# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Stephan, Douglas' _publ_contact_author_email dstephan@chem.utoronto.ca loop_ _publ_author_name R.Cariou F.Dahcheh T.Graham D.Stephan data_fd003 _database_code_depnum_ccdc_archive 'CCDC 809529' #TrackingRef '- 6-fd003.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C50 H41 Cl2 N3 O P2 Pd' _chemical_formula_weight 939.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.2104(7) _cell_length_b 24.1180(10) _cell_length_c 20.0246(8) _cell_angle_alpha 90.00 _cell_angle_beta 118.446(2) _cell_angle_gamma 90.00 _cell_volume 8582.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9357 _exptl_absorpt_correction_T_max 0.9671 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 139535 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15098 _reflns_number_gt 11256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+14.7215P] 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 15098 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0720 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 P1 P 0.03838(5) 0.07277(4) 0.31343(4) 0.01584(18) Uani 1 1 d . . . Pd1 Pd 0.145726(13) 0.167279(11) 0.446682(13) 0.01647(7) Uani 1 1 d . . . Pd2 Pd 0.636760(13) 0.167101(11) 0.926127(12) 0.01471(7) Uani 1 1 d . . . P4 P 0.54034(5) 0.07382(4) 0.79145(4) 0.01613(19) Uani 1 1 d . . . Cl4 Cl 0.64819(5) 0.08406(3) 0.98662(4) 0.02167(18) Uani 1 1 d . . . Cl1 Cl 0.16935(5) 0.08667(4) 0.51634(4) 0.0261(2) Uani 1 1 d . . . P3 P 0.66905(5) 0.29440(4) 0.88178(4) 0.01619(19) Uani 1 1 d . . . Cl3 Cl 0.68922(5) 0.21166(4) 1.04167(4) 0.0260(2) Uani 1 1 d . . . P2 P 0.16432(5) 0.29530(4) 0.39083(4) 0.01683(19) Uani 1 1 d . . . Cl2 Cl 0.20757(5) 0.21755(4) 0.55668(4) 0.0282(2) Uani 1 1 d . . . N1 N 0.09694(14) 0.12373(11) 0.34427(14) 0.0166(6) Uani 1 1 d . . . O1 O 0.05283(13) 0.20523(10) 0.21958(12) 0.0247(6) Uani 1 1 d . . . N2 N 0.11835(14) 0.23842(11) 0.38003(13) 0.0166(6) Uani 1 1 d . . . C37 C 0.07785(18) 0.00428(14) 0.31617(18) 0.0188(7) Uani 1 1 d . . . C31 C -0.01146(17) 0.06970(14) 0.36708(17) 0.0176(7) Uani 1 1 d . . . C43 C -0.03075(18) 0.08173(14) 0.21469(17) 0.0181(7) Uani 1 1 d . . . C8 C 0.12008(19) 0.17691(15) 0.25221(18) 0.0225(8) Uani 1 1 d . . . C44 C -0.00937(19) 0.08620(14) 0.15824(17) 0.0206(8) Uani 1 1 d . . . H44A H 0.0411 0.0830 0.1709 0.025 Uiso 1 1 calc R . . C56 C 0.79225(19) 0.22854(15) 0.91614(18) 0.0235(8) Uani 1 1 d . . . H56A H 0.7603 0.2091 0.8724 0.028 Uiso 1 1 calc R . . C55 C 0.76484(18) 0.27309(14) 0.93949(17) 0.0192(7) Uani 1 1 d . . . C13 C 0.13867(18) 0.35259(15) 0.43295(18) 0.0225(8) Uani 1 1 d . . . C49 C 0.66314(18) 0.32360(14) 0.79567(17) 0.0184(7) Uani 1 1 d . . . C6 C -0.01237(19) 0.25921(15) 0.35124(19) 0.0233(8) Uani 1 1 d . . . H6A H 0.0053 0.2727 0.4003 0.028 Uiso 1 1 calc R . . C25 C 0.14892(19) 0.32165(13) 0.29985(17) 0.0195(8) Uani 1 1 d . . . C42 C 0.14190(19) -0.01296(15) 0.38150(19) 0.0259(8) Uani 1 1 d . . . H42A H 0.1654 0.0109 0.4227 0.031 Uiso 1 1 calc R . . C79 C 0.58576(18) 0.00680(15) 0.80306(18) 0.0208(8) Uani 1 1 d . . . C2 C 0.00986(19) 0.21957(14) 0.25439(17) 0.0194(7) Uani 1 1 d . . . C7 C 0.14094(19) 0.13574(15) 0.30744(18) 0.0211(8) Uani 1 1 d . . . C46 C -0.1378(2) 0.09992(15) 0.06437(19) 0.0272(9) Uani 1 1 d . . . H46A H -0.1734 0.1066 0.0142 0.033 Uiso 1 1 calc R . . C12 C 0.2092(2) 0.10822(16) 0.3300(2) 0.0297(9) Uani 1 1 d . . . H12A H 0.2247 0.0815 0.3680 0.036 Uiso 1 1 calc R . . C24 C 0.2978(2) 0.23779(16) 0.4356(2) 0.0279(8) Uani 1 1 d . . . H24A H 0.2687 0.2106 0.4012 0.033 Uiso 1 1 calc R . . C54 C 0.72696(19) 0.32948(16) 0.78644(19) 0.0255(8) Uani 1 1 d . . . H54A H 0.7735 0.3177 0.8246 0.031 Uiso 1 1 calc R . . C20 C 0.30777(19) 0.32454(16) 0.49836(19) 0.0281(9) Uani 1 1 d . . . H20A H 0.2852 0.3558 0.5058 0.034 Uiso 1 1 calc R . . C5 C -0.0891(2) 0.25867(15) 0.3022(2) 0.0276(8) Uani 1 1 d . . . H5A H -0.1223 0.2722 0.3183 0.033 Uiso 1 1 calc R . . C40 C 0.1373(2) -0.10115(16) 0.3244(2) 0.0279(9) Uani 1 1 d . . . H40A H 0.1570 -0.1365 0.3275 0.033 Uiso 1 1 calc R . . C19 C 0.26380(18) 0.28397(15) 0.44709(17) 0.0191(7) Uani 1 1 d . . . C39 C 0.0747(2) -0.08426(15) 0.2587(2) 0.0285(9) Uani 1 1 d . . . H39A H 0.0526 -0.1080 0.2171 0.034 Uiso 1 1 calc R . . C4 C -0.1164(2) 0.23801(16) 0.2296(2) 0.0291(9) Uani 1 1 d . . . H4A H -0.1679 0.2375 0.1967 0.035 Uiso 1 1 calc R . . C30 C 0.0784(2) 0.34195(14) 0.24842(18) 0.0254(8) Uani 1 1 d . . . H30A H 0.0401 0.3429 0.2617 0.030 Uiso 1 1 calc R . . C51 C 0.5898(2) 0.36533(15) 0.67287(18) 0.0256(8) Uani 1 1 d . . . H51A H 0.5436 0.3778 0.6348 0.031 Uiso 1 1 calc R . . C32 C -0.0319(2) 0.11862(16) 0.3890(2) 0.0280(8) Uani 1 1 d . . . H32A H -0.0177 0.1526 0.3778 0.034 Uiso 1 1 calc R . . C48 C -0.10715(18) 0.08556(14) 0.19433(19) 0.0225(8) Uani 1 1 d . . . H48A H -0.1224 0.0820 0.2312 0.027 Uiso 1 1 calc R . . C45 C -0.0624(2) 0.09537(15) 0.08387(18) 0.0252(8) Uani 1 1 d . . . H45A H -0.0475 0.0985 0.0466 0.030 Uiso 1 1 calc R . . C26 C 0.2056(2) 0.32092(14) 0.27902(19) 0.0261(8) Uani 1 1 d . . . H26A H 0.2532 0.3079 0.3130 0.031 Uiso 1 1 calc R . . C41 C 0.1704(2) -0.06554(17) 0.3850(2) 0.0330(9) Uani 1 1 d . . . H41A H 0.2126 -0.0770 0.4290 0.040 Uiso 1 1 calc R . . C81 C 0.5777(2) -0.08927(16) 0.7660(2) 0.0334(9) Uani 1 1 d . . . H81A H 0.5517 -0.1179 0.7327 0.040 Uiso 1 1 calc R . . C57 C 0.8668(2) 0.21308(16) 0.9577(2) 0.0295(9) Uani 1 1 d . . . H57A H 0.8851 0.1830 0.9423 0.035 Uiso 1 1 calc R . . C3 C -0.0672(2) 0.21822(15) 0.20613(19) 0.0259(8) Uani 1 1 d . . . H3A H -0.0856 0.2038 0.1574 0.031 Uiso 1 1 calc R . . C38 C 0.04479(19) -0.03168(15) 0.25488(19) 0.0233(8) Uani 1 1 d . . . H38A H 0.0023 -0.0205 0.2109 0.028 Uiso 1 1 calc R . . C1 C 0.03924(18) 0.23989(14) 0.32846(17) 0.0177(7) Uani 1 1 d . . . C33 C -0.0735(2) 0.11672(18) 0.4275(2) 0.0357(10) Uani 1 1 d . . . H33A H -0.0868 0.1494 0.4426 0.043 Uiso 1 1 calc R . . C84 C 0.65651(19) -0.00371(15) 0.86408(18) 0.0232(8) Uani 1 1 d . . . H84A H 0.6836 0.0248 0.8970 0.028 Uiso 1 1 calc R . . C27 C 0.1914(2) 0.33952(17) 0.2078(2) 0.0350(10) Uani 1 1 d . . . H27A H 0.2294 0.3391 0.1942 0.042 Uiso 1 1 calc R . . C36 C -0.03484(19) 0.01917(16) 0.38206(19) 0.0264(8) Uani 1 1 d . . . H36A H -0.0228 -0.0137 0.3660 0.032 Uiso 1 1 calc R . . C83 C 0.6865(2) -0.05652(17) 0.8758(2) 0.0324(9) Uani 1 1 d . . . H83A H 0.7338 -0.0632 0.9167 0.039 Uiso 1 1 calc R . . C53 C 0.7213(2) 0.35270(16) 0.7207(2) 0.0317(9) Uani 1 1 d . . . H53A H 0.7642 0.3564 0.7150 0.038 Uiso 1 1 calc R . . C82 C 0.6476(2) -0.09919(17) 0.8280(2) 0.0345(10) Uani 1 1 d . . . H82A H 0.6680 -0.1347 0.8370 0.041 Uiso 1 1 calc R . . C34 C -0.0951(2) 0.0664(2) 0.4433(2) 0.0374(10) Uani 1 1 d . . . H34A H -0.1228 0.0653 0.4694 0.045 Uiso 1 1 calc R . . C18 C 0.1385(2) 0.40677(16) 0.40890(19) 0.0303(9) Uani 1 1 d . . . H18A H 0.1526 0.4139 0.3718 0.036 Uiso 1 1 calc R . . C58 C 0.9143(2) 0.24250(18) 1.0225(2) 0.0337(10) Uani 1 1 d . . . H58A H 0.9647 0.2324 1.0502 0.040 Uiso 1 1 calc R . . C29 C 0.0646(2) 0.36079(16) 0.17747(19) 0.0340(10) Uani 1 1 d . . . H29A H 0.0175 0.3748 0.1436 0.041 Uiso 1 1 calc R . . C23 C 0.3757(2) 0.23232(17) 0.4761(2) 0.0332(9) Uani 1 1 d . . . H23A H 0.3988 0.2012 0.4689 0.040 Uiso 1 1 calc R . . C47 C -0.1600(2) 0.09463(16) 0.11914(19) 0.0279(9) Uani 1 1 d . . . H47A H -0.2108 0.0972 0.1057 0.034 Uiso 1 1 calc R . . C52 C 0.6529(2) 0.37028(15) 0.66369(19) 0.0279(9) Uani 1 1 d . . . H52A H 0.6493 0.3854 0.6193 0.033 Uiso 1 1 calc R . . C14 C 0.11909(19) 0.34263(16) 0.48984(18) 0.0268(8) Uani 1 1 d . . . H14A H 0.1206 0.3067 0.5074 0.032 Uiso 1 1 calc R . . C80 C 0.5465(2) -0.03646(15) 0.7537(2) 0.0276(8) Uani 1 1 d . . . H80A H 0.4994 -0.0299 0.7124 0.033 Uiso 1 1 calc R . . C60 C 0.8132(2) 0.30208(15) 1.00482(18) 0.0250(8) Uani 1 1 d . . . H60A H 0.7953 0.3320 1.0208 0.030 Uiso 1 1 calc R . . C50 C 0.59413(19) 0.34208(14) 0.73786(18) 0.0224(8) Uani 1 1 d . . . H50A H 0.5510 0.3387 0.7431 0.027 Uiso 1 1 calc R . . C59 C 0.8874(2) 0.28650(17) 1.0459(2) 0.0321(9) Uani 1 1 d . . . H59A H 0.9195 0.3059 1.0896 0.039 Uiso 1 1 calc R . . C35 C -0.0759(2) 0.01775(18) 0.4209(2) 0.0366(10) Uani 1 1 d . . . H35A H -0.0907 -0.0161 0.4318 0.044 Uiso 1 1 calc R . . C9 C 0.1650(2) 0.18827(17) 0.2182(2) 0.0343(10) Uani 1 1 d . . . H9A H 0.1502 0.2151 0.1804 0.041 Uiso 1 1 calc R . . C21 C 0.3850(2) 0.31844(18) 0.5383(2) 0.0359(10) Uani 1 1 d . . . H21A H 0.4141 0.3455 0.5730 0.043 Uiso 1 1 calc R . . C28 C 0.1209(3) 0.35864(17) 0.1575(2) 0.0385(11) Uani 1 1 d . . . H28A H 0.1112 0.3703 0.1094 0.046 Uiso 1 1 calc R . . C11 C 0.2543(2) 0.11992(19) 0.2970(3) 0.0438(11) Uani 1 1 d . . . H11A H 0.2995 0.1012 0.3127 0.053 Uiso 1 1 calc R . . C17 C 0.1172(2) 0.45003(18) 0.4401(2) 0.0425(11) Uani 1 1 d . . . H17A H 0.1175 0.4862 0.4242 0.051 Uiso 1 1 calc R . . C22 C 0.4189(2) 0.27292(19) 0.5271(2) 0.0361(10) Uani 1 1 d . . . H22A H 0.4709 0.2693 0.5537 0.043 Uiso 1 1 calc R . . C10 C 0.2314(3) 0.15967(19) 0.2406(3) 0.0464(12) Uani 1 1 d . . . H10A H 0.2610 0.1672 0.2176 0.056 Uiso 1 1 calc R . . C16 C 0.0956(2) 0.43950(19) 0.4949(2) 0.0465(12) Uani 1 1 d . . . H16A H 0.0798 0.4684 0.5146 0.056 Uiso 1 1 calc R . . C73 C 0.60073(18) 0.18988(14) 0.72551(16) 0.0171(7) Uani 1 1 d . . . C74 C 0.62876(18) 0.14610(14) 0.77794(17) 0.0179(7) Uani 1 1 d . . . C76 C 0.7330(2) 0.13860(16) 0.75008(19) 0.0275(9) Uani 1 1 d . . . H76A H 0.7773 0.1212 0.7583 0.033 Uiso 1 1 calc R . . C75 C 0.69577(18) 0.12138(15) 0.78941(18) 0.0213(8) Uani 1 1 d . . . H75A H 0.7160 0.0926 0.8243 0.026 Uiso 1 1 calc R . . C78 C 0.63824(19) 0.20735(15) 0.68631(17) 0.0224(8) Uani 1 1 d . . . H78A H 0.6188 0.2364 0.6517 0.027 Uiso 1 1 calc R . . C77 C 0.7040(2) 0.18182(16) 0.69856(19) 0.0263(9) Uani 1 1 d . . . H77A H 0.7290 0.1936 0.6723 0.032 Uiso 1 1 calc R . . N4 N 0.59204(14) 0.12889(11) 0.82042(13) 0.0147(6) Uani 1 1 d . . . N3 N 0.61531(14) 0.24127(11) 0.86592(13) 0.0156(6) Uani 1 1 d . . . O2 O 0.53162(12) 0.21520(10) 0.70098(11) 0.0199(5) Uani 1 1 d . . . C91 C 0.48330(18) 0.06961(14) 0.83792(17) 0.0188(7) Uani 1 1 d . . . C72 C 0.49107(19) 0.26357(14) 0.85325(18) 0.0209(8) Uani 1 1 d . . . H72A H 0.5146 0.2740 0.9041 0.025 Uiso 1 1 calc R . . C67 C 0.53539(18) 0.24624(13) 0.82044(17) 0.0169(7) Uani 1 1 d . . . C69 C 0.41949(18) 0.23226(14) 0.70251(18) 0.0206(8) Uani 1 1 d . . . H69A H 0.3955 0.2221 0.6516 0.025 Uiso 1 1 calc R . . C85 C 0.48039(18) 0.07952(14) 0.68967(17) 0.0188(7) Uani 1 1 d . . . C68 C 0.49763(18) 0.22986(14) 0.74432(17) 0.0174(7) Uani 1 1 d . . . C61 C 0.65127(18) 0.35367(14) 0.92709(17) 0.0202(8) Uani 1 1 d . . . C90 C 0.40670(19) 0.09875(14) 0.65967(19) 0.0245(8) Uani 1 1 d . . . H90A H 0.3863 0.1060 0.6918 0.029 Uiso 1 1 calc R . . C62 C 0.63581(19) 0.34583(14) 0.98735(17) 0.0215(8) Uani 1 1 d . . . H62A H 0.6338 0.3101 1.0038 0.026 Uiso 1 1 calc R . . C71 C 0.41371(19) 0.26556(15) 0.81220(19) 0.0235(8) Uani 1 1 d . . . H71A H 0.3857 0.2775 0.8353 0.028 Uiso 1 1 calc R . . C70 C 0.37747(19) 0.24969(15) 0.73632(19) 0.0231(8) Uani 1 1 d . . . H70A H 0.3252 0.2508 0.7085 0.028 Uiso 1 1 calc R . . C96 C 0.45107(19) 0.11788(16) 0.84769(18) 0.0243(8) Uani 1 1 d . . . H96A H 0.4579 0.1515 0.8290 0.029 Uiso 1 1 calc R . . C92 C 0.47234(19) 0.01951(15) 0.86585(19) 0.0249(8) Uani 1 1 d . . . H92A H 0.4934 -0.0129 0.8590 0.030 Uiso 1 1 calc R . . C66 C 0.6543(2) 0.40758(15) 0.90345(19) 0.0276(9) Uani 1 1 d . . . H66A H 0.6649 0.4134 0.8636 0.033 Uiso 1 1 calc R . . C86 C 0.5101(2) 0.06924(15) 0.64050(18) 0.0264(8) Uani 1 1 d . . . H86A H 0.5594 0.0570 0.6598 0.032 Uiso 1 1 calc R . . C63 C 0.6236(2) 0.39089(16) 1.02268(19) 0.0282(9) Uani 1 1 d . . . H63A H 0.6134 0.3854 1.0629 0.034 Uiso 1 1 calc R . . C65 C 0.6415(2) 0.45264(16) 0.9393(2) 0.0353(10) Uani 1 1 d . . . H65A H 0.6433 0.4885 0.9231 0.042 Uiso 1 1 calc R . . C93 C 0.4303(2) 0.01763(17) 0.9038(2) 0.0322(9) Uani 1 1 d . . . H93A H 0.4236 -0.0158 0.9229 0.039 Uiso 1 1 calc R . . C89 C 0.3634(2) 0.10720(16) 0.5818(2) 0.0319(9) Uani 1 1 d . . . H89A H 0.3145 0.1206 0.5620 0.038 Uiso 1 1 calc R . . C88 C 0.3932(2) 0.09575(16) 0.53409(19) 0.0319(9) Uani 1 1 d . . . H88A H 0.3639 0.1006 0.4820 0.038 Uiso 1 1 calc R . . C87 C 0.4660(2) 0.07719(16) 0.5632(2) 0.0324(9) Uani 1 1 d . . . H87A H 0.4859 0.0699 0.5307 0.039 Uiso 1 1 calc R . . C94 C 0.3981(2) 0.06566(18) 0.9133(2) 0.0328(9) Uani 1 1 d . . . H94A H 0.3694 0.0644 0.9382 0.039 Uiso 1 1 calc R . . C95 C 0.4087(2) 0.11547(17) 0.8856(2) 0.0309(9) Uani 1 1 d . . . H95A H 0.3872 0.1477 0.8924 0.037 Uiso 1 1 calc R . . C15 C 0.0975(2) 0.38601(19) 0.5203(2) 0.0373(10) Uani 1 1 d . . . H15A H 0.0842 0.3791 0.5580 0.045 Uiso 1 1 calc R . . C64 C 0.6263(2) 0.44424(16) 0.9985(2) 0.0336(10) Uani 1 1 d . . . H64A H 0.6178 0.4744 1.0224 0.040 Uiso 1 1 calc R . . C98 C 0.2299(3) 0.0203(2) 0.7600(3) 0.0486(12) Uani 1 1 d . . . N6 N -0.1078(3) 0.0722(2) -0.0985(2) 0.0748(14) Uani 1 1 d . . . N5 N 0.2005(3) 0.02470(19) 0.7967(3) 0.0662(12) Uani 1 1 d . . . C100 C -0.1429(3) 0.0377(2) -0.1429(3) 0.0542(13) Uani 1 1 d . . . C99 C -0.1882(3) -0.0041(2) -0.2003(3) 0.0602(14) Uani 1 1 d . . . C97 C 0.2676(3) 0.0149(2) 0.7134(3) 0.0591(14) 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 P1 0.0134(4) 0.0144(5) 0.0194(4) 0.0020(3) 0.0076(3) 0.0001(4) Pd1 0.01632(13) 0.01674(15) 0.01660(12) 0.00113(10) 0.00804(10) -0.00192(11) Pd2 0.01585(13) 0.01465(14) 0.01276(12) -0.00012(10) 