# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- 6a.cif' #============================================================================== _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Oliver Reiser' _publ_contact_author_email Oliver.Reiser@chemie.uni-regensburg.de _publ_section_title ; Palladium(II)- and Platinum(II)phenyl-2,6-bis(oxazole) pincer complexes: Syntheses, crystal structures, and photophysical properties ; # 0. AUDIT DETAILS _audit_creation_date 'Feb 14 10:27:15 2005' _audit_creation_method 'PLATON option' _audit_update_record ; ? 2011-04-07 # Formatted by publCIF ; _publ_section_exptl_refinement ; The data were collected at 173 K using an Oxford Cryosystems Cooler (Cosier & Glazer, 1986). The structure was solved by direct methods (SIR97) and refined by full-matrix anisotropic least squares (SHELXL97). The H-atoms were calculated geometrically and a riding model was used during refinement process. ; # Insert blank lines between references _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst.26, 343--350. Cosier, J. & Glazer, A. M. (1986). J. Appl. Cryst.19, 105--107. Flack, H. D. (1983). Acta Cryst. A39, 876--881. L. J. Farrugia, J. Appl. Cryst (1997). 30, 565. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sheldrick, G.M. SHELXS97. Program for Crystal Structure solution. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194--201. Spek, A. L. (1990). Acta Cryst. A46 C-34. STOE (1998). IPDSsoftware, version 2.89, STOE & CIE GmbH, Darmstadt, Germany. Wilson, A. J. C. (1992). International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_acknowledgements ; (type here to add acknowledgements) ; _publ_section_figure_captions ; View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. ; loop_ _publ_author_name 'Gang Xu' 'Qunli Luo' S.Eibauer A.Rausch S.Stempfhuber M.Zabel H.Yersin O.Reiser #=============================================================================== data_e027 _database_code_depnum_ccdc_archive 'CCDC 630898' #TrackingRef '- 6a.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 Br N2 O4 Pd' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C16 H15 Br N2 O4 Pd' _chemical_formula_sum 'C16 H15 Br N2 O4 Pd' _chemical_formula_iupac ? _chemical_formula_weight 485.62 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 7.5601(8) _cell_length_b 9.3101(6) _cell_length_c 24.686(3) _cell_angle_alpha 90 _cell_angle_beta 90.828(12) _cell_angle_gamma 90 _cell_volume 1737.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 25.87 _cell_special_details ; Cell parameters were determined by indexing 8000 reflections with I/sigma limit 6.0. ; _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 3.390 _exptl_crystal_density_meas_temp ? # Permitted for : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type analytical # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)' _exptl_absorpt_correction_T_min 0.4459 _exptl_absorpt_correction_T_max 0.7642 loop_ _exptl_crystal_face_index_h_ _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 2 0.0280 2 1 -1 0.1114 0 -1 3 0.1823 1 0 -2 0.0580 -2 0 -1 0.0315 -2 1 2 0.1452 -2 -1 -2 0.0679 1 1 9 0.1192 1 -1 -2 0.1332 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Data were collected applying an imaging plate system (STOE) with the following measurement parameters: Detector distance [mm] 70 Phi movement mode Oscillation Phi incr. [degrees] 0.8 Number of exposures 368 Irradiation / exposure [min] 1.00 For a detailed description of the method see: Sheldrick, G.M., Paulus, E. Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS diffractometer' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 19590 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.87 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 3360 # number of observed reflections (> n sig(I)) _reflns_number_gt 2905 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'STOE (1998)' _computing_cell_refinement 'STOE (1998)' _computing_data_reduction 'STOE (1998)' _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2, conventional R-factors R are based on F, with F set to zero for negative F^2. The observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3360 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0560 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.680 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.089 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd1 Pd Uani 0.84700(2) 0.88931(2) 0.63640(1) 1.000 0.0192(1) . . Br1 Br Uani 0.94583(4) 0.90258(3) 0.73389(1) 1.000 0.0420(1) . . O1 O Uani 0.9117(2) 1.24553(17) 0.54083(6) 1.000 0.0244(5) . . O2 O Uani 1.0448(2) 1.44383(18) 0.57572(7) 1.000 0.0289(5) . . O3 O Uani 0.61774(19) 0.51294(17) 0.58508(6) 1.000 0.0230(5) . . O4 O Uani 0.5823(2) 0.32940(18) 0.64407(6) 1.000 0.0268(5) . . N1 N Uani 0.9141(2) 1.09112(19) 0.60945(7) 1.000 0.0214(5) . . N2 N Uani 0.7485(2) 0.6830(2) 0.63412(7) 1.000 0.0220(5) . . C1 C Uani 0.9941(3) 1.2180(2) 0.62779(9) 1.000 0.0231(6) . . C2 C Uani 0.9913(3) 1.3102(2) 0.58531(9) 1.000 0.0233(6) . . C3 C Uani 0.8682(3) 1.1123(2) 0.55843(9) 1.000 0.0222(6) . . C4 C Uani 0.7836(3) 0.9980(2) 0.52737(9) 1.000 0.0223(6) . . C5 C Uani 0.7645(3) 0.8785(2) 0.56092(9) 1.000 0.0207(6) . . C6 C Uani 0.6865(3) 0.7511(2) 0.54204(9) 1.000 0.0214(6) . . C7 C Uani 0.6240(3) 0.7440(3) 0.48837(9) 1.000 0.0242(7) . . C8 C Uani 0.6437(3) 0.8637(3) 0.45505(9) 1.000 0.0264(7) . . C9 C Uani 0.7232(3) 0.9905(3) 0.47344(9) 1.000 0.0244(7) . . C10 C Uani 0.6841(3) 0.6478(2) 0.58607(9) 1.000 0.0204(6) . . C11 C Uani 0.6443(3) 0.4618(2) 0.63732(9) 1.000 0.0229(6) . . C12 C Uani 0.7251(3) 0.5642(3) 0.66802(9) 1.000 0.0236(6) . . C13 C Uani 1.1593(3) 1.5027(3) 0.61837(10) 1.000 0.0289(7) . . C14 C Uani 1.2195(3) 1.6484(3) 0.59920(12) 1.000 0.0361(8) . . C15 C Uani 0.5940(4) 0.2776(3) 0.70009(10) 1.000 0.0344(8) . . C16 C Uani 0.5070(4) 0.1329(3) 0.70192(12) 1.000 0.0382(8) . . H1 H Uiso 1.04110 1.23590 0.66300 1.000 0.0280 calc R H7 H Uiso 0.56920 0.65910 0.47490 1.000 0.0290 calc R H8 H Uiso 0.60160 0.85890 0.41860 1.000 0.0320 calc R H9 H Uiso 0.73620 1.07020 0.44980 1.000 0.0290 calc R H12 H Uiso 0.75910 0.55670 0.70510 1.000 0.0280 calc R H13A H Uiso 1.26240 1.43910 0.62480 1.000 0.0350 calc R H13B H Uiso 1.09350 1.51190 0.65260 1.000 0.0350 calc R H14A H Uiso 1.28250 1.63790 0.56500 1.000 0.0540 calc R H14B H Uiso 1.29870 1.69110 0.62650 1.000 0.0540 calc R H14C H Uiso 1.11630 1.71070 0.59360 1.000 0.0540 calc R H15A H Uiso 0.53330 0.34510 0.72460 1.000 0.0410 calc R H15B H Uiso 0.71940 0.26990 0.71190 1.000 0.0410 calc R H16A H Uiso 0.38150 0.14260 0.69220 1.000 0.0570 calc R H16B H Uiso 0.51860 0.09320 0.73860 1.000 0.0570 calc R H16C H Uiso 0.56430 0.06830 0.67620 1.000 0.0570 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0227(1) 0.0175(1) 0.0173(1) -0.0003(1) -0.0016(1) -0.0012(1) Br1 0.0642(2) 0.0370(2) 0.0242(2) 0.0012(1) -0.0171(1) -0.0061(1) O1 0.0285(8) 0.0202(8) 0.0244(8) 0.0025(7) -0.0006(6) -0.0018(6) O2 0.0339(9) 0.0206(8) 0.0320(9) 0.0033(7) -0.0032(7) -0.0041(7) O3 0.0241(8) 0.0216(8) 0.0233(8) 0.0008(7) -0.0020(6) -0.0029(6) O4 0.0306(8) 0.0217(8) 0.0281(8) 0.0031(7) -0.0016(6) -0.0051(7) N1 0.0241(9) 0.0189(10) 0.0211(9) 0.0002(8) 0.0015(7) -0.0003(7) N2 0.0235(9) 0.0202(10) 0.0224(9) 0.0002(8) -0.0007(7) -0.0015(8) C1 0.0247(10) 0.0193(11) 0.0252(11) -0.0033(9) -0.0001(9) -0.0003(9) C2 0.0235(10) 0.0205(11) 0.0260(11) -0.0018(10) 0.0006(8) 0.0000(9) C3 0.0227(10) 0.0198(11) 0.0240(11) 0.0013(9) 0.0019(8) -0.0009(9) C4 0.0221(10) 0.0228(11) 0.0220(11) 0.0003(9) 0.0009(8) 0.0012(9) C5 0.0209(10) 0.0233(11) 0.0179(10) -0.0010(9) -0.0007(8) 0.0017(8) C6 0.0211(10) 0.0218(11) 0.0212(11) -0.0016(9) 0.0016(8) 0.0001(8) C7 0.0245(11) 0.0247(12) 0.0232(11) -0.0047(9) -0.0016(9) -0.0024(9) C8 0.0274(11) 0.0321(13) 0.0195(11) -0.0020(10) -0.0026(9) 