# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Oleg Ozerov' _publ_contact_author_email OZEROV@CHEM.TAMU.EDU _publ_section_title ; Heterolytic splitting of H-X bonds at a cationic (PNP)Pd center ; loop_ _publ_author_name 'Oleg Ozerov' 'Chung-Hsing Chen.' 'Claudia M. Fafard' 'Lei Fan.' 'Bruce Foxman' ; L.C.Gregor ; 'Chengyun Guo.' 'Dmitry G. Gusev' # Attachment '2a-OTf_rev.cif' data_2a_OTf _database_code_depnum_ccdc_archive 'CCDC 756641' #TrackingRef '2a-OTf_rev.cif' # start Validation Reply Form: 0ne Alert B issue _vrf_PLAT222_2a_OTf ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.82 Ratio RESPONSE: The large ratio between H atoms likely arises from low thermal motion of H(1) (involved in a hydrogen bond) and the high apparent thermal motion of H atoms attached to disordered groups (see also vrf responses to PLAT 241 and 242). ; _vrf_PLAT241_2a_OTf ; PROBLEM: Check High Ueq as Compared to Neighbors for C21 RESPONSE: Isopropyl methyl C-atoms C230 and C231, attached to C21, are disordered; disorder was successfully resolved. However, the disorder could not be resolved for methine C-atom C21. ; _vrf_PLAT242_2a_OTf ; PROBLEM: Check Low Ueq as Compared to Neighbors for C15 RESPONSE:The isopropyl C atoms in this structure (data collected at RT) are undergoing high thermal motion or are disordered. Apart from C230 and C231, it was not possible to resolve other disorder. This then appears in relative values of atoms attached to P1, P2, and C15. ; # end Validation Reply Form _audit_creation_date 10-01-04 _audit_creation_method CRYSTALS_ver_14.01 _oxford_structure_analysis_title OZ016 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.5631(5) _cell_length_b 12.1366(7) _cell_length_c 14.1091(11) _cell_angle_alpha 76.313(6) _cell_angle_beta 84.865(6) _cell_angle_gamma 67.452(4) _cell_volume 1623.08(19) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 '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' 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' 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' 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' 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' _cell_formula_units_Z 2 # Given Formula = C27 H42 F3 N1 O3 P2 Pd1 S1 # Dc = 1.40 Fooo = 708.00 Mu = 7.79 M = 686.04 # Found Formula = C27 H42 F3 N1 O3 P2 Pd1 S1 # Dc = 1.40 FOOO = 708.00 Mu = 7.79 M = 686.04 _chemical_formula_sum 'C27 H42 F3 N1 O3 P2 Pd1 S1' _chemical_formula_moiety 'C27 H42 F3 N1 O3 P2 Pd1 S1' _chemical_compound_source ? _chemical_formula_weight 686.04 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 21 _cell_measurement_theta_max 22 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour light-orange _exptl_crystal_size_min 0.360 _exptl_crystal_size_mid 0.504 _exptl_crystal_size_max 0.792 _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 0.779 # Sheldrick geometric approximatio 0.68 0.76 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.76 _diffrn_measurement_device-type 'Enraf-Nonius CAD4' _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CAD4 EXPRESS, (Straver, 1992)' _computing_cell_refinement 'CAD4 EXPRESS, (Straver, 1992)' _computing_data_reduction 'RC93 (Watkin et al., 1994)' _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 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time 7200 _diffrn_standards_interval_count . _diffrn_standards_number 3 _diffrn_standards_decay_% 6.61 _diffrn_ambient_temperature 294 _diffrn_reflns_number 10140 _reflns_number_total 9781 _diffrn_reflns_av_R_equivalents 0.010 # Number of reflections without Friedels Law is 9781 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 9825 _diffrn_reflns_theta_min 2.432 _diffrn_reflns_theta_max 30.415 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.415 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min -15 _reflns_limit_k_max 17 _reflns_limit_l_min -19 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.04 _refine_diff_density_max 1.66 # 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 6773 _refine_ls_number_restraints 8 _refine_ls_number_parameters 357 _oxford_refine_ls_R_factor_ref 0.0545 _refine_ls_wR_factor_ref 0.0592 _refine_ls_goodness_of_fit_ref 1.0835 _refine_ls_shift/su_max 0.0096325 _refine_ls_shift/su_mean 5.3709841 # The values computed from all data _oxford_reflns_number_all 9781 _refine_ls_R_factor_all 0.0890 _refine_ls_wR_factor_all 0.0984 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6773 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_gt 0.0592 # 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 mixed # 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: 2.99 1.52 2.33 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. North, A.C.T., Phillips, D.C. & Mathews, F.S., (1968). Acta Cryst, A24, 351-359. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Straver, L. H. (1992). CAD4-EXPRESS, Nonius, Delft, The Netherlands. 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. Watkin, D.J., Prout, C.K. & Lilley, P.M.deQ. (1994). RC93, 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 0.19547(2) 0.30326(2) 0.709141(17) 0.0529 1.0000 Uani D U . . . . . S1 S 0.2810(2) 0.68817(18) 0.75074(17) 0.1232 1.0000 Uani . U . . . . . P1 P 0.14543(9) 0.23596(9) 0.86484(6) 0.0581 1.0000 Uani . . . . . . . P2 P 0.30981(10) 0.32206(10) 0.56454(6) 0.0638 1.0000 Uani . . . . . . . F1 F 0.0456(7) 0.7869(9) 0.6715(6) 0.2263 1.0000 Uani . . . . . . . F2 F 0.0635(12) 0.8602(12) 0.7935(9) 0.3276 1.0000 Uani . . . . . . . F3 F 0.0543(11) 0.6846(13) 0.8226(7) 0.2909 1.0000 Uani . . . . . . . O1 O 0.3127(13) 0.6736(10) 0.8527(8) 0.2812 1.0000 Uani . . . . . . . O2 O 0.2991(7) 0.5864(4) 0.7155(6) 0.1652 1.0000 Uani . . . . . . . O3 O 0.3167(8) 0.7817(6) 0.6857(5) 0.1585 1.0000 Uani . . . . . . . N1 N 0.3614(3) 0.3310(3) 0.76676(18) 0.0511 1.0000 Uani D . . . . . . C1 C 0.3615(3) 0.3095(3) 0.8736(2) 0.0571 1.0000 Uani . . . . . . . C2 C 0.2707(3) 0.2625(3) 0.9283(2) 0.0604 1.0000 Uani . . . . . . . C3 C 0.2712(4) 0.2464(5) 1.0297(3) 0.0794 1.0000 Uani . . . . . . . C4 C 0.3584(5) 0.2759(5) 1.0768(3) 0.0900 1.0000 Uani . . . . . . . C5 C 0.4427(5) 0.3276(5) 1.0211(3) 0.0834 1.0000 Uani . . . . . . . C6 C 0.4452(4) 0.3456(4) 0.9198(3) 0.0735 1.0000 Uani . . . . . . . C7 C 0.4866(3) 0.2633(3) 0.7190(2) 0.0556 1.0000 Uani . . . . . . . C8 C 0.4797(4) 0.2651(3) 0.6195(2) 0.0595 1.0000 Uani . . . . . . . C9 C 0.5998(4) 0.2119(4) 0.5703(3) 0.0738 1.0000 Uani . . . . . . . C10 C 0.7252(4) 0.1498(4) 0.6172(4) 0.0793 1.0000 Uani . . . . . . . C11 C 0.7274(4) 0.1410(5) 0.7169(4) 0.0837 1.0000 Uani . . . . . . . C12 C 0.6093(4) 0.1975(4) 0.7676(3) 0.0723 1.0000 Uani . . . . . . . C13 C 0.3564(7) 0.2549(9) 1.1872(4) 0.1368 1.0000 Uani . . . . . . . C14 C 0.8548(6) 0.0906(6) 0.5624(5) 0.1103 1.0000 Uani . . . . . . . C15 C 0.1852(7) 0.0710(5) 0.8983(5) 0.1065 1.0000 Uani . . . . . . . C16 C 0.1741(14) 0.0171(10) 1.0029(8) 0.1948 1.0000 Uani . . . . . . . C17 C 0.3306(9) 0.0058(6) 0.8588(9) 0.1649 1.0000 Uani . . . . . . . C18 C -0.0214(4) 0.3137(6) 0.9171(3) 0.0893 1.0000 Uani . . . . . . . C19 C -0.1332(6) 0.2895(8) 0.8745(6) 0.1292 1.0000 Uani . . . . . . . C20 C -0.0491(7) 0.4479(7) 0.8954(7) 0.1366 1.0000 Uani . . . . . . . C21 C 0.2861(8) 0.4723(6) 0.4842(4) 0.1241 1.0000 Uani . . . . . . . C22 C 0.3737(7) 0.4683(6) 0.3926(4) 0.1084 1.0000 Uani . . . . . . . C24 C 0.3219(6) 0.2100(6) 0.4921(4) 0.0961 1.0000 Uani . . . . . . . C25 C 0.1890(7) 0.2513(10) 0.4357(5) 0.1368 1.0000 Uani . . . . . . . C26 C 0.3535(8) 0.0841(6) 0.5604(6) 0.1168 1.0000 Uani . . . . . . . C27 C 0.0967(11) 0.7593(10) 0.7599(8) 0.1489 1.0000 Uani . U . . . . . H1 H 0.350(4) 0.407(4) 0.749(3) 0.060(11) 1.0000 Uiso . . . . . . . H2 H 0.0724 0.2918 0.6669 0.0998 1.0000 Uiso DR U . . . . . H31 H 0.2103 0.2145 1.0673 0.0953 1.0000 Uiso R . . . . . . H51 H 0.4988 0.3519 1.0519 0.0998 1.0000 Uiso R . . . . . . H61 H 0.5028 0.3817 0.8838 0.0878 1.0000 Uiso R . . . . . . H91 H 0.5957 0.2178 0.5037 0.0880 1.0000 Uiso R . . . . . . H111 H 0.8096 0.0962 0.7509 0.0999 1.0000 Uiso R . . . . . . H121 H 0.6136 0.1908 0.8344 0.0866 1.0000 Uiso R . . . . . . H131 H 0.4383 0.1899 1.2141 0.2027 1.0000 Uiso R . . . . . . H132 H 0.3484 0.3283 1.2058 0.2029 1.0000 Uiso R . . . . . . H133 H 0.2794 0.2345 1.2122 0.2029 1.0000 Uiso R . . . . . . H141 H 0.9178 0.1289 0.5630 0.1659 1.0000 Uiso R . . . . . . H142 H 0.8334 0.0974 0.4964 0.1661 1.0000 Uiso R . . . . . . H143 H 0.8967 0.0058 0.5935 0.1658 1.0000 Uiso R . . . . . . H151 H 0.1195 0.0527 0.8636 0.1280 1.0000 Uiso R . . . . . . H161 H 0.1971 -0.0698 1.0115 0.2889 1.0000 Uiso R . . . . . . H162 H 0.2371 0.0306 1.0397 0.2890 1.0000 Uiso R . . . . . . H163 H 0.0823 0.0543 1.0251 0.2890 1.0000 Uiso R . . . . . . H171 H 0.3481 -0.0793 0.8696 0.2469 1.0000 Uiso R . . . . . . H172 H 0.3952 0.0186 0.8938 0.2469 1.0000 Uiso R . . . . . . H173 H 0.3360 0.0400 0.7902 0.2469 1.0000 Uiso R . . . . . . H181 H -0.0185 0.2836 0.9880 0.1070 1.0000 Uiso R . . . . . . H191 H -0.2188 0.3261 0.9050 0.1930 1.0000 Uiso R . . . . . . H192 H -0.1101 0.2029 0.8864 0.1930 1.0000 Uiso R . . . . . . H193 H -0.1389 0.3218 0.8057 0.1930 1.0000 Uiso R . . . . . . H201 H -0.1256 0.4888 0.9322 0.2040 1.0000 Uiso R . . . . . . H202 H 0.0291 0.4607 0.9124 0.2038 1.0000 Uiso R . . . . . . H203 H -0.0677 0.4818 0.8272 0.2039 1.0000 Uiso R . . . . . . H221 H 0.3482 0.5486 0.3518 0.1627 1.0000 Uiso R . . . . . . H222 H 0.4690 0.4382 0.4105 0.1626 1.0000 Uiso R . . . . . . H223 H 0.3592 0.4147 0.3582 0.1629 1.0000 Uiso R . . . . . . H241 H 0.3974 0.2049 0.4460 0.1159 1.0000 Uiso R . . . . . . H251 H 0.1967 0.1930 0.3977 0.2071 1.0000 Uiso R . . . . . . H252 H 0.1141 0.2543 0.4806 0.2068 1.0000 Uiso R . . . . . . H253 H 0.1711 0.3312 0.3936 0.2069 1.0000 Uiso R . . . . . . H261 H 0.3627 0.0257 0.5224 0.1747 1.0000 Uiso R . . . . . . H262 H 0.4371 0.0607 0.5953 0.1748 1.0000 Uiso R . . . . . . H263 H 0.2800 0.0880 0.6052 0.1746 1.0000 Uiso R . . . . . . C230 C 0.1518(11) 0.5631(10) 0.4739(9) 0.1170 0.665(18) Uani . . P 1 1 . . C231 C 0.2302(18) 0.5617(11) 0.5258(12) 0.0818 0.335(18) Uani . . P 1 2 . . H2301 H 0.1533 0.6383 0.4346 0.1850 0.665(18) Uiso R . P 1 1 . . H2302 H 0.1173 0.5754 0.5375 0.1850 0.665(18) Uiso R . P 1 1 . . H2303 H 0.0924 0.5373 0.4440 0.1849 0.665(18) Uiso R . P 1 1 . . H2311 H 0.2069 0.6373 0.4785 0.1119 0.335(18) Uiso R . P 1 2 . . H2312 H 0.2935 0.5584 0.5717 0.1120 0.335(18) Uiso R . P 1 2 . . H2313 H 0.1489 0.5565 0.5597 0.1120 0.335(18) Uiso R . P 1 2 . . H211 H 0.3303 0.5053 0.5228 0.1491 0.665(18) Uiso R . P 1 1 . . H212 H 0.2026 0.4818 0.4525 0.1490 0.335(18) Uiso R . P 1 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.05089(13) 0.06496(16) 0.04363(12) -0.01765(9) 0.00305(8) -0.01984(10) S1 0.1205(12) 0.1076(11) 0.1462(15) -0.0121(10) -0.0430(11) -0.0476(9) P1 0.0541(4) 0.0674(5) 0.0497(4) -0.0083(3) 0.0043(3) -0.0231(4) P2 0.0624(5) 0.0802(6) 0.0424(4) -0.0185(4) 0.0060(3) -0.0181(4) F1 0.147(5) 0.298(9) 0.188(6) -0.004(6) -0.069(4) -0.047(5) F2 0.272(11) 0.329(13) 0.327(13) -0.214(12) 0.052(9) 0.018(9) F3 0.260(10) 0.436(15) 0.244(9) -0.070(9) 0.129(8) -0.234(11) O1 0.352(13) 0.283(10) 0.240(10) 0.045(8) -0.222(10) -0.165(10) O2 0.172(5) 0.079(3) 0.238(7) -0.038(3) -0.005(5) -0.037(3) O3 0.190(6) 0.152(5) 0.168(5) -0.023(4) 0.036(4) -0.116(5) N1 0.0532(13) 0.0566(15) 