# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_3b_3b' _database_code_depnum_ccdc_archive 'CCDC 876279' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H46 N O P Pd' _chemical_formula_sum 'C30 H46 N O P Pd' _chemical_formula_weight 574.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3755(12) _cell_length_b 47.445(6) _cell_length_c 12.2103(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.737(5) _cell_angle_gamma 90.00 _cell_volume 6010.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8603 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 30.81 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.874 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37027 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.25 _reflns_number_total 10798 _reflns_number_gt 8748 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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^)+(0.0405P)^2^+1.5017P] 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 10798 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C30 C 0.5239(3) 0.28678(8) 0.3883(3) 0.0300(8) Uani 1 1 d . . . H30 H 0.4734 0.2703 0.3782 0.036 Uiso 1 1 d R . . C29 C 0.4849(3) 0.30732(8) 0.4615(3) 0.0334(9) Uani 1 1 d . . . H29 H 0.4082 0.3048 0.5020 0.040 Uiso 1 1 d R . . C28 C 0.5585(3) 0.33182(8) 0.4754(3) 0.0269(8) Uani 1 1 d . . . H28 H 0.5316 0.3460 0.5250 0.032 Uiso 1 1 d R . . C27 C 0.6719(3) 0.33542(7) 0.4160(3) 0.0208(7) Uani 1 1 d . . . H27 H 0.7205 0.3522 0.4254 0.025 Uiso 1 1 d R . . C26 C 0.7154(3) 0.31467(7) 0.3427(3) 0.0171(7) Uani 1 1 d . . . C25 C 0.6379(3) 0.29031(7) 0.3292(3) 0.0189(7) Uani 1 1 d . . . C24 C 0.5855(4) 0.25130(9) 0.1889(4) 0.0365(9) Uani 1 1 d . . . H24A H 0.5335 0.2405 0.2406 0.055 Uiso 1 1 d R . . H24B H 0.6265 0.2384 0.1374 0.055 Uiso 1 1 d R . . H24C H 0.5300 0.2645 0.1483 0.055 Uiso 1 1 d R . . C23 C 0.7720(4) 0.24708(7) 0.3214(3) 0.0284(8) Uani 1 1 d . . . H23A H 0.8425 0.2573 0.3580 0.043 Uiso 1 1 d R . . H23B H 0.8076 0.2326 0.2734 0.043 Uiso 1 1 d R . . H23C H 0.7175 0.2382 0.3765 0.043 Uiso 1 1 d R . . C22 C 0.6903(3) 0.26784(7) 0.2525(3) 0.0205(7) Uani 1 1 d . . . C21 C 0.7753(3) 0.28379(7) 0.1708(3) 0.0197(7) Uani 1 1 d . . . H21A H 0.7203 0.2924 0.1130 0.024 Uiso 1 1 d R . . H21B H 0.8346 0.2703 0.1354 0.024 Uiso 1 1 d R . . C20 C 0.9772(4) 0.30636(9) -0.0756(3) 0.0331(9) Uani 1 1 d . . . H20A H 0.8929 0.3015 -0.0455 0.050 Uiso 1 1 d R . . H20B H 1.0290 0.2892 -0.0833 0.050 Uiso 1 1 d R . . H20C H 0.9653 0.3152 -0.1474 0.050 Uiso 1 1 d R . . C19 C 0.9773(4) 0.35559(8) 0.0064(3) 0.0312(8) Uani 1 1 d . . . H19A H 0.9713 0.3636 -0.0675 0.047 Uiso 1 1 d R . . H19B H 1.0257 0.3685 0.0542 0.047 Uiso 1 1 d R . . H19C H 0.8904 0.3529 0.0353 0.047 Uiso 1 1 d R . . C18 C 1.0471(3) 0.32705(8) 0.0025(3) 0.0238(7) Uani 1 1 d . . . H18 H 1.1370 0.3300 -0.0235 0.029 Uiso 1 1 d R . . C17 C 1.1764(4) 0.26772(8) 0.2452(3) 0.0348(9) Uani 1 1 d . . . H17A H 1.2207 0.2495 0.2400 0.052 Uiso 1 1 d R . . H17B H 1.0953 0.2653 0.2844 0.052 Uiso 1 1 d R . . H17C H 1.2314 0.2812 0.2848 0.052 Uiso 1 1 d R . . C16 C 1.2703(4) 0.28135(9) 0.0613(4) 0.0363(9) Uani 1 1 d . . . H16A H 1.3260 0.2961 0.0921 0.054 Uiso 1 1 d R . . H16B H 1.2468 0.2862 -0.0144 0.054 Uiso 1 1 d R . . H16C H 1.3163 0.2633 0.0625 0.054 Uiso 1 1 d R . . C15 C 1.1478(3) 0.27894(7) 0.1300(3) 0.0236(7) Uani 1 1 d . . . H15 H 1.0912 0.2647 0.0928 0.028 Uiso 1 1 d R . . C14 C 1.2372(3) 0.36383(7) 0.3398(3) 0.0228(7) Uani 1 1 d . . . H14A H 1.2103 0.3727 0.4084 0.034 Uiso 1 1 d R . . H14B H 1.2633 0.3785 0.2879 0.034 Uiso 1 1 d R . . H14C H 1.3101 0.3512 0.3545 0.034 Uiso 1 1 d R . . C13 C 1.1271(3) 0.34731(7) 0.2919(3) 0.0170(6) Uani 1 1 d . . . C12 C 0.9187(4) 0.29776(8) 0.5851(3) 0.0295(8) Uani 1 1 d . . . H12A H 0.9007 0.3040 0.6600 0.044 Uiso 1 1 d R . . H12B H 0.9479 0.2781 0.5864 0.044 Uiso 1 1 d R . . H12C H 0.8401 0.2993 0.5402 0.044 Uiso 1 1 d R . . C11 C 1.1483(4) 0.31421(9) 0.6065(4) 0.0412(11) Uani 1 1 d . . . H11A H 1.2132 0.3271 0.5774 0.062 Uiso 1 1 d R . . H11B H 1.1811 0.2949 0.6040 0.062 Uiso 1 1 d R . . H11C H 1.1297 0.3193 0.6824 0.062 Uiso 1 1 d R . . C10 C 1.0239(4) 0.31639(7) 0.5370(3) 0.0261(8) Uani 1 1 d . . . H10 H 1.0431 0.3092 0.4620 0.031 Uiso 1 1 d R . . C9 C 0.9433(4) 0.43618(8) 0.3068(3) 0.0325(9) Uani 1 1 d . . . H9A H 0.8682 0.4441 0.3437 0.049 Uiso 1 1 d R . . H9B H 0.9477 0.4437 0.2322 0.049 Uiso 1 1 d R . . H9C H 1.0219 0.4412 0.3475 0.049 Uiso 1 1 d R . . C8 C 0.8039(4) 0.39541(8) 0.2439(3) 0.0302(8) Uani 1 1 d . . . H8A H 0.8017 0.3749 0.2346 0.045 Uiso 1 1 d R . . H8B H 0.7987 0.4045 0.1720 0.045 Uiso 1 1 d R . . H8C H 0.7307 0.4014 0.2883 0.045 Uiso 1 1 d R . . C7 C 0.9307(3) 0.40400(7) 0.3018(3) 0.0224(7) Uani 1 1 d . . . H7 H 1.0034 0.3967 0.2569 0.027 Uiso 1 1 d R . . C6 C 0.9817(3) 0.34709(7) 0.5259(3) 0.0189(7) Uani 1 1 d . . . C5 C 0.9426(3) 0.36236(8) 0.6184(3) 0.0243(7) Uani 1 1 d . . . H5 H 0.9429 0.3533 0.6879 0.029 Uiso 1 1 d R . . C4 C 0.9037(3) 0.39030(8) 0.6102(3) 0.0268(8) Uani 1 1 d . . . H4 H 0.8780 0.4002 0.6739 0.032 Uiso 1 1 d R . . C3 C 0.9021(3) 0.40381(7) 0.5088(3) 0.0246(7) Uani 1 1 d . . . H3 H 0.8755 0.4229 0.5042 0.030 Uiso 1 1 d R . . C2 C 0.9393(3) 0.38963(7) 0.4140(3) 0.0188(7) Uani 1 1 d . . . C1 C 0.9788(3) 0.36121(7) 0.4248(3) 0.0164(6) Uani 1 1 d . . . N1 N 1.0117(2) 0.34548(5) 0.3278(2) 0.0155(5) Uani 1 1 d . . . O1 O 1.1631(2) 0.33315(5) 0.20046(18) 0.0186(5) Uani 1 1 d . . . P1 P 1.05313(8) 0.311642(17) 0.14007(7) 0.01639(17) Uani 1 1 d . . . Pd1 Pd 0.88044(2) 0.314605(5) 0.24843(2) 0.01403(7) Uani 1 1 d . . . C60 C 0.9384(3) 0.47796(8) 0.7617(3) 0.0292(8) Uani 1 1 d . . . H60 H 1.0079 0.4818 0.8109 0.035 Uiso 1 1 d R . . C59 C 0.9399(3) 0.48911(8) 0.6566(3) 0.0292(8) Uani 1 1 d . . . H59 H 1.0103 0.5004 0.6342 0.035 Uiso 1 1 d R . . C58 C 0.8393(3) 0.48375(8) 0.5847(3) 0.0288(8) Uani 1 1 d . . . H58 H 0.8407 0.4913 0.5126 0.035 Uiso 1 1 d R . . C57 C 0.7342(3) 0.46722(7) 0.6182(3) 0.0239(7) Uani 1 1 d . . . H57 H 0.6654 0.4637 0.5681 0.029 Uiso 1 1 d R . . C56 C 0.7297(3) 0.45578(7) 0.7230(3) 0.0210(7) Uani 1 1 d . . . C55 C 0.8359(3) 0.46104(7) 0.7962(3) 0.0205(7) Uani 1 1 d . . . C54 C 0.9581(3) 0.43865(9) 0.9553(3) 0.0325(9) Uani 1 1 d . . . H54A H 1.0035 0.4275 0.9004 0.049 Uiso 1 1 d R . . H54B H 0.9451 0.4272 1.0210 0.049 Uiso 1 1 d R . . H54C H 1.0096 0.4553 0.9743 0.049 Uiso 1 1 d R . . C53 C 0.7673(4) 0.46990(9) 0.9861(3) 0.0336(9) Uani 1 1 d . . . H53A H 0.8235 0.4865 0.9902 0.050 Uiso 1 1 d R . . H53B H 0.7593 0.4616 1.0592 0.050 Uiso 1 1 d R . . H53C H 0.6819 0.4755 0.9587 0.050 Uiso 1 1 d R . . C52 C 0.8256(3) 0.44801(8) 0.9080(3) 0.0234(7) Uani 1 1 d . . . C51 C 0.7333(3) 0.42274(7) 0.8948(3) 0.0214(7) Uani 1 1 d . . . H51A H 0.6953 0.4181 0.9665 0.026 Uiso 1 1 d R . . H51B H 0.7823 0.4061 0.8694 0.026 Uiso 1 1 d R . . C50 C 0.2732(3) 0.43695(8) 0.4686(3) 0.0275(8) Uani 1 1 d . . . H50A H 0.2775 0.4321 0.3906 0.041 Uiso 1 1 d R . . H50B H 0.2392 0.4561 0.4766 0.041 Uiso 1 1 d R . . H50C H 0.2164 0.4236 0.5056 0.041 Uiso 1 1 d R . . C49 C 0.4742(4) 0.40657(8) 0.4988(3) 0.0286(8) Uani 1 1 d . . . H49A H 0.4223 0.3916 0.5313 0.043 Uiso 1 1 d R . . H49B H 0.5607 0.4065 0.5320 0.043 Uiso 1 1 d R . . H49C H 0.4806 0.4034 0.4197 0.043 Uiso 1 1 d R . . C48 C 0.4093(3) 0.43540(7) 0.5202(3) 0.0210(7) Uani 1 1 d . . . H48 H 0.4630 0.4501 0.4839 0.025 Uiso 1 1 d R . . C47 C 0.3977(3) 0.49975(7) 0.6371(3) 0.0263(8) Uani 1 1 d . . . H47A H 0.3516 0.5173 0.6522 0.039 Uiso 1 1 d R . . H47B H 0.4029 0.4970 0.5578 0.039 Uiso 1 1 d R . . H47C H 0.4850 0.5008 0.6686 0.039 Uiso 1 1 d R . . C46 C 0.3067(3) 0.47969(8) 0.8118(3) 0.0274(8) Uani 1 1 d . . . H46A H 0.3909 0.4825 0.8475 0.041 Uiso 1 1 d R . . H46B H 0.2642 0.4632 0.8437 0.041 Uiso 1 1 d R . . H46C H 0.2532 0.4964 0.8228 0.041 Uiso 1 1 d R . . C45 C 0.3252(3) 0.47484(7) 0.6887(3) 0.0196(7) Uani 1 1 d . . . H45 H 0.2388 0.4730 0.6522 0.023 Uiso 1 1 d R . . C44 C 0.2223(3) 0.38267(7) 0.8229(3) 0.0240(7) Uani 1 1 d . . . H44A H 0.2173 0.3679 0.7670 0.036 Uiso 1 1 d R . . H44B H 0.1414 0.3933 0.8232 0.036 Uiso 1 1 d R . . H44C H 0.2367 0.3741 0.8950 0.036 Uiso 1 1 d R . . C43 C 0.3317(3) 0.40230(7) 0.7982(3) 0.0164(6) Uani 1 1 d . . . C42 C 0.6612(4) 0.33964(10) 0.7852(4) 0.0410(10) Uani 1 1 d . . . H42A H 0.7099 0.3573 0.7908 0.062 Uiso 1 1 d R . . H42B H 0.6683 0.3321 0.7109 0.062 Uiso 1 1 d R . . H42C H 0.6961 0.3260 0.8379 0.062 Uiso 1 1 d R . . C41 C 0.4390(4) 0.31817(8) 0.7971(4) 0.0369(9) Uani 1 1 d . . . H41A H 0.4722 0.3038 0.8476 0.055 Uiso 1 1 d R . . H41B H 0.4456 0.3113 0.7216 0.055 Uiso 1 1 d R . . H41C H 0.3485 0.3221 0.8135 0.055 Uiso 1 1 d R . . C40 C 0.5184(3) 0.34525(7) 0.8104(3) 0.0253(8) Uani 1 1 d . . . H40 H 0.4851 0.3593 0.7558 0.030 Uiso 1 1 d R . . C39 C 0.2732(4) 0.43111(9) 1.0733(4) 0.0382(10) Uani 1 1 d . . . H39A H 0.2320 0.4225 1.0088 0.057 Uiso 1 1 d R . . H39B H 0.2487 0.4510 1.0775 0.057 Uiso 1 1 d R . . H39C H 0.2449 0.4213 1.1395 0.057 Uiso 1 1 d R . . C38 C 0.4849(4) 0.44314(9) 1.1630(3) 0.0354(9) Uani 1 1 d . . . H38A H 0.4527 0.4347 1.2306 0.053 Uiso 1 1 d R . . H38B H 0.4646 0.4633 1.1620 0.053 Uiso 1 1 d R . . H38C H 0.5786 0.4406 1.1597 0.053 Uiso 1 1 d R . . C37 C 0.4202(3) 0.42862(8) 1.0636(3) 0.0255(8) Uani 1 1 d . . . H37 H 0.4462 0.4393 0.9968 0.031 Uiso 1 1 d R . . C36 C 0.5050(3) 0.35814(7) 0.9245(3) 0.0217(7) Uani 1 1 d . . . C35 C 0.5358(3) 0.34154(8) 1.0166(3) 0.0290(8) Uani 1 1 d . . . H35 H 0.5617 0.3225 1.0070 0.035 Uiso 1 1 d R . . C34 C 0.5293(3) 0.35265(8) 1.1216(3) 0.0298(8) Uani 1 1 d . . . H34 H 0.5490 0.3411 1.1832 0.036 Uiso 1 1 d R . . C33 C 0.4936(3) 0.38055(8) 1.1363(3) 0.0262(8) Uani 1 1 d . . . H33 H 0.4908 0.3880 1.2085 0.031 Uiso 1 1 d R . . C32 C 0.4612(3) 0.39816(8) 1.0479(3) 0.0217(7) Uani 1 1 d . . . C31 C 0.4668(3) 0.38618(7) 0.9418(3) 0.0179(7) Uani 1 1 d . . . N2 N 0.4401(2) 0.40437(5) 0.8489(2) 0.0165(5) Uani 1 1 d . . . O2 O 0.3044(2) 0.41839(5) 0.70892(19) 0.0188(5) Uani 1 1 d . . . P2 P 0.41666(7) 0.442168(16) 0.66832(7) 0.01541(17) Uani 1 1 d . . . Pd2 Pd 0.58681(2) 0.431922(5) 0.78237(2) 0.01457(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C30 0.0182(16) 0.0257(19) 0.046(2) 0.0025(17) 0.0066(16) -0.0022(13) C29 0.0215(17) 0.033(2) 0.046(2) 0.0062(18) 0.0153(17) 0.0045(15) C28 0.0282(18) 0.0251(18) 0.027(2) 0.0002(15) 0.0065(15) 0.0105(14) C27 0.0223(16) 0.0188(16) 0.0213(18) 0.0002(13) 0.0008(14) 0.0024(12) C26 0.0116(14) 0.0188(16) 0.0209(17) 0.0050(13) 0.0000(13) 0.0019(11) C25 0.0142(14) 0.0181(16) 0.0243(18) 0.0024(14) -0.0029(13) 0.0004(12) C24 0.0306(19) 0.031(2) 0.048(3) -0.0078(18) 0.0035(18) -0.0147(16) C23 0.038(2) 0.0192(17) 0.028(2) 0.0041(15) 0.0082(16) 0.0067(15) C22 0.0206(15) 0.0142(15) 0.0268(19) -0.0001(14) -0.0003(14) -0.0038(12) C21 0.0222(15) 0.0200(16) 0.0167(17) -0.0001(13) -0.0028(13) -0.0034(13) C20 0.041(2) 0.041(2) 0.0169(19) -0.0032(16) -0.0015(16) -0.0085(17) C19 0.035(2) 0.032(2) 0.027(2) 0.0089(16) 0.0064(16) -0.0003(16) C18 0.0260(17) 0.0288(19) 0.0166(17) 0.0024(14) 0.0046(14) -0.0032(14) C17 0.036(2) 0.028(2) 0.040(2) 0.0035(17) -0.0030(18) 0.0063(16) C16 0.0296(19) 0.034(2) 0.045(3) -0.0076(19) 0.0096(18) 0.0047(16) C15 0.0246(16) 0.0191(17) 0.0270(19) -0.0050(14) 0.0006(15) 0.0006(13) C14 0.0218(16) 0.0205(17) 0.0259(19) -0.0046(14) 0.0014(14) -0.0069(13) C13 0.0219(16) 0.0142(15) 0.0151(16) -0.0005(12) 0.0016(13) -0.0012(12) C12 0.039(2) 0.0226(18) 0.027(2) 0.0044(15) -0.0063(16) -0.0021(15) C11 0.0276(19) 0.036(2) 0.060(3) 0.018(2) 0.0109(19) 0.0084(16) C10 0.039(2) 0.0220(18) 0.0179(18) 0.0035(14) 0.0107(15) 0.0059(15) C9 0.043(2) 0.0219(19) 0.032(2) 0.0049(16) -0.0091(18) -0.0027(16) C8 0.0345(19) 0.0265(19) 0.029(2) 0.0052(16) -0.0077(16) -0.0019(15) C7 0.0250(16) 0.0188(17) 0.0233(19) 0.0003(14) -0.0037(14) -0.0007(13) C6 0.0200(15) 0.0189(16) 0.0177(17) -0.0007(13) 0.0021(13) -0.0009(12) C5 0.0287(17) 0.0279(19) 0.0163(18) -0.0009(14) 0.0028(14) 0.0008(14) C4 0.0313(18) 0.0270(19) 0.0222(19) -0.0097(15) 0.0051(15) 0.0007(14) C3 0.0271(17) 0.0161(16) 0.031(2) -0.0051(14) -0.0013(15) 0.0024(13) C2 0.0191(15) 0.0167(16) 0.0206(18) -0.0011(13) -0.0014(13) -0.0024(12) C1 0.0159(14) 0.0169(15) 0.0164(17) -0.0030(12) 0.0013(13) -0.0031(11) N1 0.0183(13) 0.0137(13) 0.0145(14) -0.0002(10) -0.0008(11) -0.0014(10) O1 0.0173(10) 0.0191(11) 0.0195(12) -0.0050(9) 0.0035(9) -0.0059(8) P1 0.0175(4) 0.0170(4) 0.0147(4) -0.0024(3) 0.0022(3) -0.0030(3) Pd1 0.01467(12) 0.01344(12) 0.01399(13) -0.00028(9) 0.00130(9) -0.00232(8) C60 0.0211(16) 0.0290(19) 0.038(2) 0.0007(16) 0.0037(16) -0.0043(14) C59 0.0215(17) 0.0241(18) 0.042(2) 0.0049(16) 0.0128(16) -0.0042(14) C58 0.0310(19) 0.0240(18) 0.032(2) 0.0087(16) 0.0118(16) 0.0037(14) C57 0.0243(16) 0.0199(17) 0.028(2) 0.0016(14) 0.0024(15) 0.0037(13) C56 0.0197(15) 0.0138(15) 0.0298(19) -0.0006(14) 0.0112(14) 0.0040(12) C55 0.0181(15) 0.0180(16) 0.0256(19) -0.0037(14) 0.0066(14) 0.0012(12) C54 0.0215(17) 0.045(2) 0.031(2) 0.0045(18) -0.0062(16) -0.0041(16) C53 0.038(2) 0.037(2) 0.026(2) -0.0093(17) 0.0037(17) -0.0055(17) C52 0.0191(16) 0.0273(18) 0.0238(19) -0.0013(15) 0.0012(14) -0.0012(13) C51 0.0185(15) 0.0267(18) 0.0191(18) -0.0012(14) 0.0010(13) -0.0011(13) C50 0.037(2) 0.0230(18) 0.0217(19) -0.0038(15) -0.0093(16) 0.0040(15) C49 0.0316(18) 0.030(2) 0.024(2) -0.0075(15) 0.0006(16) 0.0059(15) C48 0.0281(17) 0.0186(16) 0.0162(17) -0.0017(13) 0.0012(14) -0.0001(13) C47 0.0358(19) 0.0140(16) 0.029(2) 0.0022(14) 0.0012(16) 0.0023(14) C46 0.0323(18) 0.0258(18) 0.024(2) -0.0039(15) 0.0078(15) 0.0034(15) C45 0.0207(15) 0.0163(16) 0.0216(18) -0.0011(13) -0.0010(13) 0.0006(12) C44 0.0192(15) 0.0253(18) 0.027(2) 0.0056(15) 0.0003(14) -0.0038(13) C43 0.0163(14) 0.0153(15) 0.0179(17) 0.0013(13) 0.0036(13) 0.0031(12) C42 0.033(2) 0.050(3) 0.041(3) -0.008(2) 0.0075(18) 0.0067(18) C41 0.046(2) 0.027(2) 0.038(2) -0.0027(17) -0.0022(19) -0.0006(17) C40 0.0307(18) 0.0220(18) 0.0232(19) 0.0005(14) 0.0010(15) 0.0071(14) C39 0.032(2) 0.042(2) 0.040(3) -0.0048(19) 0.0006(18) 0.0082(17) C38 0.040(2) 0.040(2) 0.026(2) -0.0073(18) 0.0012(17) -0.0013(17) C37 0.0297(18) 0.0292(19) 0.0178(18) -0.0008(15) 0.0040(15) -0.0027(14) C36 0.0188(15) 0.0241(17) 0.0221(19) 0.0038(14) -0.0001(14) -0.0005(13) C35 0.0273(18) 0.0263(19) 0.033(2) 0.0092(16) -0.0034(16) 0.0020(14) C34 0.0284(18) 0.035(2) 0.026(2) 0.0154(16) -0.0038(16) -0.0019(15) C33 0.0231(16) 0.038(2) 0.0174(18) 0.0039(15) 0.0000(14) -0.0083(15) C32 0.0161(15) 0.0303(19) 0.0187(18) 0.0028(14) 0.0031(13) -0.0039(13) C31 0.0135(14) 0.0252(17) 0.0150(17) 0.0039(13) 0.0012(12) -0.0017(12) N2 0.0166(12) 0.0162(13) 0.0166(14) 0.0008(11) 0.0034(11) -0.0010(10) O2 0.0183(10) 0.0172(11) 0.0207(12) 0.0034(9) -0.0021(9) -0.0021(9) P2 0.0180(4) 0.0130(4) 0.0152(4) 0.0004(3) 0.0001(3) -0.0001(3) Pd2 0.01321(11) 0.01553(12) 0.01496(13) -0.00053(9) 0.00075(9) -0.00031(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 C30 C29 1.386(5) . ? C30 C25 1.404(5) . ? C30 H30 0.9500 . ? C29 C28 1.400(5) . ? C29 H29 0.9500 . ? C28 C27 1.400(5) . ? C28 H28 0.9500 . ? C27 C26 1.409(5) . ? C27 H27 0.9500 . ? C26 C25 1.416(4) . ? C26 Pd1 2.076(3) . ? C25 C22 1.524(5) . ? C24 C22 1.543(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23 C22 1.542(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 C21 1.538(4) . ? C21 Pd1 2.049(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20 C18 1.543(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 C18 1.537(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 P1 1.832(4) . ? C18 H18 1.0000 . ? C17 C15 1.529(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C16 C15 1.536(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 P1 1.841(3) . ? C15 H15 1.0000 . ? C14 C13 1.499(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 N1 1.283(4) . ? C13 O1 1.359(4) . ? C12 C10 1.528(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C11 C10 1.539(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C10 C6 1.527(5) . ? C10 H10 1.0000 . ? C9 C7 1.533(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 C7 1.540(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 C2 1.532(5) . ? C7 H7 1.0000 . ? C6 C1 1.403(5) . ? C6 C5 1.407(5) . ? C5 C4 1.389(5) . ? C5 H5 0.9500 . ? C4 C3 1.394(5) . ? C4 H4 0.9500 . ? C3 C2 1.398(5) . ? C3 H3 0.9500 . ? C2 C1 1.415(4) . ? C1 N1 1.445(4) . ? N1 Pd1 2.215(3) . ? O1 P1 1.693(2) . ? P1 Pd1 2.2453(8) . ? C60 C59 1.388(5) . ? C60 C55 1.401(5) . ? C60 H60 0.9500 . ? C59 C58 1.379(6) . ? C59 H59 0.9500 . ? C58 C57 1.408(5) . ? C58 H58 0.9500 . ? C57 C56 1.391(5) . ? C57 H57 0.9500 . ? C56 C55 1.431(5) . ? C56 Pd2 2.008(3) . ? C55 C52 1.504(5) . ? C54 C52 1.549(5) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C53 C52 1.539(5) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C52 C51 1.541(5) . ? C51 Pd2 2.081(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C50 C48 1.540(5) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C49 C48 1.548(5) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C48 P2 1.838(3) . ? C48 H48 1.0000 . ? C47 C45 1.540(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C46 C45 1.536(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C45 P2 1.836(3) . ? C45 H45 1.0000 . ? C44 C43 1.502(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C43 N2 1.280(4) . ? C43 O2 1.358(4) . ? C42 C40 1.540(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C41 C40 1.534(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C40 C36 1.529(5) . ? C40 H40 1.0000 . ? C39 C37 1.536(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C38 C37 1.542(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C37 C32 1.520(5) . ? C37 H37 1.0000 . ? C36 C31 1.405(5) . ? C36 C35 1.407(5) . ? C35 C34 1.388(6) . ? C35 H35 0.9500 . ? C34 C33 1.387(6) . ? C34 H34 0.9500 . ? C33 C32 1.402(5) . ? C33 H33 0.9500 . ? C32 C31 1.416(5) . ? C31 N2 1.449(4) . ? N2 Pd2 2.173(2) . ? O2 P2 1.700(2) . ? P2 Pd2 2.2867(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C29 C30 C25 120.2(3) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C30 C29 C28 119.9(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.0 . . ? C27 C28 C29 119.9(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C27 C26 121.5(3) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.3 . . ? C27 C26 C25 117.3(3) . . ? C27 C26 Pd1 128.8(2) . . ? C25 C26 Pd1 113.9(2) . . ? C30 C25 C26 121.2(3) . . ? C30 C25 C22 122.9(3) . . ? C26 C25 C22 115.8(3) . . ? C22 C24 H24A 109.3 . . ? C22 C24 H24B 109.4 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.6 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C23 H23A 109.6 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.4 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C22 C21 105.5(3) . . ? C25 C22 C23 108.0(3) . . ? C21 C22 C23 110.6(3) . . ? C25 C22 C24 114.2(3) . . ? C21 C22 C24 109.2(3) . . ? C23 C22 C24 109.2(3) . . ? C22 C21 Pd1 110.9(2) . . ? C22 C21 H21A 109.6 . . ? Pd1 C21 H21A 109.5 . . ? C22 C21 H21B 109.3 . . ? Pd1 C21 H21B 109.4 . . ? H21A C21 H21B 108.1 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C19 H19A 109.6 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C18 C20 111.2(3) . . ? C19 C18 P1 109.5(2) . . ? C20 C18 P1 108.8(2) . . ? C19 C18 H18 109.1 . . ? C20 C18 H18 109.1 . . ? P1 C18 H18 109.1 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.4 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 C15 C16 112.1(3) . . ? C17 C15 P1 109.2(2) . . ? C16 C15 P1 114.8(3) . . ? C17 C15 H15 106.8 . . ? C16 C15 H15 106.7 . . ? P1 C15 H15 106.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C13 O1 121.0(3) . . ? N1 C13 C14 127.7(3) . . ? O1 C13 C14 111.3(3) . . ? C10 C12 H12A 109.3 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.6 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.6 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.3 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C10 C12 112.4(3) . . ? C6 C10 C11 110.5(3) . . ? C12 C10 C11 110.3(3) . . ? C6 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.4 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.6 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C8 H8A 109.6 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C7 C9 113.8(3) . . ? C2 C7 C8 109.4(3) . . ? C9 C7 C8 110.7(3) . . ? C2 C7 H7 107.5 . . ? C9 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C1 C6 C5 117.2(3) . . ? C1 C6 C10 122.4(3) . . ? C5 C6 C10 120.3(3) . . ? C4 C5 C6 121.3(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.2 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 119.9 . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C7 120.9(3) . . ? C1 C2 C7 121.4(3) . . ? C6 C1 C2 122.7(3) . . ? C6 C1 N1 118.1(3) . . ? C2 C1 N1 119.1(3) . . ? C13 N1 C1 118.5(3) . . ? C13 N1 Pd1 117.8(2) . . ? C1 N1 Pd1 123.33(19) . . ? C13 O1 P1 117.72(19) . . ? O1 P1 C18 100.00(14) . . ? O1 P1 C15 100.36(14) . . ? C18 P1 C15 106.67(16) . . ? O1 P1 Pd1 104.12(8) . . ? C18 P1 Pd1 119.80(11) . . ? C15 P1 Pd1 121.52(11) . . ? C21 Pd1 C26 79.59(13) . . ? C21 Pd1 N1 174.21(11) . . ? C26 Pd1 N1 105.28(11) . . ? C21 Pd1 P1 96.14(9) . . ? C26 Pd1 P1 175.69(9) . . ? N1 Pd1 P1 78.95(7) . . ? C59 C60 C55 120.9(3) . . ? C59 C60 H60 119.6 . . ? C55 C60 H60 119.5 . . ? C58 C59 C60 120.1(3) . . ? C58 C59 H59 119.9 . . ? C60 C59 H59 120.0 . . ? C59 C58 C57 120.0(3) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C56 C57 C58 121.4(3) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C57 C56 C55 118.1(3) . . ? C57 C56 Pd2 125.9(3) . . ? C55 C56 Pd2 116.0(2) . . ? C60 C55 C56 119.6(3) . . ? C60 C55 C52 124.8(3) . . ? C56 C55 C52 115.6(3) . . ? C52 C54 H54A 109.4 . . ? C52 C54 H54B 109.4 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.6 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C53 H53A 109.6 . . ? C52 C53 H53B 109.3 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C52 C53 108.6(3) . . ? C55 C52 C51 106.0(3) . . ? C53 C52 C51 109.9(3) . . ? C55 C52 C54 112.5(3) . . ? C53 C52 C54 108.5(3) . . ? C51 C52 C54 111.3(3) . . ? C52 C51 Pd2 110.7(2) . . ? C52 C51 H51A 109.6 . . ? Pd2 C51 H51A 109.6 . . ? C52 C51 H51B 109.4 . . ? Pd2 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C49 H49A 109.4 . . ? C48 C49 H49B 109.4 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.6 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C50 C48 C49 111.8(3) . . ? C50 C48 P2 114.9(2) . . ? C49 C48 P2 107.9(2) . . ? C50 C48 H48 107.3 . . ? C49 C48 H48 107.2 . . ? P2 C48 H48 107.3 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.4 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.4 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.4 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C46 C45 C47 110.7(3) . . ? C46 C45 P2 109.3(2) . . ? C47 C45 P2 109.7(2) . . ? C46 C45 H45 109.1 . . ? C47 C45 H45 109.0 . . ? P2 C45 H45 109.1 . . ? C43 C44 H44A 109.7 . . ? C43 C44 H44B 109.3 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.4 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N2 C43 O2 121.2(3) . . ? N2 C43 C44 127.7(3) . . ? O2 C43 C44 111.1(3) . . ? C40 C42 H42A 109.6 . . ? C40 C42 H42B 109.4 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.4 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.6 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C40 C41 112.1(3) . . ? C36 C40 C42 110.5(3) . . ? C41 C40 C42 110.5(3) . . ? C36 C40 H40 107.8 . . ? C41 C40 H40 107.9 . . ? C42 C40 H40 107.9 . . ? C37 C39 H39A 109.2 . . ? C37 C39 H39B 109.6 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.6 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C38 H38A 109.3 . . ? C37 C38 H38B 109.6 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.6 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C32 C37 C39 111.3(3) . . ? C32 C37 C38 113.9(3) . . ? C39 C37 C38 109.2(3) . . ? C32 C37 H37 107.4 . . ? C39 C37 H37 107.6 . . ? C38 C37 H37 107.3 . . ? C31 C36 C35 118.1(3) . . ? C31 C36 C40 123.0(3) . . ? C35 C36 C40 118.8(3) . . ? C34 C35 C36 120.8(3) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.7 . . ? C33 C34 C35 119.9(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.0 . . ? C34 C33 C32 122.0(3) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 118.8 . . ? C33 C32 C31 116.9(3) . . ? C33 C32 C37 122.3(3) . . ? C31 C32 C37 120.8(3) . . ? C36 C31 C32 122.2(3) . . ? C36 C31 N2 119.8(3) . . ? C32 C31 N2 117.8(3) . . ? C43 N2 C31 119.4(3) . . ? C43 N2 Pd2 118.7(2) . . ? C31 N2 Pd2 121.54(19) . . ? C43 O2 P2 118.09(19) . . ? O2 P2 C45 99.44(13) . . ? O2 P2 C48 98.69(14) . . ? C45 P2 C48 105.41(15) . . ? O2 P2 Pd2 101.98(8) . . ? C45 P2 Pd2 119.56(11) . . ? C48 P2 Pd2 125.75(11) . . ? C56 Pd2 C51 79.62(14) . . ? C56 Pd2 N2 176.87(12) . . ? C51 Pd2 N2 97.86(12) . . ? C56 Pd2 P2 103.18(10) . . ? C51 Pd2 P2 176.21(9) . . ? N2 Pd2 P2 79.42(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 C30 C29 C28 0.8(6) . . . . ? C30 C29 C28 C27 -0.5(6) . . . . ? C29 C28 C27 C26 -0.8(5) . . . . ? C28 C27 C26 C25 1.7(5) . . . . ? C28 C27 C26 Pd1 -178.6(3) . . . . ? C29 C30 C25 C26 0.1(6) . . . . ? C29 C30 C25 C22 176.4(3) . . . . ? C27 C26 C25 C30 -1.3(5) . . . . ? Pd1 C26 C25 C30 178.9(3) . . . . ? C27 C26 C25 C22 -177.9(3) . . . . ? Pd1 C26 C25 C22 2.4(4) . . . . ? C30 C25 C22 C21 156.3(3) . . . . ? C26 C25 C22 C21 -27.3(4) . . . . ? C30 C25 C22 C23 -85.4(4) . . . . ? C26 C25 C22 C23 91.0(3) . . . . ? C30 C25 C22 C24 36.3(5) . . . . ? C26 C25 C22 C24 -147.3(3) . . . . ? C25 C22 C21 Pd1 40.3(3) . . . . ? C23 C22 C21 Pd1 -76.2(3) . . . . ? C24 C22 C21 Pd1 163.5(2) . . . . ? C12 C10 C6 C1 -121.1(3) . . . . ? C11 C10 C6 C1 115.2(4) . . . . ? C12 C10 C6 C5 58.3(4) . . . . ? C11 C10 C6 C5 -65.3(4) . . . . ? C1 C6 C5 C4 -0.5(5) . . . . ? C10 C6 C5 C4 -179.9(3) . . . . ? C6 C5 C4 C3 0.3(5) . . . . ? C5 C4 C3 C2 0.1(5) . . . . ? C4 C3 C2 C1 -0.2(5) . . . . ? C4 C3 C2 C7 176.7(3) . . . . ? C9 C7 C2 C3 27.7(4) . . . . ? C8 C7 C2 C3 -96.7(4) . . . . ? C9 C7 C2 C1 -155.5(3) . . . . ? C8 C7 C2 C1 80.1(4) . . . . ? C5 C6 C1 C2 0.3(5) . . . . ? C10 C6 C1 C2 179.8(3) . . . . ? C5 C6 C1 N1 -176.6(3) . . . . ? C10 C6 C1 N1 2.8(4) . . . . ? C3 C2 C1 C6 0.0(5) . . . . ? C7 C2 C1 C6 -176.9(3) . . . . ? C3 C2 C1 N1 177.0(3) . . . . ? C7 C2 C1 N1 0.1(4) . . . . ? O1 C13 N1 C1 -179.5(3) . . . . ? C14 C13 N1 C1 1.1(5) . . . . ? O1 C13 N1 Pd1 7.3(4) . . . . ? C14 C13 N1 Pd1 -172.1(3) . . . . ? C6 C1 N1 C13 -97.3(4) . . . . ? C2 C1 N1 C13 85.6(4) . . . . ? C6 C1 N1 Pd1 75.5(3) . . . . ? C2 C1 N1 Pd1 -101.6(3) . . . . ? N1 C13 O1 P1 -3.4(4) . . . . ? C14 C13 O1 P1 176.1(2) . . . . ? C13 O1 P1 C18 122.5(2) . . . . ? C13 O1 P1 C15 -128.3(2) . . . . ? C13 O1 P1 Pd1 -1.9(2) . . . . ? C19 C18 P1 O1 -72.0(3) . . . . ? C20 C18 P1 O1 166.3(2) . . . . ? C19 C18 P1 C15 -176.1(2) . . . . ? C20 C18 P1 C15 62.2(3) . . . . ? C19 C18 P1 Pd1 40.8(3) . . . . ? C20 C18 P1 Pd1 -81.0(3) . . . . ? C17 C15 P1 O1 66.4(3) . . . . ? C16 C15 P1 O1 -60.5(3) . . . . ? C17 C15 P1 C18 170.3(2) . . . . ? C16 C15 P1 C18 43.4(3) . . . . ? C17 C15 P1 Pd1 -47.3(3) . . . . ? C16 C15 P1 Pd1 -174.2(2) . . . . ? C22 C21 Pd1 C26 -32.1(2) . . . . ? C22 C21 Pd1 P1 147.3(2) . . . . ? C27 C26 Pd1 C21 -162.9(3) . . . . ? C25 C26 Pd1 C21 16.8(2) . . . . ? C27 C26 Pd1 N1 20.3(3) . . . . ? C25 C26 Pd1 N1 -160.0(2) . . . . ? C13 N1 Pd1 C26 172.8(2) . . . . ? C1 N1 Pd1 C26 -0.1(3) . . . . ? C13 N1 Pd1 P1 -6.4(2) . . . . ? C1 N1 Pd1 P1 -179.2(2) . . . . ? O1 P1 Pd1 C21 -173.17(13) . . . . ? C18 P1 Pd1 C21 76.31(16) . . . . ? C15 P1 Pd1 C21 -61.34(17) . . . . ? O1 P1 Pd1 N1 3.73(11) . . . . ? C18 P1 Pd1 N1 -106.79(15) . . . . ? C15 P1 Pd1 N1 115.55(15) . . . . ? C55 C60 C59 C58 0.4(5) . . . . ? C60 C59 C58 C57 0.7(5) . . . . ? C59 C58 C57 C56 -0.6(5) . . . . ? C58 C57 C56 C55 -0.6(5) . . . . ? C58 C57 C56 Pd2 179.9(3) . . . . ? C59 C60 C55 C56 -1.6(5) . . . . ? C59 C60 C55 C52 179.9(3) . . . . ? C57 C56 C55 C60 1.7(5) . . . . ? Pd2 C56 C55 C60 -178.8(2) . . . . ? C57 C56 C55 C52 -179.7(3) . . . . ? Pd2 C56 C55 C52 -0.2(4) . . . . ? C60 C55 C52 C53 84.4(4) . . . . ? C56 C55 C52 C53 -94.1(3) . . . . ? C60 C55 C52 C51 -157.6(3) . . . . ? C56 C55 C52 C51 24.0(4) . . . . ? C60 C55 C52 C54 -35.7(5) . . . . ? C56 C55 C52 C54 145.8(3) . . . . ? C55 C52 C51 Pd2 -36.5(3) . . . . ? C53 C52 C51 Pd2 80.7(3) . . . . ? C54 C52 C51 Pd2 -159.1(2) . . . . ? C41 C40 C36 C31 -125.5(3) . . . . ? C42 C40 C36 C31 110.7(4) . . . . ? C41 C40 C36 C35 56.3(4) . . . . ? C42 C40 C36 C35 -67.4(4) . . . . ? C31 C36 C35 C34 -0.3(5) . . . . ? C40 C36 C35 C34 177.9(3) . . . . ? C36 C35 C34 C33 -0.9(5) . . . . ? C35 C34 C33 C32 1.1(5) . . . . ? C34 C33 C32 C31 -0.1(5) . . . . ? C34 C33 C32 C37 179.1(3) . . . . ? C39 C37 C32 C33 -91.5(4) . . . . ? C38 C37 C32 C33 32.3(4) . . . . ? C39 C37 C32 C31 87.7(4) . . . . ? C38 C37 C32 C31 -148.4(3) . . . . ? C35 C36 C31 C32 1.4(5) . . . . ? C40 C36 C31 C32 -176.8(3) . . . . ? C35 C36 C31 N2 177.1(3) . . . . ? C40 C36 C31 N2 -1.0(5) . . . . ? C33 C32 C31 C36 -1.1(4) . . . . ? C37 C32 C31 C36 179.6(3) . . . . ? C33 C32 C31 N2 -177.0(3) . . . . ? C37 C32 C31 N2 3.8(4) . . . . ? O2 C43 N2 C31 -178.1(3) . . . . ? C44 C43 N2 C31 0.2(5) . . . . ? O2 C43 N2 Pd2 -4.6(4) . . . . ? C44 C43 N2 Pd2 173.6(3) . . . . ? C36 C31 N2 C43 79.2(4) . . . . ? C32 C31 N2 C43 -104.9(3) . . . . ? C36 C31 N2 Pd2 -94.1(3) . . . . ? C32 C31 N2 Pd2 81.9(3) . . . . ? N2 C43 O2 P2 -1.8(4) . . . . ? C44 C43 O2 P2 179.6(2) . . . . ? C43 O2 P2 C45 -116.7(2) . . . . ? C43 O2 P2 C48 135.9(2) . . . . ? C43 O2 P2 Pd2 6.4(2) . . . . ? C46 C45 P2 O2 68.9(2) . . . . ? C47 C45 P2 O2 -169.6(2) . . . . ? C46 C45 P2 C48 170.7(2) . . . . ? C47 C45 P2 C48 -67.8(3) . . . . ? C46 C45 P2 Pd2 -40.7(3) . . . . ? C47 C45 P2 Pd2 80.8(2) . . . . ? C50 C48 P2 O2 53.0(3) . . . . ? C49 C48 P2 O2 -72.5(2) . . . . ? C50 C48 P2 C45 -49.4(3) . . . . ? C49 C48 P2 C45 -174.9(2) . . . . ? C50 C48 P2 Pd2 164.6(2) . . . . ? C49 C48 P2 Pd2 39.1(3) . . . . ? C57 C56 Pd2 C51 162.6(3) . . . . ? C55 C56 Pd2 C51 -16.8(2) . . . . ? C57 C56 Pd2 P2 -20.0(3) . . . . ? C55 C56 Pd2 P2 160.6(2) . . . . ? C52 C51 Pd2 C56 29.9(2) . . . . ? C52 C51 Pd2 N2 -152.0(2) . . . . ? C43 N2 Pd2 C51 -176.0(2) . . . . ? C31 N2 Pd2 C51 -2.7(2) . . . . ? C43 N2 Pd2 P2 6.6(2) . . . . ? C31 N2 Pd2 P2 179.9(2) . . . . ? O2 P2 Pd2 C56 172.27(12) . . . . ? C45 P2 Pd2 C56 -79.48(15) . . . . ? C48 P2 Pd2 C56 62.21(17) . . . . ? O2 P2 Pd2 N2 -5.94(11) . . . . ? C45 P2 Pd2 N2 102.30(14) . . . . ? C48 P2 Pd2 N2 -116.00(15) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.590 _refine_diff_density_min -1.598 _refine_diff_density_rms 0.157 data_4 _database_code_depnum_ccdc_archive 'CCDC 876280' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H46 N O P Pd' _chemical_formula_sum 'C30 H46 N O P Pd' _chemical_formula_weight 574.