0.2986(13) 0.4313(8) 0.052(4) Uani 1 d . . H16 H 0.2196 0.2614 0.4331 0.063 Uiso 1 calc R . C21 C 0.2043(6) 0.1466(15) 0.3188(9) 0.052(4) Uani 1 d . . C22 C 0.2345(7) 0.0645(15) 0.3293(9) 0.053(4) Uani 1 d . . H22 H 0.2202 0.0067 0.3438 0.063 Uiso 1 calc R . C23 C 0.2876(8) 0.0636(18) 0.3188(11) 0.070(6) Uani 1 d . . H23 H 0.3075 0.0044 0.3238 0.084 Uiso 1 calc R . C24 C 0.3102(8) 0.148(2) 0.3016(12) 0.082(7) Uani 1 d . . H24 H 0.3461 0.1475 0.2967 0.099 Uiso 1 calc R . C25 C 0.2801(8) 0.2316(18) 0.2914(10) 0.070(6) Uani 1 d . . H25 H 0.2957 0.2894 0.2788 0.083 Uiso 1 calc R . C26 C 0.2270(7) 0.2354(14) 0.2991(8) 0.056(5) Uani 1 d . . H26 H 0.2068 0.2942 0.2916 0.067 Uiso 1 calc R . C31 C 0.1407(6) 0.0605(11) 0.4073(7) 0.038(3) Uani 1 d . . H31A H 0.1331 -0.0060 0.3879 0.046 Uiso 1 calc R . H31B H 0.1777 0.0611 0.4385 0.046 Uiso 1 calc R . C41 C 0.0762(6) 0.2988(12) 0.1372(8) 0.044(4) Uani 1 d . . C42 C 0.0839(7) 0.3654(11) 0.1926(9) 0.047(4) Uani 1 d . . H42 H 0.0931 0.3423 0.2389 0.056 Uiso 1 calc R . C43 C 0.0776(7) 0.4687(15) 0.1790(12) 0.063(5) Uani 1 d . . H43 H 0.0835 0.5138 0.2162 0.076 Uiso 1 calc R . C44 C 0.0624(9) 0.5023(16) 0.1098(14) 0.082(7) Uani 1 d . . H44 H 0.0586 0.5702 0.1003 0.098 Uiso 1 calc R . C45 C 0.0533(9) 0.4361(19) 0.0563(14) 0.085(7) Uani 1 d . . H45 H 0.0419 0.4592 0.0102 0.103 Uiso 1 calc R . C46 C 0.0601(7) 0.3363(14) 0.0681(9) 0.058(5) Uani 1 d . . H46 H 0.0541 0.2928 0.0301 0.069 Uiso 1 calc R . C51 C 0.1596(7) 0.1560(12) 0.1431(8) 0.044(4) Uani 1 d . . C52 C 0.1836(7) 0.0633(15) 0.1451(9) 0.058(5) Uani 1 d . . H52 H 0.1673 0.0076 0.1594 0.070 Uiso 1 calc R . C53 C 0.2323(8) 0.0552(18) 0.1253(11) 0.075(6) Uani 1 d . . H53 H 0.2484 -0.0074 0.1268 0.090 Uiso 1 calc R . C54 C 0.2574(8) 0.131(2) 0.1045(12) 0.084(7) Uani 1 d . . H54 H 0.2893 0.1208 0.0896 0.101 Uiso 1 calc R . C55 C 0.2362(8) 0.2266(18) 0.1046(13) 0.083(7) Uani 1 d . . H55 H 0.2546 0.2815 0.0929 0.099 Uiso 1 calc R . C56 C 0.1870(7) 0.2374(15) 0.1228(10) 0.062(5) Uani 1 d . . H56 H 0.1715 0.3005 0.1215 0.074 Uiso 1 calc R . C61 C 0.0559(7) 0.0976(12) 0.0735(8) 0.045(4) Uani 1 d . . H61A H 0.0726 0.1177 0.0362 0.055 Uiso 1 calc R . H61B H 0.0640 0.0275 0.0825 0.055 Uiso 1 calc R . C0 C 0.4238(16) 0.254(2) 0.1555(15) 0.148(14) Uani 1 d . . H0A H 0.4523 0.3045 0.1685 0.177 Uiso 1 calc R . H0B H 0.4034 0.2533 0.1913 0.177 Uiso 1 calc R . Cl1 Cl 0.3771(4) 0.2869(6) 0.0710(4) 0.129(3) Uani 1 d . . Cl2 Cl 0.4515(9) 0.1509(11) 0.1541(8) 0.290(10) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0253(3) 0.0326(3) 0.0259(3) 0.0007(2) 0.0128(2) 0.0015(2) S1 0.0339(19) 0.0397(18) 0.0299(16) -0.0035(13) 0.0166(15) -0.0003(16) P1 0.0264(19) 0.042(2) 0.0339(17) 0.0028(15) 0.0130(15) 0.0005(16) P2 0.031(2) 0.047(2) 0.0305(16) 0.0016(15) 0.0204(15) -0.0002(17) Cl 0.050(2) 0.046(2) 0.048(2) 0.0010(16) 0.0227(18) 0.0094(19) C 0.031(4) 0.032(4) 0.031(4) 0.000 0.010(2) 0.000 O 0.042(8) 0.029(7) 0.051(8) 0.000 0.019(7) 0.000 C1 0.041(9) 0.052(8) 0.018(6) -0.008(5) 0.015(6) 0.004(7) C2 0.042(9) 0.061(9) 0.023(6) -0.002(6) 0.016(6) 0.002(8) C3 0.052(11) 0.078(11) 0.027(7) -0.009(7) 0.019(7) 0.002(9) C4 0.061(12) 0.075(12) 0.030(7) 0.000(7) 0.011(8) 0.010(10) C5 0.044(10) 0.077(11) 0.033(7) -0.014(7) 0.010(7) 0.000(9) C6 0.027(7) 0.054(9) 0.029(7) -0.009(6) 0.013(6) 0.009(7) C11 0.044(9) 0.050(8) 0.025(6) -0.001(6) 0.019(6) -0.017(7) C12 0.049(11) 0.075(12) 0.050(9) -0.026(9) 0.004(8) 0.000(10) C13 0.051(12) 0.12(2) 0.085(15) -0.055(14) 0.006(11) 0.010(13) C14 0.084(17) 0.096(16) 0.075(14) -0.045(12) 0.028(13) -0.016(14) C15 0.042(10) 0.089(14) 0.070(12) -0.031(10) 0.015(9) -0.014(10) C16 0.049(10) 0.055(10) 0.056(9) -0.004(8) 0.020(8) -0.009(9) C21 0.014(8) 0.085(12) 0.064(10) 0.001(9) 0.021(7) -0.009(8) C22 0.033(9) 0.080(12) 0.053(9) -0.005(9) 0.025(8) -0.002(9) C23 0.037(10) 0.105(16) 0.077(13) -0.026(12) 0.031(10) 0.010(11) C24 0.029(10) 0.13(2) 0.087(15) 0.000(15) 0.015(10) -0.017(13) C25 0.045(11) 0.103(16) 0.065(11) 0.028(11) 0.022(9) 0.001(11) C26 0.036(9) 0.084(12) 0.047(9) 0.021(8) 0.007(8) -0.010(9) C31 0.035(8) 0.052(8) 0.028(7) 0.009(6) 0.007(6) -0.003(7) C41 0.038(8) 0.050(9) 0.052(8) 0.008(7) 0.026(7) -0.010(8) C42 0.044(10) 0.041(8) 0.059(10) 0.009(7) 0.019(8) -0.012(7) C43 0.035(10) 0.069(12) 0.095(14) 0.001(11) 0.035(10) 0.004(9) C44 0.058(13) 0.055(12) 0.13(2) 0.048(13) 0.017(13) 0.000(11) C45 0.071(16) 0.087(15) 0.092(16) 0.043(14) 0.009(14) 0.007(14) C46 0.050(11) 0.066(11) 0.059(10) 0.024(9) 0.018(9) -0.003(9) C51 0.039(9) 0.059(10) 0.042(8) -0.003(7) 0.026(7) -0.002(8) C52 0.043(10) 0.093(14) 0.052(10) 0.008(9) 0.036(8) -0.002(10) C53 0.045(11) 0.111(17) 0.079(14) 0.013(12) 0.032(11) 0.030(12) C54 0.044(12) 0.14(2) 0.082(15) 0.004(14) 0.049(11) -0.010(13) C55 0.052(13) 0.095(16) 0.121(19) 0.024(14) 0.059(13) 0.000(12) C56 0.043(10) 0.071(12) 0.081(13) 0.000(10) 0.030(10) 0.004(9) C61 0.044(10) 0.057(9) 0.042(8) -0.013(7) 0.025(7) 0.000(8) C0 0.27(5) 0.085(18) 0.11(2) -0.020(16) 0.10(3) 0.03(2) Cl1 0.157(7) 0.137(6) 0.125(6) -0.001(5) 0.094(6) -0.010(6) Cl2 0.48(3) 0.179(11) 0.206(13) -0.005(10) 0.075(16) 0.166(15) _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 Ir1 C 2.047(12) . ? Ir1 P2 2.294(3) . ? Ir1 P1 2.297(4) . ? Ir1 S1 2.439(4) . ? Ir1 S1 2.446(3) 2 ? Ir1 Cl 2.563(4) . ? Ir1 Ir1 3.1035(13) 2 ? S1 C1 1.817(14) . ? S1 Ir1 2.446(3) 2 ? P1 C21 1.827(15) . ? P1 C11 1.856(15) . ? P1 C31 1.863(14) . ? P2 C41 1.808(16) . ? P2 C51 1.826(16) . ? P2 C61 1.849(15) . ? C O 1.20(2) . ? C Ir1 2.047(12) 2 ? C1 C6 1.38(2) . ? C1 C2 1.39(2) . ? C2 C3 1.42(2) . ? C2 C61 1.49(2) . ? C3 C4 1.35(2) . ? C4 C5 1.39(2) . ? C5 C6 1.39(2) . ? C6 C31 1.47(2) 2 ? C11 C12 1.32(2) . ? C11 C16 1.39(2) . ? C12 C13 1.39(2) . ? C13 C14 1.39(3) . ? C14 C15 1.34(3) . ? C15 C16 1.38(2) . ? C21 C22 1.32(3) . ? C21 C26 1.42(2) . ? C22 C23 1.40(2) . ? C23 C24 1.34(3) . ? C24 C25 1.34(3) . ? C25 C26 1.38(2) . ? C31 C6 1.47(2) 2 ? C41 C42 1.38(2) . ? C41 C46 1.40(2) . ? C42 C43 1.41(2) . ? C43 C44 1.39(3) . ? C44 C45 1.35(3) . ? C45 C46 1.36(3) . ? C51 C52 1.38(3) . ? C51 C56 1.40(2) . ? C52 C53 1.38(2) . ? C53 C54 1.32(3) . ? C54 C55 1.39(3) . ? C55 C56 1.38(2) . ? C0 Cl2 1.55(3) . ? C0 Cl1 1.82(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 C Ir1 P2 99.4(3) . . ? C Ir1 P1 104.7(3) . . ? P2 Ir1 P1 97.04(13) . . ? C Ir1 S1 78.8(3) . . ? P2 Ir1 S1 92.58(12) . . ? P1 Ir1 S1 168.99(12) . . ? C Ir1 S1 78.7(3) . 