Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # SUBMISSION DETAILS _publ_contact_author_name 'S. Colbran' _publ_contact_author_address ;School of Chemistry University of New South Wales Sydney, NSW 2052, Australia ; _publ_contact_author_email s.colbran@unsw.edu.au _publ_contact_author_fax +61-2-9385-6141 _publ_contact_letter ? _publ_requested_category ? # TITLE AND AUTHOR LIST _publ_section_title ;Rhodium, palladium and platinum complexes of tris(pyridylalkyl)amine and tris(benzimidazolylmethyl)amine N4-tripodal ligands ; _publ_section_title_footnote ? loop_ _publ_author_footnote ? # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; loop_ _publ_author_name 'Stephen Colbran' 'Donald C Craig' 'David G Lonnon' data_[Rh(tmpa)Cl2]Cl.3H2O(DSC27) _database_code_depnum_ccdc_archive 'CCDC 298878' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C18 H18 Cl2 N4 Rh 1+,Cl -1,3(H2 O)' _chemical_formula_sum 'C18 H24 Cl3 N4 O3 Rh' _chemical_formula_iupac ? _chemical_formula_weight 553.7 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.959(4) _cell_length_b 16.246(8) _cell_length_c 16.345(9) _cell_angle_alpha 70.68(4) _cell_angle_beta 83.87(4) _cell_angle_gamma 88.83(3) _cell_volume 2232(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120.0 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6065 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 4 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5818 _reflns_number_gt 4695 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.040 _refine_ls_wR_factor_ref 0.054 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4695 _refine_ls_number_parameters 378 _refine_ls_goodness_of_fit_ref 1.88 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.011 _refine_diff_density_max 1.28 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description Cl/O1 0.38Cl+0.62O Cl/O2 0.39Cl+0.61O Cl/O3 0.64Cl+0.36O Cl/O4 0.59Cl+0.41O loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy RhA 0.76678(5) 0.35235(3) 0.42453(3) 0.0353(2) Uani Rh 1.0 Cl1A 0.8884(2) 0.4017(1) 0.2829(1) 0.0537(4) Uani Cl 1.0 Cl2A 0.7892(2) 0.4940(1) 0.4316(1) 0.0584(5) Uani Cl 1.0 N1A 0.9644(5) 0.3052(3) 0.4700(3) 0.041(1) Uani N 1.0 N2A 0.6589(5) 0.3027(3) 0.5472(3) 0.041(1) Uani N 1.0 N3A 0.5645(5) 0.3692(3) 0.3762(3) 0.040(1) Uani N 1.0 N4A 0.7411(5) 0.2295(3) 0.4231(3) 0.040(1) Uani N 1.0 C1A 0.8971(7) 0.1993(4) 0.4054(5) 0.049(2) Uani C 1.0 C2A 0.9984(7) 0.2288(4) 0.4589(4) 0.044(1) Uani C 1.0 C3A 1.1233(7) 0.1825(4) 0.4917(5) 0.056(2) Uani C 1.0 C4A 1.2118(7) 0.2167(5) 0.5369(5) 0.061(2) Uani C 1.0 C5A 1.1775(7) 0.2942(5) 0.5466(4) 0.057(1) Uani C 1.0 C6A 1.0534(7) 0.3388(4) 0.5128(4) 0.047(1) Uani C 1.0 C7A 0.6687(7) 0.1719(4) 0.5088(5) 0.050(2) Uani C 1.0 C8A 0.6237(7) 0.2179(4) 0.5720(4) 0.043(1) Uani C 1.0 C9A 0.5493(8) 0.1758(5) 0.6531(5) 0.060(2) Uani C 1.0 C10A 0.5068(9) 0.2226(6) 0.7089(5) 0.076(2) Uani C 1.0 C11A 0.5455(9) 0.3096(6) 0.6824(5) 0.074(2) Uani C 1.0 C12A 0.6212(8) 0.3482(5) 0.6010(4) 0.055(2) Uani C 1.0 C13A 0.6461(7) 0.2363(4) 0.3509(5) 0.051(2) Uani C 1.0 C14A 0.5270(7) 0.3027(4) 0.3508(4) 0.041(1) Uani C 1.0 C15A 0.3890(7) 0.3003(5) 0.3196(4) 0.052(2) Uani C 1.0 C16A 0.2923(7) 0.3683(5) 0.3128(5) 0.063(2) Uani C 1.0 C17A 0.3337(8) 0.4352(5) 0.3400(5) 0.062(2) Uani C 1.0 C18A 0.4690(7) 0.4346(4) 0.3712(4) 0.050(2) Uani C 1.0 RhB 0.70872(5) 0.33469(3) 0.00893(3) 0.0368(2) Uani Rh 1.0 Cl1B 0.5694(2) 0.3420(1) 0.1343(1) 0.0562(5) Uani Cl 1.0 Cl2B 0.7646(2) 0.4831(1) -0.0318(1) 0.0642(5) Uani Cl 1.0 N1B 0.5167(5) 0.3475(3) -0.0488(3) 0.043(1) Uani N 1.0 N2B 0.8176(5) 0.3219(3) -0.1024(3) 0.043(2) Uani N 1.0 N3B 0.8863(5) 0.2910(3) 0.0781(3) 0.043(1) Uani N 1.0 N4B 0.6679(5) 0.2049(3) 0.0407(3) 0.041(1) Uani N 1.0 C1B 0.5030(7) 0.1953(4) 0.0422(5) 0.053(2) Uani C 1.0 C2B 0.4436(7) 0.2702(4) -0.0290(4) 0.050(1) Uani C 1.0 C3B 0.3173(8) 0.2627(5) -0.0689(5) 0.069(1) Uani C 1.0 C4B 0.2666(9) 0.3381(6) -0.1267(6) 0.078(1) Uani C 1.0 C5B 0.3354(9) 0.4154(6) -0.1431(5) 0.070(1) Uani C 1.0 C6B 0.4619(7) 0.4193(4) -0.1030(4) 0.054(1) Uani C 1.0 C7B 0.7532(8) 0.1711(4) -0.0247(5) 0.057(2) Uani C 1.0 C8B 0.8113(7) 0.2404(4) -0.1060(4) 0.048(2) Uani C 1.0 C9B 0.8699(9) 0.2224(5) -0.1789(5) 0.069(2) Uani C 1.0 C10B 0.9298(9) 0.2887(7) -0.2501(5) 0.082(3) Uani C 1.0 C11B 0.9357(8) 0.3715(6) -0.2472(5) 0.074(3) Uani C 1.0 C12B 0.8787(7) 0.3872(5) -0.1716(5) 0.056(2) Uani C 1.0 C13B 0.7238(7) 0.1632(4) 0.1283(4) 0.051(2) Uani C 1.0 C14B 0.8698(7) 0.2072(4) 0.1283(4) 0.048(1) Uani C 1.0 C15B 0.9806(8) 0.1655(5) 0.1794(5) 0.059(2) Uani C 1.0 C16B 1.1101(8) 0.2117(5) 0.1788(5) 0.064(2) Uani C 1.0 C17B 1.1243(8) 0.2982(5) 0.1270(5) 0.061(1) Uani C 1.0 C18B 1.0118(7) 0.3354(4) 0.0772(5) 0.051(1) Uani C 1.0 Cl/OW1 0.3916(7) 0.0800(3) 0.3041(5) 0.170(4) Uani Cl/O1 1.0 Cl/OW2 0.4447(10) 0.0463(4) 0.9103(4) 0.203(5) Uani Cl/O2 1.0 Cl/OW3 0.6680(10) 0.0061(4) 0.3829(7) 0.327(7) Uani Cl/O3 1.0 Cl/OW4 0.1711(15) 0.0815(12) 0.8452(12) 0.284(8) Uani Cl/O4 0.5 Cl/OW4' 0.1866(17) 0.0736(12) 0.7478(12) 0.284(8) Uani Cl/O4 0.5 OW1 0.1000(7) 0.0092(4) 0.4048(5) 0.135(3) Uani O 1.0 OW2 0.0949(9) 0.0569(5) 0.0196(7) 0.199(5) Uani O 1.0 OW3 0.7176(10) 0.0023(5) 0.8296(6) 0.186(4) Uani O 1.0 OW4 0.0885(14) -0.0903(7) 0.3075(7) 0.280(6) Uani O 1.0 H1C1A 0.9328 0.2255 0.3420 0.049 Uani H 1.0 H2C1A 0.8975 0.1343 0.4224 0.049 Uani H 1.0 HC3A 1.1483 0.1256 0.4827 0.065 Uani H 1.0 HC4A 1.3010 0.1841 0.5624 0.074 Uani H 1.0 HC5A 1.2426 0.3197 0.5784 0.065 Uani H 1.0 HC6A 1.0293 0.3965 0.5202 0.051 Uani H 1.0 H1C7A 0.7411 0.1255 0.5350 0.050 Uani H 1.0 H2C7A 0.5769 0.1444 0.4984 0.050 Uani H 1.0 HC9A 0.5260 0.1119 0.6716 0.064 Uani H 1.0 HC10A 0.4494 0.1937 0.7671 0.094 Uani H 1.0 HC11A 0.5189 0.3446 0.7218 0.091 Uani H 1.0 HC12A 0.6486 0.4116 0.5817 0.056 Uani H 1.0 H1C13A 0.5979 0.1784 0.3606 0.051 Uani H 1.0 H2C13A 0.7100 0.2549 0.2937 0.051 Uani H 1.0 HC15A 0.3608 0.2496 0.3023 0.058 Uani H 1.0 HC16A 0.1942 0.3691 0.2886 0.078 Uani H 1.0 HC17A 0.2640 0.4848 0.3370 0.076 Uani H 1.0 HC18A 0.4973 0.4839 0.3906 0.055 Uani H 1.0 H1C1B 0.4529 0.1947 0.1001 0.053 Uani H 1.0 H2C1B 0.4803 0.1391 0.0330 0.053 Uani H 1.0 HC3B 0.2656 0.2052 -0.0563 0.084 Uani H 1.0 HC4B 0.1767 0.3351 -0.1570 0.098 Uani H 1.0 HC5B 0.2955 0.4696 -0.1841 0.085 Uani H 1.0 HC6B 0.5129 0.4769 -0.1148 0.058 Uani H 1.0 H1C7B 0.6851 0.1316 -0.0400 0.057 Uani H 1.0 H2C7B 0.8402 0.1372 0.0023 0.057 Uani H 1.0 HC9B 0.8688 0.1612 -0.1801 0.086 Uani H 1.0 HC10B 0.9694 0.2765 -0.3045 0.108 Uani H 1.0 HC11B 0.9805 0.4202 -0.2989 0.092 Uani H 1.0 HC12B 0.8832 0.4476 -0.1686 0.063 Uani H 1.0 H1C13B 0.7400 0.0996 0.1388 0.051 Uani H 1.0 H2C13B 0.6487 0.1707 0.1750 0.051 Uani H 1.0 HC15B 0.9678 0.1027 0.2163 0.070 Uani H 1.0 HC16B 1.1914 0.1828 0.2153 0.075 Uani H 1.0 HC17B 1.2156 0.3331 0.1258 0.072 Uani H 1.0 HC18B 1.0232 0.3977 0.0389 0.056 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RhA 0.0323(3) 0.0334(3) 0.0405(3) 0.0006(2) -0.0063(2) -0.0119(2) Rh Cl1A 0.0413(9) 0.069(1) 0.0430(9) 0.0016(8) -0.0033(7) -0.0090(8) Cl Cl2A 0.063(1) 0.0379(9) 0.075(1) -0.0077(8) -0.0044(9) -0.0203(9) Cl N1A 0.038(1) 0.045(2) 0.039(2) -0.001(1) -0.007(1) -0.013(2) N N2A 0.038(2) 0.040(2) 0.044(2) 0.003(2) -0.011(1) -0.012(1) N N3A 0.035(1) 0.043(2) 0.041(2) 0.005(1) -0.006(1) -0.011(2) N N4A 0.038(3) 0.038(3) 0.047(3) 0.006(2) -0.012(2) -0.019(3) N C1A 0.043(4) 0.047(4) 0.068(5) 0.015(3) -0.023(3) -0.030(4) C C2A 0.037(2) 0.046(2) 0.048(2) 0.004(1) -0.005(1) -0.014(2) C C3A 0.039(2) 0.057(3) 0.066(4) 0.008(2) -0.008(2) -0.012(2) C C4A 0.039(2) 0.072(3) 0.063(3) 0.002(2) -0.013(2) -0.006(3) C C5A 0.042(2) 0.073(3) 0.049(3) -0.008(2) -0.012(2) -0.010(3) C C6A 0.042(2) 0.057(2) 0.043(3) -0.008(2) -0.008(2) -0.014(2) C C7A 0.054(4) 0.033(4) 0.062(5) -0.002(3) -0.007(4) -0.014(3) C C8A 0.037(2) 0.041(2) 0.047(2) -0.001(2) -0.014(1) -0.004(2) C C9A 0.054(3) 0.062(2) 0.050(2) -0.010(2) -0.009(2) -0.001(2) C C10A 0.079(3) 0.090(3) 0.050(2) -0.014(3) 0.004(2) -0.012(2) C C11A 0.083(3) 0.088(3) 0.052(2) -0.007(3) 0.007(2) -0.026(2) C C12A 0.059(3) 0.060(2) 0.049(2) 0.001(2) -0.003(2) -0.023(2) C C13A 0.043(4) 0.057(4) 0.066(5) 0.010(3) -0.022(3) -0.036(4) C C14A 0.034(2) 0.049(2) 0.040(2) 0.001(1) -0.006(1) -0.014(2) C C15A 0.036(2) 0.074(3) 0.045(2) -0.002(2) -0.007(2) -0.019(3) C C16A 0.037(2) 0.091(4) 0.056(3) 0.010(2) -0.013(2) -0.018(3) C C17A 0.043(2) 0.072(3) 0.063(3) 0.021(2) -0.010(2) -0.013(3) C C18A 0.043(2) 0.049(2) 0.053(3) 0.012(2) -0.004(2) -0.012(2) C RhB 0.0363(3) 0.0303(3) 0.0415(3) 0.0014(2) -0.0067(2) -0.0083(2) Rh Cl1B 0.059(1) 0.064(1) 0.048(1) 0.0116(9) -0.0061(8) -0.0220(9) Cl Cl2B 0.067(1) 0.0332(9) 0.090(1) -0.0008(8) -0.017(1) -0.0143(9) Cl N1B 0.038(2) 0.045(2) 0.046(2) 0.007(1) -0.004(2) -0.014(2) N N2B 0.034(2) 0.047(2) 0.045(2) 0.003(2) -0.006(1) -0.009(2) N N3B 0.042(2) 0.039(2) 0.049(2) 0.004(1) -0.008(2) -0.014(2) N N4B 0.046(3) 0.028(3) 0.044(3) -0.002(2) -0.006(2) -0.005(2) N C1B 0.048(4) 0.040(4) 0.065(5) -0.008(3) -0.007(3) -0.011(4) C C2B 0.038(2) 0.055(2) 0.059(2) -0.001(2) -0.006(2) -0.021(2) C C3B 0.045(2) 0.085(3) 0.084(4) -0.001(2) -0.018(2) -0.036(3) C C4B 0.052(2) 0.106(4) 0.085(4) 0.017(2) -0.029(3) -0.040(3) C C5B 0.059(3) 0.087(3) 0.067(3) 0.028(2) -0.024(3) -0.025(3) C C6B 0.051(2) 0.056(2) 0.052(3) 0.018(2) -0.011(2) -0.014(2) C C7B 0.069(5) 0.037(4) 0.066(5) 0.002(3) 0.003(4) -0.022(4) C C8B 0.043(2) 0.053(2) 0.050(2) 0.007(2) -0.007(1) -0.020(2) C C9B 0.067(4) 0.088(3) 0.060(2) 0.016(3) -0.007(2) -0.038(2) C C10B 0.069(4) 0.123(5) 0.052(2) 0.015(4) 0.001(2) -0.031(2) C C11B 0.051(3) 0.105(4) 0.048(2) 0.002(3) 0.000(2) -0.003(2) C C12B 0.039(3) 0.062(2) 0.051(2) -0.002(2) -0.007(2) 0.001(2) C C13B 0.052(4) 0.038(4) 0.053(4) 0.003(3) -0.006(3) 0.000(3) C C14B 0.049(2) 0.042(2) 0.049(2) 0.007(1) -0.010(2) -0.008(2) C C15B 0.058(3) 0.057(2) 0.058(3) 0.016(2) -0.017(2) -0.010(2) C C16B 0.056(2) 0.073(3) 0.067(3) 0.019(2) -0.023(2) -0.024(2) C C17B 0.048(2) 0.068(3) 0.075(3) 0.009(2) -0.021(2) -0.031(3) C C18B 0.043(2) 0.050(2) 0.065(3) 0.003(2) -0.013(2) -0.023(2) C Cl/OW1 0.151(5) 0.093(4) 0.263(8) 0.007(3) -0.066(5) -0.041(4) Cl Cl/OW2 0.352(9) 0.094(4) 0.147(6) -0.019(5) 0.022(6) -0.032(4) Cl Cl/OW3 0.363(9) 0.123(5) 0.568(9) 0.068(5) -0.285(9) -0.144(7) Cl Cl/OW4 0.284(8) 0.284(8) 0.284(8) 0.0045(1) -0.0301(8) -0.094(3) Cl Cl/OW4' 0.284(8) 0.284(8) 0.284(8) 0.0045(1) -0.0301(8) -0.094(3) Cl OW1 0.130(6) 0.095(5) 0.182(8) 0.040(5) -0.069(6) -0.036(5) O OW2 0.152(8) 0.143(8) 0.331(9) 0.049(6) -0.081(9) -0.104(9) O OW3 0.205(9) 0.133(8) 0.199(9) -0.014(7) -0.027(8) -0.024(7) O OW4 0.394(9) 0.267(9) 0.184(9) -0.034(9) 0.057(9) -0.103(9) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RhA Cl1A 2.336(2) 1_555 1_555 no RhA Cl2A 2.355(2) 1_555 1_555 no RhA N1A 2.031(5) 1_555 1_555 no RhA N2A 2.038(5) 1_555 1_555 no RhA N3A 2.031(5) 1_555 1_555 no RhA N4A 2.022(5) 1_555 1_555 no N1A C2A 1.337(8) 1_555 1_555 no N1A C6A 1.347(8) 1_555 1_555 no N2A C8A 1.335(7) 1_555 1_555 no N2A C12A 1.338(8) 1_555 1_555 no N3A C14A 1.339(7) 1_555 1_555 no N3A C18A 1.338(7) 1_555 1_555 no N4A C1A 1.502(7) 1_555 1_555 no N4A C7A 1.491(8) 1_555 1_555 no N4A C13A 1.500(8) 1_555 1_555 no C1A C2A 1.511(8) 1_555 1_555 no C2A C3A 1.391(8) 1_555 1_555 no C3A C4A 1.379(10) 1_555 1_555 no C4A C5A 1.345(10) 1_555 1_555 no C5A C6A 1.378(9) 1_555 1_555 no C7A C8A 1.483(9) 1_555 1_555 no C8A C9A 1.378(9) 1_555 1_555 no C9A C10A 1.389(11) 1_555 1_555 no C10A C11A 1.374(11) 1_555 1_555 no C11A C12A 1.376(10) 1_555 1_555 no C13A C14A 1.501(8) 1_555 1_555 no C14A C15A 1.393(8) 1_555 1_555 no C15A C16A 1.372(9) 1_555 1_555 no C16A C17A 1.376(10) 1_555 1_555 no C17A C18A 1.362(9) 1_555 1_555 no RhB Cl1B 2.320(2) 1_555 1_555 no RhB Cl2B 2.328(2) 1_555 1_555 no RhB N1B 2.023(5) 1_555 1_555 no RhB N2B 2.041(5) 1_555 1_555 no RhB N3B 2.029(5) 1_555 1_555 no RhB N4B 2.029(5) 1_555 1_555 no N1B C2B 1.353(8) 1_555 1_555 no N1B C6B 1.332(8) 1_555 1_555 no N2B C8B 1.349(8) 1_555 1_555 no N2B C12B 1.343(8) 1_555 1_555 no N3B C14B 1.338(7) 1_555 1_555 no N3B C18B 1.345(8) 1_555 1_555 no N4B C1B 1.486(8) 1_555 1_555 no N4B C7B 1.491(8) 1_555 1_555 no N4B C13B 1.503(8) 1_555 1_555 no C1B C2B 1.513(9) 1_555 1_555 no C2B C3B 1.391(9) 1_555 1_555 no C3B C4B 1.379(11) 1_555 1_555 no C4B C5B 1.342(11) 1_555 1_555 no C5B C6B 1.382(10) 1_555 1_555 no C7B C8B 1.480(9) 1_555 1_555 no C8B C9B 1.368(9) 1_555 1_555 no C9B C10B 1.365(11) 1_555 1_555 no C10B C11B 1.363(12) 1_555 1_555 no C11B C12B 1.387(10) 1_555 1_555 no C13B C14B 1.504(9) 1_555 1_555 no C14B C15B 1.384(9) 1_555 1_555 no C15B C16B 1.393(10) 1_555 1_555 no C16B C17B 1.380(10) 1_555 1_555 no C17B C18B 1.366(9) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1A RhA Cl2A 89.15(6) 1_555 1_555 1_555 no Cl1A RhA N1A 89.5(1) 1_555 1_555 1_555 no Cl1A RhA N2A 176.8(1) 1_555 1_555 1_555 no Cl1A RhA N3A 90.2(1) 1_555 1_555 1_555 no Cl1A RhA N4A 93.2(2) 1_555 1_555 1_555 no Cl2A RhA N1A 98.0(1) 1_555 1_555 1_555 no Cl2A RhA N2A 94.1(1) 1_555 1_555 1_555 no Cl2A RhA N3A 96.5(1) 1_555 1_555 1_555 no Cl2A RhA N4A 177.5(1) 1_555 1_555 1_555 no N1A RhA N2A 90.3(2) 1_555 1_555 1_555 no N1A RhA N3A 165.5(2) 1_555 1_555 1_555 no N1A RhA N4A 82.6(2) 1_555 1_555 1_555 no N2A RhA N3A 89.2(2) 1_555 1_555 1_555 no N2A RhA N4A 83.6(2) 1_555 1_555 1_555 no N3A RhA N4A 82.9(2) 1_555 1_555 1_555 no RhA N1A C2A 112.4(4) 1_555 1_555 1_555 no RhA N1A C6A 127.7(4) 1_555 1_555 1_555 no C2A N1A C6A 119.7(5) 1_555 1_555 1_555 no RhA N2A C8A 114.5(4) 1_555 1_555 1_555 no RhA N2A C12A 125.4(4) 1_555 1_555 1_555 no C8A N2A C12A 120.1(6) 1_555 1_555 1_555 no RhA N3A C14A 112.3(4) 1_555 1_555 1_555 no RhA N3A C18A 127.8(4) 1_555 1_555 1_555 no C14A N3A C18A 119.8(5) 1_555 1_555 1_555 no RhA N4A C1A 105.4(4) 1_555 1_555 1_555 no RhA N4A C7A 110.7(4) 1_555 1_555 1_555 no RhA N4A C13A 106.2(4) 1_555 1_555 1_555 no C1A N4A C7A 110.4(5) 1_555 1_555 1_555 no C1A N4A C13A 112.4(5) 1_555 1_555 1_555 no C7A N4A C13A 111.4(5) 1_555 1_555 1_555 no N4A C1A C2A 107.9(5) 1_555 1_555 1_555 no N1A C2A C1A 115.7(5) 1_555 1_555 1_555 no N1A C2A C3A 121.3(6) 1_555 1_555 1_555 no C1A C2A C3A 123.0(6) 1_555 1_555 1_555 no C2A C3A C4A 118.5(7) 1_555 1_555 1_555 no C3A C4A C5A 119.6(6) 1_555 1_555 1_555 no C4A C5A C6A 120.6(7) 1_555 1_555 1_555 no N1A C6A C5A 120.4(6) 1_555 1_555 1_555 no N4A C7A C8A 114.1(5) 1_555 1_555 1_555 no N2A C8A C7A 117.0(5) 1_555 1_555 1_555 no N2A C8A C9A 120.9(6) 1_555 1_555 1_555 no C7A C8A C9A 122.1(6) 1_555 1_555 1_555 no C8A C9A C10A 119.6(7) 1_555 1_555 1_555 no C9A C10A C11A 118.5(7) 1_555 1_555 1_555 no C10A C11A C12A 119.5(7) 1_555 1_555 1_555 no N2A C12A C11A 121.5(7) 1_555 1_555 1_555 no N4A C13A C14A 108.7(5) 1_555 1_555 1_555 no N3A C14A C13A 116.3(5) 1_555 1_555 1_555 no N3A C14A C15A 120.9(6) 1_555 1_555 1_555 no C13A C14A C15A 122.6(6) 1_555 1_555 1_555 no C14A C15A C16A 119.3(7) 1_555 1_555 1_555 no C15A C16A C17A 118.4(6) 1_555 1_555 1_555 no C16A C17A C18A 120.5(7) 1_555 1_555 1_555 no N3A C18A C17A 121.1(6) 1_555 1_555 1_555 no Cl1B RhB Cl2B 89.55(7) 1_555 1_555 1_555 no Cl1B RhB N1B 89.0(1) 1_555 1_555 1_555 no Cl1B RhB N2B 175.3(1) 1_555 1_555 1_555 no Cl1B RhB N3B 89.7(2) 1_555 1_555 1_555 no Cl1B RhB N4B 92.9(2) 1_555 1_555 1_555 no Cl2B RhB N1B 96.6(2) 1_555 1_555 1_555 no Cl2B RhB N2B 93.9(2) 1_555 1_555 1_555 no Cl2B RhB N3B 97.2(1) 1_555 1_555 1_555 no Cl2B RhB N4B 177.4(2) 1_555 1_555 1_555 no N1B RhB N2B 87.5(2) 1_555 1_555 1_555 no N1B RhB N3B 166.1(2) 1_555 1_555 1_555 no N1B RhB N4B 84.3(2) 1_555 1_555 1_555 no N2B RhB N3B 93.0(2) 1_555 1_555 1_555 no N2B RhB N4B 83.7(2) 1_555 1_555 1_555 no N3B RhB N4B 82.0(2) 1_555 1_555 1_555 no RhB N1B C2B 112.0(4) 1_555 1_555 1_555 no RhB N1B C6B 128.3(5) 1_555 1_555 1_555 no C2B N1B