0.00609(10) -0.00108(11) P4 0.0147(4) 0.0146(5) 0.0178(4) -0.0009(3) 0.0067(3) 0.0005(4) Cl4 0.0261(5) 0.0178(5) 0.0170(4) 0.0019(3) 0.0069(3) -0.0011(4) Cl1 0.0316(5) 0.0228(5) 0.0245(4) 0.0054(3) 0.0139(4) -0.0018(4) P3 0.0184(4) 0.0148(5) 0.0152(4) -0.0004(3) 0.0079(3) -0.0009(4) Cl3 0.0381(5) 0.0196(5) 0.0155(4) -0.0017(3) 0.0089(4) -0.0036(4) P2 0.0182(5) 0.0150(5) 0.0174(4) -0.0013(3) 0.0086(3) -0.0024(4) Cl2 0.0355(5) 0.0279(5) 0.0174(4) -0.0014(3) 0.0096(4) -0.0072(4) N1 0.0156(14) 0.0161(16) 0.0198(13) -0.0011(11) 0.0098(11) -0.0031(12) O1 0.0353(15) 0.0215(14) 0.0209(12) -0.0001(10) 0.0162(11) -0.0035(12) N2 0.0187(15) 0.0144(16) 0.0155(13) -0.0001(11) 0.0071(11) -0.0022(12) C37 0.0181(17) 0.0148(19) 0.0272(17) 0.0034(14) 0.0137(14) 0.0019(15) C31 0.0130(17) 0.021(2) 0.0186(16) 0.0017(13) 0.0077(13) -0.0022(14) C43 0.0176(18) 0.0127(18) 0.0214(16) -0.0006(13) 0.0072(14) 0.0000(14) C8 0.0254(19) 0.021(2) 0.0270(18) -0.0093(15) 0.0175(15) -0.0100(16) C44 0.0195(18) 0.0169(19) 0.0244(17) 0.0005(14) 0.0096(14) -0.0014(15) C56 0.0207(19) 0.024(2) 0.0230(17) 0.0011(14) 0.0080(15) -0.0029(16) C55 0.0198(18) 0.020(2) 0.0167(16) 0.0045(13) 0.0078(14) -0.0040(15) C13 0.0194(18) 0.021(2) 0.0210(17) -0.0044(14) 0.0044(14) -0.0020(15) C49 0.0245(19) 0.0140(19) 0.0177(16) 0.0012(13) 0.0108(14) -0.0002(15) C6 0.026(2) 0.021(2) 0.0246(17) 0.0009(14) 0.0133(15) 0.0010(16) C25 0.0270(19) 0.0121(19) 0.0187(16) -0.0030(13) 0.0104(14) -0.0075(15) C42 0.0236(19) 0.025(2) 0.0271(18) 0.0011(15) 0.0103(16) 0.0020(16) C79 0.0241(19) 0.020(2) 0.0219(17) -0.0002(14) 0.0138(15) 0.0027(15) C2 0.0258(19) 0.0137(19) 0.0198(16) 0.0026(13) 0.0118(15) -0.0021(15) C7 0.0204(19) 0.020(2) 0.0268(18) -0.0072(14) 0.0141(15) -0.0061(15) C46 0.027(2) 0.019(2) 0.0212(18) 0.0001(14) -0.0002(15) -0.0008(16) C12 0.023(2) 0.025(2) 0.046(2) -0.0100(17) 0.0199(17) -0.0071(17) C24 0.027(2) 0.023(2) 0.034(2) 0.0027(16) 0.0152(17) -0.0032(17) C54 0.0217(19) 0.028(2) 0.0279(18) 0.0078(16) 0.0129(15) 0.0051(17) C20 0.0234(19) 0.032(2) 0.0274(18) -0.0037(16) 0.0113(15) -0.0024(17) C5 0.023(2) 0.023(2) 0.039(2) 0.0043(16) 0.0161(17) 0.0037(16) C40 0.033(2) 0.018(2) 0.043(2) 0.0059(16) 0.0270(18) 0.0071(17) C19 0.0167(17) 0.023(2) 0.0187(16) 0.0014(14) 0.0090(14) -0.0040(15) C39 0.039(2) 0.018(2) 0.036(2) -0.0030(16) 0.0240(18) -0.0015(17) C4 0.0166(19) 0.022(2) 0.037(2) 0.0052(16) 0.0038(16) -0.0004(16) C30 0.032(2) 0.015(2) 0.0279(18) 0.0011(14) 0.0127(16) -0.0063(16) C51 0.028(2) 0.022(2) 0.0196(17) 0.0037(14) 0.0048(15) 0.0015(16) C32 0.026(2) 0.024(2) 0.039(2) -0.0018(16) 0.0196(17) -0.0032(17) C48 0.0176(18) 0.020(2) 0.0275(18) -0.0014(15) 0.0090(15) -0.0005(16) C45 0.029(2) 0.021(2) 0.0231(18) 0.0002(14) 0.0107(15) -0.0086(16) C26 0.035(2) 0.019(2) 0.0303(19) -0.0019(15) 0.0200(17) -0.0039(16) C41 0.028(2) 0.031(2) 0.037(2) 0.0090(17) 0.0129(18) 0.0107(18) C81 0.046(3) 0.019(2) 0.048(2) -0.0091(17) 0.033(2) -0.0069(19) C57 0.029(2) 0.026(2) 0.035(2) 0.0112(16) 0.0160(17) 0.0080(17) C3 0.031(2) 0.016(2) 0.0206(17) 0.0040(14) 0.0039(16) -0.0037(16) C38 0.0212(19) 0.019(2) 0.0283(18) 0.0011(15) 0.0101(15) 0.0005(16) C1 0.0188(18) 0.0128(18) 0.0211(16) 0.0041(13) 0.0091(14) -0.0024(14) C33 0.032(2) 0.043(3) 0.041(2) -0.0088(19) 0.0252(19) -0.003(2) C84 0.0246(19) 0.022(2) 0.0247(18) 0.0016(14) 0.0131(15) 0.0023(16) C27 0.053(3) 0.030(2) 0.037(2) -0.0064(18) 0.033(2) -0.009(2) C36 0.025(2) 0.023(2) 0.033(2) 0.0028(15) 0.0154(16) -0.0022(16) C83 0.029(2) 0.036(3) 0.034(2) 0.0096(18) 0.0165(17) 0.0132(19) C53 0.035(2) 0.031(2) 0.043(2) 0.0090(17) 0.0298(19) 0.0040(18) C82 0.048(3) 0.024(2) 0.048(2) 0.0080(18) 0.035(2) 0.0139(19) C34 0.028(2) 0.062(3) 0.030(2) 0.0031(19) 0.0199(18) -0.003(2) C18 0.035(2) 0.024(2) 0.0218(18) -0.0005(15) 0.0055(16) 0.0003(17) C58 0.019(2) 0.044(3) 0.030(2) 0.0152(18) 0.0055(16) -0.0017(18) C29 0.037(2) 0.027(2) 0.0218(18) 0.0047(16) 0.0013(17) -0.0107(18) C23 0.030(2) 0.034(2) 0.041(2) 0.0183(18) 0.0202(18) 0.0105(19) C47 0.0198(19) 0.027(2) 0.031(2) -0.0019(16) 0.0076(16) 0.0013(16) C52 0.042(2) 0.024(2) 0.0247(18) 0.0053(15) 0.0213(17) 0.0039(18) C14 0.026(2) 0.028(2) 0.0250(18) -0.0024(15) 0.0114(15) 0.0002(17) C80 0.028(2) 0.022(2) 0.033(2) -0.0036(16) 0.0144(17) 0.0010(17) C60 0.028(2) 0.023(2) 0.0216(17) 0.0011(14) 0.0094(15) -0.0061(16) C50 0.0216(18) 0.020(2) 0.0254(17) 0.0018(14) 0.0110(15) -0.0014(15) C59 0.025(2) 0.037(3) 0.0232(18) 0.0018(17) 0.0019(16) -0.0131(18) C35 0.033(2) 0.040(3) 0.044(2) 0.0127(19) 0.0231(19) -0.005(2) C9 0.053(3) 0.027(2) 0.038(2) -0.0137(17) 0.034(2) -0.020(2) C21 0.024(2) 0.046(3) 0.029(2) -0.0065(18) 0.0059(17) -0.0102(19) C28 0.065(3) 0.029(2) 0.0226(19) -0.0028(16) 0.021(2) -0.013(2) C11 0.032(2) 0.038(3) 0.077(3) -0.023(2) 0.039(2) -0.011(2) C17 0.051(3) 0.024(2) 0.032(2) -0.0040(17) 0.0021(19) 0.007(2) C22 0.019(2) 0.056(3) 0.027(2) 0.0127(19) 0.0061(16) -0.001(2) C10 0.053(3) 0.044(3) 0.074(3) -0.025(2) 0.055(3) -0.025(2) C16 0.046(3) 0.043(3) 0.034(2) -0.018(2) 0.005(2) 0.017(2) C73 0.0176(18) 0.0201(19) 0.0139(15) -0.0059(13) 0.0078(13) -0.0027(14) C74 0.0178(18) 0.0198(19) 0.0151(15) -0.0050(13) 0.0071(13) -0.0057(15) C76 0.0202(19) 0.034(2) 0.033(2) -0.0106(17) 0.0165(16) -0.0020(17) C75 0.0189(18) 0.023(2) 0.0218(17) -0.0031(14) 0.0097(14) 0.0012(15) C78 0.028(2) 0.024(2) 0.0166(16) -0.0014(14) 0.0118(15) -0.0048(16) C77 0.028(2) 0.034(2) 0.0258(18) -0.0069(15) 0.0205(16) -0.0087(17) N4 0.0140(14) 0.0159(16) 0.0146(13) -0.0004(11) 0.0072(11) -0.0012(11) N3 0.0176(14) 0.0135(15) 0.0153(13) 0.0004(11) 0.0074(11) -0.0014(12) O2 0.0195(12) 0.0256(14) 0.0158(11) -0.0005(9) 0.0093(10) 0.0028(11) C91 0.0140(17) 0.021(2) 0.0204(16) -0.0017(14) 0.0074(14) -0.0013(15) C72 0.026(2) 0.0164(19) 0.0202(16) -0.0013(14) 0.0109(15) -0.0001(15) C67 0.0193(18) 0.0111(18) 0.0200(16) 0.0019(13) 0.0090(14) -0.0002(14) C69 0.0187(18) 0.018(2) 0.0191(16) 0.0022(13) 0.0044(14) 0.0002(15) C85 0.0179(18) 0.0148(19) 0.0178(16) -0.0016(13) 0.0038(14) -0.0027(14) C68 0.0216(18) 0.0145(18) 0.0180(16) 0.0028(13) 0.0110(14) 0.0026(14) C61 0.0223(19) 0.0172(19) 0.0174(16) -0.0013(13) 0.0065(14) 0.0022(15) C90 0.0210(19) 0.016(2) 0.0309(19) -0.0033(15) 0.0081(16) -0.0046(15) C62 0.029(2) 0.016(2) 0.0203(16) 0.0015(13) 0.0126(15) 0.0022(15) C71 0.024(2) 0.020(2) 0.0318(19) 0.0031(15) 0.0172(16) 0.0055(16) C70 0.0171(18) 0.018(2) 0.0320(19) 0.0020(15) 0.0102(15) 0.0030(15) C96 0.0218(19) 0.025(2) 0.0272(18) 0.0005(15) 0.0123(15) -0.0025(16) C92 0.026(2) 0.021(2) 0.0300(19) -0.0007(15) 0.0154(16) -0.0017(16) C66 0.038(2) 0.023(2) 0.0213(17) 0.0010(15) 0.0139(16) 0.0023(17) C86 0.0224(19) 0.029(2) 0.0241(18) -0.0036(15) 0.0078(15) -0.0084(16) C63 0.035(2) 0.026(2) 0.0241(18) 0.0005(15) 0.0147(16) 0.0084(18) C65 0.055(3) 0.017(2) 0.030(2) 0.0026(16) 0.0170(19) 0.0052(19) C93 0.037(2) 0.031(2) 0.035(2) 0.0036(17) 0.0213(18) -0.0086(19) C89 0.024(2) 0.021(2) 0.034(2) 0.0025(16) 0.0003(17) -0.0017(17) C88 0.035(2) 0.027(2) 0.0187(18) 0.0014(15) 0.0005(16) -0.0114(18) C87 0.037(2) 0.034(2) 0.0266(19) -0.0047(16) 0.0154(17) -0.0133(19) C94 0.029(2) 0.044(3) 0.036(2) -0.0056(18) 0.0249(18) -0.0066(19) C95 0.030(2) 0.032(2) 0.035(2) -0.0046(17) 0.0196(18) 0.0003(18) C15 0.033(2) 0.047(3) 0.030(2) -0.0139(19) 0.0134(18) 0.007(2) C64 0.045(2) 0.025(2) 0.0274(19) -0.0052(16) 0.0142(18) 0.0112(19) C98 0.041(3) 0.042(3) 0.050(3) 0.000(2) 0.012(2) -0.014(2) N6 0.090(4) 0.072(4) 0.055(3) -0.003(2) 0.028(3) 0.005(3) N5 0.077(3) 0.054(3) 0.079(3) -0.004(2) 0.046(3) -0.011(2) C100 0.064(3) 0.051(3) 0.053(3) 0.008(2) 0.032(3) 0.013(3) C99 0.070(3) 0.050(3) 0.064(3) -0.018(3) 0.035(3) -0.008(3) C97 0.045(3) 0.086(4) 0.051(3) 0.004(3) 0.027(2) 0.001(3) _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 P1 N1 1.611(3) . ? P1 C31 1.790(3) . ? P1 C43 1.810(3) . ? P1 C37 1.824(3) . ? Pd1 N2 2.080(3) . ? Pd1 N1 2.087(3) . ? Pd1 Cl2 2.2937(9) . ? Pd1 Cl1 2.3061(9) . ? Pd2 N4 2.079(2) . ? Pd2 N3 2.084(3) . ? Pd2 Cl4 2.2946(9) . ? Pd2 Cl3 2.3011(8) . ? P4 N4 1.617(3) . ? P4 C91 1.796(3) . ? P4 C85 1.813(3) . ? P4 C79 1.819(4) . ? P3 N3 1.611(3) . ? P3 C55 1.793(3) . ? P3 C49 1.813(3) . ? P3 C61 1.818(3) . ? P2 N2 1.612(3) . ? P2 C19 1.797(3) . ? P2 C25 1.811(3) . ? P2 C13 1.818(4) . ? N1 C7 1.429(4) . ? O1 C8 1.377(4) . ? O1 C2 1.391(4) . ? N2 C1 1.432(4) . ? C37 C38 1.387(5) . ? C37 C42 1.395(5) . ? C31 C32 1.389(5) . ? C31 C36 1.390(5) . ? C43 C44 1.393(4) . ? C43 C48 1.400(5) . ? C8 C7 1.394(5) . ? C8 C9 1.398(5) . ? C44 C45 1.376(4) . ? C56 C57 1.381(5) . ? C56 C55 1.388(5) . ? C55 C60 1.392(5) . ? C13 C18 1.392(5) . ? C13 C14 1.393(5) . ? C49 C54 1.395(5) . ? C49 C50 1.395(4) . ? C6 C5 1.386(5) . ? C6 C1 1.402(5) . ? C25 C30 1.391(5) . ? C25 C26 1.393(5) . ? C42 C41 1.381(5) . ? C79 C84 1.392(5) . ? C79 C80 1.396(5) . ? C2 C3 1.388(5) . ? C2 C1 1.398(4) . ? C7 C12 1.398(5) . ? C46 C47 1.375(5) . ? C46 C45 1.386(5) . ? C12 C11 1.386(5) . ? C24 C19 1.383(5) . ? C24 C23 1.392(5) . ? C54 C53 1.385(5) . ? C20 C21 1.381(5) . ? C20 C19 1.390(5) . ? C5 C4 1.379(5) . ? C40 C41 1.373(5) . ? C40 C39 1.383(5) . ? C39 C38 1.391(5) . ? C4 C3 1.372(5) . ? C30 C29 1.388(5) . ? C51 C52 1.379(5) . ? C51 C50 1.381(5) . ? C32 C33 1.385(5) . ? C48 C47 1.387(5) . ? C26 C27 1.388(5) . ? C81 C82 1.387(5) . ? C81 C80 1.390(5) . ? C57 C58 1.386(5) . ? C33 C34 1.378(6) . ? C84 C83 1.382(5) . ? C27 C28 1.375(6) . ? C36 C35 1.382(5) . ? C83 C82 1.370(6) . ? C53 C52 1.374(5) . ? C34 C35 1.376(6) . ? C18 C17 1.385(5) . ? C58 C59 1.373(6) . ? C29 C28 1.374(6) . ? C23 C22 1.383(6) . ? C14 C15 1.382(5) . ? C60 C59 1.376(5) . ? C9 C10 1.379(6) . ? C21 C22 1.368(6) . ? C11 C10 1.382(6) . ? C17 C16 1.385(6) . ? C16 C15 1.380(6) . ? C73 O2 1.383(4) . ? C73 C78 1.391(4) . ? C73 C74 1.404(5) . ? C74 C75 1.395(5) . ? C74 N4 1.431(4) . ? C76 C77 1.385(5) . ? C76 C75 1.387(5) . ? C78 C77 1.377(5) . ? N3 C67 1.432(4) . ? O2 C68 1.385(4) . ? C91 C96 1.392(5) . ? C91 C92 1.393(5) . ? C72 C71 1.378(5) . ? C72 C67 1.403(5) . ? C67 C68 1.398(4) . ? C69 C70 1.380(5) . ? C69 C68 1.392(5) . ? C85 C90 1.393(5) . ? C85 C86 1.398(5) . ? C61 C66 1.395(5) . ? C61 C62 1.396(4) . ? C90 C89 1.393(5) . ? C62 C63 1.382(5) . ? C71 C70 1.390(5) . ? C96 C95 1.390(5) . ? C92 C93 1.385(5) . ? C66 C65 1.392(5) . ? C86 C87 1.382(5) . ? C63 C64 1.385(5) . ? C65 C64 1.376(5) . ? C93 C94 1.385(5) . ? C89 C88 1.378(5) . ? C88 C87 1.374(5) . ? C94 C95 1.381(5) . ? C98 N5 1.151(6) . ? C98 C97 1.465(7) . ? N6 C100 1.177(6) . ? C100 C99 1.474(7) . ? 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 N1 P1 C31 108.79(15) . . ? N1 P1 C43 111.81(15) . . ? C31 P1 C43 107.36(15) . . ? N1 P1 C37 116.64(15) . . ? C31 P1 C37 107.91(15) . . ? C43 P1 C37 103.88(15) . . ? N2 Pd1 N1 85.86(10) . . ? N2 Pd1 Cl2 92.11(7) . . ? N1 Pd1 Cl2 174.89(7) . . ? N2 Pd1 Cl1 176.82(8) . . ? N1 Pd1 Cl1 92.00(8) . . ? Cl2 Pd1 Cl1 90.21(3) . . ? N4 Pd2 N3 85.52(10) . . ? N4 Pd2 Cl4 92.07(8) . . ? N3 Pd2 Cl4 174.53(7) . . ? N4 Pd2 Cl3 177.63(8) . . ? N3 Pd2 Cl3 92.87(7) . . ? Cl4 Pd2 Cl3 89.69(3) . . ? N4 P4 C91 108.97(14) . . ? N4 P4 C85 108.22(14) . . ? C91 P4 C85 109.65(15) . . ? N4 P4 C79 118.92(15) . . ? C91 P4 C79 107.04(16) . . ? C85 P4 C79 103.74(15) . . ? N3 P3 C55 108.58(15) . . ? N3 P3 C49 112.88(14) . . ? C55 P3 C49 106.62(15) . . ? N3 P3 C61 116.67(15) . . ? C55 P3 C61 108.24(15) . . ? C49 P3 C61 103.31(15) . . ? N2 P2 C19 110.85(15) . . ? N2 P2 C25 110.59(14) . . ? C19 P2 C25 106.79(15) . . ? N2 P2 C13 115.81(15) . . ? C19 P2 C13 107.81(15) . . ? C25 P2 C13 104.45(16) . . ? C7 N1 P1 118.7(2) . . ? C7 N1 Pd1 106.63(19) . . ? P1 N1 Pd1 132.65(15) . . ? C8 O1 C2 126.6(2) . . ? C1 N2 P2 116.7(2) . . ? C1 N2 Pd1 110.33(19) . . ? P2 N2 Pd1 130.95(15) . . ? C38 C37 C42 119.0(3) . . ? C38 C37 P1 121.4(3) . . ? C42 C37 P1 119.7(3) . . ? C32 C31 C36 119.6(3) . . ? C32 C31 P1 119.5(3) . . ? C36 C31 P1 120.8(3) . . ? C44 C43 C48 118.9(3) . . ? C44 C43 P1 121.3(2) . . ? C48 C43 P1 119.8(2) . . ? O1 C8 C7 126.0(3) . . ? O1 C8 C9 113.3(3) . . ? C7 C8 C9 120.4(3) . . ? C45 C44 C43 120.5(3) . . ? C57 C56 C55 120.1(3) . . ? C56 C55 C60 119.4(3) . . ? C56 C55 P3 119.1(2) . . ? C60 C55 P3 121.4(3) . . ? C18 C13 C14 119.3(3) . . ? C18 C13 P2 120.5(3) . . ? C14 C13 P2 120.2(3) . . ? C54 C49 C50 118.7(3) . . ? C54 C49 P3 121.3(2) . . ? C50 C49 P3 120.0(3) . . ? C5 C6 C1 121.5(3) . . ? C30 C25 C26 118.8(3) . . ? C30 C25 P2 119.5(3) . . ? C26 C25 P2 121.7(3) . . ? C41 C42 C37 120.0(3) . . ? C84 C79 C80 119.0(3) . . ? C84 C79 P4 121.3(3) . . ? C80 C79 P4 119.5(3) . . ? C3 C2 O1 114.0(3) . . ? C3 C2 C1 121.0(3) . . ? O1 C2 C1 124.6(3) . . ? C8 C7 C12 118.3(3) . . ? C8 C7 N1 121.8(3) . . ? C12 C7 N1 119.8(3) . . ? C47 C46 C45 120.1(3) . . ? C11 C12 C7 121.4(4) . . ? C19 C24 C23 119.5(4) . . ? C53 C54 C49 120.3(3) . . ? C21 C20 C19 120.1(4) . . ? C4 C5 C6 120.0(3) . . ? C41 C40 C39 119.8(4) . . ? C24 C19 C20 119.7(3) . . ? C24 C19 P2 120.9(3) . . ? C20 C19 P2 119.1(3) . . ? C40 C39 C38 119.8(3) . . ? C3 C4 C5 119.8(3) . . ? C29 C30 C25 120.6(4) . . ? C52 C51 C50 120.9(3) . . ? C33 C32 C31 119.9(4) . . ? C47 C48 C43 120.0(3) . . ? C44 C45 C46 120.1(3) . . ? C27 C26 C25 120.4(4) . . ? C40 C41 C42 120.9(3) . . ? C82 C81 C80 120.0(4) . . ? C56 C57 C58 119.8(4) . . ? C4 C3 C2 120.6(3) . . ? C37 C38 C39 120.5(3) . . ? C2 C1 C6 117.1(3) . . ? C2 C1 N2 121.4(3) . . ? C6 C1 N2 121.4(3) . . ? C34 C33 C32 120.0(4) . . ? C83 C84 C79 120.1(3) . . ? C28 