2 ? P2 Ir1 S1 171.40(12) . 2 ? P1 Ir1 S1 91.55(12) . 2 ? S1 Ir1 S1 78.83(13) . 2 ? C Ir1 Cl 161.9(4) . . ? P2 Ir1 Cl 92.36(13) . . ? P1 Ir1 Cl 87.27(13) . . ? S1 Ir1 Cl 87.00(13) . . ? S1 Ir1 Cl 87.67(12) 2 . ? C Ir1 Ir1 40.7(4) . 2 ? P2 Ir1 Ir1 123.18(10) . 2 ? P1 Ir1 Ir1 126.06(10) . 2 ? S1 Ir1 Ir1 50.67(8) . 2 ? S1 Ir1 Ir1 50.46(9) 2 2 ? Cl Ir1 Ir1 121.24(10) . 2 ? C1 S1 Ir1 114.9(5) . . ? C1 S1 Ir1 109.4(5) . 2 ? Ir1 S1 Ir1 78.87(10) . 2 ? C21 P1 C11 102.7(8) . . ? C21 P1 C31 102.9(8) . . ? C11 P1 C31 100.1(6) . . ? C21 P1 Ir1 118.5(6) . . ? C11 P1 Ir1 124.1(5) . . ? C31 P1 Ir1 105.1(5) . . ? C41 P2 C51 101.7(7) . . ? C41 P2 C61 108.4(7) . . ? C51 P2 C61 95.6(7) . . ? C41 P2 Ir1 116.1(5) . . ? C51 P2 Ir1 124.4(5) . . ? C61 P2 Ir1 108.2(5) . . ? O C Ir1 130.7(4) . 2 ? O C Ir1 130.7(4) . . ? Ir1 C Ir1 98.6(8) 2 . ? C6 C1 C2 122.7(13) . . ? C6 C1 S1 119.0(11) . . ? C2 C1 S1 118.0(11) . . ? C1 C2 C3 115.8(15) . . ? C1 C2 C61 125.5(13) . . ? C3 C2 C61 118.8(14) . . ? C4 C3 C2 123.1(16) . . ? C3 C4 C5 118.9(15) . . ? C4 C5 C6 121.0(16) . . ? C1 C6 C5 118.4(14) . . ? C1 C6 C31 122.1(13) . 2 ? C5 C6 C31 119.3(14) . 2 ? C12 C11 C16 118.7(14) . . ? C12 C11 P1 122.0(12) . . ? C16 C11 P1 119.0(12) . . ? C11 C12 C13 120.6(17) . . ? C12 C13 C14 120(2) . . ? C15 C14 C13 119.4(19) . . ? C14 C15 C16 119.1(18) . . ? C15 C16 C11 121.8(17) . . ? C22 C21 C26 119.4(15) . . ? C22 C21 P1 122.2(14) . . ? C26 C21 P1 118.2(14) . . ? C21 C22 C23 120.8(19) . . ? C24 C23 C22 121(2) . . ? C25 C24 C23 119.1(19) . . ? C24 C25 C26 122(2) . . ? C25 C26 C21 117.7(18) . . ? C6 C31 P1 108.7(10) 2 . ? C42 C41 C46 118.3(15) . . ? C42 C41 P2 120.2(12) . . ? C46 C41 P2 121.4(13) . . ? C41 C42 C43 119.9(16) . . ? C44 C43 C42 120(2) . . ? C45 C44 C43 119.7(19) . . ? C44 C45 C46 122(2) . . ? C45 C46 C41 120.6(19) . . ? C52 C51 C56 118.1(15) . . ? C52 C51 P2 119.9(13) . . ? C56 C51 P2 121.4(13) . . ? C53 C52 C51 118.3(18) . . ? C54 C53 C52 124(2) . . ? C53 C54 C55 120.1(18) . . ? C56 C55 C54 117.8(19) . . ? C55 C56 C51 121.9(19) . . ? C2 C61 P2 116.7(10) . . ? Cl2 C0 Cl1 112.7(17) . . ? _refine_diff_density_max 5.687 _refine_diff_density_min -4.688 _refine_diff_density_rms 0.381 #===END data_(3) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C68.5 H65 Cl F12 Ni2 O P6 S2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68.50 H65 Cl F12 Ni2 O P6 S2' _chemical_formula_weight 1535.01 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.985(12) _cell_length_b 22.435(5) _cell_length_c 16.460(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.56(2) _cell_angle_gamma 90.00 _cell_volume 13869(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 17 _exptl_crystal_description brick _exptl_crystal_colour brown _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method ? _exptl_crystal_F_000 6296 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type '\y-scan (Enraf-Nonius, 1990)' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf-Nonius_CAD4 _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9750 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.01 _reflns_number_total 9587 _reflns_number_observed 5507 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 (Enraf-Nonius, 1989)' _computing_data_reduction 'Molen (Enraf-Nonius, 1980)' _computing_structure_solution 'SHELXS-92 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_publication_material 'Shelxl-93 (Sheldrick, 1996)' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1341P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9587 _refine_ls_number_parameters 822 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_obs 0.0616 _refine_ls_wR_factor_all 0.1899 _refine_ls_wR_factor_obs 0.1666 _refine_ls_goodness_of_fit_all 0.951 _refine_ls_goodness_of_fit_obs 1.136 _refine_ls_restrained_S_all 0.951 _refine_ls_restrained_S_obs 1.136 _refine_ls_shift/esd_max 0.012 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.10956(2) 0.27282(4) 0.33263(5) 0.0387(2) Uani 1 d . . Ni2 Ni 0.11857(2) 0.18280(4) 0.18929(5) 0.0376(2) Uani 1 d . . S1 S 0.08456(4) 0.25966(7) 0.19634(10) 0.0390(4) Uani 1 d . . S2 S 0.11814(4) 0.17765(8) 0.32235(10) 0.0400(4) Uani 1 d . . P11 P 0.14288(5) 0.27159(8) 0.46263(11) 0.0451(5) Uani 1 d . . P12 P 0.08326(5) 0.35868(8) 0.33047(11) 0.0429(5) Uani 1 d . . P21 P 0.13718(5) 0.09040(8) 0.19290(11) 0.0439(4) Uani 1 d . . P22 P 0.11621(5) 0.20801(8) 0.06040(10) 0.0432(5) Uani 1 d . . C11 C 0.08830(18) 0.3269(3) 0.1419(4) 0.0430(17) Uani 1 d . . C12 C 0.1076(2) 0.3321(3) 0.0830(4) 0.0486(18) Uani 1 d . . C13 C 0.1060(3) 0.3859(4) 0.0408(5) 0.075(3) Uani 1 d . . H13 H 0.1185 0.3899 0.0003 0.090 Uiso 1 calc R . C14 C 0.0867(3) 0.4331(4) 0.0562(6) 0.089(3) Uani 1 d . . H14 H 0.0856 0.4683 0.0258 0.107 Uiso 1 calc R . C15 C 0.0690(3) 0.4278(3) 0.1165(5) 