#============================================================================= data_Mishan #============================================================================== loop_ _audit_conform_dict_name _audit_conform_dict_version _audit_conform_dict_location cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic # 1. SUBMISSION DETAILS _publ_contact_author_name 'Dr Shanke Liu ' _publ_contact_author_address ; Division of Solid Mineral Resources Institute of Geology and Geophysics, Chinese Academy of Sciences No. 19, Beitucheng Western Road, Chaoyang District, Beijing, 100029, People's Republic of China ; _publ_contact_author_email liushanke@mail.iggcas.ac.cn _publ_contact_author_fax '008610 8299 8571' _publ_contact_author_phone '008610 8299 8571' _publ_requested_journal 'Powder Diffraction' _publ_requested_category ? _publ_contact_letter ; Please consider this CIF submission for publication as a full paper in Acta Cryst. Section C. The figures, Transfer of Copyright Agreement form and powder profile will be sent on receipt of your acknowledgment letter. ; #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _iucr_compatibility_tag ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Powder Diffraction' _journal_year 2014 _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Example CIF - Not for publication ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication.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 'Liu Shanke' ; Division of Solid Mineral Resources Institute of Geology and Geophysics, Chinese Academy of Sciences No. 19, Beitucheng Western Road, Chaoyang District, Beijing, 100029, People's Republic of China ; 'Li He' ; State Key Laboratory of Lithospheric Evolution Institute of Geology and Geophysics, Chinese Academy of Sciences No. 19, Beitucheng Western Road, Chaoyang District, Beijing, 100029, People's Republic of China ; 'Liu Jianming' ; Division of Solid Mineral Resources Institute of Geology and Geophysics, Chinese Academy of Sciences No. 19, Beitucheng Western Road, Chaoyang District, Beijing, 100029, People's Republic of China ; #============================================================================== # 4. TEXT _publ_section_synopsis ; The possibility of extracting the high-quality structural data from X-ray powder diffraction for dolomite and calcite by Rietveld refinement ; _publ_section_abstract ; Obtaining optimal structural data from X-ray powder diffraction using the Rietveld method ; _publ_section_comment ; X-ray powder diffraction (XRPD) is a widely used method used for phase identification ... ; _publ_section_exptl_prep ; The authors aimed at showing how one treats preferred orientation and how different refinement ... ; _publ_section_exptl_refinement ; The Rietveld method, initially proposed by Rietveld (1967, 1969), has been significantly improved during last two decades and become an effective, reliable tool for the structural refinements. ; _publ_section_references ; Antao, S.M., Hassan, I., Mulder, W.H., Lee, P.L., and Toby, B.H. (2009): In situ study of the R-3c\\rightarrowR-3m orientational disorder in calcite. Phys Chem Minerals, 36, 159--169. Balic-Zunic, T., Katerinopoulou, A., and Edsberg, A. (2011): Application of powder X-ray diffraction and the Rietveld method to the analysis of oxidation processes and products in sulphidic mine tailings. Neues Jahrb Mineral Abh.188(1), 31--47. Ballirano, P. (2011): Laboratory parallel-beam transmission X-ray powder diffraction investigation of the thermal behavior of calcite:comparison with X-ray single-crystal and synchrotron powder diffraction data. Period Mineral. 80(1), 123--134. ... ; _publ_section_figure_captions ; Figure 1. Rietveld fit of Occ when a two terms Chebyshev polynomial, a four terms Chebyshev polynomial, profile and cell parameters and a ten terms Chebyshev polynomial were added to the refinement respectively, and the corresponding plots are Figure 1(A), (B), (C) and (D) [The log vertical scale was chosen for clarity].The red curve is observed diffraction pattern (line), and the black is calculated (line); the green curve at the bottom shows the background (crosses). ... ; _publ_section_acknowledgements ; The authors would like to acknowledge the financial support for technological innovations from the Institute of Geology and Geophysics, Chinese Academy of Sciences. Shanke Liu is indebted to Professor Jiaju Li for his tremendous help and encouragement in studying the Rietveld method.Shanke Liu is also grateful to Dr. B.H. Toby for helping with GSAS refinement skills and tremendous encouragement in preparing this paper through private communications. Two anonymous reviewers are thanked for their constructive critical suggestions aimed to improve the quality of the manuscript. ; #============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the '?' in the