data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Jorge A. R. Navarro' _publ_contact_author_address ; Department of Inorganic Chemistry Universidad de Granada Av. Fuentenueva S/N Granada 18071 SPAIN ; _publ_contact_author_email JARN@UGR.ES _publ_section_title ; Borderline Microporous-Ultramicroporous Palladium(II) Coordination Polymers. Effect of Pore Functionalization on Gas Adsorption Properties ; loop_ _publ_author_name 'Jorge A. R. Navarro' 'Conchi O. Ania' 'Elisa Barea' 'Simona Galli' 'Norberto Masiocchi' 'Jose B. Parra' ; J.M.Salas ; 'Angelo Sironi' #data_Compound_1 data_1 _database_code_depnum_ccdc_archive 'CCDC 629501' _chemical_name_systematic ; catena-bis(5-fluoro-pyrimidin-2-olate)-pd(ii) bisaquo ; _chemical_name_common 'catena-bis(5-fluoro-pyrimidin-2-olate)-pd(ii) bisaquo' _chemical_formula_moiety C8H8F2N4O4Pd1 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum C8H8F2N4O4Pd1 _chemical_formula_weight 368.59 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description # _atom_type_scat_dispersion_real # _atom_type_scat_dispersion_imag _atom_type_scat_source C C 'International Tables for Crystallography (Vol. IV)' H H 'International Tables for Crystallography (Vol. IV)' F F 'International Tables for Crystallography (Vol. IV)' N N 'International Tables for Crystallography (Vol. IV)' O O 'International Tables for Crystallography (Vol. IV)' Pd Pd 'International Tables for Crystallography (Vol. IV)' #============================================================================== # 1.5. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3m _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x, -z, -y' '-x, z+1/2, y+1/2' '-x, y+1/2, z+1/2' '-x+1/2, -y+1/2, z' '-x+1/2, -z+1/2, y' '-x+1/2, z, -y+1/2' '-x+1/2, y, -z+1/2' '-y, -x, -z' '-y, -z, -x' '-y, z+1/2, x+1/2' '-y, x+1/2, z+1/2' '-y+1/2, -x+1/2, z' '-y+1/2, -z+1/2, x' '-y+1/2, z, -x+1/2' '-y+1/2, x, -z+1/2' '-z, -x, -y' '-z, -y, -x' '-z, y+1/2, x+1/2' '-z, x+1/2, y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, -y+1/2, x' '-z+1/2, y, -x+1/2' '-z+1/2, x, -y+1/2' 'z, -x+1/2, -y+1/2' 'z, -y+1/2, -x+1/2' 'z, y, x' 'z, x, y' 'z+1/2, -x, y+1/2' 'z+1/2, -y, x+1/2' 'z+1/2, y+1/2, -x' 'z+1/2, x+1/2, -y' 'y, -x+1/2, -z+1/2' 'y, -z+1/2, -x+1/2' 'y, z, x' 'y, x, z' 'y+1/2, -x, z+1/2' 'y+1/2, -z, x+1/2' 'y+1/2, z+1/2, -x' 'y+1/2, x+1/2, -z' 'x, -y+1/2, -z+1/2' 'x, -z+1/2, -y+1/2' 'x, z, y' 'x, y, z' 'x+1/2, -y, z+1/2' 'x+1/2, -z, y+1/2' 'x+1/2, z+1/2, -y' 'x+1/2, y+1/2, -z' _cell_length_a 16.31134(85) _cell_length_b 16.31134(85) _cell_length_c 16.31134(85) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4339.79(68) _cell_formula_units_Z 12 _cell_measurement_temperature 298 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 20 # parallel to # scattering vector # in transmission _pd_spec_size_thick 0.2 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour yellow # use ICDD colour descriptions # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # 1.6. EXPERIMENTAL DATA _exptl_special_details ; ? ; # This 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 ; ? ; _diffrn_ambient_temperature 298 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_detector scintillator _diffrn_detector_type ? _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a~1~ 1.54056 CuK\a~2~ 1.54439 _diffrn_radiation_monochromator 'HOPG Graphite' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5001 _pd_meas_2theta_range_min 5 _pd_meas_2theta_range_max 105 _pd_meas_2theta_range_inc 0.02 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'D8 software (Bruker AXS, Anno@@@@@@@@@@@)' _computing_cell_refinement TOPAS-R _computing_data_reduction TOPAS-R _computing_structure_solution TOPAS-R _computing_structure_refinement TOPAS-R _computing_molecular_graphics ? _computing_publication_material TOPAS-R #============================================================================== # 1.7. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The use of a rigid body description for the 5-fluoro-pyrimidin-2-olate ligand does not allow the derivation of statistically meaningful s.u.'s for its atoms. Only center of mass and rotational angles s.u.'s are available: XYZ 0.8431(5), 0.1468(3), 0.3532(3) RX, RY, RZ -11.6(2), 227.5(2), 313.8(2) for the rigid body described by: point_for_site N1 ux = r ; uy 0.00000 uz 0.00000 point_for_site C2 ux = -r ; uy 0.00000 uz 0.00000 point_for_site C3 ux = 0.5 r ; uy = 0.866 r ; uz 0.00000 point_for_site C4 ux = 0.5 r ; uy = -0.866 r ; uz 0.00000 point_for_site C5 ux = -0.5 r ; uy = 0.866 r ; uz 0.00000 point_for_site N6 ux = -0.5 r ; uy = -0.866 r ; uz 0.00000 point_for_site O1 ux = 0.5 (r+ro) ; uy = -0.866 (r+ro); uz 0.00000 point_for_site H2 ux = - (r+rh) ; uy 0.00000 uz 0.00000 point_for_site H3 ux = 0.5 (r+rh); uy = 0.866 (r+rh); uz 0.00000 point_for_site F1 ux = -0.5 (r+rf); uy = 0.866 (r+rf); uz 0.00000 r = 1.35 ro = 1.25 rh = 0.95 rf = 1.35 ; # The next three items are given as text _pd_proc_ls_profile_function 'fundamental parameters' _pd_proc_ls_background_function polynomial _pd_proc_ls_pref_orient_corr ? _pd_proc_ls_prof_R_factor 0.116 _pd_proc_ls_prof_wR_factor 0.149 _pd_proc_ls_prof_wR_expected 0.087 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 1/[Y~i~] _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 11 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? # The following item is 'CHI squared' _refine_ls_goodness_of_fit_all 1.712 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # 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 5 _pd_proc_2theta_range_max 105 _pd_proc_2theta_range_inc 0.02 loop_ _pd_proc_wavelength 1.540562 1.544390 _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 ? #============================================================================== # 1.8. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv Pd Pd 12 0.75 0.25 0.5 1 4.98(11) N1 N 48 0.8044496 0.1870711 0.4143074 1 6.98(11) C2 C 48 0.8818304 0.1065089 0.2921526 1 6.98(11) C3 C 48 0.8818159 0.2078632 0.3935276 1 6.98(11) C4 C 48 0.7657736 0.1259979 0.3740097 1 6.98(11) C5 C 48 0.9205064 0.1675821 0.3324503 1 6.98(11) N6 N 48 0.8044641 0.08571681 0.3129324 1 6.98(11) O1 O 48 0.6941381 0.106746 0.3932503 1 6.98(11) H2 H 48 0.909057 0.07816293 0.2491722 1 6.98(11) H3 H 48 0.9090323 0.2508406 0.4218852 1 6.98(11) F1 F 48 0.9978727 0.1883742 0.3116705 1 6.98(11) O1w O 24 0.9669(16) 0.6377(12) 0.6377(12) 1 6.98(11) O2w O 24 0.9029(13) 0.5020(13) 0.5020(13) 1 6.98(11) #============================================================================== #data_Compound_2 data_2 _database_code_depnum_ccdc_archive 'CCDC 629502' _chemical_name_systematic ; catena-bis(5-fluoro-pyrimidin-2-olate)-pd(ii) ; _chemical_name_common catena-bis(5-fluoro-pyrimidin-2-olate)-pd(ii) _chemical_formula_moiety C8H4F2N4O2Pd1 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum C8H4F2N4O2Pd1 _chemical_formula_weight 332.56 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description # _atom_type_scat_dispersion_real # _atom_type_scat_dispersion_imag _atom_type_scat_source C C 'International Tables for Crystallography (Vol. IV)' H H 'International Tables for Crystallography (Vol. IV)' F F 'International Tables for Crystallography (Vol. IV)' N N 'International Tables for Crystallography (Vol. IV)' O O 'International Tables for Crystallography (Vol. IV)' Pd Pd 'International Tables for Crystallography (Vol. IV)' #============================================================================== # 1.5. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3m _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x, -z, -y' '-x, z+1/2, y+1/2' '-x, y+1/2, z+1/2' '-x+1/2, -y+1/2, z' '-x+1/2, -z+1/2, y' '-x+1/2, z, -y+1/2' '-x+1/2, y, -z+1/2' '-y, -x, -z' '-y, -z, -x' '-y, z+1/2, x+1/2' '-y, x+1/2, z+1/2' '-y+1/2, -x+1/2, z' '-y+1/2, -z+1/2, x' '-y+1/2, z, -x+1/2' '-y+1/2, x, -z+1/2' '-z, -x, -y' '-z, -y, -x' '-z, y+1/2, x+1/2' '-z, x+1/2, y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, -y+1/2, x' '-z+1/2, y, -x+1/2' '-z+1/2, x, -y+1/2' 'z, -x+1/2, -y+1/2' 'z, -y+1/2, -x+1/2' 'z, y, x' 'z, x, y' 'z+1/2, -x, y+1/2' 'z+1/2, -y, x+1/2' 'z+1/2, y+1/2, -x' 'z+1/2, x+1/2, -y' 'y, -x+1/2, -z+1/2' 'y, -z+1/2, -x+1/2' 'y, z, x' 'y, x, z' 'y+1/2, -x, z+1/2' 'y+1/2, -z, x+1/2' 'y+1/2, z+1/2, -x' 'y+1/2, x+1/2, -z' 'x, -y+1/2, -z+1/2' 'x, -z+1/2, -y+1/2' 'x, z, y' 'x, y, z' 'x+1/2, -y, z+1/2' 'x+1/2, -z, y+1/2' 'x+1/2, z+1/2, -y' 'x+1/2, y+1/2, -z' _cell_length_a 16.29569(84) _cell_length_b 16.29569(84) _cell_length_c 16.29569(84) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4327.31(67) _cell_formula_units_Z 12 _cell_measurement_temperature 400 