# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2c-rac _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H32 Fe N2 P S, B F4' _chemical_formula_sum 'C33 H32 B F4 Fe N2 P S' _chemical_formula_weight 662.30 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8546(5) _cell_length_b 7.6314(4) _cell_length_c 36.279(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.896(5) _cell_angle_gamma 90.00 _cell_volume 2989.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9600 _cell_measurement_theta_min 2.7839 _cell_measurement_theta_max 28.5841 _exptl_crystal_description box _exptl_crystal_colour orange _exptl_crystal_size_max 0.540 _exptl_crystal_size_mid 0.399 _exptl_crystal_size_min 0.182 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_T_min 0.84287 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. CrysAlisPro (Agilent Technologies, 2010) ; _exptl_special_details ? _diffrn_ambient_temperature 180(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 'Xcalibur, Sapphire1, long nozzle' _diffrn_detector_area_resol_mean 8.2632 _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27251 _diffrn_reflns_av_R_equivalents 0.0791 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5262 _reflns_number_gt 4694 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2012)' _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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. The BF4 anions appears to be disordered by rotation around one the B-F bond. The disordrerd model was refined using the tools available in SHELXL-97: the PART instruction to split the disordered model and restraining the B-F distances to their average values with the SADI instruction. SADI B1 F1 B1 F2 B1 F3 B1 F4 B1 F2A B1 F3A B1 F4A B1 7 0.079080 0.171794 0.423100 11.00000 0.03928 0.04603 = 0.04102 -0.00256 -0.00499 0.00889 F1 8 0.135557 0.015266 0.433209 11.00000 0.05200 0.05792 = 0.07142 0.00401 -0.01593 0.02106 PART 1 F2 8 0.004147 0.152957 0.390920 10.68000 0.09496 0.05449 = 0.08081 -0.00571 -0.05214 0.01129 F3 8 0.165950 0.286662 0.415777 10.68000 0.06030 0.09966 = 0.19027 0.06728 -0.05150 -0.04169 F4 8 0.016801 0.222475 0.450901 10.68000 0.14534 0.14764 = 0.08859 0.04191 0.07022 0.08687 PART 2 F2A 8 -0.039872 0.157406 0.409385 10.32000 0.03553 0.04672 = 0.18666 -0.00275 -0.05117 0.01317 F3A 8 0.152131 0.261750 0.402406 10.32000 0.19546 0.09871 = 0.13655 0.03726 0.13863 0.05962 F4A 8 0.076449 0.289568 0.451145 10.32000 0.07432 0.05203 = 0.05280 -0.00994 -0.01493 0.03512 ; _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^)+(0.0124P)^2^+18.7798P] 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 5262 _refine_ls_number_parameters 418 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.1766 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.235 _refine_ls_restrained_S_all 1.236 _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 Fe1 Fe 0.28052(7) 0.83369(12) 0.32169(2) 0.0276(2) Uani 1 1 d . . . P1 P 0.59285(13) 0.8780(2) 0.32770(4) 0.0252(3) Uani 1 1 d . . . S1 S 0.60478(14) 1.1278(2) 0.33934(4) 0.0322(4) Uani 1 1 d . . . N1 N 0.4991(4) 0.9037(6) 0.42965(12) 0.0277(10) Uani 1 1 d . . . N2 N 0.6770(4) 0.8759(7) 0.46308(13) 0.0311(11) Uani 1 1 d . . . C1 C 0.4559(5) 0.7716(7) 0.33941(14) 0.0248(12) Uani 1 1 d . . . C2 C 0.3858(5) 0.8059(8) 0.37055(14) 0.0263(12) Uani 1 1 d . . . C3 C 0.2880(5) 0.6852(9) 0.36865(16) 0.0344(14) Uani 1 1 d . . . H3 H 0.2274 0.6771 0.3857 0.041 Uiso 1 1 calc R . . C4 C 0.2946(5) 0.5788(8) 0.33756(17) 0.0351(14) Uani 1 1 d . . . H4 H 0.2382 0.4875 0.3299 0.042 Uiso 1 1 calc R . . C5 C 0.3973(5) 0.6275(8) 0.31942(16) 0.0309(13) Uani 1 1 d . . . H5 H 0.4232 0.5746 0.2978 0.037 Uiso 1 1 calc R . . C6 C 0.1083(6) 0.9352(11) 0.3128(2) 0.0501(19) Uani 1 1 d . . . H6 H 0.0403 0.9034 0.3259 0.060 Uiso 1 1 calc R . . C7 C 0.1942(7) 1.0703(10) 0.32261(19) 0.0492(19) Uani 1 1 d . . . H7 H 0.1943 1.1468 0.3433 0.059 Uiso 1 1 calc R . . C8 C 0.2787(6) 1.0703(9) 0.29632(18) 0.0397(15) Uani 1 1 d . . . H8 H 0.3477 1.1469 0.2962 0.048 Uiso 1 1 calc R . . C9 C 0.2466(6) 0.9400(10) 0.27000(17) 0.0435(17) Uani 1 1 d . . . H9 H 0.2891 0.9135 0.2491 0.052 Uiso 1 1 calc R . . C10 C 0.1406(6) 0.8557(11) 0.28008(18) 0.0483(18) Uani 1 1 d . . . H10 H 0.0981 0.7616 0.2672 0.058 Uiso 1 1 calc R . . C21 C 0.4068(5) 0.9511(8) 0.39837(14) 0.0281(12) Uani 1 1 d . . . H21A H 0.4356 1.0567 0.3859 0.034 Uiso 1 1 calc R . . H21B H 0.3273 0.9802 0.4081 0.034 Uiso 1 1 calc R . . C22 C 0.6199(6) 0.9339(8) 0.43105(15) 0.0316(13) Uani 1 1 d . . . H22 H 0.6599 0.9888 0.4120 0.038 Uiso 1 1 calc R . . C23 C 0.4747(5) 0.8252(8) 0.46279(14) 0.0294(13) Uani 1 1 d . . . C24 C 0.5879(5) 0.8063(8) 0.48398(15) 0.0288(13) Uani 1 1 d . . . C25 C 0.5953(6) 0.7366(8) 0.51924(15) 0.0314(13) Uani 1 1 d . . . H25 H 0.6729 0.7258 0.5338 0.038 Uiso 1 1 calc R . . C26 C 0.4884(6) 0.6834(8) 0.53279(16) 0.0354(14) Uani 1 1 d . . . C27 C 0.3742(6) 0.6992(8) 0.51091(16) 0.0341(14) Uani 1 1 d . . . C28 C 0.3659(5) 0.7692(8) 0.47582(15) 0.0301(13) Uani 1 1 d . . . H28 H 0.2886 0.7787 0.4611 0.036 Uiso 1 1 calc R . . C111 C 0.5990(5) 0.8360(8) 0.27868(14) 0.0283(12) Uani 1 1 d . . . C112 C 0.6338(5) 0.6739(9) 0.26600(16) 0.0345(14) Uani 1 1 d . . . H112 H 0.6567 0.5828 0.2832 0.041 Uiso 1 1 calc R . . C113 C 0.6353(6) 0.6441(9) 0.22829(17) 0.0402(15) Uani 1 1 d . . . H113 H 0.6597 0.5330 0.2197 0.048 Uiso 1 1 calc R . . C114 C 0.6016(6) 0.7751(10) 0.20347(17) 0.0394(16) Uani 1 1 d . . . H114 H 0.6011 0.7538 0.1777 0.047 Uiso 1 1 calc R . . C115 C 0.5685(6) 0.9370(10) 0.21574(17) 0.0430(16) Uani 1 1 d . . . H115 H 0.5454 1.0279 0.1985 0.052 Uiso 1 1 calc R . . C116 C 0.5691(6) 0.9671(9) 0.25353(16) 0.0357(14) Uani 1 1 d . . . H116 H 0.5485 1.0800 0.2621 0.043 Uiso 1 1 calc R . . C121 C 0.7181(5) 0.7564(8) 0.35236(14) 0.0258(12) Uani 1 1 d . . . C122 C 0.8278(5) 0.8422(8) 0.36484(16) 0.0316(13) Uani 1 1 d . . . H122 H 0.8370 0.9637 0.3601 0.038 Uiso 1 1 calc R . . C123 C 0.9237(6) 0.7492(9) 0.38423(17) 0.0364(14) Uani 1 1 d . . . H123 H 0.9989 0.8068 0.3928 0.044 Uiso 1 1 calc R . . C124 C 0.9094(6) 0.5729(9) 0.39101(17) 0.0380(15) Uani 1 1 d . . . H124 H 0.9748 0.5093 0.4043 0.046 Uiso 1 1 calc R . . C125 C 0.8022(6) 0.4893(9) 0.37878(16) 0.0364(14) Uani 1 1 d . . . H125 H 0.7942 0.3675 0.3834 0.044 Uiso 1 1 calc R . . C126 C 0.7051(6) 0.5785(8) 0.35987(15) 0.0318(13) Uani 1 1 d . . . H126 H 0.6300 0.5194 0.3520 0.038 Uiso 1 1 calc R . . C221 C 0.8099(5) 0.8894(9) 0.47434(18) 0.0418(16) Uani 1 1 d . . . H22A H 0.8459 0.7716 0.4769 0.063 Uiso 1 1 calc R . . H22B H 0.8234 0.9506 0.4982 0.063 Uiso 1 1 calc R . . H22C H 0.8497 0.9549 0.4556 0.063 Uiso 1 1 calc R . . C261 C 0.4945(7) 0.6086(9) 0.57156(16) 0.0462(17) Uani 1 1 d . . . H26A H 0.5810 0.6032 0.5823 0.069 Uiso 1 1 calc R . . H26B H 0.4590 0.4904 0.5705 0.069 Uiso 1 1 calc R . . H26C H 0.4473 0.6837 0.5869 0.069 Uiso 1 1 calc R . . C271 C 0.2572(6) 0.6378(10) 0.52580(19) 0.0471(17) Uani 1 1 d . . . H27A H 0.1869 0.6545 0.5069 0.071 Uiso 1 1 calc R . . H27B H 0.2436 0.7057 0.5480 0.071 Uiso 1 1 calc R . . H27C H 0.2648 0.5133 0.5322 0.071 Uiso 1 1 calc R . . B1 B 0.0791(6) 0.1718(10) 0.42309(18) 0.0434(18) Uani 1 1 d D . . F1 F 0.1356(4) 0.0154(6) 0.43322(12) 0.0618(12) Uani 1 1 d D A . F2 F 0.0044(10) 0.1528(19) 0.3910(3) 0.081(4) Uani 0.68 1 d PD A 1 F3 F 0.1662(10) 0.2858(18) 0.4157(4) 0.121(7) Uani 0.68 1 d PD A 1 F4 F 0.0165(13) 0.223(2) 0.4509(3) 0.121(6) Uani 0.68 1 d PD A 1 F2A F -0.0400(14) 0.158(4) 0.4094(9) 0.096(11) Uani 0.32 1 d PD A 2 F3A F 0.151(3) 0.263(3) 0.4024(9) 0.138(18) Uani 0.32 1 d PD A 2 F4A F 0.0774(19) 0.288(2) 0.4512(5) 0.059(6) Uani 0.32 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0247(4) 0.0318(5) 0.0254(4) 0.0012(3) -0.0014(3) 0.0011(4) P1 0.0245(7) 0.0271(8) 0.0236(7) -0.0008(6) 0.0001(5) 0.0002(6) S1 0.0386(8) 0.0241(8) 0.0334(8) -0.0010(6) 0.0012(6) -0.0017(6) N1 0.032(3) 0.029(3) 0.022(2) -0.0017(19) 0.0002(19) 0.004(2) N2 0.031(3) 0.031(3) 0.030(2) -0.005(2) -0.003(2) 0.004(2) C1 0.025(3) 0.025(3) 0.024(3) 0.001(2) 0.001(2) -0.001(2) C2 0.028(3) 0.029(3) 0.022(3) 0.003(2) -0.001(2) 0.004(2) C3 0.029(3) 0.041(4) 0.034(3) 0.008(3) 0.002(2) 0.002(3) C4 0.025(3) 0.036(3) 0.042(3) -0.007(3) -0.005(2) -0.007(3) C5 0.030(3) 0.024(3) 0.037(3) -0.006(2) -0.001(2) -0.005(2) C6 0.027(3) 0.069(5) 0.054(4) 0.023(4) 0.004(3) 0.018(4) C7 0.060(5) 0.048(4) 0.037(4) 0.002(3) -0.007(3) 0.030(4) C8 0.037(3) 0.034(4) 0.045(4) 0.012(3) -0.009(3) 0.004(3) C9 0.037(4) 0.064(5) 0.028(3) 0.012(3) -0.003(3) 0.004(3) C10 0.037(4) 0.063(5) 0.040(4) 0.007(3) -0.016(3) -0.011(4) C21 0.030(3) 0.029(3) 0.024(3) 0.002(2) -0.001(2) 0.007(2) C22 0.040(3) 0.031(3) 0.023(3) -0.006(2) 0.001(2) 0.001(3) C23 0.037(3) 0.029(3) 0.022(3) -0.004(2) -0.002(2) 0.011(3) C24 0.032(3) 0.029(3) 0.025(3) -0.008(2) 0.000(2) 0.006(3) C25 0.037(3) 0.031(3) 0.025(3) -0.005(2) -0.004(2) 0.007(3) C26 0.052(4) 0.026(3) 0.027(3) -0.002(2) 0.001(3) 0.011(3) C27 0.043(4) 0.029(3) 0.031(3) -0.004(3) 0.005(3) 0.004(3) C28 0.029(3) 0.033(3) 0.028(3) -0.004(2) 0.002(2) 0.009(3) C111 0.022(3) 0.037(3) 0.025(3) -0.001(3) -0.001(2) -0.003(3) C112 0.034(3) 0.037(4) 0.032(3) -0.002(3) -0.002(2) 0.002(3) C113 0.038(3) 0.046(4) 0.037(3) -0.012(3) 0.005(3) 0.002(3) C114 0.030(3) 0.060(5) 0.027(3) -0.008(3) 0.000(2) -0.011(3) C115 0.048(4) 0.051(4) 0.030(3) 0.007(3) 0.004(3) -0.005(3) C116 0.036(3) 0.041(4) 0.030(3) 0.001(3) 0.002(2) 0.000(3) C121 0.024(3) 0.032(3) 0.022(3) -0.001(2) 0.003(2) 0.004(2) C122 0.028(3) 0.031(3) 0.037(3) 0.001(3) 0.003(2) 0.003(3) C123 0.026(3) 0.038(4) 0.044(4) 0.000(3) -0.004(3) 0.005(3) C124 0.033(3) 0.041(4) 0.038(3) 0.007(3) -0.002(3) 0.011(3) C125 0.036(3) 0.036(4) 0.037(3) 0.005(3) 0.006(3) 0.002(3) C126 0.038(3) 0.030(3) 0.027(3) 0.003(2) 0.002(2) 0.000(3) C221 0.027(3) 0.050(4) 0.046(4) -0.005(3) -0.006(3) -0.002(3) C261 0.073(5) 0.037(4) 0.028(3) 0.002(3) 0.005(3) 0.011(4) C271 0.055(4) 0.046(4) 0.043(4) 0.005(3) 0.013(3) 0.004(3) B1 0.039(4) 0.049(5) 0.041(4) -0.003(4) -0.004(3) 0.010(4) F1 0.052(3) 0.058(3) 0.071(3) 0.004(2) -0.016(2) 0.021(2) F2 0.095(8) 0.054(5) 0.081(6) -0.007(5) -0.053(6) 0.014(7) F3 0.059(7) 0.098(9) 0.192(15) 0.070(9) -0.054(9) -0.045(7) F4 0.137(13) 0.150(14) 0.086(9) 0.040(8) 0.065(10) 0.084(10) F2A 0.031(9) 0.044(10) 0.20(3) 0.00(2) -0.051(13) 0.013(9) F3A 0.19(4) 0.11(2) 0.14(2) 0.039(17) 0.14(3) 0.07(2) F4A 0.064(12) 0.052(11) 0.057(11) -0.012(9) -0.013(9) 0.035(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 2.002(5) . ? Fe1 C6 2.019(6) . ? Fe1 C2 2.019(5) . ? Fe1 C8 2.026(6) . ? Fe1 C5 2.027(6) . ? Fe1 C4 2.030(7) . ? Fe1 C10 2.035(6) . ? Fe1 C7 2.036(7) . ? Fe1 C3 2.041(6) . ? Fe1 C9 2.042(6) . ? P1 C1 1.783(6) . ? P1 C121 1.806(6) . ? P1 C111 1.815(5) . ? P1 S1 1.954(2) . ? N1 C22 1.328(8) . ? N1 C23 1.393(7) . ? N1 C21 1.479(7) . ? N2 C22 1.335(7) . ? N2 C24 1.394(7) . ? N2 C221 1.462(7) . ? C1 C5 1.430(8) . ? C1 C2 1.449(7) . ? C2 C3 1.402(8) . ? C2 C21 1.500(8) . ? C3 C4 1.398(9) . ? C4 C5 1.402(8) . ? C6 C10 1.408(10) . ? C6 C7 1.412(11) . ? C7 C8 1.389(10) . ? C8 C9 1.398(10) . ? C9 C10 1.399(9) . ? C23 C28 1.384(8) . ? C23 C24 1.388(8) . ? C24 C25 1.380(8) . ? C25 C26 1.368(9) . ? C26 C27 1.407(9) . ? C26 C261 1.513(8) . ? C27 C28 1.375(8) . ? C27 C271 1.505(9) . ? C111 C116 1.370(8) . ? C111 C112 1.386(9) . ? C112 