# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 ####################################################################### # # 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_compound4 _database_code_depnum_ccdc_archive 'CCDC 763269' #TrackingRef '- combined CIFS.cif' _audit_creation_date 08-11-27 _audit_creation_method CRYSTALS_ver_12.85 _audit_update_record ; 2008-11-28 - Report on C40 H29 F4 Fe I P2 Pd by Anthony C. Willis for Gopa Kar and Martin Bennett 2008-11-24 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title '11271621 ben0705' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.9111(7) _cell_length_b 17.6801(8) _cell_length_c 15.0706(6) _cell_angle_alpha 90 _cell_angle_beta 115.165(3) _cell_angle_gamma 90 _cell_volume 3596.0(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1 ' _symmetry_space_group_name_Hall -P2yab 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 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H29 F4 Fe1 I1 P2 Pd1 # Dc = 1.73 Fooo = 1840.00 Mu = 19.00 M = 936.76 # Found Formula = C40 H29 F4 Fe1 I1 P2 Pd1 # Dc = 1.73 FOOO = 1840.00 Mu = 19.00 M = 936.76 _chemical_formula_sum 'C40 H29 F4 Fe I P2 Pd' _chemical_formula_moiety 'C40 H29 F4 Fe I P2 Pd' _chemical_compound_source 'from RMITU' _chemical_formula_weight 936.76 _cell_measurement_reflns_used 302704 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25 _cell_measurement_temperature 200 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 1.900 # Sheldrick geometric approximatio 0.71 0.93 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.160 -1 0 0 0.180 0 1 0 0.060 0 -1 0 0.120 0 0 1 0.001 0 0 -1 0.035 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; #_diffrn_reflns_av_R_equivalents 0.082 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 0.5 deg at rate 55 sec/frame, crystal-detector distance 32mm, multiple scan sets so over 95 percent of data collected with 4-fold redundancy or more. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 40041 _reflns_number_total 6366 _diffrn_reflns_av_R_equivalents 0.123 # Number of reflections with Friedels Law is 6366 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6446 _diffrn_reflns_theta_min 2.740 _diffrn_reflns_theta_max 25.158 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.158 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 3.16 _oxford_diffrn_Wilson_scale 52.29 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.36 _refine_diff_density_max 1.56 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 6339 _refine_ls_number_restraints 0 _refine_ls_number_parameters 443 _oxford_refine_ls_R_factor_ref 0.1078 _refine_ls_wR_factor_ref 0.1778 _refine_ls_goodness_of_fit_ref 0.9123 _refine_ls_shift/su_max 0.000264 # The values computed from all data _oxford_reflns_number_all 6339 _refine_ls_R_factor_all 0.1078 _refine_ls_wR_factor_all 0.1778 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3747 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_gt 0.1543 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; #============================================================================== # 4. TEXT 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.62227(6) 0.30565(4) 0.29051(7) 0.0585 1.0000 Uani . . . . . . . Pd1 Pd 0.58766(6) 0.45106(4) 0.26394(6) 0.0366 1.0000 Uani . . . . . . . Fe1 Fe 0.85822(12) 0.43703(10) 0.17660(12) 0.0469 1.0000 Uani . . . . . . . P1 P 0.5195(2) 0.56716(14) 0.2574(2) 0.0386 1.0000 Uani . . . . . . . P2 P 0.7574(2) 0.47676(14) 0.3437(2) 0.0377 1.0000 Uani . . . . . . . F3 F 0.3746(6) 0.3175(4) 0.1564(6) 0.0745 1.0000 Uani . . . . . . . F4 F 0.1908(6) 0.3563(5) 0.1185(7) 0.0865 1.0000 Uani . . . . . . . F5 F 0.1425(5) 0.4986(5) 0.1434(5) 0.0719 1.0000 Uani . . . . . . . F6 F 0.2821(5) 0.6095(4) 0.2019(5) 0.0621 1.0000 Uani . . . . . . . C1 C 0.4046(8) 0.5176(6) 0.2173(7) 0.0393 1.0000 Uani . . . . . . . C2 C 0.4375(7) 0.4437(5) 0.2083(9) 0.0413 1.0000 Uani . . . . . . . C3 C 0.3597(10) 0.3901(7) 0.1730(9) 0.0574 1.0000 Uani . . . . . . . C4 C 0.2618(9) 0.4112(8) 0.1537(9) 0.0549 1.0000 Uani . . . . . . . C5 C 0.2371(9) 0.4826(8) 0.1631(9) 0.0572 1.0000 Uani . . . . . . . C6 C 0.3082(8) 0.5371(7) 0.1933(8) 0.0474 1.0000 Uani . . . . . . . C11 C 0.5437(8) 0.6131(5) 0.3738(8) 0.0428 1.0000 Uani . . . . . . . C12 C 0.4960(8) 0.5880(6) 0.4290(9) 0.0436 1.0000 Uani . . . . . . . C13 C 0.5193(10) 0.6173(6) 0.5206(10) 0.0584 1.0000 Uani . . . . . . . C14 C 0.5944(11) 0.6708(7) 0.5599(10) 0.0630 1.0000 Uani . . . . . . . C15 C 0.6435(9) 0.6954(6) 0.5059(10) 0.0541 1.0000 Uani . . . . . . . C16 C 0.6199(8) 0.6678(6) 0.4128(9) 0.0490 1.0000 Uani . . . . . . . C21 C 0.5075(8) 0.6374(6) 0.1658(8) 0.0413 1.0000 Uani . . . . . . . C22 C 0.5182(9) 0.6122(7) 0.0837(8) 0.0530 1.0000 Uani . . . . . . . C23 C 0.5017(10) 0.6636(9) 0.0064(11) 0.0707 1.0000 Uani . . . . . . . C24 C 0.4779(10) 0.7360(9) 0.0115(11) 0.0737 1.0000 Uani . . . . . . . C25 C 0.4685(13) 0.7624(8) 0.0941(12) 0.0873 1.0000 Uani . . . . . . . C26 C 0.4827(9) 0.7123(6) 0.1731(9) 0.0534 1.0000 Uani . . . . . . . C31 C 0.7985(7) 0.4462(5) 0.4703(7) 0.0381 1.0000 Uani . . . . . . . C32 C 0.7482(9) 0.4714(7) 0.5230(9) 0.0564 1.0000 Uani . . . . . . . C33 C 0.7748(10) 0.4488(8) 0.6172(9) 0.0644 1.0000 Uani . . . . . . . C34 C 0.8517(10) 0.3965(8) 0.6602(9) 0.0611 1.0000 Uani . . . . . . . C35 C 0.9005(10) 0.3711(7) 0.6103(10) 0.0595 1.0000 Uani . . . . . . . C36 C 0.8749(8) 0.3938(6) 0.5141(8) 0.0459 1.0000 Uani . . . . . . . C41 C 0.7939(7) 0.5761(6) 0.3560(8) 0.0344 1.0000 Uani . . . . . . . C42 C 0.7591(8) 0.6194(5) 0.2700(9) 0.0425 1.0000 Uani . . . . . . . C43 C 0.7829(9) 0.6961(6) 0.2739(10) 0.0561 1.0000 Uani . . . . . . . C44 C 0.8395(9) 0.7295(6) 0.3627(10) 0.0566 1.0000 Uani . . . . . . . C45 C 0.8768(9) 0.6868(6) 0.4478(10) 0.0564 1.0000 Uani . . . . . . . C46 C 0.8499(8) 0.6106(6) 0.4425(9) 0.0444 1.0000 Uani . . . . . . . C51 C 0.8462(8) 0.4361(6) 0.3025(9) 0.0528 1.0000 Uani . . . . . . . C52 C 0.9361(8) 0.4712(7) 0.3177(8) 0.0448 1.0000 Uani . . . . . . . C53 C 0.9934(8) 0.4220(9) 0.2890(10) 0.0743 1.0000 Uani . . . . . . . C54 C 0.9411(10) 0.3521(7) 0.2625(10) 0.0632 1.0000 Uani . . . . . . . C55 C 0.8503(10) 0.3600(6) 0.2728(10) 0.0566 1.0000 Uani . . . . . . . C61 C 0.7335(11) 0.4805(8) 0.0667(10) 0.0692 1.0000 Uani . . . . . . . C62 C 0.8159(12) 0.5296(9) 0.0858(10) 0.0733 1.0000 Uani . . . . . . . C63 C 0.8864(13) 0.4879(12) 0.0722(12) 0.0892 1.0000 Uani . . . . . . . C64 C 0.8518(13) 0.4120(11) 0.0436(10) 0.0863 1.0000 Uani . . . . . . . C65 C 0.7548(12) 0.4074(9) 0.0410(10) 0.0769 1.0000 Uani . . . . . . . H121 H 0.4438 0.5480 0.4021 0.0504 1.0000 Uiso R . . . . . . H131 H 0.4824 0.6001 0.5590 0.0698 1.0000 Uiso R . . . . . . H141 H 0.6125 0.6914 0.6271 0.0727 1.0000 Uiso R . . . . . . H151 H 0.6974 0.7339 0.5346 0.0605 1.0000 Uiso R . . . . . . H161 H 0.6557 0.6860 0.3739 0.0580 1.0000 Uiso R . . . . . . H221 H 0.5373 0.5586 0.0792 0.0633 1.0000 Uiso R . . . . . . H231 H 0.5080 0.6454 -0.0536 0.0839 1.0000 Uiso R . . . . . . H241 H 0.4666 0.7711 -0.0443 0.0880 1.0000 Uiso R . . . . . . H251 H 0.4520 0.8167 0.0982 0.0985 1.0000 Uiso R . . . . . . H261 H 0.4749 0.7305 0.2322 0.0618 1.0000 Uiso R . . . . . . H321 H 0.6912 0.5069 0.4915 0.0661 1.0000 Uiso R . . . . . . H331 H 0.7395 0.4694 0.6554 0.0800 1.0000 Uiso R . . . . . . H341 H 0.8699 0.3784 0.7285 0.0748 1.0000 Uiso R . . . . . . H351 H 0.9568 0.3350 0.6425 0.0672 1.0000 Uiso R . . . . . . H361 H 0.9107 0.3726 0.4767 0.0528 1.0000 Uiso R . . . . . . H421 H 0.7170 0.5953 0.2056 0.0497 1.0000 Uiso R . . . . . . H431 H 0.7589 0.7266 0.2122 0.0687 1.0000 Uiso R . . . . . . H441 H 0.8539 0.7850 0.3658 0.0712 1.0000 Uiso R . . . . . . H451 H 0.9221 0.7100 0.5117 0.0672 1.0000 Uiso R . . . . . . H461 H 0.8725 0.5806 0.5044 0.0510 1.0000 Uiso R . . . . . . H521 H 0.9563 0.5232 0.3447 0.0527 1.0000 Uiso R . . . . . . H531 H 1.0583 0.4338 0.2876 0.0835 1.0000 Uiso R . . . . . . H541 H 0.9638 0.3055 0.2406 0.0811 1.0000 Uiso R . . . . . . H551 H 0.7994 0.3198 0.2612 0.0729 1.0000 Uiso R . . . . . . H611 H 0.6706 0.4952 0.0708 0.0780 1.0000 Uiso R . . . . . . H621 H 0.8211 0.5840 0.1055 0.0896 1.0000 Uiso R . . . . . . H631 H 0.9525 0.5075 0.0808 0.1095 1.0000 Uiso R . . . . . . H641 H 0.8885 0.3703 0.0284 0.1067 1.0000 Uiso R . . . . . . H651 H 0.7108 0.3620 0.0244 0.0879 1.0000 Uiso 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 I1 0.0558(5) 0.0281(4) 0.0785(6) 0.0063(4) 0.0161(5) -0.0030(3) Pd1 0.0377(5) 0.0265(4) 0.0426(5) -0.0002(4) 0.0141(4) -0.0022(3) Fe1 0.0409(9) 0.0535(10) 0.0457(10) -0.0038(8) 0.0179(8) 0.0040(8) P1 0.0406(16) 0.0324(14) 0.0425(16) -0.0023(12) 0.0174(14) -0.0008(12) P2 0.0401(16) 0.0266(13) 0.0463(17) 0.0025(12) 0.0183(14) 0.0035(11) F3 0.067(5) 0.036(4) 0.102(6) -0.010(4) 0.017(4) -0.015(3) F4 0.063(5) 0.080(5) 0.101(7) -0.005(5) 0.021(5) -0.037(4) F5 0.036(4) 0.114(6) 0.063(5) -0.007(4) 0.019(4) -0.005(4) F6 0.053(4) 0.067(5) 0.063(5) -0.010(4) 0.021(4) 0.014(3) C1 0.041(6) 0.042(6) 0.031(6) 0.000(5) 0.011(5) 0.003(5) C2 0.022(5) 0.028(5) 0.070(8) 0.004(5) 0.015(5) -0.006(4) C3 0.067(9) 0.053(8) 0.043(8) 0.006(6) 0.014(7) 0.000(6) C4 0.042(7) 0.062(8) 0.058(8) 0.005(7) 0.019(6) -0.018(6) C5 0.038(7) 0.083(10) 0.051(8) 0.005(7) 0.020(6) 0.000(7) C6 0.043(7) 0.058(8) 0.043(7) 0.000(6) 0.019(6) 0.002(6) C11 0.046(7) 0.030(6) 0.044(7) 0.002(5) 0.012(6) 0.006(5) C12 0.037(6) 0.041(6) 0.048(7) 0.001(6) 0.013(6) -0.002(5) C13 0.075(10) 0.035(7) 0.065(10) 0.010(6) 0.029(8) 0.003(6) C14 0.093(11) 0.045(7) 0.044(8) -0.009(6) 0.022(8) 0.002(7) C15 0.049(7) 0.038(6) 0.065(9) -0.010(6) 0.013(7) 0.000(5) C16 0.047(7) 0.039(6) 0.059(8) -0.010(6) 0.020(6) 0.005(5) C21 0.037(6) 0.039(6) 0.043(7) 0.004(5) 0.012(6) 0.002(5) C22 0.052(8) 0.061(8) 0.045(7) 0.006(6) 0.020(6) 0.012(6) C23 0.055(8) 0.087(10) 0.068(9) 0.023(8) 0.024(7) 0.016(8) C24 0.074(10) 0.081(11) 0.065(10) 0.028(8) 0.028(8) 0.008(8) C25 0.109(13) 0.040(8) 0.097(12) 0.018(8) 0.028(11) 0.014(8) C26 0.055(8) 0.038(6) 0.062(8) 0.003(6) 0.020(7) 0.008(5) C31 0.035(6) 0.033(5) 0.038(6) 0.000(5) 0.008(5) -0.002(5) C32 0.040(7) 0.072(8) 0.053(8) 0.012(6) 0.016(6) 0.007(6) C33 0.058(8) 0.087(10) 0.055(8) 0.015(7) 0.031(7) 0.008(7) C34 0.067(9) 0.078(9) 0.041(7) 0.015(7) 0.026(7) -0.001(7) C35 0.063(9) 0.050(7) 0.056(9) 0.010(6) 0.015(7) 0.005(6) C36 0.051(7) 0.033(6) 0.049(7) 0.006(5) 0.016(6) 0.003(5) C41 0.030(6) 0.036(6) 0.041(6) 0.001(5) 0.019(5) 0.000(4) C42 0.047(7) 0.030(6) 0.048(7) 0.001(5) 0.017(6) 0.000(4) C43 0.065(8) 0.032(6) 0.075(9) 0.012(6) 0.032(8) -0.004(6) C44 0.068(9) 0.032(6) 0.077(10) -0.007(7) 0.039(8) -0.008(6) C45 0.053(8) 0.038(7) 0.077(10) -0.013(6) 0.026(7) -0.007(5) C46 0.033(7) 0.035(6) 0.059(8) -0.004(5) 0.014(6) -0.004(5) C51 0.030(6) 0.034(6) 0.067(8) -0.014(6) -0.006(6) 0.004(5) C52 0.039(6) 0.058(7) 0.035(6) -0.017(5) 0.013(5) -0.010(5) C53 0.016(6) 0.118(12) 0.075(10) -0.044(9) 0.006(6) 0.007(7) C54 0.074(10) 0.049(7) 0.079(10) 0.012(7) 0.045(9) 0.022(7) C55 0.082(10) 0.030(6) 0.070(9) 0.000(6) 0.044(8) -0.004(6) C61 0.060(9) 0.085(10) 0.050(8) 0.001(7) 0.011(7) 0.027(8) C62 0.085(11) 0.084(11) 0.055(9) 0.021(8) 0.033(8) 0.011(9) C63 0.076(11) 0.126(15) 0.073(11) 0.024(11) 0.038(10) 0.013(11) C64 0.093(13) 0.131(15) 0.043(8) 0.016(9) 0.037(9) 0.065(11) C65 0.083(11) 0.080(10) 0.056(9) -0.022(8) 0.019(8) 0.002(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.16704(14) loop_ _oxford_twin_element_scale_factors 0.7680(19) 0.2320(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 . Pd1 . 2.6192(10) yes Pd1 . P1 . 2.274(3) yes Pd1 . P2 . 2.338(3) yes Pd1 . C2 . 2.034(10) yes Fe1 . C51 . 1.981(14) yes Fe1 . C52 . 2.033(11) yes Fe1 . C53 . 2.025(12) yes Fe1 . C54 . 2.024(12) yes Fe1 . C55 . 2.028(12) yes Fe1 . C61 . 2.042(13) yes Fe1 . C62 . 2.053(14) yes Fe1 . C63 . 2.006(16) yes Fe1 . C64 . 2.016(13) yes Fe1 . C65 . 2.036(14) yes P1 . C1 . 1.785(11) yes P1 . C11 . 1.823(11) yes P1 . C21 . 1.809(11) yes P2 . C31 . 1.820(10) yes P2 . C41 . 1.825(10) yes P2 . C51 . 1.831(12) yes F3 . C3 . 1.346(14) yes F4 . C4 . 1.367(13) yes F5 . C5 . 1.341(13) yes F6 . C6 . 1.359(13) yes C1 . C2 . 1.422(14) yes C1 . C6 . 1.369(15) yes C2 . C3 . 1.415(15) yes C3 . C4 . 1.410(18) yes C4 . C5 . 1.339(18) yes C5 . C6 . 1.361(17) yes C11 . C12 . 1.377(15) yes C11 . C16 . 1.416(15) yes C12 . C13 . 1.374(17) yes C12 . H121 . 1.000 no C13 . C14 . 1.391(17) yes C13 . H131 . 1.000 no C14 . C15 . 1.377(18) yes C14 . H141 . 1.000 no C15 . C16 . 1.383(17) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C21 . C22 . 1.388(16) yes C21 . C26 . 1.390(14) yes C22 . C23 . 1.414(16) yes C22 . H221 . 1.000 no C23 . C24 . 1.34(2) yes C23 . H231 . 1.000 no C24 . C25 . 1.39(2) yes C24 . H241 . 1.000 no C25 . C26 . 1.426(18) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C31 . C32 . 1.378(16) yes C31 . C36 . 1.398(14) yes C32 . C33 . 1.361(17) yes C32 . H321 . 1.000 no C33 . C34 . 1.398(17) yes C33 . H331 . 1.000 no C34 . C35 . 1.328(17) yes C34 . H341 . 1.000 no C35 . C36 . 1.392(17) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no C41 . C42 . 1.402(14) yes C41 . C46 . 1.357(14) yes C42 . C43 . 1.396(14) yes C42 . H421 . 1.000 no C43 . C44 . 1.376(17) yes C43 . H431 . 1.000 no C44 . C45 . 1.385(17) yes C44 . H441 . 1.000 no C45 . C46 . 1.398(14) yes C45 . H451 . 1.000 no C46 . H461 . 1.000 no C51 . C52 . 1.405(15) yes C51 . C55 . 1.427(15) yes C52 . C53 . 1.410(16) yes C52 . H521 . 1.000 no C53 . C54 . 1.424(19) yes C53 . H531 . 1.000 no C54 . C55 . 1.432(17) yes C54 . H541 . 1.000 no C55 . H551 . 1.000 no C61 . C62 . 1.430(19) yes C61 . C65 . 1.422(18) yes C61 . H611 . 1.000 no C62 . C63 . 1.37(2) yes C62 . H621 . 1.000 no C63 . C64 . 1.44(2) yes C63 . H631 . 1.000 no C64 . C65 . 1.43(2) yes C64 . H641 . 1.000 no C65 . H651 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I1 . Pd1 . P1 . 161.43(8) yes I1 . Pd1 . P2 . 90.71(7) yes P1 . Pd1 . P2 . 102.30(10) yes I1 . Pd1 . C2 . 96.4(3) yes P1 . Pd1 . C2 . 69.3(3) yes P2 . Pd1 . C2 . 170.2(3) yes C51 . Fe1 . C52 . 40.9(4) yes C51 . Fe1 . C53 . 70.2(5) yes C52 . Fe1 . C53 . 40.7(5) yes C51 . Fe1 . C54 . 70.1(5) yes C52 . Fe1 . C54 . 68.2(5) yes C53 . Fe1 . C54 . 41.2(6) yes C51 . Fe1 . C55 . 41.7(4) yes C52 . Fe1 . C55 . 68.4(5) yes C53 . Fe1 . C55 . 69.7(6) yes C54 . Fe1 . C55 . 41.4(5) yes C51 . Fe1 . C61 . 111.0(5) yes C52 . Fe1 . C61 . 130.9(5) yes C53 . Fe1 . C61 . 165.3(6) yes C54 . Fe1 . C61 . 153.6(6) yes C55 . Fe1 . C61 . 121.5(6) yes C51 . Fe1 . C62 . 121.2(5) yes C52 . Fe1 . C62 . 109.7(6) yes C53 . Fe1 . C62 . 125.3(7) yes C54 . Fe1 . C62 . 161.6(6) yes C55 . Fe1 . C62 . 156.4(6) yes C51 . Fe1 . C63 . 152.9(7) yes C52 . Fe1 . C63 . 118.1(7) yes C53 . Fe1 . C63 . 104.4(7) yes C54 . Fe1 . C63 . 124.1(6) yes C55 . Fe1 . C63 . 163.1(7) yes C51 . Fe1 . C64 . 165.0(7) yes C52 . Fe1 . C64 . 150.5(6) yes C53 . Fe1 . C64 . 114.4(6) yes C54 . Fe1 . C64 . 103.4(6) yes C55 . Fe1 . C64 . 124.8(7) yes C51 . Fe1 . C65 . 128.4(6) yes C52 . Fe1 . C65 . 167.8(6) yes C53 . Fe1 . C65 . 149.9(6) yes C54 . Fe1 . C65 . 116.6(6) yes C55 . Fe1 . C65 . 107.2(6) yes C61 . Fe1 . C62 . 40.9(5) yes C61 . Fe1 . C63 . 67.5(6) yes C62 . Fe1 . C63 . 39.4(6) yes C61 . Fe1 . C64 . 68.6(6) yes C62 . Fe1 . C64 . 69.0(6) yes C63 . Fe1 . C64 . 41.9(7) yes C61 . Fe1 . C65 . 40.8(5) yes C62 . Fe1 . C65 . 69.4(6) yes C63 . Fe1 . C65 . 69.5(7) yes C64 . Fe1 . C65 . 41.4(6) yes Pd1 . P1 . C1 . 