0.0014(9) C9 0.0273(11) 0.0247(12) 0.0213(11) 0.0041(9) 0.0020(9) 0.0012(9) C10 0.0194(10) 0.0188(11) 0.0230(11) -0.0012(9) 0.0003(8) -0.0004(8) C11 0.0217(10) 0.0227(12) 0.0242(11) 0.0034(9) 0.0016(8) 0.0000(9) C12 0.0260(11) 0.0221(11) 0.0227(11) 0.0016(9) 0.0012(9) -0.0005(9) C13 0.0257(11) 0.0238(12) 0.0372(13) -0.0004(11) -0.0014(10) -0.0037(9) C14 0.0287(12) 0.0242(13) 0.0554(17) 0.0005(12) 0.0029(11) -0.0024(10) C15 0.0439(14) 0.0315(14) 0.0277(13) 0.0047(11) 0.0020(11) -0.0049(11) C16 0.0442(15) 0.0313(14) 0.0394(15) 0.0109(12) 0.0084(12) -0.0035(11) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pd1 Br1 2.5125(4) . . yes Pd1 N1 2.0591(18) . . yes Pd1 N2 2.0605(18) . . yes Pd1 C5 1.959(2) . . yes O1 C2 1.383(3) . . yes O1 C3 1.356(2) . . yes O2 C2 1.331(3) . . yes O2 C13 1.460(3) . . yes O3 C10 1.352(2) . . yes O3 C11 1.387(3) . . yes O4 C11 1.330(3) . . yes O4 C15 1.466(3) . . yes N1 C1 1.399(3) . . yes N1 C3 1.316(3) . . yes N2 C10 1.317(3) . . yes N2 C12 1.400(3) . . yes C1 C2 1.355(3) . . no C3 C4 1.454(3) . . no C4 C5 1.396(3) . . no C4 C9 1.403(3) . . no C5 C6 1.401(3) . . no C6 C7 1.402(3) . . no C6 C10 1.452(3) . . no C7 C8 1.394(4) . . no C8 C9 1.398(4) . . no C11 C12 1.358(3) . . no C13 C14 1.509(4) . . no C15 C16 1.500(4) . . no C1 H1 0.9490 . . no C7 H7 0.9503 . . no C8 H8 0.9511 . . no C9 H9 0.9500 . . no C12 H12 0.9497 . . no C13 H13A 0.9898 . . no C13 H13B 0.9904 . . no C14 H14A 0.9802 . . no C14 H14B 0.9793 . . no C14 H14C 0.9804 . . no C15 H15A 0.9898 . . no C15 H15B 0.9904 . . no C16 H16A 0.9795 . . no C16 H16B 0.9808 . . no C16 H16C 0.9800 . . 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 Br1 Pd1 N1 101.15(5) . . . yes Br1 Pd1 N2 100.04(5) . . . yes Br1 Pd1 C5 178.73(7) . . . yes N1 Pd1 N2 158.81(7) . . . yes N1 Pd1 C5 79.40(7) . . . yes N2 Pd1 C5 79.41(7) . . . yes C2 O1 C3 104.40(16) . . . yes C2 O2 C13 113.66(19) . . . yes C10 O3 C11 104.68(16) . . . yes C11 O4 C15 113.98(18) . . . yes Pd1 N1 C1 140.63(14) . . . yes Pd1 N1 C3 112.52(13) . . . yes C1 N1 C3 106.85(17) . . . yes Pd1 N2 C10 112.66(14) . . . yes Pd1 N2 C12 140.26(15) . . . yes C10 N2 C12 107.07(18) . . . yes N1 C1 C2 106.41(19) . . . yes O1 C2 O2 113.32(18) . . . yes O1 C2 C1 109.91(17) . . . yes O2 C2 C1 136.8(2) . . . yes O1 C3 N1 112.44(18) . . . yes O1 C3 C4 127.38(19) . . . yes N1 C3 C4 120.17(18) . . . yes C3 C4 C5 108.60(19) . . . no C3 C4 C9 132.2(2) . . . no C5 C4 C9 119.2(2) . . . no Pd1 C5 C4 119.29(15) . . . yes Pd1 C5 C6 119.11(15) . . . yes C4 C5 C6 121.6(2) . . . no C5 C6 C7 119.3(2) . . . no C5 C6 C10 108.75(19) . . . no C7 C6 C10 132.0(2) . . . no C6 C7 C8 118.9(2) . . . no C7 C8 C9 122.2(2) . . . no C4 C9 C8 118.9(2) . . . no O3 C10 N2 112.31(18) . . . yes O3 C10 C6 127.61(19) . . . yes N2 C10 C6 120.07(18) . . . yes O3 C11 O4 112.84(18) . . . yes O3 C11 C12 109.63(18) . . . yes O4 C11 C12 137.5(2) . . . yes N2 C12 C11 106.31(19) . . . yes O2 C13 C14 106.8(2) . . . yes O4 C15 C16 107.7(2) . . . yes N1 C1 H1 126.79 . . . no C2 C1 H1 126.80 . . . no C6 C7 H7 120.61 . . . no C8 C7 H7 120.54 . . . no C7 C8 H8 118.91 . . . no C9 C8 H8 118.91 . . . no C4 C9 H9 120.59 . . . no C8 C9 H9 120.54 . . . no N2 C12 H12 126.84 . . . no C11 C12 H12 126.85 . . . no O2 C13 H13A 110.39 . . . no O2 C13 H13B 110.35 . . . no C14 C13 H13A 110.34 . . . no C14 C13 H13B 110.32 . . . no H13A C13 H13B 108.60 . . . no C13 C14 H14A 109.45 . . . no C13 C14 H14B 109.47 . . . no C13 C14 H14C 109.45 . . . no H14A C14 H14B 109.47 . . . no H14A C14 H14C 109.46 . . . no H14B C14 H14C 109.53 . . . no O4 C15 H15A 110.22 . . . no O4 C15 H15B 110.24 . . . no C16 C15 H15A 110.15 . . . no C16 C15 H15B 110.14 . . . no H15A C15 H15B 108.44 . . . no C15 C16 H16A 109.48 . . . no C15 C16 H16B 109.44 . . . no C15 C16 H16C 109.48 . . . no H16A C16 H16B 109.53 . . . no H16A C16 H16C 109.48 . . . no H16B C16 H16C 109.41 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Pd1 N1 C1 1.9(2) . . . . no N2 Pd1 N1 C1 -178.92(19) . . . . no C5 Pd1 N1 C1 -179.3(2) . . . . no Br1 Pd1 N1 C3 -177.71(13) . . . . no N2 Pd1 N1 C3 1.5(3) . . . . no C5 Pd1 N1 C3 1.13(15) . . . . no Br1 Pd1 N2 C10 179.26(14) . . . . no N1 Pd1 N2 C10 0.1(3) . . . . no C5 Pd1 N2 C10 0.42(15) . . . . no Br1 Pd1 N2 C12 0.1(2) . . . . no N1 Pd1 N2 C12 -179.1(2) . . . . no C5 Pd1 N2 C12 -178.8(2) . . . . no N2 Pd1 C5 C4 179.31(19) . . . . no N1 Pd1 C5 C6 179.63(19) . . . . no N1 Pd1 C5 C4 -0.83(17) . . . . no N2 Pd1 C5 C6 -0.24(17) . . . . no C3 O1 C2 C1 -0.2(2) . . . . no C2 O1 C3 N1 0.1(2) . . . . no C2 O1 C3 C4 -178.8(2) . . . . no C3 O1 C2 O2 179.69(18) . . . . no C13 O2 C2 C1 11.4(4) . . . . no C13 O2 C2 O1 -168.45(17) . . . . no C2 O2 C13 C14 175.44(19) . . . . no C10 O3 C11 O4 178.59(18) . . . . no C10 O3 C11 C12 -0.3(2) . . . . no C11 O3 C10 N2 0.0(2) . . . . no C11 O3 C10 C6 -178.5(2) . . . . no C15 O4 C11 C12 3.7(4) . . . . no C11 O4 C15 C16 175.7(2) . . . . no C15 O4 C11 O3 -174.72(19) . . . . no C1 N1 C3 O1 0.0(2) . . . . no Pd1 N1 C3 C4 -1.3(3) . . . . no C1 N1 C3 C4 179.0(2) . . . . no Pd1 N1 C1 C2 -179.66(16) . . . . no C3 N1 C1 C2 -0.1(2) . . . . no Pd1 N1 C3 O1 179.69(13) . . . . no C10 N2 C12 C11 -0.4(2) . . . . no C12 N2 C10 C6 178.9(2) . . . . no Pd1 N2 C10 C6 -0.6(3) . . . . no Pd1 N2 C12 C11 178.82(16) . . . . no Pd1 N2 C10 O3 -179.23(13) . . . . no C12 N2 C10 O3 0.2(2) . . . . no N1 C1 C2 O2 -179.7(2) . . . . no N1 C1 C2 O1 0.1(3) . . . . no N1 C3 C4 C9 -179.5(2) . . . . no O1 C3 C4 C9 -0.6(4) . . . . no N1 C3 C4 C5 0.7(3) . . . . no O1 C3 C4 C5 179.5(2) . . . . no C3 C4 C5 C6 179.9(2) . . . . no C9 C4 C5 Pd1 -179.50(17) . . . . no C3 C4 C9 C8 -179.2(2) . . . . no C5 C4 C9 C8 0.7(3) . . . . no C3 C4 C5 Pd1 0.4(3) . . . . no C9 C4 C5 C6 0.0(3) . . . . no C4 C5 C6 C10 -179.5(2) . . . . no C4 C5 C6 C7 -0.9(3) . . . . no Pd1 C5 C6 C10 0.0(3) . . . . no Pd1 C5 C6 C7 178.69(17) . . . . no C5 C6 C7 C8 0.9(3) . . . . no C7 C6 C10 O3 0.4(4) . . . . no C5 C6 C10 N2 0.4(3) . . . . no C5 C6 C10 O3 178.8(2) . . . . no C10 C6 C7 C8 179.2(2) . . . . no C7 C6 C10 N2 -178.1(2) . . . . no C6 C7 C8 C9 -0.2(3) . . . . no C7 C8 C9 C4 -0.6(4) . . . . no O3 C11 C12 N2 0.4(2) . . . . no O4 C11 C12 N2 -178.0(2) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd1 C14 3.726(3) . 1_545 no Pd1 C16 3.806(3) . 1_565 no Pd1 H14C 2.8441 . 1_545 no Pd1 H16C 2.8932 . 1_565 no Br1 N1 3.5431(18) . . no Br1 N2 3.5163(18) . . no Br1 H1 2.9816 . 2_746 no Br1 H12 3.0342 . 2_756 no Br1 H13B 3.0001 . 2_746 no Br1 H15B 3.1023 . 2_756 no O1 N1 2.222(2) . . no O2 C10 3.336(3) . 1_565 no O2 C11 3.412(3) . 1_565 no O3 C2 3.397(3) . 1_545 no O3 C14 3.287(3) . 1_445 no O4 C1 3.311(3) . 1_545 no O3 H14A 2.8260 . 1_445 no O3 H7 2.5874 . 3_666 no O4 H13A 2.6618 . 1_445 no O4 H8 2.7088 . 3_666 no N1 Br1 3.5431(18) . . no N1 O1 2.222(2) . . no N1 C4 2.403(3) . . no N1 C5 2.568(3) . . no N2 Br1 3.5163(18) . . no N2 C5 2.569(3) . . no N2 C6 2.400(3) . . no C1 O4 3.311(3) . 1_565 no C1 C11 3.496(3) . 1_565 no C1 C15 3.578(4) . 1_565 no C1 C8 3.524(3) . 3_776 no C2 O3 3.397(3) . 1_565 no C2 C11 3.259(3) . 1_565 no C2 C8 3.363(3) . 3_776 no C2 C7 3.489(3) . 3_776 no C3 C4 3.554(3) . 3_776 no C3 C9 3.339(3) . 3_776 no C4 C3 3.554(3) . 3_776 no C4 C4 3.558(3) . 3_776 no C4 C8 3.510(3) . 3_676 no C5 C3 2.315(3) . . no C5 C10 2.319(3) . . no C5 N1 2.568(3) . . no C5 N2 2.569(3) . . no C7 C2 3.489(3) . 3_776 no C8 C1 3.524(3) . 3_776 no C8 C2 3.363(3) . 3_776 no C8 C4 3.510(3) . 3_676 no C8 C9 3.577(3) . 3_676 no C9 C8 3.577(3) . 3_676 no C9 C3 3.339(3) . 3_776 no C10 O2 3.336(3) . 1_545 no C10 C14 3.532(3) . 1_445 no C11 O2 3.412(3) . 1_545 no C11 C2 3.259(3) . 1_545 no C11 C1 3.496(3) . 1_545 no C12 C13 3.567(3) . 1_545 no C13 C12 3.567(3) . 1_565 no C14 C10 3.532(3) . 1_665 no C14 O3 3.287(3) . 1_665 no C14 Pd1 3.726(3) . 1_565 no C15 C1 3.578(4) . 1_545 no C16 Pd1 3.806(3) . 