# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_d8_10098 _database_code_depnum_ccdc_archive 'CCDC 863743' #TrackingRef '9134_web_deposit_cif_file_0_DanielTofan_1327008424.Ni2(P2dmb2)5-D8_10098.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H112 Ni2 P10' _chemical_formula_weight 1320.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3941(2) _cell_length_b 12.6121(2) _cell_length_c 14.3410(2) _cell_angle_alpha 66.0080(10) _cell_angle_beta 82.3230(10) _cell_angle_gamma 66.7130(10) _cell_volume 1728.51(5) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9798 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 69.01 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 3.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3030 _exptl_absorpt_correction_T_max 0.6504 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Bruker D8 three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 34473 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 68.24 _reflns_number_total 6166 _reflns_number_gt 5529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.9665P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6166 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Ni1 Ni 0.38043(3) 0.50075(3) 0.61115(3) 0.02364(12) Uani 1 1 d . . . P1 P 0.25154(5) 0.51878(5) 0.73204(4) 0.02565(14) Uani 1 1 d . A . P2 P 0.29235(6) 0.60837(6) 0.82252(5) 0.03503(16) Uani 1 1 d . . . C11 C 0.0799(2) 0.6252(2) 0.69335(18) 0.0357(5) Uani 1 1 d . . . H11A H 0.0783 0.7063 0.6405 0.043 Uiso 1 1 calc R A . H11B H 0.0435 0.5880 0.6615 0.043 Uiso 1 1 calc R . . C12 C -0.0058(2) 0.6506(2) 0.77786(18) 0.0379(5) Uani 1 1 d . A . C13 C 0.0204(2) 0.7064(3) 0.82903(19) 0.0413(6) Uani 1 1 d . . . C14 C 0.1353(3) 0.7435(3) 0.8028(2) 0.0438(6) Uani 1 1 d . A . H14A H 0.1360 0.7886 0.8452 0.053 Uiso 1 1 calc R . . H14B H 0.1262 0.8023 0.7304 0.053 Uiso 1 1 calc R . . C15 C 0.2756(3) 0.4990(3) 0.95436(18) 0.0425(6) Uani 1 1 d . A . H15A H 0.2981 0.5231 1.0052 0.051 Uiso 1 1 calc R . . H15B H 0.1856 0.5058 0.9640 0.051 Uiso 1 1 calc R . . C16 C 0.3609(2) 0.3663(3) 0.97152(18) 0.0414(6) Uani 1 1 d . . . C17 C 0.3377(2) 0.3097(2) 0.91925(18) 0.0385(6) Uani 1 1 d . A . C18 C 0.2276(2) 0.3827(2) 0.84092(18) 0.0353(5) Uani 1 1 d . . . H18A H 0.1475 0.4142 0.8748 0.042 Uiso 1 1 calc R A . H18B H 0.2183 0.3258 0.8136 0.042 Uiso 1 1 calc R . . C121 C -0.1157(2) 0.6067(3) 0.7975(2) 0.0489(7) Uani 1 1 d . . . H12A H -0.1671 0.6286 0.8522 0.073 Uiso 1 1 calc R A . H12B H -0.0822 0.5156 0.8179 0.073 Uiso 1 1 calc R . . H12C H -0.1692 0.6474 0.7351 0.073 Uiso 1 1 calc R . . C131 C -0.0524(3) 0.7313(3) 0.9195(2) 0.0520(7) Uani 1 1 d . A . H13A H -0.1272 0.7082 0.9297 0.078 Uiso 1 1 calc R . . H13B H -0.0805 0.8205 0.9061 0.078 Uiso 1 1 calc R . . H13C H 0.0034 0.6813 0.9809 0.078 Uiso 1 1 calc R . . C161 C 0.4704(3) 0.3082(4) 1.0478(2) 0.0623(9) Uani 1 1 d . A . H16A H 0.5259 0.2255 1.0484 0.093 Uiso 1 1 calc R . . H16B H 0.4366 0.2994 1.1159 0.093 Uiso 1 1 calc R . . H16C H 0.5197 0.3621 1.0285 0.093 Uiso 1 1 calc R . . C171 C 0.4118(3) 0.1764(3) 0.9312(2) 0.0538(7) Uani 1 1 d . . . H17A H 0.4804 0.1373 0.9830 0.081 Uiso 1 1 calc R A . H17B H 0.4488 0.1745 0.8659 0.081 Uiso 1 1 calc R . . H17C H 0.3545 0.1302 0.9524 0.081 Uiso 1 1 calc R . . P3 P 0.42329(10) 0.33400(9) 0.57937(8) 0.0235(2) Uani 0.50 1 d P A -1 P4 P 0.54882(10) 0.34198(10) 0.44552(8) 0.0235(2) Uani 0.50 1 d P . -1 C21 C 0.4966(7) 0.1592(6) 0.6588(5) 0.0299(14) Uani 0.50 1 d P A -1 H21A H 0.4677 0.1463 0.7295 0.036 Uiso 0.50 1 calc PR A -1 H21B H 0.4580 0.1180 0.6330 0.036 Uiso 0.50 1 calc PR A -1 C22 C 0.6384(16) 0.0886(13) 0.6657(12) 0.037(5) Uani 0.50 1 d P A -1 C23 C 0.710(2) 0.1057(16) 0.5911(16) 0.033(4) Uani 0.50 1 d P A -1 C24 C 0.6534(5) 0.1714(4) 0.4831(4) 0.0318(10) Uani 0.50 1 d P A -1 H24A H 0.6025 0.1273 0.4755 0.038 Uiso 0.50 1 calc PR A -1 H24B H 0.7243 0.1640 0.4349 0.038 Uiso 0.50 1 calc PR A -1 C25 C 0.4350(5) 0.3526(6) 0.3563(5) 0.0270(9) Uani 0.50 1 d P A -1 H25A H 0.3635 0.4351 0.3378 0.032 Uiso 0.50 1 calc PR A -1 H25B H 0.4798 0.3494 0.2928 0.032 Uiso 0.50 1 calc PR A -1 C26 C 0.3797(11) 0.2519(7) 0.3969(8) 0.0300(17) Uani 0.50 1 d P A -1 C27 C 0.3034(6) 0.2439(7) 0.4780(6) 0.0317(16) Uani 0.50 1 d P A -1 C28 C 0.2793(4) 0.3366(4) 0.5278(4) 0.0292(9) Uani 0.50 1 d P A -1 H28A H 0.2204 0.3204 0.5845 0.035 Uiso 0.50 1 calc PR A -1 H28B H 0.2348 0.4221 0.4768 0.035 Uiso 0.50 1 calc PR A -1 C221 C 0.6936(6) 0.0173(5) 0.7797(4) 0.0452(12) Uani 0.50 1 d P A -1 H22A H 0.6934 -0.0675 0.8073 0.068 Uiso 0.50 1 calc PR A -1 H22B H 0.6403 0.0628 0.8213 0.068 Uiso 0.50 1 calc PR A -1 H22C H 0.7814 0.0127 0.7811 0.068 Uiso 0.50 1 calc PR A -1 C231 C 0.8577(6) 0.0354(6) 0.5951(5) 0.0439(14) Uani 0.50 1 d P A -1 H23A H 0.8969 0.0926 0.5473 0.066 Uiso 0.50 1 calc PR A -1 H23B H 0.8779 -0.0361 0.5762 0.066 Uiso 0.50 1 calc PR A -1 H23C H 0.8913 0.0056 0.6645 0.066 Uiso 0.50 1 calc PR A -1 C261 C 0.4207(6) 0.1613(5) 0.3437(4) 0.0393(12) Uani 0.50 1 d P A -1 H26A H 0.3899 0.0932 0.3811 0.059 Uiso 0.50 1 calc PR A -1 H26B H 0.5142 0.1264 0.3419 0.059 Uiso 0.50 1 calc PR A -1 H26C H 0.3844 0.2056 0.2738 0.059 Uiso 0.50 1 calc PR A -1 C271 C 0.2403(5) 0.1518(5) 0.5244(4) 0.0352(11) Uani 0.50 1 d P A -1 H27A H 0.2634 0.0962 0.4875 0.053 Uiso 0.50 1 calc PR A -1 H27B H 0.1473 0.1965 0.5201 0.053 Uiso 0.50 1 calc PR A -1 H27C H 0.2686 0.1021 0.5962 0.053 Uiso 0.50 1 calc PR A -1 P5 P 0.56618(10) 0.48252(10) 0.65398(8) 0.0230(2) Uani 0.50 1 d P A -1 P6 P 0.70822(10) 0.47006(10) 0.53230(8) 0.0243(2) Uani 0.50 1 d P . -1 C31 C 0.6509(5) 0.3298(5) 0.7602(3) 0.0281(9) Uani 0.50 1 d P A -1 H31A H 0.6029 0.3287 0.8233 0.034 Uiso 0.50 1 calc PR A -1 H31B H 0.6476 0.2618 0.7441 0.034 Uiso 0.50 1 calc PR A -1 C32 C 0.7895(7) 0.3003(6) 0.7825(5) 0.0302(14) Uani 0.50 1 d P A -1 C33 C 0.8726(7) 0.2938(7) 0.7093(5) 0.0316(14) Uani 0.50 1 d P A -1 C34 C 0.8334(19) 0.3106(14) 0.6068(15) 0.035(3) Uani 0.50 1 d P A -1 H34A H 0.7998 0.2455 0.6167 0.042 Uiso 0.50 1 calc PR A -1 H34B H 0.9104 0.2964 0.5652 0.042 Uiso 0.50 1 calc PR A -1 C35 C 0.7907(4) 0.5672(5) 0.5429(4) 0.0345(10) Uani 0.50 1 d P A -1 H35A H 0.8422 0.5201 0.6077 0.041 Uiso 0.50 1 calc PR A -1 H35B H 0.8508 0.5779 0.4864 0.041 Uiso 0.50 1 calc PR A -1 C36 C 0.7039(6) 0.6969(7) 0.5403(5) 0.0311(13) Uani 0.50 1 d P A -1 C37 C 0.6148(10) 0.7043(9) 0.6128(7) 0.030(2) Uani 0.50 1 d P A -1 C38 C 0.6041(5) 0.5881(6) 0.6966(4) 0.0294(10) Uani 0.50 1 d P A -1 H38A H 0.5368 0.6142 0.7430 0.035 Uiso 0.50 1 calc PR A -1 H38B H 0.6859 0.5390 0.7367 0.035 Uiso 0.50 1 calc PR A -1 C321 C 0.8150(5) 0.2889(5) 0.8865(4) 0.0389(11) Uani 0.50 1 d P A -1 H32A H 0.9075 0.2565 0.8992 0.058 Uiso 0.50 1 calc PR A -1 H32B H 0.7790 0.2312 0.9380 0.058 Uiso 0.50 1 calc PR A -1 H32C H 0.7753 0.3714 0.8904 0.058 Uiso 0.50 1 calc PR A -1 C331 C 1.0123(5) 0.2678(6) 0.7204(4) 0.0448(12) Uani 0.50 1 d P A -1 H33A H 1.0299 0.2599 0.7884 0.067 Uiso 0.50 1 calc PR A -1 H33B H 1.0331 0.3370 0.6684 0.067 Uiso 0.50 1 calc PR A -1 H33C H 1.0647 0.1897 0.7114 0.067 Uiso 0.50 1 calc PR A -1 C361 C 0.7304(6) 0.8060(7) 0.4627(5) 0.0464(14) Uani 0.50 1 d P A -1 H36A H 0.6643 0.8838 0.4643 0.070 Uiso 0.50 1 calc PR A -1 H36B H 0.7302 0.8051 0.3947 0.070 Uiso 0.50 1 calc PR A -1 H36C H 0.8143 0.8008 0.4780 0.070 Uiso 0.50 1 calc PR A -1 C371 C 0.5305(6) 0.8289(5) 0.6194(5) 0.0444(13) Uani 0.50 1 d P A -1 H37A H 0.5828 0.8615 0.6405 0.067 Uiso 0.50 1 calc PR A -1 H37B H 0.4646 0.8171 0.6694 0.067 Uiso 0.50 1 calc PR A -1 H37C H 0.4898 0.8886 0.5523 0.067 Uiso 0.50 1 calc PR A -1 P7 P 0.31092(10) 0.65929(9) 0.48008(8) 0.0234(2) Uani 0.50 1 d P A -1 P8 P 0.45424(10) 0.66489(10) 0.35839(8) 0.0238(2) Uani 0.50 1 d P . -1 C41 C 0.1640(19) 0.7205(14) 0.4006(14) 0.035(3) Uani 0.50 1 d P A -1 H41A H 0.0944 0.7069 0.4473 0.042 Uiso 0.50 1 calc PR A -1 H41B H 0.1395 0.8122 0.3642 0.042 Uiso 0.50 1 calc PR A -1 C42 C 0.1695(7) 0.6673(7) 0.3233(5) 0.0314(14) Uani 0.50 1 d P A -1 C43 C 0.2564(6) 0.6748(6) 0.2478(5) 0.0268(13) Uani 0.50 1 d P A -1 C44 C 0.3465(4) 0.7376(6) 0.2435(3) 0.0297(9) Uani 0.50 1 d P A -1 H44A H 0.2952 0.8260 0.2331 0.036 Uiso 0.50 1 calc PR A -1 H44B H 0.4000 0.7377 0.1831 0.036 Uiso 0.50 1 calc PR A -1 C45 C 0.4799(7) 0.8057(6) 0.3515(5) 0.0299(14) Uani 0.50 1 d P A -1 H45A H 0.5154 0.7886 0.4178 0.036 Uiso 0.50 1 calc PR A -1 H45B H 0.5417 0.8248 0.2981 0.036 Uiso 0.50 1 calc PR A -1 C46 C 0.3550(18) 0.9148(16) 0.3269(14) 0.051(6) Uani 0.50 1 d P A -1 C47 C 0.266(2) 0.9232(16) 0.4064(12) 0.029(3) Uani 0.50 1 d P A -1 C48 C 0.2888(5) 0.8050(4) 0.4988(4) 0.0310(10) Uani 0.50 1 d P A -1 H48A H 0.2156 0.8205 0.5438 0.037 Uiso 0.50 1 calc PR A -1 H48B H 0.3658 0.7877 0.5360 0.037 Uiso 0.50 1 calc PR A -1 C421 C 0.0685(5) 0.6153(6) 0.3276(4) 0.0435(12) Uani 0.50 1 d P A -1 H42A H -0.0106 0.6842 0.2934 0.065 Uiso 0.50 1 calc PR A -1 H42B H 0.0520 0.5715 0.3990 0.065 Uiso 0.50 1 calc PR A -1 H42C H 0.0988 0.5566 0.2932 0.065 Uiso 0.50 1 calc PR A -1 C431 C 0.2668(5) 0.6303(5) 0.1646(4) 0.0376(11) Uani 0.50 1 d P A -1 H43A H 0.3562 0.5786 0.1597 0.056 Uiso 0.50 1 calc PR A -1 H43B H 0.2373 0.7025 0.0998 0.056 Uiso 0.50 1 calc PR A -1 H43C H 0.2139 0.5805 0.1796 0.056 Uiso 0.50 1 calc PR A -1 C461 C 0.3529(6) 1.0306(5) 0.2341(4) 0.0477(13) Uani 0.50 1 d P A -1 H46A H 0.3418 1.0204 0.1720 0.072 Uiso 0.50 1 calc PR A -1 H46B H 0.4337 1.0418 0.2320 0.072 Uiso 0.50 1 calc PR A -1 H46C H 0.2819 1.1043 0.2383 0.072 Uiso 0.50 1 calc PR A -1 C471 C 0.1448(7) 1.0277(6) 0.3978(5) 0.0546(17) Uani 0.50 1 d P A -1 H47A H 0.1452 1.1022 0.3383 0.082 Uiso 0.50 1 calc PR A -1 H47B H 0.1332 1.0453 0.4597 0.082 Uiso 0.50 1 calc PR A -1 H47C H 0.0745 1.0056 0.3896 0.082 Uiso 0.50 1 calc PR A -1 C1S C 0.8174(7) 0.0016(7) 1.0384(5) 0.0568(16) Uani 0.50 1 d P B -1 H1S1 H 0.7597 0.0571 0.9784 0.085 Uiso 0.50 1 calc PR B -1 H1S2 H 0.7738 0.0130 1.0993 0.085 Uiso 0.50 1 calc PR B -1 H1S3 H 0.8422 -0.0857 1.0468 0.085 Uiso 0.50 1 calc PR B -1 C2S C 0.9340(7) 0.0325(6) 1.0242(6) 0.0525(14) Uani 0.50 1 d P B -1 H2S1 H 0.9928 -0.0258 1.0843 0.063 Uiso 0.50 1 calc PR B -1 H2S2 H 0.9087 0.1184 1.0216 0.063 Uiso 0.50 1 calc PR B -1 C3S C 1.0048(7) 0.0248(6) 0.9285(5) 0.0497(14) Uani 0.50 1 d P B -1 H3S1 H 1.0304 -0.0614 0.9318 0.060 Uiso 0.50 1 calc PR B -1 H3S2 H 0.9451 0.0820 0.8689 0.060 Uiso 0.50 1 calc PR B -1 C4S C 1.1223(9) 0.0569(8) 0.9106(6) 0.0665(18) Uani 0.50 1 d P B -1 H4S1 H 1.0953 0.1469 0.8970 0.080 Uiso 0.50 1 calc PR B -1 H4S2 H 1.1763 0.0085 0.9741 0.080 Uiso 0.50 1 calc PR B -1 C5S C 1.2024(9) 0.0317(9) 0.8240(6) 0.085(3) Uani 0.50 1 d P B -1 H5S1 H 1.2509 -0.0585 0.8450 0.127 Uiso 0.50 1 calc PR B -1 H5S2 H 1.2618 0.0754 0.8058 0.127 Uiso 0.50 1 calc PR B -1 H5S3 H 1.1467 0.0619 0.7647 0.127 Uiso 0.50 1 calc PR B -1 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 0.0210(2) 0.0294(2) 0.0279(2) -0.01731(15) 0.00357(14) -0.01127(16) P1 0.0237(3) 0.0342(3) 0.0244(3) -0.0145(2) 0.0034(2) -0.0136(2) P2 0.0362(3) 0.0523(4) 0.0324(3) -0.0261(3) 0.0096(2) -0.0248(3) C11 0.0255(11) 0.0490(14) 0.0301(11) -0.0157(10) 0.0008(9) -0.0113(11) C12 0.0248(11) 0.0473(14) 0.0301(12) -0.0116(10) 0.0027(9) -0.0063(11) C13 0.0360(13) 0.0466(14) 0.0338(13) -0.0167(11) 0.0082(10) -0.0092(12) C14 0.0496(15) 0.0461(15) 0.0431(14) -0.0278(12) 0.0142(11) -0.0184(13) C15 0.0425(14) 0.0680(18) 0.0261(11) -0.0228(12) 0.0055(10) -0.0265(14) C16 0.0304(12) 0.0621(17) 0.0248(11) -0.0109(11) 0.0037(9) -0.0178(12) C17 0.0330(12) 0.0478(14) 0.0269(11) -0.0058(10) 0.0068(9) -0.0185(11) C18 0.0322(12) 0.0429(13) 0.0344(12) -0.0126(10) 0.0057(9) -0.0217(11) C121 0.0268(12) 0.0700(19) 0.0423(15) -0.0173(13) 0.0040(10) -0.0166(13) C131 0.0477(16) 0.0588(18) 0.0421(15) -0.0257(13) 0.0157(12) -0.0111(14) C161 0.0432(16) 0.101(3) 0.0318(14) -0.0206(15) -0.0022(12) -0.0212(17) C171 0.0611(18) 0.0477(16) 0.0354(14) -0.0056(12) 0.0075(12) -0.0163(15) P3 0.0249(5) 0.0237(5) 0.0247(5) -0.0105(4) 0.0028(4) -0.0113(4) P4 0.0251(5) 0.0240(5) 0.0243(5) -0.0112(4) 0.0020(4) -0.0106(4) C21 0.044(4) 0.019(3) 0.028(3) -0.006(2) 0.004(2) -0.017(2) C22 0.037(7) 0.029(6) 0.026(6) 0.016(4) -0.015(5) -0.017(5) C23 0.018(5) 0.017(7) 0.060(5) -0.022(5) -0.006(3) 0.008(6) C24 0.031(2) 0.029(2) 0.039(3) -0.019(2) 0.009(2) -0.011(2) C25 0.033(3) 0.028(3) 0.029(3) -0.015(2) 0.004(2) -0.017(3) C26 0.035(3) 0.027(4) 0.036(3) -0.015(4) -0.005(2) -0.014(4) C27 0.031(3) 0.031(3) 0.042(4) -0.021(4) -0.002(3) -0.013(3) C28 0.024(2) 0.033(2) 0.039(3) -0.019(2) 0.0014(18) -0.014(2) C221 0.046(3) 0.036(3) 0.043(3) -0.015(2) -0.006(2) -0.003(3) C231 0.036(3) 0.033(3) 0.064(4) -0.026(3) 0.000(2) -0.008(3) C261 0.047(3) 0.043(3) 0.046(3) -0.030(2) 0.007(2) -0.023(3) C271 0.034(3) 0.036(3) 0.047(3) -0.021(2) 0.007(2) -0.021(2) P5 0.0234(5) 0.0278(5) 0.0220(5) -0.0113(4) 0.0027(4) -0.0126(4) P6 0.0231(5) 0.0323(6) 0.0221(5) -0.0130(4) 0.0025(4) -0.0130(5) C31 0.026(3) 0.033(3) 0.024(2) -0.007(2) -0.0024(17) -0.012(2) C32 0.020(3) 0.034(3) 0.032(4) -0.008(3) -0.006(2) -0.009(3) C33 0.034(4) 0.039(4) 0.023(4) -0.013(3) -0.002(2) -0.014(3) C34 