# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Murielle Chavarot-Kerlidou' _publ_contact_author_email MURIELLE.CHAVAROT-KERLIDOU@UPMC.FR _publ_section_title ; First example of an enantiopure planar chiral ligand built on a ((eta)5-cyclohexadienyl)Mn(CO)3 scaffold ; loop_ _publ_author_name 'Murielle Chavarot-Kerlidou' 'Derya Cetiner' 'Patrick Herson' 'Beatrice Jacques' 'Elina Payet' ; E.Rose ; 'Francoise Rose-munch' 'Jean-Philippe Tranchier' # Attachment 'ccdc652209.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 652209' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; Because desorder, the phenyl ring C(7)-C(12) is refined as a rigid-body with an mean anisotropic thermal parameter. One water molecule in desorder over two sites at 50% occupancy per site is found.These half water molecules are refined isotropicaly.No hydrogen is found in the difference map. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 31.6307(18) _cell_length_b 16.4534(17) _cell_length_c 12.6803(13) _cell_angle_alpha 90 _cell_angle_beta 107.395(6) _cell_angle_gamma 90 _cell_volume 6297.4(10) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' 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 -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 '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' _cell_formula_units_Z 8 # Given Formula = C31 H29 Cl1 Mn1 O5 P1 Pd1 # Dc = 1.50 Fooo = 2848.00 Mu = 11.44 M = 709.32 # Found Formula = C31 H27 Cl1 Mn1 O5 P1 Pd1 # Dc = 1.49 FOOO = 2848.00 Mu = 11.44 M = 707.31 _chemical_formula_sum 'C31 H29 Cl1 Mn1 O5 P1 Pd1' _chemical_formula_moiety 'C31 H27 Cl1 Mn1 O4 P1 Pd1,H2 O1' _chemical_compound_source ? _chemical_formula_weight 709.32 _cell_measurement_reflns_used 95 _cell_measurement_theta_min 4 _cell_measurement_theta_max 23 _cell_measurement_temperature 250 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 1.144 # Sheldrick geometric approximatio 0.89 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.89 # 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 & \w scans' # 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 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 250 _diffrn_reflns_number 42305 _reflns_number_total 9115 _diffrn_reflns_av_R_equivalents 0.043 # Number of reflections with Friedels Law is 9115 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9187 _diffrn_reflns_theta_min 2.535 _diffrn_reflns_theta_max 30.003 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.003 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -44 _reflns_limit_h_max 42 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.37 _refine_diff_density_max 1.91 # 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>3.0\s(I) _refine_ls_number_reflns 3875 _refine_ls_number_restraints 0 _refine_ls_number_parameters 308 _oxford_refine_ls_R_factor_ref 0.0599 _refine_ls_wR_factor_ref 0.0703 _refine_ls_goodness_of_fit_ref 1.4488 _refine_ls_shift/su_max 0.001089 # The values computed from all data _oxford_reflns_number_all 9113 _refine_ls_R_factor_all 0.1285 _refine_ls_wR_factor_all 0.1155 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4550 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_gt 0.0734 # 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 refu # 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: 1.74 -0.219 1.17 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Pd1 Pd 0.210404(19) 0.32384(4) 0.88104(5) 0.0330 1.0000 Uani . . . . . . . Mn1 Mn 0.07299(4) 0.35426(7) 0.67264(9) 0.0334 1.0000 Uani . . . . . . . Cl1 Cl 0.16890(8) 0.31470(15) 1.00992(17) 0.0512 1.0000 Uani . . . . . . . P1 P 0.17287(6) 0.23653(11) 0.73854(15) 0.0291 1.0000 Uani . . . . . . . C1 C 0.0863(3) 0.3933(5) 0.5182(6) 0.0334 1.0000 Uani . . . . . . . C2 C 0.1252(2) 0.3605(4) 0.5916(5) 0.0275 1.0000 Uani . . . . . . . C3 C 0.1237(2) 0.2805(4) 0.6388(5) 0.0286 1.0000 Uani . . . . . . . C4 C 0.0813(2) 0.2400(4) 0.6024(6) 0.0341 1.0000 Uani . . . . . . . C5 C 0.0451(3) 0.2746(5) 0.5252(6) 0.0381 1.0000 Uani . . . . . . . C6 C 0.0515(2) 0.3382(5) 0.4451(6) 0.0350 1.0000 Uani . . . . . . . C13 C 0.1658(3) 0.4854(5) 0.6042(7) 0.0488 1.0000 Uani . . . . . . . C21 C 0.1514(3) 0.1375(5) 0.7788(7) 0.0441 1.0000 Uani . . . . . . . C22 C 0.1570(3) 0.0663(6) 0.7262(9) 0.0569 1.0000 Uani . . . . . . . C23 C 0.1437(4) -0.0049(6) 0.7624(11) 0.0731 1.0000 Uani . . . . . . . C24 C 0.1250(4) -0.0052(7) 0.8499(12) 0.0782 1.0000 Uani . . . . . . . C25 C 0.1190(4) 0.0678(7) 0.8968(9) 0.0642 1.0000 Uani . . . . . . . C26 C 0.1325(3) 0.1392(6) 0.8594(8) 0.0551 1.0000 Uani . . . . . . . C31 C 0.2059(3) 0.2008(4) 