85.3(4) yes Pd1 . P1 . C11 . 117.3(3) yes C1 . P1 . C11 . 108.3(5) yes Pd1 . P1 . C21 . 123.4(4) yes C1 . P1 . C21 . 108.0(5) yes C11 . P1 . C21 . 110.0(5) yes Pd1 . P2 . C31 . 106.8(3) yes Pd1 . P2 . C41 . 116.8(3) yes C31 . P2 . C41 . 103.0(5) yes Pd1 . P2 . C51 . 122.0(3) yes C31 . P2 . C51 . 105.6(5) yes C41 . P2 . C51 . 100.7(5) yes P1 . C1 . C2 . 99.4(7) yes P1 . C1 . C6 . 135.5(9) yes C2 . C1 . C6 . 124.9(10) yes C1 . C2 . Pd1 . 105.4(7) yes C1 . C2 . C3 . 112.9(10) yes Pd1 . C2 . C3 . 141.4(9) yes C2 . C3 . F3 . 122.3(11) yes C2 . C3 . C4 . 120.8(11) yes F3 . C3 . C4 . 116.9(11) yes C3 . C4 . F4 . 117.1(12) yes C3 . C4 . C5 . 122.3(11) yes F4 . C4 . C5 . 120.5(11) yes F5 . C5 . C4 . 119.2(12) yes F5 . C5 . C6 . 121.4(12) yes C4 . C5 . C6 . 119.5(11) yes F6 . C6 . C1 . 121.6(10) yes F6 . C6 . C5 . 118.9(10) yes C1 . C6 . C5 . 119.4(11) yes P1 . C11 . C12 . 119.7(8) yes P1 . C11 . C16 . 119.9(9) yes C12 . C11 . C16 . 119.9(11) yes C11 . C12 . C13 . 120.7(11) yes C11 . C12 . H121 . 119.7 no C13 . C12 . H121 . 119.6 no C12 . C13 . C14 . 119.9(12) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C13 . C14 . C15 . 119.9(12) yes C13 . C14 . H141 . 120.1 no C15 . C14 . H141 . 120.1 no C14 . C15 . C16 . 121.2(11) yes C14 . C15 . H151 . 119.4 no C16 . C15 . H151 . 119.4 no C11 . C16 . C15 . 118.4(12) yes C11 . C16 . H161 . 120.8 no C15 . C16 . H161 . 120.8 no P1 . C21 . C22 . 116.6(8) yes P1 . C21 . C26 . 122.5(9) yes C22 . C21 . C26 . 120.7(11) yes C21 . C22 . C23 . 118.9(12) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 120.6 no C22 . C23 . C24 . 121.6(14) yes C22 . C23 . H231 . 119.2 no C24 . C23 . H231 . 119.2 no C23 . C24 . C25 . 120.2(13) yes C23 . C24 . H241 . 119.9 no C25 . C24 . H241 . 119.9 no C24 . C25 . C26 . 120.2(13) yes C24 . C25 . H251 . 119.9 no C26 . C25 . H251 . 119.9 no C25 . C26 . C21 . 118.5(13) yes C25 . C26 . H261 . 120.8 no C21 . C26 . H261 . 120.8 no P2 . C31 . C32 . 119.1(8) yes P2 . C31 . C36 . 122.4(9) yes C32 . C31 . C36 . 118.3(10) yes C31 . C32 . C33 . 121.2(11) yes C31 . C32 . H321 . 119.4 no C33 . C32 . H321 . 119.4 no C32 . C33 . C34 . 119.7(12) yes C32 . C33 . H331 . 120.2 no C34 . C33 . H331 . 120.2 no C33 . C34 . C35 . 120.0(12) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 120.0 no C34 . C35 . C36 . 121.2(12) yes C34 . C35 . H351 . 119.4 no C36 . C35 . H351 . 119.4 no C31 . C36 . C35 . 119.4(11) yes C31 . C36 . H361 . 120.3 no C35 . C36 . H361 . 120.3 no P2 . C41 . C42 . 117.0(8) yes P2 . C41 . C46 . 124.5(8) yes C42 . C41 . C46 . 118.5(9) yes C41 . C42 . C43 . 120.2(11) yes C41 . C42 . H421 . 119.9 no C43 . C42 . H421 . 119.9 no C42 . C43 . C44 . 119.9(11) yes C42 . C43 . H431 . 120.1 no C44 . C43 . H431 . 120.1 no C43 . C44 . C45 . 120.3(11) yes C43 . C44 . H441 . 119.8 no C45 . C44 . H441 . 119.9 no C44 . C45 . C46 . 118.7(12) yes C44 . C45 . H451 . 120.6 no C46 . C45 . H451 . 120.7 no C45 . C46 . C41 . 122.2(11) yes C45 . C46 . H461 . 118.9 no C41 . C46 . H461 . 118.9 no P2 . C51 . Fe1 . 134.0(6) yes P2 . C51 . C52 . 123.3(8) yes Fe1 . C51 . C52 . 71.5(7) yes P2 . C51 . C55 . 127.6(9) yes Fe1 . C51 . C55 . 70.9(7) yes C52 . C51 . C55 . 107.5(10) yes C51 . C52 . Fe1 . 67.5(7) yes C51 . C52 . C53 . 109.8(11) yes Fe1 . C52 . C53 . 69.4(7) yes C51 . C52 . H521 . 125.1 no Fe1 . C52 . H521 . 129.7 no C53 . C52 . H521 . 125.1 no C52 . C53 . Fe1 . 70.0(6) yes C52 . C53 . C54 . 106.8(11) yes Fe1 . C53 . C54 . 69.4(7) yes C52 . C53 . H531 . 126.6 no Fe1 . C53 . H531 . 125.6 no C54 . C53 . H531 . 126.6 no C53 . C54 . Fe1 . 69.4(7) yes C53 . C54 . C55 . 108.4(10) yes Fe1 . C54 . C55 . 69.5(7) yes C53 . C54 . H541 . 125.8 no Fe1 . C54 . H541 . 126.9 no C55 . C54 . H541 . 125.8 no C54 . C55 . C51 . 107.2(11) yes C54 . C55 . Fe1 . 69.1(7) yes C51 . C55 . Fe1 . 67.4(7) yes C54 . C55 . H551 . 126.4 no C51 . C55 . H551 . 126.4 no Fe1 . C55 . H551 . 128.6 no Fe1 . C61 . C62 . 70.0(8) yes Fe1 . C61 . C65 . 69.4(8) yes C62 . C61 . C65 . 109.5(13) yes Fe1 . C61 . H611 . 127.0 no C62 . C61 . H611 . 125.3 no C65 . C61 . H611 . 125.2 no C61 . C62 . Fe1 . 69.2(8) yes C61 . C62 . C63 . 107.0(15) yes Fe1 . C62 . C63 . 68.5(9) yes C61 . C62 . H621 . 126.5 no Fe1 . C62 . H621 . 127.3 no C63 . C62 . H621 . 126.5 no C62 . C63 . Fe1 . 72.1(9) yes C62 . C63 . C64 . 110.3(16) yes Fe1 . C63 . C64 . 69.4(9) yes C62 . C63 . H631 . 124.9 no Fe1 . C63 . H631 . 125.3 no C64 . C63 . H631 . 124.8 no C63 . C64 . Fe1 . 68.7(9) yes C63 . C64 . C65 . 106.8(13) yes Fe1 . C64 . C65 . 70.1(8) yes C63 . C64 . H641 . 126.6 no Fe1 . C64 . H641 . 126.1 no C65 . C64 . H641 . 126.6 no C64 . C65 . C61 . 106.4(14) yes C64 . C65 . Fe1 . 68.5(8) yes C61 . C65 . Fe1 . 69.8(8) yes C64 . C65 . H651 . 126.8 no C61 . C65 . H651 . 126.8 no Fe1 . C65 . H651 . 126.5 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag I1 Pd1 P1 C1 . . . . -36.7(5) no I1 Pd1 P1 C11 . . . . 71.5(5) no I1 Pd1 P1 C21 . . . . -145.2(4) no I1 Pd1 P2 C31 . . . . -64.5(3) no I1 Pd1 P2 C41 . . . . -179.2(5) no I1 Pd1 P2 C51 . . . . 56.8(5) no I1 Pd1 C2 C1 . . . . 162.0(8) no I1 Pd1 C2 C3 . . . . -11(2) no Pd1 P1 C1 C2 . . . . -6.1(7) no Pd1 P1 C1 C6 . . . . 178(1) no Pd1 P1 C11 C12 . . . . -74.4(9) no Pd1 P1 C11 C16 . . . . 97.8(8) no Pd1 P1 C21 C22 . . . . 16(1) no Pd1 P1 C21 C26 . . . . -167.9(8) no Pd1 P2 C31 C32 . . . . -51.9(9) no Pd1 P2 C31 C36 . . . . 123.5(8) no Pd1 P2 C41 C42 . . . . -54(1) no Pd1 P2 C41 C46 . . . . 124(1) no Pd1 P2 C51 Fe1 . . . . 56.2(9) no Pd1 P2 C51 C52 . . . . 152.3(8) no Pd1 P2 C51 C55 . . . . -44(1) no Pd1 C2 C1 P1 . . . . 7.1(9) no Pd1 C2 C1 C6 . . . . -176(1) no Pd1 C2 C3 F3 . . . . -10(3) no Pd1 C2 C3 C4 . . . . 170(1) no Fe1 C51 P2 C31 . . . . 178.1(7) no Fe1 C51 P2 C41 . . . . -74.9(8) no Fe1 C51 C52 C53 . . . . -56.3(9) no Fe1 C51 C55 C54 . . . . 57.8(9) no Fe1 C52 C51 P2 . . . . -131.1(9) no Fe1 C52 C51 C55 . . . . 62.2(9) no Fe1 C52 C53 C54 . . . . -59.9(9) no Fe1 C53 C52 C51 . . . . 55.2(8) no Fe1 C53 C54 C55 . . . . -58.7(9) no Fe1 C54 C53 C52 . . . . 60.3(8) no Fe1 C54 C55 C51 . . . . -56.7(8) no Fe1 C55 C51 P2 . . . . 131.4(9) no Fe1 C55 C51 C52 . . . . -62.6(9) no Fe1 C55 C54 C53 . . . . 58.7(9) no Fe1 C61 C62 C63 . . . . 58(1) no Fe1 C61 C65 C64 . . . . -59.0(9) no Fe1 C62 C61 C65 . . . . -58(1) no Fe1 C62 C63 C64 . . . . 59(1) no Fe1 C63 C62 C61 . . . . -59(1) no Fe1 C63 C64 C65 . . . . 60(1) no Fe1 C64 C63 C62 . . . . -61(1) no Fe1 C64 C65 C61 . . . . 60(1) no Fe1 C65 C61 C62 . . . . 59(1) no Fe1 C65 C64 C63 . . . . -59(1) no P1 Pd1 P2 C31 . . . . 102.1(3) no P1 Pd1 P2 C41 . . . . -12.5(5) no P1 Pd1 P2 C51 . . . . -136.5(5) no P1 Pd1 C2 C1 . . . . -5.8(7) no P1 Pd1 C2 C3 . . . . -179(2) no P1 C1 C2 C3 . . . . -178(1) no P1 C1 C6 F6 . . . . -3(2) no P1 C1 C6 C5 . . . . 179(1) no P1 C11 C12 C13 . . . . 174.4(8) no P1 C11 C16 C15 . . . . -173.0(8) no P1 C21 C22 C23 . . . . 175.0(9) no P1 C21 C26 C25 . . . . -176(1) no P2 Pd1 P1 C1 . . . . -170.2(4) no P2 Pd1 P1 C11 . . . . -62.1(5) no P2 Pd1 P1 C21 . . . . 81.2(4) no P2 C31 C32 C33 . . . . 179(1) no P2 C31 C36 C35 . . . . -178.0(8) no P2 C41 C42 C43 . . . . 179(1) no P2 C41 C46 C45 . . . . 179(1) no P2 C51 Fe1 C52 . . . . 119(1) no P2 C51 Fe1 C53 . . . . 154(1) no P2 C51 Fe1 C54 . . . . -161.8(9) no P2 C51 Fe1 C55 . . . . -124(1) no P2 C51 Fe1 C61 . . . . -10(1) no P2 C51 Fe1 C62 . . . . 34(1) no P2 C51 Fe1 C63 . . . . 71(2) no P2 C51 Fe1 C64 . . . . -95(2) no P2 C51 Fe1 C65 . . . . -53(1) no P2 C51 C52 C53 . . . . 172.6(9) no P2 C51 C55 C54 . . . . -170.8(9) no F3 C3 C2 C1 . . . . 178(1) no F3 C3 C4 F4 . . . . -1(2) no F3 C3 C4 C5 . . . . -177(1) no F4 C4 C3 C2 . . . . 179(1) no F4 C4 C5 F5 . . . . 4(2) no F4 C4 C5 C6 . . . . -176(1) no F5 C5 C4 C3 . . . . 180(1) no F5 C5 C6 F6 . . . . -1(2) no F5 C5 C6 C1 . . . . 177(1) no F6 C6 C1 C2 . . . . -179(1) no F6 C6 C5 C4 . . . . 180(1) no C1 P1 Pd1 C2 . . . . 4.5(6) no C1 P1 C11 C12 . . . . 19.8(9) no C1 P1 C11 C16 . . . . -168.0(8) no C1 P1 C21 C22 . . . . -80(1) no C1 P1 C21 C26 . . . . 96(1) no C1 C2 C3 C4 . . . . -2(2) no C1 C6 C5 C4 . . . . -3(2) no C2 Pd1 P1 C11 . . . . 112.6(6) no C2 Pd1 P1 C21 . . . . -104.0(6) no C2 C1 P1 C11 . . . . -123.3(8) no C2 C1 P1 C21 . . . . 117.5(8) no C2 C1 C6 C5 . . . . 4(2) no C2 C3 C4 C5 . . . . 3(2) no C3 C2 C1 C6 . . . . -1(2) no C3 C4 C5 C6 . . . . -1(2) no C6 C1 P1 C11 . . . . 61(1) no C6 C1 P1 C21 . . . . -58(1) no C11 P1 C21 C22 . . . . 161.5(9) no C11 P1 C21 C26 . . . . -22(1) no C11 C12 C13 C14 . . . . -2(2) no C11 C16 C15 C14 . . . . -0(2) no C12 C11 P1 C21 . . . . 137.7(8) no C12 C11 C16 C15 . . . . -1(2) no C12 C13 C14 C15 . . . . 1(2) no C13 C12 C11 C16 . . . . 2(2) no C13 C14 C15 C16 . . . . -0(2) no C16 C11 P1 C21 . . . . -50.1(9) no C21 C22 C23 C24 . . . . 1(2) no C21 C26 C25 C24 . . . . 1(2) no C22 C21 C26 C25 . . . . 0(2) no C22 C23 C24 C25 . . . . -0(2) no C23 C22 C21 C26 . . . . -1(2) no C23 C24 C25 C26 . . . . -1(2) no C31 P2 C41 C42 . . . . -171(1) no C31 P2 C41 C46 . . . . 8(1) no C31 P2 C51 C52 . . . . -86(1) no C31 P2 C51 C55 . . . . 78(1) no C31 C32 C33 C34 . . . . -3(2) no C31 C36 C35 C34 . . . . 2(2) no C32 C31 P2 C41 . . . . 71.7(9) no C32 C31 P2 C51 . . . . 176.9(8) no C32 C31 C36 C35 . . . . -3(2) no C32 C33 C34 C35 . . . . 2(2) no C33 C32 C31 C36 . . . . 3(2) no C33 C34 C35 C36 . . . . -2(2) no C36 C31 P2 C41 . . . . -113.0(9) no C36 C31 P2 C51 . . . . -7.8(9) no C41 P2 C51 C52 . . . . 21(1) no C41 P2 C51 C55 . . . . -175(1) no C41 C42 C43 C44 . . . . -1(2) no C41 C46 C45 C44 . . . . 4(2) no C42 C41 P2 C51 . . . . 80(1) no C42 C41 C46 C45 . . . . -2(2) no C42 C43 C44 C45 . . . . 3(2) no C43 C42 C41 C46 . . . . 1(2) no C43 C44 C45 C46 . . . . -5(2) no C46 C41 P2 C51 . . . . -101(1) no C51 Fe1 C52 C53 . . . . 123(1) no C51 Fe1 C53 C52 . . . . -35.7(8) no C51 Fe1 C53 C54 . . . . 82(1) no C51 Fe1 C54 C53 . . . . -82.2(9) no C51 Fe1 C54 C55 . . . . 37.7(7) no C51 Fe1 C55 C54 . . . . -120.0(9) no C51 Fe1 C61 C62 . . . . 114(1) no C51 Fe1 C61 C65 . . . . -125(1) no C51 Fe1 C62 C61 . . . . -87(1) no C51 Fe1 C62 C63 . . . . 154.4(9) no C51 Fe1 C63 C62 . . . . -54(2) no C51 Fe1 C63 C64 . . . . -175(1) no C51 Fe1 C64 C63 . . . . 171(2) no C51 Fe1 C64 C65 . . . . 53(3) no C51 Fe1 C65 C61 . . . . 77(1) no C51 Fe1 C65 C64 . . . . -164.8(9) no C51 C52 Fe1 C53 . . . . -123(1) no C51 C52 Fe1 C54 . . . . -84.4(8) no C51 C52 Fe1 C55 . . . . -39.6(7) no C51 C52 Fe1 C61 . . . . 74(1) no C51 C52 Fe1 C62 . . . . 115.2(8) no C51 C52 Fe1 C63 . . . . 157.6(9) no C51 C52 Fe1 C64 . . . . -163(1) no C51 C52 Fe1 C65 . . . . 31(3) no C51 C52 C53 C54 . . . . -5(1) no C51 C55 Fe1 C52 . . . . 38.9(7) no C51 C55 Fe1 C53 . . . . 82.6(8) no C51 C55 Fe1 C54 . . . . 120.0(9) no C51 C55 Fe1 C61 . . . . -86.7(8) no C51 C55 Fe1 C62 . . . . -51(2) no C51 C55 Fe1 C63 . . . . 155(2) no C51 C55 Fe1 C64 . . . . -171.2(8) no C51 C55 Fe1 C65 . . . . -129.1(8) no C51 C55 C54 C53 . . . . 2(2) no C52 Fe1 C51 C55 . . . . -117(1) no C52 Fe1 C53 C54 . . . . 118(1) no C52 Fe1 C54 C53 . . . . -38.3(9) no C52 Fe1 C54 C55 . . . . 81.6(8) no C52 Fe1 C55 C54 . . . . -81.1(8) no C52 Fe1 C61 C62 . . . . 71(1) no C52 Fe1 C61 C65 . . . . -167(1) no C52 Fe1 C62 C61 . . . . -130.4(9) no C52 Fe1 C62 C63 . . . . 111(1) no C52 Fe1 C63 C62 . . . . -87.3(9) no C52 Fe1 C63 C64 . . . . 152.0(9) no C52 Fe1 C64 C63 . . . . -57(2) no C52 Fe1 C64 C65 . . . . -176(1) no C52 Fe1 C65 C61 . . . . 52(3) no C52 Fe1 C65 C64 . . . . 169(3) no C52 C51 Fe1 C53 . . . . 35.4(8) no C52 C51 Fe1 C54 . . . . 79.4(7) no C52 C51 Fe1 C55 . . . . 117(1) no C52 C51 Fe1 C61 . . . . -128.9(7) no C52 C51 Fe1 C62 . . . . -84.5(8) no C52 C51 Fe1 C63 . . . . -48(2) no C52 C51 Fe1 C64 . . . . 146(2) no C52 C51 Fe1 C65 . . . . -172.0(8) no C52 C51 C55 C54 . . . . -5(1) no C52 C53 Fe1 C54 . . . . -118(1) no C52 C53 Fe1 C55 . . . . -80.2(9) no C52 C53 Fe1 C61 . . . . 61(3) no C52 C53 Fe1 C62 . . . . 79(1) no C52 C53 Fe1 C63 . . . . 116(1) no C52 C53 Fe1 C64 . . . . 159.8(9) no C52 C53 Fe1 C65 . . . . -170(1) no C52 C53 C54 C55 . . . . 2(2) no C53 Fe1 C51 C55 . . . . -81.5(8) no C53 Fe1 C54 C55 . . . . 120(1) no C53 Fe1 C55 C54 . . . . -37.5(8) no C53 Fe1 C61 C62 . . . . 22(3) no C53 Fe1 C61 C65 . . . . 143(3) no C53 Fe1 C62 C61 . . . . -173(1) no C53 Fe1 C62 C63 . . . . 68(1) no C53 Fe1 C63 C62 . . . . -128.7(9) no C53 Fe1 C63 C64 . . . . 111(1) no C53 Fe1 C64 C63 . . . . -84(1) no C53 Fe1 C64 C65 . . . . 157.3(9) no C53 Fe1 C65 C61 . . . . -162(1) no C53 Fe1 C65 C64 . . . . -45(2) no C53 C52 Fe1 C54 . . . . 38.8(9) no C53 C52 Fe1 C55 . . . . 83.6(9) no C53 C52 Fe1 C61 . . . . -163(1) no C53 C52 Fe1 C62 . . . . -122(1) no C53 C52 Fe1 C63 . . . . -79(1) no C53 C52 Fe1 C64 . . . . -40(2) no C53 C52 Fe1 C65 . . . . 155(3) no C53 C52 C51 C55 . . . . 6(1) no C53 C54 Fe1 C55 . . . . -120(1) no C53 C54 Fe1 C61 . . . . -180(2) no C53 C54 Fe1 C62 . . . . 49(2) no C53 C54 Fe1 C63 . . . . 72(1) no C53 C54 Fe1 C64 . . . . 112(1) no C53 C54 Fe1 C65 . . . . 154(1) no C54 Fe1 C51 C55 . . . . -37.5(7) no C54 Fe1 C61 C62 . . . . -159(2) no C54 Fe1 C61 C65 . . . . -38(2) no C54 Fe1 C62 C61 . . . . 149(2) no C54 Fe1 C62 C63 . . . . 30(2) no C54 Fe1 C63 C62 . . . . -168.9(8) no C54 Fe1 C63 C64 . . . . 70(1) no C54 Fe1 C64 C63 . . . . -127(1) no C54 Fe1 C64 C65 . . . . 115(1) no C54 Fe1 C65 C61 . . . . 162(1) no C54 Fe1 C65 C64 . . . . -80(1) no C54 C53 Fe1 C55 . . . . 38(1) no C54 C53 Fe1 C61 . . . . 179(3) no C54 C53 Fe1 C62 . . . . -163(1) no C54 C53 Fe1 C63 . . . . -126(1) no C54 C53 Fe1 C64 . . . . -82(1) no C54 C53 Fe1 C65 . . . . -52(2) no C54 C55 Fe1 C61 . . . . 153.2(8) no C54 C55 Fe1 C62 . . . . -171(1) no C54 C55 Fe1 C63 . . . . 35(2) no C54 C55 Fe1 C64 . . . . 69(1) no C54 C55 Fe1 C65 . . . . 110.9(8) no C55 Fe1 C61 C62 . . . . 159.2(9) no C55 Fe1 C61 C65 . . . . -80(1) no C55 Fe1 C62 C61 . . . . -49(2) no C55 Fe1 C62 C63 . . . . -168(1) no C55 Fe1 C63 C62 . . . . 164(2) no C55 Fe1 C63 C64 . . . . 43(2) no C55 Fe1 C64 C63 . . . . -166.0(9) no C55 Fe1 C64 C65 . . . . 76(1) no C55 Fe1 C65 C61 . . . . 119(1) no C55 Fe1 C65 C64 . . . . -124(1) no C55 C51 Fe1 C61 . . . . 114.3(8) no C55 C51 Fe1 C62 . . . . 158.6(8) no C55 C51 Fe1 C63 . . . . -164(1) no C55 C51 Fe1 C64 . . . . 29(3) no C55 C51 Fe1 C65 . . . . 71.1(9) no C55 C54 Fe1 C61 . . . . -60(2) no C55 C54 Fe1 C62 . . . . 169(2) no C55 C54 Fe1 C63 . . . . -168.4(8) no C55 C54 Fe1 C64 . . . . -128.1(8) no C55 C54 Fe1 C65 . . . . -86(1) no C61 Fe1 C62 C63 . . . . -119(1) no C61 Fe1 C63 C62 . . . . 38.2(8) no C61 Fe1 C63 C64 . . . . -82(1) no C61 Fe1 C64 C63 . . . . 80(1) no C61 Fe1 C64 C65 . . . . -38.4(9) no C61 Fe1 C65 C64 . . . . 118(2) no C61 C62 Fe1 C63 . . . . 119(1) no C61 C62 Fe1 C64 . . . . 81(1) no C61 C62 Fe1 C65 . . . . 37(1) no C61 C62 C63 C64 . . . . 0(2) no C61 C65 Fe1 C62 . . . . -37(1) no C61 C65 Fe1 C63 . . . . -79(1) no C61 C65 Fe1 C64 . . . . -118(2) no C61 C65 C64 C63 . . . . 1(2) no C62 Fe1 C61 C65 . . . . 121(2) no C62 Fe1 C63 C64 . . . . -121(1) no C62 Fe1 C64 C63 . . . . 36(1) no C62 Fe1 C64 C65 . . . . -82(1) no C62 Fe1 C65 C64 . . . . 81(1) no C62 C61 Fe1 C63 . . . . -37(1) no C62 C61 Fe1 C64 . . . . -82(1) no C62 C61 Fe1 C65 . . . . -121(2) no C62 C61 C65 C64 . . . . -0(2) no C62 C63 Fe1 C64 . . . . 121(1) no C62 C63 Fe1 C65 . . . . 82(1) no C62 C63 C64 C65 . . . . -1(2) no C63 Fe1 C61 C65 . . . . 84(1) no C63 Fe1 C64 C65 . . . . -118(1) no C63 Fe1 C65 C64 . . . . 39(1) no C63 C62 Fe1 C64 . . . . -38(1) no C63 C62 Fe1 C65 . . . . -82(1) no C63 C62 C61 C65 . . . . 