0.026(4) 0.051(7) 0.032(5) -0.018(5) 0.000(3) -0.017(5) C35 0.033(2) 0.055(3) 0.033(2) -0.025(2) 0.0113(19) -0.029(2) C36 0.031(3) 0.044(4) 0.032(3) -0.017(3) 0.002(2) -0.025(3) C37 0.033(3) 0.032(5) 0.034(4) -0.020(4) -0.004(3) -0.012(5) C38 0.033(3) 0.044(3) 0.023(2) -0.019(2) 0.009(2) -0.023(2) C321 0.034(3) 0.055(3) 0.027(2) -0.016(2) -0.001(2) -0.016(3) C331 0.032(3) 0.066(4) 0.038(3) -0.019(3) 0.000(2) -0.021(3) C361 0.054(4) 0.051(4) 0.049(4) -0.016(3) 0.010(3) -0.042(3) C371 0.044(3) 0.043(3) 0.065(4) -0.035(3) -0.001(3) -0.019(3) P7 0.0248(5) 0.0241(5) 0.0216(5) -0.0094(4) 0.0023(4) -0.0096(4) P8 0.0265(5) 0.0244(5) 0.0216(5) -0.0092(4) 0.0026(4) -0.0109(4) C41 0.025(3) 0.046(6) 0.023(4) -0.008(4) -0.003(2) -0.007(5) C42 0.028(4) 0.038(4) 0.023(4) -0.006(3) -0.007(2) -0.011(3) C43 0.023(4) 0.027(3) 0.025(3) -0.007(2) -0.005(2) -0.005(3) C44 0.029(3) 0.036(3) 0.021(2) -0.008(2) 0.0003(16) -0.012(2) C45 0.045(4) 0.025(4) 0.029(3) -0.012(3) 0.007(2) -0.023(3) C46 0.053(10) 0.052(10) 0.049(10) -0.030(8) 0.020(7) -0.015(7) C47 0.040(10) 0.015(7) 0.029(4) -0.012(4) 0.011(4) -0.007(7) C48 0.040(3) 0.022(2) 0.032(2) -0.0127(19) 0.006(2) -0.011(2) C421 0.033(3) 0.058(3) 0.041(3) -0.016(2) 0.000(2) -0.022(3) C431 0.044(3) 0.051(3) 0.026(2) -0.013(2) -0.001(2) -0.026(3) C461 0.061(4) 0.028(3) 0.043(3) -0.004(2) 0.008(3) -0.017(3) C471 0.056(4) 0.033(3) 0.058(4) -0.017(3) 0.017(3) -0.006(3) C1S 0.052(4) 0.056(4) 0.051(4) -0.017(3) 0.002(3) -0.014(3) C2S 0.065(4) 0.039(3) 0.054(4) -0.020(3) -0.002(3) -0.017(3) C3S 0.060(4) 0.038(3) 0.048(3) -0.016(3) 0.003(3) -0.016(3) C4S 0.090(6) 0.065(5) 0.062(5) -0.024(4) 0.010(4) -0.048(5) C5S 0.110(7) 0.103(6) 0.072(5) -0.043(5) 0.041(5) -0.073(6) _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 P7 2.0610(11) . ? Ni1 P8 2.1142(11) 2_666 ? Ni1 P1 2.1425(6) . ? Ni1 P5 2.1811(11) . ? Ni1 P3 2.1857(11) . ? Ni1 P4 2.2412(10) 2_666 ? Ni1 P6 2.2436(11) 2_666 ? P1 C18 1.880(2) . ? P1 C11 1.882(2) . ? P1 P2 2.2239(8) . ? P2 C15 1.872(3) . ? P2 C14 1.876(3) . ? C11 C12 1.509(3) . ? C12 C13 1.329(4) . ? C12 C121 1.510(4) . ? C13 C14 1.511(4) . ? C13 C131 1.519(3) . ? C15 C16 1.500(4) . ? C16 C17 1.333(4) . ? C16 C161 1.510(4) . ? C17 C171 1.501(4) . ? C17 C18 1.518(3) . ? P3 C28 1.871(4) . ? P3 C21 1.901(7) . ? P3 P4 2.2280(14) . ? P4 C25 1.873(5) . ? P4 C24 1.881(5) . ? P4 Ni1 2.2411(10) 2_666 ? C21 C22 1.498(19) . ? C22 C23 1.26(2) . ? C22 C221 1.585(16) . ? C23 C24 1.52(2) . ? C23 C231 1.56(2) . ? C25 C26 1.510(8) . ? C26 C27 1.350(14) . ? C26 C261 1.516(9) . ? C27 C271 1.487(9) . ? C27 C28 1.525(7) . ? P5 C31 1.871(5) . ? P5 C38 1.876(4) . ? P5 P6 2.2262(14) . ? P6 C35 1.873(4) . ? P6 C34 1.901(17) . ? P6 Ni1 2.2436(11) 2_666 ? C31 C32 1.519(7) . ? C32 C33 1.323(9) . ? C32 C321 1.496(8) . ? C33 C34 1.499(19) . ? C33 C331 1.510(8) . ? C35 C36 1.528(9) . ? C36 C37 1.357(12) . ? C36 C361 1.489(8) . ? C37 C38 1.509(9) . ? C37 C371 1.519(10) . ? P7 C41 1.862(17) . ? P7 C48 1.879(5) . ? P7 P8 2.2241(14) . ? P8 C44 1.867(5) . ? P8 C45 1.873(6) . ? P8 Ni1 2.1143(11) 2_666 ? C41 C42 1.496(17) . ? C42 C43 1.366(9) . ? C42 C421 1.518(8) . ? C43 C431 1.485(8) . ? C43 C44 1.506(8) . ? C45 C46 1.495(19) . ? C46 C47 1.427(19) . ? C46 C461 1.52(2) . ? C47 C471 1.46(2) . ? C47 C48 1.492(17) . ? C1S C2S 1.494(9) . ? C2S C3S 1.515(8) . ? C3S C4S 1.509(10) . ? C4S C5S 1.506(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 P7 Ni1 P8 131.97(4) . 2_666 ? P7 Ni1 P1 109.20(3) . . ? P8 Ni1 P1 118.82(3) 2_666 . ? P7 Ni1 P5 109.05(4) . . ? P8 Ni1 P5 56.69(4) 2_666 . ? P1 Ni1 P5 108.82(3) . . ? P7 Ni1 P3 109.83(4) . . ? P8 Ni1 P3 48.33(4) 2_666 . ? P1 Ni1 P3 115.87(3) . . ? P5 Ni1 P3 103.81(4) . . ? P7 Ni1 P4 56.07(4) . 2_666 ? P8 Ni1 P4 105.71(4) 2_666 2_666 ? P1 Ni1 P4 108.86(3) . 2_666 ? P5 Ni1 P4 55.84(4) . 2_666 ? P3 Ni1 P4 135.09(4) . 2_666 ? P7 Ni1 P6 49.44(4) . 2_666 ? P8 Ni1 P6 104.98(4) 2_666 2_666 ? P1 Ni1 P6 115.45(3) . 2_666 ? P5 Ni1 P6 135.10(4) . 2_666 ? P3 Ni1 P6 63.35(4) . 2_666 ? P4 Ni1 P6 101.23(4) 2_666 2_666 ? C18 P1 C11 99.81(11) . . ? C18 P1 Ni1 124.03(8) . . ? C11 P1 Ni1 116.68(8) . . ? C18 P1 P2 98.45(8) . . ? C11 P1 P2 99.07(8) . . ? Ni1 P1 P2 114.54(3) . . ? C15 P2 C14 101.04(12) . . ? C15 P2 P1 99.59(9) . . ? C14 P2 P1 99.40(9) . . ? C12 C11 P1 116.04(16) . . ? C13 C12 C11 119.4(2) . . ? C13 C12 C121 125.6(2) . . ? C11 C12 C121 115.1(2) . . ? C12 C13 C14 120.2(2) . . ? C12 C13 C131 125.3(3) . . ? C14 C13 C131 114.5(2) . . ? C13 C14 P2 114.18(19) . . ? C16 C15 P2 110.84(17) . . ? C17 C16 C15 119.6(2) . . ? C17 C16 C161 125.2(3) . . ? C15 C16 C161 115.3(3) . . ? C16 C17 C171 125.4(2) . . ? C16 C17 C18 119.1(2) . . ? C171 C17 C18 115.5(2) . . ? C17 C18 P1 112.52(15) . . ? C28 P3 C21 98.1(3) . . ? C28 P3 Ni1 111.75(14) . . ? C21 P3 Ni1 133.6(2) . . ? C28 P3 P4 100.33(15) . . ? C21 P3 P4 98.9(2) . . ? Ni1 P3 P4 109.21(5) . . ? C25 P4 C24 98.2(2) . . ? C25 P4 P3 97.86(18) . . ? C24 P4 P3 100.79(15) . . ? C25 P4 Ni1 115.2(2) . 2_666 ? C24 P4 Ni1 125.02(17) . 2_666 ? P3 P4 Ni1 115.16(5) . 2_666 ? C22 C21 P3 121.3(7) . . ? C23 C22 C21 123.9(15) . . ? C23 C22 C221 121.6(15) . . ? C21 C22 C221 112.7(11) . . ? C22 C23 C24 119.8(19) . . ? C22 C23 C231 125.5(17) . . ? C24 C23 C231 112.6(14) . . ? C23 C24 P4 114.9(7) . . ? C26 C25 P4 115.5(6) . . ? C27 C26 C25 120.2(7) . . ? C27 C26 C261 124.2(8) . . ? C25 C26 C261 115.5(8) . . ? C26 C27 C271 126.0(6) . . ? C26 C27 C28 117.7(7) . . ? C271 C27 C28 116.3(5) . . ? C27 C28 P3 116.5(4) . . ? C31 P5 C38 98.6(3) . . ? C31 P5 Ni1 113.23(19) . . ? C38 P5 Ni1 128.40(19) . . ? C31 P5 P6 99.86(17) . . ? C38 P5 P6 99.71(15) . . ? Ni1 P5 P6 112.71(5) . . ? C35 P6 C34 97.2(5) . . ? C35 P6 P5 99.98(15) . . ? C34 P6 P5 98.7(6) . . ? C35 P6 Ni1 125.58(16) . 2_666 ? C34 P6 Ni1 119.0(4) . 2_666 ? P5 P6 Ni1 111.82(5) . 2_666 ? C32 C31 P5 116.5(4) . . ? C33 C32 C321 126.7(6) . . ? C33 C32 C31 118.8(6) . . ? C321 C32 C31 114.4(5) . . ? C32 C33 C34 121.3(10) . . ? C32 C33 C331 124.3(6) . . ? C34 C33 C331 114.4(10) . . ? C33 C34 P6 115.1(8) . . ? C36 C35 P6 116.0(4) . . ? C37 C36 C361 124.5(7) . . ? C37 C36 C35 118.3(7) . . ? C361 C36 C35 117.0(5) . . ? C36 C37 C38 121.4(8) . . ? C36 C37 C371 121.5(7) . . ? C38 C37 C371 116.9(7) . . ? C37 C38 P5 115.9(5) . . ? C41 P7 C48 99.0(4) . . ? C41 P7 Ni1 130.1(5) . . ? C48 P7 Ni1 111.88(15) . . ? C41 P7 P8 99.4(6) . . ? C48 P7 P8 100.33(15) . . ? Ni1 P7 P8 111.75(5) . . ? C44 P8 C45 99.9(3) . . ? C44 P8 Ni1 123.44(19) . 2_666 ? C45 P8 Ni1 115.9(2) . 2_666 ? C44 P8 P7 100.00(15) . . ? C45 P8 P7 98.0(2) . . ? Ni1 P8 P7 115.46(5) 2_666 . ? C42 C41 P7 117.9(12) . . ? C43 C42 C41 120.5(9) . . ? C43 C42 C421 122.1(6) . . ? C41 C42 C421 117.2(9) . . ? C42 C43 C431 125.1(6) . . ? C42 C43 C44 119.0(6) . . ? C431 C43 C44 115.8(5) . . ? C43 C44 P8 115.6(4) . . ? C46 C45 P8 109.2(9) . . ? C47 C46 C45 118.7(15) . . ? C47 C46 C461 121.4(14) . . ? C45 C46 C461 115.6(12) . . ? C46 C47 C471 125.9(14) . . ? C46 C47 C48 115.8(15) . . ? C471 C47 C48 117.2(13) . . ? C47 C48 P7 118.1(8) . . ? C1S C2S C3S 113.7(6) . . ? C4S C3S C2S 115.4(6) . . ? C5S C4S C3S 115.1(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.848 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.065 data_x8_10081-cut _database_code_depnum_ccdc_archive 'CCDC 863744' #TrackingRef '9135_web_deposit_cif_file_1_DanielTofan_1327008424.Pt2-X8_10081-cut.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H114 O2 P8 Pt2' _chemical_formula_weight 1829.72 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 20.4091(11) _cell_length_b 16.3489(9) _cell_length_c 26.2219(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.9700(10) _cell_angle_gamma 90.00 _cell_volume 8114.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9033 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.81 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 3.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8386 _exptl_absorpt_correction_T_max 0.9644 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 105960 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 30.51 _reflns_number_total 24728 _reflns_number_gt 21491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7.0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+6.4798P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.490(3) _refine_ls_number_reflns 24728 _refine_ls_number_parameters 988 _refine_ls_number_restraints 469 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0612 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.003 _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 Pt1 Pt 0.028159(6) -0.108820(10) -0.442097(6) 0.01857(3) Uani 1 1 d . . . Pt2 Pt -0.028172(7) 0.071937(9) -0.558049(6) 0.02012(3) Uani 1 1 d . . . P1 P 0.02556(5) -0.15031(7) -0.52652(4) 0.0221(2) Uani 1 1 d . . . P4 P -0.01023(5) -0.05350(7) -0.59051(4) 0.0209(2) Uani 1 1 d . . . P2 P -0.08265(5) -0.05475(7) -0.46019(4) 0.0220(2) Uani 1 1 d . . . P5 P -0.11233(5) 0.04693(7) -0.52083(4) 0.0217(2) Uani 1 1 d . . . P3 P 0.10255(5) 0.00292(7) -0.41943(4) 0.0210(2) Uani 1 1 d . . . P6 P 0.07280(5) 0.10039(7) -0.48301(4) 0.0210(2) Uani 1 1 d . . . P7 P 0.06263(5) -0.20244(7) -0.37341(4) 0.0204(2) Uani 1 1 d . . . P8 P -0.05923(5) 0.17145(7) -0.62215(4) 0.0191(2) Uani 1 1 d . B . C41 C -0.0035(2) -0.2691(3) -0.36261(18) 0.0241(9) Uani 1 1 d . . . C71 C 0.0102(2) 0.2377(3) -0.62884(17) 0.0209(8) Uani 1 1 d . . . C81 C -0.1052(2) 0.1412(3) -0.69464(17) 0.0220(8) Uani 1 1 d . . . C51 C 0.1057(2) -0.1586(3) -0.30469(16) 0.0241(9) Uani 1 1 d . . . C17 C 0.1107(3) -0.1909(4) -0.5881(2) 0.0403(14) Uani 1 1 d . . . C84 C -0.1826(3) 0.0918(3) -0.8023(2) 0.0322(11) Uani 1 1 d . . . H84 H -0.2099 0.0757 -0.8390 0.039 Uiso 1 1 calc R . . C61 C 0.1280(2) -0.2800(3) -0.37425(18) 0.0297(10) Uani 1 1 d . . . C13 C -0.1262(2) -0.1663(3) -0.63575(19) 0.0295(11) Uani 1 1 d . . . C14 C -0.0729(2) -0.1145(3) -0.64826(18) 0.0298(10) Uani 1 1 d . . . H14A H -0.0990 -0.0763 -0.6783 0.036 Uiso 1 1 calc R . . H14B H -0.0448 -0.1509 -0.6624 0.036 Uiso 1 1 calc R . . C21 C -0.1144(2) -0.0114(3) -0.40751(19) 0.0315(11) Uani 1 1 d . . . H21A H -0.1667 -0.0124 -0.4228 0.038 Uiso 1 1 calc R . . H21B H -0.0983 -0.0478 -0.3749 0.038 Uiso 1 1 calc R . . C16 C 0.0882(3) -0.1338(3) -0.6279(2) 0.0336(11) Uani 1 1 d . . . C28 C -0.1576(2) -0.1256(3) -0.4969(2) 0.0318(11) Uani 1 1 d . . . H28A H -0.1510 -0.1463 -0.5301 0.038 Uiso 1 1 calc R . . H28B H -0.1544 -0.1731 -0.4727 0.038 Uiso 1 1 calc R . . C38 C 0.0994(2) 0.0625(3) -0.35968(18) 0.0277(10) Uani 1 1 d . . . H38A H 0.0493 0.0737 -0.3660 0.033 Uiso 1 1 calc R . . H38B H 0.1187 0.0279 -0.3264 0.033 Uiso 1 1 calc R . . C34 C 0.1624(2) 0.1266(3) -0.48356(19) 0.0312(11) Uani 1 1 d . . . H34A H 0.1557 0.1634 -0.5151 0.037 Uiso 1 1 calc R . . H34B H 0.1889 0.1576 -0.4496 0.037 Uiso 1 1 calc R . . C36 C 0.1220(2) 0.2020(3) -0.38649(18) 0.0333(11) Uani 1 1 d . . . C33 C 0.2072(2) 0.0557(3) -0.48728(18) 0.0301(10) Uani 1 1 d . . . C52 C 0.0644(2) -0.1154(3) -0.28204(18) 0.0285(9) Uani 1 1 d . . . H52 H 0.0146 -0.1145 -0.3005 0.034 Uiso 1 1 calc R . . C11 C -0.0263(3) -0.2386(3) -0.56604(18) 0.0302(10) Uani 1 1 d . . . H11A H -0.0054 -0.2559 -0.5928 0.036 Uiso 1 1 calc R . . H11B H -0.0207 -0.2845 -0.5402 0.036 Uiso 1 1 calc R . . C23 C -0.1063(2) 0.1372(3) -0.4248(2) 0.0340(11) Uani 1 1 d . . . C27 C -0.2303(2) -0.0909(3) -0.5140(2) 0.0345(11) Uani 1 1 d . . . C72 C 0.0020(3) 0.3207(3) -0.6406(2) 0.0409(13) Uani 1 1 d . . . H72 H -0.0411 0.3463 -0.6434 0.049 Uiso 1 1 calc R . . C37 C 0.1392(2) 0.1432(3) -0.34814(17) 0.0306(11) Uani 1 1 d . . . C22 C -0.0903(3) 0.0750(3) -0.3886(2) 0.0343(12) Uani 1 1 d . . . C45 C -0.1145(3) -0.3424(3) -0.4040(2) 0.0447(13) Uani 1 1 d . . . H45 H -0.1543 -0.3562 -0.4359 0.054 Uiso 1 1 calc R . . C74 C 0.1162(3) 0.3302(3) -0.6446(2) 0.0439(13) Uani 1 1 d . . . H74 H 0.1536 0.3620 -0.6475 0.053 Uiso 1 1 calc R . . C24 C -0.1499(2) 0.1210(3) -0.4848(2) 0.0332(11) Uani 1 1 d . . . H24A H -0.1575 0.1737 -0.5047 0.040 Uiso 1 1 calc R . . H24B H -0.1967 0.1005 -0.4876 0.040 Uiso 1 1 calc R . . C55 C 0.2099(3) -0.1145(4) -0.2273(2) 0.0534(18) Uani 1 1 d . . . H55 H 0.2599 -0.1129 -0.2091 0.064 Uiso 1 1 calc R . . C54 C 0.1665(4) -0.0733(4) -0.2056(2) 0.0525(17) Uani 1 1 d . . . H54 H 0.1867 -0.0449 -0.1717 0.063 Uiso 1 1 calc R . . C44 C -0.1083(3) -0.3731(3) -0.3533(2) 0.0446(14) Uani 1 1 d . . . H44 H -0.1435 -0.4085 -0.3501 0.054 Uiso 1 1 calc R . . C86 C -0.0968(2) 0.1797(3) -0.73931(17) 0.0304(10) Uani 1 1 d . . . H86 H -0.0644 0.2238 -0.7330 0.036 Uiso 1 1 calc R . . C26 C -0.2485(2) -0.0276(3) -0.5487(2) 0.0337(11) Uani 1 1 d . . . C25 C -0.1967(2) 0.0064(3) -0.57156(18) 0.0302(10) Uani 1 1 d . . . H25A H -0.2203 0.0509 -0.5975 0.036 Uiso 1 1 calc R . . H25B H -0.1852 -0.0373 -0.5931 0.036 Uiso 1 1 calc R . . C12 C -0.1043(2) -0.2247(3) -0.59694(19) 0.0334(11) Uani 1 1 d . . . C42 C 0.0020(2) -0.3006(3) -0.31154(17) 0.0301(10) Uani 1 1 d . . . H42 H 0.0417 -0.2870 -0.2795 0.036 Uiso 1 1 calc R . . C85 C -0.1349(2) 0.1548(3) -0.79269(18) 