C6B 119.7(6) 1_555 1_555 1_555 no RhB N2B C8B 113.8(4) 1_555 1_555 1_555 no RhB N2B C12B 125.9(5) 1_555 1_555 1_555 no C8B N2B C12B 120.0(6) 1_555 1_555 1_555 no RhB N3B C14B 112.5(4) 1_555 1_555 1_555 no RhB N3B C18B 127.8(4) 1_555 1_555 1_555 no C14B N3B C18B 119.7(5) 1_555 1_555 1_555 no RhB N4B C1B 105.8(4) 1_555 1_555 1_555 no RhB N4B C7B 109.9(4) 1_555 1_555 1_555 no RhB N4B C13B 105.8(4) 1_555 1_555 1_555 no C1B N4B C7B 112.1(5) 1_555 1_555 1_555 no C1B N4B C13B 113.3(5) 1_555 1_555 1_555 no C7B N4B C13B 109.6(5) 1_555 1_555 1_555 no N4B C1B C2B 110.4(5) 1_555 1_555 1_555 no N1B C2B C1B 115.5(5) 1_555 1_555 1_555 no N1B C2B C3B 121.4(6) 1_555 1_555 1_555 no C1B C2B C3B 123.0(6) 1_555 1_555 1_555 no C2B C3B C4B 117.1(7) 1_555 1_555 1_555 no C3B C4B C5B 121.4(7) 1_555 1_555 1_555 no C4B C5B C6B 119.4(7) 1_555 1_555 1_555 no N1B C6B C5B 120.9(7) 1_555 1_555 1_555 no N4B C7B C8B 113.7(5) 1_555 1_555 1_555 no N2B C8B C7B 116.5(6) 1_555 1_555 1_555 no N2B C8B C9B 120.9(6) 1_555 1_555 1_555 no C7B C8B C9B 122.3(6) 1_555 1_555 1_555 no C8B C9B C10B 119.3(8) 1_555 1_555 1_555 no C9B C10B C11B 120.1(7) 1_555 1_555 1_555 no C10B C11B C12B 119.1(7) 1_555 1_555 1_555 no N2B C12B C11B 120.4(7) 1_555 1_555 1_555 no N4B C13B C14B 108.0(5) 1_555 1_555 1_555 no N3B C14B C13B 116.4(5) 1_555 1_555 1_555 no N3B C14B C15B 120.8(6) 1_555 1_555 1_555 no C13B C14B C15B 122.7(6) 1_555 1_555 1_555 no C14B C15B C16B 119.4(7) 1_555 1_555 1_555 no C15B C16B C17B 118.8(6) 1_555 1_555 1_555 no C16B C17B C18B 119.1(7) 1_555 1_555 1_555 no N3B C18B C17B 122.3(6) 1_555 1_555 1_555 no #===END data_DSC77[Rh(pmea)Cl2][PF6].CH3CN _database_code_depnum_ccdc_archive 'CCDC 298879' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C19 H20 Cl2 N4 Rh 1+,F6 P 1-,C2 H3 N' _chemical_formula_sum 'C21 H23 Cl2 F6 N5 P Rh' _chemical_formula_iupac ? _chemical_formula_weight 664.2 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 13.427(7) _cell_length_b 12.607(4) _cell_length_c 15.476(8) _cell_angle_alpha 90 _cell_angle_beta 101.84(2) _cell_angle_gamma 90 _cell_volume 2564(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.72 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328.0 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4698 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 4496 _reflns_number_gt 2596 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.057 _refine_ls_wR_factor_ref 0.067 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2596 _refine_ls_number_parameters 282 _refine_ls_goodness_of_fit_ref 1.62 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.006 _refine_diff_density_max 1.32 _refine_diff_density_min -1.24 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Rh 0.39558(5) 0.71213(5) 0.27540(4) 0.0407(2) Uani Rh 1.0 Cl1 0.4745(2) 0.8139(2) 0.3996(1) 0.0539(6) Uani Cl 1.0 Cl2 0.4018(2) 0.8602(2) 0.1857(2) 0.0659(7) Uani Cl 1.0 N1 0.5327(5) 0.6642(5) 0.2516(4) 0.046(2) Uani N 1.0 N2 0.3799(5) 0.5822(5) 0.3484(4) 0.041(2) Uani N 1.0 N3 0.2498(6) 0.7568(6) 0.2858(5) 0.055(2) Uani N 1.0 N4 0.3503(6) 0.6090(5) 0.1706(4) 0.053(2) Uani N 1.0 C1 0.4234(8) 0.6237(8) 0.1119(6) 0.061(3) Uani C 1.0 C2 0.5293(8) 0.6289(7) 0.1688(6) 0.056(2) Uani C 1.0 C3 0.6154(9) 0.5989(8) 0.1407(7) 0.073(3) Uani C 1.0 C4 0.7091(9) 0.6034(8) 0.1983(9) 0.075(3) Uani C 1.0 C5 0.7110(8) 0.6375(8) 0.2810(8) 0.068(3) Uani C 1.0 C6 0.6236(7) 0.6690(7) 0.3081(6) 0.054(2) Uani C 1.0 C7 0.3628(8) 0.4975(7) 0.2060(6) 0.063(3) Uani C 1.0 C8 0.3552(7) 0.4916(7) 0.3017(6) 0.053(2) Uani C 1.0 C9 0.3319(8) 0.4006(7) 0.3404(7) 0.068(3) Uani C 1.0 C10 0.3346(9) 0.3988(8) 0.4291(8) 0.078(3) Uani C 1.0 C11 0.3595(9) 0.4910(8) 0.4777(7) 0.076(3) Uani C 1.0 C12 0.3812(7) 0.5811(7) 0.4356(5) 0.054(2) Uani C 1.0 C13 0.2454(9) 0.6291(9) 0.1221(7) 0.078(3) Uani C 1.0 C14 0.1694(10) 0.6147(12) 0.1777(9) 0.115(5) Uani C 1.0 C15 0.1635(9) 0.7098(11) 0.2407(9) 0.105(5) Uani C 1.0 C16 0.0701(10) 0.7405(18) 0.2532(11) 0.154(7) Uani C 1.0 C17 0.0595(11) 0.8202(14) 0.3091(11) 0.119(5) Uani C 1.0 C18 0.1433(11) 0.8606(11) 0.3571(8) 0.094(4) Uani C 1.0 C19 0.2359(8) 0.8278(9) 0.3430(7) 0.077(3) Uani C 1.0 P1 0.1340(5) 0.1771(8) 0.5078(7) 0.063(3) Uani P 0.55 F1 0.0169(6) 0.1870(18) 0.4947(14) 0.164(6) Uani F 0.55 F2 0.1398(12) 0.1403(14) 0.6042(9) 0.155(4) Uani F 0.55 F3 0.1458(14) 0.2938(8) 0.5393(10) 0.161(6) Uani F 0.55 F4 0.2510(6) 0.1671(14) 0.5209(8) 0.101(3) Uani F 0.55 F5 0.1281(11) 0.2139(14) 0.4114(7) 0.154(4) Uani F 0.55 F6 0.1221(15) 0.0603(10) 0.4763(13) 0.198(7) Uani F 0.55 P1' 0.1361(7) 0.1597(11) 0.5010(10) 0.067(3) Uani P 0.45 F1' 0.0365(9) 0.2212(21) 0.5019(16) 0.132(5) Uani F 0.45 F2' 0.1432(15) 0.1283(17) 0.5989(12) 0.152(4) Uani F 0.45 F3' 0.1987(14) 0.2613(12) 0.5307(12) 0.134(4) Uani F 0.45 F4' 0.2357(12) 0.0981(15) 0.5002(11) 0.117(6) Uani F 0.45 F5' 0.1289(15) 0.1911(18) 0.4032(9) 0.167(4) Uani F 0.45 F6' 0.0735(17) 0.0581(16) 0.4713(19) 0.258(8) Uani F 0.45 N1An 0.1224(50) 0.5841(51) 0.5392(58) 0.472(9) Uani N 0.5 C1An 0.1009(33) 0.5541(38) 0.4641(56) 0.472(9) Uani C 0.5 C2An 0.0757(64) 0.5189(73) 0.3763(59) 0.472(9) Uani C 0.5 N1An' -0.0421(55) 0.5114(45) 0.3511(55) 0.472(9) Uani N 0.5 C1An' 0.0132(43) 0.5196(38) 0.4223(51) 0.472(9) Uani C 0.5 C2An' 0.0778(70) 0.5291(69) 0.5056(55) 0.472(9) Uani C 0.5 H1C1 0.4079 0.6911 0.0777 0.061 Uani H 1.0 H2C1 0.4185 0.5626 0.0700 0.061 Uani H 1.0 HC3 0.6106 0.5739 0.0787 0.073 Uani H 1.0 HC4 0.7730 0.5822 0.1791 0.075 Uani H 1.0 HC5 0.7775 0.6400 0.3242 0.068 Uani H 1.0 HC6 0.6278 0.6955 0.3696 0.054 Uani H 1.0 H1C7 0.4310 0.4703 0.2000 0.063 Uani H 1.0 H2C7 0.3083 0.4520 0.1705 0.063 Uani H 1.0 HC9 0.3128 0.3353 0.3040 0.068 Uani H 1.0 HC10 0.3190 0.3320 0.4586 0.078 Uani H 1.0 HC11 0.3616 0.4916 0.5427 0.076 Uani H 1.0 HC12 0.3983 0.6477 0.4705 0.054 Uani H 1.0 H1C13 0.2294 0.5789 0.0711 0.078 Uani H 1.0 H2C13 0.2410 0.7037 0.0996 0.078 Uani H 1.0 H1C14 0.1874 0.5494 0.2143 0.115 Uani H 1.0 H2C14 0.1010 0.6052 0.1382 0.115 Uani H 1.0 HC16 0.0081 0.7032 0.2204 0.154 Uani H 1.0 HC17 -0.0092 0.8474 0.3137 0.119 Uani H 1.0 HC18 0.1393 0.9147 0.4035 0.094 Uani H 1.0 HC19 0.2979 0.8613 0.3798 0.077 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Rh 0.0535(4) 0.0373(3) 0.0279(3) -0.0009(4) 0.0008(2) -0.0018(3) Rh Cl1 0.069(1) 0.051(1) 0.039(1) -0.011(1) 0.004(1) -0.0119(9) Cl Cl2 0.095(2) 0.052(1) 0.048(1) 0.007(1) 0.006(1) 0.012(1) Cl N1 0.064(5) 0.041(4) 0.034(4) 0.002(4) 0.010(4) 0.005(3) N N2 0.051(4) 0.038(4) 0.031(3) 0.000(3) 0.003(3) 0.002(3) N N3 0.054(5) 0.057(5) 0.052(4) 0.001(4) 0.007(4) -0.005(4) N N4 0.068(5) 0.052(4) 0.033(4) 0.002(4) -0.004(4) -0.003(3) N C1 0.081(7) 0.064(6) 0.037(5) -0.001(5) 0.008(5) -0.003(4) C C2 0.079(7) 0.044(5) 0.048(5) -0.004(5) 0.023(5) -0.001(4) C C3 0.095(9) 0.058(6) 0.077(8) -0.001(6) 0.045(7) -0.004(5) C C4 0.074(8) 0.055(6) 0.102(9) -0.005(6) 0.035(7) -0.012(6) C C5 0.060(7) 0.053(6) 0.093(8) -0.003(5) 0.017(6) -0.002(6) C C6 0.064(6) 0.049(5) 0.047(5) -0.002(5) 0.005(5) 0.001(4) C C7 0.080(8) 0.047(5) 0.056(6) -0.006(5) 0.001(5) -0.014(5) C C8 0.060(6) 0.047(5) 0.048(5) -0.005(5) 0.005(5) -0.007(4) C C9 0.092(8) 0.044(6) 0.070(7) -0.010(5) 0.018(6) 0.003(5) C C10 0.102(9) 0.057(6) 0.080(8) -0.023(6) 0.029(7) 0.007(6) C C11 0.105(9) 0.067(6) 0.056(6) -0.007(6) 0.020(6) 0.015(6) C C12 0.068(6) 0.057(6) 0.035(5) -0.006(5) 0.004(4) -0.001(4) C C13 0.077(7) 0.093(8) 0.054(6) -0.004(7) -0.006(6) -0.013(6) C C14 0.089(9) 0.136(9) 0.098(9) -0.009(9) -0.030(8) -0.039(9) C C15 0.068(8) 0.134(9) 0.100(9) 0.032(8) -0.013(7) -0.047(9) C C16 0.060(9) 0.252(9) 0.134(9) 0.043(9) -0.015(8) -0.071(9) C C17 0.084(9) 0.148(9) 0.125(9) 0.027(9) 0.026(9) -0.036(9) C C18 0.089(9) 0.107(9) 0.086(9) 0.011(8) 0.018(7) -0.032(8) C C19 0.070(7) 0.084(8) 0.073(7) 0.014(6) 0.008(6) -0.027(6) C P1 0.060(3) 0.061(6) 0.065(4) 0.009(3) 0.006(2) 0.004(3) P F1 0.061(3) 0.250(9) 0.177(8) 0.023(4) 0.015(2) 0.040(9) F F2 0.143(5) 0.229(8) 0.110(3) 0.092(5) 0.064(3) 0.090(4) F F3 0.196(9) 0.072(7) 0.208(7) 0.030(4) 0.023(8) -0.039(3) F F4 0.061(2) 0.135(7) 0.105(4) 0.020(3) 0.013(2) 0.021(3) F F5 0.144(5) 0.247(9) 0.075(5) 0.104(6) 0.029(2) 0.055(3) F F6 0.199(9) 0.088(4) 0.287(8) -0.028(5) 0.004(9) -0.068(4) F P1' 0.063(3) 0.062(5) 0.073(4) 0.005(3) 0.004(2) 0.000(3) P F1' 0.079(3) 0.201(9) 0.119(6) 0.061(6) 0.024(3) 0.040(6) F F2' 0.140(5) 0.208(7) 0.124(3) 0.081(5) 0.067(3) 0.097(4) F F3' 0.125(6) 0.072(7) 0.195(6) -0.021(3) 0.010(4) -0.020(3) F F4' 0.128(6) 0.120(6) 0.107(6) 0.072(7) 0.031(5) 0.011(4) F F5' 0.155(6) 0.279(9) 0.062(5) 0.111(6) 0.012(2) 0.022(3) F F6' 0.201(9) 0.144(6) 0.399(9) -0.086(9) -0.008(9) -0.079(7) F N1An 0.262(9) 0.284(9) 0.777(9) 0.075(9) -0.112(9) -0.159(9) N C1An 0.262(9) 0.284(9) 0.777(9) 0.075(9) -0.112(9) -0.159(9) C C2An 0.262(9) 0.284(9) 0.777(9) 0.075(9) -0.112(9) -0.159(9) C N1An' 0.262(9) 0.284(9) 0.777(9) 0.075(9) -0.112(9) -0.159(9) N C1An' 0.262(9) 0.284(9) 0.777(9) 0.075(9) -0.112(9) -0.159(9) C C2An' 0.262(9) 0.284(9) 0.777(9) 0.075(9) -0.112(9) -0.159(9) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh Cl1 2.371(2) 1_555 1_555 no Rh Cl2 2.338(2) 1_555 1_555 no Rh N1 2.042(7) 1_555 1_555 no Rh N2 2.025(6) 1_555 1_555 no Rh N3 2.075(7) 1_555 1_555 no Rh N4 2.070(7) 1_555 1_555 no N1 C2 1.349(10) 1_555 1_555 no N1 C6 1.349(11) 1_555 1_555 no N2 C8 1.357(10) 1_555 1_555 no N2 C12 1.345(9) 1_555 1_555 no N3 C15 1.360(13) 1_555 1_555 no N3 C19 1.299(12) 1_555 1_555 no N4 C1 1.479(11) 1_555 1_555 no N4 C7 1.505(11) 1_555 1_555 no N4 C13 1.476(12) 1_555 1_555 no C1 C2 1.514(13) 1_555 1_555 no C2 C3 1.368(13) 1_555 1_555 no C3 C4 1.386(15) 1_555 1_555 no C4 C5 1.345(15) 1_555 1_555 no C5 C6 1.382(13) 1_555 1_555 no C7 C8 1.508(12) 1_555 1_555 no C8 C9 1.360(12) 1_555 1_555 no C9 C10 1.366(14) 1_555 1_555 no C10 C11 1.387(14) 1_555 1_555 no C11 C12 1.370(12) 1_555 1_555 no C13 C14 1.475(18) 1_555 1_555 no C14 C15 1.558(17) 1_555 1_555 no C15 C16 1.363(18) 1_555 1_555 no C16 C17 1.352(20) 1_555 1_555 no C17 C18 1.317(18) 1_555 1_555 no C18 C19 1.370(15) 1_555 1_555 no P1 F1 1.549(3) 1_555 1_555 no N1An C1An 1.200(10) 1_555 1_555 no C1An C2An 1.403(10) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Rh Cl2 89.14(8) 1_555 1_555 1_555 no Cl1 Rh N1 92.1(2) 1_555 1_555 1_555 no Cl1 Rh N2 93.8(2) 1_555 1_555 1_555 no Cl1 Rh N3 93.6(2) 1_555 1_555 1_555 no Cl1 Rh N4 170.0(2) 1_555 1_555 1_555 no Cl2 Rh N1 89.2(2) 1_555 1_555 1_555 no Cl2 Rh N2 175.9(2) 1_555 1_555 1_555 no Cl2 Rh N3 88.8(2) 1_555 1_555 1_555 no Cl2 Rh N4 94.4(2) 1_555 1_555 1_555 no N1 Rh N2 93.5(3) 1_555 1_555 1_555 no N1 Rh N3 174.0(3) 1_555 1_555 1_555 no N1 Rh N4 78.7(3) 1_555 1_555 1_555 no N2 Rh N3 88.2(3) 1_555 1_555 1_555 no N2 Rh N4 83.2(3) 1_555 1_555 1_555 no N3 Rh N4 95.8(3) 1_555 1_555 1_555 no Rh N1 C2 114.4(6) 1_555 1_555 1_555 no Rh N1 C6 126.8(6) 1_555 1_555 1_555 no C2 N1 C6 118.7(8) 1_555 1_555 1_555 no Rh N2 C8 115.2(5) 1_555 1_555 1_555 no Rh N2 C12 125.9(5) 1_555 1_555 1_555 no C8 N2 C12 118.5(7) 1_555 1_555 1_555 no Rh N3 C15 124.1(7) 1_555 1_555 1_555 no Rh N3 C19 120.6(7) 1_555 1_555 1_555 no C15 N3 C19 115.1(9) 1_555 1_555 1_555 no Rh N4 C1 106.1(5) 1_555 1_555 1_555 no Rh N4 C7 108.0(5) 1_555 1_555 1_555 no Rh N4 C13 112.8(6) 1_555 1_555 1_555 no C1 N4 C7 107.6(7) 1_555 1_555 1_555 no C1 N4 C13 110.5(7) 1_555 1_555 1_555 no C7 N4 C13 111.6(8) 1_555 1_555 1_555 no N4 C1 C2 108.1(7) 1_555 1_555 1_555 no N1 C2 C1 114.3(8) 1_555 1_555 1_555 no N1 C2 C3 121.8(9) 1_555 1_555 1_555 no C1 C2 C3 123.9(9) 1_555 1_555 1_555 no C2 C3 C4 120.0(10) 1_555 1_555 1_555 no C3 C4 C5 117.5(10) 1_555 1_555 1_555 no C4 C5 C6 121.9(10) 1_555 1_555 1_555 no N1 C6 C5 120.1(9) 1_555 1_555 1_555 no N4 C7 C8 112.3(7) 1_555 1_555 1_555 no N2 C8 C7 115.1(7) 1_555 1_555 1_555 no N2 C8 C9 122.0(8) 1_555 1_555 1_555 no C7 C8 C9 122.8(8) 1_555 1_555 1_555 no C8 C9 C10 119.7(9) 1_555 1_555 1_555 no C9 C10 C11 119.0(9) 1_555 1_555 1_555 no C10 C11 C12 119.2(9) 1_555 1_555 1_555 no N2 C12 C11 121.7(8) 1_555 1_555 1_555 no N4 C13 C14 112.6(9) 1_555 1_555 1_555 no C13 C14 C15 113.6(11) 1_555 1_555 1_555 no N3 C15 C14 120.6(10) 1_555 1_555 1_555 no N3 C15 C16 121.0(12) 1_555 1_555 1_555 no C14 C15 C16 118.3(13) 1_555 1_555 1_555 no C15 C16 C17 121.6(15) 1_555 1_555 1_555 no C16 C17 C18 117.2(13) 1_555 1_555 1_555 no C17 C18 C19 119.5(11) 1_555 1_555 1_555 no N3 C19 C18 125.3(10) 1_555 1_555 1_555 no N1An C1An C2An 180.0 1_555 1_555 1_555 no #===END data_Rh(tbima)(DSC101) _database_code_depnum_ccdc_archive 'CCDC 298880' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C24 H21 Cl2 Rh N7 1+,Cl -1,C2 H6 O S,H2 O' _chemical_formula_sum 'C26 H29 Cl3 N7 O2 Rh S' _chemical_formula_iupac ? _chemical_formula_weight 712.9 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 10.240(4) _cell_length_b 13.863(5) _cell_length_c 20.939(9) _cell_angle_alpha 90 _cell_angle_beta 101.65(2) _cell_angle_gamma 90 _cell_volume 2911(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.63 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448.0 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.92 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5421 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5113 _reflns_number_gt 3784 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.044 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3784 _refine_ls_number_parameters 347 _refine_ls_goodness_of_fit_ref 1.36 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.013 _refine_diff_density_max 0.54 _refine_diff_density_min -0.83 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Rh 0.44554(3) 0.26216(2) 0.31736(1) 0.0313(1) Uani Rh 1.0 Cl1 0.37278(11) 0.38479(8) 0.24117(5) 0.0449(3) Uani Cl 1.0 Cl2 0.49867(11) 0.17032(8) 0.23288(5) 0.0433(3) Uani Cl 1.0 N1 0.1736(4) 0.0548(3) 0.3330(2) 0.0472(9) Uani N 1.0 N2 0.2696(3) 0.1892(3) 0.3086(2) 0.0387(8) Uani N 1.0 N3 0.8396(3) 0.2594(3) 0.3998(2) 0.0438(9) Uani N 1.0 N4 0.6404(3) 0.3008(3) 0.3446(2) 0.0365(8) Uani N 1.0 N5 0.4056(4) 0.3270(3) 0.5014(2) 0.0436(9) Uani N 1.0 N6 0.4074(3) 0.3325(2) 0.3962(2) 0.0349(8) Uani N 1.0 N7 0.5077(3) 0.1528(2) 0.3848(2) 0.0382(8) Uani N 1.0 C1 0.4252(4) 0.0655(3) 0.3613(2) 0.044(1) Uani C 1.0 C2 0.2877(4) 0.1025(3) 0.3359(2) 0.040(1) Uani C 1.0 C3 0.0719(5) 0.1141(4) 0.3018(2) 0.048(1) Uani C 1.0 C4 -0.0656(5) 0.1000(4) 0.2842(2) 0.058(1) Uani C 1.0 C5 -0.1379(5) 0.1749(5) 0.2517(3) 0.066(2) Uani C 1.0 C6 -0.0786(5) 0.2624(4) 0.2373(3) 0.063(2) Uani C 1.0 C7 0.0582(5) 0.2756(4) 0.2544(2) 0.052(1) Uani C 1.0 C8 0.1326(4) 0.1998(3) 0.2870(2) 0.041(1) Uani C 1.0 C9 0.6537(4) 0.1358(3) 0.3869(2) 0.044(1) Uani C 1.0 C10 0.7129(4) 0.2320(3) 0.3780(2) 0.037(1) Uani C 1.0 C11 0.8505(4) 0.3531(3) 0.3788(2) 0.044(1) Uani C 1.0 C12 0.9577(4) 0.4159(4) 0.3870(2) 0.053(1) Uani C 1.0 C13 0.9319(5) 0.5068(4) 0.3605(3) 0.059(1) Uani C 1.0 C14 0.8049(5) 0.5339(4) 0.3275(2) 0.052(1) Uani C 1.0 C15 0.6985(4) 0.4709(3) 0.3179(2) 0.041(1) Uani C 1.0 C16 0.7247(4) 0.3795(3) 0.3438(2) 0.036(1) Uani C 1.0 C17 0.4856(5) 0.1811(3) 0.4507(2) 0.046(1) Uani C 1.0 C18 0.4332(4) 0.2805(3) 0.4494(2) 0.039(1) Uani C 1.0 C19 0.3609(4) 0.4180(3) 0.4805(2) 0.041(1) Uani C 1.0 C20 0.3193(5) 0.4953(4) 0.5131(2) 0.054(1) Uani C 1.0 C21 0.2806(5) 0.5779(4) 0.4773(3) 0.055(1) Uani C 1.0 C22 0.2857(5) 0.5836(3) 0.4114(3) 0.053(1) Uani C 1.0 C23 0.3250(4) 0.5055(3) 0.3780(2) 0.043(1) Uani C 1.0 C24 0.3619(4) 0.4225(3) 0.4137(2) 0.0348(9) Uani C 1.0 Cl3 0.23776(15) -0.12011(11) 0.42893(7) 0.0745(4) Uani Cl 1.0 S1D 1.15600(15) 0.16145(12) 0.51783(8) 0.0778(7) Uani S 1.0 O1D 1.0532(4) 0.1597(3) 0.4576(2) 0.096(2) Uani O 1.0 C2D 1.1141(8) 0.2524(5) 0.5677(3) 0.114(1) Uani C 1.0 C1D 1.1222(7) 0.0676(4) 0.5676(3) 0.102(1) Uani C 1.0 OW1 0.4890(4) 0.1972(3) 0.6035(2) 0.075(1) Uani O 