C113 1.389(8) . ? C113 C114 1.370(10) . ? C114 C115 1.374(10) . ? C115 C116 1.389(8) . ? C121 C122 1.393(8) . ? C121 C126 1.395(8) . ? C122 C123 1.390(8) . ? C123 C124 1.379(9) . ? C124 C125 1.361(9) . ? C125 C126 1.376(8) . ? B1 F3 1.332(10) . ? B1 F4 1.332(10) . ? B1 F3A 1.335(14) . ? B1 F2A 1.341(13) . ? B1 F2 1.356(9) . ? B1 F4A 1.356(13) . ? B1 F1 1.374(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 C1 Fe1 C6 167.5(3) . . ? C1 Fe1 C2 42.2(2) . . ? C6 Fe1 C2 127.8(3) . . ? C1 Fe1 C8 108.7(2) . . ? C6 Fe1 C8 67.6(3) . . ? C2 Fe1 C8 118.1(3) . . ? C1 Fe1 C5 41.6(2) . . ? C6 Fe1 C5 149.7(3) . . ? C2 Fe1 C5 69.8(2) . . ? C8 Fe1 C5 130.6(3) . . ? C1 Fe1 C4 68.9(2) . . ? C6 Fe1 C4 117.0(3) . . ? C2 Fe1 C4 68.3(2) . . ? C8 Fe1 C4 168.5(3) . . ? C5 Fe1 C4 40.4(2) . . ? C1 Fe1 C10 150.4(3) . . ? C6 Fe1 C10 40.6(3) . . ? C2 Fe1 C10 166.3(3) . . ? C8 Fe1 C10 67.5(3) . . ? C5 Fe1 C10 117.1(3) . . ? C4 Fe1 C10 108.5(3) . . ? C1 Fe1 C7 128.9(3) . . ? C6 Fe1 C7 40.8(3) . . ? C2 Fe1 C7 107.4(3) . . ? C8 Fe1 C7 40.0(3) . . ? C5 Fe1 C7 168.4(3) . . ? C4 Fe1 C7 150.1(3) . . ? C10 Fe1 C7 68.3(3) . . ? C1 Fe1 C3 69.2(2) . . ? C6 Fe1 C3 107.7(3) . . ? C2 Fe1 C3 40.4(2) . . ? C8 Fe1 C3 150.7(3) . . ? C5 Fe1 C3 68.4(2) . . ? C4 Fe1 C3 40.2(2) . . ? C10 Fe1 C3 128.9(3) . . ? C7 Fe1 C3 117.3(3) . . ? C1 Fe1 C9 117.7(2) . . ? C6 Fe1 C9 67.9(3) . . ? C2 Fe1 C9 151.7(3) . . ? C8 Fe1 C9 40.2(3) . . ? C5 Fe1 C9 109.0(3) . . ? C4 Fe1 C9 130.0(3) . . ? C10 Fe1 C9 40.1(3) . . ? C7 Fe1 C9 67.8(3) . . ? C3 Fe1 C9 167.3(3) . . ? C1 P1 C121 104.6(3) . . ? C1 P1 C111 105.6(3) . . ? C121 P1 C111 107.0(3) . . ? C1 P1 S1 115.5(2) . . ? C121 P1 S1 111.4(2) . . ? C111 P1 S1 112.1(2) . . ? C22 N1 C23 108.4(5) . . ? C22 N1 C21 125.1(5) . . ? C23 N1 C21 126.4(5) . . ? C22 N2 C24 108.3(5) . . ? C22 N2 C221 125.2(5) . . ? C24 N2 C221 126.5(5) . . ? C5 C1 C2 107.0(5) . . ? C5 C1 P1 124.6(4) . . ? C2 C1 P1 128.4(4) . . ? C5 C1 Fe1 70.2(3) . . ? C2 C1 Fe1 69.5(3) . . ? P1 C1 Fe1 127.2(3) . . ? C3 C2 C1 107.4(5) . . ? C3 C2 C21 125.5(5) . . ? C1 C2 C21 127.0(5) . . ? C3 C2 Fe1 70.6(3) . . ? C1 C2 Fe1 68.3(3) . . ? C21 C2 Fe1 123.1(4) . . ? C4 C3 C2 108.7(5) . . ? C4 C3 Fe1 69.5(4) . . ? C2 C3 Fe1 69.0(3) . . ? C3 C4 C5 109.5(5) . . ? C3 C4 Fe1 70.3(4) . . ? C5 C4 Fe1 69.7(4) . . ? C4 C5 C1 107.4(5) . . ? C4 C5 Fe1 69.9(4) . . ? C1 C5 Fe1 68.3(3) . . ? C10 C6 C7 108.2(6) . . ? C10 C6 Fe1 70.3(4) . . ? C7 C6 Fe1 70.3(4) . . ? C8 C7 C6 107.0(6) . . ? C8 C7 Fe1 69.6(4) . . ? C6 C7 Fe1 69.0(4) . . ? C7 C8 C9 109.5(6) . . ? C7 C8 Fe1 70.4(4) . . ? C9 C8 Fe1 70.5(4) . . ? C8 C9 C10 107.6(6) . . ? C8 C9 Fe1 69.3(3) . . ? C10 C9 Fe1 69.7(4) . . ? C9 C10 C6 107.7(7) . . ? C9 C10 Fe1 70.2(3) . . ? C6 C10 Fe1 69.1(4) . . ? N1 C21 C2 112.3(5) . . ? N1 C22 N2 110.1(5) . . ? C28 C23 C24 121.1(5) . . ? C28 C23 N1 132.2(5) . . ? C24 C23 N1 106.7(5) . . ? C25 C24 C23 121.2(6) . . ? C25 C24 N2 132.3(5) . . ? C23 C24 N2 106.4(5) . . ? C26 C25 C24 118.5(5) . . ? C25 C26 C27 120.2(5) . . ? C25 C26 C261 119.3(6) . . ? C27 C26 C261 120.5(6) . . ? C28 C27 C26 121.7(6) . . ? C28 C27 C271 118.4(6) . . ? C26 C27 C271 119.9(6) . . ? C27 C28 C23 117.4(5) . . ? C116 C111 C112 119.0(5) . . ? C116 C111 P1 119.6(5) . . ? C112 C111 P1 121.5(5) . . ? C111 C112 C113 120.3(6) . . ? C114 C113 C112 119.9(6) . . ? C113 C114 C115 120.3(6) . . ? C114 C115 C116 119.5(6) . . ? C111 C116 C115 120.9(6) . . ? C122 C121 C126 119.6(5) . . ? C122 C121 P1 119.6(5) . . ? C126 C121 P1 120.7(5) . . ? C123 C122 C121 119.7(6) . . ? C124 C123 C122 119.7(6) . . ? C125 C124 C123 120.5(6) . . ? C124 C125 C126 121.0(6) . . ? C125 C126 C121 119.4(6) . . ? F3 B1 F4 112.8(12) . . ? F3 B1 F3A 22.6(18) . . ? F4 B1 F3A 130.3(15) . . ? F3 B1 F2A 130.8(16) . . ? F4 B1 F2A 75.9(14) . . ? F3A B1 F2A 116(2) . . ? F3 B1 F2 105.7(10) . . ? F4 B1 F2 112.0(9) . . ? F3A B1 F2 84.7(18) . . ? F2A B1 F2 37.3(13) . . ? F3 B1 F4A 77.8(12) . . ? F4 B1 F4A 35.8(9) . . ? F3A B1 F4A 97.8(16) . . ? F2A B1 F4A 104.1(15) . . ? F2 B1 F4A 131.5(11) . . ? F3 B1 F1 108.4(8) . . ? F4 B1 F1 107.6(8) . . ? F3A B1 F1 109.3(14) . . ? F2A B1 F1 114.7(13) . . ? F2 B1 F1 110.4(8) . . ? F4A B1 F1 114.1(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.776 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 940117' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2d-rac _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 Fe N2 P S, B F4, 0.5(C H2 Cl2), 0.5(C4 H10 O)' _chemical_formula_sum 'C44.50 H48 B Cl F4 Fe N2 O0.50 P S' _chemical_formula_weight 859.99 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/C _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.6211(11) _cell_length_b 9.1000(4) _cell_length_c 34.9740(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.942(2) _cell_angle_gamma 90.00 _cell_volume 8055.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 30.89 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ? _diffrn_ambient_temperature 180(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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42944 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8245 _reflns_number_gt 6886 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT (Bruker, 2011)' _computing_data_reduction SAINT _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^ > 2\s(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^)+(0.0499P)^2^+9.1186P] 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 8245 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.752585(11) 0.06799(3) 0.063180(7) 0.02195(9) Uani 1 1 d . . . P1 P 0.61603(2) 0.07940(5) 0.041452(14) 0.02375(12) Uani 1 1 d . . . S1 S 0.59786(3) -0.10506(6) 0.064774(16) 0.03784(15) Uani 1 1 d . . . N1 N 0.67845(6) 0.18167(17) 0.16393(4) 0.0213(3) Uani 1 1 d . . . N2 N 0.68428(6) 0.33355(17) 0.21292(4) 0.0227(3) Uani 1 1 d . . . C1 C 0.67932(8) 0.15606(19) 0.06054(5) 0.0210(4) Uani 1 1 d . . . C2 C 0.70780(8) 0.1579(2) 0.09981(5) 0.0210(4) Uani 1 1 d . . . C3 C 0.75436(8) 0.2440(2) 0.09961(5) 0.0225(4) Uani 1 1 d . . . H3 H 0.7804 0.2638 0.1214 0.027 Uiso 1 1 calc R . . C4 C 0.75523(8) 0.2949(2) 0.06148(6) 0.0250(4) Uani 1 1 d . . . H4 H 0.7818 0.3552 0.0534 0.030 Uiso 1 1 calc R . . C5 C 0.70992(8) 0.2408(2) 0.03743(5) 0.0231(4) Uani 1 1 d . . . H5 H 0.7011 0.2577 0.0104 0.028 Uiso 1 1 calc R . . C6 C 0.77704(11) -0.1287(3) 0.08723(7) 0.0438(6) Uani 1 1 d . . . H6 H 0.7699 -0.1646 0.1114 0.053 Uiso 1 1 calc R . . C7 C 0.82112(10) -0.0432(3) 0.08143(7) 0.0416(6) Uani 1 1 d . . . H7 H 0.8489 -0.0111 0.1009 0.050 Uiso 1 1 calc R . . C8 C 0.81626(10) -0.0141(3) 0.04121(7) 0.0390(5) Uani 1 1 d . . . H8 H 0.8404 0.0407 0.0289 0.047 Uiso 1 1 calc R . . C9 C 0.76967(10) -0.0801(2) 0.02284(6) 0.0389(6) Uani 1 1 d . . . H9 H 0.7566 -0.0770 -0.0041 0.047 Uiso 1 1 calc R . . C10 C 0.74550(11) -0.1516(2) 0.05100(7) 0.0410(6) Uani 1 1 d . . . H10 H 0.7135 -0.2059 0.0464 0.049 Uiso 1 1 calc R . . C21 C 0.69516(8) 0.0796(2) 0.13519(5) 0.0241(4) Uani 1 1 d . . . H21A H 0.6666 0.0075 0.1272 0.029 Uiso 1 1 calc R . . H21B H 0.7268 0.0247 0.1474 0.029 Uiso 1 1 calc R . . C22 C 0.71124(8) 0.2481(2) 0.19200(5) 0.0215(4) Uani 1 1 d . . . H22 H 0.7485 0.2361 0.1964 0.026 Uiso 1 1 calc R . . C23 C 0.62731(8) 0.2255(2) 0.16678(5) 0.0267(4) Uani 1 1 d . . . C24 C 0.63103(8) 0.3234(2) 0.19759(6) 0.0292(4) Uani 1 1 d . . . C25 C 0.58648(10) 0.3909(3) 0.20783(7) 0.0478(7) Uani 1 1 d . . . H25 H 0.5893 0.4611 0.2282 0.057 Uiso 1 1 calc R . . C26 C 0.53821(11) 0.3523(4) 0.18741(8) 0.0657(10) Uani 1 1 d . . . C27 C 0.53408(10) 0.2476(4) 0.15692(7) 0.0611(9) Uani 1 1 d . . . C28 C 0.57865(9) 0.1846(3) 0.14623(6) 0.0411(6) Uani 1 1 d . . . H28 H 0.5761 0.1157 0.1256 0.049 Uiso 1 1 calc R . . C111 C 0.61605(8) 0.0651(2) -0.01043(5) 0.0264(4) Uani 1 1 d . . . C112 C 0.63415(9) -0.0624(2) -0.02580(6) 0.0319(5) Uani 1 1 d . . . H112 H 0.6460 -0.1424 -0.0092 0.038 Uiso 1 1 calc R . . C113 C 0.63504(10) -0.0734(3) -0.06540(7) 0.0378(5) Uani 1 1 d . . . H113 H 0.6478 -0.1605 -0.0757 0.045 Uiso 1 1 calc R . . C114 C 0.61747(10) 0.0413(3) -0.08968(6) 0.0396(5) Uani 1 1 d . . . H114 H 0.6179 0.0330 -0.1167 0.048 Uiso 1 1 calc R . . C115 C 0.59927(11) 0.1680(3) -0.07481(7) 0.0422(6) Uani 1 1 d . . . H115 H 0.5874 0.2474 -0.0916 0.051 Uiso 1 1 calc R . . C116 C 0.59825(10) 0.1801(2) -0.03527(6) 0.0354(5) Uani 1 1 d . . . H116 H 0.5853 0.2674 -0.0252 0.042 Uiso 1 1 calc R . . C121 C 0.56982(8) 0.2270(2) 0.04580(6) 0.0276(4) Uani 1 1 d . . . C122 C 0.51591(10) 0.1988(3) 0.03729(8) 0.0441(6) Uani 1 1 d . . . H122 H 0.5038 0.1021 0.0306 0.053 Uiso 1 1 calc R . . C123 C 0.48000(11) 0.3106(3) 0.03853(10) 0.0583(8) Uani 1 1 d . . . H123 H 0.4433 0.2909 0.0322 0.070 Uiso 1 1 calc R . . C124 C 0.49690(11) 0.4510(3) 0.04889(10) 0.0589(8) Uani 1 1 d . . . H124 H 0.4719 0.5270 0.0504 0.071 Uiso 1 1 calc R . . C125 C 0.55014(11) 0.4808(3) 0.05707(9) 0.0516(7) Uani 1 1 d . . . H125 H 0.5619 0.5777 0.0639 0.062 Uiso 1 1 calc R . . C126 C 0.58672(9) 0.3692(2) 0.05537(7) 0.0356(5) Uani 1 1 d . . . H126 H 0.6234 0.3903 0.0608 0.043 Uiso 1 1 calc R . . C231 C 0.70717(9) 0.4190(2) 0.24759(5) 0.0272(4) Uani 1 1 d . . . H23A H 0.6783 0.4679 0.2585 0.033 Uiso 1 1 calc R . . H23B H 0.7305 0.4965 0.2398 0.033 Uiso 1 1 calc R . . C232 C 0.73869(8) 0.3241(2) 0.27865(5) 0.0241(4) Uani 1 1 d . . . C233 C 0.71196(8) 0.2357(2) 0.30240(5) 0.0260(4) Uani 1 1 d . . . C234 C 0.74154(9) 0.1512(2) 0.33130(5) 0.0288(4) Uani 1 1 d . . . H234 H 0.7236 0.0893 0.3468 0.035 Uiso 1 1 calc R . . C235 C 0.79616(9) 0.1547(2) 0.33803(6) 0.0287(5) Uani 1 1 d . . . C236 C 0.82170(9) 0.2424(2) 0.31421(6) 0.0282(4) Uani 1 1 d . . . H236 H 0.8592 0.2450 0.3183 0.034 Uiso 1 1 calc R . . C237 C 0.79396(8) 0.3270(2) 0.28440(5) 0.0251(4) Uani 1 1 d . . . C238 C 0.65260(9) 0.2332(3) 0.29890(7) 0.0357(5) Uani 1 1 d . . . H23C H 0.6400 0.3300 0.3056 0.054 Uiso 1 1 calc R . . H23D H 0.6420 0.1592 0.3166 0.054 Uiso 1 1 calc R . . H23E H 0.6372 0.2087 0.2722 0.054 Uiso 1 1 calc R . . C239 C 0.82720(10) 0.0706(2) 0.37114(6) 0.0385(5) Uani 1 1 d . . . H23F H 0.8329 0.1330 0.3943 0.058 Uiso 1 1 calc R . . H23G H 0.8614 0.0418 0.3643 0.058 Uiso 1 1 calc R . . H23H H 0.8075 -0.0175 0.3764 0.058 Uiso 1 1 calc R . . C240 C 0.82536(9) 0.4201(2) 0.26049(6) 0.0347(5) Uani 1 1 d . . . H24A H 0.8198 0.5242 0.2658 0.052 Uiso 1 1 calc R . . H24B H 0.8137 0.4003 0.2330 0.052 Uiso 1 1 calc R . . H24C H 0.8630 0.3964 0.2672 0.052 Uiso 1 1 calc R . . C261 C 0.48847(14) 0.4209(6) 0.19774(11) 0.116(2) Uani 1 1 d . . . H26A H 0.4978 0.4907 0.2190 0.174 Uiso 1 1 calc R . . H26B H 0.4657 0.3439 0.2057 0.174 Uiso 1 1 calc R . . H26C H 0.4696 0.4727 0.1752 0.174 Uiso 1 1 calc R . . C271 C 0.48003(12) 0.2016(6) 0.13643(10) 0.0946(15) Uani 1 1 d . . . H27A H 0.4839 0.1222 0.1182 0.142 Uiso 1 1 calc R . . H27B H 0.4626 0.2858 0.1223 0.142 Uiso 1 1 calc R . . H27C H 0.4586 0.1672 0.1555 0.142 Uiso 1 1 calc R . . B1 B 0.86689(11) 0.1797(3) 0.18391(7) 0.0363(6) Uani 1 1 d . . . F1 F 0.81779(6) 0.1154(2) 0.18382(5) 0.0631(5) Uani 1 1 d . . . F2 F 0.85882(9) 0.32738(19) 0.17658(5) 0.0775(6) Uani 1 1 d . . . F3 F 0.89050(6) 0.1200(2) 0.15501(4) 0.0600(5) Uani 1 1 d . . . F4 F 0.89691(6) 0.15555(19) 0.21968(4) 0.0560(4) 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 Fe1 0.03167(17) 0.01782(14) 0.01660(14) -0.00160(10) 0.00447(11) 0.00257(11) P1 