0.0440(12) -0.0131(10) 0.0048(9) -0.0209(11) C1 0.0530(15) 0.0673(19) 0.0494(15) -0.0198(13) -0.0019(12) -0.0163(14) C2 0.0546(16) 0.074(2) 0.0438(14) -0.0136(14) 0.0016(12) -0.0141(15) C3 0.063(2) 0.111(3) 0.0481(17) -0.0172(19) 0.0037(14) -0.017(2) C4 0.071(2) 0.128(4) 0.0513(19) -0.032(2) -0.0055(17) -0.007(2) C5 0.068(2) 0.114(3) 0.069(2) -0.041(2) -0.0145(18) -0.019(2) C6 0.066(2) 0.094(3) 0.067(2) -0.031(2) -0.0063(16) -0.0261(19) C7 0.0508(15) 0.0631(18) 0.0524(15) -0.0147(13) 0.0070(12) -0.0211(14) C8 0.0611(17) 0.0654(19) 0.0513(16) -0.0151(14) 0.0101(13) -0.0237(15) C9 0.066(2) 0.087(3) 0.064(2) -0.0229(19) 0.0200(16) -0.0252(19) C10 0.059(2) 0.087(3) 0.086(3) -0.028(2) 0.0202(18) -0.0190(19) C11 0.0517(19) 0.099(3) 0.086(3) -0.023(2) 0.0040(18) -0.0124(19) C12 0.0604(19) 0.085(2) 0.064(2) -0.0182(18) 0.0018(15) -0.0177(18) C13 0.100(4) 0.231(8) 0.056(2) -0.051(4) -0.006(2) -0.023(5) C14 0.073(3) 0.131(5) 0.115(4) -0.047(4) 0.034(3) -0.020(3) C15 0.117(4) 0.079(3) 0.127(5) 0.013(3) -0.031(4) -0.053(3) C16 0.257(14) 0.175(9) 0.147(8) 0.077(7) -0.050(8) -0.130(9) C17 0.135(6) 0.068(3) 0.257(12) -0.028(5) -0.015(7) -0.001(4) C18 0.0553(19) 0.136(4) 0.064(2) -0.022(2) 0.0103(16) -0.025(2) C19 0.070(3) 0.172(7) 0.138(6) -0.009(5) -0.001(3) -0.051(4) C20 0.087(4) 0.140(6) 0.176(7) -0.097(6) 0.001(4) 0.001(4) C21 0.133(5) 0.104(4) 0.071(3) 0.016(3) 0.028(3) 0.000(3) C22 0.119(4) 0.131(5) 0.063(3) 0.001(3) 0.014(3) -0.050(4) C24 0.091(3) 0.142(5) 0.073(3) -0.064(3) 0.020(2) -0.043(3) C25 0.107(4) 0.246(9) 0.094(4) -0.091(5) 0.014(3) -0.077(5) C26 0.124(5) 0.109(4) 0.141(5) -0.079(4) 0.038(4) -0.048(4) C27 0.140(6) 0.166(6) 0.133(5) -0.028(5) -0.006(5) -0.050(5) C230 0.088(6) 0.118(7) 0.111(7) 0.014(5) -0.009(5) -0.023(5) C231 0.089(10) 0.056(7) 0.083(9) 0.000(6) -0.002(7) -0.018(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.0532(18) 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 . P1 . 2.2465(9) yes Pd1 . P2 . 2.2854(9) yes Pd1 . N1 . 2.164(3) yes Pd1 . H2 . 1.543 no S1 . O1 . 1.461(9) yes S1 . O2 . 1.380(6) yes S1 . O3 . 1.431(6) yes S1 . C27 . 1.809(11) yes P1 . C2 . 1.825(4) yes P1 . C15 . 1.831(5) yes P1 . C18 . 1.834(4) yes P2 . C8 . 1.829(4) yes P2 . C21 . 1.843(6) yes P2 . C24 . 1.847(5) yes F1 . C27 . 1.320(12) yes F2 . C27 . 1.327(14) yes F3 . C27 . 1.291(13) yes N1 . C1 . 1.468(4) yes N1 . C7 . 1.465(4) yes N1 . H1 . 0.85(4) no C1 . C2 . 1.385(5) yes C1 . C6 . 1.390(5) yes C2 . C3 . 1.398(5) yes C3 . C4 . 1.376(7) yes C3 . H31 . 0.937 no C4 . C5 . 1.369(8) yes C4 . C13 . 1.517(6) yes C5 . C6 . 1.394(6) yes C5 . H51 . 0.932 no C6 . H61 . 0.930 no C7 . C8 . 1.407(5) yes C7 . C12 . 1.377(5) yes C8 . C9 . 1.391(5) yes C9 . C10 . 1.384(7) yes C9 . H91 . 0.928 no C10 . C11 . 1.387(7) yes C10 . C14 . 1.519(6) yes C11 . C12 . 1.398(6) yes C11 . H111 . 0.932 no C12 . H121 . 0.930 no C13 . H131 . 0.953 no C13 . H132 . 0.959 no C13 . H133 . 0.953 no C14 . H141 . 0.948 no C14 . H142 . 0.956 no C14 . H143 . 0.959 no C15 . C16 . 1.479(11) yes C15 . C17 . 1.556(12) yes C15 . H151 . 1.000 no C16 . H161 . 0.967 no C16 . H162 . 0.961 no C16 . H163 . 0.960 no C17 . H171 . 0.952 no C17 . H172 . 0.956 no C17 . H173 . 0.964 no C18 . C19 . 1.523(8) yes C18 . C20 . 1.499(10) yes C18 . H181 . 0.979 no C19 . H191 . 0.956 no C19 . H192 . 0.958 no C19 . H193 . 0.955 no C20 . H201 . 0.954 no C20 . H202 . 0.956 no C20 . H203 . 0.958 no C21 . C22 . 1.519(8) yes C21 . C230 . 1.418(12) yes C21 . H211 . 0.984 no C21 . C22 . 1.519(8) yes C21 . C231 . 1.273(16) yes C21 . H212 . 0.979 no C22 . H221 . 0.956 no C22 . H222 . 0.964 no C22 . H223 . 0.960 no C24 . C25 . 1.526(9) yes C24 . C26 . 1.530(10) yes C24 . H241 . 0.976 no C25 . H251 . 0.960 no C25 . H252 . 0.964 no C25 . H253 . 0.967 no C26 . H261 . 0.957 no C26 . H262 . 0.960 no C26 . H263 . 0.951 no C230 . H2301 . 0.955 no C230 . H2302 . 0.961 no C230 . H2303 . 0.965 no C231 . H2311 . 0.956 no C231 . H2312 . 0.955 no C231 . H2313 . 0.960 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 P1 . Pd1 . P2 . 162.05(4) yes P1 . Pd1 . N1 . 86.56(7) yes P2 . Pd1 . N1 . 84.27(7) yes P1 . Pd1 . H2 . 94.3 no P2 . Pd1 . H2 . 95.8 no N1 . Pd1 . H2 . 176.6 no O1 . S1 . O2 . 119.6(5) yes O1 . S1 . O3 . 113.4(5) yes O2 . S1 . O3 . 116.0(5) yes O1 . S1 . C27 . 97.3(7) yes O2 . S1 . C27 . 103.1(5) yes O3 . S1 . C27 . 103.0(5) yes Pd1 . P1 . C2 . 100.35(11) yes Pd1 . P1 . C15 . 113.7(3) yes C2 . P1 . C15 . 106.1(2) yes Pd1 . P1 . C18 . 120.79(17) yes C2 . P1 . C18 . 105.7(2) yes C15 . P1 . C18 . 108.5(3) yes Pd1 . P2 . C8 . 95.45(11) yes Pd1 . P2 . C21 . 122.00(19) yes C8 . P2 . C21 . 106.3(3) yes Pd1 . P2 . C24 . 114.90(19) yes C8 . P2 . C24 . 104.2(2) yes C21 . P2 . C24 . 110.6(3) yes Pd1 . N1 . C1 . 113.6(2) yes Pd1 . N1 . C7 . 106.33(19) yes C1 . N1 . C7 . 117.9(3) yes Pd1 . N1 . H1 . 109(3) no C1 . N1 . H1 . 103(3) no C7 . N1 . H1 . 107(3) no N1 . C1 . C2 . 120.3(3) yes N1 . C1 . C6 . 119.9(3) yes C2 . C1 . C6 . 119.7(3) yes P1 . C2 . C1 . 118.8(2) yes P1 . C2 . C3 . 122.3(3) yes C1 . C2 . C3 . 118.7(4) yes C2 . C3 . C4 . 122.3(4) yes C2 . C3 . H31 . 119.3 no C4 . C3 . H31 . 118.5 no C3 . C4 . C5 . 118.0(4) yes C3 . C4 . C13 . 120.2(6) yes C5 . C4 . C13 . 121.7(5) yes C4 . C5 . C6 . 121.5(4) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 119.5 no C5 . C6 . C1 . 119.7(4) yes C5 . C6 . H61 . 119.6 no C1 . C6 . H61 . 120.7 no N1 . C7 . C8 . 118.2(3) yes N1 . C7 . C12 . 122.8(3) yes C8 . C7 . C12 . 119.0(3) yes P2 . C8 . C7 . 117.7(2) yes P2 . C8 . C9 . 122.7(3) yes C7 . C8 . C9 . 119.2(3) yes C8 . C9 . C10 . 122.3(4) yes C8 . C9 . H91 . 119.0 no C10 . C9 . H91 . 118.8 no C9 . C10 . C11 . 117.4(3) yes C9 . C10 . C14 . 121.5(5) yes C11 . C10 . C14 . 121.1(5) yes C10 . C11 . C12 . 121.6(4) yes C10 . C11 . H111 . 119.2 no C12 . C11 . H111 . 119.2 no C11 . C12 . C7 . 120.2(4) yes C11 . C12 . H121 . 120.0 no C7 . C12 . H121 . 119.8 no C4 . C13 . H131 . 110.3 no C4 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.6 no C4 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.3 no H132 . C13 . H133 . 108.7 no C10 . C14 . H141 . 110.3 no C10 . C14 . H142 . 110.2 no H141 . C14 . H142 . 109.2 no C10 . C14 . H143 . 109.3 no H141 . C14 . H143 . 108.7 no H142 . C14 . H143 . 109.2 no P1 . C15 . C16 . 116.8(7) yes P1 . C15 . C17 . 108.0(4) yes C16 . C15 . C17 . 110.8(8) yes P1 . C15 . H151 . 108.4 no C16 . C15 . H151 . 105.7 no C17 . C15 . H151 . 106.7 no C15 . C16 . H161 . 109.3 no C15 . C16 . H162 . 109.2 no H161 . C16 . H162 . 109.4 no C15 . C16 . H163 . 109.9 no H161 . C16 . H163 . 109.3 no H162 . C16 . H163 . 109.8 no C15 . C17 . H171 . 108.5 no C15 . C17 . H172 . 107.7 no H171 . C17 . H172 . 110.3 no C15 . C17 . H173 . 110.1 no H171 . C17 . H173 . 110.6 no H172 . C17 . H173 . 109.4 no P1 . C18 . C19 . 110.2(4) yes P1 . C18 . C20 . 108.3(4) yes C19 . C18 . C20 . 111.0(5) yes P1 . C18 . H181 . 109.6 no C19 . C18 . H181 . 109.3 no C20 . C18 . H181 . 108.5 no C18 . C19 . H191 . 109.7 no C18 . C19 . H192 . 109.0 no H191 . C19 . H192 . 109.3 no C18 . C19 . H193 . 109.5 no H191 . C19 . H193 . 110.6 no H192 . C19 . H193 . 108.8 no C18 . C20 . H201 . 110.4 no C18 . C20 . H202 . 109.9 no H201 . C20 . H202 . 108.4 no C18 . C20 . H203 . 109.7 no H201 . C20 . H203 . 109.4 no H202 . C20 . H203 . 109.0 no P2 . C21 . C22 . 115.1(5) yes P2 . C21 . C230 . 117.8(6) yes C22 . C21 . C230 . 116.0(6) yes P2 . C21 . H211 . 101.2 no C22 . C21 . H211 . 101.4 no C230 . C21 . H211 . 101.0 no P2 . C21 . C22 . 115.1(5) yes P2 . C21 . C231 . 113.9(7) yes C22 . C21 . C231 . 127.8(9) yes P2 . C21 . H212 . 95.9 no C22 . C21 . H212 . 95.9 no C231 . C21 . H212 . 96.0 no C21 . C22 . H221 . 109.7 no C21 . C22 . H222 . 109.5 no H221 . C22 . H222 . 109.6 no C21 . C22 . H223 . 108.8 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.7 no P2 . C24 . C25 . 110.0(4) yes P2 . C24 . C26 . 109.2(4) yes C25 . C24 . C26 . 111.6(6) yes P2 . C24 . H241 . 108.7 no C25 . C24 . H241 . 109.0 no C26 . C24 . H241 . 108.4 no C24 . C25 . H251 . 109.3 no C24 . C25 . H252 . 109.7 no H251 . C25 . H252 . 107.8 no C24 . C25 . H253 . 109.8 no H251 . C25 . H253 . 110.2 no H252 . C25 . H253 . 109.9 no C24 . C26 . H261 . 109.0 no C24 . C26 . H262 . 109.8 no H261 . C26 . H262 . 109.8 no C24 . C26 . H263 . 109.0 no H261 . C26 . H263 . 109.4 no H262 . C26 . H263 . 109.8 no S1 . C27 . F2 . 109.9(9) yes S1 . C27 . F1 . 107.5(8) yes F2 . C27 . F1 . 109.9(10) yes S1 . C27 . F3 . 108.1(9) yes F2 . C27 . F3 . 107.5(11) yes F1 . C27 . F3 . 113.9(11) yes C21 . C230 . H2301 . 110.2 no C21 . C230 . H2302 . 108.7 no H2301 . C230 . H2302 . 109.1 no C21 . C230 . H2303 . 110.3 no H2301 . C230 . H2303 . 109.2 no H2302 . C230 . H2303 . 109.3 no C21 . C231 . H2311 . 110.0 no C21 . C231 . H2312 . 108.8 no H2311 . C231 . H2312 . 109.3 no C21 . C231 . H2313 . 110.1 no H2311 . C231 . H2313 . 109.5 no H2312 . C231 . H2313 . 109.2 no #===END data_3x _database_code_depnum_ccdc_archive 'CCDC 756642' #TrackingRef 'MS-0027-combcifs.cif' _audit_creation_date 07-07-08 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'OZ105_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 7.4428(3) _cell_length_b 14.0784(5) _cell_length_c 16.0196(6) _cell_angle_alpha 80.6324(17) _cell_angle_beta 78.8425(18) _cell_angle_gamma 80.3944(17) _cell_volume 1608.92(11) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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' 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' _cell_formula_units_Z 2 # Given Formula = C35 H47 N1 P2 Pd1 # Dc = 1.34 Fooo = 680.00 Mu = 7.00 M = 650.11 # Found Formula = C35 H47 N1 P2 Pd1 # Dc = 1.34 FOOO = 680.00 Mu = 7.00 M = 650.11 _chemical_formula_sum 'C35 H47 N1 P2 Pd1' _chemical_formula_moiety 'C35 H47 N1 P2 Pd1' _chemical_compound_source ? _chemical_formula_weight 650.11 _cell_measurement_reflns_used 9878 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.700 # Sheldrick geometric approximatio 0.87 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.91 _diffrn_measurement_device_type 'KappaCCD ApexII' _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 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _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 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 49214 _reflns_number_total 9404 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections with Friedels Law is 9404 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9445 _diffrn_reflns_theta_min 1.308 _diffrn_reflns_theta_max 30.069 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.069 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.21 _refine_diff_density_max 2.17 # 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 9404 _refine_ls_number_restraints 0 _refine_ls_number_parameters 353 _oxford_refine_ls_R_factor_ref 0.0504 _refine_ls_wR_factor_ref 0.1333 _refine_ls_goodness_of_fit_ref 0.9847 _refine_ls_shift/su_max 0.004126 # The values computed from all data _oxford_reflns_number_all 9404 _refine_ls_R_factor_all 0.0504 _refine_ls_wR_factor_all 0.1333 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8158 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_gt 0.1269 # 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^) + ( 0.00P)^2^ + 1.31P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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 (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. 