1.0 HN1 0.1635 -0.0114 0.3503 0.047 Uani H 1.0 HN3 0.9124 0.2197 0.4263 0.044 Uani H 1.0 HN5 0.4154 0.3007 0.5466 0.044 Uani H 1.0 H1C1 0.4254 0.0195 0.3981 0.044 Uani H 1.0 H2C1 0.4605 0.0323 0.3259 0.044 Uani H 1.0 HC4 -0.1090 0.0390 0.2945 0.058 Uani H 1.0 HC5 -0.2366 0.1674 0.2377 0.066 Uani H 1.0 HC6 -0.1361 0.3153 0.2144 0.063 Uani H 1.0 HC7 0.1015 0.3366 0.2438 0.052 Uani H 1.0 H1C9 0.6655 0.0911 0.3510 0.044 Uani H 1.0 H2C9 0.6971 0.1075 0.4299 0.044 Uani H 1.0 HC12 1.0486 0.3965 0.4108 0.053 Uani H 1.0 HC13 1.0064 0.5545 0.3650 0.059 Uani H 1.0 HC14 0.7906 0.6012 0.3104 0.052 Uani H 1.0 HC15 0.6078 0.4902 0.2937 0.041 Uani H 1.0 H1C17 0.5722 0.1775 0.4828 0.046 Uani H 1.0 H2C17 0.4201 0.1358 0.4641 0.046 Uani H 1.0 HC20 0.3172 0.4916 0.5606 0.054 Uani H 1.0 HC21 0.2483 0.6347 0.4991 0.055 Uani H 1.0 HC22 0.2605 0.6454 0.3875 0.053 Uani H 1.0 HC23 0.3264 0.5092 0.3305 0.043 Uani H 1.0 H1C1D 1.1263 0.3167 0.5481 0.196 Uani H 1.0 H2C1D 1.0190 0.2446 0.5716 0.114 Uani H 1.0 H3C1D 1.1732 0.2479 0.6119 0.134 Uani H 1.0 H1C2D 1.1399 0.0044 0.5479 0.154 Uani H 1.0 H2C2D 1.1807 0.0739 0.6118 0.133 Uani H 1.0 H3C2D 1.0266 0.0707 0.5715 0.124 Uani H 1.0 H1OW1 0.5002 0.2373 0.6440 0.075 Uani H 1.0 H2OW1 0.5784 0.1759 0.5967 0.075 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Rh 0.0282(2) 0.0332(2) 0.0317(2) 0.0017(1) 0.0041(1) 0.0005(1) Rh Cl1 0.0477(7) 0.0459(6) 0.0387(6) 0.0059(5) 0.0032(5) 0.0062(5) Cl Cl2 0.0422(6) 0.0449(6) 0.0443(6) -0.0005(5) 0.0119(5) -0.0077(5) Cl N1 0.043(2) 0.052(2) 0.048(2) -0.014(2) 0.013(2) 0.001(2) N N2 0.031(2) 0.046(2) 0.038(2) -0.002(2) 0.005(2) -0.002(2) N N3 0.032(2) 0.049(2) 0.048(2) 0.006(2) 0.001(2) 0.001(2) N N4 0.029(2) 0.041(2) 0.038(2) -0.001(2) 0.001(2) -0.002(2) N N5 0.050(2) 0.051(2) 0.032(2) 0.000(2) 0.011(2) 0.002(2) N N6 0.036(2) 0.039(2) 0.030(2) 0.002(2) 0.008(2) -0.001(2) N N7 0.037(2) 0.036(2) 0.039(2) 0.003(2) 0.003(2) 0.005(2) N C1 0.042(3) 0.035(3) 0.053(3) -0.002(2) 0.006(2) 0.008(2) C C2 0.039(3) 0.039(3) 0.042(3) -0.002(2) 0.007(2) 0.000(2) C C3 0.041(3) 0.063(3) 0.040(3) -0.007(2) 0.010(2) -0.008(2) C C4 0.035(3) 0.093(4) 0.049(3) -0.019(3) 0.011(2) -0.014(3) C C5 0.032(3) 0.117(5) 0.048(3) -0.002(3) 0.004(2) -0.014(3) C C6 0.039(3) 0.096(5) 0.051(3) 0.019(3) 0.004(2) -0.004(3) C C7 0.041(3) 0.064(3) 0.049(3) 0.006(2) 0.006(2) -0.004(3) C C8 0.035(2) 0.053(3) 0.034(2) 0.001(2) 0.007(2) -0.008(2) C C9 0.036(3) 0.040(3) 0.053(3) 0.009(2) 0.003(2) 0.005(2) C C10 0.029(2) 0.040(2) 0.041(2) 0.003(2) 0.003(2) -0.001(2) C C11 0.034(3) 0.054(3) 0.043(3) -0.001(2) 0.007(2) -0.005(2) C C12 0.033(3) 0.067(3) 0.057(3) -0.010(2) 0.004(2) -0.008(3) C C13 0.052(3) 0.063(4) 0.064(3) -0.024(3) 0.013(3) -0.003(3) C C14 0.058(3) 0.053(3) 0.046(3) -0.010(3) 0.013(2) 0.004(2) C C15 0.045(3) 0.045(3) 0.032(2) -0.004(2) 0.007(2) 0.004(2) C C16 0.033(2) 0.044(3) 0.030(2) -0.004(2) 0.008(2) -0.004(2) C C17 0.056(3) 0.046(3) 0.036(3) 0.011(2) 0.008(2) 0.008(2) C C18 0.036(2) 0.045(3) 0.037(2) -0.002(2) 0.008(2) 0.000(2) C C19 0.037(3) 0.048(3) 0.038(2) -0.002(2) 0.008(2) -0.004(2) C C20 0.054(3) 0.066(3) 0.043(3) -0.006(3) 0.017(2) -0.018(3) C C21 0.056(3) 0.053(3) 0.056(3) 0.001(3) 0.013(3) -0.016(3) C C22 0.046(3) 0.043(3) 0.065(3) 0.006(2) 0.003(2) -0.004(2) C C23 0.044(3) 0.043(3) 0.043(3) 0.005(2) 0.009(2) -0.004(2) C C24 0.030(2) 0.040(2) 0.034(2) -0.001(2) 0.006(2) -0.007(2) C Cl3 0.0625(9) 0.087(1) 0.0705(9) 0.0096(8) 0.0063(7) 0.0229(8) Cl S1D 0.0562(9) 0.091(1) 0.084(1) 0.0037(8) 0.0089(7) 0.0102(8) S O1D 0.088(3) 0.119(3) 0.074(1) 0.047(3) 0.0022(9) 0.016(1) O C2D 0.137(6) 0.081(2) 0.117(3) 0.008(2) 0.009(4) -0.009(2) C C1D 0.131(4) 0.082(2) 0.093(2) 0.031(2) 0.018(2) 0.027(2) C OW1 0.093(3) 0.088(3) 0.044(2) 0.013(2) 0.018(2) 0.004(2) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh Cl1 2.347(1) 1_555 1_555 no Rh Cl2 2.331(1) 1_555 1_555 no Rh N2 2.041(3) 1_555 1_555 no Rh N4 2.033(3) 1_555 1_555 no Rh N6 2.022(3) 1_555 1_555 no Rh N7 2.082(3) 1_555 1_555 no N1 C2 1.333(5) 1_555 1_555 no N1 C3 1.383(6) 1_555 1_555 no N2 C2 1.327(5) 1_555 1_555 no N2 C8 1.393(5) 1_555 1_555 no N3 C10 1.340(5) 1_555 1_555 no N3 C11 1.383(6) 1_555 1_555 no N4 C10 1.318(5) 1_555 1_555 no N4 C16 1.394(5) 1_555 1_555 no N5 C18 1.344(5) 1_555 1_555 no N5 C19 1.383(6) 1_555 1_555 no N6 C18 1.308(5) 1_555 1_555 no N6 C24 1.406(5) 1_555 1_555 no N7 C1 1.500(5) 1_555 1_555 no N7 C9 1.504(5) 1_555 1_555 no N7 C17 1.495(5) 1_555 1_555 no C1 C2 1.493(6) 1_555 1_555 no C3 C4 1.396(6) 1_555 1_555 no C3 C8 1.404(6) 1_555 1_555 no C4 C5 1.373(8) 1_555 1_555 no C5 C6 1.415(8) 1_555 1_555 no C6 C7 1.387(7) 1_555 1_555 no C7 C8 1.392(6) 1_555 1_555 no C9 C10 1.492(6) 1_555 1_555 no C11 C12 1.384(6) 1_555 1_555 no C11 C16 1.396(6) 1_555 1_555 no C12 C13 1.381(7) 1_555 1_555 no C13 C14 1.395(7) 1_555 1_555 no C14 C15 1.379(6) 1_555 1_555 no C15 C16 1.384(6) 1_555 1_555 no C17 C18 1.477(6) 1_555 1_555 no C19 C20 1.383(6) 1_555 1_555 no C19 C24 1.401(6) 1_555 1_555 no C20 C21 1.382(7) 1_555 1_555 no C21 C22 1.393(7) 1_555 1_555 no C22 C23 1.391(6) 1_555 1_555 no C23 C24 1.382(6) 1_555 1_555 no S1D O1D 1.471(4) 1_555 1_555 no S1D C2D 1.744(5) 1_555 1_555 no S1D C1D 1.744(5) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Rh Cl2 88.31(4) 1_555 1_555 1_555 no Cl1 Rh N2 98.3(1) 1_555 1_555 1_555 no Cl1 Rh N4 99.2(1) 1_555 1_555 1_555 no Cl1 Rh N6 96.8(1) 1_555 1_555 1_555 no Cl1 Rh N7 179.31(9) 1_555 1_555 1_555 no Cl2 Rh N2 89.9(1) 1_555 1_555 1_555 no Cl2 Rh N4 89.5(1) 1_555 1_555 1_555 no Cl2 Rh N6 174.9(1) 1_555 1_555 1_555 no Cl2 Rh N7 91.8(1) 1_555 1_555 1_555 no N2 Rh N4 162.5(1) 1_555 1_555 1_555 no N2 Rh N6 90.0(1) 1_555 1_555 1_555 no N2 Rh N7 81.0(1) 1_555 1_555 1_555 no N4 Rh N6 89.1(1) 1_555 1_555 1_555 no N4 Rh N7 81.5(1) 1_555 1_555 1_555 no N6 Rh N7 83.2(1) 1_555 1_555 1_555 no C2 N1 C3 107.2(4) 1_555 1_555 1_555 no Rh N2 C2 111.5(3) 1_555 1_555 1_555 no Rh N2 C8 142.2(3) 1_555 1_555 1_555 no C2 N2 C8 106.2(4) 1_555 1_555 1_555 no C10 N3 C11 107.0(4) 1_555 1_555 1_555 no Rh N4 C10 112.0(3) 1_555 1_555 1_555 no Rh N4 C16 141.1(3) 1_555 1_555 1_555 no C10 N4 C16 106.8(3) 1_555 1_555 1_555 no C18 N5 C19 106.9(4) 1_555 1_555 1_555 no Rh N6 C18 112.9(3) 1_555 1_555 1_555 no Rh N6 C24 140.4(3) 1_555 1_555 1_555 no C18 N6 C24 106.7(3) 1_555 1_555 1_555 no Rh N7 C1 106.9(2) 1_555 1_555 1_555 no Rh N7 C9 107.4(3) 1_555 1_555 1_555 no Rh N7 C17 110.6(3) 1_555 1_555 1_555 no C1 N7 C9 112.0(3) 1_555 1_555 1_555 no C1 N7 C17 109.5(3) 1_555 1_555 1_555 no C9 N7 C17 110.4(3) 1_555 1_555 1_555 no N7 C1 C2 105.6(3) 1_555 1_555 1_555 no N1 C2 N2 112.7(4) 1_555 1_555 1_555 no N1 C2 C1 126.9(4) 1_555 1_555 1_555 no N2 C2 C1 120.3(4) 1_555 1_555 1_555 no N1 C3 C4 131.7(5) 1_555 1_555 1_555 no N1 C3 C8 106.4(4) 1_555 1_555 1_555 no C4 C3 C8 121.9(5) 1_555 1_555 1_555 no C3 C4 C5 116.1(5) 1_555 1_555 1_555 no C4 C5 C6 122.8(5) 1_555 1_555 1_555 no C5 C6 C7 120.8(5) 1_555 1_555 1_555 no C6 C7 C8 116.8(5) 1_555 1_555 1_555 no N2 C8 C3 107.5(4) 1_555 1_555 1_555 no N2 C8 C7 130.9(4) 1_555 1_555 1_555 no C3 C8 C7 121.6(4) 1_555 1_555 1_555 no N7 C9 C10 106.5(3) 1_555 1_555 1_555 no N3 C10 N4 112.2(4) 1_555 1_555 1_555 no N3 C10 C9 126.9(4) 1_555 1_555 1_555 no N4 C10 C9 120.8(4) 1_555 1_555 1_555 no N3 C11 C12 131.6(4) 1_555 1_555 1_555 no N3 C11 C16 106.7(4) 1_555 1_555 1_555 no C12 C11 C16 121.7(4) 1_555 1_555 1_555 no C11 C12 C13 116.2(4) 1_555 1_555 1_555 no C12 C13 C14 121.9(4) 1_555 1_555 1_555 no C13 C14 C15 122.1(5) 1_555 1_555 1_555 no C14 C15 C16 115.9(4) 1_555 1_555 1_555 no N4 C16 C11 107.3(4) 1_555 1_555 1_555 no N4 C16 C15 130.6(4) 1_555 1_555 1_555 no C11 C16 C15 122.1(4) 1_555 1_555 1_555 no N7 C17 C18 110.5(3) 1_555 1_555 1_555 no N5 C18 N6 112.7(4) 1_555 1_555 1_555 no N5 C18 C17 124.6(4) 1_555 1_555 1_555 no N6 C18 C17 122.7(4) 1_555 1_555 1_555 no N5 C19 C20 131.7(4) 1_555 1_555 1_555 no N5 C19 C24 106.7(4) 1_555 1_555 1_555 no C20 C19 C24 121.6(4) 1_555 1_555 1_555 no C19 C20 C21 117.1(4) 1_555 1_555 1_555 no C20 C21 C22 121.4(4) 1_555 1_555 1_555 no C21 C22 C23 121.7(5) 1_555 1_555 1_555 no C22 C23 C24 116.8(4) 1_555 1_555 1_555 no N6 C24 C19 106.9(4) 1_555 1_555 1_555 no N6 C24 C23 131.7(4) 1_555 1_555 1_555 no C19 C24 C23 121.4(4) 1_555 1_555 1_555 no O1D S1D C2D 107.8(2) 1_555 1_555 1_555 no O1D S1D C1D 107.8(2) 1_555 1_555 1_555 no C2D S1D C1D 94.6(4) 1_555 1_555 1_555 no #===END data_DSC73Rh(Et-tbima) _database_code_depnum_ccdc_archive 'CCDC 298881' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C30 H33 Cl2 N7 Rh 1+,Cl 1-,0.5(C3 H7 N O),H2 O' _chemical_formula_sum 'C31.5 H37.5 Cl3 N7 O1.5 Rh' _chemical_formula_iupac ? _chemical_formula_weight 747.5 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 10.694(4) _cell_length_b 14.354(3) _cell_length_c 22.877(9) _cell_angle_alpha 90 _cell_angle_beta 106.60(2) _cell_angle_gamma 90 _cell_volume 3365(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1534.0 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4810 _diffrn_reflns_av_R_equivalents 0.014 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 1 _diffrn_standards_interval_time '30 min' _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 4671 _reflns_number_gt 3363 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.079 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns ? _refine_ls_number_parameters 404 _refine_ls_goodness_of_fit_ref 1.33 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.008 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Rh 0.48667(5) 0.29463(4) 0.31661(2) 0.0426(2) Uani Rh 1.0 Cl1 0.37692(19) 0.40944(14) 0.24818(9) 0.0611(6) Uani Cl 1.0 Cl2 0.55549(22) 0.22524(14) 0.23802(9) 0.0650(6) Uani Cl 1.0 N1 0.6597(5) 0.3586(4) 0.3481(3) 0.047(2) Uani N 1.0 N2 0.8674(5) 0.3453(4) 0.4051(3) 0.051(2) Uani N 1.0 N3 0.3388(6) 0.2003(4) 0.3023(3) 0.052(2) Uani N 1.0 N4 0.2771(10) 0.0633(6) 0.3172(5) 0.135(5) Uani N 1.0 N5 0.4409(5) 0.3442(4) 0.3911(3) 0.045(1) Uani N 1.0 N6 0.4498(6) 0.3240(5) 0.4875(3) 0.054(2) Uani N 1.0 N7 0.5816(6) 0.1930(4) 0.3771(3) 0.048(2) Uani N 1.0 C1 0.7240(7) 0.2002(5) 0.3803(4) 0.056(2) Uani C 1.0 C2 0.7524(7) 0.3017(5) 0.3785(4) 0.049(2) Uani C 1.0 C3 0.8470(7) 0.4394(6) 0.3908(4) 0.055(2) Uani C 1.0 C4 0.9265(9) 0.5176(7) 0.4059(4) 0.073(3) Uani C 1.0 C5 0.8728(9) 0.6023(6) 0.3846(4) 0.075(3) Uani C 1.0 C6 0.7430(9) 0.6099(6) 0.3484(4) 0.068(2) Uani C 1.0 C7 0.6621(7) 0.5345(5) 0.3335(3) 0.049(2) Uani C 1.0 C8 0.7141(7) 0.4487(5) 0.3537(3) 0.050(2) Uani C 1.0 C9 0.9900(7) 0.3039(6) 0.4399(4) 0.067(2) Uani C 1.0 C10 1.0779(10) 0.2831(8) 0.4009(5) 0.089(3) Uani C 1.0 C11 0.5250(9) 0.0997(5) 0.3514(4) 0.072(3) Uani C 1.0 C12 0.3787(8) 0.1184(6) 0.3222(4) 0.073(3) Uani C 1.0 C13 0.1694(11) 0.1031(8) 0.2881(5) 0.104(4) Uani C 1.0 C14 0.0397(13) 0.0756(11) 0.2700(6) 0.141(6) Uani C 1.0 C15 -0.0514(12) 0.1394(13) 0.2430(6) 0.127(5) Uani C 1.0 C16 -0.0158(9) 0.2306(10) 0.2337(5) 0.100(4) Uani C 1.0 C17 0.1108(9) 0.2601(8) 0.2506(4) 0.075(3) Uani C 1.0 C18 0.2046(9) 0.1944(7) 0.2789(4) 0.067(3) Uani C 1.0 C19 0.2733(14) -0.0276(7) 0.3478(5) 0.172(5) Uani C 1.0 C20 0.3140(14) -0.0960(9) 0.3111(7) 0.172(5) Uani C 1.0 C21 0.5618(7) 0.2077(6) 0.4390(3) 0.056(2) Uani C 1.0 C22 0.4834(6) 0.2909(5) 0.4391(3) 0.044(2) Uani C 1.0 C23 0.3816(7) 0.4053(5) 0.4701(3) 0.050(2) Uani C 1.0 C24 0.3283(8) 0.4706(6) 0.5015(4) 0.060(2) Uani C 1.0 C25 0.2727(7) 0.5483(6) 0.4714(4) 0.060(2) Uani C 1.0 C26 0.2653(7) 0.5617(6) 0.4102(4) 0.061(2) Uani C 1.0 C27 0.3151(7) 0.4981(6) 0.3772(4) 0.057(2) Uani C 1.0 C28 0.3757(7) 0.4196(5) 0.4083(3) 0.048(2) Uani C 1.0 C29 0.4786(8) 0.2796(6) 0.5492(4) 0.063(2) Uani C 1.0 C30 0.3693(10) 0.2213(7) 0.5562(5) 0.082(3) Uani C 1.0 Cl3 0.5000 0.0000 0.5000 0.096(1) Uani Cl 1.0 Cl3' 0.8549(6) 0.2888(3) 0.0528(3) 0.074(1) Uani Cl 0.5 O1D 0.8814(18) 0.2894(12) 0.0434(11) 0.161(6) Uani O 0.5 N1D 0.9639(9) 0.4290(9) 0.0722(4) 0.077(4) Uani N 0.5 C1D 0.8648(11) 0.3740(12) 0.0427(6) 0.101(5) Uani C 0.5 C2D 1.0908(11) 0.3915(13) 0.1052(9) 0.110(6) Uani C 0.5 C3D 0.9501(18) 0.5296(12) 0.0730(9) 0.114(5) Uani C 0.5 OW1 0.7794(15) 0.4809(10) -0.0054(7) 0.102(5) Uani O 0.5 OW2 1.0258(19) 0.5693(13) 0.0686(10) 0.144(5) Uani O 0.5 H1C1 0.7413 0.1677 0.3448 0.056 Uani H 1.0 H2C1 0.7792 0.1720 0.4191 0.056 Uani H 1.0 HC4 1.0194 0.5123 0.4313 0.073 Uani H 1.0 HC5 0.9273 0.6599 0.3951 0.075 Uani H 1.0 HC6 0.7085 0.6726 0.3328 0.068 Uani H 1.0 HC7 0.5689 0.5414 0.3090 0.049 Uani H 1.0 H1C9 0.9712 0.2445 0.4586 0.067 Uani H 1.0 H2C9 1.0356 0.3481 0.4729 0.067 Uani H 1.0 H1C10 1.1609 0.2548 0.4265 0.089 Uani H 1.0 H2C10 1.0335 0.2385 0.3679 0.089 Uani H 1.0 H3C10 1.0979 0.3422 0.3822 0.089 Uani H 1.0 H1C11 0.5380 0.0523 0.3846 0.072 Uani H 1.0 H2C11 0.5667 0.0773 0.3200 0.072 Uani H 1.0 HC14 0.0142 0.0102 0.2766 0.141 Uani H 1.0 HC15 -0.1455 0.1211 0.2296 0.127 Uani H 1.0 HC16 -0.0859 0.2760 0.2138 0.100 Uani H 1.0 HC17 0.1350 0.3253 0.2430 0.075 Uani H 1.0 H1C19 0.1828 -0.0412 0.3496 0.172 Uani H 1.0 H2C19 0.3344 -0.0269 0.3900 0.172 Uani H 1.0 H1C20 0.3134 -0.1591 0.3295 0.172 Uani H 1.0 H2C20 0.2526 -0.0954 0.2689 0.172 Uani H 1.0 H3C20 0.4042 -0.0811 0.3093 0.172 Uani H 1.0 H1C21 0.6487 0.2153 0.4699 0.056 Uani H 1.0 H2C21 0.5162 0.1523 0.4497 0.056 Uani H 1.0 HC24 0.3310 0.4602 0.5451 0.060 Uani H 1.0 HC25 0.2365 0.5968 0.4935 0.060 Uani H 1.0 HC26 0.2224 0.6194 0.3893 0.061 Uani H 1.0 HC27 0.3079 0.5082 0.3331 0.057 Uani H 1.0 H1C29 0.4963 0.3298 0.5808 0.063 Uani H 1.0 H2C29 0.5578 0.2394 0.5555 0.063 Uani H 1.0 H1C30 0.3935 0.1934 0.5980 0.082 Uani H 1.0 H2C30 0.2896 0.2608 0.5503 0.082 Uani H 1.0 H3C30 0.3511 0.1704 0.5251 0.082 Uani H 1.0 HC1D 0.7785 0.4015 0.0204 0.128 Uani H 0.5 H1C2D 1.0890 0.3221 0.1016 0.167 Uani H 0.5 H2C2D 1.1589 0.4173 0.0874 0.117 Uani H 0.5 H3C2D 1.1117 0.4095 0.1491 0.139 Uani H 0.5 H1C3D 0.8596 0.5474 0.0491 0.162 Uani H 0.5 H2C3D 0.9671 0.5515 0.1161 0.137 Uani H 0.5 H3C3D 1.0143 0.5593 0.0544 0.140 Uani H 0.5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Rh 0.0441(4) 0.0401(4) 0.0396(4) -0.0054(3) 0.0055(2) 0.0046(3) Rh Cl1 0.063(1) 0.062(1) 0.051(1) 0.002(1) 0.0035(9) 0.0164(9) Cl Cl2 0.080(1) 0.063(1) 0.052(1) -0.001(1) 0.018(1) -0.005(1) Cl N1 0.045(3) 0.046(4) 0.046(3) -0.007(3) 0.007(3) 0.008(3) N N2 0.037(3) 0.056(4) 0.056(4) -0.010(3) 0.006(3) 0.004(3) N N3 0.049(4) 0.057(4) 0.042(3) -0.013(3) 0.001(3) 0.010(3) N N4 0.117(7) 0.079(6) 0.149(9) -0.056(6) -0.057(7) 0.069(6) N N5 0.043(3) 0.047(4) 0.044(4) -0.002(3) 0.012(3) -0.001(3) N N6 0.047(4) 0.065(4) 0.046(4) -0.010(3) 0.008(3) 0.005(3) N N7 0.045(3) 0.045(4) 0.050(4) -0.005(3) 0.004(3) 0.002(3) N C1 0.053(5) 0.049(5) 0.067(5) 0.011(4) 0.016(4) 0.010(4) C C2 0.050(4) 0.042(4) 0.055(4) -0.005(4) 0.014(4) 0.004(4) C C3 0.044(4) 0.063(5) 0.056(5) -0.012(4) 0.011(4) 0.010(4) C C4 0.061(5) 0.082(7) 0.072(6) -0.036(5) 0.012(5) -0.005(5) C C5 0.079(6) 0.063(6) 0.082(6) -0.029(5) 0.019(5) 0.007(5) C C6 0.084(6) 0.054(5) 0.062(5) -0.019(5) 0.015(5) 0.016(4) C C7 0.060(5) 0.043(4) 0.042(4) -0.008(4) 0.011(4) 0.007(3) C C8 0.051(4) 0.058(5) 0.039(4) -0.012(4) 0.010(3) -0.002(4) C C9 0.045(5) 0.081(7) 0.071(6) -0.002(4) 0.008(4) 0.013(5) C C10 0.061(6) 0.115(9) 0.090(7) 0.010(6) 0.022(5) -0.010(6) C C11 0.081(6) 0.036(5) 0.079(6) -0.019(4) -0.008(5) 0.002(4) C C12 0.068(6) 0.061(6) 0.068(6) -0.032(5) -0.014(4) 0.015(5) C C13 0.090(7) 0.109(9) 0.077(7) -0.054(7) -0.034(6) 0.041(6) C C14 0.095(9) 0.181(9) 0.108(9) -0.086(9) -0.035(7) 0.060(9) C C15 0.079(8) 0.184(9) 0.092(9) -0.068(9) -0.014(7) 0.014(9) C C16 0.054(6) 0.160(9) 0.067(7) -0.002(7) -0.013(5) -0.001(7) C C17 0.061(6) 0.099(7) 0.059(5) -0.013(6) 0.006(4) -0.007(5) C C18 0.067(6) 0.086(7) 0.042(4) -0.029(5) 0.007(4) 0.002(4) C C19 0.111(6) 0.225(7) 0.155(9) 0.017(9) -0.001(7) -0.076(9) C