0.0348(11) Uani 1 1 d . . . H85 H -0.1282 0.1812 -0.8226 0.042 Uiso 1 1 calc R . . C32 C 0.2250(2) -0.0032(3) -0.44875(18) 0.0293(10) Uani 1 1 d . . . C321 C 0.2747(2) -0.0722(3) -0.4458(2) 0.0403(12) Uani 1 1 d . . . H32A H 0.2785 -0.0792 -0.4817 0.061 Uiso 1 1 calc R . . H32B H 0.2568 -0.1228 -0.4357 0.061 Uiso 1 1 calc R . . H32C H 0.3214 -0.0597 -0.4181 0.061 Uiso 1 1 calc R . . C161 C 0.0797(3) -0.1441(3) -0.68734(19) 0.0442(13) Uani 1 1 d . . . H16A H 0.0858 -0.2018 -0.6946 0.066 Uiso 1 1 calc R . . H16B H 0.1154 -0.1112 -0.6946 0.066 Uiso 1 1 calc R . . H16C H 0.0325 -0.1259 -0.7113 0.066 Uiso 1 1 calc R . . C62 C 0.1285(3) -0.3625(4) -0.3570(2) 0.0486(15) Uani 1 1 d . . . H62 H 0.0948 -0.3803 -0.3423 0.058 Uiso 1 1 calc R . . C75 C 0.1236(2) 0.2486(3) -0.6368(2) 0.0356(11) Uani 1 1 d . . . H75 H 0.1650 0.2224 -0.6371 0.043 Uiso 1 1 calc R . . C43 C -0.0506(3) -0.3520(3) -0.3074(2) 0.0369(11) Uani 1 1 d . . . H43 H -0.0465 -0.3725 -0.2725 0.044 Uiso 1 1 calc R . . C65 C 0.2266(3) -0.3130(4) -0.4004(2) 0.0491(15) Uani 1 1 d . . . H65 H 0.2608 -0.2960 -0.4147 0.059 Uiso 1 1 calc R . . C46 C -0.0622(2) -0.2912(3) -0.40819(19) 0.0340(10) Uani 1 1 d . . . H46 H -0.0668 -0.2709 -0.4433 0.041 Uiso 1 1 calc R . . C331 C 0.2334(3) 0.0619(3) -0.5340(2) 0.0410(12) Uani 1 1 d . . . H33A H 0.2684 0.0189 -0.5302 0.061 Uiso 1 1 calc R . . H33B H 0.2552 0.1156 -0.5330 0.061 Uiso 1 1 calc R . . H33C H 0.1936 0.0552 -0.5691 0.061 Uiso 1 1 calc R . . C76 C 0.0714(2) 0.2025(3) -0.6285(2) 0.0341(10) Uani 1 1 d . . . H76 H 0.0781 0.1452 -0.6225 0.041 Uiso 1 1 calc R . . C56 C 0.1786(2) -0.1585(3) -0.27622(19) 0.0398(12) Uani 1 1 d . . . H56 H 0.2078 -0.1890 -0.2903 0.048 Uiso 1 1 calc R . . C35 C 0.0625(2) 0.1876(3) -0.44118(17) 0.0294(10) Uani 1 1 d . . . H35A H 0.0561 0.2380 -0.4634 0.035 Uiso 1 1 calc R . . H35B H 0.0185 0.1790 -0.4343 0.035 Uiso 1 1 calc R . . C64 C 0.2266(3) -0.3925(5) -0.3829(3) 0.0569(17) Uani 1 1 d . . . H64 H 0.2605 -0.4305 -0.3854 0.068 Uiso 1 1 calc R . . C31 C 0.2004(2) 0.0009(3) -0.40110(17) 0.0292(10) Uani 1 1 d . . . H31A H 0.2208 0.0506 -0.3794 0.035 Uiso 1 1 calc R . . H31B H 0.2199 -0.0468 -0.3770 0.035 Uiso 1 1 calc R . . C66 C 0.1765(2) -0.2579(3) -0.39713(19) 0.0358(11) Uani 1 1 d . . . H66 H 0.1755 -0.2039 -0.4109 0.043 Uiso 1 1 calc R . . C15 C 0.0657(2) -0.0529(3) -0.61267(19) 0.0300(10) Uani 1 1 d . . . H15A H 0.0541 -0.0161 -0.6448 0.036 Uiso 1 1 calc R . . H15B H 0.1066 -0.0289 -0.5827 0.036 Uiso 1 1 calc R . . C271 C -0.2767(3) -0.1294(4) -0.4880(3) 0.0528(15) Uani 1 1 d . . . H27A H -0.2596 -0.1147 -0.4489 0.079 Uiso 1 1 calc R . . H27B H -0.2756 -0.1890 -0.4916 0.079 Uiso 1 1 calc R . . H27C H -0.3253 -0.1098 -0.5064 0.079 Uiso 1 1 calc R . . C18 C 0.1126(2) -0.1732(3) -0.53180(18) 0.0359(11) Uani 1 1 d . . . H18A H 0.1443 -0.1259 -0.5169 0.043 Uiso 1 1 calc R . . H18B H 0.1337 -0.2208 -0.5080 0.043 Uiso 1 1 calc R . . C221 C -0.0529(3) 0.0845(4) -0.3277(2) 0.0456(13) Uani 1 1 d . . . H22A H -0.0329 0.1396 -0.3195 0.068 Uiso 1 1 calc R . . H22B H -0.0149 0.0440 -0.3142 0.068 Uiso 1 1 calc R . . H22C H -0.0866 0.0760 -0.3095 0.068 Uiso 1 1 calc R . . C82 C -0.1523(3) 0.0770(3) -0.70595(19) 0.0389(12) Uani 1 1 d . . . H82 H -0.1586 0.0490 -0.6764 0.047 Uiso 1 1 calc R . . C261 C -0.3187(2) 0.0159(4) -0.5662(3) 0.0535(15) Uani 1 1 d . . . H26A H -0.3198 0.0602 -0.5917 0.080 Uiso 1 1 calc R . . H26B H -0.3250 0.0386 -0.5338 0.080 Uiso 1 1 calc R . . H26C H -0.3568 -0.0230 -0.5846 0.080 Uiso 1 1 calc R . . C231 C -0.0885(3) 0.2257(3) -0.4099(2) 0.0471(14) Uani 1 1 d . . . H23A H -0.0437 0.2292 -0.3783 0.071 Uiso 1 1 calc R . . H23B H -0.1261 0.2509 -0.4005 0.071 Uiso 1 1 calc R . . H23C H -0.0841 0.2545 -0.4413 0.071 Uiso 1 1 calc R . . C131 C -0.2026(3) -0.1531(3) -0.6744(2) 0.0486(14) Uani 1 1 d . . . H13A H -0.2084 -0.1705 -0.7116 0.073 Uiso 1 1 calc R . . H13B H -0.2145 -0.0950 -0.6748 0.073 Uiso 1 1 calc R . . H13C H -0.2339 -0.1854 -0.6616 0.073 Uiso 1 1 calc R . . C83 C -0.1906(3) 0.0523(4) -0.7593(2) 0.0448(14) Uani 1 1 d . . . H83 H -0.2226 0.0078 -0.7659 0.054 Uiso 1 1 calc R . . C73 C 0.0531(3) 0.3673(3) -0.6484(3) 0.0506(14) Uani 1 1 d . . . H73 H 0.0457 0.4241 -0.6562 0.061 Uiso 1 1 calc R . . C361 C 0.1575(3) 0.2836(3) -0.3802(2) 0.0512(15) Uani 1 1 d . . . H36A H 0.1900 0.2908 -0.3420 0.077 Uiso 1 1 calc R . . H36B H 0.1218 0.3270 -0.3900 0.077 Uiso 1 1 calc R . . H36C H 0.1840 0.2865 -0.4045 0.077 Uiso 1 1 calc R . . C53 C 0.0953(3) -0.0737(3) -0.2330(2) 0.0436(13) Uani 1 1 d . . . H53 H 0.0662 -0.0448 -0.2181 0.052 Uiso 1 1 calc R . . C371 C 0.1983(3) 0.1482(4) -0.29275(19) 0.0498(14) Uani 1 1 d . . . H37A H 0.2310 0.1918 -0.2932 0.075 Uiso 1 1 calc R . . H37B H 0.2235 0.0959 -0.2843 0.075 Uiso 1 1 calc R . . H37C H 0.1787 0.1603 -0.2647 0.075 Uiso 1 1 calc R . . C121 C -0.1523(3) -0.2850(4) -0.5843(2) 0.0493(14) Uani 1 1 d . . . H12A H -0.1996 -0.2614 -0.5947 0.074 Uiso 1 1 calc R . . H12B H -0.1333 -0.2973 -0.5449 0.074 Uiso 1 1 calc R . . H12C H -0.1549 -0.3355 -0.6051 0.074 Uiso 1 1 calc R . . C171 C 0.1338(3) -0.2768(4) -0.5959(2) 0.0559(16) Uani 1 1 d . . . H17A H 0.1316 -0.2831 -0.6336 0.084 Uiso 1 1 calc R . . H17B H 0.1023 -0.3167 -0.5889 0.084 Uiso 1 1 calc R . . H17C H 0.1823 -0.2859 -0.5701 0.084 Uiso 1 1 calc R . . C63 C 0.1776(3) -0.4167(4) -0.3616(3) 0.0583(17) Uani 1 1 d . . . H63 H 0.1775 -0.4717 -0.3499 0.070 Uiso 1 1 calc R . . C91 C -0.1215(2) 0.2480(3) -0.61544(17) 0.0218(8) Uani 1 1 d U . . C94 C -0.2134(3) 0.3576(5) -0.5957(2) 0.0581(17) Uani 1 1 d U . . H94 H -0.2427 0.4013 -0.5932 0.070 Uiso 1 1 calc R A 1 C92 C -0.1898(6) 0.2536(10) -0.6541(4) 0.037(3) Uani 0.59(2) 1 d PU B 1 H92 H -0.2041 0.2230 -0.6872 0.045 Uiso 0.59(2) 1 calc PR B 1 C93 C -0.2367(7) 0.3053(12) -0.6429(4) 0.057(4) Uani 0.59(2) 1 d PU B 1 H93 H -0.2849 0.3059 -0.6670 0.068 Uiso 0.59(2) 1 calc PR B 1 C95 C -0.1471(10) 0.3449(16) -0.5527(9) 0.035(3) Uani 0.59(2) 1 d PU B 1 H95 H -0.1340 0.3696 -0.5175 0.042 Uiso 0.59(2) 1 calc PR B 1 C96 C -0.1010(8) 0.2904(11) -0.5677(7) 0.027(3) Uani 0.59(2) 1 d PU B 1 H96 H -0.0537 0.2841 -0.5424 0.032 Uiso 0.59(2) 1 calc PR B 1 C92A C -0.1710(10) 0.2938(16) -0.6578(7) 0.046(5) Uani 0.41(2) 1 d PU B 2 H92A H -0.1749 0.2832 -0.6944 0.056 Uiso 0.41(2) 1 calc PR B 2 C93A C -0.2146(10) 0.3534(17) -0.6497(7) 0.058(6) Uani 0.41(2) 1 d PU B 2 H93A H -0.2430 0.3885 -0.6782 0.070 Uiso 0.41(2) 1 calc PR B 2 C95A C -0.1586(17) 0.333(2) -0.5597(14) 0.051(7) Uani 0.41(2) 1 d PU B 2 H95A H -0.1461 0.3606 -0.5254 0.061 Uiso 0.41(2) 1 calc PR B 2 C96A C -0.1150(15) 0.2760(18) -0.5614(11) 0.042(5) Uani 0.41(2) 1 d PU B 2 H96A H -0.0808 0.2538 -0.5288 0.051 Uiso 0.41(2) 1 calc PR B 2 C11S C -0.1137(4) -0.6257(6) -0.2467(4) 0.090(2) Uani 1 1 d U . . C12S C -0.1409(4) -0.5510(7) -0.2621(4) 0.103(3) Uani 1 1 d U . . H12S H -0.1647 -0.5377 -0.2998 0.123 Uiso 1 1 calc R . . C13S C -0.1323(5) -0.4884(6) -0.2175(5) 0.132(4) Uani 1 1 d U . . H13S H -0.1523 -0.4354 -0.2264 0.159 Uiso 1 1 calc R . . C14S C -0.0968(6) -0.5092(6) -0.1668(5) 0.126(4) Uani 1 1 d U . . H14S H -0.0935 -0.4745 -0.1369 0.152 Uiso 1 1 calc R . . C15S C -0.0643(8) -0.5844(5) -0.1589(5) 0.165(6) Uani 1 1 d U . . H15S H -0.0314 -0.5949 -0.1228 0.198 Uiso 1 1 calc R . . C16S C -0.0729(6) -0.6457(6) -0.1958(3) 0.114(3) Uani 1 1 d U . . H16S H -0.0517 -0.6980 -0.1860 0.137 Uiso 1 1 calc R . . C17S C -0.1251(6) -0.6880(9) -0.2881(4) 0.163(5) Uani 1 1 d U . . H17D H -0.1757 -0.6920 -0.3104 0.244 Uiso 1 1 calc R . . H17E H -0.1080 -0.7407 -0.2704 0.244 Uiso 1 1 calc R . . H17F H -0.0994 -0.6735 -0.3118 0.244 Uiso 1 1 calc R . . O2S O 0.0064(4) 0.4172(4) -0.4525(3) 0.091(2) Uani 0.798(7) 1 d PDU C 1 C21S C -0.0293(4) 0.4893(5) -0.4467(3) 0.064(2) Uani 0.798(7) 1 d PDU C 1 H21C H -0.0014 0.5187 -0.4124 0.077 Uiso 0.798(7) 1 calc PR C 1 H21D H -0.0763 0.4758 -0.4460 0.077 Uiso 0.798(7) 1 calc PR C 1 C22S C -0.0367(5) 0.5402(6) -0.4963(4) 0.073(3) Uani 0.798(7) 1 d PDU C 1 H22D H -0.0793 0.5240 -0.5281 0.088 Uiso 0.798(7) 1 calc PR C 1 H22E H -0.0402 0.5990 -0.4886 0.088 Uiso 0.798(7) 1 calc PR C 1 C23S C 0.0253(7) 0.5245(8) -0.5068(5) 0.103(4) Uani 0.798(7) 1 d PDU C 1 H23D H 0.0624 0.5655 -0.4883 0.123 Uiso 0.798(7) 1 calc PR C 1 H23E H 0.0152 0.5255 -0.5468 0.123 Uiso 0.798(7) 1 calc PR C 1 C24S C 0.0476(6) 0.4412(6) -0.4836(4) 0.087(3) Uani 0.798(7) 1 d PDU C 1 H24C H 0.0408 0.4017 -0.5137 0.104 Uiso 0.798(7) 1 calc PR C 1 H24D H 0.0983 0.4417 -0.4596 0.104 Uiso 0.798(7) 1 calc PR C 1 O2P O 0.0502(19) 0.5624(17) -0.4597(12) 0.143(10) Uani 0.202(7) 1 d PDU C 2 C21P C 0.0300(17) 0.493(2) -0.4334(9) 0.123(9) Uani 0.202(7) 1 d PDU C 2 H21E H -0.0004 0.5113 -0.4138 0.147 Uiso 0.202(7) 1 calc PR C 2 H21F H 0.0725 0.4662 -0.4066 0.147 Uiso 0.202(7) 1 calc PR C 2 C22P C -0.009(2) 0.4354(19) -0.4779(11) 0.119(10) Uani 0.202(7) 1 d PDU C 2 H22F H 0.0216 0.3887 -0.4792 0.143 Uiso 0.202(7) 1 calc PR C 2 H22G H -0.0515 0.4142 -0.4732 0.143 Uiso 0.202(7) 1 calc PR C 2 C23P C -0.0261(18) 0.483(2) -0.5243(8) 0.098(9) Uani 0.202(7) 1 d PDU C 2 H23F H -0.0673 0.5180 -0.5288 0.117 Uiso 0.202(7) 1 calc PR C 2 H23G H -0.0370 0.4483 -0.5576 0.117 Uiso 0.202(7) 1 calc PR C 2 C24P C 0.0389(15) 0.533(3) -0.5140(8) 0.098(8) Uani 0.202(7) 1 d PDU C 2 H24E H 0.0789 0.4986 -0.5144 0.118 Uiso 0.202(7) 1 calc PR C 2 H24F H 0.0305 0.5776 -0.5409 0.118 Uiso 0.202(7) 1 calc PR C 2 O3S O 0.0712(5) 0.3427(5) -0.2748(4) 0.189(4) Uani 1 1 d DU . . C31S C 0.0490(6) 0.4262(7) -0.2990(4) 0.141(4) Uani 1 1 d DU . . H31C H 0.0595 0.4339 -0.3326 0.169 Uiso 1 1 calc R . . H31D H -0.0021 0.4352 -0.3081 0.169 Uiso 1 1 calc R . . C32S C 0.0923(8) 0.4821(7) -0.2544(5) 0.162(5) Uani 1 1 d DU . . H32D H 0.1068 0.5303 -0.2704 0.195 Uiso 1 1 calc R . . H32E H 0.0642 0.5013 -0.2331 0.195 Uiso 1 1 calc R . . C33S C 0.1510(6) 0.4404(9) -0.2205(5) 0.161(5) Uani 1 1 d DU . . H33D H 0.1551 0.4452 -0.1818 0.193 Uiso 1 1 calc R . . H33E H 0.1941 0.4637 -0.2236 0.193 Uiso 1 1 calc R . . C34S C 0.1433(6) 0.3549(8) -0.2373(5) 0.158(5) Uani 1 1 d DU . . H34C H 0.1764 0.3414 -0.2557 0.190 Uiso 1 1 calc R . . H34D H 0.1540 0.3190 -0.2048 0.190 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 Pt1 0.01764(6) 0.02181(8) 0.01677(7) 0.00342(7) 0.00702(5) 0.00301(7) Pt2 0.02214(7) 0.02013(8) 0.01651(7) 0.00233(7) 0.00541(5) -0.00106(7) P1 0.0249(5) 0.0236(6) 0.0179(5) 0.0022(4) 0.0082(4) 0.0021(4) P4 0.0249(5) 0.0209(6) 0.0166(5) 0.0012(4) 0.0075(4) -0.0020(4) P2 0.0191(5) 0.0252(6) 0.0239(5) 0.0066(4) 0.0105(4) 0.0040(4) P5 0.0191(5) 0.0219(6) 0.0232(5) 0.0046(4) 0.0071(4) 0.0027(4) P3 0.0181(4) 0.0278(6) 0.0172(5) 0.0016(4) 0.0068(4) -0.0008(4) P6 0.0225(5) 0.0224(6) 0.0180(5) 0.0007(4) 0.0076(4) -0.0038(4) P7 0.0219(5) 0.0227(6) 0.0177(5) 0.0044(4) 0.0086(4) 0.0060(4) P8 0.0200(5) 0.0203(6) 0.0167(5) 0.0017(4) 0.0064(4) -0.0012(4) C41 0.024(2) 0.023(2) 0.023(2) 0.0018(18) 0.0071(17) 0.0029(17) C71 0.0206(18) 0.020(2) 0.022(2) 0.0016(17) 0.0081(16) 0.0024(16) C81 0.0213(19) 0.021(2) 0.022(2) 0.0040(17) 0.0066(16) 0.0010(16) C51 0.025(2) 0.032(3) 0.0152(19) 0.0053(17) 0.0074(16) 0.0017(18) C17 0.049(3) 0.042(3) 0.040(3) 0.003(3) 0.029(3) 0.010(3) C84 0.030(2) 0.038(3) 0.022(2) -0.003(2) 0.0022(18) -0.001(2) C61 0.028(2) 0.039(3) 0.024(2) 0.003(2) 0.0117(18) 0.012(2) C13 0.031(2) 0.029(3) 0.025(2) -0.005(2) 0.0056(19) -0.008(2) C14 0.035(2) 0.028(3) 0.018(2) 0.0003(19) 0.0007(18) -0.010(2) C21 0.027(2) 0.048(3) 0.027(2) 0.007(2) 0.0187(19) 0.007(2) C16 0.038(3) 0.035(3) 0.035(3) -0.004(2) 0.022(2) 0.002(2) C28 0.026(2) 0.029(3) 0.040(3) 0.013(2) 0.0116(19) 0.0001(19) C38 0.032(2) 0.031(3) 0.024(2) -0.0010(18) 0.0151(19) 0.0000(19) C34 0.028(2) 0.043(3) 0.024(2) -0.001(2) 0.0108(18) -0.014(2) C36 0.039(3) 0.040(3) 0.022(2) -0.007(2) 0.012(2) -0.012(2) C33 0.022(2) 0.045(3) 0.026(2) -0.001(2) 0.0121(18) -0.007(2) C52 0.041(2) 0.021(2) 0.026(2) -0.0038(18) 0.0144(19) -0.0018(19) C11 0.050(3) 0.017(2) 0.025(2) 0.0006(18) 0.016(2) -0.004(2) C23 0.029(2) 0.036(3) 0.042(3) -0.004(2) 0.020(2) 0.005(2) C27 0.021(2) 0.036(3) 0.048(3) 0.007(2) 0.015(2) -0.0013(19) C72 0.033(3) 0.039(3) 0.057(3) 0.005(3) 0.024(2) 0.000(2) C37 0.037(2) 0.038(3) 0.017(2) -0.0079(19) 0.0100(18) -0.011(2) C22 0.033(2) 0.046(3) 0.032(3) -0.007(2) 0.021(2) 0.007(2) C45 0.041(3) 0.034(3) 0.049(3) 0.002(3) 0.005(2) -0.014(2) C74 0.030(2) 0.037(3) 0.070(4) -0.003(3) 0.024(3) -0.010(2) C24 0.028(2) 0.030(3) 0.040(3) 0.005(2) 0.012(2) 0.0070(19) C55 0.041(3) 0.072(5) 0.027(3) 0.004(3) -0.011(2) -0.019(3) C54 0.077(5) 0.053(4) 0.024(3) -0.004(3) 0.014(3) -0.019(3) C44 0.042(3) 0.034(3) 0.057(4) 0.002(3) 0.018(3) -0.015(2) C86 0.028(2) 0.042(3) 0.023(2) -0.002(2) 0.0111(17) -0.006(2) C26 0.0168(19) 0.038(3) 0.043(3) 0.002(2) 0.0077(18) -0.0011(19) C25 0.022(2) 0.029(3) 0.031(2) 0.010(2) 0.0010(17) -0.0010(18) C12 0.039(3) 0.033(3) 0.032(3) -0.011(2) 0.017(2) -0.015(2) C42 0.036(2) 0.033(3) 0.024(2) -0.0016(19) 0.0150(18) -0.004(2) C85 0.038(2) 0.048(3) 0.022(2) -0.002(2) 0.0151(19) -0.004(2) C32 0.0183(19) 0.041(3) 0.028(2) -0.003(2) 0.0086(17) -0.0027(18) C321 