# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. #============================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 _journal_year 2005 _publ_contact_author_name 'Jianhua Lin' _publ_contact_author_address ; State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P. R. China. ; _publ_contact_author_email jhlin@pku.edu.cn _publ_contact_author_fax 8610-62751708 _publ_contact_author_phone 8610-62751715 _publ_section_title ; MCuB7O12 nH2O (M=Na, K ): A new copper borate with 14-ring channel ; # 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 'Tao Yang' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P. R. China. ; 'Guobao Li' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P. R. China. ; 'Liping You' ; Electron Microscopy Laboratory, College of Physics, Peking University, Beijing 100871, P. R. China. ; 'Jing Ju' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P. R. China. ; 'Fuhui Liao' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P. R. China. ; 'Jianhua Lin' ; State Key Laboratory of Rare Earth Materials Chemistry and Applications, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, P. R. China. ; #============================================================================== # Supplementary Material (ESI) for Chemical Communications # This journal is ?The Royal Society of Chemistry 2005 data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 273078' # 4. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'H2 B7 O13 Cu1 Na1' _chemical_formula_structural NaCuB7O12.H2O _chemical_formula_analytical ? _chemical_formula_iupac 'H2 B7 O13 Cu1 Na1' _chemical_formula_sum NaCuB7O12.H2O _chemical_formula_weight 372.20 _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 Cu Cu 'International Tables for Crystallography (Vol. IV)' Na Na 'International Tables for Crystallography (Vol. IV)' O O 'International Tables for Crystallography (Vol. IV)' B B 'International Tables for Crystallography (Vol. IV)' H H 'International Tables for Crystallography (Vol. IV)' #============================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pnnm _chemical_name_mineral Structure _cell_length_a 12.7372 _cell_length_b 4.69546 _cell_length_c 15.17928 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 907.8274 _cell_formula_units_Z 4 _cell_measurement_temperature 295 loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x, y, -z' 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.135 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 230 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 10 # 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 cream # 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 ? #============================================================================== # 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 295 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker AXS D8' _diffrn_detector 'Position sensitive detector' _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~ 1.540596 _diffrn_radiation_monochromator 'Single gobel mirroirs' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7858 _pd_meas_2theta_range_min 7 _pd_meas_2theta_range_max 120 _pd_meas_2theta_range_inc 0.0144 # 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, 2001)' _computing_cell_refinement 'TOPAS (Bruker V3.1, AXS, 2004)' _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics 'SCHAKAL (Keller, Univ. Freiburg, Germany 1999)' _computing_publication_material TOPAS #============================================================================== # 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 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 ; axis (001), r(March-Dollase) 0.936(3) ; _pd_proc_ls_prof_R_factor 0.038 _pd_proc_ls_prof_wR_factor 0.053 _pd_proc_ls_prof_wR_expected 0.015 _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 60 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 3.62 _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 7 _pd_proc_2theta_range_max 120 _pd_proc_2theta_range_inc 0.0144 loop_ _pd_proc_wavelength 1.540596 _pd_block_diffractogram_id Compound_1 # 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 ? #============================================================================== # 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_U_iso_or_equiv Cu Cu 4 0 0 0.4004(4) 1 0.0093(4) Na Na 4 0.20943(1) 0.4090(4) 0 1 0.0783(2) B1 