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6645(5) _cell_length_b 12.6885(4) _cell_length_c 14.5290(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.6740(10) _cell_angle_gamma 90.00 _cell_volume 2884.63(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7848 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.82 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8183 _exptl_absorpt_correction_T_max 0.9122 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28673 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 28.68 _reflns_number_total 7280 _reflns_number_gt 6073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were found in subsequent difference Fourier maps and included as isotropic atoms. These atoms were refined riding on their respective carbon atoms. The highest residuals were found in close proximity to the metal atoms and have no chemical sense. ; _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^)+(0.0303P)^2^+1.2710P] 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 7280 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0245 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0562 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.236689(6) 0.998412(7) 0.148899(6) 0.01322(4) Uani 1 1 d . . . P1 P 0.295047(19) 0.95563(3) 0.29177(2) 0.01357(7) Uani 1 1 d . . . O1 O 0.13559(6) 1.05146(8) 0.23668(6) 0.01872(19) Uani 1 1 d . . . N1 N 0.20624(7) 0.97590(9) 0.36139(7) 0.0142(2) Uani 1 1 d . . . C1 C 0.18442(8) 1.05461(10) 0.02866(9) 0.0154(2) Uani 1 1 d . . . C2 C 0.09839(8) 1.08022(10) 0.01171(9) 0.0187(3) Uani 1 1 d . . . H2 H 0.0591 1.0705 0.0589 0.022 Uiso 1 1 d R . . C3 C 0.06945(9) 1.11990(11) -0.07352(10) 0.0228(3) Uani 1 1 d . . . H3 H 0.0107 1.1367 -0.0841 0.027 Uiso 1 1 d R . . C4 C 0.12614(9) 1.13493(11) -0.14308(10) 0.0220(3) Uani 1 1 d . . . H4 H 0.1064 1.1626 -0.2010 0.026 Uiso 1 1 d R . . C5 C 0.21215(8) 1.10928(10) -0.12758(9) 0.0186(3) Uani 1 1 d . . . H5 H 0.2510 1.1191 -0.1751 0.022 Uiso 1 1 d R . . C6 C 0.24102(8) 1.06944(10) -0.04268(9) 0.0155(2) Uani 1 1 d . . . C7 C 0.33274(8) 1.03931(11) -0.01739(9) 0.0166(2) Uani 1 1 d . . . C8 C 0.32729(8) 0.95561(10) 0.05936(9) 0.0166(2) Uani 1 1 d . . . H8A H 0.3835 0.9489 0.0930 0.020 Uiso 1 1 d R . . H8B H 0.3124 0.8864 0.0317 0.020 Uiso 1 1 d R . . C9 C 0.38003(10) 0.99644(11) -0.09979(10) 0.0231(3) Uani 1 1 d . . . H9A H 0.3472 0.9382 -0.1282 0.035 Uiso 1 1 d R . . H9B H 0.4366 0.9710 -0.0785 0.035 Uiso 1 1 d R . . H9C H 0.3864 1.0527 -0.1451 0.035 Uiso 1 1 d R . . C10 C 0.38047(8) 1.13676(11) 0.02085(10) 0.0213(3) Uani 1 1 d . . . H10A H 0.3799 1.1919 -0.0264 0.032 Uiso 1 1 d R . . H10B H 0.4397 1.1177 0.0381 0.032 Uiso 1 1 d R . . H10C H 0.3523 1.1628 0.0752 0.032 Uiso 1 1 d R . . C11 C 0.06691(8) 1.06592(11) 0.37743(10) 0.0213(3) Uani 1 1 d . . . H11A H 0.0777 1.1389 0.3967 0.032 Uiso 1 1 d R . . H11B H 0.0640 1.0209 0.4320 0.032 Uiso 1 1 d R . . H11C H 0.0126 1.0621 0.3413 0.032 Uiso 1 1 d R . . C12 C 0.13814(8) 1.02883(10) 0.31954(9) 0.0159(2) Uani 1 1 d . . . C13 C 0.19597(8) 0.92028(10) 0.44801(9) 0.0148(2) Uani 1 1 d . . . C14 C 0.22394(8) 0.96572(11) 0.53223(9) 0.0176(2) Uani 1 1 d . . . C15 C 0.21637(9) 0.90562(11) 0.61213(10) 0.0229(3) Uani 1 1 d . . . H15 H 0.2337 0.9350 0.6702 0.027 Uiso 1 1 d R . . C16 C 0.18416(10) 0.80426(12) 0.60819(10) 0.0245(3) Uani 1 1 d . . . H16 H 0.1820 0.7637 0.6630 0.029 Uiso 1 1 d R . . C17 C 0.15507(9) 0.76166(11) 0.52489(9) 0.0205(3) Uani 1 1 d . . . H17 H 0.1321 0.6924 0.5233 0.025 Uiso 1 1 d R . . C18 C 0.15894(8) 0.81877(10) 0.44323(9) 0.0159(2) Uani 1 1 d . . . C19 C 0.25955(8) 1.07677(10) 0.54179(9) 0.0183(3) Uani 1 1 d . . . H19 H 0.2662 1.1058 0.4786 0.022 Uiso 1 1 d R . . C20 C 0.19784(9) 1.14854(12) 0.59187(10) 0.0253(3) Uani 1 1 d . . . H20A H 0.1419 1.1484 0.5586 0.038 Uiso 1 1 d R . . H20B H 0.2206 1.2205 0.5942 0.038 Uiso 1 1 d R . . H20C H 0.1916 1.1225 0.6547 0.038 Uiso 1 1 d R . . C21 C 0.34774(9) 1.07704(12) 0.59277(10) 0.0248(3) Uani 1 1 d . . . H21A H 0.3418 1.0551 0.6568 0.037 Uiso 1 1 d R . . H21B H 0.3719 1.1482 0.5915 0.037 Uiso 1 1 d R . . H21C H 0.3857 1.0280 0.5625 0.037 Uiso 1 1 d R . . C22 C 0.11995(8) 0.77145(10) 0.35475(9) 0.0178(3) Uani 1 1 d . . . H22 H 0.1437 0.8098 0.3015 0.021 Uiso 1 1 d R . . C23 C 0.02257(9) 0.78633(12) 0.35042(12) 0.0283(3) Uani 1 1 d . . . H23A H -0.0013 0.7558 0.4056 0.042 Uiso 1 1 d R . . H23B H -0.0023 0.7510 0.2955 0.042 Uiso 1 1 d R . . H23C H 0.0091 0.8617 0.3474 0.042 Uiso 1 1 d R . . C24 C 0.13990(9) 0.65375(11) 0.34448(10) 0.0218(3) Uani 1 1 d . . . H24A H 0.2019 0.6431 0.3490 0.033 Uiso 1 1 d R . . H24B H 0.1171 0.6288 0.2844 0.033 Uiso 1 1 d R . . H24C H 0.1134 0.6141 0.3935 0.033 Uiso 1 1 d R . . C25 C 0.37212(8) 1.05639(10) 0.33412(9) 0.0173(2) Uani 1 1 d . . . H25 H 0.3818 1.0491 0.4023 0.021 Uiso 1 1 d R . . C26 C 0.33598(9) 1.16613(11) 0.31157(10) 0.0219(3) Uani 1 1 d . . . H26A H 0.3771 1.2199 0.3331 0.033 Uiso 1 1 d R . . H26B H 0.2822 1.1758 0.3424 0.033 Uiso 1 1 d R . . H26C H 0.3255 1.1728 0.2448 0.033 Uiso 1 1 d R . . C27 C 0.45703(9) 1.04194(12) 0.28731(10) 0.0241(3) Uani 1 1 d . . . H27A H 0.4472 1.0466 0.2203 0.036 Uiso 1 1 d R . . H27B H 0.4811 0.9727 0.3035 0.036 Uiso 1 1 d R . . H27C H 0.4971 1.0972 0.3082 0.036 Uiso 1 1 d R . . C28 C 0.33919(8) 0.82694(10) 0.33076(9) 0.0178(3) Uani 1 1 d . . . H28 H 0.2888 0.7802 0.3396 0.021 Uiso 1 1 d R . . C29 C 0.38834(9) 0.77728(11) 0.25211(10) 0.0245(3) Uani 1 1 d . . . H29A H 0.4406 0.8177 0.2431 0.037 Uiso 1 1 d R . . H29B H 0.3523 0.7782 0.1952 0.037 Uiso 1 1 d R . . H29C H 0.4034 0.7044 0.2681 0.037 Uiso 1 1 d R . . C30 C 0.39226(9) 0.82483(12) 0.42204(10) 0.0237(3) Uani 1 1 d . . . H30A H 0.4095 0.7522 0.4364 0.036 Uiso 1 1 d R . . H30B H 0.3579 0.8522 0.4714 0.036 Uiso 1 1 d R . . H30C H 0.4433 0.8687 0.4168 0.036 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01475(6) 0.01376(6) 0.01124(6) 0.00098(3) 0.00146(4) 0.00127(3) P1 0.01371(14) 0.01395(15) 0.01322(15) 0.00162(12) 0.00239(11) 0.00128(11) O1 0.0194(4) 0.0221(5) 0.0146(5) 0.0038(4) 0.0012(3) 0.0051(4) N1 0.0147(5) 0.0157(5) 0.0126(5) 0.0019(4) 0.0029(4) 0.0019(4) C1 0.0185(6) 0.0137(6) 0.0139(6) -0.0016(5) 0.0001(5) 0.0003(4) C2 0.0184(6) 0.0196(6) 0.0183(7) -0.0014(5) 0.0031(5) 0.0013(5) C3 0.0181(6) 0.0258(7) 0.0242(7) -0.0005(6) -0.0022(5) 0.0051(5) C4 0.0249(7) 0.0243(7) 0.0162(7) 0.0024(5) -0.0043(5) 0.0042(5) C5 0.0220(6) 0.0188(6) 0.0150(6) 0.0008(5) 0.0017(5) 0.0004(5) C6 0.0173(6) 0.0132(6) 0.0159(6) -0.0017(5) 0.0004(5) 0.0001(4) C7 0.0165(6) 0.0188(6) 0.0146(6) 0.0016(5) 0.0024(5) 0.0019(5) C8 0.0179(6) 0.0175(6) 0.0147(6) 0.0015(5) 0.0028(5) 0.0032(5) C9 0.0216(7) 0.0314(8) 0.0168(7) 0.0023(5) 0.0057(5) 0.0062(5) C10 0.0197(6) 0.0221(7) 0.0219(7) 0.0052(5) -0.0019(5) -0.0021(5) C11 0.0191(6) 0.0254(7) 0.0199(7) 0.0040(5) 0.0052(5) 0.0070(5) C12 0.0162(6) 0.0149(6) 0.0168(6) 0.0008(5) 0.0015(5) 0.0011(5) C13 0.0149(5) 0.0172(6) 0.0126(6) 0.0031(5) 0.0025(4) 0.0032(4) C14 0.0184(6) 0.0185(6) 0.0159(6) 0.0009(5) 0.0022(5) 0.0025(5) C15 0.0305(7) 0.0250(7) 0.0132(6) 0.0009(5) 0.0009(5) 0.0006(6) C16 0.0341(7) 0.0246(7) 0.0151(7) 0.0069(5) 0.0031(6) 0.0005(6) C17 0.0238(6) 0.0182(6) 0.0200(7) 0.0040(5) 0.0046(5) -0.0005(5) C18 0.0140(5) 0.0184(6) 0.0156(6) 0.0020(5) 0.0034(5) 0.0019(5) C19 0.0208(6) 0.0199(6) 0.0144(6) 0.0002(5) 0.0009(5) 0.0004(5) C20 0.0286(7) 0.0237(7) 0.0239(7) -0.0039(6) 0.0025(6) 0.0030(6) C21 0.0249(7) 0.0253(7) 0.0238(7) -0.0016(6) -0.0034(6) -0.0004(5) C22 0.0189(6) 0.0179(6) 0.0165(6) 0.0022(5) 0.0003(5) -0.0014(5) C23 0.0209(7) 0.0256(7) 0.0376(9) 0.0013(6) -0.0070(6) 0.0003(5) C24 0.0260(7) 0.0187(6) 0.0206(7) 0.0002(5) 0.0004(5) -0.0007(5) C25 0.0177(6) 0.0191(6) 0.0153(6) 0.0018(5) 0.0011(5) -0.0031(5) C26 0.0297(7) 0.0170(6) 0.0191(7) 0.0001(5) 0.0025(5) -0.0033(5) C27 0.0178(6) 0.0293(7) 0.0254(7) 0.0030(6) 0.0045(5) -0.0036(6) C28 0.0180(6) 0.0156(6) 0.0202(7) 0.0038(5) 0.0041(5) 0.0027(5) C29 0.0270(7) 0.0212(7) 0.0260(7) 0.0026(6) 0.0094(6) 0.0069(5) C30 0.0219(6) 0.0251(7) 0.0241(7) 0.0081(6) 0.0014(5) 0.0065(5) _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 C1 2.0241(13) . ? Pd1 C8 2.0431(12) . ? Pd1 O1 2.1854(9) . ? Pd1 P1 2.2939(3) . ? P1 N1 1.7765(11) . ? P1 C25 1.8444(13) . ? P1 C28 1.8517(13) . ? O1 C12 1.2366(16) . ? N1 C12 1.3777(17) . ? N1 C13 1.4583(16) . ? C1 C2 1.3969(17) . ? C1 C6 1.4077(17) . ? C2 C3 1.3928(19) . ? C2 H2 0.9500 . ? C3 C4 1.389(2) . ? C3 H3 0.9500 . ? C4 C5 1.3942(19) . ? C4 H4 0.9500 . ? C5 C6 1.3891(18) . ? C5 H5 0.9500 . ? C6 C7 1.5154(17) . ? C7 C10 1.5355(19) . ? C7 C9 1.5364(18) . ? C7 C8 1.5452(18) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.5038(17) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.4042(18) . ? C13 C18 1.4129(18) . ? C14 C15 1.3986(18) . ? C14 C19 1.5194(19) . ? C15 C16 1.382(2) . ? C15 H15 0.9500 . ? C16 C17 1.383(2) . ? C16 H16 0.9500 . ? C17 C18 1.3941(18) . ? C17 H17 0.9500 . ? C18 C22 1.5208(18) . ? C19 C20 1.5359(18) . ? C19 C21 1.5367(19) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.5346(18) . ? C22 C23 1.5353(18) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.5328(18) . ? C25 C26 1.5329(19) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.5323(19) . ? C28 C29 1.5420(18) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 C1 Pd1 C8 79.00(5) . . ? C1 Pd1 O1 96.90(4) . . ? C8 Pd1 O1 175.81(4) . . ? C1 Pd1 P1 172.94(4) . . ? C8 Pd1 P1 104.71(4) . . ? O1 Pd1 P1 79.27(3) . . ? N1 P1 C25 103.15(6) . . ? N1 P1 C28 104.16(5) . . ? C25 P1 C28 106.25(6) . . ? N1 P1 Pd1 101.03(4) . . ? C25 P1 Pd1 111.40(4) . . ? C28 P1 Pd1 127.80(5) . . ? C12 O1 Pd1 120.35(8) . . ? C12 N1 C13 120.16(10) . . ? C12 N1 P1 115.47(9) . . ? C13 N1 P1 122.83(8) . . ? C2 C1 C6 118.33(12) . . ? C2 C1 Pd1 125.61(10) . . ? C6 C1 Pd1 116.06(9) . . ? C3 C2 C1 120.81(12) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.25(12) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.74(13) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.04(12) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.82(12) . . ? C5 C6 C7 124.95(11) . . ? C1 C6 C7 114.23(11) . . ? C6 C7 C10 108.95(11) . . ? C6 C7 C9 112.74(11) . . ? C10 C7 C9 108.83(11) . . ? C6 C7 C8 105.35(10) . . ? C10 C7 C8 109.56(11) . . ? C9 C7 C8 111.33(11) . . ? C7 C8 Pd1 109.89(8) . . ? C7 C8 H8A 109.7 . . ? Pd1 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? Pd1 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C12 N1 122.14(11) . . ? O1 C12 C11 118.74(12) . . ? N1 C12 C11 119.02(11) . . ? C14 C13 C18 121.86(12) . . ? C14 C13 N1 120.72(11) . . ? C18 C13 N1 117.40(11) . . ? C15 C14 C13 117.67(12) . . ? C15 C14 C19 118.35(12) . . ? C13 C14 C19 123.97(12) . . ? C16 C15 C14 121.21(13) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.31(13) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 121.06(13) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 117.78(12) . . ? C17 C18 C22 118.85(12) . . ? C13 C18 C22 123.31(11) . . ? C14 C19 C20 110.89(11) . . ? C14 C19 C21 111.35(11) . . ? C20 C19 C21 109.99(11) . . ? C14 C19 H19 108.2 . . ? C20 C19 H19 108.2 . . ? C21 C19 H19 108.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 C24 113.01(11) . . ? C18 C22 C23 110.19(11) . . ? C24 C22 C23 108.79(11) . . ? C18 C22 H22 108.2 . . ? C24 C22 H22 108.2 . . ? C23 C22 H22 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 109.47(11) . . ? C27 C25 P1 109.70(9) . . ? C26 C25 P1 109.20(9) . . ? C27 C25 H25 109.5 . . ? C26 C25 H25 109.5 . . ? P1 C25 H25 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.4 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 111.40(11) . . ? C30 C28 P1 117.39(10) . . ? C29 C28 P1 109.02(9) . . ? C30 C28 H28 106.1 . . ? C29 C28 H28 106.1 . . ? P1 C28 H28 106.1 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.4 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Pd1 P1 N1 -171.21(5) . . . . ? O1 Pd1 P1 N1 10.14(5) . . . . ? C8 Pd1 P1 C25 79.81(6) . . . . ? O1 Pd1 P1 C25 -98.84(5) . . . . ? C8 Pd1 P1 C28 -53.38(7) . . . . ? O1 Pd1 P1 C28 127.96(6) . . . . ? C1 Pd1 O1 C12 176.15(10) . . . . ? P1 Pd1 O1 C12 -9.86(10) . . . . ? C25 P1 N1 C12 102.67(10) . . . . ? C28 P1 N1 C12 -146.51(10) . . . . ? Pd1 P1 N1 C12 -12.62(10) . . . . ? C25 P1 N1 C13 -91.47(11) . . . . ? C28 P1 N1 C13 19.34(11) . . . . ? Pd1 P1 N1 C13 153.23(9) . . . . ? C8 Pd1 C1 C2 160.82(12) . . . . ? O1 Pd1 C1 C2 -20.08(12) . . . . ? C8 Pd1 C1 C6 -19.82(9) . . . . ? O1 Pd1 C1 C6 159.29(9) . . . . ? C6 C1 C2 C3 -0.30(19) . . . . ? Pd1 C1 C2 C3 179.05(10) . . . . ? C1 C2 C3 C4 -0.2(2) . . . . ? C2 C3 C4 C5 0.6(2) . . . . ? C3 C4 C5 C6 -0.4(2) . . . . ? C4 C5 C6 C1 -0.1(2) . . . . ? C4 C5 C6 C7 -179.63(12) . . . . ? C2 C1 C6 C5 0.47(18) . . . . ? Pd1 C1 C6 C5 -178.94(10) . . . . ? C2 C1 C6 C7 -179.98(11) . . . . ? Pd1 C1 C6 C7 0.61(14) . . . . ? C5 C6 C7 C10 88.15(15) . . . . ? C1 C6 C7 C10 -91.37(13) . . . . ? C5 C6 C7 C9 -32.77(18) . . . . ? C1 C6 C7 C9 147.70(12) . . . . ? C5 C6 C7 C8 -154.38(12) . . . . ? C1 C6 C7 C8 26.10(14) . . . . ? C6 C7 C8 Pd1 -41.26(12) . . . . ? C10 C7 C8 Pd1 75.80(11) . . . . ? C9 C7 C8 Pd1 -163.77(9) . . . . ? C1 Pd1 C8 C7 33.89(9) . . . . ? P1 Pd1 C8 C7 -139.95(8) . . . . ? Pd1 O1 C12 N1 4.23(17) . . . . ? Pd1 O1 C12 C11 -179.41(9) . . . . ? C13 N1 C12 O1 -159.44(12) . . . . ? P1 N1 C12 O1 6.82(17) . . . . ? C13 N1 C12 C11 24.21(18) . . . . ? P1 N1 C12 C11 -169.53(10) . . . . ? C12 N1 C13 C14 -100.19(15) . . . . ? P1 N1 C13 C14 94.60(13) . . . . ? C12 N1 C13 C18 81.29(15) . . . . ? P1 N1 C13 C18 -83.92(13) . . . . ? C18 C13 C14 C15 1.89(18) . . . . ? N1 C13 C14 C15 -176.56(11) . . . . ? C18 C13 C14 C19 -176.43(12) . . . . ? N1 C13 C14 C19 5.11(18) . . . . ? C13 C14 C15 C16 1.3(2) . . . . ? C19 C14 C15 C16 179.74(13) . . . . ? C14 C15 C16 C17 -2.9(2) . . . . ? C15 C16 C17 C18 1.2(2) . . . . ? C16 C17 C18 C13 1.91(19) . . . . ? C16 C17 C18 C22 -175.41(12) . . . . ? C14 C13 C18 C17 -3.48(18) . . . . ? N1 C13 C18 C17 175.03(11) . . . . ? C14 C13 C18 C22 173.71(12) . . . . ? N1 C13 C18 C22 -7.79(17) . . . . ? C15 C14 C19 C20 -67.18(16) . . . . ? C13 C14 C19 C20 111.13(14) . . . . ? C15 C14 C19 C21 55.64(16) . . . . ? C13 C14 C19 C21 -126.04(13) . . . . ? C17 C18 C22 C24 -42.48(16) . . . . ? C13 C18 C22 C24 140.36(12) . . . . ? C17 C18 C22 C23 79.46(15) . . . . ? C13 C18 C22 C23 -97.70(14) . . . . ? N1 P1 C25 C27 174.16(9) . . . . ? C28 P1 C25 C27 64.90(10) . . . . ? Pd1 P1 C25 C27 -78.23(10) . . . . ? N1 P1 C25 C26 -65.88(10) . . . . ? C28 P1 C25 C26 -175.13(9) . . . . ? Pd1 P1 C25 C26 41.74(10) . . . . ? N1 P1 C28 C30 -76.89(10) . . . . ? C25 P1 C28 C30 31.64(11) . . . . ? Pd1 P1 C28 C30 166.65(7) . . . . ? N1 P1 C28 C29 155.29(9) . . . . ? C25 P1 C28 C29 -96.17(10) . . . . ? Pd1 P1 C28 C29 38.83(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.583 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.053 data_6 _database_code_depnum_ccdc_archive 'CCDC 876281' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C30 H47 N O P Pd' _chemical_formula_sum 'C62 H59 B F24 N O P Pd' _chemical_formula_weight 1438.28 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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' F F 0.0727 0.0534 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.419(3) _cell_length_b 13.523(3) _cell_length_c 19.347(4) _cell_angle_alpha 78.15(3) _cell_angle_beta 82.33(3) _cell_angle_gamma 82.15(3) _cell_volume 3131.5(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9621 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 64.05 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 3.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3844 _exptl_absorpt_correction_T_max 0.5184 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _diffrn_ambient_temperature 120(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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10135 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 64.05 _reflns_number_total 10135 _reflns_number_gt 9653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1291P)^2^+6.6178P] 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 SHELXL _refine_ls_extinction_coef 0.00065(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10135 _refine_ls_number_parameters 933 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.06807(2) 0.47345(2) 0.293849(16) 0.031 Uani 1 1 d . . . P1 P 0.02233(9) 0.32064(9) 0.30802(6) 0.034 Uani 1 1 d . . . F1 F 0.5450(3) 0.4090(2) 0.57953(18) 0.056 Uani 1 1 d U . . F2 F 0.3833(3) 0.4797(2) 0.56348(18) 0.055 Uani 1 1 d U . . F3 F 0.4391(3) 0.4562(2) 0.66608(17) 0.054 Uani 1 1 d U . . F4 F 0.1170(3) 0.2600(3) 0.56180(19) 0.058 Uani 1 1 d U . . F5 F 0.0919(3) 0.1599(3) 0.66120(18) 0.057 Uani 1 1 d U . . F6 F 0.1751(3) 0.1019(3) 0.57178(19) 0.061 Uani 1 1 d U . . F7A F 0.7726(3) 0.1937(3) 0.5281(2) 0.043 Uani 0.70 1 d PDU A 1 F8A F 0.8666(5) 0.0490(4) 0.5282(3) 0.072 Uani 0.70 1 d PDU A 1 F9A F 0.9345(5) 0.1583(5) 0.5577(3) 0.071 Uani 0.70 1 d PDU A 1 F7B F 0.8122(11) 0.0615(9) 0.5216(6) 0.063 Uani 0.30 1 d PDU A 2 F8B F 0.9421(10) 0.0584(10) 0.5580(7) 0.075 Uani 0.30 1 d PDU A 2 F9B F 0.9077(10) 0.1924(9) 0.5669(7) 0.062 Uani 0.30 1 d PDU A 2 F10A F 0.9773(5) -0.0887(5) 0.8008(3) 0.059 Uani 0.59 1 d PDU B 1 F11A F 0.8381(5) -0.0950(5) 0.8767(3) 0.060 Uani 0.59 1 d PDU B 1 F12A F 0.9188(5) 0.0426(4) 0.8460(3) 0.052 Uani 0.59 1 d PDU B 1 F10B F 0.8633(7) -0.1164(6) 0.8543(5) 0.059 Uani 0.41 1 d PDU B 2 F11B F 0.8844(7) 0.0322(7) 0.8630(5) 0.056 Uani 0.41 1 d PDU B 2 F12B F 0.9936(6) -0.0457(7) 0.7882(5) 0.057 Uani 0.41 1 d PDU B 2 F13 F 0.5962(3) 0.1708(3) 0.9598(2) 0.064 Uani 1 1 d U . . F14 F 0.4584(4) 0.2799(3) 0.9508(2) 0.076 Uani 1 1 d U . . F15 F 0.4622(4) 0.1540(3) 1.0393(2) 0.076 Uani 1 1 d U . . F16A F 0.1144(6) 0.0238(6) 0.9081(4) 0.078 Uani 0.56 1 d PDU C 1 F17A F 0.2063(6) -0.1184(5) 0.9313(4) 0.073 Uani 0.56 1 d PDU C 1 F18A F 0.1726(7) -0.0325(7) 1.0109(4) 0.086 Uani 0.56 1 d PDU C 1 F16B F 0.1627(8) -0.0833(8) 0.9037(5) 0.077 Uani 0.44 1 d PDU C 2 F17B F 0.2044(8) -0.0954(7) 1.0041(5) 0.075 Uani 0.44 1 d PDU C 2 F18B F 0.1157(8) 0.0354(7) 0.9711(6) 0.085 Uani 0.44 1 d PDU C 2 F19A F 0.5219(7) -0.4240(6) 0.7990(4) 0.063 Uani 0.47 1 d PDU D 1 F20A F 0.3492(7) -0.3707(7) 0.8137(5) 0.074 Uani 0.47 1 d PDU D 1 F21A F 0.4576(7) -0.3302(7) 0.8752(4) 0.066 Uani 0.47 1 d PDU D 1 F19B F 0.4760(6) -0.4306(5) 0.7918(4) 0.064 Uani 0.53 1 d PDU D 2 F20B F 0.3464(6) -0.3417(6) 0.8409(4) 0.071 Uani 0.53 1 d PDU D 2 F21B F 0.5040(6) -0.3407(6) 0.8685(4) 0.066 Uani 0.53 1 d PDU D 2 F22 F 0.5922(3) -0.1660(3) 0.5223(2) 0.072 Uani 1 1 d U . . F23 F 0.4739(3) -0.2704(3) 0.5444(2) 0.072 Uani 1 1 d U . . F24 F 0.4245(3) -0.1111(3) 0.5195(2) 0.068 Uani 1 1 d U . . O1 O -0.0136(3) 0.3176(2) 0.22869(17) 0.038 Uani 1 1 d . . . N1 N 0.0341(3) 0.4778(3) 0.18593(19) 0.033 Uani 1 1 d . . . C1 C 0.0801(4) 0.4603(4) 0.3999(2) 0.036 Uani 1 1 d . . . H1A H 0.0164 0.4978 0.4234 0.043 Uiso 1 1 d R . . H1B H 0.0875 0.3882 0.4245 0.043 Uiso 1 1 d R . . C2 C 0.1852(4) 0.5094(4) 0.3974(3) 0.037 Uani 1 1 d . . . C3 C 0.1960(4) 0.5807(4) 0.3244(3) 0.037 Uani 1 1 d . . . C4 C 0.1050(4) 0.6456(4) 0.3001(3) 0.039 Uani 1 1 d . . . H4 H 0.0359 0.6425 0.3278 0.046 Uiso 1 1 d R . . C5 C 0.1149(4) 0.7156(4) 0.2352(3) 0.043 Uani 1 1 d . . . H5 H 0.0525 0.7591 0.2196 0.051 Uiso 1 1 d R . . C6 C 0.2143(5) 0.7209(4) 0.1943(3) 0.049 Uani 1 1 d . . . H6 H 0.2211 0.7686 0.1509 0.058 Uiso 1 1 d R . . C7 C 0.3044(5) 0.6563(5) 0.2169(3) 0.051 Uani 1 1 d . . . H7 H 0.3732 0.6595 0.1888 0.061 Uiso 1 1 d R . . C8 C 0.2953(4) 0.5864(4) 0.2804(3) 0.042 Uani 1 1 d . . . H8 H 0.3577 0.5415 0.2944 0.051 Uiso 1 1 d R . . C9 C 0.2824(4) 0.4272(4) 0.4058(3) 0.041 Uani 1 1 d . . . H9A H 0.3486 0.4586 0.4069 0.062 Uiso 1 1 d R . . H9B H 0.2923 0.3916 0.3657 0.062 Uiso 1 1 d R . . H9C H 0.2684 0.3787 0.4503 0.062 Uiso 1 1 d R . . C10 C 0.1750(4) 0.5713(4) 0.4573(3) 0.042 Uani 1 1 d . . . H10A H 0.1651 0.5257 0.5035 0.063 Uiso 1 1 d R . . H10B H 0.1118 0.6232 0.4522 0.063 Uiso 1 1 d R . . H10C H 0.2415 0.6043 0.4541 0.063 Uiso 1 1 d R . . C11 C 0.0328(4) 0.5672(4) 0.1298(2) 0.036 Uani 1 1 d . . . C12 C -0.0618(4) 0.6356(4) 0.1269(2) 0.039 Uani 1 1 d . . . C13 C -0.0607(5) 0.7225(4) 0.0741(3) 0.046 Uani 1 1 d . . . H13 H -0.1246 0.7699 0.0702 0.055 Uiso 1 1 d R . . C14 C 0.0317(4) 0.7413(4) 0.0276(3) 0.044 Uani 1 1 d . . . H14 H 0.0306 0.8007 -0.0086 0.053 Uiso 1 1 d R . . C15 C 0.1251(4) 0.6738(4) 0.0331(3) 0.043 Uani 1 1 d . . . H15 H 0.1886 0.6884 0.0013 0.051 Uiso 1 1 d R . . C16 C 0.1290(4) 0.5843(4) 0.0845(2) 0.037 Uani 1 1 d . . . C17 C -0.1632(4) 0.6213(5) 0.1801(3) 0.052 Uani 1 1 d . . . H17 H -0.1461 0.5613 0.2184 0.062 Uiso 1 1 d R . . C18 C -0.1963(6) 0.7161(8) 0.2135(5) 0.092 Uani 1 1 d . . . H18A H -0.1375 0.7262 0.2396 0.138 Uiso 1 1 d R . . H18B H -0.2630 0.7066 0.2463 0.138 Uiso 1 1 d R . . H18C H -0.2100 0.7759 0.1761 0.138 Uiso 1 1 d R . . C19 C -0.2585(6) 0.6041(8) 0.1471(5) 0.098 Uani 1 1 d . . . H19A H -0.3166 0.5821 0.1843 0.147 Uiso 1 1 d R . . H19B H -0.2363 0.5515 0.1183 0.147 Uiso 1 1 d R . . H19C H -0.2855 0.6676 0.1167 0.147 Uiso 1 1 d R . . C20 C 0.2325(4) 0.5105(4) 0.0904(3) 0.043 Uani 1 1 d . . . H20 H 0.2411 0.4877 0.1421 0.052 Uiso 1 1 d R . . C21 C 0.2274(5) 0.4160(5) 0.0600(3) 0.057 Uani 1 1 d . . . H21A H 0.1704 0.3769 0.0883 0.086 Uiso 1 1 d R . . H21B H 0.2982 0.3739 0.0614 0.086 Uiso 1 1 d R . . H21C H 0.2103 0.4365 0.0107 0.086 Uiso 1 1 d R . . C22 C 0.3358(5) 0.5587(5) 0.0552(3) 0.057 Uani 1 1 d . . . H22A H 0.3349 0.5728 0.0035 0.086 Uiso 1 1 d R . . H22B H 0.4008 0.5120 0.0678 0.086 Uiso 1 1 d R . . H22C H 0.3374 0.6224 0.0715 0.086 Uiso 1 1 d R . . C23 C -0.0065(4) 0.4000(4) 0.1766(3) 0.038 Uani 1 1 d . . . C24 C -0.0509(5) 0.3849(4) 0.1122(3) 0.049 Uani 1 1 d . . . H24A H -0.0440 0.4454 0.0747 0.073 Uiso 1 1 d R . . H24B H -0.1282 0.3739 0.1237 0.073 Uiso 1 1 d R . . H24C H -0.0097 0.3255 0.0955 0.073 Uiso 1 1 d R . . C25 C -0.0979(4) 0.2805(4) 0.3660(3) 0.043 Uani 1 1 d . . . H25 H -0.0817 0.2734 0.4161 0.051 Uiso 1 1 d R . . C26 C -0.1941(4) 0.3642(5) 0.3536(3) 0.052 Uani 1 1 d . . . H26A H -0.2128 0.3721 0.3049 0.078 Uiso 1 1 d R . . H26B H -0.1736 0.4286 0.3606 0.078 Uiso 1 1 d R . . H26C H -0.2575 0.3453 0.3873 0.078 Uiso 1 1 d R . . C27 C -0.1268(5) 0.1777(4) 0.3571(3) 0.055 Uani 1 1 d . . . H27A H -0.1936 0.1610 0.3880 0.082 Uiso 1 1 d R . . H27B H -0.0665 0.1251 0.3700 0.082 Uiso 1 1 d R . . H27C H -0.1384 0.1812 0.3075 0.082 Uiso 1 1 d R . . C28 C 0.1315(4) 0.2163(4) 0.3159(3) 0.042 Uani 1 1 d . . . H28 H 0.1039 0.1568 0.3034 0.050 Uiso 1 1 d R . . C29 C 0.2291(4) 0.2432(4) 0.2631(3) 0.051 Uani 1 1 d . . . H29A H 0.2573 0.3022 0.2735 0.076 Uiso 1 1 d R . . H29B H 0.2069 0.2596 0.2150 0.076 Uiso 1 1 d R . . H29C H 0.2864 0.1854 0.2666 0.076 Uiso 1 1 d R . . C30 C 0.1615(5) 0.1843(4) 0.3924(3) 0.051 Uani 1 1 d . . . H30A H 0.2159 0.1242 0.3957 0.076 Uiso 1 1 d R . . H30B H 0.0960 0.1682 0.4249 0.076 Uiso 1 1 d R . . H30C H 0.1921 0.2401 0.4055 0.076 Uiso 1 1 d R . . C31 C 0.4312(4) 0.1332(4) 0.6870(2) 0.033 Uani 1 1 d . . . C32 C 0.3330(4) 0.1202(4) 0.6642(2) 0.033 Uani 1 1 d . . . H32 H 0.3079 0.0549 0.6761 0.040 Uiso 1 1 d R . . C33 C 0.2706(3) 0.1997(4) 0.6247(2) 0.034 Uani 1 1 d . . . C34 C 0.3050(4) 0.2959(4) 0.6059(2) 0.035 Uani 1 1 d . . . H34 H 0.2628 0.3502 0.5785 0.042 Uiso 1 1 d R . . C35 C 0.4017(4) 0.3109(3) 0.6278(2) 0.034 Uani 1 1 d . . . C36 C 0.4624(4) 0.2317(3) 0.6678(2) 0.033 Uani 1 1 d . . . H36 H 0.5279 0.2447 0.6830 0.040 Uiso 1 1 d R . . C37 C 0.1644(4) 0.1802(4) 0.6044(3) 0.039 Uani 1 1 d . . . C38 C 0.4409(4) 0.4132(4) 0.6088(3) 0.039 Uani 1 1 d . . . C39 C 0.6316(4) 0.0490(3) 0.7241(2) 0.033 Uani 1 1 d . . . C40 C 0.6810(4) 0.0844(4) 0.6561(3) 0.036 Uani 1 1 d . . . H40 H 0.6360 0.1094 0.6188 0.043 Uiso 1 1 d R . . C41 C 0.7938(4) 0.0849(4) 0.6403(3) 0.040 Uani 1 1 d . A . C42 C 0.8621(4) 0.0481(4) 0.6933(3) 0.042 Uani 1 1 d . . . H42 H 0.9391 0.0488 0.6834 0.050 Uiso 1 1 d R . . C43 C 0.8152(4) 0.0107(4) 0.7613(3) 0.039 Uani 1 1 d . B . C44 C 0.7025(4) 0.0108(4) 0.7760(3) 0.038 Uani 1 1 d . . . H44 H 0.6730 -0.0156 0.8230 0.045 Uiso 1 1 d R . . C45 C 0.8405(4) 0.1205(4) 0.5659(3) 0.047 Uani 1 1 d D . . C46 C 0.8881(4) -0.0296(4) 0.8188(3) 0.048 Uani 1 1 d D . . C47 C 0.4468(4) 0.0523(3) 0.8195(2) 0.034 Uani 1 1 d . . . C48 C 0.4889(4) 0.1079(4) 0.8610(2) 0.036 Uani 1 1 d . . . H48 H 0.5541 0.1382 0.8431 0.044 Uiso 1 1 d R . . C49 C 0.4388(4) 0.1203(4) 0.9280(3) 0.039 Uani 1 1 d . . . C50 C 0.3428(4) 0.0774(4) 0.9554(3) 0.042 Uani 1 1 d . . . H50 H 0.3087 0.0849 1.0013 0.050 Uiso 1 1 d R . . C51 C 0.2979(4) 0.0241(4) 0.9151(3) 0.042 Uani 1 1 d . C . C52 C 0.3486(4) 0.0132(4) 0.8479(2) 0.037 Uani 1 1 d . . . H52 H 0.3150 -0.0223 0.8205 0.045 Uiso 1 1 d R . . C53 C 0.4874(5) 0.1807(4) 0.9691(3) 0.046 Uani 1 1 d . . . C54 C 0.1962(4) -0.0240(4) 0.9427(3) 0.050 Uani 1 1 d D . . C55 C 0.4853(3) -0.0697(3) 0.7205(2) 0.034 Uani 1 1 d . . . C56 C 0.4750(4) -0.1580(4) 0.7718(3) 0.036 Uani 1 1 d . . . H56 H 0.4733 -0.1546 0.8205 0.043 Uiso 1 1 d R . . C57 C 0.4669(4) -0.2509(4) 0.7544(3) 0.040 Uani 1 1 d . D . C58 C 0.4718(4) -0.2607(4) 0.6842(3) 0.041 Uani 1 1 d . . . H58 H 0.4666 -0.3245 0.6722 0.050 Uiso 1 1 d R . . C59 C 0.4846(4) -0.1746(4) 0.6316(3) 0.038 Uani 1 1 d . . . C60 C 0.4910(4) -0.0817(4) 0.6502(2) 0.035 Uani 1 1 d . . . H60 H 0.4991 -0.0241 0.6132 0.042 Uiso 1 1 d R . . C61 C 0.4930(4) -0.1814(4) 0.5556(3) 0.044 Uani 1 1 d . . . C62 C 0.4508(5) -0.3420(4) 0.8115(3) 0.053 Uani 1 1 d D . . B1 B 0.4995(4) 0.0414(4) 0.7384(3) 0.033 Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.031 0.031 0.031 -0.006 -0.003 -0.003 P1 0.034 0.032 0.035 -0.007 -0.004 -0.006 F1 0.048 0.052 0.065 -0.007 0.003 -0.012 F2 0.056 0.049 0.059 0.002 -0.015 -0.009 F3 0.062 0.049 0.056 -0.014 -0.007 -0.011 F4 0.049 0.060 0.064 0.001 -0.019 -0.008 F5 0.045 0.071 0.057 -0.008 -0.005 -0.015 F6 0.055 0.066 0.070 -0.026 -0.017 -0.006 F7A 0.038 0.047 0.038 0.001 -0.002 -0.002 F8A 0.075 0.068 0.069 -0.014 0.003 -0.004 F9A 0.062 0.076 0.071 -0.006 -0.005 -0.012 F7B 0.063 0.065 0.061 -0.012 -0.007 -0.009 F8B 0.073 0.076 0.073 -0.012 -0.003 -0.005 F9B 0.062 0.061 0.063 -0.011 -0.004 -0.010 F10A 0.056 0.060 0.060 -0.011 -0.011 0.000 F11A 0.058 0.061 0.059 -0.006 -0.011 -0.002 F12A 0.053 0.055 0.052 -0.012 -0.010 -0.011 F10B 0.059 0.059 0.059 -0.010 -0.012 -0.003 F11B 0.058 0.059 0.055 -0.014 -0.009 -0.007 F12B 0.052 0.059 0.058 -0.007 -0.010 -0.004 F13 0.062 0.071 0.066 -0.024 -0.012 -0.010 F14 0.083 0.065 0.084 -0.022 -0.020 -0.005 F15 0.085 0.086 0.064 -0.022 -0.008 -0.021 F16A 0.068 0.080 0.085 -0.008 -0.011 -0.014 F17A 0.069 0.070 0.078 -0.008 -0.001 -0.012 F18A 0.084 0.091 0.084 -0.017 -0.003 -0.015 F16B 0.074 0.080 0.077 -0.014 -0.006 -0.016 F17B 0.071 0.074 0.078 -0.007 -0.007 -0.011 F18B 0.079 0.081 0.090 -0.013 0.000 -0.010 F19A 0.063 0.058 0.063 -0.008 -0.007 -0.003 F20A 0.073 0.072 0.074 -0.009 -0.005 -0.015 F21A 0.068 0.064 0.064 -0.008 -0.002 -0.007 F19B 0.067 0.058 0.065 -0.010 -0.006 -0.008 F20B 0.071 0.069 0.069 -0.009 0.001 -0.010 F21B 0.066 0.064 0.065 -0.004 -0.009 -0.008 F22 0.069 0.088 0.061 -0.023 0.001 -0.013 F23 0.088 0.068 0.067 -0.025 -0.009 -0.016 F24 0.075 0.073 0.059 -0.019 -0.018 0.004 O1 0.042 0.038 0.036 -0.009 -0.005 -0.007 N1 0.034 0.037 0.027 -0.006 -0.004 0.000 C1 0.040 