Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm #============================================================================= # PROCESSING SUMMARY _journal_coden_Cambridge 1350 _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Daniel M. Toebbens' _publ_contact_author_address ;University of Innsbruck Institute of Mineralogy and Crystallography Innrain 52 A-6020 Innsbruck Austria ; _publ_contact_author_email daniel.toebbens@uibk.ac.at _publ_contact_author_phone +435125075532 _publ_requested_coeditor_name ? _publ_requested_category ? # Definition of non standard CIF items (Reliability indices used in FULLPROF) loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_info _publ_manuscript_incl_extra_defn # Name Explanation Standard? # ------ ----------- --------- '_pd_proc_ls_prof_cR_factor' 'Prof. R-factor CORRECTED for background' no '_pd_proc_ls_prof_cwR_factor' 'wProf.R-factor CORRECTED for background' no '_pd_proc_ls_prof_cwR_expected' 'wProf.Expected CORRECTED for background' no '_pd_proc_ls_prof_chi2' 'Chi-square for all considered points' no '_pd_proc_ls_prof_echi2' 'Chi-2 for points with Bragg contribution' no #============================================================================= # 3. TITLE AND AUTHOR LIST # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address D.M.Toebbens ;University of Innsbruck Institute of Mineralogy and Petrography Innrain 52 A-6020 Innsbruck Austria ; M.Hummel ;University of Innsbruck Institute of General, Inorganic and Theoretical Chemistry Innrain 52a A-6020 Innsbruck Austria ; R.Kaindl ;University of Innsbruck Institute of Mineralogy and Petrography Innrain 52 A-6020 Innsbruck Austria ; H.Schottenberger ;University of Innsbruck Institute of General, Inorganic and Theoretical Chemistry Innrain 52a A-6020 Innsbruck Austria ; V.Kahlenberg ;University of Innsbruck Institute of Mineralogy and Petrography Innrain 52 A-6020 Innsbruck Austria ; #============================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep # Details of the preparation of the sample(s) # should be given here. ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================= #============================================================================= # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_Mg[acacac]2 _database_code_depnum_ccdc_archive 'CCDC 657357' #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; 'bis(3-acetyl-2,4-pentandionato-O2,O3)magnesium(II)' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Mg O6' # 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 'C14 H18 Mg O6' _chemical_formula_iupac ? _chemical_formula_weight 306.59 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source mg 5.42040 2.82750 2.17350 79.26110 1.22690 0.38080 2.30730 7.19370 0.85840 0.16500 0.17700 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/A' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z -x+1/2,y+1/2,-z -x,-y,-z x+1/2,-y+1/2,z _cell_length_a 8.31089(9) _cell_length_b 12.15064(12) _cell_length_c 8.06761(9) _cell_angle_alpha 90.00000 _cell_angle_beta 106.7228(8) _cell_angle_gamma 90.00000 _cell_volume 780.233(14) _cell_formula_units_Z 2 _cell_measurement_temperature 297(1) _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour white # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; 'external standard' ; _diffrn_ambient_temperature 297 _diffrn_source 'sealed X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_source_target Cu _diffrn_radiation_monochromator 'curved Ge(111)' _diffrn_measurement_device_type 'STOE STADI MP' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector 'linear PSD' _diffrn_detector_type STOE # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 11795 _pd_meas_2theta_range_min 2.06000 _pd_meas_2theta_range_max 120.00000 _pd_meas_2theta_range_inc 0.010001 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function TCH-Pseudo-Voigt _pd_proc_ls_background_function 'linear interpolation' _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 3.0871 _pd_proc_ls_prof_wR_factor 4.1182 _pd_proc_ls_prof_wR_expected 3.8105 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 18.3533 _pd_proc_ls_prof_cwR_factor 13.9841 _pd_proc_ls_prof_cwR_expected 12.9394 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 1.1680 _pd_proc_ls_prof_echi2 1.1953 # Items related to LS refinement _refine_ls_R_I_factor 4.2413 _refine_ls_number_reflns 1224 _refine_ls_number_parameters 67 _refine_ls_number_restraints 21 _refine_ls_shift/su_max 0.05 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0842 _pd_proc_2theta_range_max 120.0242 _pd_proc_2theta_range_inc 0.010001 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution EXPO2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. 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_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Mg 0.50000 0.50000 0.00000 0.0319(16) 1.00000 Uiso Mg O1 0.3958(6) 0.4878(3) 0.2029(6) 0.0409(9) 1.00000 Uiso O O2 0.2807(6) 0.4329(3) -0.1337(6) 0.0409(9) 1.00000 Uiso O O3 0.0936(6) 0.1612(4) 0.0412(6) 0.0409(9) 1.00000 Uiso O C1 0.2546(7) 0.4278(6) 0.3932(6) 0.0409(9) 1.00000 Uiso C H1a 0.1717(7) 0.3622(6) 0.4084(6) 0.0409(9) 1.00000 Uiso H H1b 0.3685(7) 0.4259(6) 0.5004(6) 0.0409(9) 1.00000 Uiso H H1c 0.1926(7) 0.5063(6) 0.3912(6) 0.0409(9) 1.00000 Uiso H C2 0.2984(8) 0.4121(5) 0.2247(6) 0.0409(9) 1.00000 Uiso C C3 0.2221(9) 0.3346(4) 0.0931(5) 0.0409(9) 1.00000 Uiso C C4 0.1965(8) 0.3598(6) -0.0830(5) 0.0409(9) 1.00000 Uiso C C5 0.0654(7) 0.2980(5) -0.2223(7) 0.0409(9) 1.00000 Uiso C H5a 0.0028(7) 0.2385(5) -0.1623(7) 0.0409(9) 1.00000 Uiso H H5b 0.1261(7) 0.2558(5) -0.3063(7) 0.0409(9) 1.00000 Uiso H H5c -0.0261(7) 0.3557(5) -0.2976(7) 0.0409(9) 1.00000 Uiso H C6 0.1869(10) 0.2226(4) 0.1441(6) 0.0409(9) 1.00000 Uiso C C7 0.2526(8) 0.1772(5) 0.3284(6) 0.0409(9) 1.00000 Uiso C H7a 0.3341(8) 0.2375(5) 0.4102(6) 0.0409(9) 1.00000 Uiso H H7b 0.1477(8) 0.1599(5) 0.3787(6) 0.0409(9) 1.00000 Uiso H H7c 0.3224(8) 0.1022(5) 0.3267(6) 0.0409(9) 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds 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 Mg O1 2.0657 . . yes Mg O2 2.0047 . . yes Mg O3 2.0984 . 2_555 yes Mg O1 2.0657 . 3_665 yes Mg O2 2.0047 . 3_665 yes Mg O3 2.0984 . 4_555 yes O1 C2 1.2705 . . yes O2 C4 1.2691 . . yes O3 C6 1.2151 . . yes C1 C2 1.5171 . . no C2 C3 1.4243 . . no C3 C4 1.4084 . . no C3 C6 1.4752 . . no C4 C5 1.5196 . . no C6 C7 1.5317 . . no C1 H1A 1.0834 . . no C1 H1B 1.0832 . . no C1 H1C 1.0820 . . no C5 H5A 1.0829 . . no C5 H5B 1.0832 . . no C5 H5C 1.0830 . . no C7 H7A 1.0835 . . no C7 H7B 1.0828 . . no C7 H7C 1.0825 . . 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 O1 Mg O2 82.74 . . . yes O1 Mg O3 88.38 . . 2_555 yes O1 Mg O1 180.00 . . 3_665 yes O1 Mg O2 97.26 . . 3_665 yes O1 Mg O3 91.62 . . 4_555 yes O2 Mg O3 93.22 . . 2_555 yes O1 Mg O2 97.26 3_665 . . yes O2 Mg O2 180.00 . . 3_665 yes O2 Mg O3 86.78 . . 4_555 yes O1 Mg O3 91.62 3_665 . 2_555 yes O2 Mg O3 86.78 3_665 . 2_555 yes O3 Mg O3 180.00 2_555 . 4_555 yes O1 Mg O2 82.74 3_665 . 3_665 yes O1 Mg O3 88.38 3_665 . 4_555 yes O2 Mg O3 93.22 3_665 . 