0.073(3) Uani 1 d . . H15 H 0.0568 0.4607 0.1288 0.088 Uiso 1 calc R . C16 C 0.0685(2) 0.3753(3) 0.1607(4) 0.0498(18) Uani 1 d . . C17 C 0.1316(2) 0.2847(3) 0.0643(4) 0.0535(19) Uani 1 d . . H17A H 0.1542 0.2871 0.1067 0.064 Uiso 1 calc R . H17B H 0.1359 0.2939 0.0104 0.064 Uiso 1 calc R . C18 C 0.05026(19) 0.3705(3) 0.2281(4) 0.0514(18) Uani 1 d . . H18A H 0.0336 0.3374 0.2164 0.062 Uiso 1 calc R . H18B H 0.0369 0.4067 0.2302 0.062 Uiso 1 calc R . C21 C 0.15880(18) 0.1446(3) 0.3805(4) 0.0437(17) Uani 1 d . . C22 C 0.18552(18) 0.1751(3) 0.4404(4) 0.0485(18) Uani 1 d . . C23 C 0.2144(2) 0.1419(4) 0.4869(5) 0.067(2) Uani 1 d . . H23 H 0.2323 0.1607 0.5279 0.081 Uiso 1 calc R . C24 C 0.2167(2) 0.0832(5) 0.4731(5) 0.081(3) Uani 1 d . . H24 H 0.2358 0.0618 0.5063 0.097 Uiso 1 calc R . C25 C 0.1918(2) 0.0538(4) 0.4118(5) 0.073(3) Uani 1 d . . H25 H 0.1948 0.0137 0.4014 0.087 Uiso 1 calc R . C26 C 0.1620(2) 0.0843(3) 0.3652(4) 0.0524(19) Uani 1 d . . C27 C 0.18555(18) 0.2419(3) 0.4542(4) 0.0533(19) Uani 1 d . . H27A H 0.1918 0.2615 0.4077 0.064 Uiso 1 calc R . H27B H 0.2038 0.2515 0.5054 0.064 Uiso 1 calc R . C28 C 0.1356(2) 0.0552(3) 0.2927(4) 0.0535(19) Uani 1 d . . H28A H 0.1118 0.0591 0.3001 0.064 Uiso 1 calc R . H28B H 0.1410 0.0131 0.2912 0.064 Uiso 1 calc R . C111 C 0.12952(18) 0.2202(3) 0.5322(4) 0.0477(17) Uani 1 d . . C112 C 0.1546(2) 0.2006(4) 0.6067(5) 0.068(2) Uani 1 d . . H112 H 0.1775 0.2166 0.6205 0.082 Uiso 1 calc R . C113 C 0.1465(3) 0.1595(4) 0.6581(5) 0.080(3) Uani 1 d . . H113 H 0.1635 0.1463 0.7059 0.096 Uiso 1 calc R . C114 C 0.1124(3) 0.1376(4) 0.6375(6) 0.093(3) Uani 1 d . . H114 H 0.1061 0.1100 0.6731 0.111 Uiso 1 calc R . C115 C 0.0875(2) 0.1551(4) 0.5666(6) 0.076(3) Uani 1 d . . H115 H 0.0647 0.1389 0.5538 0.091 Uiso 1 calc R . C116 C 0.0958(2) 0.1959(3) 0.5149(5) 0.060(2) Uani 1 d . . H116 H 0.0786 0.2078 0.4668 0.071 Uiso 1 calc R . C121 C 0.1539(2) 0.3398(3) 0.5224(4) 0.0540(19) Uani 1 d . . C122 C 0.1317(3) 0.3591(4) 0.5702(5) 0.077(3) Uani 1 d . . H122 H 0.1127 0.3357 0.5753 0.092 Uiso 1 calc R . C123 C 0.1386(3) 0.4154(5) 0.6115(6) 0.099(4) Uani 1 d . . H123 H 0.1240 0.4284 0.6441 0.119 Uiso 1 calc R . C124 C 0.1659(3) 0.4504(5) 0.6043(7) 0.103(4) Uani 1 d . . H124 H 0.1698 0.4874 0.6307 0.124 Uiso 1 calc R . C125 C 0.1871(3) 0.4307(5) 0.5585(8) 0.113(4) Uani 1 d . . H125 H 0.2062 0.4545 0.5550 0.135 Uiso 1 calc R . C126 C 0.1821(3) 0.3761(4) 0.5152(6) 0.086(3) Uani 1 d . . H126 H 0.1971 0.3644 0.4827 0.103 Uiso 1 calc R . C211 C 0.1116(2) 0.4230(3) 0.3380(4) 0.0493(18) Uani 1 d . . C212 C 0.1443(2) 0.4148(4) 0.3267(6) 0.072(2) Uani 1 d . . H212 H 0.1526 0.3764 0.3223 0.086 Uiso 1 calc R . C213 C 0.1658(3) 0.4634(6) 0.3215(7) 0.107(4) Uani 1 d . . H213 H 0.1881 0.4578 0.3127 0.129 Uiso 1 calc R . C214 C 0.1533(4) 0.5205(5) 0.3296(7) 0.107(4) Uani 1 d . . H214 H 0.1677 0.5532 0.3279 0.128 Uiso 1 calc R . C215 C 0.1204(3) 0.5287(4) 0.3399(6) 0.093(3) Uani 1 d . . H215 H 0.1124 0.5673 0.3452 0.112 Uiso 1 calc R . C216 C 0.0983(2) 0.4810(4) 0.3426(5) 0.069(2) Uani 1 d . . H216 H 0.0753 0.4870 0.3474 0.083 Uiso 1 calc R . C221 C 0.05636(18) 0.3611(3) 0.4041(4) 0.0449(17) Uani 1 d . . C222 C 0.03334(19) 0.3127(3) 0.4013(5) 0.0556(19) Uani 1 d . . H222 H 0.0328 0.2819 0.3632 0.067 Uiso 1 calc R . C223 C 0.0115(2) 0.3103(4) 0.4547(5) 0.065(2) Uani 1 d . . H223 H -0.0036 0.2779 0.4527 0.078 Uiso 1 calc R . C224 C 0.0118(3) 0.3545(5) 0.5091(6) 0.083(3) Uani 1 d . . H224 H -0.0028 0.3527 0.5453 0.100 Uiso 1 calc R . C225 C 0.0337(3) 0.4025(4) 0.5117(6) 0.091(3) Uani 1 d . . H225 H 0.0337 0.4333 0.5495 0.110 Uiso 1 calc R . C226 C 0.0555(2) 0.4057(4) 0.4596(5) 0.074(2) Uani 1 d . . H226 H 0.0700 0.4389 0.4619 0.089 Uiso 1 calc R . C311 C 0.1830(2) 0.0756(4) 0.1945(5) 0.059(2) Uani 1 d . . C312 C 0.1947(3) 0.0192(4) 0.1829(6) 0.086(3) Uani 1 d . . H312 H 0.1784 -0.0116 0.1655 0.103 Uiso 1 calc R . C313 C 0.2302(4) 0.0082(6) 0.1968(8) 0.115(4) Uani 1 d . . H313 H 0.2383 -0.0300 0.1901 0.138 Uiso 1 calc R . C314 C 0.2531(3) 0.0528(8) 0.2201(9) 0.130(5) Uani 1 d . . H314 H 0.2773 0.0451 0.2284 0.156 Uiso 1 calc R . C315 C 0.2428(3) 0.1095(7) 0.2325(7) 0.119(4) Uani 1 d . . H315 H 0.2599 0.1393 0.2492 0.142 Uiso 1 calc R . C316 C 0.2075(2) 0.1228(5) 0.2202(5) 0.077(3) Uani 1 d . . H316 H 0.1999 0.1611 0.2284 0.092 Uiso 1 calc R . C321 C 0.1085(2) 0.0443(3) 0.1122(4) 0.0463(17) Uani 1 d . . C322 C 0.0749(2) 0.0323(3) 0.1194(5) 0.060(2) Uani 1 d . . H322 H 0.0684 0.0455 0.1667 0.072 Uiso 1 calc R . C323 C 0.0505(2) 0.0007(4) 0.0566(6) 0.081(3) Uani 1 d . . H323 H 0.0280 -0.0080 0.0634 0.097 Uiso 1 calc R . C324 C 0.0589(3) -0.0171(5) -0.0125(6) 0.094(3) Uani 1 d . . H324 H 0.0424 -0.0375 -0.0547 0.113 Uiso 1 calc R . C325 C 0.0922(3) -0.0052(4) -0.0211(6) 0.089(3) Uani 1 d . . H325 H 0.0981 -0.0180 -0.0693 0.107 Uiso 1 calc R . C326 C 0.1176(3) 0.0258(3) 0.0412(5) 0.070(2) Uani 1 d . . H326 H 0.1401 0.0337 0.0345 0.084 Uiso 1 calc R . C411 C 0.1427(2) 0.1724(3) -0.0001(5) 0.057(2) Uani 1 d . . C412 C 0.1279(3) 0.1406(4) -0.0721(5) 0.069(2) Uani 1 d . . H412 H 0.1033 0.1351 -0.0900 0.083 Uiso 1 calc R . C413 C 0.1498(3) 0.1163(4) -0.1189(6) 0.090(3) Uani 1 d . . H413 H 0.1396 0.0949 -0.1678 0.108 Uiso 1 calc R . C414 C 0.1850(4) 0.1232(5) -0.0947(8) 0.109(4) Uani 1 d . . H414 H 0.1992 0.1076 -0.1267 0.130 Uiso 1 calc R . C415 C 0.1996(3) 0.1532(6) -0.0229(8) 0.111(4) Uani 1 d . . H415 H 0.2242 0.1573 -0.0052 0.133 Uiso 1 calc R . C416 C 0.1793(3) 0.1780(4) 0.0253(6) 0.082(3) Uani 1 d . . H416 H 0.1902 0.1984 0.0747 0.098 Uiso 1 calc R . C421 C 0.0707(2) 0.2077(3) -0.0071(4) 