C27 C26 119.8(4) . . ? C35 C36 C31 120.0(4) . . ? C82 C83 C84 121.0(4) . . ? C52 C53 C54 120.6(3) . . ? C83 C82 C81 119.8(4) . . ? C35 C34 C33 120.4(4) . . ? C17 C18 C13 120.1(4) . . ? C59 C58 C57 120.3(3) . . ? C28 C29 C30 119.7(4) . . ? C22 C23 C24 120.3(4) . . ? C46 C47 C48 120.3(3) . . ? C53 C52 C51 119.4(3) . . ? C15 C14 C13 120.1(4) . . ? C81 C80 C79 120.2(3) . . ? C59 C60 C55 120.1(4) . . ? C51 C50 C49 120.1(3) . . ? C58 C59 C60 120.3(3) . . ? C34 C35 C36 120.0(4) . . ? C10 C9 C8 120.0(4) . . ? C22 C21 C20 120.4(4) . . ? C29 C28 C27 120.8(3) . . ? C10 C11 C12 119.4(4) . . ? C16 C17 C18 120.1(4) . . ? C21 C22 C23 120.0(4) . . ? C9 C10 C11 120.5(4) . . ? C15 C16 C17 119.9(4) . . ? O2 C73 C78 113.3(3) . . ? O2 C73 C74 125.3(3) . . ? C78 C73 C74 121.0(3) . . ? C75 C74 C73 117.3(3) . . ? C75 C74 N4 121.1(3) . . ? C73 C74 N4 121.6(3) . . ? C77 C76 C75 119.8(3) . . ? C76 C75 C74 121.7(3) . . ? C77 C78 C73 120.2(3) . . ? C78 C77 C76 119.9(3) . . ? C74 N4 P4 117.0(2) . . ? C74 N4 Pd2 112.30(19) . . ? P4 N4 Pd2 128.50(14) . . ? C67 N3 P3 120.6(2) . . ? C67 N3 Pd2 107.49(19) . . ? P3 N3 Pd2 129.34(14) . . ? C73 O2 C68 127.5(2) . . ? C96 C91 C92 119.6(3) . . ? C96 C91 P4 119.0(3) . . ? C92 C91 P4 121.4(3) . . ? C71 C72 C67 121.8(3) . . ? C68 C67 C72 117.1(3) . . ? C68 C67 N3 122.3(3) . . ? C72 C67 N3 120.3(3) . . ? C70 C69 C68 120.3(3) . . ? C90 C85 C86 119.0(3) . . ? C90 C85 P4 121.0(3) . . ? C86 C85 P4 119.8(2) . . ? O2 C68 C69 113.1(3) . . ? O2 C68 C67 125.4(3) . . ? C69 C68 C67 121.2(3) . . ? C66 C61 C62 118.9(3) . . ? C66 C61 P3 120.8(3) . . ? C62 C61 P3 120.3(3) . . ? C89 C90 C85 120.3(3) . . ? C63 C62 C61 120.3(3) . . ? C72 C71 C70 120.0(3) . . ? C69 C70 C71 119.6(3) . . ? C95 C96 C91 119.5(3) . . ? C93 C92 C91 120.4(3) . . ? C65 C66 C61 120.2(3) . . ? C87 C86 C85 120.1(3) . . ? C62 C63 C64 120.3(3) . . ? C64 C65 C66 120.1(4) . . ? C92 C93 C94 119.9(4) . . ? C88 C89 C90 119.9(3) . . ? C87 C88 C89 120.3(3) . . ? C88 C87 C86 120.5(4) . . ? C95 C94 C93 120.0(3) . . ? C94 C95 C96 120.5(4) . . ? C16 C15 C14 120.3(4) . . ? C65 C64 C63 120.1(3) . . ? N5 C98 C97 179.8(6) . . ? N6 C100 C99 178.1(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.490 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.072 # Attachment '- 7-fd.cif' data_fd _database_code_depnum_ccdc_archive 'CCDC 809530' #TrackingRef '- 7-fd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H43 Cl6 N3 P2 Pd' _chemical_formula_weight 970.83 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' Cl Cl 0.1484 0.1585 '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' 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 orthorhombic _symmetry_space_group_name_H-M Ibca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x, -y, -z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1/2, y+1, -z+1' '-x, -y, -z' 'x, y-1/2, -z' '-x, y, z-1/2' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z' _cell_length_a 12.260(4) _cell_length_b 20.121(6) _cell_length_c 35.895(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8855(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6435 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67942 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.57 _reflns_number_total 5096 _reflns_number_gt 3947 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0168P)^2^+144.6233P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5096 _refine_ls_number_parameters 262 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.176 _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 0.0000 0.2500 0.421006(16) 0.02937(16) Uani 1 2 d SD . . Cl1 Cl 0.0000 0.2500 0.35624(5) 0.0371(4) Uani 1 2 d S . . P1 P 0.18457(12) 0.35619(7) 0.39647(4) 0.0317(3) Uani 1 1 d . A . N1 N 0.1073(4) 0.3274(3) 0.42822(14) 0.0366(11) Uani 1 1 d . . . N2 N 0.0000 0.2500 0.47688(19) 0.0455(19) Uani 1 2 d SD . . H2 H -0.0508(8) 0.2772(7) 0.4837(2) 0.055 Uiso 0.50 1 d PD . . C1 C 0.1112(5) 0.4099(3) 0.36483(17) 0.0349(13) Uani 1 1 d . . . C2 C 0.0002(6) 0.4178(3) 0.36959(19) 0.0463(15) Uani 1 1 d . A . H2A H -0.0368 0.3928 0.3874 0.056 Uiso 1 1 calc R . . C3 C -0.0554(7) 0.4629(4) 0.3478(3) 0.068(2) Uani 1 1 d . . . H3A H -0.1302 0.4683 0.3508 0.082 Uiso 1 1 calc R A . C4 C 0.0002(10) 0.5004(4) 0.3213(2) 0.074(3) Uani 1 1 d . A . H4A H -0.0378 0.5311 0.3069 0.089 Uiso 1 1 calc R . . C5 C 0.1065(8) 0.4930(4) 0.3164(2) 0.066(2) Uani 1 1 d . . . H5A H 0.1424 0.5177 0.2982 0.080 Uiso 1 1 calc R A . C6 C 0.1648(6) 0.4484(3) 0.3383(2) 0.0522(18) Uani 1 1 d . A . H6A H 0.2398 0.4442 0.3351 0.063 Uiso 1 1 calc R . . C7 C 0.2554(5) 0.2904(3) 0.37231(17) 0.0364(13) Uani 1 1 d . . . C8 C 0.2892(6) 0.2952(4) 0.3359(2) 0.0527(18) Uani 1 1 d . A . H8A H 0.2728 0.3331 0.3222 0.063 Uiso 1 1 calc R . . C9 C 0.3470(8) 0.2444(5) 0.3196(2) 0.076(3) Uani 1 1 d . . . H9A H 0.3710 0.2488 0.2951 0.091 Uiso 1 1 calc R A . C10 C 0.3696(7) 0.1879(5) 0.3388(3) 0.074(3) Uani 1 1 d . A . H10A H 0.4086 0.1539 0.3274 0.089 Uiso 1 1 calc R . . C11 C 0.3353(8) 0.1806(4) 0.3749(3) 0.073(3) Uani 1 1 d . . . H11A H 0.3489 0.1413 0.3878 0.088 Uiso 1 1 calc R A . C12 C 0.2789(6) 0.2334(3) 0.3925(2) 0.0542(18) Uani 1 1 d . A . H12A H 0.2579 0.2300 0.4173 0.065 Uiso 1 1 calc R . . C13 C 0.2872(5) 0.4096(3) 0.41630(17) 0.0385(14) Uani 1 1 d . . . C14 C 0.3945(5) 0.3884(4) 0.42121(19) 0.0455(15) Uani 1 1 d . A . H14A H 0.4168 0.3473 0.4122 0.055 Uiso 1 1 calc R . . C15 C 0.4685(7) 0.4297(4) 0.4399(2) 0.064(2) Uani 1 1 d . . . H15A H 0.5398 0.4154 0.4436 0.076 Uiso 1 1 calc R A . C16 C 0.4366(8) 0.4912(5) 0.4527(2) 0.072(3) Uani 1 1 d . A . H16A H 0.4870 0.5186 0.4645 0.086 Uiso 1 1 calc R . . C17 C 0.3295(7) 0.5125(4) 0.4482(2) 0.066(2) Uani 1 1 d . . . H17A H 0.3073 0.5534 0.4576 0.080 Uiso 1 1 calc R A . C18 C 0.2569(7) 0.4722(4) 0.4295(2) 0.0563(19) Uani 1 1 d . A . H18A H 0.1859 0.4870 0.4257 0.068 Uiso 1 1 calc R . . C19 C 0.1192(6) 0.3429(4) 0.46823(18) 0.0534(18) Uani 1 1 d D A 1 H19A H 0.1898 0.3274 0.4768 0.064 Uiso 1 1 calc R A 1 H19B H 0.1165 0.3907 0.4716 0.064 Uiso 1 1 calc R A 1 C20 C 0.0357(11) 0.3127(5) 0.4901(3) 0.044(3) Uani 0.50 1 d PD A 1 H20A H 0.0626 0.3074 0.5154 0.053 Uiso 0.50 1 calc PR A 1 H20B H -0.0264 0.3425 0.4911 0.053 Uiso 0.50 1 calc PR A 1 C19A C 0.1192(6) 0.3429(4) 0.46823(18) 0.0534(18) Uani 0.00 1 d PD A 2 H19C H 0.1948 0.3535 0.4734 0.064 Uiso 0.00 1 calc PR A 2 H19D H 0.0757 0.3818 0.4741 0.064 Uiso 0.00 1 calc PR A 2 C20A C 0.0860(10) 0.2892(5) 0.4916(3) 0.040(3) Uani 0.50 1 d PD A 2 H20C H 0.1485 0.2607 0.4960 0.048 Uiso 0.50 1 calc PR A 2 H20D H 0.0632 0.3071 0.5154 0.048 Uiso 0.50 1 calc PR A 2 Cl3 Cl 0.02636(18) 0.34503(12) 0.26056(7) 0.0786(7) Uani 1 1 d . . . Cl4 Cl -0.1980(2) 0.38770(16) 0.25815(7) 0.0920(8) Uani 1 1 d . . . C1S C -0.1032(7) 0.3368(5) 0.2805(2) 0.067(2) Uani 1 1 d . . . H1SA H -0.1266 0.2909 0.2788 0.081 Uiso 1 1 calc R . . H1SB H -0.0996 0.3486 0.3067 0.081 Uiso 1 1 calc R . . Cl2 Cl 0.2078(3) 0.15558(14) 0.50569(12) 0.0557(10) Uani 0.50 1 d P . . 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 0.0274(3) 0.0337(3) 0.0270(3) 0.000 0.000 -0.0038(3) Cl1 0.0396(10) 0.0442(11) 0.0274(9) 0.000 0.000 -0.0134(10) P1 0.0285(7) 0.0284(7) 0.0381(8) -0.0002(6) -0.0013(6) -0.0025(6) N1 0.036(3) 0.038(3) 0.035(3) -0.002(2) -0.001(2) -0.009(2) N2 0.046(4) 0.060(5) 0.030(3) 0.000 0.000 -0.024(4) C1 0.037(3) 0.026(3) 0.041(3) -0.003(2) -0.005(3) 0.000(2) C2 0.045(3) 0.041(3) 0.053(4) 0.000(3) -0.003(3) 0.011(3) C3 0.059(5) 0.059(5) 0.086(6) 0.004(5) -0.010(5) 0.023(4) C4 0.103(7) 0.044(4) 0.076(6) 0.015(4) -0.023(6) 0.019(5) C5 0.084(6) 0.046(4) 0.069(5) 0.023(4) -0.009(5) -0.008(4) C6 0.056(4) 0.043(4) 0.058(4) 0.010(3) -0.008(4) -0.010(3) C7 0.025(3) 0.036(3) 0.048(3) -0.005(3) -0.001(3) -0.001(2) C8 0.054(4) 0.050(4) 0.054(4) -0.002(3) 0.013(3) 0.006(3) C9 0.080(6) 0.081(6) 0.068(5) -0.010(5) 0.029(5) 0.019(5) C10 0.062(5) 0.065(5) 0.096(7) -0.022(5) 0.012(5) 0.019(4) C11 0.072(6) 0.050(5) 0.097(7) 0.005(5) -0.005(5) 0.020(4) C12 0.053(4) 0.046(4) 0.064(5) 0.003(3) 0.002(4) 0.010(3) C13 0.035(3) 0.039(3) 0.042(3) 0.002(3) 0.000(3) -0.012(3) C14 0.039(3) 0.048(4) 0.049(4) 0.010(3) -0.008(3) -0.009(3) C15 0.049(4) 0.079(6) 0.062(5) 0.012(4) -0.020(4) -0.020(4) C16 0.080(6) 0.081(6) 0.054(5) 0.000(4) -0.016(4) -0.042(5) C17 0.074(6) 0.060(5) 0.066(5) -0.021(4) 0.004(4) -0.025(4) C18 0.055(4) 0.047(4) 0.066(5) -0.011(4) 0.005(4) -0.012(4) C19 0.054(4) 0.068(5) 0.038(3) -0.005(3) 0.001(3) -0.024(4) C20 0.067(10) 0.035(7) 0.032(6) -0.012(5) -0.006(6) 0.008(7) C19A 0.054(4) 0.068(5) 0.038(3) -0.005(3) 0.001(3) -0.024(4) C20A 0.064(9) 0.028(6) 0.028(6) -0.003(5) -0.005(6) 0.000(6) Cl3 0.0615(13) 0.0792(15) 0.0952(17) -0.0140(13) 0.0163(12) 0.0035(11) Cl4 0.0696(15) 0.129(2) 0.0773(16) 0.0096(15) -0.0044(12) 0.0319(16) C1S 0.056(5) 0.089(6) 0.057(5) 0.003(5) 0.004(4) 0.006(5) Cl2 0.0547(18) 0.0256(13) 0.087(3) 0.0008(16) -0.035(2) -0.0009(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.006(7) . ? Pd1 N1 2.055(5) 2 ? Pd1 N1 2.055(5) . ? Pd1 Cl1 2.325(2) . ? P1 N1 1.591(5) . ? P1 C13 1.801(6) . ? P1 C7 1.805(6) . ? P1 C1 1.807(6) . ? N1 C19 1.476(8) . ? N2 C20 1.418(8) 2 ? N2 C20 1.418(8) . ? N2 C20A 1.419(8) . ? N2 C20A 1.419(8) 2 ? N2 H2 0.865(10) . ? C1 C2 1.381(10) . ? C1 C6 1.394(9) . ? C2 C3 1.379(10) . ? C2 H2A 0.9300 . ? C3 C4 1.391(13) . ? C3 H3A 0.9300 . ? C4 C5 1.325(14) . ? C4 H4A 0.9300 . ? C5 C6 1.390(10) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.375(9) . ? C7 C12 1.386(9) . ? C8 C9 1.374(11) . ? C8 H8A 0.9300 . ? C9 C10 1.359(13) . ? C9 H9A 0.9300 . ? C10 C11 1.371(13) . ? C10 H10A 0.9300 . ? C11 C12 1.416(11) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.394(9) . ? C13 C18 1.396(9) . ? C14 C15 1.400(10) . ? C14 H14A 0.9300 . ? C15 C16 1.378(13) . ? C15 H15A 0.9300 . ? C16 C17 1.391(13) . ? C16 H16A 0.9300 . ? C17 C18 1.379(10) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.426(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H2 1.300(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20A H20C 0.9700 . ? C20A H20D 0.9700 . ? Cl3 C1S 1.751(8) . ? Cl4 C1S 1.745(9) . ? C1S H1SA 0.9700 . ? C1S H1SB 0.9700 . ? Cl2 Cl2 1.113(8) 8_545 ? 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 Pd1 N1 82.76(14) . 2 ? N2 Pd1 N1 82.76(14) . . ? N1 Pd1 N1 165.5(3) 2 . ? N2 Pd1 Cl1 180.000(1) . . ? N1 Pd1 Cl1 97.24(14) 2 . ? N1 Pd1 Cl1 97.24(14) . . ? N1 P1 C13 110.5(3) . . ? N1 P1 C7 111.3(3) . . ? C13 P1 C7 106.9(3) . . ? N1 P1 C1 111.8(3) . . ? C13 P1 C1 103.9(3) . . ? C7 P1 C1 112.1(3) . . ? C19 N1 P1 124.2(4) . . ? C19 N1 Pd1 110.2(4) . . ? P1 N1 Pd1 124.5(3) . . ? C20 N2 C20 140.8(11) 2 . ? C20 N2 C20A 126.9(8) 2 . ? C20 N2 C20A 31.9(7) . . ? C20 N2 C20A 31.9(7) 2 2 ? C20 N2 C20A 126.9(8) . 2 ? C20A N2 C20A 136.4(10) . 2 ? C20 N2 Pd1 109.6(5) 2 . ? C20 N2 Pd1 109.6(5) . . ? C20A N2 Pd1 111.8(5) . . ? C20A N2 Pd1 111.8(5) 2 . ? C20 N2 H2 104.2(9) 2 . ? C20 N2 H2 64.1(6) . . ? C20A N2 H2 94.5(9) . . ? C20A N2 H2 73.2(10) 2 . ? Pd1 N2 H2 106.5(9) . . ? C2 C1 C6 119.1(6) . . ? C2 C1 P1 118.8(5) . . ? C6 C1 P1 121.9(5) . . ? C3 C2 C1 119.5(7) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 120.2(8) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 120.8(8) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.2(8) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 120.2(7) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C8 C7 C12 119.5(6) . . ? C8 C7 P1 123.4(5) . . ? C12 C7 P1 117.1(5) . . ? C9 C8 C7 120.5(7) . . ? C9 C8 H8A 119.8 . . ? C7 C8 H8A 119.8 . . ? C10 C9 C8 120.8(8) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 120.5(8) . . ? C9 C10 H10A 119.8 . . ? C11 C10 H10A 119.8 . . ? C10 C11 C12 119.3(8) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C7 C12 C11 119.4(7) . . ? C7 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C14 C13 C18 119.0(6) . . ? C14 C13 P1 121.8(5) . . ? C18 C13 P1 119.1(5) . . ? C13 C14 C15 119.4(7) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 120.6(8) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 120.4(7) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 119.0(8) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C13 121.6(8) . . ? C17 C18 H18A 119.2 . . ? C13 C18 H18A 119.2 . . ? C20 C19 N1 112.1(7) . . ? C20 C19 H19A 109.2 . . ? N1 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? N1 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N2 C20 C19 114.5(6) . . ? N2 C20 H2 36.8(5) . . ? C19 C20 H2 136.2(10) . . ? N2 C20 H20A 108.6 . . ? C19 C20 H20A 108.6 . . ? H2 C20 H20A 112.4 . . ? N2 C20 H20B 108.6 . . ? C19 C20 H20B 108.6 . . ? H2 C20 H20B 72.9 . . ? H20A C20 H20B 107.6 . . ? N2 C20A H20C 108.6 . . ? N2 C20A H20D 108.6 . . ? H20C C20A H20D 107.6 . . ? Cl4 C1S Cl3 111.1(5) . . ? Cl4 C1S H1SA 109.4 . . ? Cl3 C1S H1SA 109.4 . . ? Cl4 C1S H1SB 109.4 . . ? Cl3 C1S H1SB 109.4 . . ? H1SA C1S H1SB 108.0 . . ? 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 C13 P1 N1 C19 0.1(7) . . . . ? C7 P1 N1 C19 118.7(6) . . . . ? C1 P1 N1 C19 -115.1(6) . . . . ? C13 P1 N1 Pd1 -166.6(3) . . . . ? C7 P1 N1 Pd1 -47.9(4) . . . . ? C1 P1 N1 Pd1 78.3(4) . . . . ? N2 Pd1 N1 C19 -3.7(4) . . . . ? N1 Pd1 N1 C19 -3.7(4) 2 . . . ? Cl1 Pd1 N1 C19 176.3(4) . . . . ? N2 Pd1 N1 P1 164.5(4) . . . . ? N1 Pd1 N1 P1 164.5(4) 2 . . . ? Cl1 Pd1 N1 P1 -15.5(4) . . . . ? N1 Pd1 N2 C20 21.0(6) 2 . . 2 ? N1 Pd1 N2 C20 -159.0(6) . . . 2 ? Cl1 Pd1 N2 C20 -19(100) . . . 