4_555 yes Mg O1 C2 126.21 . . . yes Mg O2 C4 127.70 . . . yes Mg O3 C6 144.68 2_545 . . yes O1 C2 C1 111.08 . . . yes O1 C2 C3 122.70 . . . yes C1 C2 C3 125.51 . . . no C2 C3 C4 120.92 . . . no C2 C3 C6 118.91 . . . no C4 C3 C6 119.83 . . . no O2 C4 C3 122.69 . . . yes O2 C4 C5 116.87 . . . yes C3 C4 C5 120.44 . . . no O3 C6 C3 120.97 . . . yes O3 C6 C7 114.91 . . . yes C3 C6 C7 123.99 . . . no C2 C1 H1A 109.47 . . . no C2 C1 H1B 109.44 . . . no C2 C1 H1C 109.48 . . . no H1A C1 H1B 109.39 . . . no H1A C1 H1C 109.55 . . . no H1B C1 H1C 109.49 . . . no C4 C5 H5A 109.50 . . . no C4 C5 H5B 109.43 . . . no C4 C5 H5C 109.46 . . . no H5A C5 H5B 109.50 . . . no H5A C5 H5C 109.44 . . . no H5B C5 H5C 109.50 . . . no C6 C7 H7A 109.48 . . . no C6 C7 H7B 109.46 . . . no C6 C7 H7C 109.48 . . . no H7A C7 H7B 109.43 . . . no H7A C7 H7C 109.49 . . . no H7B C7 H7C 109.48 . . . 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 C2 C3 C6 O3 165.33 . . . . no C2 C3 C6 C7 -10.45 . . . . no C4 C3 C6 O3 -21.27 . . . . no C4 C3 C6 C7 162.95 . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #============================================================================= # Additional structures (last six sections and associated data_? identifiers) # may be added at this point. #============================================================================= # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # Attachment 'Pd[acacac]2.cif' #============================================================================= #============================================================================= # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_Pd[acacac]2 _database_code_depnum_ccdc_archive 'CCDC 657358' #============================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; 'bis(3-acetyl-2,4-pentandionato-O2,O3)palladium(II)' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 O6 Pd' # 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 'C14 H18 O6 Pd' _chemical_formula_iupac ? _chemical_formula_weight 388.70 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source pd 19.33190 0.69866 15.50170 7.98929 5.29537 25.20520 0.60584 76.89860 5.26593 -0.05900 3.93400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 h 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P B C A' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz #<--must include 'x,y,z' x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 -x,-y,-z -x+1/2,y+1/2,z x,-y+1/2,z+1/2 x+1/2,y,-z+1/2 _cell_length_a 13.39752(15) _cell_length_b 13.43165(8) _cell_length_c 8.49767(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 1529.16(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour white # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; 'external standard' ; _diffrn_ambient_temperature 296 _diffrn_source 'sealed X-ray tube' _diffrn_radiation_type 'Cu K\a' _diffrn_source_target Cu _diffrn_radiation_monochromator 'curved Ge(111)' _diffrn_measurement_device_type 'STOE STADI MP' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? # Not in version 2.0.1 _diffrn_detector 'linear PSD' _diffrn_detector_type STOE # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 12794 _pd_meas_2theta_range_min 2.06000 _pd_meas_2theta_range_max 129.99001 _pd_meas_2theta_range_inc 0.010001 #============================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function ? _pd_proc_ls_background_function ? _pd_proc_ls_pref_orient_corr ; ? ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 5.5913 _pd_proc_ls_prof_wR_factor 7.1901 _pd_proc_ls_prof_wR_expected 6.3130 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 17.1073 _pd_proc_ls_prof_cwR_factor 15.2119 _pd_proc_ls_prof_cwR_expected 13.3563 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 1.2972 _pd_proc_ls_prof_echi2 1.3257 # Items related to LS refinement _refine_ls_R_I_factor 3.8205 _refine_ls_number_reflns 1349 _refine_ls_number_parameters 79 _refine_ls_number_restraints 21 _refine_ls_shift/su_max 0.05 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0657 _pd_proc_2theta_range_max 129.9957 _pd_proc_2theta_range_inc 0.010001 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution FOX _computing_structure_refinement FULLPROF _computing_molecular_graphics ? _computing_publication_material ? #============================================================================= # 9. 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_occupancy _atom_site_adp_type # Not in version 2.0.1 _atom_site_type_symbol Pd 0.00000 0.00000 0.00000 0.0267(3) 1.00000 Uiso Pd C1 0.2153(7) -0.0155(8) -0.3701(11) 0.0378(11) 1.00000 Uiso C C2 0.1272(7) 0.0224(7) -0.2760(9) 0.0378(11) 1.00000 Uiso C C3 0.0664(6) 0.0983(6) -0.3349(8) 0.0378(11) 1.00000 Uiso C C4 -0.0191(6) 0.1350(6) -0.2601(8) 0.0378(11) 1.00000 Uiso C C5 -0.0714(9) 0.2213(5) -0.3359(11) 0.0378(11) 1.00000 Uiso C C6 0.0968(8) 0.1505(6) -0.4826(5) 0.0378(11) 1.00000 Uiso C C7 0.1618(7) 0.2413(4) -0.4792(17) 0.0378(11) 1.00000 Uiso C O1 0.1116(8) -0.0285(5) -0.1513(7) 0.0378(11) 1.00000 Uiso O O2 -0.0584(7) 0.1048(5) -0.1327(6) 0.0378(11) 1.00000 Uiso O O3 0.0684(8) 0.1229(5) -0.6108(6) 0.0378(11) 1.00000 Uiso O H1a 0.2250(7) 0.0301(8) -0.4739(11) 0.36(3) 1.00000 Uiso H H1b 0.2821(7) -0.0120(8) -0.2985(11) 0.36(3) 1.00000 Uiso H H1c 0.2018(7) -0.0919(8) -0.4050(11) 0.36(3) 1.00000 Uiso H H5a -0.0328(9) 0.2416(5) -0.4432(11) 0.36(3) 1.00000 Uiso H H5b -0.1476(9) 0.2004(5) -0.3634(11) 0.36(3) 1.00000 Uiso H H5c -0.0717(9) 0.2840(5) -0.2559(11) 0.36(3) 1.00000 Uiso H H7a 0.1820(7) 0.2581(4) -0.3587(17) 0.36(3) 1.00000 Uiso H H7b 0.1216(7) 0.3037(4) -0.5292(17) 0.36(3) 1.00000 Uiso H H7c 0.2287(7) 0.2276(4) -0.5473(17) 0.36(3) 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds 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 Pd O1 2.0087 . . yes Pd O2 1.9660 . . yes Pd O1 2.0087 . 5_566 yes Pd O2 1.9660 . 5_566 yes O1 C2 1.2783 . . yes O2 C4 1.2704 . . yes O3 C6 1.2120 . . yes C1 C2 1.5138 . . no C2 C3 1.3976 . . no C3 C4 1.3997 . . no C3 C6 1.4942 . . no C4 C5 1.4998 . . no C6 C7 1.4989 . . no C1 H1A 1.0817 . . no C1 H1B 1.0832 . . no C1 H1C 1.0834 . . no C5 H5A 1.0831 . . no C5 H5B 1.0843 . . no C5 H5C 1.0823 . . no C7 H7A 1.0829 . . no C7 H7B 1.0831 . . no C7 H7C 1.0826 . . 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 O1 Pd O2 93.76 . . . yes O1 Pd O1 180.00 . . 5_566 yes O1 Pd O2 86.24 . . 5_566 yes O1 Pd O2 86.24 5_566 . . yes O2 Pd O2 180.00 . . 5_566 yes O1 Pd O2 93.76 5_566 . 5_566 yes Pd O1 C2 123.39 . . . yes Pd O2 C4 123.54 . . . yes O1 C2 C1 112.68 . . . yes O1 C2 C3 126.28 . . . yes C1 C2 C3 120.70 . . . no C2 C3 C4 124.84 . . . no C2 C3 C6 118.96 . . . no C4 C3 C6 116.06 . . . no O2 C4 C3 127.86 . . . yes O2 C4 C5 114.78 . . . yes C3 C4 C5 117.35 . . . no O3 C6 C3 121.73 . . . yes O3 C6 C7 116.65 . . . yes C3 C6 C7 121.60 . . . no C2 C1 H1A 109.51 . . . no C2 C1 H1B 109.44 . . . no C2 C1 H1C 109.45 . . . no H1A C1 H1B 109.52 . . . no H1A C1 H1C 109.46 . . . no H1B C1 H1C 109.44 . . . no C4 C5 H5A 109.45 . . . no C4 C5 H5B 109.41 . . . no C4 C5 H5C 109.47 . . . no H5A C5 H5B 109.47 . . . no H5A C5 H5C 109.55 . . . no H5B C5 H5C 109.47 . . . no C6 C7 H7A 109.45 . . . no C6 C7 H7B 109.46 . . . no C6 C7 H7C 109.41 . . . no H7A C7 H7B 109.51 . . . no H7A C7 H7C 109.51 . . . no H7B C7 H7C 109.48 . . . 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 C2 C3 C6 O3 -92.09 . . . . no C2 C3 C6 C7 89.56 . . . . no C4 C3 C6 O3 92.10 . . . . no C4 C3 C6 C7 -86.25 . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ?