# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _audit_creation_method CRYSTALS_ver_12-03-99 _publ_contact_author_name 'Sofia I. Pascu' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK ; _publ_contact_author_email sip22@cam.ac.uk _publ_contact_author_fax '(01223) 336362' _publ_contact_author_phone '(01223) 336317' loop_ _publ_author_name 'Sofia Ioana Pascu' 'Karl S. Coleman' 'Andrew R. Cowley' 'Malcolm L. H. Green' 'Nicholas H. Rees' ####################### ## denoted 1 in text ## ####################### data_1 _database_code_depnum_ccdc_archive 'CCDC 236196' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 11.5760(10) _cell_angle_alpha 90 _cell_length_b 23.162(3) _cell_angle_beta 117.850(10) _cell_length_c 11.1710(10) _cell_angle_gamma 90 _cell_volume 2648.3(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.3740 2.4560 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Ni ' 0.2850 1.1130 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 2 _chemical_formula_sum ' C56 H52 Br4 N2 Ni2 P2 ' _chemical_formula_moiety ' C56 H52 Br4 N2 Ni2 P2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1252.03 _cell_measurement_reflns_used 9465 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26.70 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.827 _diffrn_measurement_device_type ; Nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; Xpress Data collection (MAC Science, 1989) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.56 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 9465 _reflns_number_total 5338 _diffrn_reflns_av_R_equivalents 0.11 # Number of reflections with Friedels Law is 0 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5531 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 26.70 _diffrn_measured_fraction_theta_max 0.97 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _reflns_limit_h_min -14 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _refine_diff_density_min -1.96 _refine_diff_density_max 4.20 _refine_ls_number_reflns 2572 _refine_ls_number_restraints 3 _refine_ls_number_parameters 298 #_refine_ls_R_factor_ref 0.1170 _refine_ls_wR_factor_ref 0.1041 _refine_ls_goodness_of_fit_ref 1.0730 #_reflns_number_all 5338 _refine_ls_R_factor_all 0.1762 _refine_ls_wR_factor_all 0.1087 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 2572 _refine_ls_R_factor_gt 0.1170 _refine_ls_wR_factor_gt 0.1041 _refine_ls_shift/su_max 0.003577 _refine_ls_structure_factor_coef F _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: 3.07 0.636 2.37 0.210 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _refine_special_details ; The largest peaks and deepest troughs of the difference Fourier map lie close to the Br atoms, suggesting that these may be disordered. However attempts to model this did not lead to substantial improvements in the agreement of calculated and observed structure factors The large anisotropic thermal parameters of several of the C atoms may also be indicative of unresolved disorder, but in view of the paucity of observed diffraction data, it is not possible to model this meaningfully ; ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. MAC Science, (1989) Xpress Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. 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 trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Ni1 Ni -0.08394(18) -0.15130(9) 0.03175(18) 0.0340 1.0000 Uani . . . . . . Br1 Br 0.11147(16) -0.14273(8) 0.01740(17) 0.0489 1.0000 Uani . . . . . . Br2 Br 0.02387(17) -0.15833(8) 0.26553(15) 0.0460 1.0000 Uani . . . . . . P1 P -0.2569(4) -0.1737(2) 0.0455(4) 0.0419 1.0000 Uani . U . . . . N1 N -0.1982(12) -0.1378(5) -0.1574(11) 0.0355 1.0000 Uani . U . . . . C1 C -0.3674(15) -0.1892(7) -0.1354(16) 0.0467 1.0000 Uani . U . . . . C2 C -0.3196(13) -0.1546(6) -0.2126(15) 0.0372 1.0000 Uani . U . . . . C3 C -0.3321(18) -0.1183(9) 0.0953(17) 0.0547 1.0000 Uani . . . . . . C4 C -0.259(2) -0.0684(9) 0.158(2) 0.0681 1.0000 Uani . . . . . . C5 C -0.320(3) -0.0260(13) 0.198(3) 0.1176 1.0000 Uani . . . . . . C6 C -0.449(3) -0.0306(18) 0.170(3) 0.1233 1.0000 Uani . . . . . . C7 C -0.521(3) -0.0811(16) 0.108(3) 0.1027 1.0000 Uani . . . . . . C8 C -0.460(2) -0.1223(11) 0.070(2) 0.0735 1.0000 Uani . . . . . . C9 C -0.2584(15) -0.2378(8) 0.1357(15) 0.0484 1.0000 Uani . . . . . . C10 C -0.2621(18) -0.2333(8) 0.2616(18) 0.0538 1.0000 Uani . . . . . . C11 C -0.263(2) -0.2817(10) 0.329(2) 0.0749 1.0000 Uani . . . . . . C12 C -0.264(2) -0.3371(8) 0.2738(18) 0.0603 1.0000 Uani . . . . . . C13 C -0.2552(17) -0.3419(8) 0.1537(18) 0.0509 1.0000 Uani . . . . . . C14 C -0.2508(14) -0.2923(7) 0.0879(16) 0.0394 1.0000 Uani . . . . . . C15 C -0.4169(13) -0.1430(7) -0.3613(15) 0.0370 1.0000 Uani . . . . . . C16 C -0.4641(17) -0.1891(9) -0.4527(19) 0.0621 1.0000 Uani . . . . . . C17 C -0.565(3) -0.1768(12) -0.584(2) 0.0835 1.0000 Uani . . . . . . C18 C -0.6081(19) -0.1238(15) -0.619(2) 0.0925 1.0000 Uani . . . . . . C19 C -0.562(2) -0.0767(10) -0.531(2) 0.0793 1.0000 Uani . . . . . . C20 C -0.4692(15) -0.0872(8) -0.4021(17) 0.0509 1.0000 Uani . . . . . . C21 C -0.1583(17) -0.1001(8) -0.2356(19) 0.0510 1.0000 Uani . . . . . . C22 C -0.1202(17) -0.1268(11) -0.323(2) 0.0689 1.0000 Uani . . . . . . C23 C -0.0854(18) -0.0877(14) -0.408(2) 0.0873 1.0000 Uani . . . . . . C24 C -0.088(2) -0.0270(12) -0.379(2) 0.0734 1.0000 Uani . . . . . . C25 C -0.110(2) -0.0066(10) -0.282(3) 0.0813 1.0000 Uani . . . . . . C26 C -0.1514(17) -0.0423(7) -0.208(2) 0.0581 1.0000 Uani . . . . . . C27 C -0.117(2) -0.1895(10) -0.344(2) 0.0751 1.0000 Uani . . . . . . C28 C -0.1767(18) -0.0175(8) -0.102(3) 0.0675 1.0000 Uani . . . . . . H11 H -0.3643 -0.2312 -0.1545 0.0449 1.0000 Uiso . . . . . . H12 H -0.4591 -0.1781 -0.1593 0.0449 1.0000 Uiso . . . . . . H41 H -0.1678 -0.0634 0.1726 0.0800 1.0000 Uiso . . . . . . H51 H -0.2688 0.0086 0.2487 0.1394 1.0000 Uiso . . . . . . H61 H -0.4919 0.0019 0.1935 0.1535 1.0000 Uiso . . . . . . H71 H -0.6127 -0.0865 0.0930 0.1296 1.0000 Uiso . . . . . . H81 H -0.5116 -0.1571 0.0205 0.0941 1.0000 Uiso . . . . . . H101 H -0.2640 -0.1945 0.2998 0.0650 1.0000 Uiso . . . . . . H111 H -0.2634 -0.2785 0.4181 0.0926 1.0000 Uiso . . . . . . H121 H -0.2703 -0.3726 0.3211 0.0741 1.0000 Uiso . . . . . . H131 H -0.2525 -0.3807 0.1159 0.0651 1.0000 Uiso . . . . . . H141 H -0.2418 -0.2956 0.0033 0.0444 1.0000 Uiso . . . . . . H161 H -0.4281 -0.2290 -0.4262 0.0638 1.0000 Uiso . . . . . . H171 H -0.6037 -0.2088 -0.6515 0.0975 1.0000 Uiso . . . . . . H181 H -0.6777 -0.1167 -0.7136 0.0976 1.0000 Uiso . . . . . . H191 H -0.5972 -0.0369 -0.5610 0.0767 1.0000 Uiso . . . . . . H201 H -0.4369 -0.0548 -0.3352 0.0541 1.0000 Uiso . . . . . . H231 H -0.0622 -0.1022 -0.4779 0.0974 1.0000 Uiso . . . . . . H241 H -0.0726 0.0014 -0.4369 0.0845 1.0000 Uiso . . . . . . H251 H -0.0966 0.0355 -0.2604 0.0853 1.0000 Uiso . . . . . . H271 H -0.0857 -0.1967 -0.4123 0.0974 1.0000 Uiso . . . . . . H272 H -0.2070 -0.2058 -0.3779 0.0974 1.0000 Uiso . . . . . . H273 H -0.0566 -0.2085 -0.2566 0.0974 1.0000 Uiso . . . . . . H281 H -0.1658 0.0254 -0.1007 0.0778 1.0000 Uiso . . . . . . H282 H -0.2680 -0.0270 -0.1212 0.0778 1.0000 Uiso . . . . . . H283 H -0.1136 -0.0339 -0.0124 0.0778 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0311(9) 0.0362(11) 0.0266(9) 0.0010(8) 0.0067(7) -0.0011(8) Br1 0.0347(8) 0.0643(12) 0.0419(9) -0.0084(8) 0.0130(7) 0.0028(8) Br2 0.0430(9) 0.0540(11) 0.0262(7) 0.0041(7) 0.0036(6) -0.0051(8) P1 0.039(2) 0.056(3) 0.0241(18) 0.0030(18) 0.0091(17) -0.0110(19) N1 0.036(5) 0.046(7) 0.011(5) 0.004(5) 0.000(4) -0.005(5) C1 0.035(9) 0.043(10) 0.034(4) -0.002(6) -0.007(5) -0.009(7) C2 0.029(5) 0.020(7) 0.041(8) 0.000(6) -0.001(5) 0.010(5) C3 0.050(10) 0.077(13) 0.026(8) 0.008(8) 0.009(8) -0.015(9) C4 0.074(14) 0.059(12) 0.067(13) -0.003(10) 0.030(11) 0.004(11) C5 0.11(2) 0.14(2) 0.10(2) -0.060(19) 0.046(18) 0.031(19) C6 0.10(2) 0.19(4) 0.10(2) 0.02(2) 0.058(19) 0.08(2) C7 0.084(19) 0.14(3) 0.10(2) 0.010(19) 0.056(17) 0.021(19) C8 0.059(13) 0.098(17) 0.079(15) 0.018(13) 0.044(12) -0.001(12) C9 0.038(9) 0.069(12) 0.024(8) 0.010(8) 0.003(7) -0.008(8) C10 0.058(11) 0.064(12) 0.041(10) -0.009(9) 0.024(9) -0.014(9) C11 0.099(17) 0.079(15) 0.053(13) 0.011(11) 0.041(12) -0.017(13) C12 0.093(15) 0.050(11) 0.041(10) 0.011(8) 0.035(10) -0.009(10) C13 0.054(10) 0.055(11) 0.054(10) 0.004(9) 0.034(9) -0.004(9) C14 0.025(7) 0.047(10) 0.039(9) -0.003(7) 0.009(7) -0.009(7) C15 0.033(8) 0.039(10) 0.046(9) 0.004(7) 0.025(7) -0.003(7) C16 0.039(10) 0.074(13) 0.046(11) -0.010(10) -0.002(9) -0.008(9) C17 0.10(2) 0.089(18) 0.050(14) -0.010(13) 0.030(14) -0.030(15) C18 0.032(10) 0.17(3) 0.040(12) 0.028(15) -0.012(9) -0.033(14) C19 0.051(11) 0.095(16) 0.045(12) 0.038(12) -0.016(10) -0.007(11) C20 0.033(9) 0.054(11) 0.048(10) 0.001(8) 0.004(8) -0.019(8) C21 0.039(9) 0.059(12) 0.057(11) 0.011(9) 0.025(9) -0.004(8) C22 0.034(9) 0.13(2) 0.058(12) -0.002(12) 0.034(9) -0.022(11) C23 0.022(9) 0.17(3) 0.052(13) 0.018(15) 0.002(9) -0.015(12) C24 0.056(12) 0.103(19) 0.052(13) 0.041(13) 0.018(11) 0.001(12) C25 0.051(12) 0.082(16) 0.080(18) 0.029(13) 0.005(12) -0.007(11) C26 0.049(10) 0.039(10) 0.086(14) 0.028(10) 0.031(10) -0.003(8) C27 0.075(14) 0.077(15) 0.092(17) -0.028(13) 0.054(13) -0.027(12) C28 0.042(10) 0.036(11) 0.116(19) 0.005(11) 0.030(12) 0.009(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . Br1 . 2.350(2) yes Ni1 . Br2 . 2.315(2) yes Ni1 . P1 . 2.142(5) yes Ni1 . N1 . 1.924(11) yes Ni1 . C2 . 2.818(13) yes P1 . C1 . 1.853(15) yes P1 . C3 . 1.78(2) yes P1 . C9 . 1.800(17) yes N1 . C2 . 1.303(19) yes N1 . C21 . 1.45(2) yes C1 . C2 . 1.46(2) yes C1 . H12 . 1.000 no C1 . C2 . 1.46(2) yes C1 . H11 . 1.000 no C2 . C15 . 1.53(2) yes C3 . C4 . 1.41(3) yes C3 . C8 . 1.38(3) yes C4 . C5 . 1.40(3) yes C4 . H41 . 1.000 no C5 . C6 . 1.38(4) yes C5 . H51 . 1.000 no C6 . C7 . 1.42(4) yes C6 . H61 . 1.000 no C7 . C8 . 1.37(4) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.43(2) yes C9 . C14 . 1.39(2) yes C10 . C11 . 1.35(3) yes C10 . H101 . 1.000 no C11 . C12 . 1.42(3) yes C11 . H111 . 1.000 no C12 . C13 . 1.39(2) yes C12 . H121 . 1.000 no C13 . C14 . 1.38(2) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.40(2) yes C15 . C20 . 1.41(2) yes C16 . C17 . 1.41(3) yes C16 . H161 . 1.000 no C17 . C18 . 1.31(4) yes C17 . H171 . 1.000 no C18 . C19 . 1.40(4) yes C18 . H181 . 1.000 no C19 . C20 . 1.35(2) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.39(3) yes C21 . C26 . 1.37(2) yes C22 . C23 . 1.50(3) yes C22 . C27 . 1.48(3) yes C23 . C24 . 1.45(4) yes C23 . H231 . 1.000 no C24 . C25 . 1.30(3) yes C24 . H241 . 1.000 no C25 . C26 . 1.41(3) yes C25 . H251 . 1.000 no C26 . C28 . 1.46(3) yes C27 . H272 . 1.000 no C27 . H273 . 1.000 no C27 . H271 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no C28 . H281 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . Ni1 . Br2 . 93.10(9) yes Br1 . Ni1 . P1 . 170.85(17) yes Br2 . Ni1 . P1 . 