data_? line below # by a unique identifier. #============================================================================== data_Occdata # 5. CHEMICAL DATA _chemical_name_systematic ; Calcium Carbonate ; _chemical_name_common 'calcite' _chemical_formula_moiety 'CaCO3' _chemical_formula_structural 'CaCO3' _chemical_formula_analytical ? _chemical_formula_mineral 'calcite' _chemical_formula_sum 'C2 Ca1 O3' _chemical_formula_weight 100.09 _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 #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _space_group_crystal_system trigonal _space_group_name_H-M_alt 'R -3 c' _space_group_name_Hall '-R 3 2' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -y,-x,z+1/2 5 -x+y,y,z+1/2 6 x,x-y,z+1/2 7 -x,-y,-z 8 y,-x+y,-z 9 x-y,x,-z 10 y,x,-z+1/2 11 x-y,-y,-z+1/2 12 -x,-x+y,-z+1/2 13 x+2/3,y+1/3,z+1/3 14 -y+2/3,x-y+1/3,z+1/3 15 -x+y+2/3,-x+1/3,z+1/3 16 -y+2/3,-x+1/3,z+5/6 17 -x+y+2/3,y+1/3,z+5/6 18 x+2/3,x-y+1/3,z+5/6 19 -x+2/3,-y+1/3,-z+1/3 20 y+2/3,-x+y+1/3,-z+1/3 21 x-y+2/3,x+1/3,-z+1/3 22 y+2/3,x+1/3,-z+5/6 23 x-y+2/3,-y+1/3,-z+5/6 24 -x+2/3,-x+y+1/3,-z+5/6 25 x+1/3,y+2/3,z+2/3 26 -y+1/3,x-y+2/3,z+2/3 27 -x+y+1/3,-x+2/3,z+2/3 28 -y+1/3,-x+2/3,z+1/6 29 -x+y+1/3,y+2/3,z+1/6 30 x+1/3,x-y+2/3,z+1/6 31 -x+1/3,-y+2/3,-z+2/3 32 y+1/3,-x+y+2/3,-z+2/3 33 x-y+1/3,x+2/3,-z+2/3 34 y+1/3,x+2/3,-z+1/6 35 x-y+1/3,-y+2/3,-z+1/6 36 -x+1/3,-x+y+2/3,-z+1/6 _cell_length_a 4.98676(5) _cell_length_b 4.98676(5) _cell_length_c 17.0506(2) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 367.204(9) _cell_formula_units_Z 6 _cell_measurement_temperature 298 _pd_calibration_special_details ; ? ; _cell_special_details ; ? ; _exptl_crystal_density_diffrn 2.717 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 ? # 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 ; 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 ? _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 101.325 _pd_prep_temperature ? # 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 ? #======================================================================= # 7. 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 'Rigaku D/max-2400' _diffrn_detector 'NaI 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 none # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 6850 _pd_meas_2theta_range_min 3 _pd_meas_2theta_range_max 140 _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 'GSAS and EXPGUI' _computing_cell_refinement 'GSAS and EXPGUI' _computing_data_reduction 'GSAS and EXPGUI' _computing_structure_solution 'GSAS and EXPGUI' _computing_structure_refinement 'GSAS and EXPGUI' _computing_molecular_graphics 'GSAS and EXPGUI' _computing_publication_material 'GSAS and EXPGUI' #============================================================================== # 8. 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 'The third CW profile function' _pd_proc_ls_background_function 'Shifted Chebyshev polynomial' _pd_proc_ls_pref_orient_corr 'Spherical harmonics function' ; ; _pd_proc_ls_prof_R_factor 0.105 _pd_proc_ls_prof_wR_factor 0.149 _pd_proc_ls_prof_wR_expected 0.0979 _refine_special_details ; ? ; _refine_ls_structure_factor_coef Inet _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme sigma _refine_ls_weighting_details '1/[Y~i~+\s(Y~i~)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_parameters 39 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 2.31 _refine_ls_R_I_factor .142 _refine_ls_restrained_S_all 4 _refine_ls_shift/su_max ? _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 3 _pd_proc_2theta_range_max 140 _pd_proc_2theta_range_inc 0.02 loop_ _pd_proc_wavelength 1.540560 1.544390 # Each refinement must be accompanied by a listing of the powder data # in CIF format. Each listing should be sent as a separate file consisting # of one data block containing a single powder profile. The value of # _pd_block_diffractogram_id is used to associate each refinement with # its corresponding powder profile, since it must match the value # of _pd_block_id in the file containing the powder data. _pd_block_diffractogram_id Calcite-Mishan-SDC-2 # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? #============================================================================== # 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_adp_type _atom_site_occupancy _atom_site_type_symbol Ca1 0.00000 0.00000 0.00000 1.33(3) Biso 1.00 Ca C1 0.00000 0.00000 0.25000 1.02(10) Biso 1.00 C O1 0.25733(0) 0.00000 0.25000 1.72(6) Biso 1.00 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 #============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA #============================================================================== # Additional structures (sections 5-10 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 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./