2 ? N1 Pd1 N2 C20 -159.0(6) 2 . . . ? N1 Pd1 N2 C20 21.0(6) . . . . ? Cl1 Pd1 N2 C20 161(100) . . . . ? N1 Pd1 N2 C20A 167.0(6) 2 . . . ? N1 Pd1 N2 C20A -13.0(6) . . . . ? Cl1 Pd1 N2 C20A 127(100) . . . . ? N1 Pd1 N2 C20A -13.0(6) 2 . . 2 ? N1 Pd1 N2 C20A 167.0(6) . . . 2 ? Cl1 Pd1 N2 C20A -53(100) . . . 2 ? N1 P1 C1 C2 -3.3(6) . . . . ? C13 P1 C1 C2 -122.4(5) . . . . ? C7 P1 C1 C2 122.5(5) . . . . ? N1 P1 C1 C6 170.3(5) . . . . ? C13 P1 C1 C6 51.2(6) . . . . ? C7 P1 C1 C6 -63.9(6) . . . . ? C6 C1 C2 C3 0.7(10) . . . . ? P1 C1 C2 C3 174.4(6) . . . . ? C1 C2 C3 C4 -0.3(12) . . . . ? C2 C3 C4 C5 0.7(14) . . . . ? C3 C4 C5 C6 -1.4(14) . . . . ? C4 C5 C6 C1 1.7(13) . . . . ? C2 C1 C6 C5 -1.4(10) . . . . ? P1 C1 C6 C5 -174.9(6) . . . . ? N1 P1 C7 C8 151.9(6) . . . . ? C13 P1 C7 C8 -87.3(6) . . . . ? C1 P1 C7 C8 25.8(7) . . . . ? N1 P1 C7 C12 -30.2(6) . . . . ? C13 P1 C7 C12 90.6(6) . . . . ? C1 P1 C7 C12 -156.2(5) . . . . ? C12 C7 C8 C9 -0.8(11) . . . . ? P1 C7 C8 C9 177.1(7) . . . . ? C7 C8 C9 C10 1.6(14) . . . . ? C8 C9 C10 C11 -0.2(16) . . . . ? C9 C10 C11 C12 -2.0(15) . . . . ? C8 C7 C12 C11 -1.4(11) . . . . ? P1 C7 C12 C11 -179.4(6) . . . . ? C10 C11 C12 C7 2.8(13) . . . . ? N1 P1 C13 C14 102.7(6) . . . . ? C7 P1 C13 C14 -18.6(6) . . . . ? C1 P1 C13 C14 -137.2(6) . . . . ? N1 P1 C13 C18 -72.6(6) . . . . ? C7 P1 C13 C18 166.1(5) . . . . ? C1 P1 C13 C18 47.4(6) . . . . ? C18 C13 C14 C15 1.3(10) . . . . ? P1 C13 C14 C15 -174.1(5) . . . . ? C13 C14 C15 C16 -1.2(11) . . . . ? C14 C15 C16 C17 1.7(13) . . . . ? C15 C16 C17 C18 -2.2(13) . . . . ? C16 C17 C18 C13 2.3(12) . . . . ? C14 C13 C18 C17 -1.9(11) . . . . ? P1 C13 C18 C17 173.6(6) . . . . ? P1 N1 C19 C20 177.3(7) . . . . ? Pd1 N1 C19 C20 -14.4(9) . . . . ? C20 N2 C20 C19 143.7(12) 2 . . . ? C20A N2 C20 C19 63.8(6) . . . . ? C20A N2 C20 C19 -175.7(12) 2 . . . ? Pd1 N2 C20 C19 -36.3(12) . . . . ? N1 C19 C20 N2 33.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.350 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.121 # Attachment '- 9-FD014_0m.cif' data_fd014_0m _database_code_depnum_ccdc_archive 'CCDC 809531' #TrackingRef '- 9-FD014_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H51 Cl2 N3 P2 Pd' _chemical_formula_weight 596.90 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n 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 8.6503(2) _cell_length_b 26.8756(5) _cell_length_c 12.0880(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.1560(10) _cell_angle_gamma 90.00 _cell_volume 2805.98(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6967 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.43 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6779 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21416 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4934 _reflns_number_gt 4160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+8.4318P] 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 4934 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.74762(3) 0.145897(10) 0.58784(2) 0.01466(9) Uani 1 1 d . . . P2 P 0.80506(11) 0.04684(3) 0.76201(8) 0.0180(2) Uani 1 1 d . . . Cl1 Cl 0.90232(11) 0.18621(3) 0.72391(7) 0.0218(2) Uani 1 1 d . . . P1 P 0.84569(11) 0.24510(3) 0.43740(8) 0.0168(2) Uani 1 1 d . . . C15 C 0.7275(5) 0.05463(14) 0.8996(3) 0.0266(9) Uani 1 1 d . . . H15A H 0.7739 0.0283 0.9495 0.032 Uiso 1 1 calc R . . N3 N 0.7114(4) 0.07911(11) 0.6670(3) 0.0233(7) Uani 1 1 d . . . C8 C 0.8036(4) 0.25388(14) 0.2878(3) 0.0237(9) Uani 1 1 d . . . H8A H 0.6883 0.2556 0.2772 0.028 Uiso 1 1 calc R . . C2 C 1.0402(4) 0.22179(14) 0.4698(3) 0.0215(8) Uani 1 1 d . . . H2A H 1.0551 0.2225 0.5524 0.026 Uiso 1 1 calc R . . C1 C 1.0672(5) 0.16779(15) 0.4357(4) 0.0278(9) Uani 1 1 d . . . H1A H 1.1744 0.1584 0.4562 0.042 Uiso 1 1 calc R . . H1B H 1.0480 0.1645 0.3554 0.042 Uiso 1 1 calc R . . H1C H 0.9964 0.1460 0.4737 0.042 Uiso 1 1 calc R . . C7 C 0.8650(6) 0.30233(17) 0.2385(4) 0.0378(11) Uani 1 1 d . . . H7A H 0.8367 0.3035 0.1590 0.057 Uiso 1 1 calc R . . H7B H 0.9780 0.3035 0.2502 0.057 Uiso 1 1 calc R . . H7C H 0.8194 0.3309 0.2751 0.057 Uiso 1 1 calc R . . C3 C 1.1633(5) 0.25637(15) 0.4267(4) 0.0312(10) Uani 1 1 d . . . H3A H 1.2663 0.2426 0.4456 0.047 Uiso 1 1 calc R . . H3B H 1.1544 0.2893 0.4608 0.047 Uiso 1 1 calc R . . H3C H 1.1482 0.2594 0.3461 0.047 Uiso 1 1 calc R . . Cl2 Cl 0.66490(16) 0.05853(5) 0.26461(12) 0.0566(4) Uani 1 1 d . . . N1 N 0.7245(3) 0.20673(12) 0.4854(3) 0.0255(8) Uani 1 1 d . . . C21 C 1.0051(4) 0.06732(14) 0.7756(3) 0.0190(8) Uani 1 1 d . . . H21A H 1.0014 0.1026 0.8014 0.023 Uiso 1 1 calc R . . C19 C 0.8771(5) -0.03214(15) 0.6259(4) 0.0304(10) Uani 1 1 d . . . H19A H 0.8662 -0.0677 0.6090 0.046 Uiso 1 1 calc R . . H19B H 0.9868 -0.0242 0.6408 0.046 Uiso 1 1 calc R . . H19C H 0.8360 -0.0126 0.5624 0.046 Uiso 1 1 calc R . . C22 C 1.0889(4) 0.06865(15) 0.6667(3) 0.0255(9) Uani 1 1 d . . . H22A H 1.1956 0.0800 0.6816 0.038 Uiso 1 1 calc R . . H22B H 1.0348 0.0915 0.6147 0.038 Uiso 1 1 calc R . . H22C H 1.0896 0.0352 0.6344 0.038 Uiso 1 1 calc R . . C17 C 0.8273(6) -0.05588(15) 0.8221(4) 0.0410(12) Uani 1 1 d . . . H17A H 0.8138 -0.0901 0.7951 0.062 Uiso 1 1 calc R . . H17B H 0.7588 -0.0501 0.8827 0.062 Uiso 1 1 calc R . . H17C H 0.9351 -0.0508 0.8489 0.062 Uiso 1 1 calc R . . C14 C 0.5513(5) 0.04751(19) 0.8926(5) 0.0477(13) Uani 1 1 d . . . H14A H 0.5115 0.0517 0.9664 0.072 Uiso 1 1 calc R . . H14B H 0.5263 0.0140 0.8651 0.072 Uiso 1 1 calc R . . H14C H 0.5035 0.0722 0.8419 0.072 Uiso 1 1 calc R . . N2 N 0.5951(4) 0.11699(13) 0.4728(3) 0.0250(7) Uani 1 1 d . . . H2B H 0.6473 0.0965 0.4253 0.030 Uiso 1 1 calc R . . C5 C 0.8376(5) 0.30799(15) 0.4973(3) 0.0295(9) Uani 1 1 d . . . H5A H 0.9032 0.3303 0.4531 0.035 Uiso 1 1 calc R . . C20 C 1.1015(4) 0.03944(16) 0.8655(3) 0.0281(9) Uani 1 1 d . . . H20A H 1.2079 0.0521 0.8688 0.042 Uiso 1 1 calc R . . H20B H 1.1019 0.0038 0.8481 0.042 Uiso 1 1 calc R . . H20C H 1.0565 0.0445 0.9373 0.042 Uiso 1 1 calc R . . C4 C 0.8994(6) 0.31033(16) 0.6171(4) 0.0396(12) Uani 1 1 d . . . H4A H 0.8921 0.3446 0.6443 0.059 Uiso 1 1 calc R . . H4B H 1.0078 0.2996 0.6222 0.059 Uiso 1 1 calc R . . H4C H 0.8381 0.2883 0.6623 0.059 Uiso 1 1 calc R . . C6 C 0.6710(6) 0.32737(18) 0.4854(4) 0.0434(12) Uani 1 1 d . . . H6A H 0.6664 0.3608 0.5173 0.065 Uiso 1 1 calc R . . H6B H 0.6030 0.3050 0.5245 0.065 Uiso 1 1 calc R . . H6C H 0.6371 0.3286 0.4068 0.065 Uiso 1 1 calc R . . C16 C 0.7689(6) 0.10514(16) 0.9506(4) 0.0377(11) Uani 1 1 d . . . H16A H 0.7255 0.1077 1.0236 0.056 Uiso 1 1 calc R . . H16B H 0.7260 0.1316 0.9023 0.056 Uiso 1 1 calc R . . H16C H 0.8817 0.1086 0.9586 0.056 Uiso 1 1 calc R . . C9 C 0.8527(5) 0.20880(17) 0.2212(4) 0.0357(11) Uani 1 1 d . . . H9A H 0.8286 0.2148 0.1421 0.053 Uiso 1 1 calc R . . H9B H 0.7966 0.1793 0.2447 0.053 Uiso 1 1 calc R . . H9C H 0.9642 0.2034 0.2341 0.053 Uiso 1 1 calc R . . C18 C 0.7870(5) -0.01962(13) 0.7280(3) 0.0223(8) Uani 1 1 d . . . H18A H 0.6753 -0.0253 0.7059 0.027 Uiso 1 1 calc R . . C11 C 0.5187(6) 0.15840(19) 0.4076(5) 0.0522(15) Uani 1 1 d . . . H11A H 0.5471 0.1558 0.3296 0.063 Uiso 1 1 calc R . . H11B H 0.4050 0.1545 0.4088 0.063 Uiso 1 1 calc R . . C13 C 0.5751(6) 0.05511(19) 0.6054(5) 0.0610(18) Uani 1 1 d . . . H13A H 0.6126 0.0270 0.5614 0.073 Uiso 1 1 calc R . . H13B H 0.5051 0.0414 0.6599 0.073 Uiso 1 1 calc R . . C10 C 0.5618(5) 0.20797(19) 0.4498(5) 0.0517(15) Uani 1 1 d . . . H10A H 0.5434 0.2332 0.3908 0.062 Uiso 1 1 calc R . . H10B H 0.4987 0.2168 0.5128 0.062 Uiso 1 1 calc R . . C12 C 0.4909(6) 0.0873(2) 0.5348(4) 0.0563(16) Uani 1 1 d . . . H12A H 0.4260 0.1094 0.5787 0.068 Uiso 1 1 calc R . . H12B H 0.4217 0.0679 0.4831 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01441(14) 0.01468(14) 0.01478(15) 0.00165(12) -0.00014(10) -0.00041(11) P2 0.0207(5) 0.0124(4) 0.0207(5) 0.0023(4) -0.0004(4) -0.0017(4) Cl1 0.0289(5) 0.0170(4) 0.0188(5) -0.0001(4) -0.0028(4) -0.0045(4) P1 0.0179(5) 0.0166(5) 0.0162(5) 0.0032(4) 0.0026(4) 0.0028(4) C15 0.032(2) 0.021(2) 0.028(2) 0.0020(18) 0.0094(18) -0.0030(17) N3 0.0203(16) 0.0187(16) 0.0300(19) 0.0070(15) -0.0059(14) -0.0069(13) C8 0.025(2) 0.029(2) 0.018(2) 0.0070(17) 0.0035(16) -0.0021(17) C2 0.0175(18) 0.024(2) 0.023(2) 0.0025(17) 0.0036(15) 0.0002(15) C1 0.024(2) 0.024(2) 0.035(2) 0.0029(19) 0.0059(18) 0.0041(17) C7 0.049(3) 0.039(3) 0.026(2) 0.015(2) 0.008(2) -0.003(2) C3 0.021(2) 0.030(2) 0.043(3) 0.005(2) 0.0066(18) -0.0042(17) Cl2 0.0605(8) 0.0530(8) 0.0574(9) -0.0297(7) 0.0152(7) 0.0015(6) N1 0.0153(16) 0.0321(19) 0.0293(19) 0.0175(16) 0.0042(13) 0.0045(14) C21 0.0191(18) 0.0174(18) 0.020(2) 0.0001(16) -0.0019(15) -0.0002(15) C19 0.036(2) 0.021(2) 0.033(2) -0.0065(19) -0.0030(19) -0.0014(18) C22 0.024(2) 0.024(2) 0.029(2) 0.0015(18) 0.0058(17) -0.0029(16) C17 0.073(3) 0.013(2) 0.036(3) 0.0053(19) -0.008(2) -0.001(2) C14 0.037(3) 0.052(3) 0.057(3) -0.002(3) 0.020(2) -0.011(2) N2 0.0191(16) 0.038(2) 0.0180(17) -0.0017(15) 0.0004(13) -0.0067(14) C5 0.042(2) 0.022(2) 0.024(2) 0.0004(18) -0.0040(18) 0.0096(18) C20 0.023(2) 0.034(2) 0.026(2) 0.0022(19) -0.0067(17) 0.0036(17) C4 0.058(3) 0.026(2) 0.033(3) -0.010(2) -0.012(2) 0.016(2) C6 0.056(3) 0.040(3) 0.034(3) -0.008(2) -0.007(2) 0.030(2) C16 0.050(3) 0.029(2) 0.036(3) -0.008(2) 0.018(2) -0.003(2) C9 0.036(2) 0.049(3) 0.022(2) -0.005(2) 0.0034(19) 0.002(2) C18 0.031(2) 0.0134(18) 0.021(2) 0.0020(16) -0.0068(16) -0.0046(16) C11 0.036(3) 0.060(3) 0.057(3) -0.027(3) -0.031(2) 0.034(2) C13 0.038(3) 0.045(3) 0.097(5) 0.041(3) -0.027(3) -0.028(2) C10 0.025(2) 0.055(3) 0.074(4) 0.038(3) -0.006(2) -0.008(2) C12 0.044(3) 0.093(4) 0.032(3) 0.011(3) -0.007(2) -0.041(3) _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 N2 2.019(3) . ? Pd1 N1 2.054(3) . ? Pd1 N3 2.066(3) . ? Pd1 Cl1 2.3297(9) . ? P2 N3 1.620(3) . ? P2 C21 1.814(4) . ? P2 C18 1.838(4) . ? P2 C15 1.840(4) . ? P1 N1 1.602(3) . ? P1 C2 1.818(4) . ? P1 C8 1.840(4) . ? P1 C5 1.842(4) . ? C15 C16 1.525(6) . ? C15 C14 1.534(6) . ? N3 C13 1.505(5) . ? C8 C9 1.528(6) . ? C8 C7 1.538(5) . ? C2 C3 1.527(5) . ? C2 C1 1.530(5) . ? N1 C10 1.450(5) . ? C21 C20 1.530(5) . ? C21 C22 1.538(5) . ? C19 C18 1.533(6) . ? C17 C18 1.524(5) . ? N2 C12 1.444(5) . ? N2 C11 1.496(6) . ? C5 C4 1.517(6) . ? C5 C6 1.532(6) . ? C11 C10 1.467(7) . ? C13 C12 1.392(7) . ? 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 Pd1 N1 81.52(13) . . ? N2 Pd1 N3 82.81(13) . . ? N1 Pd1 N3 163.43(12) . . ? N2 Pd1 Cl1 173.43(10) . . ? N1 Pd1 Cl1 95.08(10) . . ? N3 Pd1 Cl1 99.96(9) . . ? N3 P2 C21 109.81(16) . . ? N3 P2 C18 109.17(17) . . ? C21 P2 C18 112.57(18) . . ? N3 P2 C15 112.79(18) . . ? C21 P2 C15 106.09(18) . . ? C18 P2 C15 106.40(18) . . ? N1 P1 C2 108.46(17) . . ? N1 P1 C8 109.92(18) . . ? C2 P1 C8 112.73(18) . . ? N1 P1 C5 114.11(19) . . ? C2 P1 C5 106.63(18) . . ? C8 P1 C5 105.02(18) . . ? C16 C15 C14 110.1(4) . . ? C16 C15 P2 112.2(3) . . ? C14 C15 P2 110.3(3) . . ? C13 N3 P2 118.0(3) . . ? C13 N3 Pd1 106.2(2) . . ? P2 N3 Pd1 135.29(17) . . ? C9 C8 C7 110.8(3) . . ? C9 C8 P1 111.7(3) . . ? C7 C8 P1 115.8(3) . . ? C3 C2 C1 111.5(3) . . ? C3 C2 P1 111.8(3) . . ? C1 C2 P1 115.0(3) . . ? C10 N1 P1 121.4(3) . . ? C10 N1 Pd1 105.0(3) . . ? P1 N1 Pd1 133.38(18) . . ? C20 C21 C22 110.8(3) . . ? C20 C21 P2 113.3(3) . . ? C22 C21 P2 114.9(3) . . ? C12 N2 C11 114.5(4) . . ? C12 N2 Pd1 104.9(3) . . ? C11 N2 Pd1 109.2(3) . . ? C4 C5 C6 110.8(4) . . ? C4 C5 P1 113.2(3) . . ? C6 C5 P1 109.3(3) . . ? C17 C18 C19 110.8(3) . . ? C17 C18 P2 116.2(3) . . ? C19 C18 P2 110.7(3) . . ? C10 C11 N2 113.4(4) . . ? C12 C13 N3 113.9(4) . . ? N1 C10 C11 107.8(4) . . ? C13 C12 N2 110.0(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.382 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.090 # Attachment '- 11-rc008_0m.cif' data_rc008_0m _database_code_depnum_ccdc_archive 'CCDC 809532' #TrackingRef '- 11-rc008_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H39 Br0.50 Cl1.50 N3 Ni P2' _chemical_formula_weight 775.52 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 12.0407(13) _cell_length_b 22.977(3) _cell_length_c 13.4590(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.437(5) _cell_angle_gamma 90.00 _cell_volume 3692.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 1.