0.0506(18) Uani 1 d . . C422 C 0.0614(2) 0.2459(4) -0.0760(5) 0.072(2) Uani 1 d . . H422 H 0.0779 0.2723 -0.0874 0.086 Uiso 1 calc R . C423 C 0.0257(3) 0.2434(5) -0.1288(5) 0.090(3) Uani 1 d . . H423 H 0.0182 0.2688 -0.1748 0.108 Uiso 1 calc R . C424 C 0.0030(3) 0.2032(5) -0.1105(7) 0.091(3) Uani 1 d . . H424 H -0.0203 0.2014 -0.1443 0.109 Uiso 1 calc R . C425 C 0.0133(2) 0.1661(5) -0.0450(7) 0.095(3) Uani 1 d . . H425 H -0.0028 0.1381 -0.0353 0.114 Uiso 1 calc R . C426 C 0.0463(2) 0.1684(4) 0.0073(5) 0.066(2) Uani 1 d . . H426 H 0.0526 0.1430 0.0536 0.079 Uiso 1 calc R . P01 P 0.22954(8) 0.31168(16) 0.25718(19) 0.0993(9) Uani 1 d . . F11 F 0.2306(2) 0.2736(4) 0.1814(5) 0.180(4) Uani 1 d . . F12 F 0.2078(2) 0.3597(4) 0.1943(5) 0.179(4) Uani 1 d . . F13 F 0.2499(2) 0.2657(3) 0.3252(5) 0.149(3) Uani 1 d . . F14 F 0.2239(2) 0.3503(4) 0.3338(4) 0.150(3) Uani 1 d . . F15 F 0.19330(18) 0.2775(4) 0.2558(4) 0.157(3) Uani 1 d . . F16 F 0.2645(2) 0.3437(4) 0.2609(6) 0.187(4) Uani 1 d . . P02 P 0.0000 0.13156(15) 0.2500 0.0763(10) Uani 1 d S . F21 F 0.0260(3) 0.1770(5) 0.2803(13) 0.312(9) Uani 1 d . . F22 F -0.0102(12) 0.1422(8) 0.3241(17) 0.32(2) Uani 0.50 d P . F23 F 0.0017(6) 0.0937(9) 0.1741(10) 0.155(6) Uani 0.50 d P . F24 F 0.0314(3) 0.0876(5) 0.2786(11) 0.253(6) Uani 1 d . . P03 P 0.0000 0.43505(16) 0.7500 0.0821(11) Uani 1 d S . F31 F 0.0268(2) 0.4312(4) 0.8390(4) 0.166(3) Uani 1 d . . F32 F 0.0332(2) 0.4385(5) 0.7147(5) 0.171(3) Uani 1 d . . F33 F -0.0019(14) 0.5009(5) 0.768(3) 0.186(12) Uani 0.50 d P . F34 F 0.0075(7) 0.3704(5) 0.7227(9) 0.157(9) Uani 0.50 d P . C01 C 0.1029(6) 0.2979(10) 0.7572(13) 0.236(10) Uiso 1 d . . H01A H 0.0975 0.2630 0.7225 0.353 Uiso 1 calc R . H01B H 0.0998 0.3327 0.7220 0.353 Uiso 1 calc R . H01C H 0.0872 0.3001 0.7931 0.353 Uiso 1 calc R . C02 C 0.1356(6) 0.2953(9) 0.8029(14) 0.191(8) Uiso 1 d . . H02A H 0.1345 0.2563 0.8278 0.229 Uiso 1 calc R . H02B H 0.1468 0.2875 0.7581 0.229 Uiso 1 calc R . O01 O 0.1577(6) 0.3116(9) 0.8474(14) 0.283(9) Uiso 1 d . . C03 C 0.1935(5) 0.3267(7) 0.9093(10) 0.162(6) Uiso 1 d . . H03A H 0.2089 0.3380 0.8744 0.195 Uiso 1 calc R . H03B H 0.2027 0.2890 0.9352 0.195 Uiso 1 calc R . C04 C 0.2017(8) 0.3755(14) 0.987(2) 0.378(17) Uiso 1 d . . H04A H 0.2267 0.3753 1.0156 0.567 Uiso 1 calc R . H04B H 0.1884 0.3651 1.0265 0.567 Uiso 1 calc R . H04C H 0.1949 0.4146 0.9650 0.567 Uiso 1 calc R . Cl Cl 0.03832(12) 0.08173(19) 0.7597(3) 0.1593(14) Uiso 1 d . . C0 C 0.0105(6) 0.0537(11) 0.7858(13) 0.120(8) Uiso 0.50 d P . H0A H 0.0167 0.0139 0.8078 0.144 Uiso 0.50 calc PR . H0B H 0.0021 0.0774 0.8259 0.144 Uiso 0.50 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 Ni1 0.0430(5) 0.0411(5) 0.0304(4) -0.0035(4) 0.0072(4) 0.0028(4) Ni2 0.0413(5) 0.0402(5) 0.0306(4) -0.0003(4) 0.0084(4) 0.0044(4) S1 0.0443(10) 0.0389(9) 0.0320(8) -0.0007(7) 0.0074(7) 0.0030(8) S2 0.0428(10) 0.0447(10) 0.0306(9) -0.0010(7) 0.0067(7) 0.0041(8) P11 0.0455(11) 0.0541(11) 0.0329(9) -0.0053(8) 0.0057(8) -0.0022(9) P12 0.0462(11) 0.0423(10) 0.0397(10) -0.0047(8) 0.0107(8) 0.0011(8) P21 0.0501(11) 0.0420(10) 0.0398(10) 0.0018(8) 0.0126(8) 0.0043(9) P22 0.0491(12) 0.0479(11) 0.0312(9) -0.0011(8) 0.0087(8) 0.0015(9) C11 0.056(4) 0.038(4) 0.031(3) 0.002(3) 0.004(3) 0.000(3) C12 0.064(5) 0.041(4) 0.038(4) 0.003(3) 0.009(4) -0.005(4) C13 0.108(8) 0.063(6) 0.056(5) 0.009(4) 0.025(5) -0.011(5) C14 0.138(10) 0.054(6) 0.086(7) 0.023(5) 0.049(7) 0.015(6) C15 0.108(7) 0.047(5) 0.055(5) 0.011(4) 0.005(5) 0.021(5) C16 0.060(5) 0.042(4) 0.039(4) -0.006(3) -0.001(3) 0.005(4) C17 0.060(5) 0.065(5) 0.037(4) 0.010(4) 0.015(3) -0.004(4) C18 0.049(4) 0.056(5) 0.045(4) -0.005(3) 0.005(3) 0.012(4) C21 0.040(4) 0.054(5) 0.035(4) 0.004(3) 0.007(3) 0.010(3) C22 0.043(4) 0.066(5) 0.033(4) 0.001(3) 0.003(3) 0.008(4) C23 0.050(5) 0.096(7) 0.049(5) -0.004(5) 0.002(4) 0.015(5) C24 0.072(7) 0.106(8) 0.056(6) 0.007(5) 0.002(5) 0.037(6) C25 0.083(7) 0.068(6) 0.062(5) 0.014(5) 0.010(5) 0.033(5) C26 0.059(5) 0.057(5) 0.040(4) 0.019(4) 0.012(4) 0.013(4) C27 0.037(4) 0.076(5) 0.044(4) -0.009(4) 0.005(3) -0.004(4) C28 0.078(5) 0.037(4) 0.048(4) 0.002(3) 0.020(4) 0.003(4) C111 0.047(5) 0.058(5) 0.039(4) -0.005(3) 0.014(3) 0.003(4) C112 0.059(5) 0.089(6) 0.052(5) 0.007(4) 0.009(4) -0.005(5) C113 0.077(7) 0.100(7) 0.059(5) 0.032(5) 0.012(5) 0.004(6) C114 0.106(9) 0.093(8) 0.082(7) 0.037(6) 0.031(6) -0.012(6) C115 0.069(6) 0.081(6) 0.087(7) 0.009(5) 0.036(6) -0.010(5) C116 0.048(5) 0.069(5) 0.062(5) 0.000(4) 0.016(4) 0.009(4) C121 0.061(5) 0.058(5) 0.036(4) -0.010(3) 0.002(4) -0.002(4) C122 0.098(7) 0.074(6) 0.056(5) -0.017(5) 0.017(5) 0.008(5) C123 0.128(10) 0.092(8) 0.062(6) -0.022(6) 0.002(6) 0.025(7) C124 0.110(10) 0.082(8) 0.097(8) -0.045(7) -0.009(7) 0.003(7) C125 0.118(10) 0.071(7) 0.138(10) -0.046(7) 0.014(8) -0.032(7) C126 0.078(7) 0.079(7) 0.096(7) -0.015(6) 0.017(5) -0.020(5) C211 0.061(5) 0.047(4) 0.041(4) -0.004(3) 0.016(4) -0.004(4) C212 0.073(6) 0.054(5) 0.098(7) 0.004(5) 0.039(5) -0.008(4) C213 0.090(8) 0.109(9) 0.134(10) 0.011(8) 0.050(7) -0.033(7) C214 0.144(11) 0.072(7) 0.118(9) -0.010(6) 0.059(8) -0.056(8) C215 0.153(11) 0.055(6) 0.087(7) -0.005(5) 0.060(7) -0.022(6) C216 0.083(6) 0.052(5) 0.076(6) 0.003(4) 0.026(5) 0.004(5) C221 0.046(4) 0.044(4) 0.047(4) -0.001(3) 0.016(3) -0.003(3) C222 0.059(5) 0.051(5) 0.055(4) 0.006(4) 0.011(4) 0.006(4) C223 0.063(5) 0.072(6) 0.065(5) 0.014(5) 0.024(4) -0.005(4) C224 0.079(7) 0.105(8) 0.079(7) 0.017(6) 0.044(6) 0.015(6) C225 0.134(9) 0.080(7) 0.085(7) -0.016(5) 0.071(7) -0.014(7) C226 0.094(7) 0.071(6) 0.064(5) -0.027(5) 0.034(5) -0.017(5) C311 