0.0317(3) 0.0192(2) 0.0192(2) -0.00184(18) 0.0005(2) -0.0049(2) S1 0.0542(4) 0.0245(3) 0.0331(3) 0.0035(2) 0.0014(3) -0.0149(2) N1 0.0240(8) 0.0246(8) 0.0153(7) -0.0005(6) 0.0035(6) -0.0007(6) N2 0.0250(9) 0.0259(8) 0.0167(7) -0.0018(6) 0.0019(6) 0.0052(7) C1 0.0284(10) 0.0168(9) 0.0173(8) -0.0021(7) 0.0016(7) -0.0006(7) C2 0.0280(10) 0.0177(9) 0.0168(8) -0.0023(7) 0.0023(7) 0.0026(7) C3 0.0288(10) 0.0195(9) 0.0187(9) -0.0039(7) 0.0023(8) 0.0023(8) C4 0.0299(11) 0.0185(9) 0.0270(10) -0.0008(7) 0.0057(8) -0.0003(8) C5 0.0332(11) 0.0194(9) 0.0162(8) 0.0017(7) 0.0021(8) 0.0017(8) C6 0.0717(18) 0.0282(11) 0.0358(12) 0.0104(9) 0.0220(12) 0.0238(12) C7 0.0455(14) 0.0342(12) 0.0411(13) -0.0097(10) -0.0058(11) 0.0192(11) C8 0.0450(14) 0.0300(11) 0.0465(13) -0.0006(10) 0.0212(11) 0.0105(10) C9 0.0579(16) 0.0318(12) 0.0274(11) -0.0104(9) 0.0076(10) 0.0133(11) C10 0.0510(15) 0.0187(10) 0.0550(15) -0.0069(10) 0.0136(12) 0.0011(10) C21 0.0340(11) 0.0213(9) 0.0174(9) -0.0012(7) 0.0054(8) 0.0012(8) C22 0.0227(10) 0.0244(9) 0.0169(8) 0.0014(7) 0.0018(7) 0.0026(7) C23 0.0253(10) 0.0386(11) 0.0169(9) 0.0011(8) 0.0055(8) -0.0007(9) C24 0.0262(11) 0.0422(12) 0.0185(9) 0.0005(8) 0.0018(8) 0.0076(9) C25 0.0378(14) 0.0786(19) 0.0261(11) -0.0093(12) 0.0024(10) 0.0246(13) C26 0.0314(14) 0.130(3) 0.0344(13) -0.0137(16) 0.0025(11) 0.0273(16) C27 0.0257(13) 0.124(3) 0.0315(13) -0.0085(15) -0.0006(10) 0.0023(15) C28 0.0290(12) 0.0704(17) 0.0235(10) -0.0036(10) 0.0029(9) -0.0066(11) C111 0.0308(11) 0.0255(10) 0.0207(9) -0.0024(7) -0.0024(8) -0.0059(8) C112 0.0379(12) 0.0270(11) 0.0284(10) -0.0056(8) -0.0020(9) -0.0030(9) C113 0.0433(13) 0.0365(12) 0.0331(11) -0.0147(10) 0.0042(10) -0.0021(10) C114 0.0467(14) 0.0501(14) 0.0211(10) -0.0071(9) 0.0025(10) -0.0093(11) C115 0.0528(15) 0.0436(13) 0.0270(11) 0.0056(10) -0.0036(10) 0.0001(11) C116 0.0480(14) 0.0296(11) 0.0267(10) -0.0003(8) 0.0003(10) 0.0028(10) C121 0.0306(11) 0.0289(10) 0.0227(9) -0.0012(8) 0.0021(8) -0.0025(8) C122 0.0330(13) 0.0397(13) 0.0588(16) -0.0070(11) 0.0041(11) -0.0084(10) C123 0.0304(14) 0.0585(18) 0.085(2) -0.0025(16) 0.0064(14) -0.0009(12) C124 0.0422(16) 0.0507(17) 0.082(2) -0.0026(15) 0.0049(15) 0.0171(13) C125 0.0475(16) 0.0315(13) 0.0718(18) -0.0095(12) -0.0039(14) 0.0054(11) C126 0.0315(12) 0.0300(11) 0.0424(12) -0.0066(9) -0.0031(10) -0.0019(9) C231 0.0363(11) 0.0253(10) 0.0184(9) -0.0051(7) -0.0005(8) 0.0053(8) C232 0.0338(11) 0.0216(9) 0.0159(8) -0.0050(7) 0.0007(8) 0.0031(8) C233 0.0313(11) 0.0260(10) 0.0204(9) -0.0056(7) 0.0028(8) -0.0002(8) C234 0.0409(12) 0.0261(10) 0.0195(9) -0.0018(8) 0.0050(9) -0.0016(9) C235 0.0415(13) 0.0206(9) 0.0217(9) -0.0044(7) -0.0022(9) 0.0019(8) C236 0.0299(11) 0.0255(10) 0.0273(10) -0.0056(8) -0.0012(8) 0.0023(8) C237 0.0319(11) 0.0219(9) 0.0213(9) -0.0049(7) 0.0036(8) 0.0014(8) C238 0.0316(12) 0.0413(13) 0.0349(11) -0.0009(10) 0.0077(9) 0.0014(10) C239 0.0510(15) 0.0300(11) 0.0292(11) 0.0018(9) -0.0097(10) 0.0060(10) C240 0.0382(12) 0.0329(11) 0.0336(11) 0.0006(9) 0.0080(10) -0.0010(9) C261 0.0455(19) 0.236(6) 0.062(2) -0.038(3) -0.0044(16) 0.067(3) C271 0.0255(15) 0.197(5) 0.059(2) -0.022(2) 0.0010(14) -0.010(2) B1 0.0330(14) 0.0484(15) 0.0286(12) 0.0061(11) 0.0076(11) 0.0100(11) F1 0.0339(8) 0.0905(13) 0.0654(10) 0.0364(9) 0.0093(7) 0.0049(8) F2 0.1410(19) 0.0467(9) 0.0457(9) 0.0099(7) 0.0177(10) 0.0097(10) F3 0.0410(8) 0.1016(13) 0.0379(8) -0.0144(8) 0.0080(7) 0.0175(8) F4 0.0558(10) 0.0796(11) 0.0297(7) 0.0036(7) -0.0026(7) 0.0140(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Fe1 C2 2.0211(19) . ? Fe1 C1 2.030(2) . ? Fe1 C6 2.035(2) . ? Fe1 C7 2.041(2) . ? Fe1 C5 2.0428(19) . ? Fe1 C3 2.0428(18) . ? Fe1 C10 2.045(2) . ? Fe1 C9 2.047(2) . ? Fe1 C8 2.049(2) . ? Fe1 C4 2.0674(19) . ? P1 C1 1.7958(19) . ? P1 C121 1.813(2) . ? P1 C111 1.819(2) . ? P1 S1 1.9539(7) . ? N1 C22 1.334(2) . ? N1 C23 1.388(3) . ? N1 C21 1.480(2) . ? N2 C22 1.332(2) . ? N2 C24 1.389(3) . ? N2 C231 1.483(2) . ? C1 C5 1.435(3) . ? C1 C2 1.452(2) . ? C2 C3 1.428(3) . ? C2 C21 1.506(3) . ? C3 C4 1.415(3) . ? C4 C5 1.412(3) . ? C6 C10 1.408(4) . ? C6 C7 1.412(4) . ? C7 C8 1.418(3) . ? C8 C9 1.400(4) . ? C9 C10 1.402(3) . ? C23 C28 1.390(3) . ? C23 C24 1.390(3) . ? C24 C25 1.391(3) . ? C25 C26 1.374(4) . ? C26 C27 1.421(4) . ? C26 C261 1.513(4) . ? C27 C28 1.380(4) . ? C27 C271 1.516(4) . ? C111 C112 1.388(3) . ? C111 C116 1.391(3) . ? C112 C113 1.392(3) . ? C113 C114 1.376(3) . ? C114 C115 1.376(4) . ? C115 C116 1.392(3) . ? C121 C126 1.389(3) . ? C121 C122 1.391(3) . ? C122 C123 1.377(4) . ? C123 C124 1.379(4) . ? C124 C125 1.376(4) . ? C125 C126 1.389(3) . ? C231 C232 1.518(3) . ? C232 C237 1.399(3) . ? C232 C233 1.408(3) . ? C233 C234 1.396(3) . ? C233 C238 1.507(3) . ? C234 C235 1.383(3) . ? C235 C236 1.389(3) . ? C235 C239 1.507(3) . ? C236 C237 1.398(3) . ? C237 C240 1.508(3) . ? B1 F3 1.369(3) . ? B1 F2 1.378(3) . ? B1 F4 1.381(3) . ? B1 F1 1.387(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 C2 Fe1 C1 42.00(7) . . ? C2 Fe1 C6 105.23(8) . . ? C1 Fe1 C6 126.10(10) . . ? C2 Fe1 C7 123.23(9) . . ? C1 Fe1 C7 162.64(9) . . ? C6 Fe1 C7 40.54(11) . . ? C2 Fe1 C5 69.53(7) . . ? C1 Fe1 C5 41.27(8) . . ? C6 Fe1 C5 165.64(10) . . ? C7 Fe1 C5 153.49(10) . . ? C2 Fe1 C3 41.15(8) . . ? C1 Fe1 C3 69.49(7) . . ? C6 Fe1 C3 117.16(9) . . ? C7 Fe1 C3 105.01(8) . . ? C5 Fe1 C3 68.28(7) . . ? C2 Fe1 C10 119.13(9) . . ? C1 Fe1 C10 108.95(9) . . ? C6 Fe1 C10 40.38(10) . . ? C7 Fe1 C10 67.98(10) . . ? C5 Fe1 C10 129.51(9) . . ? C3 Fe1 C10 152.70(9) . . ? C2 Fe1 C9 155.06(9) . . ? C1 Fe1 C9 121.59(9) . . ? C6 Fe1 C9 67.71(9) . . ? C7 Fe1 C9 67.88(9) . . ? C5 Fe1 C9 111.10(8) . . ? C3 Fe1 C9 163.67(10) . . ? C10 Fe1 C9 40.08(10) . . ? C2 Fe1 C8 161.58(9) . . ? C1 Fe1 C8 155.68(9) . . ? C6 Fe1 C8 67.82(10) . . ? C7 Fe1 C8 40.56(10) . . ? C5 Fe1 C8 121.19(9) . . ? C3 Fe1 C8 125.30(9) . . ? C10 Fe1 C8 67.41(10) . . ? C9 Fe1 C8 39.97(10) . . ? C2 Fe1 C4 68.79(8) . . ? C1 Fe1 C4 68.81(8) . . ? C6 Fe1 C4 151.80(10) . . ? C7 Fe1 C4 118.27(9) . . ? C5 Fe1 C4 40.19(8) . . ? C3 Fe1 C4 40.27(7) . . ? C10 Fe1 C4 166.45(9) . . ? C9 Fe1 C4 128.77(9) . . ? C8 Fe1 C4 108.77(9) . . ? C1 P1 C121 104.17(9) . . ? C1 P1 C111 104.98(9) . . ? C121 P1 C111 103.79(9) . . ? C1 P1 S1 116.01(7) . . ? C121 P1 S1 113.61(7) . . ? C111 P1 S1 113.07(7) . . ? C22 N1 C23 108.10(16) . . ? C22 N1 C21 124.65(16) . . ? C23 N1 C21 127.25(16) . . ? C22 N2 C24 108.12(16) . . ? C22 N2 C231 125.64(17) . . ? C24 N2 C231 126.18(16) . . ? C5 C1 C2 106.76(16) . . ? C5 C1 P1 122.69(14) . . ? C2 C1 P1 130.40(15) . . ? C5 C1 Fe1 69.84(11) . . ? C2 C1 Fe1 68.67(11) . . ? P1 C1 Fe1 129.70(10) . . ? C3 C2 C1 107.39(16) . . ? C3 C2 C21 123.38(16) . . ? C1 C2 C21 129.13(17) . . ? C3 C2 Fe1 70.24(11) . . ? C1 C2 Fe1 69.33(10) . . ? C21 C2 Fe1 123.02(13) . . ? C4 C3 C2 108.66(16) . . ? C4 C3 Fe1 70.80(11) . . ? C2 C3 Fe1 68.61(10) . . ? C5 C4 C3 108.37(17) . . ? C5 C4 Fe1 68.97(11) . . ? C3 C4 Fe1 68.93(11) . . ? C4 C5 C1 108.81(16) . . ? C4 C5 Fe1 70.85(11) . . ? C1 C5 Fe1 68.89(11) . . ? C10 C6 C7 108.2(2) . . ? C10 C6 Fe1 70.21(12) . . ? C7 C6 Fe1 69.97(13) . . ? C6 C7 C8 107.2(2) . . ? C6 C7 Fe1 69.49(14) . . ? C8 C7 Fe1 70.04(13) . . ? C9 C8 C7 108.2(2) . . ? C9 C8 Fe1 69.92(13) . . ? C7 C8 Fe1 69.40(13) . . ? C8 C9 C10 108.3(2) . . ? C8 C9 Fe1 70.11(12) . . ? C10 C9 Fe1 69.89(12) . . ? C9 C10 C6 108.0(2) . . ? C9 C10 Fe1 70.03(12) . . ? C6 C10 Fe1 69.41(13) . . ? N1 C21 C2 112.50(15) . . ? N2 C22 N1 110.35(17) . . ? N1 C23 C28 131.8(2) . . ? N1 C23 C24 106.75(17) . . ? C28 C23 C24 121.4(2) . . ? N2 C24 C23 106.66(17) . . ? N2 C24 C25 131.8(2) . . ? C23 C24 C25 121.5(2) . . ? C26 C25 C24 117.5(2) . . ? C25 C26 C27 121.1(2) . . ? C25 C26 C261 119.6(3) . . ? C27 C26 C261 119.3(3) . . ? C28 C27 C26 120.9(2) . . ? C28 C27 C271 119.4(3) . . ? C26 C27 C271 119.7(3) . . ? C27 C28 C23 117.5(2) . . ? C112 C111 C116 118.93(19) . . ? C112 C111 P1 119.86(15) . . ? C116 C111 P1 121.20(16) . . ? C111 C112 C113 120.2(2) . . ? C114 C113 C112 120.3(2) . . ? C115 C114 C113 120.0(2) . . ? C114 C115 C116 120.1(2) . . ? C111 C116 C115 120.4(2) . . ? C126 C121 C122 119.1(2) . . ? C126 C121 P1 121.83(17) . . ? C122 C121 P1 119.01(17) . . ? C123 C122 C121 120.2(2) . . ? C122 C123 C124 120.6(3) . . ? C125 C124 C123 119.8(3) . . ? C124 C125 C126 120.1(2) . . ? C121 C126 C125 120.3(2) . . ? N2 C231 C232 112.68(15) . . ? C237 C232 C233 120.00(18) . . ? C237 C232 C231 120.41(18) . . ? C233 C232 C231 119.57(19) . . ? C234 C233 C232 118.85(19) . . ? C234 C233 C238 118.56(19) . . ? C232 C233 C238 122.55(18) . . ? C235 C234 C233 122.1(2) . . ? C234 C235 C236 118.01(18) . . ? C234 C235 C239 121.2(2) . . ? C236 C235 C239 120.7(2) . . ? C235 C236 C237 122.1(2) . . ? C236 C237 C232 118.86(19) . . ? C236 C237 C240 118.03(19) . . ? C232 C237 C240 123.10(18) . . ? F3 B1 F2 108.7(2) . . ? F3 B1 F4 111.0(2) . . ? F2 B1 F4 111.7(2) . . ? F3 B1 F1 109.6(2) . . ? F2 B1 F1 107.5(2) . . ? F4 B1 F1 108.2(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.353 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.078 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 -0.147 0.250 225.7 89.1 2 0.500 0.147 0.750 225.8 89.4 3 0.000 0.353 0.250 225.7 89.1 4 0.000 0.647 0.750 225.8 89.4 _platon_squeeze_details ; Some residual electron density were difficult to modelize and therefore, the SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution of the electron density in the solvent region from the intensity data, and the solvent-free model was employed for the final refinement. There are four cavities of 226 \%A^3^ per unitl cell. PLATON estimated that each cavity contains 89 electrons which may correspond to a mixture of dichloromethane CH~2~Cl~2~ and ether (C~2~H~5~)~2~O as suggested by the crystallization process. ; _database_code_depnum_ccdc_archive 'CCDC 940118' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4B-S _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H35 Cl2 Fe N2 P Pd, 1.5(C H2 Cl2), 0.5(C4 H10 0)' _chemical_formula_sum 'C39.50 H43 Cl5 Fe N2 O0.50 P Pd' _chemical_formula_weight 924.23 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' Fe Fe 0.3463 0.8444 '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' 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 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 31.0431(10) _cell_length_b 9.7619(3) _cell_length_c 12.6606(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.076(2) _cell_angle_gamma 90.00 _cell_volume 3821.