0.6508(6) 0.0358 1.0000 Uani . . . . . . . C32 C 0.2490(3) 0.1751(5) 0.7026(7) 0.0463 1.0000 Uani . . . . . . . C33 C 0.2750(3) 0.1424(6) 0.6399(10) 0.0577 1.0000 Uani . . . . . . . C34 C 0.2563(4) 0.1371(6) 0.5255(9) 0.0578 1.0000 Uani . . . . . . . C35 C 0.2141(3) 0.1616(6) 0.4742(8) 0.0546 1.0000 Uani . . . . . . . C36 C 0.1884(3) 0.1943(5) 0.5369(7) 0.0429 1.0000 Uani . . . . . . . C41 C 0.1047(3) 0.4281(6) 0.7715(7) 0.0475 1.0000 Uani . . . . . . . C42 C 0.0583(3) 0.3023(6) 0.7835(7) 0.0497 1.0000 Uani . . . . . . . C43 C 0.0227(3) 0.4149(5) 0.6324(6) 0.0426 1.0000 Uani . . . . . . . C50 C 0.2578(3) 0.4104(6) 0.9858(8) 0.0579 1.0000 Uani . . . . . . . C51 C 0.2553(4) 0.4206(7) 0.8770(10) 0.0714 1.0000 Uani . . . . . . . C52 C 0.2607(3) 0.3579(6) 0.8094(9) 0.0583 1.0000 Uani . . . . . . . O1 O 0.16459(17) 0.4004(3) 0.6325(4) 0.0352 1.0000 Uani . . . . . . . O41 O 0.1246(3) 0.4764(4) 0.8303(6) 0.0752 1.0000 Uani . . . . . . . O42 O 0.0491(2) 0.2713(5) 0.8542(5) 0.0704 1.0000 Uani . . . . . . . O43 O -0.0084(2) 0.4531(5) 0.6077(6) 0.0645 1.0000 Uani . . . . . . . O100 O 0.0013(13) 0.087(2) 0.639(3) 0.205(14) 0.5000 Uiso . . . . . . . O200 O 0.0388(13) 0.041(2) 0.508(3) 0.194(13) 0.5000 Uiso . . . . . . . C7 C 0.0608 0.3081 0.3399 0.0868 1.0000 Uani . . . . . . . C8 C 0.0648 0.3654 0.2629 0.0868 1.0000 Uani . . . . . . . C9 C 0.0755 0.3409 0.1692 0.0868 1.0000 Uani . . . . . . . C10 C 0.0823 0.2590 0.1525 0.0868 1.0000 Uani . . . . . . . C11 C 0.0783 0.2017 0.2295 0.0868 1.0000 Uani . . . . . . . C12 C 0.0676 0.2262 0.3232 0.0868 1.0000 Uani . . . . . . . H11 H 0.0824 0.4544 0.5143 0.107(9) 1.0000 Uiso . . . . . . . H41 H 0.0781 0.1847 0.6339 0.107(9) 1.0000 Uiso . . . . . . . H51 H 0.0137 0.2572 0.5213 0.107(9) 1.0000 Uiso . . . . . . . H61 H 0.0232 0.3703 0.4178 0.107(9) 1.0000 Uiso . . . . . . . H81 H 0.0602 0.4214 0.2744 0.107(9) 1.0000 Uiso . . . . . . . H91 H 0.0782 0.3801 0.1166 0.107(9) 1.0000 Uiso . . . . . . . H101 H 0.0896 0.2423 0.0884 0.107(9) 1.0000 Uiso . . . . . . . H111 H 0.0829 0.1457 0.2180 0.107(9) 1.0000 Uiso . . . . . . . H121 H 0.0649 0.1870 0.3758 0.107(9) 1.0000 Uiso . . . . . . . H131 H 0.1967 0.5074 0.6397 0.107(9) 1.0000 Uiso . . . . . . . H132 H 0.1445 0.5173 0.6324 0.107(9) 1.0000 Uiso . . . . . . . H133 H 0.1583 0.4922 0.5225 0.107(9) 1.0000 Uiso . . . . . . . H221 H 0.1701 0.0672 0.6622 0.107(9) 1.0000 Uiso . . . . . . . H231 H 0.1486 -0.0579 0.7282 0.107(9) 1.0000 Uiso . . . . . . . H241 H 0.1163 -0.0584 0.8774 0.107(9) 1.0000 Uiso . . . . . . . H251 H 0.1043 0.0681 0.9575 0.107(9) 1.0000 Uiso . . . . . . . H261 H 0.1282 0.1933 0.8943 0.107(9) 1.0000 Uiso . . . . . . . H321 H 0.2616 0.1780 0.7855 0.107(9) 1.0000 Uiso . . . . . . . H331 H 0.3065 0.1242 0.6777 0.107(9) 1.0000 Uiso . . . . . . . H341 H 0.2745 0.1133 0.4796 0.107(9) 1.0000 Uiso . . . . . . . H351 H 0.2014 0.1574 0.3913 0.107(9) 1.0000 Uiso . . . . . . . H361 H 0.1569 0.2132 0.4986 0.107(9) 1.0000 Uiso . . . . . . . H501 H 0.2536 0.4575 1.0322 0.107(9) 1.0000 Uiso . . . . . . . H502 H 0.2632 0.3548 1.0198 0.107(9) 1.0000 Uiso . . . . . . . H511 H 0.2501 0.4777 0.8442 0.107(9) 1.0000 Uiso . . . . . . . H521 H 0.2668 0.3010 0.8410 0.107(9) 1.0000 Uiso . . . . . . . H522 H 0.2596 0.3672 0.7308 0.107(9) 1.0000 Uiso . . . . . . . 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 0.0348(3) 0.0347(3) 0.0289(3) 0.0011(3) 0.0087(2) 0.0069(3) Mn1 0.0357(6) 0.0417(6) 0.0260(5) 0.0036(5) 0.0141(5) 0.0113(5) Cl1 0.0613(13) 0.0607(14) 0.0380(10) -0.0033(10) 0.0248(9) 0.0048(11) P1 0.0332(9) 0.0302(9) 0.0258(8) 0.0033(7) 0.0116(7) 0.0067(7) C1 0.040(4) 0.037(4) 0.025(3) 0.004(3) 0.014(3) 0.006(3) C2 0.034(4) 0.028(3) 0.021(3) -0.001(3) 0.011(3) 0.002(3) C3 0.036(4) 0.028(4) 0.025(3) 0.001(3) 0.013(3) 0.004(3) C4 0.032(4) 0.033(4) 0.039(4) 0.000(3) 0.014(3) 0.000(3) C5 0.035(4) 0.047(5) 0.034(4) -0.002(3) 0.013(3) -0.006(3) C6 0.031(3) 0.048(5) 0.025(3) 0.004(3) 0.007(3) 0.003(3) C13 0.061(6) 0.037(4) 0.044(5) 0.007(4) 0.008(4) -0.008(4) C21 0.033(4) 0.052(5) 0.039(4) -0.012(4) -0.002(3) 0.019(4) C22 0.065(6) 0.041(5) 0.070(6) 0.005(4) 0.029(5) 0.000(4) C23 0.091(8) 0.035(5) 0.108(9) 0.008(5) 0.051(7) 0.002(5) C24 0.086(8) 0.047(6) 0.113(10) 0.031(6) 0.047(8) -0.005(5) C25 0.059(6) 0.071(7) 0.069(6) 0.023(6) 0.030(5) -0.005(5) C26 0.045(5) 0.064(6) 0.056(5) 0.032(5) 0.014(4) -0.007(4) C31 0.048(4) 0.025(3) 0.039(4) 0.003(3) 0.020(3) 0.002(3) C32 0.052(5) 0.038(4) 0.056(5) 0.008(4) 0.025(4) 0.012(4) C33 0.055(5) 0.039(5) 0.096(8) 0.011(5) 0.047(6) 0.016(4) C34 0.079(7) 0.040(5) 0.076(7) -0.008(5) 0.056(6) -0.002(5) C35 0.068(6) 0.057(6) 