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 C1 C 1.0779(4) 0.4070(2) 0.6977(2) 0.0141 1.0000 Uani . . . . . . . C2 C 1.1419(4) 0.4947(2) 0.6613(2) 0.0164 1.0000 Uani . . . . . . . C3 C 1.2109(5) 0.5148(2) 0.5745(2) 0.0194 1.0000 Uani . . . . . . . C4 C 1.2002(5) 0.4449(2) 0.5236(2) 0.0198 1.0000 Uani . . . . . . . C5 C 1.1374(5) 0.3578(2) 0.5577(2) 0.0172 1.0000 Uani . . . . . . . C6 C 1.0830(4) 0.3322(2) 0.6467(2) 0.0135 1.0000 Uani . . . . . . . C7 C 1.0684(4) 0.1595(2) 0.64744(19) 0.0136 1.0000 Uani . . . . . . . C8 C 1.2119(4) 0.1425(2) 0.5770(2) 0.0157 1.0000 Uani . . . . . . . C9 C 1.2504(5) 0.0544(2) 0.5446(2) 0.0174 1.0000 Uani . . . . . . . C10 C 1.1530(5) -0.0237(2) 0.5802(2) 0.0185 1.0000 Uani . . . . . . . C11 C 1.0163(5) -0.0093(2) 0.6512(2) 0.0165 1.0000 Uani . . . . . . . C12 C 0.9733(4) 0.0792(2) 0.68463(19) 0.0139 1.0000 Uani . . . . . . . C13 C 1.2838(6) 0.6089(3) 0.5359(3) 0.0270 1.0000 Uani . . . . . . . C14 C 1.1967(5) -0.1185(3) 0.5436(2) 0.0238 1.0000 Uani . . . . . . . C15 C 0.7540(4) 0.4899(2) 0.8041(2) 0.0150 1.0000 Uani . . . . . . . C16 C 0.6384(5) 0.4966(3) 0.8931(2) 0.0208 1.0000 Uani . . . . . . . C17 C 0.6351(5) 0.4774(3) 0.7391(2) 0.0213 1.0000 Uani . . . . . . . C18 C 1.0772(5) 0.4048(2) 0.8864(2) 0.0181 1.0000 Uani . . . . . . . C19 C 1.1302(5) 0.5062(3) 0.8809(2) 0.0243 1.0000 Uani . . . . . . . C20 C 1.2454(5) 0.3250(3) 0.8857(3) 0.0267 1.0000 Uani . . . . . . . C21 C 0.5755(5) 0.1029(2) 0.7594(2) 0.0181 1.0000 Uani . . . . . . . C22 C 0.5379(5) 0.1950(2) 0.6965(3) 0.0237 1.0000 Uani . . . . . . . C23 C 0.5378(5) 0.0134(3) 0.7268(3) 0.0250 1.0000 Uani . . . . . . . C24 C 0.8587(5) -0.0164(2) 0.8572(2) 0.0177 1.0000 Uani . . . . . . . C25 C 1.0476(5) -0.0190(3) 0.8816(2) 0.0259 1.0000 Uani . . . . . . . C26 C 0.7073(6) -0.0193(3) 0.9363(2) 0.0249 1.0000 Uani . . . . . . . C27 C 0.7405(5) 0.2354(2) 0.9285(2) 0.0167 1.0000 Uani . . . . . . . C28 C 0.6652(5) 0.2377(2) 1.0010(2) 0.0201 1.0000 Uani . . . . . . . C29 C 0.5753(5) 0.2426(2) 1.0884(2) 0.0196 1.0000 Uani . . . . . . . C30 C 0.6753(6) 0.2487(3) 1.1526(2) 0.0252 1.0000 Uani . . . . . . . C31 C 0.5865(7) 0.2548(3) 1.2368(2) 0.0302 1.0000 Uani . . . . . . . C32 C 0.3971(6) 0.2561(3) 1.2601(2) 0.0282 1.0000 Uani . . . . . . . C33 C 0.2955(6) 0.2501(2) 1.1968(2) 0.0253 1.0000 Uani . . . . . . . C34 C 0.3823(5) 0.2430(2) 1.1127(2) 0.0216 1.0000 Uani . . . . . . . C35 C 0.2995(8) 0.2634(3) 1.3513(3) 0.0395 1.0000 Uani . . . . . . . Pd1 Pd 0.87398(3) 0.238606(16) 0.808382(14) 0.0107 1.0000 Uani . . . . . . . P2 P 0.81114(11) 0.09446(6) 0.78253(5) 0.0126 1.0000 Uani . . . . . . . N5 N 1.0249(4) 0.24443(19) 0.68574(16) 0.0136 1.0000 Uani . . . . . . . P1 P 0.94671(11) 0.38877(6) 0.80482(5) 0.0123 1.0000 Uani . . . . . . . H21 H 1.1380 0.5425 0.6974 0.0198 1.0000 Uiso R . . . . . . H41 H 1.2377 0.4580 0.4632 0.0226 1.0000 Uiso R . . . . . . H51 H 1.1304 0.3135 0.5199 0.0197 1.0000 Uiso R . . . . . . H81 H 1.2836 0.1928 0.5512 0.0187 1.0000 Uiso R . . . . . . H91 H 1.3463 0.0467 0.4966 0.0203 1.0000 Uiso R . . . . . . H111 H 0.9496 -0.0613 0.6780 0.0197 1.0000 Uiso R . . . . . . H131 H 1.3777 0.5979 0.4877 0.0309 1.0000 Uiso R . . . . . . H132 H 1.3337 0.6326 0.5775 0.0309 1.0000 Uiso R . . . . . . H133 H 1.1858 0.6555 0.5182 0.0309 1.0000 Uiso R . . . . . . H141 H 1.1702 -0.1703 0.5881 0.0283 1.0000 Uiso R . . . . . . H142 H 1.3240 -0.1285 0.5188 0.0283 1.0000 Uiso R . . . . . . H143 H 1.1235 -0.1165 0.5007 0.0283 1.0000 Uiso R . . . . . . H151 H 0.8049 0.5489 0.7851 0.0178 1.0000 Uiso R . . . . . . H161 H 0.7154 0.5043 0.9317 0.0246 1.0000 Uiso R . . . . . . H162 H 0.5439 0.5509 0.8903 0.0246 1.0000 Uiso R . . . . . . H163 H 0.5838 0.4389 0.9128 0.0246 1.0000 Uiso R . . . . . . H171 H 0.7109 0.4734 0.6844 0.0255 1.0000 Uiso R . . . . . . H172 H 0.5406 0.5315 0.7351 0.0255 1.0000 Uiso R . . . . . . H173 H 0.5806 0.4195 0.7576 0.0255 1.0000 Uiso R . . . . . . H181 H 0.9996 0.3928 0.9405 0.0223 1.0000 Uiso R . . . . . . H191 H 1.0223 0.5530 0.8815 0.0309 1.0000 Uiso R . . . . . . H192 H 1.1869 0.5089 0.9286 0.0309 1.0000 Uiso R . . . . . . H193 H 1.2143 0.5197 0.8291 0.0309 1.0000 Uiso R . . . . . . H201 H 1.2059 0.2634 0.8893 0.0318 1.0000 Uiso R . . . . . . H202 H 1.3034 0.3257 0.9334 0.0318 1.0000 Uiso R . . . . . . H203 H 1.3308 0.3364 0.8340 0.0318 1.0000 Uiso R . . . . . . H211 H 0.4918 0.1105 0.8116 0.0218 1.0000 Uiso R . . . . . . H221 H 0.5625 0.2493 0.7185 0.0293 1.0000 Uiso R . . . . . . H222 H 0.4122 0.2044 0.6892 0.0293 1.0000 Uiso R . . . . . . H223 H 0.6158 0.1884 0.6426 0.0293 1.0000 Uiso R . . . . . . H231 H 0.5622 -0.0426 0.7671 0.0315 1.0000 Uiso R . . . . . . H232 H 0.4121 0.0215 0.7197 0.0315 1.0000 Uiso R . . . . . . H233 H 0.6157 0.0055 0.6732 0.0315 1.0000 Uiso R . . . . . . H241 H 0.8614 -0.0712 0.8292 0.0205 1.0000 Uiso R . . . . . . H251 H 1.1392 -0.0171 0.8313 0.0299 1.0000 Uiso R . . . . . . H252 H 1.0462 0.0356 0.9098 0.0299 1.0000 Uiso R . . . . . . H253 H 1.0752 -0.0771 0.9190 0.0299 1.0000 Uiso R . . . . . . H261 H 0.5913 -0.0176 0.9192 0.0292 1.0000 Uiso R . . . . . . H262 H 0.7036 0.0352 0.9648 0.0292 1.0000 Uiso R . . . . . . H263 H 0.7326 -0.0775 0.9740 0.0292 1.0000 Uiso R . . . . . . H301 H 0.8053 0.2486 1.1385 0.0292 1.0000 Uiso R . . . . . . H311 H 0.6575 0.2581 1.2793 0.0358 1.0000 Uiso R . . . . . . H331 H 0.1655 0.2508 1.2116 0.0284 1.0000 Uiso R . . . . . . H341 H 0.3107 0.2384 1.0708 0.0252 1.0000 Uiso R . . . . . . H351 H 0.1771 0.2959 1.3509 0.0453 1.0000 Uiso R . . . . . . H352 H 0.3649 0.2989 1.3781 0.0453 1.0000 Uiso R . . . . . . H353 H 0.2955 0.2000 1.3823 0.0453 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 C1 0.0146(13) 0.0140(13) 0.0133(13) -0.0031(10) -0.0007(10) -0.0017(11) C2 0.0172(14) 0.0150(13) 0.0173(14) -0.0032(11) -0.0021(11) -0.0030(11) C3 0.0168(14) 0.0167(14) 0.0214(16) 0.0008(12) 0.0018(12) -0.0022(12) C4 0.0232(16) 0.0198(15) 0.0136(14) -0.0007(11) 0.0014(12) -0.0021(12) C5 0.0195(15) 0.0181(14) 0.0117(13) -0.0031(11) 0.0022(11) -0.0007(12) C6 0.0125(13) 0.0137(13) 0.0135(13) -0.0025(10) -0.0013(10) -0.0002(10) C7 0.0147(13) 0.0149(13) 0.0113(13) -0.0041(10) -0.0032(10) 0.0009(11) C8 0.0138(13) 0.0181(14) 0.0150(14) -0.0028(11) -0.0029(11) -0.0008(11) C9 0.0161(14) 0.0202(15) 0.0146(14) -0.0066(11) -0.0006(11) 0.0030(11) C10 0.0212(15) 0.0167(14) 0.0183(15) -0.0091(12) -0.0063(12) 0.0052(12) C11 0.0199(15) 0.0127(13) 0.0167(14) -0.0041(11) -0.0029(11) 0.0006(11) C12 0.0150(13) 0.0141(13) 0.0115(13) -0.0035(10) -0.0009(10) 0.0008(10) C13 0.0288(19) 0.0200(16) 0.0284(19) 0.0048(14) 0.0022(15) -0.0089(14) C14 0.0277(18) 0.0203(16) 0.0228(17) -0.0115(13) -0.0036(14) 0.0058(13) C15 0.0151(13) 0.0098(12) 0.0196(14) -0.0047(11) -0.0028(11) 0.0024(10) C16 0.0184(15) 0.0218(15) 0.0213(16) -0.0083(13) 0.0005(12) 0.0007(12) C17 0.0188(15) 0.0217(15) 0.0232(16) -0.0032(13) -0.0061(13) 0.0009(12) C18 0.0187(15) 0.0238(15) 0.0135(14) -0.0054(11) -0.0035(11) -0.0039(12) C19 0.0258(17) 0.0288(18) 0.0227(17) -0.0105(14) -0.0058(14) -0.0072(14) C20 0.0228(17) 0.0286(18) 0.0282(19) -0.0003(14) -0.0093(14) 0.0002(14) C21 0.0155(14) 0.0195(14) 0.0196(15) -0.0072(12) -0.0006(11) -0.0016(12) C22 0.0254(17) 0.0165(15) 0.0314(19) -0.0065(13) -0.0122(15) 0.0025(13) C23 0.0241(17) 0.0215(16) 0.033(2) -0.0073(14) -0.0099(15) -0.0040(13) C24 0.0244(16) 0.0132(13) 0.0137(14) -0.0017(11) 0.0001(12) -0.0016(12) C25 0.0264(18) 0.0265(17) 0.0219(17) 0.0000(14) -0.0054(14) 0.0031(14) C26 0.0330(19) 0.0216(16) 0.0184(16) -0.0022(13) 0.0023(14) -0.0075(14) C27 0.0187(14) 0.0135(13) 0.0181(14) -0.0043(11) -0.0026(11) -0.0009(11) C28 0.0254(17) 0.0146(14) 0.0184(15) -0.0036(11) -0.0013(12) 0.0009(12) C29 0.0306(18) 0.0101(13) 0.0152(14) -0.0027(11) 0.0019(13) -0.0002(12) C30 0.034(2) 0.0233(16) 0.0159(15) -0.0042(13) -0.0007(14) 0.0007(14) C31 0.052(3) 0.0242(17) 0.0134(16) -0.0040(13) -0.0063(16) 0.0000(17) C32 0.048(2) 0.0166(15) 0.0148(15) -0.0024(12) 0.0052(15) -0.0014(15) C33 0.0340(19) 0.0147(14) 0.0223(17) -0.0014(12) 0.0064(14) -0.0035(13) C34 0.0317(18) 0.0128(13) 0.0185(15) -0.0024(11) 0.0014(13) -0.0043(13) C35 0.065(3) 0.034(2) 0.0148(17) -0.0068(15) 0.0084(18) -0.007(2) Pd1 0.01323(11) 0.01018(10) 0.00809(10) -0.00259(7) -0.00004(7) -0.00062(7) P2 0.0146(3) 0.0118(3) 0.0110(3) -0.0030(3) -0.0006(3) -0.0010(3) N5 0.0164(12) 0.0138(11) 0.0092(11) -0.0034(9) 0.0019(9) -0.0013(9) P1 0.0142(3) 0.0123(3) 0.0106(3) -0.0037(3) -0.0011(3) -0.0017(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4881(8) loop_ _oxford_twin_element_scale_factors 0.8408(16) 0.1592(16) 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 C1 . C2 . 1.395(4) yes C1 . C6 . 1.425(4) yes C1 . P1 . 1.804(3) yes C2 . C3 . 1.385(5) yes C2 . H21 . 0.950 no C3 . C4 . 1.397(5) yes C3 . C13 . 1.509(5) yes C4 . C5 . 1.377(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.409(4) yes C5 . H51 . 0.950 no C6 . N5 . 1.389(4) yes C7 . C8 . 1.417(4) yes C7 . C12 . 1.420(4) yes C7 . N5 . 1.394(4) yes C8 . C9 . 1.386(4) yes C8 . H81 . 0.950 no C9 . C10 . 1.400(5) yes C9 . H91 . 0.950 no C10 . C11 . 1.388(5) yes C10 . C14 . 1.507(4) yes C11 . C12 . 1.401(4) yes C11 . H111 . 0.950 no C12 . P2 . 1.804(3) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . C16 . 1.525(5) yes C15 . C17 . 1.538(5) yes C15 . P1 . 1.845(3) yes C15 . H151 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . C19 . 1.528(5) yes C18 . C20 . 1.536(5) yes C18 . P1 . 1.834(3) yes C18 . H181 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . C22 . 1.530(5) yes C21 . C23 . 1.526(5) yes C21 . P2 . 1.842(3) yes C21 . H211 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . C25 . 1.524(5) yes C24 . C26 . 1.524(5) yes C24 . P2 . 1.833(3) yes C24 . H241 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . C28 . 1.191(5) yes C27 . Pd1 . 1.984(3) yes C28 . C29 . 1.438(5) yes C29 . C30 . 1.402(5) yes C29 . C34 . 1.413(5) yes C30 . C31 . 1.391(5) yes C30 . H301 . 0.950 no C31 . C32 . 1.384(6) yes C31 . H311 . 0.950 no C32 . C33 . 1.397(6) yes C32 . C35 . 1.512(5) yes C33 . C34 . 1.389(5) yes C33 . H331 . 0.950 no C34 . H341 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 no Pd1 . P2 . 2.2746(8) yes Pd1 . N5 . 2.062(3) yes Pd1 . P1 . 2.2574(8) yes 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 C2 . C1 . C6 . 121.0(3) yes C2 . C1 . P1 . 122.9(2) yes C6 . C1 . P1 . 115.2(2) yes C1 . C2 . C3 . 122.6(3) yes C1 . C2 . H21 . 118.7 no C3 . C2 . H21 . 118.7 no C2 . C3 . C4 . 116.1(3) yes C2 . C3 . C13 . 122.3(3) yes C4 . C3 . C13 . 121.5(3) yes C3 . C4 . C5 . 122.5(3) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 118.8 no C4 . C5 . C6 . 122.1(3) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 119.0 no C1 . C6 . C5 . 115.2(3) yes C1 . C6 . N5 . 119.4(3) yes C5 . C6 . N5 . 125.2(3) yes C8 . C7 . C12 . 115.6(3) yes C8 . C7 . N5 . 125.4(3) yes C12 . C7 . N5 . 118.8(3) yes C7 . C8 . C9 . 121.7(3) yes C7 . C8 . H81 . 119.1 no C9 . C8 . H81 . 119.1 no C8 . C9 . C10 . 122.4(3) yes C8 . C9 . H91 . 118.8 no C10 . C9 . H91 . 118.8 no C9 . C10 . C11 . 116.6(3) yes C9 . C10 . C14 . 121.4(3) yes C11 . C10 . C14 . 122.0(3) yes C10 . C11 . C12 . 122.2(3) yes C10 . C11 . H111 . 118.9 no C12 . C11 . H111 . 118.9 no C7 . C12 . C11 . 121.5(3) yes C7 . C12 . P2 . 116.1(2) yes C11 . C12 . P2 . 122.2(2) yes C3 . C13 . H131 . 