0.027(2) 0.057(3) 0.039(3) -0.001(3) 0.015(2) 0.002(2) C161 0.073(4) 0.038(3) 0.030(3) -0.002(2) 0.030(3) 0.001(3) C62 0.049(3) 0.043(3) 0.063(4) 0.022(3) 0.031(3) 0.022(3) C75 0.026(2) 0.040(3) 0.046(3) 0.000(2) 0.020(2) 0.000(2) C43 0.044(3) 0.037(3) 0.037(3) -0.001(2) 0.023(2) -0.012(2) C65 0.036(3) 0.064(4) 0.053(3) 0.006(3) 0.023(3) 0.021(3) C46 0.042(3) 0.027(2) 0.030(2) -0.002(2) 0.009(2) 0.001(2) C331 0.032(2) 0.058(4) 0.040(3) -0.002(2) 0.021(2) -0.012(2) C76 0.032(2) 0.030(3) 0.049(3) -0.004(2) 0.025(2) -0.001(2) C56 0.034(2) 0.055(4) 0.025(2) 0.007(2) 0.006(2) -0.002(2) C35 0.034(2) 0.027(2) 0.026(2) -0.0041(19) 0.0105(18) -0.0043(19) C64 0.047(3) 0.061(4) 0.068(4) 0.020(4) 0.028(3) 0.039(3) C31 0.0199(19) 0.042(3) 0.023(2) -0.0003(19) 0.0041(16) -0.0016(18) C66 0.030(2) 0.044(3) 0.036(3) 0.010(2) 0.0150(19) 0.009(2) C15 0.035(2) 0.032(3) 0.030(2) -0.0003(19) 0.020(2) -0.006(2) C271 0.033(3) 0.058(4) 0.074(4) 0.020(3) 0.028(3) -0.001(3) C18 0.035(2) 0.047(3) 0.028(2) 0.006(2) 0.014(2) 0.013(2) C221 0.048(3) 0.063(4) 0.031(3) -0.004(2) 0.020(2) 0.006(3) C82 0.045(3) 0.045(3) 0.022(2) 0.003(2) 0.008(2) -0.019(2) C261 0.028(2) 0.052(4) 0.074(4) 0.007(3) 0.012(3) 0.008(2) C231 0.041(3) 0.049(4) 0.056(3) -0.019(3) 0.024(3) 0.003(3) C131 0.036(3) 0.047(3) 0.048(3) -0.005(3) -0.001(2) -0.004(2) C83 0.038(3) 0.058(4) 0.026(3) 0.001(3) -0.002(2) -0.021(3) C73 0.045(3) 0.035(3) 0.076(4) 0.013(3) 0.028(3) -0.002(2) C361 0.077(4) 0.038(3) 0.034(3) -0.009(2) 0.016(3) -0.030(3) C53 0.071(4) 0.036(3) 0.029(3) 0.000(2) 0.025(3) -0.006(3) C371 0.053(3) 0.061(4) 0.026(3) -0.005(3) 0.004(2) -0.019(3) C121 0.058(3) 0.050(4) 0.042(3) -0.006(3) 0.020(3) -0.029(3) C171 0.084(4) 0.049(4) 0.049(3) 0.005(3) 0.041(3) 0.026(3) C63 0.056(4) 0.043(4) 0.078(5) 0.019(3) 0.027(3) 0.025(3) C91 0.0228(18) 0.026(2) 0.0179(19) 0.0020(16) 0.0086(15) -0.0023(16) C94 0.045(3) 0.089(5) 0.042(3) -0.002(3) 0.018(3) 0.034(3) C92 0.029(4) 0.063(8) 0.018(4) 0.000(4) 0.008(3) 0.013(5) C93 0.041(6) 0.088(10) 0.031(5) 0.001(5) 0.002(4) 0.038(6) C95 0.039(5) 0.027(7) 0.036(7) -0.013(5) 0.012(4) -0.001(4) C96 0.025(4) 0.027(6) 0.030(6) -0.006(5) 0.012(4) 0.000(4) C92A 0.034(8) 0.071(12) 0.028(5) -0.007(7) 0.004(6) 0.026(7) C93A 0.040(9) 0.082(14) 0.035(6) -0.007(8) -0.005(6) 0.039(9) C95A 0.070(12) 0.039(13) 0.031(7) -0.025(8) 0.002(7) 0.018(10) C96A 0.064(12) 0.043(12) 0.024(5) 0.012(7) 0.021(8) 0.025(9) C11S 0.064(5) 0.135(7) 0.073(5) 0.017(4) 0.027(4) -0.013(5) C12S 0.065(5) 0.150(7) 0.075(5) 0.066(4) 0.004(4) -0.006(5) C13S 0.092(6) 0.080(6) 0.158(8) 0.039(5) -0.030(6) -0.033(5) C14S 0.163(10) 0.055(5) 0.128(7) 0.005(5) 0.016(7) -0.008(5) C15S 0.251(13) 0.044(5) 0.123(7) -0.007(5) -0.019(9) 0.021(6) C16S 0.176(9) 0.080(6) 0.053(4) 0.010(4) 0.005(5) -0.007(6) C17S 0.122(8) 0.269(13) 0.112(8) -0.093(9) 0.061(7) -0.042(9) O2S 0.095(5) 0.084(5) 0.104(6) 0.034(4) 0.049(4) 0.021(4) C21S 0.049(4) 0.071(6) 0.078(5) -0.012(4) 0.032(4) -0.004(4) C22S 0.091(6) 0.064(6) 0.076(6) 0.003(4) 0.044(5) 0.023(5) C23S 0.100(8) 0.117(8) 0.115(8) 0.032(7) 0.067(7) 0.010(7) C24S 0.092(7) 0.095(7) 0.100(7) 0.002(5) 0.068(6) 0.033(5) O2P 0.15(2) 0.122(17) 0.139(17) -0.034(14) 0.033(16) -0.017(15) C21P 0.138(19) 0.121(18) 0.108(13) -0.021(14) 0.044(15) 0.016(17) C22P 0.114(17) 0.108(16) 0.111(16) 0.009(12) 0.015(16) -0.002(14) C23P 0.104(15) 0.085(17) 0.106(13) -0.003(12) 0.043(14) 0.001(13) C24P 0.065(14) 0.115(18) 0.147(15) -0.010(14) 0.076(13) 0.032(12) O3S 0.193(8) 0.116(6) 0.224(10) 0.033(6) 0.040(7) 0.029(6) C31S 0.154(9) 0.161(9) 0.102(7) 0.058(6) 0.040(6) 0.078(8) C32S 0.253(15) 0.123(7) 0.142(10) -0.005(7) 0.109(9) 0.048(8) C33S 0.122(8) 0.273(14) 0.118(9) -0.004(9) 0.080(6) -0.024(8) C34S 0.149(8) 0.222(11) 0.121(10) 0.097(8) 0.070(7) 0.121(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P7 2.2656(11) . ? Pt1 P1 2.2969(10) . ? Pt1 P2 2.3061(10) . ? Pt1 P3 2.3067(11) . ? Pt2 P8 2.2531(11) . ? Pt2 P4 2.3016(11) . ? Pt2 P6 2.3023(10) . ? Pt2 P5 2.3074(10) . ? P1 C11 1.859(5) . ? P1 C18 1.870(4) . ? P1 P4 2.2219(15) . ? P4 C15 1.848(4) . ? P4 C14 1.864(4) . ? P2 C21 1.871(4) . ? P2 C28 1.872(5) . ? P2 P5 2.2222(15) . ? P5 C25 1.860(4) . ? P5 C24 1.867(5) . ? P3 C38 1.866(4) . ? P3 C31 1.871(4) . ? P3 P6 2.2204(15) . ? P6 C35 1.858(4) . ? P6 C34 1.884(4) . ? P7 C51 1.830(4) . ? P7 C41 1.837(5) . ? P7 C61 1.847(4) . ? P8 C91 1.838(4) . ? P8 C71 1.843(4) . ? P8 C81 1.845(4) . ? C41 C46 1.386(6) . ? C41 C42 1.399(6) . ? C71 C76 1.373(6) . ? C71 C72 1.388(7) . ? C81 C82 1.379(6) . ? C81 C86 1.395(6) . ? C51 C52 1.392(6) . ? C51 C56 1.393(6) . ? C17 C16 1.347(7) . ? C17 C18 1.491(7) . ? C17 C171 1.518(8) . ? C84 C83 1.362(7) . ? C84 C85 1.373(7) . ? C61 C66 1.384(6) . ? C61 C62 1.421(7) . ? C13 C12 1.344(7) . ? C13 C14 1.509(6) . ? C13 C131 1.524(6) . ? C21 C22 1.518(7) . ? C16 C15 1.501(7) . ? C16 C161 1.513(6) . ? C28 C27 1.493(6) . ? C38 C37 1.519(6) . ? C34 C33 1.502(7) . ? C36 C37 1.340(7) . ? C36 C361 1.499(7) . ? C36 C35 1.511(6) . ? C33 C32 1.344(6) . ? C33 C331 1.513(6) . ? C52 C53 1.382(6) . ? C11 C12 1.509(7) . ? C23 C22 1.344(7) . ? C23 C231 1.507(7) . ? C23 C24 1.514(7) . ? C27 C26 1.334(7) . ? C27 C271 1.499(6) . ? C72 C73 1.367(7) . ? C37 C371 1.503(6) . ? C22 C221 1.499(7) . ? C45 C44 1.383(7) . ? C45 C46 1.394(7) . ? C74 C75 1.349(7) . ? C74 C73 1.394(7) . ? C55 C54 1.392(9) . ? C55 C56 1.400(8) . ? C54 C53 1.360(9) . ? C44 C43 1.375(7) . ? C86 C85 1.384(6) . ? C26 C25 1.502(6) . ? C26 C261 1.510(6) . ? C12 C121 1.510(6) . ? C42 C43 1.400(6) . ? C32 C321 1.500(6) . ? C32 C31 1.512(6) . ? C62 C63 1.376(7) . ? C75 C76 1.387(6) . ? C65 C64 1.378(9) . ? C65 C66 1.390(7) . ? C64 C63 1.374(8) . ? C82 C83 1.383(7) . ? C91 C96 1.354(18) . ? C91 C92 1.387(11) . ? C91 C92A 1.405(18) . ? C91 C96A 1.45(3) . ? C94 C95A 1.23(3) . ? C94 C93A 1.41(2) . ? C94 C95 1.42(2) . ? C94 C93 1.433(15) . ? C92 C93 1.386(14) . ? C95 C96 1.45(3) . ? C92A C93A 1.39(2) . ? C95A C96A 1.30(5) . ? C11S C16S 1.322(11) . ? C11S C12S 1.339(13) . ? C11S C17S 1.444(13) . ? C12S C13S 1.512(15) . ? C13S C14S 1.299(13) . ? C14S C15S 1.375(13) . ? C15S C16S 1.358(13) . ? O2S C21S 1.424(9) . ? O2S C24S 1.427(9) . ? C21S C22S 1.502(10) . ? C22S C23S 1.416(12) . ? C23S C24S 1.491(12) . ? O2P C24P 1.442(16) . ? O2P C21P 1.466(16) . ? C21P C22P 1.476(16) . ? C22P C23P 1.372(18) . ? C23P C24P 1.494(17) . ? O3S C34S 1.445(11) . ? O3S C31S 1.502(10) . ? C31S C32S 1.486(12) . ? C32S C33S 1.376(10) . ? C33S C34S 1.456(12) . ? 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 P7 Pt1 P1 117.07(4) . . ? P7 Pt1 P2 114.29(4) . . ? P1 Pt1 P2 104.34(4) . . ? P7 Pt1 P3 110.58(4) . . ? P1 Pt1 P3 104.94(4) . . ? P2 Pt1 P3 104.46(4) . . ? P8 Pt2 P4 114.00(4) . . ? P8 Pt2 P6 113.81(4) . . ? P4 Pt2 P6 106.30(4) . . ? P8 Pt2 P5 113.41(4) . . ? P4 Pt2 P5 104.19(4) . . ? P6 Pt2 P5 104.14(4) . . ? C11 P1 C18 99.3(2) . . ? C11 P1 P4 100.03(15) . . ? C18 P1 P4 98.02(16) . . ? C11 P1 Pt1 124.72(15) . . ? C18 P1 Pt1 116.76(15) . . ? P4 P1 Pt1 113.58(5) . . ? C15 P4 C14 98.5(2) . . ? C15 P4 P1 99.42(16) . . ? C14 P4 P1 99.45(15) . . ? C15 P4 Pt2 112.33(15) . . ? C14 P4 Pt2 128.44(17) . . ? P1 P4 Pt2 114.10(5) . . ? C21 P2 C28 99.9(2) . . ? C21 P2 P5 99.69(16) . . ? C28 P2 P5 98.25(15) . . ? C21 P2 Pt1 125.26(15) . . ? C28 P2 Pt1 114.71(15) . . ? P5 P2 Pt1 114.69(5) . . ? C25 P5 C24 98.5(2) . . ? C25 P5 P2 100.17(15) . . ? C24 P5 P2 100.18(16) . . ? C25 P5 Pt2 113.40(15) . . ? C24 P5 Pt2 127.61(16) . . ? P2 P5 Pt2 112.86(5) . . ? C38 P3 C31 99.3(2) . . ? C38 P3 P6 99.80(15) . . ? C31 P3 P6 99.85(15) . . ? C38 P3 Pt1 113.81(14) . . ? C31 P3 Pt1 126.07(17) . . ? P6 P3 Pt1 113.96(5) . . ? C35 P6 C34 98.9(2) . . ? C35 P6 P3 99.60(15) . . ? C34 P6 P3 100.10(16) . . ? C35 P6 Pt2 113.36(14) . . ? C34 P6 Pt2 126.92(15) . . ? P3 P6 Pt2 113.74(5) . . ? C51 P7 C41 101.0(2) . . ? C51 P7 C61 101.4(2) . . ? C41 P7 C61 99.8(2) . . ? C51 P7 Pt1 114.20(15) . . ? C41 P7 Pt1 119.70(14) . . ? C61 P7 Pt1 117.73(15) . . ? C91 P8 C71 101.08(19) . . ? C91 P8 C81 100.26(19) . . ? C71 P8 C81 99.89(19) . . ? C91 P8 Pt2 115.59(14) . . ? C71 P8 Pt2 118.92(13) . . ? C81 P8 Pt2 117.91(15) . . ? C46 C41 C42 117.6(4) . . ? C46 C41 P7 118.0(4) . . ? C42 C41 P7 124.4(3) . . ? C76 C71 C72 116.5(4) . . ? C76 C71 P8 118.9(3) . . ? C72 C71 P8 124.2(3) . . ? C82 C81 C86 117.2(4) . . ? C82 C81 P8 118.0(3) . . ? C86 C81 P8 124.8(3) . . ? C52 C51 C56 117.9(4) . . ? C52 C51 P7 118.3(3) . . ? C56 C51 P7 123.5(4) . . ? C16 C17 C18 120.4(5) . . ? C16 C17 C171 124.8(5) . . ? C18 C17 C171 114.8(5) . . ? C83 C84 C85 119.9(5) . . ? C66 C61 C62 117.7(4) . . ? C66 C61 P7 117.5(4) . . ? C62 C61 P7 124.6(4) . . ? C12 C13 C14 120.1(4) . . ? C12 C13 C131 124.8(5) . . ? C14 C13 C131 114.7(4) . . ? C13 C14 P4 117.1(3) . . ? C22 C21 P2 115.7(3) . . ? C17 C16 C15 117.1(4) . . ? C17 C16 C161 126.5(5) . . ? C15 C16 C161 116.3(4) . . ? C27 C28 P2 116.6(4) . . ? C37 C38 P3 115.9(3) . . ? C33 C34 P6 116.2(3) . . ? C37 C36 C361 125.2(4) . . ? C37 C36 C35 119.5(4) . . ? C361 C36 C35 115.3(4) . . ? C32 C33 C34 120.3(4) . . ? C32 C33 C331 125.4(4) . . ? C34 C33 C331 114.1(4) . . ? C53 C52 C51 120.7(5) . . ? C12 C11 P1 116.7(3) . . ? C22 C23 C231 124.9(5) . . ? C22 C23 C24 119.6(5) . . ? C231 C23 C24 115.4(5) . . ? C26 C27 C28 119.5(4) . . ? C26 C27 C271 125.0(4) . . ? C28 C27 C271 115.4(4) . . ? C73 C72 C71 122.9(5) . . ? C36 C37 C371 125.2(5) . . ? C36 C37 C38 120.2(4) . . ? C371 C37 C38 114.6(4) . . ? C23 C22 C221 124.5(5) . . ? C23 C22 C21 120.7(5) . . ? C221 C22 C21 114.7(5) . . ? C44 C45 C46 119.8(5) . . ? C75 C74 C73 119.3(5) . . ? C23 C24 P5 116.6(3) . . ? C54 C55 C56 118.8(5) . . ? C53 C54 C55 120.1(5) . . ? C43 C44 C45 119.4(5) . . ? C85 C86 C81 121.2(4) . . ? C27 C26 C25 120.0(4) . . ? C27 C26 C261 124.3(4) . . ? C25 C26 C261 115.7(4) . . ? C26 C25 P5 116.6(3) . . ? C13 C12 C11 119.8(4) . . ? C13 C12 C121 124.8(5) . . ? C11 C12 C121 115.1(4) . . ? C41 C42 C43 120.4(4) . . ? C84 C85 C86 119.9(4) . . ? C33 C32 C321 124.4(4) . . ? C33 C32 C31 120.6(4) . . ? C321 C32 C31 114.8(4) . . ? C63 C62 C61 120.1(5) . . ? C74 C75 C76 120.9(4) . . ? C44 C43 C42 120.9(5) . . ? C64 C65 C66 120.0(5) . . ? C41 C46 C45 122.0(5) . . ? C71 C76 C75 121.4(5) . . ? C51 C56 C55 121.4(5) . . ? C36 C35 P6 116.8(3) . . ? C63 C64 C65 119.8(5) . . ? C32 C31 P3 116.1(3) . . ? C61 C66 C65 121.3(5) . . ? C16 C15 P4 117.0(3) . . ? C17 C18 P1 116.1(3) . . ? C81 C82 C83 121.6(5) . . ? C84 C83 C82 120.2(5) . . ? C72 C73 C74 118.9(5) . . ? C54 C53 C52 121.2(5) . . ? C64 C63 C62 121.0(6) . . ? C96 C91 C92 121.3(9) . . ? C96 C91 C92A 109.9(11) . . ? C92 C91 C92A 32.6(8) . . ? C96 C91 C96A 17.9(12) . . ? C92 C91 C96A 113.1(12) . . ? C92A C91 C96A 112.4(13) . . ? C96 C91 P8 116.9(7) . . ? C92 C91 P8 121.1(6) . . ? C92A C91 P8 127.3(7) . . ? C96A C91 P8 119.7(11) . . ? C95A C94 C93A 115(2) . . ? C95A C94 C95 10(3) . . ? C93A C94 C95 116.4(12) . . ? C95A C94 C93 112.5(17) . . ? C93A C94 C93 39.3(8) . . ? C95 C94 C93 120.6(11) . . ? C93 C92 C91 118.1(10) . . ? C92 C93 C94 121.0(9) . . ? C94 C95 C96 113.5(16) . . ? C91 C96 C95 123.9(13) . . ? C93A C92A C91 124.4(14) . . ? C92A C93A C94 114.7(15) . . ? C94 C95A C96A 130(3) . . ? C95A C96A C91 116(2) . . ? C16S C11S C12S 124.3(10) . . ? C16S C11S C17S 116.6(11) . . ? C12S C11S C17S 118.9(10) . . ? C11S C12S C13S 117.9(8) . . ? C14S C13S C12S 118.2(10) . . ? C13S C14S C15S 116.2(11) . . ? C16S C15S C14S 128.7(10) . . ? C11S C16S C15S 113.6(10) . . ? C21S O2S C24S 105.5(6) . . ? O2S C21S C22S 104.8(6) . . ? C23S C22S C21S 105.1(7) . . ? C22S C23S C24S 104.2(8) . . ? O2S C24S C23S 109.2(7) . . ? C24P O2P C21P 103.4(17) . . ? O2P C21P C22P 106.6(14) . . ? C23P C22P C21P 103.1(16) . . ? C22P C23P C24P 103.2(17) . . ? O2P C24P C23P 99.6(16) . . ? C34S O3S C31S 103.4(9) . . ? C32S C31S O3S 103.3(8) . . ? C33S C32S C31S 108.8(9) . . ? C32S C33S C34S 108.1(9) . . ? O3S C34S C33S 107.8(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.095 _refine_diff_density_min -1.067 _refine_diff_density_rms 0.111 data_d8_10132 _database_code_depnum_ccdc_archive 'CCDC 863745' #TrackingRef '9136_web_deposit_cif_file_2_DanielTofan_1327008424.Pd2-D8_10132.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H106 O P8 Pd2' _chemical_formula_weight 1580.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3521(3) _cell_length_b 14.0198(3) _cell_length_c 23.3487(5) _cell_angle_alpha 74.0590(10) _cell_angle_beta 80.7290(10) _cell_angle_gamma 82.8510(10) _cell_volume 3823.39(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9907 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 69.13 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 5.