C20 0.111(6) 0.225(7) 0.155(9) 0.017(9) -0.001(7) -0.076(9) C C21 0.052(5) 0.070(6) 0.043(4) 0.003(4) 0.009(3) 0.017(4) C C22 0.037(4) 0.052(4) 0.038(4) -0.005(3) 0.002(3) 0.004(4) C C23 0.036(4) 0.054(5) 0.052(5) -0.012(4) 0.001(3) 0.001(4) C C24 0.051(5) 0.074(6) 0.054(5) -0.013(4) 0.015(4) -0.013(5) C C25 0.043(4) 0.060(5) 0.075(6) -0.004(4) 0.014(4) -0.014(5) C C26 0.046(4) 0.058(5) 0.078(6) -0.001(4) 0.018(4) -0.004(5) C C27 0.046(4) 0.059(5) 0.062(5) 0.004(4) 0.010(4) 0.007(4) C C28 0.044(4) 0.051(5) 0.045(4) -0.010(4) 0.006(3) -0.002(4) C C29 0.071(5) 0.080(6) 0.038(4) 0.002(5) 0.014(4) 0.016(4) C C30 0.096(7) 0.080(7) 0.078(7) -0.028(6) 0.041(6) 0.007(5) C Cl3 0.146(4) 0.067(2) 0.074(2) -0.008(2) 0.031(2) 0.022(2) Cl Cl3' 0.063(3) 0.067(3) 0.084(4) 0.015(2) 0.006(3) 0.004(3) Cl O1D 0.158(9) 0.152(8) 0.203(9) -0.063(9) 0.100(9) -0.072(9) O N1D 0.063(6) 0.115(7) 0.054(7) -0.007(5) 0.021(5) -0.008(6) N C1D 0.079(6) 0.160(9) 0.076(8) -0.034(7) 0.038(5) -0.038(7) C C2D 0.077(6) 0.153(8) 0.096(9) 0.013(7) 0.017(6) 0.009(9) C C3D 0.101(7) 0.117(7) 0.130(9) 0.002(6) 0.040(6) -0.003(6) C OW1 0.113(9) 0.084(9) 0.119(9) -0.008(8) 0.048(9) 0.022(9) O OW2 0.151(9) 0.121(7) 0.172(9) -0.025(6) 0.067(9) 0.000(6) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh Cl1 2.344(2) 1_555 1_555 no Rh Cl2 2.350(2) 1_555 1_555 no Rh N1 2.006(5) 1_555 1_555 no Rh N3 2.036(6) 1_555 1_555 no Rh N5 2.032(6) 1_555 1_555 no Rh N7 2.068(6) 1_555 1_555 no N1 C2 1.319(9) 1_555 1_555 no N1 C8 1.409(9) 1_555 1_555 no N2 C2 1.358(9) 1_555 1_555 no N2 C3 1.392(10) 1_555 1_555 no N2 C9 1.453(9) 1_555 1_555 no N3 C12 1.289(10) 1_555 1_555 no N3 C18 1.383(10) 1_555 1_555 no N4 C12 1.322(11) 1_555 1_555 no N4 C13 1.288(13) 1_555 1_555 no N4 C19 1.486(6) 1_555 1_555 no N5 C22 1.307(9) 1_555 1_555 no N5 C28 1.403(9) 1_555 1_555 no N6 C22 1.345(10) 1_555 1_555 no N6 C23 1.374(9) 1_555 1_555 no N6 C29 1.498(10) 1_555 1_555 no N7 C1 1.507(9) 1_555 1_555 no N7 C11 1.517(9) 1_555 1_555 no N7 C21 1.504(10) 1_555 1_555 no C1 C2 1.492(10) 1_555 1_555 no C3 C4 1.391(11) 1_555 1_555 no C3 C8 1.439(10) 1_555 1_555 no C4 C5 1.374(13) 1_555 1_555 no C5 C6 1.402(12) 1_555 1_555 no C6 C7 1.366(10) 1_555 1_555 no C7 C8 1.376(10) 1_555 1_555 no C9 C10 1.501(13) 1_555 1_555 no C11 C12 1.539(12) 1_555 1_555 no C13 C14 1.387(14) 1_555 1_555 no C13 C18 1.396(12) 1_555 1_555 no C14 C15 1.351(19) 1_555 1_555 no C15 C16 1.396(18) 1_555 1_555 no C16 C17 1.366(13) 1_555 1_555 no C17 C18 1.394(13) 1_555 1_555 no C19 C20 1.438(8) 1_555 1_555 no C21 C22 1.459(10) 1_555 1_555 no C23 C24 1.398(11) 1_555 1_555 no C23 C28 1.411(10) 1_555 1_555 no C24 C25 1.355(12) 1_555 1_555 no C25 C26 1.394(12) 1_555 1_555 no C26 C27 1.384(11) 1_555 1_555 no C27 C28 1.391(10) 1_555 1_555 no C29 C30 1.484(12) 1_555 1_555 no O1D C1D 1.226(6) 1_555 1_555 no N1D C1D 1.339(5) 1_555 1_555 no N1D C2D 1.453(5) 1_555 1_555 no N1D C3D 1.453(9) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Rh Cl2 89.62(8) 1_555 1_555 1_555 no Cl1 Rh N1 98.8(2) 1_555 1_555 1_555 no Cl1 Rh N3 98.2(2) 1_555 1_555 1_555 no Cl1 Rh N5 96.9(2) 1_555 1_555 1_555 no Cl1 Rh N7 179.4(2) 1_555 1_555 1_555 no Cl2 Rh N1 90.6(2) 1_555 1_555 1_555 no Cl2 Rh N3 89.6(2) 1_555 1_555 1_555 no Cl2 Rh N5 173.4(2) 1_555 1_555 1_555 no Cl2 Rh N7 90.7(2) 1_555 1_555 1_555 no N1 Rh N3 163.0(2) 1_555 1_555 1_555 no N1 Rh N5 87.5(2) 1_555 1_555 1_555 no N1 Rh N7 81.7(2) 1_555 1_555 1_555 no N3 Rh N5 90.3(2) 1_555 1_555 1_555 no N3 Rh N7 81.3(2) 1_555 1_555 1_555 no N5 Rh N7 82.8(2) 1_555 1_555 1_555 no Rh N1 C2 112.6(5) 1_555 1_555 1_555 no Rh N1 C8 140.1(5) 1_555 1_555 1_555 no C2 N1 C8 106.9(6) 1_555 1_555 1_555 no C2 N2 C3 106.3(6) 1_555 1_555 1_555 no C2 N2 C9 128.1(7) 1_555 1_555 1_555 no C3 N2 C9 125.6(6) 1_555 1_555 1_555 no Rh N3 C12 112.7(5) 1_555 1_555 1_555 no Rh N3 C18 140.8(6) 1_555 1_555 1_555 no C12 N3 C18 106.5(7) 1_555 1_555 1_555 no C12 N4 C13 111.8(8) 1_555 1_555 1_555 no C12 N4 C19 128.0(10) 1_555 1_555 1_555 no C13 N4 C19 119.5(10) 1_555 1_555 1_555 no Rh N5 C22 112.9(5) 1_555 1_555 1_555 no Rh N5 C28 139.7(5) 1_555 1_555 1_555 no C22 N5 C28 107.3(6) 1_555 1_555 1_555 no C22 N6 C23 107.8(6) 1_555 1_555 1_555 no C22 N6 C29 126.4(7) 1_555 1_555 1_555 no C23 N6 C29 125.7(7) 1_555 1_555 1_555 no Rh N7 C1 106.3(4) 1_555 1_555 1_555 no Rh N7 C11 107.3(4) 1_555 1_555 1_555 no Rh N7 C21 110.9(4) 1_555 1_555 1_555 no C1 N7 C11 111.4(6) 1_555 1_555 1_555 no C1 N7 C21 110.9(5) 1_555 1_555 1_555 no C11 N7 C21 110.0(6) 1_555 1_555 1_555 no N7 C1 C2 106.1(6) 1_555 1_555 1_555 no N1 C2 N2 113.6(6) 1_555 1_555 1_555 no N1 C2 C1 119.4(6) 1_555 1_555 1_555 no N2 C2 C1 127.1(7) 1_555 1_555 1_555 no N2 C3 C4 132.9(7) 1_555 1_555 1_555 no N2 C3 C8 106.9(6) 1_555 1_555 1_555 no C4 C3 C8 120.2(8) 1_555 1_555 1_555 no C3 C4 C5 117.5(8) 1_555 1_555 1_555 no C4 C5 C6 121.4(8) 1_555 1_555 1_555 no C5 C6 C7 122.4(8) 1_555 1_555 1_555 no C6 C7 C8 117.3(7) 1_555 1_555 1_555 no N1 C8 C3 106.3(6) 1_555 1_555 1_555 no N1 C8 C7 132.4(7) 1_555 1_555 1_555 no C3 C8 C7 121.2(7) 1_555 1_555 1_555 no N2 C9 C10 112.1(8) 1_555 1_555 1_555 no N7 C11 C12 104.9(6) 1_555 1_555 1_555 no N3 C12 N4 109.5(8) 1_555 1_555 1_555 no N3 C12 C11 120.4(7) 1_555 1_555 1_555 no N4 C12 C11 129.9(8) 1_555 1_555 1_555 no N4 C13 C14 134.3(11) 1_555 1_555 1_555 no N4 C13 C18 104.7(8) 1_555 1_555 1_555 no C14 C13 C18 120.8(11) 1_555 1_555 1_555 no C13 C14 C15 118.2(12) 1_555 1_555 1_555 no C14 C15 C16 120.9(10) 1_555 1_555 1_555 no C15 C16 C17 122.6(11) 1_555 1_555 1_555 no C16 C17 C18 116.4(10) 1_555 1_555 1_555 no N3 C18 C13 107.1(8) 1_555 1_555 1_555 no N3 C18 C17 131.9(8) 1_555 1_555 1_555 no C13 C18 C17 121.1(9) 1_555 1_555 1_555 no N4 C19 C20 105.7(6) 1_555 1_555 1_555 no N7 C21 C22 110.6(6) 1_555 1_555 1_555 no N5 C22 N6 111.9(6) 1_555 1_555 1_555 no N5 C22 C21 122.6(7) 1_555 1_555 1_555 no N6 C22 C21 125.4(6) 1_555 1_555 1_555 no N6 C23 C24 132.9(7) 1_555 1_555 1_555 no N6 C23 C28 106.3(7) 1_555 1_555 1_555 no C24 C23 C28 120.7(7) 1_555 1_555 1_555 no C23 C24 C25 118.3(7) 1_555 1_555 1_555 no C24 C25 C26 121.0(8) 1_555 1_555 1_555 no C25 C26 C27 122.5(8) 1_555 1_555 1_555 no C26 C27 C28 116.8(8) 1_555 1_555 1_555 no N5 C28 C23 106.6(6) 1_555 1_555 1_555 no N5 C28 C27 132.7(7) 1_555 1_555 1_555 no C23 C28 C27 120.8(7) 1_555 1_555 1_555 no N6 C29 C30 112.7(7) 1_555 1_555 1_555 no C1D N1D C2D 122.1(3) 1_555 1_555 1_555 no C1D N1D C3D 121.6(3) 1_555 1_555 1_555 no C2D N1D C3D 116.4(5) 1_555 1_555 1_555 no O1D C1D N1D 119.1(3) 1_555 1_555 1_555 no #===END data_DSC32[Rh(bepa)Cl3] _database_code_depnum_ccdc_archive 'CCDC 298882' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C14 H16 Cl3 N3 Rh' _chemical_formula_sum 'C14 H16 Cl3 N3 Rh' _chemical_formula_iupac ? _chemical_formula_weight 435.6 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 8.989(3) _cell_length_b 14.037(4) _cell_length_c 12.400(4) _cell_angle_alpha 90 _cell_angle_beta 93.09(1) _cell_angle_gamma 90 _cell_volume 1562.3(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _cell_measurement_temperature 294 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.85 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868.0 _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.77 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 2928 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 2743 _reflns_number_gt 2573 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.023 _refine_ls_wR_factor_ref 0.039 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2573 _refine_ls_number_parameters 190 _refine_ls_goodness_of_fit_ref 1.62 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.029 _refine_diff_density_max 0.84 _refine_diff_density_min -0.87 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Rh 0.23735(2) 0.15934(1) 0.25092(1) 0.0246(1) Uani Rh 1.0 Cl1 0.27965(9) 0.02740(5) 0.36879(6) 0.0423(2) Uani Cl 1.0 Cl2 0.12879(8) 0.06635(5) 0.11263(5) 0.0401(2) Uani Cl 1.0 Cl3 0.33044(8) 0.25643(5) 0.39479(5) 0.0358(2) Uani Cl 1.0 N1 0.4406(2) 0.1348(2) 0.1865(2) 0.0292(5) Uani N 1.0 N2 0.0247(3) 0.1801(2) 0.3061(2) 0.0328(5) Uani N 1.0 N3 0.2198(2) 0.2701(2) 0.1410(2) 0.0293(5) Uani N 1.0 C1 0.3399(3) 0.3437(2) 0.1472(2) 0.0337(6) Uani C 1.0 C2 0.4954(3) 0.3082(2) 0.1816(2) 0.0352(6) Uani C 1.0 C3 0.5326(3) 0.2061(2) 0.1570(2) 0.0306(6) Uani C 1.0 C4 0.6650(3) 0.1843(2) 0.1109(2) 0.0412(7) Uani C 1.0 C5 0.7059(3) 0.0913(2) 0.0911(2) 0.0439(7) Uani C 1.0 C6 0.6098(3) 0.0197(2) 0.1187(2) 0.0422(7) Uani C 1.0 C7 0.4795(3) 0.0439(2) 0.1665(2) 0.0362(6) Uani C 1.0 C8 0.0723(3) 0.3179(2) 0.1361(2) 0.0404(6) Uani C 1.0 C9 0.0256(3) 0.3467(2) 0.2475(3) 0.0427(7) Uani C 1.0 C10 -0.0433(3) 0.2652(2) 0.3042(2) 0.0355(6) Uani C 1.0 C11 -0.1813(3) 0.2753(2) 0.3466(2) 0.0446(7) Uani C 1.0 C12 -0.2552(3) 0.1985(3) 0.3870(2) 0.0473(7) Uani C 1.0 C13 -0.1855(4) 0.1105(3) 0.3867(3) 0.0458(7) Uani C 1.0 C14 -0.0469(3) 0.1047(2) 0.3457(2) 0.0402(6) Uani C 1.0 H1C1 0.3116 0.3933 0.2002 0.034 Uani H 1.0 H2C1 0.3447 0.3732 0.0740 0.034 Uani H 1.0 H1C2 0.5089 0.3168 0.2616 0.035 Uani H 1.0 H2C2 0.5683 0.3493 0.1450 0.035 Uani H 1.0 HC4 0.7329 0.2373 0.0913 0.041 Uani H 1.0 HC5 0.8021 0.0763 0.0578 0.044 Uani H 1.0 HC6 0.6340 -0.0486 0.1045 0.042 Uani H 1.0 HC7 0.4109 -0.0083 0.1871 0.036 Uani H 1.0 H1C8 -0.0039 0.2733 0.1030 0.040 Uani H 1.0 H2C8 0.0777 0.3763 0.0903 0.040 Uani H 1.0 H1C9 -0.0484 0.3998 0.2398 0.043 Uani H 1.0 H2C9 0.1154 0.3689 0.2916 0.043 Uani H 1.0 HC11 -0.2284 0.3398 0.3481 0.045 Uani H 1.0 HC12 -0.3564 0.2059 0.4156 0.047 Uani H 1.0 HC13 -0.2347 0.0527 0.4156 0.046 Uani H 1.0 HC14 0.0034 0.0412 0.3452 0.040 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Rh 0.0280(2) 0.0215(2) 0.0249(2) 0.0005(1) 0.0070(1) 0.0001(1) Rh Cl1 0.0548(4) 0.0309(4) 0.0422(4) 0.0052(3) 0.0109(3) 0.0108(3) Cl Cl2 0.0418(4) 0.0385(4) 0.0405(4) -0.0077(3) 0.0062(3) -0.0119(3) Cl Cl3 0.0458(4) 0.0348(4) 0.0271(3) -0.0039(3) 0.0055(3) -0.0022(3) Cl N1 0.031(1) 0.028(1) 0.029(1) -0.0012(9) 0.0061(9) -0.0015(9) N N2 0.033(1) 0.035(1) 0.031(1) 0.001(1) 0.0084(9) -0.002(1) N N3 0.034(1) 0.027(1) 0.027(1) 0.0023(9) 0.0035(8) 0.0043(8) N C1 0.043(2) 0.027(1) 0.032(1) -0.001(1) 0.006(1) 0.005(1) C C2 0.038(2) 0.031(1) 0.037(1) -0.008(1) 0.009(1) 0.000(1) C C3 0.032(1) 0.035(1) 0.025(1) -0.002(1) 0.005(1) 0.002(1) C C4 0.032(2) 0.056(2) 0.037(2) -0.004(1) 0.009(1) 0.002(1) C C5 0.037(2) 0.061(2) 0.034(2) 0.011(1) 0.009(1) -0.005(1) C C6 0.041(2) 0.048(2) 0.038(2) 0.014(1) 0.005(1) -0.008(1) C C7 0.041(2) 0.032(1) 0.036(1) 0.007(1) 0.005(1) -0.001(1) C C8 0.039(2) 0.041(2) 0.041(2) 0.007(1) 0.002(1) 0.011(1) C C9 0.043(2) 0.031(2) 0.055(2) 0.010(1) 0.015(1) 0.002(1) C C10 0.034(1) 0.040(2) 0.033(1) 0.005(1) 0.003(1) -0.002(1) C C11 0.036(2) 0.057(2) 0.041(2) 0.012(1) 0.007(1) -0.005(1) C C12 0.032(2) 0.072(2) 0.038(2) -0.002(2) 0.008(1) -0.010(2) C C13 0.041(2) 0.057(2) 0.041(2) -0.010(1) 0.011(1) -0.003(1) C C14 0.041(2) 0.039(2) 0.042(2) -0.005(1) 0.012(1) -0.003(1) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh Cl1 2.377(1) 1_555 1_555 no Rh Cl2 2.327(1) 1_555 1_555 no Rh Cl3 2.362(1) 1_555 1_555 no Rh N1 2.062(2) 1_555 1_555 no Rh N2 2.085(2) 1_555 1_555 no Rh N3 2.068(2) 1_555 1_555 no N1 C3 1.361(3) 1_555 1_555 no N1 C7 1.350(3) 1_555 1_555 no N2 C10 1.341(3) 1_555 1_555 no N2 C14 1.345(3) 1_555 1_555 no N3 C1 1.494(3) 1_555 1_555 no N3 C8 1.485(3) 1_555 1_555 no C1 C2 1.523(4) 1_555 1_555 no C2 C3 1.507(4) 1_555 1_555 no C3 C4 1.381(4) 1_555 1_555 no C4 C5 1.382(4) 1_555 1_555 no C5 C6 1.381(4) 1_555 1_555 no C6 C7 1.384(4) 1_555 1_555 no C8 C9 1.520(4) 1_555 1_555 no C9 C10 1.495(4) 1_555 1_555 no C10 C11 1.381(4) 1_555 1_555 no C11 C12 1.375(4) 1_555 1_555 no C12 C13 1.385(5) 1_555 1_555 no C13 C14 1.373(4) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Rh Cl2 93.60(3) 1_555 1_555 1_555 no Cl1 Rh Cl3 86.95(2) 1_555 1_555 1_555 no Cl1 Rh N1 89.56(6) 1_555 1_555 1_555 no Cl1 Rh N2 91.50(7) 1_555 1_555 1_555 no Cl1 Rh N3 174.23(6) 1_555 1_555 1_555 no Cl2 Rh Cl3 175.97(2) 1_555 1_555 1_555 no Cl2 Rh N1 88.06(6) 1_555 1_555 1_555 no Cl2 Rh N2 87.99(6) 1_555 1_555 1_555 no Cl2 Rh N3 85.52(6) 1_555 1_555 1_555 no Cl3 Rh N1 95.94(6) 1_555 1_555 1_555 no Cl3 Rh N2 88.00(6) 1_555 1_555 1_555 no Cl3 Rh N3 94.33(6) 1_555 1_555 1_555 no N1 Rh N2 175.97(7) 1_555 1_555 1_555 no N1 Rh N3 84.72(8) 1_555 1_555 1_555 no N2 Rh N3 94.16(9) 1_555 1_555 1_555 no Rh N1 C3 123.1(2) 1_555 1_555 1_555 no Rh N1 C7 118.2(2) 1_555 1_555 1_555 no C3 N1 C7 118.6(2) 1_555 1_555 1_555 no Rh N2 C10 123.0(2) 1_555 1_555 1_555 no Rh N2 C14 118.3(2) 1_555 1_555 1_555 no C10 N2 C14 118.7(2) 1_555 1_555 1_555 no Rh N3 C1 117.2(2) 1_555 1_555 1_555 no Rh N3 C8 113.8(2) 1_555 1_555 1_555 no C1 N3 C8 109.3(2) 1_555 1_555 1_555 no N3 C1 C2 116.0(2) 1_555 1_555 1_555 no C1 C2 C3 117.7(2) 1_555 1_555 1_555 no N1 C3 C2 120.0(2) 1_555 1_555 1_555 no N1 C3 C4 119.9(3) 1_555 1_555 1_555 no C2 C3 C4 120.0(2) 1_555 1_555 1_555 no C3 C4 C5 121.7(3) 1_555 1_555 1_555 no C4 C5 C6 117.9(3) 1_555 1_555 1_555 no C5 C6 C7 118.9(3) 1_555 1_555 1_555 no N1 C7 C6 123.0(3) 1_555 1_555 1_555 no N3 C8 C9 111.9(2) 1_555 1_555 1_555 no C8 C9 C10 111.4(2) 1_555 1_555 1_555 no N2 C10 C9 119.3(2) 1_555 1_555 1_555 no N2 C10 C11 120.2(3) 1_555 1_555 1_555 no C9 C10 C11 120.3(3) 1_555 1_555 1_555 no C10 C11 C12 121.3(3) 1_555 1_555 1_555 no C11 C12 C13 118.1(3) 1_555 1_555 1_555 no C12 C13 C14 118.3(3) 1_555 1_555 1_555 no N2 C14 C13 123.4(3) 1_555 1_555 1_555 no #===END data_DSC109[Pd(tmpa)Cl]Cl2.2H2O _database_code_depnum_ccdc_archive 'CCDC 298883' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C18 H18 Cl N4 Pd 1+,Cl 1-,2(H2 O)' _chemical_formula_sum 'C18 H22 Cl2 N4 O2 Pd' _chemical_formula_iupac ? _chemical_formula_weight 503.7 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 15.007(3) _cell_length_b 7.6373(6) _cell_length_c 19.041(4) _cell_angle_alpha 90 _cell_angle_beta 111.862(7) _cell_angle_gamma 90 _cell_volume 2025.