0(2) no C63 C64 Fe1 C65 . . . . 118(1) no C64 Fe1 C61 C65 . . . . 39(1) no C64 C63 Fe1 C65 . . . . -38(1) no data_compound5 _database_code_depnum_ccdc_archive 'CCDC 763270' #TrackingRef '- combined CIFS.cif' _audit_creation_date 09-02-05 _audit_creation_method CRYSTALS_ver_12.85 _audit_update_record ; 2009-02-09 - Report on C58 H39 F8 Fe I2 P3 Pd2 by Anthony C. Willis for Gopa Kar and Martin Bennett 2009-02-09 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title '2041754 ben0706' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.185(2) _cell_length_b 19.347(2) _cell_length_c 20.540(2) _cell_angle_alpha 90 _cell_angle_beta 99.952(5) _cell_angle_gamma 90 _cell_volume 5552.1(11) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C58 H39 F8 Fe1 I2 P3 Pd2 # Dc = 1.80 Fooo = 2912.00 Mu = 21.62 M = 1503.31 # Found Formula = C58 H39 F8 Fe1 I2 P3 Pd2 # Dc = 1.80 FOOO = 2912.00 Mu = 21.62 M = 1503.31 _chemical_formula_sum 'C58 H39 F8 Fe I2 P3 Pd2' _chemical_formula_moiety 'C58 H39 F8 Fe I2 P3 Pd2' _chemical_compound_source 'from RMITU' _chemical_formula_weight 1503.31 _cell_measurement_reflns_used 309291 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 23 _cell_measurement_temperature 200 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 2.162 # Sheldrick geometric approximatio 0.72 0.79 # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.090 -1 0 0 0.060 0 1 0 0.140 0 -1 0 0.160 0 0 1 0.020 0 0 -1 0.090 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_special_details ; CCD data collecting conditions- phi and omega scans of width 0.5 deg at rate 90 sec/frame, crystal-detector distance 35mm, multiple scan sets so over 95 percent of data collected with 3-fold redundancy or more. ; # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 40444 #7626 _reflns_number_total 7626 _diffrn_reflns_av_R_equivalents 0.21 # from denzo #0.290 # Number of reflections with Friedels Law is 7626 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7677 _diffrn_reflns_theta_min 2.561 _diffrn_reflns_theta_max 22.946 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.95 # 22.487 _diffrn_measured_fraction_theta_full 0.993 # 0.996 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 3.79 _oxford_diffrn_Wilson_scale 329.48 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.08 _refine_diff_density_max 1.82 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2157 _refine_ls_number_restraints 313 _refine_ls_number_parameters 263 _oxford_refine_ls_R_factor_ref 0.1045 _refine_ls_wR_factor_ref 0.0932 _refine_ls_goodness_of_fit_ref 1.0894 _refine_ls_shift/su_max 0.003836 # The values computed from all data _oxford_reflns_number_all 7590 _refine_ls_R_factor_all 0.2574 _refine_ls_wR_factor_all 0.1506 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2157 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_gt 0.0932 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.67 -0.550 1.16 ; #============================================================================== # 4. TEXT 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens I1 I 0.5255(2) 0.56310(13) 0.59190(12) 0.0784 1.0000 Uani . U . . . . . I2 I 0.4124(2) 0.66256(15) 0.72427(12) 0.0831 1.0000 Uani . U . . . . . Pd1 Pd 0.5435(2) 0.69785(16) 0.57876(15) 0.0756 1.0000 Uani . U . . . . . Pd2 Pd 0.3561(2) 0.62011(16) 0.60093(14) 0.0740 1.0000 Uani . U . . . . . Fe1 Fe -0.0110(5) 0.6822(4) 0.4899(3) 0.1058 1.0000 Uani . U . . . . . P1 P 0.5981(8) 0.8108(6) 0.5868(5) 0.0783 1.0000 Uani . U . . . . . P2 P 0.4387(7) 0.7011(5) 0.4776(5) 0.0702 1.0000 Uani . U . . . . . P3 P 0.1986(9) 0.6458(6) 0.6059(6) 0.0905 1.0000 Uani . U . . . . . F3 F 0.6933(16) 0.6109(12) 0.7195(10) 0.1069 1.0000 Uani . U . . . . . F4 F 0.857(2) 0.6530(12) 0.7788(12) 0.1367 1.0000 Uani . U . . . . . F5 F 0.933(2) 0.7784(14) 0.7506(15) 0.1671 1.0000 Uani . U . . . . . F6 F 0.8182(17) 0.8612(11) 0.6598(13) 0.1218 1.0000 Uani . U . . . . . F33 F 0.2308(15) 0.4955(10) 0.5345(9) 0.0868 1.0000 Uani . U . . . . . F34 F 0.1801(15) 0.4609(10) 0.4080(9) 0.0867 1.0000 Uani . U . . . . . F35 F 0.2353(16) 0.5357(11) 0.3096(9) 0.0942 1.0000 Uani . U . . . . . F36 F 0.3479(17) 0.6442(11) 0.3392(9) 0.1006 1.0000 Uani . U . . . . . C1 C 0.7006(17) 0.7725(13) 0.6387(11) 0.0772(18) 1.0000 Uiso G U . . . . . C2 C 0.6691(14) 0.7068(14) 0.6524(11) 0.0756(16) 1.0000 Uiso G U . . . . . C3 C 0.7235(18) 0.6664(10) 0.7011(12) 0.077(2) 1.0000 Uiso G U . . . . . C4 C 0.8094(17) 0.6918(13) 0.7362(11) 0.078(2) 1.0000 Uiso G U . . . . . C5 C 0.8409(14) 0.7575(14) 0.7225(12) 0.079(2) 1.0000 Uiso G U . . . . . C6 C 0.7865(19) 0.7979(10) 0.6738(12) 0.078(2) 1.0000 Uiso G U . . . . . C11 C 0.6293(19) 0.8602(13) 0.5193(10) 0.084(2) 1.0000 Uiso G U . . . . . C12 C 0.7110(17) 0.8420(11) 0.4942(12) 0.086(3) 1.0000 Uiso G U . . . . . C13 C 0.7331(15) 0.8759(13) 0.4390(12) 0.086(3) 1.0000 Uiso G U . . . . . C14 C 0.6735(18) 0.9281(13) 0.4089(10) 0.086(3) 1.0000 Uiso G U . . . . . C15 C 0.5918(17) 0.9463(11) 0.4339(12) 0.086(3) 1.0000 Uiso G U . . . . . C16 C 0.5697(15) 0.9124(13) 0.4891(12) 0.085(3) 1.0000 Uiso G U . . . . . C21 C 0.5532(18) 0.8706(12) 0.6399(11) 0.078(2) 1.0000 Uiso G U . . . . . C22 C 0.4771(17) 0.8525(10) 0.6711(12) 0.079(3) 1.0000 Uiso G U . . . . . C23 C 0.4443(15) 0.8989(13) 0.7140(12) 0.079(3) 1.0000 Uiso G U . . . . . C24 C 0.4875(18) 0.9634(12) 0.7256(11) 0.079(3) 1.0000 Uiso G U . . . . . C25 C 0.5637(17) 0.9815(10) 0.6943(12) 0.079(3) 1.0000 Uiso G U . . . . . C26 C 0.5965(15) 0.9351(13) 0.6515(11) 0.078(3) 1.0000 Uiso G U . . . . . C31 C 0.3500(15) 0.6317(10) 0.4523(11) 0.0661(16) 1.0000 Uiso G U . . . . . C32 C 0.3204(17) 0.5937(12) 0.5026(8) 0.0651(15) 1.0000 Uiso G U . . . . . C33 C 0.2610(17) 0.5366(11) 0.4873(10) 0.0651(19) 1.0000 Uiso G U . . . . . C34 C 0.2311(15) 0.5176(10) 0.4216(11) 0.065(2) 1.0000 Uiso G U . . . . . C35 C 0.2607(17) 0.5556(12) 0.3713(8) 0.065(2) 1.0000 Uiso G U . . . . . C36 C 0.3201(16) 0.6127(11) 0.3866(10) 0.0659(19) 1.0000 Uiso G U . . . . . C41 C 0.3674(17) 0.7783(10) 0.4584(12) 0.072(2) 1.0000 Uiso G U . . . . . C42 C 0.3553(16) 0.8220(12) 0.5102(9) 0.073(3) 1.0000 Uiso G U . . . . . C43 C 0.3070(17) 0.8844(11) 0.4970(10) 0.073(3) 1.0000 Uiso G U . . . . . C44 C 0.2707(16) 0.9032(10) 0.4320(11) 0.073(3) 1.0000 Uiso G U . . . . . C45 C 0.2828(16) 0.8595(12) 0.3802(8) 0.073(3) 1.0000 Uiso G U . . . . . C46 C 0.3312(17) 0.7971(11) 0.3933(10) 0.073(3) 1.0000 Uiso G U . . . . . C51 C 0.5236(15) 0.6898(13) 0.4190(10) 0.074(2) 1.0000 Uiso G U . . . . . C52 C 0.5637(17) 0.6252(11) 0.4117(10) 0.074(3) 1.0000 Uiso G U . . . . . C53 C 0.6271(16) 0.6166(10) 0.3676(11) 0.075(3) 1.0000 Uiso G U . . . . . C54 C 0.6505(15) 0.6726(13) 0.3309(10) 0.075(3) 1.0000 Uiso G U . . . . . C55 C 0.6105(17) 0.7372(11) 0.3382(11) 0.075(3) 1.0000 Uiso G U . . . . . C56 C 0.5470(16) 0.7458(10) 0.3823(12) 0.075(3) 1.0000 Uiso G U . . . . . C61 C 0.154(2) 0.5859(13) 0.6587(12) 0.093(3) 1.0000 Uiso G U . . . . . C62 C 0.2068(15) 0.5288(15) 0.6845(13) 0.093(3) 1.0000 Uiso G U . . . . . C63 C 0.1667(19) 0.4803(12) 0.7218(13) 0.093(3) 1.0000 Uiso G U . . . . . C64 C 0.0735(19) 0.4889(13) 0.7331(13) 0.093(3) 1.0000 Uiso G U . . . . . C65 C 0.0203(15) 0.5461(15) 0.7072(13) 0.093(3) 1.0000 Uiso G U . . . . . C66 C 0.0604(19) 0.5946(12) 0.6700(13) 0.093(3) 1.0000 Uiso G U . . . . . C71 C 0.180(2) 0.7278(11) 0.6452(14) 0.091(3) 1.0000 Uiso G U . . . . . C72 C 0.1882(19) 0.7839(15) 0.6040(10) 0.093(3) 1.0000 Uiso G U . . . . . C73 C 0.1751(19) 0.8510(12) 0.6258(12) 0.093(3) 1.0000 Uiso G U . . . . . C74 C 0.1543(18) 0.8618(11) 0.6888(13) 0.093(3) 1.0000 Uiso G U . . . . . C75 C 0.1465(18) 0.8056(15) 0.7300(10) 0.093(3) 1.0000 Uiso G U . . . . . C76 C 0.1595(19) 0.7386(12) 0.7082(12) 0.092(3) 1.0000 Uiso G U . . . . . C81 C 0.119(2) 0.6440(15) 0.5259(11) 0.0933(19) 1.0000 Uiso G U . . . . . C82 C 0.124(2) 0.6826(13) 0.4688(14) 0.095(2) 1.0000 Uiso G U . . . . . C83 C 0.060(2) 0.6534(15) 0.4162(11) 0.096(2) 1.0000 Uiso G U . . . . . C84 C 0.0154(18) 0.5968(15) 0.4407(14) 0.096(2) 1.0000 Uiso G U . . . . . C85 C 0.051(2) 0.5910(14) 0.5086(13) 0.095(2) 1.0000 Uiso G U . . . . . C91 C -0.0567(19) 0.7487(15) 0.5548(11) 0.095(2) 1.0000 Uiso G U . . . . . C92 C -0.057(2) 0.7825(13) 0.4937(15) 0.096(2) 1.0000 Uiso G U . . . . . C93 C -0.119(2) 0.7462(15) 0.4442(11) 0.095(2) 1.0000 Uiso G U . . . . . C94 C -0.1568(19) 0.6900(14) 0.4747(14) 0.095(2) 1.0000 Uiso G U . . . . . C95 C -0.119(2) 0.6916(14) 0.5430(13) 0.096(2) 1.0000 Uiso G U . . . . . H121 H 0.754 0.8045 0.5159 0.1029 1.0000 Uiso G . . . . . . H131 H 0.7918 0.8628 0.4210 0.1035 1.0000 Uiso G . . . . . . H141 H 0.689 0.9525 0.3692 0.1034 1.0000 Uiso G . . . . . . H151 H 0.549 0.9838 0.4122 0.1028 1.0000 Uiso G . . . . . . H161 H 0.5110 0.9255 0.5071 0.1017 1.0000 Uiso G . . . . . . H221 H 0.446 0.8062 0.6628 0.0946 1.0000 Uiso G . . . . . . H231 H 0.3896 0.8859 0.7364 0.0946 1.0000 Uiso G . . . . . . H241 H 0.464 0.9967 0.7564 0.0947 1.0000 Uiso G . . . . . . H251 H 0.595 1.0278 0.7027 0.0944 1.0000 Uiso G . . . . . . H261 H 0.651 0.9481 0.6291 0.0939 1.0000 Uiso G . . . . . . H421 H 0.381 0.8085 0.5569 0.0870 1.0000 Uiso G . . . . . . H431 H 0.298 0.9158 0.5342 0.0878 1.0000 Uiso G . . . . . . H441 H 0.236 0.9481 0.4226 0.0881 1.0000 Uiso G . . . . . . H451 H 0.257 0.8730 0.3335 0.0882 1.0000 Uiso G . . . . . . H461 H 0.340 0.7657 0.3562 0.0878 1.0000 Uiso G . . . . . . H521 H 0.547 0.5850 0.4380 0.0892 1.0000 Uiso G . . . . . . H531 H 0.656 0.5702 0.3623 0.0898 1.0000 Uiso G . . . . . . H541 H 0.696 0.6664 0.2993 0.0906 1.0000 Uiso G . . . . . . H551 H 0.627 0.7774 0.3118 0.0903 1.0000 Uiso G . . . . . . H561 H 0.518 0.7922 0.3875 0.0896 1.0000 Uiso G . . . . . . H621 H 0.2738 0.523 0.6764 0.1116 1.0000 Uiso G . . . . . . H631 H 0.205 0.4392 0.7404 0.1118 1.0000 Uiso G . . . . . . H641 H 0.045 0.4541 0.7598 0.1117 1.0000 Uiso G . . . . . . H651 H -0.0467 0.552 0.7153 0.1118 1.0000 Uiso G . . . . . . H661 H 0.022 0.6357 0.6513 0.1116 1.0000 Uiso G . . . . . . H721 H 0.203 0.776 0.5587 0.1114 1.0000 Uiso G . . . . . . H731 H 0.181 0.8912 0.5962 0.1121 1.0000 Uiso G . . . . . . H741 H 0.145 0.9098 0.7045 0.1121 1.0000 Uiso G . . . . . . H751 H 0.131 0.813 0.7753 0.1115 1.0000 Uiso G . . . . . . H761 H 0.154 0.6983 0.7378 0.1102 1.0000 Uiso G . . . . . . H821 H 0.166 0.7237 0.466 0.1145 1.0000 Uiso G . . . . . . H831 H 0.049 0.670 0.3694 0.1149 1.0000 Uiso G . . . . . . H841 H -0.034 0.566 0.415 0.1147 1.0000 Uiso G . . . . . . H851 H 0.033 0.5550 0.5390 0.1142 1.0000 Uiso G . . . . . . H911 H -0.019 0.763 0.5986 0.1139 1.0000 Uiso G . . . . . . H921 H -0.019 0.8248 0.487 0.1149 1.0000 Uiso G . . . . . . H931 H -0.132 0.758 0.3961 0.1141 1.0000 Uiso G . . . . . . H941 H -0.203 0.6551 0.452 0.1145 1.0000 Uiso G . . . . . . H951 H -0.134 0.6583 0.5771 0.1150 1.0000 Uiso G . . . . . . 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 I1 0.0890(18) 0.0680(14) 0.0719(17) 0.0005(14) -0.0043(14) 0.0114(15) I2 0.096(2) 0.089(2) 0.0599(14) -0.0076(15) 0.0004(13) -0.0019(17) Pd1 0.0860(18) 0.0690(14) 0.0685(18) -0.0080(15) 0.0043(13) 0.0044(15) Pd2 0.0836(15) 0.073(2) 0.0604(14) -0.0020(15) -0.0004(14) 0.0034(14) Fe1 0.098(2) 0.109(3) 0.111(3) -0.0057(18) 0.0198(18) 0.016(3) P1 0.082(4) 0.074(2) 0.076(5) -0.006(2) 0.005(2) -0.002(2) P2 0.082(5) 0.063(3) 0.065(3) -0.005(2) 0.0101(17) -0.0029(18) P3 0.089(2) 0.096(4) 0.088(3) -0.003(2) 0.0191(19) 0.002(3) F3 0.099(15) 0.117(15) 0.095(15) 0.036(11) -0.009(10) -0.029(10) F4 0.17(2) 0.081(13) 0.123(19) 0.003(11) -0.066(14) -0.014(12) F5 0.148(18) 0.107(18) 0.20(3) 0.020(17) -0.088(19) -0.045(14) F6 0.119(17) 0.070(12) 0.16(2) 0.011(11) -0.020(13) -0.011(9) F33 0.101(16) 0.089(14) 0.068(6) 0.007(8) 0.009(10) -0.024(10) F34 0.101(16) 0.079(12) 0.071(9) 0.012(7) -0.010(10) -0.022(9) F35 0.136(19) 0.075(13) 0.064(4) 0.003(8) -0.005(11) -0.005(11) F36 0.138(19) 0.103(17) 0.063(6) -0.016(10) 0.026(11) -0.054(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.0716(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag I1 . Pd1 . 2.638(4) yes I1 . Pd2 . 2.679(4) yes I2 . Pd2 . 2.652(4) yes Pd1 . Pd2 . 3.155(5) yes Pd1 . P1 . 2.315(11) yes Pd1 . P2 . 2.337(10) yes Pd1 . C2 . 2.135(19) yes Pd2 . P3 . 2.308(12) yes Pd2 . C32 . 2.060(15) yes Fe1 . C81 . 2.00(3) yes Fe1 . C82 . 2.03(3) yes Fe1 . C83 . 2.04(3) yes Fe1 . C84 . 2.00(3) yes Fe1 . C85 . 1.98(3) yes Fe1 . C91 . 2.04(3) yes Fe1 . C92 . 2.05(3) yes Fe1 . C93 . 2.06(3) yes Fe1 . C94 . 2.04(3) yes Fe1 . C95 . 2.03(3) yes P1 . C1 . 1.81(2) yes P1 . C11 . 1.80(2) yes P1 . C21 . 1.78(2) yes P2 . C31 . 1.852(19) yes P2 . C41 . 1.81(2) yes P2 . C51 . 1.857(19) yes P3 . C61 . 1.78(2) yes P3 . C71 . 1.82(2) yes P3 . C81 . 1.83(2) yes F3 . C3 . 1.24(3) yes F4 . C4 . 1.26(3) yes F5 . C5 . 1.39(3) yes F6 . C6 . 1.35(3) yes F33 . C33 . 1.38(2) yes F34 . C34 . 1.32(2) yes F35 . C35 . 1.31(2) yes F36 . C36 . 1.27(2) yes C1 . C2 . 1.392 yes C1 . C6 . 1.393 yes C2 . C3 . 1.394 yes C3 . C4 . 1.394 yes C4 . C5 . 1.392 yes C5 . C6 . 1.393 yes C11 . C12 . 1.392 yes C11 . C16 . 1.392 yes C12 . C13 . 1.392 yes C12 . H121 . 1.00 no C13 . C14 . 1.392 yes C13 . H131 . 1.00 no C14 . C15 . 1.392 yes C14 . H141 . 1.00 no C15 . C16 . 1.392 yes C15 . H151 . 1.00 no C16 . H161 . 1.00 no C21 . C22 . 1.392 yes C21 . C26 . 1.393 yes C22 . C23 . 1.393 yes C22 . H221 . 1.00 no C23 . C24 . 1.393 yes C23 . H231 . 1.00 no C24 . C25 . 1.392 yes C24 . H241 . 1.00 no C25 . C26 . 1.393 yes C25 . H251 . 1.00 no C26 . H261 . 1.00 no C31 . C32 . 1.391 yes C31 . C36 . 1.391 yes C32 . C33 . 1.391 yes C33 . C34 . 1.392 yes C34 . C35 . 1.391 yes C35 . C36 . 1.391 yes C41 . C42 . 1.393 yes C41 . C46 . 1.394 yes C42 . C43 . 1.393 yes C42 . H421 . 1.00 no C43 . C44 . 1.394 yes C43 . H431 . 1.00 no C44 . C45 . 1.393 yes C44 . H441 . 1.00 no C45 . C46 . 1.393 yes C45 . H451 . 1.00 no C46 . H461 . 1.00 no C51 . C52 . 1.391 yes C51 . C56 . 1.392 yes C52 . C53 . 1.392 yes C52 . H521 . 1.00 no C53 . C54 . 1.392 yes C53 . H531 . 1.00 no C54 . C55 . 1.391 yes C54 . H541 . 1.00 no C55 . C56 . 1.392 yes C55 . H551 . 1.00 no C56 . H561 . 1.00 no C61 . C62 . 1.391 yes C61 . C66 . 1.392 yes C62 . C63 . 1.392 yes C62 . H621 . 1.00 no C63 . C64 . 1.392 yes C63 . H631 . 1.00 no C64 . C65 . 1.391 yes C64 . H641 . 1.00 no C65 . C66 . 1.392 yes C65 . H651 . 1.00 no C66 . H661 . 1.00 no C71 . C72 . 1.394 yes C71 . C76 . 1.392 yes C72 . C73 . 1.394 yes C72 . H721 . 1.00 no C73 . C74 . 1.392 yes C73 . H731 . 1.00 no C74 . C75 . 1.394 yes C74 . H741 . 1.00 no C75 . C76 . 1.394 yes C75 . H751 . 1.00 no C76 . H761 . 1.00 no C81 . C82 . 1.403 yes C81 . C85 . 1.403 yes C82 . C83 . 1.403 yes C82 . H821 . 1.00 no C83 . C84 . 1.402 yes C83 . H831 . 1.00 no C84 . C85 . 1.403 yes C84 . H841 . 1.00 no C85 . H851 . 1.00 no C91 . C92 . 1.414 yes C91 . C95 . 1.405 yes C91 . H911 . 1.00 no C92 . C93 . 1.409 yes C92 . H921 . 1.00 no C93 . C94 . 1.409 yes C93 . H931 . 1.00 no C94 . C95 . 1.415 yes C94 . H941 . 1.00 no C95 . H951 . 1.00 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Pd1 . I1 . Pd2 . 72.78(11) yes I1 . Pd1 . Pd2 . 54.21(10) yes I1 . Pd1 . P1 . 164.3(3) yes Pd2 . Pd1 . P1 . 136.1(3) yes I1 . Pd1 . P2 . 93.4(3) yes Pd2 . Pd1 . P2 . 73.7(3) yes P1 . Pd1 . P2 . 101.1(4) yes I1 . Pd1 . C2 . 95.2(7) yes Pd2 . Pd1 . C2 . 123.9(7) yes P1 . Pd1 . C2 . 69.2(8) yes P2 . Pd1 . C2 . 162.2(7) yes Pd1 . Pd2 . I1 . 53.01(10) yes Pd1 . Pd2 . I2 . 