1_545 no C1 H15B 2.9970 . 1_565 no C1 H13B 2.9006 . . no C1 H13A 2.8916 . . no C10 H14A 3.0743 . 1_445 no C11 H13A 2.9069 . 1_445 no C12 H15B 2.9469 . . no C12 H13B 2.8583 . 1_545 no C12 H15A 2.8763 . . no C12 H16B 2.9839 . 2_656 no C13 H1 2.8654 . . no C14 H9 2.9070 . 3_786 no C15 H12 2.8846 . . no C16 H8 3.0759 . 3_666 no H1 C13 2.8654 . . no H1 Br1 2.9816 . 2_756 no H7 O3 2.5874 . 3_666 no H8 O4 2.7088 . 3_666 no H8 C16 3.0759 . 3_666 no H9 C14 2.9070 . 3_786 no H9 H14C 2.5665 . 3_786 no H12 C15 2.8846 . . no H12 Br1 3.0342 . 2_746 no H12 H16B 2.5572 . 2_656 no H13A O4 2.6618 . 1_665 no H13A C1 2.8916 . . no H13A C11 2.9069 . 1_665 no H13B C1 2.9006 . . no H13B C12 2.8583 . 1_565 no H13B Br1 3.0001 . 2_756 no H14A O3 2.8260 . 1_665 no H14A C10 3.0743 . 1_665 no H14C Pd1 2.8441 . 1_565 no H14C H9 2.5665 . 3_786 no H15A C12 2.8763 . . no H15A H16B 2.5149 . 2_656 no H15B C1 2.9970 . 1_545 no H15B C12 2.9469 . . no H15B Br1 3.1023 . 2_746 no H16B C12 2.9839 . 2_646 no H16B H12 2.5572 . 2_646 no H16B H15A 2.5149 . 2_646 no H16C Pd1 2.8932 . 1_545 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C7 H7 O3 0.9500 2.5900 3.501(3) 161.00 3_666 yes #===END # Attachment '- 6c.cif' # CIF-file generated for Luo0426 Luo/Reiser #============================================================================== data_e121 _database_code_depnum_ccdc_archive 'CCDC 817026' #TrackingRef '- 6c.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H13 Br N2 O5 Pd' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C16 H13 Br N2 O5 Pd' _chemical_formula_sum 'C16 H13 Br N2 O5 Pd' _chemical_formula_iupac ? _chemical_formula_weight 499.60 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.6564(11) _cell_length_b 10.0610(12) _cell_length_c 10.5897(12) _cell_angle_alpha 107.986(13) _cell_angle_beta 112.136(12) _cell_angle_gamma 100.062(13) _cell_volume 855.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.93 _cell_special_details ; Cell parameters were determined by indexing 8000 reflections with I/sigma limit 6.0. ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow to orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 3.449 _exptl_crystal_density_meas_temp ? # Permitted for : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type analytical # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)' _exptl_absorpt_correction_T_min 0.3711 _exptl_absorpt_correction_T_max 0.7039 loop_ _exptl_crystal_face_index_h_ _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 3 0.0382 0 -3 -1 0.0734 1 1 -2 0.1694 -1 1 1 0.1313 1 -2 2 0.1349 0 3 1 0.0721 -1 2 -3 0.0887 -1 -1 3 0.1173 2 -1 -3 0.1573 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Data were collected applying an imaging plate system (STOE) with the following measurement parameters: Detector distance [mm] 60 Phi movement mode Oscillation Phi incr. [degrees] 1.4 Number of exposures 190 Irradiation / exposure [min] 4.00 For a detailed description of the method see: Sheldrick, G.M., Paulus, E. Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS diffractometer' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 10880 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.93 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_max 0.919 _diffrn_measured_fraction_theta_full 0.919 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 3756 # number of observed reflections (> n sig(I)) _reflns_number_gt 3258 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'STOE (1998)' _computing_cell_refinement 'STOE (1998)' _computing_data_reduction 'STOE (1998)' _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2, conventional R-factors R are based on F, with F set to zero for negative F^2. The observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment ' constr' _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3756 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.466 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.070 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd1 Pd Uani 0.26087(2) 0.44111(2) 0.45582(2) 1.000 0.0339(1) . . Br1 Br Uani 0.22659(4) 0.16727(3) 0.37439(3) 1.000 0.0529(1) . . O1 O Uani 0.4075(2) 0.7356(2) 0.2933(2) 1.000 0.0513(6) . . O2 O Uani 0.4737(4) 0.3490(3) 0.0563(3) 1.000 0.0805(10) . . O3 O Uani 0.3694(3) 0.2551(2) 0.1779(2) 1.000 0.0571(7) . . O4 O Uani 0.1141(2) 0.55672(19) 0.7779(2) 1.000 0.0461(6) . . O5 O Uani 0.0410(3) 0.3860(2) 0.8594(2) 1.000 0.0557(7) . . N1 N Uani 0.3496(2) 0.5316(2) 0.3326(2) 1.000 0.0383(6) . . N2 N Uani 0.1783(3) 0.4365(2) 0.6067(2) 1.000 0.0389(6) . . C1 C Uani 0.2621(3) 0.6452(2) 0.5348(3) 1.000 0.0383(7) . . C2 C Uani 0.3107(3) 0.7446(3) 0.4814(3) 1.000 0.0419(7) . . C3 C Uani 0.3073(3) 0.8892(3) 0.5347(3) 1.000 0.0500(9) . . C4 C Uani 0.2501(4) 0.9293(3) 0.6392(4) 1.000 0.0563(10) . . C5 C Uani 0.1983(4) 0.8300(3) 0.6926(3) 1.000 0.0509(9) . . C6 C Uani 0.2069(3) 0.6875(3) 0.6413(3) 1.000 0.0417(7) . . C7 C Uani 0.3571(3) 0.6721(3) 0.3702(3) 1.000 0.0414(7) . . C8 C Uani 0.4374(4) 0.6273(3) 0.2021(3) 1.000 0.0532(9) . . C9 C Uani 0.4030(3) 0.5020(3) 0.2230(3) 1.000 0.0440(8) . . C10 C Uani 0.4196(3) 0.3623(3) 0.1433(3) 1.000 0.0470(8) . . C11 C Uani 0.3748(4) 0.1109(3) 0.1036(4) 1.000 0.0652(11) . . C12 C Uani 0.1651(3) 0.5620(3) 0.6767(3) 1.000 0.0396(7) . . C13 C Uani 0.0938(3) 0.4137(3) 0.7672(3) 1.000 0.0441(8) . . C14 C Uani 0.1329(3) 0.3376(3) 0.6637(3) 1.000 0.0420(8) . . C15 C Uani 0.0237(4) 0.2364(3) 0.8516(3) 1.000 0.0514(9) . . C16 C Uani -0.0287(4) 0.2231(4) 0.9652(4) 1.000 0.0616(11) . . H3A H Uiso 0.34300 0.95860 0.50060 1.000 0.0600 calc R H4A H Uiso 0.24630 1.02700 0.67500 1.000 0.0680 calc R H5A H Uiso 0.15810 0.85880 0.76230 1.000 0.0610 calc R H8A H Uiso 0.47620 0.63840 0.13450 1.000 0.0640 calc R H11A H Uiso 0.28420 0.06050 0.00350 1.000 0.0780 calc R H11B H Uiso 0.37040 0.05240 0.16160 1.000 0.0780 calc R H11C H Uiso 0.47340 0.12190 0.09530 1.000 0.0780 calc R H14A H Uiso 0.13020 0.23760 0.63540 1.000 0.0500 calc R H15A H Uiso 0.12590 0.21800 0.87350 1.000 0.0620 calc R H15B H Uiso -0.05590 0.16290 0.75010 1.000 0.0620 calc R H16A H Uiso 0.05080 0.29670 1.06500 1.000 0.0740 calc R H16B H Uiso -0.04050 0.12360 0.96290 1.000 0.0740 calc R H16C H Uiso -0.13040 0.24050 0.94170 1.000 0.0740 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0392(1) 0.0293(1) 0.0365(1) 0.0150(1) 0.0193(1) 0.0114(1) Br1 0.0774(2) 0.0352(1) 0.0624(2) 0.0228(1) 0.0441(2) 0.0227(1) O1 0.0576(11) 0.0502(10) 0.0581(11) 0.0332(9) 0.0309(10) 0.0150(8) O2 0.125(2) 0.0765(16) 0.0840(17) 0.0401(14) 0.0825(18) 0.0401(15) O3 0.0748(14) 0.0472(10) 0.0619(12) 0.0207(9) 0.0461(12) 0.0182(9) O4 0.0577(11) 0.0394(9) 0.0490(10) 0.0167(8) 0.0333(10) 0.0163(8) O5 0.0778(14) 0.0488(10) 0.0578(12) 0.0239(9) 0.0471(12) 0.0196(9) N1 0.0400(11) 0.0388(10) 0.0386(10) 0.0188(8) 0.0189(9) 0.0114(8) N2 0.0458(11) 0.0344(9) 0.0404(10) 0.0164(8) 0.0233(10) 0.0121(8) C1 0.0389(12) 0.0304(10) 0.0437(13) 0.0148(9) 0.0175(11) 0.0113(9) C2 0.0414(13) 0.0344(11) 0.0481(14) 0.0201(10) 0.0172(12) 0.0106(9) C3 0.0508(15) 0.0354(12) 0.0603(17) 0.0242(12) 0.0195(14) 0.0120(11) C4 0.0624(18) 0.0335(12) 0.0694(19) 0.0199(12) 0.0259(17) 0.0200(12) C5 0.0575(16) 0.0389(13) 0.0551(16) 0.0135(11) 0.0282(15) 0.0186(11) C6 0.0437(13) 0.0344(11) 0.0454(13) 0.0148(10) 0.0207(12) 0.0120(10) C7 0.0423(13) 0.0399(12) 0.0444(13) 0.0239(10) 0.0186(12) 0.0097(9) C8 0.0576(17) 0.0588(16) 0.0541(16) 0.0320(14) 0.0313(15) 0.0148(13) C9 0.0413(13) 0.0523(14) 0.0399(13) 0.0216(11) 0.0199(12) 0.0111(10) C10 0.0441(14) 0.0565(15) 0.0408(13) 0.0221(12) 0.0207(12) 0.0113(11) C11 0.078(2) 0.0473(16) 0.070(2) 0.0153(14) 0.0420(19) 0.0176(14) C12 0.0419(13) 0.0368(11) 0.0388(12) 0.0123(9) 0.0204(11) 0.0117(9) C13 0.0523(15) 0.0398(12) 0.0454(13) 0.0173(10) 0.0285(13) 0.0137(10) C14 0.0509(14) 0.0386(12) 0.0438(13) 0.0196(10) 0.0269(12) 0.0145(10) C15 0.0604(17) 0.0500(15) 0.0476(14) 0.0228(12) 0.0281(14) 0.0143(12) C16 0.0659(19) 0.0699(19) 0.0588(18) 0.0334(16) 0.0359(17) 0.0151(15) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pd1 Br1 2.5382(5) . . yes Pd1 N1 2.138(2) . . yes Pd1 N2 2.045(2) . . yes Pd1 C1 1.959(2) . . yes O1 C7 1.349(4) . . yes O1 C8 1.369(4) . . yes O2 C10 1.204(5) . . yes O3 C10 1.314(4) . . yes O3 C11 1.442(4) . . yes O4 C12 1.348(4) . . yes O4 C13 1.381(4) . . yes O5 C13 1.336(4) . . yes O5 C15 1.458(4) . . yes N1 C7 1.326(4) . . yes N1 C9 1.412(4) . . yes N2 C12 1.308(4) . . yes N2 C14 1.402(4) . . yes C1 C2 1.388(4) . . no C1 C6 1.405(4) . . no C2 C3 1.400(4) . . no C2 C7 1.449(4) . . no C3 C4 1.398(5) . . no C4 C5 1.398(5) . . no C5 C6 1.397(5) . . no C6 C12 1.458(5) . . no C8 C9 1.353(5) . . no C9 C10 1.470(4) . . no C13 C14 1.351(4) . . no C15 C16 1.502(5) . . no C3 H3A 0.9498 . . no C4 H4A 0.9509 . . no C5 H5A 0.9500 . . no C8 H8A 0.9498 . . no C11 H11A 0.9800 . . no C11 H11B 0.9796 . . no C11 H11C 0.9792 . . no C14 H14A 0.9495 . . no C15 H15A 0.9899 . . no C15 H15B 0.9904 . . no C16 H16A 0.9804 . . no C16 H16B 0.9791 . . no C16 H16C 0.9797 . . 