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.65 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016.0 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.88 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3668 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 3547 _reflns_number_gt 3012 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_ref 0.047 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3012 _refine_ls_number_parameters 244 _refine_ls_goodness_of_fit_ref 1.81 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.017 _refine_diff_density_max 0.82 _refine_diff_density_min -0.73 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Pd 0.30921(2) 0.28766(4) 0.56282(1) 0.0323(1) Uani Pd 1.0 Cl1 0.45002(7) 0.20603(15) 0.65814(6) 0.0523(3) Uani Cl 1.0 N1 0.2875(2) 0.5129(4) 0.6099(2) 0.0371(7) Uani N 1.0 N2 0.3006(2) 0.0793(4) 0.4957(2) 0.0379(7) Uani N 1.0 N3 0.3672(2) 0.4253(5) 0.4316(2) 0.0458(8) Uani N 1.0 N4 0.1871(2) 0.3579(4) 0.4777(2) 0.0348(6) Uani N 1.0 C1 0.1312(2) 0.4631(5) 0.5135(2) 0.0406(8) Uani C 1.0 C2 0.1984(2) 0.5811(5) 0.5705(2) 0.0401(8) Uani C 1.0 C3 0.1751(3) 0.7468(5) 0.5866(2) 0.049(1) Uani C 1.0 C4 0.2423(3) 0.8443(6) 0.6431(3) 0.057(1) Uani C 1.0 C5 0.3306(3) 0.7727(6) 0.6828(3) 0.055(1) Uani C 1.0 C6 0.3509(3) 0.6057(6) 0.6652(2) 0.0468(9) Uani C 1.0 C7 0.1392(3) 0.1897(5) 0.4441(2) 0.047(1) Uani C 1.0 C8 0.2141(3) 0.0661(5) 0.4390(2) 0.0411(8) Uani C 1.0 C9 0.1992(3) -0.0485(5) 0.3806(2) 0.053(1) Uani C 1.0 C10 0.2754(4) -0.1485(6) 0.3786(2) 0.057(1) Uani C 1.0 C11 0.3629(3) -0.1368(6) 0.4365(3) 0.057(1) Uani C 1.0 C12 0.3737(3) -0.0232(5) 0.4948(2) 0.049(1) Uani C 1.0 C13 0.2047(3) 0.4751(5) 0.4204(2) 0.0431(9) Uani C 1.0 C14 0.2746(3) 0.4066(5) 0.3880(2) 0.0371(8) Uani C 1.0 C15 0.2451(3) 0.3351(6) 0.3170(2) 0.053(1) Uani C 1.0 C16 0.3136(4) 0.2738(7) 0.2889(3) 0.065(1) Uani C 1.0 C17 0.4075(4) 0.2924(7) 0.3345(3) 0.072(2) Uani C 1.0 C18 0.4326(3) 0.3696(7) 0.4041(3) 0.059(1) Uani C 1.0 Cl2 0.04419(11) 0.14818(19) 0.60535(8) 0.0779(4) Uani Cl 1.0 OW1 0.0454(2) 0.4823(4) 0.6881(2) 0.0632(8) Uani O 1.0 OW2 0.0719(3) -0.1497(5) 0.7271(2) 0.079(1) Uani O 1.0 H1C1 0.0994 0.3830 0.5386 0.041 Uani H 1.0 H2C1 0.0813 0.5338 0.4739 0.041 Uani H 1.0 HC3 0.1101 0.7965 0.5576 0.049 Uani H 1.0 HC4 0.2266 0.9654 0.6547 0.057 Uani H 1.0 HC5 0.3797 0.8407 0.7241 0.055 Uani H 1.0 HC6 0.4151 0.5532 0.6948 0.047 Uani H 1.0 H1C7 0.0901 0.2116 0.3923 0.047 Uani H 1.0 H2C7 0.1072 0.1380 0.4769 0.047 Uani H 1.0 HC9 0.1341 -0.0602 0.3397 0.053 Uani H 1.0 HC10 0.2664 -0.2288 0.3350 0.057 Uani H 1.0 HC11 0.4181 -0.2099 0.4363 0.057 Uani H 1.0 HC12 0.4372 -0.0159 0.5378 0.049 Uani H 1.0 H1C13 0.2224 0.5813 0.4535 0.043 Uani H 1.0 H2C13 0.1351 0.4808 0.3871 0.043 Uani H 1.0 HC15 0.1750 0.3266 0.2853 0.053 Uani H 1.0 HC16 0.2942 0.2189 0.2377 0.065 Uani H 1.0 HC17 0.4588 0.2494 0.3170 0.072 Uani H 1.0 HC18 0.5022 0.3851 0.4356 0.059 Uani H 1.0 H1OW1 0.0496 0.3780 0.6577 0.063 Uani H 1.0 H2OW1 0.0068 0.4517 0.7193 0.063 Uani H 1.0 H1OW2 0.0613 -0.0666 0.6841 0.079 Uani H 1.0 H2OW2 0.0609 -0.2724 0.7074 0.079 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Pd 0.0274(2) 0.0354(2) 0.0319(2) 0.0008(1) 0.0084(1) 0.0034(1) Pd Cl1 0.0418(5) 0.0637(7) 0.0394(5) 0.0120(5) 0.0013(4) 0.0032(5) Cl N1 0.032(2) 0.042(2) 0.038(2) 0.000(1) 0.015(1) 0.000(1) N N2 0.038(2) 0.033(2) 0.042(2) -0.002(1) 0.014(1) 0.003(1) N N3 0.042(2) 0.050(2) 0.045(2) -0.002(2) 0.017(1) 0.004(2) N N4 0.028(1) 0.038(2) 0.037(2) 0.000(1) 0.010(1) 0.004(1) N C1 0.028(2) 0.049(2) 0.045(2) 0.002(2) 0.015(2) -0.001(2) C C2 0.034(2) 0.048(2) 0.043(2) 0.002(2) 0.019(2) 0.007(2) C C3 0.044(2) 0.049(3) 0.057(3) 0.009(2) 0.023(2) 0.001(2) C C4 0.063(3) 0.050(3) 0.064(3) 0.002(2) 0.029(2) -0.010(2) C C5 0.053(3) 0.051(3) 0.056(3) -0.002(2) 0.015(2) -0.010(2) C C6 0.041(2) 0.053(3) 0.042(2) 0.000(2) 0.010(2) -0.005(2) C C7 0.037(2) 0.042(2) 0.052(2) -0.008(2) 0.005(2) -0.005(2) C C8 0.047(2) 0.033(2) 0.039(2) -0.005(2) 0.010(2) 0.007(2) C C9 0.067(3) 0.034(2) 0.048(2) 0.000(2) 0.010(2) 0.002(2) C C10 0.085(3) 0.036(2) 0.052(3) -0.009(2) 0.028(2) -0.005(2) C C11 0.070(3) 0.035(2) 0.078(3) -0.002(2) 0.040(3) -0.004(2) C C12 0.047(2) 0.038(2) 0.065(3) 0.000(2) 0.022(2) 0.002(2) C C13 0.044(2) 0.045(2) 0.043(2) 0.009(2) 0.018(2) 0.011(2) C C14 0.042(2) 0.034(2) 0.034(2) 0.002(2) 0.013(2) 0.008(2) C C15 0.063(3) 0.054(3) 0.041(2) -0.002(2) 0.018(2) 0.003(2) C C16 0.088(4) 0.066(3) 0.056(3) -0.006(3) 0.044(3) -0.005(2) C C17 0.086(4) 0.065(3) 0.094(4) 0.004(3) 0.065(4) 0.004(3) C C18 0.047(2) 0.066(3) 0.070(3) 0.002(2) 0.028(2) 0.012(3) C Cl2 0.0920(9) 0.0674(8) 0.0831(9) 0.0005(7) 0.0425(8) 0.0092(7) Cl OW1 0.060(2) 0.046(2) 0.061(2) -0.008(2) -0.003(1) 0.002(1) O OW2 0.093(3) 0.068(2) 0.068(2) -0.010(2) 0.020(2) 0.006(2) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl1 2.300(1) 1_555 1_555 no Pd N1 2.022(3) 1_555 1_555 no Pd N2 2.015(3) 1_555 1_555 no Pd N4 2.015(3) 1_555 1_555 no N1 C2 1.369(4) 1_555 1_555 no N1 C6 1.330(5) 1_555 1_555 no N2 C8 1.348(4) 1_555 1_555 no N2 C12 1.353(5) 1_555 1_555 no N3 C14 1.335(4) 1_555 1_555 no N3 C18 1.342(5) 1_555 1_555 no N4 C1 1.496(5) 1_555 1_555 no N4 C7 1.495(5) 1_555 1_555 no N4 C13 1.508(5) 1_555 1_555 no C1 C2 1.481(5) 1_555 1_555 no C2 C3 1.377(5) 1_555 1_555 no C3 C4 1.386(6) 1_555 1_555 no C4 C5 1.371(6) 1_555 1_555 no C5 C6 1.382(6) 1_555 1_555 no C7 C8 1.498(6) 1_555 1_555 no C8 C9 1.367(5) 1_555 1_555 no C9 C10 1.388(6) 1_555 1_555 no C10 C11 1.367(6) 1_555 1_555 no C11 C12 1.370(6) 1_555 1_555 no C13 C14 1.497(5) 1_555 1_555 no C14 C15 1.369(5) 1_555 1_555 no C15 C16 1.405(6) 1_555 1_555 no C16 C17 1.360(8) 1_555 1_555 no C17 C18 1.368(7) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd N1 97.65(8) 1_555 1_555 1_555 no Cl1 Pd N2 96.29(9) 1_555 1_555 1_555 no Cl1 Pd N4 178.76(8) 1_555 1_555 1_555 no N1 Pd N2 166.1(1) 1_555 1_555 1_555 no N1 Pd N4 83.2(1) 1_555 1_555 1_555 no N2 Pd N4 82.8(1) 1_555 1_555 1_555 no Pd N1 C2 111.5(2) 1_555 1_555 1_555 no Pd N1 C6 128.1(3) 1_555 1_555 1_555 no C2 N1 C6 119.7(3) 1_555 1_555 1_555 no Pd N2 C8 112.4(3) 1_555 1_555 1_555 no Pd N2 C12 127.2(3) 1_555 1_555 1_555 no C8 N2 C12 119.4(3) 1_555 1_555 1_555 no C14 N3 C18 117.7(4) 1_555 1_555 1_555 no Pd N4 C1 105.8(2) 1_555 1_555 1_555 no Pd N4 C7 105.3(2) 1_555 1_555 1_555 no Pd N4 C13 112.9(2) 1_555 1_555 1_555 no C1 N4 C7 113.2(3) 1_555 1_555 1_555 no C1 N4 C13 106.8(3) 1_555 1_555 1_555 no C7 N4 C13 112.7(3) 1_555 1_555 1_555 no N4 C1 C2 108.5(3) 1_555 1_555 1_555 no N1 C2 C1 115.4(3) 1_555 1_555 1_555 no N1 C2 C3 120.3(4) 1_555 1_555 1_555 no C1 C2 C3 124.2(3) 1_555 1_555 1_555 no C2 C3 C4 119.7(4) 1_555 1_555 1_555 no C3 C4 C5 119.2(4) 1_555 1_555 1_555 no C4 C5 C6 119.3(4) 1_555 1_555 1_555 no N1 C6 C5 121.7(4) 1_555 1_555 1_555 no N4 C7 C8 108.4(3) 1_555 1_555 1_555 no N2 C8 C7 115.1(3) 1_555 1_555 1_555 no N2 C8 C9 121.1(4) 1_555 1_555 1_555 no C7 C8 C9 123.8(3) 1_555 1_555 1_555 no C8 C9 C10 119.2(4) 1_555 1_555 1_555 no C9 C10 C11 119.8(4) 1_555 1_555 1_555 no C10 C11 C12 118.9(4) 1_555 1_555 1_555 no N2 C12 C11 121.6(4) 1_555 1_555 1_555 no N4 C13 C14 115.4(3) 1_555 1_555 1_555 no N3 C14 C13 115.7(3) 1_555 1_555 1_555 no N3 C14 C15 122.5(4) 1_555 1_555 1_555 no C13 C14 C15 121.8(3) 1_555 1_555 1_555 no C14 C15 C16 119.6(4) 1_555 1_555 1_555 no C15 C16 C17 117.0(5) 1_555 1_555 1_555 no C16 C17 C18 120.6(4) 1_555 1_555 1_555 no N3 C18 C17 122.6(4) 1_555 1_555 1_555 no #===END data_DSC90[Pd(pmea)Cl]Cl.H2O _database_code_depnum_ccdc_archive 'CCDC 298884' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C19 H20 Cl N4 Pd 1+,Cl -1,H2 O' _chemical_formula_sum 'C19 H22 Cl2 N4 O Pd' _chemical_formula_iupac ? _chemical_formula_weight 499.7 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.982(4) _cell_length_b 8.457(4) _cell_length_c 15.152(6) _cell_angle_alpha 75.76(2) _cell_angle_beta 84.97(3) _cell_angle_gamma 85.00(3) _cell_volume 985.3(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.68 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504.0 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.86 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3727 _diffrn_reflns_av_R_equivalents 0.011 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 3458 _reflns_number_gt 3059 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.056 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3059 _refine_ls_number_parameters 244 _refine_ls_goodness_of_fit_ref 1.55 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.015 _refine_diff_density_max 1.44 _refine_diff_density_min -1.25 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Pd 0.79319(4) 0.31351(4) 0.30657(2) 0.0336(1) Uani Pd 1.0 Cl1 0.79801(17) 0.24714(17) 0.46344(7) 0.0562(3) Uani Cl 1.0 N1 0.6956(4) 0.1068(4) 0.2980(2) 0.0382(8) Uani N 1.0 N2 0.9104(4) 0.5225(4) 0.2847(2) 0.0380(8) Uani N 1.0 N3 0.4252(5) 0.4560(5) 0.3051(3) 0.054(1) Uani N 1.0 N4 0.7848(4) 0.3759(4) 0.1689(2) 0.0359(8) Uani N 1.0 C1 0.7952(6) 0.2155(6) 0.1403(3) 0.047(1) Uani C 1.0 C2 0.7034(6) 0.0869(6) 0.2120(3) 0.044(1) Uani C 1.0 C3 0.6345(7) -0.0408(6) 0.1919(4) 0.054(1) Uani C 1.0 C4 0.5521(7) -0.1544(6) 0.2623(4) 0.059(1) Uani C 1.0 C5 0.5455(7) -0.1321(6) 0.3500(4) 0.056(1) Uani C 1.0 C6 0.6168(6) -0.0015(5) 0.3662(3) 0.045(1) Uani C 1.0 C7 0.9368(6) 0.4707(6) 0.1346(3) 0.043(1) Uani C 1.0 C8 0.9615(5) 0.5805(5) 0.1965(3) 0.0391(9) Uani C 1.0 C9 1.0390(6) 0.7253(6) 0.1663(3) 0.051(1) Uani C 1.0 C10 1.0715(7) 0.8117(6) 0.2303(4) 0.055(1) Uani C 1.0 C11 1.0215(7) 0.7490(6) 0.3202(4) 0.057(1) Uani C 1.0 C12 0.9386(6) 0.6087(6) 0.3461(3) 0.047(1) Uani C 1.0 C13 0.6346(6) 0.4866(6) 0.1355(3) 0.045(1) Uani C 1.0 C14 0.4632(6) 0.4112(6) 0.1519(3) 0.049(1) Uani C 1.0 C15 0.3911(5) 0.3652(5) 0.2484(3) 0.043(1) Uani C 1.0 C16 0.2877(6) 0.2345(6) 0.2765(4) 0.052(1) Uani C 1.0 C17 0.2199(7) 0.1943(7) 0.3647(4) 0.064(2) Uani C 1.0 C18 0.2549(7) 0.2887(7) 0.4232(4) 0.063(1) Uani C 1.0 C19 0.3545(7) 0.4146(7) 0.3913(4) 0.060(1) Uani C 1.0 Cl2 0.22070(15) 0.15265(15) 0.04463(9) 0.0541(3) Uani Cl 1.0 OW 0.5953(5) 0.1998(5) -0.0443(3) 0.0626(9) Uani O 1.0 H1C1 0.9163 0.1762 0.1327 0.047 Uani H 1.0 H2C1 0.7422 0.2330 0.0809 0.047 Uani H 1.0 HC3 0.6425 -0.0536 0.1278 0.054 Uani H 1.0 HC4 0.4996 -0.2488 0.2493 0.059 Uani H 1.0 HC5 0.4886 -0.2115 0.4015 0.056 Uani H 1.0 HC6 0.6105 0.0139 0.4298 0.045 Uani H 1.0 H1C7 0.9207 0.5388 0.0715 0.043 Uani H 1.0 H2C7 1.0385 0.3931 0.1335 0.043 Uani H 1.0 HC9 1.0716 0.7680 0.1000 0.051 Uani H 1.0 HC10 1.1295 0.9161 0.2110 0.055 Uani H 1.0 HC11 1.0460 0.8068 0.3673 0.057 Uani H 1.0 HC12 0.8979 0.5686 0.4115 0.047 Uani H 1.0 H1C13 0.6558 0.5301 0.0682 0.045 Uani H 1.0 H2C13 0.6262 0.5790 0.1664 0.045 Uani H 1.0 H1C14 0.4760 0.3099 0.1283 0.049 Uani H 1.0 H2C14 0.3806 0.4921 0.1160 0.049 Uani H 1.0 HC16 0.2632 0.1703 0.2323 0.052 Uani H 1.0 HC17 0.1474 0.0998 0.3864 0.064 Uani H 1.0 HC18 0.2071 0.2638 0.4879 0.063 Uani H 1.0 HC19 0.3774 0.4816 0.4343 0.060 Uani H 1.0 H1OW 0.4776 0.1857 -0.0165 0.063 Uani H 1.0 H2OW 0.6532 0.0902 -0.0446 0.063 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Pd 0.0406(2) 0.0330(2) 0.0243(2) -0.0048(1) 0.0046(1) -0.0027(1) Pd Cl1 0.0666(8) 0.0716(8) 0.0262(5) -0.0186(6) 0.0011(5) -0.0005(5) Cl N1 0.043(2) 0.036(2) 0.033(2) -0.002(2) 0.005(2) -0.004(2) N N2 0.043(2) 0.040(2) 0.030(2) -0.004(2) 0.000(2) -0.007(2) N N3 0.059(2) 0.054(3) 0.048(2) -0.008(2) 0.007(2) -0.013(2) N N4 0.045(2) 0.035(2) 0.027(2) -0.007(2) 0.006(1) -0.007(1) N C1 0.056(3) 0.048(3) 0.038(2) -0.009(2) 0.007(2) -0.016(2) C C2 0.046(2) 0.044(3) 0.041(2) -0.002(2) 0.003(2) -0.012(2) C C3 0.062(3) 0.048(3) 0.055(3) -0.006(2) 0.005(2) -0.020(2) C C4 0.066(3) 0.042(3) 0.071(4) -0.010(2) 0.003(3) -0.018(3) C C5 0.063(3) 0.038(3) 0.058(3) -0.012(2) 0.008(3) 0.001(2) C C6 0.050(2) 0.039(2) 0.039(2) -0.006(2) 0.009(2) -0.001(2) C C7 0.050(3) 0.047(3) 0.031(2) -0.013(2) 0.012(2) -0.009(2) C C8 0.038(2) 0.041(2) 0.037(2) -0.007(2) 0.003(2) -0.008(2) C C9 0.050(3) 0.050(3) 0.049(3) -0.016(2) 0.003(2) -0.003(2) C C10 0.059(3) 0.046(3) 0.061(3) -0.020(2) -0.007(2) -0.006(2) C C11 0.067(3) 0.052(3) 0.057(3) -0.011(3) -0.016(3) -0.018(3) C C12 0.057(3) 0.048(3) 0.040(3) -0.004(2) -0.007(2) -0.013(2) C C13 0.055(3) 0.041(2) 0.035(2) -0.005(2) 0.000(2) 0.000(2) C C14 0.051(3) 0.048(3) 0.044(3) -0.008(2) -0.005(2) -0.005(2) C C15 0.042(2) 0.036(2) 0.047(3) 0.001(2) 0.001(2) -0.003(2) C C16 0.047(3) 0.046(3) 0.059(3) -0.002(2) -0.003(2) -0.008(2) C C17 0.044(3) 0.058(3) 0.076(4) -0.007(2) 0.010(3) 0.006(3) C C18 0.062(3) 0.068(4) 0.051(3) 0.002(3) 0.014(3) -0.005(3) C C19 0.064(3) 0.067(4) 0.051(3) -0.002(3) 0.005(3) -0.020(3) C Cl2 0.0557(7) 0.0500(7) 0.0520(7) -0.0037(5) 0.0101(5) -0.0082(5) Cl OW 0.058(2) 0.052(2) 0.074(3) -0.008(2) 0.002(2) -0.009(2) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl1 2.307(1) 1_555 1_555 no Pd N1 2.012(4) 1_555 1_555 no Pd N2 2.013(4) 1_555 1_555 no Pd N4 2.027(3) 1_555 1_555 no N1 C2 1.349(6) 1_555 1_555 no N1 C6 1.351(5) 1_555 1_555 no N2 C8 1.345(5) 1_555 1_555 no N2 C12 1.359(6) 1_555 1_555 no N3 C15 1.342(6) 1_555 1_555 no N3 C19 1.352(6) 1_555 1_555 no N4 C1 1.516(5) 1_555 1_555 no N4 C7 1.496(5) 1_555 1_555 no N4 C13 1.500(6) 1_555 1_555 no C1 C2 1.523(6) 1_555 1_555 no C2 C3 1.362(6) 1_555 1_555 no C3 C4 1.406(7) 1_555 1_555 no C4 C5 1.383(8) 1_555 1_555 no C5 C6 1.368(7) 1_555 1_555 no C7 C8 1.508(6) 1_555 1_555 no C8 C9 1.378(6) 1_555 1_555 no C9 C10 1.403(7) 1_555 1_555 no C10 C11 1.372(7) 1_555 1_555 no C11 C12 1.364(7) 1_555 1_555 no C13 C14 1.534(6) 1_555 1_555 no C14 C15 1.495(7) 1_555 1_555 no C15 C16 1.397(6) 1_555 1_555 no C16 C17 1.370(8) 1_555 1_555 no C17 C18 1.389(9) 1_555 1_555 no C18 C19 1.351(8) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd N1 96.1(1) 1_555 1_555 1_555 no Cl1 Pd N2 96.3(1) 1_555 1_555 1_555 no Cl1 Pd N4 178.7(1) 1_555 1_555 1_555 no N1 Pd N2 166.6(1) 1_555 1_555 1_555 no N1 Pd N4 84.4(1) 1_555 1_555 1_555 no N2 Pd N4 83.3(1) 1_555 1_555 1_555 no Pd N1 C2 113.2(3) 1_555 1_555 1_555 no Pd N1 C6 127.0(3) 1_555 1_555 1_555 no C2 N1 C6 119.6(4) 1_555 1_555 1_555 no Pd N2 C8 112.8(3) 1_555 1_555 1_555 no Pd N2 C12 128.4(3) 1_555 1_555 1_555 no C8 N2 C12 118.7(4) 1_555 1_555 1_555 no C15 N3 C19 116.7(4) 1_555 1_555 1_555 no Pd N4 C1 105.5(3) 1_555 1_555 1_555 no Pd N4 C7 104.9(3) 1_555 1_555 1_555 no Pd N4 C13 114.2(3) 1_555 1_555 1_555 no C1 N4 C7 112.3(3) 1_555 1_555 1_555 no C1 N4 C13 113.1(3) 1_555 1_555 1_555 no C7 N4 C13 106.7(3) 1_555 1_555 1_555 no N4 C1 C2 110.5(3) 1_555 1_555 1_555 no N1 C2 C1 115.4(4) 1_555 1_555 1_555 no N1 C2 C3 121.7(4) 1_555 1_555 1_555 no C1 C2 C3 122.9(4) 1_555 1_555 1_555 no C2 C3 C4 119.3(5) 1_555 1_555 1_555 no C3 C4 C5 118.1(5) 1_555 1_555 1_555 no C4 C5 C6 120.1(4) 1_555 1_555 1_555 no N1 C6 C5 121.2(4) 1_555 1_555 1_555 no N4 C7 C8 109.8(3) 1_555 1_555 1_555 no N2 C8 C7 115.0(4) 1_555 1_555 1_555 no N2 C8 C9 122.2(4) 1_555 1_555 1_555 no C7 C8 C9 122.7(4) 1_555 1_555 1_555 no C8 C9 C10 118.8(4) 1_555 1_555 1_555 no C9 C10 C11 118.1(4) 1_555 1_555 1_555 no C10 C11 C12 120.8(5) 1_555 1_555 1_555 no N2 C12 C11 121.3(5) 1_555 1_555 1_555 no N4 C13 C14 117.0(4) 1_555 1_555 1_555 no C13 C14 C15 116.8(4) 1_555 1_555 1_555 no N3 C15 C14 117.9(4) 1_555 1_555 1_555 no N3 C15 C16 122.1(5) 1_555 1_555 1_555 no C14 C15 C16 120.0(4) 1_555 1_555 1_555 no C15 C16 C17 119.8(5) 1_555 1_555 1_555 no C16 C17 C18 118.1(5) 1_555 1_555 1_555 no C17 C18 C19 119.1(5) 1_555 1_555 1_555 no N3 C19 C18 124.3(5) 1_555 1_555 1_555 no #===END data_DSC68[Pd(tpa~OH)Cl]Cl.2H2O _database_code_depnum_ccdc_archive 'CCDC 298885' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C19 H20 Cl N4 O Pd 1+,Cl 1-,2(H2 O)' _chemical_formula_sum 'C19 H24 Cl2 N4 O3 Pd' _chemical_formula_iupac ? _chemical_formula_weight 533.7 # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.380(6) _cell_length_b 12.362(7) _cell_length_c 12.357(7) _cell_angle_alpha 66.43(5) _cell_angle_beta 71.09(5) _cell_angle_gamma 71.31(5) _cell_volume 1083(1) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.64 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540.0 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.94 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3987 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ;One ring, one chlorine and two waters were disordered over two sites each. The two positions of the ring were refined as identical refineable planar groups, with both assigned to a single 15-parameter TLX rigid body thermal group. ; _reflns_number_total 3790 _reflns_number_gt 2937 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.041 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2937 _refine_ls_number_parameters 269 _refine_ls_goodness_of_fit_ref 1.23 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.014 _refine_diff_density_max 0.65 _refine_diff_density_min -0.59 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy Pd 0.41158(4) 0.36032(3) 0.62272(3) 0.0413(1) Uani Pd 1.0 Cl 0.2808(2) 0.3668(1) 0.4829(1) 0.0564(3) Uani Cl 1.0 O1 0.3266(13) -0.1328(7) 0.7284(8) 0.101(3) Uani O 0.5 O1' 0.5692(11) -0.1308(7) 0.6448(7) 0.088(2) Uani O 0.5 N1 0.2061(5) 0.4604(3) 0.7064(3) 0.0489(9) Uani N 1.0 N2 0.6493(5) 0.2729(3) 0.5565(3) 0.053(1) Uani N 1.0 N3 0.4162(8) 0.1043(5) 0.7933(6) 0.041(1) Uani N 0.5 N3' 0.4876(8) 0.0915(5) 0.7881(6) 0.042(1) Uani N 0.5 N4 0.5186(5) 0.3437(3) 0.7545(3) 0.0490(9) Uani N 1.0 C1 0.4393(7) 0.4584(4) 0.7828(5) 0.058(1) Uani C 1.0 C2 0.2498(6) 0.4943(4) 0.7825(4) 