0.052(5) -0.015(4) 0.037(5) -0.004(5) C36 0.055(5) 0.043(5) 0.039(4) -0.012(3) 0.026(4) -0.006(4) C41 0.059(5) 0.053(5) 0.032(4) -0.001(4) 0.017(4) 0.021(4) C42 0.042(4) 0.072(6) 0.041(4) 0.011(4) 0.020(4) 0.021(4) C43 0.044(5) 0.056(5) 0.031(4) 0.004(4) 0.017(3) 0.014(4) C50 0.065(6) 0.059(6) 0.046(5) -0.016(4) 0.009(4) -0.015(5) C51 0.067(7) 0.063(7) 0.082(8) -0.005(6) 0.019(6) -0.017(6) C52 0.062(6) 0.056(6) 0.067(6) -0.009(5) 0.034(5) -0.015(5) O1 0.039(3) 0.032(3) 0.032(3) 0.007(2) 0.008(2) 0.001(2) O41 0.110(6) 0.053(4) 0.045(4) -0.020(3) -0.003(4) 0.018(4) O42 0.066(4) 0.108(6) 0.051(4) 0.031(4) 0.038(3) 0.024(4) O43 0.057(4) 0.078(5) 0.064(4) 0.020(4) 0.026(3) 0.037(4) C7 0.093(2) 0.093(2) 0.093(2) 0.043(2) 0.058(2) 0.043(2) C8 0.093(2) 0.093(2) 0.093(2) 0.043(2) 0.058(2) 0.043(2) C9 0.093(2) 0.093(2) 0.093(2) 0.043(2) 0.058(2) 0.043(2) C10 0.093(2) 0.093(2) 0.093(2) 0.043(2) 0.058(2) 0.043(2) C11 0.093(2) 0.093(2) 0.093(2) 0.043(2) 0.058(2) 0.043(2) C12 0.093(2) 0.093(2) 0.093(2) 0.043(2) 0.058(2) 0.043(2) _refine_ls_extinction_method None 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 Pd1 . Cl1 . 2.387(2) yes Pd1 . P1 . 2.336(2) yes Pd1 . C50 . 2.202(9) yes Pd1 . C51 . 2.143(11) yes Pd1 . C52 . 2.129(9) yes Pd1 . H502 . 2.095 no Pd1 . H521 . 2.030 no Mn1 . C1 . 2.218(7) yes Mn1 . C2 . 2.192(7) yes Mn1 . C3 . 2.154(7) yes Mn1 . C4 . 2.130(7) yes Mn1 . C5 . 2.236(8) yes Mn1 . C41 . 1.818(10) yes Mn1 . C42 . 1.820(9) yes Mn1 . C43 . 1.817(8) yes P1 . C3 . 1.835(7) yes P1 . C21 . 1.893(10) yes P1 . C31 . 1.835(8) yes C1 . C2 . 1.408(10) yes C1 . C6 . 1.512(11) yes C1 . H11 . 1.013 no C2 . C3 . 1.452(10) yes C2 . O1 . 1.367(9) yes C3 . C4 . 1.443(10) yes C4 . C5 . 1.388(11) yes C4 . H41 . 1.011 no C5 . C6 . 1.513(10) yes C5 . H51 . 1.021 no C6 . C7 . 1.532(7) yes C6 . H61 . 1.009 no C13 . O1 . 1.447(9) yes C13 . H131 . 1.013 no C13 . H132 . 0.999 no C13 . H133 . 0.998 no C21 . C22 . 1.384(12) yes C21 . C26 . 1.331(13) yes C22 . C23 . 1.369(13) yes C22 . H221 . 1.015 no C23 . C24 . 1.405(16) yes C23 . H231 . 1.005 no C24 . C25 . 1.378(17) yes C24 . H241 . 1.011 no C25 . C26 . 1.382(13) yes C25 . H251 . 1.012 no C26 . H261 . 1.022 no C31 . C32 . 1.393(12) yes C31 . C36 . 1.388(11) yes C32 . C33 . 1.411(12) yes C32 . H321 . 1.008 no C33 . C34 . 1.396(15) yes C33 . H331 . 1.011 no C34 . C35 . 1.359(15) yes C34 . H341 . 1.011 no C35 . C36 . 1.402(11) yes C35 . H351 . 1.010 no C36 . H361 . 1.020 no C41 . O41 . 1.141(11) yes C42 . O42 . 1.143(10) yes C43 . O43 . 1.130(10) yes C50 . C51 . 1.367(15) yes C50 . H501 . 1.006 no C50 . H502 . 1.005 no C51 . C52 . 1.383(15) yes C51 . H511 . 1.022 no C52 . H521 . 1.015 no C52 . H522 . 0.998 no C7 . C8 . 1.39001(10) yes C7 . C12 . 1.39001(13) yes C8 . C9 . 1.39000(12) yes C8 . H81 . 0.950 no C9 . C10 . 1.39001(13) yes C9 . H91 . 0.950 no C10 . C11 . 1.39001(10) yes C10 . H101 . 0.950 no C11 . C12 . 1.39000(12) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 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 Cl1 . Pd1 . P1 . 103.56(8) yes Cl1 . Pd1 . C50 . 92.5(3) yes P1 . Pd1 . C50 . 164.0(3) yes Cl1 . Pd1 . C51 . 124.5(3) yes P1 . Pd1 . C51 . 128.7(3) yes C50 . Pd1 . C51 . 36.6(4) yes Cl1 . Pd1 . C52 . 160.5(3) yes P1 . Pd1 . C52 . 96.0(3) yes C50 . Pd1 . C52 . 68.0(4) yes C51 . Pd1 . C52 . 37.8(4) yes Cl1 . Pd1 . H502 . 84.5 no P1 . Pd1 . H502 . 153.2 no C50 . Pd1 . H502 . 26.9 no C51 . Pd1 . H502 . 58.1 no C52 . Pd1 . H502 . 77.6 no Cl1 . Pd1 . H521 . 149.7 no P1 . Pd1 . H521 . 88.5 no C50 . Pd1 . H521 . 77.3 no C51 . Pd1 . H521 . 59.6 no C52 . Pd1 . H521 . 28.1 no H502 . Pd1 . H521 . 73.5 no C1 . Mn1 . C2 . 37.2(3) yes C1 . Mn1 . C3 . 68.8(3) yes C2 . Mn1 . C3 . 39.0(3) yes C1 . Mn1 . C4 . 78.8(3) yes C2 . Mn1 . C4 . 68.9(3) yes C3 . Mn1 . C4 . 39.4(3) yes C1 . Mn1 . C5 . 64.1(3) yes C2 . Mn1 . C5 . 78.5(3) yes C3 . Mn1 . C5 . 68.6(3) yes C4 . Mn1 . C5 . 37.0(3) yes C1 . Mn1 . C41 . 101.8(3) yes C2 . Mn1 . C41 . 87.4(3) yes C3 . Mn1 . C41 . 102.9(3) yes C4 . Mn1 . C41 . 140.0(3) yes C5 . Mn1 . C41 . 165.2(3) yes C1 . Mn1 . C42 . 167.9(4) yes C2 . Mn1 . C42 . 141.8(3) yes C3 . Mn1 . C42 . 105.4(3) yes C4 . Mn1 . C42 . 90.0(4) yes C5 . Mn1 . C42 . 104.0(4) yes C1 . Mn1 . C43 . 88.6(3) yes C2 . Mn1 . C43 . 124.2(3) yes C3 . Mn1 . C43 . 153.5(3) yes C4 . Mn1 . C43 . 125.1(3) yes C5 . Mn1 . C43 . 89.6(3) yes C41 . Mn1 . C42 . 89.8(4) yes C41 . Mn1 . C43 . 94.8(4) yes C42 . Mn1 . C43 . 94.1(4) yes Pd1 . P1 . C3 . 114.9(2) yes Pd1 . P1 . C21 . 117.5(2) yes C3 . P1 . C21 . 103.1(3) yes Pd1 . P1 . C31 . 114.6(3) yes C3 . P1 . C31 . 103.1(3) yes C21 . P1 . C31 . 