82.43(12) yes I1 . Pd2 . I2 . 93.91(12) yes Pd1 . Pd2 . P3 . 138.6(3) yes I1 . Pd2 . P3 . 168.0(3) yes I2 . Pd2 . P3 . 91.4(3) yes Pd1 . Pd2 . C32 . 92.7(7) yes I1 . Pd2 . C32 . 84.3(7) yes I2 . Pd2 . C32 . 174.9(7) yes P3 . Pd2 . C32 . 91.2(7) yes C81 . Fe1 . C82 . 40.7(5) yes C81 . Fe1 . C83 . 68.5(6) yes C82 . Fe1 . C83 . 40.3(5) yes C81 . Fe1 . C84 . 69.1(7) yes C82 . Fe1 . C84 . 68.4(6) yes C83 . Fe1 . C84 . 40.6(5) yes C81 . Fe1 . C85 . 41.2(5) yes C82 . Fe1 . C85 . 68.8(6) yes C83 . Fe1 . C85 . 68.8(7) yes C84 . Fe1 . C85 . 41.2(5) yes C81 . Fe1 . C91 . 111.5(10) yes C82 . Fe1 . C91 . 123.7(11) yes C83 . Fe1 . C91 . 156.0(12) yes C84 . Fe1 . C91 . 163.3(12) yes C85 . Fe1 . C91 . 128.1(11) yes C81 . Fe1 . C92 . 127.7(12) yes C82 . Fe1 . C92 . 108.7(10) yes C83 . Fe1 . C92 . 119.2(11) yes C84 . Fe1 . C92 . 152.4(12) yes C85 . Fe1 . C92 . 165.5(12) yes C81 . Fe1 . C93 . 162.0(13) yes C82 . Fe1 . C93 . 123.4(11) yes C83 . Fe1 . C93 . 104.4(10) yes C84 . Fe1 . C93 . 117.0(11) yes C85 . Fe1 . C93 . 153.4(13) yes C81 . Fe1 . C94 . 157.7(12) yes C82 . Fe1 . C94 . 158.8(12) yes C83 . Fe1 . C94 . 121.7(11) yes C84 . Fe1 . C94 . 104.8(10) yes C85 . Fe1 . C94 . 120.2(11) yes C81 . Fe1 . C95 . 124.1(11) yes C82 . Fe1 . C95 . 159.3(12) yes C83 . Fe1 . C95 . 159.7(13) yes C84 . Fe1 . C95 . 124.5(12) yes C85 . Fe1 . C95 . 109.1(10) yes C91 . Fe1 . C92 . 40.5(5) yes C91 . Fe1 . C93 . 67.9(6) yes C92 . Fe1 . C93 . 40.1(5) yes C91 . Fe1 . C94 . 68.0(6) yes C92 . Fe1 . C94 . 67.5(6) yes C93 . Fe1 . C94 . 40.2(5) yes C91 . Fe1 . C95 . 40.4(5) yes C92 . Fe1 . C95 . 67.9(6) yes C93 . Fe1 . C95 . 68.0(6) yes C94 . Fe1 . C95 . 40.6(5) yes Pd1 . P1 . C1 . 83.1(10) yes Pd1 . P1 . C11 . 124.8(10) yes C1 . P1 . C11 . 113.1(13) yes Pd1 . P1 . C21 . 120.4(10) yes C1 . P1 . C21 . 103.9(12) yes C11 . P1 . C21 . 106.7(13) yes Pd1 . P2 . C31 . 121.8(9) yes Pd1 . P2 . C41 . 117.5(9) yes C31 . P2 . C41 . 102.1(12) yes Pd1 . P2 . C51 . 100.9(8) yes C31 . P2 . C51 . 102.6(12) yes C41 . P2 . C51 . 110.8(12) yes Pd2 . P3 . C61 . 109.8(11) yes Pd2 . P3 . C71 . 114.9(11) yes C61 . P3 . C71 . 101.8(14) yes Pd2 . P3 . C81 . 114.3(11) yes C61 . P3 . C81 . 107.6(15) yes C71 . P3 . C81 . 107.5(14) yes P1 . C1 . C2 . 103.9(16) yes P1 . C1 . C6 . 134.7(16) yes C2 . C1 . C6 . 120.0 yes C1 . C2 . Pd1 . 100.9(14) yes C1 . C2 . C3 . 120.0 yes Pd1 . C2 . C3 . 139.0(14) yes C2 . C3 . F3 . 122(2) yes C2 . C3 . C4 . 120.0 yes F3 . C3 . C4 . 118(2) yes C3 . C4 . F4 . 118(2) yes C3 . C4 . C5 . 120.0 yes F4 . C4 . C5 . 122(2) yes F5 . C5 . C4 . 119(2) yes F5 . C5 . C6 . 120(2) yes C4 . C5 . C6 . 120.0 yes C1 . C6 . C5 . 120.0 yes C1 . C6 . F6 . 120(2) yes C5 . C6 . F6 . 120(2) yes P1 . C11 . C12 . 118.7(16) yes P1 . C11 . C16 . 121.1(16) yes C12 . C11 . C16 . 120.0 yes C11 . C12 . C13 . 120.0 yes C11 . C12 . H121 . 120. no C13 . C12 . H121 . 120. no C12 . C13 . C14 . 120. yes C12 . C13 . H131 . 120. no C14 . C13 . H131 . 120. no C13 . C14 . C15 . 120. yes C13 . C14 . H141 . 120. no C15 . C14 . H141 . 120. no C14 . C15 . C16 . 120. yes C14 . C15 . H151 . 120. no C16 . C15 . H151 . 120. no C15 . C16 . C11 . 120. yes C15 . C16 . H161 . 120. no C11 . C16 . H161 . 120. no P1 . C21 . C22 . 120.4(15) yes P1 . C21 . C26 . 119.5(15) yes C22 . C21 . C26 . 120. yes C21 . C22 . C23 . 120. yes C21 . C22 . H221 . 120. no C23 . C22 . H221 . 120. no C22 . C23 . C24 . 120. yes C22 . C23 . H231 . 120. no C24 . C23 . H231 . 120. no C23 . C24 . C25 . 120. yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 120.0 no C24 . C25 . C26 . 120. yes C24 . C25 . H251 . 120.0 no C26 . C25 . H251 . 120.0 no C25 . C26 . C21 . 120.0 yes C25 . C26 . H261 . 120. no C21 . C26 . H261 . 120. no P2 . C31 . C32 . 116.8(14) yes P2 . C31 . C36 . 122.9(14) yes C32 . C31 . C36 . 120.0 yes C31 . C32 . Pd2 . 122.9(13) yes C31 . C32 . C33 . 120. yes Pd2 . C32 . C33 . 117.1(13) yes F33 . C33 . C32 . 123.3(18) yes F33 . C33 . C34 . 116.7(18) yes C32 . C33 . C34 . 120.0) yes C33 . C34 . F34 . 119.3(18) yes C33 . C34 . C35 . 120.0 yes F34 . C34 . C35 . 120.5(19) yes C34 . C35 . F35 . 119.6(19) yes C34 . C35 . C36 . 120. yes F35 . C35 . C36 . 120.4(19) yes C31 . C36 . C35 . 120.0 yes C31 . C36 . F36 . 122.3(19) yes C35 . C36 . F36 . 117.7(19) yes P2 . C41 . C42 . 118.2(14) yes P2 . C41 . C46 . 121.6(14) yes C42 . C41 . C46 . 120.0 yes C41 . C42 . C43 . 120. yes C41 . C42 . H421 . 120.0 no C43 . C42 . H421 . 120.0 no C42 . C43 . C44 . 120.0 yes C42 . C43 . H431 . 120. no C44 . C43 . H431 . 120. no C43 . C44 . C45 . 120.0 yes C43 . C44 . H441 . 120. no C45 . C44 . H441 . 120. no C44 . C45 . C46 . 120. yes C44 . C45 . H451 . 120.0 no C46 . C45 . H451 . 120.0 no C41 . C46 . C45 . 120.0 yes C41 . C46 . H461 . 120. no C45 . C46 . H461 . 120. no P2 . C51 . C52 . 119.9(15) yes P2 . C51 . C56 . 120.1(15) yes C52 . C51 . C56 . 120. yes C51 . C52 . C53 . 120. yes C51 . C52 . H521 . 120.0 no C53 . C52 . H521 . 120.0 no C52 . C53 . C54 . 120.0 yes C52 . C53 . H531 . 120.0 no C54 . C53 . H531 . 120. no C53 . C54 . C55 . 120. yes C53 . C54 . H541 . 120.0 no C55 . C54 . H541 . 120.0 no C54 . C55 . C56 . 120. yes C54 . C55 . H551 . 120.0 no C56 . C55 . H551 . 120.0 no C51 . C56 . C55 . 120.0 yes C51 . C56 . H561 . 120. no C55 . C56 . H561 . 120.0 no P3 . C61 . C62 . 121.5(18) yes P3 . C61 . C66 . 118.3(18) yes C62 . C61 . C66 . 120. yes C61 . C62 . C63 . 120. yes C61 . C62 . H621 . 120.0 no C63 . C62 . H621 . 120.0 no C62 . C63 . C64 . 120.0 yes C62 . C63 . H631 . 120. no C64 . C63 . H631 . 120. no C63 . C64 . C65 . 120. yes C63 . C64 . H641 . 120.0 no C65 . C64 . H641 . 120.0 no C64 . C65 . C66 . 120. yes C64 . C65 . H651 . 120.0 no C66 . C65 . H651 . 120.0 no C61 . C66 . C65 . 120.0 yes C61 . C66 . H661 . 120. no C65 . C66 . H661 . 120. no P3 . C71 . C72 . 112.2(17) yes P3 . C71 . C76 . 127.8(17) yes C72 . C71 . C76 . 120. yes C71 . C72 . C73 . 120. yes C71 . C72 . H721 . 120. no C73 . C72 . H721 . 120. no C72 . C73 . C74 . 120. yes C72 . C73 . H731 . 120.0 no C74 . C73 . H731 . 120.0 no C73 . C74 . C75 . 120. yes C73 . C74 . H741 . 120.0 no C75 . C74 . H741 . 120.0 no C74 . C75 . C76 . 120.0 yes C74 . C75 . H751 . 120. no C76 . C75 . H751 . 120. no C75 . C76 . C71 . 120. yes C75 . C76 . H761 . 120.0 no C71 . C76 . H761 . 120.0 no P3 . C81 . Fe1 . 135.6(15) yes P3 . C81 . C82 . 128.8(19) yes Fe1 . C81 . C82 . 70.9(11) yes P3 . C81 . C85 . 122.0(19) yes Fe1 . C81 . C85 . 68.7(11) yes C82 . C81 . C85 . 108. yes C81 . C82 . Fe1 . 68.4(11) yes C81 . C82 . C83 . 108.0 yes Fe1 . C82 . C83 . 70.0(11) yes C81 . C82 . H821 . 126.0 no Fe1 . C82 . H821 . 127.2 no C83 . C82 . H821 . 126.0 no C82 . C83 . Fe1 . 69.7(11) yes C82 . C83 . C84 . 108. yes Fe1 . C83 . C84 . 68.5(11) yes C82 . C83 . H831 . 126. no Fe1 . C83 . H831 . 127.4 no C84 . C83 . H831 . 126.0 no C83 . C84 . Fe1 . 70.9(11) yes C83 . C84 . C85 . 108.0 yes Fe1 . C84 . C85 . 68.5(11) yes C83 . C84 . H841 . 126.0 no Fe1 . C84 . H841 . 126.0 no C85 . C84 . H841 . 126.0 no C84 . C85 . C81 . 108.0 yes C84 . C85 . Fe1 . 70.3(11) yes C81 . C85 . Fe1 . 70.0(11) yes C84 . C85 . H851 . 126.0 no C81 . C85 . H851 . 126.0) no Fe1 . C85 . H851 . 126.0 no Fe1 . C91 . C92 . 70.3(11) yes Fe1 . C91 . C95 . 69.6(11) yes C92 . C91 . C95 . 108.0) yes Fe1 . C91 . H911 . 125.6 no C92 . C91 . H911 . 126.0 no C95 . C91 . H911 . 126.0 no C91 . C92 . Fe1 . 69.2(11) yes C91 . C92 . C93 . 108. yes Fe1 . C92 . C93 . 70.3(11) yes C91 . C92 . H921 . 126. no Fe1 . C92 . H921 . 126. no C93 . C92 . H921 . 126.0 no C92 . C93 . Fe1 . 69.6(11) yes C92 . C93 . C94 . 107.6 yes Fe1 . C93 . C94 . 69.2(11) yes C92 . C93 . H931 . 126. no Fe1 . C93 . H931 . 126.2 no C94 . C93 . H931 . 126. no C93 . C94 . Fe1 . 70.6(11) yes C93 . C94 . C95 . 108. yes Fe1 . C94 . C95 . 69.3(11) yes C93 . C94 . H941 . 125.9 no Fe1 . C94 . H941 . 125.9 no C95 . C94 . H941 . 125.9 no C94 . C95 . C91 . 107.9 yes C94 . C95 . Fe1 . 70.1(11) yes C91 . C95 . Fe1 . 70.0(11) yes C94 . C95 . H951 . 126.0 no C91 . C95 . H951 . 126.0 no Fe1 . C95 . H951 . 126.0 no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F3 F35 3.10(3) . 2_666 no F5 C75 3.17(4) . 1_655 no F5 C76 3.56(4) . 1_655 no F6 C63 3.33(3) . 3_656 no F6 C64 3.48(3) . 3_656 no F33 C53 3.38(3) . 2_666 no F34 C95 3.28(3) . 2_566 no F34 C65 3.37(3) . 2_566 no F35 C74 3.23(3) . 4_564 no F36 C23 3.22(3) . 4_564 no F36 C75 3.45(3) . 4_564 no C12 C93 3.34(4) . 1_655 no C12 C92 3.49(4) . 1_655 no C12 C94 3.55(4) . 1_655 no C13 C93 3.26(4) . 1_655 no C13 C92 3.50(3) . 1_655 no C15 C25 3.43(3) . 2_676 no C24 C53 3.58(3) . 4_565 no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag I1 Pd1 P1 C1 . . . . 2(2) no I1 Pd1 P1 C11 . . . . 116(1) no I1 Pd1 P1 C21 . . . . -100(2) no I1 Pd1 P2 C31 . . . . 21(1) no I1 Pd1 P2 C41 . . . . 148(1) no I1 Pd1 P2 C51 . . . . -91.4(9) no I1 Pd1 C2 C1 . . . . 165(2) no I1 Pd1 C2 C3 . . . . -9(3) no I1 Pd2 P3 C61 . . . . 46(2) no I1 Pd2 P3 C71 . . . . 160(2) no I1 Pd2 P3 C81 . . . . -75(2) no I1 Pd2 C32 C31 . . . . -78(2) no I1 Pd2 C32 C33 . . . . 104(2) no I2 Pd2 I1 Pd1 . . . . -77.5(1) no I2 Pd2 P3 C61 . . . . -71(1) no I2 Pd2 P3 C71 . . . . 43(1) no I2 Pd2 P3 C81 . . . . 168(1) no Pd1 I1 Pd2 P3 . . . . 166(2) no Pd1 I1 Pd2 C32 . . . . 97.7(7) no Pd1 P1 C1 C2 . . . . -14(2) no Pd1 P1 C1 C6 . . . . -180(3) no Pd1 P1 C11 C12 . . . . -70(2) no Pd1 P1 C11 C16 . . . . 106(2) no Pd1 P1 C21 C22 . . . . -8(2) no Pd1 P1 C21 C26 . . . . 171(2) no Pd1 P2 C31 C32 . . . . 25(2) no Pd1 P2 C31 C36 . . . . -149(2) no Pd1 P2 C41 C42 . . . . -19(2) no Pd1 P2 C41 C46 . . . . 156(2) no Pd1 P2 C51 C52 . . . . 74(2) no Pd1 P2 C51 C56 . . . . -106(2) no Pd1 C2 C1 P1 . . . . 16(2) no Pd1 C2 C1 C6 . . . . -176(2) no Pd1 C2 C3 F3 . . . . -14(4) no Pd1 C2 C3 C4 . . . . 174(2) no Pd2 I1 Pd1 P1 . . . . 136(1) no Pd2 I1 Pd1 P2 . . . . -67.0(3) no Pd2 I1 Pd1 C2 . . . . 128.6(6) no Pd2 P3 C61 C62 . . . . -7(2) no Pd2 P3 C61 C66 . . . . 178(2) no Pd2 P3 C71 C72 . . . . 76(2) no Pd2 P3 C71 C76 . . . . -104(3) no Pd2 P3 C81 Fe1 . . . . -161(2) no Pd2 P3 C81 C82 . . . . -59(3) no Pd2 P3 C81 C85 . . . . 108(2) no Pd2 C32 C31 P2 . . . . 9(3) no Pd2 C32 C31 C36 . . . . -177(2) no Pd2 C32 C33 F33 . . . . -4(3) no Pd2 C32 C33 C34 . . . . 177(2) no Fe1 C81 P3 C61 . . . . 77(3) no Fe1 C81 P3 C71 . . . . -32(3) no Fe1 C81 C82 C83 . . . . -59(2) no Fe1 C81 C85 C84 . . . . 61(2) no Fe1 C82 C81 P3 . . . . -133(3) no Fe1 C82 C81 C85 . . . . 58(2) no Fe1 C82 C83 C84 . . . . -58(2) no Fe1 C83 C82 C81 . . . . 58(2) no Fe1 C83 C84 C85 . . . . -58(2) no Fe1 C84 C83 C82 . . . . 59(2) no Fe1 C84 C85 C81 . . . . -61(2) no Fe1 C85 C81 P3 . . . . 131(2) no Fe1 C85 C81 C82 . . . . -60(2) no Fe1 C85 C84 C83 . . . . 60(2) no Fe1 C91 C92 C93 . . . . 60(2) no Fe1 C91 C95 C94 . . . . -60(2) no Fe1 C92 C91 C95 . . . . -60(2) no Fe1 C92 C93 C94 . . . . 59(2) no Fe1 C93 C92 C91 . . . . -59(2) no Fe1 C93 C94 C95 . . . . 60(2) no Fe1 C94 C93 C92 . . . . -59(2) no Fe1 C94 C95 C91 . . . . 60(2) no Fe1 C95 C91 C92 . . . . 60(2) no Fe1 C95 C94 C93 . . . . -60(2) no P1 Pd1 P2 C31 . . . . -165(1) no P1 Pd1 P2 C41 . . . . -38(1) no P1 Pd1 P2 C51 . . . . 82.5(9) no P1 Pd1 C2 C1 . . . . -13(1) no P1 Pd1 C2 C3 . . . . 173(3) no P1 C1 C2 C3 . . . . -168(2) no P1 C1 C6 F6 . . . . -17(4) no P1 C1 C6 C5 . . . . 164(2) no P1 C11 C12 C13 . . . . 175(2) no P1 C11 C16 C15 . . . . -175(2) no P1 C21 C22 C23 . . . . 178(2) no P1 C21 C26 C25 . . . . -178(2) no P2 Pd1 P1 C1 . . . . -154.8(9) no P2 Pd1 P1 C11 . . . . -41(1) no P2 Pd1 P1 C21 . . . . 103(1) no P2 Pd1 C2 C1 . . . . 47(3) no P2 Pd1 C2 C3 . . . . -128(3) no P2 C31 C32 C33 . . . . -174(2) no P2 C31 C36 F36 . . . . -4(3) no P2 C31 C36 C35 . . . . 174(2) no P2 C41 C42 C43 . . . . 175(2) no P2 C41 C46 C45 . . . . -175(2) no P2 C51 C52 C53 . . . . 180(2) no P2 C51 C56 C55 . . . . -180(2) no P3 Pd2 C32 C31 . . . . 113(2) no P3 Pd2 C32 C33 . . . . -65(2) no P3 C61 C62 C63 . . . . -175(2) no P3 C61 C66 C65 . . . . 175(2) no P3 C71 C72 C73 . . . . 179(2) no P3 C71 C76 C75 . . . . -179(2) no P3 C81 Fe1 C82 . . . . 127(3) no P3 C81 Fe1 C83 . . . . 164(3) no P3 C81 Fe1 C84 . . . . -153(3) no P3 C81 Fe1 C85 . . . . -114(3) no P3 C81 Fe1 C91 . . . . 10(3) no P3 C81 Fe1 C92 . . . . 53(3) no P3 C81 Fe1 C93 . . . . 94(4) no P3 C81 Fe1 C94 . . . . -75(4) no P3 C81 Fe1 C95 . . . . -34(3) no P3 C81 C82 C83 . . . . 168(2) no P3 C81 C85 C84 . . . . -169(2) no F3 C3 C2 C1 . . . . 172(3) no F3 C3 C4 F4 . . . . 9(4) no F3 C3 C4 C5 . . . . -173(3) no F4 C4 C3 C2 . . . . -179(3) no F4 C4 C5 F5 . . . . 8(4) no F4 C4 C5 C6 . . . . 179(3) no F5 C5 C4 C3 . . . . -170(3) no F5 C5 C6 F6 . . . . -8(4) no F5 C5 C6 C1 . . . . 170(3) no F6 C6 C1 C2 . . . . 179(3) no F6 C6 C5 C4 . . . . -179(3) no F33 C33 C32 C31 . . . . 178(2) no F33 C33 C34 F34 . . . . -3(3) no F33 C33 C34 C35 . . . . -178(2) no F34 C34 C33 C32 . . . . 176(2) no F34 C34 C35 F35 . . . . 2(3) no F34 C34 C35 C36 . . . . -176(2) no F35 C35 C34 C33 . . . . 177(2) no F35 C35 C36 F36 . . . . 0(4) no F35 C35 C36 C31 . . . . -177(2) no F36 C36 C31 C32 . . . . -177(2) no F36 C36 C35 C34 . . . . 178(2) no C1 P1 Pd1 C2 . . . . 10(1) no C1 P1 C11 C12 . . . . 28(2) no C1 P1 C11 C16 . . . . -157(2) no C1 P1 C21 C22 . . . . -98(2) no C1 P1 C21 C26 . . . . 81(2) no C1 C2 C3 C4 . . . . 0(4) no C1 C6 C5 C4 . . . . -0(4) no C2 Pd1 P1 C11 . . . . 123(1) no C2 Pd1 P1 C21 . . . . -93(1) no C2 Pd1 P2 C31 . . . . 140(3) no C2 Pd1 P2 C41 . . . . -93(3) no C2 Pd1 P2 C51 . . . . 28(3) no C2 C1 P1 C11 . . . . -139(2) no C2 C1 P1 C21 . . . . 105(2) no C2 C1 C6 C5 . . . . 0(4) no C2 C3 C4 C5 . . . . -0(4) no C3 C2 C1 C6 . . . . -0(4) no C3 C4 C5 C6 . . . . 0(4) no C6 C1 P1 C11 . . . . 55(3) no C6 C1 P1 C21 . . . . -60(3) no C11 P1 C21 C22 . . . . 143(2) no C11 P1 C21 C26 . . . . -39(2) no C11 C12 C13 C14 . . . . 0(3) no C11 C16 C15 C14 . . . . -0(3) no C12 C11 P1 C21 . . . . 142(2) no C12 C11 C16 C15 . . . . 0(3) no C12 C13 C14 C15 . . . . -0(3) no C13 C12 C11 C16 . . . . -0(3) no C13 C14 C15 C16 . . . . 0(3) no C16 C11 P1 C21 . . . . -43(2) no C21 C22 C23 C24 . . . . 0(3) no C21 C26 C25 C24 . . . . 0(3) no C22 C21 C26 C25 . . . . 0(3) no C22 C23 C24 C25 . . . . -0(3) no C23 C22 C21 C26 . . . . -0(3) no C23 C24 C25 C26 . . . . 0(3) no C31 P2 C41 C42 . . . . 117(2) no C31 P2 C41 C46 . . . . -68(2) no C31 P2 C51 C52 . . . . -52(2) no C31 P2 C51 C56 . . . . 128(2) no C31 C32 C33 C34 . . . . -0(4) no C31 C36 C35 C34 . . . . 0(3) no C32 Pd2 P3 C61 . . . . 114(1) no C32 Pd2 P3 C71 . . . . -133(1) no C32 Pd2 P3 C81 . . . . -8(1) no C32 C31 P2 C41 . . . . -108(2) no C32 C31 P2 C51 . . . . 137(2) no C32 C31 C36 C35 . . . . -0(3) no C32 C33 C34 C35 . . . . 0(3) no C33 C32 C31 C36 . . . . 0(3) no C33 C34 C35 C36 . . . . -0(3) no C36 C31 P2 C41 . . . . 78(2) no C36 C31 P2 C51 . . . . -37(2) no C41 P2 C51 C52 . . . . -161(2) no C41 P2 C51 C56 . . . . 19(2) no C41 C42 C43 C44 . . . . 0(4) no C41 C46 C45 C44 . . . . 0(4) no C42 C41 P2 C51 . . . . -135(2) no C42 C41 C46 C45 . . . . -0(4) no C42 C43 C44 C45 . . . . -0(4) no C43 C42 C41 C46 . . . . 0(4) no C43 C44 C45 C46 . . . . -0(4) no C46 C41 P2 C51 . . . . 41(2) no C51 C52 C53 C54 . . . . 0(3) no C51 C56 C55 C54 . . . . -0(3) no C52 C51 C56 C55 . . . . 0(3) no C52 C53 C54 C55 . . . . -0(3) no C53 C52 C51 C56 . . . . -0(3) no C53 C54 C55 C56 . . . . 0(3) no C61 P3 C71 C72 . . . . -165(2) no C61 P3 C71 C76 . . . . 14(3) no C61 P3 C81 C82 . . . . 179(3) no C61 P3 C81 C85 . . . . -14(3) no C61 C62 C63 C64 . . . . 