0.053(1) Uani C 1.0 C3 0.1276(8) 0.5602(4) 0.8514(5) 0.064(1) Uani C 1.0 C4 -0.0431(8) 0.5916(4) 0.8404(5) 0.067(1) Uani C 1.0 C5 -0.0839(7) 0.5577(5) 0.7629(5) 0.066(1) Uani C 1.0 C6 0.0435(6) 0.4920(4) 0.6959(4) 0.056(1) Uani C 1.0 C7 0.7094(6) 0.3291(4) 0.7040(5) 0.061(1) Uani C 1.0 C8 0.7693(6) 0.2657(4) 0.6124(5) 0.059(1) Uani C 1.0 C9 0.9399(7) 0.2099(5) 0.5783(6) 0.084(2) Uani C 1.0 C10 0.9864(8) 0.1622(6) 0.4859(7) 0.097(2) Uani C 1.0 C11 0.8655(9) 0.1683(6) 0.4320(6) 0.085(2) Uani C 1.0 C12 0.6965(7) 0.2239(5) 0.4687(5) 0.066(1) Uani C 1.0 C13 0.4757(6) 0.2397(4) 0.8663(4) 0.057(1) Uani C 1.0 C14 0.5275(10) 0.1250(5) 0.8371(7) 0.0444(9) Uani C 0.5 C15 0.6781(10) 0.0406(7) 0.8609(8) 0.062(2) Uani C 0.5 C16 0.7125(10) -0.0655(6) 0.8390(7) 0.073(2) Uani C 0.5 C17 0.6013(10) -0.0881(5) 0.7947(7) 0.070(1) Uani C 0.5 C18 0.4525(9) -0.0009(6) 0.7724(6) 0.055(1) Uani C 0.5 C19 0.3141(18) -0.0133(10) 0.7211(11) 0.081(3) Uani C 0.5 C14' 0.5590(11) 0.1167(5) 0.8561(8) 0.049(1) Uani C 0.5 C15' 0.7106(11) 0.0441(6) 0.8908(9) 0.072(2) Uani C 0.5 C16' 0.7878(10) -0.0551(6) 0.8544(7) 0.084(2) Uani C 0.5 C17' 0.7174(10) -0.0822(6) 0.7854(7) 0.078(1) Uani C 0.5 C18' 0.5657(9) -0.0067(6) 0.7531(6) 0.057(1) Uani C 0.5 C19' 0.4792(18) -0.0251(10) 0.6740(11) 0.079(2) Uani C 0.5 Cl2 0.1652(4) -0.2490(3) 0.5040(3) 0.0786(8) Uani Cl 0.5 Cl2' 0.4532(4) -0.3225(3) 0.8968(3) 0.0700(6) Uani Cl 0.5 OW1 0.9058(10) 0.1362(8) 1.1045(9) 0.102(3) Uani O 0.5 OW1' 0.5468(11) -0.3990(8) 0.9301(7) 0.084(2) Uani O 0.5 OW2 1.0455(11) 0.2179(9) 0.8498(9) 0.105(3) Uani O 0.5 OW2' -0.1051(10) -0.1172(8) 1.1748(8) 0.087(2) Uani O 0.5 H1C1 0.4981 0.5237 0.7203 0.058 Uani H 1.0 H2C1 0.4531 0.4463 0.8646 0.058 Uani H 1.0 HC3 0.1603 0.5849 0.9077 0.064 Uani H 1.0 HC4 -0.1352 0.6390 0.8896 0.067 Uani H 1.0 HC5 -0.2061 0.5802 0.7545 0.066 Uani H 1.0 HC6 0.0130 0.4678 0.6383 0.056 Uani H 1.0 H1C7 0.7705 0.2807 0.7716 0.061 Uani H 1.0 H2C7 0.7377 0.4108 0.6644 0.061 Uani H 1.0 HC9 1.0282 0.2041 0.6198 0.084 Uani H 1.0 HC10 1.1098 0.1230 0.4589 0.097 Uani H 1.0 HC11 0.8986 0.1327 0.3659 0.085 Uani H 1.0 HC12 0.6071 0.2277 0.4290 0.066 Uani H 1.0 H1C13 0.3484 0.2566 0.9013 0.057 Uani H 1.0 H2C13 0.5390 0.2300 0.9269 0.057 Uani H 1.0 HC15 0.7596 0.0570 0.8933 0.082 Uani H 0.5 HC16 0.8207 -0.1275 0.8557 0.098 Uani H 0.5 HC17 0.6267 -0.1658 0.7787 0.092 Uani H 0.5 H1C19 0.3276 0.0389 0.6340 0.091 Uani H 0.5 H2C19 0.1969 0.0158 0.7679 0.082 Uani H 0.5 HC15' 0.7623 0.0638 0.9413 0.096 Uani H 0.5 HC16' 0.8974 -0.1086 0.8786 0.114 Uani H 0.5 HC17' 0.7741 -0.1548 0.7589 0.103 Uani H 0.5 H1C19' 0.4777 0.0460 0.5976 0.081 Uani H 0.5 H2C19' 0.3578 -0.0323 0.7183 0.081 Uani H 0.5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Pd 0.0414(2) 0.0445(2) 0.0406(2) -0.0116(1) -0.0145(1) -0.0109(1) Pd Cl 0.0590(7) 0.0702(8) 0.0497(7) -0.0173(6) -0.0214(6) -0.0198(6) Cl O1 0.146(8) 0.085(6) 0.102(7) -0.037(6) -0.044(6) -0.041(5) O O1' 0.095(6) 0.087(6) 0.098(6) -0.008(5) -0.009(5) -0.065(5) O N1 0.057(2) 0.049(2) 0.045(2) -0.007(2) -0.022(2) -0.015(2) N N2 0.044(2) 0.052(2) 0.051(2) -0.012(2) -0.012(2) -0.005(2) N N3 0.031(2) 0.045(1) 0.042(2) 0.004(1) -0.017(2) -0.010(1) N N3' 0.031(3) 0.045(1) 0.041(2) 0.005(1) -0.016(2) -0.010(1) N N4 0.056(2) 0.049(2) 0.047(2) -0.016(2) -0.026(2) -0.007(2) N C1 0.071(3) 0.056(3) 0.063(3) -0.018(2) -0.028(3) -0.022(3) C C2 0.070(3) 0.045(3) 0.047(3) -0.016(2) -0.020(2) -0.012(2) C C3 0.090(4) 0.054(3) 0.054(3) -0.015(3) -0.019(3) -0.022(2) C C4 0.087(4) 0.049(3) 0.052(3) 0.001(3) -0.010(3) -0.019(2) C C5 0.059(3) 0.068(3) 0.060(3) 0.002(3) -0.016(3) -0.020(3) C C6 0.050(3) 0.060(3) 0.056(3) -0.003(2) -0.021(2) -0.019(2) C C7 0.052(3) 0.060(3) 0.069(3) -0.024(2) -0.028(3) 0.000(3) C C8 0.051(3) 0.051(3) 0.062(3) -0.017(2) -0.016(2) 0.001(2) C C9 0.042(3) 0.077(4) 0.094(5) -0.011(3) -0.015(3) 0.008(4) C C10 0.057(4) 0.082(4) 0.095(5) 0.001(3) 0.014(4) -0.011(4) C C11 0.074(4) 0.076(4) 0.071(4) -0.001(3) 0.004(3) -0.021(3) C C12 0.067(4) 0.062(3) 0.052(3) -0.009(3) 0.000(3) -0.016(3) C C13 0.068(3) 0.060(3) 0.046(3) -0.020(3) -0.025(2) -0.008(2) C C14 0.036(3) 0.053(1) 0.036(2) 0.002(1) -0.022(2) -0.005(1) C C15 0.036(3) 0.065(2) 0.060(3) -0.001(2) -0.028(2) 0.011(2) C C16 0.032(2) 0.054(1) 0.080(3) 0.009(1) -0.007(2) 0.009(2) C C17 0.055(3) 0.044(1) 0.075(4) 0.004(1) 0.004(3) -0.012(1) C C18 0.053(2) 0.047(1) 0.058(2) -0.004(2) -0.013(2) -0.015(1) C C19 0.106(5) 0.069(2) 0.085(6) -0.038(4) -0.038(5) -0.016(3) C C14' 0.041(3) 0.059(1) 0.039(2) -0.001(1) -0.025(2) -0.002(1) C C15' 0.047(3) 0.079(2) 0.065(3) -0.010(2) -0.040(3) 0.020(2) C C16' 0.031(3) 0.067(2) 0.093(4) 0.005(2) -0.018(2) 0.024(2) C C17' 0.045(2) 0.047(1) 0.085(4) 0.010(1) 0.008(3) -0.001(1) C C18' 0.050(2) 0.045(1) 0.059(2) 0.002(2) -0.005(2) -0.014(1) C C19' 0.114(5) 0.059(2) 0.072(4) -0.027(3) -0.013(4) -0.028(2) C Cl2 0.074(2) 0.081(2) 0.084(2) 0.003(2) -0.027(2) -0.039(2) Cl Cl2' 0.065(1) 0.065(1) 0.096(2) -0.005(1) -0.030(1) -0.042(1) Cl OW1 0.061(5) 0.114(7) 0.117(7) -0.012(5) -0.023(5) -0.029(6) O OW1' 0.072(5) 0.100(5) 0.079(4) -0.004(4) -0.017(4) -0.040(4) O OW2 0.063(5) 0.101(7) 0.124(8) 0.003(5) -0.029(5) -0.021(6) O OW2' 0.061(5) 0.107(7) 0.105(7) 0.005(5) -0.032(5) -0.054(6) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl 2.292(1) 1_555 1_555 no Pd N1 2.017(4) 1_555 1_555 no Pd N2 2.019(4) 1_555 1_555 no Pd N4 2.015(3) 1_555 1_555 no O1 C19 1.415(13) 1_555 1_555 no O1' C19' 1.406(13) 1_555 1_555 no N1 C2 1.352(5) 1_555 1_555 no N1 C6 1.327(6) 1_555 1_555 no N2 C8 1.357(6) 1_555 1_555 no N2 C12 1.340(6) 1_555 1_555 no N3 C14 1.348(5) 1_555 1_555 no N3 C18 1.348(5) 1_555 1_555 no N3' C14' 1.348(5) 1_555 1_555 no N3' C18' 1.348(5) 1_555 1_555 no N4 C1 1.488(6) 1_555 1_555 no N4 C7 1.496(6) 1_555 1_555 no N4 C13 1.499(5) 1_555 1_555 no C1 C2 1.507(7) 1_555 1_555 no C2 C3 1.376(7) 1_555 1_555 no C3 C4 1.394(7) 1_555 1_555 no C4 C5 1.354(7) 1_555 1_555 no C5 C6 1.376(7) 1_555 1_555 no C7 C8 1.494(8) 1_555 1_555 no C8 C9 1.381(7) 1_555 1_555 no C9 C10 1.380(10) 1_555 1_555 no C10 C11 1.351(10) 1_555 1_555 no C11 C12 1.376(8) 1_555 1_555 no C13 C14 1.498(7) 1_555 1_555 no C13 C14' 1.494(6) 1_555 1_555 no C14 C15 1.385(6) 1_555 1_555 no C15 C16 1.367(6) 1_555 1_555 no C16 C17 1.367(6) 1_555 1_555 no C17 C18 1.385(6) 1_555 1_555 no C18 C19 1.561(13) 1_555 1_555 no C14' C15' 1.385(6) 1_555 1_555 no C15' C16' 1.367(6) 1_555 1_555 no C16' C17' 1.367(6) 1_555 1_555 no C17' C18' 1.385(6) 1_555 1_555 no C18' C19' 1.508(13) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Pd N1 96.3(1) 1_555 1_555 1_555 no Cl Pd N2 96.6(1) 1_555 1_555 1_555 no Cl Pd N4 175.6(1) 1_555 1_555 1_555 no N1 Pd N2 166.2(1) 1_555 1_555 1_555 no N1 Pd N4 83.4(1) 1_555 1_555 1_555 no N2 Pd N4 84.2(2) 1_555 1_555 1_555 no Pd N1 C2 111.8(3) 1_555 1_555 1_555 no Pd N1 C6 128.2(3) 1_555 1_555 1_555 no C2 N1 C6 120.1(4) 1_555 1_555 1_555 no Pd N2 C8 112.2(3) 1_555 1_555 1_555 no Pd N2 C12 128.1(4) 1_555 1_555 1_555 no C8 N2 C12 119.6(4) 1_555 1_555 1_555 no C14 N3 C18 119.2(5) 1_555 1_555 1_555 no C14' N3' C18' 119.2(5) 1_555 1_555 1_555 no Pd N4 C1 105.1(3) 1_555 1_555 1_555 no Pd N4 C7 107.2(3) 1_555 1_555 1_555 no Pd N4 C13 111.5(3) 1_555 1_555 1_555 no C1 N4 C7 112.1(4) 1_555 1_555 1_555 no C1 N4 C13 109.0(4) 1_555 1_555 1_555 no C7 N4 C13 111.8(4) 1_555 1_555 1_555 no N4 C1 C2 109.4(4) 1_555 1_555 1_555 no N1 C2 C1 115.6(4) 1_555 1_555 1_555 no N1 C2 C3 121.2(5) 1_555 1_555 1_555 no C1 C2 C3 123.3(4) 1_555 1_555 1_555 no C2 C3 C4 118.1(5) 1_555 1_555 1_555 no C3 C4 C5 119.8(5) 1_555 1_555 1_555 no C4 C5 C6 119.7(5) 1_555 1_555 1_555 no N1 C6 C5 121.1(5) 1_555 1_555 1_555 no N4 C7 C8 111.3(4) 1_555 1_555 1_555 no N2 C8 C7 116.6(4) 1_555 1_555 1_555 no N2 C8 C9 120.5(5) 1_555 1_555 1_555 no C7 C8 C9 122.8(5) 1_555 1_555 1_555 no C8 C9 C10 118.9(6) 1_555 1_555 1_555 no C9 C10 C11 120.1(6) 1_555 1_555 1_555 no C10 C11 C12 119.5(6) 1_555 1_555 1_555 no N2 C12 C11 121.3(6) 1_555 1_555 1_555 no N4 C13 C14 110.7(5) 1_555 1_555 1_555 no N4 C13 C14' 115.7(5) 1_555 1_555 1_555 no N3 C14 C13 117.0(5) 1_555 1_555 1_555 no N3 C14 C15 121.6(4) 1_555 1_555 1_555 no C13 C14 C15 121.3(6) 1_555 1_555 1_555 no C14 C15 C16 118.4(5) 1_555 1_555 1_555 no C15 C16 C17 120.9(7) 1_555 1_555 1_555 no C16 C17 C18 118.4(5) 1_555 1_555 1_555 no N3 C18 C17 121.6(4) 1_555 1_555 1_555 no N3 C18 C19 114.1(7) 1_555 1_555 1_555 no C17 C18 C19 124.3(7) 1_555 1_555 1_555 no O1 C19 C18 114.2(9) 1_555 1_555 1_555 no N3' C14' C13 111.7(5) 1_555 1_555 1_555 no N3' C14' C15' 121.6(4) 1_555 1_555 1_555 no C13 C14' C15' 125.7(6) 1_555 1_555 1_555 no C14' C15' C16' 118.4(5) 1_555 1_555 1_555 no C15' C16' C17' 120.9(7) 1_555 1_555 1_555 no C16' C17' C18' 118.4(5) 1_555 1_555 1_555 no N3' C18' C17' 121.6(4) 1_555 1_555 1_555 no N3' C18' C19' 115.2(7) 1_555 1_555 1_555 no C17' C18' C19' 123.2(7) 1_555 1_555 1_555 no O1' C19' C18' 110.4(10) 1_555 1_555 1_555 no #===END data_DSC93[Pt(tmpa)Cl]Cl.2H2O _database_code_depnum_ccdc_archive 'CCDC 298886' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C18 H18 N4 Cl Pt 1+,Cl 1-,2(H2 O)' _chemical_formula_sum 'C18 H22 Cl2 N4 O2 Pt' _chemical_formula_iupac ? _chemical_formula_weight 592.4 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z 3 -x,-y,-z 4 -x,y,1/2-z 5 1/2+x,1/2+y,z 6 1/2+x,1/2-y,1/2+z 7 1/2-x,1/2-y,-z 8 1/2-x,1/2+y,1/2-z _cell_length_a 26.767(5) _cell_length_b 10.707(1) _cell_length_c 30.131(5) _cell_angle_alpha 90 _cell_angle_beta 105.575(8) _cell_angle_gamma 90 _cell_volume 8318(2) _cell_formula_units_Z 16 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _cell_measurement_temperature 294 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.89 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576.0 _exptl_absorpt_coefficient_mu 7.095 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.70 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 5884 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5749 _reflns_number_gt 3856 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.023 _refine_ls_wR_factor_ref 0.028 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3856 _refine_ls_number_parameters 343 _refine_ls_goodness_of_fit_ref 0.93 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.020 _refine_diff_density_max 0.96 _refine_diff_density_min -0.99 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy PtA 0.51064(1) 0.03256(3) 0.09971(1) 0.0364(1) Uani Pt 1.0 ClA 0.53630(8) -0.10176(20) 0.05078(6) 0.0574(5) Uani Cl 1.0 N1A 0.4345(2) -0.0001(5) 0.0764(2) 0.044(1) Uani N 1.0 N2A 0.5821(2) 0.0870(6) 0.1346(2) 0.041(2) Uani N 1.0 N3A 0.3941(2) 0.3511(6) 0.0991(2) 0.046(1) Uani N 1.0 N4A 0.4886(2) 0.1436(5) 0.1455(2) 0.035(1) Uani N 1.0 C1A 0.4393(3) 0.0887(7) 0.1511(2) 0.043(2) Uani C 1.0 C2A 0.4074(3) 0.0413(7) 0.1055(3) 0.048(2) Uani C 1.0 C3A 0.3540(3) 0.0334(9) 0.0939(3) 0.068(2) Uani C 1.0 C4A 0.3281(3) -0.0168(9) 0.0516(4) 0.079(2) Uani C 1.0 C5A 0.3555(4) -0.0556(8) 0.0216(3) 0.074(2) Uani C 1.0 C6A 0.4087(3) -0.0482(7) 0.0346(3) 0.058(2) Uani C 1.0 C7A 0.5330(3) 0.1336(7) 0.1890(2) 0.045(2) Uani C 1.0 C8A 0.5833(3) 0.1375(7) 0.1764(2) 0.042(2) Uani C 1.0 C9A 0.6282(3) 0.1839(7) 0.2045(3) 0.054(2) Uani C 1.0 C10A 0.6733(3) 0.1780(8) 0.1907(3) 0.062(3) Uani C 1.0 C11A 0.6718(3) 0.1286(7) 0.1480(3) 0.059(2) Uani C 1.0 C12A 0.6257(3) 0.0864(7) 0.1210(3) 0.050(2) Uani C 1.0 C13A 0.4823(3) 0.2803(6) 0.1315(2) 0.036(2) Uani C 1.0 C14A 0.4372(3) 0.3067(6) 0.0902(2) 0.038(2) Uani C 1.0 C15A 0.4428(3) 0.2922(7) 0.0461(2) 0.044(1) Uani C 1.0 C16A 0.4011(3) 0.3245(7) 0.0097(2) 0.056(2) Uani C 1.0 C17A 0.3563(3) 0.3706(8) 0.0177(3) 0.062(2) Uani C 1.0 C18A 0.3548(3) 0.3826(8) 0.0630(3) 0.058(2) Uani C 1.0 PtB 0.58781(1) 0.53015(3) 0.11913(1) 0.0308(1) Uani Pt 1.0 ClB 0.57421(7) 0.39657(19) 0.05766(6) 0.0501(5) Uani Cl 1.0 N1B 0.6625(2) 0.4830(5) 0.1462(2) 0.036(1) Uani N 1.0 N2B 0.5150(2) 0.5955(5) 0.1059(2) 0.034(1) Uani N 1.0 N3B 0.7072(2) 0.8038(6) 0.1931(2) 0.052(2) Uani N 1.0 N4B 0.5990(2) 0.6381(5) 0.1765(2) 0.032(1) Uani N 1.0 C1B 0.6408(3) 0.5726(7) 0.2124(2) 0.044(2) Uani C 1.0 C2B 0.6802(3) 0.5188(7) 0.1911(2) 0.040(1) Uani C 1.0 C3B 0.7306(3) 0.4978(7) 0.2153(3) 0.055(2) Uani C 1.0 C4B 0.7640(3) 0.4443(8) 0.1928(3) 0.064(2) Uani C 1.0 C5B 0.7466(3) 0.4111(8) 0.1471(3) 0.058(2) Uani C 1.0 C6B 0.6951(3) 0.4321(6) 0.1243(3) 0.043(2) Uani C 1.0 C7B 0.5473(3) 0.6378(7) 0.1874(2) 0.042(2) Uani C 1.0 C8B 0.5042(3) 0.6452(6) 0.1432(2) 0.038(1) Uani C 1.0 C9B 0.4558(3) 0.6923(7) 0.1418(3) 0.049(2) Uani C 1.0 C10B 0.4173(3) 0.6881(7) 0.1004(3) 0.051(2) Uani C 1.0 C11B 0.4292(3) 0.6418(7) 0.0618(2) 0.043(2) Uani C 1.0 C12B 0.4780(3) 0.5961(7) 0.0649(2) 0.039(2) Uani C 1.0 C13B 0.6137(3) 0.7716(7) 0.1702(2) 0.042(2) Uani C 1.0 C14B 0.6643(3) 0.7875(7) 0.1577(2) 0.044(2) Uani C 1.0 C15B 0.6654(3) 0.7866(8) 0.1125(3) 0.056(2) Uani C 1.0 C16B 0.7125(4) 0.8030(9) 0.1025(3) 0.070(3) Uani C 1.0 C17B 0.7565(3) 0.8172(9) 0.1377(3) 0.072(3) Uani C 1.0 C18B 0.7517(3) 0.8153(9) 0.1823(3) 0.066(3) Uani C 1.0 Cl1 0.76310(9) 1.13311(23) 0.07538(7) 0.0704(7) Uani Cl 1.0 Cl2 0.5000(0) 0.8772(3) 0.2500(0) 0.0511(7) Uani Cl 1.0 Cl3 0.5000(0) 0.4031(3) 0.2500(0) 0.0591(8) Uani Cl 1.0 OW1 0.3835(2) 0.3962(7) 0.1910(2) 0.083(2) Uani O 1.0 OW2 0.7976(2) 1.1360(6) -0.0182(2) 0.072(2) Uani O 1.0 OW3 0.3292(3) 0.6325(6) 0.1776(2) 0.093(2) Uani O 1.0 OW4 0.3796(2) 0.8627(7) 0.2081(3) 0.116(3) Uani O 1.0 H1C1A 0.4194 0.1542 0.1628 0.043 Uani H 1.0 H2C1A 0.4476 0.0181 0.1737 0.043 Uani H 1.0 HC3A 0.3342 0.0633 0.1158 0.085 Uani H 1.0 HC4A 0.2895 -0.0248 0.0428 0.102 Uani H 1.0 HC5A 0.3369 -0.0889 -0.0095 0.091 Uani H 1.0 HC6A 0.4288 -0.0784 0.0131 0.068 Uani H 1.0 H1C7A 0.5302 0.0531 0.2050 0.045 Uani H 1.0 H2C7A 0.5314 0.2051 0.2099 0.045 Uani H 1.0 HC9A 0.6284 0.2219 0.2348 0.067 Uani H 1.0 HC10A 0.7067 0.2091 0.2114 0.080 Uani H 1.0 HC11A 0.7040 0.1240 0.1372 0.073 Uani H 1.0 HC12A 0.6243 0.0536 0.0896 0.060 Uani H 1.0 H1C13A 0.5148 0.3084 0.1241 0.036 Uani H 1.0 H2C13A 0.4772 0.3295 0.1581 0.036 Uani H 1.0 HC15A 0.4758 0.2596 0.0408 0.050 Uani H 1.0 HC16A 0.4034 0.3143 -0.0227 0.072 Uani H 1.0 HC17A 0.3259 0.3945 -0.0083 0.080 Uani H 1.0 HC18A 0.3226 0.4169 0.0691 0.075 Uani H 1.0 H1C1B 0.6249 0.5039 0.2265 0.044 Uani H 1.0 H2C1B 0.6580 0.6338 0.2368 0.044 Uani H 1.0 HC3B 0.7430 0.5208 0.2486 0.064 Uani H 1.0 HC4B 0.8011 0.4296 0.2099 0.083 Uani H 1.0 HC5B 0.7707 0.3725 0.1307 0.070 Uani H 1.0 HC6B 0.6820 0.4091 0.0911 0.045 Uani H 1.0 H1C7B 0.5451 0.7113 0.2072 0.042 Uani H 1.0 H2C7B 0.5436 0.5591 0.2041 0.042 Uani H 1.0 HC9B 0.4486 0.7287 0.1700 0.069 Uani H 1.0 HC10B 0.3814 0.7182 0.0986 0.069 Uani H 1.0 HC11B 0.4023 0.6415 0.0315 0.055 Uani H 1.0 HC12B 0.4863 0.5629 0.0367 0.051 Uani H 1.0 H1C13B 0.6164 0.8173 0.1997 0.042 Uani H 1.0 H2C13B 0.5855 0.8096 0.1451 0.042 Uani H 1.0 HC15B 0.6328 0.7744 0.0873 0.067 Uani H 1.0 HC16B 0.7143 0.8043 0.0697 0.091 Uani H 1.0 HC17B 0.7911 0.8287 0.1315 0.090 Uani H 1.0 HC18B 0.7840 0.8231 0.2081 0.084 Uani H 1.0 H1OW1 0.3846 0.3807 0.1586 0.083 Uani H 1.0 H2OW1 0.4197 0.3994 0.2116 0.083 Uani H 1.0 H1OW2 0.7877 1.1321 0.0115 0.072 Uani H 1.0 H2OW2 0.7792 1.2074 -0.0371 0.072 Uani H 1.0 H1OW3 0.3485 0.5516 0.1833 0.093 Uani H 1.0 H2OW3 0.3075 0.6355 0.1449 0.093 Uani H 1.0 H1OW4 0.3655 0.7775 0.1984 0.116 Uani H 1.0 H2OW4 0.4181 0.8577 0.2209 0.116 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PtA 0.0384(2) 0.0309(2) 0.0381(2) 0.0008(1) 0.0075(1) 0.0033(1) Pt ClA 0.067(1) 0.051(1) 0.053(1) 0.012(1) 0.014(1) -0.006(1) Cl N1A 0.044(2) 0.031(3) 0.052(3) -0.002(2) 0.003(2) 0.009(2) N N2A 0.042(2) 0.035(3) 0.047(2) 0.004(2) 0.011(2) 0.007(2) N N3A 0.048(2) 0.040(3) 0.053(2) 0.007(2) 0.016(2) 0.003(2) N N4A 0.036(3) 0.036(4) 0.035(3) -0.001(3) 0.014(3) 0.004(3) N C1A 