0.058(5) 0.061(5) 0.058(5) 0.000(4) 0.016(4) 0.012(4) C312 0.084(7) 0.085(7) 0.086(7) 0.001(5) 0.018(5) 0.045(6) C313 0.100(10) 0.120(10) 0.126(10) -0.010(8) 0.033(8) 0.055(8) C314 0.071(9) 0.194(16) 0.131(11) -0.008(11) 0.035(8) 0.056(10) C315 0.057(7) 0.180(14) 0.119(10) -0.010(9) 0.023(6) 0.008(8) C316 0.045(5) 0.107(7) 0.080(6) -0.006(5) 0.020(5) 0.002(5) C321 0.061(5) 0.037(4) 0.044(4) -0.002(3) 0.019(4) 0.002(3) C322 0.065(6) 0.060(5) 0.052(5) -0.004(4) 0.009(4) 0.006(4) C323 0.066(6) 0.085(7) 0.076(7) -0.008(5) -0.007(5) -0.004(5) C324 0.110(9) 0.092(7) 0.057(6) -0.001(5) -0.016(6) -0.027(7) C325 0.134(10) 0.078(7) 0.052(5) -0.016(5) 0.021(6) -0.010(7) C326 0.104(7) 0.056(5) 0.054(5) -0.009(4) 0.026(5) -0.005(5) C411 0.068(6) 0.063(5) 0.042(4) 0.017(4) 0.019(4) 0.010(4) C412 0.095(7) 0.073(6) 0.043(5) 0.001(4) 0.024(5) 0.015(5) C413 0.147(11) 0.079(7) 0.058(6) -0.003(5) 0.051(7) 0.044(7) C414 0.131(11) 0.111(9) 0.105(9) 0.012(7) 0.067(9) 0.054(9) C415 0.084(8) 0.145(11) 0.122(10) -0.007(8) 0.061(8) 0.026(7) C416 0.072(7) 0.095(7) 0.081(6) -0.003(5) 0.026(5) 0.013(5) C421 0.054(5) 0.053(4) 0.039(4) -0.001(3) 0.003(3) 0.007(4) C422 0.075(6) 0.081(6) 0.050(5) 0.000(4) 0.000(4) 0.009(5) C423 0.097(8) 0.095(7) 0.052(5) -0.004(5) -0.025(5) 0.034(6) C424 0.064(7) 0.088(7) 0.097(8) -0.018(6) -0.020(6) 0.006(6) C425 0.052(6) 0.091(7) 0.121(9) 0.003(7) -0.013(6) -0.012(5) C426 0.049(5) 0.066(5) 0.074(6) 0.007(4) -0.001(4) 0.004(4) P01 0.079(2) 0.129(3) 0.0773(18) -0.0087(19) 0.0001(15) -0.0208(18) F11 0.199(9) 0.221(9) 0.129(6) -0.082(6) 0.059(6) -0.028(7) F12 0.183(8) 0.191(9) 0.131(6) 0.037(6) -0.012(6) 0.001(7) F13 0.130(6) 0.144(6) 0.144(6) 0.018(5) -0.013(5) 0.014(5) F14 0.129(6) 0.200(8) 0.103(5) -0.040(5) 0.005(4) 0.014(5) F15 0.098(5) 0.242(9) 0.116(5) 0.017(5) 0.002(4) -0.059(6) F16 0.101(5) 0.210(9) 0.240(10) 0.004(7) 0.031(6) -0.068(6) P02 0.077(2) 0.054(2) 0.105(3) 0.000 0.038(2) 0.000 F21 0.140(8) 0.151(9) 0.60(3) -0.073(14) 0.021(12) -0.075(7) F22 0.76(7) 0.093(12) 0.25(3) -0.002(16) 0.39(4) 0.01(3) F23 0.21(2) 0.152(15) 0.104(12) -0.070(12) 0.042(13) -0.003(15) F24 0.201(11) 0.191(11) 0.342(19) -0.003(11) 0.031(13) 0.078(9) P03 0.108(3) 0.071(2) 0.072(2) 0.000 0.031(2) 0.000 F31 0.153(7) 0.231(10) 0.092(5) 0.023(5) -0.004(4) -0.032(7) F32 0.141(7) 0.249(11) 0.141(7) -0.004(6) 0.070(6) 0.036(7) F33 0.233(19) 0.089(8) 0.27(4) -0.07(2) 0.13(2) 0.05(2) F34 0.26(2) 0.062(7) 0.118(17) -0.036(7) -0.005(15) 0.019(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S2 2.1748(19) . ? Ni1 P12 2.178(2) . ? Ni1 P11 2.185(2) . ? Ni1 S1 2.2128(18) . ? Ni1 Ni2 3.1959(12) . ? Ni2 P22 2.1736(19) . ? Ni2 P21 2.192(2) . ? Ni2 S1 2.1972(18) . ? Ni2 S2 2.1978(17) . ? S1 C11 1.781(6) . ? S2 C21 1.780(7) . ? P11 C111 1.797(7) . ? P11 C121 1.808(7) . ? P11 C27 1.832(7) . ? P12 C211 1.803(7) . ? P12 C221 1.804(7) . ? P12 C18 1.844(7) . ? P21 C311 1.809(8) . ? P21 C321 1.813(7) . ? P21 C28 1.839(7) . ? P22 C411 1.802(8) . ? P22 C17 1.816(7) . ? P22 C421 1.822(7) . ? C11 C12 1.383(9) . ? C11 C16 1.415(9) . ? C12 C13 1.385(10) . ? C12 C17 1.501(10) . ? C13 C14 1.361(12) . ? C14 C15 1.358(12) . ? C15 C16 1.388(10) . ? C16 C18 1.472(9) . ? C21 C26 1.387(10) . ? C21 C22 1.406(9) . ? C22 C23 1.396(10) . ? C22 C27 1.514(10) . ? C23 C24 1.345(12) . ? C24 C25 1.367(12) . ? C25 C26 1.388(10) . ? C26 C28 1.501(10) . ? C111 C116 1.380(10) . ? C111 C112 1.419(10) . ? C112 C113 1.344(11) . ? C113 C114 1.374(12) . ? C114 C115 1.360(12) . ? C115 C116 1.349(11) . ? C121 C122 1.386(11) . ? C121 C126 1.399(11) . ? C122 C123 1.424(13) . ? C123 C124 1.355(15) . ? C124 C125 1.335(15) . ? C125 C126 1.405(13) . ? C211 C212 1.350(10) . ? C211 C216 1.411(10) . ? C212 C213 1.390(12) . ? C213 C214 1.387(15) . ? C214 C215 1.353(14) . ? C215 C216 1.381(12) . ? C221 C226 1.363(9) . ? C221 C222 1.401(9) . ? C222 C223 1.380(10) . ? C223 C224 1.333(12) . ? C224 C225 1.367(12) . ? C225 C226 1.361(11) . ? C311 C312 1.377(11) . ? C311 C316 1.413(11) . ? C312 C313 1.363(14) . ? C313 C314 1.327(17) . ? C314 C315 1.366(17) . ? C315 C316 1.372(13) . ? C321 C322 1.373(10) . ? C321 C326 1.373(10) . ? C322 C323 1.398(11) . ? C323 C324 1.329(13) . ? C324 C325 1.368(14) . ? C325 C326 1.405(12) . ? C411 C412 1.372(10) . ? C411 C416 1.380(11) . ? C412 C413 1.406(11) . ? C413 C414 1.331(15) . ? C414 C415 1.345(16) . ? C415 C416 1.380(12) . ? C421 C426 1.364(10) . ? C421 C422 1.390(10) . ? C422 C423 1.432(12) . ? C423 C424 1.352(14) . ? C424 C425 1.335(13) . ? C425 C426 1.344(11) . ? P01 F11 1.523(7) . ? P01 F16 1.526(7) . ? P01 F13 1.572(7) . ? P01 F12 1.574(8) . ? P01 F14 1.593(7) . ? P01 F15 1.602(7) . ? P02 F22 1.401(15) 2 ? P02 F22 1.401(15) . ? P02 F21 1.431(8) . ? P02 F21 1.431(8) 2 ? P02 F23 1.528(13) . ? P02 F23 1.528(13) 2 ? P02 F24 1.545(10) 2 ? P02 F24 1.545(10) . ? F22 F23 1.14(2) 2 ? F23 F22 1.14(2) 2 ? F23 F24 1.68(2) 2 ? F24 F23 1.68(2) 2 ? P03 F33 1.511(13) . ? P03 F33 1.511(13) 2_556 ? P03 F32 1.556(7) 2_556 ? P03 F32 1.556(8) . ? P03 F31 1.557(7) . ? P03 F31 1.557(7) 2_556 ? P03 F34 1.569(11) 2_556 ? P03 F34 1.569(11) . ? F33 F33 0.64(6) 2_556 ? F34 F34 1.19(3) 2_556 ? C01 C02 1.30(2) . ? C02 O01 1.04(3) . ? O01 C03 1.53(2) . ? C03 C04 1.65(3) . ? Cl C0 1.42(2) . ? Cl C0 1.95(2) 2_556 ? C0 C0 1.24(4) 2_556 ? C0 Cl 1.95(2) 2_556 ? 