101.7(3) yes Mn1 . C1 . C2 . 70.4(4) yes Mn1 . C1 . C6 . 94.1(4) yes C2 . C1 . C6 . 120.5(7) yes Mn1 . C1 . H11 . 106.1 no C2 . C1 . H11 . 118.9 no C6 . C1 . H11 . 120.6 no Mn1 . C2 . C1 . 72.4(4) yes Mn1 . C2 . C3 . 69.1(4) yes C1 . C2 . C3 . 119.4(7) yes Mn1 . C2 . O1 . 125.0(4) yes C1 . C2 . O1 . 125.7(6) yes C3 . C2 . O1 . 114.7(6) yes Mn1 . C3 . P1 . 127.8(3) yes Mn1 . C3 . C2 . 71.9(4) yes P1 . C3 . C2 . 121.1(5) yes Mn1 . C3 . C4 . 69.4(4) yes P1 . C3 . C4 . 123.6(5) yes C2 . C3 . C4 . 115.3(6) yes Mn1 . C4 . C3 . 71.2(4) yes Mn1 . C4 . C5 . 75.7(5) yes C3 . C4 . C5 . 121.9(7) yes Mn1 . C4 . H41 . 126.1 no C3 . C4 . H41 . 118.9 no C5 . C4 . H41 . 119.2 no Mn1 . C5 . C4 . 67.4(4) yes Mn1 . C5 . C6 . 93.3(5) yes C4 . C5 . C6 . 120.6(7) yes Mn1 . C5 . H51 . 109.9 no C4 . C5 . H51 . 120.4 no C6 . C5 . H51 . 119.0 no C5 . C6 . C1 . 102.8(6) yes C5 . C6 . C7 . 117.5(6) yes C1 . C6 . C7 . 115.6(5) yes C5 . C6 . H61 . 108.0 no C1 . C6 . H61 . 107.8 no C7 . C6 . H61 . 104.7 no O1 . C13 . H131 . 109.1 no O1 . C13 . H132 . 110.4 no H131 . C13 . H132 . 108.5 no O1 . C13 . H133 . 110.5 no H131 . C13 . H133 . 108.6 no H132 . C13 . H133 . 109.7 no P1 . C21 . C22 . 119.4(7) yes P1 . C21 . C26 . 117.9(7) yes C22 . C21 . C26 . 122.6(9) yes C21 . C22 . C23 . 117.8(9) yes C21 . C22 . H221 . 120.8 no C23 . C22 . H221 . 121.3 no C22 . C23 . C24 . 120.7(10) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 119.5 no C23 . C24 . C25 . 118.9(9) yes C23 . C24 . H241 . 119.8 no C25 . C24 . H241 . 121.3 no C24 . C25 . C26 . 119.8(10) yes C24 . C25 . H251 . 119.1 no C26 . C25 . H251 . 121.1 no C25 . C26 . C21 . 120.1(10) yes C25 . C26 . H261 . 119.8 no C21 . C26 . H261 . 120.1 no P1 . C31 . C32 . 117.8(6) yes P1 . C31 . C36 . 122.4(6) yes C32 . C31 . C36 . 119.7(7) yes C31 . C32 . C33 . 120.3(9) yes C31 . C32 . H321 . 120.3 no C33 . C32 . H321 . 119.4 no C32 . C33 . C34 . 118.2(9) yes C32 . C33 . H331 . 120.1 no C34 . C33 . H331 . 121.7 no C33 . C34 . C35 . 121.9(8) yes C33 . C34 . H341 . 119.0 no C35 . C34 . H341 . 119.0 no C34 . C35 . C36 . 119.7(9) yes C34 . C35 . H351 . 120.5 no C36 . C35 . H351 . 119.8 no C35 . C36 . C31 . 120.1(9) yes C35 . C36 . H361 . 119.9 no C31 . C36 . H361 . 120.0 no Mn1 . C41 . O41 . 177.4(8) yes Mn1 . C42 . O42 . 178.4(9) yes Mn1 . C43 . O43 . 179.5(9) yes Pd1 . C50 . C51 . 69.3(6) yes Pd1 . C50 . H501 . 131.8 no C51 . C50 . H501 . 121.2 no Pd1 . C50 . H502 . 70.6 no C51 . C50 . H502 . 119.8 no H501 . C50 . H502 . 119.0 no C50 . C51 . Pd1 . 74.0(6) yes C50 . C51 . C52 . 123.6(11) yes Pd1 . C51 . C52 . 70.6(6) yes C50 . C51 . H511 . 118.6 no Pd1 . C51 . H511 . 131.9 no C52 . C51 . H511 . 117.8 no C51 . C52 . Pd1 . 71.7(6) yes C51 . C52 . H521 . 119.1 no Pd1 . C52 . H521 . 70.5 no C51 . C52 . H522 . 122.1 no Pd1 . C52 . H522 . 131.2 no H521 . C52 . H522 . 118.7 no C13 . O1 . C2 . 117.3(6) yes C6 . C7 . C8 . 118.3(3) yes C6 . C7 . C12 . 121.6(3) yes C8 . C7 . C12 . 120.000(8) yes C7 . C8 . C9 . 120.000(8) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.0 no C8 . C9 . C10 . 120.000(5) yes C8 . C9 . H91 . 120.0 no C10 . C9 . H91 . 120.0 no C9 . C10 . C11 . 120.000(3) yes C9 . C10 . H101 . 120.0 no C11 . C10 . H101 . 120.0 no C10 . C11 . C12 . 120.000(8) yes C10 . C11 . H111 . 120.0 no C12 . C11 . H111 . 120.0 no C7 . C12 . C11 . 120.000(3) yes C7 . C12 . H121 . 120.0 no C11 . C12 . H121 . 120.0 no C50 . H502 . Pd1 . 82.5 no C52 . H521 . Pd1 . 81.4 no # Attachment 'ccdc690313.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 690313' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 11.3085(19) _cell_length_b 15.525(3) _cell_length_c 20.700(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3634.0(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,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' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 '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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C38 H36 Cl1 Mn1 N1 O4 P1 Pd1 # Dc = 1.46 Fooo = 1624.00 Mu = 9.99 M = 798.46 # Found Formula = C38 H36 Cl1 Mn1 N1 O4 P1 Pd1 # Dc = 1.46 FOOO = 1624.00 Mu = 9.99 M = 798.46 _chemical_formula_sum 'C38 H36 Cl1 Mn1 N1 O4 P1 Pd1' _chemical_formula_moiety 'C38 H36 Cl1 Mn1 N1 O4 P1 Pd1' _chemical_compound_source ? _chemical_formula_weight 798.46 _cell_measurement_reflns_used 328 _cell_measurement_theta_min 3 _cell_measurement_theta_max 24 _cell_measurement_temperature 200 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.999 # Sheldrick geometric approximatio 0.83 0.84 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.84 # 