0.040(4) 0.043(5) 0.052(5) -0.002(4) 0.019(4) 0.009(4) C C2A 0.039(2) 0.043(3) 0.061(3) -0.007(2) 0.010(2) 0.012(2) C C3A 0.040(2) 0.068(4) 0.095(4) -0.016(3) 0.014(2) 0.010(3) C C4A 0.047(2) 0.072(4) 0.105(5) -0.022(3) -0.005(2) 0.013(3) C C5A 0.066(3) 0.058(4) 0.078(4) -0.023(3) -0.014(2) 0.009(3) C C6A 0.065(3) 0.041(3) 0.058(3) -0.011(3) -0.002(2) 0.004(3) C C7A 0.041(4) 0.058(6) 0.035(4) 0.003(4) 0.007(3) 0.010(4) C C8A 0.043(2) 0.037(3) 0.044(2) 0.004(2) 0.007(2) 0.008(2) C C9A 0.050(2) 0.049(4) 0.054(2) 0.001(2) -0.001(2) 0.005(2) C C10A 0.041(2) 0.048(4) 0.086(4) 0.001(2) 0.000(2) 0.009(3) C C11A 0.043(2) 0.039(4) 0.096(4) 0.005(2) 0.023(2) 0.012(3) C C12A 0.050(2) 0.038(3) 0.067(3) 0.005(2) 0.024(2) 0.008(2) C C13A 0.039(4) 0.026(4) 0.042(4) 0.002(3) 0.008(3) 0.000(3) C C14A 0.047(2) 0.028(4) 0.039(2) 0.003(2) 0.013(2) 0.003(2) C C15A 0.061(2) 0.034(3) 0.037(2) 0.006(2) 0.013(2) 0.002(2) C C16A 0.078(3) 0.043(4) 0.041(2) 0.009(3) 0.003(2) 0.002(2) C C17A 0.066(3) 0.048(5) 0.059(2) 0.010(3) -0.006(2) 0.003(3) C C18A 0.050(2) 0.051(4) 0.069(3) 0.011(2) 0.007(2) 0.003(3) C PtB 0.0331(2) 0.0329(2) 0.0274(1) -0.0001(1) 0.0097(1) -0.0012(1) Pt ClB 0.049(1) 0.059(1) 0.042(1) 0.001(1) 0.0116(9) -0.017(1) Cl N1B 0.037(2) 0.031(2) 0.040(2) 0.002(2) 0.011(1) 0.001(2) N N2B 0.035(2) 0.030(3) 0.040(2) -0.002(2) 0.013(1) 0.000(2) N N3B 0.048(2) 0.055(3) 0.048(2) -0.010(2) 0.002(2) 0.001(2) N N4B 0.033(3) 0.034(4) 0.030(3) 0.004(3) 0.012(2) -0.005(3) N C1B 0.048(5) 0.054(5) 0.027(4) 0.004(4) 0.002(3) 0.004(3) C C2B 0.042(2) 0.036(3) 0.040(2) 0.000(2) 0.004(2) 0.002(2) C C3B 0.046(2) 0.050(4) 0.057(2) 0.001(2) -0.004(2) 0.005(2) C C4B 0.040(2) 0.060(4) 0.086(3) 0.008(2) 0.003(2) 0.007(3) C C5B 0.042(2) 0.049(4) 0.085(4) 0.009(2) 0.022(2) 0.004(3) C C6B 0.043(2) 0.035(3) 0.056(2) 0.004(2) 0.021(2) 0.001(2) C C7B 0.035(4) 0.057(6) 0.041(4) -0.002(4) 0.020(3) -0.005(4) C C8B 0.040(2) 0.033(2) 0.040(2) -0.001(2) 0.013(1) -0.003(2) C C9B 0.048(3) 0.049(3) 0.055(2) 0.006(3) 0.021(2) -0.009(3) C C10B 0.039(2) 0.047(4) 0.066(3) 0.007(2) 0.015(2) -0.002(3) C C11B 0.039(2) 0.037(4) 0.051(2) -0.002(2) 0.006(2) 0.004(2) C C12B 0.042(2) 0.036(3) 0.039(2) -0.003(2) 0.011(1) 0.000(2) C C13B 0.046(5) 0.029(4) 0.051(5) 0.006(4) 0.012(4) -0.009(4) C C14B 0.048(2) 0.037(4) 0.041(2) -0.004(2) 0.004(2) 0.003(2) C C15B 0.062(2) 0.060(4) 0.044(2) -0.016(3) 0.010(2) 0.002(3) C C16B 0.074(3) 0.081(5) 0.060(2) -0.027(4) 0.025(3) -0.009(4) C C17B 0.062(3) 0.081(6) 0.076(4) -0.020(3) 0.024(3) -0.009(4) C C18B 0.050(2) 0.077(5) 0.066(3) -0.015(2) 0.008(2) 0.000(4) C Cl1 0.075(2) 0.087(2) 0.048(1) 0.027(1) 0.015(1) 0.011(1) Cl Cl2 0.059(2) 0.044(2) 0.047(2) 0.0000(0) 0.008(1) 0.0000(0) Cl Cl3 0.073(2) 0.060(2) 0.042(2) 0.0000(0) 0.012(1) 0.0000(0) Cl OW1 0.060(4) 0.126(6) 0.066(4) 0.010(4) 0.022(3) -0.013(4) O OW2 0.075(4) 0.079(5) 0.068(4) 0.024(3) 0.031(3) 0.007(3) O OW3 0.114(5) 0.101(6) 0.051(4) 0.030(4) 0.000(4) -0.006(4) O OW4 0.055(4) 0.116(7) 0.179(7) 0.019(4) 0.034(5) -0.001(5) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PtA ClA 2.293(2) 1_555 1_555 no PtA N1A 2.000(6) 1_555 1_555 no PtA N2A 2.006(6) 1_555 1_555 no PtA N4A 2.026(5) 1_555 1_555 no N1A C2A 1.353(9) 1_555 1_555 no N1A C6A 1.365(9) 1_555 1_555 no N2A C8A 1.364(8) 1_555 1_555 no N2A C12A 1.336(8) 1_555 1_555 no N3A C14A 1.341(8) 1_555 1_555 no N3A C18A 1.338(9) 1_555 1_555 no N4A C1A 1.494(8) 1_555 1_555 no N4A C7A 1.518(8) 1_555 1_555 no N4A C13A 1.521(8) 1_555 1_555 no C1A C2A 1.500(10) 1_555 1_555 no C2A C3A 1.381(10) 1_555 1_555 no C3A C4A 1.387(12) 1_555 1_555 no C4A C5A 1.371(13) 1_555 1_555 no C5A C6A 1.374(11) 1_555 1_555 no C7A C8A 1.493(9) 1_555 1_555 no C8A C9A 1.364(9) 1_555 1_555 no C9A C10A 1.381(10) 1_555 1_555 no C10A C11A 1.380(11) 1_555 1_555 no C11A C12A 1.361(10) 1_555 1_555 no C13A C14A 1.507(9) 1_555 1_555 no C14A C15A 1.386(9) 1_555 1_555 no C15A C16A 1.383(9) 1_555 1_555 no C16A C17A 1.376(11) 1_555 1_555 no C17A C18A 1.381(10) 1_555 1_555 no PtB ClB 2.290(2) 1_555 1_555 no PtB N1B 2.010(5) 1_555 1_555 no PtB N2B 2.008(5) 1_555 1_555 no PtB N4B 2.034(5) 1_555 1_555 no N1B C2B 1.364(8) 1_555 1_555 no N1B C6B 1.342(8) 1_555 1_555 no N2B C8B 1.342(8) 1_555 1_555 no N2B C12B 1.361(8) 1_555 1_555 no N3B C14B 1.352(8) 1_555 1_555 no N3B C18B 1.323(9) 1_555 1_555 no N4B C1B 1.503(8) 1_555 1_555 no N4B C7B 1.507(8) 1_555 1_555 no N4B C13B 1.508(8) 1_555 1_555 no C1B C2B 1.490(9) 1_555 1_555 no C2B C3B 1.368(9) 1_555 1_555 no C3B C4B 1.384(11) 1_555 1_555 no C4B C5B 1.378(11) 1_555 1_555 no C5B C6B 1.383(10) 1_555 1_555 no C7B C8B 1.513(9) 1_555 1_555 no C8B C9B 1.380(9) 1_555 1_555 no C9B C10B 1.389(10) 1_555 1_555 no C10B C11B 1.378(10) 1_555 1_555 no C11B C12B 1.373(9) 1_555 1_555 no C13B C14B 1.510(9) 1_555 1_555 no C14B C15B 1.368(9) 1_555 1_555 no C15B C16B 1.386(11) 1_555 1_555 no C16B C17B 1.367(11) 1_555 1_555 no C17B C18B 1.382(10) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag ClA PtA N1A 96.8(2) 1_555 1_555 1_555 no ClA PtA N2A 96.4(2) 1_555 1_555 1_555 no ClA PtA N4A 176.9(2) 1_555 1_555 1_555 no N1A PtA N2A 166.7(2) 1_555 1_555 1_555 no N1A PtA N4A 83.4(2) 1_555 1_555 1_555 no N2A PtA N4A 83.3(2) 1_555 1_555 1_555 no PtA N1A C2A 112.8(5) 1_555 1_555 1_555 no PtA N1A C6A 127.2(5) 1_555 1_555 1_555 no C2A N1A C6A 119.7(7) 1_555 1_555 1_555 no PtA N2A C8A 112.4(4) 1_555 1_555 1_555 no PtA N2A C12A 128.8(5) 1_555 1_555 1_555 no C8A N2A C12A 118.7(6) 1_555 1_555 1_555 no C14A N3A C18A 117.2(6) 1_555 1_555 1_555 no PtA N4A C1A 105.9(4) 1_555 1_555 1_555 no PtA N4A C7A 104.1(4) 1_555 1_555 1_555 no PtA N4A C13A 113.9(4) 1_555 1_555 1_555 no C1A N4A C7A 112.7(5) 1_555 1_555 1_555 no C1A N4A C13A 112.0(5) 1_555 1_555 1_555 no C7A N4A C13A 108.1(5) 1_555 1_555 1_555 no N4A C1A C2A 109.4(5) 1_555 1_555 1_555 no N1A C2A C1A 115.6(6) 1_555 1_555 1_555 no N1A C2A C3A 121.1(8) 1_555 1_555 1_555 no C1A C2A C3A 123.3(7) 1_555 1_555 1_555 no C2A C3A C4A 118.9(9) 1_555 1_555 1_555 no C3A C4A C5A 120.0(8) 1_555 1_555 1_555 no C4A C5A C6A 119.5(8) 1_555 1_555 1_555 no N1A C6A C5A 120.8(8) 1_555 1_555 1_555 no N4A C7A C8A 109.2(5) 1_555 1_555 1_555 no N2A C8A C7A 115.2(6) 1_555 1_555 1_555 no N2A C8A C9A 120.9(7) 1_555 1_555 1_555 no C7A C8A C9A 123.8(7) 1_555 1_555 1_555 no C8A C9A C10A 119.6(8) 1_555 1_555 1_555 no C9A C10A C11A 119.2(7) 1_555 1_555 1_555 no C10A C11A C12A 118.7(7) 1_555 1_555 1_555 no N2A C12A C11A 122.8(7) 1_555 1_555 1_555 no N4A C13A C14A 114.5(5) 1_555 1_555 1_555 no N3A C14A C13A 116.3(6) 1_555 1_555 1_555 no N3A C14A C15A 123.5(6) 1_555 1_555 1_555 no C13A C14A C15A 120.1(6) 1_555 1_555 1_555 no C14A C15A C16A 117.4(7) 1_555 1_555 1_555 no C15A C16A C17A 120.5(7) 1_555 1_555 1_555 no C16A C17A C18A 117.6(7) 1_555 1_555 1_555 no N3A C18A C17A 123.8(7) 1_555 1_555 1_555 no ClB PtB N1B 95.5(2) 1_555 1_555 1_555 no ClB PtB N2B 97.0(2) 1_555 1_555 1_555 no ClB PtB N4B 175.9(2) 1_555 1_555 1_555 no N1B PtB N2B 167.1(2) 1_555 1_555 1_555 no N1B PtB N4B 83.9(2) 1_555 1_555 1_555 no N2B PtB N4B 83.4(2) 1_555 1_555 1_555 no PtB N1B C2B 112.0(4) 1_555 1_555 1_555 no PtB N1B C6B 127.6(5) 1_555 1_555 1_555 no C2B N1B C6B 120.2(6) 1_555 1_555 1_555 no PtB N2B C8B 112.9(4) 1_555 1_555 1_555 no PtB N2B C12B 127.8(4) 1_555 1_555 1_555 no C8B N2B C12B 119.4(6) 1_555 1_555 1_555 no C14B N3B C18B 116.5(7) 1_555 1_555 1_555 no PtB N4B C1B 105.0(4) 1_555 1_555 1_555 no PtB N4B C7B 104.4(4) 1_555 1_555 1_555 no PtB N4B C13B 114.6(4) 1_555 1_555 1_555 no C1B N4B C7B 113.1(5) 1_555 1_555 1_555 no C1B N4B C13B 111.3(5) 1_555 1_555 1_555 no C7B N4B C13B 108.3(5) 1_555 1_555 1_555 no N4B C1B C2B 110.3(5) 1_555 1_555 1_555 no N1B C2B C1B 116.0(6) 1_555 1_555 1_555 no N1B C2B C3B 120.8(7) 1_555 1_555 1_555 no C1B C2B C3B 123.0(6) 1_555 1_555 1_555 no C2B C3B C4B 118.9(7) 1_555 1_555 1_555 no C3B C4B C5B 120.4(7) 1_555 1_555 1_555 no C4B C5B C6B 118.6(7) 1_555 1_555 1_555 no N1B C6B C5B 121.1(7) 1_555 1_555 1_555 no N4B C7B C8B 109.7(5) 1_555 1_555 1_555 no N2B C8B C7B 115.5(6) 1_555 1_555 1_555 no N2B C8B C9B 122.1(6) 1_555 1_555 1_555 no C7B C8B C9B 122.2(6) 1_555 1_555 1_555 no C8B C9B C10B 118.6(7) 1_555 1_555 1_555 no C9B C10B C11B 119.0(7) 1_555 1_555 1_555 no C10B C11B C12B 120.2(7) 1_555 1_555 1_555 no N2B C12B C11B 120.6(6) 1_555 1_555 1_555 no N4B C13B C14B 114.8(6) 1_555 1_555 1_555 no N3B C14B C13B 116.4(6) 1_555 1_555 1_555 no N3B C14B C15B 123.1(7) 1_555 1_555 1_555 no C13B C14B C15B 120.5(7) 1_555 1_555 1_555 no C14B C15B C16B 118.7(7) 1_555 1_555 1_555 no C15B C16B C17B 119.3(8) 1_555 1_555 1_555 no C16B C17B C18B 117.9(8) 1_555 1_555 1_555 no N3B C18B C17B 124.5(8) 1_555 1_555 1_555 no #===END #===END data_dsc86_Pd2(tbima)2 _database_code_depnum_ccdc_archive 'CCDC 298887' _audit_creation_method 'RAELSPUB and manual entry' _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_cell_refinement 'CAD4 Version 5.0, (Schagen et al, 1989)' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1996)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety '2(C24 H21 Cl N7 Pd 1+), 2(Cl 1-), C2 H6 O, 4(H2 O)' _chemical_formula_sum 'C50 H56 Cl4 N14 O5 Pd2' _chemical_formula_iupac ? _chemical_formula_weight 1287.7 _chemical_absolute_configuration ? # CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 13.458(6) _cell_length_b 16.263(7) _cell_length_c 16.263(7) _cell_angle_alpha 71.28(4) _cell_angle_beta 76.90(4) _cell_angle_gamma 81.75(3) _cell_volume 3400(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad 0.1 _exptl_crystal_density_diffrn 1.26 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308.0 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 4810 _diffrn_reflns_av_R_equivalents 0.165 _diffrn_reflns_theta_max 18 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 18 _diffrn_measured_fraction_theta_full 1.00 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 1 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 29 # REFINEMENT DATA _refine_special_details ; An exploratory data set to theta 18 degrees was collected for a crystal which proved to be unstable. Unfortunately the remaining crystals decomposed, and attempts to grow new crystals proved unsuccessful. However, the limited and poor quality data set was sufficient to allow determination of the structure and elucidation of the stereochemistry. For refinement the six benzimidazoles were modelled as identical refineable planar groups, with their thermal motions described using rigid body thermal parameters. The disordered ethanol was treated similarly. The remaining atoms were refined with single atom positional and thermal parameters. ; _reflns_number_total 4565 _reflns_number_gt 3197 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.110 _refine_ls_wR_factor_ref 0.179 _refine_ls_abs_structure_Flack ? _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3197 _refine_ls_number_parameters 220 _refine_ls_goodness_of_fit_ref 3.48 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.009 _refine_diff_density_max 1.48 _refine_diff_density_min -1.59 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy PdA 0.4040(2) 0.5498(2) 0.6648(1) 0.046(1) Uani Pd 1.0 ClA 0.2520(7) 0.6216(6) 0.6368(7) 0.097(4) Uani Cl 1.0 N1A 0.3307(11) 0.4484(10) 0.7554(8) 0.041(5) Uani N 1.0 N2A 0.2882(12) 0.3144(9) 0.8288(10) 0.054(4) Uani N 1.0 N3A 0.5410(11) 0.4811(11) 0.6882(10) 0.049(4) Uani N 1.0 N4A 0.6696(13) 0.3789(10) 0.6983(11) 0.071(7) Uani N 1.0 N5A 0.5210(14) 0.3440(10) 0.4117(11) 0.066(5) Uani N 1.0 N6A 0.4070(14) 0.2601(13) 0.5084(10) 0.084(7) Uani N 1.0 N7A 0.4308(18) 0.3901(16) 0.6104(15) 0.058(5) Uani N 1.0 C1A 0.3523(23) 0.3374(20) 0.6751(19) 0.059(5) Uani C 1.0 C2A 0.3312(12) 0.3678(12) 0.7510(9) 0.047(4) Uani C 1.0 C3A 0.2851(9) 0.4481(10) 0.8402(8) 0.045(4) Uani C 1.0 C4A 0.2682(13) 0.5186(11) 0.8746(12) 0.055(4) Uani C 1.0 C5A 0.2203(15) 0.4917(15) 0.9625(12) 0.071(7) Uani C 1.0 C6A 0.1946(14) 0.4076(16) 1.0069(11) 0.076(7) Uani C 1.0 C7A 0.2131(13) 0.3424(13) 0.9696(10) 0.068(4) Uani C 1.0 C8A 0.2590(9) 0.3640(10) 0.8852(10) 0.053(4) Uani C 1.0 C9A 0.5453(24) 0.3707(20) 0.6134(19) 0.063(6) Uani C 1.0 C10A 0.5807(14) 0.4087(11) 0.6680(10) 0.056(5) Uani C 1.0 C11A 0.6071(11) 0.4998(10) 0.7341(8) 0.060(4) Uani C 1.0 C12A 0.5961(15) 0.5701(12) 0.7683(13) 0.072(6) Uani C 1.0 C13A 0.6787(18) 0.5660(15) 0.8101(13) 0.098(9) Uani C 1.0 C14A 0.7581(17) 0.5014(18) 0.8155(13) 0.111(9) Uani C 1.0 C15A 0.7640(13) 0.4353(15) 0.7809(13) 0.099(9) Uani C 1.0 C16A 0.6869(12) 0.4354(11) 0.7399(9) 0.074(7) Uani C 1.0 C17A 0.4123(25) 0.4072(20) 0.5238(19) 0.066(7) Uani C 1.0 C18A 0.4474(15) 0.3395(11) 0.4807(11) 0.064(5) Uani C 1.0 C19A 0.5293(13) 0.2636(10) 0.3932(9) 0.079(5) Uani C 1.0 C20A 0.5967(17) 0.2385(15) 0.3261(12) 0.099(9) Uani C 1.0 C21A 0.5813(22) 0.1523(16) 0.3293(15) 0.127(8) Uani C 1.0 C22A 0.5095(24) 0.1013(13) 0.3904(17) 0.144(7) Uani C 1.0 C23A 0.4467(20) 0.1296(12) 0.4535(15) 0.130(7) Uani C 1.0 C24A 0.4576(14) 0.2120(11) 0.4541(10) 0.093(6) Uani C 1.0 PdB 0.1273(2) 0.8353(1) -0.0280(2) 0.047(1) Uani Pd 1.0 ClB 0.2274(8) 0.8897(7) -0.1590(6) 0.096(3) Uani Cl 1.0 N1B 0.2507(10) 0.8136(10) 0.0249(10) 0.050(4) Uani N 1.0 N2B 0.3561(13) 0.8066(10) 0.1108(11) 0.060(5) Uani N 1.0 N3B 0.0442(11) 0.7863(9) 0.0883(9) 0.046(4) Uani N 1.0 N4B -0.0270(12) 0.7666(11) 0.2242(10) 0.062(4) Uani N 1.0 N5B -0.0062(11) 1.1552(10) 0.0839(9) 0.044(6) Uani N 1.0 N6B 0.1407(11) 1.1184(10) 0.1294(11) 0.054(6) Uani N 1.0 N7B 0.1206(17) 0.9506(14) 0.0777(15) 0.049(4) Uani N 1.0 C1B 0.2159(22) 0.9280(18) 0.1001(19) 0.053(4) Uani C 1.0 C2B 0.2710(13) 0.8496(9) 0.0798(11) 0.051(4) Uani C 1.0 C3B 0.3261(10) 0.7436(8) 0.0196(9) 0.060(4) Uani C 1.0 C4B 0.3354(14) 0.6869(12) -0.0304(12) 0.071(7) Uani C 1.0 C5B 0.4216(16) 0.6250(12) -0.0179(15) 0.089(9) Uani C 1.0 C6B 0.4863(14) 0.6221(12) 0.0362(16) 0.093(9) Uani C 1.0 C7B 0.4728(13) 0.6790(12) 0.0827(14) 0.081(8) Uani C 1.0 C8B 0.3913(11) 0.7402(10) 0.0736(10) 0.065(5) Uani C 1.0 C9B 0.0319(22) 0.9146(19) 0.1468(19) 0.053(4) Uani C 1.0 C10B 0.0191(12) 0.8240(9) 0.1504(12) 0.050(4) Uani C 1.0 C11B 0.0130(9) 0.6998(9) 0.1231(10) 0.054(4) Uani C 1.0 C12B 0.0238(14) 0.6355(12) 0.0812(12) 0.061(6) Uani C 1.0 C13B -0.0173(15) 0.5568(11) 0.1382(16) 0.077(9) Uani C 1.0 C14B -0.0614(15) 0.5463(12) 0.2229(16) 0.086(8) Uani C 1.0 C15B -0.0693(14) 0.6112(13) 0.2593(12) 0.080(6) Uani C 1.0 C16B -0.0313(10) 0.6886(11) 0.2079(10) 0.064(4) Uani C 1.0 C17B 0.1040(19) 1.0418(19) 0.0321(17) 0.045(9) Uani C 1.0 C18B 0.0803(13) 1.1034(9) 0.0809(10) 0.043(6) Uani C 1.0 C19B -0.0023(11) 1.2067(8) 0.1370(8) 0.055(6) Uani C 1.0 C20B -0.0767(13) 1.2706(11) 0.1588(13) 0.073(9) Uani C 1.0 C21B -0.0443(18) 1.3078(12) 0.2139(13) 0.095(9) Uani C 1.0 C22B 0.0479(20) 1.2836(14) 0.2414(13) 0.099(9) Uani C 1.0 C23B 0.1164(16) 1.2212(13) 0.2178(12) 0.084(9) Uani C 1.0 C24B 0.0898(12) 1.1829(9) 0.1650(9) 0.061(6) Uani C 1.0 Cl1 0.3105(21) 0.1249(10) 0.8785(23) 0.462(9) Uani Cl 1.0 Cl2 0.8068(16) 0.2316(14) 0.6715(15) 0.261(9) Uani Cl 1.0 OW1 0.5324(20) 0.1620(16) 0.7811(17) 0.114(9) Uani O 1.0 OW2 0.2287(34) 0.1959(28) 0.6325(29) 0.228(9) Uani O 1.0 OW3 0.1632(50) 0.4140(42) 0.4612(42) 0.403(9) Uani O 1.0 OW4 0.0367(47) 0.2011(37) 0.6135(38) 0.363(9) Uani O 1.0 O1Et 0.3030(28) 0.0573(23) 0.1940(23) 0.056(8) Uani O 0.38 C1Et 0.4058(30) 0.0788(32) 0.1721(29) 0.056(8) Uani C 0.38 C2Et 0.4206(42) 0.1479(39) 0.0898(33) 0.056(8) Uani C 0.38 O1Et' 0.3365(26) 0.0597(22) 0.1446(23) 0.056(8) Uani O 0.39 C1Et' 0.4140(32) 0.1179(29) 0.1039(27) 0.056(8) Uani C 0.39 C2Et' 0.3953(45) 0.1900(29) 0.1417(39) 0.056(8) Uani C 0.39 O1Et'' 0.3353(43) 0.1162(39) 0.1372(36) 0.056(8) Uani O 0.23 C1Et'' 0.4287(51) 0.0919(53) 0.1665(42) 0.056(8) Uani C 0.23 C2Et'' 0.5080(48) 0.0701(67) 0.0989(61) 0.056(8) Uani C 0.23 HN2A 0.2793 