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.67 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_F_000 1880 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6396 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32604 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 30.72 _reflns_number_total 11489 _reflns_number_gt 10600 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2011)' _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^ > 2\s(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^)+(0.0437P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(12) _refine_ls_number_reflns 11489 _refine_ls_number_parameters 418 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0326 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.827846(4) 0.535124(14) -0.005013(11) 0.01753(4) Uani 1 1 d . . . Fe1 Fe 0.771414(12) 0.60013(4) 0.34255(3) 0.02877(8) Uani 1 1 d . . . P1 P 0.852140(16) 0.53191(8) 0.16733(4) 0.01959(9) Uani 1 1 d . . . Cl1 Cl 0.84386(2) 0.30358(6) -0.02980(5) 0.03196(14) Uani 1 1 d . . . Cl2 Cl 0.795116(19) 0.56231(5) -0.18094(4) 0.02592(13) Uani 1 1 d . . . N1 N 0.79204(7) 0.80874(19) 0.04788(14) 0.0207(4) Uani 1 1 d . . . N2 N 0.84682(6) 0.82802(19) -0.04380(15) 0.0214(4) Uani 1 1 d . . . C1 C 0.82264(7) 0.6337(2) 0.25473(17) 0.0216(4) Uani 1 1 d . . . C2 C 0.78794(8) 0.7289(2) 0.22758(17) 0.0216(4) Uani 1 1 d . . . C3 C 0.78060(9) 0.8048(3) 0.3214(2) 0.0281(5) Uani 1 1 d . . . H3 H 0.7604 0.8744 0.3257 0.034 Uiso 1 1 calc R . . C4 C 0.80905(9) 0.7565(3) 0.40553(19) 0.0336(6) Uani 1 1 d . . . H4 H 0.8106 0.7880 0.4751 0.040 Uiso 1 1 calc R . . C5 C 0.83507(9) 0.6509(3) 0.36645(19) 0.0303(5) Uani 1 1 d . . . H5 H 0.8564 0.6016 0.4062 0.036 Uiso 1 1 calc R . . C6 C 0.70848(10) 0.5390(5) 0.3098(3) 0.0538(8) Uani 1 1 d . . . H6 H 0.6891 0.5746 0.2566 0.065 Uiso 1 1 calc R . . C7 C 0.71488(13) 0.5877(4) 0.4142(3) 0.0622(10) Uani 1 1 d . . . H7 H 0.7002 0.6599 0.4429 0.075 Uiso 1 1 calc R . . C8 C 0.74782(16) 0.5065(5) 0.4681(3) 0.0725(13) Uani 1 1 d . . . H8 H 0.7590 0.5171 0.5382 0.087 Uiso 1 1 calc R . . C9 C 0.76082(15) 0.4056(4) 0.3955(4) 0.0664(12) Uani 1 1 d . . . H9 H 0.7817 0.3382 0.4098 0.080 Uiso 1 1 calc R . . C10 C 0.73631(12) 0.4273(3) 0.2990(3) 0.0554(10) Uani 1 1 d . . . H10 H 0.7381 0.3761 0.2376 0.067 Uiso 1 1 calc R . . C21 C 0.76342(7) 0.7470(3) 0.12130(18) 0.0236(4) Uani 1 1 d . . . C22 C 0.82252(7) 0.7361(2) 0.00392(16) 0.0194(4) Uani 1 1 d . . . C23 C 0.79708(9) 0.9469(2) 0.02955(18) 0.0257(5) Uani 1 1 d . . . H23 H 0.7803 1.0179 0.0529 0.031 Uiso 1 1 calc R . . C24 C 0.83106(9) 0.9583(2) -0.0288(2) 0.0285(5) Uani 1 1 d . . . H24 H 0.8420 1.0393 -0.0544 0.034 Uiso 1 1 calc R . . C25 C 0.88583(9) 0.7888(3) -0.0940(2) 0.0346(6) Uani 1 1 d . . . C111 C 0.90583(8) 0.6056(3) 0.17802(19) 0.0321(6) Uani 1 1 d . . . C112 C 0.93793(8) 0.5368(5) 0.1284(2) 0.0547(8) Uani 1 1 d . . . H112 H 0.9316 0.4545 0.0933 0.066 Uiso 1 1 calc R . . C113 C 0.97950(11) 0.5919(7) 0.1315(3) 0.0838(17) Uani 1 1 d . . . H113 H 1.0011 0.5451 0.0999 0.101 Uiso 1 1 calc R . . C114 C 0.98898(13) 0.7178(7) 0.1822(4) 0.095(2) Uani 1 1 d . . . H114 H 1.0167 0.7547 0.1839 0.114 Uiso 1 1 calc R . . C115 C 0.95765(16) 0.7846(5) 0.2283(4) 0.0838(17) Uani 1 1 d . . . H115 H 0.9640 0.8677 0.2622 0.101 Uiso 1 1 calc R . . C116 C 0.91538(11) 0.7314(4) 0.2265(3) 0.0483(8) Uani 1 1 d . . . H116 H 0.8940 0.7800 0.2575 0.058 Uiso 1 1 calc R . . C121 C 0.85833(8) 0.3664(3) 0.23407(19) 0.0276(5) Uani 1 1 d . . . C122 C 0.82603(10) 0.2687(3) 0.2161(2) 0.0358(6) Uani 1 1 d . . . H122 H 0.8028 0.2857 0.1662 0.043 Uiso 1 1 calc R . . C123 C 0.82789(12) 0.1458(3) 0.2718(2) 0.0456(7) Uani 1 1 d . . . H123 H 0.8058 0.0819 0.2606 0.055 Uiso 1 1 calc R . . C124 C 0.86309(14) 0.1196(4) 0.3443(3) 0.0560(9) Uani 1 1 d . . . H124 H 0.8649 0.0370 0.3810 0.067 Uiso 1 1 calc R . . C125 C 0.89523(13) 0.2152(4) 0.3618(3) 0.0538(9) Uani 1 1 d . . . H125 H 0.9186 0.1969 0.4108 0.065 Uiso 1 1 calc R . . C126 C 0.89341(10) 0.3387(3) 0.3076(2) 0.0375(6) Uani 1 1 d . . . H126 H 0.9154 0.4027 0.3201 0.045 Uiso 1 1 calc R . . C251 C 0.90557(8) 0.9013(3) -0.1578(2) 0.0280(5) Uani 1 1 d . . . C252 C 0.93142(9) 1.0022(3) -0.1060(2) 0.0352(6) Uani 1 1 d . . . C253 C 0.95402(9) 1.0915(3) -0.1669(3) 0.0476(8) Uani 1 1 d . . . H253 H 0.9712 1.1591 -0.1329 0.057 Uiso 1 1 calc R . . C254 C 0.95166(10) 1.0827(4) -0.2767(3) 0.0480(8) Uani 1 1 d . . . C255 C 0.92476(10) 0.9870(4) -0.3257(2) 0.0461(8) Uani 1 1 d . . . H255 H 0.9219 0.9833 -0.3993 0.055 Uiso 1 1 calc R . . C256 C 0.90153(9) 0.8952(3) -0.2694(2) 0.0353(6) Uani 1 1 d . . . C257 C 0.93693(12) 1.0162(4) 0.0125(2) 0.0543(9) Uani 1 1 d . . . H25A H 0.9146 0.9655 0.0431 0.081 Uiso 1 1 calc R . . H25B H 0.9350 1.1111 0.0315 0.081 Uiso 1 1 calc R . . H25C H 0.9647 0.9809 0.0388 0.081 Uiso 1 1 calc R . . C258 C 0.97865(15) 1.1737(5) -0.3401(4) 0.0944(19) Uani 1 1 d . . . H25D H 1.0081 1.1428 -0.3326 0.142 Uiso 1 1 calc R . . H25E H 0.9772 1.2661 -0.3148 0.142 Uiso 1 1 calc R . . H25F H 0.9678 1.1703 -0.4135 0.142 Uiso 1 1 calc R . . C259 C 0.87403(12) 0.7910(4) -0.3299(3) 0.0541(9) Uani 1 1 d . . . H25G H 0.8702 0.8168 -0.4033 0.081 Uiso 1 1 calc R . . H25H H 0.8463 0.7862 -0.3019 0.081 Uiso 1 1 calc R . . H25I H 0.8879 0.7031 -0.3234 0.081 Uiso 1 1 calc R . . C100 C 0.87780(11) 0.3610(4) 0.7272(2) 0.0481(8) Uani 1 1 d . . . H10A H 0.8523 0.3898 0.7604 0.058 Uiso 1 1 calc R . . H10B H 0.8825 0.2646 0.7427 0.058 Uiso 1 1 calc R . . Cl11 Cl 0.92208(4) 0.45413(12) 0.78031(10) 0.0745(3) Uani 1 1 d . . . Cl12 Cl 0.86878(5) 0.38336(17) 0.59015(9) 0.0964(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02010(7) 0.01204(6) 0.02052(7) -0.00061(6) 0.00212(5) 0.00057(7) Fe1 0.0365(2) 0.02499(18) 0.02631(16) 0.00383(13) 0.01093(14) -0.00146(15) P1 0.0197(2) 0.0176(2) 0.0213(2) 0.0025(3) 0.00088(17) 0.0006(3) Cl1 0.0443(4) 0.0143(2) 0.0365(3) -0.0031(2) -0.0008(3) 0.0055(2) Cl2 0.0306(3) 0.0243(3) 0.0222(2) 0.00037(18) -0.00102(19) -0.0027(2) N1 0.0299(10) 0.0152(8) 0.0172(8) 0.0009(7) 0.0030(7) 0.0058(7) N2 0.0264(10) 0.0124(9) 0.0256(9) 0.0004(7) 0.0039(8) 0.0004(7) C1 0.0248(11) 0.0184(10) 0.0213(9) -0.0008(8) 0.0005(8) -0.0013(8) C2 0.0279(11) 0.0191(10) 0.0182(9) 0.0021(8) 0.0034(8) -0.0002(8) C3 0.0383(14) 0.0220(11) 0.0245(10) -0.0024(9) 0.0053(10) 0.0001(10) C4 0.0445(16) 0.0347(14) 0.0214(11) -0.0070(10) 0.0012(10) -0.0008(12) C5 0.0363(14) 0.0316(13) 0.0218(10) 0.0001(9) -0.0044(10) 0.0017(11) C6 0.0395(15) 0.0510(18) 0.074(2) -0.010(2) 0.0207(14) -0.0176(19) C7 0.066(2) 0.054(2) 0.074(2) -0.0062(18) 0.048(2) -0.0104(18) C8 0.098(3) 0.073(3) 0.0521(19) 0.0230(19) 0.034(2) -0.020(2) C9 0.085(3) 0.044(2) 0.077(3) 0.0318(19) 0.041(2) -0.0005(19) C10 0.051(2) 0.0386(18) 0.081(3) -0.0125(17) 0.0299(19) -0.0228(15) C21 0.0222(11) 0.0263(11) 0.0224(10) 0.0015(9) 0.0028(8) 0.0038(9) C22 0.0271(11) 0.0136(10) 0.0167(9) -0.0003(7) -0.0018(8) 0.0015(8) C23 0.0376(14) 0.0133(9) 0.0265(11) 0.0012(8) 0.0040(10) 0.0080(9) C24 0.0405(14) 0.0121(9) 0.0329(12) 0.0008(9) 0.0040(10) 0.0023(9) C25 0.0292(13) 0.0243(12) 0.0532(16) 0.0091(11) 0.0201(12) 0.0054(10) C111 0.0217(11) 0.0473(16) 0.0265(11) 0.0136(11) -0.0022(9) -0.0078(11) C112 0.0259(12) 0.092(3) 0.0463(15) 0.013(2) 0.0027(11) 0.005(2) C113 0.0244(16) 0.157(5) 0.071(3) 0.034(3) 0.0090(16) 0.002(2) C114 0.031(2) 0.170(6) 0.082(3) 0.063(4) -0.012(2) -0.039(3) C115 0.071(3) 0.094(3) 0.080(3) 0.040(3) -0.034(2) -0.056(3) C116 0.0467(18) 0.0480(19) 0.0482(17) 0.0109(14) -0.0073(14) -0.0237(15) C121 0.0341(13) 0.0221(11) 0.0269(11) 0.0053(9) 0.0055(10) 0.0046(10) C122 0.0450(16) 0.0252(12) 0.0371(14) 0.0065(10) 0.0036(12) 0.0001(11) C123 0.069(2) 0.0268(14) 0.0425(15) 0.0082(12) 0.0116(15) -0.0091(14) C124 0.093(3) 0.0285(15) 0.0481(17) 0.0183(14) 0.0140(18) 0.0169(17) C125 0.064(2) 0.051(2) 0.0463(17) 0.0178(15) 0.0018(16) 0.0268(17) C126 0.0409(16) 0.0362(15) 0.0348(13) 0.0099(11) 0.0004(12) 0.0073(12) C251 0.0229(12) 0.0234(11) 0.0383(13) 0.0075(10) 0.0055(10) 0.0043(9) C252 0.0285(12) 0.0341(15) 0.0422(14) 0.0110(11) -0.0011(10) 0.0000(10) C253 0.0252(14) 0.0371(15) 0.080(2) 0.0141(16) 0.0031(14) -0.0033(12) C254 0.0377(16) 0.0467(17) 0.0627(19) 0.0287(15) 0.0222(14) 0.0094(13) C255 0.0386(16) 0.060(2) 0.0414(15) 0.0176(14) 0.0145(13) 0.0125(14) C256 0.0254(13) 0.0443(16) 0.0369(13) 0.0072(12) 0.0069(10) 0.0087(11) C257 0.0596(19) 0.056(2) 0.0449(16) 0.0018(16) -0.0086(14) -0.0096(18) C258 0.075(3) 0.083(3) 0.134(4) 0.069(3) 0.064(3) 0.016(2) C259 0.0472(19) 0.067(2) 0.0475(18) -0.0128(16) -0.0016(15) 0.0125(17) C100 0.0445(18) 0.054(2) 0.0457(17) -0.0048(15) 0.0056(14) 0.0097(15) Cl11 0.0658(6) 0.0645(6) 0.0908(7) -0.0172(6) -0.0069(6) 0.0014(5) Cl12 0.1194(11) 0.1260(12) 0.0436(5) -0.0018(6) 0.0057(6) -0.0338(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C22 1.973(2) . ? Pd1 P1 2.2449(5) . ? Pd1 Cl1 2.3414(6) . ? Pd1 Cl2 2.3798(5) . ? Fe1 C2 2.023(2) . ? Fe1 C8 2.026(3) . ? Fe1 C5 2.034(3) . ? Fe1 C3 2.039(3) . ? Fe1 C4 2.041(3) . ? Fe1 C1 2.046(2) . ? Fe1 C7 2.049(3) . ? Fe1 C9 2.050(3) . ? Fe1 C6 2.050(3) . ? Fe1 C10 2.057(3) . ? P1 C1 1.797(2) . ? P1 C111 1.809(3) . ? P1 C121 1.825(2) . ? N1 C22 1.342(3) . ? N1 C23 1.380(3) . ? N1 C21 1.471(3) . ? N2 C22 1.349(3) . ? N2 C24 1.382(3) . ? N2 C25 1.468(3) . ? C1 C2 1.441(3) . ? C1 C5 1.443(3) . ? C2 C3 1.435(3) . ? C2 C21 1.497(3) . ? C3 C4 1.404(4) . ? C4 C5 1.425(4) . ? C6 C7 1.403(5) . ? C6 C10 1.405(5) . ? C7 C8 1.420(6) . ? C8 C9 1.429(6) . ? C9 C10 1.397(6) . ? C23 C24 1.345(4) . ? C25 C251 1.524(3) . ? C111 C116 1.393(4) . ? C111 C112 1.397(5) . ? C112 C113 1.396(5) . ? C113 C114 1.405(8) . ? C114 C115 1.346(8) . ? C115 C116 1.409(5) . ? C121 C122 1.388(4) . ? C121 C126 1.395(4) . ? C122 C123 1.390(4) . ? C123 C124 1.387(5) . ? C124 C125 1.370(6) . ? C125 C126 1.386(4) . ? C251 C252 1.398(4) . ? C251 C256 1.409(4) . ? C252 C253 1.394(4) . ? C252 C257 1.501(4) . ? C253 C254 1.388(5) . ? C254 C255 1.365(5) . ? C254 C258 1.501(4) . ? C255 C256 1.386(4) . ? C256 C259 1.494(5) . ? C100 Cl11 1.733(4) . ? C100 Cl12 1.747(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 C22 Pd1 P1 88.90(6) . . ? C22 Pd1 Cl1 170.93(7) . . ? P1 Pd1 Cl1 93.43(2) . . ? C22 Pd1 Cl2 84.93(6) . . ? P1 Pd1 Cl2 171.96(2) . . ? Cl1 Pd1 Cl2 93.46(2) . . ? C2 Fe1 C8 167.69(16) . . ? C2 Fe1 C5 69.56(10) . . ? C8 Fe1 C5 114.03(16) . . ? C2 Fe1 C3 41.37(9) . . ? C8 Fe1 C3 127.57(16) . . ? C5 Fe1 C3 68.62(11) . . ? C2 Fe1 C4 69.13(10) . . ? C8 Fe1 C4 105.38(16) . . ? C5 Fe1 C4 40.93(11) . . ? C3 Fe1 C4 40.26(11) . . ? C2 Fe1 C1 41.46(9) . . ? C8 Fe1 C1 148.33(16) . . ? C5 Fe1 C1 41.41(9) . . ? C3 Fe1 C1 69.33(10) . . ? C4 Fe1 C1 69.31(10) . . ? C2 Fe1 C7 129.57(15) . . ? C8 Fe1 C7 40.77(18) . . ? C5 Fe1 C7 143.84(14) . . ? C3 Fe1 C7 104.56(15) . . ? C4 Fe1 C7 110.75(14) . . ? C1 Fe1 C7 170.90(14) . . ? C2 Fe1 C9 150.34(14) . . ? C8 Fe1 C9 41.04(18) . . ? C5 Fe1 C9 111.04(15) . . ? C3 Fe1 C9 168.19(15) . . ? C4 Fe1 C9 131.89(16) . . ? C1 Fe1 C9 118.77(14) . . ? C7 Fe1 C9 68.39(17) . . ? C2 Fe1 C6 109.46(13) . . ? C8 Fe1 C6 67.85(18) . . ? C5 Fe1 C6 175.69(13) . . ? C3 Fe1 C6 113.62(16) . . ? C4 Fe1 C6 143.07(14) . . ? C1 Fe1 C6 135.19(11) . . ? C7 Fe1 C6 40.02(15) . . ? C9 Fe1 C6 67.59(18) . . ? C2 Fe1 C10 118.61(13) . . ? C8 Fe1 C10 67.68(17) . . ? C5 Fe1 C10 136.43(13) . . ? C3 Fe1 C10 147.70(15) . . ? C4 Fe1 C10 171.65(15) . . ? C1 Fe1 C10 113.88(12) . . ? C7 Fe1 C10 67.41(15) . . ? C9 Fe1 C10 39.78(18) . . ? C6 Fe1 C10 40.00(16) . . ? C1 P1 C111 104.48(12) . . ? C1 P1 C121 104.07(11) . . ? C111 P1 C121 105.00(12) . . ? C1 P1 Pd1 116.42(7) . . ? C111 P1 Pd1 107.17(8) . . ? C121 P1 Pd1 118.35(8) . . ? C22 N1 C23 110.6(2) . . ? C22 N1 C21 122.23(19) . . ? C23 N1 C21 126.2(2) . . ? C22 N2 C24 109.4(2) . . ? C22 N2 C25 122.43(19) . . ? C24 N2 C25 128.0(2) . . ? C2 C1 C5 106.8(2) . . ? C2 C1 P1 128.36(16) . . ? C5 C1 P1 124.14(18) . . ? C2 C1 Fe1 68.43(13) . . ? C5 C1 Fe1 68.85(14) . . ? P1 C1 Fe1 135.13(13) . . ? C3 C2 C1 107.8(2) . . ? C3 C2 C21 125.3(2) . . ? C1 C2 C21 126.9(2) . . ? C3 C2 Fe1 69.92(14) . . ? C1 C2 Fe1 70.11(13) . . ? C21 C2 Fe1 125.39(16) . . ? C4 C3 C2 108.6(2) . . ? C4 C3 Fe1 69.93(16) . . ? C2 C3 Fe1 