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 Br1 Pd1 N1 111.11(6) . . . yes Br1 Pd1 N2 90.94(6) . . . yes Br1 Pd1 C1 169.58(9) . . . yes N1 Pd1 N2 157.94(8) . . . yes N1 Pd1 C1 78.89(10) . . . yes N2 Pd1 C1 79.06(10) . . . yes C7 O1 C8 104.9(2) . . . yes C10 O3 C11 118.0(3) . . . yes C12 O4 C13 104.3(2) . . . yes C13 O5 C15 113.4(3) . . . yes Pd1 N1 C7 110.04(17) . . . yes Pd1 N1 C9 145.34(19) . . . yes C7 N1 C9 104.6(2) . . . yes Pd1 N2 C12 114.04(19) . . . yes Pd1 N2 C14 139.0(2) . . . yes C12 N2 C14 107.0(2) . . . yes Pd1 C1 C2 120.3(2) . . . yes Pd1 C1 C6 119.1(2) . . . yes C2 C1 C6 120.6(3) . . . no C1 C2 C3 120.3(3) . . . no C1 C2 C7 109.4(3) . . . no C3 C2 C7 130.3(3) . . . no C2 C3 C4 118.6(3) . . . no C3 C4 C5 122.0(3) . . . no C4 C5 C6 118.6(3) . . . no C1 C6 C5 120.0(3) . . . no C1 C6 C12 108.5(3) . . . no C5 C6 C12 131.5(3) . . . no O1 C7 N1 113.5(2) . . . yes O1 C7 C2 125.1(3) . . . yes N1 C7 C2 121.4(3) . . . yes O1 C8 C9 109.5(3) . . . yes N1 C9 C8 107.6(3) . . . yes N1 C9 C10 127.7(3) . . . yes C8 C9 C10 124.8(3) . . . no O2 C10 O3 124.3(3) . . . yes O2 C10 C9 123.2(3) . . . yes O3 C10 C9 112.6(3) . . . yes O4 C12 N2 112.7(3) . . . yes O4 C12 C6 128.1(3) . . . yes N2 C12 C6 119.2(3) . . . yes O4 C13 O5 113.2(2) . . . yes O4 C13 C14 110.1(3) . . . yes O5 C13 C14 136.6(3) . . . yes N2 C14 C13 105.9(3) . . . yes O5 C15 C16 107.7(3) . . . yes C2 C3 H3A 120.75 . . . no C4 C3 H3A 120.68 . . . no C3 C4 H4A 119.01 . . . no C5 C4 H4A 119.03 . . . no C4 C5 H5A 120.71 . . . no C6 C5 H5A 120.68 . . . no O1 C8 H8A 125.24 . . . no C9 C8 H8A 125.26 . . . no O3 C11 H11A 109.44 . . . no O3 C11 H11B 109.46 . . . no O3 C11 H11C 109.45 . . . no H11A C11 H11B 109.48 . . . no H11A C11 H11C 109.54 . . . no H11B C11 H11C 109.46 . . . no N2 C14 H14A 127.06 . . . no C13 C14 H14A 127.03 . . . no O5 C15 H15A 110.15 . . . no O5 C15 H15B 110.11 . . . no C16 C15 H15A 110.21 . . . no C16 C15 H15B 110.25 . . . no H15A C15 H15B 108.43 . . . no C15 C16 H16A 109.41 . . . no C15 C16 H16B 109.42 . . . no C15 C16 H16C 109.41 . . . no H16A C16 H16B 109.52 . . . no H16A C16 H16C 109.52 . . . no H16B C16 H16C 109.54 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Pd1 N1 C7 176.08(16) . . . . no N2 Pd1 N1 C7 -2.1(3) . . . . no C1 Pd1 N1 C7 -0.83(19) . . . . no Br1 Pd1 N1 C9 -2.6(3) . . . . no N2 Pd1 N1 C9 179.3(3) . . . . no C1 Pd1 N1 C9 -179.5(3) . . . . no Br1 Pd1 N2 C12 -176.3(2) . . . . no N1 Pd1 N2 C12 2.0(4) . . . . no C1 Pd1 N2 C12 0.8(2) . . . . no Br1 Pd1 N2 C14 5.8(3) . . . . no N1 Pd1 N2 C14 -175.9(2) . . . . no C1 Pd1 N2 C14 -177.2(3) . . . . no N1 Pd1 C1 C2 1.0(2) . . . . no N2 Pd1 C1 C2 -179.5(3) . . . . no N1 Pd1 C1 C6 178.4(2) . . . . no N2 Pd1 C1 C6 -2.1(2) . . . . no C8 O1 C7 N1 -1.4(3) . . . . no C8 O1 C7 C2 -179.9(3) . . . . no C7 O1 C8 C9 1.0(3) . . . . no C11 O3 C10 C9 178.1(3) . . . . no C11 O3 C10 O2 -2.0(5) . . . . no C13 O4 C12 C6 -179.4(3) . . . . no C12 O4 C13 O5 -179.3(2) . . . . no C12 O4 C13 C14 0.5(3) . . . . no C13 O4 C12 N2 -0.3(3) . . . . no C15 O5 C13 C14 2.0(5) . . . . no C15 O5 C13 O4 -178.3(2) . . . . no C13 O5 C15 C16 177.4(3) . . . . no C9 N1 C7 C2 179.8(3) . . . . no C7 N1 C9 C10 179.6(3) . . . . no C7 N1 C9 C8 -0.5(3) . . . . no Pd1 N1 C9 C8 178.2(2) . . . . no Pd1 N1 C7 C2 0.6(3) . . . . no Pd1 N1 C7 O1 -178.02(18) . . . . no Pd1 N1 C9 C10 -1.7(5) . . . . no C9 N1 C7 O1 1.2(3) . . . . no C14 N2 C12 C6 179.2(3) . . . . no Pd1 N2 C12 C6 0.6(3) . . . . no Pd1 N2 C14 C13 178.3(2) . . . . no Pd1 N2 C12 O4 -178.50(18) . . . . no C12 N2 C14 C13 0.2(3) . . . . no C14 N2 C12 O4 0.1(3) . . . . no Pd1 C1 C6 C5 -176.3(2) . . . . no Pd1 C1 C2 C3 178.2(2) . . . . no C6 C1 C2 C7 -178.3(3) . . . . no Pd1 C1 C6 C12 2.9(3) . . . . no C2 C1 C6 C12 -179.8(3) . . . . no Pd1 C1 C2 C7 -1.0(3) . . . . no C2 C1 C6 C5 1.0(4) . . . . no C6 C1 C2 C3 0.9(4) . . . . no C7 C2 C3 C4 177.2(3) . . . . no C1 C2 C7 N1 0.2(4) . . . . no C1 C2 C3 C4 -1.7(4) . . . . no C3 C2 C7 O1 -0.4(5) . . . . no C3 C2 C7 N1 -178.9(3) . . . . no C1 C2 C7 O1 178.6(3) . . . . no C2 C3 C4 C5 0.7(5) . . . . no C3 C4 C5 C6 1.1(5) . . . . no C4 C5 C6 C12 179.1(3) . . . . no C4 C5 C6 C1 -2.0(5) . . . . no C1 C6 C12 N2 -2.2(4) . . . . no C5 C6 C12 O4 -4.1(5) . . . . no C1 C6 C12 O4 176.8(3) . . . . no C5 C6 C12 N2 176.9(3) . . . . no O1 C8 C9 C10 179.6(3) . . . . no O1 C8 C9 N1 -0.3(3) . . . . no C8 C9 C10 O2 3.9(5) . . . . no N1 C9 C10 O3 3.6(4) . . . . no N1 C9 C10 O2 -176.2(3) . . . . no C8 C9 C10 O3 -176.2(3) . . . . no O5 C13 C14 N2 179.2(3) . . . . no O4 C13 C14 N2 -0.4(3) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd1 O3 3.588(3) . . no Pd1 C7 3.993(3) . 2_666 no Pd1 Pd1 4.2136(6) . 2_666 no Pd1 O3 3.945(2) . 2_666 no Pd1 O4 3.542(2) . 2_566 no Pd1 N1 3.486(2) . 2_666 no Pd1 C5 4.177(4) . 2_566 no Pd1 C6 4.095(3) . 2_566 no Pd1 C10 3.777(3) . 2_666 no Pd1 C8 4.046(3) . 2_666 no Pd1 C9 3.501(3) . 2_666 no Pd1 C12 3.804(3) . 2_566 no Pd1 C13 4.150(3) . 2_566 no Pd1 H16A 3.5049 . 1_554 no Br1 O3 3.144(3) . . no Br1 N2 3.286(2) . . no Br1 C3 3.744(3) . 1_545 no Br1 C11 3.601(4) . . no Br1 C14 3.540(3) . . no Br1 C7 3.595(3) . 2_666 no Br1 H11B 3.1069 . . no Br1 H14A 3.1572 . . no Br1 H3A 2.9804 . 1_545 no Br1 H15B 3.0388 . 2_556 no O2 C8 3.222(5) . 2_665 no O2 C12 3.298(5) . 2_666 no O3 Pd1 3.945(2) . 2_666 no O3 Br1 3.144(3) . . no O3 N1 2.840(3) . . no O3 Pd1 3.588(3) . . no O3 C1 3.411(4) . 2_666 no O4 C16 3.405(4) . 2_567 no O4 Pd1 3.542(2) . 2_566 no O2 H11C 2.4439 . . no O2 H8A 2.7632 . . no O2 H11A 2.9081 . . no O2 H8A 2.2817 . 2_665 no N1 O3 2.840(3) . . no N1 C1 2.607(4) . . no N1 C2 2.420(4) . . no N1 Pd1 3.486(2) . 2_666 no N2 Br1 3.286(2) . . no N2 C1 2.550(3) . . no N2 C6 2.387(4) . . no N2 C6 3.359(4) . 2_566 no C1 N1 2.607(4) . . no C1 N2 2.550(3) . . no C1 C7 2.316(4) . . no C1 C12 2.324(4) . . no C1 O3 3.411(4) . 2_666 no C1 C13 3.496(4) . 2_566 no C2 C13 3.495(4) . 2_566 no C3 Br1 3.744(3) . 1_565 no C5 C14 3.522(4) . 2_566 no C5 Pd1 4.177(4) . 2_566 no C6 C14 3.533(4) . 2_566 no C6 Pd1 4.095(3) . 2_566 no C6 N2 3.359(4) . 2_566 no C7 Br1 3.595(3) . 2_666 no C7 Pd1 3.993(3) . 2_666 no C8 Pd1 4.046(3) . 2_666 no C8 O2 3.222(5) . 2_665 no C9 Pd1 3.501(3) . 2_666 no C10 C12 3.546(4) . 2_666 no C10 Pd1 3.777(3) . 2_666 no C10 C15 3.571(5) . 1_554 no C11 Br1 3.601(4) . . no C12 C12 3.530(4) . 2_566 no C12 Pd1 3.804(3) . 2_566 no C12 C10 3.546(4) . 2_666 no C12 O2 3.298(5) . 2_666 no C13 C2 3.495(4) . 2_566 no C13 Pd1 4.150(3) . 2_566 no C13 C1 3.496(4) . 2_566 no C14 C6 3.533(4) . 2_566 no C14 C5 3.522(4) . 2_566 no C15 C10 3.571(5) . 1_556 no C16 O4 3.405(4) . 2_567 no C3 H15B 2.8854 . 2_566 no C5 H11A 3.0757 . 1_566 no C5 H11C 2.9590 . 