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 & \w scans' # 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 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 200 _diffrn_reflns_number 28746 _reflns_number_total 12398 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 7188 # Number of reflections without Friedels Law is 12398 # Theoretical number of reflections is about 7285 _diffrn_reflns_theta_min 2.803 _diffrn_reflns_theta_max 33.775 _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.695 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _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 0.88 # 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 12383 _refine_ls_number_restraints 0 _refine_ls_number_parameters 425 _oxford_refine_ls_R_factor_ref 0.0407 _refine_ls_wR_factor_ref 0.0727 _refine_ls_goodness_of_fit_ref 0.9775 _refine_ls_shift/su_max 0.001240 # The values computed from all data _oxford_reflns_number_all 12383 _refine_ls_R_factor_all 0.0407 _refine_ls_wR_factor_all 0.0727 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10613 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_gt 0.0661 _refine_ls_abs_structure_Flack 0.027(13) _refine_ls_abs_structure_details 'Flack (1983), 5210 Friedel-pairs' # 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 ad _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refu # 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^) + ( 0.04P)^2^ + 0.66P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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 Pd1 Pd 0.210144(14) 0.313334(9) 0.440686(6) 0.0196 1.0000 Uani . . . . . . . Mn1 Mn 0.04142(3) 0.40808(2) 0.223018(15) 0.0242 1.0000 Uani . . . . . . . Cl1 Cl 0.18734(6) 0.41600(4) 0.52816(2) 0.0362 1.0000 Uani . . . . . . . C1 C 0.2015(2) 0.44094(12) 0.16471(9) 0.0259 1.0000 Uani . . . . . . . C2 C 0.2213(2) 0.46290(12) 0.23012(9) 0.0223 1.0000 Uani . . . . . . . C3 C 0.2023(2) 0.39884(12) 0.28043(9) 0.0213 1.0000 Uani . . . . . . . C4 C 0.16493(19) 0.31467(14) 0.25902(9) 0.0236 1.0000 Uani . . . . . . . C5 C 0.1528(2) 0.29581(13) 0.19268(10) 0.0264 1.0000 Uani . . . . . . . C6 C 0.2225(2) 0.34763(13) 0.14346(9) 0.0275 1.0000 Uani . . . . . . . C7 C 0.3541(2) 0.32413(13) 0.13647(10) 0.0282 1.0000 Uani . . . . . . . C8 C 0.4277(3) 0.37541(17) 0.09860(14) 0.0420 1.0000 Uani . . . . . . . C9 C 0.5481(3) 0.35561(17) 0.09239(15) 0.0456 1.0000 Uani . . . . . . . C10 C 0.5950(3) 0.28426(19) 0.12411(16) 0.0466 1.0000 Uani . . . . . . . C11 C 0.5220(3) 0.23210(19) 0.16050(15) 0.0492 1.0000 Uani . . . . . . . C12 C 0.4013(3) 0.25166(17) 0.16691(13) 0.0410 1.0000 Uani . . . . . . . C13 C 0.2485(2) 0.61290(15) 0.20473(12) 0.0345 1.0000 Uani . . . . . . . C21 C 0.3814(2) 0.46611(14) 0.36816(11) 0.0276 1.0000 Uani . . . . . . . C22 C 0.4180(3) 0.51045(16) 0.42397(13) 0.0384 1.0000 Uani . . . . . . . C23 C 0.5324(3) 0.5428(2) 0.42732(17) 0.0564 1.0000 Uani . . . . . . . C24 C 0.6125(3) 0.5287(2) 0.3772(2) 0.0671 1.0000 Uani . . . . . . . C25 C 0.5781(3) 0.4822(2) 0.32309(18) 0.0559 1.0000 Uani . . . . . . . C26 C 0.4619(2) 0.45184(18) 0.31783(13) 0.0379 1.0000 Uani . . . . . . . C31 C 0.1296(2) 0.50922(13) 0.38774(10) 0.0251 1.0000 Uani . . . . . . . C32 C 0.1604(2) 0.59654(14) 0.38529(12) 0.0338 1.0000 Uani . . . . . . . C33 C 0.0789(3) 0.65952(16) 0.40391(15) 0.0484 1.0000 Uani . . . . . . . C34 C -0.0331(3) 0.6355(2) 0.42518(14) 0.0497 1.0000 Uani . . . . . . . C35 C -0.0643(3) 0.5497(2) 0.42812(14) 0.0441 1.0000 Uani . . . . . . . C36 C 0.0169(2) 0.48598(16) 0.40911(12) 0.0327 1.0000 Uani . . . . . . . C41 C -0.0382(2) 0.39773(14) 0.14791(12) 0.0328 1.0000 Uani . . . . . . . C42 C -0.0217(2) 0.51410(15) 0.24289(12) 0.0328 1.0000 Uani . . . . . . . C43 C -0.0747(2) 0.35797(17) 0.27083(13) 0.0370 1.0000 Uani . . . . . . . C51 C 0.27221(19) 0.21582(12) 0.38590(9) 0.0217 1.0000 Uani . . . . . . . C52 C 0.3636(2) 0.21930(15) 0.34003(11) 0.0285 1.0000 Uani . . . . . . . C53 C 0.4172(2) 0.14376(18) 0.31761(12) 0.0389 1.0000 Uani . . . . . . . C54 C 0.3813(3) 0.06344(17) 0.33993(13) 0.0435 1.0000 Uani . . . . . . . C55 C 0.2900(3) 0.05869(14) 0.38531(12) 0.0369 1.0000 Uani . . . . . . . C56 C 0.2364(2) 0.13454(13) 0.40868(10) 0.0251 1.0000 Uani . . . . . . . C57 C 0.1406(2) 0.13196(13) 0.45938(11) 0.0265 1.0000 Uani . . . . . . . C58 C 0.0182(2) 0.13848(18) 0.42801(13) 0.0376 1.0000 Uani . . . . . . . C59 C 0.2732(2) 0.18504(16) 0.54423(11) 0.0350 1.0000 Uani . . . . . . . C60 C 0.0677(2) 0.22307(16) 0.54958(12) 0.0371 1.0000 Uani . . . . . . . O1 O 0.24600(15) 0.54388(9) 0.25165(7) 0.0268 1.0000 Uani . . . . . . . O41 O -0.0855(2) 0.38995(13) 0.09785(10) 0.0500 1.0000 Uani . . . . . . . O42 O -0.0630(2) 0.57926(13) 0.25512(11) 0.0517 1.0000 Uani . . . . . . . O43 O -0.1503(2) 0.32654(17) 0.30058(12) 0.0610 1.0000 Uani . . . . . . . P1 P 0.23078(5) 0.42098(3) 0.36666(2) 0.0202 1.0000 Uani . . . . . . . N1 N 0.16728(17) 0.20651(11) 0.50414(9) 0.0243 1.0000 Uani . . . . . . . H11 H 0.1756 0.4832 0.1346 0.0506(16) 1.0000 Uiso . . . . . . . H41 H 0.1483 0.2713 0.2901 0.0506(16) 1.0000 Uiso . . . . . . . H51 H 0.1013 0.2510 0.1789 0.0506(16) 1.0000 Uiso . . . . . . . H61 H 0.1860 0.3400 0.1025 0.0506(16) 1.0000 Uiso . . . . . . . H81 H 0.3963 0.4242 0.0769 0.0506(16) 1.0000 Uiso . . . . . . . H91 H 0.5976 0.3910 0.0664 0.0506(16) 1.0000 Uiso . . . . . . . H101 H 0.6768 0.2715 0.1207 0.0506(16) 1.0000 Uiso . . . . . . . H111 H 0.5535 0.1825 0.1813 0.0506(16) 1.0000 Uiso . . . . . . . H121 H 0.3518 0.2156 0.1922 0.0506(16) 1.0000 Uiso . . . . . . . H131 H 0.2666 0.6655 0.2258 0.0506(16) 1.0000 Uiso . . . . . . . H132 H 0.3070 0.6010 0.1731 0.0506(16) 1.0000 Uiso . . . . . . . H133 H 0.1733 0.6173 0.1845 0.0506(16) 1.0000 Uiso . . . . . . . H221 H 0.3650 0.5182 0.4590 0.0506(16) 1.0000 Uiso . . . . . . . H231 H 0.5566 0.5748 0.4641 0.0506(16) 1.0000 Uiso . . . . . . . H241 H 0.6904 0.5512 0.3800 0.0506(16) 1.0000 Uiso . . . . . . . H251 H 0.6335 0.4708 0.2898 0.0506(16) 1.0000 Uiso . . . . . . . H261 H 0.4378 0.4214 0.2802 0.0506(16) 1.0000 Uiso . . . . . . . H321 H 0.2367 0.6130 0.3709 0.0506(16) 1.0000 Uiso . . . . . . . H331 H 0.1000 0.7186 0.4023 0.0506(16) 1.0000 Uiso . . . . . . . H341 H -0.0881 0.6785 0.4378 0.0506(16) 1.0000 Uiso . . . . . . . H351 H -0.1408 0.5337 0.4429 0.0506(16) 1.0000 Uiso . . . . . . . H361 H -0.0050 0.4268 0.4108 0.0506(16) 1.0000 Uiso . . . . . . . H521 H 0.3894 0.2735 0.3239 0.0506(16) 1.0000 Uiso . . . . . . . H531 H 0.4790 0.1471 0.2866 0.0506(16) 1.0000 Uiso . . . . . . . H541 H 0.4184 0.0125 0.3247 0.0506(16) 1.0000 Uiso . . . . . . . H551 H 0.2637 0.0041 0.4003 0.0506(16) 1.0000 Uiso . . . . . . . H571 H 0.1460 0.0795 0.4828 0.0506(16) 1.0000 Uiso . . . . . . . H581 H -0.0409 0.1367 0.4607 0.0506(16) 1.0000 Uiso . . . . . . . H582 H 0.0124 0.1910 0.4048 0.0506(16) 1.0000 Uiso . . . . . . . H583 H 0.0073 0.0914 0.3993 0.0506(16) 1.0000 Uiso . . . . . . . H591 H 0.2904 0.2317 0.5724 0.0506(16) 1.0000 Uiso . . . . . . . H592 H 0.2576 0.1348 0.5689 0.0506(16) 1.0000 Uiso . . . . . . . H593 H 0.3391 0.1750 0.5167 0.0506(16) 1.0000 Uiso . . . . . . . H601 H 0.0872 0.2702 0.5769 0.0506(16) 1.0000 Uiso . . . . . . . H602 H 0.0541 0.1732 0.5751 0.0506(16) 1.0000 Uiso . . . . . . . H603 H -0.0017 0.2365 0.5257 0.0506(16) 1.0000 Uiso . . . . . . . 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 0.02593(7) 0.01941(6) 0.01340(5) 0.00201(5) -0.00017(6) -0.00066(6) Mn1 0.03033(17) 0.02350(14) 0.01876(13) 0.00174(11) -0.00543(12) -0.00042(13) Cl1 0.0608(4) 0.0291(2) 0.0188(2) -0.00404(18) -0.0018(2) 0.0048(3) C1 0.0380(12) 0.0243(8) 0.0153(8) 0.0026(6) -0.0037(9) 0.0025(9) C2 0.0290(10) 0.0205(8) 0.0174(8) 0.0022(6) -0.0012(8) 0.0004(8) C3 0.0272(10) 0.0203(8) 0.0165(7) 0.0011(6) -0.0033(8) -0.0003(8) C4 0.0319(10) 0.0197(8) 0.0193(8) 0.0032(7) -0.0036(7) -0.0009(8) C5 0.0354(11) 0.0234(10) 0.0203(9) -0.0004(7) -0.0059(8) -0.0022(8) C6 0.0408(13) 0.0252(9) 0.0163(8) -0.0012(7) -0.0037(9) -0.0011(9) C7 0.0437(13) 0.0225(9) 0.0185(8) -0.0015(7) -0.0001(8) 0.0005(9) C8 0.0540(17) 0.0297(11) 0.0422(14) 0.0067(10) 0.0011(13) -0.0013(11) C9 0.0515(17) 0.0345(13) 0.0508(17) 0.0023(11) 0.0102(14) -0.0070(12) C10 0.0470(16) 0.0451(14) 0.0477(16) 0.0004(12) 0.0066(13) 0.0058(12) C11 0.0555(18) 0.0496(15) 0.0425(15) 0.0126(12) 0.0132(14) 0.0202(14) C12 0.0536(16) 0.0350(12) 0.0345(13) 0.0092(10) 0.0132(12) 0.0084(11) C13 0.0497(14) 0.0244(10) 0.0295(11) 0.0084(8) -0.0069(10) -0.0060(9) C21 0.0280(11) 0.0267(9) 0.0281(10) 0.0100(8) -0.0066(9) -0.0045(8) C22 0.0464(15) 0.0315(11) 0.0374(13) 0.0058(10) -0.0197(11) -0.0079(11) C23 0.0580(19) 0.0499(16) 0.061(2) 0.0180(14) -0.0347(17) -0.0223(15) C24 0.0407(17) 0.076(2) 0.084(3) 0.046(2) -0.0322(18) -0.0273(16) C25 0.0294(13) 0.074(2) 0.064(2) 0.0410(18) -0.0021(14) -0.0074(14) C26 0.0294(12) 0.0484(14) 0.0361(12) 0.0174(11) -0.0016(10) -0.0012(11) C31 0.0327(11) 0.0232(9) 0.0193(9) 0.0007(7) -0.0032(8) 0.0019(8) C32 0.0500(14) 0.0229(9) 0.0284(11) 0.0027(8) -0.0022(10) 0.0025(10) C33 0.077(2) 0.0260(11) 0.0423(15) 0.0021(10) -0.0001(15) 0.0152(12) C34 0.0609(19) 0.0483(15) 0.0398(15) 0.0035(11) 0.0000(13) 0.0299(14) C35 0.0366(14) 0.0605(17) 0.0353(14) 0.0023(12) 0.0002(11) 0.0133(12) C36 