0(4) no C61 C66 C65 C64 . . . . -0(4) no C62 C61 P3 C71 . . . . -129(2) no C62 C61 P3 C81 . . . . 118(2) no C62 C61 C66 C65 . . . . 0(4) no C62 C63 C64 C65 . . . . -0(4) no C63 C62 C61 C66 . . . . -0(4) no C63 C64 C65 C66 . . . . 0(4) no C66 C61 P3 C71 . . . . 55(2) no C66 C61 P3 C81 . . . . -58(2) no C71 P3 C81 C82 . . . . 70(3) no C71 P3 C81 C85 . . . . -123(3) no C71 C72 C73 C74 . . . . 0(4) no C71 C76 C75 C74 . . . . -0(4) no C72 C71 P3 C81 . . . . -52(2) no C72 C71 C76 C75 . . . . 0(4) no C72 C73 C74 C75 . . . . -0(4) no C73 C72 C71 C76 . . . . -0(4) no C73 C74 C75 C76 . . . . 0(4) no C76 C71 P3 C81 . . . . 128(3) no C81 Fe1 C82 C83 . . . . 120(2) no C81 Fe1 C83 C82 . . . . -37(2) no C81 Fe1 C83 C84 . . . . 83(2) no C81 Fe1 C84 C83 . . . . -81(2) no C81 Fe1 C84 C85 . . . . 39(2) no C81 Fe1 C85 C84 . . . . -118(2) no C81 Fe1 C91 C92 . . . . 123(2) no C81 Fe1 C91 C95 . . . . -118(2) no C81 Fe1 C92 C91 . . . . -79(2) no C81 Fe1 C92 C93 . . . . 161(2) no C81 Fe1 C93 C92 . . . . -54(4) no C81 Fe1 C93 C94 . . . . -174(3) no C81 Fe1 C94 C93 . . . . 175(3) no C81 Fe1 C94 C95 . . . . 56(4) no C81 Fe1 C95 C91 . . . . 83(2) no C81 Fe1 C95 C94 . . . . -158(2) no C81 C82 Fe1 C83 . . . . -120(2) no C81 C82 Fe1 C84 . . . . -83(2) no C81 C82 Fe1 C85 . . . . -38(2) no C81 C82 Fe1 C91 . . . . 84(2) no C81 C82 Fe1 C92 . . . . 127(2) no C81 C82 Fe1 C93 . . . . 169(2) no C81 C82 Fe1 C94 . . . . -158(3) no C81 C82 Fe1 C95 . . . . 50(4) no C81 C82 C83 C84 . . . . 0(3) no C81 C85 Fe1 C82 . . . . 37(2) no C81 C85 Fe1 C83 . . . . 81(2) no C81 C85 Fe1 C84 . . . . 118(2) no C81 C85 Fe1 C91 . . . . -80(2) no C81 C85 Fe1 C92 . . . . -46(6) no C81 C85 Fe1 C93 . . . . 161(2) no C81 C85 Fe1 C94 . . . . -164(2) no C81 C85 Fe1 C95 . . . . -121(2) no C81 C85 C84 C83 . . . . -1(3) no C82 Fe1 C81 C85 . . . . -119(2) no C82 Fe1 C83 C84 . . . . 120(2) no C82 Fe1 C84 C83 . . . . -37(2) no C82 Fe1 C84 C85 . . . . 82(2) no C82 Fe1 C85 C84 . . . . -81(2) no C82 Fe1 C91 C92 . . . . 79(2) no C82 Fe1 C91 C95 . . . . -162(2) no C82 Fe1 C92 C91 . . . . -120(2) no C82 Fe1 C92 C93 . . . . 120(2) no C82 Fe1 C93 C92 . . . . -79(2) no C82 Fe1 C93 C94 . . . . 162(2) no C82 Fe1 C94 C93 . . . . -46(4) no C82 Fe1 C94 C95 . . . . -165(3) no C82 Fe1 C95 C91 . . . . 46(4) no C82 Fe1 C95 C94 . . . . 165(3) no C82 C81 Fe1 C83 . . . . 37(2) no C82 C81 Fe1 C84 . . . . 81(2) no C82 C81 Fe1 C85 . . . . 119(2) no C82 C81 Fe1 C91 . . . . -117(2) no C82 C81 Fe1 C92 . . . . -74(2) no C82 C81 Fe1 C93 . . . . -32(4) no C82 C81 Fe1 C94 . . . . 159(3) no C82 C81 Fe1 C95 . . . . -161(2) no C82 C81 C85 C84 . . . . 1(3) no C82 C83 Fe1 C84 . . . . -120(2) no C82 C83 Fe1 C85 . . . . -82(2) no C82 C83 Fe1 C91 . . . . 57(3) no C82 C83 Fe1 C92 . . . . 85(2) no C82 C83 Fe1 C93 . . . . 125(2) no C82 C83 Fe1 C94 . . . . 165(2) no C82 C83 Fe1 C95 . . . . -170(3) no C82 C83 C84 C85 . . . . 0(3) no C83 Fe1 C81 C85 . . . . -82(2) no C83 Fe1 C84 C85 . . . . 120(2) no C83 Fe1 C85 C84 . . . . -37(2) no C83 Fe1 C91 C92 . . . . 38(3) no C83 Fe1 C91 C95 . . . . 157(2) no C83 Fe1 C92 C91 . . . . -163(2) no C83 Fe1 C92 C93 . . . . 77(2) no C83 Fe1 C93 C92 . . . . -118(2) no C83 Fe1 C93 C94 . . . . 122(2) no C83 Fe1 C94 C93 . . . . -74(2) no C83 Fe1 C94 C95 . . . . 167(2) no C83 Fe1 C95 C91 . . . . -153(3) no C83 Fe1 C95 C94 . . . . -34(4) no C83 C82 Fe1 C84 . . . . 37(2) no C83 C82 Fe1 C85 . . . . 82(2) no C83 C82 Fe1 C91 . . . . -156(2) no C83 C82 Fe1 C92 . . . . -113(2) no C83 C82 Fe1 C93 . . . . -71(2) no C83 C82 Fe1 C94 . . . . -38(4) no C83 C82 Fe1 C95 . . . . 170(3) no C83 C82 C81 C85 . . . . -0(3) no C83 C84 Fe1 C85 . . . . -120(2) no C83 C84 Fe1 C91 . . . . -176(3) no C83 C84 Fe1 C92 . . . . 52(3) no C83 C84 Fe1 C93 . . . . 81(2) no C83 C84 Fe1 C94 . . . . 122(2) no C83 C84 Fe1 C95 . . . . 161(2) no C84 Fe1 C81 C85 . . . . -38(2) no C84 Fe1 C91 C92 . . . . -148(3) no C84 Fe1 C91 C95 . . . . -29(4) no C84 Fe1 C92 C91 . . . . 161(2) no C84 Fe1 C92 C93 . . . . 41(3) no C84 Fe1 C93 C92 . . . . -160(2) no C84 Fe1 C93 C94 . . . . 81(2) no C84 Fe1 C94 C93 . . . . -114(2) no C84 Fe1 C94 C95 . . . . 126(2) no C84 Fe1 C95 C91 . . . . 170(2) no C84 Fe1 C95 C94 . . . . -71(2) no C84 C83 Fe1 C85 . . . . 38(2) no C84 C83 Fe1 C91 . . . . 177(2) no C84 C83 Fe1 C92 . . . . -155(2) no C84 C83 Fe1 C93 . . . . -115(2) no C84 C83 Fe1 C94 . . . . -75(2) no C84 C83 Fe1 C95 . . . . -50(4) no C84 C85 Fe1 C91 . . . . 162(2) no C84 C85 Fe1 C92 . . . . -164(5) no C84 C85 Fe1 C93 . . . . 43(3) no C84 C85 Fe1 C94 . . . . 78(2) no C84 C85 Fe1 C95 . . . . 121(2) no C85 Fe1 C91 C92 . . . . 168(2) no C85 Fe1 C91 C95 . . . . -74(2) no C85 Fe1 C92 C91 . . . . -42(6) no C85 Fe1 C92 C93 . . . . -161(5) no C85 Fe1 C93 C92 . . . . 170(3) no C85 Fe1 C93 C94 . . . . 51(3) no C85 Fe1 C94 C93 . . . . -156(2) no C85 Fe1 C94 C95 . . . . 85(2) no C85 Fe1 C95 C91 . . . . 127(2) no C85 Fe1 C95 C94 . . . . -114(2) no C85 C81 Fe1 C91 . . . . 124(2) no C85 C81 Fe1 C92 . . . . 167(2) no C85 C81 Fe1 C93 . . . . -152(3) no C85 C81 Fe1 C94 . . . . 39(4) no C85 C81 Fe1 C95 . . . . 80(2) no C85 C84 Fe1 C91 . . . . -57(4) no C85 C84 Fe1 C92 . . . . 172(2) no C85 C84 Fe1 C93 . . . . -160(2) no C85 C84 Fe1 C94 . . . . -119(2) no C85 C84 Fe1 C95 . . . . -79(2) no C91 Fe1 C92 C93 . . . . -120(2) no C91 Fe1 C93 C92 . . . . 38(2) no C91 Fe1 C93 C94 . . . . -82(2) no C91 Fe1 C94 C93 . . . . 81(2) no C91 Fe1 C94 C95 . . . . -38(2) no C91 Fe1 C95 C94 . . . . 119(2) no C91 C92 Fe1 C93 . . . . 120(2) no C91 C92 Fe1 C94 . . . . 82(2) no C91 C92 Fe1 C95 . . . . 38(2) no C91 C92 C93 C94 . . . . -0(3) no C91 C95 Fe1 C92 . . . . -38(2) no C91 C95 Fe1 C93 . . . . -82(2) no C91 C95 Fe1 C94 . . . . -119(2) no C91 C95 C94 C93 . . . . -1(3) no C92 Fe1 C91 C95 . . . . 118(2) no C92 Fe1 C93 C94 . . . . -119(2) no C92 Fe1 C94 C93 . . . . 38(2) no C92 Fe1 C94 C95 . . . . -82(2) no C92 Fe1 C95 C94 . . . . 81(2) no C92 C91 Fe1 C93 . . . . -37(2) no C92 C91 Fe1 C94 . . . . -81(2) no C92 C91 Fe1 C95 . . . . -118(2) no C92 C91 C95 C94 . . . . 1(3) no C92 C93 Fe1 C94 . . . . 119(2) no C92 C93 Fe1 C95 . . . . 81(2) no C92 C93 C94 C95 . . . . 0(3) no C93 Fe1 C91 C95 . . . . 81(2) no C93 Fe1 C94 C95 . . . . -119(2) no C93 Fe1 C95 C94 . . . . 37(2) no C93 C92 Fe1 C94 . . . . -37(2) no C93 C92 Fe1 C95 . . . . -81(2) no C93 C92 C91 C95 . . . . -0(3) no C93 C94 Fe1 C95 . . . . 119(2) no C94 Fe1 C91 C95 . . . . 38(2) no C94 C93 Fe1 C95 . . . . -38(2) no #------------------------------------------------------------------------------ # start Validation Reply Form _vrf_THETM01_ben0706 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: ... Diffraction data were only collected to 2\q = 23\% as there were no measurable intensities beyond that point. ; _vrf_PLAT023_ben0706 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.95 Deg. RESPONSE: ... Diffraction data were only collected to 2\q = 23\% as there were no measurable intensities beyond that point. ; _vrf_PLAT026_ben0706 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 28 Perc. RESPONSE: ... The initial diffraction pattern showed strong rings, suggesting that the crystal had largely decomposed and was now essentially a powder. There were, however, some very weak spots at low 2\q which, it was hoped, might indicate the presence of some crystallinity inside the sample. Diffraction data were only collected to 2\q = 23\% as there were no measurable intensities beyond that point. Even so, data were of very poor quality as indicated by the poor merging R~int~. ; _vrf_PLAT201_ben0706 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 58 RESPONSE: ... ; _vrf_PLAT601_ben0706 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 240.00 A**3 RESPONSE: ... The computer program SQUEEZE [van der Sluis and Spek, 1990] within PLATON was used to account for any electron density in this region. ; # end Validation Reply Form #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 763271' #TrackingRef '- combined CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H29 Br F4 Fe P2 Pd' _chemical_formula_sum 'C40 H29 Br F4 Fe P2 Pd' _chemical_formula_weight 889.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9344(5) _cell_length_b 17.4528(9) _cell_length_c 14.7656(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.348(2) _cell_angle_gamma 90.00 _cell_volume 3478.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2054 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 20.92 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 2.226 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8663 _exptl_absorpt_correction_T_max 0.9568 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20791 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.1129 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6742 _reflns_number_gt 4136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP32 (Farugia)' _computing_publication_material 'Ciftab (Sheldrick)' _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^)+(0.0263P)^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 6742 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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 0.76334(2) 0.55062(2) 0.08876(2) 0.01869(10) Uani 1 1 d . . . Br1 Br 0.78230(4) 0.68911(3) 0.12219(4) 0.03513(16) Uani 1 1 d . . . Fe1 Fe 0.67658(5) 0.57123(4) 0.36080(5) 0.0271(2) Uani 1 1 d . . . P1 P 0.75809(9) 0.43330(7) 0.02219(8) 0.0200(3) Uani 1 1 d . . . P2 P 0.84338(9) 0.52599(7) 0.26041(8) 0.0180(3) Uani 1 1 d . . . F3 F 0.6546(2) 0.68415(19) -0.1257(2) 0.0491(9) Uani 1 1 d . . . F4 F 0.6171(2) 0.6446(2) -0.3120(2) 0.0550(10) Uani 1 1 d . . . F5 F 0.6429(2) 0.50087(19) -0.36062(19) 0.0470(9) Uani 1 1 d . . . F6 F 0.7026(2) 0.38895(18) -0.21723(19) 0.0381(8) Uani 1 1 d . . . C1 C 0.7165(3) 0.4827(3) -0.0946(3) 0.0215(12) Uani 1 1 d . . . C2 C 0.7068(3) 0.5572(3) -0.0663(3) 0.0238(12) Uani 1 1 d . . . C3 C 0.6715(3) 0.6112(3) -0.1416(4) 0.0308(13) Uani 1 1 d . . . C4 C 0.6508(4) 0.5903(4) -0.2396(4) 0.0387(15) Uani 1 1 d . . . C5 C 0.6626(4) 0.5178(4) -0.2643(3) 0.0311(14) Uani 1 1 d . . . C6 C 0.6930(3) 0.4608(3) -0.1930(3) 0.0279(13) Uani 1 1 d . . . C11 C 0.8753(3) 0.3865(3) 0.0486(3) 0.0202(11) Uani 1 1 d . . . C12 C 0.9319(3) 0.4106(3) -0.0005(3) 0.0267(12) Uani 1 1 d . . . H12 H 0.9056 0.4472 -0.0529 0.032 Uiso 1 1 calc R . . C13 C 1.0257(4) 0.3816(3) 0.0265(4) 0.0354(14) Uani 1 1 d . . . H13 H 1.0637 0.3982 -0.0075 0.042 Uiso 1 1 calc R . . C14 C 1.0639(4) 0.3291(3) 0.1020(4) 0.0388(15) Uani 1 1 d . . . H14 H 1.1285 0.3091 0.1202 0.047 Uiso 1 1 calc R . . C15 C 1.0089(4) 0.3049(3) 0.1522(4) 0.0370(14) Uani 1 1 d . . . H15 H 1.0363 0.2691 0.2056 0.044 Uiso 1 1 calc R . . C16 C 0.9150(4) 0.3327(3) 0.1249(3) 0.0271(12) Uani 1 1 d . . . H16 H 0.8769 0.3150 0.1583 0.033 Uiso 1 1 calc R . . C21 C 0.6661(3) 0.3630(3) 0.0112(3) 0.0205(12) Uani 1 1 d . . . C22 C 0.5819(3) 0.3889(3) 0.0210(3) 0.0273(13) Uani 1 1 d . . . H22 H 0.5780 0.4408 0.0383 0.033 Uiso 1 1 calc R . . C23 C 0.5043(4) 0.3393(4) 0.0059(4) 0.0397(15) Uani 1 1 d . . . H23 H 0.4472 0.3573 0.0121 0.048 Uiso 1 1 calc R . . C24 C 0.5103(4) 0.2641(4) -0.0182(4) 0.0464(17) Uani 1 1 d . . . H24 H 0.4573 0.2300 -0.0283 0.056 Uiso 1 1 calc R . . C25 C 0.5926(4) 0.2381(3) -0.0278(4) 0.0441(15) Uani 1 1 d . . . H25 H 0.5964 0.1859 -0.0443 0.053 Uiso 1 1 calc R . . C26 C 0.6698(4) 0.2874(3) -0.0135(3) 0.0336(14) Uani 1 1 d . . . H26 H 0.7262 0.2689 -0.0208 0.040 Uiso 1 1 calc R . . C31 C 0.9708(3) 0.5569(3) 0.3001(3) 0.0201(11) Uani 1 1 d . . . C32 C 1.0234(3) 0.5292(3) 0.2483(3) 0.0360(15) Uani 1 1 d . . . H32 H 0.9930 0.4943 0.1944 0.043 Uiso 1 1 calc R . . C33 C 1.1188(4) 0.5526(4) 0.2754(4) 0.0441(16) Uani 1 1 d . . . H33 H 1.1551 0.5327 0.2413 0.053 Uiso 1 1 calc R . . C34 C 1.1630(4) 0.6048(3) 0.3518(4) 0.0392(15) Uani 1 1 d . . . H34 H 1.2284 0.6221 0.3681 0.047 Uiso 1 1 calc R . . C35 C 1.1133(4) 0.6315(3) 0.4037(4) 0.0315(13) Uani 1 1 d . . . H35 H 1.1446 0.6665 0.4574 0.038 Uiso 1 1 calc R . . C36 C 1.0170(3) 0.6077(3) 0.3784(3) 0.0251(12) Uani 1 1 d . . . H36 H 0.9825 0.6264 0.4150 0.030 Uiso 1 1 calc R . . C41 C 0.8544(3) 0.4252(3) 0.2969(3) 0.0181(11) Uani 1 1 d . . . C42 C 0.7680(3) 0.3810(3) 0.2638(3) 0.0214(11) Uani 1 1 d . . . H42 H 0.7059 0.4042 0.2242 0.026 Uiso 1 1 calc R . . C43 C 0.7714(4) 0.3046(3) 0.2877(3) 0.0320(13) Uani 1 1 d . . . H43 H 0.7119 0.2758 0.2655 0.038 Uiso 1 1 calc R . . C44 C 0.8607(4) 0.2700(3) 0.3435(4) 0.0344(14) Uani 1 1 d . . . H44 H 0.8633 0.2169 0.3587 0.041 Uiso 1 1 calc R . . C45 C 0.9470(4) 0.3128(3) 0.3777(3) 0.0321(13) Uani 1 1 d . . . H45 H 1.0090 0.2894 0.4173 0.039 Uiso 1 1 calc R . . C46 C 0.9427(3) 0.3887(3) 0.3542(3) 0.0246(12) Uani 1 1 d . . . H46 H 1.0025 0.4175 0.3781 0.030 Uiso 1 1 calc R . . C51 C 0.8080(3) 0.5702(3) 0.3500(3) 0.0206(11) Uani 1 1 d . . . C52 C 0.8171(3) 0.5335(3) 0.4415(3) 0.0253(12) Uani 1 1 d . . . H52 H 0.8362 0.4818 0.4603 0.030 Uiso 1 1 calc R . . C53 C 0.7928(3) 0.5874(3) 0.4972(4) 0.0322(14) Uani 1 1 d . . . H53 H 0.7933 0.5784 0.5609 0.039 Uiso 1 1 calc R . . C54 C 0.7673(4) 0.6572(3) 0.4444(4) 0.0360(14) Uani 1 1 d . . . H54 H 0.7479 0.7030 0.4659 0.043 Uiso 1 1 calc R . . C55 C 0.7759(3) 0.6466(3) 0.3529(3) 0.0296(13) Uani 1 1 d . . . H55 H 0.7624 0.6842 0.3023 0.036 Uiso 1 1 calc R . . C61 C 0.5648(3) 0.5275(4) 0.2347(4) 0.0385(15) Uani 1 1 d . . . H61 H 0.5689 0.5117 0.1750 0.046 Uiso 1 1 calc R . . C62 C 0.5824(4) 0.4802(4) 0.3174(4) 0.0455(16) Uani 1 1 d . . . H62 H 0.6014 0.4278 0.3247 0.055 Uiso 1 1 calc R . . C63 C 0.5660(4) 0.5261(5) 0.3875(4) 0.059(2) Uani 1 1 d . . . H63 H 0.5708 0.5092 0.4505 0.071 Uiso 1 1 calc R . . C64 C 0.5415(4) 0.6013(5) 0.3493(4) 0.060(2) Uani 1 1 d . . . H64 H 0.5283 0.6436 0.3820 0.072 Uiso 1 1 calc R . . C65 C 0.5405(4) 0.6015(4) 0.2532(4) 0.0493(17) Uani 1 1 d . . . H65 H 0.5259 0.6441 0.2091 0.059 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 0.0170(2) 0.0184(2) 0.0167(2) 0.00192(16) 0.00347(16) 0.00038(18) Br1 0.0484(4) 0.0194(3) 0.0278(3) 0.0021(2) 0.0070(3) -0.0046(3) Fe1 0.0197(4) 0.0407(6) 0.0188(4) -0.0018(3) 0.0063(3) 0.0028(4) P1 0.0189(7) 0.0225(8) 0.0158(6) -0.0008(5) 0.0050(6) 0.0012(6) P2 0.0172(7) 0.0179(8) 0.0167(7) -0.0005(5) 0.0053(6) -0.0002(6) F3 0.066(2) 0.029(2) 0.0368(18) 0.0131(14) 0.0067(16) 0.0050(17) F4 0.067(2) 0.058(3) 0.0304(18) 0.0210(16) 0.0112(17) 0.0037(19) F5 0.0384(19) 0.085(3) 0.0166(16) 0.0059(15) 0.0103(15) 0.0042(18) F6 0.0375(18) 0.047(2) 0.0291(17) -0.0070(14) 0.0134(15) 0.0098(16) C1 0.011(3) 0.032(3) 0.023(3) 0.002(2) 0.009(2) 0.000(2) C2 0.016(3) 0.035(4) 0.020(3) 0.004(2) 0.007(2) 0.000(2) C3 0.022(3) 0.041(4) 0.024(3) 0.004(2) 0.005(3) -0.004(3) C4 0.024(3) 0.056(5) 0.030(3) 0.021(3) 0.006(3) 0.002(3) C5 0.022(3) 0.053(4) 0.015(3) 0.000(3) 0.004(2) -0.002(3) C6 0.024(3) 0.034(4) 0.024(3) -0.004(2) 0.009(2) -0.003(3) C11 0.015(3) 0.023(3) 0.018(3) -0.008(2) 0.002(2) 0.002(2) C12 0.027(3) 0.019(3) 0.033(3) -0.006(2) 0.012(3) -0.002(2) C13 0.020(3) 0.031(4) 0.058(4) -0.010(3) 0.021(3) -0.006(3) C14 0.019(3) 0.027(4) 0.064(4) -0.008(3) 0.012(3) 0.006(3) C15 0.030(3) 0.027(4) 0.038(3) -0.001(3) -0.001(3) 0.003(3) C16 0.027(3) 0.023(3) 0.028(3) -0.001(2) 0.008(3) 0.004(2) C21 0.021(3) 0.026(3) 0.012(3) -0.002(2) 0.004(2) -0.004(2) C22 0.023(3) 0.038(4) 0.021(3) -0.007(2) 0.009(2) -0.003(3) C23 0.024(3) 0.067(5) 0.029(3) -0.004(3) 0.012(3) -0.007(3) C24 0.043(4) 0.051(5) 0.040(4) -0.003(3) 0.012(3) -0.026(3) C25 0.044(4) 0.029(4) 0.045(4) -0.004(3) 0.005(3) -0.004(3) C26 0.029(3) 