86.09(13) yes Br1 . Ni1 . N1 . 95.8(4) yes Br2 . Ni1 . N1 . 169.2(4) yes P1 . Ni1 . N1 . 86.1(4) yes Br1 . Ni1 . C2 . 117.6(4) yes Br2 . Ni1 . C2 . 149.2(4) yes P1 . Ni1 . C2 . 63.1(4) yes N1 . Ni1 . C2 . 23.5(5) yes Ni1 . P1 . C1 . 99.3(6) yes Ni1 . P1 . C3 . 117.3(6) yes C1 . P1 . C3 . 107.0(8) yes Ni1 . P1 . C9 . 119.6(6) yes C1 . P1 . C9 . 105.5(8) yes C3 . P1 . C9 . 106.6(8) yes Ni1 . N1 . C2 . 120.5(10) yes Ni1 . N1 . C21 . 120.6(10) yes C2 . N1 . C21 . 118.1(13) yes P1 . C1 . C2 . 106.1(10) yes P1 . C1 . H12 . 110.302 no C2 . C1 . H12 . 110.314 no P1 . C1 . C2 . 106.1(10) yes P1 . C1 . H11 . 110.294 no C2 . C1 . H11 . 110.305 no C1 . C2 . N1 . 120.4(13) yes C1 . C2 . Ni1 . 84.6(8) yes N1 . C2 . Ni1 . 36.0(7) yes C1 . C2 . C15 . 116.5(12) yes N1 . C2 . C15 . 123.0(14) yes Ni1 . C2 . C15 . 158.9(11) yes P1 . C3 . C4 . 118.6(15) yes P1 . C3 . C8 . 121.5(16) yes C4 . C3 . C8 . 120(2) yes C3 . C4 . C5 . 117(2) yes C3 . C4 . H41 . 121.296 no C5 . C4 . H41 . 121.309 no C4 . C5 . C6 . 122(3) yes C4 . C5 . H51 . 119.109 no C6 . C5 . H51 . 119.124 no C5 . C6 . C7 . 120(3) yes C5 . C6 . H61 . 119.887 no C7 . C6 . H61 . 119.895 no C6 . C7 . C8 . 117(3) yes C6 . C7 . H71 . 121.387 no C8 . C7 . H71 . 121.364 no C3 . C8 . C7 . 123(2) yes C3 . C8 . H81 . 118.317 no C7 . C8 . H81 . 118.335 no P1 . C9 . C10 . 120.2(14) yes P1 . C9 . C14 . 121.0(13) yes C10 . C9 . C14 . 118.7(15) yes C9 . C10 . C11 . 119.9(18) yes C9 . C10 . H101 . 120.084 no C11 . C10 . H101 . 120.059 no C10 . C11 . C12 . 120.4(19) yes C10 . C11 . H111 . 119.803 no C12 . C11 . H111 . 119.786 no C11 . C12 . C13 . 120.0(16) yes C11 . C12 . H121 . 119.977 no C13 . C12 . H121 . 119.988 no C12 . C13 . C14 . 118.9(16) yes C12 . C13 . H131 . 120.538 no C14 . C13 . H131 . 120.526 no C9 . C14 . C13 . 121.8(16) yes C9 . C14 . H141 . 119.082 no C13 . C14 . H141 . 119.090 no C2 . C15 . C16 . 119.7(14) yes C2 . C15 . C20 . 119.8(14) yes C16 . C15 . C20 . 120.1(15) yes C15 . C16 . C17 . 117.1(19) yes C15 . C16 . H161 . 121.474 no C17 . C16 . H161 . 121.463 no C16 . C17 . C18 . 121(2) yes C16 . C17 . H171 . 119.659 no C18 . C17 . H171 . 119.637 no C17 . C18 . C19 . 123.7(18) yes C17 . C18 . H181 . 118.158 no C19 . C18 . H181 . 118.127 no C18 . C19 . C20 . 117(2) yes C18 . C19 . H191 . 121.355 no C20 . C19 . H191 . 121.353 no C15 . C20 . C19 . 121.1(18) yes C15 . C20 . H201 . 119.479 no C19 . C20 . H201 . 119.467 no N1 . C21 . C22 . 116.6(16) yes N1 . C21 . C26 . 116.9(16) yes C22 . C21 . C26 . 126.3(18) yes C21 . C22 . C23 . 116(2) yes C21 . C22 . C27 . 126.4(18) yes C23 . C22 . C27 . 117(2) yes C22 . C23 . C24 . 114(2) yes C22 . C23 . H231 . 123.039 no C24 . C23 . H231 . 123.066 no C23 . C24 . C25 . 125(2) yes C23 . C24 . H241 . 117.665 no C25 . C24 . H241 . 117.663 no C24 . C25 . C26 . 122(2) yes C24 . C25 . H251 . 119.054 no C26 . C25 . H251 . 119.062 no C25 . C26 . C21 . 116(2) yes C25 . C26 . C28 . 120.0(19) yes C21 . C26 . C28 . 123.8(16) yes C22 . C27 . H272 . 109.473 no C22 . C27 . H273 . 109.468 no H272 . C27 . H273 . 109.471 no C22 . C27 . H271 . 109.465 no C26 . C28 . H282 . 109.453 no C26 . C28 . H283 . 109.466 no H282 . C28 . H283 . 109.489 no C26 . C28 . H281 . 109.454 no #===END ####################### ## denoted 2 in text ## ####################### data_2 _database_code_depnum_ccdc_archive 'CCDC 236197' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 13.5350(6) _cell_angle_alpha 90 _cell_length_b 23.464(2) _cell_angle_beta 90 _cell_length_c 27.850(3) _cell_angle_gamma 90 _cell_volume 8844.7(12) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a b ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x+1/2,-y+1/2,z -x+1/2,y+1/2,-z -x,-y+1/2,z+1/2 x,y+1/2,-z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.3740 2.4560 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'Ni ' 0.2850 1.1130 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C41.24 H39.47 Br2 Cl2.47 N Ni O P2 ' _chemical_formula_moiety ' C40 H37 Br2 N Ni O P2, C1.24 H2.47 Cl2.47 ' _chemical_compound_source ; ? ; _chemical_formula_weight 933.10 _cell_measurement_reflns_used 49653 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3775.3 _exptl_absorpt_coefficient_mu 2.498 _diffrn_measurement_device_type ; Nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; Xpress Data collection (MAC Science, 1989) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_T_max 0.536 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 49653 _reflns_number_total 8500 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 8500 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9045 _diffrn_reflns_theta_min 1.700 _diffrn_reflns_theta_max 26.434 _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.951 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _refine_diff_density_min -1.16 _refine_diff_density_max 1.05 _refine_ls_number_reflns 3915 _refine_ls_number_restraints 165 _refine_ls_number_parameters 512 #_refine_ls_R_factor_ref 0.0581 _refine_ls_wR_factor_ref 0.0658 _refine_ls_goodness_of_fit_ref 1.2474 #_reflns_number_all 8464 _refine_ls_R_factor_all 0.1310 _refine_ls_wR_factor_all 0.0962 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3915 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_gt 0.0658 _refine_ls_shift/su_max 0.008007 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.64 0.420 1.28 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. MAC Science, (1989) Xpress Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. 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 trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Ni1 Ni 0.71521(6) 0.13231(4) 0.12001(4) 0.0368 1.0000 Uani . . . . . . Br1 Br 0.76739(6) 0.09558(4) 0.04071(3) 0.0516 1.0000 Uani . . . . . . Br2 Br 0.78451(5) 0.22673(3) 0.13904(3) 0.0521 1.0000 Uani . . . . . . P1 P 0.56570(13) 0.16962(8) 0.09310(8) 0.0398 1.0000 Uani . . . . . . N1 N 0.6287(4) 0.1251(2) 0.1828(2) 0.0351 1.0000 Uani . . . . . . C1 C 0.5282(5) 0.2005(3) 0.1504(3) 0.0471 1.0000 Uani . . . . . . C2 C 0.5524(5) 0.1575(3) 0.1894(3) 0.0363 1.0000 Uani . . . . . . C3 C 0.4669(5) 0.1182(4) 0.0799(4) 0.0838 1.0000 Uani D U . . . . C4 C 0.4906(5) 0.0726(4) 0.0514(4) 0.0845 1.0000 Uani D U . . . . C5 C 0.4238(5) 0.0298(4) 0.0442(4) 0.0849 1.0000 Uani D U . . . . C6 C 0.3294(5) 0.0353(4) 0.0604(4) 0.0846 1.0000 Uani D U . . . . C7 C 0.3054(5) 0.0793(4) 0.0899(4) 0.0841 1.0000 Uani D U . . . . C8 C 0.3740(6) 0.1210(4) 0.0996(4) 0.0839 1.0000 Uani D U . . . . C9 C 0.5568(6) 0.2265(3) 0.0491(3) 0.0496 1.0000 Uani . . . . . . C10 C 0.6412(8) 0.2480(6) 0.0290(5) 0.1084 1.0000 Uani . . . . . . C11 C 0.6343(11) 0.2932(6) -0.0040(6) 0.1370 1.0000 Uani . . . . . . C12 C 0.5457(10) 0.3151(4) -0.0172(5) 0.0899 1.0000 Uani . . . . . . C13 C 0.4639(9) 0.2961(5) 0.0047(4) 0.0823 1.0000 Uani . . . . . . C14 C 0.4674(6) 0.2520(4) 0.0374(3) 0.0620 1.0000 Uani . . . . . . C15 C 0.4863(5) 0.1577(3) 0.2318(3) 0.0389 1.0000 Uani . . . . . . C16 C 0.4630(6) 0.2095(3) 0.2529(3) 0.0482 1.0000 Uani . . . . . . C17 C 0.4051(7) 0.2119(4) 0.2932(3) 0.0588 1.0000 Uani . . . . . . C18 C 0.3680(7) 0.1625(5) 0.3126(3) 0.0661 1.0000 Uani . . . . . . C19 C 0.3858(6) 0.1118(4) 0.2905(4) 0.0599 1.0000 Uani . . . . . . C20 C 0.4475(5) 0.1081(3) 0.2509(3) 0.0496 1.0000 Uani . . . . . . C21 C 0.6609(5) 0.0857(3) 0.2192(3) 0.0421 1.0000 Uani . . . . . . C22 C 0.7083(6) 0.1050(4) 0.2603(3) 0.0552 1.0000 Uani . . . . . . C23 C 0.7439(6) 0.0654(5) 0.2924(3) 0.0705 1.0000 Uani . . . . . . C24 C 0.7330(8) 0.0080(5) 0.2837(5) 0.0819 1.0000 Uani . . . . . . C25 C 0.6862(8) -0.0110(4) 0.2420(5) 0.0760 1.0000 Uani . . . . . . C26 C 0.6506(6) 0.0272(4) 0.2102(4) 0.0586 1.0000 Uani . . . . . . C27 C 0.7245(7) 0.1673(4) 0.2688(3) 0.0640 1.0000 Uani . . . . . . C28 C 0.6004(8) 0.0074(4) 0.1643(4) 0.0710 1.0000 Uani . . . . . . O1 O 0.8311(3) 0.0910(2) 0.15142(19) 0.0441 1.0000 Uani . . . . . . P2 P 0.93628(13) 0.10237(8) 0.13761(7) 0.0406 1.0000 Uani . . . . . . C29 C 1.0068(5) 0.1266(3) 0.1881(3) 0.0378 1.0000 Uani . . . . . . C30 C 0.9682(6) 0.1195(3) 0.2348(3) 0.0460 1.0000 Uani . . . . . . C31 C 1.0210(6) 0.1375(4) 0.2740(3) 0.0541 1.0000 Uani . . . . . . C32 C 1.1131(7) 0.1617(4) 0.2683(3) 0.0543 1.0000 Uani . . . . . . C33 C 1.1512(6) 0.1689(3) 0.2228(3) 0.0520 1.0000 Uani . . . . . . C34 C 1.0998(5) 0.1505(3) 0.1832(3) 0.0457 1.0000 Uani . . . . . . C35 C 0.9988(5) 0.0413(3) 0.1132(3) 0.0415 1.0000 Uani . . . . . . C36 C 1.0156(6) -0.0058(4) 0.1426(3) 0.0563 1.0000 Uani . . . . . . C37 C 1.0602(7) -0.0540(4) 0.1233(4) 0.0620 1.0000 Uani . . . . . . C38 C 1.0916(6) -0.0545(4) 0.0765(4) 0.0577 1.0000 Uani . . . . . . C39 C 1.0781(6) -0.0071(4) 0.0480(3) 0.0548 1.0000 Uani . . . . . . C40 C 1.0309(5) 0.0399(4) 0.0668(3) 0.0509 1.0000 Uani . . . . . . C41 C 0.851(2) 0.1716(10) 0.4413(7) 0.1694 0.506(11) Uani D U P . . . Cl1 Cl 0.8881(7) 0.1109(5) 0.4064(3) 0.1681 0.506(11) Uani D U P . . . Cl2 Cl 0.7627(8) 0.2028(5) 0.4011(3) 0.1709 0.506(11) Uani D U P . . . C42 C 0.703(2) 0.4429(14) 0.4563(13) 0.2185 0.450(15) Uani D U P . . . Cl3 Cl 0.8053(13) 0.4330(6) 0.4184(6) 0.2170 0.450(15) Uani D U P . . . Cl4 Cl 0.6457(13) 0.3831(6) 0.4303(6) 0.2198 0.450(15) Uani D U P . . . C43 C 0.5830(17) 0.2967(12) 0.404(2) 0.1789 0.280(12) Uani D U P . . . Cl5 Cl 0.6890(19) 0.3410(8) 0.4046(7) 0.1778 0.280(12) Uani D U P . . . Cl6 Cl 0.6492(19) 0.2339(8) 0.3883(6) 0.1802 0.280(12) Uani D U P . . . H1 H 0.950(7) 0.141(4) 0.103(4) 0.09(3) 1.0000 Uiso . . . . . . H11 H 0.5651 0.2367 0.1562 0.0565 1.0000 Uiso . . . . . . H12 H 0.4556 0.2084 0.1501 0.0565 1.0000 Uiso . . . . . . H41 H 0.5571 0.0706 0.0358 0.1014 1.0000 Uiso . . . . . . H51 H 0.4443 -0.0057 0.0269 0.1019 1.0000 Uiso . . . . . . H61 H 0.2779 0.0070 0.0508 0.1015 1.0000 Uiso . . . . . . H71 H 0.2380 0.0815 0.1045 0.1010 1.0000 Uiso . . . . . . H81 H 0.3562 0.1536 0.1211 0.1007 1.0000 Uiso . . . . . . H101 H 0.7071 0.2318 0.0377 0.1300 1.0000 Uiso . . . . . . H111 H 0.6962 0.3095 -0.0180 0.1643 1.0000 Uiso . . . . . . H121 H 0.5414 0.3448 -0.0429 0.1079 1.0000 Uiso . . . . . . H131 H 0.3990 0.3143 -0.0027 0.0987 1.0000 Uiso . . . . . . H141 H 0.4050 0.2383 0.0527 0.0744 1.0000 Uiso . . . . . . H161 H 0.4888 0.2456 0.2385 0.0578 1.0000 Uiso . . . . . . H171 H 0.3899 0.2494 0.3085 0.0706 1.0000 Uiso . . . . . . H181 H 0.3280 0.1638 0.3428 0.0793 1.0000 Uiso . . . . . . H191 H 0.3538 0.0764 0.3031 0.0719 1.0000 Uiso . . . . . . H201 H 0.4637 0.0703 0.2364 0.0594 1.0000 Uiso . . . . . . H231 H 0.7778 0.0784 0.3224 0.0845 1.0000 Uiso . . . . . . H241 H 0.7588 -0.0203 0.3075 0.0982 1.0000 Uiso . . . . . . H251 H 0.6792 -0.0528 0.2357 0.0912 1.0000 Uiso . . . . . . H271 H 0.6940 0.1896 0.2420 0.0768 1.0000 Uiso . . . . . . H272 H 0.7970 0.1754 0.2701 0.0768 1.0000 Uiso . . . . . . H273 H 0.6933 0.1786 0.2999 0.0768 1.0000 Uiso . . . . . . H281 H 0.5990 -0.0352 0.1634 0.0853 1.0000 Uiso . . . . . . H282 H 0.6379 0.0221 0.1359 0.0853 1.0000 Uiso . . . . . . H283 H 0.5312 0.0224 0.1633 