0.0301(12) 0.0382(12) 0.0299(11) -0.0001(9) -0.0056(10) 0.0027(10) C41 0.0390(13) 0.0286(10) 0.0308(11) 0.0002(8) -0.0097(10) 0.0050(10) C42 0.0387(13) 0.0328(11) 0.0270(10) 0.0006(9) -0.0076(10) 0.0028(10) C43 0.0379(14) 0.0402(13) 0.0328(12) 0.0014(10) -0.0013(11) 0.0002(11) C51 0.0248(10) 0.0232(8) 0.0171(8) 0.0007(6) -0.0010(7) 0.0047(8) C52 0.0284(11) 0.0356(10) 0.0214(9) 0.0046(8) 0.0008(8) 0.0067(9) C53 0.0374(13) 0.0526(15) 0.0267(11) 0.0033(10) 0.0049(10) 0.0145(12) C54 0.0556(17) 0.0379(13) 0.0370(13) -0.0040(10) 0.0048(12) 0.0199(12) C55 0.0464(14) 0.0263(10) 0.0381(12) 0.0005(8) 0.0021(12) 0.0078(11) C56 0.0265(11) 0.0242(9) 0.0246(9) -0.0029(7) -0.0021(8) 0.0030(8) C57 0.0267(11) 0.0233(9) 0.0294(10) 0.0045(7) -0.0002(8) -0.0026(8) C58 0.0270(12) 0.0457(13) 0.0402(14) 0.0005(11) -0.0039(10) -0.0068(10) C59 0.0401(13) 0.0379(11) 0.0269(10) 0.0130(9) -0.0092(9) -0.0063(11) C60 0.0398(13) 0.0406(12) 0.0309(12) 0.0052(9) 0.0127(10) -0.0002(10) O1 0.0408(9) 0.0209(6) 0.0187(6) 0.0041(5) -0.0045(6) -0.0020(6) O41 0.0684(14) 0.0445(11) 0.0370(10) -0.0059(8) -0.0269(10) 0.0074(10) O42 0.0649(14) 0.0426(10) 0.0477(11) -0.0063(9) -0.0117(10) 0.0210(10) O43 0.0562(13) 0.0697(15) 0.0571(14) 0.0082(12) 0.0174(11) -0.0173(12) P1 0.0257(3) 0.0194(2) 0.01551(19) 0.00253(16) -0.00232(18) -0.00231(19) N1 0.0254(8) 0.0271(8) 0.0204(8) 0.0042(6) 0.0017(7) -0.0024(7) _refine_ls_extinction_method None 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 Pd1 . Cl1 . 2.4260(6) yes Pd1 . C51 . 2.0175(19) yes Pd1 . P1 . 2.2794(6) yes Pd1 . N1 . 2.1705(17) yes Mn1 . C1 . 2.235(2) yes Mn1 . C2 . 2.210(2) yes Mn1 . C3 . 2.178(2) yes Mn1 . C4 . 2.147(2) yes Mn1 . C5 . 2.240(2) yes Mn1 . C41 . 1.804(2) yes Mn1 . C42 . 1.841(2) yes Mn1 . C43 . 1.819(3) yes C1 . C2 . 1.414(3) yes C1 . C6 . 1.532(3) yes C1 . H11 . 0.951 no C2 . C3 . 1.456(3) yes C2 . O1 . 1.363(2) yes C3 . C4 . 1.443(3) yes C3 . P1 . 1.8459(19) yes C4 . C5 . 1.411(3) yes C4 . H41 . 0.950 no C5 . C6 . 1.519(3) yes C5 . H51 . 0.950 no C6 . C7 . 1.539(3) yes C6 . H61 . 0.950 no C7 . C8 . 1.393(4) yes C7 . C12 . 1.396(3) yes C8 . C9 . 1.401(5) yes C8 . H81 . 0.950 no C9 . C10 . 1.393(4) yes C9 . H91 . 0.952 no C10 . C11 . 1.380(4) yes C10 . H101 . 0.949 no C11 . C12 . 1.404(4) yes C11 . H111 . 0.951 no C12 . H121 . 0.949 no C13 . O1 . 1.446(3) yes C13 . H131 . 0.949 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C21 . C22 . 1.407(3) yes C21 . C26 . 1.401(4) yes C21 . P1 . 1.842(2) yes C22 . C23 . 1.389(4) yes C22 . H221 . 0.949 no C23 . C24 . 1.394(6) yes C23 . H231 . 0.949 no C24 . C25 . 1.389(6) yes C24 . H241 . 0.950 no C25 . C26 . 1.400(4) yes C25 . H251 . 0.949 no C26 . H261 . 0.950 no C31 . C32 . 1.400(3) yes C31 . C36 . 1.397(3) yes C31 . P1 . 1.837(2) yes C32 . C33 . 1.398(4) yes C32 . H321 . 0.949 no C33 . C34 . 1.392(5) yes C33 . H331 . 0.949 no C34 . C35 . 1.379(5) yes C34 . H341 . 0.949 no C35 . C36 . 1.406(4) yes C35 . H351 . 0.951 no C36 . H361 . 0.952 no C41 . O41 . 1.172(3) yes C42 . O42 . 1.142(3) yes C43 . O43 . 1.161(3) yes C51 . C52 . 1.405(3) yes C51 . C56 . 1.407(3) yes C52 . C53 . 1.399(3) yes C52 . H521 . 0.951 no C53 . C54 . 1.391(4) yes C53 . H531 . 0.950 no C54 . C55 . 1.398(4) yes C54 . H541 . 0.950 no C55 . C56 . 1.410(3) yes C55 . H551 . 0.951 no C56 . C57 . 1.509(3) yes C57 . C58 . 1.533(3) yes C57 . N1 . 1.513(3) yes C57 . H571 . 0.950 no C58 . H581 . 0.950 no C58 . H582 . 0.948 no C58 . H583 . 0.950 no C59 . N1 . 1.495(3) yes C59 . H591 . 0.950 no C59 . H592 . 0.949 no C59 . H593 . 0.951 no C60 . N1 . 1.489(3) yes C60 . H601 . 0.950 no C60 . H602 . 0.949 no C60 . H603 . 0.950 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 Cl1 . Pd1 . C51 . 161.71(6) yes Cl1 . Pd1 . P1 . 91.78(2) yes C51 . Pd1 . P1 . 97.85(6) yes Cl1 . Pd1 . N1 . 91.52(5) yes C51 . Pd1 . N1 . 81.06(8) yes P1 . Pd1 . N1 . 171.87(5) yes C1 . Mn1 . C2 . 37.09(7) yes C1 . Mn1 . C3 . 68.46(8) yes C2 . Mn1 . C3 . 38.75(7) yes C1 . Mn1 . C4 . 79.32(8) yes C2 . Mn1 . C4 . 68.79(8) yes C3 . Mn1 . C4 . 38.98(7) yes C1 . Mn1 . C5 . 64.58(8) yes C2 . Mn1 . C5 . 78.51(8) yes C3 . Mn1 . C5 . 68.41(7) yes C4 . Mn1 . C5 . 37.44(7) yes C1 . Mn1 . C41 . 87.65(10) yes C2 . Mn1 . C41 . 123.43(10) yes C3 . Mn1 . C41 . 151.81(10) yes C4 . Mn1 . C41 . 124.31(9) yes C5 . Mn1 . C41 . 88.26(9) yes C1 . Mn1 . C42 . 103.35(10) yes C2 . Mn1 . C42 . 89.88(10) yes C3 . Mn1 . C42 . 105.14(9) yes C4 . Mn1 . C42 . 141.16(9) yes C5 . Mn1 . C42 . 167.54(10) yes C1 . Mn1 . C43 . 167.48(10) yes C2 . Mn1 . C43 . 142.46(10) yes C3 . Mn1 . C43 . 106.15(10) yes C4 . Mn1 . C43 . 89.54(10) yes C5 . Mn1 . C43 . 