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2083 _exptl_absorpt_correction_T_max 0.5471 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Bruker D8 three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 73677 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 68.24 _reflns_number_total 13542 _reflns_number_gt 12207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+32.7533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13542 _refine_ls_number_parameters 906 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.256 _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 Pd1 Pd 0.68029(4) 0.15566(3) 0.198912(18) 0.01873(12) Uani 1 1 d . . . Pd2 Pd 0.79297(3) 0.32205(3) 0.290542(19) 0.01873(12) Uani 1 1 d . . . P1 P 0.87351(13) 0.15026(12) 0.18358(7) 0.0212(3) Uani 1 1 d . . . P2 P 0.93138(12) 0.22756(11) 0.24289(7) 0.0195(3) Uani 1 1 d . . . P3 P 0.62860(12) 0.32689(11) 0.16357(7) 0.0195(3) Uani 1 1 d . . . P4 P 0.69455(13) 0.41719(11) 0.21306(7) 0.0206(3) Uani 1 1 d . . . P5 P 0.62719(13) 0.10740(11) 0.30399(7) 0.0205(3) Uani 1 1 d . . . P6 P 0.67103(13) 0.21032(11) 0.35242(7) 0.0210(3) Uani 1 1 d . . . P7 P 0.61844(13) 0.04810(11) 0.15547(7) 0.0199(3) Uani 1 1 d . . . P8 P 0.86987(13) 0.41900(12) 0.33522(7) 0.0212(3) Uani 1 1 d . . . C15 C 0.9973(5) 0.1153(5) 0.2931(3) 0.0241(13) Uani 1 1 d . . . H15A H 1.0318 0.1371 0.3223 0.029 Uiso 1 1 calc R . . H15B H 0.9391 0.0720 0.3161 0.029 Uiso 1 1 calc R . . C16 C 1.0836(5) 0.0544(5) 0.2613(3) 0.0245(13) Uani 1 1 d . . . C18 C 0.9365(5) 0.0206(5) 0.2119(3) 0.0271(14) Uani 1 1 d . . . H18A H 0.8918 -0.0111 0.2500 0.033 Uiso 1 1 calc R . . H18B H 0.9311 -0.0172 0.1825 0.033 Uiso 1 1 calc R . . C14 C 1.0576(5) 0.2779(5) 0.1939(3) 0.0246(13) Uani 1 1 d . . . H14A H 1.0891 0.3199 0.2138 0.029 Uiso 1 1 calc R . . H14B H 1.1127 0.2214 0.1904 0.029 Uiso 1 1 calc R . . C12 C 1.0013(5) 0.2981(5) 0.0944(3) 0.0270(14) Uani 1 1 d . . . C161 C 1.1990(6) 0.0522(5) 0.2749(3) 0.0321(15) Uani 1 1 d . . . H16A H 1.2494 0.0133 0.2512 0.048 Uiso 1 1 calc R . . H16B H 1.2019 0.0215 0.3178 0.048 Uiso 1 1 calc R . . H16C H 1.2209 0.1203 0.2645 0.048 Uiso 1 1 calc R . . C17 C 1.0551(5) 0.0102(5) 0.2228(3) 0.0247(13) Uani 1 1 d . . . C11 C 0.9756(5) 0.1899(5) 0.1136(3) 0.0275(14) Uani 1 1 d . . . H11A H 1.0455 0.1480 0.1200 0.033 Uiso 1 1 calc R . . H11B H 0.9474 0.1751 0.0800 0.033 Uiso 1 1 calc R . . C13 C 1.0394(5) 0.3384(5) 0.1315(3) 0.0266(14) Uani 1 1 d . . . C131 C 1.0719(6) 0.4440(5) 0.1157(3) 0.0353(16) Uani 1 1 d . . . H13A H 1.1523 0.4431 0.1115 0.053 Uiso 1 1 calc R . . H13B H 1.0386 0.4757 0.1476 0.053 Uiso 1 1 calc R . . H13C H 1.0460 0.4816 0.0777 0.053 Uiso 1 1 calc R . . C121 C 0.9872(6) 0.3546(6) 0.0304(3) 0.0377(17) Uani 1 1 d . . . H12A H 0.9327 0.4116 0.0307 0.056 Uiso 1 1 calc R . . H12B H 0.9621 0.3105 0.0101 0.056 Uiso 1 1 calc R . . H12C H 1.0578 0.3783 0.0091 0.056 Uiso 1 1 calc R . . C171 C 1.1348(6) -0.0513(5) 0.1873(3) 0.0337(16) Uani 1 1 d . . . H17A H 1.2105 -0.0439 0.1919 0.050 Uiso 1 1 calc R . . H17B H 1.1251 -0.0279 0.1447 0.050 Uiso 1 1 calc R . . H17C H 1.1200 -0.1215 0.2024 0.050 Uiso 1 1 calc R . . C25 C 0.7893(5) 0.4873(5) 0.1498(3) 0.0264(13) Uani 1 1 d . . . H25A H 0.8201 0.5372 0.1641 0.032 Uiso 1 1 calc R . . H25B H 0.8514 0.4402 0.1398 0.032 Uiso 1 1 calc R . . C261 C 0.7440(6) 0.6522(5) 0.0766(3) 0.0337(15) Uani 1 1 d . . . H26A H 0.7196 0.6809 0.0371 0.051 Uiso 1 1 calc R . . H26B H 0.8191 0.6691 0.0754 0.051 Uiso 1 1 calc R . . H26C H 0.6946 0.6790 0.1068 0.051 Uiso 1 1 calc R . . C28 C 0.7019(5) 0.3765(5) 0.0861(3) 0.0238(13) Uani 1 1 d . . . H28A H 0.7794 0.3479 0.0854 0.029 Uiso 1 1 calc R . . H28B H 0.6685 0.3514 0.0579 0.029 Uiso 1 1 calc R . . C23 C 0.4671(5) 0.4698(5) 0.2418(3) 0.0255(13) Uani 1 1 d . . . C26 C 0.7421(5) 0.5404(4) 0.0929(3) 0.0245(13) Uani 1 1 d . . . C21 C 0.4916(5) 0.4005(5) 0.1542(3) 0.0236(13) Uani 1 1 d . . . H21A H 0.5037 0.4666 0.1263 0.028 Uiso 1 1 calc R . . H21B H 0.4470 0.3660 0.1358 0.028 Uiso 1 1 calc R . . C24 C 0.5754(5) 0.5143(5) 0.2167(3) 0.0253(13) Uani 1 1 d . . . H24A H 0.5898 0.5561 0.2422 0.030 Uiso 1 1 calc R . . H24B H 0.5701 0.5580 0.1759 0.030 Uiso 1 1 calc R . . C22 C 0.4273(5) 0.4147(5) 0.2128(3) 0.0249(13) Uani 1 1 d . . . C27 C 0.7024(5) 0.4884(5) 0.0622(3) 0.0244(13) Uani 1 1 d . . . C221 C 0.3203(5) 0.3664(5) 0.2322(3) 0.0300(15) Uani 1 1 d . . . H22A H 0.2962 0.3623 0.2748 0.045 Uiso 1 1 calc R . . H22B H 0.3309 0.2992 0.2261 0.045 Uiso 1 1 calc R . . H22C H 0.2642 0.4062 0.2083 0.045 Uiso 1 1 calc R . . C231 C 0.4071(6) 0.4968(5) 0.2979(3) 0.0321(15) Uani 1 1 d . . . H23A H 0.3792 0.5671 0.2877 0.048 Uiso 1 1 calc R . . H23B H 0.4580 0.4853 0.3277 0.048 Uiso 1 1 calc R . . H23C H 0.3454 0.4553 0.3146 0.048 Uiso 1 1 calc R . . C271 C 0.6566(6) 0.5321(5) 0.0035(3) 0.0339(16) Uani 1 1 d . . . H27A H 0.6702 0.6026 -0.0114 0.051 Uiso 1 1 calc R . . H27B H 0.5771 0.5257 0.0098 0.051 Uiso 1 1 calc R . . H27C H 0.6926 0.4963 -0.0260 0.051 Uiso 1 1 calc R . . C361 C 0.4148(6) 0.1796(5) 0.4763(3) 0.0326(15) Uani 1 1 d . . . H36A H 0.3740 0.1213 0.4966 0.049 Uiso 1 1 calc R . . H36B H 0.3672 0.2404 0.4781 0.049 Uiso 1 1 calc R . . H36C H 0.4794 0.1773 0.4963 0.049 Uiso 1 1 calc R . . C371 C 0.3567(6) 0.0280(5) 0.4152(3) 0.0294(14) Uani 1 1 d . . . H37A H 0.3363 0.0261 0.4578 0.044 Uiso 1 1 calc R . . H37B H 0.3988 -0.0346 0.4115 0.044 Uiso 1 1 calc R . . H37C H 0.2900 0.0367 0.3960 0.044 Uiso 1 1 calc R . . C321 C 0.8382(6) -0.1166(5) 0.3760(3) 0.0363(17) Uani 1 1 d . . . H32A H 0.9087 -0.1165 0.3901 0.054 Uiso 1 1 calc R . . H32B H 0.8508 -0.1140 0.3331 0.054 Uiso 1 1 calc R . . H32C H 0.8035 -0.1775 0.3985 0.054 Uiso 1 1 calc R . . C36 C 0.4515(5) 0.1795(5) 0.4116(3) 0.0270(14) Uani 1 1 d . . . C38 C 0.4730(5) 0.1204(5) 0.3202(3) 0.0288(14) Uani 1 1 d . . . H38A H 0.4459 0.1855 0.2953 0.035 Uiso 1 1 calc R . . H38B H 0.4438 0.0680 0.3075 0.035 Uiso 1 1 calc R . . C33 C 0.7861(5) 0.0350(5) 0.4153(3) 0.0246(13) Uani 1 1 d . . . C331 C 0.8903(6) 0.0320(6) 0.4422(3) 0.0360(16) Uani 1 1 d . . . H33A H 0.8730 0.0189 0.4860 0.054 Uiso 1 1 calc R . . H33B H 0.9221 0.0962 0.4260 0.054 Uiso 1 1 calc R . . H33C H 0.9432 -0.0209 0.4321 0.054 Uiso 1 1 calc R . . C31 C 0.6545(5) -0.0133(5) 0.3615(3) 0.0254(13) Uani 1 1 d . . . H31A H 0.5946 -0.0186 0.3957 0.030 Uiso 1 1 calc R . . H31B H 0.6510 -0.0688 0.3434 0.030 Uiso 1 1 calc R . . C35 C 0.5270(5) 0.2588(5) 0.3769(3) 0.0281(14) Uani 1 1 d . . . H35A H 0.5310 0.3042 0.4023 0.034 Uiso 1 1 calc R . . H35B H 0.4942 0.2984 0.3409 0.034 Uiso 1 1 calc R . . C34 C 0.7014(5) 0.1193(5) 0.4244(3) 0.0250(13) Uani 1 1 d . . . H34A H 0.7284 0.1551 0.4497 0.030 Uiso 1 1 calc R . . H34B H 0.6323 0.0910 0.4463 0.030 Uiso 1 1 calc R . . C32 C 0.7635(5) -0.0268(5) 0.3857(3) 0.0242(13) Uani 1 1 d . . . C37 C 0.4260(5) 0.1135(5) 0.3850(3) 0.0250(13) Uani 1 1 d . . . C43 C 0.8406(6) -0.0981(5) 0.0466(3) 0.0321(15) Uani 1 1 d . . . H43 H 0.8734 -0.1634 0.0477 0.038 Uiso 1 1 calc R . . C42 C 0.7607(5) -0.0823(5) 0.0938(3) 0.0273(14) Uani 1 1 d . . . H42 H 0.7371 -0.1372 0.1257 0.033 Uiso 1 1 calc R . . C44 C 0.8720(5) -0.0200(5) -0.0012(3) 0.0307(15) Uani 1 1 d . . . H44 H 0.9250 -0.0315 -0.0334 0.037 Uiso 1 1 calc R . . C41 C 0.7158(5) 0.0140(4) 0.0939(3) 0.0215(12) Uani 1 1 d . . . C45 C 0.8257(6) 0.0757(5) -0.0020(3) 0.0326(15) Uani 1 1 d . . . H45 H 0.8463 0.1299 -0.0351 0.039 Uiso 1 1 calc R . . C46 C 0.7493(6) 0.0923(5) 0.0454(3) 0.0293(14) Uani 1 1 d . . . H46 H 0.7194 0.1583 0.0449 0.035 Uiso 1 1 calc R . . C52 C 0.4655(5) 0.0446(5) 0.0756(3) 0.0258(13) Uani 1 1 d . . . H52 H 0.5138 -0.0064 0.0632 0.031 Uiso 1 1 calc R . . C51 C 0.4933(5) 0.0870(4) 0.1184(3) 0.0210(12) Uani 1 1 d . . . C54 C 0.2971(5) 0.1510(5) 0.0688(3) 0.0275(14) Uani 1 1 d . . . H54 H 0.2302 0.1724 0.0521 0.033 Uiso 1 1 calc R . . C56 C 0.4210(5) 0.1621(5) 0.1355(3) 0.0235(13) Uani 1 1 d . . . H56 H 0.4386 0.1916 0.1646 0.028 Uiso 1 1 calc R . . C53 C 0.3684(5) 0.0762(5) 0.0512(3) 0.0281(14) Uani 1 1 d . . . H53 H 0.3503 0.0468 0.0222 0.034 Uiso 1 1 calc R . . C55 C 0.3239(5) 0.1943(5) 0.1107(3) 0.0272(14) Uani 1 1 d . . . H55 H 0.2759 0.2460 0.1225 0.033 Uiso 1 1 calc R . . C61 C 0.5830(6) -0.0737(5) 0.2061(3) 0.0254(13) Uani 1 1 d . . . C66 C 0.6617(6) -0.1313(5) 0.2406(3) 0.0302(15) Uani 1 1 d . . . H66 H 0.7335 -0.1096 0.2349 0.036 Uiso 1 1 calc R . . C65 C 0.6376(7) -0.2192(5) 0.2828(3) 0.0357(17) Uani 1 1 d . . . H65 H 0.6931 -0.2579 0.3051 0.043 Uiso 1 1 calc R . . C62 C 0.4775(6) -0.1083(5) 0.2157(3) 0.0347(16) Uani 1 1 d . . . H62 H 0.4228 -0.0715 0.1921 0.042 Uiso 1 1 calc R . . C63 C 0.4524(7) -0.1949(6) 0.2587(4) 0.0441(19) Uani 1 1 d . . . H63 H 0.3803 -0.2163 0.2653 0.053 Uiso 1 1 calc R . . C64 C 0.5326(7) -0.2510(5) 0.2927(3) 0.0395(18) Uani 1 1 d . . . H64 H 0.5154 -0.3106 0.3224 0.047 Uiso 1 1 calc R . . C71 C 0.9428(5) 0.5246(5) 0.2835(3) 0.0255(13) Uani 1 1 d . . . C72 C 1.0573(6) 0.5263(5) 0.2694(3) 0.0346(16) Uani 1 1 d . . . H72 H 1.1039 0.4734 0.2902 0.042 Uiso 1 1 calc R . . C76 C 0.8779(6) 0.6038(5) 0.2531(3) 0.0308(15) Uani 1 1 d . . . H76 H 0.8001 0.6043 0.2619 0.037 Uiso 1 1 calc R . . C74 C 1.0367(7) 0.6823(6) 0.1953(3) 0.0413(18) Uani 1 1 d . . . H74 H 1.0685 0.7350 0.1647 0.050 Uiso 1 1 calc R . . C73 C 1.1032(7) 0.6038(6) 0.2258(4) 0.0425(18) Uani 1 1 d . . . H73 H 1.1810 0.6035 0.2165 0.051 Uiso 1 1 calc R . . C75 C 0.9241(6) 0.6830(5) 0.2098(3) 0.0358(16) Uani 1 1 d . . . H75 H 0.8779 0.7376 0.1903 0.043 Uiso 1 1 calc R . . C81 C 0.7794(5) 0.4914(4) 0.3824(3) 0.0230(13) Uani 1 1 d . . . C85 C 0.7445(6) 0.6063(5) 0.4448(3) 0.0324(15) Uani 1 1 d . . . H85 H 0.7715 0.6489 0.4637 0.039 Uiso 1 1 calc R . . C83 C 0.5935(6) 0.5347(5) 0.4243(3) 0.0302(15) Uani 1 1 d . . . H83 H 0.5166 0.5286 0.4286 0.036 Uiso 1 1 calc R . . C84 C 0.6328(6) 0.5957(5) 0.4520(3) 0.0337(16) Uani 1 1 d . . . H84 H 0.5830 0.6307 0.4762 0.040 Uiso 1 1 calc R . . C82 C 0.6671(5) 0.4817(5) 0.3898(3) 0.0266(14) Uani 1 1 d . . . H82 H 0.6402 0.4388 0.3712 0.032 Uiso 1 1 calc R . . C86 C 0.8170(6) 0.5544(5) 0.4099(3) 0.0283(14) Uani 1 1 d . . . H86 H 0.8935 0.5621 0.4047 0.034 Uiso 1 1 calc R . . C92 C 1.0663(5) 0.3027(5) 0.3622(3) 0.0291(14) Uani 1 1 d . . . H92 H 1.0802 0.3083 0.3203 0.035 Uiso 1 1 calc R . . C91 C 0.9710(5) 0.3535(5) 0.3857(3) 0.0233(13) Uani 1 1 d . . . C93 C 1.1397(6) 0.2450(5) 0.3992(3) 0.0332(15) Uani 1 1 d . . . H93 H 1.2049 0.2140 0.3821 0.040 Uiso 1 1 calc R . . C94 C 1.1196(6) 0.2320(6) 0.4603(3) 0.0403(18) Uani 1 1 d . . . H94 H 1.1696 0.1912 0.4856 0.048 Uiso 1 1 calc R . . C96 C 0.9524(6) 0.3395(5) 0.4475(3) 0.0330(15) Uani 1 1 d . . . H96 H 0.8884 0.3717 0.4650 0.040 Uiso 1 1 calc R . . C95 C 1.0251(7) 0.2793(6) 0.4846(3) 0.0425(19) Uani 1 1 d . . . H95 H 1.0101 0.2705 0.5268 0.051 Uiso 1 1 calc R . . C26S C 0.7391(7) 0.2929(6) 0.5827(4) 0.0442(19) Uani 1 1 d . . . C23S C 0.9022(8) 0.3046(7) 0.6502(4) 0.051(2) Uani 1 1 d . . . H23S H 0.9577 0.3082 0.6732 0.062 Uiso 1 1 calc R . . C25S C 0.7892(8) 0.2080(7) 0.6183(4) 0.054(2) Uani 1 1 d . . . H25S H 0.7681 0.1445 0.6195 0.064 Uiso 1 1 calc R . . C21S C 0.7736(8) 0.3833(6) 0.5820(4) 0.051(2) Uani 1 1 d . . . H21S H 0.7408 0.4427 0.5581 0.061 Uiso 1 1 calc R . . C24S C 0.8683(7) 0.2140(7) 0.6516(4) 0.050(2) Uani 1 1 d . . . H24S H 0.9003 0.1548 0.6761 0.060 Uiso 1 1 calc R . . C22S C 0.8541(8) 0.3901(7) 0.6148(4) 0.057(2) Uani 1 1 d . . . H22S H 0.8766 0.4533 0.6132 0.069 Uiso 1 1 calc R . . C27S C 0.6540(8) 0.2836(8) 0.5469(5) 0.061(3) Uani 1 1 d . . . H27D H 0.6442 0.3455 0.5154 0.091 Uiso 1 1 calc R . . H27E H 0.5842 0.2709 0.5732 0.091 Uiso 1 1 calc R . . H27F H 0.6773 0.2283 0.5283 0.091 Uiso 1 1 calc R . . O1S O 0.3597(7) -0.3171(6) 0.0405(4) 0.047(2) Uani 0.727(14) 1 d PDU A 1 C11S C 0.4588(12) -0.2799(11) 0.0447(7) 0.048(3) Uani 0.727(14) 1 d PDU A 1 H11C H 0.4888 -0.2376 0.0053 0.057 Uiso 0.727(14) 1 calc PR A 1 H11D H 0.5147 -0.3351 0.0583 0.057 Uiso 0.727(14) 1 calc PR A 1 C12S C 0.4276(17) -0.2196(16) 0.0901(9) 0.050(4) Uani 0.727(14) 1 d PDU A 1 H12D H 0.4913 -0.2162 0.1101 0.060 Uiso 0.727(14) 1 calc PR A 1 H12E H 0.3983 -0.1511 0.0711 0.060 Uiso 0.727(14) 1 calc PR A 1 C13S C 0.3401(11) -0.2765(10) 0.1338(5) 0.045(3) Uani 0.727(14) 1 d PDU A 1 H13D H 0.2786 -0.2307 0.1460 0.054 Uiso 0.727(14) 1 calc PR A 1 H13E H 0.3707 -0.3183 0.1702 0.054 Uiso 0.727(14) 1 calc PR A 1 C14S C 0.3019(12) -0.3406(11) 0.0995(6) 0.042(3) Uani 0.727(14) 1 d PDU A 1 H14C H 0.3174 -0.4119 0.1194 0.050 Uiso 0.727(14) 1 calc PR A 1 H14D H 0.2217 -0.3269 0.0981 0.050 Uiso 0.727(14) 1 calc PR A 1 O1P O 0.2671(17) -0.2626(16) 0.1135(10) 0.051(6) Uani 0.273(14) 1 d PDU A 2 C11P C 0.354(2) -0.222(3) 0.1294(14) 0.052(7) Uani 0.273(14) 1 d PDU A 2 H11E H 0.3810 -0.2671 0.1661 0.062 Uiso 0.273(14) 1 calc PR A 2 H11F H 0.3298 -0.1563 0.1366 0.062 Uiso 0.273(14) 1 calc PR A 2 C12P C 0.442(4) -0.214(4) 0.076(2) 0.048(8) Uani 0.273(14) 1 d PDU A 2 H12F H 0.4295 -0.1520 0.0441 0.058 Uiso 0.273(14) 1 calc PR A 2 H12G H 0.5165 -0.2169 0.0874 0.058 Uiso 0.273(14) 1 calc PR A 2 C13P C 0.430(3) -0.304(3) 0.0546(19) 0.048(7) Uani 0.273(14) 1 d PDU A 2 H13F H 0.4853 -0.3593 0.0696 0.057 Uiso 0.273(14) 1 calc PR A 2 H13G H 0.4398 -0.2879 0.0101 0.057 Uiso 0.273(14) 1 calc PR A 2 C14P C 0.315(3) -0.331(3) 0.081(2) 0.050(8) Uani 0.273(14) 1 d PDU A 2 H14E H 0.2716 -0.3284 0.0479 0.061 Uiso 0.273(14) 1 calc PR A 2 H14F H 0.3171 -0.3998 0.1072 0.061 Uiso 0.273(14) 1 calc PR A 2 