0.041 0.027 -0.007 -0.001 -0.008 C2 0.034 0.037 0.041 -0.010 -0.002 -0.005 C3 0.037 0.036 0.039 -0.010 -0.004 -0.006 C4 0.039 0.034 0.045 -0.011 -0.005 -0.006 C5 0.044 0.033 0.052 -0.006 -0.009 -0.005 C6 0.062 0.039 0.045 0.001 -0.008 -0.018 C7 0.046 0.059 0.049 -0.007 0.004 -0.017 C8 0.038 0.045 0.043 -0.008 -0.003 -0.005 C9 0.041 0.041 0.042 -0.007 -0.009 -0.005 C10 0.041 0.050 0.040 -0.014 -0.006 -0.008 C11 0.040 0.041 0.029 -0.006 -0.006 -0.003 C12 0.041 0.040 0.033 -0.006 -0.001 0.001 C13 0.049 0.044 0.041 -0.006 -0.007 0.005 C14 0.053 0.042 0.035 -0.001 -0.004 -0.009 C15 0.045 0.047 0.037 -0.009 0.000 -0.010 C16 0.041 0.043 0.028 -0.008 -0.003 -0.006 C17 0.044 0.063 0.034 0.004 0.004 0.010 C18 0.061 0.140 0.090 -0.067 0.026 -0.031 C19 0.064 0.144 0.105 -0.067 0.034 -0.055 C20 0.042 0.050 0.036 -0.007 0.000 -0.004 C21 0.054 0.059 0.059 -0.022 0.001 0.007 C22 0.043 0.065 0.056 -0.001 0.006 -0.006 C23 0.034 0.044 0.038 -0.013 -0.004 0.001 C24 0.060 0.049 0.041 -0.011 -0.011 -0.008 C25 0.042 0.046 0.040 -0.005 0.002 -0.014 C26 0.040 0.058 0.056 -0.012 0.004 -0.007 C27 0.058 0.053 0.055 -0.011 0.005 -0.022 C28 0.043 0.030 0.053 -0.010 -0.010 -0.001 C29 0.039 0.044 0.071 -0.020 -0.006 0.001 C30 0.056 0.038 0.058 -0.003 -0.018 0.000 C31 0.028 0.041 0.029 -0.008 0.000 -0.002 C32 0.032 0.038 0.030 -0.009 0.001 -0.003 C33 0.027 0.040 0.034 -0.007 -0.002 -0.003 C34 0.034 0.039 0.030 -0.005 -0.004 0.003 C35 0.034 0.037 0.031 -0.007 0.002 -0.004 C36 0.027 0.040 0.033 -0.009 -0.003 -0.002 C37 0.033 0.043 0.041 -0.007 -0.003 -0.006 C38 0.034 0.038 0.042 -0.004 -0.006 -0.003 C39 0.032 0.032 0.037 -0.009 -0.004 0.000 C40 0.029 0.038 0.041 -0.012 -0.004 -0.001 C41 0.034 0.037 0.050 -0.014 -0.001 -0.007 C42 0.029 0.041 0.060 -0.018 -0.006 -0.005 C43 0.036 0.038 0.046 -0.019 -0.010 0.002 C44 0.037 0.036 0.042 -0.013 -0.005 0.000 C45 0.037 0.046 0.058 -0.015 0.012 -0.011 C46 0.038 0.050 0.058 -0.021 -0.012 0.006 C47 0.032 0.034 0.033 -0.003 -0.003 0.003 C48 0.037 0.034 0.036 -0.004 -0.005 0.001 C49 0.042 0.036 0.038 -0.005 -0.007 0.003 C50 0.045 0.044 0.032 -0.006 0.000 0.004 C51 0.036 0.046 0.037 -0.002 -0.003 0.003 C52 0.031 0.043 0.036 -0.007 -0.005 0.001 C53 0.057 0.044 0.037 -0.011 -0.004 0.000 C54 0.039 0.072 0.038 -0.013 0.003 -0.003 C55 0.025 0.037 0.038 -0.007 -0.004 0.000 C56 0.030 0.039 0.038 -0.007 -0.003 0.000 C57 0.035 0.036 0.046 -0.005 -0.004 -0.001 C58 0.035 0.037 0.054 -0.013 -0.003 -0.004 C59 0.030 0.046 0.040 -0.012 -0.004 -0.003 C60 0.030 0.036 0.036 -0.006 -0.002 -0.001 C61 0.042 0.047 0.047 -0.017 -0.004 -0.003 C62 0.061 0.040 0.057 -0.008 0.002 -0.011 B1 0.031 0.035 0.032 -0.006 -0.003 -0.004 _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 C1 2.047(4) . ? Pd1 P1 2.1712(13) . ? Pd1 N1 2.172(4) . ? Pd1 C4 2.463(5) . ? Pd1 C3 2.491(5) . ? P1 O1 1.664(3) . ? P1 C28 1.816(5) . ? P1 C25 1.818(5) . ? F1 C38 1.339(6) . ? F2 C38 1.326(6) . ? F3 C38 1.349(6) . ? F4 C37 1.335(6) . ? F5 C37 1.332(6) . ? F6 C37 1.324(6) . ? F7A C45 1.366(7) . ? F8A C45 1.308(7) . ? F9A C45 1.315(7) . ? F7B C45 1.390(11) . ? F8B C45 1.425(12) . ? F9B C45 1.370(11) . ? F10A C46 1.325(7) . ? F11A C46 1.407(8) . ? F12A C46 1.320(7) . ? F10B C46 1.287(10) . ? F11B C46 1.304(9) . ? F12B C46 1.372(9) . ? F13 C53 1.331(7) . ? F14 C53 1.327(7) . ? F15 C53 1.339(7) . ? F16A C54 1.313(8) . ? F17A C54 1.326(8) . ? F18A C54 1.298(9) . ? F16B C54 1.346(10) . ? F17B C54 1.374(10) . ? F18B C54 1.327(10) . ? F19A C62 1.360(9) . ? F20A C62 1.363(9) . ? F21A C62 1.289(9) . ? F19B C62 1.315(8) . ? F20B C62 1.345(9) . ? F21B C62 1.363(9) . ? F22 C61 1.335(7) . ? F23 C61 1.324(6) . ? F24 C61 1.335(7) . ? O1 C23 1.344(6) . ? N1 C23 1.280(6) . ? N1 C11 1.450(6) . ? C1 C2 1.533(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C9 1.526(7) . ? C2 C3 1.539(7) . ? C2 C10 1.546(7) . ? C3 C4 1.403(7) . ? C3 C8 1.404(7) . ? C4 C5 1.411(7) . ? C4 H4 0.9500 . ? C5 C6 1.377(8) . ? C5 H5 0.9500 . ? C6 C7 1.383(8) . ? C6 H6 0.9500 . ? C7 C8 1.390(8) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.392(7) . ? C11 C16 1.401(7) . ? C12 C13 1.391(7) . ? C12 C17 1.524(7) . ? C13 C14 1.379(8) . ? C13 H13 0.9500 . ? C14 C15 1.376(8) . ? C14 H14 0.9500 . ? C15 C16 1.400(7) . ? C15 H15 0.9500 . ? C16 C20 1.517(7) . ? C17 C19 1.483(10) . ? C17 C18 1.534(10) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.525(8) . ? C20 C22 1.531(7) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.490(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.530(7) . ? C25 C26 1.537(8) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.511(8) . ? C28 C30 1.535(8) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.396(6) . ? C31 C36 1.400(7) . ? C31 B1 1.636(7) . ? C32 C33 1.391(7) . ? C32 H32 0.9500 . ? C33 C34 1.387(7) . ? C33 C37 1.495(6) . ? C34 C35 1.380(7) . ? C34 H34 0.9500 . ? C35 C36 1.382(7) . ? C35 C38 1.488(7) . ? C36 H36 0.9500 . ? C39 C40 1.394(7) . ? C39 C44 1.396(7) . ? C39 B1 1.641(6) . ? C40 C41 1.394(7) . ? C40 H40 0.9500 . ? C41 C42 1.388(7) . ? C41 C45 1.488(7) . ? C42 C43 1.388(8) . ? C42 H42 0.9500 . ? C43 C44 1.390(7) . ? C43 C46 1.498(7) . ? C44 H44 0.9500 . ? C47 C52 1.394(7) . ? C47 C48 1.397(7) . ? C47 B1 1.646(7) . ? C48 C49 1.393(7) . ? C48 H48 0.9500 . ? C49 C50 1.390(7) . ? C49 C53 1.481(7) . ? C50 C51 1.377(8) . ? C50 H50 0.9500 . ? C51 C52 1.395(7) . ? C51 C54 1.485(7) . ? C52 H52 0.9500 . ? C55 C60 1.393(7) . ? C55 C56 1.397(7) . ? C55 B1 1.646(7) . ? C56 C57 1.385(7) . ? C56 H56 0.9500 . ? C57 C58 1.384(7) . ? C57 C62 1.493(7) . ? C58 C59 1.392(7) . ? C58 H58 0.9500 . ? C59 C60 1.391(7) . ? C59 C61 1.480(7) . ? C60 H60 0.9500 . ? 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 C1 Pd1 P1 92.75(14) . . ? C1 Pd1 N1 171.97(16) . . ? P1 Pd1 N1 81.55(11) . . ? C1 Pd1 C4 78.05(18) . . ? P1 Pd1 C4 169.63(12) . . ? N1 Pd1 C4 107.09(16) . . ? C1 Pd1 C3 64.21(17) . . ? P1 Pd1 C3 145.41(12) . . ? N1 Pd1 C3 123.41(15) . . ? C4 Pd1 C3 32.89(16) . . ? O1 P1 C28 100.5(2) . . ? O1 P1 C25 101.2(2) . . ? C28 P1 C25 108.9(2) . . ? O1 P1 Pd1 102.71(13) . . ? C28 P1 Pd1 117.31(17) . . ? C25 P1 Pd1 122.03(18) . . ? C23 O1 P1 119.2(3) . . ? C23 N1 C11 118.5(4) . . ? C23 N1 Pd1 115.2(3) . . ? C11 N1 Pd1 125.1(3) . . ? C2 C1 Pd1 100.9(3) . . ? C2 C1 H1A 111.5 . . ? Pd1 C1 H1A 111.5 . . ? C2 C1 H1B 111.7 . . ? Pd1 C1 H1B 111.6 . . ? H1A C1 H1B 109.4 . . ? C9 C2 C1 109.8(4) . . ? C9 C2 C3 111.7(4) . . ? C1 C2 C3 105.2(4) . . ? C9 C2 C10 109.5(4) . . ? C1 C2 C10 110.4(4) . . ? C3 C2 C10 110.1(4) . . ? C4 C3 C8 117.2(4) . . ? C4 C3 C2 120.0(4) . . ? C8 C3 C2 122.7(4) . . ? C4 C3 Pd1 72.4(3) . . ? C8 C3 Pd1 115.5(3) . . ? C2 C3 Pd1 83.7(3) . . ? C3 C4 C5 120.8(5) . . ? C3 C4 Pd1 74.7(3) . . ? C5 C4 Pd1 116.6(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.5 . . ? Pd1 C4 H4 79.5 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.5(5) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.1 . . ? C6 C7 C8 120.6(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.5 . . ? C7 C8 C3 121.5(5) . . ? C7 C8 H8 119.3 . . ? C3 C8 H8 119.2 . . ? C2 C9 H9A 109.6 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.3 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 H10A 109.4 . . ? C2 C10 H10B 109.4 . . ? H10A C10 H10B 109.5 . . ? C2 C10 H10C 109.6 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 123.2(4) . . ? C12 C11 N1 118.1(4) . . ? C16 C11 N1 118.5(4) . . ? C13 C12 C11 117.5(5) . . ? C13 C12 C17 119.3(5) . . ? C11 C12 C17 123.2(4) . . ? C14 C13 C12 121.1(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 121.7(5) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.1 . . ? C15 C16 C11 116.4(5) . . ? C15 C16 C20 121.3(4) . . ? C11 C16 C20 122.3(4) . . ? C19 C17 C12 112.6(5) . . ? C19 C17 C18 107.5(6) . . ? C12 C17 C18 110.1(5) . . ? C19 C17 H17 108.7 . . ? C12 C17 H17 108.7 . . ? C18 C17 H17 109.1 . . ? C17 C18 H18A 109.7 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.7 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.6 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.3 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 C21 112.8(4) . . ? C16 C20 C22 113.3(4) . . ? C21 C20 C22 108.4(5) . . ? C16 C20 H20 107.4 . . ? C21 C20 H20 107.5 . . ? C22 C20 H20 107.2 . . ? C20 C21 H21A 109.4 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.4 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.2 . . ? C20 C22 H22B 109.8 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.4 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 O1 120.8(4) . . ? N1 C23 C24 128.4(5) . . ? O1 C23 C24 110.8(4) . . ? C23 C24 H24A 109.3 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 111.6(5) . . ? C27 C25 P1 113.0(4) . . ? C26 C25 P1 109.1(4) . . ? C27 C25 H25 107.6 . . ? C26 C25 H25 107.7 . . ? P1 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.3 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.7 . . ? C25 C27 H27B 109.3 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.4 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 112.3(5) . . ? C29 C28 P1 110.3(4) . . ? C30 C28 P1 111.5(4) . . ? C29 C28 H28 107.4 . . ? C30 C28 H28 107.5 . . ? P1 C28 H28 107.5 . . ? C28 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.6 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.4 . . ? C28 C30 H30B 109.6 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 115.6(4) . . ? C32 C31 B1 121.8(4) . . ? C36 C31 B1 122.4(4) . . ? C33 C32 C31 122.2(4) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C34 C33 C32 120.5(4) . . ? C34 C33 C37 120.6(4) . . ? C32 C33 C37 118.8(4) . . ? C35 C34 C33 118.5(4) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.7 . . ? C34 C35 C36 120.5(4) . . ? C34 C35 C38 119.9(4) . . ? C36 C35 C38 119.5(4) . . ? C35 C36 C31 122.7(4) . . ? C35 C36 H36 118.5 . . ? C31 C36 H36 118.8 . . ? F6 C37 F5 106.6(4) . . ? F6 C37 F4 107.2(4) . . ? F5 C37 F4 105.7(4) . . ? F6 C37 C33 112.6(4) . . ? F5 C37 C33 111.4(4) . . ? F4 C37 C33 112.9(4) . . ? F2 C38 F1 106.6(4) . . ? F2 C38 F3 106.1(4) . . ? F1 C38 F3 105.2(4) . . ? F2 C38 C35 114.0(4) . . ? F1 C38 C35 111.9(4) . . ? F3 C38 C35 112.4(4) . . ? C40 C39 C44 115.8(4) . . ? C40 C39 B1 120.8(4) . . ? C44 C39 B1 123.0(4) . . ? C41 C40 C39 122.8(4) . . ? C41 C40 H40 118.5 . . ? C39 C40 H40 118.8 . . ? C42 C41 C40 120.1(5) . . ? C42 C41 C45 120.3(4) . . ? C40 C41 C45 119.5(5) . . ? C41 C42 C43 118.3(4) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.9 . . ? C42 C43 C44 120.8(4) . . ? C42 C43 C46 118.8(4) . . ? C44 C43 C46 120.4(5) . . ? C43 C44 C39 122.2(5) . . ? C43 C44 H44 118.7 . . ? C39 C44 H44 119.1 . . ? F8A C45 F9A 99.9(5) . . ? F8A C45 F7A 106.1(5) . . ? F9A C45 F7A 105.1(5) . . ? F8A C45 F9B 123.2(7) . . ? F7A C45 F9B 89.4(7) . . ? F9A C45 F7B 124.1(7) . . ? F7A C45 F7B 82.4(6) . . ? F9B C45 F7B 141.7(9) . . ? F8A C45 F8B 51.8(6) . . ? F9A C45 F8B 58.4(6) . . ? F7A C45 F8B 141.7(7) . . ? F9B C45 F8B 82.4(8) . . ? F7B C45 F8B 81.5(8) . . ? F8A C45 C41 114.7(5) . . ? F9A C45 C41 116.2(5) . . ? F7A C45 C41 113.3(4) . . ? F9B C45 C41 107.4(7) . . ? F7B C45 C41 110.2(6) . . ? F8B C45 C41 104.9(7) . . ? F10B C46 F11B 108.6(7) . . ? F10B C46 F12A 125.3(6) . . ? F10B C46 F10A 79.8(6) . . ? F11B C46 F10A 123.6(6) . . ? F12A C46 F10A 107.7(5) . . ? F10B C46 F12B 106.4(7) . . ? F11B C46 F12B 109.1(6) . . ? F12A C46 F12B 88.2(5) . . ? F11B C46 F11A 85.6(6) . . ? F12A C46 F11A 105.6(5) . . ? F10A C46 F11A 101.2(5) . . ? F12B C46 F11A 125.5(6) . . ? F10B C46 C43 111.1(6) . . ? F11B C46 C43 112.7(6) . . ? F12A C46 C43 113.2(5) . . ? F10A C46 C43 115.3(5) . . ? F12B C46 C43 108.7(5) . . ? F11A C46 C43 112.9(5) . . ? C52 C47 C48 115.9(4) . . ? C52 C47 B1 120.0(4) . . ? C48 C47 B1 123.8(4) . . ? C49 C48 C47 122.3(5) . . ? C49 C48 H48 118.7 . . ? C47 C48 H48 119.0 . . ? C50 C49 C48 120.0(5) . . ? C50 C49 C53 120.5(5) . . ? C48 C49 C53 119.5(5) . . ? C51 C50 C49 119.1(4) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.4 . . ? C50 C51 C52 120.2(5) . . ? C50 C51 C54 120.8(4) . . ? C52 C51 C54 119.0(5) . . ? C47 C52 C51 122.4(5) . . ? C47 C52 H52 119.0 . . ? C51 C52 H52 118.6 . . ? F14 C53 F13 104.6(5) . . ? F14 C53 F15 107.8(4) . . ? F13 C53 F15 104.7(4) . . ? F14 C53 C49 112.8(5) . . ? F13 C53 C49 113.3(4) . . ? F15 C53 C49 113.0(5) . . ? F18A C54 F16A 111.7(6) . . ? F18A C54 F17A 104.9(7) . . ? F16A C54 F17A 105.0(6) . . ? F18A C54 F18B 57.9(6) . . ? F16A C54 F18B 57.1(6) . . ? F17A C54 F18B 134.1(7) . . ? F18A C54 F16B 124.4(7) . . ? F16A C54 F16B 68.9(6) . . ? F18B C54 F16B 113.9(7) . . ? F16A C54 F17B 134.3(7) . . ? F17A C54 F17B 67.5(6) . . ? F18B C54 F17B 94.7(7) . . ? F16B C54 F17B 97.5(7) . . ? F18A C54 C51 113.4(6) . . ? F16A C54 C51 110.6(5) . . ? F17A C54 C51 110.7(5) . . ? F18B C54 C51 115.1(6) . . ? F16B C54 C51 117.7(6) . . ? F17B C54 C51 114.1(6) . . ? C60 C55 C56 115.6(4) . . ? C60 C55 B1 120.2(4) . . ? C56 C55 B1 124.1(4) . . ? C57 C56 C55 122.3(4) . . ? C57 C56 H56 118.6 . . ? C55 C56 H56 119.1 . . ? C58 C57 C56 120.9(5) . . ? C58 C57 C62 118.8(5) . . ? C56 C57 C62 120.2(5) . . ? C57 C58 C59 118.2(5) . . ? C57 C58 H58 121.0 . . ? C59 C58 H58 120.9 . . ? C60 C59 C58 120.0(4) . . ? C60 C59 C61 119.5(4) . . ? C58 C59 C61 120.4(5) . . ? C59 C60 C55 122.9(4) . . ? C59 C60 H60 118.2 . . ? C55 C60 H60 118.9 . . ? F23 C61 F22 105.7(4) . . ? F23 C61 F24 106.5(4) . . ? F22 C61 F24 105.0(5) . . ? F23 C61 C59 114.2(5) . . ? F22 C61 C59 112.1(4) . . ? F24 C61 C59 112.6(4) . . ? F21A C62 F19B 122.4(7) . . ? F21A C62 F20B 77.4(6) . . ? F19B C62 F20B 105.3(6) . . ? F21A C62 F19A 107.9(7) . . ? F20B C62 F19A 127.4(6) . . ? F21A C62 F20A 104.9(7) . . ? F19B C62 F20A 79.5(6) . . ? F19A C62 F20A 105.5(7) . . ? F19B C62 F21B 109.6(6) . . ? F20B C62 F21B 101.6(6) . . ? F19A C62 F21B 88.3(6) . . ? F20A C62 F21B 126.4(7) . . ? F21A C62 C57 115.6(6) . . ? F19B C62 C57 115.7(5) . . ? F20B C62 C57 112.0(5) . . ? F19A C62 C57 111.7(5) . . ? F20A C62 C57 110.5(6) . . ? F21B C62 C57 111.5(5) . . ? C31 B1 C39 111.9(4) . . ? C31 B1 C47 104.4(4) . . ? C39 B1 C47 113.5(4) . . ? C31 B1 C55 110.6(4) . . ? C39 B1 C55 104.5(4) . . ? C47 B1 C55 112.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 P1 O1 170.82(18) . . . . ? N1 Pd1 P1 O1 -3.49(16) . . . . ? C4 Pd1 P1 O1 143.6(7) . . . . ? C3 Pd1 P1 O1 -143.4(2) . . . . ? C1 Pd1 P1 C28 -80.2(2) . . . . ? N1 Pd1 P1 C28 105.5(2) . . . . ? C4 Pd1 P1 C28 -107.4(7) . . . . ? C3 Pd1 P1 C28 -34.4(3) . . . . ? C1 Pd1 P1 C25 58.7(3) . . . . ? N1 Pd1 P1 C25 -115.6(2) . . . . ? C4 Pd1 P1 C25 31.5(7) . . . . ? C3 Pd1 P1 C25 104.5(3) . . . . ? C28 P1 O1 C23 -120.3(4) . . . . ? C25 P1 O1 C23 127.9(4) . . . . ? Pd1 P1 O1 C23 1.1(3) . . . . ? P1 Pd1 N1 C23 6.5(3) . . . . ? C4 Pd1 N1 C23 -167.6(3) . . . . ? C3 Pd1 N1 C23 160.6(3) . . . . ? P1 Pd1 N1 C11 173.4(4) . . . . ? C4 Pd1 N1 C11 -0.7(4) . . . . ? C3 Pd1 N1 C11 -32.5(4) . . . . ? P1 Pd1 C1 C2 137.5(3) . . . . ? C4 Pd1 C1 C2 -47.3(3) . . . . ? C3 Pd1 C1 C2 -15.7(3) . . . . ? Pd1 C1 C2 C9 -96.4(4) . . . . ? Pd1 C1 C2 C3 24.1(4) . . . . ? Pd1 C1 C2 C10 142.8(3) . . . . ? C9 C2 C3 C4 165.3(4) . . . . ? C1 C2 C3 C4 46.2(5) . . . . ? C10 C2 C3 C4 -72.7(5) . . . . ? C9 C2 C3 C8 -16.5(6) . . . . ? C1 C2 C3 C8 -135.6(5) . . . . ? C10 C2 C3 C8 105.5(5) . . . . ? C9 C2 C3 Pd1 99.8(3) . . . . ? C1 C2 C3 Pd1 -19.3(3) . . . . ? C10 C2 C3 Pd1 -138.2(3) . . . . ? C1 Pd1 C3 C4 -108.9(3) . . . . ? P1 Pd1 C3 C4 -161.5(2) . . . . ? N1 Pd1 C3 C4 68.2(3) . . . . ? C1 Pd1 C3 C8 138.7(4) . . . . ? P1 Pd1 C3 C8 86.1(4) . . . . ? N1 Pd1 C3 C8 -44.2(4) . . . . ? C4 Pd1 C3 C8 -112.4(5) . . . . ? C1 Pd1 C3 C2 15.4(3) . . . . ? P1 Pd1 C3 C2 -37.2(4) . . . . ? N1 Pd1 C3 C2 -167.5(2) . . . . ? C4 Pd1 C3 C2 124.3(4) . . . . ? C8 C3 C4 C5 -2.0(7) . . . . ? C2 C3 C4 C5 176.3(4) . . . . ? Pd1 C3 C4 C5 -112.1(4) . . . . ? C8 C3 C4 Pd1 110.1(4) . . . . ? C2 C3 C4 Pd1 -71.6(4) . . . . ? C1 Pd1 C4 C3 60.6(3) . . . . ? P1 Pd1 C4 C3 88.4(7) . . . . ? N1 Pd1 C4 C3 -125.8(3) . . . . ? C1 Pd1 C4 C5 177.7(4) . . . . ? P1 Pd1 C4 C5 -154.4(5) . . . . ? N1 Pd1 C4 C5 -8.6(4) . . . . ? C3 Pd1 C4 C5 117.2(5) . . . . ? C3 C4 C5 C6 0.4(7) . . . . ? Pd1 C4 C5 C6 -87.0(5) . . . . ? C4 C5 C6 C7 0.6(8) . . . . ? C5 C6 C7 C8 0.1(8) . . . . ? C6 C7 C8 C3 -1.8(8) . . . . ? C4 C3 C8 C7 2.7(7) . . . . ? C2 C3 C8 C7 -175.5(5) . . . . ? Pd1 C3 C8 C7 85.2(6) . . . . ? C23 N1 C11 C12 84.0(6) . . . . ? Pd1 N1 C11 C12 -82.6(5) . . . . ? C23 N1 C11 C16 -100.6(5) . . . . ? Pd1 N1 C11 C16 92.9(5) . . . . ? C16 C11 C12 C13 3.0(7) . . . . ? N1 C11 C12 C13 178.2(4) . . . . ? C16 C11 C12 C17 -174.7(5) . . . . ? N1 C11 C12 C17 0.5(7) . . . . ? C11 C12 C13 C14 -1.7(8) . . . . ? C17 C12 C13 C14 176.1(5) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C16 1.2(8) . . . . ? C14 C15 C16 C11 0.0(7) . . . . ? C14 C15 C16 C20 -179.7(5) . . . . ? C12 C11 C16 C15 -2.1(7) . . . . ? N1 C11 C16 C15 -177.3(4) . . . . ? C12 C11 C16 C20 177.6(5) . . . . ? N1 C11 C16 C20 2.4(7) . . . . ? C13 C12 C17 C19 68.2(8) . . . . ? C11 C12 C17 C19 -114.2(7) . . . . ? C13 C12 C17 C18 -51.8(7) . . . . ? C11 C12 C17 C18 125.9(6) . . . . ? C15 C16 C20 C21 -103.9(6) . . . . ? C11 C16 C20 C21 76.4(6) . . . . ? C15 C16 C20 C22 19.7(7) . . . . ? C11 C16 C20 C22 -160.0(5) . . . . ? C11 N1 C23 O1 -175.8(4) . . . . ? Pd1 N1 C23 O1 -7.9(6) . . . . ? C11 N1 C23 C24 4.2(7) . . . . ? Pd1 N1 C23 C24 172.0(4) . . . . ? P1 O1 C23 N1 4.6(6) . . . . ? P1 O1 C23 C24 -175.4(3) . . . . ? O1 P1 C25 C27 56.1(4) . . . . ? C28 P1 C25 C27 -49.2(5) . . . . ? Pd1 P1 C25 C27 168.9(3) . . . . ? O1 P1 C25 C26 -68.7(4) . . . . ? C28 P1 C25 C26 -174.0(4) . . . . ? Pd1 P1 C25 C26 44.2(4) . . . . ? O1 P1 C28 C29 68.6(4) . . . . ? C25 P1 C28 C29 174.4(4) . . . . ? Pd1 P1 C28 C29 -41.8(4) . . . . ? O1 P1 C28 C30 -165.9(4) . . . . ? C25 P1 C28 C30 -60.1(4) . . . . ? Pd1 P1 C28 C30 83.8(4) . . . . ? C36 C31 C32 C33 0.4(6) . . . . ? B1 C31 C32 C33 175.5(4) . . . . ? C31 C32 C33 C34 0.4(7) . . . . ? C31 C32 C33 C37 -178.0(4) . . . . ? C32 C33 C34 C35 -0.5(7) . . . . ? C37 C33 C34 C35 177.9(4) . . . . ? C33 C34 C35 C36 -0.3(7) . . . . ? C33 C34 C35 C38 -179.8(4) . . . . ? C34 C35 C36 C31 1.2(7) . . . . ? C38 C35 C36 C31 -179.3(4) . . . . ? C32 C31 C36 C35 -1.2(6) . . . . ? B1 C31 C36 C35 -176.3(4) . . . . ? C34 C33 C37 F6 128.3(5) . . . . ? C32 C33 C37 F6 -53.3(6) . . . . ? C34 C33 C37 F5 -112.0(5) . . . . ? C32 C33 C37 F5 66.4(6) . . . . ? C34 C33 C37 F4 6.7(6) . . . . ? C32 C33 C37 F4 -174.9(4) . . . . ? C34 C35 C38 F2 -8.1(6) . . . . ? C36 C35 C38 F2 172.4(4) . . . . ? C34 C35 C38 F1 -129.1(5) . . . . ? C36 C35 C38 F1 51.3(6) . . . . ? C34 C35 C38 F3 112.7(5) . . . . ? C36 C35 C38 F3 -66.8(6) . . . . ? C44 C39 C40 C41 -1.7(7) . . . . ? B1 C39 C40 C41 -174.9(4) . . . . ? C39 C40 C41 C42 0.7(7) . . . . ? C39 C40 C41 C45 177.7(4) . . . . ? C40 C41 C42 C43 0.4(7) . . . . ? C45 C41 C42 C43 -176.6(4) . . . . ? C41 C42 C43 C44 -0.4(7) . . . . ? C41 C42 C43 C46 179.8(4) . . . . ? C42 C43 C44 C39 -0.7(7) . . . . ? C46 C43 C44 C39 179.1(4) . . . . ? C40 C39 C44 C43 1.7(7) . . . . ? B1 C39 C44 C43 174.8(4) . . . . ? C42 C41 C45 F8A 86.3(6) . . . . ? C40 C41 C45 F8A -90.8(6) . . . . ? C42 C41 C45 F9A -29.7(7) . . . . ? C40 C41 C45 F9A 153.2(5) . . . . ? C42 C41 C45 F7A -151.6(5) . . . . ? C40 C41 C45 F7A 31.3(6) . . . . ? C42 C41 C45 F9B -54.6(8) . . . . ? C40 C41 C45 F9B 128.3(7) . . . . ? C42 C41 C45 F7B 118.1(8) . . . . ? C40 C41 C45 F7B -58.9(8) . . . . ? C42 C41 C45 F8B 31.9(8) . . . . ? C40 C41 C45 F8B -145.1(7) . . . . ? C42 C43 C46 F10B -132.4(6) . . . . ? C44 C43 C46 F10B 47.9(7) . . . . ? C42 C43 C46 F11B 105.5(6) . . . . ? C44 C43 C46 F11B -74.3(7) . . . . ? C42 C43 C46 F12A 80.6(6) . . . . ? C44 C43 C46 F12A -99.1(6) . . . . ? C42 C43 C46 F10A -44.0(7) . . . . ? C44 C43 C46 F10A 136.2(5) . . . . ? C42 C43 C46 F12B -15.6(7) . . . . ? C44 C43 C46 F12B 164.6(6) . . . . ? C42 C43 C46 F11A -159.6(5) . . . . ? C44 C43 C46 F11A 20.7(7) . . . . ? C52 C47 C48 C49 2.6(7) . . . . ? B1 C47 C48 C49 176.4(4) . . . . ? C47 C48 C49 C50 -0.7(7) . . . . ? C47 C48 C49 C53 -179.6(4) . . . . ? C48 C49 C50 C51 -0.8(7) . . . . ? C53 C49 C50 C51 178.1(5) . . . . ? C49 C50 C51 C52 0.2(7) . . . . ? C49 C50 C51 C54 179.2(5) . . . . ? C48 C47 C52 C51 -3.2(7) . . . . ? B1 C47 C52 C51 -177.2(4) . . . . ? C50 C51 C52 C47 1.9(7) . . . . ? C54 C51 C52 C47 -177.2(5) . . . . ? C50 C49 C53 F14 -95.6(6) . . . . ? C48 C49 C53 F14 83.3(6) . . . . ? C50 C49 C53 F13 145.8(5) . . . . ? C48 C49 C53 F13 -35.3(7) . . . . ? C50 C49 C53 F15 26.9(7) . . . . ? C48 C49 C53 F15 -154.2(5) . . . . ? C50 C51 C54 F18A -16.3(8) . . . . ? C52 C51 C54 F18A 162.8(6) . . . . ? C50 C51 C54 F16A 110.1(6) . . . . ? C52 C51 C54 F16A -70.8(7) . . . . ? C50 C51 C54 F17A -133.9(6) . . . . ? C52 C51 C54 F17A 45.1(7) . . . . ? C50 C51 C54 F18B 47.8(8) . . . . ? C52 C51 C54 F18B -133.2(7) . . . . ? C50 C51 C54 F16B -173.5(7) . . . . ? C52 C51 C54 F16B 5.5(9) . . . . ? C50 C51 C54 F17B -60.1(8) . . . . ? C52 C51 C54 F17B 118.9(7) . . . . ? C60 C55 C56 C57 -2.4(6) . . . . ? B1 C55 C56 C57 -177.8(4) . . . . ? C55 C56 C57 C58 1.9(7) . . . . ? C55 C56 C57 C62 -177.1(4) . . . . ? C56 C57 C58 C59 -0.3(7) . . . . ? C62 C57 C58 C59 178.7(5) . . . . ? C57 C58 C59 C60 -0.7(7) . . . . ? C57 C58 C59 C61 178.5(4) . . . . ? C58 C59 C60 C55 0.1(7) . . . . ? C61 C59 C60 C55 -179.1(4) . . . . ? C56 C55 C60 C59 1.3(6) . . . . ? B1 C55 C60 C59 177.0(4) . . . . ? C60 C59 C61 F23 -172.9(4) . . . . ? C58 C59 C61 F23 7.9(7) . . . . ? C60 C59 C61 F22 66.9(6) . . . . ? C58 C59 C61 F22 -112.3(5) . . . . ? C60 C59 C61 F24 -51.2(6) . . . . ? C58 C59 C61 F24 129.5(5) . . . . ? C58 C57 C62 F21A 173.6(6) . . . . ? C56 C57 C62 F21A -7.4(8) . . . . ? C58 C57 C62 F19B 20.4(8) . . . . ? C56 C57 C62 F19B -160.5(6) . . . . ? C58 C57 C62 F20B -100.3(7) . . . . ? C56 C57 C62 F20B 78.7(7) . . . . ? C58 C57 C62 F19A 49.6(7) . . . . ? C56 C57 C62 F19A -131.3(6) . . . . ? C58 C57 C62 F20A -67.5(7) . . . . ? C56 C57 C62 F20A 111.6(7) . . . . ? C58 C57 C62 F21B 146.6(6) . . . . ? C56 C57 C62 F21B -34.3(7) . . . . ? C32 C31 B1 C39 149.4(4) . . . . ? C36 C31 B1 C39 -35.8(6) . . . . ? C32 C31 B1 C47 -87.4(5) . . . . ? C36 C31 B1 C47 87.3(5) . . . . ? C32 C31 B1 C55 33.3(6) . . . . ? C36 C31 B1 C55 -151.9(4) . . . . ? C40 C39 B1 C31 -34.5(6) . . . . ? C44 C39 B1 C31 152.8(4) . . . . ? C40 C39 B1 C47 -152.3(4) . . . . ? C44 C39 B1 C47 35.0(6) . . . . ? C40 C39 B1 C55 85.2(5) . . . . ? C44 C39 B1 C55 -87.5(5) . . . . ? C52 C47 B1 C31 80.5(5) . . . . ? C48 C47 B1 C31 -93.1(5) . . . . ? C52 C47 B1 C39 -157.5(4) . . . . ? C48 C47 B1 C39 29.0(6) . . . . ? C52 C47 B1 C55 -39.3(6) . . . . ? C48 C47 B1 C55 147.2(4) . . . . ? C60 C55 B1 C31 42.9(5) . . . . ? C56 C55 B1 C31 -141.9(4) . . . . ? C60 C55 B1 C39 -77.7(5) . . . . ? C56 C55 B1 C39 97.6(5) . . . . ? C60 C55 B1 C47 158.9(4) . . . . ? C56 C55 B1 C47 -25.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 64.05 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.621 _refine_diff_density_min -0.919 _refine_diff_density_rms 0.127 data_7a _database_code_depnum_ccdc_archive 'CCDC 876282' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C32 H50 N2 Ni O P' _chemical_formula_sum 'C64 H62 B F24 N2 Ni O P' _chemical_formula_weight 1431.65 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.26610(10) _cell_length_b 20.4994(2) _cell_length_c 27.7574(3) _cell_angle_alpha 103.1860(10) _cell_angle_beta 92.1610(9) _cell_angle_gamma 102.9160(10) _cell_volume 6594.59(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9137 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 33.05 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8506 _exptl_absorpt_correction_T_max 0.8821 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57638 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.25 _reflns_number_total 23856 _reflns_number_gt 20545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+1.2921P] 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 23856 _refine_ls_number_parameters 1717 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1686 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.482 _refine_ls_shift/su_max 0.000 _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 0.83875(3) 0.211912(18) 0.849553(13) 0.017 Uani 1 1 d . . . P1 P 0.84695(7) 0.28534(4) 0.80775(3) 0.019 Uani 1 1 d . . . O1 O 0.8080(2) 0.35015(11) 0.84679(8) 0.025 Uani 1 1 d . . . N1 N 0.7902(2) 0.28135(13) 0.90101(9) 0.020 Uani 1 1 d . . . N2 N 0.8355(2) 0.15211(13) 0.89261(9) 0.022 Uani 1 1 d . . . C1 C 0.7630(3) 0.27043(15) 0.94928(11) 0.020 Uani 1 1 d . . . C2 C 0.8512(3) 0.28473(16) 0.98628(11) 0.023 Uani 1 1 d . . . C3 C 0.8237(3) 0.27452(17) 1.03286(11) 0.025 Uani 1 1 d . . . H3 H 0.8816 0.2854 1.0592 0.030 Uiso 1 1 calc R . . C4 C 0.7138(3) 0.24892(17) 1.04133(11) 0.025 Uani 1 1 d . . . H4 H 0.6965 0.2430 1.0734 0.030 Uiso 1 1 calc R . . C5 C 0.6290(3) 0.23189(16) 1.00322(12) 0.023 Uani 1 1 d . . . H5 H 0.5539 0.2137 1.0093 0.028 Uiso 1 1 calc R . . C6 C 0.6517(3) 0.24098(15) 0.95604(11) 0.022 Uani 1 1 d . . . C7 C 0.9730(3) 0.31013(18) 0.97651(12) 0.029 Uani 1 1 d . . . H7 H 0.9774 0.2952 0.9399 0.035 Uiso 1 1 calc R . . C8 C 1.0112(3) 0.3885(2) 0.99135(18) 0.048 Uani 1 1 d . . . H8A H 0.9624 0.4082 0.9729 0.072 Uiso 1 1 calc R . . H8B H 1.0889 0.4028 0.9836 0.072 Uiso 1 1 calc R . . H8C H 1.0069 0.4049 1.0271 0.072 Uiso 1 1 calc R . . C9 C 1.0534(3) 0.2782(2) 1.00201(14) 0.038 Uani 1 1 d . . . H9A H 1.1269 0.2875 0.9889 0.057 Uiso 1 1 calc R . . H9B H 1.0230 0.2283 0.9956 0.057 Uiso 1 1 calc R . . H9C H 1.0618 0.2985 1.0379 0.057 Uiso 1 1 calc R . . C10 C 0.5572(3) 0.21777(17) 0.91426(12) 0.025 Uani 1 1 d . . . H10 H 0.5887 0.2298 0.8838 0.030 Uiso 1 1 calc R . . C11 C 0.5122(3) 0.13961(18) 0.90277(14) 0.036 Uani 1 1 d . . . H11A H 0.5738 0.1170 0.8944 0.054 Uiso 1 1 calc R . . H11B H 0.4544 0.1249 0.8746 0.054 Uiso 1 1 calc R . . H11C H 0.4794 0.1267 0.9319 0.054 Uiso 1 1 calc R . . C12 C 0.4635(3) 0.2549(2) 0.92697(15) 0.039 Uani 1 1 d . . . H12A H 0.4332 0.2452 0.9574 0.059 Uiso 1 1 calc R . . H12B H 0.4036 0.2386 0.8996 0.059 Uiso 1 1 calc R . . H12C H 0.4935 0.3047 0.9320 0.059 Uiso 1 1 calc R . . C13 C 0.7809(3) 0.33826(16) 0.89142(11) 0.023 Uani 1 1 d . . . C14 C 0.7426(3) 0.39622(18) 0.92325(13) 0.034 Uani 1 1 d . . . H14A H 0.7346 0.3885 0.9566 0.050 Uiso 1 1 calc R . . H14B H 0.6699 0.3987 0.9088 0.050 Uiso 1 1 calc R . . H14C H 0.7979 0.4397 0.9253 0.050 Uiso 1 1 calc R . . C15 C 0.9822(3) 0.33324(17) 0.79456(12) 0.027 Uani 1 1 d . . . H15 H 0.9713 0.3770 0.7873 0.033 Uiso 1 1 calc R . . C16 C 1.0653(3) 0.3524(2) 0.84124(14) 0.039 Uani 1 1 d . . . H16A H 1.0752 0.3103 0.8500 0.058 Uiso 1 1 calc R . . H16B H 1.0358 0.3804 0.8689 0.058 Uiso 1 1 calc R . . H16C H 1.1378 0.3789 0.8347 0.058 Uiso 1 1 calc R . . C17 C 1.0292(3) 0.29387(19) 0.74942(13) 0.032 Uani 1 1 d . . . H17A H 1.0963 0.3241 0.7414 0.049 Uiso 1 1 calc R . . H17B H 0.9722 0.2789 0.7209 0.049 Uiso 1 1 calc R . . H17C H 1.0491 0.2534 0.7571 0.049 Uiso 1 1 calc R . . C18 C 0.7441(3) 0.26913(18) 0.75466(12) 0.028 Uani 1 1 d . . . H18 H 0.7584 0.2303 0.7284 0.033 Uiso 1 1 calc R . . C19 C 0.6264(3) 0.2450(2) 0.77113(13) 0.034 Uani 1 1 d . . . H19A H 0.6098 0.2824 0.7965 0.051 Uiso 1 1 calc R . . H19B H 0.6243 0.2048 0.7850 0.051 Uiso 1 1 calc R . . H19C H 0.5703 0.2323 0.7424 0.051 Uiso 1 1 calc R . . C20 C 0.7506(4) 0.3309(2) 0.73189(15) 0.042 Uani 1 1 d . . . H20A H 0.6922 0.3190 0.7041 0.063 Uiso 1 1 calc R . . H20B H 0.8246 0.3432 0.7198 0.063 Uiso 1 1 calc R . . H20C H 0.7391 0.3702 0.7571 0.063 Uiso 1 1 calc R . . C21 C 0.8895(3) 0.15191(15) 0.79322(11) 0.024 Uani 1 1 d . . . H21A H 0.8833 0.1710 0.7638 0.028 Uiso 1 1 calc R . . H21B H 0.9702 0.1551 0.8011 0.028 Uiso 1 1 calc R . . C22 C 0.8283(3) 0.07434(16) 0.77816(12) 0.025 Uani 1 1 d . . . C23 C 0.7013(3) 0.06779(18) 0.77129(15) 0.039 Uani 1 1 d . . . H23A H 0.6628 0.0193 0.7573 0.058 Uiso 1 1 calc R . . H23B H 0.6857 0.0956 0.7486 0.058 Uiso 1 1 calc R . . H23C H 0.6742 0.0843 0.8035 0.058 Uiso 1 1 calc R . . C24 C 0.8665(4) 0.04273(18) 0.72711(12) 0.041 Uani 1 1 d . . . H24A H 0.9483 0.0492 0.7301 0.061 Uiso 1 1 calc R . . H24B H 0.8448 0.0657 0.7023 0.061 Uiso 1 1 calc R . . H24C H 0.8306 -0.0067 0.7168 0.061 Uiso 1 1 calc R . . C25 C 0.8598(3) 0.03389(14) 0.81431(11) 0.020 Uani 1 1 d . . . C26 C 0.7797(3) -0.01366(16) 0.83118(12) 0.025 Uani 1 1 d . . . H26 H 0.7026 -0.0212 0.8202 0.030 Uiso 1 1 calc R . . C27 C 0.8108(3) -0.05013(16) 0.86374(12) 0.030 Uani 1 1 d . . . H27 H 0.7549 -0.0823 0.8747 0.036 Uiso 1 1 calc R . . C28 C 0.9224(3) -0.04005(17) 0.88031(12) 0.028 Uani 1 1 d . . . H28 H 0.9434 -0.0643 0.9031 0.033 Uiso 1 1 calc R . . C29 C 1.0031(3) 0.00583(17) 0.86321(12) 0.027 Uani 1 1 d . . . H29 H 1.0801 0.0127 0.8740 0.032 Uiso 1 1 calc R . . C30 C 0.9723(3) 0.04186(16) 0.83033(11) 0.023 Uani 1 1 d . . . H30 H 1.0289 0.0726 0.8185 0.027 Uiso 1 1 calc R . . C31 C 0.8296(3) 0.12513(16) 0.92451(11) 0.024 Uani 1 1 d . . . C32 C 0.8200(4) 0.09175(18) 0.96569(13) 0.035 Uani 1 1 d . . . H32A H 0.7979 0.1219 0.9945 0.052 Uiso 1 1 calc R . . H32B H 0.8926 0.0829 0.9744 0.052 Uiso 1 1 calc R . . H32C H 0.7631 