0.2510 0.8426 0.067 Uani H 1.0 HN4A 0.7142 0.3258 0.6918 0.086 Uani H 1.0 HN6A 0.3510 0.2402 0.5588 0.118 Uani H 1.0 H1C1A 0.3780 0.2746 0.6905 0.070 Uani H 1.0 H2C1A 0.2882 0.3448 0.6521 0.067 Uani H 1.0 HC4A 0.2872 0.5792 0.8418 0.060 Uani H 1.0 HC5A 0.2045 0.5363 0.9938 0.087 Uani H 1.0 HC6A 0.1612 0.3940 1.0684 0.095 Uani H 1.0 HC7A 0.1942 0.2818 1.0023 0.081 Uani H 1.0 H1C9A 0.5850 0.3936 0.5542 0.072 Uani H 1.0 H2C9A 0.5595 0.3061 0.6343 0.073 Uani H 1.0 HC12A 0.5382 0.6164 0.7639 0.071 Uani H 1.0 HC13A 0.6792 0.6125 0.8369 0.117 Uani H 1.0 HC14A 0.8131 0.5032 0.8458 0.139 Uani H 1.0 HC15A 0.8218 0.3890 0.7852 0.109 Uani H 1.0 H1C17A 0.4468 0.4609 0.4872 0.069 Uani H 1.0 H2C17A 0.3367 0.4185 0.5269 0.088 Uani H 1.0 HC20A 0.6482 0.2761 0.2824 0.108 Uani H 1.0 HC21A 0.6249 0.1274 0.2848 0.150 Uani H 1.0 HC22A 0.5035 0.0415 0.3882 0.181 Uani H 1.0 HC23A 0.3951 0.0921 0.4974 0.160 Uani H 1.0 HN2B 0.3875 0.8206 0.1528 0.066 Uani H 1.0 HN4B -0.0531 0.7787 0.2801 0.073 Uani H 1.0 HN6B 0.2094 1.0882 0.1379 0.080 Uani H 1.0 H1C1B 0.2065 0.9173 0.1630 0.058 Uani H 1.0 H2C1B 0.2591 0.9781 0.0695 0.058 Uani H 1.0 HC4B 0.2881 0.6898 -0.0692 0.072 Uani H 1.0 HC5B 0.4360 0.5812 -0.0501 0.105 Uani H 1.0 HC6B 0.5449 0.5766 0.0414 0.110 Uani H 1.0 HC7B 0.5200 0.6762 0.1216 0.088 Uani H 1.0 H1C9B -0.0320 0.9520 0.1348 0.057 Uani H 1.0 H2C9B 0.0448 0.9145 0.2028 0.062 Uani H 1.0 HC12B 0.0558 0.6440 0.0199 0.062 Uani H 1.0 HC13B -0.0140 0.5065 0.1156 0.088 Uani H 1.0 HC14B -0.0884 0.4891 0.2587 0.103 Uani H 1.0 HC15B -0.1013 0.6028 0.3206 0.041 Uani H 1.0 H1C17B 0.0458 1.0476 0.0024 0.043 Uani H 1.0 H2C17B 0.1676 1.0590 -0.0112 0.057 Uani H 1.0 HC20B -0.1431 1.2875 0.1385 0.080 Uani H 1.0 HC21B -0.0909 1.3540 0.2336 0.117 Uani H 1.0 HC22B 0.0650 1.3128 0.2799 0.123 Uani H 1.0 HC23B 0.1828 1.2043 0.2382 0.097 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PdA 0.040(2) 0.048(2) 0.043(2) 0.008(1) -0.007(1) -0.012(1) Pd ClA 0.043(6) 0.093(8) 0.120(8) 0.024(5) -0.024(6) 0.008(6) Cl N1A 0.041(5) 0.047(7) 0.034(6) 0.012(5) -0.014(4) -0.013(5) N N2A 0.055(7) 0.050(7) 0.051(6) 0.005(5) -0.009(5) -0.011(5) N N3A 0.042(5) 0.058(7) 0.044(5) 0.009(5) -0.011(4) -0.016(4) N N4A 0.043(5) 0.081(9) 0.078(9) 0.021(6) -0.013(5) -0.022(8) N N5A 0.090(9) 0.049(9) 0.047(9) -0.010(9) 0.023(8) -0.022(9) N N6A 0.116(9) 0.076(9) 0.056(9) -0.042(9) 0.026(8) -0.030(9) N N7A 0.061(6) 0.074(8) 0.047(6) 0.005(6) -0.008(5) -0.032(6) N C1A 0.061(6) 0.066(8) 0.057(7) 0.002(5) -0.010(6) -0.033(6) C C2A 0.047(5) 0.049(7) 0.043(6) 0.009(5) -0.012(4) -0.017(5) C C3A 0.045(5) 0.054(6) 0.035(6) 0.010(4) -0.011(4) -0.014(5) C C4A 0.056(5) 0.067(7) 0.045(6) 0.008(5) -0.006(4) -0.027(5) C C5A 0.072(7) 0.096(9) 0.047(6) 0.002(9) 0.001(5) -0.036(7) C C6A 0.077(8) 0.104(9) 0.040(5) -0.002(9) 0.002(5) -0.022(5) C C7A 0.069(8) 0.080(9) 0.041(5) 0.000(8) -0.003(5) -0.006(6) C C8A 0.053(6) 0.058(6) 0.039(5) 0.006(5) -0.009(4) -0.009(5) C C9A 0.058(6) 0.071(8) 0.059(7) 0.012(6) -0.001(5) -0.033(7) C C10A 0.044(5) 0.063(7) 0.054(6) 0.015(5) -0.008(4) -0.021(5) C C11A 0.044(5) 0.079(8) 0.060(6) 0.004(5) -0.017(4) -0.023(5) C C12A 0.058(6) 0.094(9) 0.074(9) -0.010(6) -0.017(6) -0.037(8) C C13A 0.070(7) 0.146(9) 0.101(9) -0.023(9) -0.029(9) -0.054(9) C C14A 0.062(6) 0.174(9) 0.113(9) -0.013(8) -0.041(9) -0.048(9) C C15A 0.048(5) 0.145(9) 0.106(9) 0.008(6) -0.036(6) -0.031(9) C C16A 0.042(5) 0.098(9) 0.078(9) 0.012(5) -0.022(5) -0.023(7) C C17A 0.072(9) 0.060(9) 0.056(9) 0.007(9) 0.013(9) -0.028(9) C C18A 0.081(9) 0.053(9) 0.050(9) -0.011(9) 0.021(8) -0.023(8) C C19A 0.118(9) 0.058(9) 0.057(9) -0.012(8) 0.020(8) -0.032(8) C C20A 0.138(9) 0.089(9) 0.072(9) -0.003(9) 0.017(9) -0.056(9) C C21A 0.210(9) 0.089(9) 0.093(9) 0.004(9) -0.005(9) -0.068(9) C C22A 0.280(9) 0.072(9) 0.092(9) -0.032(9) -0.014(9) -0.050(9) C C23A 0.249(9) 0.074(9) 0.075(9) -0.065(9) 0.004(9) -0.035(9) C C24A 0.154(9) 0.063(9) 0.060(9) -0.038(9) 0.017(9) -0.029(9) C PdB 0.039(2) 0.040(2) 0.062(2) 0.013(1) -0.012(1) -0.020(1) Pd ClB 0.080(7) 0.114(8) 0.075(7) -0.017(6) 0.000(6) -0.010(6) Cl N1B 0.032(5) 0.046(5) 0.069(6) 0.015(4) -0.008(5) -0.023(4) N N2B 0.040(6) 0.051(8) 0.088(9) 0.014(4) -0.022(7) -0.021(6) N N3B 0.034(5) 0.041(6) 0.060(7) 0.012(4) -0.007(5) -0.018(5) N N4B 0.047(6) 0.070(7) 0.059(7) 0.004(5) -0.004(5) -0.016(5) N N5B 0.025(8) 0.052(8) 0.056(9) 0.016(6) -0.003(7) -0.032(7) N N6B 0.038(8) 0.053(8) 0.076(9) 0.012(6) -0.020(8) -0.026(6) N N7B 0.039(6) 0.044(6) 0.068(7) 0.014(4) -0.012(5) -0.026(5) N C1B 0.042(6) 0.046(6) 0.073(8) 0.012(4) -0.016(6) -0.025(6) C C2B 0.036(5) 0.045(6) 0.072(7) 0.013(4) -0.014(5) -0.021(5) C C3B 0.035(5) 0.054(6) 0.090(8) 0.020(4) -0.012(5) -0.032(5) C C4B 0.042(6) 0.068(7) 0.109(9) 0.028(6) -0.012(5) -0.050(7) C C5B 0.049(7) 0.079(9) 0.149(9) 0.037(8) -0.021(7) -0.064(9) C C6B 0.046(6) 0.075(9) 0.163(9) 0.036(7) -0.030(7) -0.055(9) C C7B 0.042(5) 0.064(9) 0.137(9) 0.026(6) -0.031(7) -0.036(9) C C8B 0.037(5) 0.054(7) 0.103(9) 0.019(4) -0.021(6) -0.028(6) C C9B 0.042(6) 0.056(6) 0.064(7) 0.015(5) -0.007(5) -0.031(5) C C10B 0.038(5) 0.052(6) 0.057(7) 0.011(4) -0.005(5) -0.021(5) C C11B 0.041(5) 0.043(6) 0.072(7) 0.008(4) -0.013(4) -0.014(5) C C12B 0.049(6) 0.040(6) 0.095(9) 0.011(4) -0.024(6) -0.020(5) C C13B 0.063(9) 0.043(6) 0.122(9) 0.003(5) -0.038(9) -0.010(5) C C14B 0.069(9) 0.057(6) 0.116(9) -0.010(7) -0.034(9) 0.008(7) C C15B 0.063(8) 0.072(7) 0.087(9) -0.011(7) -0.018(8) 0.007(7) C C16B 0.049(6) 0.060(6) 0.070(7) 0.000(5) -0.010(5) -0.006(5) C C17B 0.023(9) 0.057(9) 0.047(9) 0.011(8) 0.015(9) -0.028(8) C C18B 0.023(9) 0.052(8) 0.053(9) 0.014(6) -0.001(7) -0.027(6) C C19B 0.044(9) 0.055(8) 0.076(9) 0.014(6) -0.008(7) -0.042(6) C C20B 0.058(9) 0.060(8) 0.113(9) 0.013(7) 0.000(9) -0.060(8) C C21B 0.104(9) 0.073(9) 0.129(9) 0.001(9) -0.004(9) -0.076(9) C C22B 0.133(9) 0.078(9) 0.115(9) -0.010(9) -0.030(9) -0.064(9) C C23B 0.106(9) 0.068(9) 0.101(9) -0.005(8) -0.045(9) -0.041(9) C C24B 0.060(9) 0.057(8) 0.079(9) 0.008(6) -0.024(7) -0.036(7) C Cl1 0.384(9) 0.082(9) 0.674(9) -0.059(9) 0.333(9) -0.058(9) Cl Cl2 0.213(9) 0.271(9) 0.310(9) 0.093(9) -0.098(9) -0.117(9) Cl OW1 0.118(9) 0.097(9) 0.125(9) -0.021(9) -0.072(9) 0.007(9) O OW2 0.228(9) 0.228(9) 0.228(9) -0.018(1) -0.044(4) -0.068(6) O OW3 0.403(9) 0.403(9) 0.403(9) -0.031(3) -0.078(8) -0.121(9) O OW4 0.363(9) 0.363(9) 0.363(9) -0.028(3) -0.070(7) -0.108(9) O O1Et 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) O C1Et 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) C C2Et 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) C O1Et' 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) O C1Et' 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) C C2Et' 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) C O1Et'' 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) O C1Et'' 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) C C2Et'' 0.056(8) 0.056(8) 0.056(8) -0.0043(6) -0.011(2) -0.017(3) C # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PdA ClA 2.274(8) 1_555 1_555 no PdA N1A 2.049(14) 1_555 1_555 no PdA N3A 2.063(14) 1_555 1_555 no PdA N5A 2.036(15) 1_555 2_666 no N1A C2A 1.336(11) 1_555 1_555 no N1A C3A 1.424(11) 1_555 1_555 no N2A C2A 1.371(12) 1_555 1_555 no N2A C8A 1.393(14) 1_555 1_555 no N3A C10A 1.336(11) 1_555 1_555 no N3A C11A 1.424(11) 1_555 1_555 no N4A C10A 1.371(12) 1_555 1_555 no N4A C16A 1.393(14) 1_555 1_555 no N5A PdA 2.036(15) 1_555 2_666 no N5A C18A 1.336(11) 1_555 1_555 no N5A C19A 1.424(11) 1_555 1_555 no N6A C18A 1.371(12) 1_555 1_555 no N6A C24A 1.393(14) 1_555 1_555 no N7A C1A 1.477(35) 1_555 1_555 no N7A C9A 1.537(37) 1_555 1_555 no N7A C17A 1.471(36) 1_555 1_555 no C1A C2A 1.473(30) 1_555 1_555 no C3A C4A 1.413(14) 1_555 1_555 no C3A C8A 1.385(16) 1_555 1_555 no C4A C5A 1.429(16) 1_555 1_555 no C5A C6A 1.384(19) 1_555 1_555 no C6A C7A 1.364(19) 1_555 1_555 no C7A C8A 1.372(17) 1_555 1_555 no C9A C10A 1.450(33) 1_555 1_555 no C11A C12A 1.413(14) 1_555 1_555 no C11A C16A 1.385(16) 1_555 1_555 no C12A C13A 1.429(16) 1_555 1_555 no C13A C14A 1.384(19) 1_555 1_555 no C14A C15A 1.364(19) 1_555 1_555 no C15A C16A 1.372(17) 1_555 1_555 no C17A C18A 1.474(31) 1_555 1_555 no C19A C20A 1.413(14) 1_555 1_555 no C19A C24A 1.385(16) 1_555 1_555 no C20A C21A 1.429(16) 1_555 1_555 no C21A C22A 1.384(19) 1_555 1_555 no C22A C23A 1.364(19) 1_555 1_555 no C23A C24A 1.372(17) 1_555 1_555 no PdB ClB 2.287(9) 1_555 1_555 no PdB N1B 1.995(15) 1_555 1_555 no PdB N3B 1.999(14) 1_555 1_555 no PdB N5B 2.026(14) 1_555 2_575 no N1B C2B 1.336(11) 1_555 1_555 no N1B C3B 1.424(11) 1_555 1_555 no N2B C2B 1.371(12) 1_555 1_555 no N2B C8B 1.393(14) 1_555 1_555 no N3B C10B 1.336(11) 1_555 1_555 no N3B C11B 1.424(11) 1_555 1_555 no N4B C10B 1.371(12) 1_555 1_555 no N4B C16B 1.393(14) 1_555 1_555 no N5B PdB 2.026(14) 1_555 2_575 no N5B C18B 1.336(11) 1_555 1_555 no N5B C19B 1.424(11) 1_555 1_555 no N6B C18B 1.371(12) 1_555 1_555 no N6B C24B 1.393(14) 1_555 1_555 no N7B C1B 1.386(32) 1_555 1_555 no N7B C9B 1.503(35) 1_555 1_555 no N7B C17B 1.447(32) 1_555 1_555 no C1B C2B 1.480(29) 1_555 1_555 no C3B C4B 1.413(14) 1_555 1_555 no C3B C8B 1.385(16) 1_555 1_555 no C4B C5B 1.429(16) 1_555 1_555 no C5B C6B 1.384(19) 1_555 1_555 no C6B C7B 1.364(19) 1_555 1_555 no C7B C8B 1.372(17) 1_555 1_555 no C9B C10B 1.488(31) 1_555 1_555 no C11B C12B 1.413(14) 1_555 1_555 no C11B C16B 1.385(16) 1_555 1_555 no C12B C13B 1.429(16) 1_555 1_555 no C13B C14B 1.384(19) 1_555 1_555 no C14B C15B 1.364(19) 1_555 1_555 no C15B C16B 1.372(17) 1_555 1_555 no C17B C18B 1.451(28) 1_555 1_555 no C19B C20B 1.413(14) 1_555 1_555 no C19B C24B 1.385(16) 1_555 1_555 no C20B C21B 1.429(16) 1_555 1_555 no C21B C22B 1.384(19) 1_555 1_555 no C22B C23B 1.364(19) 1_555 1_555 no C23B C24B 1.372(17) 1_555 1_555 no O1Et C1Et 1.413(21) 1_555 1_555 no C1Et C2Et 1.473(22) 1_555 1_555 no O1Et' C1Et' 1.413(21) 1_555 1_555 no C1Et' C2Et' 1.473(22) 1_555 1_555 no O1Et'' C1Et'' 1.413(21) 1_555 1_555 no C1Et'' C2Et'' 1.473(22) 1_555 1_555 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag ClA PdA N1A 91.1(5) 1_555 1_555 1_555 no ClA PdA N3A 177.8(5) 1_555 1_555 1_555 no ClA PdA N5A 90.4(6) 1_555 1_555 2_666 no N1A PdA N3A 88.1(6) 1_555 1_555 1_555 no N1A PdA N5A 172.2(7) 1_555 1_555 2_666 no N3A PdA N5A 90.7(7) 1_555 1_555 2_666 no PdA N1A C2A 126.8(9) 1_555 1_555 1_555 no PdA N1A C3A 124.7(9) 1_555 1_555 1_555 no C2A N1A C3A 107.7(8) 1_555 1_555 1_555 no C2A N2A C8A 108.1(9) 1_555 1_555 1_555 no PdA N3A C10A 126.7(9) 1_555 1_555 1_555 no PdA N3A C11A 125.5(10) 1_555 1_555 1_555 no C10A N3A C11A 107.7(8) 1_555 1_555 1_555 no C10A N4A C16A 108.1(9) 1_555 1_555 1_555 no PdA N5A C18A 127.4(10) 2_666 1_555 1_555 no PdA N5A C19A 124.4(10) 2_666 1_555 1_555 no C18A N5A C19A 107.7(8) 1_555 1_555 1_555 no C18A N6A C24A 108.1(9) 1_555 1_555 1_555 no C1A N7A C9A 121.9(23) 1_555 1_555 1_555 no C1A N7A C17A 111.6(23) 1_555 1_555 1_555 no C9A N7A C17A 111.7(22) 1_555 1_555 1_555 no N7A C1A C2A 108.3(22) 1_555 1_555 1_555 no N1A C2A N2A 109.9(7) 1_555 1_555 1_555 no N1A C2A C1A 128.9(17) 1_555 1_555 1_555 no N2A C2A C1A 120.1(17) 1_555 1_555 1_555 no N1A C3A C4A 127.9(11) 1_555 1_555 1_555 no N1A C3A C8A 107.2(9) 1_555 1_555 1_555 no C4A C3A C8A 124.9(9) 1_555 1_555 1_555 no C3A C4A C5A 110.9(11) 1_555 1_555 1_555 no C4A C5A C6A 123.7(13) 1_555 1_555 1_555 no C5A C6A C7A 122.3(13) 1_555 1_555 1_555 no C6A C7A C8A 116.8(13) 1_555 1_555 1_555 no N2A C8A C3A 107.2(10) 1_555 1_555 1_555 no N2A C8A C7A 131.6(13) 1_555 1_555 1_555 no C3A C8A C7A 121.3(12) 1_555 1_555 1_555 no N7A C9A C10A 115.2(22) 1_555 1_555 1_555 no N3A C10A N4A 109.9(7) 1_555 1_555 1_555 no N3A C10A C9A 126.8(18) 1_555 1_555 1_555 no N4A C10A C9A 122.9(18) 1_555 1_555 1_555 no N3A C11A C12A 127.9(11) 1_555 1_555 1_555 no N3A C11A C16A 107.2(9) 1_555 1_555 1_555 no C12A C11A C16A 124.9(9) 1_555 1_555 1_555 no C11A C12A C13A 110.9(11) 1_555 1_555 1_555 no C12A C13A C14A 123.7(13) 1_555 1_555 1_555 no C13A C14A C15A 122.3(13) 1_555 1_555 1_555 no C14A C15A C16A 116.8(13) 1_555 1_555 1_555 no N4A C16A C11A 107.2(10) 1_555 1_555 1_555 no N4A C16A C15A 131.6(12) 1_555 1_555 1_555 no C11A C16A C15A 121.3(12) 1_555 1_555 1_555 no N7A C17A C18A 118.5(24) 1_555 1_555 1_555 no N5A C18A N6A 109.9(7) 1_555 1_555 1_555 no N5A C18A C17A 127.2(18) 1_555 1_555 1_555 no N6A C18A C17A 122.9(18) 1_555 1_555 1_555 no N5A C19A C20A 127.9(11) 1_555 1_555 1_555 no N5A C19A C24A 107.2(9) 1_555 1_555 1_555 no C20A C19A C24A 124.9(9) 1_555 1_555 1_555 no C19A C20A C21A 110.9(11) 1_555 1_555 1_555 no C20A C21A C22A 123.7(13) 1_555 1_555 1_555 no C21A C22A C23A 122.3(13) 1_555 1_555 1_555 no C22A C23A C24A 116.8(13) 1_555 1_555 1_555 no N6A C24A C19A 107.2(10) 1_555 1_555 1_555 no N6A C24A C23A 131.6(13) 1_555 1_555 1_555 no C19A C24A C23A 121.3(12) 1_555 1_555 1_555 no ClB PdB N1B 89.5(5) 1_555 1_555 1_555 no ClB PdB N3B 178.0(5) 1_555 1_555 1_555 no ClB PdB N5B 89.9(5) 1_555 1_555 2_575 no N1B PdB N3B 88.5(6) 1_555 1_555 1_555 no N1B PdB N5B 173.9(7) 1_555 1_555 2_575 no N3B PdB N5B 91.9(6) 1_555 1_555 2_575 no PdB N1B C2B 128.8(9) 1_555 1_555 1_555 no PdB N1B C3B 122.9(10) 1_555 1_555 1_555 no C2B N1B C3B 107.7(8) 1_555 1_555 1_555 no C2B N2B C8B 108.1(9) 1_555 1_555 1_555 no PdB N3B C10B 126.5(9) 1_555 1_555 1_555 no PdB N3B C11B 125.3(10) 1_555 1_555 1_555 no C10B N3B C11B 107.7(8) 1_555 1_555 1_555 no C10B N4B C16B 108.1(9) 1_555 1_555 1_555 no PdB N5B C18B 129.8(9) 2_575 1_555 1_555 no PdB N5B C19B 122.5(9) 2_575 1_555 1_555 no C18B N5B C19B 107.7(8) 1_555 1_555 1_555 no C18B N6B C24B 108.1(9) 1_555 1_555 1_555 no C1B N7B C9B 115.3(23) 1_555 1_555 1_555 no C1B N7B C17B 113.8(22) 1_555 1_555 1_555 no C9B N7B C17B 114.1(20) 1_555 1_555 1_555 no N7B C1B C2B 115.0(23) 1_555 1_555 1_555 no N1B C2B N2B 109.9(7) 1_555 1_555 1_555 no N1B C2B C1B 125.9(17) 1_555 1_555 1_555 no N2B C2B C1B 124.1(16) 1_555 1_555 1_555 no N1B C3B C4B 127.9(11) 1_555 1_555 1_555 no N1B C3B C8B 107.2(9) 1_555 1_555 1_555 no C4B C3B C8B 124.9(9) 1_555 1_555 1_555 no C3B C4B C5B 110.9(10) 1_555 1_555 1_555 no C4B C5B C6B 123.7(13) 1_555 1_555 1_555 no C5B C6B C7B 122.3(13) 1_555 1_555 1_555 no C6B C7B C8B 116.8(14) 1_555 1_555 1_555 no N2B C8B C3B 107.2(10) 1_555 1_555 1_555 no N2B C8B C7B 131.6(12) 1_555 1_555 1_555 no C3B C8B C7B 121.3(12) 1_555 1_555 1_555 no N7B C9B C10B 110.4(21) 1_555 1_555 1_555 no N3B C10B N4B 109.9(7) 1_555 1_555 1_555 no N3B C10B C9B 129.2(17) 1_555 1_555 1_555 no N4B C10B C9B 120.8(17) 1_555 1_555 1_555 no N3B C11B C12B 127.9(11) 1_555 1_555 1_555 no N3B C11B C16B 107.2(9) 1_555 1_555 1_555 no C12B C11B C16B 124.9(9) 1_555 1_555 1_555 no C11B C12B C13B 110.9(11) 1_555 1_555 1_555 no C12B C13B C14B 123.7(13) 1_555 1_555 1_555 no C13B C14B C15B 122.3(13) 1_555 1_555 1_555 no C14B C15B C16B 116.8(13) 1_555 1_555 1_555 no N4B C16B C11B 107.2(10) 1_555 1_555 1_555 no N4B C16B C15B 131.6(13) 1_555 1_555 1_555 no C11B C16B C15B 121.3(12) 1_555 1_555 1_555 no N7B C17B C18B 117.8(22) 1_555 1_555 1_555 no N5B C18B N6B 109.9(7) 1_555 1_555 1_555 no N5B C18B C17B 123.5(16) 1_555 1_555 1_555 no N6B C18B C17B 126.6(16) 1_555 1_555 1_555 no N5B C19B C20B 127.9(11) 1_555 1_555 1_555 no N5B C19B C24B 107.2(9) 1_555 1_555 1_555 no C20B C19B C24B 124.9(9) 1_555 1_555 1_555 no C19B C20B C21B 110.9(10) 1_555 1_555 1_555 no C20B C21B C22B 123.7(13) 1_555 1_555 1_555 no C21B C22B C23B 122.3(13) 1_555 1_555 1_555 no C22B C23B C24B 116.8(13) 1_555 1_555 1_555 no N6B C24B C19B 107.2(10) 1_555 1_555 1_555 no N6B C24B C23B 131.6(12) 1_555 1_555 1_555 no C19B C24B C23B 121.3(12) 1_555 1_555 1_555 no O1Et C1Et C2Et 108.9(9) 1_555 1_555 1_555 no O1Et' C1Et' C2Et' 108.9(9) 1_555 1_555 1_555 no O1Et'' C1Et'' C2Et'' 108.9(9) 1_555 1_555 1_555 no