109.4 no C3 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C3 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no C10 . C14 . H141 . 109.4 no C10 . C14 . H142 . 109.5 no H141 . C14 . H142 . 109.5 no C10 . C14 . H143 . 109.5 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no C16 . C15 . C17 . 111.4(3) yes C16 . C15 . P1 . 112.2(2) yes C17 . C15 . P1 . 108.7(2) yes C16 . C15 . H151 . 108.1 no C17 . C15 . H151 . 108.1 no P1 . C15 . H151 . 108.1 no C15 . C16 . H161 . 109.4 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C15 . C17 . H171 . 109.4 no C15 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no C15 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C19 . C18 . C20 . 112.4(3) yes C19 . C18 . P1 . 115.8(2) yes C20 . C18 . P1 . 108.4(2) yes C19 . C18 . H181 . 106.6 no C20 . C18 . H181 . 106.6 no P1 . C18 . H181 . 106.6 no C18 . C19 . H191 . 109.4 no C18 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.4 no C18 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C22 . C21 . C23 . 111.4(3) yes C22 . C21 . P2 . 108.6(2) yes C23 . C21 . P2 . 114.4(2) yes C22 . C21 . H211 . 107.4 no C23 . C21 . H211 . 107.4 no P2 . C21 . H211 . 107.4 no C21 . C22 . H221 . 109.4 no C21 . C22 . H222 . 109.5 no H221 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.4 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C21 . C23 . H231 . 109.4 no C21 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C21 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C25 . C24 . C26 . 111.2(3) yes C25 . C24 . P2 . 108.8(2) yes C26 . C24 . P2 . 110.3(2) yes C25 . C24 . H241 . 108.8 no C26 . C24 . H241 . 108.8 no P2 . C24 . H241 . 108.8 no C24 . C25 . H251 . 109.5 no C24 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C24 . C25 . H253 . 109.5 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C24 . C26 . H261 . 109.5 no C24 . C26 . H262 . 109.5 no H261 . C26 . H262 . 109.5 no C24 . C26 . H263 . 109.5 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C28 . C27 . Pd1 . 176.4(3) yes C27 . C28 . C29 . 178.7(4) yes C28 . C29 . C30 . 121.3(3) yes C28 . C29 . C34 . 121.3(3) yes C30 . C29 . C34 . 117.4(3) yes C29 . C30 . C31 . 120.8(4) yes C29 . C30 . H301 . 119.6 no C31 . C30 . H301 . 119.6 no C30 . C31 . C32 . 121.5(4) yes C30 . C31 . H311 . 119.2 no C32 . C31 . H311 . 119.2 no C31 . C32 . C33 . 118.3(3) yes C31 . C32 . C35 . 121.8(4) yes C33 . C32 . C35 . 119.9(4) yes C32 . C33 . C34 . 120.9(4) yes C32 . C33 . H331 . 119.6 no C34 . C33 . H331 . 119.5 no C29 . C34 . C33 . 121.0(4) yes C29 . C34 . H341 . 119.5 no C33 . C34 . H341 . 119.5 no C32 . C35 . H351 . 109.5 no C32 . C35 . H352 . 109.3 no H351 . C35 . H352 . 109.5 no C32 . C35 . H353 . 109.5 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C27 . Pd1 . P2 . 98.00(9) yes C27 . Pd1 . N5 . 176.79(12) yes P2 . Pd1 . N5 . 84.29(8) yes C27 . Pd1 . P1 . 92.84(9) yes P2 . Pd1 . P1 . 168.39(3) yes N5 . Pd1 . P1 . 85.05(8) yes C21 . P2 . C24 . 108.97(16) yes C21 . P2 . C12 . 108.37(15) yes C24 . P2 . C12 . 106.02(14) yes C21 . P2 . Pd1 . 112.54(11) yes C24 . P2 . Pd1 . 119.93(11) yes C12 . P2 . Pd1 . 99.90(11) yes C7 . N5 . C6 . 123.4(3) yes C7 . N5 . Pd1 . 118.4(2) yes C6 . N5 . Pd1 . 118.1(2) yes C15 . P1 . C18 . 106.71(15) yes C15 . P1 . C1 . 103.36(15) yes C18 . P1 . C1 . 112.06(15) yes C15 . P1 . Pd1 . 116.44(11) yes C18 . P1 . Pd1 . 116.76(11) yes C1 . P1 . Pd1 . 100.65(10) yes #===END data_6x _database_code_depnum_ccdc_archive 'CCDC 756643' #TrackingRef 'MS-0027-combcifs.cif' _audit_creation_date 07-07-07 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'OZ106_0ma in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.1054(8) _cell_length_b 12.5938(16) _cell_length_c 13.8501(9) _cell_angle_alpha 101.203(4) _cell_angle_beta 111.981(3) _cell_angle_gamma 99.265(4) _cell_volume 1856.2(3) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-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' 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' _cell_formula_units_Z 2 # Given Formula = C38 H62 N1 P3 Pd1 # Dc = 1.31 Fooo = 776.00 Mu = 6.56 M = 732.24 # Found Formula = C38 H62 N1 P3 Pd1 # Dc = 1.31 FOOO = 776.00 Mu = 6.56 M = 732.24 _chemical_formula_sum 'C38 H62 N1 P3 Pd1' _chemical_formula_moiety 'C38 H62 N1 P3 Pd1' _chemical_compound_source ? _chemical_formula_weight 732.24 _cell_measurement_reflns_used 9842 _cell_measurement_theta_min 2 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour clear _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_max 0.36 _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.656 # Sheldrick geometric approximatio 0.81 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.90 _diffrn_measurement_device_type 'KappaCCD ApexII' _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 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _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 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 49993 _reflns_number_total 10867 _diffrn_reflns_av_R_equivalents 0.059 # Number of reflections with Friedels Law is 10867 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 10890 _diffrn_reflns_theta_min 1.651 _diffrn_reflns_theta_max 30.062 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.062 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -17 _reflns_limit_h_max 15 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.92 _refine_diff_density_max 0.62 # 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 10867 _refine_ls_number_restraints 0 _refine_ls_number_parameters 388 _oxford_refine_ls_R_factor_ref 0.0363 _refine_ls_wR_factor_ref 0.0786 _refine_ls_goodness_of_fit_ref 0.8815 _refine_ls_shift/su_max 0.000936 # The values computed from all data _oxford_reflns_number_all 10867 _refine_ls_R_factor_all 0.0363 _refine_ls_wR_factor_all 0.0786 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9217 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_gt 0.0706 # 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, 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: 33.9 52.1 28.2 10.6 2.00 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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 (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; 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 C1 C 0.05829(16) 0.28521(15) 0.27465(15) 0.0133 1.0000 Uani . . . . . . . C2 C -0.01139(17) 0.33065(15) 0.32464(15) 0.0156 1.0000 Uani . . . . . . . C3 C -0.06742(17) 0.41415(15) 0.29462(16) 0.0167 1.0000 Uani . . . . . . . C4 C -0.05183(18) 0.45189(16) 0.21086(16) 0.0170 1.0000 Uani . . . . . . . C5 C 0.01790(17) 0.40967(15) 0.16068(15) 0.0158 1.0000 Uani . . . . . . . C6 C 0.07537(16) 0.32460(14) 0.19093(14) 0.0128 1.0000 Uani . . . . . . . C7 C 0.14762(16) 0.28691(15) 0.04928(14) 0.0133 1.0000 Uani . . . . . . . C8 C 0.04112(17) 0.28717(16) -0.03967(15) 0.0161 1.0000 Uani . . . . . . . C9 C 0.04098(18) 0.28027(17) -0.14040(16) 0.0190 1.0000 Uani . . . . . . . C10 C 0.14647(19) 0.27689(16) -0.15864(15) 0.0173 1.0000 Uani . . . . . . . C11 C 0.25281(17) 0.27936(15) -0.07069(15) 0.0159 1.0000 Uani . . . . . . . C12 C 0.25486(16) 0.28218(15) 0.03139(14) 0.0133 1.0000 Uani . . . . . . . C13 C -0.1353(2) 0.46641(18) 0.35447(19) 0.0229 1.0000 Uani . . . . . . . C14 C 0.1441(2) 0.2658(2) -0.26972(17) 0.0255 1.0000 Uani . . . . . . . C15 C 0.17338(17) 0.19979(16) 0.45750(14) 0.0155 1.0000 Uani . . . . . . . C16 C 0.27821(19) 0.30587(19) 0.52123(16) 0.0233 1.0000 Uani . . . . . . . C17 C 0.2052(2) 0.09871(19) 0.49718(17) 0.0239 1.0000 Uani . . . . . . . C18 C 0.01316(17) 0.04381(15) 0.24357(15) 0.0163 1.0000 Uani . . . . . . . C19 C -0.03055(19) 0.01992(17) 0.12091(16) 0.0206 1.0000 Uani . . . . . . . C20 C -0.0959(2) 0.04082(18) 0.27497(19) 0.0240 1.0000 Uani . . . . . . . C21 C 0.47461(17) 0.20505(16) 0.07794(15) 0.0152 1.0000 Uani . . . . . . . C22 C 0.60168(18) 0.20056(18) 0.15632(16) 0.0202 1.0000 Uani . . . . . . . C23 C 0.39973(18) 0.08966(16) -0.00001(16) 0.0180 1.0000 Uani . . . . . . . C24 C 0.48192(18) 0.41177(16) 0.22087(16) 0.0174 1.0000 Uani . . . . . . . C25 C 0.5228(2) 0.47565(18) 0.15138(19) 0.0261 1.0000 Uani . . . . . . . C26 C 0.4153(2) 0.47765(17) 0.27608(18) 0.0229 1.0000 Uani . . . . . . . C27 C 0.56070(16) 0.19618(15) 0.39977(14) 0.0143 1.0000 Uani . . . . . . . C28 C 0.57777(18) 0.29747(16) 0.49067(16) 0.0178 1.0000 Uani . . . . . . . C29 C 0.70696(19) 0.37586(17) 0.53977(17) 0.0216 1.0000 Uani . . . . . . . C30 C 0.8054(2) 0.3128(2) 0.57954(19) 0.0276 1.0000 Uani . . . . . . . C31 C 0.78990(19) 0.21281(18) 0.48945(19) 0.0239 1.0000 Uani . . . . . . . C32 C 0.66072(17) 0.13409(16) 0.44078(16) 0.0176 1.0000 Uani . . . . . . . C33 C 0.40134(17) -0.02026(15) 0.24738(15) 0.0152 1.0000 Uani . . . . . . . C34 C 0.4373(2) -0.11118(16) 0.30436(17) 0.0206 1.0000 Uani . . . . . . . C35 C 0.4438(2) -0.21286(18) 0.2283(2) 0.0271 1.0000 Uani . . . . . . . C36 C 0.3208(2) -0.26378(18) 0.1288(2) 0.0281 1.0000 Uani . . . . . . . C37 C 0.2816(2) -0.17445(17) 0.07287(17) 0.0219 1.0000 Uani . . . . . . . C38 C 0.27627(18) -0.07229(16) 0.14974(16) 0.0180 1.0000 Uani . . . . . . . Pd1 Pd 0.276638(12) 0.200848(11) 0.239879(10) 0.0110 1.0000 Uani . . . . . . . P1 P 0.13429(4) 0.17688(4) 0.31151(4) 0.0117 1.0000 Uani . . . . . . . N1 N 0.15215(14) 0.28260(13) 0.14940(12) 0.0135 1.0000 Uani . . . . . . . P2 P 0.38414(4) 0.26747(4) 0.14502(4) 0.0120 1.0000 Uani . . . . . . . P3 P 0.40007(4) 0.10432(4) 0.34643(4) 0.0138 1.0000 Uani . . . . . . . H21 H -0.0207 0.3034 0.3812 0.0205 1.0000 Uiso R . . . . . . H41 H -0.0901 0.5081 0.1877 0.0211 1.0000 Uiso R . . . . . . H51 H 0.0273 0.4384 0.1049 0.0205 1.0000 Uiso R . . . . . . H81 H -0.0317 0.2922 -0.0300 0.0197 1.0000 Uiso R . . . . . . H91 H -0.0332 0.2777 -0.1991 0.0225 1.0000 Uiso R . . . . . . H111 H 0.3264 0.2791 -0.0804 0.0207 1.0000 Uiso R . . . . . . H131 H -0.1690 0.4131 0.3827 0.0320 1.0000 Uiso R . . . . . . H132 H -0.2000 0.4896 0.3061 0.0320 1.0000 Uiso R . . . . . . H133 H -0.0799 0.5295 0.4123 0.0320 1.0000 Uiso R . . . . . . H141 H 0.2238 0.2650 -0.2663 0.0333 1.0000 Uiso R . . . . . . H142 H 0.1205 0.3275 -0.2944 0.0333 1.0000 Uiso R . . . . . . H143 H 0.0866 0.1980 -0.3185 0.0333 1.0000 Uiso R . . . . . . H151 H 0.1033 0.2120 0.4689 0.0198 1.0000 Uiso R . . . . . . H161 H 0.2555 0.3668 0.4946 0.0261 1.0000 Uiso R . . . . . . H162 H 0.2940 0.3218 0.5958 0.0261 1.0000 Uiso R . . . . . . H163 H 0.3503 0.2950 0.5129 0.0261 1.0000 Uiso R . . . . . . H171 H 0.1382 0.0344 0.4559 0.0327 1.0000 Uiso R . . . . . . H172 H 0.2204 0.1129 0.5715 0.0327 1.0000 Uiso R . . . . . . H173 H 0.2767 0.0861 0.4886 0.0327 1.0000 Uiso R . . . . . . H181 H 0.0494 -0.0142 0.2647 0.0193 1.0000 Uiso R . . . . . . H191 H 0.0383 0.0222 0.1033 0.0221 1.0000 Uiso R . . . . . . H192 H -0.0706 0.0749 0.0969 0.0221 1.0000 Uiso R . . . . . . H193 H -0.0865 -0.0521 0.0862 0.0221 1.0000 Uiso R . . . . . . H201 H -0.0667 0.0558 0.3514 0.0288 1.0000 Uiso R . . . . . . H202 H -0.1364 0.0959 0.2518 0.0288 1.0000 Uiso R . . . . . . H203 H -0.1523 -0.0311 0.2411 0.0288 1.0000 Uiso R . . . . . . H211 H 0.4885 0.2517 0.0351 0.0190 1.0000 Uiso R . . . . . . H221 H 0.6462 0.2733 0.2037 0.0250 1.0000 Uiso R . . . . . . H222 H 0.6458 0.1751 0.1163 0.0250 1.0000 Uiso R . . . . . . H223 H 0.5918 0.1506 0.1975 0.0250 1.0000 Uiso R . . . . . . H231 H 0.3216 0.0949 -0.0476 0.0217 1.0000 Uiso R . . . . . . H232 H 0.4425 0.0634 -0.0411 0.0217 1.0000 Uiso R . . . . . . H233 H 0.3885 0.0389 0.0401 0.0217 1.0000 Uiso R . . . . . . H241 H 0.5542 0.4059 0.2764 0.0200 1.0000 Uiso R . . . . . . H251 H 0.5638 0.4337 0.1178 0.0303 1.0000 Uiso R . . . . . . H252 H 0.5773 0.5464 0.1960 0.0303 1.0000 Uiso R . . . . . . H253 H 0.4526 0.4864 0.0972 0.0303 1.0000 Uiso R . . . . . . H261 H 0.3907 0.4369 0.3188 0.0260 1.0000 Uiso R . . . . . . H262 H 0.4694 0.5484 0.3212 0.0260 1.0000 Uiso R . . . . . . H263 H 0.3447 0.4884 0.2224 0.0260 1.0000 Uiso R . . . . . . H271 H 0.5694 0.2227 0.3426 0.0175 1.0000 Uiso R . . . . . . H281 H 0.5638 0.2714 0.5461 0.0212 1.0000 Uiso R . . . . . . H282 H 0.5194 0.3380 0.4619 0.0212 1.0000 Uiso R . . . . . . H291 H 0.7151 0.4338 0.5992 0.0246 1.0000 Uiso R . . . . . . H292 H 0.7185 0.4077 0.4863 0.0246 1.0000 Uiso R . . . . . . H301 H 0.8845 0.3624 0.6041 0.0288 1.0000 Uiso R . . . . . . H302 H 0.7988 0.2872 0.6378 0.0288 1.0000 Uiso R . . . . . . H311 H 0.8487 0.1727 0.5183 0.0270 1.0000 Uiso R . . . . . . H312 H 0.8036 0.2390 0.4340 0.0270 1.0000 Uiso R . . . . . . H321 H 0.6496 0.1029 0.4947 0.0208 1.0000 Uiso R . . . . . . H322 H 0.6529 0.0757 0.3818 0.0208 1.0000 Uiso R . . . . . . H331 H 0.4612 0.0029 0.2217 0.0187 1.0000 Uiso R . . . . . . H341 H 0.5158 -0.0802 0.3638 0.0248 1.0000 Uiso R . . . . . . H342 H 0.3776 -0.1346 0.3302 0.0248 1.0000 Uiso R . . . . . . H351 H 0.4632 -0.2676 0.2660 0.0329 1.0000 Uiso R . . . . . . H352 H 0.5065 -0.1905 0.2054 0.0329 1.0000 Uiso R . . . . . . H361 H 0.3297 -0.3222 0.0796 0.0330 1.0000 Uiso R . . . . . . H362 H 0.2597 -0.2933 0.1507 0.0330 1.0000 Uiso R . . . . . . H371 H 0.3390 -0.1507 0.0449 0.0250 1.0000 Uiso R . . . . . . H372 H 0.2021 -0.2063 0.0149 0.0250 1.0000 Uiso R . . . . . . H381 H 0.2155 -0.0947 0.1748 0.0210 1.0000 Uiso R . . . . . . H382 H 0.2549 -0.0181 0.1118 0.0210 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 C1 0.0135(7) 0.0129(7) 0.0162(8) 0.0050(6) 0.0082(6) 0.0045(6) C2 0.0169(8) 0.0154(8) 0.0189(8) 0.0067(6) 0.0106(7) 0.0058(6) C3 0.0169(8) 0.0135(8) 0.0230(9) 0.0037(7) 0.0116(7) 0.0057(6) C4 0.0190(8) 0.0148(8) 0.0190(8) 0.0054(6) 0.0082(7) 0.0081(6) C5 0.0184(8) 0.0161(8) 0.0166(8) 0.0069(6) 0.0087(7) 0.0077(6) C6 0.0125(7) 0.0127(7) 0.0132(7) 0.0024(6) 0.0060(6) 0.0033(6) C7 0.0137(7) 0.0133(7) 0.0139(7) 0.0044(6) 0.0061(6) 0.0046(6) C8 0.0142(8) 0.0210(8) 0.0141(8) 0.0066(6) 0.0051(6) 0.0069(6) C9 0.0189(8) 0.0224(9) 0.0150(8) 0.0069(7) 0.0052(7) 0.0066(7) C10 0.0241(9) 0.0168(8) 0.0138(8) 0.0065(6) 0.0093(7) 0.0071(7) C11 0.0180(8) 0.0168(8) 0.0172(8) 0.0069(6) 0.0098(7) 0.0067(6) C12 0.0135(7) 0.0146(7) 0.0134(7) 0.0038(6) 0.0068(6) 0.0050(6) C13 0.0270(10) 0.0204(9) 0.0329(11) 0.0099(8) 0.0213(9) 0.0123(8) C14 0.0342(11) 0.0327(11) 0.0163(9) 0.0109(8) 0.0135(8) 0.0143(9) C15 0.0168(8) 0.0205(8) 0.0124(7) 0.0057(6) 0.0076(6) 0.0078(7) C16 0.0215(9) 0.0295(10) 0.0144(8) 0.0002(7) 0.0076(7) 0.0021(8) C17 0.0316(11) 0.0317(11) 0.0186(9) 0.0144(8) 0.0141(8) 0.0173(9) C18 0.0171(8) 0.0137(8) 0.0174(8) 0.0026(6) 0.0075(7) 0.0035(6) C19 0.0203(9) 0.0183(8) 0.0169(8) -0.0005(7) 0.0051(7) 0.0016(7) C20 0.0214(9) 0.0214(9) 0.0292(10) 0.0041(8) 0.0144(8) -0.0001(7) C21 0.0151(8) 0.0181(8) 0.0143(7) 0.0038(6) 0.0081(6) 0.0058(6) C22 0.0163(8) 0.0282(10) 0.0180(8) 0.0048(7) 0.0090(7) 0.0084(7) C23 0.0189(8) 0.0166(8) 0.0190(8) 0.0024(7) 0.0085(7) 0.0070(7) C24 0.0168(8) 0.0161(8) 0.0173(8) 0.0022(6) 0.0067(7) 0.0026(6) C25 0.0286(10) 0.0200(9) 0.0273(10) 0.0039(8) 0.0138(9) -0.0022(8) C26 0.0248(10) 0.0162(8) 0.0243(10) -0.0021(7) 0.0111(8) 0.0038(7) C27 0.0137(7) 0.0170(8) 0.0130(7) 0.0055(6) 0.0052(6) 0.0060(6) C28 0.0178(8) 0.0177(8) 0.0175(8) 0.0023(7) 0.0085(7) 0.0043(7) C29 0.0201(9) 0.0188(9) 0.0228(9) -0.0003(7) 0.0101(7) 0.0018(7) C30 0.0175(9) 0.0275(10) 0.0271(10) 0.0022(8) 0.0021(8) 0.0018(8) C31 0.0154(8) 0.0223(9) 0.0302(10) 0.0050(8) 0.0061(8) 0.0060(7) C32 0.0142(8) 0.0178(8) 0.0201(8) 0.0063(7) 0.0051(7) 0.0064(6) C33 0.0158(8) 0.0143(7) 0.0166(8) 0.0052(6) 0.0071(6) 0.0052(6) C34 0.0242(9) 0.0160(8) 0.0216(9) 0.0073(7) 0.0072(7) 0.0083(7) C35 0.0321(11) 0.0175(9) 0.0327(11) 0.0074(8) 0.0126(9) 0.0110(8) C36 0.0342(12) 0.0182(9) 0.0302(11) 0.0023(8) 0.0141(9) 0.0060(8) C37 0.0231(9) 0.0200(9) 0.0194(9) 0.0004(7) 0.0094(7) 0.0016(7) C38 0.0164(8) 0.0183(8) 0.0177(8) 0.0037(7) 0.0063(7) 0.0039(7) Pd1 0.01084(6) 0.01246(6) 0.01051(6) 0.00357(4) 0.00462(4) 0.00461(4) P1 0.01288(19) 0.01244(19) 0.01110(18) 0.00386(15) 0.00556(15) 0.00450(15) N1 0.0128(6) 0.0171(7) 0.0138(7) 0.0062(5) 0.0068(5) 0.0072(5) P2 0.01175(18) 0.01280(19) 0.01241(19) 0.00307(15) 0.00588(15) 0.00406(15) P3 0.01363(19) 0.0159(2) 0.01283(19) 0.00515(16) 0.00515(16) 0.00593(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5013(4) 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 C1 . C2 . 1.399(2) yes C1 . C6 . 1.415(2) yes C1 . P1 . 1.8142(18) yes C2 . C3 . 1.388(3) yes C2 . H21 . 0.950 no C3 . C4 . 1.399(3) yes C3 . C13 . 1.506(3) yes C4 . C5 . 1.385(3) yes C4 . H41 . 0.950 no C5 . C6 . 1.415(2) yes C5 . H51 . 0.950 no C6 . N1 . 1.384(2) yes C7 . C8 . 1.412(2) yes C7 . C12 . 1.418(2) yes C7 . N1 . 1.379(2) yes C8 . C9 . 1.380(3) yes C8 . H81 . 0.950 no C9 . C10 . 1.397(3) yes C9 . H91 . 0.950 no C10 . C11 . 1.393(3) yes C10 . C14 . 1.506(3) yes C11 . C12 . 1.398(2) yes C11 . H111 . 0.950 no C12 . P2 . 1.8230(18) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . C16 . 1.527(3) yes C15 . C17 . 1.530(3) yes C15 . P1 . 1.8462(18) yes C15 . H151 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . C19 . 1.528(3) yes C18 . C20 . 1.535(3) yes C18 . P1 . 1.8458(19) yes C18 . H181 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . C22 . 1.533(3) yes C21 . C23 . 1.527(3) yes C21 . P2 . 1.8536(18) yes C21 . H211 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . C25 . 1.532(3) yes C24 . C26 . 1.534(3) yes C24 . P2 . 1.8552(19) yes C24 . H241 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . C28 . 1.533(3) yes C27 . C32 . 1.537(2) yes C27 . P3 . 1.8798(19) yes C27 . H271 . 0.950 no C28 . C29 . 1.526(3) yes C28 . H281 . 0.950 no C28 . H282 . 0.950 no C29 . C30 . 1.528(3) yes C29 . H291 . 0.950 no C29 . H292 . 0.950 no C30 . C31 . 1.522(3) yes C30 . H301 . 0.950 no C30 . H302 . 0.950 no C31 . C32 . 1.528(3) yes C31 . H311 . 0.950 no C31 . H312 . 0.950 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C33 . C34 . 1.542(3) yes C33 . C38 . 1.534(3) yes C33 . P3 . 1.8792(19) yes C33 . H331 . 0.950 no C34 . C35 . 1.525(3) yes C34 . H341 . 0.950 no C34 . H342 . 0.950 no C35 . C36 . 1.530(3) yes C35 . H351 . 0.950 no C35 . H352 . 0.950 no C36 . C37 . 1.525(3) yes C36 . H361 . 0.950 no C36 . H362 . 0.950 no C37 . C38 . 1.529(3) yes C37 . H371 . 0.950 no C37 . H372 . 0.950 no C38 . H381 . 0.950 no C38 . H382 . 0.950 no Pd1 . P1 . 2.2964(5) yes Pd1 . N1 . 2.1186(15) yes Pd1 . P2 . 2.3410(5) yes Pd1 . P3 . 2.3494(5) yes 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 C2 . C1 . C6 . 120.42(16) yes C2 . C1 . P1 . 124.12(14) yes C6 . C1 . P1 . 115.45(13) yes C1 . C2 . C3 . 122.40(17) yes C1 . C2 . H21 . 118.8 no C3 . C2 . H21 . 118.8 no C2 . C3 . C4 . 117.09(17) yes C2 . C3 . C13 . 121.18(17) yes C4 . C3 . C13 . 121.63(17) yes C3 . C4 . C5 . 121.93(17) yes C3 . C4 . H41 . 119.0 no C5 . C4 . H41 . 119.0 no C4 . C5 . C6 . 121.28(17) yes C4 . C5 . H51 . 119.4 no C6 . C5 . H51 . 119.4 no C5 . C6 . C1 . 116.88(16) yes C5 . C6 . N1 . 124.85(16) yes C1 . C6 . N1 . 118.16(16) yes C8 . C7 . C12 . 117.25(16) yes C8 . C7 . N1 . 124.74(16) yes C12 . C7 . N1 . 117.82(16) yes C7 . C8 . C9 . 121.17(17) yes C7 . C8 . H81 . 119.4 no C9 . C8 . H81 . 119.4 no C8 . C9 . C10 . 122.04(18) yes C8 . C9 . H91 . 119.0 no C10 . C9 . H91 . 119.0 no C9 . C10 . C11 . 117.16(17) yes C9 . C10 . C14 . 121.51(18) yes C11 . C10 . C14 . 121.27(18) yes C10 . C11 . C12 . 122.21(17) yes C10 . C11 . H111 . 118.9 no C12 . C11 . H111 . 118.9 no C7 . C12 . C11 . 120.10(16) yes C7 . C12 . P2 . 115.10(13) yes C11 . C12 . P2 . 124.57(13) yes C3 . C13 . H131 . 109.5 no C3 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C3 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no C10 . C14 . H141 . 109.5 no C10 . C14 . H142 . 109.5 no H141 . C14 . H142 . 109.5 no C10 . C14 . H143 . 109.5 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no C16 . C15 . C17 . 111.65(17) yes C16 . C15 . P1 . 109.03(13) yes C17 . C15 . P1 . 112.60(13) yes C16 . C15 . H151 . 107.8 no C17 . C15 . H151 . 107.8 no P1 . C15 . H151 . 107.8 no C15 . C16 . H161 . 109.5 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no C15 . C17 . H171 . 109.5 no C15 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no C15 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no C19 . C18 . C20 . 110.90(17) yes C19 . C18 . P1 . 109.43(13) yes C20 . C18 . P1 . 113.59(13) yes C19 . C18 . H181 . 107.6 no C20 . C18 . H181 . 107.6 no P1 . C18 . H181 . 107.6 no C18 . C19 . H191 . 109.5 no C18 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no C18 . C20 . H201 . 109.5 no C18 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C18 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C22 . C21 . C23 . 111.24(16) yes C22 . C21 . P2 . 114.33(13) yes C23 . C21 . P2 . 110.56(13) yes C22 . C21 . H211 . 106.7 no C23 . C21 . H211 . 106.7 no P2 . C21 . H211 . 106.8 no C21 . C22 . H221 . 109.4 no C21 . C22 . H222 . 109.5 no H221 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.4 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C21 . C23 . H231 . 109.5 no C21 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C21 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C25 . C24 . C26 . 110.56(17) yes C25 . C24 . P2 . 113.78(14) yes C26 . C24 . P2 . 110.00(13) yes C25 . C24 . H241 . 107.4 no C26 . C24 . H241 . 107.4 no P2 . C24 . H241 . 107.4 no C24 . C25 . H251 . 109.5 no C24 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C24 . C25 . H253 . 109.5 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no C24 . C26 . H261 . 109.5 no C24 . C26 . H262 . 109.5 no H261 . C26 . H262 . 109.5 no C24 . C26 . H263 . 109.5 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no C28 . C27 . C32 . 110.33(15) yes C28 . C27 . P3 . 108.82(12) yes C32 . C27 . P3 . 112.91(13) yes C28 . C27 . H271 . 108.2 no C32 . C27 . H271 . 108.2 no P3 . C27 . H271 . 108.2 no C27 . C28 . C29 . 112.22(16) yes C27 . C28 . H281 . 108.8 no C29 . C28 . H281 . 108.8 no C27 . C28 . H282 . 108.8 no C29 . C28 . H282 . 108.8 no H281 . C28 . H282 . 109.5 no C28 . C29 . C30 . 111.07(17) yes C28 . C29 . H291 . 109.1 no C30 . C29 . H291 . 109.1 no C28 . C29 . H292 . 109.1 no C30 . C29 . H292 . 109.1 no H291 . C29 . H292 . 109.5 no C29 . C30 . C31 . 111.28(18) yes C29 . C30 . H301 . 109.0 no C31 . C30 . H301 . 109.0 no C29 . C30 . H302 . 109.0 no C31 . C30 . H302 . 109.0 no H301 . C30 . H302 . 109.5 no C30 . C31 . C32 . 111.52(18) yes C30 . C31 . H311 . 108.9 no C32 . C31 . H311 . 108.9 no C30 . C31 . H312 . 109.0 no C32 . C31 . H312 . 109.0 no H311 . C31 . H312 . 109.5 no C27 . C32 . C31 . 111.47(16) yes C27 . C32 . H321 . 109.0 no C31 . C32 . H321 . 109.0 no C27 . C32 . H322 . 109.0 no C31 . C32 . H322 . 108.9 no H321 . C32 . H322 . 109.5 no C34 . C33 . C38 . 108.28(15) yes C34 . C33 . P3 . 109.93(13) yes C38 . C33 . P3 . 112.91(13) yes C34 . C33 . H331 . 108.6 no C38 . C33 . H331 . 108.5 no P3 . C33 . H331 . 