0.0480 0.9559 0.052 Uiso 1 1 calc R . . Ni2 Ni 0.86658(4) 0.25222(2) 0.355916(14) 0.026 Uani 1 1 d . . . P2 P 0.96462(8) 0.30127(4) 0.30922(3) 0.025 Uani 1 1 d . . . O2 O 1.01531(19) 0.23719(11) 0.27544(8) 0.024 Uani 1 1 d . . . N3 N 0.9169(2) 0.16948(13) 0.32099(9) 0.023 Uani 1 1 d . . . N4 N 0.7588(3) 0.19856(15) 0.38713(11) 0.036 Uani 1 1 d . . . C33 C 0.8825(3) 0.10304(17) 0.33245(12) 0.027 Uani 1 1 d . . . C34 C 0.9277(3) 0.09526(19) 0.37735(13) 0.034 Uani 1 1 d . . . C35 C 0.8927(4) 0.0312(2) 0.38853(15) 0.042 Uani 1 1 d . . . H35 H 0.9237 0.0238 0.4182 0.051 Uiso 1 1 calc R . . C36 C 0.8136(4) -0.02168(19) 0.35717(15) 0.041 Uani 1 1 d . . . H36 H 0.7909 -0.0650 0.3652 0.049 Uiso 1 1 calc R . . C37 C 0.7676(3) -0.01153(19) 0.31406(15) 0.039 Uani 1 1 d . . . H37 H 0.7124 -0.0480 0.2930 0.046 Uiso 1 1 calc R . . C38 C 0.8002(3) 0.05101(17) 0.30078(13) 0.030 Uani 1 1 d . . . C39 C 1.0133(4) 0.1549(2) 0.41211(14) 0.043 Uani 1 1 d . . . H39 H 1.0023 0.1986 0.4047 0.052 Uiso 1 1 calc R . . C40 C 0.9970(5) 0.1598(3) 0.46689(16) 0.057 Uani 1 1 d . . . H40A H 1.0100 0.1184 0.4758 0.086 Uiso 1 1 calc R . . H40B H 0.9202 0.1636 0.4729 0.086 Uiso 1 1 calc R . . H40C H 1.0505 0.2007 0.4872 0.086 Uiso 1 1 calc R . . C41 C 1.1321(4) 0.1503(3) 0.40160(17) 0.064 Uani 1 1 d . . . H41A H 1.1436 0.1059 0.4056 0.095 Uiso 1 1 calc R . . H41B H 1.1857 0.1880 0.4249 0.095 Uiso 1 1 calc R . . H41C H 1.1438 0.1538 0.3675 0.095 Uiso 1 1 calc R . . C42 C 0.7451(4) 0.06232(18) 0.25393(15) 0.039 Uani 1 1 d . . . H42 H 0.7984 0.1020 0.2456 0.047 Uiso 1 1 calc R . . C43 C 0.6404(5) 0.0852(4) 0.2636(2) 0.083 Uani 1 1 d . . . H43A H 0.6155 0.1007 0.2351 0.125 Uiso 1 1 calc R . . H43B H 0.6541 0.1234 0.2934 0.125 Uiso 1 1 calc R . . H43C H 0.5821 0.0467 0.2687 0.125 Uiso 1 1 calc R . . C44 C 0.7310(5) 0.0035(3) 0.20923(18) 0.067 Uani 1 1 d . . . H44A H 0.6730 -0.0356 0.2137 0.100 Uiso 1 1 calc R . . H44B H 0.8023 -0.0103 0.2050 0.100 Uiso 1 1 calc R . . H44C H 0.7086 0.0177 0.1797 0.100 Uiso 1 1 calc R . . C45 C 0.9866(3) 0.17615(16) 0.28786(11) 0.023 Uani 1 1 d . . . C46 C 1.0441(3) 0.12426(17) 0.26037(12) 0.027 Uani 1 1 d . . . H46A H 1.0252 0.0824 0.2727 0.040 Uiso 1 1 calc R . . H46B H 1.1256 0.1433 0.2655 0.040 Uiso 1 1 calc R . . H46C H 1.0195 0.1130 0.2248 0.040 Uiso 1 1 calc R . . C47 C 1.0963(3) 0.36671(17) 0.32820(12) 0.033 Uani 1 1 d . . . H47 H 1.0783 0.4106 0.3461 0.039 Uiso 1 1 calc R . . C48 C 1.1599(4) 0.3806(2) 0.28357(14) 0.041 Uani 1 1 d . . . H48A H 1.2314 0.4143 0.2955 0.062 Uiso 1 1 calc R . . H48B H 1.1144 0.3989 0.2625 0.062 Uiso 1 1 calc R . . H48C H 1.1743 0.3375 0.2643 0.062 Uiso 1 1 calc R . . C49 C 1.1686(4) 0.3440(2) 0.36446(14) 0.042 Uani 1 1 d . . . H49A H 1.1869 0.3008 0.3476 0.063 Uiso 1 1 calc R . . H49B H 1.1270 0.3369 0.3930 0.063 Uiso 1 1 calc R . . H49C H 1.2381 0.3798 0.3759 0.063 Uiso 1 1 calc R . . C50 C 0.8867(3) 0.32246(17) 0.25959(12) 0.029 Uani 1 1 d . . . H50 H 0.9316 0.3184 0.2302 0.035 Uiso 1 1 calc R . . C51 C 0.8705(4) 0.3963(2) 0.27302(14) 0.042 Uani 1 1 d . . . H51A H 0.8369 0.4063 0.2437 0.062 Uiso 1 1 calc R . . H51B H 0.9435 0.4289 0.2841 0.062 Uiso 1 1 calc R . . H51C H 0.8207 0.4009 0.2998 0.062 Uiso 1 1 calc R . . C52 C 0.7742(3) 0.2694(2) 0.24405(13) 0.036 Uani 1 1 d . . . H52A H 0.7275 0.2723 0.2720 0.054 Uiso 1 1 calc R . . H52B H 0.7876 0.2230 0.2344 0.054 Uiso 1 1 calc R . . H52C H 0.7356 0.2789 0.2158 0.054 Uiso 1 1 calc R . . C53 C 0.8316(4) 0.34129(19) 0.38522(13) 0.039 Uani 1 1 d . . . H53A H 0.8854 0.3779 0.3745 0.047 Uiso 1 1 calc R . . H53B H 0.7557 0.3402 0.3712 0.047 Uiso 1 1 calc R . . C54 C 0.8350(4) 0.36219(19) 0.44301(13) 0.037 Uani 1 1 d . . . C55 C 0.9490(4) 0.3602(2) 0.46524(15) 0.050 Uani 1 1 d . . . H55A H 0.9545 0.3774 0.5014 0.075 Uiso 1 1 calc R . . H55B H 1.0084 0.3894 0.4516 0.075 Uiso 1 1 calc R . . H55C H 0.9576 0.3127 0.4570 0.075 Uiso 1 1 calc R . . C56 C 0.8233(5) 0.4379(2) 0.45730(17) 0.058 Uani 1 1 d . . . H56A H 0.7503 0.4403 0.4431 0.088 Uiso 1 1 calc R . . H56B H 0.8835 0.4672 0.4442 0.088 Uiso 1 1 calc R . . H56C H 0.8287 0.4540 0.4936 0.088 Uiso 1 1 calc R . . C57 C 0.7359(3) 0.31812(18) 0.46202(12) 0.030 Uani 1 1 d . . . C58 C 0.7497(3) 0.28633(19) 0.50028(13) 0.033 Uani 1 1 d . . . H58 H 0.8231 0.2917 0.5153 0.040 Uiso 1 1 calc R . . C59 C 0.6584(4) 0.2469(2) 0.51686(15) 0.044 Uani 1 1 d . . . H59 H 0.6697 0.2264 0.5435 0.053 Uiso 1 1 calc R . . C60 C 0.5520(4) 0.2374(2) 0.49512(16) 0.047 Uani 1 1 d . . . H60 H 0.4897 0.2096 0.5061 0.057 Uiso 1 1 calc R . . C61 C 0.5367(4) 0.2689(2) 0.45672(17) 0.051 Uani 1 1 d . . . H61 H 0.4635 0.2625 0.4412 0.061 Uiso 1 1 calc R . . C62 C 0.6275(4) 0.3094(2) 0.44132(13) 0.040 Uani 1 1 d . . . H62 H 0.6155 0.3319 0.4159 0.048 Uiso 1 1 calc R . . C63 C 0.6966(4) 0.1562(2) 0.39845(16) 0.049 Uani 1 1 d . . . C64 C 0.6196(6) 0.0996(2) 0.4122(2) 0.085 Uani 1 1 d . . . H64A H 0.5431 0.1065 0.4106 0.127 Uiso 1 1 calc R . . H64B H 0.6423 0.0983 0.4462 0.127 Uiso 1 1 calc R . . H64C H 0.6215 0.0559 0.3892 0.127 Uiso 1 1 calc R . . B1 B 0.3274(3) 0.27070(17) 0.63198(12) 0.018 Uani 1 1 d . . . C65 C 0.3517(2) 0.28983(15) 0.69288(11) 0.018 Uani 1 1 d . . . C66 C 0.3031(2) 0.24036(15) 0.71823(11) 0.019 Uani 1 1 d . . . H66 H 0.2627 0.1961 0.6995 0.023 Uiso 1 1 calc R . . C67 C 0.3119(3) 0.25379(16) 0.76967(11) 0.022 Uani 1 1 d . . . C68 C 0.3713(3) 0.31748(17) 0.79851(11) 0.023 Uani 1 1 d . . . H68 H 0.3782 0.3266 0.8338 0.028 Uiso 1 1 calc R . . C69 C 0.4199(3) 0.36699(16) 0.77452(12) 0.025 Uani 1 1 d . . . C70 C 0.4095(3) 0.35359(15) 0.72262(11) 0.020 Uani 1 1 d . . . H70 H 0.4428 0.3891 0.7072 0.024 Uiso 1 1 calc R . . C71 C 0.2620(3) 0.19831(18) 0.79479(12) 0.028 Uani 1 1 d . . . C72 C 0.4840(3) 0.43593(18) 0.80478(12) 0.034 Uani 1 1 d . . . C73 C 0.1962(2) 0.27345(15) 0.62340(10) 0.019 Uani 1 1 d . . . C74 C 0.1042(3) 0.21686(16) 0.61281(11) 0.021 Uani 1 1 d . . . H74 H 0.1168 0.1719 0.6081 0.025 Uiso 1 1 calc R . . C75 C -0.0059(3) 0.22426(17) 0.60890(11) 0.023 Uani 1 1 d . . . C76 C -0.0282(3) 0.28901(17) 0.61564(11) 0.023 Uani 1 1 d . . . H76 H -0.1030 0.2941 0.6122 0.028 Uiso 1 1 calc R . . C77 C 0.0628(3) 0.34662(16) 0.62761(11) 0.022 Uani 1 1 d . . . C78 C 0.1716(2) 0.33865(16) 0.63144(11) 0.021 Uani 1 1 d . . . H78 H 0.2319 0.3787 0.6398 0.025 Uiso 1 1 calc R . . C79 C -0.1011(3) 0.16227(18) 0.60022(14) 0.032 Uani 1 1 d . . . C80 C 0.0420(3) 0.41765(17) 0.63652(13) 0.028 Uani 1 1 d . . . C81 C 0.3539(2) 0.19547(15) 0.60786(11) 0.020 Uani 1 1 d . . . C82 C 0.3044(3) 0.15291(15) 0.56183(11) 0.023 Uani 1 1 d . . . H82 H 0.2474 0.1657 0.5446 0.028 Uiso 1 1 calc R . . C83 C 0.3363(3) 0.09216(16) 0.54046(12) 0.028 Uani 1 1 d . . . C84 C 0.4203(3) 0.07203(16) 0.56451(12) 0.027 Uani 1 1 d . . . H84 H 0.4426 0.0310 0.5499 0.033 Uiso 1 1 calc R . . C85 C 0.4701(3) 0.11300(17) 0.60994(13) 0.027 Uani 1 1 d . . . C86 C 0.4368(3) 0.17325(16) 0.63110(12) 0.023 Uani 1 1 d . . . H86 H 0.4721 0.2003 0.6626 0.027 Uiso 1 1 calc R . . C87 C 0.2819(4) 0.0484(2) 0.49132(14) 0.041 Uani 1 1 d . . . C88 C 0.5555(3) 0.09151(19) 0.63900(16) 0.039 Uani 1 1 d . . . C89 C 0.4065(2) 0.32423(14) 0.60471(11) 0.018 Uani 1 1 d . . . C90 C 0.3656(2) 0.34167(15) 0.56272(11) 0.020 Uani 1 1 d . . . H90 H 0.2887 0.3236 0.5507 0.024 Uiso 1 1 calc R . . C91 C 0.4340(3) 0.38453(16) 0.53804(11) 0.022 Uani 1 1 d . . . C92 C 0.5465(3) 0.41280(15) 0.55424(12) 0.023 Uani 1 1 d . . . H92 H 0.5928 0.4428 0.5377 0.027 Uiso 1 1 calc R . . C93 C 0.5890(3) 0.39572(15) 0.59542(11) 0.021 Uani 1 1 d . . . C94 C 0.5208(2) 0.35189(15) 0.61966(11) 0.019 Uani 1 1 d . . . H94 H 0.5531 0.3404 0.6473 0.022 Uiso 1 1 calc R . . C95 C 0.3828(3) 0.40020(19) 0.49325(13) 0.031 Uani 1 1 d . . . C96 C 0.7097(3) 0.42263(16) 0.61512(12) 0.025 Uani 1 1 d . . . F1 F 0.4237(3) 0.48206(15) 0.81085(14) 0.083 Uani 1 1 d U . . F2 F 0.5686(2) 0.46652(15) 0.78218(11) 0.066 Uani 1 1 d U . . F3 F 0.5248(4) 0.43554(18) 0.84782(13) 0.106 Uani 1 1 d U . . F4 F 0.22092(19) 0.22217(12) 0.83747(8) 0.041 Uani 1 1 d U . . F5 F 0.33884(19) 0.16523(11) 0.80634(8) 0.041 Uani 1 1 d U . . F6 F 0.17780(17) 0.14946(11) 0.76625(8) 0.036 Uani 1 1 d U . . F7 F -0.02030(18) 0.43013(11) 0.67501(8) 0.039 Uani 1 1 d U . . F8 F -0.01371(18) 0.42750(11) 0.59764(8) 0.038 Uani 1 1 d U . . F9 F 0.13683(17) 0.46722(11) 0.64681(9) 0.042 Uani 1 1 d U . . F10 F -0.1906(2) 0.16708(13) 0.57484(10) 0.056 Uani 1 1 d U . . F11 F -0.1328(2) 0.14830(14) 0.64292(10) 0.057 Uani 1 1 d U . . F12 F -0.0736(2) 0.10477(13) 0.57512(11) 0.058 Uani 1 1 d U . . F13 F 0.2954(2) -0.01578(12) 0.48303(10) 0.056 Uani 1 1 d U . . F14 F 0.3238(2) 0.07384(14) 0.45351(9) 0.058 Uani 1 1 d U . . F15 F 0.1711(2) 0.04388(13) 0.48644(9) 0.054 Uani 1 1 d U . . F16 F 0.6015(2) 0.04501(14) 0.61099(10) 0.061 Uani 1 1 d U . . F17 F 0.5110(2) 0.06449(15) 0.67548(11) 0.061 Uani 1 1 d U . . F18 F 0.6394(2) 0.14378(13) 0.66142(10) 0.054 Uani 1 1 d U . . F19 F 0.45852(19) 0.42451(12) 0.46448(8) 0.041 Uani 1 1 d U . . F20 F 0.3222(2) 0.44714(13) 0.50536(9) 0.048 Uani 1 1 d U . . F21 F 0.3129(2) 0.34385(12) 0.46397(8) 0.047 Uani 1 1 d U . . F22 F 0.76857(18) 0.46454(12) 0.59028(9) 0.046 Uani 1 1 d U . . F23 F 0.76164(16) 0.37165(10) 0.61499(8) 0.034 Uani 1 1 d U . . F24 F 0.72209(18) 0.45761(12) 0.66312(8) 0.044 Uani 1 1 d U . . B2 B 0.3654(3) 0.28631(17) 0.14000(12) 0.018 Uani 1 1 d . . . C97 C 0.2387(2) 0.30029(15) 0.14301(10) 0.017 Uani 1 1 d . . . C98 C 0.2237(3) 0.36787(15) 0.15144(10) 0.019 Uani 1 1 d . . . H98 H 0.2880 0.4052 0.1558 0.023 Uiso 1 1 calc R . . C99 C 0.1181(3) 0.38189(15) 0.15365(10) 0.020 Uani 1 1 d . . . C100 C 0.0215(3) 0.32847(15) 0.14757(10) 0.019 Uani 1 1 d . . . H100 H -0.0510 0.3377 0.1482 0.023 Uiso 1 1 calc R . . C101 C 0.0348(2) 0.26178(15) 0.14055(10) 0.018 Uani 1 1 d . . . C102 C 0.1412(2) 0.24811(15) 0.13899(10) 0.018 Uani 1 1 d . . . H102 H 0.1476 0.2019 0.1351 0.022 Uiso 1 1 calc R . . C103 C 0.1059(3) 0.45485(16) 0.16151(12) 0.023 Uani 1 1 d . . . C104 C -0.0656(2) 0.20196(16) 0.13248(11) 0.020 Uani 1 1 d . . . C105 C 0.3665(2) 0.21056(15) 0.10427(11) 0.017 Uani 1 1 d . . . C106 C 0.2919(3) 0.18058(15) 0.06144(11) 0.019 Uani 1 1 d . . . H106 H 0.2338 0.2021 0.0550 0.023 Uiso 1 1 calc R . . C107 C 0.3001(3) 0.11992(16) 0.02777(11) 0.023 Uani 1 1 d . . . C108 C 0.3842(3) 0.08741(15) 0.03581(11) 0.022 Uani 1 1 d . . . H108 H 0.3902 0.0463 0.0131 0.027 Uiso 1 1 calc R . . C109 C 0.4597(3) 0.11644(15) 0.07796(12) 0.022 Uani 1 1 d . . . C110 C 0.4512(2) 0.17665(15) 0.11122(11) 0.019 Uani 1 1 d . . . H110 H 0.5044 0.1954 0.1395 0.023 Uiso 1 1 calc R . . C111 C 0.2157(3) 0.09003(16) -0.01633(12) 0.026 Uani 1 1 d . . . C112 C 0.5497(3) 0.08053(16) 0.08681(13) 0.028 Uani 1 1 d . . . C113 C 0.4411(2) 0.33911(14) 0.11084(11) 0.019 Uani 1 1 d . . . C114 C 0.3922(3) 0.35496(15) 0.07027(11) 0.021 Uani 1 1 d . . . H114 H 0.3133 0.3387 0.0623 0.025 Uiso 1 1 calc R . . C115 C 0.4538(3) 0.39368(15) 0.04079(12) 0.023 Uani 1 1 d . . . C116 C 0.5688(3) 0.41847(16) 0.05140(13) 0.026 Uani 1 1 d . . . H116 H 0.6114 0.4453 0.0318 0.031 Uiso 1 1 calc R . . C117 C 0.6200(3) 0.40329(16) 0.09130(13) 0.026 Uani 1 1 d . . . C118 C 0.5577(3) 0.36448(15) 0.12066(12) 0.022 Uani 1 1 d . . . H118 H 0.5953 0.3551 0.1479 0.027 Uiso 1 1 calc R . . C119 C 0.3919(3) 0.40981(17) -0.00063(13) 0.028 Uani 1 1 d . . . C120 C 0.7437(3) 0.43192(18) 0.10504(16) 0.037 Uani 1 1 d . . . C121 C 0.4136(2) 0.29614(15) 0.19778(11) 0.020 Uani 1 1 d . . . C122 C 0.3942(2) 0.24164(16) 0.22130(11) 0.021 Uani 1 1 d . . . H122 H 0.3576 0.1967 0.2024 0.025 Uiso 1 1 calc R . . C123 C 0.4266(3) 0.25093(17) 0.27154(12) 0.024 Uani 1 1 d . . . C124 C 0.4793(3) 0.31604(18) 0.30055(12) 0.028 Uani 1 1 d . . . H124 H 0.5017 0.3225 0.3348 0.034 Uiso 1 1 calc R . . C125 C 0.4986(3) 0.37099(17) 0.27857(13) 0.029 Uani 1 1 d . . . C126 C 0.4666(3) 0.36129(16) 0.22801(12) 0.025 Uani 1 1 d . . . H126 H 0.4812 0.4000 0.2137 0.029 Uiso 1 1 calc R . . C127 C 0.4046(3) 0.19194(19) 0.29565(12) 0.031 Uani 1 1 d . . . C128 C 0.5526(4) 0.44255(19) 0.30939(14) 0.041 Uani 1 1 d . . . F25 F 0.1980(2) 0.50045(14) 0.17258(16) 0.083 Uani 1 1 d U . . F26 F 0.0338(3) 0.46902(15) 0.19455(12) 0.072 Uani 1 1 d U . . F27 F 0.0555(3) 0.46529(15) 0.12149(11) 0.068 Uani 1 1 d U . . F28 F -0.16280(15) 0.22178(10) 0.13566(7) 0.028 Uani 1 1 d U . . F29 F -0.06376(15) 0.16325(9) 0.16546(7) 0.028 Uani 1 1 d U . . F30 F -0.07282(16) 0.15872(10) 0.08735(7) 0.029 Uani 1 1 d U . . F31 F 0.2317(3) 0.03354(17) -0.04501(12) 0.083 Uani 1 1 d U . . F32 F 0.2129(3) 0.13269(16) -0.04458(11) 0.075 Uani 1 1 d U . . F33 F 0.1128(2) 0.07415(19) -0.00377(11) 0.078 Uani 1 1 d U . . F34 F 0.5106(2) 0.01719(14) 0.08915(14) 0.071 Uani 1 1 d U . . F35 F 0.6206(2) 0.11334(13) 0.12628(10) 0.054 Uani 1 1 d U . . F36 F 0.6162(2) 0.07559(16) 0.04906(11) 0.064 Uani 1 1 d U . . F37 F 0.45961(17) 0.43209(10) -0.03361(7) 0.033 Uani 1 1 d U . . F38 F 0.33644(17) 0.45923(11) 0.01578(8) 0.035 Uani 1 1 d U . . F39 F 0.31373(17) 0.35486(11) -0.02695(8) 0.035 Uani 1 1 d U . . F40 F 0.8006(2) 0.43576(14) 0.06470(10) 0.054 Uani 1 1 d U . . F41 F 0.79050(17) 0.39367(12) 0.12895(8) 0.040 Uani 1 1 d U . . F42 F 0.7669(2) 0.49495(14) 0.13451(13) 0.070 Uani 1 1 d U . . F43 F 0.3222(3) 0.19545(17) 0.32567(13) 0.075 Uani 1 1 d U . . F44 F 0.4919(2) 0.19091(13) 0.32486(10) 0.055 Uani 1 1 d U . . F45 F 0.3751(3) 0.13108(13) 0.26423(10) 0.063 Uani 1 1 d U . . F46 F 0.6320(2) 0.47736(14) 0.28584(11) 0.063 Uani 1 1 d U . . F47 F 0.6085(3) 0.44252(16) 0.35069(12) 0.078 Uani 1 1 d U . . F48 F 0.4811(2) 0.48192(14) 0.31711(12) 0.066 Uani 1 1 d U . . 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 0.024 0.015 0.015 0.006 0.003 0.005 P1 0.028 0.017 0.016 0.007 0.005 0.008 O1 0.040 0.020 0.020 0.009 0.010 0.013 N1 0.023 0.020 0.018 0.006 0.004 0.006 N2 0.030 0.019 0.019 0.006 0.006 0.009 C1 0.028 0.016 0.015 0.003 0.005 0.007 C2 0.026 0.022 0.021 0.005 0.004 0.005 C3 0.027 0.031 0.016 0.006 -0.001 0.005 C4 0.030 0.029 0.017 0.009 0.008 0.009 C5 0.023 0.023 0.025 0.008 0.006 0.006 C6 0.026 0.018 0.022 0.005 0.003 0.006 C7 0.026 0.036 0.023 0.009 0.005 0.001 C8 0.034 0.042 0.062 0.016 0.008 -0.004 C9 0.024 0.056 0.035 0.018 0.004 0.007 C10 0.028 0.027 0.021 0.008 0.001 0.004 C11 0.036 0.029 0.037 0.005 -0.006 0.002 C12 0.038 0.042 0.038 0.006 -0.007 0.016 C13 0.031 0.021 0.019 0.006 0.005 0.008 C14 0.054 0.027 0.026 0.009 0.015 0.019 C15 0.035 0.022 0.027 0.011 0.010 0.004 C16 0.035 0.036 0.035 0.002 0.005 -0.008 C17 0.036 0.033 0.033 0.014 0.013 0.010 C18 0.033 0.034 0.020 0.010 0.001 0.014 C19 0.034 0.045 0.027 0.012 -0.001 0.016 C20 0.052 0.052 0.035 0.026 0.004 0.022 C21 0.037 0.017 0.021 0.008 0.008 0.010 C22 0.038 0.018 0.021 0.006 -0.001 0.010 C23 0.041 0.024 0.047 0.007 -0.020 0.006 C24 0.083 0.024 0.018 0.006 0.002 0.021 C25 0.030 0.013 0.016 0.002 0.003 0.006 C26 0.028 0.019 0.026 0.003 0.001 0.003 C27 0.044 0.017 0.027 0.008 0.009 0.003 C28 0.045 0.022 0.020 0.007 0.002 0.015 C29 0.031 0.026 0.023 0.002 -0.001 0.014 C30 0.027 0.020 0.022 0.005 0.004 0.005 C31 0.035 0.019 0.020 0.004 0.007 0.010 C32 0.058 0.028 0.024 0.014 0.012 0.014 Ni2 0.045 0.022 0.016 0.006 0.011 0.014 P2 0.043 0.019 0.014 0.004 0.007 0.011 O2 0.037 0.019 0.018 0.004 0.007 0.009 N3 0.033 0.019 0.019 0.005 0.004 0.009 N4 0.055 0.028 0.032 0.008 0.023 0.019 C33 0.037 0.022 0.027 0.009 0.012 0.014 C34 0.047 0.033 0.028 0.015 0.010 0.015 C35 0.066 0.039 0.034 0.021 0.015 0.023 C36 0.062 0.025 0.045 0.017 0.026 0.018 C37 0.046 0.024 0.047 0.006 0.016 0.011 C38 0.039 0.020 0.034 0.004 0.010 0.013 C39 0.058 0.044 0.030 0.017 -0.004 0.010 C40 0.084 0.061 0.032 0.015 0.002 0.026 C41 0.060 0.093 0.037 0.026 0.002 0.007 C42 0.050 0.021 0.042 0.003 -0.006 0.008 C43 0.085 0.123 0.066 0.024 0.015 0.069 C44 0.091 0.076 0.041 0.001 -0.003 0.051 C45 0.029 0.021 0.017 0.004 -0.001 0.008 C46 0.033 0.026 0.026 0.007 0.006 0.013 C47 0.053 0.022 0.018 0.000 0.001 0.004 C48 0.054 0.033 0.027 0.006 0.003 -0.006 C49 0.048 0.044 0.031 0.008 -0.001 0.007 C50 0.048 0.029 0.017 0.008 0.010 0.018 C51 0.072 0.037 0.029 0.015 0.014 0.032 C52 0.041 0.046 0.026 0.010 0.006 0.020 C53 0.073 0.029 0.024 0.010 0.023 0.026 C54 0.063 0.028 0.023 0.004 0.019 0.015 C55 0.053 0.053 0.032 -0.003 0.013 0.001 C56 0.108 0.029 0.041 0.005 0.041 0.019 C57 0.050 0.028 0.017 0.002 0.011 0.020 C58 0.045 0.036 0.023 0.009 0.007 0.014 C59 0.068 0.034 0.033 0.010 0.020 0.017 C60 0.051 0.034 0.051 -0.003 0.025 0.008 C61 0.042 0.056 0.047 -0.014 0.004 0.023 C62 0.054 0.047 0.024 0.002 0.007 0.030 C63 0.071 0.030 0.050 0.005 0.038 0.020 C64 0.117 0.028 0.107 0.008 0.080 0.008 B1 0.017 0.017 0.018 0.003 0.000 0.001 C65 0.018 0.017 0.020 0.003 0.002 0.008 C66 0.017 0.018 0.023 0.004 0.002 0.005 C67 0.020 0.026 0.023 0.008 0.005 0.010 C68 0.025 0.030 0.017 0.003 0.002 0.013 C69 0.029 0.024 0.024 0.005 0.002 0.012 C70 0.024 0.016 0.019 0.003 0.001 0.006 C71 0.029 0.034 0.024 0.012 0.004 0.007 C72 0.052 0.025 0.020 -0.004 0.000 0.007 C73 0.020 0.023 0.013 0.004 0.003 0.002 C74 0.024 0.021 0.016 0.005 0.000 0.001 C75 0.023 0.028 0.017 0.008 0.001 0.000 C76 0.018 0.031 0.019 0.008 0.001 0.002 C77 0.021 0.026 0.018 0.005 0.004 0.004 C78 0.019 0.022 0.018 0.001 0.002 0.003 C79 0.024 0.032 0.040 0.015 -0.001 0.000 C80 0.018 0.028 0.037 0.004 0.006 0.006 C81 0.022 0.016 0.020 0.004 0.007 0.000 C82 0.030 0.018 0.020 0.004 0.004 0.004 C83 0.035 0.020 0.023 0.002 0.004 0.001 C84 0.032 0.019 0.029 0.000 0.008 0.006 C85 0.022 0.023 0.034 0.001 0.006 0.006 C86 0.020 0.021 0.023 -0.001 0.002 0.002 C87 0.063 0.029 0.028 -0.004 -0.001 0.017 C88 0.030 0.029 0.050 -0.009 -0.004 0.015 C89 0.020 0.015 0.018 0.001 0.003 0.006 C90 0.019 0.021 0.020 0.004 0.002 0.006 C91 0.025 0.020 0.023 0.007 0.005 0.010 C92 0.026 0.018 0.027 0.008 0.008 0.008 C93 0.022 0.017 0.024 0.003 0.004 0.006 C94 0.021 0.017 0.019 0.004 0.002 0.006 C95 0.034 0.034 0.032 0.016 0.004 0.012 C96 0.022 0.021 0.029 0.005 0.005 0.003 F1 0.083 0.048 0.103 -0.013 0.010 0.017 F2 0.058 0.055 0.062 -0.008 0.009 -0.009 F3 0.158 0.068 0.065 0.026 -0.049 -0.026 F4 0.048 0.048 0.030 0.015 0.014 0.009 F5 0.045 0.041 0.047 0.025 0.003 0.014 F6 0.037 0.036 0.034 0.016 0.003 -0.003 F7 0.038 0.039 0.039 0.001 0.012 0.014 F8 0.037 0.039 0.046 0.017 0.006 0.016 F9 0.029 0.029 0.066 0.003 0.005 0.007 F10 0.042 0.050 0.070 0.023 -0.019 -0.004 F11 0.051 0.061 0.057 0.029 0.009 -0.010 F12 0.047 0.039 0.075 0.001 0.003 -0.002 F13 0.073 0.037 0.050 -0.008 -0.011 0.019 F14 0.078 0.063 0.033 0.006 0.006 0.018 F15 0.056 0.048 0.046 -0.009 -0.013 0.009 F16 0.059 0.056 0.065 -0.015 -0.006 0.039 F17 0.055 0.071 0.065 0.030 -0.006 0.023 F18 0.036 0.049 0.067 -0.006 -0.012 0.018 F19 0.046 0.050 0.035 0.025 0.007 0.014 F20 0.053 0.055 0.050 0.025 0.006 0.033 F21 0.050 0.050 0.038 0.019 -0.014 0.004 F22 0.031 0.050 0.058 0.030 0.002 -0.004 F23 0.025 0.033 0.044 0.007 -0.001 0.010 F24 0.032 0.047 0.041 -0.010 -0.002 0.005 B2 0.020 0.015 0.018 0.003 0.000 0.005 C97 0.021 0.020 0.013 0.005 0.003 0.006 C98 0.022 0.018 0.016 0.006 0.002 0.003 C99 0.025 0.020 0.014 0.004 0.002 0.006 C100 0.022 0.023 0.014 0.007 0.003 0.008 C101 0.021 0.022 0.011 0.006 0.002 0.005 C102 0.023 0.019 0.014 0.005 0.003 0.006 C103 0.025 0.021 0.026 0.007 0.003 0.008 C104 0.021 0.023 0.018 0.008 0.002 0.005 C105 0.019 0.016 0.018 0.008 0.005 0.002 C106 0.023 0.017 0.018 0.005 0.004 0.004 C107 0.027 0.019 0.020 0.006 0.005 0.003 C108 0.028 0.017 0.022 0.003 0.008 0.005 C109 0.022 0.020 0.025 0.009 0.006 0.004 C110 0.020 0.017 0.020 0.007 0.004 0.004 C111 0.032 0.023 0.021 0.002 0.003 0.006 C112 0.029 0.018 0.037 0.002 0.004 0.010 C113 0.021 0.011 0.024 0.001 0.004 0.005 C114 0.020 0.017 0.026 0.005 0.006 0.005 C115 0.025 0.017 0.029 0.008 0.009 0.008 C116 0.024 0.017 0.040 0.011 0.014 0.006 C117 0.022 0.016 0.042 0.005 0.007 0.007 C118 0.021 0.016 0.030 0.004 0.003 0.006 C119 0.028 0.027 0.035 0.017 0.014 0.007 C120 0.022 0.024 0.064 0.009 0.010 0.003 C121 0.020 0.019 0.021 0.002 0.002 0.009 C122 0.020 0.021 0.021 0.004 0.001 0.006 C123 0.025 0.027 0.023 0.005 0.002 0.010 C124 0.030 0.035 0.020 0.003 -0.004 0.012 C125 0.031 0.026 0.028 0.000 -0.004 0.011 C126 0.029 0.021 0.023 0.002 -0.003 0.009 C127 0.036 0.036 0.022 0.010 -0.001 0.006 C128 0.060 0.029 0.030 -0.004 -0.014 0.013 F25 0.053 0.032 0.159 0.011 -0.008 0.018 F26 0.094 0.055 0.082 0.020 0.048 0.038 F27 0.094 0.052 0.067 0.021 -0.010 0.031 F28 0.020 0.031 0.032 0.011 0.003 0.005 F29 0.028 0.027 0.030 0.016 0.001 0.002 F30 0.030 0.028 0.024 0.001 0.001 0.000 F31 0.086 0.074 0.073 -0.033 -0.036 0.043 F32 0.089 0.067 0.060 0.029 -0.034 -0.005 F33 0.049 0.115 0.049 0.009 0.001 -0.007 F34 0.060 0.041 0.123 0.037 -0.003 0.017 F35 0.052 0.054 0.058 -0.001 -0.013 0.032 F36 0.062 0.078 0.064 0.015 0.019 0.043 F37 0.035 0.036 0.035 0.018 0.014 0.008 F38 0.038 0.037 0.041 0.021 0.014 0.019 F39 0.032 0.037 0.037 0.018 0.001 0.003 F40 0.034 0.069 0.070 0.036 0.014 0.010 F41 0.026 0.046 0.048 0.012 -0.003 0.006 F42 0.042 0.043 0.109 -0.010 0.003 0.006 F43 0.077 0.082 0.084 0.046 0.038 0.025 F44 0.060 0.052 0.057 0.026 -0.015 0.013 F45 0.099 0.040 0.046 0.020 -0.011 0.001 F46 0.057 0.049 0.065 -0.001 0.002 -0.003 F47 0.097 0.062 0.062 0.011 -0.033 0.004 F48 0.062 0.045 0.077 -0.014 0.009 0.016 _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 N2 1.893(3) . ? Ni1 C21 1.971(3) . ? Ni1 N1 1.984(2) . ? Ni1 P1 2.0880(8) . ? P1 O1 1.683(2) . ? P1 C18 1.823(3) . ? P1 C15 1.826(3) . ? O1 C13 1.356(4) . ? N1 C13 1.282(4) . ? N1 C1 1.447(4) . ? N2 C31 1.143(4) . ? C1 C2 1.395(4) . ? C1 C6 1.403(4) . ? C2 C3 1.398(4) . ? C2 C7 1.524(4) . ? C3 C4 1.383(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 C10 1.522(4) . ? C7 C8 1.522(5) . ? C7 C9 1.533(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.524(5) . ? C10 C11 1.527(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.488(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.534(5) . ? C15 C16 1.536(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.528(5) . ? C18 C19 1.540(5) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.551(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C25 1.529(4) . ? C22 C23 1.535(5) . ? C22 C24 1.554(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C30 1.395(4) . ? C25 C26 1.396(4) . ? C26 C27 1.390(5) . ? C26 H26 0.9500 . ? C27 C28 1.382(5) . ? C27 H27 0.9500 . ? C28 C29 1.383(5) . ? C28 H28 0.9500 . ? C29 C30 1.388(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.456(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Ni2 N4 1.892(3) . ? Ni2 C53 1.969(3) . ? Ni2 N3 1.990(3) . ? Ni2 P2 2.0757(9) . ? P2 O2 1.685(2) . ? P2 C47 1.825(4) . ? P2 C50 1.833(3) . ? O2 C45 1.348(4) . ? N3 C45 1.288(4) . ? N3 C33 1.444(4) . ? N4 C63 1.132(5) . ? C33 C38 1.397(5) . ? C33 C34 1.402(5) . ? C34 C35 1.397(5) . ? C34 C39 1.530(6) . ? C35 C36 1.381(6) . ? C35 H35 0.9500 . ? C36 C37 1.382(6) . ? C36 H36 0.9500 . ? C37 C38 1.392(5) . ? C37 H37 0.9500 . ? C38 C42 1.531(5) . ? C39 C41 1.516(7) . ? C39 C40 1.524(6) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.476(7) . ? C42 C44 1.494(6) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.489(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C49 1.532(5) . ? C47 C48 1.536(5) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C52 1.531(5) . ? C50 C51 1.534(5) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.559(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.519(6) . ? C54 C57 1.532(5) . ? C54 C56 1.552(5) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C62 1.386(6) . ? C57 C58 1.390(5) . ? C58 C59 1.387(6) . ? C58 H58 0.9500 . ? C59 C60 1.370(7) . ? C59 H59 0.9500 . ? C60 C61 1.394(7) . ? C60 H60 0.9500 . ? C61 C62 1.377(6) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.458(6) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? B1 C73 1.634(4) . ? B1 C89 1.636(4) . ? B1 C81 1.644(4) . ? B1 C65 1.645(4) . ? C65 C70 1.393(4) . ? C65 C66 1.402(4) . ? C66 C67 1.386(4) . ? C66 H66 0.9500 . ? C67 C68 1.389(5) . ? C67 C71 1.496(4) . ? C68 C69 1.377(5) . ? C68 H68 0.9500 . ? C69 C70 1.399(4) . ? C69 C72 1.494(5) . ? C70 H70 0.9500 . ? C71 F4 1.337(4) . ? C71 F6 1.346(4) . ? C71 F5 1.346(4) . ? C72 F3 1.280(5) . ? C72 F1 1.312(5) . ? C72 F2 1.342(5) . ? C73 C74 1.392(4) . ? C73 C78 1.406(4) . ? C74 C75 1.395(4) . ? C74 H74 0.9500 . ? C75 C76 1.387(5) . ? C75 C79 1.487(4) . ? C76 C77 1.398(4) . ? C76 H76 0.9500 . ? C77 C78 1.383(4) . ? C77 C80 1.501(5) . ? C78 H78 0.9500 . ? C79 F10 1.317(4) . ? C79 F11 1.334(4) . ? C79 F12 1.345(5) . ? C80 F8 1.334(4) . ? C80 F9 1.334(4) . ? C80 F7 1.347(4) . ? C81 C86 1.397(4) . ? C81 C82 1.399(4) . ? C82 C83 1.398(5) . ? C82 H82 0.9500 . ? C83 C84 1.393(5) . ? C83 C87 1.489(5) . ? C84 C85 1.378(5) . ? C84 H84 0.9500 . ? C85 C86 1.396(4) . ? C85 C88 1.499(5) . ? C86 H86 0.9500 . ? C87 F13 1.332(4) . ? C87 F15 1.341(5) . ? C87 F14 1.344(5) . ? C88 F18 1.323(4) . ? C88 F16 1.330(4) . ? C88 F17 1.339(5) . ? C89 C94 1.397(4) . ? C89 C90 1.401(4) . ? C90 C91 1.390(4) . ? C90 H90 0.9500 . ? C91 C92 1.385(5) . ? C91 C95 1.502(4) . ? C92 C93 1.386(4) . ? C92 H92 0.9500 . ? C93 C94 1.393(4) . ? C93 C96 1.493(4) . ? C94 H94 0.9500 . ? C95 F19 1.334(4) . ? C95 F20 1.336(4) . ? C95 F21 1.344(4) . ? C96 F22 1.329(4) . ? C96 F23 1.340(4) . ? C96 F24 1.346(4) . ? B2 C121 1.640(4) . ? B2 C113 1.642(4) . ? B2 C105 1.644(4) . ? B2 C97 1.644(4) . ? C97 C102 1.396(4) . ? C97 C98 1.406(4) . ? C98 C99 1.388(4) . ? C98 H98 0.9500 . ? C99 C100 1.397(4) . ? C99 C103 1.504(4) . ? C100 C101 1.383(4) . ? C100 H100 0.9500 . ? C101 C102 1.395(4) . ? C101 C104 1.500(4) . ? C102 H102 0.9500 . ? C103 F25 1.270(4) . ? C103 F26 1.328(4) . ? C103 F27 1.334(4) . ? C104 F28 1.343(4) . ? C104 F29 1.344(3) . ? C104 F30 1.346(4) . ? C105 C106 1.400(4) . ? C105 C110 1.404(4) . ? C106 C107 1.401(4) . ? C106 H106 0.9500 . ? C107 C108 1.385(4) . ? C107 C111 1.491(4) . ? C108 C109 1.391(4) . ? C108 H108 0.9500 . ? C109 C110 1.390(4) . ? C109 C112 1.499(4) . ? C110 H110 0.9500 . ? C111 F32 1.306(4) . ? C111 F31 1.306(4) . ? C111 F33 1.312(4) . ? C112 F34 1.297(4) . ? C112 F35 1.319(4) . ? C112 F36 1.352(4) . ? C113 C114 1.391(4) . ? C113 C118 1.402(4) . ? C114 C115 1.395(4) . ? C114 H114 0.9500 . ? C115 C116 1.383(5) . ? C115 C119 1.492(5) . ? C116 C117 1.382(5) . ? C116 H116 0.9500 . ? C117 C118 1.396(5) . ? C117 C120 1.500(5) . ? C118 H118 0.9500 . ? C119 F39 1.346(4) . ? C119 F37 1.347(4) . ? C119 F38 1.349(4) . ? C120 F42 1.325(5) . ? C120 F41 1.340(5) . ? C120 F40 1.350(5) . ? C121 C122 1.399(4) . ? C121 C126 1.403(4) . ? C122 C123 1.394(4) . ? C122 H122 0.9500 . ? C123 C124 1.390(5) . ? C123 C127 1.490(5) . ? C124 C125 1.379(5) . ? C124 H124 0.9500 . ? C125 C126 1.400(5) . ? C125 C128 1.508(5) . ? C126 H126 0.9500 . ? C127 F45 1.314(4) . ? C127 F44 1.325(4) . ? C127 F43 1.338(5) . ? C128 F48 1.311(5) . ? C128 F47 1.314(5) . ? C128 F46 1.354(5) . ? 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 N2 Ni1 C21 95.52(12) . . ? N2 Ni1 N1 91.90(10) . . ? C21 Ni1 N1 172.53(11) . . ? N2 Ni1 P1 174.79(8) . . ? C21 Ni1 P1 88.77(9) . . ? N1 Ni1 P1 83.78(7) . . ? O1 P1 C18 100.21(14) . . ? O1 P1 C15 98.95(14) . . ? C18 P1 C15 109.34(16) . . ? O1 P1 Ni1 102.83(8) . . ? C18 P1 Ni1 119.66(12) . . ? C15 P1 Ni1 120.74(11) . . ? C13 O1 P1 115.19(19) . . ? C13 N1 C1 117.8(3) . . ? C13 N1 Ni1 119.4(2) . . ? C1 N1 Ni1 122.80(19) . . ? C31 N2 Ni1 168.2(3) . . ? C2 C1 C6 122.5(3) . . ? C2 C1 N1 118.0(3) . . ? C6 C1 N1 119.3(3) . . ? C1 C2 C3 117.4(3) . . ? C1 C2 C7 121.6(3) . . ? C3 C2 C7 121.0(3) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 117.4(3) . . ? C5 C6 C10 119.6(3) . . ? C1 C6 C10 122.9(3) . . ? C8 C7 C2 111.9(3) . . ? C8 C7 C9 110.2(3) . . ? C2 C7 C9 112.4(3) . . ? C8 C7 H7 107.3 . . ? C2 C7 H7 107.3 . . ? C9 C7 H7 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 111.2(3) . . ? C6 C10 C11 110.2(3) . . ? C12 C10 C11 111.1(3) . . ? C6 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 O1 118.8(3) . . ? N1 C13 C14 128.7(3) . . ? O1 C13 C14 112.