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6434 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74042 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8424 _reflns_number_gt 5601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0432P)^2^+2.1460P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8424 _refine_ls_number_parameters 441 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.60827(3) 0.084617(16) 0.36262(3) 0.01935(11) Uani 1 1 d D . . P1 P 0.42383(6) 0.19695(3) 0.38068(6) 0.02279(18) Uani 1 1 d . . . P2 P 0.76847(6) -0.01223(3) 0.24651(6) 0.02257(18) Uani 1 1 d . . . N3 N 0.7324(2) 0.02224(10) 0.33934(17) 0.0218(5) Uani 1 1 d . . . N2 N 0.6544(2) 0.06452(10) 0.50758(17) 0.0226(5) Uani 1 1 d . . . H2B H 0.6107 0.0335 0.5241 0.027 Uiso 1 1 calc R . . N1 N 0.50022(19) 0.14409(11) 0.42196(17) 0.0229(6) Uani 1 1 d . . . C37 C 1.0783(3) -0.02877(15) 0.1531(3) 0.0382(9) Uani 1 1 d . . . H37A H 1.1115 -0.0501 0.1041 0.046 Uiso 1 1 calc R . . C38 C 1.1420(3) 0.00950(15) 0.2148(2) 0.0334(8) Uani 1 1 d . . . H38A H 1.2196 0.0136 0.2099 0.040 Uiso 1 1 calc R . . C39 C 1.0934(3) 0.04193(14) 0.2839(2) 0.0307(7) Uani 1 1 d . . . H39A H 1.1371 0.0693 0.3250 0.037 Uiso 1 1 calc R . . C40 C 0.9809(3) 0.03460(13) 0.2936(2) 0.0269(7) Uani 1 1 d . . . H40A H 0.9477 0.0571 0.3412 0.032 Uiso 1 1 calc R . . C35 C 0.9163(2) -0.00562(13) 0.2340(2) 0.0253(7) Uani 1 1 d . . . C36 C 0.9662(3) -0.03627(15) 0.1618(2) 0.0353(8) Uani 1 1 d . . . H36A H 0.9226 -0.0625 0.1184 0.042 Uiso 1 1 calc R . . C34 C 0.6246(3) -0.10415(14) 0.2412(2) 0.0284(7) Uani 1 1 d . . . H34A H 0.5696 -0.0743 0.2369 0.034 Uiso 1 1 calc R . . C33 C 0.5920(3) -0.16166(14) 0.2411(2) 0.0310(8) Uani 1 1 d . . . H33A H 0.5147 -0.1712 0.2361 0.037 Uiso 1 1 calc R . . C29 C 0.7375(2) -0.08936(13) 0.2474(2) 0.0252(7) Uani 1 1 d . . . C30 C 0.8167(3) -0.13382(14) 0.2571(2) 0.0314(8) Uani 1 1 d . . . H30A H 0.8942 -0.1246 0.2631 0.038 Uiso 1 1 calc R . . C32 C 0.6710(3) -0.20540(14) 0.2483(2) 0.0320(8) Uani 1 1 d . . . H32A H 0.6483 -0.2450 0.2465 0.038 Uiso 1 1 calc R . . C31 C 0.7833(3) -0.19127(14) 0.2580(3) 0.0350(8) Uani 1 1 d . . . H31A H 0.8380 -0.2213 0.2653 0.042 Uiso 1 1 calc R . . C22 C 0.7774(3) -0.00119(14) 0.4385(2) 0.0280(7) Uani 1 1 d . . . H22A H 0.8561 -0.0135 0.4382 0.034 Uiso 1 1 calc R . . H22B H 0.7332 -0.0356 0.4542 0.034 Uiso 1 1 calc R . . C21 C 0.7712(3) 0.04537(14) 0.5169(2) 0.0315(8) Uani 1 1 d . . . H21A H 0.7948 0.0295 0.5847 0.038 Uiso 1 1 calc R . . H21B H 0.8207 0.0784 0.5054 0.038 Uiso 1 1 calc R . . C20 C 0.6299(3) 0.11480(14) 0.5674(2) 0.0303(7) Uani 1 1 d . . . H20A H 0.6828 0.1469 0.5589 0.036 Uiso 1 1 calc R . . H20B H 0.6371 0.1043 0.6392 0.036 Uiso 1 1 calc R . . C19 C 0.5114(3) 0.13349(14) 0.5310(2) 0.0300(7) Uani 1 1 d . . . H19A H 0.4583 0.1027 0.5458 0.036 Uiso 1 1 calc R . . H19B H 0.4933 0.1695 0.5661 0.036 Uiso 1 1 calc R . . C6 C 0.1953(3) 0.20221(14) 0.3024(2) 0.0324(8) Uani 1 1 d . . . H6A H 0.2199 0.2156 0.2422 0.039 Uiso 1 1 calc R . . C5 C 0.0817(3) 0.19558(15) 0.3071(3) 0.0369(8) Uani 1 1 d . . . H5A H 0.0290 0.2045 0.2503 0.044 Uiso 1 1 calc R . . C4 C 0.0450(3) 0.17619(15) 0.3937(3) 0.0380(9) Uani 1 1 d . . . H4A H -0.0328 0.1719 0.3971 0.046 Uiso 1 1 calc R . . C3 C 0.1217(3) 0.16305(17) 0.4754(3) 0.0437(9) Uani 1 1 d . . . H3A H 0.0963 0.1493 0.5351 0.052 Uiso 1 1 calc R . . C2 C 0.2352(3) 0.16952(16) 0.4718(2) 0.0383(9) Uani 1 1 d . . . H2A H 0.2871 0.1603 0.5290 0.046 Uiso 1 1 calc R . . C18 C 0.4339(3) 0.16378(14) 0.1849(2) 0.0293(7) Uani 1 1 d . . . H18A H 0.4420 0.1252 0.2100 0.035 Uiso 1 1 calc R . . C17 C 0.4239(3) 0.17392(15) 0.0826(2) 0.0356(8) Uani 1 1 d . . . H17A H 0.4271 0.1422 0.0377 0.043 Uiso 1 1 calc R . . C16 C 0.4092(3) 0.23016(16) 0.0452(3) 0.0408(9) Uani 1 1 d . . . H16A H 0.4003 0.2368 -0.0251 0.049 Uiso 1 1 calc R . . C15 C 0.4076(3) 0.27615(16) 0.1105(3) 0.0382(8) Uani 1 1 d . . . H15A H 0.3982 0.3147 0.0852 0.046 Uiso 1 1 calc R . . C14 C 0.4197(3) 0.26663(14) 0.2125(2) 0.0314(7) Uani 1 1 d . . . H14A H 0.4197 0.2987 0.2570 0.038 Uiso 1 1 calc R . . C13 C 0.4320(2) 0.21018(13) 0.2506(2) 0.0238(7) Uani 1 1 d . . . C11 C 0.4291(3) 0.34904(16) 0.5415(3) 0.0515(11) Uani 1 1 d . . . H11A H 0.3781 0.3738 0.5693 0.062 Uiso 1 1 calc R . . C12 C 0.3895(3) 0.29991(15) 0.4883(3) 0.0403(9) Uani 1 1 d . . . H12A H 0.3117 0.2913 0.4794 0.048 Uiso 1 1 calc R . . C10 C 0.5403(3) 0.36215(15) 0.5541(3) 0.0415(9) Uani 1 1 d . . . H10A H 0.5666 0.3960 0.5903 0.050 Uiso 1 1 calc R . . C9 C 0.6147(3) 0.32611(15) 0.5143(3) 0.0402(9) Uani 1 1 d . . . H9A H 0.6923 0.3353 0.5230 0.048 Uiso 1 1 calc R . . C8 C 0.5770(3) 0.27682(14) 0.4619(2) 0.0335(8) Uani 1 1 d . . . H8A H 0.6287 0.2520 0.4351 0.040 Uiso 1 1 calc R . . C7 C 0.4636(3) 0.26352(13) 0.4483(2) 0.0259(7) Uani 1 1 d . . . C23 C 0.7000(2) 0.01533(14) 0.1296(2) 0.0267(7) Uani 1 1 d . . . C24 C 0.6755(3) -0.02213(17) 0.0477(2) 0.0393(9) Uani 1 1 d . . . H24A H 0.6857 -0.0629 0.0568 0.047 Uiso 1 1 calc R . . C28 C 0.6847(3) 0.07449(15) 0.1157(2) 0.0341(8) Uani 1 1 d . . . H28A H 0.7000 0.1004 0.1708 0.041 Uiso 1 1 calc R . . C27 C 0.6466(3) 0.09610(18) 0.0205(3) 0.0447(10) Uani 1 1 d . . . H27A H 0.6362 0.1368 0.0108 0.054 Uiso 1 1 calc R . . C26 C 0.6239(3) 0.0582(2) -0.0601(3) 0.0482(11) Uani 1 1 d . . . H26A H 0.5994 0.0731 -0.1251 0.058 Uiso 1 1 calc R . . C25 C 0.6369(3) -0.0005(2) -0.0459(3) 0.0476(10) Uani 1 1 d . . . H25A H 0.6192 -0.0265 -0.1006 0.057 Uiso 1 1 calc R . . C1 C 0.2739(2) 0.18948(13) 0.3848(2) 0.0272(7) Uani 1 1 d . . . Br1 Br 0.4462(4) 0.0201(3) 0.3191(4) 0.0144(8) Uiso 0.25 1 d PD . . Br2 Br 0.7367(3) 0.16245(16) 0.33715(18) 0.0124(7) Uiso 0.25 1 d PD . . Cl1 Cl 0.4594(3) 0.0180(2) 0.3126(3) 0.0201(6) Uani 0.75 1 d PD . . Cl2 Cl 0.7349(4) 0.16114(19) 0.3378(3) 0.0541(12) Uani 0.75 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0191(2) 0.0198(2) 0.01898(19) 0.00095(15) 0.00183(14) 0.00121(16) P1 0.0211(4) 0.0231(4) 0.0241(4) -0.0019(3) 0.0025(3) 0.0024(3) P2 0.0200(4) 0.0246(4) 0.0234(4) -0.0028(3) 0.0038(3) -0.0002(3) N3 0.0248(14) 0.0189(13) 0.0213(12) 0.0010(10) 0.0020(10) 0.0041(11) N2 0.0265(14) 0.0196(13) 0.0221(12) 0.0004(10) 0.0051(10) 0.0024(11) N1 0.0213(13) 0.0276(14) 0.0199(13) -0.0001(10) 0.0026(10) 0.0049(11) C37 0.0282(19) 0.048(2) 0.041(2) -0.0059(17) 0.0129(16) 0.0004(17) C38 0.0213(17) 0.039(2) 0.0407(19) 0.0123(16) 0.0056(15) 0.0027(15) C39 0.0256(18) 0.0282(18) 0.0363(18) 0.0070(15) -0.0037(14) -0.0024(15) C40 0.0271(17) 0.0237(17) 0.0291(17) 0.0033(13) 0.0005(14) 0.0005(14) C35 0.0242(17) 0.0256(17) 0.0262(16) 0.0004(13) 0.0039(13) 0.0009(14) C36 0.0289(18) 0.042(2) 0.0362(19) -0.0121(16) 0.0096(15) -0.0047(16) C34 0.0251(17) 0.0265(18) 0.0344(18) -0.0055(14) 0.0068(14) 0.0024(14) C33 0.0276(18) 0.0325(19) 0.0339(18) -0.0062(14) 0.0074(14) -0.0054(15) C29 0.0249(16) 0.0273(18) 0.0235(15) -0.0073(13) 0.0036(12) -0.0017(14) C30 0.0227(17) 0.031(2) 0.0405(19) -0.0053(15) 0.0048(14) 0.0014(15) C32 0.037(2) 0.0248(19) 0.0357(18) -0.0065(14) 0.0083(15) -0.0038(15) C31 0.033(2) 0.0240(19) 0.049(2) -0.0057(15) 0.0083(16) 0.0048(15) C22 0.0322(18) 0.0278(18) 0.0240(16) 0.0055(13) 0.0030(14) 0.0097(14) C21 0.0354(19) 0.034(2) 0.0235(16) 0.0040(14) -0.0020(14) 0.0091(16) C20 0.040(2) 0.0301(19) 0.0203(15) -0.0019(13) 0.0021(14) 0.0047(15) C19 0.0354(19) 0.0327(19) 0.0228(16) 0.0008(14) 0.0071(14) 0.0074(15) C6 0.0281(18) 0.036(2) 0.0327(18) -0.0022(15) 0.0009(14) 0.0012(15) C5 0.0264(18) 0.039(2) 0.043(2) -0.0073(16) -0.0041(15) 0.0073(16) C4 0.0214(18) 0.044(2) 0.050(2) -0.0154(18) 0.0095(16) 0.0010(16) C3 0.0282(19) 0.061(3) 0.044(2) -0.0019(19) 0.0121(17) -0.0006(18) C2 0.0269(18) 0.057(2) 0.0317(18) -0.0004(17) 0.0058(15) 0.0059(17) C18 0.0310(18) 0.0313(19) 0.0250(16) 0.0022(14) 0.0005(14) 0.0027(15) C17 0.038(2) 0.041(2) 0.0279(17) -0.0030(15) 0.0038(15) -0.0057(16) C16 0.039(2) 0.054(3) 0.0285(18) 0.0132(17) 0.0025(15) -0.0064(18) C15 0.036(2) 0.038(2) 0.040(2) 0.0149(17) 0.0042(16) -0.0005(17) C14 0.0278(18) 0.0302(19) 0.0364(18) 0.0020(15) 0.0056(14) -0.0005(15) C13 0.0179(15) 0.0278(18) 0.0255(16) 0.0012(13) 0.0021(12) 0.0035(13) C11 0.048(2) 0.043(2) 0.062(3) -0.026(2) 0.005(2) 0.011(2) C12 0.034(2) 0.036(2) 0.051(2) -0.0145(17) 0.0042(17) 0.0039(17) C10 0.054(2) 0.030(2) 0.037(2) -0.0072(16) -0.0056(17) -0.0032(18) C9 0.040(2) 0.037(2) 0.042(2) -0.0051(17) -0.0013(17) -0.0053(17) C8 0.0338(19) 0.0308(19) 0.0361(18) -0.0071(15) 0.0052(15) -0.0008(15) C7 0.0277(17) 0.0238(17) 0.0252(16) -0.0008(13) 0.0001(13) 0.0026(14) C23 0.0166(15) 0.039(2) 0.0254(16) 0.0003(14) 0.0044(12) -0.0006(14) C24 0.0310(19) 0.056(2) 0.0312(18) -0.0044(17) 0.0040(15) -0.0055(17) C28 0.0292(18) 0.044(2) 0.0292(17) 0.0034(15) 0.0050(14) 0.0013(16) C27 0.035(2) 0.058(3) 0.042(2) 0.0227(19) 0.0064(17) 0.0053(18) C26 0.028(2) 0.088(3) 0.0267(19) 0.016(2) -0.0017(15) -0.008(2) C25 0.037(2) 0.080(3) 0.0247(18) -0.0023(19) 0.0026(16) -0.013(2) C1 0.0243(17) 0.0257(18) 0.0317(17) -0.0065(14) 0.0035(14) 0.0021(14) Cl1 0.0124(11) 0.0223(10) 0.0258(11) -0.0037(6) 0.0035(8) -0.0028(9) Cl2 0.0468(13) 0.0317(11) 0.0854(19) 0.0062(7) 0.0152(7) -0.0049(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.012(2) . ? Ni1 N1 2.114(2) . ? Ni1 N3 2.123(2) . ? Ni1 Cl2 2.379(4) . ? Ni1 Cl1 2.386(4) . ? Ni1 Br2 2.417(3) . ? Ni1 Br1 2.461(5) . ? P1 N1 1.580(2) . ? P1 C13 1.793(3) . ? P1 C7 1.812(3) . ? P1 C1 1.821(3) . ? P2 N3 1.587(2) . ? P2 C23 1.795(3) . ? P2 C29 1.811(3) . ? P2 C35 1.815(3) . ? N3 C22 1.475(4) . ? N2 C20 1.460(4) . ? N2 C21 1.463(4) . ? N1 C19 1.477(4) . ? C37 C38 1.374(5) . ? C37 C36 1.380(4) . ? C38 C39 1.379(4) . ? C39 C40 1.389(4) . ? C40 C35 1.393(4) . ? C35 C36 1.397(4) . ? C34 C33 1.379(4) . ? C34 C29 1.393(4) . ? C33 C32 1.379(4) . ? C29 C30 1.392(4) . ? C30 C31 1.380(4) . ? C32 C31 1.380(4) . ? C22 C21 1.511(4) . ? C20 C19 1.510(4) . ? C6 C5 1.387(4) . ? C6 C1 1.392(4) . ? C5 C4 1.372(5) . ? C4 C3 1.374(5) . ? C3 C2 1.382(5) . ? C2 C1 1.393(4) . ? C18 C13 1.387(4) . ? C18 C17 1.387(4) . ? C17 C16 1.390(5) . ? C16 C15 1.376(5) . ? C15 C14 1.379(4) . ? C14 C13 1.395(4) . ? C11 C10 1.361(5) . ? C11 C12 1.388(5) . ? C12 C7 1.381(4) . ? C10 C9 1.378(5) . ? C9 C8 1.379(4) . ? C8 C7 1.388(4) . ? C23 C28 1.381(4) . ? C23 C24 1.399(4) . ? C24 C25 1.378(5) . ? C28 C27 1.395(5) . ? C27 C26 1.390(5) . ? C26 C25 1.370(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 N2 Ni1 N1 83.57(9) . . ? N2 Ni1 N3 82.94(9) . . ? N1 Ni1 N3 166.36(9) . . ? N2 Ni1 Cl2 101.81(12) . . ? N1 Ni1 Cl2 90.70(13) . . ? N3 Ni1 Cl2 90.11(13) . . ? N2 Ni1 Cl1 103.25(13) . . ? N1 Ni1 Cl1 92.55(12) . . ? N3 Ni1 Cl1 92.47(13) . . ? Cl2 Ni1 Cl1 154.93(15) . . ? N2 Ni1 Br2 101.90(9) . . ? N1 Ni1 Br2 90.65(10) . . ? N3 Ni1 Br2 90.17(10) . . ? Cl2 Ni1 Br2 0.1(2) . . ? Cl1 Ni1 Br2 154.84(13) . . ? N2 Ni1 Br1 101.73(15) . . ? N1 Ni1 Br1 88.38(14) . . ? N3 Ni1 Br1 96.31(14) . . ? Cl2 Ni1 Br1 156.18(17) . . ? Cl1 Ni1 Br1 4.3(2) . . ? Br2 Ni1 Br1 156.09(15) . . ? N1 P1 C13 111.77(13) . . ? N1 P1 C7 111.61(13) . . ? C13 P1 C7 107.65(14) . . ? N1 P1 C1 116.81(14) . . ? C13 P1 C1 103.02(14) . . ? C7 P1 C1 105.23(14) . . ? N3 P2 C23 111.90(14) . . ? N3 P2 C29 113.95(13) . . ? C23 P2 C29 106.22(14) . . ? N3 P2 C35 113.74(13) . . ? C23 P2 C35 103.52(14) . . ? C29 P2 C35 106.69(14) . . ? C22 N3 P2 115.12(19) . . ? C22 N3 Ni1 107.19(17) . . ? P2 N3 Ni1 136.28(14) . . ? C20 N2 C21 116.8(2) . . ? C20 N2 Ni1 107.63(18) . . ? C21 N2 Ni1 107.05(17) . . ? C19 N1 P1 116.75(19) . . ? C19 N1 Ni1 106.73(17) . . ? P1 N1 Ni1 136.28(13) . . ? C38 C37 C36 120.2(3) . . ? C37 C38 C39 120.1(3) . . ? C38 C39 C40 120.1(3) . . ? C39 C40 C35 120.3(3) . . ? C40 C35 C36 118.4(3) . . ? C40 C35 P2 118.9(2) . . ? C36 C35 P2 122.5(2) . . ? C37 C36 C35 120.7(3) . . ? C33 C34 C29 120.6(3) . . ? C34 C33 C32 120.3(3) . . ? C30 C29 C34 118.5(3) . . ? C30 C29 P2 125.4(2) . . ? C34 C29 P2 116.0(2) . . ? C31 C30 C29 120.4(3) . . ? C33 C32 C31 119.6(3) . . ? C32 C31 C30 120.5(3) . . ? N3 C22 C21 109.1(2) . . ? N2 C21 C22 106.7(3) . . ? N2 C20 C19 107.2(2) . . ? N1 C19 C20 109.2(2) . . ? C5 C6 C1 120.9(3) . . ? C4 C5 C6 120.1(3) . . ? C5 C4 C3 119.6(3) . . ? C4 C3 C2 120.9(3) . . ? C3 C2 C1 120.3(3) . . ? C13 C18 C17 119.8(3) . . ? C18 C17 C16 120.4(3) . . ? C15 C16 C17 119.6(3) . . ? C16 C15 C14 120.4(3) . . ? C15 C14 C13 120.4(3) . . ? C18 C13 C14 119.4(3) . . ? C18 C13 P1 120.0(2) . . ? C14 C13 P1 120.0(2) . . ? C10 C11 C12 120.8(3) . . ? C7 C12 C11 119.8(3) . . ? C11 C10 C9 119.7(3) . . ? C10 C9 C8 120.4(3) . . ? C9 C8 C7 120.1(3) . . ? C12 C7 C8 119.3(3) . . ? C12 C7 P1 124.4(2) . . ? C8 C7 P1 116.3(2) . . ? C28 C23 C24 119.2(3) . . ? C28 C23 P2 120.3(2) . . ? C24 C23 P2 120.0(3) . . ? C25 C24 C23 120.7(4) . . ? C23 C28 C27 119.8(3) . . ? C26 C27 C28 120.1(4) . . ? C25 C26 C27 120.0(3) . . ? C26 C25 C24 120.1(4) . . ? C6 C1 C2 118.2(3) . . ? C6 C1 P1 122.0(2) . . ? C2 C1 P1 119.8(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.871 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.081 # Attachment '- 12-fd011_0m (2).cif' data_fd011_0m _database_code_depnum_ccdc_archive 'CCDC 809533' #TrackingRef '- 12-fd011_0m (2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H51 Cl2 N3 Ni P2' _chemical_formula_weight 549.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 8.6286(6) _cell_length_b 32.013(2) _cell_length_c 10.8902(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.150(2) _cell_angle_gamma 90.00 _cell_volume 2969.