B 8 0.17403(7) 0.411(2) 0.3467(1) 1 0.0088(2) B2 B 8 0.06223(8) 0.2065(1) 0.2181(3) 1 0.0088(2) B3 B 8 0.18460(2) 0.5608(9) 0.191(3) 1 0.0088(2) B4 B 4 0.12175(3) 0.4382(9) 0.5 1 0.0088(2) O1 O 8 0.07946(5) 0.2303(8) 0.3102(7) 1 0.0051(1) O2 O 4 0.06973(4) 0.1811(2) 0.5 1 0.0051(1) O3 O 8 0.2024(5) 0.6145(2) 0.2789(1) 1 0.0051(1) O4 O 8 0.25526(3) 0.2111(1) 0.3695(5) 1 0.0051(1) O5 O 8 0.14022(5) 0.5729(5) 0.4227(6) 1 0.0051(1) O6 O 8 0.11137(2) 0.3772(5) 0.1613(1) 1 0.0051(1) O7 O 4 0 0 0.1850(8) 1 0.0051(1) O8 O 4 0.90182(4) 0.0473(6) 0 1 0.1591(2) #============================================================================== #============================================================================== data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 274697' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'H2 B7 O13 Cu1 K1' _chemical_formula_structural KCuB7O12.H2O _chemical_formula_analytical ? _chemical_formula_iupac 'H2 B7 O13 Cu1 K1' _chemical_formula_sum KCuB7O12.H2O _chemical_formula_weight 388.31 _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 Cu Cu 'International Tables for Crystallography (Vol. IV)' K K 'International Tables for Crystallography (Vol. IV)' O O 'International Tables for Crystallography (Vol. IV)' B B 'International Tables for Crystallography (Vol. IV)' H H 'International Tables for Crystallography (Vol. IV)' #============================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pnnm _chemical_name_mineral Structure _cell_length_a 12.6406 _cell_length_b 4.75296 _cell_length_c 15.38502 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 924.3361 _cell_formula_units_Z 4 _cell_measurement_temperature 295 loop_ _symmetry_equiv_pos_as_xyz '-x, -y, -z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x, y, -z' 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.135 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 230 # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial 10 # 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 cream # 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 ? #============================================================================== # 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 295 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Cu _diffrn_source_type ? _diffrn_measurement_device_type 'Bruker AXS D8' _diffrn_detector 'Position sensitive detector' _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~ 1.540596 _diffrn_radiation_monochromator 'Single gobel mirroirs' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 7858 _pd_meas_2theta_range_min 7 _pd_meas_2theta_range_max 120 _pd_meas_2theta_range_inc 0.0144 # 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, 2001)' _computing_cell_refinement 'TOPAS (Bruker V3.1, AXS, 2004)' _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics 'SCHAKAL (Keller, Univ. Freiburg, Germany 1999)' _computing_publication_material TOPAS #============================================================================== # 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 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 ; axis (001), r(March-Dollase) 0.936(3) ; _pd_proc_ls_prof_R_factor 0.034 _pd_proc_ls_prof_wR_factor 0.050 _pd_proc_ls_prof_wR_expected 0.013 _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 60 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 3.62 _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 7 _pd_proc_2theta_range_max 120 _pd_proc_2theta_range_inc 0.0144 loop_ _pd_proc_wavelength 1.540596 _pd_block_diffractogram_id Compound_1 # 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 ? #============================================================================== # 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_U_iso_or_equiv B4 B 8 0.1718(7) 0.4109(4) 0.3466(4) 1 0.0013(5) B3 B 8 0.0700(6) 0.1922(5) 0.2268(5) 1 0.0013(5) B2 B 8 0.1881(5) 0.5834(6) 0.1963(2) 1 0.0013(5) B1 B 4 0.1233(9) 0.414(9) 0.5 1 0.0013(5) K K 4 0.1931(5) 0.3554(7) 0 1 0.040(3) O8 O 4 0.9691(8) 0.168(1) 0 1 0.304(4) O7 O 4 0 0 0.1912(8) 1 0.0051(3) O6 O 4 0.0700(9) 0.1784(2) 0.5 1 0.0051(3) O5 O 8 0.1111(2) 0.380(7) 0.167(1) 1 0.0051(3) O4 O 8 0.1415(1) 0.5681(7) 0.4210(5) 1 0.0051(3) O3 O 8 0.2590(7) 0.2147(8) 0.3681(5) 1 0.0051(3) O2 O 8 0.0773(5) 0.2250(4) 0.3134(3) 1 0.0051(3) O1 O 8 0.1989(1) 0.6230(3) 0.282(8) 1 0.0051(3) Cu Cu 4 0 0 0.401(9) 1 0.0130(2)