108.5 no C33 . C34 . C35 . 112.09(17) yes C33 . C34 . H341 . 108.8 no C35 . C34 . H341 . 108.8 no C33 . C34 . H342 . 108.8 no C35 . C34 . H342 . 108.8 no H341 . C34 . H342 . 109.5 no C34 . C35 . C36 . 111.00(18) yes C34 . C35 . H351 . 109.1 no C36 . C35 . H351 . 109.1 no C34 . C35 . H352 . 109.1 no C36 . C35 . H352 . 109.1 no H351 . C35 . H352 . 109.5 no C35 . C36 . C37 . 110.11(18) yes C35 . C36 . H361 . 109.3 no C37 . C36 . H361 . 109.3 no C35 . C36 . H362 . 109.3 no C37 . C36 . H362 . 109.3 no H361 . C36 . H362 . 109.5 no C36 . C37 . C38 . 112.58(17) yes C36 . C37 . H371 . 108.7 no C38 . C37 . H371 . 108.7 no C36 . C37 . H372 . 108.7 no C38 . C37 . H372 . 108.7 no H371 . C37 . H372 . 109.5 no C33 . C38 . C37 . 110.82(16) yes C33 . C38 . H381 . 109.1 no C37 . C38 . H381 . 109.1 no C33 . C38 . H382 . 109.1 no C37 . C38 . H382 . 109.2 no H381 . C38 . H382 . 109.5 no P1 . Pd1 . N1 . 81.31(4) yes P1 . Pd1 . P2 . 160.661(17) yes N1 . Pd1 . P2 . 79.86(4) yes P1 . Pd1 . P3 . 93.087(17) yes N1 . Pd1 . P3 . 174.34(4) yes P2 . Pd1 . P3 . 105.789(18) yes C15 . P1 . C18 . 105.26(9) yes C15 . P1 . C1 . 104.81(8) yes C18 . P1 . C1 . 105.66(8) yes C15 . P1 . Pd1 . 124.44(6) yes C18 . P1 . Pd1 . 114.65(6) yes C1 . P1 . Pd1 . 99.95(6) yes C6 . N1 . C7 . 123.00(15) yes C6 . N1 . Pd1 . 118.73(12) yes C7 . N1 . Pd1 . 118.20(11) yes C24 . P2 . C21 . 103.61(9) yes C24 . P2 . C12 . 105.72(9) yes C21 . P2 . C12 . 102.55(8) yes C24 . P2 . Pd1 . 110.31(6) yes C21 . P2 . Pd1 . 132.74(6) yes C12 . P2 . Pd1 . 98.90(6) yes C27 . P3 . C33 . 102.80(8) yes C27 . P3 . Pd1 . 103.71(6) yes C33 . P3 . Pd1 . 105.38(6) yes #===END data_7b-Barf _database_code_depnum_ccdc_archive 'CCDC 756644' #TrackingRef 'MS-0027-combcifs.cif' _audit_creation_date 07-10-01 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'OZ116_0m in C2/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 38.6776(13) _cell_length_b 13.0413(4) _cell_length_c 26.3169(8) _cell_angle_alpha 90 _cell_angle_beta 99.898(2) _cell_angle_gamma 90 _cell_volume 13076.8(7) _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' 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 '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' 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 8 # Given Formula = C62.75 H57.75 B1 F24 N3 P2 Pd1 # Dc = 1.51 Fooo = 6018.00 Mu = 4.43 M = 1489.03 # Found Formula = C62.75 H57.75 B1 F24 N3 P2 Pd1 # Dc = 1.51 FOOO = 6018.00 Mu = 4.43 M = 1489.03 _chemical_formula_sum 'C62.75 H57.75 B1 F24 N3 P2 Pd1' _chemical_formula_moiety 'C62.75 H57.75 B1 F24 N3 P2 Pd1' _chemical_compound_source ? _chemical_formula_weight 1489.03 _cell_measurement_reflns_used 7438 _cell_measurement_theta_min 2 _cell_measurement_theta_max 22 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 6018 _exptl_absorpt_coefficient_mu 0.443 # Sheldrick geometric approximatio 0.90 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Apex2, (Bruker AXS, 2006)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device 'Bruker-Nonius Kappa ApexII CCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2, (Bruker AXS, 2006)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _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 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 120 _diffrn_reflns_number 74698 _reflns_number_total 12773 _diffrn_reflns_av_R_equivalents 0.127 # Number of reflections with Friedels Law is 12773 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12923 _diffrn_reflns_theta_min 1.069 _diffrn_reflns_theta_max 26.051 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.009 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -47 _reflns_limit_h_max 46 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 1.44 _oxford_diffrn_Wilson_scale 208.87 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.90 _refine_diff_density_max 2.21 # 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 12773 _refine_ls_number_restraints 7 _refine_ls_number_parameters 844 _oxford_refine_ls_R_factor_ref 0.1004 _refine_ls_wR_factor_ref 0.1815 _refine_ls_goodness_of_fit_ref 0.9732 _refine_ls_shift/su_max 0.013717 # The values computed from all data _oxford_reflns_number_all 12773 _refine_ls_R_factor_all 0.1004 _refine_ls_wR_factor_all 0.1815 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8991 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_gt 0.1619 # 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^) + ( 0.07P)^2^ +*****P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Bruker Analytical X-ray Systems, Inc., 2006. Apex2, Version 2 User Manual, M86-E01078, Madison, WI. 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 0.615272(10) 0.46472(3) 0.479313(14) 0.0182 1.0000 Uani . . . . . . . P1 P 0.65635(4) 0.39292(10) 0.54276(5) 0.0193 1.0000 Uani . . . . . . . P2 P 0.57469(4) 0.56820(11) 0.42975(5) 0.0197 1.0000 Uani . . . . . . . N1 N 0.61533(11) 0.5769(3) 0.53160(16) 0.0211 1.0000 Uani . . . . . . . N2 N 0.61531(12) 0.3478(4) 0.42715(17) 0.0303 1.0000 Uani . . . . . . . C1 C 0.64000(15) 0.2907(4) 0.5800(2) 0.0254 1.0000 Uani . . . . . . . C2 C 0.60346(17) 0.3180(5) 0.5899(3) 0.0404 1.0000 Uani . . . . . . . C3 C 0.66482(18) 0.2631(5) 0.6292(2) 0.0356 1.0000 Uani . . . . . . . C4 C 0.69776(14) 0.3488(5) 0.5256(2) 0.0269 1.0000 Uani . . . . . . . C5 C 0.71089(17) 0.4296(5) 0.4912(2) 0.0403 1.0000 Uani . . . . . . . C6 C 0.69476(17) 0.2434(5) 0.4999(2) 0.0393 1.0000 Uani . . . . . . . C7 C 0.66695(14) 0.5034(4) 0.58351(19) 0.0219 1.0000 Uani . . . . . . . C8 C 0.69672(14) 0.5107(4) 0.6219(2) 0.0245 1.0000 Uani . . . . . . . C9 C 0.70534(15) 0.6004(5) 0.6487(2) 0.0290 1.0000 Uani . . . . . . . C10 C 0.68322(16) 0.6844(4) 0.6364(2) 0.0307 1.0000 Uani . . . . . . . C11 C 0.65375(15) 0.6796(4) 0.5984(2) 0.0266 1.0000 Uani . . . . . . . C12 C 0.64411(13) 0.5872(4) 0.57119(19) 0.0194 1.0000 Uani . . . . . . . C13 C 0.73774(17) 0.6077(5) 0.6901(2) 0.0421 1.0000 Uani . . . . . . . C14 C 0.58590(13) 0.6414(4) 0.52765(19) 0.0195 1.0000 Uani . . . . . . . C15 C 0.57545(14) 0.6921(4) 0.5695(2) 0.0234 1.0000 Uani . . . . . . . C16 C 0.54592(15) 0.7534(4) 0.5623(2) 0.0268 1.0000 Uani . . . . . . . C17 C 0.52521(15) 0.7684(4) 0.5142(2) 0.0281 1.0000 Uani . . . . . . . C18 C 0.53430(14) 0.7140(4) 0.4731(2) 0.0261 1.0000 Uani . . . . . . . C19 C 0.56392(13) 0.6514(4) 0.47950(19) 0.0206 1.0000 Uani . . . . . . . C20 C 0.49307(17) 0.8357(5) 0.5071(3) 0.0405 1.0000 Uani . . . . . . . C21 C 0.53315(15) 0.5129(5) 0.3983(2) 0.0314 1.0000 Uani . . . . . . . C22 C 0.51825(18) 0.4454(5) 0.4364(3) 0.0486 1.0000 Uani . . . . . . . C23 C 0.53653(17) 0.4547(6) 0.3495(3) 0.0439 1.0000 Uani . . . . . . . C24 C 0.59249(16) 0.6440(5) 0.3815(2) 0.0310 1.0000 Uani . . . . . . . C25 C 0.62806(18) 0.6880(6) 0.4069(3) 0.0457 1.0000 Uani . . . . . . . C26 C 0.5677(2) 0.7284(5) 0.3564(3) 0.0458 1.0000 Uani . . . . . . . C27 C 0.62905(17) 0.3455(5) 0.3849(2) 0.0442 1.0000 Uani D U . . . . . C29 C 0.60268(17) 0.2515(5) 0.4323(3) 0.0451 1.0000 Uani D . . . . . . C30 C 0.90609(14) 0.5429(4) 0.24563(19) 0.0233 1.0000 Uani . . . . . . . C31 C 0.92922(15) 0.5118(5) 0.2133(2) 0.0275 1.0000 Uani . . . . . . . C32 C 0.95469(15) 0.5773(5) 0.1995(2) 0.0302 1.0000 Uani . . . . . . . C33 C 0.95731(16) 0.6768(5) 0.2174(2) 0.0317 1.0000 Uani . . . . . . . C34 C 0.93520(16) 0.7088(4) 0.2500(2) 0.0301 1.0000 Uani . . . . . . . C35 C 0.91020(14) 0.6433(4) 0.2638(2) 0.0259 1.0000 Uani . . . . . . . C36 C 0.93741(17) 0.8161(5) 0.2700(3) 0.0372 1.0000 Uani . . . . . . . C37 C 0.97808(18) 0.5383(6) 0.1643(3) 0.0430 1.0000 Uani . . . . . . . C38 C 0.84234(13) 0.5109(4) 0.20488(19) 0.0201 1.0000 Uani . . . . . . . C39 C 0.83936(14) 0.4642(4) 0.1565(2) 0.0265 1.0000 Uani . . . . . . . C40 C 0.81720(16) 0.5017(5) 0.1133(2) 0.0290 1.0000 Uani . . . . . . . C41 C 0.79667(15) 0.5875(5) 0.1164(2) 0.0291 1.0000 Uani . . . . . . . C42 C 0.79970(14) 0.6359(4) 0.1638(2) 0.0242 1.0000 Uani . . . . . . . C43 C 0.82227(14) 0.5988(4) 0.2068(2) 0.0235 1.0000 Uani . . . . . . . C44 C 0.8161(2) 0.4497(7) 0.0629(3) 0.0568 1.0000 Uani . . . . . . . C45 C 0.77943(16) 0.7317(5) 0.1687(2) 0.0333 1.0000 Uani . . . . . . . C46 C 0.87979(13) 0.3511(4) 0.25370(18) 0.0199 1.0000 Uani . . . . . . . C47 C 0.85333(15) 0.2785(4) 0.2368(2) 0.0244 1.0000 Uani . . . . . . . C48 C 0.85933(16) 0.1741(4) 0.2404(2) 0.0290 1.0000 Uani . . . . . . . C49 C 0.89173(16) 0.1351(4) 0.2626(2) 0.0299 1.0000 Uani . . . . . . . C50 C 0.91812(15) 0.2047(4) 0.2808(2) 0.0271 1.0000 Uani . . . . . . . C51 C 0.91210(15) 0.3097(4) 0.2764(2) 0.0252 1.0000 Uani . . . . . . . C52 C 0.83073(18) 0.1014(5) 0.2219(3) 0.0392 1.0000 Uani . . . . . . . C53 C 0.95292(19) 0.1654(6) 0.3046(3) 0.0453 1.0000 Uani . . . . . . . C54 C 0.85979(14) 0.4956(4) 0.30952(19) 0.0207 1.0000 Uani . . . . . . . C55 C 0.82490(14) 0.4985(4) 0.3162(2) 0.0224 1.0000 Uani . . . . . . . C56 C 0.81515(15) 0.5082(4) 0.3643(2) 0.0256 1.0000 Uani . . . . . . . C57 C 0.84072(15) 0.5136(4) 0.4083(2) 0.0252 1.0000 Uani . . . . . . . C58 C 0.87562(15) 0.5102(4) 0.4032(2) 0.0229 1.0000 Uani . . . . . . . C59 C 0.88519(15) 0.5015(4) 0.3550(2) 0.0217 1.0000 Uani . . . . . . . C60 C 0.77743(16) 0.5136(5) 0.3682(2) 0.0344 1.0000 Uani . . . . . . . C61 C 0.90246(17) 0.5100(4) 0.4515(2) 0.0306 1.0000 Uani . . . . . . . B1 B 0.87176(16) 0.4738(5) 0.2540(2) 0.0221 1.0000 Uani . . . . . . . H11 H 0.6376 0.2310 0.5590 0.0306 1.0000 Uiso R . . . . . . H23 H 0.5882 0.3267 0.5578 0.0532 1.0000 Uiso R . . . . . . H22 H 0.5947 0.2653 0.6091 0.0532 1.0000 Uiso R . . . . . . H21 H 0.6048 0.3804 0.6088 0.0532 1.0000 Uiso R . . . . . . H33 H 0.6868 0.2418 0.6213 0.0420 1.0000 Uiso R . . . . . . H32 H 0.6681 0.3219 0.6508 0.0420 1.0000 Uiso R . . . . . . H31 H 0.6551 0.2093 0.6466 0.0420 1.0000 Uiso R . . . . . . H41 H 0.7144 0.3438 0.5566 0.0319 1.0000 Uiso R . . . . . . H53 H 0.6940 0.4390 0.4608 0.0496 1.0000 Uiso R . . . . . . H52 H 0.7324 0.4078 0.4821 0.0496 1.0000 Uiso R . . . . . . H51 H 0.7144 0.4926 0.5095 0.0496 1.0000 Uiso R . . . . . . H63 H 0.6779 0.2460 0.4691 0.0462 1.0000 Uiso R . . . . . . H62 H 0.6876 0.1946 0.5228 0.0462 1.0000 Uiso R . . . . . . H61 H 0.7169 0.2239 0.4919 0.0462 1.0000 Uiso R . . . . . . H81 H 0.7115 0.4527 0.6295 0.0281 1.0000 Uiso R . . . . . . H101 H 0.6888 0.7470 0.6544 0.0377 1.0000 Uiso R . . . . . . H111 H 0.6397 0.7390 0.5903 0.0317 1.0000 Uiso R . . . . . . H131 H 0.7530 0.6584 0.6806 0.0472 1.0000 Uiso R . . . . . . H133 H 0.7311 0.6261 0.7221 0.0472 1.0000 Uiso R . . . . . . H132 H 0.7494 0.5433 0.6936 0.0472 1.0000 Uiso R . . . . . . H151 H 0.5889 0.6841 0.6031 0.0291 1.0000 Uiso R . . . . . . H161 H 0.5394 0.7872 0.5913 0.0325 1.0000 Uiso R . . . . . . H181 H 0.5201 0.7200 0.4400 0.0311 1.0000 Uiso R . . . . . . H202 H 0.4729 0.7955 0.4949 0.0495 1.0000 Uiso R . . . . . . H201 H 0.4907 0.8667 0.5389 0.0495 1.0000 Uiso R . . . . . . H203 H 0.4955 0.8875 0.4825 0.0495 1.0000 Uiso R . . . . . . H211 H 0.5171 0.5675 0.3889 0.0367 1.0000 Uiso R . . . . . . H221 H 0.5345 0.3919 0.4474 0.0570 1.0000 Uiso R . . . . . . H222 H 0.5146 0.4849 0.4653 0.0570 1.0000 Uiso R . . . . . . H223 H 0.4966 0.4167 0.4201 0.0570 1.0000 Uiso R . . . . . . H233 H 0.5529 0.4004 0.3579 0.0492 1.0000 Uiso R . . . . . . H232 H 0.5144 0.4274 0.3343 0.0492 1.0000 Uiso R . . . . . . H231 H 0.5447 0.4999 0.3258 0.0492 1.0000 Uiso R . . . . . . H241 H 0.5966 