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6281 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22133 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5222 _reflns_number_gt 4616 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0278P)^2^+4.6141P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5222 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.76741(4) 0.131122(10) -0.01424(3) 0.01718(10) Uani 1 1 d . . . P1 P 0.83915(9) 0.07843(2) 0.24977(7) 0.01832(16) Uani 1 1 d . . . P2 P 0.43412(9) 0.18002(2) -0.13977(7) 0.02002(17) Uani 1 1 d . . . Cl1 Cl 0.86731(9) 0.19139(2) 0.07166(7) 0.02809(18) Uani 1 1 d . . . N1 N 0.8313(3) 0.08370(7) 0.1013(2) 0.0188(5) Uani 1 1 d . . . N3 N 0.5521(3) 0.14098(7) -0.1059(2) 0.0198(5) Uani 1 1 d . . . C2 C 1.0338(3) 0.08571(9) 0.3402(3) 0.0234(6) Uani 1 1 d . . . H2A H 1.0240 0.0836 0.4302 0.028 Uiso 1 1 calc R . . N2 N 0.7900(3) 0.08812(7) -0.1522(2) 0.0204(5) Uani 1 1 d . . . H2 H 0.8772 0.0944 -0.1887 0.025 Uiso 1 1 d . . . C10 C 0.9037(4) 0.05049(9) 0.0345(3) 0.0247(7) Uani 1 1 d . . . H10A H 0.9044 0.0237 0.0802 0.030 Uiso 1 1 calc R . . H10B H 1.0133 0.0580 0.0279 0.030 Uiso 1 1 calc R . . C8 C 0.7121(4) 0.11865(9) 0.2970(3) 0.0246(6) Uani 1 1 d . . . H8A H 0.7337 0.1448 0.2523 0.030 Uiso 1 1 calc R . . C13 C 0.5111(3) 0.10211(9) -0.1783(3) 0.0248(7) Uani 1 1 d . . . H13A H 0.4144 0.1065 -0.2393 0.030 Uiso 1 1 calc R . . H13B H 0.4918 0.0791 -0.1218 0.030 Uiso 1 1 calc R . . C18 C 0.2314(3) 0.16259(10) -0.1506(3) 0.0277(7) Uani 1 1 d . . . H18A H 0.2139 0.1428 -0.2226 0.033 Uiso 1 1 calc R . . C11 C 0.8078(4) 0.04622(9) -0.0935(3) 0.0268(7) Uani 1 1 d . . . H11A H 0.8612 0.0271 -0.1448 0.032 Uiso 1 1 calc R . . H11B H 0.7033 0.0344 -0.0872 0.032 Uiso 1 1 calc R . . C21 C 0.4474(4) 0.20489(10) -0.2899(3) 0.0311(7) Uani 1 1 d . . . H21A H 0.3842 0.2312 -0.2938 0.037 Uiso 1 1 calc R . . C7 C 0.7423(5) 0.12891(11) 0.4369(3) 0.0397(9) Uani 1 1 d . . . H7A H 0.6696 0.1508 0.4545 0.060 Uiso 1 1 calc R . . H7B H 0.8506 0.1387 0.4606 0.060 Uiso 1 1 calc R . . H7C H 0.7260 0.1038 0.4846 0.060 Uiso 1 1 calc R . . C12 C 0.6464(4) 0.09100(9) -0.2451(3) 0.0253(7) Uani 1 1 d . . . H12A H 0.6257 0.0640 -0.2888 0.030 Uiso 1 1 calc R . . H12B H 0.6591 0.1127 -0.3075 0.030 Uiso 1 1 calc R . . C1 C 1.0982(4) 0.12919(10) 0.3176(3) 0.0334(8) Uani 1 1 d . . . H1A H 1.2026 0.1325 0.3673 0.050 Uiso 1 1 calc R . . H1B H 1.0275 0.1505 0.3418 0.050 Uiso 1 1 calc R . . H1C H 1.1057 0.1323 0.2292 0.050 Uiso 1 1 calc R . . C15 C 0.4883(4) 0.22067(9) -0.0242(3) 0.0306(7) Uani 1 1 d . . . H15A H 0.6046 0.2241 -0.0167 0.037 Uiso 1 1 calc R . . C5 C 0.7797(4) 0.02580(9) 0.2885(3) 0.0299(7) Uani 1 1 d . . . H5A H 0.8686 0.0071 0.2758 0.036 Uiso 1 1 calc R . . C17 C 0.2043(4) 0.13676(11) -0.0371(3) 0.0353(8) Uani 1 1 d . . . H17A H 0.0944 0.1278 -0.0473 0.053 Uiso 1 1 calc R . . H17B H 0.2287 0.1538 0.0382 0.053 Uiso 1 1 calc R . . H17C H 0.2726 0.1121 -0.0296 0.053 Uiso 1 1 calc R . . C3 C 1.1511(4) 0.05242(10) 0.3126(3) 0.0340(8) Uani 1 1 d . . . H3A H 1.2532 0.0576 0.3640 0.051 Uiso 1 1 calc R . . H3B H 1.1621 0.0537 0.2245 0.051 Uiso 1 1 calc R . . H3C H 1.1129 0.0247 0.3317 0.051 Uiso 1 1 calc R . . C20 C 0.3792(4) 0.17858(12) -0.4031(3) 0.0412(9) Uani 1 1 d . . . H20A H 0.3898 0.1938 -0.4794 0.062 Uiso 1 1 calc R . . H20B H 0.2680 0.1730 -0.4010 0.062 Uiso 1 1 calc R . . H20C H 0.4363 0.1521 -0.4014 0.062 Uiso 1 1 calc R . . C22 C 0.6164(4) 0.21763(12) -0.2956(4) 0.0458(9) Uani 1 1 d . . . H22A H 0.6215 0.2312 -0.3756 0.069 Uiso 1 1 calc R . . H22B H 0.6835 0.1928 -0.2872 0.069 Uiso 1 1 calc R . . H22C H 0.6528 0.2371 -0.2278 0.069 Uiso 1 1 calc R . . C6 C 0.6356(5) 0.00898(11) 0.2023(3) 0.0445(9) Uani 1 1 d . . . H6A H 0.6111 -0.0192 0.2290 0.067 Uiso 1 1 calc R . . H6B H 0.6577 0.0079 0.1168 0.067 Uiso 1 1 calc R . . H6C H 0.5458 0.0274 0.2058 0.067 Uiso 1 1 calc R . . C16 C 0.4563(5) 0.20768(11) 0.1045(3) 0.0461(10) Uani 1 1 d . . . H16A H 0.4885 0.2302 0.1640 0.069 Uiso 1 1 calc R . . H16B H 0.5160 0.1823 0.1311 0.069 Uiso 1 1 calc R . . H16C H 0.3439 0.2022 0.1008 0.069 Uiso 1 1 calc R . . C4 C 0.7603(5) 0.02028(11) 0.4257(3) 0.0417(9) Uani 1 1 d . . . H4A H 0.7286 -0.0085 0.4396 0.063 Uiso 1 1 calc R . . H4B H 0.6796 0.0396 0.4457 0.063 Uiso 1 1 calc R . . H4C H 0.8602 0.0263 0.4792 0.063 Uiso 1 1 calc R . . C9 C 0.5390(4) 0.10791(12) 0.2542(4) 0.0428(9) Uani 1 1 d . . . H9A H 0.4729 0.1301 0.2803 0.064 Uiso 1 1 calc R . . H9B H 0.5144 0.0813 0.2915 0.064 Uiso 1 1 calc R . . H9C H 0.5188 0.1054 0.1633 0.064 Uiso 1 1 calc R . . C19 C 0.1079(4) 0.19682(12) -0.1816(4) 0.0475(10) Uani 1 1 d . . . H19A H 0.0028 0.1847 -0.1863 0.071 Uiso 1 1 calc R . . H19B H 0.1183 0.2095 -0.2618 0.071 Uiso 1 1 calc R . . H19C H 0.1232 0.2183 -0.1166 0.071 Uiso 1 1 calc R . . C14 C 0.4170(5) 0.26387(10) -0.0597(4) 0.0482(10) Uani 1 1 d . . . H14A H 0.4541 0.2839 0.0066 0.072 Uiso 1 1 calc R . . H14B H 0.3023 0.2621 -0.0706 0.072 Uiso 1 1 calc R . . H14C H 0.4493 0.2732 -0.1375 0.072 Uiso 1 1 calc R . . Cl2 Cl 0.05878(9) 0.07693(3) 0.68132(7) 0.03305(19) 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 Ni1 0.02010(19) 0.01642(18) 0.01453(18) -0.00127(14) 0.00126(14) 0.00101(14) P1 0.0216(4) 0.0181(3) 0.0150(4) 0.0005(3) 0.0022(3) -0.0009(3) P2 0.0216(4) 0.0197(4) 0.0189(4) 0.0024(3) 0.0038(3) 0.0034(3) Cl1 0.0291(4) 0.0215(3) 0.0322(4) -0.0066(3) 0.0003(3) -0.0040(3) N1 0.0232(12) 0.0182(11) 0.0135(12) -0.0018(9) -0.0014(10) 0.0041(9) N3 0.0209(12) 0.0172(11) 0.0201(12) -0.0029(9) -0.0009(10) 0.0006(9) C2 0.0264(16) 0.0280(15) 0.0148(14) 0.0005(12) 0.0009(12) -0.0016(12) N2 0.0218(13) 0.0239(12) 0.0157(12) -0.0007(10) 0.0031(10) 0.0038(10) C10 0.0319(17) 0.0213(14) 0.0201(15) -0.0026(12) 0.0022(13) 0.0083(12) C8 0.0275(16) 0.0276(15) 0.0213(15) 0.0036(12) 0.0119(13) 0.0043(13) C13 0.0219(15) 0.0231(15) 0.0267(16) -0.0050(12) -0.0044(13) -0.0006(12) C18 0.0196(15) 0.0368(17) 0.0263(16) 0.0047(13) 0.0027(13) 0.0035(13) C11 0.0378(18) 0.0194(14) 0.0220(16) -0.0053(12) 0.0006(14) 0.0087(13) C21 0.0366(19) 0.0324(17) 0.0259(17) 0.0123(14) 0.0099(14) 0.0080(14) C7 0.058(2) 0.0415(19) 0.0249(17) -0.0022(15) 0.0225(17) 0.0095(17) C12 0.0343(17) 0.0238(15) 0.0164(14) -0.0020(12) 0.0000(13) 0.0035(13) C1 0.0317(18) 0.0325(17) 0.0334(18) -0.0020(14) -0.0024(14) -0.0087(14) C15 0.0371(19) 0.0203(15) 0.0332(18) -0.0037(13) 0.0018(15) 0.0059(13) C5 0.0388(19) 0.0219(15) 0.0270(17) 0.0056(13) -0.0009(14) -0.0078(13) C17 0.0252(17) 0.045(2) 0.0361(19) 0.0095(16) 0.0056(14) -0.0040(15) C3 0.0309(18) 0.0419(19) 0.0275(17) 0.0008(15) -0.0002(14) 0.0086(15) C20 0.047(2) 0.056(2) 0.0215(17) 0.0076(16) 0.0065(15) 0.0082(18) C22 0.044(2) 0.048(2) 0.049(2) 0.0163(18) 0.0203(18) -0.0026(17) C6 0.052(2) 0.0367(19) 0.042(2) 0.0058(16) -0.0027(18) -0.0197(17) C16 0.075(3) 0.0340(19) 0.0288(19) -0.0088(15) 0.0062(19) 0.0054(18) C4 0.061(2) 0.0333(18) 0.0307(19) 0.0101(15) 0.0059(17) -0.0129(17) C9 0.0276(18) 0.049(2) 0.055(2) 0.0141(18) 0.0168(17) 0.0079(16) C19 0.0295(19) 0.061(2) 0.053(2) 0.017(2) 0.0075(17) 0.0170(18) C14 0.068(3) 0.0226(17) 0.053(2) -0.0031(16) 0.007(2) 0.0123(17) Cl2 0.0318(4) 0.0456(5) 0.0224(4) -0.0063(3) 0.0063(3) 0.0041(3) _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 N3 1.989(2) . ? Ni1 N1 1.992(2) . ? Ni1 N2 2.070(2) . ? Ni1 Cl1 2.2547(8) . ? P1 N1 1.617(2) . ? P1 C8 1.818(3) . ? P1 C2 1.822(3) . ? P1 C5 1.830(3) . ? P2 N3 1.617(2) . ? P2 C15 1.819(3) . ? P2 C18 1.822(3) . ? P2 C21 1.839(3) . ? N1 C10 1.481(4) . ? N3 C13 1.486(3) . ? C2 C3 1.532(4) . ? C2 C1 1.533(4) . ? N2 C12 1.472(4) . ? N2 C11 1.483(4) . ? C10 C11 1.510(4) . ? C8 C9 1.532(5) . ? C8 C7 1.539(4) . ? C13 C12 1.513(4) . ? C18 C19 1.528(4) . ? C18 C17 1.536(4) . ? C21 C22 1.525(5) . ? C21 C20 1.531(5) . ? C15 C16 1.529(5) . ? C15 C14 1.537(4) . ? C5 C6 1.532(4) . ? C5 C4 1.540(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 N3 Ni1 N1 125.45(10) . . ? N3 Ni1 N2 85.95(9) . . ? N1 Ni1 N2 84.43(9) . . ? N3 Ni1 Cl1 109.71(7) . . ? N1 Ni1 Cl1 109.94(7) . . ? N2 Ni1 Cl1 142.79(7) . . ? N1 P1 C8 106.14(13) . . ? N1 P1 C2 114.56(13) . . ? C8 P1 C2 107.59(14) . . ? N1 P1 C5 110.97(13) . . ? C8 P1 C5 112.53(15) . . ? C2 P1 C5 105.16(14) . . ? N3 P2 C15 108.17(13) . . ? N3 P2 C18 109.94(13) . . ? C15 P2 C18 113.73(16) . . ? N3 P2 C21 114.32(14) . . ? C15 P2 C21 105.06(15) . . ? C18 P2 C21 105.66(15) . . ? C10 N1 P1 117.52(18) . . ? C10 N1 Ni1 109.46(17) . . ? P1 N1 Ni1 132.40(13) . . ? C13 N3 P2 115.97(18) . . ? C13 N3 Ni1 104.96(16) . . ? P2 N3 Ni1 137.81(13) . . ? C3 C2 C1 109.4(3) . . ? C3 C2 P1 112.7(2) . . ? C1 C2 P1 110.9(2) . . ? C12 N2 C11 111.8(2) . . ? C12 N2 Ni1 106.92(17) . . ? C11 N2 Ni1 107.68(17) . . ? N1 C10 C11 107.8(2) . . ? C9 C8 C7 110.7(3) . . ? C9 C8 P1 111.0(2) . . ? C7 C8 P1 114.6(2) . . ? N3 C13 C12 108.4(2) . . ? C19 C18 C17 111.9(3) . . ? C19 C18 P2 115.0(2) . . ? C17 C18 P2 112.3(2) . . ? N2 C11 C10 108.7(2) . . ? C22 C21 C20 111.2(3) . . ? C22 C21 P2 110.3(2) . . ? C20 C21 P2 114.0(2) . . ? N2 C12 C13 108.3(2) . . ? C16 C15 C14 110.6(3) . . ? C16 C15 P2 112.1(2) . . ? C14 C15 P2 114.9(2) . . ? C6 C5 C4 110.6(3) . . ? C6 C5 P1 114.4(2) . . ? C4 C5 P1 114.0(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.369 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.064 # Attachment '- 13a-t1.cif' data_t1 _database_code_depnum_ccdc_archive 'CCDC 809534' #TrackingRef '- 13a-t1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 Cl F6 N3 Ni P3' _chemical_formula_weight 861.80 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmn2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 21.7288(9) _cell_length_b 7.6413(3) _cell_length_c 11.6265(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1930.42(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6626 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54670 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 33.56 _reflns_number_total 7697 _reflns_number_gt 6879 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0664P)^2^+0.5035P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(10) _refine_ls_number_reflns 7697 _refine_ls_number_parameters 253 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.38746(4) 0.37948(3) 0.02000(8) Uani 1 2 d S . . P2 P 0.5000 0.42139(14) 0.45927(10) 0.0408(2) Uani 1 2 d S . . P1 P 0.140166(19) 0.27238(5) 0.41221(5) 0.01731(8) Uani 1 1 d . . . F1 F 0.5000 0.2123(6) 0.4502(5) 0.1035(14) Uani 1 2 d S . . F2 F 0.44909(11) 0.4213(5) 0.3617(3) 0.0995(10) Uani 1 1 d . . . F3 F 0.44939(12) 0.4134(5) 0.5557(2) 0.1071(12) Uani 1 1 d . . . F4 F 0.5000 0.6217(5) 0.4628(5) 0.144(3) Uani 1 2 d S . . N1 N 0.0000 0.6179(3) 0.3131(3) 0.0314(6) Uani 1 2 d S . . N2 N 0.08797(6) 0.41612(17) 0.38607(16) 0.0206(3) Uani 1 1 d . . . Cl1 Cl 0.0000 0.10770(7) 0.40931(6) 0.02197(12) Uani 1 2 d S . . C2 C 0.21236(8) 0.3878(2) 0.43375(16) 0.0202(3) Uani 1 1 d . . . C5 C 0.12410(8) 0.1572(3) 0.54380(16) 0.0205(3) Uani 1 1 d . . . C7 C 0.05778(10) 0.7075(3) 0.3413(2) 0.0337(5) Uani 1 1 d . . . H7A H 0.0577 0.7461 0.4208 0.040 Uiso 1 1 calc R . . H7B H 0.0637 0.8084 0.2919 0.040 Uiso 1 1 calc R . . C8 C 0.11387(11) 0.1217(3) 0.20312(18) 0.0267(4) Uani 1 1 d . . . H8A H 0.0809 0.1994 0.2016 0.032 Uiso 1 1 calc R . . C9 C 0.15428(9) 0.1197(2) 0.29683(17) 0.0221(3) Uani 1 1 d . . . C10 C 0.10719(9) 0.5754(3) 0.3218(2) 0.0307(4) Uani 1 1 d . . . H10A H 0.1113 0.5499 0.2404 0.037 Uiso 1 1 calc R . . H10B H 0.1463 0.6183 0.3503 0.037 Uiso 1 1 calc R . . C10B C 0.12351(13) 0.0052(3) 0.1112(2) 0.0388(5) Uani 1 1 d . . . H10C H 0.0966 0.0051 0.0490 0.047 Uiso 1 1 calc R . . C11 C 0.14073(10) -0.0174(3) 0.55911(19) 0.0279(4) Uani 1 1 d . . . H11A H 0.1602 -0.0780 0.5000 0.033 Uiso 1 1 calc R . . C12 C 0.12825(14) -0.1006(3) 0.6625(2) 0.0411(6) Uani 1 1 d . . . H12A H 0.1391 -0.2174 0.6724 0.049 Uiso 1 1 calc R . . C13 C 0.31711(10) 0.5967(3) 0.4595(2) 0.0340(5) Uani 1 1 d . . . H13A H 0.3521 0.6654 0.4687 0.041 Uiso 1 1 calc R . . C14 C 0.25988(11) 0.3845(3) 0.35335(19) 0.0342(5) Uani 1 1 d . . . H14A H 0.2569 0.3112 0.2898 0.041 Uiso 1 1 calc R . . C15 C 0.20422(10) 0.0028(3) 0.2967(2) 0.0306(4) Uani 1 1 d . . . H15A H 0.2314 0.0010 0.3586 0.037 Uiso 1 1 calc R . . C17 C 0.17242(15) -0.1084(3) 0.1129(3) 0.0466(7) Uani 1 1 d . . . H17A H 0.1783 -0.1852 0.0518 0.056 Uiso 1 1 calc R . . C19 C 0.21318(13) -0.1102(3) 0.2045(3) 0.0417(6) Uani 1 1 d . . . H19A H 0.2465 -0.1867 0.2043 0.050 Uiso 1 1 calc R . . C21 C 0.08344(12) 0.1628(4) 0.7369(2) 0.0378(5) Uani 1 1 d . . . H21A H 0.0644 0.2234 0.7965 0.045 Uiso 1 1 calc R . . C22 C 0.09961(14) -0.0102(4) 0.7517(2) 0.0451(6) Uani 1 1 d . . . H22A H 0.0914 -0.0663 0.8210 0.054 Uiso 1 1 calc R . . C23 C 0.31132(10) 0.4883(4) 0.3665(2) 0.0391(5) Uani 1 1 d . . . H23A H 0.3424 0.4845 0.3116 0.047 Uiso 1 1 calc R . . C25 C 0.09548(10) 0.2472(3) 0.63348(18) 0.0281(4) Uani 1 1 d . . . H25A H 0.0845 0.3639 0.6240 0.034 Uiso 1 1 calc R . . C26 C 0.21914(11) 0.4947(4) 0.5282(2) 0.0459(7) Uani 1 1 d . . . H26A H 0.1891 0.4946 0.5853 0.055 Uiso 1 1 calc R . . C27 C 0.27021(14) 0.6025(5) 0.5395(3) 0.0601(11) Uani 1 1 d . . . H27A H 0.2728 0.6793 0.6014 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01275(12) 0.01442(12) 0.03282(17) 0.00358(12) 0.000 0.000 P2 0.0268(4) 0.0472(5) 0.0485(5) 0.0140(4) 0.000 0.000 P1 0.01377(15) 0.01660(15) 0.02154(17) -0.00025(17) -0.00009(14) -0.00049(13) F1 0.110(3) 0.083(3) 0.118(4) 0.015(3) 0.000 0.000 F2 0.0517(12) 0.171(3) 0.0757(18) -0.0079(18) -0.0206(13) 0.0249(15) F3 0.0536(14) 0.204(4) 0.0640(16) 0.0221(18) 0.0224(12) 0.0027(16) F4 0.280(9) 0.048(2) 0.103(4) 0.010(2) 0.000 0.000 N1 0.0184(10) 0.0227(11) 0.0529(17) 0.0092(10) 0.000 0.000 N2 0.0133(5) 0.0161(5) 0.0323(8) 0.0041(6) -0.0011(5) -0.0011(4) Cl1 0.0157(2) 0.0163(2) 0.0339(3) 0.0012(2) 0.000 0.000 C2 0.0148(6) 0.0223(7) 0.0235(9) -0.0007(6) -0.0008(6) -0.0018(5) C5 0.0162(7) 0.0228(7) 0.0225(8) 0.0014(6) -0.0013(6) -0.0023(6) C7 0.0256(9) 0.0176(7) 0.0578(14) 0.0084(8) 0.0008(9) -0.0021(7) C8 0.0288(9) 0.0288(9) 0.0225(8) -0.0018(7) 0.0020(7) -0.0090(7) C9 0.0222(8) 0.0196(7) 0.0244(8) -0.0028(6) 0.0047(6) -0.0045(6) C10 0.0186(8) 0.0228(8) 0.0507(13) 0.0125(8) 0.0012(8) -0.0024(6) C10B 0.0522(14) 0.0418(13) 0.0225(9) -0.0083(9) 0.0056(9) -0.0199(11) C11 0.0290(9) 0.0238(8) 0.0309(9) 0.0050(7) -0.0032(7) 0.0018(7) C12 0.0491(14) 0.0349(12) 0.0392(13) 0.0174(10) -0.0067(11) -0.0038(10) C13 0.0224(9) 0.0395(11) 0.0401(12) -0.0078(9) 0.0003(8) -0.0119(8) C14 0.0287(9) 0.0432(11) 0.0307(11) -0.0110(8) 0.0086(8) -0.0147(8) C15 0.0278(9) 0.0255(9) 0.0383(11) -0.0035(8) 0.0109(8) 0.0005(7) C17 0.0626(18) 0.0346(12) 0.0427(14) -0.0157(10) 0.0254(13) -0.0140(11) C19 0.0443(14) 0.0292(10) 0.0515(15) -0.0085(10) 0.0249(12) -0.0007(9) C21 0.0326(10) 0.0545(14) 0.0264(10) -0.0027(10) 0.0047(8) -0.0097(10) C22 0.0497(15) 0.0582(17) 0.0275(11) 0.0124(11) -0.0010(10) -0.0171(13) C23 0.0256(9) 0.0514(13) 0.0403(12) -0.0108(11) 0.0124(9) -0.0140(9) C25 0.0255(9) 0.0329(10) 0.0258(9) -0.0046(7) 0.0021(7) -0.0030(7) C26 0.0304(11) 0.0624(17) 0.0448(13) -0.0307(12) 0.0166(10) -0.0247(11) C27 0.0430(15) 0.085(2) 0.0519(16) -0.0401(16) 0.0185(12) -0.0400(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.922(2) . ? Ni1 N2 1.9256(13) . ? Ni1 N2 1.9256(13) 4 ? Ni1 Cl1 2.1657(6) . ? P2 F4 1.531(4) . ? P2 F3 1.571(3) . ? P2 F3 1.571(3) 4_655 ? P2 F2 1.584(3) 4_655 ? P2 F2 1.584(3) . ? P2 F1 1.601(5) . ? P1 N2 1.6078(14) . ? P1 C5 1.7993(19) . ? P1 C9 1.8042(19) . ? P1 C2 1.8169(17) . ? N1 C7 1.467(3) 4 ? N1 C7 1.467(3) . ? N2 C10 1.488(2) . ? C2 C26 1.377(3) . ? C2 C14 1.393(3) . ? C5 C11 1.393(3) . ? C5 C25 1.395(3) . ? C7 C10 1.491(3) . ? C8 C9 1.399(3) . ? C8 C10B 1.407(3) . ? C9 C15 1.405(3) . ? C10B C17 1.372(4) . ? C11 C12 1.387(3) . ? C12 C22 1.393(4) . ? C13 C23 1.368(3) . ? C13 C27 1.380(4) . ? C14 C23 1.379(3) . ? C15 C19 1.390(3) . ? C17 C19 1.385(5) . ? C21 C22 1.379(4) . ? C21 C25 1.389(3) . ? C26 C27 1.388(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 84.94(4) . . ? N1 Ni1 N2 84.94(4) . 