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 111.1(3) . . ? C17 C15 P1 113.0(2) . . ? C16 C15 P1 108.9(2) . . ? C17 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? P1 C15 H15 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 111.3(3) . . ? C20 C18 P1 113.8(3) . . ? C19 C18 P1 108.1(2) . . ? C20 C18 H18 107.8 . . ? C19 C18 H18 107.8 . . ? P1 C18 H18 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Ni1 118.1(2) . . ? C22 C21 H21A 107.8 . . ? Ni1 C21 H21A 107.8 . . ? C22 C21 H21B 107.8 . . ? Ni1 C21 H21B 107.8 . . ? H21A C21 H21B 107.1 . . ? C25 C22 C23 112.7(3) . . ? C25 C22 C21 113.0(3) . . ? C23 C22 C21 109.0(3) . . ? C25 C22 C24 106.6(3) . . ? C23 C22 C24 108.0(3) . . ? C21 C22 C24 107.4(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C30 C25 C26 117.4(3) . . ? C30 C25 C22 120.2(3) . . ? C26 C25 C22 122.3(3) . . ? C27 C26 C25 121.1(3) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.0(3) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 120.5(3) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C25 121.3(3) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? N2 C31 C32 178.5(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 Ni2 C53 96.25(14) . . ? N4 Ni2 N3 91.75(12) . . ? C53 Ni2 N3 171.98(14) . . ? N4 Ni2 P2 168.92(11) . . ? C53 Ni2 P2 87.66(11) . . ? N3 Ni2 P2 84.37(8) . . ? O2 P2 C47 98.88(15) . . ? O2 P2 C50 99.98(13) . . ? C47 P2 C50 108.93(16) . . ? O2 P2 Ni2 102.47(8) . . ? C47 P2 Ni2 125.79(11) . . ? C50 P2 Ni2 115.38(12) . . ? C45 O2 P2 115.7(2) . . ? C45 N3 C33 118.5(3) . . ? C45 N3 Ni2 118.4(2) . . ? C33 N3 Ni2 123.1(2) . . ? C63 N4 Ni2 166.6(3) . . ? C38 C33 C34 122.5(3) . . ? C38 C33 N3 119.5(3) . . ? C34 C33 N3 117.8(3) . . ? C35 C34 C33 117.5(4) . . ? C35 C34 C39 121.8(3) . . ? C33 C34 C39 120.7(3) . . ? C36 C35 C34 121.0(4) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C35 C36 C37 120.1(3) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 121.4(4) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C37 C38 C33 117.4(3) . . ? C37 C38 C42 120.7(3) . . ? C33 C38 C42 121.8(3) . . ? C41 C39 C40 111.0(4) . . ? C41 C39 C34 110.6(4) . . ? C40 C39 C34 113.0(4) . . ? C41 C39 H39 107.3 . . ? C40 C39 H39 107.3 . . ? C34 C39 H39 107.3 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C44 112.9(4) . . ? C43 C42 C38 111.7(4) . . ? C44 C42 C38 114.4(3) . . ? C43 C42 H42 105.7 . . ? C44 C42 H42 105.7 . . ? C38 C42 H42 105.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C45 O2 118.8(3) . . ? N3 C45 C46 128.4(3) . . ? O2 C45 C46 112.8(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C47 C48 111.1(3) . . ? C49 C47 P2 109.0(3) . . ? C48 C47 P2 112.2(2) . . ? C49 C47 H47 108.1 . . ? C48 C47 H47 108.1 . . ? P2 C47 H47 108.1 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C50 C51 111.4(3) . . ? C52 C50 P2 109.9(2) . . ? C51 C50 P2 113.4(2) . . ? C52 C50 H50 107.3 . . ? C51 C50 H50 107.3 . . ? P2 C50 H50 107.3 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 Ni2 116.5(2) . . ? C54 C53 H53A 108.2 . . ? Ni2 C53 H53A 108.2 . . ? C54 C53 H53B 108.2 . . ? Ni2 C53 H53B 108.2 . . ? H53A C53 H53B 107.3 . . ? C55 C54 C57 113.7(3) . . ? C55 C54 C56 108.2(4) . . ? C57 C54 C56 107.3(3) . . ? C55 C54 C53 108.9(3) . . ? C57 C54 C53 111.7(3) . . ? C56 C54 C53 106.7(3) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C62 C57 C58 117.6(4) . . ? C62 C57 C54 120.0(3) . . ? C58 C57 C54 122.4(3) . . ? C59 C58 C57 121.2(4) . . ? C59 C58 H58 119.4 . . ? C57 C58 H58 119.4 . . ? C60 C59 C58 120.5(4) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C61 119.1(4) . . ? C59 C60 H60 120.5 . . ? C61 C60 H60 120.5 . . ? C62 C61 C60 120.1(4) . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C57 121.6(4) . . ? C61 C62 H62 119.2 . . ? C57 C62 H62 119.2 . . ? N4 C63 C64 177.4(4) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C73 B1 C89 109.8(2) . . ? C73 B1 C81 114.7(2) . . ? C89 B1 C81 104.7(2) . . ? C73 B1 C65 103.3(2) . . ? C89 B1 C65 114.7(2) . . ? C81 B1 C65 110.0(2) . . ? C70 C65 C66 115.8(3) . . ? C70 C65 B1 125.7(3) . . ? C66 C65 B1 118.2(3) . . ? C67 C66 C65 122.3(3) . . ? C67 C66 H66 118.9 . . ? C65 C66 H66 118.9 . . ? C66 C67 C68 120.8(3) . . ? C66 C67 C71 120.0(3) . . ? C68 C67 C71 119.1(3) . . ? C69 C68 C67 118.1(3) . . ? C69 C68 H68 121.0 . . ? C67 C68 H68 121.0 . . ? C68 C69 C70 120.9(3) . . ? C68 C69 C72 119.0(3) . . ? C70 C69 C72 120.0(3) . . ? C65 C70 C69 122.1(3) . . ? C65 C70 H70 119.0 . . ? C69 C70 H70 119.0 . . ? F4 C71 F6 106.7(3) . . ? F4 C71 F5 106.0(3) . . ? F6 C71 F5 106.1(3) . . ? F4 C71 C67 113.2(3) . . ? F6 C71 C67 112.9(3) . . ? F5 C71 C67 111.5(3) . . ? F3 C72 F1 107.7(4) . . ? F3 C72 F2 107.3(4) . . ? F1 C72 F2 100.1(3) . . ? F3 C72 C69 114.5(3) . . ? F1 C72 C69 112.4(3) . . ? F2 C72 C69 113.7(3) . . ? C74 C73 C78 116.2(3) . . ? C74 C73 B1 125.8(3) . . ? C78 C73 B1 117.8(3) . . ? C73 C74 C75 122.0(3) . . ? C73 C74 H74 119.0 . . ? C75 C74 H74 119.0 . . ? C76 C75 C74 120.9(3) . . ? C76 C75 C79 119.3(3) . . ? C74 C75 C79 119.6(3) . . ? C75 C76 C77 118.0(3) . . ? C75 C76 H76 121.0 . . ? C77 C76 H76 121.0 . . ? C78 C77 C76 120.6(3) . . ? C78 C77 C80 119.8(3) . . ? C76 C77 C80 119.6(3) . . ? C77 C78 C73 122.3(3) . . ? C77 C78 H78 118.8 . . ? C73 C78 H78 118.8 . . ? F10 C79 F11 107.6(3) . . ? F10 C79 F12 105.9(3) . . ? F11 C79 F12 104.6(3) . . ? F10 C79 C75 114.1(3) . . ? F11 C79 C75 111.4(3) . . ? F12 C79 C75 112.5(3) . . ? F8 C80 F9 106.4(3) . . ? F8 C80 F7 106.0(3) . . ? F9 C80 F7 106.8(3) . . ? F8 C80 C77 112.9(3) . . ? F9 C80 C77 112.7(3) . . ? F7 C80 C77 111.6(3) . . ? C86 C81 C82 115.7(3) . . ? C86 C81 B1 120.4(3) . . ? C82 C81 B1 123.7(3) . . ? C83 C82 C81 122.1(3) . . ? C83 C82 H82 119.0 . . ? C81 C82 H82 119.0 . . ? C84 C83 C82 120.6(3) . . ? C84 C83 C87 119.0(3) . . ? C82 C83 C87 120.4(3) . . ? C85 C84 C83 118.4(3) . . ? C85 C84 H84 120.8 . . ? C83 C84 H84 120.8 . . ? C84 C85 C86 120.4(3) . . ? C84 C85 C88 120.7(3) . . ? C86 C85 C88 118.7(3) . . ? C85 C86 C81 122.7(3) . . ? C85 C86 H86 118.6 . . ? C81 C86 H86 118.6 . . ? F13 C87 F15 107.1(3) . . ? F13 C87 F14 106.3(3) . . ? F15 C87 F14 105.9(3) . . ? F13 C87 C83 112.7(3) . . ? F15 C87 C83 112.3(3) . . ? F14 C87 C83 112.0(3) . . ? F18 C88 F16 106.5(3) . . ? F18 C88 F17 105.1(3) . . ? F16 C88 F17 107.3(3) . . ? F18 C88 C85 112.8(3) . . ? F16 C88 C85 112.8(3) . . ? F17 C88 C85 111.8(3) . . ? C94 C89 C90 115.6(3) . . ? C94 C89 B1 122.3(3) . . ? C90 C89 B1 122.0(3) . . ? C91 C90 C89 122.1(3) . . ? C91 C90 H90 118.9 . . ? C89 C90 H90 118.9 . . ? C92 C91 C90 121.3(3) . . ? C92 C91 C95 120.3(3) . . ? C90 C91 C95 118.4(3) . . ? C91 C92 C93 117.5(3) . . ? C91 C92 H92 121.2 . . ? C93 C92 H92 121.2 . . ? C92 C93 C94 121.1(3) . . ? C92 C93 C96 121.5(3) . . ? C94 C93 C96 117.4(3) . . ? C93 C94 C89 122.3(3) . . ? C93 C94 H94 118.9 . . ? C89 C94 H94 118.9 . . ? F19 C95 F20 106.1(3) . . ? F19 C95 F21 106.3(3) . . ? F20 C95 F21 106.1(3) . . ? F19 C95 C91 113.5(3) . . ? F20 C95 C91 112.5(3) . . ? F21 C95 C91 111.8(3) . . ? F22 C96 F23 107.5(3) . . ? F22 C96 F24 106.8(3) . . ? F23 C96 F24 104.0(3) . . ? F22 C96 C93 113.6(3) . . ? F23 C96 C93 112.0(3) . . ? F24 C96 C93 112.2(3) . . ? C121 B2 C113 114.4(2) . . ? C121 B2 C105 113.1(2) . . ? C113 B2 C105 101.8(2) . . ? C121 B2 C97 105.3(2) . . ? C113 B2 C97 109.5(2) . . ? C105 B2 C97 112.9(2) . . ? C102 C97 C98 116.0(3) . . ? C102 C97 B2 123.7(3) . . ? C98 C97 B2 120.3(3) . . ? C99 C98 C97 122.2(3) . . ? C99 C98 H98 118.9 . . ? C97 C98 H98 118.9 . . ? C98 C99 C100 120.7(3) . . ? C98 C99 C103 120.4(3) . . ? C100 C99 C103 118.9(3) . . ? C101 C100 C99 117.9(3) . . ? C101 C100 H100 121.0 . . ? C99 C100 H100 121.0 . . ? C100 C101 C102 121.1(3) . . ? C100 C101 C104 120.6(3) . . ? C102 C101 C104 118.3(3) . . ? C101 C102 C97 122.0(3) . . ? C101 C102 H102 119.0 . . ? C97 C102 H102 119.0 . . ? F25 C103 F26 110.1(3) . . ? F25 C103 F27 106.8(3) . . ? F26 C103 F27 100.2(3) . . ? F25 C103 C99 114.5(3) . . ? F26 C103 C99 112.3(3) . . ? F27 C103 C99 112.0(3) . . ? F28 C104 F29 106.4(2) . . ? F28 C104 F30 106.6(2) . . ? F29 C104 F30 105.9(2) . . ? F28 C104 C101 112.6(2) . . ? F29 C104 C101 113.0(2) . . ? F30 C104 C101 111.9(2) . . ? C106 C105 C110 116.0(3) . . ? C106 C105 B2 121.8(3) . . ? C110 C105 B2 121.7(3) . . ? C105 C106 C107 122.3(3) . . ? C105 C106 H106 118.9 . . ? C107 C106 H106 118.9 . . ? C108 C107 C106 120.4(3) . . ? C108 C107 C111 120.4(3) . . ? C106 C107 C111 119.2(3) . . ? C107 C108 C109 118.4(3) . . ? C107 C108 H108 120.8 . . ? C109 C108 H108 120.8 . . ? C110 C109 C108 121.0(3) . . ? C110 C109 C112 120.9(3) . . ? C108 C109 C112 118.1(3) . . ? C109 C110 C105 122.0(3) . . ? C109 C110 H110 119.0 . . ? C105 C110 H110 119.0 . . ? F32 C111 F31 106.6(3) . . ? F32 C111 F33 104.7(3) . . ? F31 C111 F33 105.8(3) . . ? F32 C111 C107 113.0(3) . . ? F31 C111 C107 113.7(3) . . ? F33 C111 C107 112.3(3) . . ? F34 C112 F35 109.2(3) . . ? F34 C112 F36 104.3(3) . . ? F35 C112 F36 103.7(3) . . ? F34 C112 C109 113.3(3) . . ? F35 C112 C109 114.0(3) . . ? F36 C112 C109 111.5(3) . . ? C114 C113 C118 115.8(3) . . ? C114 C113 B2 120.1(3) . . ? C118 C113 B2 123.8(3) . . ? C113 C114 C115 123.0(3) . . ? C113 C114 H114 118.5 . . ? C115 C114 H114 118.5 . . ? C116 C115 C114 120.1(3) . . ? C116 C115 C119 121.5(3) . . ? C114 C115 C119 118.3(3) . . ? C117 C116 C115 118.3(3) . . ? C117 C116 H116 120.8 . . ? C115 C116 H116 120.8 . . ? C116 C117 C118 121.2(3) . . ? C116 C117 C120 119.6(3) . . ? C118 C117 C120 119.1(3) . . ? C117 C118 C113 121.5(3) . . ? C117 C118 H118 119.2 . . ? C113 C118 H118 119.2 . . ? F39 C119 F37 106.2(3) . . ? F39 C119 F38 105.7(3) . . ? F37 C119 F38 106.4(2) . . ? F39 C119 C115 112.6(3) . . ? F37 C119 C115 113.1(3) . . ? F38 C119 C115 112.3(3) . . ? F42 C120 F41 106.3(3) . . ? F42 C120 F40 106.8(3) . . ? F41 C120 F40 105.9(3) . . ? F42 C120 C117 112.3(3) . . ? F41 C120 C117 113.1(3) . . ? F40 C120 C117 112.0(3) . . ? C122 C121 C126 116.0(3) . . ? C122 C121 B2 122.1(3) . . ? C126 C121 B2 121.7(3) . . ? C123 C122 C121 122.3(3) . . ? C123 C122 H122 118.9 . . ? C121 C122 H122 118.9 . . ? C124 C123 C122 120.5(3) . . ? C124 C123 C127 118.4(3) . . ? C122 C123 C127 121.2(3) . . ? C125 C124 C123 118.6(3) . . ? C125 C124 H124 120.7 . . ? C123 C124 H124 120.7 . . ? C124 C125 C126 120.7(3) . . ? C124 C125 C128 119.8(3) . . ? C126 C125 C128 119.5(3) . . ? C125 C126 C121 122.0(3) . . ? C125 C126 H126 119.0 . . ? C121 C126 H126 119.0 . . ? F45 C127 F44 106.6(3) . . ? F45 C127 F43 106.4(3) . . ? F44 C127 F43 104.4(3) . . ? F45 C127 C123 114.1(3) . . ? F44 C127 C123 113.1(3) . . ? F43 C127 C123 111.4(3) . . ? F48 C128 F47 112.5(4) . . ? F48 C128 F46 102.9(3) . . ? F47 C128 F46 103.1(4) . . ? F48 C128 C125 112.2(3) . . ? F47 C128 C125 113.0(3) . . ? F46 C128 C125 112.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Ni1 P1 O1 -179.23(13) . . . . ? N1 Ni1 P1 O1 0.32(12) . . . . ? C21 Ni1 P1 C18 70.97(16) . . . . ? N1 Ni1 P1 C18 -109.48(15) . . . . ? C21 Ni1 P1 C15 -70.50(16) . . . . ? N1 Ni1 P1 C15 109.05(15) . . . . ? C18 P1 O1 C13 122.4(2) . . . . ? C15 P1 O1 C13 -125.9(2) . . . . ? Ni1 P1 O1 C13 -1.4(2) . . . . ? N2 Ni1 N1 C13 177.9(3) . . . . ? P1 Ni1 N1 C13 0.9(2) . . . . ? N2 Ni1 N1 C1 -2.9(2) . . . . ? P1 Ni1 N1 C1 -180.0(2) . . . . ? C21 Ni1 N2 C31 173.7(14) . . . . ? N1 Ni1 N2 C31 -5.5(14) . . . . ? C13 N1 C1 C2 -97.3(3) . . . . ? Ni1 N1 C1 C2 83.5(3) . . . . ? C13 N1 C1 C6 87.7(4) . . . . ? Ni1 N1 C1 C6 -91.4(3) . . . . ? C6 C1 C2 C3 -5.8(5) . . . . ? N1 C1 C2 C3 179.5(3) . . . . ? C6 C1 C2 C7 173.9(3) . . . . ? N1 C1 C2 C7 -0.9(4) . . . . ? C1 C2 C3 C4 2.2(5) . . . . ? C7 C2 C3 C4 -177.4(3) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? C4 C5 C6 C1 -2.3(5) . . . . ? C4 C5 C6 C10 176.5(3) . . . . ? C2 C1 C6 C5 5.8(4) . . . . ? N1 C1 C6 C5 -179.5(3) . . . . ? C2 C1 C6 C10 -172.9(3) . . . . ? N1 C1 C6 C10 1.8(4) . . . . ? C1 C2 C7 C8 94.4(4) . . . . ? C3 C2 C7 C8 -86.0(4) . . . . ? C1 C2 C7 C9 -140.9(3) . . . . ? C3 C2 C7 C9 38.7(4) . . . . ? C5 C6 C10 C12 59.7(4) . . . . ? C1 C6 C10 C12 -121.5(3) . . . . ? C5 C6 C10 C11 -63.9(4) . . . . ? C1 C6 C10 C11 114.8(3) . . . . ? C1 N1 C13 O1 178.7(3) . . . . ? Ni1 N1 C13 O1 -2.1(4) . . . . ? C1 N1 C13 C14 -1.5(5) . . . . ? Ni1 N1 C13 C14 177.7(3) . . . . ? P1 O1 C13 N1 2.3(4) . . . . ? P1 O1 C13 C14 -177.5(2) . . . . ? O1 P1 C15 C17 -165.4(2) . . . . ? C18 P1 C15 C17 -61.2(3) . . . . ? Ni1 P1 C15 C17 83.8(3) . . . . ? O1 P1 C15 C16 70.6(3) . . . . ? C18 P1 C15 C16 174.8(2) . . . . ? Ni1 P1 C15 C16 -40.2(3) . . . . ? O1 P1 C18 C20 61.1(3) . . . . ? C15 P1 C18 C20 -42.3(3) . . . . ? Ni1 P1 C18 C20 172.3(2) . . . . ? O1 P1 C18 C19 -63.1(3) . . . . ? C15 P1 C18 C19 -166.5(2) . . . . ? Ni1 P1 C18 C19 48.1(3) . . . . ? N2 Ni1 C21 C22 47.5(2) . . . . ? P1 Ni1 C21 C22 -135.5(2) . . . . ? Ni1 C21 C22 C25 -74.5(3) . . . . ? Ni1 C21 C22 C23 51.6(3) . . . . ? Ni1 C21 C22 C24 168.3(2) . . . . ? C23 C22 C25 C30 -170.9(3) . . . . ? C21 C22 C25 C30 -46.8(4) . . . . ? C24 C22 C25 C30 70.8(4) . . . . ? C23 C22 C25 C26 11.4(4) . . . . ? C21 C22 C25 C26 135.5(3) . . . . ? C24 C22 C25 C26 -106.8(4) . . . . ? C30 C25 C26 C27 1.7(4) . . . . ? C22 C25 C26 C27 179.5(3) . . . . ? C25 C26 C27 C28 0.1(5) . . . . ? C26 C27 C28 C29 -1.4(5) . . . . ? C27 C28 C29 C30 0.8(5) . . . . ? C28 C29 C30 C25 1.1(5) . . . . ? C26 C25 C30 C29 -2.3(4) . . . . ? C22 C25 C30 C29 179.9(3) . . . . ? N4 Ni2 P2 O2 -69.6(5) . . . . ? C53 Ni2 P2 O2 179.42(16) . . . . ? N3 Ni2 P2 O2 0.33(12) . . . . ? N4 Ni2 P2 C47 179.6(6) . . . . ? C53 Ni2 P2 C47 68.7(2) . . . . ? N3 Ni2 P2 C47 -110.42(17) . . . . ? N4 Ni2 P2 C50 37.9(5) . . . . ? C53 Ni2 P2 C50 -73.03(18) . . . . ? N3 Ni2 P2 C50 107.88(14) . . . . ? C47 P2 O2 C45 126.8(2) . . . . ? C50 P2 O2 C45 -122.0(2) . . . . ? Ni2 P2 O2 C45 -3.0(2) . . . . ? N4 Ni2 N3 C45 172.1(3) . . . . ? P2 Ni2 N3 C45 2.5(2) . . . . ? N4 Ni2 N3 C33 -10.5(3) . . . . ? P2 Ni2 N3 C33 180.0(3) . . . . ? C53 Ni2 N4 C63 158.6(17) . . . . ? N3 Ni2 N4 C63 -20.9(17) . . . . ? P2 Ni2 N4 C63 48(2) . . . . ? C45 N3 C33 C38 -79.3(4) . . . . ? Ni2 N3 C33 C38 103.2(3) . . . . ? C45 N3 C33 C34 105.4(4) . . . . ? Ni2 N3 C33 C34 -72.1(4) . . . . ? C38 C33 C34 C35 3.9(5) . . . . ? N3 C33 C34 C35 179.0(3) . . . . ? C38 C33 C34 C39 -176.9(3) . . . . ? N3 C33 C34 C39 -1.7(5) . . . . ? C33 C34 C35 C36 -2.1(6) . . . . ? C39 C34 C35 C36 178.7(4) . . . . ? C34 C35 C36 C37 -0.3(6) . . . . ? C35 C36 C37 C38 0.9(6) . . . . ? C36 C37 C38 C33 0.7(5) . . . . ? C36 C37 C38 C42 -177.6(3) . . . . ? C34 C33 C38 C37 -3.2(5) . . . . ? N3 C33 C38 C37 -178.3(3) . . . . ? C34 C33 C38 C42 175.1(3) . . . . ? N3 C33 C38 C42 0.1(5) . . . . ? C35 C34 C39 C41 86.0(5) . . . . ? C33 C34 C39 C41 -93.2(4) . . . . ? C35 C34 C39 C40 -39.1(5) . . . . ? C33 C34 C39 C40 141.6(4) . . . . ? C37 C38 C42 C43 85.3(5) . . . . ? C33 C38 C42 C43 -93.0(5) . . . . ? C37 C38 C42 C44 -44.4(6) . . . . ? C33 C38 C42 C44 137.3(4) . . . . ? C33 N3 C45 O2 177.2(3) . . . . ? Ni2 N3 C45 O2 -5.3(4) . . . . ? C33 N3 C45 C46 -3.8(5) . . . . ? Ni2 N3 C45 C46 173.8(3) . . . . ? P2 O2 C45 N3 5.5(4) . . . . ? P2 O2 C45 C46 -173.7(2) . . . . ? O2 P2 C47 C49 -68.5(3) . . . . ? C50 P2 C47 C49 -172.3(2) . . . . ? Ni2 P2 C47 C49 44.0(3) . . . . ? O2 P2 C47 C48 55.0(3) . . . . ? C50 P2 C47 C48 -48.8(3) . . . . ? Ni2 P2 C47 C48 167.5(2) . . . . ? O2 P2 C50 C52 78.5(2) . . . . ? C47 P2 C50 C52 -178.4(2) . . . . ? Ni2 P2 C50 C52 -30.5(3) . . . . ? O2 P2 C50 C51 -156.0(3) . . . . ? C47 P2 C50 C51 -52.9(3) . . . . ? Ni2 P2 C50 C51 95.0(3) . . . . ? N4 Ni2 C53 C54 54.1(3) . . . . ? P2 Ni2 C53 C54 -136.3(3) . . . . ? Ni2 C53 C54 C55 54.8(4) . . . . ? Ni2 C53 C54 C57 -71.5(4) . . . . ? Ni2 C53 C54 C56 171.4(3) . . . . ? C55 C54 C57 C62 -173.5(3) . . . . ? C56 C54 C57 C62 66.9(4) . . . . ? C53 C54 C57 C62 -49.8(4) . . . . ? C55 C54 C57 C58 7.2(5) . . . . ? C56 C54 C57 C58 -112.4(4) . . . . ? C53 C54 C57 C58 130.9(4) . . . . ? C62 C57 C58 C59 0.5(5) . . . . ? C54 C57 C58 C59 179.8(3) . . . . ? C57 C58 C59 C60 1.2(6) . . . . ? C58 C59 C60 C61 -1.2(6) . . . . ? C59 C60 C61 C62 -0.4(6) . . . . ? C60 C61 C62 C57 2.2(6) . . . . ? C58 C57 C62 C61 -2.2(5) . . . . ? C54 C57 C62 C61 178.5(3) . . . . ? C73 B1 C65 C70 -102.2(3) . . . . ? C89 B1 C65 C70 17.3(4) . . . . ? C81 B1 C65 C70 134.9(3) . . . . ? C73 B1 C65 C66 72.2(3) . . . . ? C89 B1 C65 C66 -168.3(3) . . . . ? C81 B1 C65 C66 -50.7(3) . . . . ? C70 C65 C66 C67 -0.1(4) . . . . ? B1 C65 C66 C67 -175.0(3) . . . . ? C65 C66 C67 C68 -0.8(4) . . . . ? C65 C66 C67 C71 -177.8(3) . . . . ? C66 C67 C68 C69 0.7(4) . . . . ? C71 C67 C68 C69 177.7(3) . . . . ? C67 C68 C69 C70 0.2(5) . . . . ? C67 C68 C69 C72 179.9(3) . . . . ? C66 C65 C70 C69 1.1(4) . . . . ? B1 C65 C70 C69 175.6(3) . . . . ? C68 C69 C70 C65 -1.1(5) . . . . ? C72 C69 C70 C65 179.2(3) . . . . ? C66 C67 C71 F4 -145.4(3) . . . . ? C68 C67 C71 F4 37.6(4) . . . . ? C66 C67 C71 F6 -24.1(4) . . . . ? C68 C67 C71 F6 158.9(3) . . . . ? C66 C67 C71 F5 95.3(3) . . . . ? C68 C67 C71 F5 -81.8(4) . . . . ? C68 C69 C72 F3 25.6(5) . . . . ? C70 C69 C72 F3 -154.7(4) . . . . ? C68 C69 C72 F1 -97.7(4) . . . . ? C70 C69 C72 F1 81.9(4) . . . . ? C68 C69 C72 F2 149.4(3) . . . . ? C70 C69 C72 F2 -30.9(5) . . . . ? C89 B1 C73 C74 139.1(3) . . . . ? C81 B1 C73 C74 21.6(4) . . . . ? C65 B1 C73 C74 -98.1(3) . . . . ? C89 B1 C73 C78 -46.7(3) . . . . ? C81 B1 C73 C78 -164.2(3) . . . . ? C65 B1 C73 C78 76.1(3) . . . . ? C78 C73 C74 C75 1.9(4) . . . . ? B1 C73 C74 C75 176.2(3) . . . . ? C73 C74 C75 C76 -0.2(5) . . . . ? C73 C74 C75 C79 -176.7(3) . . . . ? C74 C75 C76 C77 -1.5(4) . . . . ? C79 C75 C76 C77 175.1(3) . . . . ? C75 C76 C77 C78 1.4(4) . . . . ? C75 C76 C77 C80 -178.4(3) . . . . ? C76 C77 C78 C73 0.4(5) . . . . ? C80 C77 C78 C73 -179.9(3) . . . . ? C74 C73 C78 C77 -2.0(4) . . . . ? B1 C73 C78 C77 -176.7(3) . . . . ? C76 C75 C79 F10 33.9(5) . . . . ? C74 C75 C79 F10 -149.6(3) . . . . ? C76 C75 C79 F11 -88.3(4) . . . . ? C74 C75 C79 F11 88.3(4) . . . . ? C76 C75 C79 F12 154.6(3) . . . . ? C74 C75 C79 F12 -28.8(4) . . . . ? C78 C77 C80 F8 121.8(3) . . . . ? C76 C77 C80 F8 -58.4(4) . . . . ? C78 C77 C80 F9 1.2(4) . . . . ? C76 C77 C80 F9 -179.1(3) . . . . ? C78 C77 C80 F7 -119.0(3) . . . . ? C76 C77 C80 F7 60.8(4) . . . . ? C73 B1 C81 C86 -146.8(3) . . . . ? C89 B1 C81 C86 92.8(3) . . . . ? C65 B1 C81 C86 -30.9(4) . . . . ? C73 B1 C81 C82 39.1(4) . . . . ? C89 B1 C81 C82 -81.3(3) . . . . ? C65 B1 C81 C82 155.0(3) . . . . ? C86 C81 C82 C83 -0.2(4) . . . . ? B1 C81 C82 C83 174.2(3) . . . . ? C81 C82 C83 C84 -0.5(5) . . . . ? C81 C82 C83 C87 -179.8(3) . . . . ? C82 C83 C84 C85 0.6(5) . . . . ? C87 C83 C84 C85 179.9(3) . . . . ? C83 C84 C85 C86 -0.1(5) . . . . ? C83 C84 C85 C88 176.0(3) . . . . ? C84 C85 C86 C81 -0.6(5) . . . . ? C88 C85 C86 C81 -176.8(3) . . . . ? C82 C81 C86 C85 0.7(5) . . . . ? B1 C81 C86 C85 -173.8(3) . . . . ? C84 C83 C87 F13 19.7(5) . . . . ? C82 C83 C87 F13 -161.1(3) . . . . ? C84 C83 C87 F15 140.8(3) . . . . ? C82 C83 C87 F15 -40.0(5) . . . . ? C84 C83 C87 F14 -100.2(4) . . . . ? C82 C83 C87 F14 79.0(4) . . . . ? C84 C85 C88 F18 141.0(3) . . . . ? C86 C85 C88 F18 -42.8(5) . . . . ? C84 C85 C88 F16 20.3(5) . . . . ? C86 C85 C88 F16 -163.5(3) . . . . ? C84 C85 C88 F17 -100.7(4) . . . . ? C86 C85 C88 F17 75.4(4) . . . . ? C73 B1 C89 C94 156.2(3) . . . . ? C81 B1 C89 C94 -80.2(3) . . . . ? C65 B1 C89 C94 40.4(4) . . . . ? C73 B1 C89 C90 -28.2(4) . . . . ? C81 B1 C89 C90 95.4(3) . . . . ? C65 B1 C89 C90 -144.0(3) . . . . ? C94 C89 C90 C91 -0.9(4) . . . . ? B1 C89 C90 C91 -176.8(3) . . . . ? C89 C90 C91 C92 -0.6(5) . . . . ? C89 C90 C91 C95 179.8(3) . . . . ? C90 C91 C92 C93 1.2(4) . . . . ? C95 C91 C92 C93 -179.3(3) . . . . ? C91 C92 C93 C94 -0.2(4) . . . . ? C91 C92 C93 C96 178.9(3) . . . . ? C92 C93 C94 C89 -1.5(5) . . . . ? C96 C93 C94 C89 179.4(3) . . . . ? C90 C89 C94 C93 2.0(4) . . . . ? B1 C89 C94 C93 177.9(3) . . . . ? C92 C91 C95 F19 18.4(4) . . . . ? C90 C91 C95 F19 -162.1(3) . . . . ? C92 C91 C95 F20 -102.1(4) . . . . ? C90 C91 C95 F20 77.4(4) . . . . ? C92 C91 C95 F21 138.6(3) . . . . ? C90 C91 C95 F21 -41.9(4) . . . . ? C92 C93 C96 F22 1.5(4) . . . . ? C94 C93 C96 F22 -179.4(3) . . . . ? C92 C93 C96 F23 -120.6(3) . . . . ? C94 C93 C96 F23 58.6(4) . . . . ? C92 C93 C96 F24 122.8(3) . . . . ? C94 C93 C96 F24 -58.0(4) . . . . ? C121 B2 C97 C102 -93.1(3) . . . . ? C113 B2 C97 C102 143.4(3) . . . . ? C105 B2 C97 C102 30.7(4) . . . . ? C121 B2 C97 C98 85.0(3) . . . . ? C113 B2 C97 C98 -38.5(3) . . . . ? C105 B2 C97 C98 -151.2(3) . . . . ? C102 C97 C98 C99 -2.5(4) . . . . ? B2 C97 C98 C99 179.2(3) . . . . ? C97 C98 C99 C100 0.1(4) . . . . ? C97 C98 C99 C103 -178.5(3) . . . . ? C98 C99 C100 C101 1.6(4) . . . . ? C103 C99 C100 C101 -179.8(3) . . . . ? C99 C100 C101 C102 -0.7(4) . . . . ? C99 C100 C101 C104 -178.4(3) . . . . ? C100 C101 C102 C97 -1.8(4) . . . . ? C104 C101 C102 C97 175.9(3) . . . . ? C98 C97 C102 C101 3.3(4) . . . . ? B2 C97 C102 C101 -178.4(3) . . . . ? C98 C99 C103 F25 -9.4(5) . . . . ? C100 C99 C103 F25 172.0(3) . . . . ? C98 C99 C103 F26 -135.8(3) . . . . ? C100 C99 C103 F26 45.5(4) . . . . ? C98 C99 C103 F27 112.3(3) . . . . ? C100 C99 C103 F27 -66.3(4) . . . . ? C100 C101 C104 F28 -3.3(4) . . . . ? C102 C101 C104 F28 179.0(2) . . . . ? C100 C101 C104 F29 -123.9(3) . . . . ? C102 C101 C104 F29 58.4(3) . . . . ? C100 C101 C104 F30 116.8(3) . . . . ? C102 C101 C104 F30 -61.0(3) . . . . ? C121 B2 C105 C106 153.9(3) . . . . ? C113 B2 C105 C106 -82.8(3) . . . . ? C97 B2 C105 C106 34.5(4) . . . . ? C121 B2 C105 C110 -34.7(4) . . . . ? C113 B2 C105 C110 88.6(3) . . . . ? C97 B2 C105 C110 -154.1(3) . . . . ? C110 C105 C106 C107 0.8(4) . . . . ? B2 C105 C106 C107 172.7(3) . . . . ? C105 C106 C107 C108 -0.5(5) . . . . ? C105 C106 C107 C111 178.4(3) . . . . ? C106 C107 C108 C109 0.1(4) . . . . ? C111 C107 C108 C109 -178.7(3) . . . . ? C107 C108 C109 C110 -0.1(4) . . . . ? C107 C108 C109 C112 179.3(3) . . . . ? C108 C109 C110 C105 0.5(5) . . . . ? C112 C109 C110 C105 -178.8(3) . . . . ? C106 C105 C110 C109 -0.9(4) . . . . ? B2 C105 C110 C109 -172.7(3) . . . . ? C108 C107 C111 F32 -122.7(4) . . . . ? C106 C107 C111 F32 58.4(4) . . . . ? C108 C107 C111 F31 -1.1(5) . . . . ? C106 C107 C111 F31 -179.9(3) . . . . ? C108 C107 C111 F33 119.1(4) . . . . ? C106 C107 C111 F33 -59.8(4) . . . . ? C110 C109 C112 F34 122.0(4) . . . . ? C108 C109 C112 F34 -57.4(4) . . . . ? C110 C109 C112 F35 -3.7(5) . . . . ? C108 C109 C112 F35 176.9(3) . . . . ? C110 C109 C112 F36 -120.7(3) . . . . ? C108 C109 C112 F36 59.9(4) . . . . ? C121 B2 C113 C114 -156.1(3) . . . . ? C105 B2 C113 C114 81.6(3) . . . . ? C97 B2 C113 C114 -38.1(4) . . . . ? C121 B2 C113 C118 31.3(4) . . . . ? C105 B2 C113 C118 -91.0(3) . . . . ? C97 B2 C113 C118 149.2(3) . . . . ? C118 C113 C114 C115 -0.1(4) . . . . ? B2 C113 C114 C115 -173.3(3) . . . . ? C113 C114 C115 C116 -0.3(5) . . . . ? C113 C114 C115 C119 -177.7(3) . . . . ? C114 C115 C116 C117 0.6(5) . . . . ? C119 C115 C116 C117 178.0(3) . . . . ? C115 C116 C117 C118 -0.6(5) . . . . ? C115 C116 C117 C120 -177.4(3) . . . . ? C116 C117 C118 C113 0.2(5) . . . . ? C120 C117 C118 C113 177.1(3) . . . . ? C114 C113 C118 C117 0.1(4) . . . . ? B2 C113 C118 C117 173.0(3) . . . . ? C116 C115 C119 F39 138.2(3) . . . . ? C114 C115 C119 F39 -44.4(4) . . . . ? C116 C115 C119 F37 17.9(4) . . . . ? C114 C115 C119 F37 -164.7(3) . . . . ? C116 C115 C119 F38 -102.6(3) . . . . ? C114 C115 C119 F38 74.8(4) . . . . ? C116 C117 C120 F42 85.3(4) . . . . ? C118 C117 C120 F42 -91.6(4) . . . . ? C116 C117 C120 F41 -154.5(3) . . . . ? C118 C117 C120 F41 28.6(5) . . . . ? C116 C117 C120 F40 -34.9(4) . . . . ? C118 C117 C120 F40 148.2(3) . . . . ? C113 B2 C121 C122 -151.9(3) . . . . ? C105 B2 C121 C122 -35.9(4) . . . . ? C97 B2 C121 C122 87.8(3) . . . . ? C113 B2 C121 C126 34.9(4) . . . . ? C105 B2 C121 C126 150.9(3) . . . . ? C97 B2 C121 C126 -85.4(3) . . . . ? C126 C121 C122 C123 -0.9(4) . . . . ? B2 C121 C122 C123 -174.4(3) . . . . ? C121 C122 C123 C124 0.7(5) . . . . ? C121 C122 C123 C127 179.9(3) . . . . ? C122 C123 C124 C125 0.1(5) . . . . ? C127 C123 C124 C125 -179.1(3) . . . . ? C123 C124 C125 C126 -0.6(5) . . . . ? C123 C124 C125 C128 178.3(3) . . . . ? C124 C125 C126 C121 0.3(5) . . . . ? C128 C125 C126 C121 -178.5(3) . . . . ? C122 C121 C126 C125 0.4(5) . . . . ? B2 C121 C126 C125 174.0(3) . . . . ? C124 C123 C127 F45 -167.4(3) . . . . ? C122 C123 C127 F45 13.3(5) . . . . ? C124 C123 C127 F44 -45.3(4) . . . . ? C122 C123 C127 F44 135.5(3) . . . . ? C124 C123 C127 F43 72.0(4) . . . . ? C122 C123 C127 F43 -107.2(4) . . . . ? C124 C125 C128 F48 -107.8(4) . . . . ? C126 C125 C128 F48 71.0(5) . . . . ? C124 C125 C128 F47 20.7(6) . . . . ? C126 C125 C128 F47 -160.4(4) . . . . ? C124 C125 C128 F46 136.8(4) . . . . ? C126 C125 C128 F46 -44.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.165 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.086 data_7b _database_code_depnum_ccdc_archive 'CCDC 876283' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H12 B F24, C32 H50 N2 O P Pd' _chemical_formula_sum 'C64 H62 B F24 N2 O P Pd' _chemical_formula_weight 1479.34 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.0211(6) _cell_length_b 12.5738(2) _cell_length_c 26.4997(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.5640(10) _cell_angle_gamma 90.00 _cell_volume 13549.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9715 _cell_measurement_theta_min 4.33 _cell_measurement_theta_max 31.92 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6000 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8847 _exptl_absorpt_correction_T_max 0.8985 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53449 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -59 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 4.33 _diffrn_reflns_theta_max 32.64 _reflns_number_total 24568 _reflns_number_gt 17881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+1.1894P] 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 24568 _refine_ls_number_parameters 931 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.359710(3) 0.448501(8) 0.981711(4) 0.01754(3) Uani 1 1 d . . . P1 P 0.357985(9) 0.50755(3) 0.903683(14) 0.02091(7) Uani 1 1 d . . . O1 O 0.39742(3) 0.54209(9) 0.90185(4) 0.0243(2) Uani 1 1 d . . . N1 N 0.41023(3) 0.49896(10) 0.98547(5) 0.0203(2) Uani 1 1 d . . . N2 N 0.36733(3) 0.38403(11) 1.05493(5) 0.0243(2) Uani 1 1 d . . . C1 C 0.43335(3) 0.48909(12) 1.03115(6) 0.0212(3) Uani 1 1 d . . . C2 C 0.44698(4) 0.38833(13) 1.04329(6) 0.0268(3) Uani 1 1 d . . . C3 C 0.46742(4) 0.37744(14) 1.08958(7) 0.0314(3) Uani 1 1 d . . . H3 H 0.4772 0.3104 1.0987 0.038 Uiso 1 1 d R . . C4 C 0.47363(4) 0.46244(15) 1.12223(7) 0.0318(3) Uani 1 1 d . . . H4 H 0.4875 0.4534 1.1536 0.038 Uiso 1 1 d R . . C5 C 0.45984(4) 0.56101(14) 1.10961(6) 0.0296(3) Uani 1 1 d . . . H5 H 0.4644 0.6188 1.1326 0.036 Uiso 1 1 d R . . C6 C 0.43937(4) 0.57699(12) 1.06374(6) 0.0240(3) Uani 1 1 d . . . C7 C 0.44061(5) 0.29471(14) 1.00739(8) 0.0355(4) Uani 1 1 d . . . H7 H 0.4200 0.3101 0.9839 0.043 Uiso 1 1 d R . . C8 C 0.46821(7) 0.2818(2) 0.97507(11) 0.0646(7) Uani 1 1 d . . . H8A H 0.4719 0.3494 0.9583 0.097 Uiso 1 1 d R . . H8B H 0.4623 0.2269 0.9493 0.097 Uiso 1 1 d R . . H8C H 0.4884 0.2608 0.9968 0.097 Uiso 1 1 d R . . C9 C 0.43542(8) 0.19024(17) 1.03490(11) 0.0633(7) Uani 1 1 d . . . H9A H 0.4562 0.1678 1.0545 0.095 Uiso 1 1 d R . . H9B H 0.4278 0.1354 1.0098 0.095 Uiso 1 1 d R . . H9C H 0.4189 0.2006 1.0580 0.095 Uiso 1 1 d R . . C10 C 0.42329(4) 0.68439(12) 1.05096(6) 0.0272(3) Uani 1 1 d . . . H10 H 0.4207 0.6927 1.0131 0.033 Uiso 1 1 d R . . C11 C 0.38909(5) 0.68751(16) 1.06712(9) 0.0432(4) Uani 1 1 d . . . H11A H 0.3760 0.6285 1.0511 0.065 Uiso 1 1 d R . . H11B H 0.3785 0.7551 1.0564 0.065 Uiso 1 1 d R . . H11C H 0.3908 0.6809 1.1042 0.065 Uiso 1 1 d R . . C12 C 0.44363(5) 0.77845(15) 1.07409(8) 0.0421(4) Uani 1 1 d . . . H12A H 0.4444 0.7770 1.1112 0.063 Uiso 1 1 d R . . H12B H 0.4335 0.8451 1.0608 0.063 Uiso 1 1 d R . . H12C H 0.4660 0.7735 1.0651 0.063 Uiso 1 1 d R . . C13 C 0.41938(4) 0.53526(12) 0.94445(6) 0.0224(3) Uani 1 1 d . . . C14 C 0.45265(4) 0.57371(14) 0.93617(7) 0.0296(3) Uani 1 1 d . . . H14A H 0.4680 0.5639 0.9674 0.044 Uiso 1 1 d R . . H14B H 0.4515 0.6493 0.9272 0.044 Uiso 1 1 d R . . H14C H 0.4604 0.5332 0.9085 0.044 Uiso 1 1 d R . . C15 C 0.35328(4) 0.41376(15) 0.85075(6) 0.0309(3) Uani 1 1 d . . . H15 H 0.3639 0.4457 0.8225 0.037 Uiso 1 1 d R . . C16 C 0.37167(5) 0.31101(15) 0.86708(7) 0.0399(4) Uani 1 1 d . . . H16A H 0.3616 0.2773 0.8945 0.060 Uiso 1 1 d R . . H16B H 0.3947 0.3275 0.8792 0.060 Uiso 1 1 d R . . H16C H 0.3705 0.2624 0.8380 0.060 Uiso 1 1 d R . . C17 C 0.31719(5) 0.39189(19) 0.83040(7) 0.0438(5) Uani 1 1 d . . . H17A H 0.3160 0.3465 0.8002 0.066 Uiso 1 1 d R . . H17B H 0.3060 0.4594 0.8214 0.066 Uiso 1 1 d R . . H17C H 0.3065 0.3560 0.8567 0.066 Uiso 1 1 d R . . C18 C 0.33809(4) 0.63296(13) 0.88405(6) 0.0284(3) Uani 1 1 d . . . H18 H 0.3138 0.6223 0.8820 0.034 Uiso 1 1 d R . . C19 C 0.34824(5) 0.71571(14) 0.92545(8) 0.0364(4) Uani 1 1 d . . . H19A H 0.3718 0.7309 0.9269 0.055 Uiso 1 1 d R . . H19B H 0.3438 0.6880 0.9584 0.055 Uiso 1 1 d R . . H19C H 0.3356 0.7812 0.9176 0.055 Uiso 1 1 d R . . C20 C 0.34540(6) 0.67231(19) 0.83185(8) 0.0472(5) Uani 1 1 d . . . H20A H 0.3345 0.7409 0.8241 0.071 Uiso 1 1 d R . . H20B H 0.3371 0.6203 0.8057 0.071 Uiso 1 1 d R . . H20C H 0.3692 0.6807 0.8324 0.071 Uiso 1 1 d R . . C21 C 0.31175(4) 0.39472(12) 0.97495(6) 0.0229(3) Uani 1 1 d . . . H21A H 0.3045 0.3792 0.9386 0.027 Uiso 1 1 d R . . H21B H 0.3116 0.3266 0.9936 0.027 Uiso 1 1 d R . . C22 C 0.28599(4) 0.46872(14) 0.99409(6) 0.0266(3) Uani 1 1 d . . . C23 C 0.29964(4) 0.52008(17) 1.04495(7) 0.0373(4) Uani 1 1 d . . . H23A H 0.3174 0.5692 1.0397 0.056 Uiso 1 1 d R . . H23B H 0.3082 0.4647 1.0692 0.056 Uiso 1 1 d R . . H23C H 0.2821 0.5593 1.0585 0.056 Uiso 1 1 d R . . C24 C 0.25674(4) 0.39796(17) 1.00450(7) 0.0366(4) Uani 1 1 d . . . H24A H 0.2391 0.4430 1.0142 0.055 Uiso 1 1 d R . . H24B H 0.2640 0.3483 1.0322 0.055 Uiso 1 1 d R . . H24C H 0.2486 0.3579 0.9737 0.055 Uiso 1 1 d R . . C25 C 0.27309(4) 