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 0.0170(2) 0.0194(2) 0.0211(2) -0.00787(16) -0.00442(16) 0.00174(16) Pd2 0.0160(2) 0.0195(2) 0.0219(2) -0.00838(16) -0.00284(16) 0.00099(16) P1 0.0177(8) 0.0233(8) 0.0242(8) -0.0099(6) -0.0036(6) 0.0016(6) P2 0.0165(8) 0.0198(7) 0.0238(7) -0.0090(6) -0.0031(6) 0.0003(6) P3 0.0166(8) 0.0188(7) 0.0245(7) -0.0076(6) -0.0044(6) -0.0007(6) P4 0.0169(8) 0.0203(7) 0.0258(8) -0.0085(6) -0.0039(6) 0.0005(6) P5 0.0186(8) 0.0207(7) 0.0234(7) -0.0072(6) -0.0042(6) -0.0014(6) P6 0.0187(8) 0.0221(8) 0.0235(7) -0.0084(6) -0.0024(6) -0.0005(6) P7 0.0189(8) 0.0189(7) 0.0236(7) -0.0086(6) -0.0048(6) 0.0010(6) P8 0.0167(8) 0.0250(8) 0.0231(7) -0.0096(6) -0.0034(6) 0.0023(6) C15 0.025(3) 0.023(3) 0.026(3) -0.007(2) -0.006(2) -0.003(2) C16 0.021(3) 0.023(3) 0.026(3) -0.004(2) -0.004(2) 0.003(2) C18 0.027(4) 0.020(3) 0.037(4) -0.011(3) -0.007(3) 0.001(3) C14 0.018(3) 0.023(3) 0.033(3) -0.010(3) -0.002(2) -0.002(2) C12 0.014(3) 0.034(4) 0.029(3) -0.006(3) 0.002(2) 0.004(3) C161 0.027(4) 0.033(4) 0.039(4) -0.012(3) -0.013(3) 0.005(3) C17 0.020(3) 0.020(3) 0.033(3) -0.008(3) -0.006(3) 0.005(2) C11 0.020(3) 0.038(4) 0.025(3) -0.012(3) 0.000(2) 0.003(3) C13 0.014(3) 0.030(3) 0.034(3) -0.006(3) 0.001(2) -0.002(2) C131 0.026(4) 0.036(4) 0.040(4) -0.003(3) -0.004(3) -0.002(3) C121 0.026(4) 0.052(5) 0.031(4) -0.004(3) -0.002(3) -0.004(3) C171 0.032(4) 0.030(4) 0.041(4) -0.015(3) -0.008(3) 0.010(3) C25 0.022(3) 0.026(3) 0.032(3) -0.010(3) -0.002(3) -0.003(3) C261 0.033(4) 0.030(4) 0.037(4) -0.005(3) -0.004(3) -0.006(3) C28 0.022(3) 0.025(3) 0.026(3) -0.009(3) -0.001(2) -0.004(2) C23 0.018(3) 0.027(3) 0.030(3) -0.007(3) -0.004(2) 0.005(2) C26 0.022(3) 0.018(3) 0.033(3) -0.007(3) 0.000(3) -0.005(2) C21 0.017(3) 0.022(3) 0.032(3) -0.006(3) -0.007(2) 0.001(2) C24 0.022(3) 0.023(3) 0.034(3) -0.013(3) -0.005(3) 0.003(2) C22 0.016(3) 0.023(3) 0.034(3) -0.007(3) -0.005(2) 0.006(2) C27 0.021(3) 0.022(3) 0.029(3) -0.007(3) -0.001(2) -0.004(2) C221 0.021(4) 0.026(3) 0.045(4) -0.014(3) -0.006(3) 0.003(3) C231 0.028(4) 0.033(4) 0.036(4) -0.015(3) -0.003(3) 0.004(3) C271 0.041(4) 0.030(4) 0.031(4) -0.007(3) -0.008(3) -0.001(3) C361 0.024(4) 0.040(4) 0.037(4) -0.018(3) 0.001(3) -0.004(3) C371 0.023(4) 0.034(4) 0.032(3) -0.009(3) -0.006(3) -0.004(3) C321 0.038(4) 0.032(4) 0.034(4) -0.006(3) -0.005(3) 0.011(3) C36 0.017(3) 0.028(3) 0.032(3) -0.006(3) -0.002(2) 0.004(3) C38 0.021(4) 0.038(4) 0.027(3) -0.009(3) -0.005(3) 0.003(3) C33 0.019(3) 0.029(3) 0.026(3) -0.002(3) -0.004(2) -0.007(2) C331 0.026(4) 0.051(5) 0.029(4) -0.004(3) -0.007(3) -0.006(3) C31 0.030(4) 0.019(3) 0.026(3) -0.005(2) -0.005(3) -0.001(3) C35 0.025(4) 0.024(3) 0.034(4) -0.013(3) 0.000(3) 0.005(3) C34 0.028(4) 0.027(3) 0.022(3) -0.006(2) -0.004(2) -0.005(3) C32 0.025(4) 0.020(3) 0.025(3) -0.002(2) -0.002(2) -0.001(2) C37 0.018(3) 0.029(3) 0.026(3) -0.005(3) -0.004(2) 0.001(2) C43 0.024(4) 0.032(4) 0.047(4) -0.023(3) -0.009(3) 0.007(3) C42 0.024(4) 0.026(3) 0.034(3) -0.012(3) -0.007(3) 0.002(3) C44 0.018(3) 0.045(4) 0.035(4) -0.023(3) -0.001(3) -0.002(3) C41 0.020(3) 0.021(3) 0.028(3) -0.013(2) -0.006(2) -0.002(2) C45 0.034(4) 0.032(4) 0.033(4) -0.012(3) -0.001(3) -0.004(3) C46 0.025(4) 0.028(3) 0.036(4) -0.012(3) -0.002(3) 0.000(3) C52 0.021(3) 0.028(3) 0.032(3) -0.014(3) -0.001(2) -0.003(3) C51 0.015(3) 0.021(3) 0.027(3) -0.006(2) -0.002(2) -0.003(2) C54 0.018(3) 0.031(4) 0.033(3) -0.005(3) -0.007(3) 0.000(3) C56 0.024(3) 0.021(3) 0.027(3) -0.009(2) -0.003(2) -0.002(2) C53 0.021(3) 0.036(4) 0.031(3) -0.013(3) -0.006(3) -0.005(3) C55 0.022(3) 0.025(3) 0.033(3) -0.008(3) -0.001(3) 0.002(3) C61 0.031(4) 0.021(3) 0.026(3) -0.010(2) -0.002(3) 0.001(3) C66 0.033(4) 0.028(3) 0.033(4) -0.012(3) -0.009(3) 0.001(3) C65 0.048(5) 0.029(4) 0.031(4) -0.009(3) -0.013(3) 0.006(3) C62 0.031(4) 0.031(4) 0.040(4) -0.005(3) -0.004(3) -0.003(3) C63 0.036(5) 0.043(5) 0.048(5) -0.006(4) 0.001(3) -0.008(3) C64 0.054(5) 0.024(4) 0.038(4) -0.005(3) -0.003(3) -0.007(3) C71 0.024(4) 0.028(3) 0.028(3) -0.012(3) 0.000(2) -0.007(3) C72 0.029(4) 0.029(4) 0.046(4) -0.011(3) -0.002(3) -0.002(3) C76 0.027(4) 0.029(4) 0.038(4) -0.011(3) -0.006(3) -0.002(3) C74 0.049(5) 0.033(4) 0.041(4) -0.008(3) 0.005(3) -0.014(3) C73 0.031(4) 0.039(4) 0.056(5) -0.013(4) 0.004(3) -0.008(3) C75 0.042(5) 0.025(3) 0.042(4) -0.008(3) -0.011(3) 0.000(3) C81 0.022(3) 0.021(3) 0.027(3) -0.009(2) -0.002(2) 0.002(2) C85 0.031(4) 0.034(4) 0.039(4) -0.019(3) -0.005(3) -0.003(3) C83 0.020(4) 0.033(4) 0.037(4) -0.012(3) 0.001(3) 0.001(3) C84 0.034(4) 0.033(4) 0.034(4) -0.015(3) 0.002(3) 0.003(3) C82 0.023(4) 0.028(3) 0.031(3) -0.011(3) -0.005(3) -0.002(3) C86 0.021(4) 0.030(4) 0.038(4) -0.016(3) -0.003(3) -0.006(3) C92 0.023(4) 0.033(4) 0.032(4) -0.012(3) -0.004(3) 0.001(3) C91 0.015(3) 0.023(3) 0.036(3) -0.012(3) -0.006(2) -0.002(2) C93 0.023(4) 0.031(4) 0.048(4) -0.015(3) -0.008(3) 0.003(3) C94 0.037(4) 0.043(4) 0.042(4) -0.009(3) -0.018(3) 0.008(3) C96 0.023(4) 0.040(4) 0.035(4) -0.012(3) -0.004(3) 0.004(3) C95 0.038(5) 0.055(5) 0.032(4) -0.010(3) -0.007(3) 0.006(4) C26S 0.041(5) 0.047(5) 0.043(4) -0.016(4) 0.000(3) 0.005(4) C23S 0.044(5) 0.060(6) 0.050(5) -0.018(4) -0.004(4) 0.001(4) C25S 0.054(6) 0.043(5) 0.055(5) -0.006(4) -0.003(4) 0.007(4) C21S 0.059(6) 0.038(5) 0.045(5) -0.011(4) 0.004(4) 0.016(4) C24S 0.044(5) 0.048(5) 0.050(5) -0.005(4) -0.002(4) 0.002(4) C22S 0.061(6) 0.050(5) 0.062(6) -0.022(4) -0.003(5) 0.002(4) C27S 0.059(6) 0.064(6) 0.064(6) -0.027(5) -0.016(5) 0.009(5) O1S 0.059(6) 0.043(4) 0.043(5) -0.015(3) -0.005(4) -0.015(4) C11S 0.052(7) 0.040(7) 0.054(7) -0.016(6) 0.005(5) -0.014(5) C12S 0.051(9) 0.046(7) 0.060(10) -0.025(7) -0.001(6) -0.016(6) C13S 0.043(7) 0.047(7) 0.050(6) -0.023(5) -0.001(5) -0.011(6) C14S 0.042(6) 0.040(7) 0.047(8) -0.014(6) -0.004(5) -0.008(5) O1P 0.043(10) 0.051(12) 0.058(12) -0.017(9) 0.012(9) -0.014(9) C11P 0.047(14) 0.048(15) 0.066(14) -0.028(11) 0.007(11) -0.009(12) C12P 0.035(13) 0.049(14) 0.061(17) -0.017(13) 0.002(12) -0.009(11) C13P 0.045(13) 0.055(15) 0.044(14) -0.018(12) 0.000(11) -0.005(12) C14P 0.056(14) 0.049(15) 0.049(18) -0.019(12) 0.005(14) -0.018(11) _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 P7 2.2941(15) . ? Pd1 P1 2.3505(16) . ? Pd1 P3 2.3562(15) . ? Pd1 P5 2.3638(15) . ? Pd2 P8 2.2930(16) . ? Pd2 P6 2.3350(16) . ? Pd2 P4 2.3473(15) . ? Pd2 P2 2.3555(15) . ? P1 C18 1.870(6) . ? P1 C11 1.891(6) . ? P1 P2 2.222(2) . ? P2 C15 1.868(6) . ? P2 C14 1.869(6) . ? P3 C28 1.874(6) . ? P3 C21 1.881(6) . ? P3 P4 2.228(2) . ? P4 C25 1.857(7) . ? P4 C24 1.884(6) . ? P5 C38 1.877(7) . ? P5 C31 1.881(6) . ? P5 P6 2.223(2) . ? P6 C34 1.871(6) . ? P6 C35 1.881(6) . ? P7 C51 1.844(6) . ? P7 C61 1.848(7) . ? P7 C41 1.849(6) . ? P8 C91 1.841(6) . ? P8 C81 1.852(6) . ? P8 C71 1.860(7) . ? C15 C16 1.510(8) . ? C16 C17 1.334(9) . ? C16 C161 1.504(9) . ? C18 C17 1.510(9) . ? C14 C13 1.506(9) . ? C12 C13 1.327(10) . ? C12 C121 1.512(9) . ? C12 C11 1.518(9) . ? C17 C171 1.523(9) . ? C13 C131 1.513(10) . ? C25 C26 1.502(9) . ? C261 C26 1.510(9) . ? C28 C27 1.514(8) . ? C23 C22 1.336(9) . ? C23 C24 1.510(9) . ? C23 C231 1.516(9) . ? C26 C27 1.334(9) . ? C21 C22 1.516(9) . ? C22 C221 1.507(9) . ? C27 C271 1.508(9) . ? C361 C36 1.506(9) . ? C371 C37 1.504(9) . ? C321 C32 1.512(9) . ? C36 C37 1.339(9) . ? C36 C35 1.510(9) . ? C38 C37 1.512(9) . ? C33 C32 1.327(9) . ? C33 C331 1.511(9) . ? C33 C34 1.516(9) . ? C31 C32 1.513(9) . ? C43 C44 1.374(10) . ? C43 C42 1.402(9) . ? C42 C41 1.395(9) . ? C44 C45 1.388(10) . ? C41 C46 1.391(9) . ? C45 C46 1.386(9) . ? C52 C53 1.382(9) . ? C52 C51 1.399(9) . ? C51 C56 1.396(8) . ? C54 C55 1.386(9) . ? C54 C53 1.391(9) . ? C56 C55 1.386(9) . ? C61 C66 1.395(9) . ? C61 C62 1.410(10) . ? C66 C65 1.382(10) . ? C65 C64 1.388(11) . ? C62 C63 1.379(10) . ? C63 C64 1.395(11) . ? C71 C76 1.381(9) . ? C71 C72 1.402(10) . ? C72 C73 1.379(11) . ? C76 C75 1.391(10) . ? C74 C75 1.376(11) . ? C74 C73 1.388(12) . ? C81 C86 1.384(9) . ? C81 C82 1.389(9) . ? C85 C84 1.385(10) . ? C85 C86 1.387(9) . ? C83 C84 1.378(10) . ? C83 C82 1.398(9) . ? C92 C93 1.381(10) . ? C92 C91 1.411(9) . ? C91 C96 1.387(9) . ? C93 C94 1.374(11) . ? C94 C95 1.387(11) . ? C96 C95 1.388(10) . ? C26S C21S 1.382(12) . ? C26S C25S 1.389(12) . ? C26S C27S 1.483(12) . ? C23S C24S 1.376(13) . ? C23S C22S 1.382(13) . ? C25S C24S 1.367(13) . ? C21S C22S 1.376(14) . ? O1S C11S 1.416(14) . ? O1S C14S 1.416(13) . ? C11S C12S 1.506(15) . ? C12S C13S 1.502(17) . ? C13S C14S 1.514(14) . ? O1P C14P 1.411(19) . ? O1P C11P 1.414(18) . ? C11P C12P 1.52(2) . ? C12P C13P 1.50(2) . ? C13P C14P 1.507(19) . ? 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 P7 Pd1 P1 111.35(6) . . ? P7 Pd1 P3 117.85(5) . . ? P1 Pd1 P3 102.41(6) . . ? P7 Pd1 P5 109.41(6) . . ? P1 Pd1 P5 106.63(5) . . ? P3 Pd1 P5 108.49(5) . . ? P8 Pd2 P6 117.04(6) . . ? P8 Pd2 P4 112.40(6) . . ? P6 Pd2 P4 105.03(6) . . ? P8 Pd2 P2 110.40(6) . . ? P6 Pd2 P2 106.60(5) . . ? P4 Pd2 P2 104.43(5) . . ? C18 P1 C11 98.0(3) . . ? C18 P1 P2 101.1(2) . . ? C11 P1 P2 99.9(2) . . ? C18 P1 Pd1 111.1(2) . . ? C11 P1 Pd1 132.1(2) . . ? P2 P1 Pd1 110.15(7) . . ? C15 P2 C14 99.0(3) . . ? C15 P2 P1 97.4(2) . . ? C14 P2 P1 99.8(2) . . ? C15 P2 Pd2 116.1(2) . . ? C14 P2 Pd2 124.7(2) . . ? P1 P2 Pd2 115.13(8) . . ? C28 P3 C21 98.9(3) . . ? C28 P3 P4 100.1(2) . . ? C21 P3 P4 97.9(2) . . ? C28 P3 Pd1 110.1(2) . . ? C21 P3 Pd1 132.9(2) . . ? P4 P3 Pd1 111.88(7) . . ? C25 P4 C24 100.8(3) . . ? C25 P4 P3 98.3(2) . . ? C24 P4 P3 100.0(2) . . ? C25 P4 Pd2 110.5(2) . . ? C24 P4 Pd2 128.7(2) . . ? P3 P4 Pd2 113.88(7) . . ? C38 P5 C31 98.7(3) . . ? C38 P5 P6 100.7(2) . . ? C31 P5 P6 98.4(2) . . ? C38 P5 Pd1 109.2(2) . . ? C31 P5 Pd1 131.3(2) . . ? P6 P5 Pd1 113.99(8) . . ? C34 P6 C35 99.7(3) . . ? C34 P6 P5 100.1(2) . . ? C35 P6 P5 97.6(2) . . ? C34 P6 Pd2 124.6(2) . . ? C35 P6 Pd2 119.0(2) . . ? P5 P6 Pd2 111.24(7) . . ? C51 P7 C61 100.6(3) . . ? C51 P7 C41 100.3(3) . . ? C61 P7 C41 103.4(3) . . ? C51 P7 Pd1 118.9(2) . . ? C61 P7 Pd1 116.1(2) . . ? C41 P7 Pd1 115.0(2) . . ? C91 P8 C81 101.6(3) . . ? C91 P8 C71 103.8(3) . . ? C81 P8 C71 97.3(3) . . ? C91 P8 Pd2 115.8(2) . . ? C81 P8 Pd2 119.4(2) . . ? C71 P8 Pd2 116.1(2) . . ? C16 C15 P2 115.1(4) . . ? C17 C16 C161 124.9(6) . . ? C17 C16 C15 119.8(6) . . ? C161 C16 C15 115.3(6) . . ? C17 C18 P1 116.6(4) . . ? C13 C14 P2 114.9(4) . . ? C13 C12 C121 122.5(6) . . ? C13 C12 C11 120.7(6) . . ? C121 C12 C11 116.7(6) . . ? C16 C17 C18 119.7(6) . . ? C16 C17 C171 124.6(6) . . ? C18 C17 C171 115.7(6) . . ? C12 C11 P1 117.3(4) . . ? C12 C13 C14 120.7(6) . . ? C12 C13 C131 124.7(6) . . ? C14 C13 C131 114.6(6) . . ? C26 C25 P4 117.2(5) . . ? C27 C28 P3 117.6(4) . . ? C22 C23 C24 119.8(6) . . ? C22 C23 C231 124.2(6) . . ? C24 C23 C231 115.9(6) . . ? C27 C26 C25 119.8(6) . . ? C27 C26 C261 126.0(6) . . ? C25 C26 C261 114.1(6) . . ? C22 C21 P3 113.6(4) . . ? C23 C24 P4 112.8(4) . . ? C23 C22 C221 125.6(6) . . ? C23 C22 C21 118.7(6) . . ? C221 C22 C21 115.7(6) . . ? C26 C27 C271 125.1(6) . . ? C26 C27 C28 119.5(6) . . ? C271 C27 C28 115.4(5) . . ? C37 C36 C361 125.1(6) . . ? C37 C36 C35 119.9(6) . . ? C361 C36 C35 115.0(6) . . ? C37 C38 P5 115.9(4) . . ? C32 C33 C331 127.1(6) . . ? C32 C33 C34 119.0(6) . . ? C331 C33 C34 113.9(6) . . ? C32 C31 P5 115.6(4) . . ? C36 C35 P6 114.8(4) . . ? C33 C34 P6 113.3(4) . . ? C33 C32 C321 124.4(6) . . ? C33 C32 C31 120.4(6) . . ? C321 C32 C31 115.2(6) . . ? C36 C37 C371 125.3(6) . . ? C36 C37 C38 119.0(6) . . ? C371 C37 C38 115.7(6) . . ? C44 C43 C42 120.7(6) . . ? C41 C42 C43 120.0(6) . . ? C43 C44 C45 119.5(6) . . ? C46 C41 C42 118.5(6) . . ? C46 C41 P7 116.3(5) . . ? C42 C41 P7 125.1(5) . . ? C46 C45 C44 120.1(7) . . ? C45 C46 C41 121.1(6) . . ? C53 C52 C51 120.6(6) . . ? C56 C51 C52 118.5(6) . . ? C56 C51 P7 117.3(5) . . ? C52 C51 P7 124.2(5) . . ? C55 C54 C53 119.8(6) . . ? C55 C56 C51 120.9(6) . . ? C52 C53 C54 120.3(6) . . ? C54 C55 C56 119.9(6) . . ? C66 C61 C62 117.7(6) . . ? C66 C61 P7 118.5(5) . . ? C62 C61 P7 123.6(5) . . ? C65 C66 C61 121.4(7) . . ? C66 C65 C64 120.1(7) . . ? C63 C62 C61 121.1(7) . . ? C62 C63 C64 120.1(8) . . ? C65 C64 C63 119.6(7) . . ? C76 C71 C72 117.9(6) . . ? C76 C71 P8 116.7(5) . . ? C72 C71 P8 125.2(5) . . ? C73 C72 C71 120.8(7) . . ? C71 C76 C75 121.5(7) . . ? C75 C74 C73 119.3(7) . . ? C72 C73 C74 120.5(7) . . ? C74 C75 C76 120.0(7) . . ? C86 C81 C82 118.8(6) . . ? C86 C81 P8 124.0(5) . . ? C82 C81 P8 117.2(5) . . ? C84 C85 C86 119.7(6) . . ? C84 C83 C82 119.7(6) . . ? C83 C84 C85 120.3(6) . . ? C81 C82 C83 120.5(6) . . ? C81 C86 C85 121.0(6) . . ? C93 C92 C91 121.2(6) . . ? C96 C91 C92 117.0(6) . . ? C96 C91 P8 123.5(5) . . ? C92 C91 P8 118.9(5) . . ? C94 C93 C92 120.8(7) . . ? C93 C94 C95 119.0(7) . . ? C91 C96 C95 121.5(6) . . ? C94 C95 C96 120.5(7) . . ? C21S C26S C25S 117.1(9) . . ? C21S C26S C27S 123.1(8) . . ? C25S C26S C27S 119.9(9) . . ? C24S C23S C22S 118.9(9) . . ? C24S C25S C26S 121.3(9) . . ? C22S C21S C26S 122.1(8) . . ? C25S C24S C23S 121.0(9) . . ? C21S C22S C23S 119.8(9) . . ? C11S O1S C14S 106.2(10) . . ? O1S C11S C12S 105.0(11) . . ? C13S C12S C11S 102.9(10) . . ? C12S C13S C14S 104.3(9) . . ? O1S C14S C13S 107.7(9) . . ? C14P O1P C11P 107.3(18) . . ? O1P C11P C12P 104.3(18) . . ? C13P C12P C11P 102.7(16) . . ? C12P C13P C14P 104.5(14) . . ? O1P C14P C13P 107.7(16) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.960 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.133 data_d8_10112 _database_code_depnum_ccdc_archive 'CCDC 863746' #TrackingRef '9137_web_deposit_cif_file_3_DanielTofan_1327008424.Ni2-D8_10112.