68.71(14) . . ? C3 C4 C5 108.5(2) . . ? C3 C4 Fe1 69.81(15) . . ? C5 C4 Fe1 69.27(15) . . ? C4 C5 C1 108.3(2) . . ? C4 C5 Fe1 69.80(15) . . ? C1 C5 Fe1 69.73(14) . . ? C7 C6 C10 108.5(4) . . ? C7 C6 Fe1 70.0(2) . . ? C10 C6 Fe1 70.27(18) . . ? C6 C7 C8 107.4(4) . . ? C6 C7 Fe1 70.00(17) . . ? C8 C7 Fe1 68.7(2) . . ? C7 C8 C9 108.0(4) . . ? C7 C8 Fe1 70.51(19) . . ? C9 C8 Fe1 70.38(19) . . ? C10 C9 C8 107.1(4) . . ? C10 C9 Fe1 70.39(19) . . ? C8 C9 Fe1 68.6(2) . . ? C9 C10 C6 109.0(3) . . ? C9 C10 Fe1 69.8(2) . . ? C6 C10 Fe1 69.73(18) . . ? N1 C21 C2 109.22(19) . . ? N1 C22 N2 106.1(2) . . ? N1 C22 Pd1 127.93(18) . . ? N2 C22 Pd1 125.63(17) . . ? C24 C23 N1 106.2(2) . . ? C23 C24 N2 107.7(2) . . ? N2 C25 C251 115.3(2) . . ? C116 C111 C112 119.3(3) . . ? C116 C111 P1 122.8(2) . . ? C112 C111 P1 117.7(3) . . ? C113 C112 C111 119.7(5) . . ? C112 C113 C114 120.4(5) . . ? C115 C114 C113 119.4(4) . . ? C114 C115 C116 121.5(5) . . ? C111 C116 C115 119.6(4) . . ? C122 C121 C126 119.1(2) . . ? C122 C121 P1 119.16(19) . . ? C126 C121 P1 121.6(2) . . ? C121 C122 C123 120.9(3) . . ? C124 C123 C122 119.3(3) . . ? C125 C124 C123 120.1(3) . . ? C124 C125 C126 121.0(3) . . ? C125 C126 C121 119.6(3) . . ? C252 C251 C256 119.8(2) . . ? C252 C251 C25 120.0(2) . . ? C256 C251 C25 119.8(2) . . ? C253 C252 C251 118.5(3) . . ? C253 C252 C257 118.6(3) . . ? C251 C252 C257 122.9(3) . . ? C254 C253 C252 122.1(3) . . ? C255 C254 C253 118.2(3) . . ? C255 C254 C258 120.6(4) . . ? C253 C254 C258 121.1(4) . . ? C254 C255 C256 122.3(3) . . ? C255 C256 C251 118.9(3) . . ? C255 C256 C259 118.5(3) . . ? C251 C256 C259 122.6(3) . . ? Cl11 C100 Cl12 111.8(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.72 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.567 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.078 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.322 0.500 188 86 ' ' 2 0.500 0.178 0.500 188 86 ' ' _platon_squeeze_details ; Some residual electron density were difficult to modelize and therefore, the SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution of the electron density in the solvent region from the intensity data, and the solvent-free model was employed for the final refinement. There are two cavities of 188 \%A^3^ per unitl cell. PLATON estimated that each cavity contains 86 electrons which may correspond to a mixture of dichloromethane CH~2~Cl~2~ and ether (C~2~H~5~)~2~O as suggested by the crystallization process ; _database_code_depnum_ccdc_archive 'CCDC 940119' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4c-S _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C33 H31 Cl2 Fe N2 P Pd), 0.5(C3 H6 O)' _chemical_formula_sum 'C67.50 H65 Cl4 Fe2 N4 O0.50 P2 Pd2' _chemical_formula_weight 1468.47 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.8749(3) _cell_length_b 15.7967(4) _cell_length_c 16.9843(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.010(2) _cell_angle_gamma 90.00 _cell_volume 3137.49(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 22084 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 28.50 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.284 _exptl_absorpt_correction_T_min 0.81076 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. CrysAlisPro (Agilent Technologies, 2012) ; _exptl_special_details ? _diffrn_ambient_temperature 180(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 'Xcalibur, Sapphire1, long nozzle' _diffrn_detector_area_resol_mean 8.2632 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34705 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.10 _reflns_number_total 13118 _reflns_number_gt 12155 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2012)' _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^ > 2\s(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^)+(0.0377P)^2^+0.1612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(12) _refine_ls_number_reflns 13118 _refine_ls_number_parameters 727 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 0.18648(2) 0.237338(14) 0.000643(14) 0.02305(6) Uani 1 1 d . . . Fe1 Fe 0.55949(4) 0.19610(3) -0.02574(3) 0.02662(10) Uani 1 1 d . . . Cl11 Cl 0.01496(8) 0.27789(6) -0.08110(5) 0.0385(2) Uani 1 1 d . . . Cl12 Cl 0.22862(8) 0.38075(5) 0.02471(6) 0.0404(2) Uani 1 1 d . . . P1 P 0.33672(7) 0.18061(5) 0.08466(5) 0.02196(16) Uani 1 1 d . . . N11 N 0.2258(2) 0.08867(16) -0.09118(16) 0.0236(6) Uani 1 1 d . . . N12 N 0.0797(2) 0.06174(18) -0.03453(16) 0.0274(6) Uani 1 1 d . . . C1 C 0.1592(3) 0.1211(2) -0.0414(2) 0.0267(7) Uani 1 1 d . . . C11 C 0.4468(3) 0.1414(2) 0.03493(18) 0.0253(7) Uani 1 1 d . . . C12 C 0.4299(3) 0.1135(2) -0.04690(19) 0.0236(7) Uani 1 1 d . . . C13 C 0.5324(3) 0.0730(2) -0.0590(2) 0.0307(8) Uani 1 1 d . . . H13 H 0.5450 0.0473 -0.1073 0.037 Uiso 1 1 calc R . . C14 C 0.6123(3) 0.0774(2) 0.0130(2) 0.0356(8) Uani 1 1 d . . . H14 H 0.6879 0.0554 0.0211 0.043 Uiso 1 1 calc R . . C15 C 0.5615(3) 0.1197(2) 0.0706(2) 0.0307(8) Uani 1 1 d . . . H15 H 0.5971 0.1318 0.1239 0.037 Uiso 1 1 calc R . . C16 C 0.5239(5) 0.3216(3) -0.0427(3) 0.0570(14) Uani 1 1 d . . . H16 H 0.4618 0.3509 -0.0267 0.068 Uiso 1 1 calc R . . C17 C 0.5252(4) 0.2824(3) -0.1148(3) 0.0501(11) Uani 1 1 d . . . H17 H 0.4623 0.2803 -0.1578 0.060 Uiso 1 1 calc R . . C18 C 0.6291(5) 0.2470(3) -0.1157(3) 0.0612(13) Uani 1 1 d . . . H18 H 0.6500 0.2169 -0.1594 0.073 Uiso 1 1 calc R . . C19 C 0.6972(4) 0.2612(4) -0.0460(4) 0.0783(19) Uani 1 1 d . . . H19 H 0.7740 0.2423 -0.0318 0.094 Uiso 1 1 calc R . . C20 C 0.6363(6) 0.3090(4) 0.0035(3) 0.079(2) Uani 1 1 d . . . H20 H 0.6640 0.3286 0.0562 0.095 Uiso 1 1 calc R . . C111 C 0.4088(3) 0.2352(2) 0.17366(19) 0.0283(7) Uani 1 1 d . . . C112 C 0.4594(3) 0.1886(3) 0.2390(2) 0.0388(8) Uani 1 1 d . . . H112 H 0.4578 0.1285 0.2364 0.047 Uiso 1 1 calc R . . C113 C 0.5124(4) 0.2282(3) 0.3080(2) 0.0499(11) Uani 1 1 d . . . H113 H 0.5487 0.1951 0.3518 0.060 Uiso 1 1 calc R . . C114 C 0.5131(4) 0.3126(3) 0.3138(3) 0.0566(13) Uani 1 1 d . . . H114 H 0.5490 0.3394 0.3617 0.068 Uiso 1 1 calc R . . C115 C 0.4627(6) 0.3592(3) 0.2514(4) 0.088(2) Uani 1 1 d . . . H115 H 0.4617 0.4192 0.2559 0.105 Uiso 1 1 calc R . . C116 C 0.4121(5) 0.3213(3) 0.1805(3) 0.0674(16) Uani 1 1 d . . . H116 H 0.3795 0.3554 0.1363 0.081 Uiso 1 1 calc R . . C121 C 0.2875(3) 0.0861(2) 0.12951(19) 0.0251(7) Uani 1 1 d . . . C122 C 0.3409(5) 0.0095(3) 0.1282(4) 0.0680(17) Uani 1 1 d . . . H122 H 0.4021 0.0033 0.0992 0.082 Uiso 1 1 calc R . . C133 C 0.2279(3) -0.0487(2) -0.1677(2) 0.0284(7) Uani 1 1 d . . . H133 H 0.2906 -0.0355 -0.1935 0.034 Uiso 1 1 calc R . . C123 C 0.3063(6) -0.0589(3) 0.1689(5) 0.110(3) Uani 1 1 d . . . H123 H 0.3453 -0.1114 0.1687 0.132 Uiso 1 1 calc R . . C131 C 0.3278(3) 0.1311(2) -0.10854(19) 0.0230(6) Uani 1 1 d . . . H13A H 0.3140 0.1929 -0.1116 0.028 Uiso 1 1 calc R . . H13B H 0.3427 0.1119 -0.1613 0.028 Uiso 1 1 calc R . . C132 C 0.1902(3) 0.0080(2) -0.11616(19) 0.0245(7) Uani 1 1 d . . . C134 C 0.1720(3) -0.1242(2) -0.1803(2) 0.0320(8) Uani 1 1 d . . . C124 C 0.2177(5) -0.0520(3) 0.2089(4) 0.078(2) Uani 1 1 d . . . H124 H 0.1934 -0.0997 0.2356 0.093 Uiso 1 1 calc R . . C125 C 0.1632(4) 0.0241(2) 0.2107(2) 0.0376(9) Uani 1 1 d . . . H125 H 0.0999 0.0292 0.2378 0.045 Uiso 1 1 calc R . . C135 C 0.0798(3) -0.1442(2) -0.1405(2) 0.0332(8) Uani 1 1 d . . . C126 C 0.2003(3) 0.0932(2) 0.1731(2) 0.0291(7) Uani 1 1 d . . . H126 H 0.1653 0.1467 0.1773 0.035 Uiso 1 1 calc R . . C136 C 0.0418(3) -0.0862(2) -0.0899(2) 0.0319(8) Uani 1 1 d . . . H136 H -0.0208 -0.0987 -0.0638 0.038 Uiso 1 1 calc R . . C137 C 0.0976(3) -0.0101(2) -0.07891(19) 0.0267(7) Uani 1 1 d . . . C138 C 0.0225(4) -0.2292(3) -0.1518(3) 0.0500(11) Uani 1 1 d . . . H13C H -0.0355 -0.2334 -0.1173 0.075 Uiso 1 1 calc R . . H13D H 0.0796 -0.2739 -0.1375 0.075 Uiso 1 1 calc R . . H13E H -0.0141 -0.2358 -0.2077 0.075 Uiso 1 1 calc R . . C139 C 0.2103(4) -0.1884(3) -0.2361(3) 0.0509(11) Uani 1 1 d . . . H13F H 0.2671 -0.1626 -0.2641 0.076 Uiso 1 1 calc R . . H13G H 0.1442 -0.2069 -0.2752 0.076 Uiso 1 1 calc R . . H13H H 0.2442 -0.2372 -0.2052 0.076 Uiso 1 1 calc R . . C140 C -0.0130(3) 0.0704(3) 0.0099(2) 0.0371(9) Uani 1 1 d . . . H14A H -0.0100 0.1267 0.0344 0.056 Uiso 1 1 calc R . . H14B H -0.0056 0.0271 0.0518 0.056 Uiso 1 1 calc R . . H14C H -0.0861 0.0632 -0.0263 0.056 Uiso 1 1 calc R . . Pd2 Pd 0.37767(2) 0.191554(17) 0.654801(15) 0.03036(7) Uani 1 1 d . . . Fe2 Fe 0.18353(5) 0.45389(3) 0.70806(3) 0.02811(11) Uani 1 1 d . . . Cl21 Cl 0.45010(9) 0.06767(6) 0.71958(6) 0.0433(2) Uani 1 1 d . . . Cl22 Cl 0.56102(10) 0.22667(10) 0.63963(10) 0.0790(4) Uani 1 1 d . . . P2 P 0.29700(8) 0.30558(6) 0.58862(5) 0.02742(19) Uani 1 1 d . . . N21 N 0.1560(2) 0.18069(17) 0.71360(16) 0.0260(6) Uani 1 1 d . . . N22 N 0.1760(3) 0.07621(19) 0.63550(18) 0.0338(7) Uani 1 1 d . . . C2 C 0.2246(3) 0.1492(2) 0.6656(2) 0.0294(7) Uani 1 1 d . . . C21 C 0.1857(3) 0.3584(2) 0.62816(19) 0.0262(7) Uani 1 1 d . . . C22 C 0.1331(3) 0.3322(2) 0.69451(19) 0.0254(7) Uani 1 1 d . . . C23 C 0.0377(3) 0.3846(2) 0.6960(2) 0.0337(8) Uani 1 1 d . . . H23 H -0.0132 0.3806 0.7333 0.040 Uiso 1 1 calc R . . C24 C 0.0298(3) 0.4443(3) 0.6332(2) 0.0392(9) Uani 1 1 d . . . H24 H -0.0268 0.4871 0.6212 0.047 Uiso 1 1 calc R . . C25 C 0.1211(3) 0.4291(2) 0.5913(2) 0.0337(8) Uani 1 1 d . . . H25 H 0.1369 0.4602 0.5465 0.040 Uiso 1 1 calc R . . C26 C 0.3411(4) 0.4738(3) 0.7736(3) 0.0511(11) Uani 1 1 d . . . H26 H 0.4054 0.4375 0.7764 0.061 Uiso 1 1 calc R . . C27 C 0.3134(5) 0.5387(3) 0.7191(3) 0.0545(12) Uani 1 1 d . . . H27 H 0.3540 0.5539 0.6777 0.065 Uiso 1 1 calc R . . C28 C 0.2159(5) 0.5776(3) 0.7357(3) 0.0566(14) Uani 1 1 d . . . H28 H 0.1786 0.6250 0.7081 0.068 Uiso 1 1 calc R . . C29 C 0.1813(4) 0.5355(3) 0.7998(3) 0.0607(14) Uani 1 1 d . . . H29 H 0.1165 0.5484 0.8235 0.073 Uiso 1 1 calc R . . C30 C 0.2617(5) 0.4699(3) 0.8227(3) 0.0540(13) Uani 1 1 d . . . H30 H 0.2606 0.4303 0.8647 0.065 Uiso 1 1 calc R . . C211 C 0.3849(4) 0.3906(2) 0.5612(2) 0.0382(9) Uani 1 1 d . . . C212 C 0.4783(4) 0.4196(3) 0.6150(3) 0.0518(11) Uani 1 1 d . . . H212 H 0.4997 0.3920 0.6651 0.062 Uiso 1 1 calc R . . C213 C 0.5403(5) 0.4885(4) 0.5962(4) 0.0754(18) Uani 1 1 d . . . H213 H 0.6037 0.5082 0.6338 0.090 Uiso 1 1 calc R . . C214 C 0.5119(6) 0.5280(4) 0.5252(4) 0.082(2) Uani 1 1 d . . . H214 H 0.5555 0.5751 0.5128 0.099 Uiso 1 1 calc R . . C215 C 0.4191(6) 0.5000(4) 0.4701(4) 0.0785(19) Uani 1 1 d . . . H215 H 0.3987 0.5280 0.4202 0.094 Uiso 1 1 calc R . . C216 C 0.3567(5) 0.4315(3) 0.4882(3) 0.0586(13) Uani 1 1 d . . . H216 H 0.2936 0.4121 0.4503 0.070 Uiso 1 1 calc R . . C221 C 0.2230(3) 0.2615(2) 0.49510(19) 0.0271(7) Uani 1 1 d . . . C222 C 0.2870(3) 0.2306(2) 0.4397(2) 0.0353(8) Uani 1 1 d . . . H222 H 0.3676 0.2378 0.4485 0.042 Uiso 1 1 calc R . . C223 C 0.2323(4) 0.1897(3) 0.3725(2) 0.0431(9) Uani 1 1 d . . . H223 H 0.2755 0.1689 0.3345 0.052 Uiso 1 1 calc R . . C224 C 0.1171(4) 0.1787(2) 0.3595(2) 0.0418(10) Uani 1 1 d . . . H224 H 0.0808 0.1496 0.3130 0.050 Uiso 1 1 calc R . . C225 C 0.0530(4) 0.2090(3) 0.4125(2) 0.0449(10) Uani 1 1 d . . . H225 H -0.0277 0.2020 0.4026 0.054 Uiso 1 1 calc R . . C226 C 0.1068(3) 0.2506(3) 0.4816(2) 0.0385(9) Uani 1 1 d . . . H226 H 0.0628 0.2712 0.5192 0.046 Uiso 1 1 calc R . . C231 C 0.1750(3) 0.2634(2) 0.75154(19) 