0.0853 1.0000 Uiso . . . . . . H301 H 0.9021 0.1012 0.2393 0.0551 1.0000 Uiso . . . . . . H311 H 0.9925 0.1332 0.3069 0.0649 1.0000 Uiso . . . . . . H321 H 1.1521 0.1738 0.2970 0.0652 1.0000 Uiso . . . . . . H331 H 1.2169 0.1878 0.2186 0.0624 1.0000 Uiso . . . . . . H341 H 1.1298 0.1545 0.1505 0.0548 1.0000 Uiso . . . . . . H361 H 0.9957 -0.0049 0.1772 0.0676 1.0000 Uiso . . . . . . H371 H 1.0695 -0.0886 0.1437 0.0744 1.0000 Uiso . . . . . . H381 H 1.1243 -0.0892 0.0631 0.0692 1.0000 Uiso . . . . . . H391 H 1.1022 -0.0069 0.0140 0.0657 1.0000 Uiso . . . . . . H401 H 1.0199 0.0740 0.0459 0.0611 1.0000 Uiso . . . . . . H411 H 0.9077 0.1978 0.4477 0.2033 0.5064 Uiso . . . . . . H412 H 0.8201 0.1601 0.4724 0.2033 0.5064 Uiso . . . . . . H421 H 0.7183 0.4385 0.4913 0.2624 0.4500 Uiso . . . . . . H422 H 0.6670 0.4796 0.4510 0.2624 0.4500 Uiso . . . . . . H431 H 0.5503 0.2940 0.4363 0.2147 0.2795 Uiso . . . . . . H432 H 0.5332 0.3082 0.3795 0.2147 0.2795 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0309(5) 0.0299(5) 0.0495(6) -0.0018(4) 0.0001(4) 0.0015(4) Br1 0.0454(4) 0.0574(5) 0.0520(5) -0.0101(4) 0.0021(4) 0.0075(4) Br2 0.0383(4) 0.0353(4) 0.0828(6) -0.0100(4) 0.0077(4) -0.0080(3) P1 0.0307(9) 0.0343(10) 0.0546(13) -0.0006(9) -0.0002(8) 0.0023(8) N1 0.026(3) 0.027(3) 0.052(4) -0.002(3) 0.001(2) -0.003(2) C1 0.027(4) 0.038(4) 0.076(6) 0.002(4) 0.004(3) 0.002(3) C2 0.031(4) 0.024(3) 0.055(5) -0.001(3) -0.006(3) -0.001(3) C3 0.048(2) 0.078(3) 0.125(4) -0.040(3) 0.018(2) -0.019(2) C4 0.049(2) 0.079(3) 0.126(4) -0.041(3) 0.019(2) -0.019(2) C5 0.049(2) 0.079(3) 0.126(4) -0.041(3) 0.019(2) -0.019(2) C6 0.049(2) 0.079(3) 0.126(4) -0.041(3) 0.018(2) -0.019(2) C7 0.048(2) 0.079(3) 0.126(4) -0.040(3) 0.019(2) -0.019(2) C8 0.048(2) 0.078(3) 0.125(4) -0.040(3) 0.019(2) -0.019(2) C9 0.055(5) 0.044(4) 0.050(5) 0.001(4) 0.000(4) 0.013(4) C10 0.065(7) 0.113(9) 0.148(11) 0.087(9) 0.006(7) 0.006(6) C11 0.101(10) 0.116(11) 0.194(17) 0.094(12) 0.028(10) 0.011(9) C12 0.105(9) 0.061(7) 0.104(9) 0.035(6) 0.021(7) 0.024(6) C13 0.092(8) 0.101(8) 0.054(6) 0.004(6) -0.001(6) 0.057(7) C14 0.055(5) 0.080(6) 0.051(5) 0.017(5) 0.005(4) 0.019(5) C15 0.032(4) 0.037(4) 0.048(5) 0.000(3) -0.001(3) -0.003(3) C16 0.051(4) 0.029(4) 0.064(6) -0.006(4) 0.014(4) -0.002(3) C17 0.061(5) 0.057(6) 0.059(6) -0.012(5) 0.004(4) 0.018(4) C18 0.059(5) 0.082(7) 0.057(6) 0.001(6) 0.012(5) 0.014(5) C19 0.048(5) 0.059(6) 0.073(6) 0.017(5) 0.004(4) -0.001(4) C20 0.040(4) 0.045(5) 0.064(5) 0.013(4) 0.011(4) 0.000(3) C21 0.040(4) 0.038(4) 0.048(5) 0.006(4) 0.006(3) 0.006(3) C22 0.040(4) 0.072(6) 0.054(5) 0.005(4) 0.001(4) -0.001(4) C23 0.042(5) 0.113(9) 0.056(6) 0.020(6) 0.002(4) 0.003(5) C24 0.065(6) 0.084(8) 0.096(9) 0.050(7) 0.004(6) 0.015(6) C25 0.067(6) 0.055(6) 0.106(9) 0.023(6) 0.014(6) 0.018(5) C26 0.055(5) 0.042(5) 0.079(7) 0.010(5) 0.012(5) 0.001(4) C27 0.057(5) 0.079(7) 0.056(6) -0.015(5) -0.005(4) -0.005(5) C28 0.084(7) 0.040(5) 0.089(8) -0.001(5) 0.009(6) 0.000(5) O1 0.036(3) 0.040(3) 0.056(3) 0.007(2) 0.003(2) 0.006(2) P2 0.0349(10) 0.0364(10) 0.0504(12) 0.0030(10) 0.0009(8) 0.0041(8) C29 0.036(4) 0.022(4) 0.055(5) 0.010(3) 0.000(3) 0.012(3) C30 0.045(4) 0.037(4) 0.055(6) 0.003(4) 0.001(4) -0.002(3) C31 0.058(5) 0.052(5) 0.052(6) -0.004(4) 0.002(4) 0.011(4) C32 0.064(6) 0.049(5) 0.050(6) -0.010(4) -0.013(4) 0.006(4) C33 0.043(4) 0.037(4) 0.075(7) 0.003(4) -0.013(4) -0.004(4) C34 0.037(4) 0.031(4) 0.069(6) 0.006(4) 0.005(4) 0.001(3) C35 0.035(4) 0.043(5) 0.047(5) 0.007(4) 0.001(3) 0.000(3) C36 0.062(5) 0.052(5) 0.055(5) -0.008(4) 0.003(4) 0.008(4) C37 0.070(6) 0.039(5) 0.077(7) -0.012(4) -0.006(5) 0.012(4) C38 0.048(5) 0.050(5) 0.075(7) -0.026(5) -0.007(4) 0.003(4) C39 0.050(5) 0.067(6) 0.048(5) -0.013(5) -0.007(4) 0.018(4) C40 0.039(4) 0.069(6) 0.044(5) 0.012(4) 0.001(4) 0.011(4) C41 0.156(6) 0.267(10) 0.085(4) -0.002(5) -0.009(4) -0.059(6) Cl1 0.154(6) 0.267(10) 0.084(4) -0.005(5) -0.010(4) -0.060(6) Cl2 0.160(6) 0.267(10) 0.086(4) 0.001(5) -0.008(4) -0.058(6) C42 0.323(17) 0.151(9) 0.181(11) 0.011(7) 0.003(9) 0.063(8) Cl3 0.323(17) 0.149(9) 0.179(11) 0.010(7) 0.003(9) 0.063(8) Cl4 0.324(17) 0.153(9) 0.183(11) 0.012(7) 0.003(9) 0.062(8) C43 0.237(18) 0.176(14) 0.124(10) -0.011(9) 0.031(10) -0.070(12) Cl5 0.236(18) 0.175(14) 0.123(10) -0.011(9) 0.030(10) -0.070(12) Cl6 0.237(18) 0.177(14) 0.126(11) -0.011(9) 0.031(10) -0.070(12) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . Br1 . 2.4736(13) yes Ni1 . Br2 . 2.4634(12) yes Ni1 . P1 . 2.329(2) yes Ni1 . N1 . 2.111(6) yes Ni1 . O1 . 2.041(5) yes Ni1 . P2 . 3.112(2) yes P1 . C1 . 1.824(9) yes P1 . C3 . 1.839(6) yes P1 . C9 . 1.816(8) yes N1 . C2 . 1.295(8) yes N1 . C21 . 1.439(9) yes C1 . C2 . 1.518(11) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C15 . 1.483(10) yes C3 . C4 . 1.371(7) yes C3 . C8 . 1.373(7) yes C4 . C5 . 1.366(7) yes C4 . H41 . 1.000 no C5 . C6 . 1.362(7) yes C5 . H51 . 1.000 no C6 . C7 . 1.360(7) yes C6 . H61 . 1.000 no C7 . C8 . 1.375(7) yes C7 . H71 . 1.000 no C8 . H81 . 1.000 no C9 . C10 . 1.368(13) yes C9 . C14 . 1.390(11) yes C10 . C11 . 1.406(15) yes C10 . H101 . 1.000 no C11 . C12 . 1.356(18) yes C11 . H111 . 1.000 no C12 . C13 . 1.341(15) yes C12 . H121 . 1.000 no C13 . C14 . 1.378(14) yes C13 . H131 . 1.000 no C14 . H141 . 1.000 no C15 . C16 . 1.387(10) yes C15 . C20 . 1.382(10) yes C16 . C17 . 1.371(12) yes C16 . H161 . 1.000 no C17 . C18 . 1.373(13) yes C17 . H171 . 1.000 no C18 . C19 . 1.360(13) yes C18 . H181 . 1.000 no C19 . C20 . 1.385(12) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.389(11) yes C21 . C26 . 1.401(11) yes C22 . C23 . 1.377(13) yes C22 . C27 . 1.498(13) yes C23 . C24 . 1.376(16) yes C23 . H231 . 1.000 no C24 . C25 . 1.397(17) yes C24 . H241 . 1.000 no C25 . C26 . 1.350(13) yes C25 . H251 . 1.000 no C26 . C28 . 1.521(14) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C27 . H273 . 1.000 no C28 . H281 . 1.000 no C28 . H282 . 1.000 no C28 . H283 . 1.000 no O1 . P2 . 1.498(5) yes P2 . C29 . 1.791(8) yes P2 . C35 . 1.799(8) yes P2 . H1 . 1.32(10) no C29 . C30 . 1.412(11) yes C29 . C34 . 1.386(10) yes C30 . C31 . 1.373(12) yes C30 . H301 . 1.000 no C31 . C32 . 1.378(13) yes C31 . H311 . 1.000 no C32 . C33 . 1.378(12) yes C32 . H321 . 1.000 no C33 . C34 . 1.375(12) yes C33 . H331 . 1.000 no C34 . H341 . 1.000 no C35 . C36 . 1.393(11) yes C35 . C40 . 1.362(11) yes C36 . C37 . 1.391(12) yes C36 . H361 . 1.000 no C37 . C38 . 1.370(13) yes C37 . H371 . 1.000 no C38 . C39 . 1.378(13) yes C38 . H381 . 1.000 no C39 . C40 . 1.379(11) yes C39 . H391 . 1.000 no C40 . H401 . 1.000 no C41 . Cl1 . 1.794(9) yes C41 . Cl2 . 1.794(9) yes C41 . H411 . 1.000 no C41 . H412 . 1.000 no Cl2 . Cl6 . 1.74(3) yes C42 . Cl3 . 1.756(10) yes C42 . Cl4 . 1.759(10) yes C42 . H421 . 1.001 no C42 . H422 . 0.999 no Cl3 . Cl4 . 2.479(18) yes Cl4 . Cl5 . 1.35(2) yes C43 . Cl5 . 1.771(10) yes C43 . Cl6 . 1.781(10) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no Cl5 . Cl6 . 2.609(18) 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 Br1 . Ni1 . Br2 . 113.38(5) yes Br1 . Ni1 . P1 . 95.27(6) yes Br2 . Ni1 . P1 . 93.56(6) yes Br1 . Ni1 . N1 . 150.44(15) yes Br2 . Ni1 . N1 . 96.04(15) yes P1 . Ni1 . N1 . 79.34(16) yes Br1 . Ni1 . O1 . 89.86(15) yes Br2 . Ni1 . O1 . 92.44(14) yes P1 . Ni1 . O1 . 169.84(15) yes N1 . Ni1 . O1 . 91.9(2) yes Br1 . Ni1 . P2 . 77.73(5) yes Br2 . Ni1 . P2 . 78.65(5) yes P1 . Ni1 . P2 . 166.16(7) yes N1 . Ni1 . P2 . 112.61(16) yes O1 . Ni1 . P2 . 24.00(14) yes Ni1 . P1 . C1 . 96.3(2) yes Ni1 . P1 . C3 . 116.7(4) yes C1 . P1 . C3 . 103.5(4) yes Ni1 . P1 . C9 . 123.4(3) yes C1 . P1 . C9 . 106.3(4) yes C3 . P1 . C9 . 107.5(5) yes Ni1 . N1 . C2 . 120.8(5) yes Ni1 . N1 . C21 . 117.8(4) yes C2 . N1 . C21 . 121.3(6) yes P1 . C1 . C2 . 107.6(5) yes P1 . C1 . H11 . 109.952 no C2 . C1 . H11 . 109.948 no P1 . C1 . H12 . 109.953 no C2 . C1 . H12 . 109.945 no H11 . C1 . H12 . 109.465 no C1 . C2 . N1 . 117.5(7) yes C1 . C2 . C15 . 115.9(6) yes N1 . C2 . C15 . 126.6(7) yes P1 . C3 . C4 . 117.3(5) yes P1 . C3 . C8 . 123.6(5) yes C4 . C3 . C8 . 118.9(5) yes C3 . C4 . C5 . 120.3(5) yes C3 . C4 . H41 . 119.865 no C5 . C4 . H41 . 119.873 no C4 . C5 . C6 . 120.2(5) yes C4 . C5 . H51 . 119.918 no C6 . C5 . H51 . 119.929 no C5 . C6 . C7 . 119.8(5) yes C5 . C6 . H61 . 120.083 no C7 . C6 . H61 . 120.085 no C6 . C7 . C8 . 119.8(5) yes C6 . C7 . H71 . 120.091 no C8 . C7 . H71 . 120.098 no C7 . C8 . C3 . 120.4(5) yes C7 . C8 . H81 . 119.811 no C3 . C8 . H81 . 119.820 no P1 . C9 . C10 . 119.5(7) yes P1 . C9 . C14 . 122.2(7) yes C10 . C9 . C14 . 118.1(8) yes C9 . C10 . C11 . 119.4(10) yes C9 . C10 . H101 . 120.294 no C11 . C10 . H101 . 120.295 no C10 . C11 . C12 . 121.4(12) yes C10 . C11 . H111 . 119.284 no C12 . C11 . H111 . 119.291 no C11 . C12 . C13 . 118.7(10) yes C11 . C12 . H121 . 120.654 no C13 . C12 . H121 . 120.651 no C12 . C13 . C14 . 121.5(9) yes C12 . C13 . H131 . 119.231 no C14 . C13 . H131 . 119.240 no C9 . C14 . C13 . 120.5(9) yes C9 . C14 . H141 . 119.737 no C13 . C14 . H141 . 119.734 no C2 . C15 . C16 . 118.5(6) yes C2 . C15 . C20 . 122.2(7) yes C16 . C15 . C20 . 119.2(7) yes C15 . C16 . C17 . 120.8(7) yes C15 . C16 . H161 . 119.606 no C17 . C16 . H161 . 119.604 no C16 . C17 . C18 . 119.8(8) yes C16 . C17 . H171 . 120.100 no C18 . C17 . H171 . 120.131 no C17 . C18 . C19 . 119.7(8) yes C17 . C18 . H181 . 120.132 no C19 . C18 . H181 . 120.137 no C18 . C19 . C20 . 121.4(8) yes C18 . C19 . H191 . 119.323 no C20 . C19 . H191 . 119.310 no C19 . C20 . C15 . 118.9(8) yes C19 . C20 . H201 . 120.543 no C15 . C20 . H201 . 120.539 no N1 . C21 . C22 . 120.7(7) yes N1 . C21 . C26 . 118.2(7) yes C22 . C21 . C26 . 120.9(7) yes C21 . C22 . C23 . 118.5(9) yes C21 . C22 . C27 . 121.1(8) yes C23 . C22 . C27 . 120.4(8) yes C22 . C23 . C24 . 120.6(10) yes C22 . C23 . H231 . 119.700 no C24 . C23 . H231 . 119.716 no C23 . C24 . C25 . 120.5(9) yes C23 . C24 . H241 . 119.739 no C25 . C24 . H241 . 119.766 no C24 . C25 . C26 . 119.7(9) yes C24 . C25 . H251 . 120.144 no C26 . C25 . H251 . 120.156 no C21 . C26 . C25 . 119.9(9) yes C21 . C26 . C28 . 119.6(8) yes C25 . C26 . C28 . 120.6(9) yes C22 . C27 . H271 . 109.464 no C22 . C27 . H272 . 109.471 no H271 . C27 . H272 . 109.474 no C22 . C27 . H273 . 109.464 no H271 . C27 . H273 . 109.473 no H272 . C27 . H273 . 109.482 no C26 . C28 . H281 . 109.467 no C26 . C28 . H282 . 109.466 no H281 . C28 . H282 . 109.466 no C26 . C28 . H283 . 109.477 no H281 . C28 . H283 . 109.478 no H282 . C28 . H283 . 109.473 no Ni1 . O1 . P2 . 122.4(3) yes Ni1 . P2 . O1 . 33.64(19) yes Ni1 . P2 . C29 . 124.3(2) yes O1 . P2 . C29 . 111.2(3) yes Ni1 . P2 . C35 . 125.0(2) yes O1 . P2 . C35 . 113.7(3) yes C29 . P2 . C35 . 107.4(3) yes Ni1 . P2 . H1 . 82(4) no O1 . P2 . H1 . 116(4) no C29 . P2 . H1 . 106(4) no C35 . P2 . H1 . 102(4) no P2 . C29 . C30 . 119.2(6) yes P2 . C29 . C34 . 122.4(6) yes C30 . C29 . C34 . 118.3(7) yes C29 . C30 . C31 . 120.3(7) yes C29 . C30 . H301 . 119.855 no C31 . C30 . H301 . 