2_666 no C6 H11C 3.0211 . 2_666 no C10 H15A 2.8648 . 1_554 no C14 H15B 2.8950 . . no C14 H15A 2.8503 . . no C15 H14A 2.8437 . . no H3A Br1 2.9804 . 1_565 no H5A H11A 2.3909 . 1_566 no H8A O2 2.7632 . . no H8A O2 2.2817 . 2_665 no H11A O2 2.9081 . . no H11A C5 3.0757 . 1_544 no H11A H5A 2.3909 . 1_544 no H11B Br1 3.1069 . . no H11C O2 2.4439 . . no H11C C5 2.9590 . 2_666 no H11C C6 3.0211 . 2_666 no H14A Br1 3.1572 . . no H14A C15 2.8437 . . no H15A C10 2.8648 . 1_556 no H15A C14 2.8503 . . no H15B C14 2.8950 . . no H15B Br1 3.0388 . 2_556 no H15B C3 2.8854 . 2_566 no H16A Pd1 3.5049 . 1_556 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C8 H8A O2 0.9500 2.2800 3.222(5) 171.00 2_665 yes _vrf_PLAT029_e121 ; PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.92 RESPONSE:There is a missing cusp of data due to data collection by rotation around the spindle axis only. ; #===END # Attachment '- 7a.cif' # CIF-file generated for Luo Luo02013 #============================================================================== data_e029a _database_code_depnum_ccdc_archive 'CCDC 817027' #TrackingRef '- 7a.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 Br N2 O4 Pt' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C16 H15 Br N2 O4 Pt' _chemical_formula_iupac ? _chemical_formula_weight 574.28 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 33.697(4) _cell_length_b 5.2354(4) _cell_length_c 19.994(2) _cell_angle_alpha 90 _cell_angle_beta 96.702(14) _cell_angle_gamma 90 _cell_volume 3503.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173 _cell_measurement_reflns_used 6831 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.87 _cell_special_details ; Cell parameters were determined by indexing 6831 reflections with I/sigma limit 6.0. ; _exptl_crystal_description rod _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.020 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 10.313 _exptl_crystal_density_meas_temp ? # Permitted for # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type numerical # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details 'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)' _exptl_absorpt_correction_T_min 0.1554 _exptl_absorpt_correction_T_max 0.2564 loop_ _exptl_crystal_face_index_h_ _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 15 -1 1 0.0921 -9 1 15 0.1250 15 1 -1 0.0715 -15 0 -1 0.0894 1 0 -8 0.1170 10 -11 15 0.1011 -10 3 3 0.1048 4 -3 -10 0.1118 5 7 -15 0.1196 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Data were collected applying an imaging plate system (STOE) with the following measurement parameters: Detector distance [mm] 70 Phi movement mode Oscillation Phi incr. [degrees] 1.0 Number of exposures 277 Irradiation / exposure [min] 6.00 For a detailed description of the method see: Sheldrick, G.M., Paulus, E. Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS diffractometer' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 6524 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.87 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_max 0.495 _diffrn_measured_fraction_theta_full 0.495 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 1688 # number of observed reflections (> n sig(I)) _reflns_number_gt 1450 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'STOE (1998)' _computing_cell_refinement 'STOE (1998)' _computing_data_reduction 'STOE (1998)' _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 1688 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1272 _refine_ls_wR_factor_gt 0.1225 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.792 _refine_diff_density_min -1.567 _refine_diff_density_rms 0.204 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt Uani 0.14236(1) 0.94609(8) 0.50458(2) 1.000 0.0320(2) . . Br1 Br Uani 0.20858(5) 0.9491(3) 0.57516(8) 1.000 0.0533(5) . . O1 O Uani 0.1222(3) 0.4111(16) 0.3566(4) 1.000 0.039(3) . . O2 O Uani 0.1721(2) 0.1449(18) 0.3350(3) 1.000 0.044(3) . . O3 O Uani 0.0610(3) 1.4671(16) 0.5544(4) 1.000 0.040(3) . . O4 O Uani 0.0789(3) 1.7442(17) 0.6404(3) 1.000 0.043(3) . . N1 N Uani 0.1490(3) 0.6537(18) 0.4404(4) 1.000 0.032(3) . . N2 N Uani 0.1161(3) 1.239(2) 0.5487(4) 1.000 0.037(3) . . C1 C Uani 0.0888(4) 0.937(2) 0.4526(6) 1.000 0.033(4) . . C2 C Uani 0.0602(4) 1.110(2) 0.4680(5) 1.000 0.035(3) . . C3 C Uani 0.0223(4) 1.103(2) 0.4320(5) 1.000 0.040(4) . . C4 C Uani 0.0130(4) 0.919(2) 0.3840(6) 1.000 0.042(4) . . C5 C Uani 0.0428(3) 0.742(3) 0.3691(5) 1.000 0.042(3) . . C6 C Uani 0.0802(3) 0.751(3) 0.4026(4) 1.000 0.036(3) . . C7 C Uani 0.1171(4) 0.604(3) 0.3998(6) 1.000 0.043(4) . . C8 C Uani 0.1793(4) 0.488(2) 0.4253(5) 1.000 0.037(4) . . C9 C Uani 0.1622(3) 0.330(2) 0.3732(5) 1.000 0.035(3) . . C10 C Uani 0.2131(4) 0.067(3) 0.3489(7) 1.000 0.048(5) . . C11 C Uani 0.2204(4) -0.123(3) 0.2927(5) 1.000 0.049(4) . . C12 C Uani 0.0788(3) 1.273(2) 0.5237(4) 1.000 0.035(3) . . C13 C Uani 0.1244(5) 1.423(2) 0.6002(6) 1.000 0.042(4) . . C14 C Uani 0.0908(4) 1.552(2) 0.6025(6) 1.000 0.039(4) . . C15 C Uani 0.1112(4) 1.841(3) 0.6914(5) 1.000 0.048(4) . . C16 C Uani 0.0922(5) 2.030(3) 0.7319(6) 1.000 0.045(5) . . H3A H Uiso 0.00280 1.22640 0.44080 1.000 0.0480 calc R H4A H Uiso -0.01320 0.90920 0.36080 1.000 0.0510 calc R H5A H Uiso 0.03640 0.61580 0.33540 1.000 0.0500 calc R H8 H Uiso 0.20610 0.48310 0.44630 1.000 0.0450 calc R H10A H Uiso 0.21790 -0.01580 0.39360 1.000 0.0580 calc R H10B H Uiso 0.23110 0.21620 0.34830 1.000 0.0580 calc R H11A H Uiso 0.20220 -0.26910 0.29390 1.000 0.0580 calc R H11B H Uiso 0.21540 -0.03840 0.24890 1.000 0.0580 calc R H11C H Uiso 0.24810 -0.18360 0.29980 1.000 0.0580 calc R H13 H Uiso 0.14900 1.44780 0.62760 1.000 0.0500 calc R H15A H Uiso 0.12280 1.69940 0.72010 1.000 0.0580 calc R H15B H Uiso 0.13270 1.92160 0.66900 1.000 0.0580 calc R H16A H Uiso 0.08110 2.16930 0.70280 1.000 0.0550 calc R H16B H Uiso 0.07070 1.94770 0.75310 1.000 0.0550 calc R H16C H Uiso 0.11210 2.09860 0.76690 1.000 0.0550 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0337(3) 0.0342(4) 0.0283(3) 0.0007(1) 0.0048(2) 0.0011(2) Br1 0.0410(8) 0.0634(11) 0.0531(8) -0.0087(6) -0.0049(6) 0.0036(6) O1 0.043(5) 0.050(6) 0.021(3) -0.003(3) -0.003(3) 0.016(4) O2 0.038(4) 0.052(5) 0.039(4) -0.015(4) -0.002(3) 0.002(4) O3 0.039(5) 0.040(5) 0.044(4) 0.001(3) 0.012(4) 0.004(4) O4 0.050(5) 0.046(5) 0.035(4) 0.002(4) 0.010(3) 0.008(4) N1 0.039(5) 0.031(5) 0.027(4) 0.002(3) 0.011(3) 0.002(4) N2 0.045(5) 0.035(6) 0.030(4) 0.007(4) 0.003(3) -0.004(5) C1 0.020(5) 0.040(8) 0.038(7) 0.007(5) 0.002(5) -0.003(4) C2 0.041(6) 0.041(6) 0.025(4) 0.007(4) 0.011(4) -0.006(5) C3 0.033(6) 0.049(8) 0.039(6) 0.003(5) 0.003(4) 0.010(5) C4 0.041(7) 0.040(8) 0.046(6) 0.011(5) 0.008(5) 0.002(5) C5 0.045(6) 0.044(7) 0.036(5) -0.002(5) 0.006(4) -0.001(6) C6 0.040(6) 0.045(7) 0.022(4) -0.002(5) -0.003(4) 0.008(5) C7 0.038(7) 0.052(8) 0.039(6) 0.004(5) 0.010(5) -0.004(6) C8 0.043(7) 0.047(7) 0.023(5) 0.000(4) 0.012(4) 0.002(5) C9 0.035(5) 0.030(6) 0.039(5) -0.001(4) 0.004(4) 0.003(5) C10 0.029(6) 0.064(11) 0.051(7) -0.016(6) 0.003(5) 0.006(6) C11 0.054(7) 0.050(8) 0.043(6) -0.014(6) 0.010(5) 0.002(7) C12 0.036(5) 0.039(6) 0.030(4) 0.002(4) 0.009(4) 0.001(5) C13 0.055(8) 0.041(8) 0.030(5) -0.009(4) 0.010(5) -0.003(6) C14 0.049(8) 0.036(7) 0.033(6) -0.002(4) 0.013(5) -0.006(5) C15 0.073(9) 0.049(8) 0.023(5) -0.003(5) 0.008(5) 0.005(7) C16 0.051(9) 0.062(9) 0.022(6) -0.004(5) 0.000(6) 0.013(7) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pt1 Br1 2.4973(17) . . yes Pt1 N1 2.027(9) . . yes Pt1 N2 2.024(10) . . yes Pt1 C1 1.975(13) . . yes O1 C7 1.353(16) . . yes O1 C9 1.415(14) . . yes O2 C9 1.301(13) . . yes O2 C10 1.436(15) . . yes O3 C12 1.362(13) . . yes O3 C14 1.380(15) . . yes O4 C14 1.349(14) . . yes O4 C15 1.491(15) . . yes N1 C7 1.296(16) . . yes N1 C8 1.399(16) . . yes N2 C12 1.310(14) . . yes N2 C13 1.414(15) . . yes C1 C2 1.383(17) . . no C1 C6 1.401(17) . . no C2 C3 1.391(18) . . no C2 C12 1.483(14) . . no C3 C4 1.370(15) . . no C4 C5 1.423(18) . . no C5 C6 1.357(14) . . no C6 C7 1.469(19) . . no C8 C9 1.401(15) . . no C10 C11 1.54(2) . . no C13 C14 1.32(2) . . no C15 C16 1.47(2) . . no C3 H3A 0.9500 . . no C4 H4A 0.9500 . . no C5 H5A 0.9500 . . no C8 H8 0.9500 . . no C10 H10A 0.9900 . . no C10 H10B 0.9900 . . no C11 H11A 0.9800 . . no C11 H11B 0.9800 . . no C11 H11C 0.9800 . . no C13 H13 0.9500 . . no C15 H15A 0.9900 . . no C15 H15B 0.9900 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . 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 Br1 Pt1 N1 101.8(3) . . . yes Br1 Pt1 N2 99.0(3) . . . yes Br1 Pt1 C1 177.2(4) . . . yes N1 Pt1 N2 159.2(4) . . . yes N1 Pt1 C1 79.1(4) . . . yes N2 Pt1 C1 80.1(4) . . . yes C7 O1 C9 105.2(9) . . . yes C9 O2 C10 113.9(9) . . . yes C12 O3 C14 103.4(9) . . . yes C14 O4 C15 113.4(10) . . . yes Pt1 N1 C7 113.8(9) . . . yes Pt1 N1 C8 137.9(8) . . . yes C7 N1 C8 108.3(10) . . . yes Pt1 N2 C12 112.7(7) . . . yes Pt1 N2 C13 140.8(9) . . . yes C12 N2 C13 106.6(10) . . . yes Pt1 C1 C2 119.0(8) . . . yes Pt1 C1 C6 119.5(9) . . . yes C2 C1 C6 121.5(11) . . . no C1 C2 C3 119.3(10) . . . no C1 C2 C12 107.4(11) . . . no C3 C2 C12 133.3(10) . . . no C2 C3 C4 120.1(11) . . . no C3 C4 C5 119.7(12) . . . no C4 C5 C6 120.8(12) . . . no C1 C6 C5 118.6(12) . . . no C1 C6 C7 106.6(10) . . . no C5 C6 C7 134.8(12) . . . no O1 C7 N1 113.1(12) . . . yes O1 C7 C6 125.9(11) . . . yes N1 C7 C6 121.0(12) . . . yes N1 C8 C9 106.2(10) . . . yes O1 C9 O2 112.8(8) . . . yes O1 C9 C8 107.2(9) . . . yes O2 C9 C8 139.9(10) . . . yes O2 C10 C11 105.9(10) . . . yes O3 C12 N2 112.5(9) . . . yes O3 C12 C2 126.7(10) . . . yes N2 C12 C2 120.8(10) . . . yes N2 C13 C14 106.0(12) . . . yes O3 C14 O4 113.1(11) . . . yes O3 C14 C13 111.5(10) . . . yes O4 C14 C13 135.4(12) . . . yes O4 C15 C16 106.0(11) . . . yes C2 C3 H3A 120.00 . . . no C4 C3 H3A 120.00 . . . no C3 C4 H4A 120.00 . . . no C5 C4 H4A 120.00 . . . no C4 C5 H5A 120.00 . . . no C6 C5 H5A 120.00 . . . no N1 C8 H8 127.00 . . . no C9 C8 H8 127.00 . . . no O2 C10 H10A 111.00 . . . no O2 C10 H10B 111.00 . . . no C11 C10 H10A 111.00 . . . no C11 C10 H10B 110.00 . . . no H10A C10 H10B 109.00 . . . no C10 C11 H11A 109.00 . . . no C10 C11 H11B 110.00 . . . no C10 C11 H11C 109.00 . . . no H11A C11 H11B 109.00 . . . no H11A C11 H11C 109.00 . . . no H11B C11 H11C 110.00 . . . no N2 C13 H13 127.00 . . . no C14 C13 H13 127.00 . . . no O4 C15 H15A 110.00 . . . no O4 C15 H15B 110.00 . . . no C16 C15 H15A 111.00 . . . no C16 C15 H15B 111.00 . . . no H15A C15 H15B 109.00 . . . no C15 C16 H16A 110.00 . . . no C15 C16 H16B 109.00 . . . no C15 C16 H16C 110.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Pt1 N1 C7 176.6(8) . . . . no N2 Pt1 N1 C7 -2.9(16) . . . . no C1 Pt1 N1 C7 -0.7(9) . . . . no Br1 Pt1 N1 C8 -5.6(11) . . . . no N2 Pt1 N1 C8 174.9(10) . . . . no C1 Pt1 N1 C8 177.1(11) . . . . no Br1 Pt1 N2 C12 -176.1(7) . . . . no N1 Pt1 N2 C12 3.4(15) . . . . no C1 Pt1 N2 C12 1.2(8) . . . . no Br1 Pt1 N2 C13 2.1(13) . . . . no N1 Pt1 N2 C13 -178.5(11) . . . . no C1 Pt1 N2 C13 179.4(13) . . . . no N1 Pt1 C1 C2 179.8(10) . . . . no N2 Pt1 C1 C2 -1.0(9) . . . . no N1 Pt1 C1 C6 1.8(9) . . . . no N2 Pt1 C1 C6 -179.0(10) . . . . no C9 O1 C7 N1 0.7(14) . . . . no C7 O1 C9 O2 -179.1(10) . . . . no C7 O1 C9 C8 -1.7(12) . . . . no C9 O1 C7 C6 -179.9(12) . . . . no C10 O2 C9 O1 177.4(9) . . . . no C10 O2 C9 C8 1.2(19) . . . . no C9 O2 C10 C11 -172.1(10) . . . . no C14 O3 C12 N2 -0.8(11) . . . . no C12 O3 C14 C13 1.3(12) . . . . no C12 O3 C14 O4 -178.6(9) . . . . no C14 O3 C12 C2 179.3(10) . . . . no C14 O4 C15 C16 -174.7(10) . . . . no C15 O4 C14 O3 -178.7(9) . . . . no C15 O4 C14 C13 1.5(19) . . . . no C7 N1 C8 C9 -1.6(12) . . . . no C8 N1 C7 O1 0.6(14) . . . . no Pt1 N1 C7 O1 179.0(8) . . . . no Pt1 N1 C8 C9 -179.5(8) . . . . no Pt1 N1 C7 C6 -0.5(15) . . . . no C8 N1 C7 C6 -178.9(11) . . . . no C12 N2 C13 C14 0.8(13) . . . . no C13 N2 C12 O3 0.0(12) . . . . no Pt1 N2 C12 C2 -1.3(12) . . . . no Pt1 N2 C12 O3 178.8(6) . . . . no Pt1 N2 C13 C14 -177.5(9) . . . . no C13 N2 C12 C2 180.0(9) . . . . no Pt1 C1 C6 C7 -2.4(13) . . . . no Pt1 C1 C2 C3 -179.4(8) . . . . no C2 C1 C6 C7 179.8(11) . . . . no Pt1 C1 C2 C12 0.7(12) . . . . no C2 C1 C6 C5 -0.2(18) . . . . no C6 C1 C2 C12 178.6(10) . . . . no Pt1 C1 C6 C5 177.7(9) . . . . no C6 C1 C2 C3 -1.5(17) . . . . no C3 C2 C12 N2 -179.5(11) . . . . no C3 C2 C12 O3 0.4(19) . . . . no C1 C2 C3 C4 3.0(16) . . . . no C12 C2 C3 C4 -177.1(11) . . . . no C1 C2 C12 O3 -179.6(10) . . . . no C1 C2 C12 N2 0.5(14) . . . . no C2 C3 C4 C5 -2.7(17) . . . . no C3 C4 C5 C6 1.0(18) . . . . no C4 C5 C6 C1 0.5(18) . . . . no C4 C5 C6 C7 -179.5(13) . . . . no C5 C6 C7 N1 -178.2(13) . . . . no C5 C6 C7 O1 2(2) . . . . no C1 C6 C7 O1 -177.6(12) . . . . no C1 C6 C7 N1 1.8(17) . . . . no N1 C8 C9 O1 2.0(11) . . . . no N1 C8 C9 O2 178.4(13) . . . . no N2 C13 C14 O4 178.5(13) . . . . no N2 C13 C14 O3 -1.3(13) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt1 C8 3.546(11) . 1_565 no Pt1 C9 3.435(10) . 1_565 no Pt1 C13 3.434(11) . 1_545 no Pt1 C14 3.450(12) . 1_545 no Br1 N1 3.524(9) . . no Br1 N2 3.451(10) . . no Br1 H8 2.9800 . 7_566 no Br1 H10B 2.9700 . 7_566 no Br1 H11C 3.0800 . 7_556 no O1 C1 3.408(14) . 1_545 no O2 C15 3.329(13) . 4_574 no O2 C16 3.323(17) . 4_574 no O3 C1 3.394(14) . 1_565 no O1 H15A 2.7900 . 4_574 no O2 H15A 2.7900 . 4_574 no O2 H16C 2.6300 . 4_574 no O3 H3A 2.6900 . 3_586 no O4 H4A 2.8600 . 3_586 no N1 Br1 3.524(9) . . no N1 C1 2.548(16) . . no N1 C6 2.408(14) . . no N2 Br1 3.451(10) . . no N2 C1 2.574(15) . . no N2 C2 2.429(15) . . no N2 H15B 2.9200 . 1_545 no C1 O1 3.408(14) . 1_565 no C1 O3 3.394(14) . 1_545 no C1 N1 2.548(16) . . no C1 N2 2.574(15) . . no C1 C7 2.302(19) . . no C1 C12 2.311(15) . . no C2 C7 3.583(19) . 1_565 no C3 C3 3.431(16) . 3_576 no C5 C16 3.576(18) . 4_584 no C6 C12 3.486(16) . 1_545 no C7 C12 3.399(16) . 1_545 no C7 C2 3.583(19) . 1_545 no C8 Pt1 3.546(11) . 1_545 no C9 Pt1 3.435(10) . 1_545 no C12 C7 3.399(16) . 1_565 no C12 C6 3.486(16) . 1_565 no C13 Pt1 3.434(11) . 1_565 no C14 Pt1 3.450(12) . 1_565 no C15 O2 3.329(13) . 4_575 no C16 O2 3.323(17) . 4_575 no C16 C5 3.576(18) . 4_585 no C5 H16B 3.0700 . 4_584 no C7 H16C 3.0700 . 4_584 no C8 H10A 3.0100 . 1_565 no C8 H11A 3.1000 . 1_565 no C8 H10B 2.8400 . . no C8 H10A 3.0400 . . no C9 H11A 3.0400 . 1_565 no C10 H8 2.9500 . . no C13 H15B 2.9600 . 1_545 no C13 H15B 2.9500 . . no C13 H15A 2.8100 . . no C13 H16A 2.9700 . 1_545 no C14 H16A 2.8800 . 1_545 no C15 H13 2.8000 . . no C16 H4A 3.0800 . 3_586 no H3A O3 2.6900 . 3_586 no H4A O4 2.8600 . 3_586 no H4A C16 3.0800 . 3_586 no H4A H16A 2.5200 . 3_586 no H8 C10 2.9500 . . no H8 Br1 2.9800 . 7_566 no H10A C8 3.0100 . 1_545 no H10A C8 3.0400 . . no H10B C8 2.8400 . . no H10B Br1 2.9700 . 7_566 no H11A C8 3.1000 . 1_545 no H11A C9 3.0400 . 1_545 no H11B H11C 2.4900 . 6_555 no H11C H11B 2.4900 . 6_545 no H11C Br1 3.0800 . 7_556 no H13 C15 2.8000 . . no H13 H15A 2.5100 . . no H15A C13 2.8100 . . no H15A H13 2.5100 . . no H15A O1 2.7900 . 4_575 no H15A O2 2.7900 . 4_575 no H15B N2 2.9200 . 1_565 no H15B C13 2.9500 . . no H15B C13 2.9600 . 1_565 no H16A C13 2.9700 . 1_565 no H16A C14 2.8800 . 1_565 no H16A H4A 2.5200 . 3_586 no H16B C5 3.0700 . 4_585 no H16C O2 2.6300 . 4_575 no H16C C7 3.0700 . 4_585 no _vrf_REFLT03_e029a ; PROBLEM: Reflection count < 85% complete RESPONSE: all examined crystals were twinned, therefore only the unaffected reflections of the major twin component were used for structure solution and structure refinement. ; _vrf_PLAT029_e029a ; PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.50 RESPONSE: all examined crystals were twinned, therefore only the unaffected reflections of the major twin component were used for structure solution and structure refinement. ; _vrf_PLAT088_e029a ; PROBLEM: Poor Data / Parameter Ratio ..... 