103.04(10) yes C41 . Mn1 . C42 . 94.51(11) yes C41 . Mn1 . C43 . 94.05(12) yes C42 . Mn1 . C43 . 88.89(12) yes Mn1 . C1 . C2 . 70.48(13) yes Mn1 . C1 . C6 . 93.70(14) yes C2 . C1 . C6 . 118.58(17) yes Mn1 . C1 . H11 . 105.1 no C2 . C1 . H11 . 120.6 no C6 . C1 . H11 . 120.8 no Mn1 . C2 . C1 . 72.43(14) yes Mn1 . C2 . C3 . 69.44(12) yes C1 . C2 . C3 . 119.80(17) yes Mn1 . C2 . O1 . 124.46(15) yes C1 . C2 . O1 . 124.61(16) yes C3 . C2 . O1 . 115.25(16) yes Mn1 . C3 . C2 . 71.81(12) yes Mn1 . C3 . C4 . 69.35(11) yes C2 . C3 . C4 . 116.24(16) yes Mn1 . C3 . P1 . 131.37(11) yes C2 . C3 . P1 . 122.60(14) yes C4 . C3 . P1 . 121.10(13) yes Mn1 . C4 . C3 . 71.68(12) yes Mn1 . C4 . C5 . 74.87(12) yes C3 . C4 . C5 . 121.01(18) yes Mn1 . C4 . H41 . 125.8 no C3 . C4 . H41 . 119.5 no C5 . C4 . H41 . 119.5 no Mn1 . C5 . C4 . 67.69(12) yes Mn1 . C5 . C6 . 93.88(13) yes C4 . C5 . C6 . 119.51(18) yes Mn1 . C5 . H51 . 108.0 no C4 . C5 . H51 . 120.2 no C6 . C5 . H51 . 120.3 no C1 . C6 . C5 . 103.17(17) yes C1 . C6 . C7 . 113.62(19) yes C5 . C6 . C7 . 116.06(18) yes C1 . C6 . H61 . 107.9 no C5 . C6 . H61 . 107.9 no C7 . C6 . H61 . 107.9 no C6 . C7 . C8 . 119.7(2) yes C6 . C7 . C12 . 121.3(2) yes C8 . C7 . C12 . 119.1(2) yes C7 . C8 . C9 . 120.4(2) yes C7 . C8 . H81 . 119.9 no C9 . C8 . H81 . 119.7 no C8 . C9 . C10 . 120.1(3) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 120.1 no C9 . C10 . C11 . 119.7(3) yes C9 . C10 . H101 . 120.2 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 120.4(3) yes C10 . C11 . H111 . 119.9 no C12 . C11 . H111 . 119.8 no C11 . C12 . C7 . 120.2(2) yes C11 . C12 . H121 . 119.9 no C7 . C12 . H121 . 119.9 no O1 . C13 . H131 . 109.5 no O1 . C13 . H132 . 109.4 no H131 . C13 . H132 . 109.6 no O1 . C13 . H133 . 109.4 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no C22 . C21 . C26 . 119.7(2) yes C22 . C21 . P1 . 118.2(2) yes C26 . C21 . P1 . 121.89(19) yes C21 . C22 . C23 . 119.5(3) yes C21 . C22 . H221 . 120.2 no C23 . C22 . H221 . 120.3 no C22 . C23 . C24 . 120.7(3) yes C22 . C23 . H231 . 119.9 no C24 . C23 . H231 . 119.4 no C23 . C24 . C25 . 120.0(3) yes C23 . C24 . H241 . 120.0 no C25 . C24 . H241 . 119.9 no C24 . C25 . C26 . 120.0(3) yes C24 . C25 . H251 . 119.9 no C26 . C25 . H251 . 120.1 no C21 . C26 . C25 . 119.9(3) yes C21 . C26 . H261 . 120.1 no C25 . C26 . H261 . 120.0 no C32 . C31 . C36 . 119.2(2) yes C32 . C31 . P1 . 123.95(19) yes C36 . C31 . P1 . 116.80(17) yes C31 . C32 . C33 . 120.2(3) yes C31 . C32 . H321 . 119.9 no C33 . C32 . H321 . 119.9 no C32 . C33 . C34 . 120.0(3) yes C32 . C33 . H331 . 120.0 no C34 . C33 . H331 . 120.0 no C33 . C34 . C35 . 120.4(3) yes C33 . C34 . H341 . 119.6 no C35 . C34 . H341 . 120.0 no C34 . C35 . C36 . 120.0(3) yes C34 . C35 . H351 . 120.0 no C36 . C35 . H351 . 120.0 no C35 . C36 . C31 . 120.2(2) yes C35 . C36 . H361 . 119.9 no C31 . C36 . H361 . 119.9 no Mn1 . C41 . O41 . 177.1(2) yes Mn1 . C42 . O42 . 178.7(2) yes Mn1 . C43 . O43 . 178.8(2) yes Pd1 . C51 . C52 . 127.38(16) yes Pd1 . C51 . C56 . 112.62(14) yes C52 . C51 . C56 . 118.22(18) yes C51 . C52 . C53 . 120.7(2) yes C51 . C52 . H521 . 119.7 no C53 . C52 . H521 . 119.6 no C52 . C53 . C54 . 121.0(2) yes C52 . C53 . H531 . 119.8 no C54 . C53 . H531 . 119.2 no C53 . C54 . C55 . 119.1(2) yes C53 . C54 . H541 . 120.5 no C55 . C54 . H541 . 120.4 no C54 . C55 . C56 . 120.3(2) yes C54 . C55 . H551 . 119.8 no C56 . C55 . H551 . 119.9 no C55 . C56 . C51 . 120.7(2) yes C55 . C56 . C57 . 121.7(2) yes C51 . C56 . C57 . 117.62(18) yes C56 . C57 . C58 . 110.63(19) yes C56 . C57 . N1 . 105.22(17) yes C58 . C57 . N1 . 112.89(19) yes C56 . C57 . H571 . 109.4 no C58 . C57 . H571 . 109.3 no N1 . C57 . H571 . 109.3 no C57 . C58 . H581 . 109.3 no C57 . C58 . H582 . 109.5 no H581 . C58 . H582 . 109.6 no C57 . C58 . H583 . 109.3 no H581 . C58 . H583 . 109.4 no H582 . C58 . H583 . 109.6 no N1 . C59 . H591 . 109.6 no N1 . C59 . H592 . 109.5 no H591 . C59 . H592 . 109.5 no N1 . C59 . H593 . 109.4 no H591 . C59 . H593 . 109.4 no H592 . C59 . H593 . 109.4 no N1 . C60 . H601 . 109.5 no N1 . C60 . H602 . 109.5 no H601 . C60 . H602 . 109.5 no N1 . C60 . H603 . 109.5 no H601 . C60 . H603 . 109.4 no H602 . C60 . H603 . 109.5 no C13 . O1 . C2 . 117.89(16) yes C3 . P1 . C21 . 104.38(10) yes C3 . P1 . C31 . 105.07(9) yes C21 . P1 . C31 . 106.74(10) yes C3 . P1 . Pd1 . 119.72(6) yes C21 . P1 . Pd1 . 111.24(7) yes C31 . P1 . Pd1 . 108.86(7) yes C57 . N1 . C59 . 109.22(18) yes C57 . N1 . C60 . 111.61(17) yes C59 . N1 . C60 . 107.07(18) yes C57 . N1 . Pd1 . 104.97(13) yes C59 . N1 . Pd1 . 109.11(13) yes C60 . N1 . Pd1 . 114.77(14) yes