119.857 no C30 . C31 . C32 . 120.3(8) yes C30 . C31 . H311 . 119.833 no C32 . C31 . H311 . 119.822 no C31 . C32 . C33 . 119.8(8) yes C31 . C32 . H321 . 120.111 no C33 . C32 . H321 . 120.092 no C32 . C33 . C34 . 120.6(7) yes C32 . C33 . H331 . 119.709 no C34 . C33 . H331 . 119.700 no C29 . C34 . C33 . 120.6(8) yes C29 . C34 . H341 . 119.723 no C33 . C34 . H341 . 119.717 no P2 . C35 . C36 . 119.1(6) yes P2 . C35 . C40 . 121.8(6) yes C36 . C35 . C40 . 119.1(7) yes C35 . C36 . C37 . 119.2(8) yes C35 . C36 . H361 . 120.383 no C37 . C36 . H361 . 120.373 no C36 . C37 . C38 . 120.5(9) yes C36 . C37 . H371 . 119.753 no C38 . C37 . H371 . 119.736 no C37 . C38 . C39 . 120.1(8) yes C37 . C38 . H381 . 119.936 no C39 . C38 . H381 . 119.930 no C38 . C39 . C40 . 119.1(8) yes C38 . C39 . H391 . 120.465 no C40 . C39 . H391 . 120.463 no C39 . C40 . C35 . 121.8(8) yes C39 . C40 . H401 . 119.089 no C35 . C40 . H401 . 119.093 no Cl1 . C41 . Cl2 . 99.9(7) yes Cl1 . C41 . H411 . 111.808 no Cl2 . C41 . H411 . 111.812 no Cl1 . C41 . H412 . 111.800 no Cl2 . C41 . H412 . 111.805 no H411 . C41 . H412 . 109.469 no C41 . Cl2 . Cl6 . 152.6(12) yes Cl3 . C42 . Cl4 . 89.7(8) yes Cl3 . C42 . H421 . 114.096 no Cl4 . C42 . H421 . 114.110 no Cl3 . C42 . H422 . 114.228 no Cl4 . C42 . H422 . 114.244 no H421 . C42 . H422 . 109.453 no C42 . Cl3 . Cl4 . 45.2(5) yes C42 . Cl4 . Cl3 . 45.1(5) yes C42 . Cl4 . Cl5 . 127.5(15) yes Cl3 . Cl4 . Cl5 . 84.0(12) yes Cl5 . C43 . Cl6 . 94.6(8) yes Cl5 . C43 . H431 . 113.066 no Cl6 . C43 . H431 . 113.058 no Cl5 . C43 . H432 . 113.081 no Cl6 . C43 . H432 . 113.052 no H431 . C43 . H432 . 109.460 no C43 . Cl5 . Cl4 . 94.6(18) yes C43 . Cl5 . Cl6 . 42.9(5) yes Cl4 . Cl5 . Cl6 . 134.8(15) yes C43 . Cl6 . Cl2 . 137.9(19) yes C43 . Cl6 . Cl5 . 42.6(5) yes Cl2 . Cl6 . Cl5 . 100.8(12) yes #===END ####################### ## denoted 6 in text ## ####################### data_6 _database_code_depnum_ccdc_archive 'CCDC 236198' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 9.9766(2) _cell_angle_alpha 90 _cell_length_b 13.5588(3) _cell_angle_beta 90 _cell_length_c 21.8426(7) _cell_angle_gamma 90 _cell_volume 2954.66(13) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 c n ' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y,-z x,-y+1/2,z+1/2 x+1/2,y+1/2,-z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration unk 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_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Br ' -0.3740 2.4560 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 International_Tables_Vol_IV_Table_2.2B '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_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C32 H34 Br2 N1 P1 Pd1 ' _chemical_formula_moiety ' C32 H34 Br2 N1 P1 Pd1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 729.81 _cell_measurement_reflns_used 3507 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 3.409 _diffrn_measurement_device_type ; Nonius Kappa CCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.71 # Sheldrick geometric definitions 0.51 0.71 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 6526 _reflns_number_total 6291 _diffrn_reflns_av_R_equivalents 0.00 # Number of reflections with Friedels Law is 6291 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 3385 _diffrn_reflns_theta_min 2.395 _diffrn_reflns_theta_max 27.531 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 21.199 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -0.91 _refine_diff_density_max 1.10 _refine_ls_number_reflns 4082 _refine_ls_number_restraints 43 _refine_ls_number_parameters 335 #_refine_ls_R_factor_ref 0.0394 _refine_ls_wR_factor_ref 0.0344 _refine_ls_goodness_of_fit_ref 1.1158 #_reflns_number_all 6275 _refine_ls_R_factor_all 0.0779 _refine_ls_wR_factor_all 0.0664 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4082 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_gt 0.0344 _refine_ls_shift/su_max 0.000561 _refine_ls_abs_structure_Flack 0.15(2) _refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs' _refine_ls_structure_factor_coef F _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: 0.253 0.941E-01 0.129 0.732E-01 0.551E-01 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. 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 trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Pd1 Pd -0.04860(10) 0.29143(4) 0.20027(2) 0.0191 1.0000 Uani . . . . 3 . Br1 Br -0.23062(16) 0.20392(6) 0.25743(3) 0.0310 1.0000 Uani . . . . 3 . Br2 Br -0.16572(17) 0.27364(5) 0.10341(3) 0.0295 1.0000 Uani . . . . 3 . N1 N 0.0798(5) 0.3028(4) 0.2758(2) 0.0176 1.0000 Uani . . . . 3 . P1 P 0.11136(19) 0.38260(13) 0.15844(8) 0.0197 1.0000 Uani . . . . 3 . C1 C 0.1638(7) 0.4487(5) 0.2278(3) 0.0236 1.0000 Uani . . . . 3 . C2 C 0.1648(7) 0.3745(5) 0.2789(3) 0.0212 1.0000 Uani . . . . 3 . C3 C 0.0750(6) 0.2303(5) 0.3236(3) 0.0204 1.0000 Uani . . . . 3 . C4 C 0.0195(7) 0.2557(6) 0.3807(3) 0.0286 1.0000 Uani . . . . 3 . C5 C 0.0129(8) 0.1831(6) 0.4268(4) 0.0361 1.0000 Uani . . . . 3 . C6 C 0.0569(9) 0.0893(7) 0.4143(4) 0.0444 1.0000 Uani . . . . 3 . C7 C 0.1099(8) 0.0630(6) 0.3584(4) 0.0356 1.0000 Uani . . . . 3 . C8 C 0.1196(7) 0.1340(5) 0.3115(3) 0.0268 1.0000 Uani . . . . 3 . C9 C 0.1765(9) 0.1044(6) 0.2499(4) 0.0363 1.0000 Uani . . . . 3 . C10 C 0.0897(12) 0.0313(9) 0.2170(6) 0.0829 1.0000 Uani . . . . 3 . C11 C 0.3205(8) 0.0613(6) 0.2543(4) 0.0404 1.0000 Uani . . . . 3 . C12 C -0.0342(9) 0.3579(6) 0.3961(3) 0.0343 1.0000 Uani . . . . 3 . C13 C 0.0335(10) 0.3993(7) 0.4549(4) 0.0487 1.0000 Uani . . . . 3 . C14 C -0.1866(9) 0.3569(7) 0.4049(4) 0.0476 1.0000 Uani . . . . 3 . C15 C 0.2671(7) 0.3890(5) 0.3275(3) 0.0205 1.0000 Uani . . . . 3 . C16 C 0.2792(8) 0.4817(5) 0.3550(3) 0.0263 1.0000 Uani . . . . 3 . C17 C 0.3705(8) 0.4971(6) 0.4008(4) 0.0363 1.0000 Uani . . . . 3 . C18 C 0.4564(10) 0.4219(6) 0.4179(3) 0.0354 1.0000 Uani . . . . 3 . C19 C 0.4515(9) 0.3318(5) 0.3889(4) 0.0369 1.0000 Uani . . . . 3 . C20 C 0.3526(7) 0.3137(5) 0.3455(4) 0.0333 1.0000 Uani . . . . 3 . C21 C 0.0866(6) 0.4759(5) 0.1000(3) 0.0201 1.0000 Uani . . . . 3 . C22 C -0.0408(9) 0.5143(5) 0.0878(3) 0.0281 1.0000 Uani . . . . 3 . C23 C -0.0540(10) 0.5895(5) 0.0462(3) 0.0329 1.0000 Uani . . . . 3 . C24 C 0.0563(9) 0.6272(6) 0.0156(4) 0.0344 1.0000 Uani . . . . 3 . C25 C 0.1823(9) 0.5888(6) 0.0282(4) 0.0368 1.0000 Uani . . . . 3 . C26 C 0.1969(8) 0.5144(6) 0.0697(4) 0.0312 1.0000 Uani . . . . 3 . C27 C 0.2528(7) 0.3072(6) 0.1344(3) 0.0327 1.0000 Uani . U . . 3 . C28 C 0.3750(7) 0.3127(6) 0.1625(4) 0.0340 1.0000 Uani . U . . 3 . C29 C 0.4789(7) 0.2484(6) 0.1458(4) 0.0358 1.0000 Uani . U . . 3 . C30 C 0.4584(9) 0.1828(5) 0.0999(3) 0.0359 1.0000 Uani . U . . 3 . C31 C 0.3357(8) 0.1783(6) 0.0698(4) 0.0359 1.0000 Uani . U . . 3 . C32 C 0.2329(7) 0.2413(6) 0.0877(4) 0.0344 1.0000 Uani . U . . 3 . H11 H 0.0991 0.5030 0.2372 0.0283 1.0000 Uiso . . . . 3 . H12 H 0.2555 0.4771 0.2221 0.0283 1.0000 Uiso . . . . 3 . H51 H -0.0236 0.1997 0.4682 0.0433 1.0000 Uiso . . . . 3 . H61 H 0.0503 0.0380 0.4471 0.0532 1.0000 Uiso . . . . 3 . H71 H 0.1414 -0.0061 0.3511 0.0427 1.0000 Uiso . . . . 3 . H91 H 0.1795 0.1674 0.2261 0.0436 1.0000 Uiso . . . . 3 . H101 H 0.1315 0.0142 0.1768 0.0996 1.0000 Uiso . . . . 3 . H102 H 0.0806 -0.0297 0.2424 0.0996 1.0000 Uiso . . . . 3 . H103 H -0.0010 0.0606 0.2099 0.0996 1.0000 Uiso . . . . 3 . H111 H 0.3528 0.0431 0.2125 0.0484 1.0000 Uiso . . . . 3 . H112 H 0.3819 0.1118 0.2725 0.0484 1.0000 Uiso . . . . 3 . H113 H 0.3195 0.0013 0.2809 0.0484 1.0000 Uiso . . . . 3 . H121 H -0.0122 0.4016 0.3606 0.0412 1.0000 Uiso . . . . 3 . H131 H -0.0033 0.4663 0.4640 0.0584 1.0000 Uiso . . . . 3 . H132 H 0.0147 0.3542 0.4901 0.0584 1.0000 Uiso . . . . 3 . H133 H 0.1325 0.4039 0.4483 0.0584 1.0000 Uiso . . . . 3 . H141 H -0.2183 0.4249 0.4149 0.0571 1.0000 Uiso . . . . 3 . H142 H -0.2102 0.3112 0.4392 0.0571 1.0000 Uiso . . . . 3 . H143 H -0.2306 0.3338 0.3663 0.0571 1.0000 Uiso . . . . 3 . H161 H 0.2206 0.5372 0.3411 0.0316 1.0000 Uiso . . . . 3 . H171 H 0.3750 0.5625 0.4219 0.0436 1.0000 Uiso . . . . 3 . H181 H 0.5226 0.4330 0.4515 0.0425 1.0000 Uiso . . . . 3 . H191 H 0.5187 0.2796 0.3991 0.0442 1.0000 Uiso . . . . 3 . H201 H 0.3432 0.2464 0.3272 0.0400 1.0000 Uiso . . . . 3 . H221 H -0.1214 0.4873 0.1092 0.0338 1.0000 Uiso . . . . 3 . H231 H -0.1449 0.6175 0.0378 0.0394 1.0000 Uiso . . . . 3 . H241 H 0.0453 0.6814 -0.0150 0.0412 1.0000 Uiso . . . . 3 . H251 H 0.2629 0.6158 0.0067 0.0441 1.0000 Uiso . . . . 3 . H261 H 0.2882 0.4872 0.0783 0.0374 1.0000 Uiso . . . . 3 . H281 H 0.3905 0.3630 0.1952 0.0408 1.0000 Uiso . . . . 3 . H291 H 0.5671 0.2509 0.1675 0.0429 1.0000 Uiso . . . . 3 . H301 H 0.5324 0.1372 0.0875 0.0430 1.0000 Uiso . . . . 3 . H311 H 0.3215 0.1302 0.0357 0.0431 1.0000 Uiso . . . . 3 . H321 H 0.1442 0.2386 0.0665 0.0413 1.0000 Uiso . . . . 3 . 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 0.0172(2) 0.0205(2) 0.0196(2) 0.0023(2) -0.0024(2) -0.0017(3) Br1 0.0257(4) 0.0355(4) 0.0320(4) 0.0075(4) -0.0011(3) -0.0104(4) Br2 0.0277(4) 0.0341(4) 0.0266(3) 0.0042(3) -0.0086(3) -0.0072(3) N1 0.018(3) 0.012(3) 0.022(3) 0.002(2) 0.002(2) 0.002(2) P1 0.0180(9) 0.0229(10) 0.0182(9) 0.0017(7) -0.0011(7) -0.0018(7) C1 0.027(4) 0.026(4) 0.018(4) 0.007(3) -0.001(3) -0.007(3) C2 0.018(4) 0.023(4) 0.022(4) -0.005(3) 0.006(3) 0.005(3) C3 0.016(3) 0.022(4) 0.023(3) 0.000(3) -0.003(3) -0.009(3) C4 0.021(4) 0.039(5) 0.026(4) 0.011(3) -0.003(3) -0.007(3) C5 0.027(4) 0.045(6) 0.036(5) 0.017(4) 0.003(4) -0.003(4) C6 0.043(5) 0.038(5) 0.053(6) 0.027(4) 0.009(5) -0.003(4) C7 0.018(4) 0.029(4) 0.060(6) 0.015(4) -0.014(4) 0.005(3) C8 0.027(4) 0.029(4) 0.024(4) 0.002(3) 0.004(3) -0.006(3) C9 0.050(5) 0.025(4) 0.034(5) -0.008(4) -0.011(4) 0.006(4) C10 0.055(7) 0.095(10) 0.098(10) -0.062(8) -0.019(7) 0.009(6) C11 0.027(4) 0.054(5) 0.040(5) -0.005(4) -0.002(4) -0.001(4) C12 0.027(4) 0.047(5) 0.028(4) 0.006(3) 0.003(4) 0.006(4) C13 0.062(7) 0.053(6) 0.031(5) -0.003(4) 0.007(4) -0.002(5) C14 0.044(6) 0.059(6) 0.040(5) -0.004(4) 0.004(4) 0.007(4) C15 0.021(3) 0.019(4) 0.022(3) 0.000(3) 0.007(3) -0.004(3) C16 0.030(4) 0.030(4) 0.018(4) -0.002(3) -0.006(3) 0.001(3) C17 0.033(5) 0.041(5) 0.035(5) -0.008(4) -0.003(4) -0.007(4) C18 0.040(5) 0.047(5) 0.019(3) 0.004(3) -0.006(5) -0.004(5) C19 0.027(4) 0.031(4) 0.052(5) 0.011(3) -0.014(5) -0.003(4) C20 0.024(4) 0.024(4) 0.052(5) 0.009(3) -0.005(4) -0.005(3) C21 0.019(4) 0.021(4) 0.021(4) 0.003(3) -0.003(3) -0.006(3) C22 0.031(4) 0.022(4) 0.031(4) 0.002(3) 0.003(4) 0.006(4) C23 0.037(4) 0.029(4) 0.033(4) 0.000(3) -0.003(4) 0.012(4) C24 0.053(5) 0.025(4) 0.026(4) 0.005(3) -0.003(4) -0.001(4) C25 0.044(5) 0.035(5) 0.031(5) -0.002(4) -0.001(4) -0.015(4) C26 0.031(5) 0.036(5) 0.027(4) 0.007(3) -0.005(3) -0.002(3) C27 0.027(2) 0.039(2) 0.033(2) -0.0018(18) 0.0002(19) 0.0028(18) C28 0.027(2) 0.040(2) 0.035(2) -0.0017(18) 0.0000(19) 0.0034(18) C29 0.028(2) 0.042(2) 0.038(2) 0.0007(17) 0.001(2) 0.0049(19) C30 0.0277(19) 0.041(2) 0.039(2) -0.0006(17) 0.003(2) 0.0061(19) C31 0.029(2) 0.041(2) 0.038(2) -0.0042(18) 0.002(2) 0.0038(18) C32 0.028(2) 0.040(2) 0.035(2) -0.0041(18) 0.0001(19) 0.0025(18) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . Br1 . 