0.0265(7) Uani 1 1 d . . . H23A H 0.2577 0.2712 0.7715 0.032 Uiso 1 1 calc R . . H23B H 0.1347 0.2662 0.7979 0.032 Uiso 1 1 calc R . . C232 C 0.0632(3) 0.1273(2) 0.7153(2) 0.0281(7) Uani 1 1 d . . . C233 C -0.0264(3) 0.1305(2) 0.7578(2) 0.0319(8) Uani 1 1 d . . . H233 H -0.0361 0.1778 0.7905 0.038 Uiso 1 1 calc R . . C234 C -0.1010(4) 0.0631(3) 0.7514(2) 0.0391(9) Uani 1 1 d . . . C235 C -0.0854(4) -0.0068(2) 0.7033(2) 0.0391(9) Uani 1 1 d . . . C236 C 0.0023(4) -0.0080(2) 0.6596(2) 0.0402(9) Uani 1 1 d . . . H236 H 0.0112 -0.0542 0.6255 0.048 Uiso 1 1 calc R . . C237 C 0.0770(3) 0.0600(2) 0.6669(2) 0.0328(8) Uani 1 1 d . . . C238 C -0.1980(4) 0.0648(3) 0.7974(3) 0.0541(12) Uani 1 1 d . . . H23C H -0.1869 0.1117 0.8358 0.081 Uiso 1 1 calc R . . H23D H -0.2002 0.0112 0.8262 0.081 Uiso 1 1 calc R . . H23E H -0.2702 0.0727 0.7603 0.081 Uiso 1 1 calc R . . C239 C -0.1623(4) -0.0832(3) 0.7021(3) 0.0574(13) Uani 1 1 d . . . H23F H -0.1440 -0.1243 0.6630 0.086 Uiso 1 1 calc R . . H23G H -0.2423 -0.0656 0.6874 0.086 Uiso 1 1 calc R . . H23H H -0.1504 -0.1092 0.7553 0.086 Uiso 1 1 calc R . . C240 C 0.2191(4) 0.0211(3) 0.5786(3) 0.0514(11) Uani 1 1 d . . . H24A H 0.2944 0.0412 0.5705 0.077 Uiso 1 1 calc R . . H24B H 0.1660 0.0219 0.5275 0.077 Uiso 1 1 calc R . . H24C H 0.2259 -0.0368 0.5995 0.077 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 0.02111(12) 0.02216(11) 0.02658(12) -0.00413(10) 0.00610(9) 0.00171(10) Fe1 0.0194(2) 0.0323(2) 0.0284(2) 0.0052(2) 0.00486(17) -0.0010(2) Cl11 0.0311(5) 0.0489(5) 0.0334(5) -0.0100(4) -0.0001(4) 0.0133(4) Cl12 0.0354(5) 0.0215(4) 0.0629(6) -0.0052(4) 0.0044(4) 0.0023(4) P1 0.0233(4) 0.0193(4) 0.0243(4) -0.0020(3) 0.0069(3) -0.0008(3) N11 0.0244(15) 0.0206(13) 0.0269(14) -0.0044(10) 0.0076(11) -0.0050(11) N12 0.0258(15) 0.0292(15) 0.0291(15) -0.0086(11) 0.0098(12) -0.0064(12) C1 0.0210(17) 0.0295(18) 0.0301(17) -0.0037(14) 0.0059(13) 0.0003(14) C11 0.0271(18) 0.0273(17) 0.0220(15) 0.0057(12) 0.0058(13) 0.0032(13) C12 0.0232(17) 0.0225(16) 0.0271(16) 0.0001(12) 0.0098(13) -0.0006(13) C13 0.034(2) 0.0291(18) 0.0318(18) 0.0029(14) 0.0141(15) 0.0044(15) C14 0.028(2) 0.042(2) 0.039(2) 0.0111(16) 0.0115(16) 0.0130(16) C15 0.0283(18) 0.038(2) 0.0255(17) 0.0069(14) 0.0057(14) 0.0071(15) C16 0.060(3) 0.025(2) 0.096(4) 0.014(2) 0.043(3) -0.003(2) C17 0.050(3) 0.047(2) 0.049(3) 0.022(2) -0.005(2) -0.019(2) C18 0.084(4) 0.045(3) 0.067(3) 0.016(2) 0.046(3) 0.000(3) C19 0.027(2) 0.086(4) 0.124(5) 0.040(4) 0.018(3) -0.009(2) C20 0.114(5) 0.067(3) 0.046(3) 0.002(2) -0.014(3) -0.065(4) C111 0.0275(16) 0.0269(16) 0.0319(16) -0.0034(15) 0.0090(13) -0.0010(16) C112 0.042(2) 0.036(2) 0.0377(19) -0.0035(17) 0.0043(16) -0.0045(18) C113 0.052(3) 0.067(3) 0.0293(19) -0.0030(19) 0.0015(16) -0.005(2) C114 0.045(3) 0.069(3) 0.053(3) -0.038(2) -0.001(2) -0.002(2) C115 0.109(5) 0.034(3) 0.098(4) -0.026(3) -0.043(4) 0.001(3) C116 0.089(4) 0.029(2) 0.068(3) 0.000(2) -0.031(3) -0.001(2) C121 0.0260(17) 0.0234(16) 0.0278(17) -0.0023(12) 0.0099(13) -0.0032(13) C122 0.088(4) 0.025(2) 0.114(4) -0.004(2) 0.081(4) 0.004(2) C133 0.0339(19) 0.0274(17) 0.0254(17) -0.0026(13) 0.0090(14) -0.0008(14) C123 0.120(6) 0.027(3) 0.218(8) 0.021(4) 0.129(6) 0.014(3) C131 0.0236(16) 0.0197(15) 0.0273(16) -0.0004(12) 0.0092(13) -0.0029(12) C132 0.0286(18) 0.0217(16) 0.0238(16) -0.0007(12) 0.0062(13) -0.0002(13) C134 0.040(2) 0.0255(18) 0.0308(18) -0.0033(14) 0.0075(15) -0.0005(15) C124 0.099(5) 0.026(2) 0.131(5) 0.012(3) 0.084(4) 0.002(3) C125 0.043(2) 0.031(2) 0.045(2) -0.0030(16) 0.0238(18) -0.0040(16) C135 0.040(2) 0.0294(18) 0.0307(18) -0.0020(14) 0.0064(15) -0.0096(16) C126 0.0316(19) 0.0250(17) 0.0338(19) -0.0028(14) 0.0147(15) 0.0021(14) C136 0.036(2) 0.0319(18) 0.0281(18) 0.0001(14) 0.0058(14) -0.0128(15) C137 0.0275(18) 0.0280(17) 0.0252(16) -0.0032(13) 0.0061(13) -0.0020(14) C138 0.068(3) 0.034(2) 0.048(2) -0.0075(17) 0.013(2) -0.022(2) C139 0.068(3) 0.032(2) 0.056(3) -0.0214(19) 0.020(2) -0.009(2) C140 0.028(2) 0.046(2) 0.040(2) -0.0123(17) 0.0163(16) -0.0088(17) Pd2 0.02991(14) 0.03508(14) 0.02795(13) 0.00070(11) 0.01021(10) 0.00760(12) Fe2 0.0358(3) 0.0216(2) 0.0259(2) -0.00535(18) 0.0025(2) 0.0022(2) Cl21 0.0482(6) 0.0434(5) 0.0415(5) 0.0086(4) 0.0165(4) 0.0203(4) Cl22 0.0396(6) 0.0830(9) 0.1234(12) 0.0381(9) 0.0397(7) 0.0158(6) P2 0.0322(5) 0.0270(4) 0.0241(4) -0.0025(3) 0.0079(4) -0.0011(4) N21 0.0296(15) 0.0216(14) 0.0277(14) -0.0046(11) 0.0074(11) 0.0008(12) N22 0.0388(18) 0.0294(16) 0.0332(16) -0.0099(12) 0.0058(13) 0.0027(13) C2 0.034(2) 0.0256(16) 0.0272(17) -0.0017(13) 0.0010(14) 0.0038(15) C21 0.0319(19) 0.0233(16) 0.0234(16) -0.0043(13) 0.0050(13) 0.0003(14) C22 0.0248(18) 0.0244(17) 0.0256(17) -0.0084(13) 0.0009(13) -0.0012(13) C23 0.031(2) 0.033(2) 0.036(2) -0.0094(15) 0.0048(16) 0.0020(15) C24 0.039(2) 0.038(2) 0.036(2) -0.0076(16) -0.0064(16) 0.0124(17) C25 0.045(2) 0.0279(18) 0.0255(17) -0.0003(13) -0.0006(15) 0.0063(16) C26 0.048(3) 0.043(3) 0.056(3) -0.018(2) -0.009(2) 0.003(2) C27 0.073(4) 0.042(3) 0.048(3) -0.016(2) 0.011(2) -0.024(2) C28 0.082(4) 0.0191(19) 0.058(3) -0.0097(18) -0.016(3) 0.002(2) C29 0.053(3) 0.069(3) 0.062(3) -0.049(3) 0.015(2) -0.006(2) C30 0.087(4) 0.035(2) 0.033(2) -0.0057(17) -0.007(2) -0.017(2) C211 0.046(2) 0.0305(19) 0.043(2) -0.0105(16) 0.0223(18) -0.0090(17) C212 0.042(2) 0.049(3) 0.068(3) -0.019(2) 0.019(2) -0.012(2) C213 0.057(3) 0.064(3) 0.114(5) -0.043(3) 0.040(3) -0.032(3) C214 0.099(5) 0.055(3) 0.110(5) -0.026(3) 0.065(4) -0.039(3) C215 0.118(6) 0.052(3) 0.077(4) 0.006(3) 0.050(4) -0.018(3) C216 0.088(4) 0.042(3) 0.049(3) 0.001(2) 0.022(2) -0.022(2) C221 0.0347(19) 0.0248(17) 0.0228(16) 0.0002(12) 0.0079(13) 0.0028(13) C222 0.041(2) 0.0344(19) 0.0313(17) -0.0051(16) 0.0101(14) 0.0039(17) C223 0.057(3) 0.040(2) 0.0341(19) -0.0100(18) 0.0130(17) 0.012(2) C224 0.058(3) 0.035(2) 0.0302(19) -0.0098(15) 0.0001(17) 0.0037(18) C225 0.044(2) 0.055(3) 0.034(2) -0.0118(17) 0.0031(16) -0.0059(19) C226 0.039(2) 0.044(2) 0.0344(19) -0.0091(17) 0.0118(15) -0.0039(18) C231 0.0329(18) 0.0247(17) 0.0225(16) -0.0063(12) 0.0062(13) -0.0045(13) C232 0.0285(18) 0.0224(17) 0.0312(18) -0.0043(13) -0.0011(14) -0.0010(14) C233 0.0309(19) 0.0299(18) 0.0340(18) -0.0070(14) 0.0030(15) -0.0014(15) C234 0.035(2) 0.041(2) 0.038(2) 0.0025(16) -0.0007(16) -0.0070(17) C235 0.039(2) 0.032(2) 0.041(2) -0.0016(16) -0.0063(17) -0.0080(16) C236 0.050(3) 0.0267(19) 0.039(2) -0.0110(16) -0.0045(18) 0.0002(17) C237 0.039(2) 0.0269(18) 0.0310(18) -0.0055(14) 0.0003(15) 0.0008(15) C238 0.047(3) 0.055(3) 0.061(3) -0.006(2) 0.012(2) -0.018(2) C239 0.057(3) 0.050(3) 0.060(3) -0.010(2) -0.003(2) -0.023(2) C240 0.059(3) 0.045(2) 0.051(3) -0.024(2) 0.013(2) 0.009(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.976(3) . ? Pd1 P1 2.2664(8) . ? Pd1 Cl12 2.3406(9) . ? Pd1 Cl11 2.3460(9) . ? Fe1 C12 2.002(3) . ? Fe1 C19 2.011(5) . ? Fe1 C11 2.020(3) . ? Fe1 C17 2.024(4) . ? Fe1 C20 2.025(4) . ? Fe1 C18 2.026(4) . ? Fe1 C15 2.030(3) . ? Fe1 C13 2.035(4) . ? Fe1 C16 2.037(4) . ? Fe1 C14 2.048(4) . ? P1 C11 1.787(3) . ? P1 C121 1.819(3) . ? P1 C111 1.820(3) . ? N11 C1 1.355(4) . ? N11 C132 1.386(4) . ? N11 C131 1.458(4) . ? N12 C1 1.350(4) . ? N12 C137 1.399(4) . ? N12 C140 1.446(4) . ? C11 C15 1.433(5) . ? C11 C12 1.438(4) . ? C12 C13 1.421(5) . ? C12 C131 1.484(5) . ? C13 C14 1.413(5) . ? C14 C15 1.403(5) . ? C16 C17 1.375(7) . ? C16 C20 1.440(8) . ? C17 C18 1.356(7) . ? C18 C19 1.332(8) . ? C19 C20 1.417(9) . ? C111 C116 1.366(6) . ? C111 C112 1.379(5) . ? C112 C113 1.379(5) . ? C113 C114 1.337(7) . ? C114 C115 1.343(8) . ? C115 C116 1.384(7) . ? C121 C122 1.368(5) . ? C121 C126 1.378(4) . ? C122 C123 1.383(7) . ? C133 C134 1.363(5) . ? C133 C132 1.380(5) . ? C123 C124 1.353(7) . ? C132 C137 1.391(5) . ? C134 C135 1.419(5) . ? C134 C139 1.511(5) . ? C124 C125 1.368(6) . ? C125 C126 1.374(5) . ? C135 C136 1.385(5) . ? C135 C138 1.503(5) . ? C136 C137 1.369(5) . ? Pd2 C2 1.975(4) . ? Pd2 P2 2.2475(9) . ? Pd2 Cl22 2.3043(12) . ? Pd2 Cl21 2.3347(10) . ? Fe2 C22 2.015(3) . ? Fe2 C30 2.022(4) . ? Fe2 C29 2.027(4) . ? Fe2 C27 2.027(5) . ? Fe2 C26 2.028(4) . ? Fe2 C23 2.028(4) . ? Fe2 C28 2.031(4) . ? Fe2 C25 2.032(3) . ? Fe2 C21 2.032(3) . ? Fe2 C24 2.041(4) . ? P2 C21 1.789(3) . ? P2 C211 1.811(4) . ? P2 C221 1.815(3) . ? N21 C2 1.344(4) . ? N21 C232 1.392(4) . ? N21 C231 1.457(4) . ? N22 C2 1.349(5) . ? N22 C237 1.397(5) . ? N22 C240 1.458(5) . ? C21 C25 1.435(5) . ? C21 C22 1.441(5) . ? C22 C23 1.407(5) . ? C22 C231 1.483(5) . ? C23 C24 1.415(6) . ? C24 C25 1.417(6) . ? C26 C30 1.364(7) . ? C26 C27 1.382(7) . ? C27 C28 1.383(7) . ? C28 C29 1.397(7) . ? C29 C30 1.418(7) . ? C211 C216 1.386(6) . ? C211 C212 1.387(6) . ? C212 C213 1.382(7) . ? C213 C214 1.349(9) . ? C214 C215 1.388(9) . ? C215 C216 1.376(7) . ? C221 C226 1.370(5) . ? C221 C222 1.396(5) . ? C222 C223 1.373(5) . ? C223 C224 1.358(6) . ? C224 C225 1.363(6) . ? C225 C226 1.398(5) . ? C232 C237 1.372(5) . ? C232 C233 1.387(5) . ? C233 C234 1.377(5) . ? C234 C235 1.405(6) . ? C234 C238 1.500(6) . ? C235 C236 1.378(6) . ? C235 C239 1.512(6) . ? C236 C237 1.385(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 C1 Pd1 P1 85.51(10) . . ? C1 Pd1 Cl12 168.24(10) . . ? P1 Pd1 Cl12 98.73(3) . . ? C1 Pd1 Cl11 88.22(10) . . ? P1 Pd1 Cl11 171.11(4) . . ? Cl12 Pd1 Cl11 88.64(4) . . ? C12 Fe1 C19 157.7(2) . . ? C12 Fe1 C11 41.91(13) . . ? C19 Fe1 C11 159.5(2) . . ? C12 Fe1 C17 104.83(15) . . ? C19 Fe1 C17 65.9(2) . . ? C11 Fe1 C17 127.19(17) . . ? C12 Fe1 C20 156.5(2) . . ? C19 Fe1 C20 41.1(3) . . ? C11 Fe1 C20 124.2(2) . . ? C17 Fe1 C20 67.29(19) . . ? C12 Fe1 C18 121.66(19) . . ? C19 Fe1 C18 38.5(2) . . ? C11 Fe1 C18 161.5(2) . . ? C17 Fe1 C18 39.14(19) . . ? C20 Fe1 C18 67.0(2) . . ? C12 Fe1 C15 70.03(14) . . ? C19 Fe1 C15 123.1(2) . . ? C11 Fe1 C15 41.44(14) . . ? C17 Fe1 C15 167.24(18) . . ? C20 Fe1 C15 112.59(18) . . ? C18 Fe1 C15 153.49(19) . . ? C12 Fe1 C13 41.23(14) . . ? C19 Fe1 C13 122.4(2) . . ? C11 Fe1 C13 69.24(13) . . ? C17 Fe1 C13 115.75(17) . . ? C20 Fe1 C13 162.2(3) . . ? C18 Fe1 C13 103.63(18) . . ? C15 Fe1 C13 68.58(14) . . ? C12 Fe1 C16 118.34(18) . . ? C19 Fe1 C16 68.5(2) . . ? C11 Fe1 C16 110.44(16) . . ? C17 Fe1 C16 39.6(2) . . ? C20 Fe1 C16 41.5(2) . . ? C18 Fe1 C16 67.0(2) . . ? C15 Fe1 C16 131.73(18) . . ? C13 Fe1 C16 150.69(19) . . ? C12 Fe1 C14 69.16(15) . . ? C19 Fe1 C14 108.1(2) . . ? C11 Fe1 C14 68.71(14) . . ? C17 Fe1 C14 150.10(18) . . ? C20 Fe1 C14 128.8(2) . . ? C18 Fe1 C14 117.63(18) . . ? C15 Fe1 C14 40.25(14) . . ? C13 Fe1 C14 40.50(15) . . ? C16 Fe1 C14 168.6(2) . . ? C11 P1 C121 103.18(15) . . ? C11 P1 C111 106.24(15) . . ? C121 P1 C111 100.38(15) . . ? C11 P1 Pd1 113.60(11) . . ? C121 P1 Pd1 108.25(12) . . ? C111 P1 Pd1 122.76(12) . . ? C1 N11 C132 111.1(3) . . ? C1 N11 C131 123.2(3) . . ? C132 N11 C131 125.4(3) . . ? C1 N12 C137 110.1(3) . . ? C1 N12 C140 125.9(3) . . ? C137 N12 C140 123.9(3) . . ? N12 C1 N11 106.5(3) . . ? N12 C1 Pd1 133.5(2) . . ? N11 C1 Pd1 120.0(2) . . ? C15 C11 C12 107.4(3) . . ? C15 C11 P1 127.1(2) . . ? C12 C11 P1 124.9(2) . . ? C15 C11 Fe1 69.67(19) . . ? C12 C11 Fe1 68.38(18) . . ? P1 C11 Fe1 134.17(18) . . ? C13 C12 C11 107.3(3) . . ? C13 C12 C131 126.7(3) . . ? C11 C12 C131 125.8(3) . . ? C13 C12 Fe1 70.6(2) . . ? C11 C12 Fe1 69.71(19) . . ? C131 C12 Fe1 120.9(2) . . ? C14 