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H126 Ni2 P8' _chemical_formula_weight 1789.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.0550(2) _cell_length_b 23.0550(2) _cell_length_c 31.0318(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14284.6(3) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9780 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 69.32 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5700 _exptl_absorpt_coefficient_mu 2.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5004 _exptl_absorpt_correction_T_max 0.8164 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Bruker D8 three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 95879 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 68.24 _reflns_number_total 5759 _reflns_number_gt 5155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+22.5075P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5759 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Ni1 Ni 0.0000 0.0000 -0.317968(14) 0.01598(11) Uani 1 3 d S . . Ni2 Ni 0.0000 0.0000 -0.190335(14) 0.01738(11) Uani 1 3 d S . . P1 P 0.075706(19) 0.094269(19) -0.290690(12) 0.01774(10) Uani 1 1 d . . . P2 P 0.071466(19) 0.095833(19) -0.219016(13) 0.01867(10) Uani 1 1 d . . . C11 C 0.16889(8) 0.13940(8) -0.29911(5) 0.0233(3) Uani 1 1 d . . . H11A H 0.1774 0.1325 -0.3294 0.028 Uiso 1 1 calc R . . H11B H 0.1859 0.1879 -0.2954 0.028 Uiso 1 1 calc R . . C12 C 0.21021(8) 0.12059(8) -0.27057(6) 0.0254(4) Uani 1 1 d . . . C13 C 0.20833(8) 0.12493(8) -0.22775(6) 0.0258(4) Uani 1 1 d . . . C14 C 0.16334(8) 0.14663(8) -0.20618(5) 0.0243(3) Uani 1 1 d . . . H14A H 0.1792 0.1937 -0.2143 0.029 Uiso 1 1 calc R . . H14B H 0.1688 0.1455 -0.1746 0.029 Uiso 1 1 calc R . . C15 C 0.04893(8) 0.16292(8) -0.21409(5) 0.0237(3) Uani 1 1 d . . . H15A H 0.0031 0.1454 -0.2257 0.028 Uiso 1 1 calc R . . H15B H 0.0477 0.1724 -0.1831 0.028 Uiso 1 1 calc R . . C16 C 0.09489(9) 0.22794(8) -0.23660(6) 0.0254(4) Uani 1 1 d . . . C17 C 0.10239(8) 0.22995(8) -0.27925(6) 0.0245(3) Uani 1 1 d . . . C18 C 0.06277(8) 0.16607(8) -0.30498(5) 0.0221(3) Uani 1 1 d . . . H18A H 0.0740 0.1768 -0.3358 0.026 Uiso 1 1 calc R . . H18B H 0.0146 0.1510 -0.3016 0.026 Uiso 1 1 calc R . . C121 C 0.25760(9) 0.10355(10) -0.29372(7) 0.0351(4) Uani 1 1 d . . . H12A H 0.3013 0.1442 -0.2971 0.053 Uiso 1 1 calc R . . H12B H 0.2394 0.0850 -0.3222 0.053 Uiso 1 1 calc R . . H12C H 0.2628 0.0704 -0.2769 0.053 Uiso 1 1 calc R . . C131 C 0.25491(9) 0.11534(10) -0.19786(6) 0.0333(4) Uani 1 1 d . . . H13A H 0.2790 0.0977 -0.2142 0.050 Uiso 1 1 calc R . . H13B H 0.2287 0.0837 -0.1750 0.050 Uiso 1 1 calc R . . H13C H 0.2871 0.1585 -0.1850 0.050 Uiso 1 1 calc R . . C161 C 0.13108(10) 0.28680(9) -0.20666(6) 0.0332(4) Uani 1 1 d . . . H16A H 0.1639 0.3259 -0.2230 0.050 Uiso 1 1 calc R . . H16B H 0.1542 0.2759 -0.1843 0.050 Uiso 1 1 calc R . . H16C H 0.0987 0.2969 -0.1931 0.050 Uiso 1 1 calc R . . C171 C 0.14876(9) 0.29161(8) -0.30508(6) 0.0312(4) Uani 1 1 d . . . H17A H 0.1774 0.3281 -0.2854 0.047 Uiso 1 1 calc R . . H17B H 0.1222 0.3052 -0.3226 0.047 Uiso 1 1 calc R . . H17C H 0.1767 0.2816 -0.3239 0.047 Uiso 1 1 calc R . . P3 P 0.0000 0.0000 -0.38699(2) 0.01704(14) Uani 1 3 d S . . C31 C -0.02488(8) -0.08021(8) -0.41471(5) 0.0196(3) Uani 1 1 d . . . C32 C -0.08369(8) -0.13657(8) -0.40079(5) 0.0245(3) Uani 1 1 d . . . H32 H -0.1082 -0.1324 -0.3776 0.029 Uiso 1 1 calc R . . C33 C -0.10701(9) -0.19868(8) -0.42026(6) 0.0277(4) Uani 1 1 d . . . H33 H -0.1477 -0.2362 -0.4108 0.033 Uiso 1 1 calc R . . C34 C -0.07086(9) -0.20566(8) -0.45340(6) 0.0274(4) Uani 1 1 d . . . H34 H -0.0863 -0.2481 -0.4666 0.033 Uiso 1 1 calc R . . C35 C -0.01168(9) -0.15022(9) -0.46724(6) 0.0280(4) Uani 1 1 d . . . H35 H 0.0135 -0.1549 -0.4898 0.034 Uiso 1 1 calc R . . C36 C 0.01075(8) -0.08808(8) -0.44825(5) 0.0233(3) Uani 1 1 d . . . H36 H 0.0509 -0.0505 -0.4583 0.028 Uiso 1 1 calc R . . P4 P 0.0000 0.0000 -0.12061(2) 0.01760(14) Uani 1 3 d S . . C41 C 0.01653(8) 0.07757(8) -0.09211(5) 0.0208(3) Uani 1 1 d . . . C42 C 0.05598(8) 0.10257(8) -0.05508(5) 0.0241(3) Uani 1 1 d . . . H42 H 0.0776 0.0801 -0.0435 0.029 Uiso 1 1 calc R . . C43 C 0.06392(9) 0.16004(9) -0.03495(6) 0.0276(4) Uani 1 1 d . . . H43 H 0.0909 0.1765 -0.0099 0.033 Uiso 1 1 calc R . . C44 C 0.03258(9) 0.19349(8) -0.05130(6) 0.0279(4) Uani 1 1 d . . . H44 H 0.0377 0.2325 -0.0373 0.034 Uiso 1 1 calc R . . C45 C -0.00632(9) 0.16938(9) -0.08828(6) 0.0276(4) Uani 1 1 d . . . H45 H -0.0277 0.1921 -0.0998 0.033 Uiso 1 1 calc R . . C46 C -0.01396(8) 0.11214(8) -0.10847(5) 0.0250(3) Uani 1 1 d . . . H46 H -0.0404 0.0963 -0.1339 0.030 Uiso 1 1 calc R . . C11S C -0.02830(10) 0.34893(10) -0.26062(7) 0.0386(4) Uani 1 1 d . . . H11S H -0.0691 0.3076 -0.2628 0.046 Uiso 1 1 calc R . . C12S C 0.03204(11) 0.35009(10) -0.26279(7) 0.0408(5) Uani 1 1 d . . . H12S H 0.0328 0.3095 -0.2661 0.049 Uiso 1 1 calc R . . C13S C 0.09158(11) 0.41049(11) -0.26013(7) 0.0430(5) Uani 1 1 d . . . H13S H 0.1331 0.4113 -0.2618 0.052 Uiso 1 1 calc R . . C14S C 0.09060(11) 0.46935(10) -0.25505(7) 0.0421(5) Uani 1 1 d . . . H14S H 0.1315 0.5107 -0.2533 0.050 Uiso 1 1 calc R . . C15S C 0.03042(11) 0.46824(11) -0.25255(7) 0.0430(5) Uani 1 1 d . . . H15S H 0.0298 0.5088 -0.2489 0.052 Uiso 1 1 calc R . . C16S C -0.02933(11) 0.40785(11) -0.25533(7) 0.0411(5) Uani 1 1 d . . . H16S H -0.0709 0.4071 -0.2536 0.049 Uiso 1 1 calc R . . C21S C -0.02065(18) 0.33243(13) -0.05445(8) 0.0668(8) Uani 1 1 d . . . H21S H -0.0097 0.3382 -0.0247 0.080 Uiso 1 1 calc R . . C22S C -0.08782(16) 0.29828(15) -0.06778(9) 0.0655(8) Uani 1 1 d . . . H22S H -0.1227 0.2805 -0.0470 0.079 Uiso 1 1 calc R . . C23S C -0.10280(12) 0.29065(13) -0.11032(9) 0.0542(6) Uani 1 1 d . . . H23S H -0.1483 0.2670 -0.1193 0.065 Uiso 1 1 calc R . . C24S C -0.05311(10) 0.31673(11) -0.14033(7) 0.0413(5) Uani 1 1 d . . . H24S H -0.0641 0.3119 -0.1701 0.050 Uiso 1 1 calc R . . C25S C 0.01258(11) 0.34987(11) -0.12791(7) 0.0443(5) Uani 1 1 d . . . H25S H 0.0468 0.3678 -0.1491 0.053 Uiso 1 1 calc R . . C26S C 0.02938(13) 0.35749(11) -0.08528(8) 0.0564(7) Uani 1 1 d . . . H26S H 0.0751 0.3799 -0.0768 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01678(15) 0.01678(15) 0.0144(2) 0.000 0.000 0.00839(7) Ni2 0.01883(15) 0.01883(15) 0.0145(2) 0.000 0.000 0.00941(8) P1 0.01816(19) 0.01761(19) 0.0160(2) 0.00005(13) -0.00135(13) 0.00788(15) P2 0.0195(2) 0.01878(19) 0.0160(2) -0.00035(14) -0.00138(14) 0.00822(16) C11 0.0198(8) 0.0236(8) 0.0213(8) 0.0025(6) 0.0009(6) 0.0069(6) C12 0.0174(7) 0.0236(8) 0.0301(10) 0.0048(7) 0.0007(6) 0.0064(6) C13 0.0185(8) 0.0246(8) 0.0282(9) 0.0035(7) -0.0025(6) 0.0061(7) C14 0.0210(8) 0.0243(8) 0.0213(9) 0.0008(6) -0.0051(6) 0.0065(7) C15 0.0272(8) 0.0229(8) 0.0224(8) -0.0038(6) -0.0026(6) 0.0135(7) C16 0.0282(9) 0.0207(8) 0.0276(9) -0.0029(6) -0.0060(7) 0.0124(7) C17 0.0260(8) 0.0189(8) 0.0271(9) -0.0012(6) -0.0056(7) 0.0102(7) C18 0.0251(8) 0.0200(8) 0.0213(8) -0.0004(6) -0.0047(6) 0.0114(7) C121 0.0261(9) 0.0413(11) 0.0382(11) 0.0020(8) 0.0026(8) 0.0171(8) C131 0.0238(9) 0.0403(10) 0.0328(10) 0.0078(8) -0.0027(7) 0.0139(8) C161 0.0425(10) 0.0236(9) 0.0290(10) -0.0054(7) -0.0073(8) 0.0131(8) C171 0.0375(10) 0.0219(8) 0.0274(9) -0.0004(7) -0.0065(7) 0.0097(8) P3 0.0185(2) 0.0185(2) 0.0141(3) 0.000 0.000 0.00924(10) C31 0.0232(8) 0.0210(7) 0.0167(8) -0.0004(6) -0.0026(6) 0.0127(6) C32 0.0272(8) 0.0254(8) 0.0215(8) 0.0005(6) 0.0043(6) 0.0136(7) C33 0.0292(9) 0.0218(8) 0.0298(9) 0.0017(7) 0.0021(7) 0.0109(7) C34 0.0336(9) 0.0225(8) 0.0301(9) -0.0049(7) -0.0025(7) 0.0169(7) C35 0.0309(9) 0.0313(9) 0.0275(9) -0.0036(7) 0.0036(7) 0.0200(8) C36 0.0228(8) 0.0251(8) 0.0222(9) 0.0001(6) 0.0015(6) 0.0122(7) P4 0.0192(2) 0.0192(2) 0.0144(3) 0.000 0.000 0.00960(10) C41 0.0221(8) 0.0190(7) 0.0191(8) 0.0005(6) 0.0027(6) 0.0086(6) C42 0.0248(8) 0.0238(8) 0.0221(9) 0.0002(6) -0.0004(6) 0.0110(7) C43 0.0267(8) 0.0262(8) 0.0231(9) -0.0033(6) -0.0013(7) 0.0080(7) C44 0.0307(9) 0.0194(8) 0.0299(10) -0.0024(7) 0.0054(7) 0.0097(7) C45 0.0294(9) 0.0252(8) 0.0312(9) 0.0022(7) 0.0031(7) 0.0159(7) C46 0.0259(8) 0.0268(8) 0.0215(9) -0.0001(6) 0.0003(6) 0.0125(7) C11S 0.0351(10) 0.0348(10) 0.0373(11) 0.0028(8) 0.0040(8) 0.0110(8) C12S 0.0421(11) 0.0340(10) 0.0461(12) 0.0008(9) 0.0075(9) 0.0189(9) C13S 0.0353(11) 0.0419(11) 0.0508(13) 0.0013(9) 0.0032(9) 0.0186(9) C14S 0.0388(11) 0.0333(10) 0.0463(12) 0.0001(9) -0.0029(9) 0.0122(9) C15S 0.0489(12) 0.0359(11) 0.0466(13) 0.0028(9) 0.0005(9) 0.0231(10) C16S 0.0376(11) 0.0461(12) 0.0424(12) 0.0066(9) 0.0031(9) 0.0229(9) C21S 0.127(3) 0.0506(14) 0.0314(13) -0.0008(10) -0.0122(14) 0.0512(17) C22S 0.082(2) 0.0790(19) 0.0625(18) 0.0374(15) 0.0377(15) 0.0610(17) C23S 0.0352(11) 0.0641(15) 0.0647(16) 0.0278(12) 0.0063(10) 0.0259(11) C24S 0.0366(11) 0.0441(11) 0.0390(12) -0.0009(9) -0.0075(9) 0.0171(9) C25S 0.0328(11) 0.0453(12) 0.0422(12) 0.0014(9) -0.0026(9) 0.0101(9) C26S 0.0531(14) 0.0365(12) 0.0512(15) 0.0031(10) -0.0211(11) 0.0011(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 Ni1 P3 2.1419(8) . ? Ni1 P1 2.1664(4) . ? Ni1 P1 2.1664(4) 2 ? Ni1 P1 2.1664(4) 3 ? Ni2 P4 2.1637(8) . ? Ni2 P2 2.1790(4) . ? Ni2 P2 2.1790(4) 2 ? Ni2 P2 2.1790(4) 3 ? P1 C18 1.8760(16) . ? P1 C11 1.8791(16) . ? P1 P2 2.2274(6) . ? P2 C15 1.8679(16) . ? P2 C14 1.8805(16) . ? C11 C12 1.514(2) . ? C12 C13 1.335(3) . ? C12 C121 1.514(2) . ? C13 C14 1.514(2) . ? C13 C131 1.516(2) . ? C15 C16 1.506(2) . ? C16 C17 1.333(3) . ? C16 C161 1.506(2) . ? C17 C171 1.512(2) . ? C17 C18 1.515(2) . ? P3 C31 1.8514(16) 3 ? P3 C31 1.8514(16) 2 ? P3 C31 1.8514(16) . ? C31 C36 1.393(2) . ? C31 C32 1.397(2) . ? C32 C33 1.391(2) . ? C33 C34 1.383(2) . ? C34 C35 1.391(3) . ? C35 C36 1.388(2) . ? P4 C41 1.8558(16) 3 ? P4 C41 1.8558(16) 2 ? P4 C41 1.8558(16) . ? C41 C46 1.396(2) . ? C41 C42 1.399(2) . ? C42 C43 1.392(2) . ? C43 C44 1.390(3) . ? C44 C45 1.390(3) . ? C45 C46 1.390(2) . ? C11S C12S 1.380(3) . ? C11S C16S 1.380(3) . ? C12S C13S 1.385(3) . ? C13S C14S 1.377(3) . ? C14S C15S 1.377(3) . ? C15S C16S 1.388(3) . ? C21S C26S 1.383(4) . ? C21S C22S 1.403(4) . ? C22S C23S 1.354(4) . ? C23S C24S 1.361(3) . ? C24S C25S 1.367(3) . ? C25S C26S 1.365(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 P3 Ni1 P1 113.001(15) . . ? P3 Ni1 P1 113.003(15) . 2 ? P1 Ni1 P1 105.721(16) . 2 ? P3 Ni1 P1 113.003(15) . 3 ? P1 Ni1 P1 105.722(16) . 3 ? P1 Ni1 P1 105.720(16) 2 3 ? P4 Ni2 P2 114.108(15) . . ? P4 Ni2 P2 114.109(15) . 2 ? P2 Ni2 P2 104.463(17) . 2 ? P4 Ni2 P2 114.109(15) . 3 ? P2 Ni2 P2 104.461(17) . 3 ? P2 Ni2 P2 104.461(17) 2 3 ? C18 P1 C11 96.93(7) . . ? C18 P1 Ni1 112.90(5) . . ? C11 P1 Ni1 128.74(6) . . ? C18 P1 P2 101.19(5) . . ? C11 P1 P2 100.20(5) . . ? Ni1 P1 P2 112.74(2) . . ? C15 P2 C14 99.21(8) . . ? C15 P2 Ni2 115.08(5) . . ? C14 P2 Ni2 126.17(6) . . ? C15 P2 P1 97.34(5) . . ? C14 P2 P1 100.18(5) . . ? Ni2 P2 P1 114.11(2) . . ? C12 C11 P1 117.96(11) . . ? C13 C12 C11 120.80(16) . . ? C13 C12 C121 123.10(16) . . ? C11 C12 C121 115.84(15) . . ? C12 C13 C14 121.19(15) . . ? C12 C13 C131 123.11(16) . . ? C14 C13 C131 115.44(15) . . ? C13 C14 P2 116.42(11) . . ? C16 C15 P2 115.96(12) . . ? C17 C16 C161 125.27(16) . . ? C17 C16 C15 120.63(15) . . ? C161 C16 C15 114.07(15) . . ? C16 C17 C171 125.28(15) . . ? C16 C17 C18 119.00(15) . . ? C171 C17 C18 115.71(15) . . ? C17 C18 P1 116.66(11) . . ? C31 P3 C31 100.15(6) 3 2 ? C31 P3 C31 100.15(6) 3 . ? C31 P3 C31 100.15(6) 2 . ? C31 P3 Ni1 117.68(5) 3 . ? C31 P3 Ni1 117.68(5) 2 . ? C31 P3 Ni1 117.69(5) . . ? C36 C31 C32 118.11(15) . . ? C36 C31 P3 124.68(12) . . ? C32 C31 P3 117.21(12) . . ? C33 C32 C31 121.27(15) . . ? C34 C33 C32 119.85(16) . . ? C33 C34 C35 119.58(16) . . ? C36 C35 C34 120.37(16) . . ? C35 C36 C31 120.80(16) . . ? C41 P4 C41 99.17(7) 3 2 ? C41 P4 C41 99.17(7) 3 . ? C41 P4 C41 99.17(7) 2 . ? C41 P4 Ni2 118.46(5) 3 . ? C41 P4 Ni2 118.46(5) 2 . ? C41 P4 Ni2 118.46(5) . . ? C46 C41 C42 118.24(15) . . ? C46 C41 P4 117.23(12) . . ? C42 C41 P4 124.52(12) . . ? C43 C42 C41 120.66(16) . . ? C44 C43 C42 120.48(16) . . ? C43 C44 C45 119.34(16) . . ? C44 C45 C46 120.13(16) . . ? C45 C46 C41 121.14(16) . . ? C12S C11S C16S 120.01(19) . . ? C11S C12S C13S 120.0(2) . . ? C14S C13S C12S 120.1(2) . . ? C15S C14S C13S 120.1(2) . . ? C14S C15S C16S 120.0(2) . . ? C11S C16S C15S 119.9(2) . . ? C26S C21S C22S 119.1(2) . . ? C23S C22S C21S 119.9(2) . . ? C22S C23S C24S 120.4(2) . . ? C23S C24S C25S 120.4(2) . . ? C26S C25S C24S 120.6(2) . . ? C25S C26S C21S 119.5(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.393 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.048 data_11124 _database_code_depnum_ccdc_archive 'CCDC 863747' #TrackingRef '9138_web_deposit_cif_file_4_DanielTofan_1327008424.As2Ni2P6 11124.