2.5029(11) yes Pd1 . Br2 . 2.4289(10) yes Pd1 . N1 . 2.095(5) yes Pd1 . P1 . 2.2158(18) yes N1 . C2 . 1.293(9) yes N1 . C3 . 1.433(8) yes P1 . C1 . 1.837(7) yes P1 . C21 . 1.814(7) yes P1 . C27 . 1.820(8) yes C1 . C2 . 1.502(10) yes C1 . H11 . 1.000 no C1 . H12 . 1.000 no C2 . C15 . 1.486(10) yes C3 . C4 . 1.408(10) yes C3 . C8 . 1.405(10) yes C4 . C5 . 1.410(10) yes C4 . C12 . 1.522(11) yes C5 . C6 . 1.373(12) yes C5 . H51 . 1.000 no C6 . C7 . 1.378(12) yes C6 . H61 . 1.000 no C7 . C8 . 1.410(10) yes C7 . H71 . 1.000 no C8 . C9 . 1.513(11) yes C9 . C10 . 1.500(13) yes C9 . C11 . 1.555(11) yes C9 . H91 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . C13 . 1.555(12) yes C12 . C14 . 1.532(12) yes C12 . H121 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no C14 . H141 . 1.000 no C14 . H142 . 1.000 no C14 . H143 . 1.000 no C15 . C16 . 1.398(9) yes C15 . C20 . 1.387(10) yes C16 . C17 . 1.370(10) yes C16 . H161 . 1.000 no C17 . C18 . 1.383(12) yes C17 . H171 . 1.000 no C18 . C19 . 1.376(10) yes C18 . H181 . 1.000 no C19 . C20 . 1.390(11) yes C19 . H191 . 1.000 no C20 . H201 . 1.000 no C21 . C22 . 1.399(11) yes C21 . C26 . 1.386(10) yes C22 . C23 . 1.372(9) yes C22 . H221 . 1.000 no C23 . C24 . 1.386(12) yes C23 . H231 . 1.000 no C24 . C25 . 1.388(12) yes C24 . H241 . 1.000 no C25 . C26 . 1.364(11) yes C25 . H251 . 1.000 no C26 . H261 . 1.000 no C27 . C28 . 1.366(11) yes C27 . C32 . 1.370(10) yes C28 . C29 . 1.403(10) yes C28 . H281 . 1.000 no C29 . C30 . 1.356(10) yes C29 . H291 . 1.000 no C30 . C31 . 1.391(12) yes C30 . H301 . 1.000 no C31 . C32 . 1.392(11) yes C31 . H311 . 1.000 no C32 . H321 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . Pd1 . Br2 . 92.20(4) yes Br1 . Pd1 . N1 . 94.89(14) yes Br2 . Pd1 . N1 . 171.01(14) yes Br1 . Pd1 . P1 . 173.08(5) yes Br2 . Pd1 . P1 . 92.45(6) yes N1 . Pd1 . P1 . 81.00(15) yes Pd1 . N1 . C2 . 119.8(5) yes Pd1 . N1 . C3 . 120.2(4) yes C2 . N1 . C3 . 120.0(6) yes Pd1 . P1 . C1 . 97.9(2) yes Pd1 . P1 . C21 . 125.5(2) yes C1 . P1 . C21 . 106.2(3) yes Pd1 . P1 . C27 . 111.3(3) yes C1 . P1 . C27 . 106.9(3) yes C21 . P1 . C27 . 107.1(3) yes P1 . C1 . C2 . 106.7(5) yes P1 . C1 . H11 . 110.154 no C2 . C1 . H11 . 110.166 no P1 . C1 . H12 . 110.153 no C2 . C1 . H12 . 110.166 no H11 . C1 . H12 . 109.468 no C1 . C2 . N1 . 117.5(6) yes C1 . C2 . C15 . 116.6(6) yes N1 . C2 . C15 . 125.9(6) yes N1 . C3 . C4 . 119.4(6) yes N1 . C3 . C8 . 119.3(6) yes C4 . C3 . C8 . 121.2(6) yes C3 . C4 . C5 . 118.7(7) yes C3 . C4 . C12 . 123.8(6) yes C5 . C4 . C12 . 117.5(7) yes C4 . C5 . C6 . 119.4(8) yes C4 . C5 . H51 . 120.312 no C6 . C5 . H51 . 120.314 no C5 . C6 . C7 . 122.6(7) yes C5 . C6 . H61 . 118.695 no C7 . C6 . H61 . 118.710 no C6 . C7 . C8 . 119.6(7) yes C6 . C7 . H71 . 120.204 no C8 . C7 . H71 . 120.215 no C7 . C8 . C3 . 118.5(7) yes C7 . C8 . C9 . 119.3(7) yes C3 . C8 . C9 . 122.2(6) yes C8 . C9 . C10 . 112.6(8) yes C8 . C9 . C11 . 113.0(7) yes C10 . C9 . C11 . 108.3(7) yes C8 . C9 . H91 . 104.326 no C10 . C9 . H91 . 109.401 no C11 . C9 . H91 . 108.963 no C9 . C10 . H101 . 109.493 no C9 . C10 . H102 . 109.464 no H101 . C10 . H102 . 109.451 no C9 . C10 . H103 . 109.488 no H101 . C10 . H103 . 109.486 no H102 . C10 . H103 . 109.447 no C9 . C11 . H111 . 109.460 no C9 . C11 . H112 . 109.466 no H111 . C11 . H112 . 109.480 no C9 . C11 . H113 . 109.464 no H111 . C11 . H113 . 109.473 no H112 . C11 . H113 . 109.484 no C4 . C12 . C13 . 111.0(7) yes C4 . C12 . C14 . 111.6(7) yes C13 . C12 . C14 . 109.3(7) yes C4 . C12 . H121 . 106.907 no C13 . C12 . H121 . 109.341 no C14 . C12 . H121 . 108.668 no C12 . C13 . H131 . 109.464 no C12 . C13 . H132 . 109.454 no H131 . C13 . H132 . 109.476 no C12 . C13 . H133 . 109.468 no H131 . C13 . H133 . 109.491 no H132 . C13 . H133 . 109.474 no C12 . C14 . H141 . 109.477 no C12 . C14 . H142 . 109.463 no H141 . C14 . H142 . 109.477 no C12 . C14 . H143 . 109.469 no H141 . C14 . H143 . 109.481 no H142 . C14 . H143 . 109.459 no C2 . C15 . C16 . 119.0(6) yes C2 . C15 . C20 . 121.9(6) yes C16 . C15 . C20 . 119.2(7) yes C15 . C16 . C17 . 120.5(7) yes C15 . C16 . H161 . 119.729 no C17 . C16 . H161 . 119.723 no C16 . C17 . C18 . 119.7(7) yes C16 . C17 . H171 . 120.126 no C18 . C17 . H171 . 120.128 no C17 . C18 . C19 . 120.6(8) yes C17 . C18 . H181 . 119.701 no C19 . C18 . H181 . 119.719 no C18 . C19 . C20 . 119.7(7) yes C18 . C19 . H191 . 120.150 no C20 . C19 . H191 . 120.141 no C19 . C20 . C15 . 120.0(7) yes C19 . C20 . H201 . 120.029 no C15 . C20 . H201 . 120.016 no P1 . C21 . C22 . 121.1(5) yes P1 . C21 . C26 . 119.4(5) yes C22 . C21 . C26 . 119.3(6) yes C21 . C22 . C23 . 119.3(8) yes C21 . C22 . H221 . 120.329 no C23 . C22 . H221 . 120.327 no C22 . C23 . C24 . 121.2(8) yes C22 . C23 . H231 . 119.420 no C24 . C23 . H231 . 119.428 no C23 . C24 . C25 . 119.0(7) yes C23 . C24 . H241 . 120.468 no C25 . C24 . H241 . 120.488 no C24 . C25 . C26 . 120.4(8) yes C24 . C25 . H251 . 119.807 no C26 . C25 . H251 . 119.820 no C21 . C26 . C25 . 120.7(8) yes C21 . C26 . H261 . 119.628 no C25 . C26 . H261 . 119.634 no P1 . C27 . C28 . 122.2(6) yes P1 . C27 . C32 . 117.9(6) yes C28 . C27 . C32 . 119.9(7) yes C27 . C28 . C29 . 120.6(7) yes C27 . C28 . H281 . 119.691 no C29 . C28 . H281 . 119.715 no C28 . C29 . C30 . 119.2(8) yes C28 . C29 . H291 . 120.373 no C30 . C29 . H291 . 120.383 no C29 . C30 . C31 . 120.7(7) yes C29 . C30 . H301 . 119.631 no C31 . C30 . H301 . 119.632 no C30 . C31 . C32 . 119.3(7) yes C30 . C31 . H311 . 120.377 no C32 . C31 . H311 . 120.363 no C31 . C32 . C27 . 120.2(7) yes C31 . C32 . H321 . 119.904 no C27 . C32 . H321 . 119.904 no #===END ####################### ## denoted 7 in text ## ####################### data_7 _database_code_depnum_ccdc_archive 'CCDC 236199' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 10.4664(2) _cell_angle_alpha 90 _cell_length_b 16.3356(3) _cell_angle_beta 99.3449(9) _cell_length_c 16.3526(3) _cell_angle_gamma 90 _cell_volume 2758.78(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration unk 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'I ' -0.7260 1.8120 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Pd ' -1.1770 1.0070 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C28 H26 I2 N1 P1 Pd1 ' _chemical_formula_moiety ' C28 H26 I2 N1 P1 Pd1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 767.71 _cell_measurement_reflns_used 44207 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_meas 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 2.985 _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; COLLECT (Nonius BV, 1997) ; _computing_data_reduction ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.86 # Sheldrick geometric definitions 0.74 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 44207 _reflns_number_total 12405 _diffrn_reflns_av_R_equivalents 0.05 # Number of reflections with Friedels Law is 6501 # Number of reflections without Friedels Law is 12405 # Theoretical number of reflections is about 6322 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min -20 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -1.63 _refine_diff_density_max 1.77 _refine_ls_number_reflns 10511 _refine_ls_number_restraints 1 _refine_ls_number_parameters 595 #_refine_ls_R_factor_ref 0.0304 _refine_ls_wR_factor_ref 0.0333 _refine_ls_goodness_of_fit_ref 1.0700 #_reflns_number_all 12389 _refine_ls_R_factor_all 0.0408 _refine_ls_wR_factor_all 0.0346 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 10511 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_gt 0.0333 _refine_ls_shift/su_max 0.019763 _refine_ls_abs_structure_Flack 0.005(15) _refine_ls_abs_structure_details 'Flack, 5904 Friedel-pairs' _refine_ls_structure_factor_coef F _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: 2.15 -1.22 1.38 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _refine_special_details ; There is a small void located at ca. 0.75, 0.27, 0.27. Difference Fourier maps show no well-defined peaks in this region and consequently no attempt has been made to model solvent etc. in this region. ; ## -------------------REFERENCES ----------------------## _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, 1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. 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 trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Pd1 Pd 0.16836(4) 0.08639(4) 0.10975(2) 0.0227 1.0000 Uani . . . . . . I1 I 0.00995(5) 0.19123(4) 0.02391(3) 0.0445 1.0000 Uani . . . . . . I2 I 0.36258(4) 0.16563(4) 0.07064(2) 0.0356 1.0000 Uani . . . . . . P1 P 0.29165(14) 0.00145(9) 0.19551(8) 0.0243 1.0000 Uani . . . . . . N1 N 0.0223(4) 0.0087(3) 0.1401(3) 0.0243 1.0000 Uani . . . . . . C1 C 0.0418(5) -0.0360(3) 0.2054(3) 0.0247 1.0000 Uani . . . . . . C2 C 0.1709(6) -0.0290(4) 0.2602(3) 0.0294 1.0000 Uani . . . . . . C3 C -0.1001(5) 0.0060(4) 0.0845(4) 0.0313 1.0000 Uani . . . . . . C4 C -0.1011(7) -0.0371(4) 0.0080(4) 0.0393 1.0000 Uani . . . . . . C5 C -0.2192(9) -0.0441(6) -0.0444(5) 0.0589 1.0000 Uani . . . . . . C6 C -0.3222(10) -0.0050(7) -0.0277(6) 0.0751 1.0000 Uani . . . . . . C7 C -0.3225(8) 0.0404(6) 0.0430(7) 0.0701 1.0000 Uani . . . . . . C8 C -0.2059(7) 0.0469(4) 0.1050(5) 0.0449 1.0000 Uani . . . . . . C9 C 0.0159(8) -0.0751(4) -0.0132(4) 0.0478 1.0000 Uani . . . . . . C10 C -0.1983(9) 0.0948(5) 0.1821(7) 0.0680 1.0000 Uani . . . . . . C11 C -0.0543(5) -0.0944(3) 0.2320(3) 0.0260 1.0000 Uani . . . . . . C12 C -0.1343(6) -0.1435(4) 0.1774(4) 0.0349 1.0000 Uani . . . . . . C13 C -0.2220(6) -0.1951(4) 0.2074(4) 0.0407 1.0000 Uani . . . . . . C14 C -0.2283(6) -0.1982(4) 0.2917(5) 0.0418 1.0000 Uani . . . . . . C15 C -0.1475(6) -0.1513(4) 0.3459(4) 0.0359 1.0000 Uani . . . . . . C16 C -0.0596(5) -0.0975(4) 0.3177(3) 0.0308 1.0000 Uani . . . . . . C17 C 0.3373(5) -0.0918(3) 0.1482(3) 0.0295 1.0000 Uani . . . . . . C18 C 0.2857(10) -0.1662(4) 0.1621(7) 0.0693 1.0000 Uani . . . . . . C19 C 0.3200(11) -0.2359(5) 0.1210(9) 0.0887 1.0000 Uani . . . . . . C20 C 0.4022(9) -0.2307(5) 0.0654(6) 0.0592 1.0000 Uani . . . . . . C21 C 0.4533(13) -0.1558(6) 0.0504(7) 0.0888 1.0000 Uani . . . . . . C22 C 0.4204(11) -0.0866(5) 0.0914(6) 0.0721 1.0000 Uani . . . . . . C23 C 0.4287(6) 0.0376(3) 0.2672(3) 0.0289 1.0000 Uani . . . . . . C24 C 0.5268(7) -0.0145(4) 0.3014(5) 0.0464 1.0000 Uani . . . . . . C25 C 0.6288(8) 0.0142(5) 0.3600(5) 0.0552 1.0000 Uani . . . . . . C26 C 0.6334(6) 0.0943(5) 0.3842(4) 0.0417 1.0000 Uani . . . . . . C27 C 0.5369(6) 0.1479(4) 0.3502(4) 0.0349 1.0000 Uani . . . . . . C28 C 0.4344(6) 0.1198(4) 0.2922(4) 0.0304 1.0000 Uani . . . . . . Pd2 Pd 0.44769(3) -0.08499(4) 0.55604(2) 0.0170 1.0000 Uani . . . . . . I3 I 0.57272(4) -0.19923(4) 0.48733(2) 0.0328 1.0000 