0.030(4) 0.034(3) -0.004(2) 0.007(3) -0.003(3) C31 0.018(3) 0.021(3) 0.015(2) 0.005(2) 0.002(2) -0.001(2) C32 0.023(3) 0.060(5) 0.023(3) -0.010(3) 0.008(3) -0.007(3) C33 0.026(3) 0.081(5) 0.032(3) -0.011(3) 0.019(3) -0.009(3) C34 0.024(3) 0.049(4) 0.036(4) 0.004(3) 0.005(3) -0.016(3) C35 0.026(3) 0.031(4) 0.029(3) -0.001(2) 0.004(3) -0.005(3) C36 0.025(3) 0.022(3) 0.028(3) 0.002(2) 0.012(3) -0.002(2) C41 0.020(3) 0.024(3) 0.011(2) -0.0007(19) 0.008(2) 0.000(2) C42 0.019(3) 0.029(3) 0.014(3) 0.003(2) 0.004(2) 0.006(2) C43 0.036(3) 0.031(4) 0.027(3) 0.001(2) 0.012(3) -0.007(3) C44 0.056(4) 0.017(3) 0.030(3) 0.006(2) 0.018(3) 0.000(3) C45 0.039(3) 0.026(4) 0.023(3) 0.004(2) 0.006(3) 0.010(3) C46 0.021(3) 0.024(3) 0.023(3) 0.004(2) 0.003(2) 0.003(2) C51 0.017(3) 0.026(3) 0.016(3) -0.002(2) 0.004(2) 0.002(2) C52 0.017(3) 0.035(4) 0.022(3) 0.001(2) 0.006(2) 0.002(2) C53 0.023(3) 0.045(4) 0.025(3) -0.007(3) 0.007(3) 0.005(3) C54 0.038(3) 0.033(4) 0.039(3) -0.018(3) 0.018(3) 0.001(3) C55 0.031(3) 0.029(4) 0.024(3) -0.002(2) 0.007(3) 0.001(3) C61 0.019(3) 0.061(5) 0.025(3) -0.008(3) 0.000(3) -0.001(3) C62 0.026(3) 0.058(5) 0.050(4) 0.000(3) 0.014(3) -0.014(3) C63 0.027(4) 0.124(8) 0.032(4) -0.001(4) 0.017(3) -0.022(4) C64 0.023(3) 0.107(7) 0.043(4) -0.035(4) 0.007(3) 0.008(4) C65 0.037(4) 0.062(5) 0.035(4) -0.004(3) 0.003(3) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 2.076(4) . ? Pd1 P1 2.2582(13) . ? Pd1 P2 2.3332(12) . ? Pd1 Br1 2.4589(7) . ? Fe1 C63 2.014(5) . ? Fe1 C64 2.019(5) . ? Fe1 C55 2.022(5) . ? Fe1 C52 2.029(4) . ? Fe1 C62 2.036(6) . ? Fe1 C51 2.036(4) . ? Fe1 C53 2.038(5) . ? Fe1 C65 2.042(5) . ? Fe1 C61 2.043(5) . ? Fe1 C54 2.043(5) . ? P1 C1 1.785(5) . ? P1 C21 1.797(5) . ? P1 C11 1.816(5) . ? P2 C51 1.795(4) . ? P2 C31 1.817(4) . ? P2 C41 1.827(5) . ? F3 C3 1.337(6) . ? F4 C4 1.354(6) . ? F5 C5 1.356(5) . ? F6 C6 1.329(6) . ? C1 C2 1.393(7) . ? C1 C6 1.394(6) . ? C2 C3 1.379(7) . ? C3 C4 1.393(7) . ? C4 C5 1.348(7) . ? C5 C6 1.376(7) . ? C11 C16 1.390(6) . ? C11 C12 1.392(6) . ? C12 C13 1.378(6) . ? C12 H12 0.9500 . ? C13 C14 1.365(7) . ? C13 H13 0.9500 . ? C14 C15 1.388(7) . ? C14 H14 0.9500 . ? C15 C16 1.372(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.376(7) . ? C21 C22 1.401(6) . ? C22 C23 1.385(7) . ? C22 H22 0.9500 . ? C23 C24 1.372(8) . ? C23 H23 0.9500 . ? C24 C25 1.373(7) . ? C24 H24 0.9500 . ? C25 C26 1.381(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.384(6) . ? C31 C32 1.396(6) . ? C32 C33 1.367(6) . ? C32 H32 0.9500 . ? C33 C34 1.378(7) . ? C33 H33 0.9500 . ? C34 C35 1.357(6) . ? C34 H34 0.9500 . ? C35 C36 1.386(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.380(6) . ? C41 C42 1.400(6) . ? C42 C43 1.374(6) . ? C42 H42 0.9500 . ? C43 C44 1.372(7) . ? C43 H43 0.9500 . ? C44 C45 1.386(7) . ? C44 H44 0.9500 . ? C45 C46 1.364(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C55 1.424(6) . ? C51 C52 1.448(6) . ? C52 C53 1.397(6) . ? C52 H52 0.9500 . ? C53 C54 1.407(7) . ? C53 H53 0.9500 . ? C54 C55 1.422(6) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C61 C65 1.398(8) . ? C61 C62 1.403(7) . ? C61 H61 0.9500 . ? C62 C63 1.410(8) . ? C62 H62 0.9500 . ? C63 C64 1.413(9) . ? C63 H63 0.9500 . ? C64 C65 1.412(7) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 P1 69.41(15) . . ? C2 Pd1 P2 170.14(14) . . ? P1 Pd1 P2 102.24(5) . . ? C2 Pd1 Br1 97.14(15) . . ? P1 Pd1 Br1 163.39(4) . . ? P2 Pd1 Br1 90.09(3) . . ? C63 Fe1 C64 41.0(3) . . ? C63 Fe1 C55 161.4(3) . . ? C64 Fe1 C55 123.8(3) . . ? C63 Fe1 C52 119.1(2) . . ? C64 Fe1 C52 151.5(2) . . ? C55 Fe1 C52 69.2(2) . . ? C63 Fe1 C62 40.7(2) . . ? C64 Fe1 C62 69.2(3) . . ? C55 Fe1 C62 156.2(2) . . ? C52 Fe1 C62 109.4(2) . . ? C63 Fe1 C51 155.5(3) . . ? C64 Fe1 C51 163.2(3) . . ? C55 Fe1 C51 41.08(18) . . ? C52 Fe1 C51 41.75(17) . . ? C62 Fe1 C51 121.9(2) . . ? C63 Fe1 C53 106.5(2) . . ? C64 Fe1 C53 116.4(2) . . ? C55 Fe1 C53 68.4(2) . . ? C52 Fe1 C53 40.17(18) . . ? C62 Fe1 C53 126.9(2) . . ? C51 Fe1 C53 68.74(18) . . ? C63 Fe1 C65 68.1(3) . . ? C64 Fe1 C65 40.7(2) . . ? C55 Fe1 C65 107.3(2) . . ? C52 Fe1 C65 167.3(2) . . ? C62 Fe1 C65 68.5(2) . . ? C51 Fe1 C65 127.8(2) . . ? C53 Fe1 C65 151.2(2) . . ? C63 Fe1 C61 67.3(2) . . ? C64 Fe1 C61 67.9(2) . . ? C55 Fe1 C61 121.6(2) . . ? C52 Fe1 C61 130.5(2) . . ? C62 Fe1 C61 40.2(2) . . ? C51 Fe1 C61 111.35(19) . . ? C53 Fe1 C61 165.9(2) . . ? C65 Fe1 C61 40.0(2) . . ? C63 Fe1 C54 123.8(2) . . ? C64 Fe1 C54 103.9(2) . . ? C55 Fe1 C54 40.94(18) . . ? C52 Fe1 C54 68.4(2) . . ? C62 Fe1 C54 162.4(2) . . ? C51 Fe1 C54 69.02(19) . . ? C53 Fe1 C54 40.3(2) . . ? C65 Fe1 C54 117.5(2) . . ? C61 Fe1 C54 153.7(2) . . ? C1 P1 C21 107.8(2) . . ? C1 P1 C11 109.2(2) . . ? C21 P1 C11 110.0(2) . . ? C1 P1 Pd1 85.16(17) . . ? C21 P1 Pd1 122.77(16) . . ? C11 P1 Pd1 117.64(15) . . ? C51 P2 C31 103.5(2) . . ? C51 P2 C41 102.4(2) . . ? C31 P2 C41 104.0(2) . . ? C51 P2 Pd1 123.06(15) . . ? C31 P2 Pd1 105.91(14) . . ? C41 P2 Pd1 115.92(14) . . ? C2 C1 C6 123.8(4) . . ? C2 C1 P1 101.4(3) . . ? C6 C1 P1 134.7(4) . . ? C3 C2 C1 116.7(4) . . ? C3 C2 Pd1 139.6(4) . . ? C1 C2 Pd1 103.5(3) . . ? F3 C3 C2 123.0(5) . . ? F3 C3 C4 117.2(5) . . ? C2 C3 C4 119.8(5) . . ? C5 C4 F4 119.3(5) . . ? C5 C4 C3 122.1(5) . . ? F4 C4 C3 118.6(6) . . ? C4 C5 F5 119.6(5) . . ? C4 C5 C6 120.6(5) . . ? F5 C5 C6 119.8(5) . . ? F6 C6 C5 121.0(4) . . ? F6 C6 C1 122.0(4) . . ? C5 C6 C1 116.9(5) . . ? C16 C11 C12 118.8(4) . . ? C16 C11 P1 121.0(4) . . ? C12 C11 P1 119.8(4) . . ? C13 C12 C11 120.5(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.0(5) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.3(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.0(5) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.3(5) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? C26 C21 C22 118.4(5) . . ? C26 C21 P1 124.2(4) . . ? C22 C21 P1 117.1(4) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 119.7(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.3(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 120.8(5) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C36 C31 C32 118.9(4) . . ? C36 C31 P2 122.6(4) . . ? C32 C31 P2 118.5(4) . . ? C33 C32 C31 119.8(5) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.7(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 120.2(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 120.0(5) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 C35 120.4(4) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C46 C41 C42 117.2(5) . . ? C46 C41 P2 124.5(4) . . ? C42 C41 P2 118.3(3) . . ? C43 C42 C41 121.1(5) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C44 C43 C42 120.1(5) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.6(5) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 119.8(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 122.2(5) . . ? C45 C46 H46 118.9 . . ? C41 C46 H46 118.9 . . ? C55 C51 C52 106.5(4) . . ? C55 C51 P2 129.4(4) . . ? C52 C51 P2 123.9(4) . . ? C55 C51 Fe1 68.9(3) . . ? C52 C51 Fe1 68.9(2) . . ? P2 C51 Fe1 131.3(2) . . ? C53 C52 C51 107.8(5) . . ? C53 C52 Fe1 70.3(3) . . ? C51 C52 Fe1 69.4(2) . . ? C53 C52 H52 126.1 . . ? C51 C52 H52 126.1 . . ? Fe1 C52 H52 125.9 . . ? C52 C53 C54 109.5(5) . . ? C52 C53 Fe1 69.6(3) . . ? C54 C53 Fe1 70.0(3) . . ? C52 C53 H53 125.2 . . ? C54 C53 H53 125.2 . . ? Fe1 C53 H53 126.7 . . ? C53 C54 C55 107.5(5) . . ? C53 C54 Fe1 69.6(3) . . ? C55 C54 Fe1 68.7(3) . . ? C53 C54 H54 126.2 . . ? C55 C54 H54 126.2 . . ? Fe1 C54 H54 127.0 . . ? C54 C55 C51 108.6(4) . . ? C54 C55 Fe1 70.3(3) . . ? C51 C55 Fe1 70.0(3) . . ? C54 C55 H55 125.7 . . ? C51 C55 H55 125.7 . . ? Fe1 C55 H55 125.6 . . ? C65 C61 C62 110.0(5) . . ? C65 C61 Fe1 70.0(3) . . ? C62 C61 Fe1 69.6(3) . . ? C65 C61 H61 125.0 . . ? C62 C61 H61 125.0 . . ? Fe1 C61 H61 127.0 . . ? C61 C62 C63 106.1(6) . . ? C61 C62 Fe1 70.1(3) . . ? C63 C62 Fe1 68.8(3) . . ? C61 C62 H62 127.0 . . ? C63 C62 H62 127.0 . . ? Fe1 C62 H62 125.7 . . ? C62 C63 C64 109.4(5) . . ? C62 C63 Fe1 70.4(3) . . ? C64 C63 Fe1 69.7(4) . . ? C62 C63 H63 125.3 . . ? C64 C63 H63 125.3 . . ? Fe1 C63 H63 126.1 . . ? C65 C64 C63 107.0(6) . . ? C65 C64 Fe1 70.5(3) . . ? C63 C64 Fe1 69.3(3) . . ? C65 C64 H64 126.5 . . ? C63 C64 H64 126.5 . . ? Fe1 C64 H64 125.3 . . ? C61 C65 C64 107.5(6) . . ? C61 C65 Fe1 70.0(3) . . ? C64 C65 Fe1 68.8(3) . . ? C61 C65 H65 126.2 . . ? C64 C65 H65 126.2 . . ? Fe1 C65 H65 126.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Pd1 P1 C1 3.84(19) . . . . ? P2 Pd1 P1 C1 -170.69(14) . . . . ? Br1 Pd1 P1 C1 -33.6(2) . . . . ? C2 Pd1 P1 C21 -104.3(2) . . . . ? P2 Pd1 P1 C21 81.17(18) . . . . ? Br1 Pd1 P1 C21 -141.69(19) . . . . ? C2 Pd1 P1 C11 113.0(2) . . . . ? P2 Pd1 P1 C11 -61.53(18) . . . . ? Br1 Pd1 P1 C11 75.6(2) . . . . ? P1 Pd1 P2 C51 -140.11(19) . . . . ? Br1 Pd1 P2 C51 51.10(19) . . . . ? P1 Pd1 P2 C31 101.54(17) . . . . ? Br1 Pd1 P2 C31 -67.25(17) . . . . ? P1 Pd1 P2 C41 -13.13(16) . . . . ? Br1 Pd1 P2 C41 178.09(16) . . . . ? C21 P1 C1 C2 117.5(3) . . . . ? C11 P1 C1 C2 -123.1(3) . . . . ? Pd1 P1 C1 C2 -5.5(3) . . . . ? C21 P1 C1 C6 -60.0(5) . . . . ? C11 P1 C1 C6 59.4(5) . . . . ? Pd1 P1 C1 C6 177.1(5) . . . . ? C6 C1 C2 C3 0.2(7) . . . . ? P1 C1 C2 C3 -177.7(4) . . . . ? C6 C1 C2 Pd1 -176.1(4) . . . . ? P1 C1 C2 Pd1 6.1(3) . . . . ? P1 Pd1 C2 C3 -179.9(6) . . . . ? Br1 Pd1 C2 C3 -9.9(5) . . . . ? P1 Pd1 C2 C1 -5.0(3) . . . . ? Br1 Pd1 C2 C1 164.9(3) . . . . ? C1 C2 C3 F3 177.1(4) . . . . ? Pd1 C2 C3 F3 -8.5(8) . . . . ? C1 C2 C3 C4 -2.2(7) . . . . ? Pd1 C2 C3 C4 172.2(4) . . . . ? F3 C3 C4 C5 -178.2(5) . . . . ? C2 C3 C4 C5 1.2(8) . . . . ? F3 C3 C4 F4 1.3(7) . . . . ? C2 C3 C4 F4 -179.4(4) . . . . ? F4 C4 C5 F5 1.6(8) . . . . ? C3 C4 C5 F5 -178.9(4) . . . . ? F4 C4 C5 C6 -177.4(4) . . . . ? C3 C4 C5 C6 2.0(8) . . . . ? C4 C5 C6 F6 178.4(5) . . . . ? F5 C5 C6 F6 -0.6(7) . . . . ? C4 C5 C6 C1 -3.9(8) . . . . ? F5 C5 C6 C1 177.1(4) . . . . ? C2 C1 C6 F6 -179.5(4) . . . . ? P1 C1 C6 F6 -2.5(8) . . . . ? C2 C1 C6 C5 2.8(7) . . . . ? P1 C1 C6 C5 179.9(4) . . . . ? C1 P1 C11 C16 -167.9(4) . . . . ? C21 P1 C11 C16 -49.8(4) . . . . ? Pd1 P1 C11 C16 97.4(4) . . . . ? C1 P1 C11 C12 19.2(4) . . . . ? C21 P1 C11 C12 137.4(4) . . . . ? Pd1 P1 C11 C12 -75.4(4) . . . . ? C16 C11 C12 C13 -0.2(7) . . . . ? P1 C11 C12 C13 172.8(4) . . . . ? C11 C12 C13 C14 -0.2(8) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C16 1.2(8) . . . . ? C14 C15 C16 C11 -1.6(8) . . . . ? C12 C11 C16 C15 1.1(7) . . . . ? P1 C11 C16 C15 -171.8(4) . . . . ? C1 P1 C21 C26 95.2(4) . . . . ? C11 P1 C21 C26 -23.8(5) . . . . ? Pd1 P1 C21 C26 -169.0(3) . . . . ? C1 P1 C21 C22 -79.7(4) . . . . ? C11 P1 C21 C22 161.3(3) . . . . ? Pd1 P1 C21 C22 16.1(4) . . . . ? C26 C21 C22 C23 -0.2(7) . . . . ? P1 C21 C22 C23 175.0(3) . . . . ? C21 C22 C23 C24 0.5(7) . . . . ? C22 C23 C24 C25 -0.3(8) . . . . ? C23 C24 C25 C26 -0.2(8) . . . . ? C22 C21 C26 C25 -0.3(7) . . . . ? P1 C21 C26 C25 -175.1(4) . . . . ? C24 C25 C26 C21 0.5(8) . . . . ? C51 P2 C31 C36 -4.2(5) . . . . ? C41 P2 C31 C36 -110.9(4) . . . . ? Pd1 P2 C31 C36 126.5(4) . . . . ? C51 P2 C31 C32 176.9(4) . . . . ? C41 P2 C31 C32 70.2(4) . . . . ? Pd1 P2 C31 C32 -52.4(4) . . . . ? C36 C31 C32 C33 -0.1(8) . . . . ? P2 C31 C32 C33 178.9(4) . . . . ? C31 C32 C33 C34 -1.7(9) . . . . ? C32 C33 C34 C35 2.5(9) . . . . ? C33 C34 C35 C36 -1.5(8) . . . . ? C32 C31 C36 C35 1.0(7) . . . . ? P2 C31 C36 C35 -177.9(4) . . . . ? C34 C35 C36 C31 -0.2(8) . . . . ? C51 P2 C41 C46 -99.3(4) . . . . ? C31 P2 C41 C46 8.2(4) . . . . ? Pd1 P2 C41 C46 124.0(3) . . . . ? C51 P2 C41 C42 81.5(4) . . . . ? C31 P2 C41 C42 -171.0(3) . . . . ? Pd1 P2 C41 C42 -55.2(3) . . . . ? C46 C41 C42 C43 0.0(6) . . . . ? P2 C41 C42 C43 179.3(3) . . . . ? C41 C42 C43 C44 -1.0(7) . . . . ? C42 C43 C44 C45 1.5(7) . . . . ? C43 C44 C45 C46 -1.0(7) . . . . ? C44 C45 C46 C41 0.0(7) . . . . ? C42 C41 C46 C45 0.5(6) . . . . ? P2 C41 C46 C45 -178.7(4) . . . . ? C31 P2 C51 C55 81.1(4) . . . . ? C41 P2 C51 C55 -171.0(4) . . . . ? Pd1 P2 C51 C55 -38.4(5) . . . . ? C31 P2 C51 C52 -92.4(4) . . . . ? C41 P2 C51 C52 15.5(4) . . . . ? Pd1 P2 C51 C52 148.1(3) . . . . ? C31 P2 C51 Fe1 177.0(3) . . . . ? C41 P2 C51 Fe1 -75.2(3) . . . . ? Pd1 P2 C51 Fe1 57.5(4) . . . . ? C63 Fe1 C51 C55 -164.1(5) . . . . ? C64 Fe1 C51 C55 30.1(8) . . . . ? C52 Fe1 C51 C55 -118.4(4) . . . . ? C62 Fe1 C51 C55 157.8(3) . . . . ? C53 Fe1 C51 C55 -81.1(3) . . . . ? C65 Fe1 C51 C55 71.5(4) . . . . ? C61 Fe1 C51 C55 114.0(3) . . . . ? C54 Fe1 C51 C55 -37.7(3) . . . . ? C63 Fe1 C51 C52 -45.8(6) . . . . ? C64 Fe1 C51 C52 148.5(7) . . . . ? C55 Fe1 C51 C52 118.4(4) . . . . ? C62 Fe1 C51 C52 -83.8(3) . . . . ? C53 Fe1 C51 C52 37.3(3) . . . . ? C65 Fe1 C51 C52 -170.1(3) . . . . ? C61 Fe1 C51 C52 -127.6(3) . . . . ? C54 Fe1 C51 C52 80.7(3) . . . . ? C63 Fe1 C51 P2 71.3(6) . . . . ? C64 Fe1 C51 P2 -94.4(8) . . . . ? C55 Fe1 C51 P2 -124.5(4) . . . . ? C52 Fe1 C51 P2 117.1(5) . . . . ? C62 Fe1 C51 P2 33.3(4) . . . . ? C53 Fe1 C51 P2 154.4(4) . . . . ? C65 Fe1 C51 P2 -53.0(5) . . . . ? C61 Fe1 C51 P2 -10.5(4) . . . . ? C54 Fe1 C51 P2 -162.2(4) . . . . ? C55 C51 C52 C53 -1.1(5) . . . . ? P2 C51 C52 C53 173.7(3) . . . . ? Fe1 C51 C52 C53 -60.0(3) . . . . ? C55 C51 C52 Fe1 58.9(3) . . . . ? P2 C51 C52 Fe1 -126.3(3) . . . . ? C63 Fe1 C52 C53 -81.0(4) . . . . ? C64 Fe1 C52 C53 -42.6(7) . . . . ? C55 Fe1 C52 C53 80.7(3) . . . . ? C62 Fe1 C52 C53 -124.7(3) . . . . ? C51 Fe1 C52 C53 118.9(4) . . . . ? C65 Fe1 C52 C53 157.0(10) . . . . ? C61 Fe1 C52 C53 -164.9(3) . . . . ? C54 Fe1 C52 C53 36.7(3) . . . . ? C63 Fe1 C52 C51 160.1(3) . . . . ? C64 Fe1 C52 C51 -161.5(5) . . . . ? C55 Fe1 C52 C51 -38.2(3) . . . . ? C62 Fe1 C52 C51 116.4(3) . . . . ? C53 Fe1 C52 C51 -118.9(4) . . . . ? C65 Fe1 C52 C51 38.2(12) . . . . ? C61 Fe1 C52 C51 76.2(4) . . . . ? C54 Fe1 C52 C51 -82.2(3) . . . . ? C51 C52 C53 C54 0.7(6) . . . . ? Fe1 C52 C53 C54 -58.8(4) . . . . ? C51 C52 C53 Fe1 59.4(3) . . . . ? C63 Fe1 C53 C52 115.9(4) . . . . ? C64 Fe1 C53 C52 158.8(4) . . . . ? C55 Fe1 C53 C52 -83.0(3) . . . . ? C62 Fe1 C53 C52 75.9(4) . . . . ? C51 Fe1 C53 C52 -38.7(3) . . . . ? C65 Fe1 C53 C52 -169.8(4) . . . . ? C61 Fe1 C53 C52 54.4(10) . . . . ? C54 Fe1 C53 C52 -121.0(4) . . . . ? C63 Fe1 C53 C54 -123.2(4) . . . . ? C64 Fe1 C53 C54 -80.2(4) . . . . ? C55 Fe1 C53 C54 37.9(3) . . . . ? C52 Fe1 C53 C54 121.0(4) . . . . ? C62 Fe1 C53 C54 -163.2(3) . . . . ? C51 Fe1 C53 C54 82.2(3) . . . . ? C65 Fe1 C53 C54 -48.8(6) . . . . ? C61 Fe1 C53 C54 175.4(8) . . . . ? C52 C53 C54 C55 0.0(6) . . . . ? Fe1 C53 C54 C55 -58.5(3) . . . . ? C52 C53 C54 Fe1 58.5(3) . . . . ? C63 Fe1 C54 C53 74.9(4) . . . . ? C64 Fe1 C54 C53 114.6(3) . . . . ? C55 Fe1 C54 C53 -119.3(4) . . . . ? C52 Fe1 C54 C53 -36.5(3) . . . . ? C62 Fe1 C54 C53 49.9(9) . . . . ? C51 Fe1 C54 C53 -81.5(3) . . . . ? C65 Fe1 C54 C53 155.8(3) . . . . ? C61 Fe1 C54 C53 -177.5(4) . . . . ? C63 Fe1 C54 C55 -165.8(3) . . . . ? C64 Fe1 C54 C55 -126.2(3) . . . . ? C52 Fe1 C54 C55 82.8(3) . . . . ? C62 Fe1 C54 C55 169.2(7) . . . . ? C51 Fe1 C54 C55 37.8(3) . . . . ? C53 Fe1 C54 C55 119.3(4) . . . . ? C65 Fe1 C54 C55 -84.9(3) . . . . ? C61 Fe1 C54 C55 -58.2(6) . . . . ? C53 C54 C55 C51 -0.7(6) . . . . ? Fe1 C54 C55 C51 -59.7(3) . . . . ? C53 C54 C55 Fe1 59.0(4) . . . . ? C52 C51 C55 C54 1.1(5) . . . . ? P2 C51 C55 C54 -173.3(3) . . . . ? Fe1 C51 C55 C54 59.9(3) . . . . ? C52 C51 C55 Fe1 -58.9(3) . . . . ? P2 C51 C55 Fe1 126.8(4) . . . . ? C63 Fe1 C55 C54 39.8(8) . . . . ? C64 Fe1 C55 C54 70.7(4) . . . . ? C52 Fe1 C55 C54 -80.6(3) . . . . ? C62 Fe1 C55 C54 -171.9(5) . . . . ? C51 Fe1 C55 C54 -119.4(4) . . . . ? C53 Fe1 C55 C54 -37.4(3) . . . . ? C65 Fe1 C55 C54 112.3(3) . . . . ? C61 Fe1 C55 C54 153.7(3) . . . . ? C63 Fe1 C55 C51 159.2(7) . . . . ? C64 Fe1 C55 C51 -169.9(3) . . . . ? C52 Fe1 C55 C51 38.8(2) . . . . ? C62 Fe1 C55 C51 -52.5(6) . . . . ? C53 Fe1 C55 C51 82.0(3) . . . . ? C65 Fe1 C55 C51 -128.3(3) . . . . ? C61 Fe1 C55 C51 -86.9(3) . . . . ? C54 Fe1 C55 C51 119.4(4) . . . . ? C63 Fe1 C61 C65 82.5(4) . . . . ? C64 Fe1 C61 C65 38.0(4) . . . . ? C55 Fe1 C61 C65 -79.1(4) . . . . ? C52 Fe1 C61 C65 -167.9(3) . . . . ? C62 Fe1 C61 C65 121.6(5) . . . . ? C51 Fe1 C61 C65 -123.9(4) . . . . ? C53 Fe1 C61 C65 148.5(8) . . . . ? C54 Fe1 C61 C65 -38.3(6) . . . . ? C63 Fe1 C61 C62 -39.0(4) . . . . ? C64 Fe1 C61 C62 -83.6(4) . . . . ? C55 Fe1 C61 C62 159.3(3) . . . . ? C52 Fe1 C61 C62 70.6(4) . . . . ? C51 Fe1 C61 C62 114.6(4) . . . . ? C53 Fe1 C61 C62 26.9(10) . . . . ? C65 Fe1 C61 C62 -121.6(5) . . . . ? C54 Fe1 C61 C62 -159.8(4) . . . . ? C65 C61 C62 C63 1.4(6) . . . . ? Fe1 C61 C62 C63 59.7(4) . . . . ? C65 C61 C62 Fe1 -58.4(4) . . . . ? C63 Fe1 C62 C61 117.1(5) . . . . ? C64 Fe1 C62 C61 79.9(4) . . . . ? C55 Fe1 C62 C61 -48.1(7) . . . . ? C52 Fe1 C62 C61 -130.5(3) . . . . ? C51 Fe1 C62 C61 -85.9(4) . . . . ? C53 Fe1 C62 C61 -172.1(3) . . . . ? C65 Fe1 C62 C61 36.1(3) . . . . ? C54 Fe1 C62 C61 149.6(7) . . . . ? C64 Fe1 C62 C63 -37.2(4) . . . . ? C55 Fe1 C62 C63 -165.2(5) . . . . ? C52 Fe1 C62 C63 112.4(4) . . . . ? C51 Fe1 C62 C63 157.0(4) . . . . ? C53 Fe1 C62 C63 70.8(5) . . . . ? C65 Fe1 C62 C63 -81.0(4) . . . . ? C61 Fe1 C62 C63 -117.1(5) . . . . ? C54 Fe1 C62 C63 32.5(9) . . . . ? C61 C62 C63 C64 -1.6(6) . . . . ? Fe1 C62 C63 C64 59.0(4) . . . . ? C61 C62 C63 Fe1 -60.6(4) . . . . ? C64 Fe1 C63 C62 120.5(5) . . . . ? C55 Fe1 C63 C62 161.0(6) . . . . ? C52 Fe1 C63 C62 -86.4(4) . . . . ? C51 Fe1 C63 C62 -53.3(6) . . . . ? C53 Fe1 C63 C62 -128.0(4) . . . . ? C65 Fe1 C63 C62 82.0(4) . . . . ? C61 Fe1 C63 C62 38.6(4) . . . . ? C54 Fe1 C63 C62 -168.7(3) . . . . ? C55 Fe1 C63 C64 40.6(8) . . . . ? C52 Fe1 C63 C64 153.1(3) . . . . ? C62 Fe1 C63 C64 -120.5(5) . . . . ? C51 Fe1 C63 C64 -173.8(4) . . . . ? C53 Fe1 C63 C64 111.5(4) . . . . ? C65 Fe1 C63 C64 -38.5(3) . . . . ? C61 Fe1 C63 C64 -81.9(4) . . . . ? C54 Fe1 C63 C64 70.8(4) . . . . ? C62 C63 C64 C65 1.3(7) . . . . ? Fe1 C63 C64 C65 60.7(4) . . . . ? C62 C63 C64 Fe1 -59.4(4) . . . . ? C63 Fe1 C64 C65 -117.8(5) . . . . ? C55 Fe1 C64 C65 76.7(4) . . . . ? C52 Fe1 C64 C65 -173.5(5) . . . . ? C62 Fe1 C64 C65 -80.8(4) . . . . ? C51 Fe1 C64 C65 53.3(9) . . . . ? C53 Fe1 C64 C65 157.3(4) . . . . ? C61 Fe1 C64 C65 -37.4(4) . . . . ? C54 Fe1 C64 C65 116.2(4) . . . . ? C55 Fe1 C64 C63 -165.6(3) . . . . ? C52 Fe1 C64 C63 -55.7(7) . . . . ? C62 Fe1 C64 C63 37.0(3) . . . . ? C51 Fe1 C64 C63 171.1(6) . . . . ? C53 Fe1 C64 C63 -84.9(4) . . . . ? C65 Fe1 C64 C63 117.8(5) . . . . ? C61 Fe1 C64 C63 80.4(4) . . . . ? C54 Fe1 C64 C63 -126.0(4) . . . . ? C62 C61 C65 C64 -0.6(6) . . . . ? Fe1 C61 C65 C64 -58.8(4) . . . . ? C62 C61 C65 Fe1 58.2(4) . . . . ? C63 C64 C65 C61 -0.5(6) . . . . ? Fe1 C64 C65 C61 59.5(4) . . . . ? C63 C64 C65 Fe1 -60.0(4) . . . . ? C63 Fe1 C65 C61 -80.3(4) . . . . ? C64 Fe1 C65 C61 -119.0(6) . . . . ? C55 Fe1 C65 C61 118.8(4) . . . . ? C52 Fe1 C65 C61 46.7(12) . . . . ? C62 Fe1 C65 C61 -36.3(3) . . . . ? C51 Fe1 C65 C61 78.1(4) . . . . ? C53 Fe1 C65 C61 -164.7(4) . . . . ? C54 Fe1 C65 C61 161.9(3) . . . . ? C63 Fe1 C65 C64 38.7(4) . . . . ? C55 Fe1 C65 C64 -122.2(4) . . . . ? C52 Fe1 C65 C64 165.7(10) . . . . ? C62 Fe1 C65 C64 82.7(4) . . . . ? C51 Fe1 C65 C64 -162.9(4) . . . . ? C53 Fe1 C65 C64 -45.7(7) . . . . ? C61 Fe1 C65 C64 119.0(6) . . . . ? C54 Fe1 C65 C64 -79.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.561 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.128 data_compound1 _database_code_depnum_ccdc_archive 'CCDC 763272' #TrackingRef '- combined CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H33 Br Fe P2 Pd' _chemical_formula_sum 'C40 H33 Br Fe P2 Pd' _chemical_formula_weight 817.76 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.5519(5) _cell_length_b 17.1919(9) _cell_length_c 36.2298(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6572.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6031 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.05 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 2.331 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25943 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5789 _reflns_number_gt 5062 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+13.4013P] 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 5789 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _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 C1 C 0.2621(4) 0.4957(2) 0.15225(11) 0.0199(9) Uani 1 1 d . . . C2 C 0.2159(4) 0.4320(2) 0.13005(11) 0.0203(9) Uani 1 1 d . . . H2 H 0.2585 0.4089 0.1104 0.024 Uiso 1 1 calc R . . C3 C 0.0953(4) 0.4108(3) 0.14319(13) 0.0311(11) Uani 1 1 d . . . H3 H 0.0446 0.3714 0.1336 0.037 Uiso 1 1 calc R . . C4 C 0.0640(4) 0.4589(3) 0.17321(14) 0.0325(12) Uani 1 1 d . . . H4 H -0.0103 0.4564 0.1870 0.039 Uiso 1 1 calc R . . C5 C 0.1654(4) 0.5118(3) 0.17890(13) 0.0263(10) Uani 1 1 d . . . H5 H 0.1685 0.5504 0.1969 0.032 Uiso 1 1 calc R . . C6 C 0.3908(4) 0.3651(3) 0.20985(13) 0.0293(10) Uani 1 1 d . . . H6 H 0.4684 0.3907 0.2092 0.035 Uiso 1 1 calc R . . C7 C 0.3489(4) 0.3077(3) 0.18476(13) 0.0285(10) Uani 1 1 d . . . H7 H 0.3942 0.2889 0.1646 0.034 Uiso 1 1 calc R . . C8 C 0.2267(4) 0.2838(2) 0.19551(13) 0.0297(10) Uani 1 1 d . . . H8 H 0.1776 0.2463 0.1838 0.036 Uiso 1 1 calc R . . C9 C 0.1917(5) 0.3267(3) 0.22720(13) 0.0325(11) Uani 1 1 d . . . H9 H 0.1154 0.3227 0.2399 0.039 Uiso 1 1 calc R . . C10 C 0.2932(5) 0.3766(3) 0.23619(12) 0.0317(11) Uani 1 1 d . . . H10 H 0.2956 0.4111 0.2560 0.038 Uiso 1 1 calc R . . C111 C 0.5110(4) 0.3841(2) 0.04905(11) 0.0172(8) Uani 1 1 d . . . C112 C 0.4584(4) 0.4497(2) 0.06668(11) 0.0169(8) Uani 1 1 d . . . C113 C 0.3644(4) 0.4901(2) 0.04825(11) 0.0202(9) Uani 1 1 d . . . H113 H 0.3275 0.5337 0.0590 0.024 Uiso 1 1 calc R . . C114 C 0.3255(4) 0.4653(2) 0.01370(11) 0.0216(9) Uani 1 1 d . . . H114 H 0.2639 0.4936 0.0012 0.026 Uiso 1 1 calc R . . C115 C 0.3761(4) 0.3992(2) -0.00278(12) 0.0231(9) Uani 1 1 d . . . H115 H 0.3471 0.3830 -0.0258 0.028 Uiso 1 1 calc R . . C116 C 0.4699(4) 0.3577(2) 0.01521(11) 0.0216(9) Uani 1 1 d . . . H116 H 0.5044 0.3131 0.0047 0.026 Uiso 1 1 calc R . . C121 C 0.7853(4) 0.3770(2) 0.05311(11) 0.0172(8) Uani 1 1 d . . . C122 C 0.7972(4) 0.3491(2) 0.01705(11) 0.0230(9) Uani 1 1 d . . . H122 H 0.7305 0.3221 0.0063 0.028 Uiso 1 1 calc R . . C123 C 0.9071(4) 0.3614(2) -0.00266(12) 0.0232(9) Uani 1 1 d . . . H123 H 0.9143 0.3429 -0.0267 0.028 Uiso 1 1 calc R . . C124 C 1.0069(4) 0.4015(2) 0.01342(12) 0.0248(10) Uani 1 1 d . . . H124 H 1.0809 0.4101 0.0001 0.030 Uiso 1 1 calc R . . C125 C 0.9970(4) 0.4286(2) 0.04893(12) 0.0243(9) Uani 1 1 d . . . H125 H 1.0646 0.4550 0.0596 0.029 Uiso 1 1 calc R . . C126 C 0.8864(4) 0.4168(2) 0.06905(11) 0.0196(9) Uani 1 1 d . . . H126 H 0.8801 0.4354 0.0931 0.023 Uiso 1 1 calc R . . C131 C 0.6435(3) 0.2642(2) 0.09538(11) 0.0182(9) Uani 1 1 d . . . C132 C 0.6473(4) 0.2021(2) 0.07146(12) 0.0245(10) Uani 1 1 d . . . H132 H 0.6528 0.2109 0.0462 0.029 Uiso 1 1 calc R . . C133 C 0.6429(4) 0.1265(3) 0.08461(14) 0.0320(11) Uani 1 1 d . . . H133 H 0.6458 0.0850 0.0682 0.038 Uiso 1 1 calc R . . C134 C 0.6343(5) 0.1128(3) 0.12163(13) 0.0318(11) Uani 1 1 d . . . H134 H 0.6290 0.0621 0.1304 0.038 Uiso 1 1 calc R . . C135 C 0.6336(5) 0.1747(3) 0.14599(13) 0.0367(12) Uani 1 1 d . . . H135 H 0.6306 0.1654 0.1713 0.044 Uiso 1 1 calc R . . C136 C 0.6374(4) 0.2501(3) 0.13304(12) 0.0274(10) Uani 1 1 d . . . H136 H 0.6359 0.2915 0.1496 0.033 Uiso 1 1 calc R . . C211 C 0.4613(4) 0.5910(2) 0.18585(12) 0.0244(10) Uani 1 1 d . . . C212 C 0.5497(4) 0.6509(3) 0.18345(14) 0.0337(11) Uani 1 1 d . . . H212 H 0.5796 0.6666 0.1605 0.040 Uiso 1 1 calc R . . C213 C 0.5933(5) 0.6872(3) 0.21534(16) 0.0456(14) Uani 1 1 d . . . H213 H 0.6528 0.7269 0.2137 0.055 Uiso 1 1 calc R . . C214 C 0.5487(5) 0.6644(3) 0.24933(16) 0.0454(14) Uani 1 1 d . . . H214 H 0.5764 0.6896 0.2705 0.054 Uiso 1 1 calc R . . C215 C 0.4634(5) 0.6046(3) 0.25197(14) 0.0425(13) Uani 1 1 d . . . H215 H 0.4344 0.5885 0.2750 0.051 Uiso 1 1 calc R . . C216 C 0.4202(5) 0.5678(3) 0.22017(12) 0.0314(11) Uani 1 1 d . . . H216 H 0.3627 0.5270 0.2221 0.038 Uiso 1 1 calc R . . C221 C 0.3673(4) 0.6275(2) 0.11462(11) 0.0193(9) Uani 1 1 d . . . C222 C 0.4613(4) 0.6638(2) 0.09372(12) 0.0229(9) Uani 1 1 d . . . H222 H 0.5433 0.6440 0.0938 0.028 Uiso 1 1 calc R . . C223 C 0.4333(4) 0.7295(2) 0.07272(12) 0.0250(10) Uani 1 1 d . . . H223 H 0.4969 0.7541 0.0593 0.030 Uiso 1 1 calc R . . C224 C 0.3111(4) 0.7580(2) 0.07183(12) 0.0266(10) Uani 1 1 d . . . H224 H 0.2923 0.8016 0.0577 0.032 Uiso 1 1 calc R . . C225 C 0.2168(4) 0.7220(2) 0.09189(12) 0.0252(10) Uani 1 1 d . . . H225 H 0.1344 0.7412 0.0910 0.030 Uiso 1 1 calc R . . C226 C 0.2440(4) 0.6570(2) 0.11352(11) 0.0211(9) Uani 1 1 d . . . H226 H 0.1801 0.6334 0.1272 0.025 Uiso 1 1 calc R . . Fe1 Fe 0.22801(5) 0.39964(3) 0.183808(16) 0.01906(15) Uani 1 1 d . . . Br1 Br 0.69772(4) 0.45300(3) 0.170227(12) 0.02653(12) Uani 1 1 d . . . Pd1 Pd 0.55274(3) 0.459905(17) 0.115704(8) 0.01596(10) Uani 1 1 d . . . P1 P 0.64128(10) 0.36426(6) 0.07964(3) 0.0161(2) Uani 1 1 d . . . P2 P 0.41016(10) 0.54389(6) 0.14324(3) 0.0174(2) 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 C1 0.021(2) 0.021(2) 0.018(2) 0.0036(17) -0.0029(17) 0.0053(17) C2 0.022(2) 0.024(2) 0.015(2) 0.0027(17) -0.0019(17) -0.0052(18) C3 0.025(2) 0.039(3) 0.029(3) 0.010(2) -0.010(2) -0.008(2) C4 0.016(2) 0.044(3) 0.037(3) 0.015(2) 0.004(2) 0.011(2) C5 0.023(2) 0.025(2) 0.032(3) 0.004(2) 0.0059(19) 0.0067(19) C6 0.024(2) 0.032(3) 0.032(3) 0.011(2) -0.007(2) 0.000(2) C7 0.031(2) 0.025(2) 0.029(3) 0.004(2) 0.002(2) 0.008(2) C8 0.031(2) 0.020(2) 0.038(3) 0.008(2) 0.000(2) -0.002(2) C9 0.033(3) 0.037(3) 0.028(3) 0.012(2) 0.007(2) 0.002(2) C10 0.045(3) 0.034(3) 0.016(2) 0.0076(19) -0.005(2) 0.002(2) C111 0.0137(19) 0.017(2) 0.021(2) 0.0057(16) 0.0022(17) -0.0015(16) C112 0.016(2) 0.019(2) 0.015(2) 0.0025(16) 0.0012(16) -0.0041(16) C113 0.020(2) 0.019(2) 0.022(2) -0.0011(17) 0.0021(17) 0.0019(17) C114 0.016(2) 0.027(2) 0.022(2) 0.0084(18) -0.0049(17) -0.0048(17) C115 0.022(2) 0.029(2) 0.018(2) -0.0017(18) -0.0008(18) -0.0022(19) C116 0.022(2) 0.019(2) 0.023(2) -0.0031(18) -0.0017(18) 0.0008(17) C121 0.018(2) 0.0143(19) 0.020(2) 0.0033(16) 0.0019(17) 0.0058(16) C122 0.023(2) 0.025(2) 0.021(2) -0.0016(18) -0.0052(18) -0.0015(18) C123 0.027(2) 0.023(2) 0.019(2) -0.0004(18) 0.0027(19) 0.0025(19) C124 0.020(2) 0.027(2) 0.027(2) 0.0105(19) 0.0019(19) 0.0001(18) C125 0.018(2) 0.025(2) 0.029(2) 0.0024(19) -0.0036(19) -0.0040(18) C126 0.023(2) 0.017(2) 0.019(2) -0.0009(17) -0.0024(17) 0.0035(17) C131 0.0107(18) 0.017(2) 0.027(2) 0.0046(17) 0.0005(17) 0.0015(16) C132 0.031(2) 0.019(2) 0.023(2) 0.0046(18) -0.0005(19) 0.0023(19) C133 0.038(3) 0.018(2) 0.040(3) -0.002(2) 0.003(2) 0.001(2) C134 0.040(3) 0.019(2) 0.037(3) 0.011(2) 0.006(2) -0.001(2) C135 0.053(3) 0.034(3) 0.023(3) 0.010(2) 0.002(2) -0.003(2) C136 0.032(2) 0.022(2) 0.028(2) 0.0017(19) 0.003(2) 0.0037(19) C211 0.026(2) 0.023(2) 0.024(2) -0.0080(18) -0.0047(19) 0.0104(19) C212 0.030(3) 0.034(3) 0.037(3) -0.007(2) -0.011(2) -0.001(2) C213 0.040(3) 0.036(3) 0.061(4) -0.018(3) -0.021(3) -0.003(2) C214 0.060(4) 0.035(3) 0.041(3) -0.019(2) -0.025(3) 0.014(3) C215 0.063(4) 0.037(3) 0.028(3) -0.011(2) -0.012(3) 0.008(3) C216 0.041(3) 0.027(2) 0.026(3) -0.007(2) -0.005(2) 0.006(2) C221 0.024(2) 0.015(2) 0.019(2) -0.0044(17) -0.0051(18) -0.0020(17) C222 0.023(2) 0.022(2) 0.025(2) -0.0030(18) 0.0020(19) 0.0016(18) C223 0.029(2) 0.020(2) 0.026(2) 0.0005(18) 0.0043(19) -0.0037(18) C224 0.040(3) 0.017(2) 0.024(2) -0.0006(18) -0.007(2) 0.0034(19) C225 0.025(2) 0.023(2) 0.027(2) -0.0016(19) -0.0058(19) 0.0060(19) C226 0.021(2) 0.022(2) 0.020(2) -0.0046(17) 0.0006(18) 0.0001(17) Fe1 0.0180(3) 0.0211(3) 0.0181(3) 0.0021(2) 0.0010(2) 0.0005(2) Br1 0.0226(2) 0.0313(3) 0.0258(2) -0.00006(19) -0.00634(18) 0.00179(18) Pd1 0.01525(17) 0.01571(17) 0.01691(17) 0.00018(12) -0.00101(12) 0.00235(12) P1 0.0166(5) 0.0151(5) 0.0166(5) 0.0004(4) 0.0006(4) 0.0018(4) P2 0.0173(5) 0.0160(5) 0.0188(5) -0.0019(4) -0.0018(4) 0.0022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.432(6) . ? C1 C2 1.444(6) . ? C1 P2 1.798(4) . ? C1 Fe1 2.040(4) . ? C2 C3 1.407(6) . ? C2 Fe1 2.030(4) . ? C2 H2 0.9300 . ? C3 C4 1.405(7) . ? C3 Fe1 2.040(4) . ? C3 H3 0.9300 . ? C4 C5 1.420(6) . ? C4 Fe1 2.044(4) . ? C4 H4 0.9300 . ? C5 Fe1 2.046(4) . ? C5 H5 0.9300 . ? C6 C7 1.414(6) . ? C6 C10 1.418(6) . ? C6 Fe1 2.048(4) . ? C6 H6 0.9300 . ? C7 C8 1.407(6) . ? C7 Fe1 2.032(4) . ? C7 H7 0.9300 . ? C8 C9 1.414(7) . ? C8 Fe1 2.036(4) . ? C8 H8 0.9300 . ? C9 C10 1.411(7) . ? C9 Fe1 2.047(4) . ? C9 H9 0.9300 . ? C10 Fe1 2.057(4) . ? C10 H10 0.9300 . ? C111 C116 1.377(6) . ? C111 C112 1.410(6) . ? C111 P1 1.799(4) . ? C112 C113 1.383(6) . ? C112 Pd1 2.043(4) . ? C113 C114 1.385(6) . ? C113 H113 0.9300 . ? C114 C115 1.390(6) . ? C114 H114 0.9300 . ? C115 C116 1.383(6) . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? C121 C126 1.393(6) . ? C121 C122 1.397(6) . ? C121 P1 1.812(4) . ? C122 C123 1.378(6) . ? C122 H122 0.9300 . ? C123 C124 1.388(6) . ? C123 H123 0.9300 . ? C124 C125 1.372(6) . ? C124 H124 0.9300 . ? C125 C126 1.390(6) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C132 1.376(6) . ? C131 C136 1.387(6) . ? C131 P1 1.813(4) . ? C132 C133 1.385(6) . ? C132 H132 0.9300 . ? C133 C134 1.365(7) . ? C133 H133 0.9300 . ? C134 C135 1.382(7) . ? C134 H134 0.9300 . ? C135 C136 1.380(6) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? C211 C216 1.376(6) . ? C211 C212 1.392(6) . ? C211 P2 1.825(4) . ? C212 C213 1.392(7) . ? C212 H212 0.9300 . ? C213 C214 1.376(8) . ? C213 H213 0.9300 . ? C214 C215 1.370(7) . ? C214 H214 0.9300 . ? C215 C216 1.391(6) . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? C221 C222 1.396(6) . ? C221 C226 1.397(6) . ? C221 P2 1.829(4) . ? C222 C223 1.393(6) . ? C222 H222 0.9300 . ? C223 C224 1.380(6) . ? C223 H223 0.9300 . ? C224 C225 1.380(6) . ? C224 H224 0.9300 . ? C225 C226 1.394(6) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? Br1 Pd1 2.5013(5) . ? Pd1 P1 2.2987(10) . ? Pd1 P2 2.3116(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 106.4(4) . . ? C5 C1 P2 130.7(3) . . ? C2 C1 P2 122.8(3) . . ? C5 C1 Fe1 69.7(2) . . ? C2 C1 Fe1 68.8(2) . . ? P2 C1 Fe1 128.9(2) . . ? C3 C2 C1 108.3(4) . . ? C3 C2 Fe1 70.2(2) . . ? C1 C2 Fe1 69.6(2) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe1 C2 H2 125.9 . . ? C4 C3 C2 108.8(4) . . ? C4 C3 Fe1 70.0(3) . . ? C2 C3 Fe1 69.4(2) . . ? C4 C3 H3 125.6 . . ? C2 C3 H3 125.6 . . ? Fe1 C3 H3 126.6 . . ? C3 C4 C5 108.2(4) . . ? C3 C4 Fe1 69.7(3) . . ? C5 C4 Fe1 69.8(2) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 126.2 . . ? C4 C5 C1 108.4(4) . . ? C4 C5 Fe1 69.6(2) . . ? C1 C5 Fe1 69.3(2) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe1 C5 H5 126.9 . . ? C7 C6 C10 107.6(4) . . ? C7 C6 Fe1 69.1(2) . . ? C10 C6 Fe1 70.1(2) . . ? C7 C6 H6 126.2 . . ? C10 C6 H6 126.2 . . ? Fe1 C6 H6 126.1 . . ? C8 C7 C6 108.2(4) . . ? C8 C7 Fe1 69.9(3) . . ? C6 C7 Fe1 70.3(3) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? Fe1 C7 H7 125.4 . . ? C7 C8 C9 108.2(4) . . ? C7 C8 Fe1 69.6(2) . . ? C9 C8 Fe1 70.2(3) . . ? C7 C8 H8 125.9 . . ? C9 C8 H8 125.9 . . ? Fe1 C8 H8 125.9 . . ? C10 C9 C8 107.9(4) . . ? C10 C9 Fe1 70.3(3) . . ? C8 C9 Fe1 69.3(2) . . ? C10 C9 H9 126.1 . . ? C8 C9 H9 126.1 . . ? Fe1 C9 H9 125.9 . . ? C9 C10 C6 108.1(4) . . ? C9 C10 Fe1 69.5(3) . . ? C6 C10 Fe1 69.5(2) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe1 C10 H10 126.7 . . ? C116 C111 C112 122.9(4) . . ? C116 C111 P1 136.6(3) . . ? C112 C111 P1 100.0(3) . . ? C113 C112 C111 117.7(4) . . ? C113 C112 Pd1 136.5(3) . . ? C111 C112 Pd1 105.7(3) . . ? C112 C113 C114 119.6(4) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C113 C114 C115 121.8(4) . . ? C113 C114 H114 119.1 . . ? C115 C114 H114 119.1 . . ? C116 C115 C114 119.6(4) . . ? C116 C115 H115 120.2 . . ? C114 C115 H115 120.2 . . ? C111 C116 C115 118.3(4) . . ? C111 C116 H116 120.8 . . ? C115 C116 H116 120.8 . . ? C126 C121 C122 119.2(4) . . ? C126 C121 P1 118.8(3) . . ? C122 C121 P1 122.0(3) . . ? C123 C122 C121 120.5(4) . . ? C123 C122 H122 119.7 . . ? C121 C122 H122 119.7 . . ? C122 C123 C124 119.8(4) . . ? C122 C123 H123 120.1 . . ? C124 C123 H123 120.1 . . ? C125 C124 C123 120.3(4) . . ? C125 C124 H124 119.9 . . ? C123 C124 H124 119.9 . . ? C124 C125 C126 120.4(4) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 119.8(4) . . ? C125 C126 H126 120.1 . . ? C121 C126 H126 120.1 . . ? C132 C131 C136 119.0(4) . . ? C132 C131 P1 122.6(3) . . ? C136 C131 P1 118.3(3) . . ? C131 C132 C133 120.7(4) . . ? C131 C132 H132 119.6 . . ? C133 C132 H132 119.6 . . ? C134 C133 C132 120.1(4) . . ? C134 C133 H133 119.9 . . ? C132 C133 H133 119.9 . . ? C133 C134 C135 119.7(4) . . ? C133 C134 H134 120.2 . . ? C135 C134 H134 120.2 . . ? C136 C135 C134 120.4(4) . . ? C136 C135 H135 119.8 . . ? C134 C135 H135 119.8 . . ? C135 C136 C131 120.0(4) . . ? C135 C136 H136 120.0 . . ? C131 C136 H136 120.0 . . ? C216 C211 C212 118.8(4) . . ? C216 C211 P2 122.9(4) . . ? C212 C211 P2 118.2(3) . . ? C211 C212 C213 120.1(5) . . ? C211 C212 H212 119.9 . . ? C213 C212 H212 119.9 . . ? C214 C213 C212 120.1(5) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C215 C214 C213 120.1(5) . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 C215 C216 119.9(5) . . ? C214 C215 H215 120.0 . . ? C216 C215 H215 120.0 . . ? C211 C216 C215 120.9(5) . . ? C211 C216 H216 119.6 . . ? C215 C216 H216 119.6 . . ? C222 C221 C226 118.9(4) . . ? C222 C221 P2 118.9(3) . . ? C226 C221 P2 122.2(3) . . ? C223 C222 C221 120.6(4) . . ? C223 C222 H222 119.7 . . ? C221 C222 H222 119.7 . . ? C224 C223 C222 119.9(4) . . ? C224 C223 H223 120.0 . . ? C222 C223 H223 120.0 . . ? C225 C224 C223 120.2(4) . . ? C225 C224 H224 119.9 . . ? C223 C224 H224 119.9 . . ? C224 C225 C226 120.5(4) . . ? C224 C225 H225 119.8 . . ? C226 C225 H225 119.8 . . ? C225 C226 C221 119.9(4) . . ? C225 C226 H226 120.0 . . ? C221 C226 H226 120.0 . . ? C2 Fe1 C7 105.60(18) . . ? C2 Fe1 C8 117.86(18) . . ? C7 Fe1 C8 40.48(18) . . ? C2 Fe1 C1 41.55(16) . . ? C7 Fe1 C1 121.90(17) . . ? C8 Fe1 C1 155.41(18) . . ? C2 Fe1 C3 40.44(17) . . ? C7 Fe1 C3 121.1(2) . . ? C8 Fe1 C3 103.74(19) . . ? C1 Fe1 C3 68.95(17) . . ? C2 Fe1 C4 68.29(18) . . ? C7 Fe1 C4 157.3(2) . . ? C8 Fe1 C4 121.38(19) . . ? C1 Fe1 C4 68.97(17) . . ? C3 Fe1 C4 40.3(2) . . ? C2 Fe1 C5 68.79(18) . . ? C7 Fe1 C5 159.66(18) . . ? C8 Fe1 C5 159.67(18) . . ? C1 Fe1 C5 41.04(16) . . ? C3 Fe1 C5 68.11(19) . . ? C4 Fe1 C5 40.62(18) . . ? C2 Fe1 C9 153.25(18) . . ? C7 Fe1 C9 68.14(18) . . ? C8 Fe1 C9 40.51(19) . . ? C1 Fe1 C9 163.56(18) . . ? C3 Fe1 C9 118.89(19) . . ? C4 Fe1 C9 106.92(19) . . ? C5 Fe1 C9 125.71(18) . . ? C2 Fe1 C6 125.05(18) . . ? C7 Fe1 C6 40.54(18) . . ? C8 Fe1 C6 68.05(18) . . ? C1 Fe1 C6 110.16(17) . . ? C3 Fe1 C6 159.3(2) . . ? C4 Fe1 C6 160.2(2) . . ? C5 Fe1 C6 125.73(19) . . ? C9 Fe1 C6 68.01(18) . . ? C2 Fe1 C10 163.57(18) . . ? C7 Fe1 C10 67.96(19) . . ? C8 Fe1 C10 67.79(19) . . ? C1 Fe1 C10 127.85(18) . . ? C3 Fe1 C10 155.92(19) . . ? C4 Fe1 C10 123.5(2) . . ? C5 Fe1 C10 111.67(19) . . ? C9 Fe1 C10 40.20(19) . . ? C6 Fe1 C10 40.42(18) . . ? C112 Pd1 P1 69.05(11) . . ? C112 Pd1 P2 96.42(11) . . ? P1 Pd1 P2 163.07(4) . . ? C112 Pd1 Br1 168.58(11) . . ? P1 Pd1 Br1 99.58(3) . . ? P2 Pd1 Br1 94.98(3) . . ? C111 P1 C121 106.95(18) . . ? C111 P1 C131 112.57(18) . . ? C121 P1 C131 105.73(18) . . ? C111 P1 Pd1 84.47(13) . . ? C121 P1 Pd1 123.77(13) . . ? C131 P1 Pd1 120.36(14) . . ? C1 P2 C211 107.9(2) . . ? C1 P2 C221 104.49(18) . . ? C211 P2 C221 101.78(19) . . ? C1 P2 Pd1 110.83(14) . . ? C211 P2 Pd1 116.72(14) . . ? C221 P2 Pd1 114.03(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.1(5) . . . . ? P2 C1 C2 C3 -176.7(3) . . . . ? Fe1 C1 C2 C3 59.8(3) . . . . ? C5 C1 C2 Fe1 -59.9(3) . . . . ? P2 C1 C2 Fe1 123.5(3) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? Fe1 C2 C3 C4 59.1(3) . . . . ? C1 C2 C3 Fe1 -59.4(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? Fe1 C3 C4 C5 59.4(3) . . . . ? C2 C3 C4 Fe1 -58.7(3) . . . . ? C3 C4 C5 C1 -0.8(5) . . . . ? Fe1 C4 C5 C1 58.6(3) . . . . ? C3 C4 C5 Fe1 -59.3(3) . . . . ? C2 C1 C5 C4 0.5(5) . . . . ? P2 C1 C5 C4 176.8(3) . . . . ? Fe1 C1 C5 C4 -58.8(3) . . . . ? C2 C1 C5 Fe1 59.3(3) . . . . ? P2 C1 C5 Fe1 -124.4(4) . . . . ? C10 C6 C7 C8 -0.1(5) . . . . ? Fe1 C6 C7 C8 -59.9(3) . . . . ? C10 C6 C7 Fe1 59.8(3) . . . . ? C6 C7 C8 C9 0.4(5) . . . . ? Fe1 C7 C8 C9 -59.8(3) . . . . ? C6 C7 C8 Fe1 60.2(3) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? Fe1 C8 C9 C10 -60.0(3) . . . . ? C7 C8 C9 Fe1 59.4(3) . . . . ? C8 C9 C10 C6 0.5(5) . . . . ? Fe1 C9 C10 C6 -58.9(3) . . . . ? C8 C9 C10 Fe1 59.4(3) . . . . ? C7 C6 C10 C9 -0.2(5) . . . . ? Fe1 C6 C10 C9 58.9(3) . . . . ? C7 C6 C10 Fe1 -59.2(3) . . . . ? C116 C111 C112 C113 -2.1(6) . . . . ? P1 C111 C112 C113 170.8(3) . . . . ? C116 C111 C112 Pd1 178.9(3) . . . . ? P1 C111 C112 Pd1 -8.2(3) . . . . ? C111 C112 C113 C114 0.0(6) . . . . ? Pd1 C112 C113 C114 178.5(3) . . . . ? C112 C113 C114 C115 1.8(6) . . . . ? C113 C114 C115 C116 -1.5(6) . . . . ? C112 C111 C116 C115 2.4(6) . . . . ? P1 C111 C116 C115 -167.4(3) . . . . ? C114 C115 C116 C111 -0.6(6) . . . . ? C126 C121 C122 C123 -0.6(6) . . . . ? P1 C121 C122 C123 178.5(3) . . . . ? C121 C122 C123 C124 0.2(6) . . . . ? C122 C123 C124 C125 0.4(6) . . . . ? C123 C124 C125 C126 -0.6(6) . . . . ? C124 C125 C126 C121 0.2(6) . . . . ? C122 C121 C126 C125 0.4(6) . . . . ? P1 C121 C126 C125 -178.8(3) . . . . ? C136 C131 C132 C133 1.1(6) . . . . ? P1 C131 C132 C133 -177.0(3) . . . . ? C131 C132 C133 C134 0.2(7) . . . . ? C132 C133 C134 C135 -1.8(7) . . . . ? C133 C134 C135 C136 2.1(8) . . . . ? C134 C135 C136 C131 -0.8(7) . . . . ? C132 C131 C136 C135 -0.8(6) . . . . ? P1 C131 C136 C135 177.3(4) . . . . ? C216 C211 C212 C213 -1.1(7) . . . . ? P2 C211 C212 C213 -178.6(4) . . . . ? C211 C212 C213 C214 -0.5(8) . . . . ? C212 C213 C214 C215 1.6(8) . . . . ? C213 C214 C215 C216 -1.2(8) . . . . ? C212 C211 C216 C215 1.5(7) . . . . ? P2 C211 C216 C215 178.9(4) . . . . ? C214 C215 C216 C211 -0.4(7) . . . . ? C226 C221 C222 C223 1.4(6) . . . . ? P2 C221 C222 C223 -177.5(3) . . . . ? C221 C222 C223 C224 -1.5(6) . . . . ? C222 C223 C224 C225 0.4(6) . . . . ? C223 C224 C225 C226 0.6(6) . . . . ? C224 C225 C226 C221 -0.7(6) . . . . ? C222 C221 C226 C225 -0.3(6) . . . . ? P2 C221 C226 C225 178.5(3) . . . . ? C3 C2 Fe1 C7 119.9(3) . . . . ? C1 C2 Fe1 C7 -120.8(3) . . . . ? C3 C2 Fe1 C8 78.1(3) . . . . ? C1 C2 Fe1 C8 -162.6(2) . . . . ? C3 C2 Fe1 C1 -119.3(4) . . . . ? C1 C2 Fe1 C3 119.3(4) . . . . ? C3 C2 Fe1 C4 -36.9(3) . . . . ? C1 C2 Fe1 C4 82.4(3) . . . . ? C3 C2 Fe1 C5 -80.7(3) . . . . ? C1 C2 Fe1 C5 38.6(2) . . . . ? C3 C2 Fe1 C9 47.7(5) . . . . ? C1 C2 Fe1 C9 167.0(4) . . . . ? C3 C2 Fe1 C6 159.7(3) . . . . ? C1 C2 Fe1 C6 -81.0(3) . . . . ? C3 C2 Fe1 C10 -175.6(6) . . . . ? C1 C2 Fe1 C10 -56.3(7) . . . . ? C8 C7 Fe1 C2 -114.8(3) . . . . ? C6 C7 Fe1 C2 126.2(3) . . . . ? C6 C7 Fe1 C8 -118.9(4) . . . . ? C8 C7 Fe1 C1 -157.0(3) . . . . ? C6 C7 Fe1 C1 84.1(3) . . . . ? C8 C7 Fe1 C3 -73.8(3) . . . . ? C6 C7 Fe1 C3 167.3(3) . . . . ? C8 C7 Fe1 C4 -43.9(6) . . . . ? C6 C7 Fe1 C4 -162.9(4) . . . . ? C8 C7 Fe1 C5 174.3(5) . . . . ? C6 C7 Fe1 C5 55.3(6) . . . . ? C8 C7 Fe1 C9 37.6(3) . . . . ? C6 C7 Fe1 C9 -81.3(3) . . . . ? C8 C7 Fe1 C6 118.9(4) . . . . ? C8 C7 Fe1 C10 81.2(3) . . . . ? C6 C7 Fe1 C10 -37.8(3) . . . . ? C7 C8 Fe1 C2 81.3(3) . . . . ? C9 C8 Fe1 C2 -159.4(3) . . . . ? C9 C8 Fe1 C7 119.2(4) . . . . ? C7 C8 Fe1 C1 52.9(5) . . . . ? C9 C8 Fe1 C1 172.1(4) . . . . ? C7 C8 Fe1 C3 122.1(3) . . . . ? C9 C8 Fe1 C3 -118.6(3) . . . . ? C7 C8 Fe1 C4 161.7(3) . . . . ? C9 C8 Fe1 C4 -79.1(3) . . . . ? C7 C8 Fe1 C5 -174.3(5) . . . . ? C9 C8 Fe1 C5 -55.0(6) . . . . ? C7 C8 Fe1 C9 -119.2(4) . . . . ? C7 C8 Fe1 C6 -37.8(3) . . . . ? C9 C8 Fe1 C6 81.4(3) . . . . ? C7 C8 Fe1 C10 -81.6(3) . . . . ? C9 C8 Fe1 C10 37.6(3) . . . . ? C5 C1 Fe1 C2 117.7(3) . . . . ? P2 C1 Fe1 C2 -115.8(4) . . . . ? C5 C1 Fe1 C7 -165.2(3) . . . . ? C2 C1 Fe1 C7 77.0(3) . . . . ? P2 C1 Fe1 C7 -38.7(4) . . . . ? C5 C1 Fe1 C8 157.2(4) . . . . ? C2 C1 Fe1 C8 39.5(5) . . . . ? P2 C1 Fe1 C8 -76.3(5) . . . . ? C5 C1 Fe1 C3 80.4(3) . . . . ? C2 C1 Fe1 C3 -37.3(3) . . . . ? P2 C1 Fe1 C3 -153.1(3) . . . . ? C5 C1 Fe1 C4 37.2(3) . . . . ? C2 C1 Fe1 C4 -80.6(3) . . . . ? P2 C1 Fe1 C4 163.7(3) . . . . ? C2 C1 Fe1 C5 -117.7(3) . . . . ? P2 C1 Fe1 C5 126.5(4) . . . . ? C5 C1 Fe1 C9 -41.2(7) . . . . ? C2 C1 Fe1 C9 -159.0(6) . . . . ? P2 C1 Fe1 C9 85.3(7) . . . . ? C5 C1 Fe1 C6 -121.7(3) . . . . ? C2 C1 Fe1 C6 120.5(3) . . . . ? P2 C1 Fe1 C6 4.8(3) . . . . ? C5 C1 Fe1 C10 -79.6(3) . . . . ? C2 C1 Fe1 C10 162.7(3) . . . . ? P2 C1 Fe1 C10 46.9(4) . . . . ? C4 C3 Fe1 C2 -120.2(4) . . . . ? C4 C3 Fe1 C7 162.7(3) . . . . ? C2 C3 Fe1 C7 -77.1(3) . . . . ? C4 C3 Fe1 C8 122.7(3) . . . . ? C2 C3 Fe1 C8 -117.0(3) . . . . ? C4 C3 Fe1 C1 -81.9(3) . . . . ? C2 C3 Fe1 C1 38.3(3) . . . . ? C2 C3 Fe1 C4 120.2(4) . . . . ? C4 C3 Fe1 C5 -37.7(3) . . . . ? C2 C3 Fe1 C5 82.6(3) . . . . ? C4 C3 Fe1 C9 82.1(3) . . . . ? C2 C3 Fe1 C9 -157.7(3) . . . . ? C4 C3 Fe1 C6 -173.4(5) . . . . ? C2 C3 Fe1 C6 -53.2(6) . . . . ? C4 C3 Fe1 C10 56.7(6) . . . . ? C2 C3 Fe1 C10 176.9(4) . . . . ? C3 C4 Fe1 C2 37.1(3) . . . . ? C5 C4 Fe1 C2 -82.3(3) . . . . ? C3 C4 Fe1 C7 -41.3(6) . . . . ? C5 C4 Fe1 C7 -160.7(4) . . . . ? C3 C4 Fe1 C8 -73.2(3) . . . . ? C5 C4 Fe1 C8 167.4(3) . . . . ? C3 C4 Fe1 C1 81.9(3) . . . . ? C5 C4 Fe1 C1 -37.5(3) . . . . ? C5 C4 Fe1 C3 -119.4(4) . . . . ? C3 C4 Fe1 C5 119.4(4) . . . . ? C3 C4 Fe1 C9 -115.0(3) . . . . ? C5 C4 Fe1 C9 125.6(3) . . . . ? C3 C4 Fe1 C6 173.1(5) . . . . ? C5 C4 Fe1 C6 53.7(6) . . . . ? C3 C4 Fe1 C10 -155.9(3) . . . . ? C5 C4 Fe1 C10 84.7(3) . . . . ? C4 C5 Fe1 C2 81.0(3) . . . . ? C1 C5 Fe1 C2 -39.0(2) . . . . ? C4 C5 Fe1 C7 158.4(5) . . . . ? C1 C5 Fe1 C7 38.4(6) . . . . ? C4 C5 Fe1 C8 -32.3(7) . . . . ? C1 C5 Fe1 C8 -152.3(5) . . . . ? C4 C5 Fe1 C1 120.0(4) . . . . ? C4 C5 Fe1 C3 37.3(3) . . . . ? C1 C5 Fe1 C3 -82.7(3) . . . . ? C1 C5 Fe1 C4 -120.0(4) . . . . ? C4 C5 Fe1 C9 -73.3(3) . . . . ? C1 C5 Fe1 C9 166.7(3) . . . . ? C4 C5 Fe1 C6 -160.4(3) . . . . ? C1 C5 Fe1 C6 79.6(3) . . . . ? C4 C5 Fe1 C10 -116.7(3) . . . . ? C1 C5 Fe1 C10 123.3(3) . . . . ? C10 C9 Fe1 C2 162.5(4) . . . . ? C8 C9 Fe1 C2 43.6(5) . . . . ? C10 C9 Fe1 C7 81.3(3) . . . . ? C8 C9 Fe1 C7 -37.6(3) . . . . ? C10 C9 Fe1 C8 118.9(4) . . . . ? C10 C9 Fe1 C1 -49.4(7) . . . . ? C8 C9 Fe1 C1 -168.3(5) . . . . ? C10 C9 Fe1 C3 -164.3(3) . . . . ? C8 C9 Fe1 C3 76.8(3) . . . . ? C10 C9 Fe1 C4 -122.3(3) . . . . ? C8 C9 Fe1 C4 118.8(3) . . . . ? C10 C9 Fe1 C5 -81.6(3) . . . . ? C8 C9 Fe1 C5 159.5(3) . . . . ? C10 C9 Fe1 C6 37.4(3) . . . . ? C8 C9 Fe1 C6 -81.5(3) . . . . ? C8 C9 Fe1 C10 -118.9(4) . . . . ? C7 C6 Fe1 C2 -71.7(3) . . . . ? C10 C6 Fe1 C2 169.5(3) . . . . ? C10 C6 Fe1 C7 -118.8(4) . . . . ? C7 C6 Fe1 C8 37.8(3) . . . . ? C10 C6 Fe1 C8 -81.1(3) . . . . ? C7 C6 Fe1 C1 -115.9(3) . . . . ? C10 C6 Fe1 C1 125.2(3) . . . . ? C7 C6 Fe1 C3 -32.3(6) . . . . ? C10 C6 Fe1 C3 -151.1(5) . . . . ? C7 C6 Fe1 C4 160.3(5) . . . . ? C10 C6 Fe1 C4 41.5(7) . . . . ? C7 C6 Fe1 C5 -159.4(3) . . . . ? C10 C6 Fe1 C5 81.8(3) . . . . ? C7 C6 Fe1 C9 81.6(3) . . . . ? C10 C6 Fe1 C9 -37.2(3) . . . . ? C7 C6 Fe1 C10 118.8(4) . . . . ? C9 C10 Fe1 C2 -151.5(6) . . . . ? C6 C10 Fe1 C2 -31.8(8) . . . . ? C9 C10 Fe1 C7 -81.8(3) . . . . ? C6 C10 Fe1 C7 37.9(3) . . . . ? C9 C10 Fe1 C8 -37.9(3) . . . . ? C6 C10 Fe1 C8 81.8(3) . . . . ? C9 C10 Fe1 C1 164.2(3) . . . . ? C6 C10 Fe1 C1 -76.2(3) . . . . ? C9 C10 Fe1 C3 35.6(6) . . . . ? C6 C10 Fe1 C3 155.2(4) . . . . ? C9 C10 Fe1 C4 76.0(3) . . . . ? C6 C10 Fe1 C4 -164.4(3) . . . . ? C9 C10 Fe1 C5 120.2(3) . . . . ? C6 C10 Fe1 C5 -120.2(3) . . . . ? C6 C10 Fe1 C9 119.6(4) . . . . ? C9 C10 Fe1 C6 -119.6(4) . . . . ? C113 C112 Pd1 P1 -171.9(4) . . . . ? C111 C112 Pd1 P1 6.7(2) . . . . ? C113 C112 Pd1 P2 17.0(4) . . . . ? C111 C112 Pd1 P2 -164.3(2) . . . . ? C113 C112 Pd1 Br1 -166.3(3) . . . . ? C111 C112 Pd1 Br1 12.3(7) . . . . ? C116 C111 P1 C121 54.7(5) . . . . ? C112 C111 P1 C121 -116.6(3) . . . . ? C116 C111 P1 C131 -61.0(5) . . . . ? C112 C111 P1 C131 127.7(3) . . . . ? C116 C111 P1 Pd1 178.3(4) . . . . ? C112 C111 P1 Pd1 7.0(2) . . . . ? C126 C121 P1 C111 136.5(3) . . . . ? C122 C121 P1 C111 -42.7(4) . . . . ? C126 C121 P1 C131 -103.3(3) . . . . ? C122 C121 P1 C131 77.5(4) . . . . ? C126 C121 P1 Pd1 41.7(4) . . . . ? C122 C121 P1 Pd1 -137.4(3) . . . . ? C132 C131 P1 C111 56.8(4) . . . . ? C136 C131 P1 C111 -121.2(3) . . . . ? C132 C131 P1 C121 -59.6(4) . . . . ? C136 C131 P1 C121 122.3(3) . . . . ? C132 C131 P1 Pd1 153.9(3) . . . . ? C136 C131 P1 Pd1 -24.2(4) . . . . ? C112 Pd1 P1 C111 -5.09(16) . . . . ? P2 Pd1 P1 C111 27.06(19) . . . . ? Br1 Pd1 P1 C111 176.03(12) . . . . ? C112 Pd1 P1 C121 101.62(19) . . . . ? P2 Pd1 P1 C121 133.78(19) . . . . ? Br1 Pd1 P1 C121 -77.26(16) . . . . ? C112 Pd1 P1 C131 -118.06(19) . . . . ? P2 Pd1 P1 C131 -85.9(2) . . . . ? Br1 Pd1 P1 C131 63.06(15) . . . . ? C5 C1 P2 C211 26.4(4) . . . . ? C2 C1 P2 C211 -157.9(3) . . . . ? Fe1 C1 P2 C211 -69.7(3) . . . . ? C5 C1 P2 C221 -81.4(4) . . . . ? C2 C1 P2 C221 94.3(4) . . . . ? Fe1 C1 P2 C221 -177.5(3) . . . . ? C5 C1 P2 Pd1 155.3(4) . . . . ? C2 C1 P2 Pd1 -29.0(4) . . . . ? Fe1 C1 P2 Pd1 59.2(3) . . . . ? C216 C211 P2 C1 22.4(4) . . . . ? C212 C211 P2 C1 -160.2(3) . . . . ? C216 C211 P2 C221 132.1(4) . . . . ? C212 C211 P2 C221 -50.6(4) . . . . ? C216 C211 P2 Pd1 -103.1(4) . . . . ? C212 C211 P2 Pd1 74.2(4) . . . . ? C222 C221 P2 C1 -161.0(3) . . . . ? C226 C221 P2 C1 20.2(4) . . . . ? C222 C221 P2 C211 86.7(3) . . . . ? C226 C221 P2 C211 -92.1(4) . . . . ? C222 C221 P2 Pd1 -39.8(4) . . . . ? C226 C221 P2 Pd1 141.4(3) . . . . ? C112 Pd1 P2 C1 68.23(17) . . . . ? P1 Pd1 P2 C1 38.2(2) . . . . ? Br1 Pd1 P2 C1 -111.10(14) . . . . ? C112 Pd1 P2 C211 -167.7(2) . . . . ? P1 Pd1 P2 C211 162.30(19) . . . . ? Br1 Pd1 P2 C211 12.98(17) . . . . ? C112 Pd1 P2 C221 -49.34(18) . . . . ? P1 Pd1 P2 C221 -79.4(2) . . . . ? Br1 Pd1 P2 C221 131.33(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.721 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.100