7.78 RESPONSE: all examined crystals were twinned, therefore only the unaffected reflections of the major twin component were used for structure solution and structure refinement. ; #===END # Attachment '- 7c.cif' # CIF-file generated for Luo 0422 Luo/Reiser #============================================================================== data_e117 _database_code_depnum_ccdc_archive 'CCDC 817028' #TrackingRef '- 7c.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H13 Br N2 O5 Pt' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural 'C16 H13 Br N2 O5 Pt' _chemical_formula_sum 'C16 H13 Br N2 O5 Pt' _chemical_formula_iupac ? _chemical_formula_weight 588.26 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.6961(10) _cell_length_b 10.0725(10) _cell_length_c 10.4364(10) _cell_angle_alpha 107.818(11) _cell_angle_beta 111.729(11) _cell_angle_gamma 99.999(12) _cell_volume 852.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 26.85 _cell_special_details ; Cell parameters were determined by indexing 8000 reflections with I/sigma limit 6.0. ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow to orange' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.291 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 10.600 _exptl_crystal_density_meas_temp ? # Permitted for : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'numerical from crystal shape (X-SHAPE, X-RED. STOE, 1996)' _exptl_absorpt_correction_T_min 0.0539 _exptl_absorpt_correction_T_max 0.3258 loop_ _exptl_crystal_face_index_h_ _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.1034 0 0 -1 0.1090 1 0 0 0.2176 0 1 0 0.0544 0 -1 0 0.0739 -1 0 0 0.2777 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Data were collected applying an imaging plate system (STOE) with the following measurement parameters: Detector distance [mm] 65 Phi movement mode Oscillation Phi incr. [degrees] 1.2 Number of exposures 240 Irradiation / exposure [min] 1.00 For a detailed description of the method see: Sheldrick, G.M., Paulus, E. Vertesy, L. & Hahn, F. (1995) Acta Cryst. B51, 89-98. ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS diffractometer' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 10760 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.85 _diffrn_reflns_theta_full 26.85 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measured_fraction_theta_full 0.932 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 3422 # number of observed reflections (> n sig(I)) _reflns_number_gt 3092 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'STOE (1998)' _computing_cell_refinement 'STOE (1998)' _computing_data_reduction 'STOE (1998)' _computing_structure_solution 'SIR-97 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2, conventional R-factors R are based on F, with F set to zero for negative F^2. The observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3422 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.676 _refine_diff_density_min -1.521 _refine_diff_density_rms 0.231 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt Uani 0.75876(2) 0.44337(2) -0.04191(2) 1.000 0.0297(1) . . Br1 Br Uani 0.73364(7) 0.17338(5) -0.12068(6) 1.000 0.0472(2) . . O1 O Uani 0.9026(5) 0.7339(4) -0.2075(4) 1.000 0.0486(11) . . O2 O Uani 0.8697(5) 0.2548(4) -0.3215(4) 1.000 0.0523(11) . . O3 O Uani 0.9790(7) 0.3542(6) -0.4382(6) 1.000 0.0783(19) . . O4 O Uani 0.6134(4) 0.5522(4) 0.2846(4) 1.000 0.0418(10) . . O5 O Uani 0.5433(5) 0.3789(4) 0.3651(4) 1.000 0.0526(11) . . N1 N Uani 0.8442(4) 0.5327(4) -0.1654(4) 1.000 0.0345(10) . . N2 N Uani 0.6759(4) 0.4354(4) 0.1083(4) 1.000 0.0350(10) . . C1 C Uani 0.7567(5) 0.6435(5) 0.0366(5) 1.000 0.0348(12) . . C2 C Uani 0.7017(6) 0.6870(5) 0.1473(5) 1.000 0.0385(12) . . C3 C Uani 0.6928(7) 0.8268(5) 0.1973(6) 1.000 0.0491(16) . . C4 C Uani 0.7430(7) 0.9272(6) 0.1405(6) 1.000 0.0533(16) . . C5 C Uani 0.8011(7) 0.8896(5) 0.0374(6) 1.000 0.0475(16) . . C6 C Uani 0.8047(5) 0.7461(5) -0.0180(5) 1.000 0.0372(12) . . C7 C Uani 0.8521(5) 0.6725(5) -0.1287(5) 1.000 0.0372(12) . . C8 C Uani 0.9334(7) 0.6244(6) -0.2988(6) 1.000 0.0491(17) . . C9 C Uani 0.9003(6) 0.5010(6) -0.2757(5) 1.000 0.0407(14) . . C10 C Uani 0.9201(6) 0.3641(6) -0.3531(5) 1.000 0.0445(14) . . C11 C Uani 0.8818(8) 0.1144(6) -0.3940(7) 1.000 0.0590(19) . . C12 C Uani 0.6626(5) 0.5606(5) 0.1806(5) 1.000 0.0367(12) . . C13 C Uani 0.5947(6) 0.4094(5) 0.2711(5) 1.000 0.0417(14) . . C14 C Uani 0.6347(6) 0.3352(5) 0.1661(5) 1.000 0.0385(14) . . C15 C Uani 0.5253(7) 0.2298(6) 0.3533(6) 1.000 0.0463(16) . . C16 C Uani 0.4695(8) 0.2115(7) 0.4664(6) 1.000 0.0570(17) . . H3 H Uiso 0.65370 0.85590 0.26890 1.000 0.0590 calc R H4 H Uiso 0.73620 1.02350 0.17490 1.000 0.0640 calc R H5 H Uiso 0.83810 0.96010 0.00450 1.000 0.0570 calc R H8 H Uiso 0.97220 0.63460 -0.36780 1.000 0.0590 calc R H11A H Uiso 0.78750 0.05780 -0.49040 1.000 0.0710 calc R H11B H Uiso 0.89170 0.06030 -0.32910 1.000 0.0710 calc R H11C H Uiso 0.97440 0.12910 -0.41210 1.000 0.0710 calc R H14 H Uiso 0.63470 0.23610 0.13750 1.000 0.0460 calc R H15A H Uiso 0.62680 0.21110 0.37530 1.000 0.0560 calc R H15B H Uiso 0.44780 0.15890 0.25000 1.000 0.0560 calc R H16A H Uiso 0.54760 0.28140 0.56830 1.000 0.0680 calc R H16B H Uiso 0.45570 0.11070 0.46030 1.000 0.0680 calc R H16C H Uiso 0.36930 0.23060 0.44390 1.000 0.0680 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0337(1) 0.0259(1) 0.0303(1) 0.0122(1) 0.0146(1) 0.0097(1) Br1 0.0717(3) 0.0301(2) 0.0531(3) 0.0188(2) 0.0383(3) 0.0206(2) O1 0.058(2) 0.0458(19) 0.056(2) 0.0322(17) 0.0312(18) 0.0150(17) O2 0.068(2) 0.0437(19) 0.056(2) 0.0179(16) 0.042(2) 0.0155(18) O3 0.125(4) 0.077(3) 0.083(3) 0.043(3) 0.084(3) 0.044(3) O4 0.0521(19) 0.0366(16) 0.0403(16) 0.0117(13) 0.0284(15) 0.0127(15) O5 0.073(2) 0.049(2) 0.0513(19) 0.0216(16) 0.0433(19) 0.0183(19) N1 0.0354(18) 0.0361(18) 0.0333(17) 0.0168(15) 0.0159(15) 0.0090(16) N2 0.040(2) 0.0307(17) 0.0371(17) 0.0149(15) 0.0202(16) 0.0094(16) C1 0.037(2) 0.029(2) 0.037(2) 0.0145(17) 0.0149(18) 0.0095(18) C2 0.039(2) 0.035(2) 0.042(2) 0.0132(19) 0.0199(19) 0.0142(19) C3 0.062(3) 0.035(2) 0.051(3) 0.012(2) 0.029(3) 0.019(2) C4 0.065(3) 0.037(2) 0.058(3) 0.019(2) 0.024(3) 0.026(3) C5 0.053(3) 0.033(2) 0.056(3) 0.023(2) 0.020(2) 0.014(2) C6 0.038(2) 0.031(2) 0.043(2) 0.0204(18) 0.0147(19) 0.0102(19) C7 0.038(2) 0.036(2) 0.039(2) 0.0211(18) 0.0153(18) 0.0089(19) C8 0.053(3) 0.058(3) 0.050(3) 0.033(2) 0.028(2) 0.018(3) C9 0.039(2) 0.047(3) 0.035(2) 0.0176(19) 0.0166(19) 0.010(2) C10 0.042(2) 0.053(3) 0.035(2) 0.018(2) 0.0165(19) 0.009(2) C11 0.068(4) 0.045(3) 0.058(3) 0.010(2) 0.033(3) 0.014(3) C12 0.040(2) 0.034(2) 0.035(2) 0.0114(17) 0.0188(18) 0.0102(19) C13 0.051(3) 0.036(2) 0.041(2) 0.0159(19) 0.024(2) 0.013(2) C14 0.047(3) 0.037(2) 0.035(2) 0.0161(18) 0.0210(19) 0.013(2) C15 0.057(3) 0.045(3) 0.041(2) 0.021(2) 0.025(2) 0.013(2) C16 0.063(3) 0.064(3) 0.053(3) 0.030(3) 0.033(3) 0.014(3) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pt1 Br1 2.5267(6) . . yes Pt1 N1 2.097(4) . . yes Pt1 N2 2.024(4) . . yes Pt1 C1 1.937(5) . . yes O1 C7 1.343(7) . . yes O1 C8 1.377(8) . . yes O2 C10 1.309(8) . . yes O2 C11 1.433(8) . . yes O3 C10 1.211(9) . . yes O4 C12 1.356(6) . . yes O4 C13 1.374(7) . . yes O5 C13 1.341(7) . . yes O5 C15 1.443(8) . . yes N1 C7 1.321(7) . . yes N1 C9 1.422(7) . . yes N2 C12 1.312(7) . . yes N2 C14 1.398(7) . . yes C1 C2 1.428(7) . . no C1 C6 1.414(7) . . no C2 C3 1.374(8) . . no C2 C12 1.444(8) . . no C3 C4 1.422(9) . . no C4 C5 1.376(9) . . no C5 C6 1.395(8) . . no C6 C7 1.443(7) . . no C8 C9 1.345(9) . . no C9 C10 1.455(8) . . no C13 C14 1.351(8) . . no C15 C16 1.514(9) . . no C3 H3 0.9499 . . no C4 H4 0.9491 . . no C5 H5 0.9502 . . no C8 H8 0.9503 . . no C11 H11A 0.9798 . . no C11 H11B 0.9802 . . no C11 H11C 0.9799 . . no C14 H14 0.9503 . . no C15 H15A 0.9901 . . no C15 H15B 0.9897 . . no C16 H16A 0.9800 . . no C16 H16B 0.9797 . . no C16 H16C 0.9796 . . 