0.55015(14) 0.95367(7) 0.0311(3) Uani 1 1 d . . . C26 C 0.27419(5) 0.65935(16) 0.96265(9) 0.0450(5) Uani 1 1 d . . . H26 H 0.2837 0.6856 0.9949 0.054 Uiso 1 1 d R . . C27 C 0.26148(6) 0.7303(2) 0.92466(12) 0.0635(8) Uani 1 1 d . . . H27 H 0.2625 0.8045 0.9313 0.076 Uiso 1 1 d R . . C28 C 0.24738(6) 0.6947(2) 0.87772(12) 0.0687(9) Uani 1 1 d . . . H28 H 0.2390 0.7438 0.8520 0.082 Uiso 1 1 d R . . C29 C 0.24561(5) 0.5863(2) 0.86830(9) 0.0562(7) Uani 1 1 d . . . H29 H 0.2355 0.5609 0.8362 0.067 Uiso 1 1 d R . . C30 C 0.25845(4) 0.51469(18) 0.90569(7) 0.0376(4) Uani 1 1 d . . . H30 H 0.2573 0.4406 0.8986 0.045 Uiso 1 1 d R . . C31 C 0.37545(4) 0.34665(13) 1.09350(6) 0.0259(3) Uani 1 1 d . . . C32 C 0.38705(5) 0.29953(17) 1.14283(7) 0.0374(4) Uani 1 1 d . . . H32A H 0.3867 0.2218 1.1399 0.056 Uiso 1 1 d R . . H32B H 0.3727 0.3216 1.1677 0.056 Uiso 1 1 d R . . H32C H 0.4096 0.3234 1.1541 0.056 Uiso 1 1 d R . . B1 B 0.38285(4) 0.02013(12) 0.73812(6) 0.0182(3) Uani 1 1 d . . . F1A F 0.34628(6) 0.49511(16) 0.72346(9) 0.0453(10) Uani 0.559(15) 1 d PDU A 1 F2A F 0.31825(6) 0.37117(19) 0.68507(14) 0.067(2) Uani 0.559(15) 1 d PDU A 1 F3A F 0.35598(9) 0.4522(2) 0.65071(9) 0.0625(18) Uani 0.559(15) 1 d PDU A 1 F1B F 0.33225(14) 0.4589(4) 0.72239(15) 0.106(5) Uani 0.441(15) 1 d PDU A 2 F2B F 0.32597(9) 0.3618(2) 0.65515(15) 0.064(2) Uani 0.441(15) 1 d PDU A 2 F3B F 0.36180(12) 0.4785(3) 0.66289(15) 0.076(2) Uani 0.441(15) 1 d PDU A 2 F4A F 0.45218(10) 0.3358(6) 0.85038(13) 0.102(3) Uani 0.419(7) 1 d PDU B 1 F5A F 0.48105(8) 0.2664(3) 0.79988(16) 0.0591(14) Uani 0.419(7) 1 d PDU B 1 F6A F 0.46753(10) 0.4231(2) 0.7898(2) 0.079(3) Uani 0.419(7) 1 d PDU B 1 F4B F 0.44731(6) 0.42335(19) 0.82518(10) 0.0551(11) Uani 0.581(7) 1 d PDU B 2 F5B F 0.47044(9) 0.27028(19) 0.82581(14) 0.090(2) Uani 0.581(7) 1 d PDU B 2 F6B F 0.47463(7) 0.3842(3) 0.76677(12) 0.0755(11) Uani 0.581(7) 1 d PDU B 2 F7A F 0.30242(8) -0.3114(3) 0.70416(17) 0.084(2) Uani 0.551(10) 1 d PDU C 1 F8A F 0.27376(11) -0.2848(4) 0.63369(11) 0.108(3) Uani 0.551(10) 1 d PDU C 1 F9A F 0.26520(8) -0.2014(2) 0.69660(18) 0.086(2) Uani 0.551(10) 1 d PDU C 1 F7B F 0.30354(11) -0.3363(3) 0.6676(3) 0.102(3) Uani 0.449(10) 1 d PDU C 2 F9B F 0.28153(17) -0.2411(5) 0.71744(14) 0.116(4) Uani 0.449(10) 1 d PDU C 2 F8B F 0.26386(8) -0.2479(3) 0.6413(2) 0.091(3) Uani 0.449(10) 1 d PDU C 2 F10 F 0.31751(5) 0.06651(14) 0.53406(5) 0.0744(5) Uani 1 1 d . . . F11 F 0.33082(4) -0.08981(13) 0.51568(4) 0.0634(4) Uani 1 1 d . . . F12 F 0.36788(3) 0.02461(15) 0.54294(5) 0.0694(5) Uani 1 1 d . . . F13 F 0.42928(3) -0.15690(9) 0.91760(4) 0.0393(2) Uani 1 1 d . . . F14 F 0.40882(3) -0.06302(11) 0.97333(4) 0.0491(3) Uani 1 1 d . . . F15 F 0.44416(3) 0.00512(10) 0.92941(4) 0.0443(3) Uani 1 1 d . . . F16 F 0.28063(4) 0.07528(18) 0.83071(6) 0.0856(6) Uani 1 1 d . . . F17 F 0.30218(3) 0.14077(11) 0.90063(6) 0.0594(4) Uani 1 1 d . . . F18 F 0.28957(4) -0.02052(12) 0.89783(8) 0.0810(6) Uani 1 1 d . . . F19 F 0.50808(3) -0.12268(10) 0.64228(5) 0.0507(3) Uani 1 1 d . . . F20 F 0.51128(4) 0.01900(13) 0.68608(6) 0.0640(4) Uani 1 1 d . . . F21 F 0.47732(3) 0.00922(11) 0.61797(5) 0.0498(3) Uani 1 1 d . . . F22 F 0.46161(6) -0.39831(11) 0.73740(7) 0.0985(8) Uani 1 1 d . . . F23 F 0.41612(3) -0.37242(9) 0.76539(6) 0.0547(4) Uani 1 1 d . . . F24 F 0.46044(3) -0.32885(9) 0.80986(5) 0.0526(3) Uani 1 1 d . . . C33 C 0.38991(4) 0.14768(11) 0.73471(5) 0.0195(2) Uani 1 1 d . . . C34 C 0.36718(4) 0.22175(11) 0.71207(5) 0.0228(3) Uani 1 1 d . . . H34 H 0.3472 0.1974 0.6934 0.027 Uiso 1 1 d R . . C35 C 0.37317(4) 0.33076(12) 0.71628(6) 0.0283(3) Uani 1 1 d . A . C36 C 0.40192(5) 0.36962(12) 0.74334(7) 0.0326(4) Uani 1 1 d . . . H36 H 0.4060 0.4439 0.7460 0.039 Uiso 1 1 d R . . C37 C 0.42463(4) 0.29731(12) 0.76641(6) 0.0287(3) Uani 1 1 d . B . C38 C 0.41883(4) 0.18872(11) 0.76191(6) 0.0234(3) Uani 1 1 d . . . H38 H 0.4349 0.1408 0.7778 0.028 Uiso 1 1 d R . . C39 C 0.34826(5) 0.40877(14) 0.69196(7) 0.0393(4) Uani 1 1 d D . . C40 C 0.45523(5) 0.33666(16) 0.79847(9) 0.0445(5) Uani 1 1 d D . . C41 C 0.35473(3) -0.02437(11) 0.69382(5) 0.0186(2) Uani 1 1 d . . . C42 C 0.33232(3) -0.10465(11) 0.70213(5) 0.0211(3) Uani 1 1 d . . . H42 H 0.3305 -0.1259 0.7361 0.025 Uiso 1 1 d R . . C43 C 0.31261(4) -0.15439(12) 0.66210(6) 0.0239(3) Uani 1 1 d . C . C44 C 0.31455(4) -0.12614(13) 0.61187(6) 0.0259(3) Uani 1 1 d . . . H44 H 0.3015 -0.1609 0.5845 0.031 Uiso 1 1 d R . . C45 C 0.33618(4) -0.04589(13) 0.60290(6) 0.0253(3) Uani 1 1 d . . . C46 C 0.35570(4) 0.00392(12) 0.64280(5) 0.0224(3) Uani 1 1 d . . . H46 H 0.3702 0.0591 0.6353 0.027 Uiso 1 1 d R . . C47 C 0.28963(4) -0.24130(15) 0.67337(7) 0.0343(4) Uani 1 1 d D . . C48 C 0.33836(5) -0.01202(19) 0.54924(6) 0.0398(4) Uani 1 1 d . . . C49 C 0.37372(4) 0.00504(10) 0.79593(5) 0.0195(3) Uani 1 1 d . . . C50 C 0.39755(4) -0.02178(11) 0.83656(5) 0.0206(3) Uani 1 1 d . . . H50 H 0.4192 -0.0381 0.8298 0.025 Uiso 1 1 d R . . C51 C 0.39070(4) -0.02545(12) 0.88681(6) 0.0231(3) Uani 1 1 d . . . C52 C 0.35959(4) -0.00136(12) 0.89847(6) 0.0275(3) Uani 1 1 d . . . H52 H 0.3548 -0.0039 0.9326 0.033 Uiso 1 1 d R . . C53 C 0.33559(4) 0.02675(12) 0.85871(6) 0.0264(3) Uani 1 1 d . . . C54 C 0.34234(4) 0.02962(11) 0.80872(6) 0.0232(3) Uani 1 1 d . . . H54 H 0.3253 0.0486 0.7824 0.028 Uiso 1 1 d R . . C55 C 0.41786(4) -0.05922(14) 0.92691(6) 0.0298(3) Uani 1 1 d . . . C56 C 0.30188(5) 0.05452(16) 0.87105(7) 0.0366(4) Uani 1 1 d . . . C57 C 0.41502(3) -0.05088(10) 0.72923(5) 0.0173(2) Uani 1 1 d . . . C58 C 0.43900(3) -0.01829(11) 0.69940(5) 0.0191(2) Uani 1 1 d . . . H58 H 0.4380 0.0518 0.6859 0.023 Uiso 1 1 d R . . C59 C 0.46431(3) -0.08570(11) 0.68908(5) 0.0197(2) Uani 1 1 d . . . C60 C 0.46678(4) -0.18863(11) 0.70845(5) 0.0211(3) Uani 1 1 d . . . H60 H 0.4839 -0.2349 0.7012 0.025 Uiso 1 1 d R . . C61 C 0.44344(4) -0.22162(10) 0.73869(5) 0.0198(3) Uani 1 1 d . . . C62 C 0.41805(3) -0.15501(11) 0.74827(5) 0.0186(2) Uani 1 1 d . . . H62 H 0.4022 -0.1807 0.7684 0.022 Uiso 1 1 d R . . C63 C 0.49000(4) -0.04519(13) 0.65859(6) 0.0256(3) Uani 1 1 d . . . C64 C 0.44566(4) -0.32979(12) 0.76239(6) 0.0268(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01878(5) 0.01860(5) 0.01509(5) -0.00070(4) 0.00165(3) -0.00126(4) P1 0.02162(17) 0.02503(17) 0.01614(15) 0.00019(13) 0.00274(12) -0.00198(14) O1 0.0221(5) 0.0317(5) 0.0198(5) 0.0007(4) 0.0048(4) -0.0027(4) N1 0.0200(6) 0.0201(5) 0.0208(6) -0.0022(4) 0.0020(4) -0.0010(4) N2 0.0216(6) 0.0285(6) 0.0223(6) 0.0015(5) 0.0005(5) -0.0035(5) C1 0.0180(6) 0.0228(6) 0.0228(7) 0.0013(5) 0.0018(5) -0.0008(5) C2 0.0215(7) 0.0241(7) 0.0344(8) 0.0014(6) 0.0023(6) 0.0003(6) C3 0.0228(7) 0.0316(8) 0.0389(9) 0.0097(7) 0.0007(6) 0.0035(6) C4 0.0233(7) 0.0419(9) 0.0284(8) 0.0071(7) -0.0029(6) -0.0012(7) C5 0.0266(8) 0.0359(8) 0.0251(7) -0.0015(6) -0.0013(6) -0.0035(6) C6 0.0228(7) 0.0261(7) 0.0226(7) -0.0004(5) 0.0014(5) -0.0020(5) C7 0.0345(9) 0.0245(7) 0.0450(10) -0.0050(7) -0.0038(7) 0.0043(7) C8 0.0863(19) 0.0543(14) 0.0606(15) -0.0247(12) 0.0372(14) -0.0184(13) C9 0.094(2) 0.0278(9) 0.0746(17) -0.0098(10) 0.0347(15) -0.0056(11) C10 0.0329(8) 0.0231(7) 0.0244(7) -0.0036(6) -0.0005(6) -0.0003(6) C11 0.0374(10) 0.0324(9) 0.0611(13) -0.0040(9) 0.0113(9) 0.0043(8) C12 0.0469(11) 0.0279(8) 0.0487(11) -0.0041(8) -0.0041(9) -0.0066(8) C13 0.0207(6) 0.0230(6) 0.0237(7) -0.0019(5) 0.0040(5) -0.0009(5) C14 0.0225(7) 0.0364(8) 0.0308(8) 0.0024(7) 0.0065(6) -0.0051(6) C15 0.0346(8) 0.0400(9) 0.0185(7) -0.0072(6) 0.0050(6) -0.0058(7) C16 0.0504(11) 0.0357(9) 0.0352(9) -0.0131(8) 0.0115(8) -0.0030(8) C17 0.0410(10) 0.0641(13) 0.0249(8) -0.0133(9) -0.0012(7) -0.0141(10) C18 0.0278(8) 0.0308(8) 0.0270(7) 0.0096(6) 0.0052(6) 0.0011(6) C19 0.0378(9) 0.0245(7) 0.0473(11) 0.0042(7) 0.0072(8) 0.0002(7) C20 0.0499(12) 0.0563(12) 0.0369(10) 0.0249(9) 0.0122(9) 0.0074(10) C21 0.0221(7) 0.0244(7) 0.0219(6) 0.0004(5) 0.0016(5) -0.0049(5) C22 0.0198(7) 0.0351(8) 0.0250(7) 0.0021(6) 0.0035(5) -0.0003(6) C23 0.0289(8) 0.0521(11) 0.0312(9) -0.0121(8) 0.0047(7) 0.0053(8) C24 0.0237(8) 0.0539(11) 0.0320(8) 0.0139(8) 0.0034(6) -0.0063(8) C25 0.0211(7) 0.0371(8) 0.0365(9) 0.0079(7) 0.0095(6) 0.0034(6) C26 0.0412(10) 0.0389(10) 0.0605(13) 0.0060(9) 0.0274(9) 0.0102(8) C27 0.0589(14) 0.0437(12) 0.097(2) 0.0265(13) 0.0461(15) 0.0232(11) C28 0.0459(13) 0.0783(18) 0.086(2) 0.0548(17) 0.0260(13) 0.0260(12) C29 0.0302(10) 0.0859(18) 0.0514(13) 0.0378(13) 0.0019(9) 0.0043(11) C30 0.0245(8) 0.0503(10) 0.0370(9) 0.0158(8) 0.0001(7) -0.0039(7) C31 0.0211(7) 0.0309(7) 0.0250(7) 0.0021(6) 0.0008(5) -0.0042(6) C32 0.0356(9) 0.0475(10) 0.0266(8) 0.0139(8) -0.0051(7) -0.0033(8) B1 0.0217(7) 0.0158(6) 0.0169(7) -0.0002(5) 0.0019(5) 0.0004(5) F1A 0.072(2) 0.0313(14) 0.0317(14) -0.0017(11) 0.0036(13) 0.0258(13) F2A 0.0456(17) 0.0336(13) 0.113(6) 0.016(2) -0.021(2) 0.0100(11) F3A 0.097(4) 0.067(3) 0.0251(16) 0.0194(17) 0.0150(19) 0.045(3) F1B 0.158(9) 0.122(8) 0.046(3) 0.035(4) 0.042(4) 0.114(8) F2B 0.065(3) 0.0381(18) 0.082(5) 0.021(2) -0.018(3) 0.0157(17) F3B 0.112(4) 0.047(3) 0.064(5) 0.042(3) -0.010(3) -0.009(3) F4A 0.059(3) 0.210(9) 0.037(2) -0.040(3) -0.0020(17) -0.050(4) F5A 0.044(2) 0.041(2) 0.084(4) -0.015(2) -0.022(2) -0.0052(15) F6A 0.072(4) 0.0247(18) 0.124(6) 0.026(2) -0.053(4) -0.025(2) F4B 0.0602(17) 0.0446(15) 0.0570(19) -0.0264(13) -0.0056(13) -0.0094(11) F5B 0.108(4) 0.0271(14) 0.110(4) 0.015(2) -0.080(4) -0.020(2) F6B 0.0542(17) 0.082(3) 0.093(2) -0.027(2) 0.0220(16) -0.0362(17) F7A 0.050(2) 0.057(3) 0.132(5) 0.062(3) -0.035(3) -0.0260(19) F8A 0.145(6) 0.146(6) 0.0349(18) -0.029(3) 0.019(3) -0.125(5) F9A 0.068(3) 0.0588(19) 0.148(6) 0.000(3) 0.077(3) -0.0150(19) F7B 0.076(3) 0.0259(17) 0.210(9) 0.022(3) 0.045(5) -0.0027(18) F9B 0.165(8) 0.144(8) 0.047(3) -0.033(3) 0.046(4) -0.132(7) F8B 0.041(2) 0.088(4) 0.126(7) 0.071(4) -0.050(3) -0.044(2) F10 0.0948(12) 0.0893(12) 0.0384(7) 0.0323(8) 0.0063(7) 0.0152(9) F11 0.0880(11) 0.0808(10) 0.0221(5) -0.0153(6) 0.0101(6) -0.0332(9) F12 0.0553(8) 0.1294(14) 0.0249(6) -0.0021(7) 0.0113(5) -0.0476(9) F13 0.0446(6) 0.0367(6) 0.0343(6) 0.0026(5) -0.0032(5) 0.0091(5) F14 0.0515(7) 0.0793(9) 0.0173(5) 0.0074(5) 0.0071(4) 0.0133(6) F15 0.0434(6) 0.0507(7) 0.0353(6) -0.0006(5) -0.0084(5) -0.0135(5) F16 0.0401(7) 0.1736(19) 0.0441(8) -0.0125(10) 0.0092(6) 0.0411(10) F17 0.0581(8) 0.0550(8) 0.0704(9) -0.0183(7) 0.0280(7) 0.0153(6) F18 0.0635(9) 0.0539(8) 0.1406(16) 0.0259(9) 0.0691(10) 0.0124(7) F19 0.0493(7) 0.0395(6) 0.0717(8) 0.0157(6) 0.0394(6) 0.0161(5) F20 0.0547(8) 0.0860(10) 0.0545(8) -0.0169(7) 0.0188(6) -0.0456(8) F21 0.0389(6) 0.0651(8) 0.0487(7) 0.0356(6) 0.0179(5) 0.0151(6) F22 0.1819(19) 0.0329(7) 0.1034(13) 0.0311(8) 0.1036(14) 0.0543(10) F23 0.0466(7) 0.0244(5) 0.0858(10) 0.0204(6) -0.0184(6) -0.0150(5) F24 0.0688(8) 0.0372(6) 0.0438(7) 0.0225(5) -0.0228(6) -0.0177(6) C33 0.0261(7) 0.0160(5) 0.0171(6) -0.0004(5) 0.0057(5) 0.0003(5) C34 0.0310(7) 0.0197(6) 0.0182(6) 0.0025(5) 0.0048(5) 0.0025(6) C35 0.0422(9) 0.0182(6) 0.0253(7) 0.0052(6) 0.0076(6) 0.0061(6) C36 0.0498(10) 0.0155(6) 0.0341(9) -0.0001(6) 0.0113(7) -0.0024(6) C37 0.0368(9) 0.0198(6) 0.0299(8) -0.0044(6) 0.0058(6) -0.0060(6) C38 0.0282(7) 0.0178(6) 0.0241(7) -0.0019(5) 0.0034(5) 0.0002(5) C39 0.0605(13) 0.0244(8) 0.0327(9) 0.0073(7) 0.0050(8) 0.0125(8) C40 0.0456(11) 0.0317(9) 0.0555(12) -0.0148(9) 0.0037(9) -0.0131(8) C41 0.0179(6) 0.0192(6) 0.0186(6) 0.0002(5) 0.0019(5) 0.0028(5) C42 0.0209(6) 0.0220(6) 0.0202(6) 0.0013(5) 0.0017(5) 0.0009(5) C43 0.0189(6) 0.0266(7) 0.0258(7) 0.0002(6) 0.0010(5) -0.0023(5) C44 0.0195(7) 0.0342(8) 0.0230(7) -0.0035(6) -0.0011(5) -0.0024(6) C45 0.0224(7) 0.0358(8) 0.0178(6) -0.0009(6) 0.0028(5) -0.0015(6) C46 0.0214(7) 0.0259(7) 0.0199(6) 0.0002(5) 0.0033(5) -0.0021(5) C47 0.0314(9) 0.0367(9) 0.0333(9) 0.0027(7) -0.0018(7) -0.0113(7) C48 0.0379(10) 0.0623(12) 0.0185(7) -0.0011(8) 0.0014(6) -0.0153(9) C49 0.0251(7) 0.0147(5) 0.0192(6) -0.0009(5) 0.0050(5) -0.0004(5) C50 0.0251(7) 0.0193(6) 0.0178(6) -0.0020(5) 0.0041(5) -0.0017(5) C51 0.0316(8) 0.0208(6) 0.0172(6) -0.0013(5) 0.0039(5) -0.0008(5) C52 0.0385(9) 0.0250(7) 0.0210(7) -0.0010(6) 0.0114(6) 0.0010(6) C53 0.0299(8) 0.0244(7) 0.0269(7) -0.0024(6) 0.0116(6) 0.0026(6) C54 0.0274(7) 0.0206(6) 0.0224(7) 0.0000(5) 0.0056(5) 0.0029(5) C55 0.0369(9) 0.0359(8) 0.0166(6) -0.0001(6) 0.0037(6) 0.0000(7) C56 0.0361(9) 0.0419(10) 0.0346(9) 0.0002(8) 0.0151(7) 0.0097(8) C57 0.0209(6) 0.0154(5) 0.0149(5) -0.0009(5) -0.0004(4) -0.0006(5) C58 0.0222(6) 0.0159(5) 0.0190(6) 0.0015(5) 0.0015(5) -0.0004(5) C59 0.0197(6) 0.0201(6) 0.0189(6) 0.0006(5) 0.0013(5) -0.0002(5) C60 0.0226(7) 0.0193(6) 0.0207(6) -0.0011(5) 0.0002(5) 0.0037(5) C61 0.0268(7) 0.0143(5) 0.0172(6) -0.0001(5) -0.0012(5) 0.0004(5) C62 0.0229(6) 0.0162(5) 0.0162(6) -0.0008(5) 0.0011(5) -0.0018(5) C63 0.0233(7) 0.0265(7) 0.0279(7) 0.0034(6) 0.0060(6) 0.0022(6) C64 0.0352(8) 0.0176(6) 0.0277(7) 0.0022(6) 0.0046(6) 0.0040(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 Pd1 C21 2.0657(14) . ? Pd1 N2 2.0881(13) . ? Pd1 N1 2.1572(12) . ? Pd1 P1 2.1893(4) . ? P1 O1 1.6820(11) . ? P1 C18 1.8197(17) . ? P1 C15 1.8233(17) . ? O1 C13 1.3510(18) . ? N1 C13 1.2796(19) . ? N1 C1 1.4415(19) . ? N2 C31 1.135(2) . ? C1 C6 1.404(2) . ? C1 C2 1.405(2) . ? C2 C3 1.399(2) . ? C2 C7 1.514(2) . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(2) . ? C4 H4 0.9500 . ? C5 C6 1.398(2) . ? C5 H5 0.9500 . ? C6 C10 1.522(2) . ? C7 C8 1.516(3) . ? C7 C9 1.531(3) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.520(3) . ? C10 C12 1.528(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.491(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.530(3) . ? C15 C17 1.532(3) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.529(3) . ? C18 C20 1.535(2) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.543(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C25 1.525(2) . ? C22 C23 1.533(2) . ? C22 C24 1.547(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.393(3) . ? C25 C30 1.405(3) . ? C26 C27 1.394(3) . ? C26 H26 0.9500 . ? C27 C28 1.376(4) . ? C27 H27 0.9500 . ? C28 C29 1.385(4) . ? C28 H28 0.9500 . ? C29 C30 1.390(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.457(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? B1 C41 1.632(2) . ? B1 C33 1.634(2) . ? B1 C49 1.635(2) . ? B1 C57 1.636(2) . ? F1A C39 1.378(4) . ? F2A C39 1.309(4) . ? F3A C39 1.298(6) . ? F1B C39 1.272(6) . ? F2B C39 1.379(6) . ? F3B C39 1.336(7) . ? F4A C40 1.398(4) . ? F5A C40 1.376(5) . ? F6A C40 1.233(4) . ? F4B C40 1.362(3) . ? F5B C40 1.221(4) . ? F6B C40 1.368(4) . ? F7A C47 1.267(3) . ? F8A C47 1.284(4) . ? F9A C47 1.340(4) . ? F7B C47 1.341(5) . ? F9B C47 1.255(5) . ? F8B C47 1.269(5) . ? F10 C48 1.333(3) . ? F11 C48 1.331(2) . ? F12 C48 1.327(2) . ? F13 C55 1.349(2) . ? F14 C55 1.3316(18) . ? F15 C55 1.343(2) . ? F16 C56 1.314(2) . ? F17 C56 1.337(2) . ? F18 C56 1.320(2) . ? F19 C63 1.3306(19) . ? F20 C63 1.333(2) . ? F21 C63 1.3230(19) . ? F22 C64 1.313(2) . ? F23 C64 1.337(2) . ? F24 C64 1.323(2) . ? C33 C34 1.396(2) . ? C33 C38 1.403(2) . ? C34 C35 1.394(2) . ? C34 H34 0.9500 . ? C35 C36 1.386(3) . ? C35 C39 1.499(2) . ? C36 C37 1.385(2) . ? C36 H36 0.9500 . ? C37 C38 1.388(2) . ? C37 C40 1.504(3) . ? C38 H38 0.9500 . ? C41 C42 1.402(2) . ? C41 C46 1.404(2) . ? C42 C43 1.394(2) . ? C42 H42 0.9500 . ? C43 C44 1.390(2) . ? C43 C47 1.499(2) . ? C44 C45 1.385(2) . ? C44 H44 0.9500 . ? C45 C46 1.389(2) . ? C45 C48 1.498(2) . ? C46 H46 0.9500 . ? C49 C50 1.397(2) . ? C49 C54 1.408(2) . ? C50 C51 1.397(2) . ? C50 H50 0.9500 . ? C51 C52 1.385(2) . ? C51 C55 1.496(2) . ? C52 C53 1.390(2) . ? C52 H52 0.9500 . ? C53 C54 1.389(2) . ? C53 C56 1.503(2) . ? C54 H54 0.9500 . ? C57 C58 1.4019(19) . ? C57 C62 1.4027(18) . ? C58 C59 1.395(2) . ? C58 H58 0.9500 . ? C59 C60 1.391(2) . ? C59 C63 1.499(2) . ? C60 C61 1.390(2) . ? C60 H60 0.9500 . ? C61 C62 1.386(2) . ? C61 C64 1.496(2) . ? C62 H62 0.9501 . ? 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 C21 Pd1 N2 88.73(5) . . ? C21 Pd1 N1 176.91(5) . . ? N2 Pd1 N1 92.63(5) . . ? C21 Pd1 P1 96.72(4) . . ? N2 Pd1 P1 172.55(4) . . ? N1 Pd1 P1 81.68(3) . . ? O1 P1 C18 99.49(7) . . ? O1 P1 C15 98.60(7) . . ? C18 P1 C15 110.03(8) . . ? O1 P1 Pd1 101.72(4) . . ? C18 P1 Pd1 121.43(5) . . ? C15 P1 Pd1 119.62(6) . . ? C13 O1 P1 119.82(9) . . ? C13 N1 C1 120.67(13) . . ? C13 N1 Pd1 116.93(10) . . ? C1 N1 Pd1 122.36(9) . . ? C31 N2 Pd1 171.24(13) . . ? C6 C1 C2 122.44(14) . . ? C6 C1 N1 119.46(13) . . ? C2 C1 N1 117.89(13) . . ? C3 C2 C1 117.63(15) . . ? C3 C2 C7 120.58(15) . . ? C1 C2 C7 121.78(15) . . ? C4 C3 C2 120.99(16) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.45(16) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 121.21(16) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 117.29(15) . . ? C5 C6 C10 120.96(14) . . ? C1 C6 C10 121.71(13) . . ? C2 C7 C8 111.01(16) . . ? C2 C7 C9 113.03(17) . . ? C8 C7 C9 109.76(18) . . ? C2 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C9 C7 H7 107.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.4 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.4 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C6 110.45(14) . . ? C11 C10 C12 110.03(15) . . ? C6 C10 C12 113.55(14) . . ? C11 C10 H10 107.5 . . ? C6 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.4 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 O1 119.66(13) . . ? N1 C13 C14 128.09(15) . . ? O1 C13 C14 112.25(13) . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 111.45(17) . . ? C16 C15 P1 109.29(12) . . ? C17 C15 P1 112.73(13) . . ? C16 C15 H15 107.7 . . ? C17 C15 H15 107.7 . . ? P1 C15 H15 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.4 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 111.11(16) . . ? C19 C18 P1 108.36(12) . . ? C20 C18 P1 113.79(13) . . ? C19 C18 H18 107.8 . . ? C20 C18 H18 107.8 . . ? P1 C18 H18 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.6 . . ? C18 C20 H20B 109.4 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Pd1 117.37(10) . . ? C22 C21 H21A 108.0 . . ? Pd1 C21 H21A 108.0 . . ? C22 C21 H21B 107.9 . . ? Pd1 C21 H21B 107.9 . . ? H21A C21 H21B 107.2 . . ? C25 C22 C23 112.80(15) . . ? C25 C22 C21 111.31(13) . . ? C23 C22 C21 110.88(13) . . ? C25 C22 C24 107.80(13) . . ? C23 C22 C24 106.71(14) . . ? C21 C22 C24 107.01(14) . . ? C22 C23 H23A 109.4 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.4 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 117.88(18) . . ? C26 C25 C22 122.76(18) . . ? C30 C25 C22 119.33(16) . . ? C25 C26 C27 120.4(2) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 121.1(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 119.3(2) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 121.1(2) . . ? C29 C30 H30 119.4 . . ? C25 C30 H30 119.5 . . ? N2 C31 C32 178.03(17) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C41 B1 C33 114.22(12) . . ? C41 B1 C49 113.99(12) . . ? C33 B1 C49 103.29(11) . . ? C41 B1 C57 102.50(11) . . ? C33 B1 C57 112.04(11) . . ? C49 B1 C57 111.10(11) . . ? C34 C33 C38 116.56(13) . . ? C34 C33 B1 124.40(13) . . ? C38 C33 B1 118.47(12) . . ? C35 C34 C33 121.37(15) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C36 C35 C34 121.12(15) . . ? C36 C35 C39 118.49(15) . . ? C34 C35 C39 120.38(16) . . ? C37 C36 C35 118.30(14) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.9 . . ? C36 C37 C38 120.66(16) . . ? C36 C37 C40 119.76(15) . . ? C38 C37 C40 119.54(16) . . ? C37 C38 C33 121.99(15) . . ? C37 C38 H38 119.0 . . ? C33 C38 H38 119.0 . . ? F1B C39 F3A 121.9(5) . . ? F1B C39 F2A 73.3(6) . . ? F3A C39 F2A 111.3(4) . . ? F1B C39 F3B 109.2(6) . . ? F2A C39 F3B 127.7(4) . . ? F3A C39 F1A 102.6(3) . . ? F2A C39 F1A 103.9(3) . . ? F3B C39 F1A 83.9(4) . . ? F1B C39 F2B 108.1(6) . . ? F3A C39 F2B 78.3(3) . . ? F3B C39 F2B 99.2(4) . . ? F1A C39 F2B 132.8(4) . . ? F1B C39 C35 115.5(3) . . ? F3A C39 C35 114.1(3) . . ? F2A C39 C35 113.5(2) . . ? F3B C39 C35 111.5(4) . . ? F1A C39 C35 110.3(2) . . ? F2B C39 C35 112.0(2) . . ? F5B C40 F6A 121.6(3) . . ? F5B C40 F4B 112.1(3) . . ? F6A C40 F4B 61.5(4) . . ? F5B C40 F6B 111.7(4) . . ? F4B C40 F6B 99.6(3) . . ? F6A C40 F5A 103.9(4) . . ? F4B C40 F5A 137.3(3) . . ? F6B C40 F5A 77.9(3) . . ? F5B C40 F4A 61.0(4) . . ? F6A C40 F4A 106.4(5) . . ? F4B C40 F4A 55.7(3) . . ? F6B C40 F4A 137.9(3) . . ? F5A C40 F4A 97.8(4) . . ? F5B C40 C37 115.7(2) . . ? F6A C40 C37 121.1(3) . . ? F4B C40 C37 108.6(2) . . ? F6B C40 C37 107.9(2) . . ? F5A C40 C37 112.7(3) . . ? F4A C40 C37 112.2(2) . . ? C42 C41 C46 115.85(13) . . ? C42 C41 B1 123.34(12) . . ? C46 C41 B1 119.92(12) . . ? C43 C42 C41 122.00(13) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C44 C43 C42 120.89(14) . . ? C44 C43 C47 119.60(14) . . ? C42 C43 C47 119.49(14) . . ? C45 C44 C43 117.99(14) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? C44 C45 C46 121.07(14) . . ? C44 C45 C48 119.32(14) . . ? C46 C45 C48 119.61(15) . . ? C45 C46 C41 122.18(14) . . ? C45 C46 H46 118.9 . . ? C41 C46 H46 118.9 . . ? F9B C47 F7A 62.6(5) . . ? F9B C47 F8B 108.9(5) . . ? F7A C47 F8B 128.6(3) . . ? F9B C47 F8A 126.5(4) . . ? F7A C47 F8A 110.7(4) . . ? F7A C47 F9A 103.7(4) . . ? F8B C47 F9A 74.1(4) . . ? F8A C47 F9A 101.9(4) . . ? F9B C47 F7B 106.0(5) . . ? F7A C47 F7B 46.1(4) . . ? F8B C47 F7B 101.2(5) . . ? F8A C47 F7B 72.9(5) . . ? F9A C47 F7B 137.8(3) . . ? F9B C47 C43 115.8(3) . . ? F7A C47 C43 114.7(2) . . ? F8B C47 C43 113.9(3) . . ? F8A C47 C43 114.3(3) . . ? F9A C47 C43 110.3(2) . . ? F7B C47 C43 109.8(3) . . ? F12 C48 F11 107.86(17) . . ? F12 C48 F10 105.35(19) . . ? F11 C48 F10 105.03(17) . . ? F12 C48 C45 112.80(15) . . ? F11 C48 C45 112.81(17) . . ? F10 C48 C45 112.40(16) . . ? C50 C49 C54 115.88(13) . . ? C50 C49 B1 121.79(12) . . ? C54 C49 B1 121.97(13) . . ? C49 C50 C51 122.30(14) . . ? C49 C50 H50 118.8 . . ? C51 C50 H50 118.9 . . ? C52 C51 C50 120.80(15) . . ? C52 C51 C55 121.68(14) . . ? C50 C51 C55 117.50(14) . . ? C51 C52 C53 117.91(14) . . ? C51 C52 H52 121.1 . . ? C53 C52 H52 121.0 . . ? C54 C53 C52 121.27(14) . . ? C54 C53 C56 120.40(16) . . ? C52 C53 C56 118.33(14) . . ? C53 C54 C49 121.82(15) . . ? C53 C54 H54 119.1 . . ? C49 C54 H54 119.1 . . ? F14 C55 F15 107.20(14) . . ? F14 C55 F13 106.37(14) . . ? F15 C55 F13 105.15(14) . . ? F14 C55 C51 113.22(15) . . ? F15 C55 C51 112.48(14) . . ? F13 C55 C51 111.88(13) . . ? F16 C56 F18 108.6(2) . . ? F16 C56 F17 105.66(17) . . ? F18 C56 F17 103.85(16) . . ? F16 C56 C53 113.58(15) . . ? F18 C56 C53 112.25(16) . . ? F17 C56 C53 112.21(17) . . ? C58 C57 C62 116.11(12) . . ? C58 C57 B1 124.12(12) . . ? C62 C57 B1 119.52(12) . . ? C59 C58 C57 121.90(13) . . ? C59 C58 H58 119.0 . . ? C57 C58 H58 119.0 . . ? C60 C59 C58 120.86(13) . . ? C60 C59 C63 119.53(13) . . ? C58 C59 C63 119.56(13) . . ? C61 C60 C59 117.92(13) . . ? C61 C60 H60 121.0 . . ? C59 C60 H60 121.0 . . ? C62 C61 C60 121.10(13) . . ? C62 C61 C64 118.56(13) . . ? C60 C61 C64 120.34(13) . . ? C61 C62 C57 122.10(13) . . ? C61 C62 H62 119.0 . . ? C57 C62 H62 118.9 . . ? F21 C63 F19 106.90(14) . . ? F21 C63 F20 106.89(15) . . ? F19 C63 F20 105.54(15) . . ? F21 C63 C59 112.65(13) . . ? F19 C63 C59 112.82(13) . . ? F20 C63 C59 111.57(13) . . ? F22 C64 F24 106.80(17) . . ? F22 C64 F23 106.42(16) . . ? F24 C64 F23 104.65(14) . . ? F22 C64 C61 113.05(14) . . ? F24 C64 C61 112.71(13) . . ? F23 C64 C61 112.59(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pd1 P1 O1 -173.92(6) . . . . ? N1 Pd1 P1 O1 3.40(5) . . . . ? C21 Pd1 P1 C18 77.16(8) . . . . ? N1 Pd1 P1 C18 -105.51(7) . . . . ? C21 Pd1 P1 C15 -66.85(8) . . . . ? N1 Pd1 P1 C15 110.48(7) . . . . ? C18 P1 O1 C13 120.67(12) . . . . ? C15 P1 O1 C13 -127.21(12) . . . . ? Pd1 P1 O1 C13 -4.40(11) . . . . ? N2 Pd1 N1 C13 172.10(11) . . . . ? P1 Pd1 N1 C13 -3.07(10) . . . . ? N2 Pd1 N1 C1 -5.56(11) . . . . ? P1 Pd1 N1 C1 179.27(11) . . . . ? C13 N1 C1 C6 85.65(18) . . . . ? Pd1 N1 C1 C6 -96.78(14) . . . . ? C13 N1 C1 C2 -99.48(17) . . . . ? Pd1 N1 C1 C2 78.09(15) . . . . ? C6 C1 C2 C3 -0.5(2) . . . . ? N1 C1 C2 C3 -175.20(13) . . . . ? C6 C1 C2 C7 -179.14(15) . . . . ? N1 C1 C2 C7 6.1(2) . . . . ? C1 C2 C3 C4 0.6(2) . . . . ? C7 C2 C3 C4 179.29(16) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C4 C5 C6 C1 0.1(2) . . . . ? C4 C5 C6 C10 177.74(15) . . . . ? C2 C1 C6 C5 0.1(2) . . . . ? N1 C1 C6 C5 174.75(13) . . . . ? C2 C1 C6 C10 -177.45(14) . . . . ? N1 C1 C6 C10 -2.8(2) . . . . ? C3 C2 C7 C8 -82.6(2) . . . . ? C1 C2 C7 C8 96.0(2) . . . . ? C3 C2 C7 C9 41.2(2) . . . . ? C1 C2 C7 C9 -140.17(19) . . . . ? C5 C6 C10 C11 -93.55(19) . . . . ? C1 C6 C10 C11 83.93(19) . . . . ? C5 C6 C10 C12 30.6(2) . . . . ? C1 C6 C10 C12 -151.93(16) . . . . ? C1 N1 C13 O1 178.86(12) . . . . ? Pd1 N1 C13 O1 1.16(18) . . . . ? C1 N1 C13 C14 -1.3(2) . . . . ? Pd1 N1 C13 C14 -178.99(13) . . . . ? P1 O1 C13 N1 2.47(19) . . . . ? P1 O1 C13 C14 -177.40(11) . . . . ? O1 P1 C15 C16 73.59(13) . . . . ? C18 P1 C15 C16 177.04(12) . . . . ? Pd1 P1 C15 C16 -35.22(14) . . . . ? O1 P1 C15 C17 -161.89(14) . . . . ? C18 P1 C15 C17 -58.44(16) . . . . ? Pd1 P1 C15 C17 89.31(14) . . . . ? O1 P1 C18 C19 -66.12(12) . . . . ? C15 P1 C18 C19 -168.97(11) . . . . ? Pd1 P1 C18 C19 43.97(13) . . . . ? O1 P1 C18 C20 57.99(15) . . . . ? C15 P1 C18 C20 -44.85(16) . . . . ? Pd1 P1 C18 C20 168.09(12) . . . . ? N2 Pd1 C21 C22 87.68(11) . . . . ? Pd1 C21 C22 C25 83.93(15) . . . . ? Pd1 C21 C22 C23 -42.51(17) . . . . ? Pd1 C21 C22 C24 -158.52(11) . . . . ? C23 C22 C25 C26 0.7(2) . . . . ? C21 C22 C25 C26 -124.66(17) . . . . ? C24 C22 C25 C26 118.27(18) . . . . ? C23 C22 C25 C30 -177.18(15) . . . . ? C21 C22 C25 C30 57.44(19) . . . . ? C24 C22 C25 C30 -59.6(2) . . . . ? C30 C25 C26 C27 -0.9(3) . . . . ? C22 C25 C26 C27 -178.78(17) . . . . ? C25 C26 C27 C28 0.5(3) . . . . ? C26 C27 C28 C29 0.5(3) . . . . ? C27 C28 C29 C30 -1.0(3) . . . . ? C28 C29 C30 C25 0.7(3) . . . . ? C26 C25 C30 C29 0.3(3) . . . . ? C22 C25 C30 C29 178.27(16) . . . . ? C41 B1 C33 C34 25.21(19) . . . . ? C49 B1 C33 C34 -99.15(15) . . . . ? C57 B1 C33 C34 141.20(13) . . . . ? C41 B1 C33 C38 -163.75(12) . . . . ? C49 B1 C33 C38 71.89(15) . . . . ? C57 B1 C33 C38 -47.76(17) . . . . ? C38 C33 C34 C35 0.3(2) . . . . ? B1 C33 C34 C35 171.48(14) . . . . ? C33 C34 C35 C36 -0.3(2) . . . . ? C33 C34 C35 C39 -179.53(15) . . . . ? C34 C35 C36 C37 -0.3(2) . . . . ? C39 C35 C36 C37 179.01(16) . . . . ? C35 C36 C37 C38 0.8(2) . . . . ? C35 C36 C37 C40 -176.64(17) . . . . ? C36 C37 C38 C33 -0.8(2) . . . . ? C40 C37 C38 C33 176.63(16) . . . . ? C34 C33 C38 C37 0.3(2) . . . . ? B1 C33 C38 C37 -171.49(14) . . . . ? C36 C35 C39 F1B -72.9(11) . . . . ? C34 C35 C39 F1B 106.4(11) . . . . ? C36 C35 C39 F3A 76.1(5) . . . . ? C34 C35 C39 F3A -104.7(5) . . . . ? C36 C35 C39 F2A -154.9(5) . . . . ? C34 C35 C39 F2A 24.4(6) . . . . ? C36 C35 C39 F3B 52.5(6) . . . . ? C34 C35 C39 F3B -128.2(5) . . . . ? C36 C35 C39 F1A -38.8(3) . . . . ? C34 C35 C39 F1A 140.4(3) . . . . ? C36 C35 C39 F2B 162.7(6) . . . . ? C34 C35 C39 F2B -18.0(6) . . . . ? C36 C37 C40 F5B 165.3(4) . . . . ? C38 C37 C40 F5B -12.2(5) . . . . ? C36 C37 C40 F6A -29.1(6) . . . . ? C38 C37 C40 F6A 153.5(5) . . . . ? C36 C37 C40 F4B 38.2(3) . . . . ? C38 C37 C40 F4B -139.2(2) . . . . ? C36 C37 C40 F6B -68.8(3) . . . . ? C38 C37 C40 F6B 113.7(3) . . . . ? C36 C37 C40 F5A -152.8(3) . . . . ? C38 C37 C40 F5A 29.7(4) . . . . ? C36 C37 C40 F4A 97.9(5) . . . . ? C38 C37 C40 F4A -79.6(5) . . . . ? C33 B1 C41 C42 -143.75(13) . . . . ? C49 B1 C41 C42 -25.33(19) . . . . ? C57 B1 C41 C42 94.83(15) . . . . ? C33 B1 C41 C46 47.47(18) . . . . ? C49 B1 C41 C46 165.90(13) . . . . ? C57 B1 C41 C46 -73.94(15) . . . . ? C46 C41 C42 C43 1.0(2) . . . . ? B1 C41 C42 C43 -168.23(13) . . . . ? C41 C42 C43 C44 0.2(2) . . . . ? C41 C42 C43 C47 178.72(15) . . . . ? C42 C43 C44 C45 -1.2(2) . . . . ? C47 C43 C44 C45 -179.65(15) . . . . ? C43 C44 C45 C46 0.9(2) . . . . ? C43 C44 C45 C48 -178.75(16) . . . . ? C44 C45 C46 C41 0.4(2) . . . . ? C48 C45 C46 C41 179.99(16) . . . . ? C42 C41 C46 C45 -1.3(2) . . . . ? B1 C41 C46 C45 168.33(14) . . . . ? C44 C43 C47 F9B -159.0(8) . . . . ? C42 C43 C47 F9B 22.5(8) . . . . ? C44 C43 C47 F7A 130.9(5) . . . . ? C42 C43 C47 F7A -47.6(6) . . . . ? C44 C43 C47 F8B -31.6(6) . . . . ? C42 C43 C47 F8B 149.9(6) . . . . ? C44 C43 C47 F8A 1.5(6) . . . . ? C42 C43 C47 F8A -177.0(5) . . . . ? C44 C43 C47 F9A -112.6(4) . . . . ? C42 C43 C47 F9A 68.9(5) . . . . ? C44 C43 C47 F7B 81.0(7) . . . . ? C42 C43 C47 F7B -97.5(7) . . . . ? C44 C45 C48 F12 -150.72(18) . . . . ? C46 C45 C48 F12 29.6(3) . . . . ? C44 C45 C48 F11 -28.2(3) . . . . ? C46 C45 C48 F11 152.17(17) . . . . ? C44 C45 C48 F10 90.3(2) . . . . ? C46 C45 C48 F10 -89.3(2) . . . . ? C41 B1 C49 C50 142.23(13) . . . . ? C33 B1 C49 C50 -93.27(15) . . . . ? C57 B1 C49 C50 27.03(18) . . . . ? C41 B1 C49 C54 -44.93(18) . . . . ? C33 B1 C49 C54 79.58(16) . . . . ? C57 B1 C49 C54 -160.13(13) . . . . ? C54 C49 C50 C51 0.8(2) . . . . ? B1 C49 C50 C51 174.05(13) . . . . ? C49 C50 C51 C52 -0.6(2) . . . . ? C49 C50 C51 C55 177.73(14) . . . . ? C50 C51 C52 C53 -0.2(2) . . . . ? C55 C51 C52 C53 -178.42(15) . . . . ? C51 C52 C53 C54 0.7(2) . . . . ? C51 C52 C53 C56 -179.16(15) . . . . ? C52 C53 C54 C49 -0.4(2) . . . . ? C56 C53 C54 C49 179.41(15) . . . . ? C50 C49 C54 C53 -0.3(2) . . . . ? B1 C49 C54 C53 -173.54(14) . . . . ? C52 C51 C55 F14 0.0(2) . . . . ? C50 C51 C55 F14 -178.33(14) . . . . ? C52 C51 C55 F15 -121.76(16) . . . . ? C50 C51 C55 F15 59.96(19) . . . . ? C52 C51 C55 F13 120.14(16) . . . . ? C50 C51 C55 F13 -58.14(19) . . . . ? C54 C53 C56 F16 3.0(3) . . . . ? C52 C53 C56 F16 -177.12(18) . . . . ? C54 C53 C56 F18 126.77(19) . . . . ? C52 C53 C56 F18 -53.4(2) . . . . ? C54 C53 C56 F17 -116.72(18) . . . . ? C52 C53 C56 F17 63.1(2) . . . . ? C41 B1 C57 C58 93.91(15) . . . . ? C33 B1 C57 C58 -28.99(18) . . . . ? C49 B1 C57 C58 -143.95(13) . . . . ? C41 B1 C57 C62 -80.03(14) . . . . ? C33 B1 C57 C62 157.08(12) . . . . ? C49 B1 C57 C62 42.12(17) . . . . ? C62 C57 C58 C59 0.3(2) . . . . ? B1 C57 C58 C59 -173.84(13) . . . . ? C57 C58 C59 C60 -0.3(2) . . . . ? C57 C58 C59 C63 -177.69(13) . . . . ? C58 C59 C60 C61 -0.6(2) . . . . ? C63 C59 C60 C61 176.80(13) . . . . ? C59 C60 C61 C62 1.5(2) . . . . ? C59 C60 C61 C64 -177.41(13) . . . . ? C60 C61 C62 C57 -1.6(2) . . . . ? C64 C61 C62 C57 177.32(13) . . . . ? C58 C57 C62 C61 0.7(2) . . . . ? B1 C57 C62 C61 175.09(13) . . . . ? C60 C59 C63 F21 137.64(15) . . . . ? C58 C59 C63 F21 -45.0(2) . . . . ? C60 C59 C63 F19 16.5(2) . . . . ? C58 C59 C63 F19 -166.12(14) . . . . ? C60 C59 C63 F20 -102.13(17) . . . . ? C58 C59 C63 F20 75.26(19) . . . . ? C62 C61 C64 F22 156.03(18) . . . . ? C60 C61 C64 F22 -25.0(2) . . . . ? C62 C61 C64 F24 -82.72(18) . . . . ? C60 C61 C64 F24 96.21(17) . . . . ? C62 C61 C64 F23 35.4(2) . . . . ? C60 C61 C64 F23 -145.69(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.911 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.064 data_8b _database_code_depnum_ccdc_archive 'CCDC 876284' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C33 H50 N2 O2 P Pd' _chemical_formula_sum 'C65 H62 B F24 N2 O2 P Pd' _chemical_formula_weight 1507.35 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3365(9) _cell_length_b 13.3092(11) _cell_length_c 21.2562(18) _cell_angle_alpha 106.599(4) _cell_angle_beta 96.181(4) _cell_angle_gamma 92.774(4) _cell_volume 3313.