Uani . . . . . . I4 I 0.22285(3) -0.14224(4) 0.49442(2) 0.0294 1.0000 Uani . . . . . . P2 P 0.36421(12) 0.02961(8) 0.59905(8) 0.0197 1.0000 Uani . . . . . . N2 N 0.6173(4) -0.0352(2) 0.6260(2) 0.0186 1.0000 Uani . . . . . . C29 C 0.6223(5) 0.0426(3) 0.6391(3) 0.0185 1.0000 Uani . . . . . . C30 C 0.5088(5) 0.0927(3) 0.5988(3) 0.0241 1.0000 Uani . . . . . . C31 C 0.7200(5) -0.0889(3) 0.6619(3) 0.0210 1.0000 Uani . . . . . . C32 C 0.6973(5) -0.1389(3) 0.7275(3) 0.0249 1.0000 Uani . . . . . . C33 C 0.8007(6) -0.1882(3) 0.7652(4) 0.0361 1.0000 Uani . . . . . . C34 C 0.9173(6) -0.1881(4) 0.7381(4) 0.0350 1.0000 Uani . . . . . . C35 C 0.9357(5) -0.1401(4) 0.6700(4) 0.0343 1.0000 Uani . . . . . . C36 C 0.8369(5) -0.0886(3) 0.6317(3) 0.0263 1.0000 Uani . . . . . . C37 C 0.5729(6) -0.1381(4) 0.7589(4) 0.0327 1.0000 Uani . . . . . . C38 C 0.8587(6) -0.0366(4) 0.5588(4) 0.0345 1.0000 Uani . . . . . . C39 C 0.7315(5) 0.0873(3) 0.6894(3) 0.0206 1.0000 Uani . . . . . . C40 C 0.7699(5) 0.1620(3) 0.6611(3) 0.0265 1.0000 Uani . . . . . . C41 C 0.8760(6) 0.2019(3) 0.7058(4) 0.0349 1.0000 Uani . . . . . . C42 C 0.9405(6) 0.1707(4) 0.7794(4) 0.0414 1.0000 Uani . . . . . . C43 C 0.8983(6) 0.0982(4) 0.8089(4) 0.0385 1.0000 Uani . . . . . . C44 C 0.7965(6) 0.0560(3) 0.7648(3) 0.0299 1.0000 Uani . . . . . . C45 C 0.3312(5) 0.0292(3) 0.7045(3) 0.0243 1.0000 Uani . . . . . . C46 C 0.3855(7) 0.0871(4) 0.7623(3) 0.0364 1.0000 Uani . . . . . . C47 C 0.3550(7) 0.0852(4) 0.8424(4) 0.0421 1.0000 Uani . . . . . . C48 C 0.2740(8) 0.0257(6) 0.8636(4) 0.0567 1.0000 Uani . . . . . . C49 C 0.2227(10) -0.0328(7) 0.8066(5) 0.0740 1.0000 Uani . . . . . . C50 C 0.2527(8) -0.0305(6) 0.7264(4) 0.0580 1.0000 Uani . . . . . . C51 C 0.2338(5) 0.0849(3) 0.5377(3) 0.0222 1.0000 Uani . . . . . . C52 C 0.1308(6) 0.1169(4) 0.5719(4) 0.0316 1.0000 Uani . . . . . . C53 C 0.0336(6) 0.1610(4) 0.5215(4) 0.0381 1.0000 Uani . . . . . . C54 C 0.0424(6) 0.1736(4) 0.4392(4) 0.0386 1.0000 Uani . . . . . . C55 C 0.1444(6) 0.1439(4) 0.4053(4) 0.0364 1.0000 Uani . . . . . . C56 C 0.2399(6) 0.0981(4) 0.4545(4) 0.0321 1.0000 Uani . . . . . . H21 H 0.1666 0.0133 0.3039 0.0358 1.0000 Uiso . . . . . . H22 H 0.1956 -0.0829 0.2871 0.0358 1.0000 Uiso . . . . . . H51 H -0.2262 -0.0790 -0.0951 0.0676 1.0000 Uiso . . . . . . H61 H -0.4042 -0.0086 -0.0685 0.0863 1.0000 Uiso . . . . . . H71 H -0.4033 0.0692 0.0520 0.0844 1.0000 Uiso . . . . . . H91 H -0.0050 -0.1019 -0.0688 0.0582 1.0000 Uiso . . . . . . H92 H 0.0490 -0.1171 0.0294 0.0582 1.0000 Uiso . . . . . . H93 H 0.0837 -0.0322 -0.0149 0.0582 1.0000 Uiso . . . . . . H101 H -0.2849 0.1194 0.1852 0.0856 1.0000 Uiso . . . . . . H102 H -0.1721 0.0582 0.2309 0.0856 1.0000 Uiso . . . . . . H103 H -0.1328 0.1395 0.1824 0.0856 1.0000 Uiso . . . . . . H121 H -0.1294 -0.1422 0.1168 0.0412 1.0000 Uiso . . . . . . H131 H -0.2811 -0.2303 0.1680 0.0489 1.0000 Uiso . . . . . . H141 H -0.2923 -0.2351 0.3125 0.0520 1.0000 Uiso . . . . . . H151 H -0.1508 -0.1551 0.4066 0.0458 1.0000 Uiso . . . . . . H161 H -0.0017 -0.0621 0.3576 0.0376 1.0000 Uiso . . . . . . H181 H 0.2228 -0.1709 0.2019 0.0901 1.0000 Uiso . . . . . . H191 H 0.2833 -0.2903 0.1329 0.1135 1.0000 Uiso . . . . . . H201 H 0.4254 -0.2807 0.0357 0.0729 1.0000 Uiso . . . . . . H211 H 0.5146 -0.1511 0.0097 0.1156 1.0000 Uiso . . . . . . H221 H 0.4574 -0.0323 0.0794 0.0938 1.0000 Uiso . . . . . . H241 H 0.5247 -0.0733 0.2840 0.0534 1.0000 Uiso . . . . . . H251 H 0.6991 -0.0242 0.3845 0.0621 1.0000 Uiso . . . . . . H261 H 0.7067 0.1142 0.4265 0.0492 1.0000 Uiso . . . . . . H271 H 0.5408 0.2067 0.3674 0.0422 1.0000 Uiso . . . . . . H281 H 0.3642 0.1585 0.2680 0.0364 1.0000 Uiso . . . . . . H301 H 0.5023 0.1442 0.6309 0.0288 1.0000 Uiso . . . . . . H302 H 0.5188 0.1067 0.5406 0.0288 1.0000 Uiso . . . . . . H331 H 0.7884 -0.2240 0.8129 0.0416 1.0000 Uiso . . . . . . H341 H 0.9900 -0.2224 0.7670 0.0396 1.0000 Uiso . . . . . . H351 H 1.0199 -0.1427 0.6487 0.0402 1.0000 Uiso . . . . . . H371 H 0.5766 -0.1780 0.8056 0.0392 1.0000 Uiso . . . . . . H372 H 0.5564 -0.0819 0.7791 0.0392 1.0000 Uiso . . . . . . H373 H 0.5015 -0.1538 0.7133 0.0392 1.0000 Uiso . . . . . . H381 H 0.9487 -0.0455 0.5474 0.0424 1.0000 Uiso . . . . . . H382 H 0.8468 0.0224 0.5718 0.0424 1.0000 Uiso . . . . . . H383 H 0.7950 -0.0524 0.5089 0.0424 1.0000 Uiso . . . . . . H401 H 0.7218 0.1868 0.6092 0.0321 1.0000 Uiso . . . . . . H411 H 0.9063 0.2544 0.6841 0.0422 1.0000 Uiso . . . . . . H421 H 1.0167 0.2002 0.8108 0.0486 1.0000 Uiso . . . . . . H431 H 0.9426 0.0760 0.8631 0.0440 1.0000 Uiso . . . . . . H441 H 0.7684 0.0028 0.7863 0.0350 1.0000 Uiso . . . . . . H461 H 0.4458 0.1297 0.7467 0.0434 1.0000 Uiso . . . . . . H471 H 0.3921 0.1271 0.8841 0.0501 1.0000 Uiso . . . . . . H481 H 0.2518 0.0246 0.9209 0.0696 1.0000 Uiso . . . . . . H491 H 0.1646 -0.0766 0.8225 0.0914 1.0000 Uiso . . . . . . H501 H 0.2162 -0.0728 0.6849 0.0712 1.0000 Uiso . . . . . . H521 H 0.1264 0.1085 0.6319 0.0386 1.0000 Uiso . . . . . . H531 H -0.0417 0.1833 0.5450 0.0460 1.0000 Uiso . . . . . . H541 H -0.0273 0.2052 0.4035 0.0450 1.0000 Uiso . . . . . . H551 H 0.1503 0.1549 0.3459 0.0430 1.0000 Uiso . . . . . . H561 H 0.3132 0.0746 0.4297 0.0384 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0326(2) 0.01757(17) 0.01801(17) -0.00037(14) 0.00454(15) -0.00074(15) I1 0.0595(3) 0.02719(18) 0.0402(2) 0.00640(16) -0.01145(19) -0.00137(18) I2 0.0496(2) 0.02970(18) 0.03216(18) -0.00393(15) 0.02091(16) -0.00804(16) P1 0.0280(7) 0.0224(6) 0.0234(6) 0.0013(5) 0.0070(5) 0.0008(5) N1 0.026(2) 0.023(2) 0.024(2) -0.0002(16) 0.0023(17) 0.0051(17) C1 0.027(3) 0.021(2) 0.027(2) 0.004(2) 0.008(2) 0.006(2) C2 0.030(3) 0.037(3) 0.022(2) 0.006(2) 0.008(2) 0.005(2) C3 0.027(3) 0.032(3) 0.031(3) 0.011(2) -0.005(2) 0.000(2) C4 0.050(4) 0.038(3) 0.026(3) 0.007(2) -0.008(3) -0.019(3) C5 0.061(5) 0.070(5) 0.037(4) 0.021(4) -0.016(3) -0.023(4) C6 0.068(6) 0.088(7) 0.060(5) 0.031(5) -0.019(5) -0.017(5) C7 0.035(4) 0.059(5) 0.117(8) 0.042(5) 0.015(4) 0.015(4) C8 0.035(3) 0.039(4) 0.062(4) 0.022(3) 0.012(3) 0.012(3) C9 0.074(5) 0.036(4) 0.034(3) -0.011(3) 0.015(3) -0.018(3) C10 0.069(5) 0.051(5) 0.093(7) 0.015(4) 0.043(5) 0.033(4) C11 0.024(2) 0.022(3) 0.034(3) 0.002(2) 0.010(2) 0.006(2) C12 0.042(3) 0.025(3) 0.037(3) -0.001(2) 0.001(2) -0.001(2) C13 0.038(3) 0.029(3) 0.056(4) 0.010(3) 0.008(3) -0.009(3) C14 0.039(3) 0.030(3) 0.062(4) 0.010(3) 0.022(3) -0.002(3) C15 0.036(3) 0.034(3) 0.045(3) 0.010(3) 0.027(3) 0.008(3) C16 0.030(3) 0.035(3) 0.029(3) 0.004(2) 0.009(2) 0.004(2) C17 0.033(3) 0.022(2) 0.035(3) -0.004(2) 0.010(2) -0.002(2) C18 0.080(6) 0.027(3) 0.118(8) -0.010(4) 0.068(6) -0.007(4) C19 0.093(7) 0.026(4) 0.165(11) -0.021(5) 0.074(8) -0.009(4) C20 0.060(5) 0.037(4) 0.085(6) -0.015(4) 0.026(4) 0.009(3) C21 0.145(10) 0.045(5) 0.099(7) -0.006(5) 0.088(8) 0.018(5) C22 0.108(7) 0.031(4) 0.096(7) -0.011(4) 0.072(6) -0.003(4) C23 0.033(3) 0.029(3) 0.025(3) 0.002(2) 0.008(2) 0.000(2) C24 0.046(4) 0.033(3) 0.054(4) -0.004(3) -0.009(3) 0.012(3) C25 0.053(4) 0.054(4) 0.048(4) -0.006(3) -0.023(3) 0.020(4) C26 0.033(3) 0.063(4) 0.027(3) -0.006(3) -0.002(2) 0.000(3) C27 0.046(3) 0.030(3) 0.030(3) -0.006(2) 0.009(2) -0.007(3) C28 0.034(3) 0.028(3) 0.029(3) -0.003(2) 0.004(2) 0.004(2) Pd2 0.01879(16) 0.01512(16) 0.01664(16) -0.00184(13) 0.00172(12) -0.00172(13) I3 0.03273(18) 0.02277(16) 0.0446(2) -0.01103(15) 0.01109(15) -0.00186(14) I4 0.02221(15) 0.02941(17) 0.03436(18) -0.00941(14) -0.00229(13) -0.00463(13) P2 0.0212(6) 0.0198(6) 0.0180(6) -0.0031(5) 0.0029(5) 0.0007(5) N2 0.0184(19) 0.0163(19) 0.0206(19) -0.0002(15) 0.0018(15) -0.0048(15) C29 0.021(2) 0.019(2) 0.016(2) 0.0001(17) 0.0041(17) -0.0030(18) C30 0.025(2) 0.018(2) 0.030(2) -0.003(2) 0.004(2) -0.0007(19) C31 0.020(2) 0.017(2) 0.023(2) 0.0026(19) -0.0036(17) -0.0024(19) C32 0.028(2) 0.016(2) 0.029(2) 0.004(2) -0.001(2) 0.001(2) C33 0.043(3) 0.020(3) 0.041(3) 0.006(2) -0.005(3) -0.002(2) C34 0.029(3) 0.027(3) 0.042(3) -0.003(2) -0.012(2) 0.004(2) C35 0.023(2) 0.029(3) 0.048(3) -0.006(3) -0.002(2) 0.001(2) C36 0.026(2) 0.022(2) 0.029(2) -0.007(2) 0.0002(19) -0.001(2) C37 0.036(3) 0.029(3) 0.033(3) 0.011(2) 0.005(2) 0.000(2) C38 0.033(3) 0.036(3) 0.037(3) -0.003(2) 0.013(2) -0.004(2) C39 0.025(2) 0.016(2) 0.021(2) 0.0002(19) 0.0051(18) -0.0030(19) C40 0.031(3) 0.022(2) 0.027(2) 0.000(2) 0.007(2) -0.004(2) C41 0.047(3) 0.022(3) 0.036(3) -0.004(2) 0.009(3) -0.018(2) C42 0.040(3) 0.037(3) 0.045(3) -0.009(3) -0.001(3) -0.015(3) C43 0.045(3) 0.034(3) 0.031(3) -0.004(2) -0.010(3) -0.004(3) C44 0.039(3) 0.024(2) 0.025(3) -0.003(2) -0.001(2) -0.009(2) C45 0.022(2) 0.032(3) 0.019(2) -0.002(2) 0.0007(18) 0.003(2) C46 0.054(4) 0.029(3) 0.026(3) -0.003(2) 0.005(2) -0.002(3) C47 0.055(4) 0.044(3) 0.026(3) -0.002(3) 0.004(3) 0.001(3) C48 0.065(5) 0.084(6) 0.025(3) -0.006(3) 0.019(3) -0.016(4) C49 0.087(7) 0.106(7) 0.035(4) -0.022(4) 0.029(4) -0.060(6) C50 0.058(4) 0.090(6) 0.030(3) -0.020(4) 0.019(3) -0.043(4) C51 0.021(2) 0.018(2) 0.027(2) -0.003(2) 0.0038(19) -0.0041(19) C52 0.028(3) 0.036(3) 0.032(3) -0.001(2) 0.009(2) 0.004(2) C53 0.035(3) 0.035(3) 0.045(3) 0.011(3) 0.009(2) 0.009(3) C54 0.033(3) 0.033(3) 0.046(3) 0.002(3) -0.003(3) 0.005(2) C55 0.042(3) 0.036(3) 0.029(3) 0.003(2) 0.001(2) 0.007(3) C56 0.037(3) 0.029(3) 0.030(3) -0.003(2) 0.005(2) 0.010(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . I1 . 2.6261(6) yes Pd1 . I2 . 2.5767(5) yes Pd1 . P1 . 2.2293(14) yes Pd1 . N1 . 2.107(5) yes P1 . C2 . 1.843(6) yes P1 . C17 . 1.808(6) yes P1 . C23 . 1.799(6) yes N1 . C1 . 1.283(7) yes N1 . C3 . 1.446(7) yes C1 . C2 . 1.500(8) yes C1 . C11 . 1.501(7) yes C2 . H22 . 1.000 no C2 . H21 . 1.000 no C3 . C4 . 1.433(9) yes C3 . C8 . 1.380(9) yes C4 . C5 . 1.390(10) yes C4 . C9 . 1.465(11) yes C5 . C6 . 1.319(15) yes C5 . H51 . 1.000 no C6 . C7 . 1.373(16) yes C6 . H61 . 1.000 no C7 . C8 . 1.459(12) yes C7 . H71 . 1.000 no C8 . C10 . 1.476(13) yes C9 . H92 . 1.000 no C9 . H93 . 1.000 no C9 . H91 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C10 . H101 . 1.000 no C11 . C12 . 1.380(8) yes C11 . C16 . 1.412(8) yes C12 . C13 . 1.394(9) yes C12 . H121 . 1.000 no C13 . C14 . 1.392(10) yes C13 . H131 . 1.000 no C14 . C15 . 1.358(10) yes C14 . H141 . 1.000 no C15 . C16 . 1.403(8) yes C15 . H151 . 1.000 no C16 . H161 . 1.000 no C17 . C18 . 1.364(9) yes C17 . C22 . 1.375(9) yes C18 . C19 . 1.399(11) yes C18 . H181 . 1.000 no C19 . C20 . 1.351(13) yes C19 . H191 . 1.000 no C20 . C21 . 1.375(13) yes C20 . H201 . 1.000 no C21 . C22 . 1.385(11) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no C23 . C24 . 1.381(9) yes C23 . C28 . 1.401(8) yes C24 . C25 . 1.394(10) yes C24 . H241 . 1.000 no C25 . C26 . 1.366(11) yes C25 . H251 . 1.000 no C26 . C27 . 1.384(10) yes C26 . H261 . 1.000 no C27 . C28 . 1.390(8) yes C27 . H271 . 1.000 no C28 . H281 . 1.000 no Pd2 . I3 . 2.6335(5) yes Pd2 . I4 . 2.5803(5) yes Pd2 . P2 . 2.2276(13) yes Pd2 . N2 . 2.113(4) yes P2 . C30 . 1.832(5) yes P2 . C45 . 