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 S2 Ni1 P12 161.56(8) . . ? S2 Ni1 P11 90.02(7) . . ? P12 Ni1 P11 100.41(7) . . ? S2 Ni1 S1 79.94(6) . . ? P12 Ni1 S1 91.38(7) . . ? P11 Ni1 S1 167.28(8) . . ? S2 Ni1 Ni2 43.32(5) . . ? P12 Ni1 Ni2 133.74(6) . . ? P11 Ni1 Ni2 124.10(6) . . ? S1 Ni1 Ni2 43.36(5) . . ? P22 Ni2 P21 101.52(7) . . ? P22 Ni2 S1 88.81(7) . . ? P21 Ni2 S1 160.20(8) . . ? P22 Ni2 S2 167.61(8) . . ? P21 Ni2 S2 90.82(7) . . ? S1 Ni2 S2 79.78(7) . . ? P22 Ni2 Ni1 124.88(6) . . ? P21 Ni2 Ni1 132.75(6) . . ? S1 Ni2 Ni1 43.75(5) . . ? S2 Ni2 Ni1 42.76(5) . . ? C11 S1 Ni2 120.4(2) . . ? C11 S1 Ni1 108.9(2) . . ? Ni2 S1 Ni1 92.89(7) . . ? C21 S2 Ni1 120.1(2) . . ? C21 S2 Ni2 108.3(2) . . ? Ni1 S2 Ni2 93.92(7) . . ? C111 P11 C121 105.3(3) . . ? C111 P11 C27 103.8(3) . . ? C121 P11 C27 105.2(3) . . ? C111 P11 Ni1 115.7(2) . . ? C121 P11 Ni1 120.9(3) . . ? C27 P11 Ni1 104.1(2) . . ? C211 P12 C221 112.7(3) . . ? C211 P12 C18 102.3(3) . . ? C221 P12 C18 102.8(3) . . ? C211 P12 Ni1 115.4(3) . . ? C221 P12 Ni1 111.8(2) . . ? C18 P12 Ni1 110.6(2) . . ? C311 P21 C321 108.5(4) . . ? C311 P21 C28 100.3(4) . . ? C321 P21 C28 104.3(3) . . ? C311 P21 Ni2 119.5(3) . . ? C321 P21 Ni2 112.7(2) . . ? C28 P21 Ni2 109.9(2) . . ? C411 P22 C17 101.9(3) . . ? C411 P22 C421 105.7(4) . . ? C17 P22 C421 106.4(3) . . ? C411 P22 Ni2 122.9(2) . . ? C17 P22 Ni2 106.5(2) . . ? C421 P22 Ni2 111.9(2) . . ? C12 C11 C16 121.5(6) . . ? C12 C11 S1 123.9(5) . . ? C16 C11 S1 114.6(5) . . ? C11 C12 C13 117.7(7) . . ? C11 C12 C17 124.7(6) . . ? C13 C12 C17 117.5(7) . . ? C14 C13 C12 122.5(8) . . ? C15 C14 C13 118.9(8) . . ? C14 C15 C16 122.6(8) . . ? C15 C16 C11 116.8(7) . . ? C15 C16 C18 122.3(7) . . ? C11 C16 C18 120.8(6) . . ? C12 C17 P22 117.5(5) . . ? C16 C18 P12 109.9(5) . . ? C26 C21 C22 121.1(6) . . ? C26 C21 S2 114.8(5) . . ? C22 C21 S2 124.0(5) . . ? C23 C22 C21 117.5(7) . . ? C23 C22 C27 118.5(7) . . ? C21 C22 C27 124.0(6) . . ? C24 C23 C22 120.7(8) . . ? C23 C24 C25 122.1(8) . . ? C24 C25 C26 119.6(8) . . ? C25 C26 C21 118.9(8) . . ? C25 C26 C28 121.3(7) . . ? C21 C26 C28 119.5(6) . . ? C22 C27 P11 114.0(5) . . ? C26 C28 P21 110.1(5) . . ? C116 C111 C112 117.0(7) . . ? C116 C111 P11 123.0(6) . . ? C112 C111 P11 120.0(6) . . ? C113 C112 C111 122.2(8) . . ? C112 C113 C114 117.7(8) . . ? C115 C114 C113 122.1(8) . . ? C116 C115 C114 119.9(9) . . ? C115 C116 C111 121.1(8) . . ? C122 C121 C126 119.4(8) . . ? C122 C121 P11 118.7(6) . . ? C126 C121 P11 121.6(6) . . ? C121 C122 C123 118.8(10) . . ? C124 C123 C122 121.7(11) . . ? C125 C124 C123 118.5(10) . . ? C124 C125 C126 123.6(11) . . ? C121 C126 C125 118.0(10) . . ? C212 C211 C216 120.6(7) . . ? C212 C211 P12 117.8(6) . . ? C216 C211 P12 120.9(6) . . ? C211 C212 C213 120.4(9) . . ? C214 C213 C212 119.2(10) . . ? C215 C214 C213 120.4(9) . . ? C214 C215 C216 121.2(9) . . ? C215 C216 C211 118.1(9) . . ? C226 C221 C222 117.5(7) . . ? C226 C221 P12 126.6(6) . . ? C222 C221 P12 115.9(5) . . ? C223 C222 C221 120.5(7) . . ? C224 C223 C222 120.2(8) . . ? C223 C224 C225 120.1(8) . . ? C226 C225 C224 120.7(9) . . ? C225 C226 C221 121.0(8) . . ? C312 C311 C316 120.5(8) . . ? C312 C311 P21 122.1(7) . . ? C316 C311 P21 116.8(6) . . ? C313 C312 C311 120.2(11) . . ? C314 C313 C312 119.2(12) . . ? C313 C314 C315 122.9(12) . . ? C314 C315 C316 120.3(12) . . ? C315 C316 C311 116.9(10) . . ? C322 C321 C326 119.0(7) . . ? C322 C321 P21 117.6(5) . . ? C326 C321 P21 123.2(6) . . ? C321 C322 C323 120.9(8) . . ? C324 C323 C322 120.6(10) . . ? C323 C324 C325 119.3(9) . . ? C324 C325 C326 121.7(9) . . ? C321 C326 C325 118.6(9) . . ? C412 C411 C416 118.1(8) . . ? C412 C411 P22 122.5(7) . . ? C416 C411 P22 119.4(7) . . ? C411 C412 C413 119.9(9) . . ? C414 C413 C412 121.4(10) . . ? C413 C414 C415 118.7(10) . . ? C414 C415 C416 122.4(11) . . ? C415 C416 C411 119.6(10) . . ? C426 C421 C422 119.9(7) . . ? C426 C421 P22 120.5(6) . . ? C422 C421 P22 119.6(6) . . ? C421 C422 C423 118.0(9) . . ? C424 C423 C422 118.6(9) . . ? C425 C424 C423 121.5(9) . . ? C424 C425 C426 121.5(10) . . ? C425 C426 C421 120.5(9) . . ? F11 P01 F16 94.4(5) . . ? F11 P01 F13 95.5(5) . . ? F16 P01 F13 90.4(5) . . ? F11 P01 F12 88.5(5) . . ? F16 P01 F12 91.2(5) . . ? F13 P01 F12 175.6(5) . . ? F11 P01 F14 173.8(5) . . ? F16 P01 F14 91.3(5) . . ? F13 P01 F14 86.8(4) . . ? F12 P01 F14 89.1(5) . . ? F11 P01 F15 86.4(5) . . ? F16 P01 F15 178.5(5) . . ? F13 P01 F15 88.4(4) . . ? F12 P01 F15 90.0(5) . . ? F14 P01 F15 87.9(4) . . ? F22 P02 F22 160.3(16) 2 . ? F22 P02 F21 80.9(15) 2 . ? F22 P02 F21 85.1(14) . . ? F22 P02 F21 85.1(13) 2 2 ? F22 P02 F21 80.9(15) . 2 ? F21 P02 F21 89.1(10) . 2 ? F22 P02 F23 45.4(10) 2 . ? F22 P02 F23 153.1(15) . . ? F21 P02 F23 120.0(13) . . ? F21 P02 F23 107.1(11) 2 . ? F22 P02 F23 153.1(15) 2 2 ? F22 P02 F23 45.4(10) . 2 ? F21 P02 F23 107.1(11) . 2 ? F21 P02 F23 120.0(13) 2 2 ? F23 P02 F23 112.4(18) . 2 ? F22 P02 F24 103.3(17) 2 2 ? F22 P02 F24 89.3(16) . 2 ? F21 P02 F24 172.7(9) . 2 ? F21 P02 F24 85.3(7) 2 2 ? F23 P02 F24 66.4(8) . 2 ? F23 P02 F24 71.9(8) 2 2 ? F22 P02 F24 89.3(15) 2 . ? F22 P02 F24 103.3(17) . . ? F21 P02 F24 85.3(7) . . ? F21 P02 F24 172.7(9) 2 . ? F23 P02 F24 71.9(8) . . ? F23 P02 F24 66.4(8) 2 . ? F24 P02 F24 100.6(10) 2 . ? F23 F22 P02 73.2(13) 2 . ? F22 F23 P02 61.4(10) 2 . ? F22 F23 F24 108.6(19) 2 2 ? P02 F23 F24 57.3(7) . 2 ? P02 F24 F23 56.3(6) . 2 ? F33 P03 F33 24(2) . 2_556 ? F33 P03 F32 77.9(14) . 2_556 ? F33 P03 F32 96.4(14) 2_556 2_556 ? F33 P03 F32 96.4(14) . . ? F33 P03 F32 77.9(14) 2_556 . ? F32 P03 F32 174.2(8) 2_556 . ? F33 P03 F31 86(2) . . ? F33 P03 F31 100(2) 2_556 . ? F32 P03 F31 93.8(4) 2_556 . ? F32 P03 F31 86.5(4) . . ? F33 P03 F31 100(2) . 2_556 ? F33 P03 F31 86(2) 2_556 2_556 ? F32 P03 F31 86.5(4) 2_556 2_556 ? F32 P03 F31 93.8(4) . 2_556 ? F31 P03 F31 173.6(7) . 2_556 ? F33 P03 F34 145.7(12) . 2_556 ? F33 P03 F34 169.0(14) 2_556 2_556 ? F32 P03 F34 72.7(9) 2_556 2_556 ? F32 P03 F34 113.0(10) . 