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7890 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.86 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8869 _exptl_absorpt_correction_T_max 0.9675 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11840 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.25 _reflns_number_total 11840 _reflns_number_gt 9326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0832P)^2^+6.0209P] 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 11840 _refine_ls_number_parameters 931 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1605 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.004 _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 0.65804(3) 0.11481(3) 0.774431(18) 0.02491(11) Uani 1 1 d . . . P1 P 0.58580(9) 0.26595(9) 0.78223(6) 0.0237(2) Uani 1 1 d . . . O1 O 0.5316(3) 0.2480(2) 0.70331(15) 0.0284(7) Uani 1 1 d . . . O2 O 0.8056(5) 0.2174(5) 0.8829(3) 0.0882(17) Uani 1 1 d . . . N1 N 0.5731(3) 0.0774(3) 0.6748(2) 0.0282(9) Uani 1 1 d . . . N2 N 0.7307(3) -0.0275(3) 0.7564(2) 0.0319(9) Uani 1 1 d . . . C1 C 0.5613(4) -0.0281(4) 0.6296(2) 0.0288(10) Uani 1 1 d . . . C2 C 0.6504(4) -0.0626(4) 0.5952(2) 0.0319(11) Uani 1 1 d . . . C3 C 0.6434(4) -0.1677(4) 0.5583(2) 0.0352(11) Uani 1 1 d . . . H3 H 0.7007 -0.1936 0.5350 0.042 Uiso 1 1 calc R . . C4 C 0.5528(5) -0.2345(4) 0.5557(2) 0.0379(12) Uani 1 1 d . . . H4 H 0.5498 -0.3046 0.5306 0.045 Uiso 1 1 calc R . . C5 C 0.4675(4) -0.1989(4) 0.5894(2) 0.0341(12) Uani 1 1 d . . . H5 H 0.4071 -0.2452 0.5868 0.041 Uiso 1 1 calc R . . C6 C 0.4694(4) -0.0947(4) 0.6275(2) 0.0308(11) Uani 1 1 d . . . C7 C 0.7495(4) 0.0129(4) 0.5983(3) 0.0388(12) Uani 1 1 d . . . H7 H 0.7625 0.0620 0.6431 0.047 Uiso 1 1 calc R . . C8 C 0.8532(5) -0.0437(5) 0.5851(4) 0.0620(19) Uani 1 1 d . . . H8A H 0.8699 -0.0798 0.6177 0.093 Uiso 1 1 calc R . . H8B H 0.9130 0.0067 0.5874 0.093 Uiso 1 1 calc R . . H8C H 0.8419 -0.0937 0.5418 0.093 Uiso 1 1 calc R . . C9 C 0.7262(6) 0.0780(5) 0.5491(3) 0.0603(18) Uani 1 1 d . . . H9A H 0.7121 0.0314 0.5048 0.090 Uiso 1 1 calc R . . H9B H 0.7886 0.1261 0.5526 0.090 Uiso 1 1 calc R . . H9C H 0.6635 0.1166 0.5595 0.090 Uiso 1 1 calc R . . C10 C 0.3784(4) -0.0581(4) 0.6694(2) 0.0299(11) Uani 1 1 d . . . H10 H 0.3779 0.0182 0.6779 0.036 Uiso 1 1 calc R . . C11 C 0.4031(5) -0.0804(4) 0.7357(3) 0.0405(12) Uani 1 1 d . . . H11A H 0.4060 -0.1548 0.7285 0.061 Uiso 1 1 calc R . . H11B H 0.3467 -0.0559 0.7627 0.061 Uiso 1 1 calc R . . H11C H 0.4723 -0.0447 0.7577 0.061 Uiso 1 1 calc R . . C12 C 0.2652(5) -0.1084(5) 0.6352(3) 0.0506(15) Uani 1 1 d . . . H12A H 0.2537 -0.0994 0.5919 0.076 Uiso 1 1 calc R . . H12B H 0.2102 -0.0754 0.6609 0.076 Uiso 1 1 calc R . . H12C H 0.2607 -0.1821 0.6316 0.076 Uiso 1 1 calc R . . C13 C 0.5239(4) 0.1508(4) 0.6587(2) 0.0304(11) Uani 1 1 d . . . C14 C 0.4543(5) 0.1465(4) 0.5965(3) 0.0405(13) Uani 1 1 d . . . H14A H 0.4545 0.0782 0.5653 0.061 Uiso 1 1 calc R . . H14B H 0.4825 0.1991 0.5783 0.061 Uiso 1 1 calc R . . H14C H 0.3809 0.1593 0.6056 0.061 Uiso 1 1 calc R . . C15 C 0.6774(4) 0.3837(4) 0.7950(2) 0.0303(11) Uani 1 1 d . . . H15 H 0.6396 0.4312 0.7741 0.036 Uiso 1 1 calc R . . C16 C 0.7077(5) 0.4409(4) 0.8686(3) 0.0416(13) Uani 1 1 d . . . H16A H 0.7452 0.3955 0.8898 0.062 Uiso 1 1 calc R . . H16B H 0.6425 0.4601 0.8884 0.062 Uiso 1 1 calc R . . H16C H 0.7546 0.5032 0.8738 0.062 Uiso 1 1 calc R . . C17 C 0.7789(4) 0.3534(4) 0.7617(3) 0.0411(13) Uani 1 1 d . . . H17A H 0.8273 0.4153 0.7683 0.062 Uiso 1 1 calc R . . H17B H 0.7582 0.3211 0.7152 0.062 Uiso 1 1 calc R . . H17C H 0.8156 0.3048 0.7806 0.062 Uiso 1 1 calc R . . C18 C 0.4666(4) 0.3036(4) 0.8249(2) 0.0269(10) Uani 1 1 d . . . H18 H 0.4897 0.3209 0.8726 0.032 Uiso 1 1 calc R . . C19 C 0.4188(4) 0.4001(4) 0.8111(3) 0.0384(12) Uani 1 1 d . . . H19A H 0.3991 0.3864 0.7643 0.058 Uiso 1 1 calc R . . H19B H 0.4724 0.4594 0.8271 0.058 Uiso 1 1 calc R . . H19C H 0.3550 0.4153 0.8332 0.058 Uiso 1 1 calc R . . C20 C 0.3807(4) 0.2105(4) 0.8055(3) 0.0331(11) Uani 1 1 d . . . H20A H 0.3225 0.2268 0.8325 0.050 Uiso 1 1 calc R . . H20B H 0.4135 0.1498 0.8122 0.050 Uiso 1 1 calc R . . H20C H 0.3519 0.1962 0.7598 0.050 Uiso 1 1 calc R . . C21 C 0.7368(4) 0.1555(4) 0.8668(3) 0.0352(11) Uani 1 1 d U . . C22 C 0.6932(6) 0.0812(7) 0.9052(4) 0.075(2) Uani 1 1 d U . . H22A H 0.6197 0.0525 0.8850 0.090 Uiso 1 1 calc R . . H22B H 0.7388 0.0228 0.9003 0.090 Uiso 1 1 calc R . . C23 C 0.6905(7) 0.1301(7) 0.9744(4) 0.077(2) Uani 1 1 d U . . C24 C 0.8005(5) 0.1683(7) 1.0057(4) 0.075(2) Uani 1 1 d . . . H24A H 0.8487 0.1136 0.9927 0.112 Uiso 1 1 calc R . . H24B H 0.8018 0.1888 1.0529 0.112 Uiso 1 1 calc R . . H24C H 0.8242 0.2279 0.9922 0.112 Uiso 1 1 calc R . . C25 C 0.6527(9) 0.0377(7) 1.0031(5) 0.096(3) Uani 1 1 d . . . H25A H 0.5920 -0.0047 0.9741 0.145 Uiso 1 1 calc R . . H25B H 0.6312 0.0671 1.0462 0.145 Uiso 1 1 calc R . . H25C H 0.7123 -0.0052 1.0062 0.145 Uiso 1 1 calc R . . C26 C 0.6054(5) 0.2083(4) 0.9773(4) 0.0601(19) Uani 1 1 d . . . C27 C 0.6321(5) 0.3141(5) 1.0053(4) 0.0561(17) Uani 1 1 d . . . H27 H 0.7052 0.3399 1.0153 0.067 Uiso 1 1 calc R . . C28 C 0.5515(5) 0.3827(4) 1.0187(3) 0.0477(14) Uani 1 1 d . . . H28 H 0.5704 0.4543 1.0378 0.057 Uiso 1 1 calc R . . C29 C 0.4437(5) 0.3452(5) 1.0039(3) 0.0474(14) Uani 1 1 d . . . H29 H 0.3895 0.3913 1.0140 0.057 Uiso 1 1 calc R . . C30 C 0.4154(5) 0.2411(4) 0.9745(3) 0.0398(13) Uani 1 1 d . . . H30 H 0.3421 0.2160 0.9639 0.048 Uiso 1 1 calc R . . C31 C 0.4956(5) 0.1731(4) 0.9603(3) 0.0450(14) Uani 1 1 d . . . H31 H 0.4759 0.1022 0.9389 0.054 Uiso 1 1 calc R . . C32 C 0.7638(4) -0.1076(4) 0.7393(3) 0.0325(11) Uani 1 1 d . . . C33 C 0.8056(5) -0.2094(4) 0.7174(3) 0.0443(13) Uani 1 1 d . . . H33A H 0.7840 -0.2520 0.7443 0.066 Uiso 1 1 calc R . . H33B H 0.8840 -0.2011 0.7212 0.066 Uiso 1 1 calc R . . H33C H 0.7766 -0.2430 0.6720 0.066 Uiso 1 1 calc R . . B1 B 0.1058(4) 0.6096(4) 0.7468(2) 0.0199(10) Uani 1 1 d . . . C34 C 0.0725(3) 0.7159(3) 0.7993(2) 0.0204(9) Uani 1 1 d . . . C35 C 0.1131(3) 0.8168(3) 0.8002(2) 0.0238(9) Uani 1 1 d . . . H35 H 0.1660 0.8229 0.7731 0.029 Uiso 1 1 calc R . . C36 C 0.0772(4) 0.9074(3) 0.8398(2) 0.0272(10) Uani 1 1 d . . . C37 C -0.0005(4) 0.9030(4) 0.8815(2) 0.0275(10) Uani 1 1 d . . . H37 H -0.0241 0.9641 0.9083 0.033 Uiso 1 1 calc R . . C38 C -0.0422(3) 0.8043(3) 0.8821(2) 0.0245(9) Uani 1 1 d . . . C39 C -0.0069(3) 0.7137(3) 0.8417(2) 0.0222(9) Uani 1 1 d . . . H39 H -0.0369 0.6489 0.8428 0.027 Uiso 1 1 calc R . . C40 C 0.1253(5) 1.0123(4) 0.8391(3) 0.0393(13) Uani 1 1 d . . . C41 C -0.1279(4) 0.7973(4) 0.9257(2) 0.0315(11) Uani 1 1 d . . . C42 C 0.0902(3) 0.5037(3) 0.7707(2) 0.0211(9) Uani 1 1 d . . . C43 C 0.1082(3) 0.5045(3) 0.8372(2) 0.0226(9) Uani 1 1 d . . . H43 H 0.1250 0.5685 0.8698 0.027 Uiso 1 1 calc R . . C44 C 0.1016(3) 0.4124(4) 0.8559(2) 0.0301(11) Uani 1 1 d . A . C45 C 0.0780(4) 0.3160(4) 0.8093(3) 0.0387(13) Uani 1 1 d . . . H45 H 0.0731 0.2546 0.8218 0.046 Uiso 1 1 calc R . . C46 C 0.0620(4) 0.3125(4) 0.7437(3) 0.0387(13) Uani 1 1 d . . . C47 C 0.0678(4) 0.4051(3) 0.7249(2) 0.0271(10) Uani 1 1 d . . . H47 H 0.0563 0.4003 0.6802 0.033 Uiso 1 1 calc R . . C48 C 0.1176(4) 0.4158(4) 0.9272(3) 0.0402(13) Uani 1 1 d . . . C49 C 0.0379(6) 0.2082(4) 0.6923(3) 0.063(2) Uani 1 1 d . . . C50 C 0.0241(3) 0.5997(3) 0.6785(2) 0.0203(9) Uani 1 1 d . . . C51 C -0.0824(3) 0.5510(3) 0.6677(2) 0.0226(9) Uani 1 1 d . . . H51 H -0.1052 0.5214 0.6992 0.027 Uiso 1 1 calc R . . C52 C -0.1547(3) 0.5449(4) 0.6124(2) 0.0283(10) Uani 1 1 d . B . C53 C -0.1245(4) 0.5870(3) 0.5633(2) 0.0271(10) Uani 1 1 d . . . H53 H -0.1729 0.5822 0.5256 0.032 Uiso 1 1 calc R . . C54 C -0.0202(4) 0.6364(3) 0.5724(2) 0.0261(10) Uani 1 1 d . . . C55 C 0.0511(3) 0.6432(3) 0.6285(2) 0.0231(9) Uani 1 1 d . . . H55 H 0.1200 0.6780 0.6335 0.028 Uiso 1 1 calc R . . C56 C -0.2659(3) 0.4936(3) 0.60519(17) 0.0415(13) Uani 1 1 d D . . C57 C 0.0155(4) 0.6840(4) 0.5215(2) 0.0353(12) Uani 1 1 d . . . C58 C 0.2337(3) 0.6135(3) 0.7342(2) 0.0212(9) Uani 1 1 d . . . C59 C 0.3207(3) 0.6701(3) 0.7811(2) 0.0212(9) Uani 1 1 d . . . H59 H 0.3055 0.7153 0.8209 0.025 Uiso 1 1 calc R . . C60 C 0.4287(3) 0.6598(3) 0.7693(2) 0.0224(9) Uani 1 1 d . . . C61 C 0.4556(3) 0.5929(3) 0.7118(2) 0.0249(10) Uani 1 1 d . . . H61 H 0.5282 0.5870 0.7042 0.030 Uiso 1 1 calc R . . C62 C 0.3714(3) 0.5347(3) 0.6655(2) 0.0238(9) Uani 1 1 d . . . C63 C 0.2634(3) 0.5461(3) 0.6764(2) 0.0230(9) Uani 1 1 d . . . H63 H 0.2085 0.5073 0.6440 0.028 Uiso 1 1 calc R . . C64 C 0.5215(3) 0.7207(3) 0.8195(2) 0.0276(10) Uani 1 1 d . . . C65 C 0.3986(4) 0.4610(4) 0.6032(2) 0.0304(11) Uani 1 1 d . . . F1 F 0.1368(3) 1.0167(2) 0.77815(16) 0.0527(9) Uani 1 1 d . . . F2 F 0.2267(3) 1.0361(3) 0.87257(19) 0.0649(11) Uani 1 1 d . . . F3 F 0.0673(3) 1.0912(2) 0.86628(19) 0.0664(12) Uani 1 1 d . . . F4 F -0.1430(4) 0.7051(3) 0.9342(2) 0.0925(17) Uani 1 1 d . . . F5 F -0.2252(3) 0.8169(4) 0.90024(19) 0.0814(14) Uani 1 1 d . . . F6 F -0.1097(3) 0.8680(3) 0.98337(16) 0.0654(11) Uani 1 1 d . . . F7A F 0.1757(7) 0.3335(6) 0.9348(4) 0.0618(15) Uani 0.50 1 d PDU A 1 F8A F 0.1631(7) 0.4966(6) 0.9662(4) 0.0611(19) Uani 0.50 1 d PDU A 1 F9A F 0.0193(6) 0.3911(7) 0.9441(4) 0.059(2) Uani 0.50 1 d PDU A 1 F7B F 0.2220(7) 0.4007(7) 0.9477(4) 0.0687(16) Uani 0.50 1 d PDU A 2 F8B F 0.1121(6) 0.5192(5) 0.9706(3) 0.0503(19) Uani 0.50 1 d PDU A 2 F9B F 0.0546(7) 0.3562(6) 0.9477(4) 0.0635(18) Uani 0.50 1 d PDU A 2 F10 F -0.0184(4) 0.2136(3) 0.6370(2) 0.0868(16) Uani 1 1 d . . . F11 F -0.0223(4) 0.1397(3) 0.7138(2) 0.0925(16) Uani 1 1 d . . . F12 F 0.1241(4) 0.1604(4) 0.6778(3) 0.1043(18) Uani 1 1 d . . . F13 F -0.0433(4) 0.6468(4) 0.46325(18) 0.0940(17) Uani 1 1 d . . . F14 F 0.1190(3) 0.6663(3) 0.51069(17) 0.0553(9) Uani 1 1 d . . . F15 F 0.0199(3) 0.7881(3) 0.54058(19) 0.0643(11) Uani 1 1 d . . . F16A F -0.3428(4) 0.5640(4) 0.5964(3) 0.0468(12) Uani 0.50 1 d PDU B 1 F17A F -0.2965(5) 0.4766(5) 0.6596(2) 0.0465(13) Uani 0.50 1 d PDU B 1 F18A F -0.2980(5) 0.4133(4) 0.5554(2) 0.0550(14) Uani 0.50 1 d PDU B 1 F16B F -0.3176(5) 0.5284(5) 0.6548(2) 0.0563(14) Uani 0.50 1 d PDU B 2 F17B F -0.2575(5) 0.3891(4) 0.6042(3) 0.0513(13) Uani 0.50 1 d PDU B 2 F18B F -0.3250(5) 0.4790(5) 0.5484(2) 0.0579(14) Uani 0.50 1 d PDU B 2 F19 F 0.4810(2) 0.4045(2) 0.61310(15) 0.0402(7) Uani 1 1 d . . . F20 F 0.4285(4) 0.5104(3) 0.56027(17) 0.0667(11) Uani 1 1 d . . . F21 F 0.3147(2) 0.3918(3) 0.57022(16) 0.0531(9) Uani 1 1 d . . . F22 F 0.5825(2) 0.6576(2) 0.84520(16) 0.0470(8) Uani 1 1 d . . . F23 F 0.4892(2) 0.7921(3) 0.87005(15) 0.0495(8) Uani 1 1 d . . . F24 F 0.5911(2) 0.7722(2) 0.79287(14) 0.0427(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02084(18) 0.01665(18) 0.0377(2) 0.00785(14) 0.00743(14) -0.00209(13) P1 0.0272(6) 0.0152(5) 0.0295(6) 0.0071(5) 0.0078(5) -0.0034(5) O1 0.0399(19) 0.0149(15) 0.0309(17) 0.0074(13) 0.0072(14) -0.0018(13) O2 0.088(4) 0.084(4) 0.083(4) 0.022(3) -0.010(3) -0.017(3) N1 0.026(2) 0.0165(19) 0.039(2) 0.0044(17) 0.0078(17) -0.0053(16) N2 0.029(2) 0.024(2) 0.040(2) 0.0054(18) 0.0022(18) 0.0019(18) C1 0.033(3) 0.019(2) 0.031(3) 0.0040(19) 0.005(2) -0.005(2) C2 0.031(3) 0.026(3) 0.036(3) 0.004(2) 0.007(2) -0.004(2) C3 0.042(3) 0.027(3) 0.034(3) 0.003(2) 0.012(2) 0.003(2) C4 0.059(3) 0.018(2) 0.032(3) 0.000(2) 0.010(2) -0.007(2) C5 0.043(3) 0.021(2) 0.036(3) 0.006(2) 0.009(2) -0.012(2) C6 0.036(3) 0.024(2) 0.032(3) 0.008(2) 0.007(2) -0.005(2) C7 0.035(3) 0.029(3) 0.045(3) -0.002(2) 0.016(2) -0.005(2) C8 0.044(3) 0.045(4) 0.082(5) -0.011(3) 0.029(3) -0.009(3) C9 0.062(4) 0.056(4) 0.061(4) 0.019(3) 0.011(3) -0.031(3) C10 0.033(3) 0.019(2) 0.038(3) 0.009(2) 0.008(2) -0.0094(19) C11 0.043(3) 0.040(3) 0.043(3) 0.016(2) 0.013(2) 0.003(2) C12 0.037(3) 0.056(4) 0.054(4) 0.013(3) 0.004(3) -0.020(3) C13 0.034(3) 0.022(2) 0.035(3) 0.008(2) 0.011(2) -0.008(2) C14 0.057(3) 0.027(3) 0.036(3) 0.011(2) -0.001(2) -0.006(2) C15 0.035(3) 0.019(2) 0.036(3) 0.008(2) 0.007(2) -0.011(2) C16 0.049(3) 0.026(3) 0.043(3) 0.003(2) 0.004(2) -0.013(2) C17 0.040(3) 0.035(3) 0.049(3) 0.014(2) 0.015(2) -0.016(2) C18 0.028(2) 0.025(2) 0.030(2) 0.0110(19) 0.0070(19) 0.0014(19) C19 0.040(3) 0.032(3) 0.046(3) 0.013(2) 0.010(2) 0.009(2) C20 0.023(2) 0.035(3) 0.041(3) 0.011(2) 0.006(2) -0.003(2) C21 0.031(2) 0.028(2) 0.046(3) 0.010(2) 0.006(2) 0.002(2) C22 0.062(4) 0.106(5) 0.069(4) 0.043(3) 0.005(3) 0.026(3) C23 0.072(4) 0.072(4) 0.085(4) 0.018(3) 0.002(3) 0.011(3) C24 0.041(4) 0.112(7) 0.086(5) 0.051(5) 0.004(3) 0.029(4) C25 0.139(9) 0.089(7) 0.081(6) 0.047(5) 0.026(6) 0.043(6) C26 0.035(3) 0.024(3) 0.115(6) 0.017(3) -0.009(3) -0.001(2) C27 0.040(3) 0.031(3) 0.091(5) 0.015(3) -0.007(3) -0.006(3) C28 0.073(4) 0.023(3) 0.044(3) 0.005(2) 0.007(3) 0.003(3) C29 0.058(4) 0.049(4) 0.039(3) 0.011(3) 0.017(3) 0.019(3) C30 0.039(3) 0.042(3) 0.042(3) 0.018(3) 0.008(2) 0.001(2) C31 0.046(3) 0.027(3) 0.062(4) 0.019(3) -0.004(3) -0.006(2) C32 0.024(2) 0.031(3) 0.039(3) 0.007(2) -0.002(2) 0.004(2) C33 0.047(3) 0.034(3) 0.050(3) 0.006(3) 0.009(3) 0.018(3) B1 0.017(2) 0.018(2) 0.026(3) 0.007(2) 0.0069(19) -0.0021(19) C34 0.020(2) 0.018(2) 0.024(2) 0.0075(17) 0.0031(17) -0.0014(17) C35 0.025(2) 0.020(2) 0.027(2) 0.0071(18) 0.0091(18) -0.0028(18) C36 0.030(2) 0.020(2) 0.033(3) 0.0091(19) 0.0073(19) -0.0007(19) C37 0.029(2) 0.024(2) 0.029(2) 0.0059(19) 0.0065(19) 0.0049(19) C38 0.020(2) 0.025(2) 0.028(2) 0.0059(19) 0.0063(18) 0.0012(18) C39 0.018(2) 0.021(2) 0.029(2) 0.0101(18) 0.0028(17) -0.0028(17) C40 0.059(4) 0.020(3) 0.041(3) 0.007(2) 0.023(3) -0.001(2) C41 0.030(3) 0.030(3) 0.032(3) 0.004(2) 0.010(2) -0.002(2) C42 0.0096(19) 0.020(2) 0.035(2) 0.0089(19) 0.0056(17) -0.0015(16) C43 0.014(2) 0.020(2) 0.035(2) 0.0095(19) 0.0046(17) -0.0033(17) C44 0.017(2) 0.033(3) 0.047(3) 0.022(2) 0.0052(19) -0.0019(19) C45 0.032(3) 0.026(3) 0.060(4) 0.022(2) -0.009(2) -0.006(2) C46 0.040(3) 0.016(2) 0.053(3) 0.007(2) -0.014(2) -0.003(2) C47 0.027(2) 0.021(2) 0.034(3) 0.0104(19) 0.0013(19) -0.0002(19) C48 0.037(3) 0.048(3) 0.046(3) 0.031(3) 0.007(2) 0.002(3) C49 0.098(6) 0.021(3) 0.060(4) 0.011(3) -0.023(4) -0.005(3) C50 0.019(2) 0.014(2) 0.026(2) 0.0019(17) 0.0074(17) -0.0010(16) C51 0.019(2) 0.024(2) 0.029(2) 0.0113(19) 0.0096(17) 0.0000(18) C52 0.021(2) 0.030(3) 0.035(3) 0.010(2) 0.0053(19) -0.0015(19) C53 0.024(2) 0.027(2) 0.030(2) 0.008(2) 0.0034(18) 0.0017(19) C54 0.032(2) 0.022(2) 0.024(2) 0.0055(18) 0.0112(19) 0.0006(19) C55 0.021(2) 0.016(2) 0.032(2) 0.0059(18) 0.0106(18) -0.0030(17) C56 0.030(3) 0.055(4) 0.040(3) 0.020(3) -0.001(2) -0.009(3) C57 0.043(3) 0.028(3) 0.038(3) 0.014(2) 0.008(2) -0.005(2) C58 0.014(2) 0.018(2) 0.031(2) 0.0079(18) 0.0050(17) -0.0025(17) C59 0.023(2) 0.015(2) 0.024(2) 0.0049(17) 0.0042(17) -0.0041(17) C60 0.019(2) 0.017(2) 0.032(2) 0.0089(18) 0.0053(18) -0.0045(17) C61 0.016(2) 0.023(2) 0.037(3) 0.010(2) 0.0073(18) -0.0006(18) C62 0.020(2) 0.020(2) 0.031(2) 0.0069(19) 0.0086(18) -0.0008(18) C63 0.019(2) 0.019(2) 0.029(2) 0.0049(18) 0.0058(17) -0.0033(17) C64 0.021(2) 0.023(2) 0.036(3) 0.007(2) 0.0041(19) -0.0060(19) C65 0.020(2) 0.032(3) 0.037(3) 0.005(2) 0.0077(19) 0.005(2) F1 0.089(3) 0.0276(16) 0.0508(19) 0.0173(14) 0.0324(18) 0.0035(16) F2 0.073(3) 0.0368(19) 0.081(3) 0.0191(18) 0.004(2) -0.0286(18) F3 0.105(3) 0.0197(16) 0.088(3) 0.0163(17) 0.063(2) 0.0179(18) F4 0.142(4) 0.046(2) 0.124(4) 0.041(2) 0.113(4) 0.031(2) F5 0.0232(17) 0.162(5) 0.064(2) 0.040(3) 0.0111(16) -0.003(2) F6 0.056(2) 0.079(3) 0.0425(19) -0.0167(18) 0.0294(16) -0.0244(19) F7A 0.076(4) 0.068(4) 0.056(3) 0.039(3) 0.003(3) 0.026(3) F8A 0.081(5) 0.062(4) 0.044(3) 0.027(3) -0.005(4) -0.003(4) F9A 0.048(4) 0.079(5) 0.067(3) 0.044(4) 0.020(4) 0.007(3) F7B 0.075(4) 0.082(4) 0.054(3) 0.028(3) -0.002(3) 0.023(3) F8B 0.068(5) 0.051(4) 0.036(3) 0.023(3) 0.000(4) 0.002(4) F9B 0.072(4) 0.069(5) 0.065(3) 0.044(3) 0.017(3) 0.003(3) F10 0.146(4) 0.0280(18) 0.067(3) 0.0108(17) -0.050(3) -0.021(2) F11 0.137(4) 0.035(2) 0.095(3) 0.024(2) -0.022(3) -0.036(2) F12 0.105(4) 0.062(3) 0.106(4) -0.038(3) 0.001(3) 0.033(3) F13 0.092(3) 0.146(4) 0.047(2) 0.056(3) -0.020(2) -0.069(3) F14 0.063(2) 0.056(2) 0.064(2) 0.0326(18) 0.0421(18) 0.0137(17) F15 0.100(3) 0.039(2) 0.077(3) 0.0350(18) 0.054(2) 0.0212(19) F16A 0.0374(18) 0.0477(19) 0.0556(19) 0.0159(15) 0.0058(15) 0.0022(15) F17A 0.0405(19) 0.055(2) 0.0506(19) 0.0257(15) 0.0079(15) -0.0035(16) F18A 0.0446(19) 0.052(2) 0.061(2) 0.0050(16) 0.0111(16) -0.0030(16) F16B 0.0449(19) 0.056(2) 0.063(2) 0.0063(16) 0.0163(16) 0.0007(17) F17B 0.0439(19) 0.0525(19) 0.0561(19) 0.0149(16) 0.0090(16) -0.0089(16) F18B 0.0515(19) 0.063(2) 0.060(2) 0.0212(16) 0.0014(16) -0.0036(16) F19 0.0270(15) 0.0298(16) 0.0539(19) -0.0041(14) 0.0048(13) 0.0059(12) F20 0.112(3) 0.050(2) 0.051(2) 0.0181(17) 0.051(2) 0.024(2) F21 0.0224(15) 0.061(2) 0.051(2) -0.0226(16) 0.0054(13) -0.0004(14) F22 0.0399(17) 0.0416(18) 0.057(2) 0.0209(16) -0.0173(14) -0.0084(14) F23 0.0306(16) 0.053(2) 0.0451(18) -0.0139(15) 0.0017(13) -0.0098(14) F24 0.0299(15) 0.0506(19) 0.0472(18) 0.0201(15) -0.0007(13) -0.0242(14) _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 C21 2.006(5) . ? Pd1 N2 2.089(4) . ? Pd1 N1 2.167(4) . ? Pd1 P1 2.2097(12) . ? P1 O1 1.683(3) . ? P1 C15 1.823(4) . ? P1 C18 1.826(5) . ? O1 C13 1.360(6) . ? O2 C21 1.107(7) . ? N1 C13 1.283(6) . ? N1 C1 1.448(6) . ? N2 C32 1.135(6) . ? C1 C6 1.394(6) . ? C1 C2 1.409(7) . ? C2 C3 1.388(7) . ? C2 C7 1.527(6) . ? C3 C4 1.381(7) . ? C4 C5 1.364(8) . ? C5 C6 1.390(7) . ? C6 C10 1.520(7) . ? C7 C8 1.528(8) . ? C7 C9 1.550(9) . ? C10 C11 1.525(7) . ? C10 C12 1.529(7) . ? C13 C14 1.481(7) . ? C15 C17 1.520(7) . ? C15 C16 1.527(7) . ? C18 C20 1.522(6) . ? C18 C19 1.527(7) . ? C21 C22 1.562(9) . ? C22 C23 1.433(11) . ? C23 C24 1.445(10) . ? C23 C26 1.506(10) . ? C23 C25 1.593(12) . ? C26 C27 1.371(8) . ? C26 C31 1.387(8) . ? C27 C28 1.380(9) . ? C28 C29 1.368(9) . ? C29 C30 1.358(8) . ? C30 C31 1.372(8) . ? C32 C33 1.441(7) . ? B1 C58 1.629(6) . ? B1 C34 1.634(6) . ? B1 C42 1.639(6) . ? B1 C50 1.645(6) . ? C34 C35 1.404(6) . ? C34 C39 1.406(6) . ? C35 C36 1.383(7) . ? C36 C37 1.383(6) . ? C36 C40 1.495(6) . ? C37 C38 1.391(6) . ? C38 C39 1.385(6) . ? C38 C41 1.495(6) . ? C40 F3 1.329(6) . ? C40 F1 1.336(6) . ? C40 F2 1.346(7) . ? C41 F4 1.298(6) . ? C41 F6 1.304(6) . ? C41 F5 1.332(6) . ? C42 C47 1.386(6) . ? C42 C43 1.403(6) . ? C43 C44 1.394(6) . ? C44 C45 1.374(7) . ? C44 C48 1.494(7) . ? C45 C46 1.373(8) . ? C46 C47 1.402(7) . ? C46 C49 1.494(8) . ? C48 F8A 1.221(12) . ? C48 F9B 1.279(11) . ? C48 F9A 1.353(10) . ? C48 F7B 1.358(10) . ? C48 F7A 1.376(9) . ? C48 F8B 1.431(11) . ? C49 F12 1.286(9) . ? C49 F10 1.322(7) . ? C49 F11 1.356(8) . ? C50 C51 1.402(6) . ? C50 C55 1.408(6) . ? C51 C52 1.378(6) . ? C52 C53 1.392(6) . ? C52 C56 1.474(6) . ? C53 C54 1.384(6) . ? C54 C55 1.381(6) . ? C54 C57 1.495(6) . ? C56 F16B 1.276(4) . ? C56 F18A 1.281(4) . ? C56 F18B 1.301(4) . ? C56 F17A 1.329(4) . ? C56 F17B 1.395(4) . ? C56 F16A 1.400(4) . ? C57 F13 1.314(6) . ? C57 F15 1.324(6) . ? C57 F14 1.341(6) . ? C58 C63 1.395(6) . ? C58 C59 1.405(6) . ? C59 C60 1.389(6) . ? C60 C61 1.376(6) . ? C60 C64 1.503(6) . ? C61 C62 1.383(6) . ? C62 C63 1.386(6) . ? C62 C65 1.487(7) . ? C64 F23 1.327(6) . ? C64 F24 1.341(5) . ? C64 F22 1.343(6) . ? C65 F19 1.328(6) . ? C65 F20 1.338(6) . ? C65 F21 1.339(6) . ? 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 C21 Pd1 N2 88.21(19) . . ? C21 Pd1 N1 177.73(18) . . ? N2 Pd1 N1 93.79(15) . . ? C21 Pd1 P1 96.55(15) . . ? N2 Pd1 P1 173.41(12) . . ? N1 Pd1 P1 81.38(11) . . ? O1 P1 C15 99.92(19) . . ? O1 P1 C18 100.4(2) . . ? C15 P1 C18 108.5(2) . . ? O1 P1 Pd1 101.14(12) . . ? C15 P1 Pd1 118.52(18) . . ? C18 P1 Pd1 123.10(15) . . ? C13 O1 P1 120.2(3) . . ? C13 N1 C1 119.9(4) . . ? C13 N1 Pd1 117.3(3) . . ? C1 N1 Pd1 122.5(3) . . ? C32 N2 Pd1 171.9(4) . . ? C6 C1 C2 122.7(4) . . ? C6 C1 N1 119.3(4) . . ? C2 C1 N1 117.5(4) . . ? C3 C2 C1 116.9(4) . . ? C3 C2 C7 122.0(4) . . ? C1 C2 C7 121.2(4) . . ? C4 C3 C2 121.1(5) . . ? C5 C4 C3 120.8(5) . . ? C4 C5 C6 121.1(4) . . ? C5 C6 C1 117.5(5) . . ? C5 C6 C10 120.6(4) . . ? C1 C6 C10 121.8(4) . . ? C2 C7 C8 112.5(4) . . ? C2 C7 C9 110.7(4) . . ? C8 C7 C9 110.0(5) . . ? C6 C10 C11 109.3(4) . . ? C6 C10 C12 113.1(4) . . ? C11 C10 C12 110.5(4) . . ? N1 C13 O1 118.9(4) . . ? N1 C13 C14 129.2(5) . . ? O1 C13 C14 111.9(4) . . ? C17 C15 C16 111.0(4) . . ? C17 C15 P1 109.3(3) . . ? C16 C15 P1 111.3(3) . . ? C20 C18 C19 110.9(4) . . ? C20 C18 P1 109.3(3) . . ? C19 C18 P1 112.6(3) . . ? O2 C21 C22 128.7(6) . . ? O2 C21 Pd1 121.2(5) . . ? C22 C21 Pd1 109.8(4) . . ? C23 C22 C21 114.9(7) . . ? C22 C23 C24 108.9(7) . . ? C22 C23 C26 104.9(7) . . ? C24 C23 C26 118.5(7) . . ? C22 C23 C25 105.3(7) . . ? C24 C23 C25 107.0(7) . . ? C26 C23 C25 111.5(7) . . ? C27 C26 C31 118.1(6) . . ? C27 C26 C23 121.4(6) . . ? C31 C26 C23 119.9(6) . . ? C26 C27 C28 120.7(6) . . ? C29 C28 C27 120.0(5) . . ? C30 C29 C28 120.3(6) . . ? C29 C30 C31 119.7(5) . . ? C30 C31 C26 121.1(5) . . ? N2 C32 C33 179.8(7) . . ? C58 B1 C34 114.2(3) . . ? C58 B1 C42 103.3(3) . . ? C34 B1 C42 113.6(3) . . ? C58 B1 C50 111.2(3) . . ? C34 B1 C50 103.8(3) . . ? C42 B1 C50 111.0(3) . . ? C35 C34 C39 115.2(4) . . ? C35 C34 B1 121.9(4) . . ? C39 C34 B1 122.6(4) . . ? C36 C35 C34 122.3(4) . . ? C35 C36 C37 121.2(4) . . ? C35 C36 C40 119.5(4) . . ? C37 C36 C40 119.2(4) . . ? C36 C37 C38 118.0(4) . . ? C39 C38 C37 120.5(4) . . ? C39 C38 C41 120.4(4) . . ? C37 C38 C41 119.1(4) . . ? C38 C39 C34 122.7(4) . . ? F3 C40 F1 107.2(4) . . ? F3 C40 F2 106.0(5) . . ? F1 C40 F2 104.9(4) . . ? F3 C40 C36 113.4(4) . . ? F1 C40 C36 112.8(4) . . ? F2 C40 C36 112.0(4) . . ? F4 C41 F6 108.9(5) . . ? F4 C41 F5 105.3(5) . . ? F6 C41 F5 103.6(4) . . ? F4 C41 C38 113.9(4) . . ? F6 C41 C38 113.0(4) . . ? F5 C41 C38 111.4(4) . . ? C47 C42 C43 115.5(4) . . ? C47 C42 B1 121.0(4) . . ? C43 C42 B1 123.2(4) . . ? C44 C43 C42 122.1(4) . . ? C45 C44 C43 120.9(5) . . ? C45 C44 C48 118.1(4) . . ? C43 C44 C48 121.0(5) . . ? C46 C45 C44 118.4(4) . . ? C45 C46 C47 120.8(5) . . ? C45 C46 C49 119.1(5) . . ? C47 C46 C49 120.1(5) . . ? C42 C47 C46 122.3(5) . . ? F8A C48 F9B 119.5(9) . . ? F8A C48 F9A 111.7(8) . . ? F8A C48 F7B 69.6(7) . . ? F9B C48 F7B 107.1(7) . . ? F9A C48 F7B 133.4(7) . . ? F8A C48 F7A 107.8(7) . . ? F9B C48 F7A 72.7(6) . . ? F9A C48 F7A 101.9(6) . . ? F9B C48 F8B 104.9(7) . . ? F9A C48 F8B 86.7(7) . . ? F7B C48 F8B 98.6(7) . . ? F7A C48 F8B 131.4(7) . . ? F8A C48 C44 116.7(6) . . ? F9B C48 C44 119.3(7) . . ? F9A C48 C44 108.0(6) . . ? F7B C48 C44 112.2(5) . . ? F7A C48 C44 109.9(6) . . ? F8B C48 C44 112.6(5) . . ? F12 C49 F10 108.6(7) . . ? F12 C49 F11 103.3(6) . . ? F10 C49 F11 105.8(6) . . ? F12 C49 C46 113.4(6) . . ? F10 C49 C46 113.3(5) . . ? F11 C49 C46 111.6(6) . . ? C51 C50 C55 114.6(4) . . ? C51 C50 B1 121.3(4) . . ? C55 C50 B1 124.1(4) . . ? C52 C51 C50 122.9(4) . . ? C51 C52 C53 120.9(4) . . ? C51 C52 C56 119.6(4) . . ? C53 C52 C56 119.5(4) . . ? C54 C53 C52 117.8(4) . . ? C55 C54 C53 120.7(4) . . ? C55 C54 C57 119.5(4) . . ? C53 C54 C57 119.8(4) . . ? C54 C55 C50 123.0(4) . . ? F16B C56 F18A 125.4(5) . . ? F16B C56 F18B 113.8(4) . . ? F18A C56 F18B 45.4(4) . . ? F18A C56 F17A 109.3(4) . . ? F18B C56 F17A 127.8(5) . . ? F16B C56 F17B 101.9(4) . . ? F18A C56 F17B 54.7(4) . . ? F18B C56 F17B 99.4(4) . . ? F17A C56 F17B 68.7(4) . . ? F16B C56 F16A 65.9(4) . . ? F18A C56 F16A 101.3(4) . . ? F18B C56 F16A 59.1(4) . . ? F17A C56 F16A 98.4(4) . . ? F17B C56 F16A 141.8(4) . . ? F16B C56 C52 114.5(4) . . ? F18A C56 C52 119.7(4) . . ? F18B C56 C52 116.2(4) . . ? F17A C56 C52 115.7(4) . . ? F17B C56 C52 108.6(4) . . ? F16A C56 C52 109.3(4) . . ? F13 C57 F15 109.9(5) . . ? F13 C57 F14 105.3(5) . . ? F15 C57 F14 102.0(4) . . ? F13 C57 C54 113.5(4) . . ? F15 C57 C54 113.0(4) . . ? F14 C57 C54 112.2(4) . . ? C63 C58 C59 115.8(4) . . ? C63 C58 B1 118.9(4) . . ? C59 C58 B1 124.8(4) . . ? C60 C59 C58 121.3(4) . . ? C61 C60 C59 121.7(4) . . ? C61 C60 C64 117.2(4) . . ? C59 C60 C64 121.2(4) . . ? C60 C61 C62 118.1(4) . . ? C61 C62 C63 120.5(4) . . ? C61 C62 C65 119.0(4) . . ? C63 C62 C65 120.5(4) . . ? C62 C63 C58 122.7(4) . . ? F23 C64 F24 106.4(4) . . ? F23 C64 F22 106.9(4) . . ? F24 C64 F22 105.4(4) . . ? F23 C64 C60 113.6(4) . . ? F24 C64 C60 112.0(4) . . ? F22 C64 C60 112.0(4) . . ? F19 C65 F20 105.5(4) . . ? F19 C65 F21 106.1(4) . . ? F20 C65 F21 105.6(4) . . ? F19 C65 C62 113.0(4) . . ? F20 C65 C62 112.8(4) . . ? F21 C65 C62 113.1(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.039 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.104 data_9 _database_code_depnum_ccdc_archive 'CCDC 876285' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C33 H51 N O2 P Pd' _chemical_formula_sum 'C65 H63 B F24 N O2 P Pd' _chemical_formula_weight 1494.34 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.3921(5) _cell_length_b 16.3003(5) _cell_length_c 24.2674(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.0410(10) _cell_angle_gamma 90.00 _cell_volume 6577.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9856 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 30.