C13 C12 108.4(3) . . ? C14 C13 Fe1 70.3(2) . . ? C12 C13 Fe1 68.13(19) . . ? C15 C14 C13 108.8(3) . . ? C15 C14 Fe1 69.2(2) . . ? C13 C14 Fe1 69.2(2) . . ? C14 C15 C11 108.1(3) . . ? C14 C15 Fe1 70.6(2) . . ? C11 C15 Fe1 68.89(18) . . ? C17 C16 C20 105.6(5) . . ? C17 C16 Fe1 69.7(3) . . ? C20 C16 Fe1 68.8(3) . . ? C18 C17 C16 110.3(4) . . ? C18 C17 Fe1 70.5(3) . . ? C16 C17 Fe1 70.7(2) . . ? C19 C18 C17 109.5(5) . . ? C19 C18 Fe1 70.1(3) . . ? C17 C18 Fe1 70.3(2) . . ? C18 C19 C20 108.9(5) . . ? C18 C19 Fe1 71.3(3) . . ? C20 C19 Fe1 70.0(3) . . ? C19 C20 C16 105.7(5) . . ? C19 C20 Fe1 68.9(3) . . ? C16 C20 Fe1 69.7(2) . . ? C116 C111 C112 117.5(4) . . ? C116 C111 P1 123.0(3) . . ? C112 C111 P1 119.5(3) . . ? C111 C112 C113 120.8(4) . . ? C114 C113 C112 120.7(4) . . ? C113 C114 C115 119.5(4) . . ? C114 C115 C116 121.0(5) . . ? C111 C116 C115 120.5(4) . . ? C122 C121 C126 118.4(3) . . ? C122 C121 P1 122.4(3) . . ? C126 C121 P1 119.0(2) . . ? C121 C122 C123 120.2(4) . . ? C134 C133 C132 117.7(3) . . ? C124 C123 C122 120.8(5) . . ? N11 C131 C12 112.2(3) . . ? C133 C132 N11 132.5(3) . . ? C133 C132 C137 121.6(3) . . ? N11 C132 C137 105.8(3) . . ? C133 C134 C135 121.0(3) . . ? C133 C134 C139 119.7(3) . . ? C135 C134 C139 119.3(3) . . ? C123 C124 C125 119.6(4) . . ? C124 C125 C126 119.7(4) . . ? C136 C135 C134 120.7(3) . . ? C136 C135 C138 118.7(3) . . ? C134 C135 C138 120.6(3) . . ? C125 C126 C121 121.1(3) . . ? C137 C136 C135 117.6(3) . . ? C136 C137 C132 121.4(3) . . ? C136 C137 N12 132.1(3) . . ? C132 C137 N12 106.5(3) . . ? C2 Pd2 P2 89.94(10) . . ? C2 Pd2 Cl22 174.04(11) . . ? P2 Pd2 Cl22 94.59(4) . . ? C2 Pd2 Cl21 86.66(10) . . ? P2 Pd2 Cl21 175.97(4) . . ? Cl22 Pd2 Cl21 88.66(4) . . ? C22 Fe2 C30 107.87(15) . . ? C22 Fe2 C29 130.67(19) . . ? C30 Fe2 C29 41.0(2) . . ? C22 Fe2 C27 147.96(18) . . ? C30 Fe2 C27 67.29(19) . . ? C29 Fe2 C27 67.6(2) . . ? C22 Fe2 C26 115.99(16) . . ? C30 Fe2 C26 39.4(2) . . ? C29 Fe2 C26 67.27(19) . . ? C27 Fe2 C26 39.86(19) . . ? C22 Fe2 C23 40.73(14) . . ? C30 Fe2 C23 113.93(18) . . ? C29 Fe2 C23 107.21(18) . . ? C27 Fe2 C23 171.26(18) . . ? C26 Fe2 C23 145.99(18) . . ? C22 Fe2 C28 170.1(2) . . ? C30 Fe2 C28 67.71(18) . . ? C29 Fe2 C28 40.3(2) . . ? C27 Fe2 C28 39.8(2) . . ? C26 Fe2 C28 66.72(19) . . ? C23 Fe2 C28 131.77(19) . . ? C22 Fe2 C25 69.73(14) . . ? C30 Fe2 C25 173.17(19) . . ? C29 Fe2 C25 145.33(19) . . ? C27 Fe2 C25 111.12(17) . . ? C26 Fe2 C25 135.29(18) . . ? C23 Fe2 C25 68.73(15) . . ? C28 Fe2 C25 115.69(17) . . ? C22 Fe2 C21 41.72(13) . . ? C30 Fe2 C21 132.74(17) . . ? C29 Fe2 C21 171.6(2) . . ? C27 Fe2 C21 117.04(17) . . ? C26 Fe2 C21 111.32(16) . . ? C23 Fe2 C21 69.03(14) . . ? C28 Fe2 C21 147.64(19) . . ? C25 Fe2 C21 41.37(14) . . ? C22 Fe2 C24 69.03(15) . . ? C30 Fe2 C24 145.1(2) . . ? C29 Fe2 C24 113.36(19) . . ? C27 Fe2 C24 133.65(19) . . ? C26 Fe2 C24 173.30(19) . . ? C23 Fe2 C24 40.69(16) . . ? C28 Fe2 C24 109.15(18) . . ? C25 Fe2 C24 40.73(15) . . ? C21 Fe2 C24 69.07(14) . . ? C21 P2 C211 104.33(17) . . ? C21 P2 C221 103.33(16) . . ? C211 P2 C221 105.79(17) . . ? C21 P2 Pd2 117.66(12) . . ? C211 P2 Pd2 120.54(15) . . ? C221 P2 Pd2 103.28(11) . . ? C2 N21 C232 110.7(3) . . ? C2 N21 C231 122.5(3) . . ? C232 N21 C231 126.6(3) . . ? C2 N22 C237 110.2(3) . . ? C2 N22 C240 125.8(3) . . ? C237 N22 C240 124.0(3) . . ? N21 C2 N22 106.4(3) . . ? N21 C2 Pd2 126.5(3) . . ? N22 C2 Pd2 126.5(3) . . ? C25 C21 C22 107.1(3) . . ? C25 C21 P2 124.9(3) . . ? C22 C21 P2 127.5(3) . . ? C25 C21 Fe2 69.28(19) . . ? C22 C21 Fe2 68.50(18) . . ? P2 C21 Fe2 133.8(2) . . ? C23 C22 C21 107.7(3) . . ? C23 C22 C231 126.8(3) . . ? C21 C22 C231 125.4(3) . . ? C23 C22 Fe2 70.1(2) . . ? C21 C22 Fe2 69.78(19) . . ? C231 C22 Fe2 124.4(2) . . ? C22 C23 C24 109.1(3) . . ? C22 C23 Fe2 69.2(2) . . ? C24 C23 Fe2 70.1(2) . . ? C23 C24 C25 108.0(3) . . ? C23 C24 Fe2 69.2(2) . . ? C25 C24 Fe2 69.3(2) . . ? C24 C25 C21 108.1(3) . . ? C24 C25 Fe2 70.0(2) . . ? C21 C25 Fe2 69.35(19) . . ? C30 C26 C27 109.5(4) . . ? C30 C26 Fe2 70.1(3) . . ? C27 C26 Fe2 70.0(3) . . ? C26 C27 C28 107.7(4) . . ? C26 C27 Fe2 70.1(3) . . ? C28 C27 Fe2 70.2(3) . . ? C27 C28 C29 108.5(4) . . ? C27 C28 Fe2 69.9(2) . . ? C29 C28 Fe2 69.7(2) . . ? C28 C29 C30 106.7(4) . . ? C28 C29 Fe2 70.0(2) . . ? C30 C29 Fe2 69.3(2) . . ? C26 C30 C29 107.6(4) . . ? C26 C30 Fe2 70.6(3) . . ? C29 C30 Fe2 69.7(2) . . ? C216 C211 C212 118.5(4) . . ? C216 C211 P2 121.0(3) . . ? C212 C211 P2 120.4(3) . . ? C213 C212 C211 120.3(5) . . ? C214 C213 C212 120.7(6) . . ? C213 C214 C215 120.1(5) . . ? C216 C215 C214 119.7(6) . . ? C215 C216 C211 120.7(5) . . ? C226 C221 C222 119.5(3) . . ? C226 C221 P2 121.0(3) . . ? C222 C221 P2 119.1(3) . . ? C223 C222 C221 119.4(4) . . ? C224 C223 C222 120.8(3) . . ? C223 C224 C225 120.7(4) . . ? C224 C225 C226 119.5(4) . . ? C221 C226 C225 120.0(3) . . ? N21 C231 C22 111.1(3) . . ? C237 C232 C233 121.5(3) . . ? C237 C232 N21 106.2(3) . . ? C233 C232 N21 132.2(3) . . ? C234 C233 C232 118.2(3) . . ? C233 C234 C235 120.3(4) . . ? C233 C234 C238 119.1(4) . . ? C235 C234 C238 120.6(4) . . ? C236 C235 C234 120.8(4) . . ? C236 C235 C239 119.6(4) . . ? C234 C235 C239 119.6(4) . . ? C235 C236 C237 118.3(3) . . ? C232 C237 C236 120.9(4) . . ? C232 C237 N22 106.4(3) . . ? C236 C237 N22 132.6(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.454 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.067 #====END # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.210 0.748 0.475 136 19 ' ' 3 0.789 0.248 0.525 135 19 ' ' _platon_squeeze_details ; Some residual electron density were difficult to modelize and therefore, the SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution of the electron density in the solvent region from the intensity data, and the solvent-free model was employed for the final refinement. There are two cavities of 136 \%A^3^ per unitl cell. PLATON estimated that each cavity contains 19 electrons which may correspond to one acetone molecule (CH~3~)~2~CO by unit cell, as suggested by the crystallization process. ; _database_code_depnum_ccdc_archive 'CCDC 940120' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4d-rac _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H41 Cl2 Fe N2 P Pd, 0.5(C H4 O)' _chemical_formula_sum 'C42.50 H43 Cl2 Fe N2 O0.50 P Pd' _chemical_formula_weight 853.91 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' Fe Fe 0.3463 0.8444 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6863(8) _cell_length_b 13.7235(9) _cell_length_c 13.9621(9) _cell_angle_alpha 75.975(6) _cell_angle_beta 77.655(6) _cell_angle_gamma 70.728(6) _cell_volume 1855.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3579 _cell_measurement_theta_min 3.6836 _cell_measurement_theta_max 29.1602 _exptl_crystal_description box _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 1.098 _exptl_absorpt_correction_T_min 0.80789 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. CrysAlisPro (Agilent Technologies) ; _exptl_special_details ? _diffrn_ambient_temperature 180(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 'Xcalibur, Eos, Gemini ultra' _diffrn_detector_area_resol_mean 16.1978 _diffrn_measurement_method '\w scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11701 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.1106 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5892 _reflns_number_gt 4205 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2012)' _computing_cell_refinement CrysAlisPro _computing_data_reduction CrysAlisPro _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996); ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0493P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5892 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.59972(5) 0.69726(4) 0.30669(4) 0.01991(16) Uani 1 1 d . . . Cl1 Cl 0.78713(15) 0.60647(13) 0.39179(11) 0.0263(4) Uani 1 1 d . . . Cl2 Cl 0.63440(17) 0.85885(13) 0.29883(13) 0.0343(4) Uani 1 1 d . . . P1 P 0.40725(16) 0.77335(13) 0.24104(12) 0.0209(4) Uani 1 1 d . . . Fe1 Fe 0.11750(9) 0.72213(7) 0.39197(7) 0.0238(3) Uani 1 1 d . . . N1 N 0.5159(5) 0.5009(4) 0.3583(4) 0.0191(12) Uani 1 1 d . . . N2 N 0.6942(5) 0.4874(4) 0.2482(4) 0.0194(12) Uani 1 1 d . . . C1 C 0.5983(6) 0.5543(5) 0.3001(4) 0.0208(15) Uani 1 1 d . . . C2 C 0.5572(6) 0.3979(5) 0.3453(4) 0.0224(15) Uani 1 1 d . . . C3 C 0.6729(6) 0.3866(5) 0.2753(4) 0.0192(14) Uani 1 1 d . . . C4 C 0.7441(6) 0.2882(5) 0.2499(5) 0.0243(15) Uani 1 1 d . . . H4 H 0.8244 0.2792 0.2035 0.029 Uiso 1 1 calc R . . C5 C 0.6932(7) 0.2038(5) 0.2953(5) 0.0297(17) Uani 1 1 d . . . C6 C 0.5735(7) 0.2168(5) 0.3645(5) 0.0294(17) Uani 1 1 d . . . C7 C 0.5071(6) 0.3134(5) 0.3895(4) 0.0215(15) Uani 1 1 d . . . H7 H 0.4275 0.3225 0.4366 0.026 Uiso 1 1 calc R . . C11 C 0.2801(6) 0.7061(5) 0.2816(4) 0.0232(15) Uani 1 1 d . . . C12 C 0.2842(6) 0.6100(5) 0.3518(4) 0.0213(15) Uani 1 1 d . . . C13 C 0.1681(6) 0.5822(6) 0.3487(5) 0.0293(17) Uani 1 1 d . . . H13 H 0.1464 0.5207 0.3859 0.035 Uiso 1 1 calc R . . C14 C 0.0918(7) 0.6600(6) 0.2822(5) 0.0301(17) Uani 1 1 d . . . H14 H 0.0090 0.6606 0.2669 0.036 Uiso 1 1 calc R . . C15 C 0.1572(6) 0.7369(5) 0.2418(4) 0.0221(15) Uani 1 1 d . . . H15 H 0.1254 0.7993 0.1954 0.027 Uiso 1 1 calc R . . C16 C 0.0899(7) 0.7066(6) 0.5436(5) 0.0348(18) Uani 1 1 d . . . H16 H 0.1390 0.6495 0.5878 0.042 Uiso 1 1 calc R . . C17 C 0.1230(7) 0.8008(6) 0.4981(5) 0.039(2) Uani 1 1 d . . . H17 H 0.1974 0.8194 0.5069 0.047 Uiso 1 1 calc R . . C18 C 0.0233(7) 0.8624(5) 0.4366(5) 0.0281(16) Uani 1 1 d . . . H18 H 0.0212 0.9292 0.3960 0.034 Uiso 1 1 calc R . . C19 C -0.0697(7) 0.8099(6) 0.4452(5) 0.0374(19) Uani 1 1 d . . . H19 H -0.1467 0.8345 0.4125 0.045 Uiso 1 1 calc R . . C20 C -0.0306(7) 0.7134(6) 0.5110(5) 0.0355(18) Uani 1 1 d . . . H20 H -0.0767 0.6616 0.5303 0.043 Uiso 1 1 calc R . . C21 C 0.3897(6) 0.5530(5) 0.4172(5) 0.0242(15) Uani 1 1 d . . . H21A H 0.4057 0.6032 0.4500 0.029 Uiso 1 1 calc R . . H21B H 0.3586 0.4998 0.4698 0.029 Uiso 1 1 calc R . . C22 C 0.8038(7) 0.5219(5) 0.1764(5) 0.0319(17) Uani 1 1 d . . . H22A H 0.7633 0.5895 0.1336 0.038 Uiso 1 1 calc R . . H22B H 0.8630 0.5349 0.2146 0.038 Uiso 1 1 calc R . . C23 C 0.8874(6) 0.4457(5) 0.1109(4) 0.0225(15) Uani 1 1 d . . . C24 C 0.8338(6) 0.4330(5) 0.0329(5) 0.0279(16) Uani 1 1 d . . . C25 C 0.9093(6) 0.3595(5) -0.0257(5) 0.0282(16) Uani 1 1 d . . . H25 H 0.8715 0.3503 -0.0775 0.034 Uiso 1 1 calc R . . C26 C 1.0386(7) 0.2989(5) -0.0109(5) 0.0295(17) Uani 1 1 d . . . C27 C 1.0916(6) 0.3155(5) 0.0648(5) 0.0277(16) Uani 1 1 d . . . H27 H 1.1809 0.2761 0.0747 0.033 Uiso 1 1 calc R . . C28 C 1.0185(6) 0.3875(5) 0.1263(5) 0.0267(16) Uani 1 1 d . . . C51 C 0.7702(7) 0.0972(5) 0.2711(6) 0.044(2) Uani 1 1 d . . . H51A H 0.8490 0.1025 0.2215 0.066 Uiso 1 1 calc R . . H51B H 0.7128 0.0709 0.2440 0.066 Uiso 1 1 calc R . . H51C H 0.7989 0.0487 0.3319 0.066 Uiso 1 1 calc R . . C61 C 0.5214(7) 0.1237(5) 0.4142(5) 0.0378(19) Uani 1 1 d . . . H61A H 0.4412 0.1459 0.4624 0.057 Uiso 1 1 calc R . . H61B H 0.5906 0.0685 0.4489 0.057 Uiso 1 1 calc R . . H61C H 0.4989 0.0965 0.3635 0.057 Uiso 1 1 calc R . . C111 C 0.4429(6) 0.7828(5) 0.1066(5) 0.0224(15) Uani 1 1 d . . . C112 C 0.4034(6) 0.7254(5) 0.0561(5) 0.0317(17) Uani 1 1 d . . . H112 H 0.3561 0.6770 0.0925 0.038 Uiso 1 1 calc R . . C113 C 0.4323(7) 