1.813(5) yes P2 . C51 . 1.801(5) yes N2 . C29 . 1.288(6) yes N2 . C31 . 1.437(6) yes C29 . C30 . 1.504(7) yes C29 . C39 . 1.488(6) yes C30 . H302 . 1.000 no C30 . H301 . 1.000 no C31 . C32 . 1.398(7) yes C31 . C36 . 1.391(7) yes C32 . C33 . 1.408(8) yes C32 . C37 . 1.475(8) yes C33 . C34 . 1.364(9) yes C33 . H331 . 1.000 no C34 . C35 . 1.399(9) yes C34 . H341 . 1.000 no C35 . C36 . 1.401(8) yes C35 . H351 . 1.000 no C36 . C38 . 1.511(8) yes C37 . H372 . 1.000 no C37 . H373 . 1.000 no C37 . H371 . 1.000 no C38 . H382 . 1.000 no C38 . H383 . 1.000 no C38 . H381 . 1.000 no C39 . C40 . 1.387(7) yes C39 . C44 . 1.403(7) yes C40 . C41 . 1.389(8) yes C40 . H401 . 1.000 no C41 . C42 . 1.378(9) yes C41 . H411 . 1.000 no C42 . C43 . 1.378(9) yes C42 . H421 . 1.000 no C43 . C44 . 1.372(8) yes C43 . H431 . 1.000 no C44 . H441 . 1.000 no C45 . C46 . 1.392(8) yes C45 . C50 . 1.360(9) yes C46 . C47 . 1.398(8) yes C46 . H461 . 1.000 no C47 . C48 . 1.371(11) yes C47 . H471 . 1.000 no C48 . C49 . 1.382(11) yes C48 . H481 . 1.000 no C49 . C50 . 1.397(10) yes C49 . H491 . 1.000 no C50 . H501 . 1.000 no C51 . C52 . 1.394(7) yes C51 . C56 . 1.389(8) yes C52 . C53 . 1.401(8) yes C52 . H521 . 1.000 no C53 . C54 . 1.378(9) yes C53 . H531 . 1.000 no C54 . C55 . 1.370(9) yes C54 . H541 . 1.000 no C55 . C56 . 1.394(8) yes C55 . H551 . 1.000 no C56 . H561 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I1 . Pd1 . I2 . 89.699(19) yes I1 . Pd1 . P1 . 173.17(4) yes I2 . Pd1 . P1 . 93.98(4) yes I1 . Pd1 . N1 . 95.70(12) yes I2 . Pd1 . N1 . 173.12(12) yes P1 . Pd1 . N1 . 81.09(12) yes Pd1 . P1 . C2 . 98.53(18) yes Pd1 . P1 . C17 . 114.9(2) yes C2 . P1 . C17 . 105.8(3) yes Pd1 . P1 . C23 . 121.64(19) yes C2 . P1 . C23 . 105.2(3) yes C17 . P1 . C23 . 108.5(3) yes Pd1 . N1 . C1 . 121.0(4) yes Pd1 . N1 . C3 . 118.2(3) yes C1 . N1 . C3 . 120.8(5) yes N1 . C1 . C2 . 117.4(5) yes N1 . C1 . C11 . 125.4(5) yes C2 . C1 . C11 . 117.2(4) yes C1 . C2 . P1 . 108.2(4) yes C1 . C2 . H22 . 109.785 no P1 . C2 . H22 . 109.785 no C1 . C2 . P1 . 108.2(4) yes C1 . C2 . H21 . 109.785 no P1 . C2 . H21 . 109.785 no N1 . C3 . C4 . 116.4(5) yes N1 . C3 . C8 . 119.7(6) yes C4 . C3 . C8 . 123.9(6) yes C3 . C4 . C5 . 117.3(7) yes C3 . C4 . C9 . 121.8(5) yes C5 . C4 . C9 . 120.9(7) yes C4 . C5 . C6 . 120.5(9) yes C4 . C5 . H51 . 119.759 no C6 . C5 . H51 . 119.757 no C5 . C6 . C7 . 123.3(8) yes C5 . C6 . H61 . 118.339 no C7 . C6 . H61 . 118.323 no C6 . C7 . C8 . 120.5(8) yes C6 . C7 . H71 . 119.739 no C8 . C7 . H71 . 119.725 no C7 . C8 . C3 . 114.2(7) yes C7 . C8 . C10 . 123.7(7) yes C3 . C8 . C10 . 122.1(7) yes C4 . C9 . H92 . 109.466 no C4 . C9 . H93 . 109.467 no H92 . C9 . H93 . 109.476 no C4 . C9 . H91 . 109.466 no C8 . C10 . H102 . 109.466 no C8 . C10 . H103 . 109.466 no H102 . C10 . H103 . 109.477 no C8 . C10 . H101 . 109.466 no C1 . C11 . C12 . 123.1(5) yes C1 . C11 . C16 . 116.6(5) yes C12 . C11 . C16 . 120.3(5) yes C11 . C12 . C13 . 119.3(6) yes C11 . C12 . H121 . 120.374 no C13 . C12 . H121 . 120.373 no C12 . C13 . C14 . 120.8(6) yes C12 . C13 . H131 . 119.620 no C14 . C13 . H131 . 119.619 no C13 . C14 . C15 . 120.1(6) yes C13 . C14 . H141 . 119.961 no C15 . C14 . H141 . 119.961 no C14 . C15 . C16 . 120.7(6) yes C14 . C15 . H151 . 119.638 no C16 . C15 . H151 . 119.638 no C11 . C16 . C15 . 118.9(6) yes C11 . C16 . H161 . 120.559 no C15 . C16 . H161 . 120.559 no P1 . C17 . C18 . 122.7(5) yes P1 . C17 . C22 . 118.5(5) yes C18 . C17 . C22 . 118.6(6) yes C17 . C18 . C19 . 120.4(7) yes C17 . C18 . H181 . 119.805 no C19 . C18 . H181 . 119.805 no C18 . C19 . C20 . 120.8(8) yes C18 . C19 . H191 . 119.575 no C20 . C19 . H191 . 119.575 no C19 . C20 . C21 . 119.0(7) yes C19 . C20 . H201 . 120.487 no C21 . C20 . H201 . 120.488 no C20 . C21 . C22 . 120.3(8) yes C20 . C21 . H211 . 119.832 no C22 . C21 . H211 . 119.833 no C21 . C22 . C17 . 120.8(8) yes C21 . C22 . H221 . 119.610 no C17 . C22 . H221 . 119.610 no P1 . C23 . C24 . 121.5(5) yes P1 . C23 . C28 . 119.7(4) yes C24 . C23 . C28 . 118.7(6) yes C23 . C24 . C25 . 120.4(6) yes C23 . C24 . H241 . 119.779 no C25 . C24 . H241 . 119.779 no C24 . C25 . C26 . 120.5(6) yes C24 . C25 . H251 . 119.727 no C26 . C25 . H251 . 119.727 no C25 . C26 . C27 . 120.1(6) yes C25 . C26 . H261 . 119.969 no C27 . C26 . H261 . 119.971 no C26 . C27 . C28 . 119.8(6) yes C26 . C27 . H271 . 120.080 no C28 . C27 . H271 . 120.080 no C23 . C28 . C27 . 120.4(5) yes C23 . C28 . H281 . 119.779 no C27 . C28 . H281 . 119.779 no I3 . Pd2 . I4 . 93.519(16) yes I3 . Pd2 . P2 . 167.91(4) yes I4 . Pd2 . P2 . 92.77(4) yes I3 . Pd2 . N2 . 94.10(11) yes I4 . Pd2 . N2 . 169.75(11) yes P2 . Pd2 . N2 . 81.03(12) yes Pd2 . P2 . C30 . 96.05(16) yes Pd2 . P2 . C45 . 116.24(19) yes C30 . P2 . C45 . 106.8(2) yes Pd2 . P2 . C51 . 123.11(17) yes C30 . P2 . C51 . 105.6(2) yes C45 . P2 . C51 . 106.7(2) yes Pd2 . N2 . C29 . 118.5(3) yes Pd2 . N2 . C31 . 119.6(3) yes C29 . N2 . C31 . 121.8(4) yes N2 . C29 . C30 . 117.2(4) yes N2 . C29 . C39 . 125.7(4) yes C30 . C29 . C39 . 117.1(4) yes C29 . C30 . P2 . 106.7(3) yes C29 . C30 . H302 . 110.167 no P2 . C30 . H302 . 110.167 no C29 . C30 . P2 . 106.7(3) yes C29 . C30 . H301 . 110.167 no P2 . C30 . H301 . 110.167 no N2 . C31 . C32 . 117.4(4) yes N2 . C31 . C36 . 119.6(4) yes C32 . C31 . C36 . 122.9(5) yes C31 . C32 . C33 . 117.1(5) yes C31 . C32 . C37 . 122.1(5) yes C33 . C32 . C37 . 120.8(5) yes C32 . C33 . C34 . 121.4(5) yes C32 . C33 . H331 . 119.291 no C34 . C33 . H331 . 119.291 no C33 . C34 . C35 . 120.3(5) yes C33 . C34 . H341 . 119.836 no C35 . C34 . H341 . 119.836 no C34 . C35 . C36 . 120.4(5) yes C34 . C35 . H351 . 119.816 no C36 . C35 . H351 . 119.818 no C35 . C36 . C31 . 117.8(5) yes C35 . C36 . C38 . 119.7(5) yes C31 . C36 . C38 . 122.5(5) yes C32 . C37 . H372 . 109.467 no C32 . C37 . H373 . 109.467 no H372 . C37 . H373 . 109.476 no C32 . C37 . H371 . 109.467 no C36 . C38 . H382 . 109.467 no C36 . C38 . H383 . 109.466 no H382 . C38 . H383 . 109.476 no C36 . C38 . H381 . 109.466 no C29 . C39 . C40 . 119.0(4) yes C29 . C39 . C44 . 121.7(4) yes C40 . C39 . C44 . 119.3(5) yes C39 . C40 . C41 . 119.1(5) yes C39 . C40 . H401 . 120.427 no C41 . C40 . H401 . 120.428 no C40 . C41 . C42 . 121.5(5) yes C40 . C41 . H411 . 119.256 no C42 . C41 . H411 . 119.255 no C41 . C42 . C43 . 118.9(5) yes C41 . C42 . H421 . 120.531 no C43 . C42 . H421 . 120.532 no C42 . C43 . C44 . 120.9(6) yes C42 . C43 . H431 . 119.546 no C44 . C43 . H431 . 119.547 no C39 . C44 . C43 . 120.1(5) yes C39 . C44 . H441 . 119.927 no C43 . C44 . H441 . 119.927 no P2 . C45 . C46 . 121.6(4) yes P2 . C45 . C50 . 118.0(4) yes C46 . C45 . C50 . 120.4(5) yes C45 . C46 . C47 . 119.4(6) yes C45 . C46 . H461 . 120.296 no C47 . C46 . H461 . 120.296 no C46 . C47 . C48 . 119.9(6) yes C46 . C47 . H471 . 120.073 no C48 . C47 . H471 . 120.073 no C47 . C48 . C49 . 120.5(6) yes C47 . C48 . H481 . 119.744 no C49 . C48 . H481 . 119.744 no C48 . C49 . C50 . 119.5(7) yes C48 . C49 . H491 . 120.239 no C50 . C49 . H491 . 120.239 no C49 . C50 . C45 . 120.3(7) yes C49 . C50 . H501 . 119.858 no C45 . C50 . H501 . 119.858 no P2 . C51 . C52 . 122.0(4) yes P2 . C51 . C56 . 118.2(4) yes C52 . C51 . C56 . 119.8(5) yes C51 . C52 . C53 . 119.5(6) yes C51 . C52 . H521 . 120.267 no C53 . C52 . H521 . 120.266 no C52 . C53 . C54 . 119.6(6) yes C52 . C53 . H531 . 120.199 no C54 . C53 . H531 . 120.198 no C53 . C54 . C55 . 121.4(6) yes C53 . C54 . H541 . 119.286 no C55 . C54 . H541 . 119.286 no C54 . C55 . C56 . 119.4(6) yes C54 . C55 . H551 . 120.308 no C56 . C55 . H551 . 120.307 no C55 . C56 . C51 . 120.3(5) yes C55 . C56 . H561 . 119.843 no C51 . C56 . H561 . 119.842 no #===END ####################### ## denoted 9 in text ## ####################### data_9 _database_code_depnum_ccdc_archive 'CCDC 236200' #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 39.359(1) _cell_angle_alpha 90 _cell_length_b 9.388(1) _cell_angle_beta 107.83(1) _cell_length_c 14.772(1) _cell_angle_gamma 90 _cell_volume 5196.1 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' 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 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . 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_IV_Table_2.2B '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_IV_Table_2.2B '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_IV_Table_2.2B '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_IV_Table_2.2B 'Pt ' -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C30 H31 N1 P1 Pt1 ' _chemical_formula_moiety ' C30 H31 N1 P1 Pt1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 631.65 _cell_measurement_reflns_used 47816 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' yellow ' _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.60 _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 5.480 _diffrn_measurement_device_type ; Enraf-nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect'(Nonius, 2000) ; _computing_data_reduction ; 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; 'DENZO' (Otwinowski & Minor, 1996) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.04 _exptl_absorpt_correction_T_max 0.11 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 47816 _reflns_number_total 5612 _diffrn_reflns_av_R_equivalents 0.028 # Number of reflections with Friedels Law is 5612 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5971 _diffrn_reflns_theta_min 3.791 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -50 _reflns_limit_h_max 48 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -1.43 _refine_diff_density_max 1.39 _refine_ls_number_reflns 5063 _refine_ls_number_restraints 127 _refine_ls_number_parameters 298 #_refine_ls_R_factor_ref 0.0272 _refine_ls_wR_factor_ref 0.0349 _refine_ls_goodness_of_fit_ref 1.3238 #_reflns_number_all 5612 _refine_ls_R_factor_all 0.0314 _refine_ls_wR_factor_all 0.0357 _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 5063 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_gt 0.0349 _refine_ls_shift/su_max 0.024402 _refine_ls_structure_factor_coef F _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: 3.51 -1.15 2.37 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## _publ_section_references ; 'Collect' (Nonius, 2000) Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. 