4 ? N2 Ni1 N2 166.16(8) . 4 ? N1 Ni1 Cl1 165.54(10) . . ? N2 Ni1 Cl1 96.08(4) . . ? N2 Ni1 Cl1 96.08(4) 4 . ? F4 P2 F3 91.1(2) . . ? F4 P2 F3 91.1(2) . 4_655 ? F3 P2 F3 88.8(2) . 4_655 ? F4 P2 F2 91.1(2) . 4_655 ? F3 P2 F2 177.8(2) . 4_655 ? F3 P2 F2 91.26(16) 4_655 4_655 ? F4 P2 F2 91.1(2) . . ? F3 P2 F2 91.26(16) . . ? F3 P2 F2 177.8(2) 4_655 . ? F2 P2 F2 88.6(2) 4_655 . ? F4 P2 F1 177.7(3) . . ? F3 P2 F1 90.5(2) . . ? F3 P2 F1 90.5(2) 4_655 . ? F2 P2 F1 87.28(19) 4_655 . ? F2 P2 F1 87.28(19) . . ? N2 P1 C5 110.99(9) . . ? N2 P1 C9 114.90(9) . . ? C5 P1 C9 110.41(9) . . ? N2 P1 C2 107.67(7) . . ? C5 P1 C2 106.72(8) . . ? C9 P1 C2 105.64(8) . . ? C7 N1 C7 117.7(3) 4 . ? C7 N1 Ni1 109.74(14) 4 . ? C7 N1 Ni1 109.74(14) . . ? C10 N2 P1 117.12(12) . . ? C10 N2 Ni1 110.58(11) . . ? P1 N2 Ni1 129.06(8) . . ? C26 C2 C14 117.82(17) . . ? C26 C2 P1 119.36(14) . . ? C14 C2 P1 122.60(14) . . ? C11 C5 C25 119.47(19) . . ? C11 C5 P1 121.79(15) . . ? C25 C5 P1 118.73(15) . . ? N1 C7 C10 105.45(18) . . ? C9 C8 C10B 119.4(2) . . ? C8 C9 C15 119.40(19) . . ? C8 C9 P1 117.73(15) . . ? C15 C9 P1 122.87(17) . . ? N2 C10 C7 105.97(16) . . ? C17 C10B C8 120.3(3) . . ? C12 C11 C5 119.9(2) . . ? C11 C12 C22 120.3(2) . . ? C23 C13 C27 119.0(2) . . ? C23 C14 C2 121.1(2) . . ? C19 C15 C9 120.2(2) . . ? C10B C17 C19 120.8(2) . . ? C17 C19 C15 119.8(2) . . ? C22 C21 C25 120.3(2) . . ? C21 C22 C12 119.8(2) . . ? C13 C23 C14 120.7(2) . . ? C21 C25 C5 120.1(2) . . ? C2 C26 C27 120.9(2) . . ? C13 C27 C26 120.5(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.249 _refine_diff_density_min -0.696 _refine_diff_density_rms 0.083 # Attachment '- 13b-rc015_0m.cif' data_rc015_0m _database_code_depnum_ccdc_archive 'CCDC 809535' #TrackingRef '- 13b-rc015_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 Cl F6 N3 Ni P3' _chemical_formula_weight 863.82 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0118(7) _cell_length_b 13.1874(10) _cell_length_c 16.4704(12) _cell_angle_alpha 67.100(4) _cell_angle_beta 89.195(4) _cell_angle_gamma 77.437(4) _cell_volume 1949.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5907 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27269 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.1757 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 29.65 _reflns_number_total 10660 _reflns_number_gt 5163 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0863P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10660 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1763 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 0.91658(6) 0.83782(5) 0.66154(4) 0.02273(18) Uani 1 1 d . . . Cl1 Cl 1.11020(11) 0.82590(10) 0.58823(7) 0.0226(3) Uani 1 1 d . . . P1 P 0.75376(13) 0.65514(11) 0.64943(8) 0.0226(3) Uani 1 1 d . . . P2 P 1.04815(13) 0.84437(11) 0.83165(8) 0.0223(3) Uani 1 1 d . . . C1 C 1.0786(6) 0.5149(5) 0.8825(4) 0.0376(14) Uani 1 1 d . . . H1A H 1.0214 0.4627 0.9038 0.045 Uiso 1 1 calc R . . N2 N 0.7967(4) 0.9917(3) 0.5875(3) 0.0248(9) Uani 1 1 d . . . C2 C 0.7015(5) 0.6311(4) 0.7601(3) 0.0218(10) Uani 1 1 d . . . C3 C 0.5474(6) 0.6464(5) 0.4437(4) 0.0372(14) Uani 1 1 d . . . H3A H 0.5683 0.6450 0.3876 0.045 Uiso 1 1 calc R . . C4 C 0.8807(6) 1.0261(4) 0.7084(3) 0.0320(12) Uani 1 1 d . . . H4A H 0.9492 1.0668 0.6750 0.038 Uiso 1 1 calc R . . H4B H 0.8539 1.0527 0.7562 0.038 Uiso 1 1 calc R . . C5 C 1.2932(5) 0.5526(4) 0.8332(3) 0.0326(13) Uani 1 1 d . . . H5A H 1.3838 0.5272 0.8197 0.039 Uiso 1 1 calc R . . C6 C 1.0969(6) 0.3500(5) 0.6720(3) 0.0411(15) Uani 1 1 d . . . H6A H 1.1681 0.2866 0.6769 0.049 Uiso 1 1 calc R . . C7 C 1.2472(5) 0.6644(4) 0.8237(3) 0.0257(11) Uani 1 1 d . . . H7A H 1.3061 0.7154 0.8040 0.031 Uiso 1 1 calc R . . C8 C 0.5955(5) 0.7107(5) 0.8605(4) 0.0338(13) Uani 1 1 d . . . H8A H 0.5529 0.7752 0.8718 0.041 Uiso 1 1 calc R . . C9 C 1.4099(5) 1.0175(4) 0.7861(4) 0.0330(13) Uani 1 1 d . . . H9A H 1.4848 1.0534 0.7750 0.040 Uiso 1 1 calc R . . C10 C 1.1896(5) 0.9129(4) 0.8190(3) 0.0231(11) Uani 1 1 d . . . C11 C 0.7369(5) 0.8670(4) 0.5247(3) 0.0315(12) Uani 1 1 d . . . H11A H 0.6606 0.8479 0.5002 0.038 Uiso 1 1 calc R . . H11B H 0.8077 0.8787 0.4815 0.038 Uiso 1 1 calc R . . C12 C 1.1297(6) 0.4497(5) 0.6651(4) 0.0417(15) Uani 1 1 d . . . H12A H 1.2229 0.4547 0.6656 0.050 Uiso 1 1 calc R . . C13 C 0.9620(6) 0.3421(5) 0.6718(4) 0.0383(14) Uani 1 1 d . . . H13A H 0.9399 0.2737 0.6764 0.046 Uiso 1 1 calc R . . C14 C 0.3857(6) 0.6468(5) 0.5525(4) 0.0378(14) Uani 1 1 d . . . H14A H 0.2958 0.6443 0.5710 0.045 Uiso 1 1 calc R . . C15 C 0.9748(5) 0.7686(4) 1.0898(3) 0.0317(13) Uani 1 1 d . . . H15A H 1.0258 0.7333 1.1457 0.038 Uiso 1 1 calc R . . N3 N 0.7965(4) 0.7736(3) 0.6099(3) 0.0253(9) Uani 1 1 d . . . C16 C 1.2387(5) 0.9491(4) 0.7345(3) 0.0314(12) Uani 1 1 d . . . H16A H 1.1970 0.9381 0.6880 0.038 Uiso 1 1 calc R . . C17 C 0.7598(5) 0.8564(5) 1.0041(4) 0.0343(13) Uani 1 1 d . . . H17A H 0.6626 0.8794 1.0014 0.041 Uiso 1 1 calc R . . C18 C 1.0254(5) 0.5421(5) 0.6574(4) 0.0362(13) Uani 1 1 d . . . H18A H 1.0476 0.6108 0.6519 0.043 Uiso 1 1 calc R . . C19 C 0.8585(6) 0.4349(4) 0.6650(3) 0.0312(12) Uani 1 1 d . . . H19A H 0.7654 0.4295 0.6652 0.037 Uiso 1 1 calc R . . C20 C 0.9671(5) 0.8357(4) 0.9315(3) 0.0264(11) Uani 1 1 d . . . C21 C 0.8355(5) 0.8061(4) 1.0853(3) 0.0317(12) Uani 1 1 d . . . H21A H 0.7906 0.7976 1.1380 0.038 Uiso 1 1 calc R . . C22 C 0.7188(5) 0.5229(4) 0.8261(3) 0.0294(12) Uani 1 1 d . . . H22A H 0.7595 0.4580 0.8149 0.035 Uiso 1 1 calc R . . C23 C 1.3479(6) 1.0007(5) 0.7193(4) 0.0379(14) Uani 1 1 d . . . H23A H 1.3810 1.0250 0.6621 0.046 Uiso 1 1 calc R . . N1 N 0.9405(4) 0.9019(3) 0.7469(2) 0.0246(9) Uani 1 1 d . . . C24 C 1.0429(5) 0.7817(4) 1.0134(3) 0.0275(11) Uani 1 1 d . . . H24A H 1.1395 0.7542 1.0169 0.033 Uiso 1 1 calc R . . C25 C 0.6144(5) 0.6040(5) 0.9266(3) 0.0319(13) Uani 1 1 d . . . H25A H 0.5853 0.5948 0.9837 0.038 Uiso 1 1 calc R . . C26 C 1.3616(5) 0.9815(5) 0.8690(4) 0.0350(13) Uani 1 1 d . . . H26A H 1.4045 0.9920 0.9153 0.042 Uiso 1 1 calc R . . C27 C 1.2086(5) 0.4790(5) 0.8618(4) 0.0344(13) Uani 1 1 d . . . H27A H 1.2399 0.4031 0.8673 0.041 Uiso 1 1 calc R . . C28 C 0.7564(5) 1.0491(4) 0.6477(3) 0.0331(13) Uani 1 1 d . . . H28A H 0.6815 1.0201 0.6826 0.040 Uiso 1 1 calc R . . H28B H 0.7232 1.1315 0.6136 0.040 Uiso 1 1 calc R . . C29 C 0.6839(5) 0.9748(4) 0.5411(3) 0.0321(12) Uani 1 1 d . . . H29A H 0.6542 1.0404 0.4842 0.038 Uiso 1 1 calc R . . H29B H 0.6043 0.9672 0.5776 0.038 Uiso 1 1 calc R . . C30 C 1.1155(5) 0.7004(4) 0.8432(3) 0.0229(11) Uani 1 1 d . . . C31 C 0.6470(5) 0.6480(4) 0.4997(3) 0.0311(12) Uani 1 1 d . . . H31A H 0.7374 0.6483 0.4815 0.037 Uiso 1 1 calc R . . C32 C 1.2518(5) 0.9303(4) 0.8858(3) 0.0297(12) Uani 1 1 d . . . H32A H 1.2187 0.9071 0.9430 0.036 Uiso 1 1 calc R . . C33 C 0.4167(6) 0.6468(4) 0.4709(4) 0.0384(14) Uani 1 1 d . . . H33A H 0.3465 0.6470 0.4326 0.046 Uiso 1 1 calc R . . C34 C 0.8897(5) 0.5355(4) 0.6577(3) 0.0237(11) Uani 1 1 d . . . C35 C 0.6391(5) 0.7236(4) 0.7777(3) 0.0317(12) Uani 1 1 d . . . H35A H 0.6258 0.7973 0.7322 0.038 Uiso 1 1 calc R . . C36 C 0.4868(5) 0.6507(4) 0.6079(3) 0.0303(12) Uani 1 1 d . . . H36A H 0.4645 0.6543 0.6631 0.036 Uiso 1 1 calc R . . C37 C 0.8264(5) 0.8734(4) 0.9263(3) 0.0292(12) Uani 1 1 d . . . H37A H 0.7753 0.9106 0.8704 0.035 Uiso 1 1 calc R . . C38 C 0.6744(6) 0.5121(5) 0.9101(3) 0.0367(14) Uani 1 1 d . . . H38A H 0.6867 0.4388 0.9561 0.044 Uiso 1 1 calc R . . C39 C 0.6182(5) 0.6493(4) 0.5829(3) 0.0256(11) Uani 1 1 d . . . C40 C 1.0294(5) 0.6255(4) 0.8729(4) 0.0334(13) Uani 1 1 d . . . H40A H 0.9385 0.6500 0.8864 0.040 Uiso 1 1 calc R . . P3 P 0.57136(14) 0.25305(12) 0.82569(9) 0.0274(3) Uani 1 1 d . . . F2 F 0.4186(3) 0.2604(3) 0.7941(2) 0.0491(9) Uani 1 1 d . . . F6 F 0.5827(4) 0.1269(3) 0.8950(2) 0.0518(9) Uani 1 1 d . . . F3 F 0.6274(3) 0.2063(3) 0.7531(2) 0.0548(10) Uani 1 1 d . . . F5 F 0.5566(4) 0.3803(3) 0.7553(2) 0.0502(9) Uani 1 1 d . . . F1 F 0.5132(4) 0.2999(3) 0.8981(2) 0.0648(11) Uani 1 1 d . . . F4 F 0.7228(4) 0.2492(3) 0.8557(3) 0.0623(11) Uani 1 1 d . . . H1 H 0.862(5) 1.025(4) 0.549(3) 0.034(15) Uiso 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 Ni1 0.0241(3) 0.0207(3) 0.0196(3) -0.0049(3) 0.0016(2) -0.0034(3) Cl1 0.0232(6) 0.0210(6) 0.0210(6) -0.0045(5) 0.0125(4) -0.0075(5) P1 0.0252(7) 0.0240(7) 0.0188(6) -0.0075(5) 0.0035(5) -0.0077(5) P2 0.0230(7) 0.0223(7) 0.0207(6) -0.0074(5) 0.0034(5) -0.0056(5) C1 0.039(3) 0.025(3) 0.049(4) -0.011(3) 0.006(3) -0.014(2) N2 0.026(2) 0.021(2) 0.020(2) -0.0014(17) 0.0021(17) -0.0043(17) C2 0.021(2) 0.023(3) 0.019(2) -0.006(2) -0.0030(18) -0.0039(19) C3 0.042(3) 0.038(3) 0.030(3) -0.016(3) -0.007(2) -0.001(3) C4 0.042(3) 0.022(3) 0.027(3) -0.007(2) 0.001(2) -0.004(2) C5 0.032(3) 0.030(3) 0.028(3) -0.009(2) 0.005(2) 0.002(2) C6 0.049(4) 0.031(3) 0.030(3) -0.006(3) 0.012(3) 0.005(3) C7 0.025(3) 0.021(3) 0.024(3) -0.003(2) 0.004(2) -0.002(2) C8 0.036(3) 0.032(3) 0.039(3) -0.021(3) 0.012(2) -0.006(2) C9 0.028(3) 0.031(3) 0.042(3) -0.015(3) 0.008(2) -0.009(2) C10 0.020(2) 0.022(3) 0.029(3) -0.011(2) 0.006(2) -0.0047(19) C11 0.034(3) 0.032(3) 0.023(3) -0.001(2) -0.005(2) -0.012(2) C12 0.035(3) 0.036(3) 0.049(4) -0.013(3) 0.015(3) -0.005(3) C13 0.056(4) 0.024(3) 0.034(3) -0.013(3) 0.004(3) -0.005(3) C14 0.031(3) 0.031(3) 0.055(4) -0.019(3) 0.004(3) -0.011(2) C15 0.037(3) 0.030(3) 0.023(3) -0.007(2) -0.001(2) -0.003(2) N3 0.028(2) 0.020(2) 0.021(2) -0.0027(17) 0.0030(17) -0.0037(17) C16 0.035(3) 0.027(3) 0.027(3) -0.004(2) -0.002(2) -0.009(2) C17 0.021(3) 0.044(3) 0.037(3) -0.017(3) 0.009(2) -0.005(2) C18 0.033(3) 0.032(3) 0.041(3) -0.012(3) 0.011(2) -0.009(2) C19 0.038(3) 0.029(3) 0.028(3) -0.011(2) 0.004(2) -0.012(2) C20 0.032(3) 0.025(3) 0.024(3) -0.010(2) 0.004(2) -0.008(2) C21 0.037(3) 0.029(3) 0.026(3) -0.009(2) 0.012(2) -0.006(2) C22 0.034(3) 0.025(3) 0.024(3) -0.007(2) 0.004(2) -0.005(2) C23 0.038(3) 0.035(3) 0.034(3) -0.004(3) 0.004(2) -0.014(3) N1 0.031(2) 0.017(2) 0.024(2) -0.0065(17) -0.0025(17) -0.0030(17) C24 0.021(3) 0.030(3) 0.028(3) -0.008(2) 0.002(2) -0.006(2) C25 0.035(3) 0.037(3) 0.021(3) -0.009(2) 0.004(2) -0.008(2) C26 0.029(3) 0.043(3) 0.045(3) -0.028(3) 0.006(2) -0.012(2) C27 0.035(3) 0.024(3) 0.044(3) -0.015(3) 0.001(3) -0.004(2) C28 0.034(3) 0.025(3) 0.034(3) -0.010(2) 0.003(2) 0.002(2) C29 0.035(3) 0.029(3) 0.026(3) -0.003(2) -0.002(2) -0.007(2) C30 0.027(3) 0.022(3) 0.018(2) -0.006(2) -0.0019(19) -0.006(2) C31 0.030(3) 0.038(3) 0.026(3) -0.013(2) 0.005(2) -0.009(2) C32 0.029(3) 0.031(3) 0.033(3) -0.014(2) 0.006(2) -0.011(2) C33 0.039(3) 0.025(3) 0.051(4) -0.016(3) -0.019(3) -0.003(2) C34 0.030(3) 0.025(3) 0.018(2) -0.010(2) 0.004(2) -0.008(2) C35 0.036(3) 0.023(3) 0.029(3) -0.004(2) 0.005(2) -0.005(2) C36 0.035(3) 0.026(3) 0.030(3) -0.011(2) 0.007(2) -0.010(2) C37 0.028(3) 0.029(3) 0.030(3) -0.012(2) 0.004(2) -0.006(2) C38 0.046(3) 0.026(3) 0.025(3) 0.002(2) 0.006(2) -0.007(2) C39 0.027(3) 0.027(3) 0.020(2) -0.004(2) 0.002(2) -0.008(2) C40 0.028(3) 0.027(3) 0.045(3) -0.015(3) 0.001(2) -0.005(2) P3 0.0279(7) 0.0251(7) 0.0290(7) -0.0096(6) 0.0029(6) -0.0082(5) F2 0.0261(17) 0.049(2) 0.064(2) -0.0134(18) 0.0029(16) -0.0101(15) F6 0.071(2) 0.0264(18) 0.045(2) 0.0007(15) -0.0064(18) -0.0138(17) F3 0.052(2) 0.069(3) 0.047(2) -0.034(2) 0.0103(17) -0.0008(18) F5 0.059(2) 0.0338(19) 0.047(2) -0.0001(16) 0.0010(17) -0.0198(16) F1 0.094(3) 0.059(3) 0.046(2) -0.030(2) 0.014(2) -0.008(2) F4 0.042(2) 0.071(3) 0.071(3) -0.022(2) -0.0126(18) -0.0180(19) _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 N1 1.942(4) . ? Ni1 N3 1.980(4) . ? Ni1 N2 2.026(4) . ? Ni1 Cl1 2.2781(12) . ? P1 N3 1.594(4) . ? P1 C39 1.789(5) . ? P1 C34 1.807(5) . ? P1 C2 1.814(5) . ? P2 N1 1.596(4) . ? P2 C20 1.798(5) . ? P2 C30 1.806(5) . ? P2 C10 1.807(5) . ? C1 C27 1.371(7) . ? C1 C40 1.380(7) . ? N2 