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 Br1 Pt1 N1 110.67(11) . . . yes Br1 Pt1 N2 90.86(12) . . . yes Br1 Pt1 C1 169.95(15) . . . yes N1 Pt1 N2 158.47(16) . . . yes N1 Pt1 C1 79.17(19) . . . yes N2 Pt1 C1 79.30(19) . . . yes C7 O1 C8 104.9(4) . . . yes C10 O2 C11 118.3(5) . . . yes C12 O4 C13 104.2(4) . . . yes C13 O5 C15 113.4(5) . . . yes Pt1 N1 C7 111.0(3) . . . yes Pt1 N1 C9 144.0(4) . . . yes C7 N1 C9 105.1(4) . . . yes Pt1 N2 C12 113.8(3) . . . yes Pt1 N2 C14 138.3(3) . . . yes C12 N2 C14 107.8(4) . . . yes Pt1 C1 C2 119.9(4) . . . yes Pt1 C1 C6 120.6(4) . . . yes C2 C1 C6 119.5(5) . . . no C1 C2 C3 119.8(5) . . . no C1 C2 C12 106.7(5) . . . no C3 C2 C12 133.5(5) . . . no C2 C3 C4 119.1(6) . . . no C3 C4 C5 122.3(6) . . . no C4 C5 C6 118.8(5) . . . no C1 C6 C5 120.5(5) . . . no C1 C6 C7 107.6(4) . . . no C5 C6 C7 132.0(5) . . . no O1 C7 N1 113.3(4) . . . yes O1 C7 C6 125.0(5) . . . yes N1 C7 C6 121.7(5) . . . yes O1 C8 C9 109.8(5) . . . yes N1 C9 C8 106.9(5) . . . yes N1 C9 C10 128.8(5) . . . yes C8 C9 C10 124.4(5) . . . no O2 C10 O3 123.8(6) . . . yes O2 C10 C9 114.0(5) . . . yes O3 C10 C9 122.2(6) . . . yes O4 C12 N2 111.9(5) . . . yes O4 C12 C2 127.8(5) . . . yes N2 C12 C2 120.3(5) . . . yes O4 C13 O5 112.9(5) . . . yes O4 C13 C14 111.0(5) . . . yes O5 C13 C14 136.1(5) . . . yes N2 C14 C13 105.2(5) . . . yes O5 C15 C16 107.8(5) . . . yes C2 C3 H3 120.41 . . . no C4 C3 H3 120.49 . . . no C3 C4 H4 118.87 . . . no C5 C4 H4 118.86 . . . no C4 C5 H5 120.60 . . . no C6 C5 H5 120.60 . . . no O1 C8 H8 125.04 . . . no C9 C8 H8 125.15 . . . no O2 C11 H11A 109.44 . . . no O2 C11 H11B 109.48 . . . no O2 C11 H11C 109.49 . . . no H11A C11 H11B 109.47 . . . no H11A C11 H11C 109.46 . . . no H11B C11 H11C 109.50 . . . no N2 C14 H14 127.37 . . . no C13 C14 H14 127.44 . . . no O5 C15 H15A 110.14 . . . no O5 C15 H15B 110.18 . . . no C16 C15 H15A 110.14 . . . no C16 C15 H15B 110.14 . . . no H15A C15 H15B 108.47 . . . no C15 C16 H16A 109.45 . . . no C15 C16 H16B 109.44 . . . no C15 C16 H16C 109.49 . . . no H16A C16 H16B 109.43 . . . no H16A C16 H16C 109.48 . . . no H16B C16 H16C 109.54 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Pt1 N1 C7 177.7(3) . . . . no N2 Pt1 N1 C7 -0.5(6) . . . . no C1 Pt1 N1 C7 -0.2(3) . . . . no Br1 Pt1 N1 C9 -3.3(6) . . . . no N2 Pt1 N1 C9 178.5(5) . . . . no C1 Pt1 N1 C9 178.9(6) . . . . no Br1 Pt1 N2 C12 -178.1(3) . . . . no N1 Pt1 N2 C12 0.1(6) . . . . no C1 Pt1 N2 C12 -0.2(4) . . . . no Br1 Pt1 N2 C14 6.4(5) . . . . no N1 Pt1 N2 C14 -175.4(4) . . . . no C1 Pt1 N2 C14 -175.7(5) . . . . no N1 Pt1 C1 C2 178.9(4) . . . . no N2 Pt1 C1 C2 -1.2(4) . . . . no N1 Pt1 C1 C6 0.8(4) . . . . no N2 Pt1 C1 C6 -179.3(4) . . . . no C8 O1 C7 N1 -1.8(6) . . . . no C8 O1 C7 C6 -179.7(5) . . . . no C7 O1 C8 C9 0.7(6) . . . . no C11 O2 C10 C9 179.1(5) . . . . no C11 O2 C10 O3 -1.3(9) . . . . no C13 O4 C12 C2 -179.4(5) . . . . no C12 O4 C13 O5 -179.0(4) . . . . no C12 O4 C13 C14 1.5(6) . . . . no C13 O4 C12 N2 -0.7(5) . . . . no C15 O5 C13 C14 0.1(9) . . . . no C15 O5 C13 O4 -179.2(5) . . . . no C13 O5 C15 C16 179.2(5) . . . . no C9 N1 C7 C6 -179.9(4) . . . . no C7 N1 C9 C10 178.7(5) . . . . no C7 N1 C9 C8 -1.6(6) . . . . no Pt1 N1 C9 C8 179.3(4) . . . . no Pt1 N1 C7 C6 -0.5(6) . . . . no Pt1 N1 C7 O1 -178.5(3) . . . . no Pt1 N1 C9 C10 -0.4(9) . . . . no C9 N1 C7 O1 2.1(6) . . . . no C14 N2 C12 C2 178.4(5) . . . . no Pt1 N2 C12 C2 1.5(6) . . . . no Pt1 N2 C14 C13 177.0(4) . . . . no Pt1 N2 C12 O4 -177.3(3) . . . . no C12 N2 C14 C13 1.3(6) . . . . no C14 N2 C12 O4 -0.4(6) . . . . no Pt1 C1 C6 C5 179.2(4) . . . . no Pt1 C1 C2 C3 -176.7(4) . . . . no C6 C1 C2 C12 -179.8(4) . . . . no Pt1 C1 C6 C7 -1.2(6) . . . . no C2 C1 C6 C7 -179.3(4) . . . . no Pt1 C1 C2 C12 2.2(6) . . . . no C2 C1 C6 C5 1.1(8) . . . . no C6 C1 C2 C3 1.4(8) . . . . no C12 C2 C3 C4 179.7(6) . . . . no C1 C2 C12 N2 -2.4(7) . . . . no C1 C2 C3 C4 -1.8(8) . . . . no C3 C2 C12 O4 -5.1(10) . . . . no C3 C2 C12 N2 176.3(6) . . . . no C1 C2 C12 O4 176.3(5) . . . . no C2 C3 C4 C5 -0.3(9) . . . . no C3 C4 C5 C6 2.8(9) . . . . no C4 C5 C6 C7 177.4(6) . . . . no C4 C5 C6 C1 -3.1(8) . . . . no C1 C6 C7 N1 1.1(6) . . . . no C5 C6 C7 O1 -1.7(9) . . . . no C1 C6 C7 O1 178.8(5) . . . . no C5 C6 C7 N1 -179.4(6) . . . . no O1 C8 C9 C10 -179.7(5) . . . . no O1 C8 C9 N1 0.6(6) . . . . no C8 C9 C10 O2 -175.2(5) . . . . no N1 C9 C10 O3 -175.1(6) . . . . no N1 C9 C10 O2 4.5(8) . . . . no C8 C9 C10 O3 5.2(9) . . . . no O5 C13 C14 N2 179.0(6) . . . . no O4 C13 C14 N2 -1.8(6) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt1 O2 3.595(4) . . no Pt1 C7 4.074(5) . 2_765 no Pt1 Pt1 4.2963(5) . 2_765 no Pt1 O2 3.953(4) . 2_765 no Pt1 O4 3.577(4) . 2_665 no Pt1 N1 3.571(4) . 2_765 no Pt1 C2 4.039(6) . 2_665 no Pt1 C3 4.136(7) . 2_665 no Pt1 C10 3.736(5) . 2_765 no Pt1 C8 4.044(6) . 2_765 no Pt1 C9 3.512(5) . 2_765 no Pt1 C12 3.784(5) . 2_665 no Pt1 C13 4.187(6) . 2_665 no Pt1 H16A 3.4661 . 1_554 no Br1 O2 3.087(4) . . no Br1 N2 3.261(4) . . no Br1 C5 3.749(6) . 1_545 no Br1 C11 3.584(7) . . no Br1 C14 3.496(5) . . no Br1 C7 3.597(5) . 2_765 no Br1 H11B 3.1521 . . no Br1 H14 3.1084 . . no Br1 H5 2.9734 . 1_545 no Br1 H15B 3.0905 . 2_655 no O2 Pt1 3.595(4) . . no O2 Br1 3.087(4) . . no O2 N1 2.881(6) . . no O2 Pt1 3.953(4) . 2_765 no O3 C12 3.267(8) . 2_765 no O3 C8 3.214(9) . 2_764 no O4 C16 3.390(8) . 2_666 no O4 Pt1 3.577(4) . 2_665 no O3 H11C 2.3598 . . no O3 H8 2.2730 . 2_764 no O3 H8 2.7114 . . no N1 O2 2.881(6) . . no N1 C1 2.574(6) . . no N1 C6 2.415(7) . . no N1 Pt1 3.571(4) . 2_765 no N2 Br1 3.261(4) . . no N2 C1 2.528(7) . . no N2 C2 2.393(7) . . no N2 C2 3.351(7) . 2_665 no C1 N1 2.574(6) . . no C1 N2 2.528(7) . . no C1 C7 2.305(7) . . no C1 C12 2.304(7) . . no C1 C13 3.525(7) . 2_665 no C2 Pt1 4.039(6) . 2_665 no C2 N2 3.351(7) . 2_665 no C2 C14 3.576(7) . 2_665 no C3 C14 3.553(7) . 2_665 no C3 Pt1 4.136(7) . 2_665 no C5 Br1 3.749(6) . 1_565 no C6 C13 3.495(7) . 2_665 no C7 Pt1 4.074(5) . 2_765 no C7 Br1 3.597(5) . 2_765 no C8 O3 3.214(9) . 2_764 no C8 Pt1 4.044(6) . 2_765 no C9 Pt1 3.512(5) . 2_765 no C10 C12 3.591(8) . 2_765 no C10 Pt1 3.736(5) . 2_765 no C10 C15 3.585(8) . 1_554 no C11 Br1 3.584(7) . . no C12 C12 3.562(7) . 2_665 no C12 O3 3.267(8) . 2_765 no C12 Pt1 3.784(5) . 2_665 no C12 C10 3.591(8) . 2_765 no C13 C1 3.525(7) . 2_665 no C13 Pt1 4.187(6) . 2_665 no C13 C6 3.495(7) . 2_665 no C14 C3 3.553(7) . 2_665 no C14 C2 3.576(7) . 2_665 no C15 C10 3.585(8) . 1_556 no C16 O4 3.390(8) . 2_666 no C2 H11C 3.0581 . 2_765 no C3 H11C 3.0285 . 2_765 no C3 H11A 3.0465 . 1_566 no C5 H15B 2.8972 . 2_665 no C10 H15A 2.8867 . 1_554 no C14 H15B 2.8659 . . no C14 H15A 2.8453 . . no C15 H14 2.8345 . . no H3 H11A 2.3819 . 1_566 no H4 H14 2.5818 . 1_565 no H5 Br1 2.9734 . 1_565 no H8 O3 2.7114 . . no H8 O3 2.2730 . 2_764 no H11A C3 3.0465 . 1_544 no H11A H3 2.3819 . 1_544 no H11B Br1 3.1521 . . no H11C O3 2.3598 . . no H11C C2 3.0582 . 2_765 no H11C C3 3.0285 . 2_765 no H14 Br1 3.1084 . . no H14 C15 2.8345 . . no H14 H4 2.5818 . 1_545 no H14 H15A 2.5971 . . no H15A C10 2.8867 . 1_556 no H15A C14 2.8453 . . no H15A H14 2.5971 . . no H15B C14 2.8659 . . no H15B Br1 3.0905 . 2_655 no H15B C5 2.8972 . 2_665 no H16A Pt1 3.4661 . 1_556 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C8 H8 O3 0.9500 2.2700 3.214(9) 170.00 2_764 yes _vrf_PLAT029_e117 ; PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.93 RESPONSE:There is a missing cusp of data due to data collection by rotation around the spindle axis only. ; #===END