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 trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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 _atom_site_attached_hydrogens Pt1 Pt 0.124068(3) 0.229358(14) -0.131771(9) 0.0207 1.0000 Uani . . . . . . P1 P 0.15463(2) 0.07154(11) -0.02348(7) 0.0239 1.0000 Uani . . . . . . N1 N 0.09558(9) 0.2514(3) -0.0284(2) 0.0207 1.0000 Uani . . . . . . C1 C 0.09718(9) 0.1526(4) 0.0339(3) 0.0205 1.0000 Uani . . . . . . C2 C 0.11936(10) 0.0219(4) 0.0288(3) 0.0278 1.0000 Uani . . . . . . C3 C 0.09101(12) 0.3706(5) -0.2285(3) 0.0338 1.0000 Uani . . . . . . C4 C 0.15201(12) 0.2086(5) -0.2282(3) 0.0333 1.0000 Uani . . . . . . C5 C 0.07458(10) 0.3785(4) -0.0334(3) 0.0240 1.0000 Uani . . . . . . C6 C 0.09296(13) 0.5064(4) -0.0007(3) 0.0351 1.0000 Uani . . . . . . C7 C 0.07219(19) 0.6313(5) -0.0121(4) 0.0529 1.0000 Uani . . . . . . C8 C 0.03569(19) 0.6289(6) -0.0538(4) 0.0583 1.0000 Uani . . . . . . C9 C 0.01905(15) 0.5040(6) -0.0858(3) 0.0498 1.0000 Uani . . . . . . C10 C 0.03786(11) 0.3746(5) -0.0761(3) 0.0325 1.0000 Uani . . . . . . C11 C 0.13256(16) 0.5071(6) 0.0456(4) 0.0525 1.0000 Uani . . . . . . C12 C 0.01860(13) 0.2391(6) -0.1104(4) 0.0425 1.0000 Uani . . . . . . C13 C 0.07906(9) 0.1520(4) 0.1088(3) 0.0220 1.0000 Uani . . . . . . C14 C 0.07270(11) 0.2754(4) 0.1552(3) 0.0249 1.0000 Uani . . . . . . C15 C 0.05673(12) 0.2653(4) 0.2268(3) 0.0286 1.0000 Uani . . . . . . C16 C 0.04657(11) 0.1343(5) 0.2535(3) 0.0318 1.0000 Uani . . . . . . C17 C 0.05288(11) 0.0114(5) 0.2087(3) 0.0340 1.0000 Uani . . . . . . C18 C 0.06879(11) 0.0204(4) 0.1368(3) 0.0290 1.0000 Uani . . . . . . C19 C 0.16893(10) -0.1019(4) -0.0541(3) 0.0279 1.0000 Uani . . . . . . C20 C 0.14856(11) -0.1642(5) -0.1377(4) 0.0423 1.0000 Uani . . . . . . C21 C 0.15684(15) -0.2989(6) -0.1632(5) 0.0561 1.0000 Uani . . . . . . C22 C 0.18590(13) -0.3729(5) -0.1061(4) 0.0482 1.0000 Uani . . . . . . C23 C 0.20635(15) -0.3122(6) -0.0235(4) 0.0518 1.0000 Uani . . . . . . C24 C 0.19816(14) -0.1760(6) 0.0032(3) 0.0469 1.0000 Uani . . . . . . C25 C 0.19184(11) 0.1359(6) 0.0763(3) 0.0547 1.0000 Uani D U . . . . C26 C 0.21395(15) 0.2381(7) 0.0557(3) 0.0774 1.0000 Uani D U . . . . C27 C 0.24251(15) 0.2909(7) 0.1271(4) 0.0816 1.0000 Uani D U . . . . C28 C 0.24938(14) 0.2414(7) 0.2190(4) 0.0755 1.0000 Uani D U . . . . C29 C 0.22556(14) 0.1558(7) 0.2403(3) 0.0738 1.0000 Uani D U . . . . C30 C 0.19655(14) 0.1028(7) 0.1688(3) 0.0703 1.0000 Uani D U . . . . H21 H 0.1305 -0.0168 0.0942 0.0353 1.0000 Uiso . . . . . . H22 H 0.1037 -0.0524 -0.0118 0.0353 1.0000 Uiso . . . . . . H71 H 0.0842 0.7241 0.0108 0.0727 1.0000 Uiso . . . . . . H81 H 0.0216 0.7190 -0.0607 0.0796 1.0000 Uiso . . . . . . H91 H -0.0074 0.5037 -0.1173 0.0633 1.0000 Uiso . . . . . . H111 H 0.1408 0.6068 0.0640 0.0659 1.0000 Uiso . . . . . . H112 H 0.1446 0.4694 0.0000 0.0659 1.0000 Uiso . . . . . . H113 H 0.1387 0.4457 0.1037 0.0659 1.0000 Uiso . . . . . . H121 H -0.0075 0.2588 -0.1388 0.0500 1.0000 Uiso . . . . . . H122 H 0.0280 0.1954 -0.1597 0.0500 1.0000 Uiso . . . . . . H123 H 0.0223 0.1716 -0.0558 0.0500 1.0000 Uiso . . . . . . H141 H 0.0797 0.3708 0.1365 0.0298 1.0000 Uiso . . . . . . H151 H 0.0525 0.3536 0.2596 0.0352 1.0000 Uiso . . . . . . H161 H 0.0348 0.1283 0.3046 0.0405 1.0000 Uiso . . . . . . H171 H 0.0460 -0.0835 0.2282 0.0437 1.0000 Uiso . . . . . . H181 H 0.0729 -0.0686 0.1044 0.0371 1.0000 Uiso . . . . . . H201 H 0.1277 -0.1115 -0.1805 0.0467 1.0000 Uiso . . . . . . H211 H 0.1416 -0.3433 -0.2235 0.0623 1.0000 Uiso . . . . . . H221 H 0.1918 -0.4697 -0.1251 0.0578 1.0000 Uiso . . . . . . H231 H 0.2274 -0.3651 0.0185 0.0614 1.0000 Uiso . . . . . . H241 H 0.2134 -0.1322 0.0638 0.0548 1.0000 Uiso . . . . . . H261 H 0.2091 0.2733 -0.0110 0.0900 1.0000 Uiso . . . . . . H271 H 0.2583 0.3653 0.1124 0.0946 1.0000 Uiso . . . . . . H281 H 0.2719 0.2692 0.2692 0.0876 1.0000 Uiso . . . . . . H291 H 0.2287 0.1303 0.3080 0.0855 1.0000 Uiso . . . . . . H401 H 0.1723 0.1407 -0.2027 0.0421 1.0000 Uiso . . . . . . H402 H 0.1616 0.3036 -0.2391 0.0421 1.0000 Uiso . . . . . . H403 H 0.1358 0.1713 -0.2897 0.0421 1.0000 Uiso . . . . . . H301 H 0.0720 0.4065 -0.2023 0.0412 1.0000 Uiso . . . . . . H302 H 0.1055 0.4526 -0.2394 0.0412 1.0000 Uiso . . . . . . H303 H 0.0797 0.3203 -0.2900 0.0412 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02620(9) 0.01920(9) 0.01802(10) -0.00082(4) 0.00873(6) -0.00151(5) P1 0.0233(4) 0.0282(5) 0.0214(5) 0.0034(3) 0.0085(3) 0.0017(3) N1 0.0227(15) 0.0224(15) 0.0197(17) -0.0021(11) 0.0105(12) -0.0010(11) C1 0.0198(15) 0.0200(17) 0.0226(18) -0.0006(12) 0.0076(13) -0.0023(12) C2 0.0287(18) 0.0244(19) 0.035(2) 0.0080(15) 0.0166(15) 0.0043(14) C3 0.046(2) 0.031(2) 0.027(2) 0.0100(16) 0.0138(17) 0.0108(17) C4 0.039(2) 0.041(3) 0.025(2) -0.0039(17) 0.0175(17) 0.0005(18) C5 0.0381(19) 0.0176(17) 0.0191(18) -0.0010(12) 0.0130(14) 0.0045(14) C6 0.062(3) 0.024(2) 0.029(2) -0.0018(15) 0.028(2) -0.0074(18) C7 0.110(5) 0.021(2) 0.052(3) 0.0024(19) 0.059(3) 0.002(2) C8 0.104(5) 0.037(3) 0.057(3) 0.023(2) 0.059(3) 0.037(3) C9 0.065(3) 0.061(3) 0.032(3) 0.020(2) 0.028(2) 0.040(3) C10 0.042(2) 0.040(2) 0.019(2) 0.0041(15) 0.0140(16) 0.0144(18) C11 0.066(3) 0.048(3) 0.052(3) -0.019(2) 0.030(3) -0.032(3) C12 0.033(2) 0.058(3) 0.035(3) -0.010(2) 0.0067(19) 0.0004(19) C13 0.0191(15) 0.0238(18) 0.0233(18) 0.0014(13) 0.0067(13) -0.0005(12) C14 0.0310(19) 0.0236(18) 0.020(2) 0.0008(13) 0.0077(15) -0.0011(14) C15 0.033(2) 0.029(2) 0.026(2) 0.0005(14) 0.0121(16) 0.0022(15) C16 0.033(2) 0.037(2) 0.031(2) 0.0019(17) 0.0181(16) -0.0011(16) C17 0.036(2) 0.030(2) 0.044(3) 0.0027(17) 0.0230(18) -0.0067(16) C18 0.037(2) 0.0230(19) 0.033(2) -0.0002(15) 0.0190(16) -0.0042(15) C19 0.0238(17) 0.031(2) 0.032(2) 0.0057(15) 0.0131(15) 0.0045(14) C20 0.029(2) 0.036(2) 0.051(3) -0.007(2) -0.0033(18) 0.0062(17) C21 0.047(3) 0.041(3) 0.068(4) -0.017(3) -0.001(3) 0.006(2) C22 0.042(2) 0.034(2) 0.069(4) -0.001(2) 0.017(2) 0.012(2) C23 0.053(3) 0.052(3) 0.049(3) 0.009(2) 0.013(2) 0.030(3) C24 0.048(3) 0.059(3) 0.030(3) 0.001(2) 0.006(2) 0.025(2) C25 0.0427(19) 0.101(3) 0.0233(17) -0.0050(18) 0.0137(15) -0.0274(19) C26 0.063(2) 0.121(3) 0.041(2) 0.002(2) 0.0049(19) -0.039(2) C27 0.066(2) 0.123(3) 0.047(2) -0.001(2) 0.0046(19) -0.040(2) C28 0.059(2) 0.121(3) 0.039(2) -0.010(2) 0.0039(19) -0.034(2) C29 0.067(2) 0.115(3) 0.0323(19) -0.003(2) 0.0041(18) -0.034(2) C30 0.064(2) 0.111(3) 0.0303(19) -0.001(2) 0.0060(17) -0.039(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . P1 . 2.2411(10) yes Pt1 . N1 . 2.164(3) yes Pt1 . C3 . 2.087(4) yes Pt1 . C4 . 2.058(4) yes P1 . C2 . 1.843(4) yes P1 . C19 . 1.825(4) yes P1 . C25 . 1.833(4) yes N1 . C1 . 1.295(5) yes N1 . C5 . 1.441(4) yes C1 . C2 . 1.521(5) yes C1 . C13 . 1.489(5) yes C2 . H21 . 1.000 no C2 . H22 . 1.000 no C3 . H301 . 1.000 no C3 . H302 . 1.000 no C3 . H303 . 1.000 no C4 . H401 . 1.000 no C4 . H402 . 1.000 no C4 . H403 . 1.000 no C5 . C6 . 1.408(5) yes C5 . C10 . 1.389(6) yes C6 . C7 . 1.410(7) yes C6 . C11 . 1.498(8) yes C7 . C8 . 1.379(9) yes C7 . H71 . 1.000 no C8 . C9 . 1.356(9) yes C8 . H81 . 1.000 no C9 . C10 . 1.407(6) yes C9 . H91 . 1.002 no C10 . C12 . 1.488(7) yes C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no C12 . H121 . 1.000 no C12 . H122 . 1.001 no C12 . H123 . 1.001 no C13 . C14 . 1.407(5) yes C13 . C18 . 1.401(5) yes C14 . C15 . 1.390(6) yes C14 . H141 . 1.000 no C15 . C16 . 1.387(6) yes C15 . H151 . 1.000 no C16 . C17 . 1.390(6) yes C16 . H161 . 1.000 no C17 . C18 . 1.391(5) yes C17 . H171 . 1.000 no C18 . H181 . 1.001 no C19 . C20 . 1.380(6) yes C19 . C24 . 1.388(6) yes C20 . C21 . 1.386(7) yes C20 . H201 . 1.000 no C21 . C22 . 1.382(7) yes C21 . H211 . 1.001 no C22 . C23 . 1.364(8) yes C22 . H221 . 1.000 no C23 . C24 . 1.404(8) yes C23 . H231 . 1.000 no C24 . H241 . 1.000 no C25 . C26 . 1.390(6) yes C25 . C30 . 1.357(5) yes C26 . C27 . 1.377(6) yes C26 . H261 . 1.001 no C27 . C28 . 1.381(6) yes C27 . H271 . 1.002 no C28 . C29 . 1.343(6) yes C28 . H281 . 1.000 no C29 . C30 . 1.389(6) yes C29 . H291 . 0.999 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 . Pt1 . N1 . 80.80(9) yes P1 . Pt1 . C3 . 174.09(12) yes N1 . Pt1 . C3 . 94.19(15) yes P1 . Pt1 . C4 . 98.49(14) yes N1 . Pt1 . C4 . 178.98(14) yes C3 . Pt1 . C4 . 86.55(18) yes Pt1 . P1 . C2 . 99.07(12) yes Pt1 . P1 . C19 . 123.50(13) yes C2 . P1 . C19 . 101.97(18) yes Pt1 . P1 . C25 . 118.55(18) yes C2 . P1 . C25 . 105.40(19) yes C19 . P1 . C25 . 105.2(2) yes Pt1 . N1 . C1 . 120.7(2) yes Pt1 . N1 . C5 . 117.1(2) yes C1 . N1 . C5 . 122.2(3) yes N1 . C1 . C2 . 116.5(3) yes N1 . C1 . C13 . 126.9(3) yes C2 . C1 . C13 . 116.6(3) yes C1 . C2 . P1 . 109.6(3) yes C1 . C2 . H21 . 109.495 no P1 . C2 . H21 . 109.382 no C1 . C2 . H22 . 109.512 no P1 . C2 . H22 . 109.398 no H21 . C2 . H22 . 109.481 no Pt1 . C3 . H301 . 109.466 no Pt1 . C3 . H302 . 109.502 no H301 . C3 . H302 . 109.457 no Pt1 . C3 . H303 . 109.485 no H301 . C3 . H303 . 109.428 no H302 . C3 . H303 . 109.489 no Pt1 . C4 . H401 . 109.468 no Pt1 . C4 . H402 . 109.493 no H401 . C4 . H402 . 109.475 no Pt1 . C4 . H403 . 109.472 no H401 . C4 . H403 . 109.440 no H402 . C4 . H403 . 109.480 no N1 . C5 . C6 . 117.5(4) yes N1 . C5 . C10 . 120.1(3) yes C6 . C5 . C10 . 122.2(4) yes C5 . C6 . C7 . 116.7(5) yes C5 . C6 . C11 . 120.9(4) yes C7 . C6 . C11 . 122.3(5) yes C6 . C7 . C8 . 121.7(5) yes C6 . C7 . H71 . 119.139 no C8 . C7 . H71 . 119.118 no C7 . C8 . C9 . 119.7(4) yes C7 . C8 . H81 . 120.168 no C9 . C8 . H81 . 120.100 no C8 . C9 . C10 . 121.9(5) yes C8 . C9 . H91 . 119.148 no C10 . C9 . H91 . 118.958 no C9 . C10 . C5 . 117.7(5) yes C9 . C10 . C12 . 120.4(4) yes C5 . C10 . C12 . 121.9(4) yes C6 . C11 . H111 . 109.426 no C6 . C11 . H112 . 109.450 no H111 . C11 . H112 . 109.481 no C6 . C11 . H113 . 109.454 no H111 . C11 . H113 . 109.476 no H112 . C11 . H113 . 109.541 no C10 . C12 . H121 . 109.560 no C10 . C12 . H122 . 109.537 no H121 . C12 . H122 . 109.440 no C10 . C12 . H123 . 109.490 no H121 . C12 . H123 . 109.424 no H122 . C12 . H123 . 109.377 no C1 . C13 . C14 . 123.7(3) yes C1 . C13 . C18 . 118.0(3) yes C14 . C13 . C18 . 118.2(3) yes C13 . C14 . C15 . 120.2(4) yes C13 . C14 . H141 . 119.887 no C15 . C14 . H141 . 119.892 no C14 . C15 . C16 . 120.9(4) yes C14 . C15 . H151 . 119.547 no C16 . C15 . H151 . 119.519 no C15 . C16 . C17 . 119.4(4) yes C15 . C16 . H161 . 120.303 no C17 . C16 . H161 . 120.263 no C16 . C17 . C18 . 120.1(4) yes C16 . C17 . H171 . 119.888 no C18 . C17 . H171 . 120.016 no C13 . C18 . C17 . 121.1(4) yes C13 . C18 . H181 . 119.420 no C17 . C18 . H181 . 119.474 no P1 . C19 . C20 . 117.5(3) yes P1 . C19 . C24 . 123.8(4) yes C20 . C19 . C24 . 118.7(4) yes C19 . C20 . C21 . 120.6(4) yes C19 . C20 . H201 . 119.722 no C21 . C20 . H201 . 119.699 no C20 . C21 . C22 . 120.8(5) yes C20 . C21 . H211 . 119.621 no C22 . C21 . H211 . 119.561 no C21 . C22 . C23 . 119.2(5) yes C21 . C22 . H221 . 120.424 no C23 . C22 . H221 . 120.404 no C22 . C23 . C24 . 120.5(4) yes C22 . C23 . H231 . 119.763 no C24 . C23 . H231 . 119.698 no C23 . C24 . C19 . 120.2(5) yes C23 . C24 . H241 . 119.915 no C19 . C24 . H241 . 119.867 no P1 . C25 . C26 . 116.8(3) yes P1 . C25 . C30 . 124.3(3) yes C26 . C25 . C30 . 118.5(4) yes C25 . C26 . C27 . 120.0(4) yes C25 . C26 . H261 . 120.018 no C27 . C26 . H261 . 119.998 no C26 . C27 . C28 . 120.0(4) yes C26 . C27 . H271 . 119.975 no C28 . C27 . H271 . 120.019 no C27 . C28 . C29 . 119.4(4) yes C27 . C28 . H281 . 120.235 no C29 . C28 . H281 . 120.361 no C28 . C29 . C30 . 120.4(4) yes C28 . C29 . H291 . 119.810 no C30 . C29 . H291 . 119.760 no C29 . C30 . C25 . 120.7(4) yes #===END