2_556 ? F31 P03 F34 79.0(8) . 2_556 ? F31 P03 F34 95.1(8) 2_556 2_556 ? F33 P03 F34 169.0(14) . . ? F33 P03 F34 145.7(12) 2_556 . ? F32 P03 F34 113.0(10) 2_556 . ? F32 P03 F34 72.7(8) . . ? F31 P03 F34 95.1(8) . . ? F31 P03 F34 79.0(8) 2_556 . ? F34 P03 F34 44.7(12) 2_556 . ? F33 F33 P03 77.8(12) 2_556 . ? F34 F34 P03 67.6(6) 2_556 . ? O01 C02 C01 154(3) . . ? C02 O01 C03 170(3) . . ? O01 C03 C04 128.0(18) . . ? C0 Cl C0 39.4(14) . 2_556 ? C0 C0 Cl 94(2) 2_556 . ? C0 C0 Cl 46.3(17) 2_556 2_556 ? Cl C0 Cl 119.2(14) . 2_556 ? _refine_diff_density_max 0.974 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.098 #===END data_(4) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H28 Cl O P2 Rh' _chemical_formula_weight 640.85 _chemical_melting_point ? _chemical_compound_source ? 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' 'Rh' 'Rh' -1.1178 0.9187 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.094(5) _cell_length_b 16.450(3) _cell_length_c 14.604(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.20(2) _cell_angle_gamma 90.00 _cell_volume 2905.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description 'hexahedral plate' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method ? _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type 'Psi scan' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Enraf-Nonius_CAD4 _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6431 _diffrn_reflns_av_R_equivalents 0.1440 _diffrn_reflns_av_sigmaI/netI 0.1274 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.21 _reflns_number_total 5225 _reflns_number_observed 2560 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD-4 (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 (Enraf-Nonius, 1989)' _computing_data_reduction 'Molen (Enraf-Nonius, 1990)' _computing_structure_solution 'SHELXS-92 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1994)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1167P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5225 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1729 _refine_ls_R_factor_obs 0.0609 _refine_ls_wR_factor_all 0.1934 _refine_ls_wR_factor_obs 0.1496 _refine_ls_goodness_of_fit_all 0.957 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 0.957 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh Rh 0.06292(5) 0.03830(4) -0.23401(4) 0.0435(2) Uani 1 d . . P1 P 0.25116(16) 0.05015(13) -0.26471(14) 0.0430(5) Uani 1 d . . P2 P 0.12015(15) -0.03206(13) 0.18917(13) 0.0389(5) Uani 1 d . . Cl Cl 0.07482(18) 0.17104(13) -0.17061(18) 0.0645(7) Uani 1 d . . C C 0.0474(7) -0.0556(6) -0.2945(7) 0.070(3) Uani 1 d . . O O 0.0325(6) -0.1141(5) -0.3364(7) 0.121(3) Uani 1 d . . C11 C 0.3311(7) 0.0803(5) -0.1620(5) 0.048(2) Uani 1 d . . H11A H 0.4058 0.0946 -0.1799 0.058 Uiso 1 calc R . H11B H 0.2974 0.1278 -0.1345 0.058 Uiso 1 calc R . C12 C 0.3350(6) 0.0125(5) -0.0931(5) 0.0428(19) Uani 1 d . . C13 C 0.4268(6) -0.0372(5) -0.0851(5) 0.050(2) Uani 1 d . . H13 H 0.4877 -0.0280 -0.1224 0.060 Uiso 1 calc R . C14 C 0.4296(7) -0.0999(5) -0.0229(6) 0.050(2) Uani 1 d . . H14 H 0.4924 -0.1324 -0.0182 0.060 Uiso 1 calc R . C15 C 0.3406(6) -0.1149(5) 0.0319(5) 0.050(2) Uani 1 d . . H15 H 0.3435 -0.1574 0.0739 0.060 Uiso 1 calc R . C16 C 0.2467(6) -0.0678(5) 0.0260(5) 0.0406(18) Uani 1 d . . C17 C 0.2454(6) -0.0047(5) -0.0382(5) 0.0437(19) Uani 1 d . . H17 H 0.1819 0.0268 -0.0441 0.052 Uiso 1 calc R . C18 C 0.1447(6) -0.0865(5) 0.0811(5) 0.046(2) Uani 1 d . . H18A H 0.1459 -0.1441 0.0950 0.055 Uiso 1 calc R . H18B H 0.0812 -0.0770 0.0418 0.055 Uiso 1 calc R . C21 C 0.3313(6) -0.0374(5) -0.3026(5) 0.0406(17) Uani 1 d . . C22 C 0.4297(6) -0.0289(6) -0.3500(5) 0.052(2) Uani 1 d . . H22 H 0.4526 0.0225 -0.3683 0.062 Uiso 1 calc R . C23 C 0.4947(7) -0.0960(6) -0.3707(6) 0.059(2) Uani 1 d . . H23 H 0.5600 -0.0891 -0.4031 0.071 Uiso 1 calc R . C24 C 0.4631(7) -0.1723(6) -0.3437(6) 0.061(2) Uani 1 d . . H24 H 0.5072 -0.2169 -0.3574 0.074 Uiso 1 calc R . C25 C 0.3666(8) -0.1825(6) -0.2967(6) 0.059(2) Uani 1 d . . H25 H 0.3445 -0.2344 -0.2792 0.071 Uiso 1 calc R . C26 C 0.3012(7) -0.1156(5) -0.2748(6) 0.054(2) Uani 1 d . . H26 H 0.2367 -0.1231 -0.2413 0.065 Uiso 1 calc R . C31 C 0.2789(7) 0.1265(5) -0.3526(6) 0.052(2) Uani 1 d . . C32 C 0.3609(7) 0.1849(6) -0.3458(7) 0.064(3) Uani 1 d . . H32 H 0.4040 0.1890 -0.2931 0.077 Uiso 1 calc R . C33 C 0.3777(8) 0.2379(6) -0.4198(10) 0.090(4) Uani 1 d . . H33 H 0.4337 0.2765 -0.4168 0.108 Uiso 1 calc R . C34 C 0.3112(12) 0.2332(8) -0.4981(9) 0.094(5) Uani 1 d . . H34 H 0.3217 0.2692 -0.5465 0.112 Uiso 1 calc R . C35 C 0.2330(12) 0.1771(7) -0.5026(7) 0.088(4) Uani 1 d . . H35 H 0.1896 0.1736 -0.5552 0.105 Uiso 1 calc R . C36 C 0.2137(9) 0.1229(6) -0.4309(6) 0.070(3) Uani 1 d . . H36 H 0.1575 0.0846 -0.4355 0.084 Uiso 1 calc R . C41 C 0.1725(6) 0.0682(5) 0.1638(5) 0.0424(18) Uani 1 d . . C42 C 0.2820(6) 0.0927(5) 0.1812(6) 0.053(2) Uani 1 d . . H42 H 0.3289 0.0582 0.2136 0.064 Uiso 1 calc R . C43 C 0.3217(8) 0.1670(6) 0.1513(7) 0.063(2) Uani 1 d . . H43 H 0.3940 0.1826 0.1643 0.075 Uiso 1 calc R . C44 C 0.2535(9) 0.2174(6) 0.1026(7) 0.072(3) Uani 1 d . . H44 H 0.2795 0.2676 0.0827 0.086 Uiso 1 calc R . C45 C 0.1471(9) 0.1945(6) 0.0828(7) 0.077(3) Uani 1 d . . H45 H 0.1025 0.2284 0.0477 0.092 Uiso 1 calc R . C46 C 0.1059(7) 0.1224(5) 0.1143(6) 0.060(2) Uani 1 d . . H46 H 0.0325 0.1090 0.1026 0.072 Uiso 1 calc R . C51 C 0.2143(6) -0.0724(5) 0.2756(5) 0.0431(19) Uani 1 d . . C52 C 0.2239(7) -0.0305(6) 0.3567(6) 0.058(2) Uani 1 d . . H52 H 0.1838 0.0172 