0.5987 0.3549 0.0359 1.0000 Uiso R . . . . . . H252 H 0.6435 0.6333 0.4191 0.0537 1.0000 Uiso R . . . . . . H251 H 0.6247 0.7303 0.4351 0.0537 1.0000 Uiso R . . . . . . H253 H 0.6379 0.7275 0.3826 0.0537 1.0000 Uiso R . . . . . . H263 H 0.5463 0.6983 0.3398 0.0572 1.0000 Uiso R . . . . . . H262 H 0.5782 0.7647 0.3317 0.0572 1.0000 Uiso R . . . . . . H261 H 0.5630 0.7745 0.3823 0.0572 1.0000 Uiso R . . . . . . H331 H 0.9740 0.7225 0.2073 0.0385 1.0000 Uiso R . . . . . . H351 H 0.8954 0.6674 0.2865 0.0314 1.0000 Uiso R . . . . . . H391 H 0.8533 0.4056 0.1529 0.0315 1.0000 Uiso R . . . . . . H411 H 0.7812 0.6125 0.0871 0.0346 1.0000 Uiso R . . . . . . H431 H 0.8242 0.6354 0.2383 0.0293 1.0000 Uiso R . . . . . . H471 H 0.8304 0.3021 0.2229 0.0292 1.0000 Uiso R . . . . . . H491 H 0.8958 0.0633 0.2654 0.0364 1.0000 Uiso R . . . . . . H511 H 0.9307 0.3550 0.2896 0.0302 1.0000 Uiso R . . . . . . H551 H 0.8069 0.4941 0.2868 0.0295 1.0000 Uiso R . . . . . . H571 H 0.8343 0.5206 0.4413 0.0320 1.0000 Uiso R . . . . . . H591 H 0.9094 0.4995 0.3528 0.0277 1.0000 Uiso R . . . . . . H291 H 0.5912 0.2294 0.4595 0.0526 1.0000 Uiso R . . . . . . H271 H 0.6401 0.4023 0.3718 0.0609 1.0000 Uiso R . . . . . . F1 F 0.96462(16) 0.8677(4) 0.25919(18) 0.0818 1.0000 Uani . . . . . . . F2 F 0.9400(2) 0.8227(4) 0.31814(19) 0.1343 1.0000 Uani . . . . . . . F3 F 0.91152(16) 0.8718(4) 0.2464(3) 0.1241 1.0000 Uani . . . . . . . F4 F 0.96010(13) 0.5129(5) 0.11853(17) 0.0782 1.0000 Uani . . . . . . . F5 F 0.99521(15) 0.4551(5) 0.1817(2) 0.0902 1.0000 Uani . . . . . . . F6 F 1.00164(13) 0.6063(4) 0.15503(19) 0.0817 1.0000 Uani . . . . . . . F7 F 0.75507(12) 0.7196(3) 0.19855(19) 0.0662 1.0000 Uani . . . . . . . F8 F 0.76215(12) 0.7658(3) 0.12373(16) 0.0618 1.0000 Uani . . . . . . . F9 F 0.79979(11) 0.8076(3) 0.18960(19) 0.0666 1.0000 Uani . . . . . . . F10 F 0.79261(13) 0.4844(4) 0.02523(14) 0.0645 1.0000 Uani . . . . . . . F11 F 0.8064(2) 0.3480(5) 0.06583(19) 0.1221 1.0000 Uani . . . . . . . F12 F 0.84490(16) 0.4393(8) 0.0486(2) 0.1628 1.0000 Uani . . . . . . . F13 F 0.8045(2) 0.1375(5) 0.1977(7) 0.2714 1.0000 Uani . . . . . . . F14 F 0.8367(2) 0.0401(8) 0.1892(4) 0.2024 1.0000 Uani . . . . . . . F15 F 0.8198(3) 0.0508(10) 0.2524(3) 0.2445 1.0000 Uani . . . . . . . F16 F 0.96875(13) 0.2194(4) 0.3427(2) 0.0962 1.0000 Uani . . . . . . . F17 F 0.97244(16) 0.1421(10) 0.2748(2) 0.2007 1.0000 Uani . . . . . . . F18 F 0.95044(15) 0.0751(4) 0.3300(3) 0.1068 1.0000 Uani . . . . . . . F19 F 0.77030(11) 0.4727(4) 0.41069(15) 0.0672 1.0000 Uani . . . . . . . F20 F 0.76520(12) 0.6077(4) 0.3654(3) 0.1172 1.0000 Uani . . . . . . . F21 F 0.75664(10) 0.4651(4) 0.33051(15) 0.0615 1.0000 Uani . . . . . . . F22 F 0.89926(9) 0.5908(3) 0.48179(12) 0.0376 1.0000 Uani . . . . . . . F23 F 0.89973(11) 0.4266(3) 0.48058(14) 0.0515 1.0000 Uani . . . . . . . F24 F 0.93536(9) 0.5106(3) 0.44242(13) 0.0371 1.0000 Uani . . . . . . . C62 C 0.7726(7) 0.198(2) 0.0408(10) 0.107(8) 0.5000 Uiso . . . . . . . C63 C 0.7805(7) 0.2021(19) -0.0086(9) 0.101(7) 0.5000 Uiso . . . . . . . C64 C 0.7416(6) 0.2465(18) 0.0489(9) 0.095(7) 0.5000 Uiso . . . . . . . C65 C 0.7893(7) 0.142(2) 0.0680(10) 0.044(7) 0.2500 Uiso . . . . . . . N301 N 0.6068(3) 0.1805(9) 0.3995(5) 0.037(4) 0.52(3) Uiso D . P 1 1 . . C28 C 0.6121(4) 0.2095(17) 0.3869(5) 0.040(4) 0.48(3) Uiso D . P 1 2 . . C281 C 0.6231(3) 0.2412(7) 0.3691(5) 0.016(3) 0.52(3) Uiso D U P 1 1 . . N30 N 0.6291(4) 0.2666(12) 0.3567(6) 0.043(4) 0.48(3) Uiso D . P 1 2 . . H311 H 0.9276 0.4439 0.2001 0.0323 1.0000 Uiso R . . . . . . H3011 H 0.6006 0.1162 0.3974 0.0376 0.52(3) Uiso R . P 1 1 . . H2811 H 0.6305 0.2143 0.3392 0.0189 0.52(3) Uiso R . P 1 1 . . H281 H 0.6079 0.1417 0.3741 0.0333 0.48(3) Uiso R . P 1 2 . . H301 H 0.6376 0.2616 0.3283 0.0517 0.48(3) Uiso R . P 1 2 . . H641 H 0.7354 0.2435 0.0823 0.1134 0.5000 Uiso R . . . . . . H631 H 0.8011 0.1691 -0.0155 0.1209 0.5000 Uiso R . . . . . . H651 H 0.8090 0.1202 0.0536 0.0533 0.2500 Uiso R . . . . . . H652 H 0.7971 0.1743 0.1002 0.0533 0.2500 Uiso R . . . . . . H653 H 0.7753 0.0838 0.0729 0.0533 0.2500 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 Pd1 0.0204(2) 0.0165(2) 0.01705(19) -0.00039(16) 0.00165(14) 0.00153(17) P1 0.0215(7) 0.0174(7) 0.0187(7) 0.0007(5) 0.0025(5) 0.0009(5) P2 0.0219(7) 0.0182(7) 0.0182(6) 0.0009(5) 0.0010(5) 0.0004(5) N1 0.024(2) 0.017(2) 0.021(2) -0.0004(17) 0.0018(18) 0.0004(19) N2 0.029(3) 0.035(3) 0.024(2) -0.010(2) -0.004(2) 0.012(2) C1 0.034(3) 0.016(3) 0.027(3) 0.000(2) 0.007(2) -0.007(2) C2 0.043(4) 0.038(4) 0.042(4) 0.010(3) 0.014(3) -0.006(3) C3 0.053(4) 0.026(3) 0.027(3) 0.012(2) 0.003(3) -0.003(3) C4 0.022(3) 0.034(3) 0.022(3) -0.003(2) -0.002(2) 0.003(2) C5 0.030(3) 0.053(4) 0.041(4) 0.003(3) 0.012(3) -0.004(3) C6 0.033(3) 0.042(4) 0.041(4) -0.013(3) -0.001(3) 0.014(3) C7 0.025(3) 0.022(3) 0.019(3) -0.001(2) 0.005(2) -0.003(2) C8 0.024(3) 0.023(3) 0.026(3) 0.002(2) 0.003(2) 0.005(2) C9 0.032(3) 0.030(3) 0.023(3) -0.005(2) 0.001(2) -0.006(3) C10 0.042(4) 0.021(3) 0.028(3) -0.007(2) 0.002(3) -0.006(3) C11 0.034(3) 0.017(3) 0.028(3) -0.003(2) 0.002(2) -0.004(2) C12 0.023(3) 0.018(3) 0.017(2) 0.001(2) 0.002(2) -0.003(2) C13 0.042(4) 0.041(4) 0.037(4) -0.012(3) -0.011(3) -0.004(3) C14 0.021(3) 0.012(3) 0.025(3) 0.000(2) 0.004(2) -0.002(2) C15 0.024(3) 0.022(3) 0.024(3) -0.002(2) 0.004(2) 0.000(2) C16 0.034(3) 0.019(3) 0.030(3) -0.004(2) 0.009(2) -0.003(2) C17 0.030(3) 0.021(3) 0.035(3) -0.002(2) 0.007(2) 0.004(2) C18 0.026(3) 0.019(3) 0.030(3) 0.002(2) -0.003(2) 0.000(2) C19 0.021(3) 0.021(3) 0.020(3) 0.001(2) 0.004(2) 0.000(2) C20 0.036(4) 0.032(4) 0.052(4) -0.008(3) 0.006(3) 0.005(3) C21 0.025(3) 0.030(3) 0.036(3) -0.008(3) -0.003(2) 0.004(2) C22 0.040(4) 0.042(4) 0.067(5) -0.014(3) 0.018(3) -0.018(3) C23 0.032(3) 0.049(4) 0.045(4) -0.015(3) -0.009(3) 0.003(3) C24 0.043(4) 0.025(3) 0.026(3) 0.003(2) 0.011(3) 0.001(3) C25 0.047(4) 0.046(4) 0.047(4) 0.006(3) 0.017(3) -0.016(3) C26 0.067(5) 0.032(4) 0.043(4) 0.021(3) 0.023(3) 0.014(3) C27 0.043(4) 0.053(4) 0.032(3) -0.019(3) -0.006(3) 0.020(3) C29 0.040(4) 0.027(4) 0.061(4) -0.015(3) -0.014(3) 0.004(3) C30 0.027(3) 0.024(3) 0.016(2) 0.004(2) -0.003(2) -0.003(2) C31 0.031(3) 0.030(3) 0.020(3) 0.003(2) 0.002(2) -0.004(2) C32 0.030(3) 0.037(4) 0.024(3) 0.004(2) 0.005(2) -0.010(3) C33 0.031(3) 0.039(4) 0.023(3) 0.009(3) 0.000(2) -0.013(3) C34 0.038(3) 0.024(3) 0.023(3) 0.005(2) -0.011(2) -0.005(3) C35 0.024(3) 0.028(3) 0.024(3) 0.005(2) -0.001(2) -0.002(2) C36 0.038(4) 0.029(4) 0.044(4) 0.005(3) 0.002(3) -0.009(3) C37 0.044(4) 0.050(4) 0.037(4) -0.001(3) 0.014(3) -0.013(4) C38 0.021(3) 0.017(3) 0.022(3) 0.007(2) 0.004(2) -0.001(2) C39 0.027(3) 0.026(3) 0.026(3) 0.004(2) 0.003(2) 0.008(2) C40 0.034(3) 0.034(3) 0.019(3) 0.002(2) 0.005(2) 0.010(3) C41 0.028(3) 0.033(3) 0.025(3) 0.012(2) -0.001(2) 0.007(3) C42 0.021(3) 0.024(3) 0.028(3) 0.008(2) 0.004(2) 0.002(2) C43 0.027(3) 0.019(3) 0.025(3) 0.003(2) 0.004(2) -0.008(2) C44 0.069(5) 0.070(6) 0.028(3) -0.004(3) -0.004(3) 0.041(4) C45 0.035(3) 0.027(3) 0.035(3) 0.002(3) -0.002(3) 0.008(3) C46 0.020(3) 0.023(3) 0.015(2) 0.005(2) 0.002(2) -0.003(2) C47 0.024(3) 0.024(3) 0.024(3) 0.000(2) 0.002(2) -0.002(2) C48 0.036(3) 0.027(3) 0.024(3) 0.001(2) 0.006(2) -0.004(3) C49 0.039(3) 0.021(3) 0.030(3) 0.002(2) 0.007(3) 0.005(3) C50 0.033(3) 0.027(3) 0.020(3) -0.002(2) 0.001(2) 0.007(3) C51 0.025(3) 0.029(3) 0.021(3) -0.002(2) 0.003(2) 0.001(2) C52 0.042(4) 0.021(3) 0.054(4) -0.006(3) 0.005(3) -0.008(3) C53 0.043(4) 0.047(4) 0.043(4) 0.000(3) -0.001(3) 0.025(3) C54 0.023(3) 0.015(3) 0.022(3) 0.003(2) -0.002(2) -0.004(2) C55 0.023(3) 0.016(3) 0.026(3) 0.002(2) 0.000(2) -0.001(2) C56 0.031(3) 0.018(3) 0.028(3) 0.003(2) 0.006(2) -0.005(2) C57 0.034(3) 0.020(3) 0.022(3) 0.003(2) 0.007(2) -0.007(2) C58 0.033(3) 0.009(3) 0.025(3) 0.001(2) 0.001(2) -0.002(2) C59 0.026(3) 0.013(3) 0.025(3) 0.004(2) -0.001(2) 0.000(2) C60 0.032(3) 0.031(4) 0.042(4) 0.000(3) 0.008(3) -0.007(3) C61 0.043(4) 0.023(3) 0.023(3) -0.001(2) -0.001(3) -0.003(3) B1 0.022(3) 0.020(3) 0.022(3) 0.001(2) -0.002(2) 0.001(3) F1 0.136(5) 0.051(3) 0.067(3) -0.021(2) 0.042(3) -0.059(3) F2 0.331(10) 0.042(3) 0.051(3) -0.022(2) 0.094(5) -0.055(4) F3 0.087(4) 0.037(3) 0.224(8) -0.043(4) -0.041(5) 0.014(3) F4 0.070(3) 0.123(5) 0.045(3) -0.036(3) 0.021(2) -0.029(3) F5 0.092(4) 0.102(4) 0.093(4) 0.028(3) 0.063(3) 0.045(3) F6 0.080(3) 0.096(4) 0.084(3) -0.030(3) 0.058(3) -0.051(3) F7 0.063(3) 0.055(3) 0.089(3) 0.003(2) 0.034(3) 0.028(2) F8 0.079(3) 0.048(3) 0.048(2) -0.0003(19) -0.017(2) 0.036(2) F9 0.053(3) 0.031(2) 0.102(4) -0.017(2) -0.027(2) 0.0063(19) F10 0.087(3) 0.070(3) 0.0267(19) -0.0076(19) -0.016(2) 0.041(3) F11 0.227(9) 0.075(4) 0.048(3) -0.025(3) -0.021(4) 0.051(5) F12 0.072(4) 0.368(13) 0.047(3) -0.080(5) 0.006(3) 0.071(6) F13 0.105(6) 0.057(5) 0.57(2) -0.019(8) -0.161(10) -0.035(4) F14 0.161(8) 0.229(10) 0.245(10) -0.202(9) 0.113(7) -0.147(8) F15 0.323(14) 0.338(15) 0.072(4) -0.021(6) 0.033(6) -0.305(13) F16 0.054(3) 0.075(4) 0.135(5) -0.030(3) -0.053(3) 0.028(3) F17 0.067(4) 0.463(17) 0.077(4) 0.034(7) 0.025(3) 0.153(7) F18 0.077(4) 0.067(4) 0.159(6) 0.033(4) -0.029(4) 0.023(3) F19 0.041(2) 0.129(4) 0.034(2) 0.007(2) 0.0142(18) -0.015(3) F20 0.037(3) 0.039(3) 0.283(9) 0.010(4) 0.049(4) 0.004(2) F21 0.035(2) 0.108(4) 0.042(2) -0.007(2) 0.0072(18) -0.026(2) F22 0.040(2) 0.044(2) 0.0267(17) -0.0103(15) 0.0009(15) -0.0109(17) F23 0.072(3) 0.037(2) 0.035(2) 0.0172(16) -0.0193(19) -0.021(2) F24 0.0314(19) 0.043(2) 0.0328(18) -0.0068(15) -0.0058(15) 0.0025(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.07887(2) 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 . P1 . 2.2971(13) yes Pd1 . P2 . 2.2983(14) yes Pd1 . N1 . 2.008(4) yes Pd1 . N2 . 2.052(5) yes P1 . C1 . 1.830(5) yes P1 . C4 . 1.830(6) yes P1 . C7 . 1.801(5) yes P2 . C19 . 1.803(5) yes P2 . C21 . 1.825(6) yes P2 . C24 . 1.834(6) yes N1 . C12 . 1.395(6) yes N1 . C14 . 1.405(7) yes N2 . C27 . 1.314(8) yes N2 . C29 . 1.363(9) yes C1 . C2 . 1.523(8) yes C1 . C3 . 1.518(8) yes C1 . H11 . 0.950 no C2 . H23 . 0.950 no C2 . H22 . 0.950 no C2 . H21 . 0.950 no C3 . H33 . 0.950 no C3 . H32 . 0.950 no C3 . H31 . 0.950 no C4 . C5 . 1.534(8) yes C4 . C6 . 1.528(8) yes C4 . H41 . 0.950 no C5 . H53 . 0.950 no C5 . H52 . 0.950 no C5 . H51 . 0.950 no C6 . H63 . 0.950 no C6 . H62 . 0.950 no C6 . H61 . 0.950 no C7 . C8 . 1.398(7) yes C7 . C12 . 1.408(7) yes C8 . C9 . 1.377(8) yes C8 . H81 . 0.950 no C9 . C10 . 1.393(8) yes C9 . C13 . 1.516(8) yes C10 . C11 . 1.382(8) yes C10 . H101 . 0.950 no C11 . C12 . 1.418(7) yes C11 . H111 . 0.950 no C13 . H131 . 0.950 no C13 . H133 . 0.950 no C13 . H132 . 0.950 no C14 . C15 . 1.403(7) yes C14 . C19 . 1.406(7) yes C15 . C16 . 1.380(8) yes C15 . H151 . 0.950 no C16 . C17 . 1.390(8) yes C16 . H161 . 0.950 no C17 . C18 . 1.389(8) yes C17 . C20 . 1.507(8) yes C18 . C19 . 1.393(7) yes C18 . H181 . 0.950 no C20 . H202 . 0.950 no C20 . H201 . 0.950 no C20 . H203 . 0.950 no C21 . C22 . 1.519(9) yes C21 . C23 . 1.517(8) yes C21 . H211 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . H233 . 0.950 no C23 . H232 . 0.950 no C23 . H231 . 0.950 no C24 . C25 . 1.534(9) yes C24 . C26 . 1.533(8) yes C24 . H241 . 0.950 no C25 . H252 . 0.950 no C25 . H251 . 0.950 no C25 . H253 . 0.950 no C26 . H263 . 0.950 no C26 . H262 . 0.950 no C26 . H261 . 0.950 no C27 . H271 . 