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 15 # perpendicular to # equatorial plane _pd_spec_size_equat 20 # parallel to # scattering vector # in transmission _pd_spec_size_thick 0.2 # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting ; packed powder pellet ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder', # 'flat_sheet' or 'irregular' _pd_char_particle_morphology plate-like _pd_char_colour yellow # use ICDD colour descriptions # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================================== # 1.6. EXPERIMENTAL DATA _exptl_special_details ; ? ; # This 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 ; ? ; _diffrn_ambient_temperature 400 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker AXS D8 Advance' _diffrn_detector 'Linear position sensitive' _diffrn_detector_type ? _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. loop_ _diffrn_radiation_type _diffrn_radiation_wavelength CuK\a~1~ 1.54056 CuK\a~2~ 1.54439 _diffrn_radiation_monochromator none # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5001 _pd_meas_2theta_range_min 5 _pd_meas_2theta_range_max 105 _pd_meas_2theta_range_inc 0.02 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? # The following fields are used to identify the programs used. _computing_data_collection 'D8 software (Bruker AXS)' _computing_cell_refinement TOPAS-R _computing_data_reduction TOPAS-R _computing_structure_solution TOPAS-R _computing_structure_refinement TOPAS-R _computing_molecular_graphics ? _computing_publication_material TOPAS-R #============================================================================== # 1.7. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; The use of a rigid body description for the 5-fluoro-pyrimidin-2-olate ligand does not allow the derivation of statistically meaningful s.u.'s for its atoms. Only center of mass and rotational angles s.u.'s are available: XYZ 0.8494(3), 0.1452(2), 0.3548(2) RX, RY, RZ -12.4(2), 227.0(2), 313.7(1) for the rigid body described by: point_for_site N1 ux = r ; uy 0.00000 uz 0.00000 point_for_site C2 ux = -r ; uy 0.00000 uz 0.00000 point_for_site C3 ux = 0.5 r ; uy = 0.866 r ; uz 0.00000 point_for_site C4 ux = 0.5 r ; uy = -0.866 r ; uz 0.00000 point_for_site C5 ux = -0.5 r ; uy = 0.866 r ; uz 0.00000 point_for_site N6 ux = -0.5 r ; uy = -0.866 r ; uz 0.00000 point_for_site O1 ux = 0.5 (r+ro) ; uy = -0.866 (r+ro); uz 0.00000 point_for_site H2 ux = - (r+rh) ; uy 0.00000 uz 0.00000 point_for_site H3 ux = 0.5 (r+rh); uy = 0.866 (r+rh); uz 0.00000 point_for_site F1 ux = -0.5 (r+rf); uy = 0.866 (r+rf); uz 0.00000 r = 1.35 ro = 1.25 rh = 0.95 rf = 1.35 ; # The next three items are given as text _pd_proc_ls_profile_function 'fundamental parameters' _pd_proc_ls_background_function polynomial _pd_proc_ls_pref_orient_corr none _pd_proc_ls_prof_R_factor 0.083 _pd_proc_ls_prof_wR_factor 0.112 _pd_proc_ls_prof_wR_expected 0.022 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 1/[Y~i~] _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 17 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? # The following item is 'CHI squared' _refine_ls_goodness_of_fit_all 5.025 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_shift/su_max .01 _refine_ls_shift/su_mean ? # 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 5 _pd_proc_2theta_range_max 105 _pd_proc_2theta_range_inc 0.02 loop_ _pd_proc_wavelength 1.540562 1.544390 _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 ? #============================================================================== # 1.8. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_symmetry_multiplicity _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_B_iso_or_equiv Pd Pd 12 0.75 0.25 0.5 1 11.29(11) N1 N 48 0.809216 0.1872055 0.4172719 1 13.29(11) C2 C 48 0.889504 0.1031145 0.2924281 1 13.29(11) C3 C 48 0.8895025 0.2075732 0.3969059 1 13.29(11) C4 C 48 0.7690735 0.1247923 0.3752159 1 13.29(11) C5 C 48 0.9296465 0.1655277 0.3344841 1 13.29(11) N6 N 48 0.8092175 0.08274675 0.3127941 1 13.29(11) O1 O 48 0.6968734 0.106476 0.3935306 1 13.29(11) H2 H 48 0.9169405 0.0743783 0.2497657 1 13.29(11) H3 H 48 0.916938 0.2502298 0.4256492 1 13.29(11) F1 F 48 1.007623 0.1853093 0.3147042 1 13.29(11) #==============================================================================