0.3652 0.069 Uiso 1 calc R . C53 C 0.2934(8) -0.0589(6) 0.4268(6) 0.070(3) Uani 1 d . . H53 H 0.2976 -0.0319 0.4827 0.083 Uiso 1 calc R . C54 C 0.3552(7) -0.1277(6) 0.4108(6) 0.057(2) Uani 1 d . . H54 H 0.4037 -0.1459 0.4559 0.068 Uiso 1 calc R . C55 C 0.3473(7) -0.1687(5) 0.3328(6) 0.053(2) Uani 1 d . . H55 H 0.3883 -0.2159 0.3247 0.064 Uiso 1 calc R . C56 C 0.2781(6) -0.1413(5) 0.2633(6) 0.049(2) Uani 1 d . . H56 H 0.2747 -0.1694 0.2082 0.058 Uiso 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 Rh 0.0395(4) 0.0460(4) 0.0451(4) -0.0028(3) 0.0016(2) 0.0000(3) P1 0.0432(11) 0.0457(13) 0.0400(11) 0.0003(10) 0.0053(9) -0.0011(9) P2 0.0372(10) 0.0421(11) 0.0375(10) -0.0008(10) 0.0003(8) 0.0042(9) Cl 0.0635(14) 0.0415(12) 0.0885(18) -0.0037(12) 0.0177(12) -0.0052(10) C 0.050(5) 0.069(7) 0.090(7) -0.040(6) 0.006(5) -0.002(5) O 0.081(5) 0.118(7) 0.164(9) -0.088(7) 0.007(5) -0.015(5) C11 0.050(5) 0.043(5) 0.052(5) -0.003(4) 0.003(4) -0.010(4) C12 0.040(4) 0.043(5) 0.045(5) -0.013(4) -0.002(3) -0.006(3) C13 0.037(4) 0.061(6) 0.051(5) -0.009(5) 0.006(3) -0.005(4) C14 0.048(5) 0.049(5) 0.052(5) -0.010(4) 0.004(4) 0.006(4) C15 0.058(5) 0.049(5) 0.043(5) -0.009(4) -0.004(4) 0.005(4) C16 0.045(4) 0.038(4) 0.039(4) -0.014(4) -0.003(3) -0.003(3) C17 0.034(4) 0.052(5) 0.045(5) -0.009(4) -0.001(3) 0.003(4) C18 0.042(4) 0.057(5) 0.040(4) -0.010(4) -0.004(3) 0.003(4) C21 0.042(4) 0.044(5) 0.036(4) 0.004(4) -0.005(3) 0.004(4) C22 0.042(4) 0.062(6) 0.052(5) 0.003(5) 0.003(4) 0.003(4) C23 0.045(5) 0.061(6) 0.070(6) -0.010(5) 0.017(4) 0.011(4) C24 0.063(6) 0.058(6) 0.062(6) -0.012(5) -0.007(5) 0.020(5) C25 0.075(6) 0.049(5) 0.053(6) -0.003(4) 0.000(5) -0.001(5) C26 0.052(5) 0.053(6) 0.056(5) -0.005(5) 0.007(4) -0.002(4) C31 0.055(5) 0.049(5) 0.052(5) 0.000(4) 0.012(4) 0.014(4) C32 0.040(5) 0.060(6) 0.093(7) 0.036(5) 0.010(5) 0.006(4) C33 0.055(6) 0.063(7) 0.152(12) 0.044(8) 0.042(7) 0.023(5) C34 0.114(10) 0.074(8) 0.093(10) 0.048(7) 0.055(8) 0.061(8) C35 0.161(12) 0.060(7) 0.041(6) 0.013(5) 0.014(7) 0.035(8) C36 0.110(8) 0.059(6) 0.041(5) -0.010(5) 0.000(5) 0.023(6) C41 0.043(4) 0.041(4) 0.043(4) 0.001(4) 0.010(3) 0.010(3) C42 0.039(5) 0.051(5) 0.069(6) 0.009(5) 0.008(4) 0.002(4) C43 0.060(6) 0.055(6) 0.073(6) 0.004(5) 0.006(5) -0.006(5) C44 0.092(8) 0.049(6) 0.076(7) 0.010(5) 0.013(6) -0.013(5) C45 0.109(9) 0.043(6) 0.079(8) 0.020(5) -0.002(7) 0.017(6) C46 0.065(6) 0.049(6) 0.066(6) -0.008(5) -0.014(5) 0.004(4) C51 0.042(4) 0.040(4) 0.047(5) 0.005(4) -0.002(4) -0.002(4) C52 0.070(6) 0.055(6) 0.048(5) -0.008(4) -0.008(4) 0.013(4) C53 0.097(8) 0.073(7) 0.038(5) -0.006(5) -0.020(5) -0.002(6) C54 0.051(5) 0.053(6) 0.067(6) 0.012(5) -0.009(4) 0.000(4) C55 0.051(5) 0.049(5) 0.060(6) 0.007(5) -0.001(4) 0.000(4) C56 0.049(5) 0.049(5) 0.048(5) 0.001(4) 0.000(4) 0.007(4) _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 Rh C 1.789(10) . ? Rh P2 2.313(2) 3 ? Rh P1 2.330(2) . ? Rh Cl 2.376(2) . ? P1 C21 1.823(8) . ? P1 C31 1.827(9) . ? P1 C11 1.849(8) . ? P2 C41 1.806(8) . ? P2 C51 1.822(8) . ? P2 C18 1.839(7) . ? P2 Rh 2.313(2) 3 ? C O 1.155(11) . ? C11 C12 1.503(11) . ? C12 C17 1.379(10) . ? C12 C13 1.383(11) . ? C13 C14 1.375(11) . ? C14 C15 1.366(11) . ? C15 C16 1.377(10) . ? C16 C17 1.399(11) . ? C16 C18 1.507(10) . ? C21 C22 1.387(11) . ? C21 C26 1.398(11) . ? C22 C23 1.388(11) . ? C23 C24 1.370(12) . ? C24 C25 1.367(12) . ? C25 C26 1.394(12) . ? C31 C32 1.384(12) . ? C31 C36 1.388(12) . ? C32 C33 1.405(14) . ? C33 C34 1.398(18) . ? C34 C35 1.323(17) . ? C35 C36 1.396(14) . ? C41 C46 1.400(11) . ? C41 C42 1.407(11) . ? C42 C43 1.384(12) . ? C43 C44 1.367(13) . ? C44 C45 1.370(13) . ? C45 C46 1.367(13) . ? C51 C52 1.375(11) . ? C51 C56 1.383(11) . ? C52 C53 1.402(12) . ? C53 C54 1.377(13) . ? C54 C55 1.327(12) . ? C55 C56 1.388(11) . ? 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 C Rh P2 90.1(3) . 3 ? C Rh P1 94.5(3) . . ? P2 Rh P1 174.23(8) 3 . ? C Rh Cl 172.8(4) . . ? P2 Rh Cl 89.27(8) 3 . ? P1 Rh Cl 86.57(8) . . ? C21 P1 C31 103.3(4) . . ? C21 P1 C11 100.4(4) . . ? C31 P1 C11 106.8(4) . . ? C21 P1 Rh 120.9(3) . . ? C31 P1 Rh 112.0(3) . . ? C11 P1 Rh 112.0(3) . . ? C41 P2 C51 104.8(4) . . ? C41 P2 C18 102.1(4) . . ? C51 P2 C18 108.3(4) . . ? C41 P2 Rh 115.8(2) . 3 ? C51 P2 Rh 112.6(3) . 3 ? C18 P2 Rh 112.3(2) . 3 ? O C Rh 176.1(10) . . ? C12 C11 P1 111.1(5) . . ? C17 C12 C13 117.5(8) . . ? C17 C12 C11 121.2(7) . . ? C13 C12 C11 121.2(7) . . ? C14 C13 C12 121.1(7) . . ? C15 C14 C13 120.3(8) . . ? C14 C15 C16 120.9(8) . . ? C15 C16 C17 117.9(7) . . ? C15 C16 C18 121.9(8) . . ? C17 C16 C18 120.1(7) . . ? C12 C17 C16 122.3(7) . . ? C16 C18 P2 119.6(5) . . ? C22 C21 C26 117.5(7) . . ? C22 C21 P1 122.1(6) . . ? C26 C21 P1 120.0(6) . . ? C21 C22 C23 121.1(8) . . ? C24 C23 C22 120.5(8) . . ? C25 C24 C23 119.8(8) . . ? C24 C25 C26 120.3(9) . . ? C25 C26 C21 120.8(8) . . ? C32 C31 C36 119.5(9) . . ? C32 C31 P1 124.1(7) . . ? C36 C31 P1 116.4(7) . . ? C31 C32 C33 118.8(10) . . ? C34 C33 C32 120.7(11) . . ? C35 C34 C33 119.2(10) . . ? C34 C35 C36 122.0(12) . . ? C31 C36 C35 119.7(11) . . ? C46 C41 C42 116.8(8) . . ? C46 C41 P2 119.0(6) . . ? C42 C41 P2 123.7(6) . . ? C43 C42 C41 121.5(8) . . ? C44 C43 C42 119.4(9) . . ? C43 C44 C45 120.5(9) . . ? C46 C45 C44 120.7(9) . . ? C45 C46 C41 121.1(9) . . ? C52 C51 C56 118.5(8) . . ? C52 C51 P2 117.7(6) . . ? C56 C51 P2 123.8(6) . . ? C51 C52 C53 120.7(9) . . ? C54 C53 C52 118.3(9) . . ? C55 C54 C53 121.7(8) . . ? C54 C55 C56 120.3(8) . . ? C51 C56 C55 120.4(8) . . ? _refine_diff_density_max 1.503 _refine_diff_density_min -1.381 _refine_diff_density_rms 0.143 #===END