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8847 _exptl_absorpt_correction_T_max 0.9210 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _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-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 61756 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.25 _reflns_number_total 11796 _reflns_number_gt 9965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1162P)^2^+2.1199P] 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 11796 _refine_ls_number_parameters 894 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1870 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.006 _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 0.33827(2) 0.24244(3) 0.107517(19) 0.014 Uani 1 1 d . . . P1 P 0.32589(9) 0.25932(9) 0.19314(7) 0.015 Uani 1 1 d . . . O1 O 0.4223(2) 0.2673(2) 0.23364(17) 0.016 Uani 1 1 d . . . O2 O 0.3500(2) 0.2213(3) 0.02364(18) 0.020 Uani 1 1 d . . . N1 N 0.4604(3) 0.2689(3) 0.1515(2) 0.014 Uani 1 1 d . . . C1 C 0.5206(3) 0.2759(3) 0.1214(2) 0.015 Uani 1 1 d . . . C2 C 0.5648(3) 0.2066(4) 0.1154(3) 0.018 Uani 1 1 d . . . C3 C 0.6175(4) 0.2145(4) 0.0818(3) 0.023 Uani 1 1 d . . . H3 H 0.6486 0.1686 0.0771 0.027 Uiso 1 1 calc R . . C4 C 0.6254(4) 0.2879(4) 0.0554(3) 0.025 Uani 1 1 d . . . H4 H 0.6612 0.2918 0.0326 0.030 Uiso 1 1 calc R . . C5 C 0.5808(4) 0.3560(4) 0.0622(3) 0.022 Uani 1 1 d . . . H5 H 0.5864 0.4061 0.0437 0.027 Uiso 1 1 calc R . . C6 C 0.5279(3) 0.3520(3) 0.0958(3) 0.016 Uani 1 1 d . . . C7 C 0.5543(4) 0.1235(4) 0.1409(3) 0.019 Uani 1 1 d . . . H7 H 0.5232 0.1322 0.1692 0.023 Uiso 1 1 calc R . . C8 C 0.5043(4) 0.0680(4) 0.0927(3) 0.028 Uani 1 1 d . . . H8A H 0.4530 0.0948 0.0736 0.042 Uiso 1 1 calc R . . H8B H 0.4941 0.0157 0.1092 0.042 Uiso 1 1 calc R . . H8C H 0.5338 0.0580 0.0646 0.042 Uiso 1 1 calc R . . C9 C 0.6343(4) 0.0833(4) 0.1730(3) 0.030 Uani 1 1 d . . . H9A H 0.6674 0.0771 0.1468 0.044 Uiso 1 1 calc R . . H9B H 0.6241 0.0291 0.1870 0.044 Uiso 1 1 calc R . . H9C H 0.6627 0.1177 0.2058 0.044 Uiso 1 1 calc R . . C10 C 0.4790(4) 0.4265(3) 0.1024(3) 0.018 Uani 1 1 d . . . H10 H 0.4611 0.4179 0.1376 0.021 Uiso 1 1 calc R . . C11 C 0.4030(4) 0.4342(4) 0.0504(3) 0.028 Uani 1 1 d . . . H11A H 0.4187 0.4418 0.0151 0.042 Uiso 1 1 calc R . . H11B H 0.3714 0.4816 0.0559 0.042 Uiso 1 1 calc R . . H11C H 0.3706 0.3843 0.0471 0.042 Uiso 1 1 calc R . . C12 C 0.5270(4) 0.5062(4) 0.1107(3) 0.027 Uani 1 1 d . . . H12A H 0.5765 0.4999 0.1426 0.040 Uiso 1 1 calc R . . H12B H 0.4947 0.5508 0.1195 0.040 Uiso 1 1 calc R . . H12C H 0.5407 0.5193 0.0753 0.040 Uiso 1 1 calc R . . C13 C 0.4802(3) 0.2722(3) 0.2069(3) 0.015 Uani 1 1 d . . . C14 C 0.5627(4) 0.2792(4) 0.2474(3) 0.022 Uani 1 1 d . . . H14A H 0.5820 0.2247 0.2622 0.033 Uiso 1 1 calc R . . H14B H 0.5617 0.3150 0.2796 0.033 Uiso 1 1 calc R . . H14C H 0.5988 0.3024 0.2271 0.033 Uiso 1 1 calc R . . C15 C 0.2915(4) 0.1755(4) 0.2294(3) 0.023 Uani 1 1 d . . . H15 H 0.3073 0.1879 0.2716 0.027 Uiso 1 1 calc R . . C16 C 0.1995(4) 0.1682(5) 0.2078(3) 0.030 Uani 1 1 d . . . H16A H 0.1825 0.1588 0.1661 0.045 Uiso 1 1 calc R . . H16B H 0.1752 0.2191 0.2164 0.045 Uiso 1 1 calc R . . H16C H 0.1820 0.1221 0.2271 0.045 Uiso 1 1 calc R . . C17 C 0.3327(5) 0.0957(4) 0.2209(3) 0.032 Uani 1 1 d . . . H17A H 0.3154 0.0511 0.2417 0.047 Uiso 1 1 calc R . . H17B H 0.3912 0.1023 0.2358 0.047 Uiso 1 1 calc R . . H17C H 0.3180 0.0824 0.1798 0.047 Uiso 1 1 calc R . . C18 C 0.2827(4) 0.3541(4) 0.2110(3) 0.021 Uani 1 1 d . . . H18 H 0.2245 0.3549 0.1883 0.025 Uiso 1 1 calc R . . C19 C 0.2872(4) 0.3604(4) 0.2749(3) 0.025 Uani 1 1 d . . . H19A H 0.3434 0.3556 0.2985 0.038 Uiso 1 1 calc R . . H19B H 0.2556 0.3162 0.2848 0.038 Uiso 1 1 calc R . . H19C H 0.2657 0.4135 0.2822 0.038 Uiso 1 1 calc R . . C20 C 0.3228(4) 0.4278(4) 0.1918(3) 0.025 Uani 1 1 d . . . H20A H 0.2925 0.4777 0.1940 0.038 Uiso 1 1 calc R . . H20B H 0.3237 0.4195 0.1519 0.038 Uiso 1 1 calc R . . H20C H 0.3781 0.4333 0.2170 0.038 Uiso 1 1 calc R . . C21 C 0.2216(4) 0.2127(4) 0.0667(3) 0.022 Uani 1 1 d . . . H21A H 0.2117 0.1538 0.0720 0.027 Uiso 1 1 calc R . . H21B H 0.1845 0.2457 0.0819 0.027 Uiso 1 1 calc R . . C22 C 0.2098(4) 0.2321(4) 0.0032(3) 0.026 Uani 1 1 d . . . H22A H 0.1666 0.1968 -0.0208 0.032 Uiso 1 1 calc R . . H22B H 0.1924 0.2899 -0.0043 0.032 Uiso 1 1 calc R . . C23 C 0.2845(4) 0.2192(4) -0.0142(3) 0.020 Uani 1 1 d . . . C24 C 0.2763(4) 0.2074(4) -0.0768(3) 0.021 Uani 1 1 d . . . H24A H 0.2379 0.2494 -0.0982 0.025 Uiso 1 1 calc R . . H24B H 0.2505 0.1534 -0.0880 0.025 Uiso 1 1 calc R . . C25 C 0.3506(4) 0.2109(4) -0.0994(3) 0.021 Uani 1 1 d . . . C26 C 0.3940(4) 0.2931(4) -0.0828(3) 0.029 Uani 1 1 d . . . H26A H 0.4358 0.2988 -0.1022 0.044 Uiso 1 1 calc R . . H26B H 0.4186 0.2951 -0.0410 0.044 Uiso 1 1 calc R . . H26C H 0.3552 0.3381 -0.0946 0.044 Uiso 1 1 calc R . . C27 C 0.4104(4) 0.1416(4) -0.0740(3) 0.027 Uani 1 1 d . . . H27A H 0.4526 0.1407 -0.0933 0.040 Uiso 1 1 calc R . . H27B H 0.3820 0.0889 -0.0799 0.040 Uiso 1 1 calc R . . H27C H 0.4346 0.1510 -0.0326 0.040 Uiso 1 1 calc R . . C28 C 0.3187(4) 0.2011(4) -0.1652(3) 0.022 Uani 1 1 d . . . C29 C 0.2806(4) 0.1272(4) -0.1883(3) 0.026 Uani 1 1 d . . . H29 H 0.2757 0.0845 -0.1629 0.031 Uiso 1 1 calc R . . C30 C 0.2504(4) 0.1154(4) -0.2470(3) 0.031 Uani 1 1 d . . . H30 H 0.2260 0.0645 -0.2615 0.037 Uiso 1 1 calc R . . C31 C 0.2554(4) 0.1773(5) -0.2846(3) 0.030 Uani 1 1 d . . . H31 H 0.2339 0.1695 -0.3250 0.036 Uiso 1 1 calc R . . C32 C 0.2915(4) 0.2501(5) -0.2634(3) 0.032 Uani 1 1 d . . . H32 H 0.2952 0.2925 -0.2893 0.038 Uiso 1 1 calc R . . C33 C 0.3231(4) 0.2627(4) -0.2039(3) 0.027 Uani 1 1 d . . . H33 H 0.3477 0.3136 -0.1899 0.033 Uiso 1 1 calc R . . C41 C 0.6802(4) 0.3123(4) -0.1146(3) 0.026 Uani 1 1 d D . . F1A F 0.6945(6) 0.3905(5) -0.1026(4) 0.048 Uani 0.50 1 d PDU A 1 F2A F 0.5987(5) 0.3060(6) -0.1290(4) 0.050 Uani 0.50 1 d PDU A 1 F3A F 0.6958(6) 0.2980(6) -0.1620(4) 0.055 Uani 0.50 1 d PDU A 1 F1B F 0.6267(6) 0.2800(7) -0.1586(4) 0.058 Uani 0.50 1 d PDU A 2 F2B F 0.7351(6) 0.3385(6) -0.1433(4) 0.053 Uani 0.50 1 d PDU A 2 F3B F 0.6623(6) 0.3829(6) -0.0960(4) 0.047 Uani 0.50 1 d PDU A 2 F4 F 0.6806(3) 0.0012(3) -0.0691(2) 0.053 Uani 1 1 d U A 3 F5 F 0.6254(3) 0.0422(3) -0.0074(2) 0.049 Uani 1 1 d U A 3 F6 F 0.7479(4) -0.0105(4) 0.0154(3) 0.084 Uani 1 1 d U A 3 F7 F 1.0232(3) 0.4723(3) 0.2900(2) 0.042 Uani 1 1 d U A 3 F8 F 1.0941(3) 0.3856(3) 0.2610(2) 0.045 Uani 1 1 d U A 3 F9 F 1.0051(3) 0.3444(3) 0.2995(2) 0.050 Uani 1 1 d U A 3 F10 F 0.7281(4) 0.5143(4) 0.1434(3) 0.079 Uani 1 1 d U A 3 F11 F 0.7453(5) 0.5194(5) 0.0625(3) 0.098 Uani 1 1 d U A 3 F12 F 0.8116(4) 0.5919(4) 0.1243(3) 0.082 Uani 1 1 d U A 3 F13 F 1.1697(2) -0.0011(3) 0.11019(18) 0.033 Uani 1 1 d U A 3 F14 F 1.0930(2) 0.0205(2) 0.02439(17) 0.033 Uani 1 1 d U A 3 F15 F 1.0712(3) -0.0824(2) 0.07306(19) 0.037 Uani 1 1 d U A 3 F16 F 0.9717(3) -0.0328(3) 0.2426(2) 0.044 Uani 1 1 d U A 3 F17 F 0.8753(4) 0.0522(5) 0.2223(3) 0.082 Uani 1 1 d U A 3 F18 F 0.9817(6) 0.0894(6) 0.2701(4) 0.107 Uani 1 1 d U A 3 F19 F 1.0129(4) 0.3587(4) -0.1510(3) 0.069 Uani 1 1 d U A 3 F20 F 0.9236(4) 0.2752(4) -0.1450(3) 0.072 Uani 1 1 d U A 3 F21 F 1.0418(5) 0.2367(5) -0.1237(3) 0.091 Uani 1 1 d U A 3 F22 F 1.1241(3) 0.5371(3) 0.0231(2) 0.043 Uani 1 1 d U A 3 F23 F 1.2091(2) 0.4432(3) 0.0577(2) 0.039 Uani 1 1 d U A 3 F24 F 1.1337(3) 0.4872(3) 0.1065(2) 0.045 Uani 1 1 d U A 3 C34 C 0.8314(3) 0.2286(3) 0.0202(2) 0.015 Uani 1 1 d . A 3 C35 C 0.7984(4) 0.1508(4) 0.0209(3) 0.020 Uani 1 1 d . A 3 H35 H 0.8244 0.1139 0.0509 0.024 Uiso 1 1 calc R A 3 C36 C 0.7287(4) 0.1250(4) -0.0206(3) 0.028 Uani 1 1 d . A 3 C37 C 0.6888(4) 0.1769(4) -0.0654(3) 0.026 Uani 1 1 d . A 3 H37 H 0.6415 0.1595 -0.0939 0.031 Uiso 1 1 calc R A 3 C38 C 0.7202(4) 0.2548(4) -0.0671(3) 0.021 Uani 1 1 d . A 3 C39 C 0.7899(3) 0.2793(4) -0.0251(3) 0.018 Uani 1 1 d . A 3 H39 H 0.8101 0.3329 -0.0275 0.021 Uiso 1 1 calc R A 3 C40 C 0.6956(4) 0.0406(5) -0.0190(4) 0.040 Uani 1 1 d . A 3 C42 C 0.9049(3) 0.3255(3) 0.1135(2) 0.014 Uani 1 1 d . A 3 C43 C 0.9605(3) 0.3330(3) 0.1683(3) 0.017 Uani 1 1 d . A 3 H43 H 1.0010 0.2923 0.1806 0.020 Uiso 1 1 calc R A 3 C44 C 0.9591(4) 0.3976(4) 0.2055(3) 0.019 Uani 1 1 d . A 3 C45 C 0.9018(4) 0.4584(4) 0.1892(3) 0.020 Uani 1 1 d . A 3 H45 H 0.9012 0.5032 0.2141 0.024 Uiso 1 1 calc R A 3 C46 C 0.8448(4) 0.4526(4) 0.1350(3) 0.019 Uani 1 1 d . A 3 C47 C 0.8466(3) 0.3872(3) 0.0985(3) 0.016 Uani 1 1 d . A 3 H47 H 0.8068 0.3844 0.0622 0.019 Uiso 1 1 calc R A 3 C48 C 1.0199(4) 0.3994(4) 0.2638(3) 0.025 Uani 1 1 d . A 3 C49 C 0.7811(3) 0.5179(4) 0.1174(3) 0.017 Uani 1 1 d . A 3 C50 C 0.9606(3) 0.1739(3) 0.0997(3) 0.016 Uani 1 1 d . A 3 C51 C 1.0109(3) 0.1247(3) 0.0777(3) 0.015 Uani 1 1 d . A 3 H51 H 1.0266 0.1439 0.0456 0.018 Uiso 1 1 calc R A 3 C52 C 1.0387(3) 0.0481(3) 0.1015(3) 0.018 Uani 1 1 d . A 3 C53 C 1.0185(4) 0.0186(4) 0.1491(3) 0.023 Uani 1 1 d . A 3 H53 H 1.0370 -0.0335 0.1651 0.028 Uiso 1 1 calc R A 3 C54 C 0.9706(4) 0.0671(4) 0.1727(3) 0.025 Uani 1 1 d . A 3 C55 C 0.9419(4) 0.1428(4) 0.1476(3) 0.020 Uani 1 1 d . A 3 H55 H 0.9083 0.1744 0.1641 0.024 Uiso 1 1 calc R A 3 C56 C 1.0924(4) -0.0029(4) 0.0772(3) 0.023 Uani 1 1 d . A 3 C57 C 0.9484(5) 0.0397(5) 0.2237(4) 0.043 Uani 1 1 d . A 3 C58 C 0.9738(3) 0.3009(3) 0.0316(2) 0.014 Uani 1 1 d . A 3 C59 C 0.9668(3) 0.2819(4) -0.0254(3) 0.017 Uani 1 1 d . A 3 H59 H 0.9319 0.2387 -0.0434 0.020 Uiso 1 1 calc R A 3 C60 C 1.0094(3) 0.3242(4) -0.0574(3) 0.019 Uani 1 1 d . A 3 C61 C 1.0618(3) 0.3868(4) -0.0327(3) 0.019 Uani 1 1 d . A 3 H61 H 1.0893 0.4170 -0.0546 0.023 Uiso 1 1 calc R A 3 C62 C 1.0730(3) 0.4041(3) 0.0252(3) 0.017 Uani 1 1 d . A 3 C63 C 1.0299(3) 0.3624(3) 0.0565(3) 0.015 Uani 1 1 d . A 3 H63 H 1.0387 0.3759 0.0959 0.018 Uiso 1 1 calc R A 3 C64 C 0.9973(4) 0.3011(4) -0.1188(3) 0.025 Uani 1 1 d . A 3 C65 C 1.1339(3) 0.4679(4) 0.0534(3) 0.019 Uani 1 1 d . A 3 B1 B 0.9175(4) 0.2569(4) 0.0671(3) 0.014 Uani 1 1 d . A 3 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 0.014 0.015 0.013 -0.001 0.004 0.000 P1 0.014 0.016 0.014 -0.002 0.004 -0.002 O1 0.015 0.020 0.014 0.000 0.004 -0.001 O2 0.020 0.020 0.018 0.000 0.004 0.001 N1 0.015 0.013 0.016 0.002 0.006 -0.001 C1 0.014 0.015 0.015 -0.001 0.006 -0.002 C2 0.018 0.015 0.021 -0.002 0.004 -0.001 C3 0.025 0.021 0.025 -0.004 0.012 0.002 C4 0.026 0.025 0.030 -0.005 0.017 -0.004 C5 0.028 0.017 0.026 0.000 0.014 -0.003 C6 0.019 0.014 0.015 -0.002 0.005 -0.001 C7 0.020 0.016 0.023 0.002 0.009 0.002 C8 0.032 0.018 0.031 0.000 0.005 -0.006 C9 0.026 0.022 0.039 0.006 0.006 0.003 C10 0.023 0.014 0.019 0.002 0.009 -0.002 C11 0.028 0.020 0.032 -0.001 0.004 0.006 C12 0.030 0.020 0.035 -0.005 0.017 -0.005 C13 0.016 0.010 0.019 0.002 0.005 0.001 C14 0.017 0.032 0.017 -0.003 0.005 -0.004 C15 0.024 0.022 0.024 0.001 0.011 -0.007 C16 0.025 0.037 0.031 -0.004 0.011 -0.013 C17 0.040 0.019 0.036 0.001 0.013 -0.004 C18 0.016 0.020 0.026 -0.002 0.005 0.002 C19 0.028 0.025 0.024 -0.006 0.011 0.002 C20 0.031 0.017 0.028 0.000 0.008 0.002 C21 0.017 0.027 0.021 -0.007 0.003 -0.003 C22 0.022 0.033 0.023 -0.005 0.005 0.004 C23 0.024 0.014 0.021 -0.001 0.006 0.003 C24 0.024 0.017 0.021 0.000 0.006 0.004 C25 0.026 0.017 0.020 0.002 0.009 0.001 C26 0.037 0.020 0.030 -0.002 0.011 -0.005 C27 0.032 0.025 0.025 0.003 0.010 0.010 C28 0.025 0.021 0.021 0.002 0.009 0.005 C29 0.036 0.021 0.023 -0.004 0.010 0.004 C30 0.035 0.030 0.030 -0.007 0.011 0.008 C31 0.028 0.047 0.016 -0.001 0.008 0.014 C32 0.033 0.042 0.024 0.012 0.015 0.016 C33 0.031 0.022 0.032 0.005 0.013 0.009 C41 0.032 0.024 0.017 -0.008 0.001 0.002 F1A 0.048 0.046 0.048 0.003 0.012 0.000 F2A 0.048 0.050 0.051 0.005 0.011 0.000 F3A 0.057 0.055 0.052 0.001 0.016 0.004 F1B 0.059 0.055 0.055 0.003 0.009 -0.001 F2B 0.053 0.054 0.052 0.005 0.016 0.001 F3B 0.049 0.046 0.046 0.001 0.014 0.006 F4 0.054 0.049 0.061 -0.011 0.024 -0.008 F5 0.053 0.048 0.052 -0.008 0.026 -0.013 F6 0.082 0.074 0.089 0.007 0.014 -0.008 F7 0.043 0.039 0.039 -0.011 0.006 0.002 F8 0.038 0.053 0.043 -0.009 0.008 0.005 F9 0.052 0.050 0.043 0.007 0.006 -0.007 F10 0.075 0.082 0.085 0.020 0.033 0.009 F11 0.102 0.095 0.092 -0.002 0.023 0.056 F12 0.077 0.068 0.097 0.001 0.019 0.003 F13 0.029 0.035 0.035 -0.002 0.008 0.007 F14 0.037 0.032 0.031 -0.001 0.013 0.008 F15 0.042 0.028 0.042 -0.005 0.014 0.001 F16 0.049 0.041 0.046 0.013 0.018 0.007 F17 0.081 0.088 0.083 0.018 0.034 0.008 F18 0.121 0.106 0.098 0.002 0.036 -0.007 F19 0.078 0.070 0.062 0.002 0.023 -0.012 F20 0.070 0.082 0.066 -0.003 0.021 -0.010 F21 0.097 0.092 0.085 -0.007 0.026 0.015 F22 0.042 0.033 0.047 0.007 0.003 -0.007 F23 0.030 0.038 0.046 -0.006 0.006 -0.001 F24 0.047 0.047 0.043 -0.009 0.017 -0.014 C34 0.018 0.015 0.013 -0.003 0.007 -0.001 C35 0.020 0.015 0.027 0.001 0.008 -0.005 C36 0.026 0.023 0.033 -0.001 0.006 -0.003 C37 0.020 0.024 0.027 -0.007 -0.001 -0.006 C38 0.022 0.020 0.021 -0.004 0.005 0.001 C39 0.019 0.017 0.018 -0.005 0.007 -0.001 C40 0.026 0.035 0.050 0.005 -0.003 -0.013 C42 0.018 0.011 0.016 0.000 0.010 -0.003 C43 0.018 0.015 0.019 0.003 0.009 -0.001 C44 0.021 0.018 0.018 -0.001 0.008 -0.003 C45 0.024 0.016 0.021 -0.002 0.011 -0.001 C46 0.020 0.016 0.024 0.003 0.010 -0.002 C47 0.017 0.015 0.016 0.003 0.007 0.001 C48 0.023 0.030 0.022 -0.007 0.005 -0.001 C49 0.021 0.018 0.015 0.003 0.011 0.001 C50 0.016 0.012 0.018 -0.002 0.001 -0.005 C51 0.014 0.012 0.018 -0.003 0.003 -0.002 C52 0.019 0.015 0.019 -0.001 0.002 -0.003 C53 0.029 0.014 0.025 0.004 0.005 0.001 C54 0.030 0.020 0.025 0.006 0.009 0.002 C55 0.023 0.014 0.027 0.003 0.012 0.001 C56 0.024 0.015 0.027 0.001 0.004 0.005 C57 0.061 0.027 0.051 0.020 0.035 0.022 C58 0.017 0.009 0.016 0.002 0.005 0.002 C59 0.017 0.015 0.019 -0.001 0.005 0.000 C60 0.015 0.022 0.021 0.005 0.006 0.002 C61 0.017 0.017 0.023 0.003 0.007 -0.002 C62 0.016 0.012 0.022 0.003 0.004 0.002 C63 0.016 0.013 0.015 0.000 0.004 0.001 C64 0.025 0.035 0.019 -0.004 0.011 -0.008 C65 0.017 0.014 0.025 0.000 0.005 -0.003 B1 0.016 0.012 0.013 -0.001 0.005 -0.001 _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 C21 2.039(6) . ? Pd1 N1 2.124(5) . ? Pd1 O2 2.133(4) . ? Pd1 P1 2.1682(16) . ? P1 O1 1.681(4) . ? P1 C15 1.820(6) . ? P1 C18 1.826(6) . ? O1 C13 1.352(7) . ? O2 C23 1.237(7) . ? N1 C13 1.287(8) . ? N1 C1 1.445(7) . ? C1 C2 1.398(8) . ? C1 C6 1.410(8) . ? C2 C3 1.399(9) . ? C2 C7 1.523(8) . ? C3 C4 1.382(9) . ? C3 H3 0.9500 . ? C4 C5 1.390(9) . ? C4 H4 0.9500 . ? C5 C6 1.399(8) . ? C5 H5 0.9500 . ? C6 C10 1.517(8) . ? C7 C9 1.529(8) . ? C7 C8 1.532(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.526(8) . ? C10 C11 1.543(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.487(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.529(9) . ? C15 C16 1.536(9) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.529(9) . ? C18 C19 1.532(9) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.528(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.494(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.495(9) . ? C24 C25 1.546(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.533(9) . ? C25 C27 1.536(8) . ? C25 C28 1.537(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.393(9) . ? C28 C29 1.410(9) . ? C29 C30 1.379(10) . ? C29 H29 0.9500 . ? C30 C31 1.382(11) . ? C30 H30 0.9500 . ? C31 C32 1.371(11) . ? C31 H31 0.9500 . ? C32 C33 1.400(11) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C41 F3A 1.280(9) . ? C41 F1B 1.303(10) . ? C41 F3B 1.307(9) . ? C41 F1A 1.316(9) . ? C41 F2A 1.360(9) . ? C41 F2B 1.404(9) . ? C41 C38 1.490(9) . ? F4 C40 1.332(10) . ? F5 C40 1.331(9) . ? F6 C40 1.332(10) . ? F7 C48 1.340(8) . ? F8 C48 1.331(8) . ? F9 C48 1.324(8) . ? F10 C49 1.262(8) . ? F11 C49 1.297(9) . ? F12 C49 1.308(9) . ? F13 C56 1.349(7) . ? F14 C56 1.340(8) . ? F15 C56 1.344(7) . ? F16 C57 1.288(8) . ? F17 C57 1.278(10) . ? F18 C57 1.371(12) . ? F19 C64 1.300(9) . ? F20 C64 1.323(9) . ? F21 C64 1.328(10) . ? F22 C65 1.329(7) . ? F23 C65 1.343(7) . ? F24 C65 1.328(8) . ? C34 C35 1.394(8) . ? C34 C39 1.396(8) . ? C34 B1 1.658(8) . ? C35 C36 1.394(9) . ? C35 H35 0.9500 . ? C36 C37 1.391(10) . ? C36 C40 1.496(10) . ? C37 C38 1.387(9) . ? C37 H37 0.9500 . ? C38 C39 1.394(9) . ? C39 H39 0.9500 . ? C42 C47 1.399(8) . ? C42 C43 1.403(8) . ? C42 B1 1.645(8) . ? C43 C44 1.391(8) . ? C43 H43 0.9500 . ? C44 C45 1.379(9) . ? C44 C48 1.498(9) . ? C45 C46 1.400(9) . ? C45 H45 0.9500 . ? C46 C47 1.392(8) . ? C46 C49 1.504(8) . ? C47 H47 0.9500 . ? C50 C55 1.392(9) . ? C50 C51 1.402(8) . ? C50 B1 1.635(8) . ? C51 C52 1.400(8) . ? C51 H51 0.9500 . ? C52 C53 1.389(9) . ? C52 C56 1.493(9) . ? C53 C54 1.389(9) . ? C53 H53 0.9500 . ? C54 C55 1.401(8) . ? C54 C57 1.471(10) . ? C55 H55 0.9500 . ? C58 C59 1.389(8) . ? C58 C63 1.405(8) . ? C58 B1 1.646(8) . ? C59 C60 1.401(8) . ? C59 H59 0.9500 . ? C60 C61 1.383(8) . ? C60 C64 1.490(9) . ? C61 C62 1.391(9) . ? C61 H61 0.9500 . ? C62 C63 1.389(8) . ? C62 C65 1.500(8) . ? C63 H63 0.9500 . ? 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 C21 Pd1 N1 177.8(2) . . ? C21 Pd1 O2 81.9(2) . . ? N1 Pd1 O2 98.69(17) . . ? C21 Pd1 P1 97.55(18) . . ? N1 Pd1 P1 81.84(14) . . ? O2 Pd1 P1 177.98(12) . . ? O1 P1 C15 100.8(3) . . ? O1 P1 C18 101.8(2) . . ? C15 P1 C18 107.7(3) . . ? O1 P1 Pd1 102.01(15) . . ? C15 P1 Pd1 120.5(2) . . ? C18 P1 Pd1 119.9(2) . . ? C13 O1 P1 118.7(4) . . ? C23 O2 Pd1 112.9(4) . . ? C13 N1 C1 120.9(5) . . ? C13 N1 Pd1 117.1(4) . . ? C1 N1 Pd1 121.8(4) . . ? C2 C1 C6 122.7(5) . . ? C2 C1 N1 119.4(5) . . ? C6 C1 N1 117.7(5) . . ? C1 C2 C3 117.5(5) . . ? C1 C2 C7 122.7(5) . . ? C3 C2 C7 119.8(5) . . ? C4 C3 C2 121.3(6) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 121.1(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 117.3(5) . . ? C5 C6 C10 120.7(5) . . ? C1 C6 C10 122.1(5) . . ? C2 C7 C9 112.9(5) . . ? C2 C7 C8 108.9(5) . . ? C9 C7 C8 111.3(5) . . ? C2 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 C12 113.2(5) . . ? C6 C10 C11 110.6(5) . . ? C12 C10 C11 110.0(5) . . ? C6 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 O1 119.3(5) . . ? N1 C13 C14 127.2(5) . . ? O1 C13 C14 113.5(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 111.8(6) . . ? C17 C15 P1 109.9(4) . . ? C16 C15 P1 110.5(5) . . ? C17 C15 H15 108.2 . . ? C16 C15 H15 108.2 . . ? P1 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 111.3(5) . . ? C20 C18 P1 109.6(4) . . ? C19 C18 P1 113.2(4) . . ? C20 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? P1 C18 H18 107.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Pd1 105.1(4) . . ? C22 C21 H21A 110.7 . . ? Pd1 C21 H21A 110.7 . . ? C22 C21 H21B 110.7 . . ? Pd1 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C23 C22 C21 112.7(5) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? O2 C23 C22 118.3(6) . . ? O2 C23 C24 123.5(6) . . ? C22 C23 C24 118.2(5) . . ? C23 C24 C25 120.9(5) . . ? C23 C24 H24A 107.1 . . ? C25 C24 H24A 107.1 . . ? C23 C24 H24B 107.1 . . ? C25 C24 H24B 107.1 . . ? H24A C24 H24B 106.8 . . ? C26 C25 C27 108.3(5) . . ? C26 C25 C28 111.3(5) . . ? C27 C25 C28 109.6(5) . . ? C26 C25 C24 109.7(5) . . ? C27 C25 C24 111.6(5) . . ? C28 C25 C24 106.3(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 117.4(6) . . ? C33 C28 C25 123.5(6) . . ? C29 C28 C25 119.1(6) . . ? C30 C29 C28 121.5(6) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 120.1(7) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 119.6(7) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 120.9(7) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C28 C33 C32 120.5(7) . . ? C28 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? F3A C41 F1B 58.6(7) . . ? F3A C41 F3B 127.2(8) . . ? F1B C41 F3B 117.0(8) . . ? F3A C41 F1A 107.4(8) . . ? F1B C41 F1A 128.0(8) . . ? F3A C41 F2A 103.6(7) . . ? F1B C41 F2A 47.2(6) . . ? F3B C41 F2A 79.6(7) . . ? F1A C41 F2A 104.2(7) . . ? F1B C41 F2B 98.2(7) . . ? F3B C41 F2B 99.7(7) . . ? F1A C41 F2B 72.7(7) . . ? F2A C41 F2B 134.8(8) . . ? F3A C41 C38 114.0(7) . . ? F1B C41 C38 116.0(7) . . ? F3B C41 C38 113.1(6) . . ? F1A C41 C38 115.1(6) . . ? F2A C41 C38 111.5(7) . . ? F2B C41 C38 110.1(6) . . ? C35 C34 C39 115.4(5) . . ? C35 C34 B1 122.5(5) . . ? C39 C34 B1 122.0(5) . . ? C34 C35 C36 122.6(6) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C37 C36 C35 120.6(6) . . ? C37 C36 C40 118.1(6) . . ? C35 C36 C40 121.3(6) . . ? C38 C37 C36 118.0(6) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? C37 C38 C39 120.4(6) . . ? C37 C38 C41 120.0(6) . . ? C39 C38 C41 119.6(5) . . ? C38 C39 C34 123.0(6) . . ? C38 C39 H39 118.5 . . ? C34 C39 H39 118.5 . . ? F5 C40 F6 112.3(7) . . ? F5 C40 F4 104.9(6) . . ? F6 C40 F4 100.7(7) . . ? F5 C40 C36 111.8(7) . . ? F6 C40 C36 113.2(6) . . ? F4 C40 C36 113.3(7) . . ? C47 C42 C43 115.3(5) . . ? C47 C42 B1 122.9(5) . . ? C43 C42 B1 121.1(5) . . ? C44 C43 C42 122.9(5) . . ? C44 C43 H43 118.6 . . ? C42 C43 H43 118.6 . . ? C45 C44 C43 120.5(6) . . ? C45 C44 C48 120.5(6) . . ? C43 C44 C48 119.0(5) . . ? C44 C45 C46 118.3(6) . . ? C44 C45 H45 120.9 . . ? C46 C45 H45 120.9 . . ? C47 C46 C45 120.5(5) . . ? C47 C46 C49 120.9(5) . . ? C45 C46 C49 118.6(5) . . ? C46 C47 C42 122.5(5) . . ? C46 C47 H47 118.8 . . ? C42 C47 H47 118.8 . . ? F9 C48 F8 107.1(6) . . ? F9 C48 F7 106.2(5) . . ? F8 C48 F7 105.5(5) . . ? F9 C48 C44 112.7(5) . . ? F8 C48 C44 112.1(5) . . ? F7 C48 C44 112.7(5) . . ? F10 C49 F11 108.2(7) . . ? F10 C49 F12 108.0(6) . . ? F11 C49 F12 99.7(6) . . ? F10 C49 C46 114.2(5) . . ? F11 C49 C46 113.4(5) . . ? F12 C49 C46 112.3(5) . . ? C55 C50 C51 115.8(5) . . ? C55 C50 B1 121.2(5) . . ? C51 C50 B1 122.6(5) . . ? C52 C51 C50 122.1(6) . . ? C52 C51 H51 119.0 . . ? C50 C51 H51 119.0 . . ? C53 C52 C51 120.7(6) . . ? C53 C52 C56 118.4(5) . . ? C51 C52 C56 120.9(5) . . ? C52 C53 C54 118.3(6) . . ? C52 C53 H53 120.8 . . ? C54 C53 H53 120.8 . . ? C53 C54 C55 120.2(6) . . ? C53 C54 C57 120.7(6) . . ? C55 C54 C57 119.0(6) . . ? C50 C55 C54 122.8(6) . . ? C50 C55 H55 118.6 . . ? C54 C55 H55 118.6 . . ? F14 C56 F15 106.4(5) . . ? F14 C56 F13 106.0(5) . . ? F15 C56 F13 105.6(5) . . ? F14 C56 C52 113.6(5) . . ? F15 C56 C52 112.2(5) . . ? F13 C56 C52 112.5(5) . . ? F17 C57 F16 111.3(7) . . ? F17 C57 F18 96.0(7) . . ? F16 C57 F18 103.7(8) . . ? F17 C57 C54 115.7(7) . . ? F16 C57 C54 116.5(6) . . ? F18 C57 C54 111.1(7) . . ? C59 C58 C63 115.7(5) . . ? C59 C58 B1 122.2(5) . . ? C63 C58 B1 122.1(5) . . ? C58 C59 C60 122.5(5) . . ? C58 C59 H59 118.7 . . ? C60 C59 H59 118.7 . . ? C61 C60 C59 120.7(6) . . ? C61 C60 C64 120.1(5) . . ? C59 C60 C64 119.2(5) . . ? C60 C61 C62 117.8(5) . . ? C60 C61 H61 121.1 . . ? C62 C61 H61 121.1 . . ? C63 C62 C61 121.0(5) . . ? C63 C62 C65 120.9(5) . . ? C61 C62 C65 118.1(5) . . ? C62 C63 C58 122.2(5) . . ? C62 C63 H63 118.9 . . ? C58 C63 H63 118.9 . . ? F19 C64 F20 106.6(6) . . ? F19 C64 F21 106.7(6) . . ? F20 C64 F21 102.3(7) . . ? F19 C64 C60 115.1(6) . . ? F20 C64 C60 113.1(6) . . ? F21 C64 C60 111.9(6) . . ? F24 C65 F22 107.4(5) . . ? F24 C65 F23 106.0(5) . . ? F22 C65 F23 105.2(5) . . ? F24 C65 C62 113.8(5) . . ? F22 C65 C62 112.2(5) . . ? F23 C65 C62 111.7(5) . . ? C50 B1 C42 111.4(5) . . ? C50 B1 C58 110.8(5) . . ? C42 B1 C58 106.2(4) . . ? C50 B1 C34 107.2(4) . . ? C42 B1 C34 112.6(5) . . ? C58 B1 C34 108.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Pd1 P1 O1 170.0(2) . . . . ? N1 Pd1 P1 O1 -7.9(2) . . . . ? C21 Pd1 P1 C15 59.6(3) . . . . ? N1 Pd1 P1 C15 -118.3(3) . . . . ? C21 Pd1 P1 C18 -78.7(3) . . . . ? N1 Pd1 P1 C18 103.5(3) . . . . ? C15 P1 O1 C13 132.6(4) . . . . ? C18 P1 O1 C13 -116.5(4) . . . . ? Pd1 P1 O1 C13 7.9(4) . . . . ? C21 Pd1 O2 C23 15.0(4) . . . . ? N1 Pd1 O2 C23 -167.2(4) . . . . ? O2 Pd1 N1 C13 -168.8(4) . . . . ? P1 Pd1 N1 C13 9.2(4) . . . . ? O2 Pd1 N1 C1 5.8(4) . . . . ? P1 Pd1 N1 C1 -176.2(4) . . . . ? C13 N1 C1 C2 82.6(7) . . . . ? Pd1 N1 C1 C2 -91.9(6) . . . . ? C13 N1 C1 C6 -101.7(6) . . . . ? Pd1 N1 C1 C6 83.8(6) . . . . ? C6 C1 C2 C3 -0.7(9) . . . . ? N1 C1 C2 C3 174.8(5) . . . . ? C6 C1 C2 C7 -177.4(5) . . . . ? N1 C1 C2 C7 -1.9(9) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C7 C2 C3 C4 176.5(6) . . . . ? C2 C3 C4 C5 0.5(10) . . . . ? C3 C4 C5 C6 0.4(10) . . . . ? C4 C5 C6 C1 -1.3(9) . . . . ? C4 C5 C6 C10 -179.4(6) . . . . ? C2 C1 C6 C5 1.4(9) . . . . ? N1 C1 C6 C5 -174.1(5) . . . . ? C2 C1 C6 C10 179.6(5) . . . . ? N1 C1 C6 C10 4.0(8) . . . . ? C1 C2 C7 C9 -133.1(6) . . . . ? C3 C2 C7 C9 50.2(8) . . . . ? C1 C2 C7 C8 102.8(7) . . . . ? C3 C2 C7 C8 -73.9(7) . . . . ? C5 C6 C10 C12 -41.6(8) . . . . ? C1 C6 C10 C12 140.3(6) . . . . ? C5 C6 C10 C11 82.3(7) . . . . ? C1 C6 C10 C11 -95.7(7) . . . . ? C1 N1 C13 O1 178.5(5) . . . . ? Pd1 N1 C13 O1 -6.8(7) . . . . ? C1 N1 C13 C14 -3.0(9) . . . . ? Pd1 N1 C13 C14 171.7(5) . . . . ? P1 O1 C13 N1 -1.4(7) . . . . ? P1 O1 C13 C14 179.9(4) . . . . ? O1 P1 C15 C17 -68.0(5) . . . . ? C18 P1 C15 C17 -174.3(5) . . . . ? Pd1 P1 C15 C17 43.0(5) . . . . ? O1 P1 C15 C16 168.2(4) . . . . ? C18 P1 C15 C16 61.9(5) . . . . ? Pd1 P1 C15 C16 -80.8(5) . . . . ? O1 P1 C18 C20 63.1(5) . . . . ? C15 P1 C18 C20 168.7(4) . . . . ? Pd1 P1 C18 C20 -48.3(5) . . . . ? O1 P1 C18 C19 -61.9(5) . . . . ? C15 P1 C18 C19 43.7(5) . . . . ? Pd1 P1 C18 C19 -173.3(4) . . . . ? O2 Pd1 C21 C22 -24.3(4) . . . . ? P1 Pd1 C21 C22 157.6(4) . . . . ? Pd1 C21 C22 C23 32.2(6) . . . . ? Pd1 O2 C23 C22 0.6(7) . . . . ? Pd1 O2 C23 C24 178.4(4) . . . . ? C21 C22 C23 O2 -22.8(8) . . . . ? C21 C22 C23 C24 159.3(5) . . . . ? O2 C23 C24 C25 -9.9(9) . . . . ? C22 C23 C24 C25 167.8(6) . . . . ? C23 C24 C25 C26 -56.5(7) . . . . ? C23 C24 C25 C27 63.6(7) . . . . ? C23 C24 C25 C28 -177.0(5) . . . . ? C26 C25 C28 C33 -5.2(9) . . . . ? C27 C25 C28 C33 -125.0(6) . . . . ? C24 C25 C28 C33 114.2(6) . . . . ? C26 C25 C28 C29 176.8(6) . . . . ? C27 C25 C28 C29 57.0(7) . . . . ? C24 C25 C28 C29 -63.8(7) . . . . ? C33 C28 C29 C30 1.3(10) . . . . ? C25 C28 C29 C30 179.5(6) . . . . ? C28 C29 C30 C31 -1.3(10) . . . . ? C29 C30 C31 C32 0.8(10) . . . . ? C30 C31 C32 C33 -0.3(10) . . . . ? C29 C28 C33 C32 -0.8(9) . . . . ? C25 C28 C33 C32 -178.9(6) . . . . ? C31 C32 C33 C28 0.3(10) . . . . ? C39 C34 C35 C36 -0.1(9) . . . . ? B1 C34 C35 C36 -175.9(6) . . . . ? C34 C35 C36 C37 0.4(10) . . . . ? C34 C35 C36 C40 179.0(7) . . . . ? C35 C36 C37 C38 -0.5(10) . . . . ? C40 C36 C37 C38 -179.2(7) . . . . ? C36 C37 C38 C39 0.4(10) . . . . ? C36 C37 C38 C41 179.3(6) . . . . ? F3A C41 C38 C37 -78.8(9) . . . . ? F1B C41 C38 C37 -13.5(10) . . . . ? F3B C41 C38 C37 125.6(8) . . . . ? F1A C41 C38 C37 156.5(7) . . . . ? F2A C41 C38 C37 38.1(9) . . . . ? F2B C41 C38 C37 -123.8(7) . . . . ? F3A C41 C38 C39 100.1(8) . . . . ? F1B C41 C38 C39 165.5(8) . . . . ? F3B C41 C38 C39 -55.4(9) . . . . ? F1A C41 C38 C39 -24.6(9) . . . . ? F2A C41 C38 C39 -142.9(7) . . . . ? F2B C41 C38 C39 55.1(8) . . . . ? C37 C38 C39 C34 -0.2(10) . . . . ? C41 C38 C39 C34 -179.1(5) . . . . ? C35 C34 C39 C38 0.0(9) . . . . ? B1 C34 C39 C38 175.8(5) . . . . ? C37 C36 C40 F5 -68.7(9) . . . . ? C35 C36 C40 F5 112.6(7) . . . . ? C37 C36 C40 F6 163.4(7) . . . . ? C35 C36 C40 F6 -15.3(11) . . . . ? C37 C36 C40 F4 49.6(9) . . . . ? C35 C36 C40 F4 -129.1(7) . . . . ? C47 C42 C43 C44 -0.7(8) . . . . ? B1 C42 C43 C44 170.1(5) . . . . ? C42 C43 C44 C45 -0.6(9) . . . . ? C42 C43 C44 C48 178.7(5) . . . . ? C43 C44 C45 C46 1.2(9) . . . . ? C48 C44 C45 C46 -178.1(5) . . . . ? C44 C45 C46 C47 -0.6(9) . . . . ? C44 C45 C46 C49 178.8(5) . . . . ? C45 C46 C47 C42 -0.7(9) . . . . ? C49 C46 C47 C42 180.0(5) . . . . ? C43 C42 C47 C46 1.3(8) . . . . ? B1 C42 C47 C46 -169.3(5) . . . . ? C45 C44 C48 F9 105.9(7) . . . . ? C43 C44 C48 F9 -73.4(7) . . . . ? C45 C44 C48 F8 -133.2(6) . . . . ? C43 C44 C48 F8 47.6(8) . . . . ? C45 C44 C48 F7 -14.3(8) . . . . ? C43 C44 C48 F7 166.5(5) . . . . ? C47 C46 C49 F10 106.9(7) . . . . ? C45 C46 C49 F10 -72.4(8) . . . . ? C47 C46 C49 F11 -17.8(9) . . . . ? C45 C46 C49 F11 162.9(7) . . . . ? C47 C46 C49 F12 -129.8(7) . . . . ? C45 C46 C49 F12 50.9(8) . . . . ? C55 C50 C51 C52 1.7(8) . . . . ? B1 C50 C51 C52 -171.1(5) . . . . ? C50 C51 C52 C53 -1.3(9) . . . . ? C50 C51 C52 C56 -179.9(5) . . . . ? C51 C52 C53 C54 -0.5(9) . . . . ? C56 C52 C53 C54 178.1(6) . . . . ? C52 C53 C54 C55 1.8(10) . . . . ? C52 C53 C54 C57 -178.9(7) . . . . ? C51 C50 C55 C54 -0.4(9) . . . . ? B1 C50 C55 C54 172.6(6) . . . . ? C53 C54 C55 C50 -1.4(10) . . . . ? C57 C54 C55 C50 179.3(7) . . . . ? C53 C52 C56 F14 165.1(5) . . . . ? C51 C52 C56 F14 -16.3(8) . . . . ? C53 C52 C56 F15 44.4(8) . . . . ? C51 C52 C56 F15 -137.0(6) . . . . ? C53 C52 C56 F13 -74.5(7) . . . . ? C51 C52 C56 F13 104.1(6) . . . . ? C53 C54 C57 F17 -137.5(8) . . . . ? C55 C54 C57 F17 41.8(11) . . . . ? C53 C54 C57 F16 -4.0(12) . . . . ? C55 C54 C57 F16 175.4(7) . . . . ? C53 C54 C57 F18 114.4(8) . . . . ? C55 C54 C57 F18 -66.3(9) . . . . ? C63 C58 C59 C60 -3.5(8) . . . . ? B1 C58 C59 C60 174.2(5) . . . . ? C58 C59 C60 C61 0.9(9) . . . . ? C58 C59 C60 C64 -178.8(5) . . . . ? C59 C60 C61 C62 2.4(9) . . . . ? C64 C60 C61 C62 -177.9(5) . . . . ? C60 C61 C62 C63 -3.0(8) . . . . ? C60 C61 C62 C65 175.9(5) . . . . ? C61 C62 C63 C58 0.4(9) . . . . ? C65 C62 C63 C58 -178.5(5) . . . . ? C59 C58 C63 C62 2.8(8) . . . . ? B1 C58 C63 C62 -174.9(5) . . . . ? C61 C60 C64 F19 -24.5(9) . . . . ? C59 C60 C64 F19 155.3(6) . . . . ? C61 C60 C64 F20 -147.4(6) . . . . ? C59 C60 C64 F20 32.4(9) . . . . ? C61 C60 C64 F21 97.6(8) . . . . ? C59 C60 C64 F21 -82.6(8) . . . . ? C63 C62 C65 F24 -8.7(8) . . . . ? C61 C62 C65 F24 172.5(5) . . . . ? C63 C62 C65 F22 -130.9(6) . . . . ? C61 C62 C65 F22 50.2(7) . . . . ? C63 C62 C65 F23 111.3(6) . . . . ? C61 C62 C65 F23 -67.6(7) . . . . ? C55 C50 B1 C42 38.3(7) . . . . ? C51 C50 B1 C42 -149.3(5) . . . . ? C55 C50 B1 C58 156.3(5) . . . . ? C51 C50 B1 C58 -31.2(7) . . . . ? C55 C50 B1 C34 -85.4(6) . . . . ? C51 C50 B1 C34 87.1(6) . . . . ? C47 C42 B1 C50 -156.6(5) . . . . ? C43 C42 B1 C50 33.3(7) . . . . ? C47 C42 B1 C58 82.6(6) . . . . ? C43 C42 B1 C58 -87.4(6) . . . . ? C47 C42 B1 C34 -36.1(7) . . . . ? C43 C42 B1 C34 153.8(5) . . . . ? C59 C58 B1 C50 90.2(6) . . . . ? C63 C58 B1 C50 -92.3(6) . . . . ? C59 C58 B1 C42 -148.6(5) . . . . ? C63 C58 B1 C42 28.9(7) . . . . ? C59 C58 B1 C34 -27.3(7) . . . . ? C63 C58 B1 C34 150.2(5) . . . . ? C35 C34 B1 C50 13.0(7) . . . . ? C39 C34 B1 C50 -162.5(5) . . . . ? C35 C34 B1 C42 -109.9(6) . . . . ? C39 C34 B1 C42 74.6(7) . . . . ? C35 C34 B1 C58 132.7(6) . . . . ? C39 C34 B1 C58 -42.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.952 _refine_diff_density_min -1.530 _refine_diff_density_rms 0.169 ###END