C28 1.469(6) . ? N2 C29 1.475(6) . ? C2 C35 1.379(7) . ? C2 C22 1.392(6) . ? C3 C31 1.377(7) . ? C3 C33 1.377(8) . ? C4 N1 1.490(6) . ? C4 C28 1.509(7) . ? C5 C27 1.368(8) . ? C5 C7 1.392(7) . ? C6 C13 1.378(8) . ? C6 C12 1.386(8) . ? C7 C30 1.379(6) . ? C8 C25 1.378(7) . ? C8 C35 1.384(7) . ? C9 C26 1.379(7) . ? C9 C23 1.383(8) . ? C10 C32 1.389(7) . ? C10 C16 1.405(7) . ? C11 N3 1.483(6) . ? C11 C29 1.531(7) . ? C12 C18 1.386(7) . ? C13 C19 1.388(7) . ? C14 C33 1.374(8) . ? C14 C36 1.394(7) . ? C15 C21 1.367(7) . ? C15 C24 1.391(7) . ? C16 C23 1.380(7) . ? C17 C21 1.387(7) . ? C17 C37 1.398(7) . ? C18 C34 1.381(7) . ? C19 C34 1.388(7) . ? C20 C37 1.380(7) . ? C20 C24 1.396(6) . ? C22 C38 1.410(7) . ? C25 C38 1.357(7) . ? C26 C32 1.382(7) . ? C30 C40 1.394(7) . ? C31 C39 1.403(7) . ? C36 C39 1.371(7) . ? P3 F4 1.586(4) . ? P3 F6 1.590(3) . ? P3 F3 1.590(3) . ? P3 F2 1.593(3) . ? P3 F1 1.594(4) . ? P3 F5 1.601(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N3 147.31(17) . . ? N1 Ni1 N2 85.92(16) . . ? N3 Ni1 N2 86.89(17) . . ? N1 Ni1 Cl1 109.35(13) . . ? N3 Ni1 Cl1 103.33(12) . . ? N2 Ni1 Cl1 104.67(13) . . ? N3 P1 C39 112.6(2) . . ? N3 P1 C34 114.3(2) . . ? C39 P1 C34 104.1(2) . . ? N3 P1 C2 108.4(2) . . ? C39 P1 C2 109.9(2) . . ? C34 P1 C2 107.4(2) . . ? N1 P2 C20 112.0(2) . . ? N1 P2 C30 106.2(2) . . ? C20 P2 C30 106.3(2) . . ? N1 P2 C10 112.5(2) . . ? C20 P2 C10 111.0(2) . . ? C30 P2 C10 108.4(2) . . ? C27 C1 C40 121.2(5) . . ? C28 N2 C29 116.3(4) . . ? C28 N2 Ni1 106.6(3) . . ? C29 N2 Ni1 108.1(3) . . ? C35 C2 C22 119.5(4) . . ? C35 C2 P1 118.2(4) . . ? C22 C2 P1 122.2(4) . . ? C31 C3 C33 118.3(5) . . ? N1 C4 C28 108.1(4) . . ? C27 C5 C7 120.2(5) . . ? C13 C6 C12 120.5(5) . . ? C30 C7 C5 119.4(5) . . ? C25 C8 C35 119.8(5) . . ? C26 C9 C23 119.1(5) . . ? C32 C10 C16 119.2(5) . . ? C32 C10 P2 125.1(4) . . ? C16 C10 P2 115.8(4) . . ? N3 C11 C29 108.5(4) . . ? C6 C12 C18 119.5(6) . . ? C6 C13 C19 119.5(6) . . ? C33 C14 C36 119.7(5) . . ? C21 C15 C24 120.9(5) . . ? C11 N3 P1 124.1(4) . . ? C11 N3 Ni1 104.6(3) . . ? P1 N3 Ni1 130.9(2) . . ? C23 C16 C10 119.6(5) . . ? C21 C17 C37 120.0(5) . . ? C34 C18 C12 120.9(6) . . ? C34 C19 C13 120.7(5) . . ? C37 C20 C24 120.6(5) . . ? C37 C20 P2 118.5(4) . . ? C24 C20 P2 120.6(4) . . ? C15 C21 C17 120.1(5) . . ? C2 C22 C38 118.4(5) . . ? C16 C23 C9 121.0(5) . . ? C4 N1 P2 121.3(3) . . ? C4 N1 Ni1 110.2(3) . . ? P2 N1 Ni1 125.7(2) . . ? C15 C24 C20 119.0(5) . . ? C38 C25 C8 119.9(5) . . ? C9 C26 C32 121.0(5) . . ? C5 C27 C1 120.0(5) . . ? N2 C28 C4 107.9(4) . . ? N2 C29 C11 107.9(4) . . ? C7 C30 C40 120.4(5) . . ? C7 C30 P2 122.0(4) . . ? C40 C30 P2 117.6(4) . . ? C3 C31 C39 121.6(5) . . ? C26 C32 C10 120.1(5) . . ? C14 C33 C3 121.4(5) . . ? C18 C34 C19 119.0(5) . . ? C18 C34 P1 120.9(4) . . ? C19 C34 P1 120.1(4) . . ? C2 C35 C8 121.0(5) . . ? C39 C36 C14 120.2(5) . . ? C20 C37 C17 119.4(5) . . ? C25 C38 C22 121.4(5) . . ? C36 C39 C31 118.6(5) . . ? C36 C39 P1 123.2(4) . . ? C31 C39 P1 118.1(4) . . ? C1 C40 C30 118.7(5) . . ? F4 P3 F6 91.1(2) . . ? F4 P3 F3 90.8(2) . . ? F6 P3 F3 89.7(2) . . ? F4 P3 F2 178.5(2) . . ? F6 P3 F2 90.43(19) . . ? F3 P3 F2 89.5(2) . . ? F4 P3 F1 90.0(2) . . ? F6 P3 F1 90.2(2) . . ? F3 P3 F1 179.2(2) . . ? F2 P3 F1 89.8(2) . . ? F4 P3 F5 90.2(2) . . ? F6 P3 F5 178.8(2) . . ? F3 P3 F5 90.4(2) . . ? F2 P3 F5 88.34(19) . . ? F1 P3 F5 89.7(2) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 29.65 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.079 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.123 # Attachment '- 18-rc002_0m.cif' data_[N(N=PPh3)2NiCl2] _database_code_depnum_ccdc_archive 'CCDC 809536' #TrackingRef '- 18-rc002_0m.cif' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C59 H50 Cl3 N3 Ni2 P2' _chemical_formula_weight 1086.73 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.823(3) _cell_length_b 8.9261(9) _cell_length_c 23.968(2) _cell_angle_alpha 90.00 _cell_angle_beta 133.969(4) _cell_angle_gamma 90.00 _cell_volume 5207.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9083 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 21713 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.1340 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.59 _reflns_number_total 5929 _reflns_number_gt 2836 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1305P)^2^+1.3647P] 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 fixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5929 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1676 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.2239 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _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 0.05672(3) 0.47369(8) 0.79546(4) 0.0375(3) Uani 1 1 d . . . Cl1 Cl 0.0000 0.6775(2) 0.7500 0.0508(6) Uani 1 2 d S . . Cl2 Cl 0.08993(7) 0.4961(2) 0.74290(10) 0.0555(5) Uani 1 1 d . . . N1 N 0.08114(18) 0.4116(5) 0.8950(2) 0.0318(10) Uani 1 1 d . . . N2 N 0.0000 0.3119(7) 0.7500 0.0336(15) Uani 1 2 d S . . P1 P 0.12589(6) 0.50303(15) 0.97414(8) 0.0303(4) Uani 1 1 d . . . C1 C 0.1902(2) 0.4039(7) 1.0433(3) 0.0351(13) Uani 1 1 d . . . C2 C 0.2358(2) 0.4651(8) 1.1122(4) 0.0455(16) Uani 1 1 d . . . H2A H 0.2339 0.5619 1.1266 0.055 Uiso 1 1 calc R . . C3 C 0.2847(3) 0.3865(9) 1.1610(4) 0.0572(19) Uani 1 1 d . . . H3A H 0.3160 0.4297 1.2091 0.069 Uiso 1 1 calc R . . C4 C 0.2889(3) 0.2478(10) 1.1415(5) 0.065(2) Uani 1 1 d . . . H4A H 0.3229 0.1956 1.1752 0.078 Uiso 1 1 calc R . . C5 C 0.2433(3) 0.1846(9) 1.0724(5) 0.065(2) Uani 1 1 d . . . H5A H 0.2456 0.0875 1.0586 0.078 Uiso 1 1 calc R . . C6 C 0.1939(3) 0.2628(7) 1.0227(4) 0.0466(16) Uani 1 1 d . . . H6A H 0.1626 0.2196 0.9747 0.056 Uiso 1 1 calc R . . C7 C 0.1407(2) 0.6680(6) 0.9491(3) 0.0320(13) Uani 1 1 d . . . C8 C 0.1159(2) 0.8042(6) 0.9370(4) 0.0430(15) Uani 1 1 d . . . H8A H 0.0938 0.8138 0.9479 0.052 Uiso 1 1 calc R . . C9 C 0.1229(3) 0.9247(7) 0.9093(4) 0.0542(18) Uani 1 1 d . . . H9A H 0.1048 1.0164 0.8996 0.065 Uiso 1 1 calc R . . C10 C 0.1558(3) 0.9144(7) 0.8956(4) 0.0498(17) Uani 1 1 d . . . H10F H 0.1615 0.9995 0.8781 0.060 Uiso 1 1 calc R . . C11 C 0.1807(3) 0.7803(7) 0.9072(4) 0.0496(16) Uani 1 1 d . . . H11A H 0.2033 0.7725 0.8973 0.060 Uiso 1 1 calc R . . C12 C 0.1728(3) 0.6580(7) 0.9331(4) 0.0464(16) Uani 1 1 d . . . H12A H 0.1896 0.5653 0.9402 0.056 Uiso 1 1 calc R . . C13 C 0.1005(2) 0.5611(6) 1.0163(3) 0.0307(12) Uani 1 1 d . . . C14 C 0.1326(2) 0.5636(7) 1.0963(3) 0.0423(15) Uani 1 1 d . . . H14A H 0.1695 0.5290 1.1313 0.051 Uiso 1 1 calc R . . C15 C 0.1108(3) 0.6160(8) 1.1241(4) 0.0527(18) Uani 1 1 d . . . H15A H 0.1328 0.6185 1.1784 0.063 Uiso 1 1 calc R . . C16 C 0.0570(3) 0.6650(7) 1.0737(4) 0.0468(16) Uani 1 1 d . . . H16A H 0.0424 0.7009 1.0936 0.056 Uiso 1 1 calc R . . C17 C 0.0246(3) 0.6624(7) 0.9951(4) 0.0442(15) Uani 1 1 d . . . H17A H -0.0123 0.6972 0.9605 0.053 Uiso 1 1 calc R . . C18 C 0.0465(2) 0.6075(7) 0.9664(4) 0.0398(14) Uani 1 1 d . . . H18A H 0.0239 0.6022 0.9120 0.048 Uiso 1 1 calc R . . C19 C 0.0521(2) 0.2844(6) 0.8863(3) 0.0317(13) Uani 1 1 d . . . C20 C 0.0623(2) 0.2097(6) 0.9464(3) 0.0360(13) Uani 1 1 d . . . H20A H 0.0894 0.2471 0.9978 0.043 Uiso 1 1 calc R . . C21 C 0.0330(3) 0.0814(7) 0.9318(4) 0.0421(15) Uani 1 1 d . . . H21A H 0.0398 0.0326 0.9730 0.051 Uiso 1 1 calc R . . C22 C -0.0053(3) 0.0258(7) 0.8586(4) 0.0448(15) Uani 1 1 d . . . H22A H -0.0241 -0.0641 0.8492 0.054 Uiso 1 1 calc R . . C23 C -0.0171(3) 0.0989(6) 0.7973(4) 0.0411(14) Uani 1 1 d . . . H23A H -0.0445 0.0598 0.7463 0.049 Uiso 1 1 calc R . . C24 C 0.0107(2) 0.2287(6) 0.8100(3) 0.0353(13) Uani 1 1 d . . . C101 C -0.3791(3) 0.5785(11) 0.1493(5) 0.075(2) Uani 1 1 d . . . H10G H -0.4124 0.5252 0.1225 0.090 Uiso 1 1 calc R . . C102 C -0.3661(3) 0.6987(9) 0.1956(5) 0.071(2) Uani 1 1 d . . . H10D H -0.3910 0.7291 0.1995 0.085 Uiso 1 1 calc R . . C103 C -0.3185(4) 0.7738(10) 0.2355(5) 0.082(3) Uani 1 1 d . . . H10E H -0.3097 0.8551 0.2681 0.098 Uiso 1 1 calc R . . C104 C -0.2826(4) 0.7321(11) 0.2286(6) 0.088(3) Uani 1 1 d . . . H10A H -0.2492 0.7854 0.2560 0.105 Uiso 1 1 calc R . . C105 C -0.2951(4) 0.6150(13) 0.1825(5) 0.080(3) Uani 1 1 d . . . H10C H -0.2704 0.5868 0.1779 0.096 Uiso 1 1 calc R . . C106 C -0.3439(4) 0.5358(11) 0.1419(5) 0.080(3) Uani 1 1 d . . . H10B H -0.3526 0.4537 0.1097 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0469(5) 0.0367(4) 0.0344(5) 0.0034(3) 0.0303(4) -0.0008(3) Cl1 0.0491(13) 0.0321(12) 0.0558(15) 0.000 0.0307(12) 0.000 Cl2 0.0547(10) 0.0797(13) 0.0502(10) 0.0088(8) 0.0432(9) 0.0050(8) N1 0.045(3) 0.028(2) 0.029(2) 0.0024(19) 0.028(2) 0.002(2) N2 0.048(4) 0.034(4) 0.037(4) 0.000 0.036(4) 0.000 P1 0.0373(8) 0.0321(8) 0.0288(8) 0.0038(6) 0.0256(7) 0.0061(6) C1 0.041(3) 0.044(3) 0.033(3) 0.006(3) 0.030(3) 0.006(3) C2 0.045(4) 0.058(4) 0.036(4) 0.011(3) 0.029(3) 0.008(3) C3 0.048(4) 0.087(6) 0.036(4) 0.011(4) 0.029(4) 0.005(4) C4 0.048(4) 0.088(6) 0.066(5) 0.040(5) 0.042(4) 0.029(4) C5 0.077(6) 0.061(5) 0.083(6) 0.018(4) 0.066(5) 0.029(4) C6 0.044(4) 0.054(4) 0.045(4) 0.007(3) 0.032(3) 0.016(3) C7 0.034(3) 0.031(3) 0.029(3) -0.002(2) 0.021(3) -0.004(2) C8 0.055(4) 0.029(3) 0.070(4) -0.007(3) 0.053(4) -0.004(3) C9 0.064(5) 0.032(3) 0.084(5) 0.002(3) 0.058(4) 0.002(3) C10 0.058(4) 0.044(4) 0.060(4) 0.003(3) 0.046(4) -0.014(3) C11 0.051(4) 0.055(4) 0.058(4) 0.011(3) 0.044(4) 0.009(3) C12 0.058(4) 0.036(4) 0.063(4) 0.009(3) 0.049(4) 0.007(3) C13 0.038(3) 0.027(3) 0.033(3) 0.001(2) 0.027(3) 0.003(2) C14 0.037(3) 0.063(4) 0.028(3) -0.001(3) 0.023(3) 0.005(3) C15 0.066(5) 0.074(5) 0.035(4) -0.006(3) 0.042(4) 0.002(4) C16 0.062(4) 0.043(4) 0.066(5) -0.003(3) 0.056(4) 0.004(3) C17 0.047(4) 0.043(4) 0.061(4) 0.000(3) 0.044(4) 0.005(3) C18 0.039(3) 0.041(4) 0.043(4) -0.001(3) 0.030(3) -0.004(3) C19 0.050(3) 0.022(3) 0.040(3) 0.005(2) 0.037(3) 0.006(2) C20 0.054(4) 0.029(3) 0.038(3) 0.007(2) 0.036(3) 0.010(3) C21 0.067(4) 0.033(3) 0.049(4) 0.013(3) 0.049(4) 0.011(3) C22 0.065(4) 0.031(3) 0.059(4) 0.003(3) 0.051(4) -0.003(3) C23 0.054(4) 0.036(3) 0.045(4) -0.007(3) 0.039(3) -0.010(3) C24 0.053(4) 0.026(3) 0.038(3) 0.004(2) 0.036(3) 0.005(3) C101 0.067(5) 0.104(7) 0.064(5) 0.011(5) 0.049(5) 0.005(5) C102 0.071(6) 0.070(6) 0.087(6) 0.011(5) 0.061(5) 0.013(5) C103 0.081(6) 0.068(6) 0.091(7) 0.014(5) 0.058(6) 0.005(5) C104 0.083(7) 0.076(6) 0.092(7) 0.041(6) 0.056(6) 0.012(5) C105 0.075(6) 0.114(8) 0.080(6) 0.050(6) 0.064(6) 0.032(6) C106 0.084(6) 0.109(7) 0.056(5) 0.018(5) 0.053(5) 0.025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.986(4) . ? Ni1 N2 2.013(5) . ? Ni1 Cl2 2.2029(17) . ? Ni1 Cl1 2.2964(18) . ? Ni1 Ni1 2.8037(15) 2_556 ? Cl1 Ni1 2.2963(18) 2_556 ? N1 C19 1.419(7) . ? N1 P1 1.603(5) . ? N2 C24 1.425(6) 2_556 ? N2 C24 1.425(6) . ? N2 Ni1 2.013(4) 2_556 ? P1 C7 1.788(6) . ? P1 C13 1.799(5) . ? P1 C1 1.805(6) . ? C1 C2 1.367(8) . ? C1 C6 1.389(8) . ? C2 C3 1.383(9) . ? C3 C4 1.365(11) . ? C4 C5 1.377(11) . ? C5 C6 1.392(9) . ? C7 C12 1.383(8) . ? C7 C8 1.388(8) . ? C8 C9 1.369(9) . ? C9 C10 1.363(9) . ? C10 C11 1.377(9) . ? C11 C12 1.371(8) . ? C13 C18 1.380(7) . ? C13 C14 1.400(7) . ? C14 C15 1.377(8) . ? C15 C16 1.380(9) . ? C16 C17 1.372(9) . ? C17 C18 1.404(8) . ? C19 C20 1.396(7) . ? C19 C24 1.413(8) . ? C20 C21 1.390(8) . ? C21 C22 1.360(9) . ? C22 C23 1.387(8) . ? C23 C24 1.386(8) . ? C101 C106 1.374(11) . ? C101 C102 1.379(11) . ? C102 C103 1.347(11) . ? C103 C104 1.389(12) . ? C104 C105 1.356(13) . ? C105 C106 1.392(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 83.99(14) . . ? N1 Ni1 Cl2 139.48(14) . . ? N2 Ni1 Cl2 115.35(7) . . ? N1 Ni1 Cl1 107.74(13) . . ? N2 Ni1 Cl1 98.23(13) . . ? Cl2 Ni1 Cl1 104.27(6) . . ? N1 Ni1 Ni1 97.88(13) . 2_556 ? N2 Ni1 Ni1 45.86(12) . 2_556 ? Cl2 Ni1 Ni1 121.43(6) . 2_556 ? Cl1 Ni1 Ni1 52.38(4) . 2_556 ? Ni1 Cl1 Ni1 75.25(7) 2_556 . ? C19 N1 P1 124.7(4) . . ? C19 N1 Ni1 112.3(3) . . ? P1 N1 Ni1 122.9(3) . . ? C24 N2 C24 117.2(6) 2_556 . ? C24 N2 Ni1 110.4(3) 2_556 2_556 ? C24 N2 Ni1 113.5(2) . 2_556 ? C24 N2 Ni1 113.5(2) 2_556 . ? C24 N2 Ni1 110.4(3) . . ? Ni1 N2 Ni1 88.3(2) 2_556 . ? N1 P1 C7 106.1(2) . . ? N1 P1 C13 112.7(2) . . ? C7 P1 C13 107.8(3) . . ? N1 P1 C1 112.5(3) . . ? C7 P1 C1 105.8(3) . . ? C13 P1 C1 111.6(2) . . ? C2 C1 C6 119.2(6) . . ? C2 C1 P1 122.9(5) . . ? C6 C1 P1 117.8(5) . . ? C1 C2 C3 120.2(7) . . ? C4 C3 C2 121.2(7) . . ? C3 C4 C5 119.2(6) . . ? C4 C5 C6 120.1(7) . . ? C1 C6 C5 120.1(6) . . ? C12 C7 C8 118.4(5) . . ? C12 C7 P1 119.7(4) . . ? C8 C7 P1 121.5(4) . . ? C9 C8 C7 120.4(6) . . ? C10 C9 C8 120.6(6) . . ? C9 C10 C11 119.8(6) . . ? C12 C11 C10 120.0(6) . . ? C11 C12 C7 120.7(6) . . ? C18 C13 C14 119.0(5) . . ? C18 C13 P1 117.4(4) . . ? C14 C13 P1 123.6(4) . . ? C15 C14 C13 120.0(5) . . ? C14 C15 C16 120.5(6) . . ? C17 C16 C15 120.6(6) . . ? C16 C17 C18 119.2(6) . . ? C13 C18 C17 120.7(6) . . ? C20 C19 C24 118.6(5) . . ? C20 C19 N1 125.6(5) . . ? C24 C19 N1 115.8(5) . . ? C21 C20 C19 120.8(6) . . ? C22 C21 C20 119.9(5) . . ? C21 C22 C23 120.7(6) . . ? C24 C23 C22 120.5(6) . . ? C23 C24 C19 119.4(5) . . ? C23 C24 N2 123.8(5) . . ? C19 C24 N2 116.8(5) . . ? C106 C101 C102 120.0(9) . . ? C103 C102 C101 121.0(8) . . ? C102 C103 C104 119.7(9) . . ? C105 C104 C103 119.9(9) . . ? C104 C105 C106 120.7(9) . . ? C101 C106 C105 118.7(9) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.871 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.093