0.950 no C27 . C281 . 1.429(8) yes C27 . H271 . 0.950 no C27 . N30 . 1.268(10) yes C29 . H291 . 0.950 no C29 . N301 . 1.293(10) yes C29 . H291 . 0.950 no C29 . C28 . 1.416(9) yes C30 . C31 . 1.397(8) yes C30 . C35 . 1.393(8) yes C30 . B1 . 1.651(8) yes C31 . C32 . 1.398(8) yes C31 . H311 . 0.950 no C32 . C33 . 1.377(9) yes C32 . C37 . 1.492(9) yes C33 . C34 . 1.378(9) yes C33 . H331 . 0.950 no C34 . C35 . 1.384(8) yes C34 . C36 . 1.492(9) yes C35 . H351 . 0.950 no C36 . F1 . 1.321(7) yes C36 . F2 . 1.256(8) yes C36 . F3 . 1.306(8) yes C37 . F4 . 1.324(8) yes C37 . F5 . 1.313(9) yes C37 . F6 . 1.323(8) yes C38 . C39 . 1.397(7) yes C38 . C43 . 1.389(8) yes C38 . B1 . 1.641(7) yes C39 . C40 . 1.391(7) yes C39 . H391 . 0.950 no C40 . C41 . 1.383(8) yes C40 . C44 . 1.482(9) yes C41 . C42 . 1.385(8) yes C41 . H411 . 0.950 no C42 . C43 . 1.391(7) yes C42 . C45 . 1.492(8) yes C43 . H431 . 0.950 no C44 . F10 . 1.304(7) yes C44 . F11 . 1.385(11) yes C44 . F12 . 1.244(10) yes C45 . F7 . 1.336(8) yes C45 . F8 . 1.331(7) yes C45 . F9 . 1.325(7) yes C46 . C47 . 1.409(7) yes C46 . C51 . 1.397(7) yes C46 . B1 . 1.630(8) yes C47 . C48 . 1.381(8) yes C47 . H471 . 0.950 no C48 . C49 . 1.385(8) yes C48 . C52 . 1.475(8) yes C49 . C50 . 1.389(8) yes C49 . H491 . 0.950 no C50 . C51 . 1.390(8) yes C50 . C53 . 1.476(8) yes C51 . H511 . 0.950 no C52 . F13 . 1.198(10) yes C52 . F14 . 1.224(9) yes C52 . F15 . 1.173(9) yes C53 . F16 . 1.291(8) yes C53 . F17 . 1.218(8) yes C53 . F18 . 1.364(9) yes C54 . C55 . 1.392(7) yes C54 . C59 . 1.415(7) yes C54 . B1 . 1.633(8) yes C55 . C56 . 1.387(8) yes C55 . H551 . 0.950 no C56 . C57 . 1.388(8) yes C56 . C60 . 1.481(8) yes C57 . C58 . 1.379(8) yes C57 . H571 . 0.950 no C58 . C59 . 1.386(7) yes C58 . C61 . 1.496(7) yes C59 . H591 . 0.950 no C60 . F19 . 1.309(7) yes C60 . F20 . 1.313(8) yes C60 . F21 . 1.325(7) yes C61 . F22 . 1.340(7) yes C61 . F23 . 1.345(7) yes C61 . F24 . 1.335(7) yes C62 . C63 . 1.39(3) yes C62 . C64 . 1.40(3) yes C62 . C65 . 1.15(3) yes C63 . C64 4_655 1.41(3) yes C63 . H631 . 0.950 no C64 . H641 . 0.950 no C65 . H651 . 0.950 no C65 . H652 . 0.950 no C65 . H653 . 0.950 no N301 . C281 . 1.357(11) yes N301 . H3011 . 0.870 no C28 . N30 . 1.342(12) yes C28 . H281 . 0.950 no C281 . H2811 . 0.950 no N30 . H301 . 0.870 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 P1 . Pd1 . P2 . 166.26(5) yes P1 . Pd1 . N1 . 83.09(13) yes P2 . Pd1 . N1 . 83.19(13) yes P1 . Pd1 . N2 . 95.93(13) yes P2 . Pd1 . N2 . 97.80(13) yes N1 . Pd1 . N2 . 178.75(19) yes Pd1 . P1 . C1 . 115.26(19) yes Pd1 . P1 . C4 . 118.34(18) yes C1 . P1 . C4 . 107.5(3) yes Pd1 . P1 . C7 . 99.50(18) yes C1 . P1 . C7 . 109.2(2) yes C4 . P1 . C7 . 106.2(3) yes Pd1 . P2 . C19 . 99.31(17) yes Pd1 . P2 . C21 . 119.2(2) yes C19 . P2 . C21 . 105.8(3) yes Pd1 . P2 . C24 . 114.1(2) yes C19 . P2 . C24 . 109.8(3) yes C21 . P2 . C24 . 107.8(3) yes Pd1 . N1 . C12 . 119.3(3) yes Pd1 . N1 . C14 . 118.7(3) yes C12 . N1 . C14 . 122.0(4) yes Pd1 . N2 . C27 . 129.1(5) yes Pd1 . N2 . C29 . 125.2(4) yes C27 . N2 . C29 . 105.5(5) yes P1 . C1 . C2 . 109.7(4) yes P1 . C1 . C3 . 113.8(4) yes C2 . C1 . C3 . 112.2(5) yes P1 . C1 . H11 . 107.1 no C2 . C1 . H11 . 106.9 no C3 . C1 . H11 . 106.7 no C1 . C2 . H23 . 109.3 no C1 . C2 . H22 . 110.4 no H23 . C2 . H22 . 109.5 no C1 . C2 . H21 . 108.8 no H23 . C2 . H21 . 109.5 no H22 . C2 . H21 . 109.5 no C1 . C3 . H33 . 109.8 no C1 . C3 . H32 . 108.6 no H33 . C3 . H32 . 109.5 no C1 . C3 . H31 . 109.9 no H33 . C3 . H31 . 109.5 no H32 . C3 . H31 . 109.5 no P1 . C4 . C5 . 108.8(4) yes P1 . C4 . C6 . 112.9(4) yes C5 . C4 . C6 . 111.3(5) yes P1 . C4 . H41 . 107.7 no C5 . C4 . H41 . 108.1 no C6 . C4 . H41 . 107.9 no C4 . C5 . H53 . 109.7 no C4 . C5 . H52 . 109.7 no H53 . C5 . H52 . 109.5 no C4 . C5 . H51 . 109.0 no H53 . C5 . H51 . 109.5 no H52 . C5 . H51 . 109.5 no C4 . C6 . H63 . 109.5 no C4 . C6 . H62 . 109.2 no H63 . C6 . H62 . 109.5 no C4 . C6 . H61 . 109.7 no H63 . C6 . H61 . 109.5 no H62 . C6 . H61 . 109.5 no P1 . C7 . C8 . 124.1(4) yes P1 . C7 . C12 . 114.5(4) yes C8 . C7 . C12 . 121.3(5) yes C7 . C8 . C9 . 121.7(5) yes C7 . C8 . H81 . 119.4 no C9 . C8 . H81 . 118.9 no C8 . C9 . C10 . 117.6(5) yes C8 . C9 . C13 . 121.3(5) yes C10 . C9 . C13 . 121.1(5) yes C9 . C10 . C11 . 122.0(5) yes C9 . C10 . H101 . 118.7 no C11 . C10 . H101 . 119.3 no C10 . C11 . C12 . 121.1(5) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 119.2 no C11 . C12 . C7 . 116.3(5) yes C11 . C12 . N1 . 124.5(5) yes C7 . C12 . N1 . 119.0(5) yes C9 . C13 . H131 . 109.2 no C9 . C13 . H133 . 109.7 no H131 . C13 . H133 . 109.5 no C9 . C13 . H132 . 109.6 no H131 . C13 . H132 . 109.5 no H133 . C13 . H132 . 109.5 no N1 . C14 . C15 . 124.3(5) yes N1 . C14 . C19 . 118.6(4) yes C15 . C14 . C19 . 116.9(5) yes C14 . C15 . C16 . 120.6(5) yes C14 . C15 . H151 . 119.6 no C16 . C15 . H151 . 119.9 no C15 . C16 . C17 . 122.7(5) yes C15 . C16 . H161 . 119.0 no C17 . C16 . H161 . 118.3 no C16 . C17 . C18 . 117.0(5) yes C16 . C17 . C20 . 122.0(5) yes C18 . C17 . C20 . 120.9(5) yes C17 . C18 . C19 . 121.2(5) yes C17 . C18 . H181 . 119.2 no C19 . C18 . H181 . 119.5 no P2 . C19 . C14 . 114.8(4) yes P2 . C19 . C18 . 123.6(4) yes C14 . C19 . C18 . 121.4(5) yes C17 . C20 . H202 . 109.5 no C17 . C20 . H201 . 110.0 no H202 . C20 . H201 . 109.5 no C17 . C20 . H203 . 109.0 no H202 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no P2 . C21 . C22 . 109.5(4) yes P2 . C21 . C23 . 112.6(4) yes C22 . C21 . C23 . 111.5(5) yes P2 . C21 . H211 . 107.9 no C22 . C21 . H211 . 107.4 no C23 . C21 . H211 . 107.7 no C21 . C22 . H221 . 108.8 no C21 . C22 . H222 . 109.9 no H221 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.7 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C21 . C23 . H233 . 109.1 no C21 . C23 . H232 . 109.9 no H233 . C23 . H232 . 109.5 no C21 . C23 . H231 . 109.4 no H233 . C23 . H231 . 109.5 no H232 . C23 . H231 . 109.5 no P2 . C24 . C25 . 108.4(4) yes P2 . C24 . C26 . 113.8(4) yes C25 . C24 . C26 . 111.6(5) yes P2 . C24 . H241 . 107.7 no C25 . C24 . H241 . 107.6 no C26 . C24 . H241 . 107.6 no C24 . C25 . H252 . 109.3 no C24 . C25 . H251 . 109.0 no H252 . C25 . H251 . 109.5 no C24 . C25 . H253 . 110.0 no H252 . C25 . H253 . 109.5 no H251 . C25 . H253 . 109.5 no C24 . C26 . H263 . 109.3 no C24 . C26 . H262 . 110.0 no H263 . C26 . H262 . 109.5 no C24 . C26 . H261 . 109.1 no H263 . C26 . H261 . 109.5 no H262 . C26 . H261 . 109.5 no N2 . C27 . H271 . 124.2 no N2 . C27 . C281 . 101.5(8) yes H271 . C27 . C281 . 134.3 no N2 . C27 . H271 . 124.2 no N2 . C27 . N30 . 123.8(11) yes H271 . C27 . N30 . 112.0 no N2 . C29 . H291 . 125.2 no N2 . C29 . N301 . 120.5(9) yes H291 . C29 . N301 . 114.3 no N2 . C29 . H291 . 125.2 no N2 . C29 . C28 . 97.1(11) yes H291 . C29 . C28 . 137.6 no C31 . C30 . C35 . 115.7(5) yes C31 . C30 . B1 . 122.4(5) yes C35 . C30 . B1 . 121.0(5) yes C30 . C31 . C32 . 122.3(6) yes C30 . C31 . H311 . 118.9 no C32 . C31 . H311 . 118.8 no C31 . C32 . C33 . 120.1(6) yes C31 . C32 . C37 . 118.8(6) yes C33 . C32 . C37 . 121.1(5) yes C32 . C33 . C34 . 118.8(5) yes C32 . C33 . H331 . 120.7 no C34 . C33 . H331 . 120.6 no C33 . C34 . C35 . 120.8(5) yes C33 . C34 . C36 . 120.0(6) yes C35 . C34 . C36 . 119.1(6) yes C30 . C35 . C34 . 122.3(6) yes C30 . C35 . H351 . 118.8 no C34 . C35 . H351 . 118.9 no C34 . C36 . F1 . 113.6(6) yes C34 . C36 . F2 . 114.2(5) yes F1 . C36 . F2 . 104.8(6) yes C34 . C36 . F3 . 111.2(5) yes F1 . C36 . F3 . 100.8(6) yes F2 . C36 . F3 . 111.3(7) yes C32 . C37 . F4 . 111.8(6) yes C32 . C37 . F5 . 112.8(5) yes F4 . C37 . F5 . 105.4(6) yes C32 . C37 . F6 . 113.3(6) yes F4 . C37 . F6 . 105.8(5) yes F5 . C37 . F6 . 107.2(6) yes C39 . C38 . C43 . 115.6(5) yes C39 . C38 . B1 . 121.7(5) yes C43 . C38 . B1 . 122.1(5) yes C38 . C39 . C40 . 122.4(5) yes C38 . C39 . H391 . 118.8 no C40 . C39 . H391 . 118.8 no C39 . C40 . C41 . 121.0(5) yes C39 . C40 . C44 . 119.4(5) yes C41 . C40 . C44 . 119.7(5) yes C40 . C41 . C42 . 117.6(5) yes C40 . C41 . H411 . 121.2 no C42 . C41 . H411 . 121.2 no C41 . C42 . C43 . 121.1(5) yes C41 . C42 . C45 . 119.6(5) yes C43 . C42 . C45 . 119.2(5) yes C42 . C43 . C38 . 122.3(5) yes C42 . C43 . H431 . 118.5 no C38 . C43 . H431 . 119.1 no C40 . C44 . F10 . 115.5(6) yes C40 . C44 . F11 . 110.8(6) yes F10 . C44 . F11 . 102.4(7) yes C40 . C44 . F12 . 115.5(7) yes F10 . C44 . F12 . 110.5(7) yes F11 . C44 . F12 . 100.2(8) yes C42 . C45 . F7 . 112.7(5) yes C42 . C45 . F8 . 113.2(5) yes F7 . C45 . F8 . 105.4(5) yes C42 . C45 . F9 . 112.2(5) yes F7 . C45 . F9 . 105.8(5) yes F8 . C45 . F9 . 106.9(5) yes C47 . C46 . C51 . 115.0(5) yes C47 . C46 . B1 . 122.2(5) yes C51 . C46 . B1 . 122.3(5) yes C46 . C47 . C48 . 122.4(5) yes C46 . C47 . H471 . 118.8 no C48 . C47 . H471 . 118.7 no C47 . C48 . C49 . 121.3(5) yes C47 . C48 . C52 . 120.2(5) yes C49 . C48 . C52 . 118.4(6) yes C48 . C49 . C50 . 117.6(5) yes C48 . C49 . H491 . 121.3 no C50 . C49 . H491 . 121.1 no C49 . C50 . C51 . 120.8(5) yes C49 . C50 . C53 . 118.8(6) yes C51 . C50 . C53 . 120.4(6) yes C46 . C51 . C50 . 122.7(5) yes C46 . C51 . H511 . 118.8 no C50 . C51 . H511 . 118.4 no C48 . C52 . F13 . 116.2(6) yes C48 . C52 . F14 . 115.5(6) yes F13 . C52 . F14 . 97.4(10) yes C48 . C52 . F15 . 118.2(7) yes F13 . C52 . F15 . 102.3(10) yes F14 . C52 . F15 . 104.3(9) yes C50 . C53 . F16 . 114.6(6) yes C50 . C53 . F17 . 115.7(6) yes F16 . C53 . F17 . 111.9(8) yes C50 . C53 . F18 . 111.9(6) yes F16 . C53 . F18 . 98.9(6) yes F17 . C53 . F18 . 101.8(8) yes C55 . C54 . C59 . 116.0(5) yes C55 . C54 . B1 . 123.3(4) yes C59 . C54 . B1 . 120.4(5) yes C54 . C55 . C56 . 122.7(5) yes C54 . C55 . H551 . 119.0 no C56 . C55 . H551 . 118.3 no C55 . C56 . C57 . 119.9(5) yes C55 . C56 . C60 . 119.5(5) yes C57 . C56 . C60 . 120.6(5) yes C56 . C57 . C58 . 119.2(5) yes C56 . C57 . H571 . 120.4 no C58 . C57 . H571 . 120.3 no C57 . C58 . C59 . 120.6(5) yes C57 . C58 . C61 . 117.8(5) yes C59 . C58 . C61 . 121.4(5) yes C54 . C59 . C58 . 121.6(5) yes C54 . C59 . H591 . 119.7 no C58 . C59 . H591 . 118.8 no C56 . C60 . F19 . 113.2(5) yes C56 . C60 . F20 . 112.9(5) yes F19 . C60 . F20 . 107.6(6) yes C56 . C60 . F21 . 113.8(5) yes F19 . C60 . F21 . 104.8(5) yes F20 . C60 . F21 . 103.7(6) yes C58 . C61 . F22 . 112.5(5) yes C58 . C61 . F23 . 111.9(5) yes F22 . C61 . F23 . 105.9(5) yes C58 . C61 . F24 . 113.1(5) yes F22 . C61 . F24 . 106.9(5) yes F23 . C61 . F24 . 106.1(5) yes C30 . B1 . C38 . 101.5(4) yes C30 . B1 . C54 . 112.5(4) yes C38 . B1 . C54 . 112.9(4) yes C30 . B1 . C46 . 112.2(4) yes C38 . B1 . C46 . 113.2(4) yes C54 . B1 . C46 . 105.0(4) yes C63 . C62 . C64 . 117(2) yes C63 . C62 . C65 . 115(3) yes C64 . C62 . C65 . 127(3) yes C64 4_655 C63 . C62 . 121(2) yes C64 4_655 C63 . H631 . 119.5 no C62 . C63 . H631 . 119.3 no C63 4_655 C64 . C62 . 121(2) yes C63 4_655 C64 . H641 . 119.9 no C62 . C64 . H641 . 118.7 no C62 . C65 . H651 . 110.2 no C62 . C65 . H652 . 109.1 no H651 . C65 . H652 . 109.5 no C62 . C65 . H653 . 109.1 no H651 . C65 . H653 . 109.5 no H652 . C65 . H653 . 109.5 no C29 . N301 . C281 . 95.6(10) yes C29 . N301 . H3011 . 132.0 no C281 . N301 . H3011 . 132.4 no C29 . C28 . N30 . 120.5(15) yes C29 . C28 . H281 . 127.3 no N30 . C28 . H281 . 112.2 no C27 . C281 . N301 . 116.9(10) yes C27 . C281 . H2811 . 122.3 no N301 . C281 . H2811 . 120.7 no C28 . N30 . C27 . 93.1(14) yes C28 . N30 . H301 . 139.8 no C27 . N30 . H301 . 127.1 no