0.7376(6) -0.0472(5) 0.042(2) Uani 1 1 d . . . H113 H 0.4034 0.6985 -0.0811 0.050 Uiso 1 1 calc R . . C114 C 0.5025(7) 0.8062(6) -0.1006(5) 0.043(2) Uani 1 1 d . . . H114 H 0.5236 0.8136 -0.1712 0.052 Uiso 1 1 calc R . . C115 C 0.5417(7) 0.8634(6) -0.0518(5) 0.041(2) Uani 1 1 d . . . H115 H 0.5878 0.9124 -0.0887 0.049 Uiso 1 1 calc R . . C116 C 0.5151(7) 0.8507(6) 0.0510(5) 0.0377(19) Uani 1 1 d . . . H116 H 0.5465 0.8889 0.0842 0.045 Uiso 1 1 calc R . . C121 C 0.3133(6) 0.9070(5) 0.2570(5) 0.0281(17) Uani 1 1 d . . . C122 C 0.3158(7) 0.9425(6) 0.3421(5) 0.0362(19) Uani 1 1 d . . . H122 H 0.3740 0.9002 0.3889 0.043 Uiso 1 1 calc R . . C123 C 0.2309(8) 1.0415(7) 0.3570(7) 0.049(2) Uani 1 1 d . . . H123 H 0.2328 1.0668 0.4141 0.059 Uiso 1 1 calc R . . C124 C 0.1463(8) 1.1018(6) 0.2919(7) 0.054(2) Uani 1 1 d . . . H124 H 0.0875 1.1678 0.3047 0.064 Uiso 1 1 calc R . . C125 C 0.1447(7) 1.0680(6) 0.2075(7) 0.051(2) Uani 1 1 d . . . H125 H 0.0853 1.1112 0.1618 0.061 Uiso 1 1 calc R . . C126 C 0.2285(7) 0.9720(6) 0.1885(6) 0.0367(18) Uani 1 1 d . . . H126 H 0.2287 0.9500 0.1290 0.044 Uiso 1 1 calc R . . C241 C 0.6963(7) 0.4992(6) 0.0110(5) 0.0382(19) Uani 1 1 d . . . H24A H 0.6291 0.4807 0.0660 0.057 Uiso 1 1 calc R . . H24B H 0.6808 0.4864 -0.0510 0.057 Uiso 1 1 calc R . . H24C H 0.6893 0.5736 0.0035 0.057 Uiso 1 1 calc R . . C261 C 1.1186(7) 0.2167(6) -0.0726(5) 0.0373(18) Uani 1 1 d . . . H26A H 1.1882 0.1645 -0.0360 0.056 Uiso 1 1 calc R . . H26B H 1.1607 0.2501 -0.1358 0.056 Uiso 1 1 calc R . . H26C H 1.0591 0.1821 -0.0861 0.056 Uiso 1 1 calc R . . C281 C 1.0841(7) 0.4005(5) 0.2065(5) 0.0325(17) Uani 1 1 d . . . H28A H 1.1730 0.3491 0.2079 0.049 Uiso 1 1 calc R . . H28B H 1.0287 0.3892 0.2715 0.049 Uiso 1 1 calc R . . H28C H 1.0929 0.4717 0.1921 0.049 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 0.0200(3) 0.0196(3) 0.0218(3) -0.0054(2) 0.0002(2) -0.0089(2) Cl1 0.0214(9) 0.0334(10) 0.0254(9) -0.0015(8) -0.0037(7) -0.0122(8) Cl2 0.0331(10) 0.0261(10) 0.0485(11) -0.0127(9) -0.0009(8) -0.0143(8) P1 0.0221(10) 0.0215(10) 0.0192(9) -0.0041(8) 0.0010(7) -0.0087(8) Fe1 0.0210(5) 0.0309(6) 0.0200(5) -0.0055(4) 0.0007(4) -0.0099(4) N1 0.014(3) 0.020(3) 0.021(3) -0.003(2) 0.005(2) -0.007(2) N2 0.018(3) 0.017(3) 0.025(3) -0.005(2) 0.003(2) -0.010(2) C1 0.016(4) 0.031(4) 0.019(3) -0.008(3) -0.001(3) -0.011(3) C2 0.023(4) 0.025(4) 0.021(4) -0.004(3) -0.006(3) -0.008(3) C3 0.024(4) 0.020(4) 0.016(3) -0.001(3) -0.004(3) -0.010(3) C4 0.022(4) 0.029(4) 0.024(4) -0.007(3) -0.001(3) -0.010(3) C5 0.032(4) 0.025(4) 0.034(4) -0.002(3) -0.012(3) -0.010(3) C6 0.040(4) 0.025(4) 0.031(4) -0.005(3) -0.010(3) -0.017(3) C7 0.024(4) 0.026(4) 0.016(3) 0.000(3) -0.003(3) -0.013(3) C11 0.025(4) 0.023(4) 0.018(4) -0.006(3) 0.002(3) -0.005(3) C12 0.022(4) 0.022(4) 0.018(3) 0.000(3) -0.001(3) -0.008(3) C13 0.034(4) 0.040(5) 0.025(4) -0.014(4) 0.006(3) -0.025(4) C14 0.027(4) 0.050(5) 0.022(4) -0.013(4) 0.001(3) -0.020(4) C15 0.021(4) 0.025(4) 0.020(4) 0.001(3) -0.009(3) -0.006(3) C16 0.037(4) 0.051(5) 0.013(4) -0.008(3) 0.003(3) -0.012(4) C17 0.037(5) 0.061(6) 0.031(4) -0.028(4) 0.010(4) -0.023(4) C18 0.028(4) 0.024(4) 0.021(4) -0.004(3) 0.002(3) 0.004(3) C19 0.020(4) 0.061(6) 0.028(4) -0.021(4) 0.003(3) -0.001(4) C20 0.031(4) 0.052(5) 0.025(4) -0.011(4) 0.009(3) -0.020(4) C21 0.019(4) 0.024(4) 0.024(4) -0.001(3) 0.003(3) -0.006(3) C22 0.039(4) 0.030(4) 0.025(4) -0.005(3) 0.011(3) -0.019(3) C23 0.020(4) 0.023(4) 0.018(3) 0.003(3) 0.004(3) -0.006(3) C24 0.023(4) 0.029(4) 0.027(4) -0.002(3) 0.001(3) -0.008(3) C25 0.029(4) 0.030(4) 0.026(4) -0.005(3) 0.000(3) -0.011(3) C26 0.030(4) 0.030(4) 0.025(4) -0.003(3) 0.005(3) -0.011(3) C27 0.023(4) 0.018(4) 0.035(4) 0.002(3) -0.001(3) -0.004(3) C28 0.026(4) 0.029(4) 0.024(4) -0.002(3) 0.004(3) -0.013(3) C51 0.042(5) 0.022(4) 0.063(5) -0.009(4) 0.003(4) -0.009(3) C61 0.056(5) 0.036(5) 0.031(4) -0.002(3) -0.001(4) -0.032(4) C111 0.019(4) 0.019(4) 0.024(4) -0.001(3) -0.001(3) -0.002(3) C112 0.027(4) 0.040(5) 0.029(4) -0.010(4) 0.002(3) -0.012(3) C113 0.043(5) 0.058(6) 0.029(4) -0.017(4) -0.004(4) -0.017(4) C114 0.034(5) 0.066(6) 0.017(4) 0.002(4) -0.004(3) -0.002(4) C115 0.034(5) 0.045(5) 0.034(5) 0.006(4) 0.011(4) -0.017(4) C116 0.033(4) 0.037(5) 0.046(5) -0.011(4) 0.006(4) -0.019(4) C121 0.024(4) 0.019(4) 0.037(4) -0.005(3) 0.008(3) -0.008(3) C122 0.030(4) 0.039(5) 0.046(5) -0.018(4) -0.003(4) -0.012(4) C123 0.044(5) 0.042(5) 0.068(6) -0.036(5) 0.015(5) -0.017(4) C124 0.038(5) 0.023(5) 0.083(7) -0.014(5) 0.021(5) -0.002(4) C125 0.035(5) 0.032(5) 0.061(6) 0.012(5) 0.001(4) 0.003(4) C126 0.035(4) 0.031(4) 0.042(5) -0.003(4) 0.002(4) -0.014(4) C241 0.035(4) 0.038(5) 0.042(5) -0.008(4) -0.004(4) -0.012(4) C261 0.039(4) 0.037(5) 0.030(4) -0.010(4) -0.001(3) -0.002(4) C281 0.032(4) 0.033(4) 0.030(4) -0.001(3) -0.004(3) -0.012(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.992(6) . ? Pd1 P1 2.2551(18) . ? Pd1 Cl2 2.3398(16) . ? Pd1 Cl1 2.3724(17) . ? P1 C11 1.807(6) . ? P1 C111 1.815(6) . ? P1 C121 1.820(6) . ? Fe1 C12 2.010(6) . ? Fe1 C15 2.022(6) . ? Fe1 C13 2.020(6) . ? Fe1 C14 2.030(6) . ? Fe1 C18 2.035(6) . ? Fe1 C16 2.043(6) . ? Fe1 C20 2.046(6) . ? Fe1 C11 2.051(6) . ? Fe1 C17 2.054(6) . ? Fe1 C19 2.052(7) . ? N1 C1 1.344(7) . ? N1 C2 1.379(7) . ? N1 C21 1.476(7) . ? N2 C1 1.342(7) . ? N2 C3 1.424(7) . ? N2 C22 1.495(7) . ? C2 C7 1.392(8) . ? C2 C3 1.392(8) . ? C3 C4 1.402(8) . ? C4 C5 1.397(8) . ? C5 C6 1.417(9) . ? C5 C51 1.502(9) . ? C6 C7 1.370(8) . ? C6 C61 1.515(8) . ? C11 C15 1.430(8) . ? C11 C12 1.433(8) . ? C12 C13 1.424(8) . ? C12 C21 1.492(8) . ? C13 C14 1.391(9) . ? C14 C15 1.397(8) . ? C16 C17 1.417(10) . ? C16 C20 1.423(9) . ? C17 C18 1.426(10) . ? C18 C19 1.378(9) . ? C19 C20 1.407(10) . ? C22 C23 1.492(8) . ? C23 C24 1.403(8) . ? C23 C28 1.398(9) . ? C24 C25 1.385(8) . ? C24 C241 1.501(9) . ? C25 C26 1.387(9) . ? C26 C27 1.394(9) . ? C26 C261 1.505(8) . ? C27 C28 1.393(8) . ? C28 C281 1.514(8) . ? C111 C112 1.383(8) . ? C111 C116 1.390(8) . ? C112 C113 1.390(9) . ? C113 C114 1.375(10) . ? C114 C115 1.362(10) . ? C115 C116 1.381(9) . ? C121 C126 1.399(10) . ? C121 C122 1.396(9) . ? C122 C123 1.398(9) . ? C123 C124 1.349(11) . ? C124 C125 1.373(11) . ? C125 C126 1.377(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 91.92(18) . . ? C1 Pd1 Cl2 170.99(17) . . ? P1 Pd1 Cl2 92.92(6) . . ? C1 Pd1 Cl1 84.74(18) . . ? P1 Pd1 Cl1 173.08(6) . . ? Cl2 Pd1 Cl1 91.22(6) . . ? C11 P1 C111 105.0(3) . . ? C11 P1 C121 102.4(3) . . ? C111 P1 C121 103.7(3) . . ? C11 P1 Pd1 116.8(2) . . ? C111 P1 Pd1 109.4(2) . . ? C121 P1 Pd1 118.1(2) . . ? C12 Fe1 C15 69.4(2) . . ? C12 Fe1 C13 41.4(2) . . ? C15 Fe1 C13 68.1(3) . . ? C12 Fe1 C14 69.1(3) . . ? C15 Fe1 C14 40.3(2) . . ? C13 Fe1 C14 40.2(3) . . ? C12 Fe1 C18 151.7(3) . . ? C15 Fe1 C18 112.6(3) . . ? C13 Fe1 C18 167.0(3) . . ? C14 Fe1 C18 132.0(3) . . ? C12 Fe1 C16 108.2(3) . . ? C15 Fe1 C16 176.3(3) . . ? C13 Fe1 C16 112.1(3) . . ? C14 Fe1 C16 142.0(3) . . ? C18 Fe1 C16 68.1(3) . . ? C12 Fe1 C20 129.5(3) . . ? C15 Fe1 C20 142.9(3) . . ? C13 Fe1 C20 104.1(3) . . ? C14 Fe1 C20 110.2(3) . . ? C18 Fe1 C20 67.1(3) . . ? C16 Fe1 C20 40.7(3) . . ? C12 Fe1 C11 41.3(2) . . ? C15 Fe1 C11 41.1(2) . . ? C13 Fe1 C11 68.8(2) . . ? C14 Fe1 C11 68.5(2) . . ? C18 Fe1 C11 120.9(3) . . ? C16 Fe1 C11 135.3(3) . . ? C20 Fe1 C11 170.8(3) . . ? C12 Fe1 C17 117.8(3) . . ? C15 Fe1 C17 137.8(3) . . ? C13 Fe1 C17 146.6(3) . . ? C14 Fe1 C17 172.7(3) . . ? C18 Fe1 C17 40.8(3) . . ? C16 Fe1 C17 40.5(3) . . ? C20 Fe1 C17 67.8(3) . . ? C11 Fe1 C17 114.6(3) . . ? C12 Fe1 C19 167.6(3) . . ? C15 Fe1 C19 114.8(3) . . ? C13 Fe1 C19 127.8(3) . . ? C14 Fe1 C19 106.1(3) . . ? C18 Fe1 C19 39.4(3) . . ? C16 Fe1 C19 68.2(3) . . ? C20 Fe1 C19 40.2(3) . . ? C11 Fe1 C19 148.9(3) . . ? C17 Fe1 C19 67.7(3) . . ? C1 N1 C2 111.1(5) . . ? C1 N1 C21 122.1(5) . . ? C2 N1 C21 126.3(5) . . ? C1 N2 C3 109.6(5) . . ? C1 N2 C22 121.1(5) . . ? C3 N2 C22 129.3(5) . . ? N2 C1 N1 107.3(5) . . ? N2 C1 Pd1 125.1(4) . . ? N1 C1 Pd1 126.6(4) . . ? N1 C2 C7 132.2(6) . . ? N1 C2 C3 106.5(5) . . ? C7 C2 C3 121.2(6) . . ? C2 C3 C4 120.4(5) . . ? C2 C3 N2 105.5(5) . . ? C4 C3 N2 134.1(5) . . ? C5 C4 C3 117.8(6) . . ? C4 C5 C6 121.3(6) . . ? C4 C5 C51 118.5(6) . . ? C6 C5 C51 120.2(6) . . ? C7 C6 C5 119.8(6) . . ? C7 C6 C61 119.8(6) . . ? C5 C6 C61 120.4(6) . . ? C6 C7 C2 119.5(6) . . ? C15 C11 C12 106.6(5) . . ? C15 C11 P1 124.8(5) . . ? C12 C11 P1 128.5(5) . . ? C15 C11 Fe1 68.4(3) . . ? C12 C11 Fe1 67.8(3) . . ? P1 C11 Fe1 132.2(3) . . ? C13 C12 C11 107.2(6) . . ? C13 C12 C21 127.4(6) . . ? C11 C12 C21 125.4(5) . . ? C13 C12 Fe1 69.7(4) . . ? C11 C12 Fe1 70.9(3) . . ? C21 C12 Fe1 123.3(4) . . ? C14 C13 C12 108.9(6) . . ? C14 C13 Fe1 70.3(4) . . ? C12 C13 Fe1 68.9(3) . . ? C13 C14 C15 108.5(6) . . ? C13 C14 Fe1 69.5(4) . . ? C15 C14 Fe1 69.5(3) . . ? C14 C15 C11 108.8(6) . . ? C14 C15 Fe1 70.1(4) . . ? C11 C15 Fe1 70.5(3) . . ? C17 C16 C20 107.3(7) . . ? C17 C16 Fe1 70.2(4) . . ? C20 C16 Fe1 69.7(4) . . ? C16 C17 C18 106.8(6) . . ? C16 C17 Fe1 69.3(4) . . ? C18 C17 Fe1 68.8(4) . . ? C19 C18 C17 109.4(7) . . ? C19 C18 Fe1 71.0(4) . . ? C17 C18 Fe1 70.3(4) . . ? C18 C19 C20 108.0(6) . . ? C18 C19 Fe1 69.6(4) . . ? C20 C19 Fe1 69.7(4) . . ? C19 C20 C16 108.4(6) . . ? C19 C20 Fe1 70.2(4) . . ? C16 C20 Fe1 69.5(4) . . ? N1 C21 C12 110.7(5) . . ? C23 C22 N2 114.7(5) . . ? C24 C23 C28 119.9(6) . . ? C24 C23 C22 119.5(6) . . ? C28 C23 C22 120.6(6) . . ? C25 C24 C23 119.7(6) . . ? C25 C24 C241 119.4(6) . . ? C23 C24 C241 120.9(6) . . ? C26 C25 C24 121.7(6) . . ? C25 C26 C27 117.6(6) . . ? C25 C26 C261 121.5(6) . . ? C27 C26 C261 120.9(6) . . ? C26 C27 C28 122.5(6) . . ? C27 C28 C23 118.5(6) . . ? C27 C28 C281 119.0(6) . . ? C23 C28 C281 122.6(6) . . ? C112 C111 C116 117.9(6) . . ? C112 C111 P1 123.6(5) . . ? C116 C111 P1 118.4(5) . . ? C111 C112 C113 120.7(6) . . ? C114 C113 C112 120.3(6) . . ? C115 C114 C113 119.6(7) . . ? C114 C115 C116 120.5(7) . . ? C115 C116 C111 120.9(6) . . ? C126 C121 C122 119.3(6) . . ? C126 C121 P1 120.0(5) . . ? C122 C121 P1 120.4(6) . . ? C121 C122 C123 118.7(7) . . ? C124 C123 C122 121.3(7) . . ? C123 C124 C125 120.3(7) . . ? C124 C125 C126 120.5(8) . . ? C125 C126 C121 119.9(7) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.621 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.116 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 79 19 ' ' _platon_squeeze_details ; Some residual electron density were difficult to modelize and therefore, the SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution of the electron density in the solvent region from the intensity data, and the solvent-free model was employed for the final refinement. There are one cavity around the origin of 79 \%A^3^. PLATON estimated that the cavity contains 19 electrons which may correspond to a molecule of methanol CH~3~OH as suggested by the crystallization process ; #====END _vrf_PLAT761_4d-rac ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.900 RESPONSE: The strategy used to define the parameters of the data collection was not correct, but the error has been detected after the crystal has been removed from the goniometer head. As the structure is correct, we kept the data as they were. The value is low but still acceptable. ; _database_code_depnum_ccdc_archive 'CCDC 940121'