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H126 As2 Ni2 P6' _chemical_formula_weight 1877.17 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 23.0523(8) _cell_length_b 23.0523(8) _cell_length_c 31.4482(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14472.9(9) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.79 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5916 _exptl_absorpt_coefficient_mu 1.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6417 _exptl_absorpt_correction_T_max 0.7116 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; 'Siemens three-circle diffractometer, Bruker APEX CCD' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 135796 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 30.51 _reflns_number_total 9827 _reflns_number_gt 8353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2009.9.0 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+27.5454P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9827 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.3333 -0.3333 -0.640064(8) 0.01489(6) Uani 1 3 d S . . Ni2 Ni 0.3333 -0.3333 -0.517540(8) 0.01336(6) Uani 1 3 d S . . As1 As 0.3333 -0.3333 -0.712467(7) 0.01599(5) Uani 1 3 d S . . As2 As 0.3333 -0.3333 -0.446020(7) 0.01537(5) Uani 1 3 d S . . P1 P 0.309532(16) -0.429482(16) -0.613397(10) 0.01696(6) Uani 1 1 d . . . P2 P 0.314828(16) -0.427899(15) -0.542704(10) 0.01578(6) Uani 1 1 d . . . C11 C 0.22037(7) -0.49760(7) -0.61863(4) 0.0225(2) Uani 1 1 d . . . H11A H 0.1914 -0.4807 -0.6075 0.027 Uiso 1 1 calc R . . H11B H 0.2101 -0.5072 -0.6493 0.027 Uiso 1 1 calc R . . C12 C 0.20204(7) -0.56228(7) -0.59632(4) 0.0236(3) Uani 1 1 d . . . C13 C 0.20711(7) -0.56393(6) -0.55386(4) 0.0226(2) Uani 1 1 d . . . C14 C 0.23041(7) -0.50003(6) -0.52883(4) 0.0209(2) Uani 1 1 d . . . H14A H 0.2307 -0.5104 -0.4983 0.025 Uiso 1 1 calc R . . H14B H 0.1970 -0.4855 -0.5326 0.025 Uiso 1 1 calc R . . C15 C 0.36396(7) -0.47180(7) -0.53389(4) 0.0210(2) Uani 1 1 d . . . H15A H 0.3792 -0.4644 -0.5039 0.025 Uiso 1 1 calc R . . H15B H 0.3330 -0.5205 -0.5374 0.025 Uiso 1 1 calc R . . C16 C 0.42441(7) -0.45235(7) -0.56183(4) 0.0225(2) Uani 1 1 d . . . C17 C 0.41851(7) -0.45662(7) -0.60436(4) 0.0236(3) Uani 1 1 d . . . C18 C 0.35186(7) -0.47900(7) -0.62585(4) 0.0223(2) Uani 1 1 d . . . H18A H 0.3210 -0.5263 -0.6180 0.027 Uiso 1 1 calc R . . H18B H 0.3587 -0.4777 -0.6570 0.027 Uiso 1 1 calc R . . C121 C 0.18031(9) -0.62121(7) -0.62548(5) 0.0323(3) Uani 1 1 d . . . H12A H 0.2144 -0.6101 -0.6475 0.048 Uiso 1 1 calc R . . H12B H 0.1377 -0.6321 -0.6389 0.048 Uiso 1 1 calc R . . H12C H 0.1747 -0.6598 -0.6091 0.048 Uiso 1 1 calc R . . C131 C 0.19217(8) -0.62532(7) -0.52843(5) 0.0299(3) Uani 1 1 d . . . H13A H 0.1505 -0.6407 -0.5124 0.045 Uiso 1 1 calc R . . H13B H 0.2290 -0.6143 -0.5086 0.045 Uiso 1 1 calc R . . H13C H 0.1873 -0.6609 -0.5477 0.045 Uiso 1 1 calc R . . C161 C 0.48869(8) -0.43511(9) -0.53879(5) 0.0324(3) Uani 1 1 d . . . H16A H 0.4923 -0.4755 -0.5358 0.049 Uiso 1 1 calc R . . H16B H 0.4884 -0.4173 -0.5106 0.049 Uiso 1 1 calc R . . H16C H 0.5270 -0.4014 -0.5551 0.049 Uiso 1 1 calc R . . C171 C 0.47514(8) -0.44610(9) -0.63352(5) 0.0312(3) Uani 1 1 d . . . H17A H 0.5166 -0.4289 -0.6170 0.047 Uiso 1 1 calc R . . H17B H 0.4810 -0.4138 -0.6557 0.047 Uiso 1 1 calc R . . H17C H 0.4645 -0.4888 -0.6467 0.047 Uiso 1 1 calc R . . C21 C 0.26800(6) -0.41439(6) -0.74318(4) 0.0191(2) Uani 1 1 d . . . C22 C 0.20369(7) -0.45000(7) -0.72649(4) 0.0242(3) Uani 1 1 d . . . H22 H 0.1934 -0.4351 -0.7009 0.029 Uiso 1 1 calc R . . C23 C 0.15396(7) -0.50720(7) -0.74666(5) 0.0277(3) Uani 1 1 d . . . H23 H 0.1102 -0.5310 -0.7348 0.033 Uiso 1 1 calc R . . C24 C 0.16854(8) -0.52942(7) -0.78413(5) 0.0278(3) Uani 1 1 d . . . H24 H 0.1347 -0.5680 -0.7982 0.033 Uiso 1 1 calc R . . C25 C 0.23294(8) -0.49487(7) -0.80086(5) 0.0266(3) Uani 1 1 d . . . H25 H 0.2432 -0.5103 -0.8262 0.032 Uiso 1 1 calc R . . C26 C 0.28261(7) -0.43752(7) -0.78055(4) 0.0228(2) Uani 1 1 d . . . H26 H 0.3265 -0.4141 -0.7922 0.027 Uiso 1 1 calc R . . C31 C 0.38965(6) -0.24839(6) -0.41627(4) 0.0182(2) Uani 1 1 d . . . C32 C 0.38631(7) -0.19249(7) -0.42997(4) 0.0236(3) Uani 1 1 d . . . H32 H 0.3571 -0.1970 -0.4526 0.028 Uiso 1 1 calc R . . C33 C 0.42524(7) -0.13019(7) -0.41090(5) 0.0265(3) Uani 1 1 d . . . H33 H 0.4221 -0.0927 -0.4203 0.032 Uiso 1 1 calc R . . C34 C 0.46871(7) -0.12303(7) -0.37814(5) 0.0267(3) Uani 1 1 d . . . H34 H 0.4954 -0.0806 -0.3651 0.032 Uiso 1 1 calc R . . C35 C 0.47314(7) -0.17807(7) -0.36452(5) 0.0269(3) Uani 1 1 d . . . H35 H 0.5033 -0.1731 -0.3424 0.032 Uiso 1 1 calc R . . C36 C 0.43342(7) -0.24059(7) -0.38329(4) 0.0223(2) Uani 1 1 d . . . H36 H 0.4362 -0.2781 -0.3735 0.027 Uiso 1 1 calc R . . C1S C 0.76851(9) 0.07563(10) -0.08707(6) 0.0417(4) Uani 1 1 d . . . H1S H 0.8094 0.0753 -0.0848 0.050 Uiso 1 1 calc R . . C2S C 0.76848(10) 0.13565(9) -0.08458(7) 0.0439(4) Uani 1 1 d . . . H2S H 0.8094 0.1764 -0.0807 0.053 Uiso 1 1 calc R . . C3S C 0.70917(10) 0.13631(9) -0.08773(6) 0.0420(4) Uani 1 1 d . . . H3S H 0.7093 0.1775 -0.0862 0.050 Uiso 1 1 calc R . . C4S C 0.64961(10) 0.07692(10) -0.09308(7) 0.0440(4) Uani 1 1 d . . . H4S H 0.6086 0.0772 -0.0950 0.053 Uiso 1 1 calc R . . C5S C 0.64963(9) 0.01691(9) -0.09564(6) 0.0418(4) Uani 1 1 d . . . H5S H 0.6086 -0.0239 -0.0993 0.050 Uiso 1 1 calc R . . C6S C 0.70904(9) 0.01625(9) -0.09280(6) 0.0383(4) Uani 1 1 d . . . H6S H 0.7090 -0.0249 -0.0948 0.046 Uiso 1 1 calc R . . C1P C 0.56199(10) -0.05691(10) -0.27736(7) 0.0478(5) Uani 1 1 d . . . H1P H 0.5170 -0.0758 -0.2869 0.057 Uiso 1 1 calc R . . C2P C 0.61300(9) -0.03521(9) -0.30620(6) 0.0371(4) Uani 1 1 d . . . H2P H 0.6032 -0.0400 -0.3358 0.044 Uiso 1 1 calc R . . C3P C 0.67824(9) -0.00652(11) -0.29289(6) 0.0444(4) Uani 1 1 d . . . H3P H 0.7134 0.0089 -0.3132 0.053 Uiso 1 1 calc R . . C4P C 0.69288(12) -0.00005(14) -0.25024(7) 0.0581(6) Uani 1 1 d . . . H4P H 0.7381 0.0199 -0.2411 0.070 Uiso 1 1 calc R . . C5P C 0.64204(16) -0.02250(13) -0.22067(7) 0.0623(7) Uani 1 1 d . . . H5P H 0.6519 -0.0185 -0.1911 0.075 Uiso 1 1 calc R . . C6P C 0.57549(14) -0.05142(11) -0.23471(7) 0.0593(6) Uani 1 1 d . . . H6P H 0.5399 -0.0671 -0.2147 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01584(8) 0.01584(8) 0.01300(11) 0.000 0.000 0.00792(4) Ni2 0.01366(8) 0.01366(8) 0.01277(11) 0.000 0.000 0.00683(4) As1 0.01743(7) 0.01743(7) 0.01309(9) 0.000 0.000 0.00872(3) As2 0.01667(6) 0.01667(6) 0.01278(9) 0.000 0.000 0.00833(3) P1 0.01983(14) 0.01683(14) 0.01482(14) -0.00049(10) 0.00084(11) 0.00961(12) P2 0.01765(14) 0.01521(13) 0.01469(14) 0.00013(10) 0.00123(10) 0.00837(11) C11 0.0229(6) 0.0203(6) 0.0213(6) -0.0019(5) -0.0017(5) 0.0086(5) C12 0.0249(6) 0.0173(6) 0.0244(6) -0.0044(5) 0.0009(5) 0.0075(5) C13 0.0235(6) 0.0166(5) 0.0241(6) -0.0015(5) 0.0033(5) 0.0074(5) C14 0.0217(6) 0.0175(5) 0.0201(6) -0.0016(4) 0.0034(5) 0.0074(5) C15 0.0269(6) 0.0218(6) 0.0194(6) 0.0031(4) 0.0030(5) 0.0160(5) C16 0.0241(6) 0.0230(6) 0.0254(6) 0.0028(5) 0.0035(5) 0.0157(5) C17 0.0278(6) 0.0242(6) 0.0248(6) 0.0037(5) 0.0057(5) 0.0175(5) C18 0.0292(7) 0.0228(6) 0.0193(6) -0.0014(5) 0.0033(5) 0.0161(5) C121 0.0409(8) 0.0219(7) 0.0272(7) -0.0072(5) 0.0002(6) 0.0106(6) C131 0.0388(8) 0.0191(6) 0.0280(7) 0.0015(5) 0.0062(6) 0.0117(6) C161 0.0307(7) 0.0396(8) 0.0353(8) 0.0013(6) -0.0017(6) 0.0239(7) C171 0.0343(8) 0.0397(8) 0.0303(7) 0.0069(6) 0.0104(6) 0.0264(7) C21 0.0223(6) 0.0188(5) 0.0162(5) 0.0001(4) -0.0013(4) 0.0101(5) C22 0.0249(6) 0.0245(6) 0.0221(6) 0.0002(5) 0.0009(5) 0.0115(5) C23 0.0225(6) 0.0239(6) 0.0321(7) 0.0016(5) -0.0003(5) 0.0082(5) C24 0.0294(7) 0.0191(6) 0.0312(7) -0.0025(5) -0.0077(6) 0.0093(5) C25 0.0332(7) 0.0240(6) 0.0231(6) -0.0040(5) -0.0021(5) 0.0146(6) C26 0.0257(6) 0.0221(6) 0.0197(6) -0.0010(5) 0.0011(5) 0.0114(5) C31 0.0177(5) 0.0185(5) 0.0161(5) -0.0005(4) 0.0005(4) 0.0073(4) C32 0.0253(6) 0.0222(6) 0.0223(6) 0.0005(5) -0.0052(5) 0.0110(5) C33 0.0275(7) 0.0196(6) 0.0296(7) 0.0007(5) -0.0030(5) 0.0096(5) C34 0.0232(6) 0.0207(6) 0.0306(7) -0.0043(5) -0.0046(5) 0.0068(5) C35 0.0238(6) 0.0261(7) 0.0284(7) -0.0043(5) -0.0088(5) 0.0107(5) C36 0.0229(6) 0.0226(6) 0.0216(6) -0.0018(5) -0.0040(5) 0.0114(5) C1S 0.0353(9) 0.0418(9) 0.0475(10) 0.0053(8) 0.0010(7) 0.0188(8) C2S 0.0369(9) 0.0325(8) 0.0524(11) 0.0015(8) -0.0003(8) 0.0100(7) C3S 0.0447(10) 0.0305(8) 0.0488(10) 0.0014(7) 0.0006(8) 0.0173(8) C4S 0.0368(9) 0.0389(9) 0.0571(12) 0.0013(8) -0.0044(8) 0.0195(8) C5S 0.0367(9) 0.0317(8) 0.0504(11) -0.0009(7) -0.0087(8) 0.0121(7) C6S 0.0442(9) 0.0316(8) 0.0399(9) 0.0024(7) -0.0030(7) 0.0195(7) C1P 0.0320(9) 0.0437(10) 0.0564(12) -0.0180(9) 0.0036(8) 0.0105(8) C2P 0.0318(8) 0.0425(9) 0.0369(8) -0.0070(7) -0.0058(7) 0.0186(7) C3P 0.0307(8) 0.0626(12) 0.0424(10) -0.0069(9) -0.0047(7) 0.0252(9) C4P 0.0582(13) 0.0925(18) 0.0501(12) -0.0251(12) -0.0262(10) 0.0576(13) C5P 0.119(2) 0.0653(14) 0.0307(9) -0.0099(9) -0.0132(12) 0.0674(16) C6P 0.0773(16) 0.0398(10) 0.0500(12) -0.0032(9) 0.0264(11) 0.0213(11) _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 P1 2.1682(3) 3_655 ? Ni1 P1 2.1682(3) 2_545 ? Ni1 P1 2.1681(3) . ? Ni1 As1 2.2769(3) . ? Ni2 P2 2.1519(3) . ? Ni2 P2 2.1519(3) 3_655 ? Ni2 P2 2.1519(3) 2_545 ? Ni2 As2 2.2492(3) . ? As1 C21 1.9695(13) 3_655 ? As1 C21 1.9695(13) . ? As1 C21 1.9695(13) 2_545 ? As2 C31 1.9629(12) 2_545 ? As2 C31 1.9629(12) . ? As2 C31 1.9629(12) 3_655 ? P1 C11 1.8681(14) . ? P1 C18 1.8768(13) . ? P1 P2 2.2258(4) . ? P2 C14 1.8724(13) . ? P2 C15 1.8788(13) . ? C11 C12 1.5046(19) . ? C12 C13 1.343(2) . ? C12 C121 1.5021(19) . ? C13 C131 1.508(2) . ? C13 C14 1.5123(18) . ? C15 C16 1.5135(18) . ? C16 C17 1.343(2) . ? C16 C161 1.513(2) . ? C17 C171 1.5124(19) . ? C17 C18 1.513(2) . ? C21 C22 1.3894(19) . ? C21 C26 1.3992(18) . ? C22 C23 1.394(2) . ? C23 C24 1.391(2) . ? C24 C25 1.390(2) . ? C25 C26 1.3975(19) . ? C31 C36 1.3945(17) . ? C31 C32 1.3968(18) . ? C32 C33 1.3923(19) . ? C33 C34 1.388(2) . ? C34 C35 1.390(2) . ? C35 C36 1.3944(19) . ? C1S C6S 1.382(3) . ? C1S C2S 1.386(3) . ? C2S C3S 1.379(3) . ? C3S C4S 1.381(3) . ? C4S C5S 1.386(3) . ? C5S C6S 1.380(3) . ? C1P C2P 1.366(3) . ? C1P C6P 1.368(3) . ? C2P C3P 1.371(2) . ? C3P C4P 1.373(3) . ? C4P C5P 1.378(4) . ? C5P C6P 1.404(4) . ? 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 P1 105.995(12) 3_655 2_545 ? P1 Ni1 P1 105.996(12) 3_655 . ? P1 Ni1 P1 105.996(12) 2_545 . ? P1 Ni1 As1 112.757(10) 3_655 . ? P1 Ni1 As1 112.757(11) 2_545 . ? P1 Ni1 As1 112.755(11) . . ? P2 Ni2 P2 107.287(11) . 3_655 ? P2 Ni2 P2 107.286(11) . 2_545 ? P2 Ni2 P2 107.288(11) 3_655 2_545 ? P2 Ni2 As2 111.578(10) . . ? P2 Ni2 As2 111.575(10) 3_655 . ? P2 Ni2 As2 111.575(10) 2_545 . ? C21 As1 C21 98.00(5) 3_655 . ? C21 As1 C21 97.99(5) 3_655 2_545 ? C21 As1 C21 98.00(5) . 2_545 ? C21 As1 Ni1 119.37(4) 3_655 . ? C21 As1 Ni1 119.37(4) . . ? C21 As1 Ni1 119.37(4) 2_545 . ? C31 As2 C31 99.17(5) 2_545 . ? C31 As2 C31 99.17(5) 2_545 3_655 ? C31 As2 C31 99.17(5) . 3_655 ? C31 As2 Ni2 118.46(4) 2_545 . ? C31 As2 Ni2 118.46(4) . . ? C31 As2 Ni2 118.46(4) 3_655 . ? C11 P1 C18 99.11(6) . . ? C11 P1 Ni1 115.78(5) . . ? C18 P1 Ni1 126.75(5) . . ? C11 P1 P2 97.48(4) . . ? C18 P1 P2 100.22(4) . . ? Ni1 P1 P2 112.694(17) . . ? C14 P2 C15 97.24(6) . . ? C14 P2 Ni2 113.92(4) . . ? C15 P2 Ni2 128.60(5) . . ? C14 P2 P1 101.19(4) . . ? C15 P2 P1 100.45(4) . . ? Ni2 P2 P1 111.432(17) . . ? C12 C11 P1 115.96(10) . . ? C13 C12 C121 125.16(13) . . ? C13 C12 C11 120.43(12) . . ? C121 C12 C11 114.39(12) . . ? C12 C13 C131 124.88(12) . . ? C12 C13 C14 118.92(12) . . ? C131 C13 C14 116.20(12) . . ? C13 C14 P2 116.68(9) . . ? C16 C15 P2 117.94(9) . . ? C17 C16 C161 123.11(13) . . ? C17 C16 C15 120.79(13) . . ? C161 C16 C15 115.82(12) . . ? C16 C17 C171 122.97(13) . . ? C16 C17 C18 121.20(12) . . ? C171 C17 C18 115.59(12) . . ? C17 C18 P1 116.58(9) . . ? C22 C21 C26 118.77(12) . . ? C22 C21 As1 117.33(10) . . ? C26 C21 As1 123.90(10) . . ? C21 C22 C23 121.12(13) . . ? C24 C23 C22 119.85(14) . . ? C25 C24 C23 119.66(13) . . ? C24 C25 C26 120.27(13) . . ? C25 C26 C21 120.32(13) . . ? C36 C31 C32 118.72(12) . . ? C36 C31 As2 123.92(10) . . ? C32 C31 As2 117.35(9) . . ? C33 C32 C31 120.96(12) . . ? C34 C33 C32 119.79(13) . . ? C33 C34 C35 119.88(13) . . ? C34 C35 C36 120.18(13) . . ? C35 C36 C31 120.46(13) . . ? C6S C1S C2S 120.06(18) . . ? C3S C2S C1S 120.16(18) . . ? C2S C3S C4S 119.83(18) . . ? C3S C4S C5S 120.02(18) . . ? C6S C5S C4S 120.18(17) . . ? C5S C6S C1S 119.74(17) . . ? C2P C1P C6P 120.2(2) . . ? C1P C2P C3P 120.64(18) . . ? C2P C3P C4P 120.1(2) . . ? C3P C4P C5P 120.1(2) . . ? C4P C5P C6P 119.23(19) . . ? C1P C6P C5P 119.8(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.811 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.060