#------------------------------------------------------------------------------ #$Date: 2012-09-20 11:36:44 +0300 (Thu, 20 Sep 2012) $ #$Revision: 67254 $ #$URL: file:///home/coder/svn-repositories/cod/cif/3/50/00/3500014.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_3500014 loop_ _publ_author_name 'Efremov, V. A.' 'Gutnikov, S. I.' 'Kartashov, A. A.' 'Lazoryak, B.I.' _publ_requested_journal 'Personal communication to COD' _publ_section_exptl_prep ; The mixture with a stoichiometric ratio of calcium carbonate and aluminum oxide was ground and annealed three times for 24 hours at 1600 \%C. After every annealing the mixture was ground again. ; _publ_section_references ;Petricek, V., Dusek, M. & Palatinus L. (2006). Jana2006. Structure Determination Software Programs. Institute of Physics, Praha, Czech Republic. Palatinus L. & Chapuis G. (2007). J. Appl. Cryst. 40, 786-790. Altomare, A., Burla, M.C., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G., Polidori G., Rizzi R. (2001). J. Appl. Cryst. 34, 392-397. Larson A.C., Von Dreele R.B. (2004). General Structure Analysis System (GSAS) Los Alamos National Laboratory Report LAUR, 86-748 Toby B.H. (2001). J. Appl. Cryst. 34, 210-221. Luterotti L., Bortolotti M. (2003). IUCr: Compcomm Newsletter 1, 43-50. ; _publ_section_title ; Average grossite crystal structure ; _journal_name_full 'Personal communication to COD' _journal_year 2012 _chemical_compound_source synthetic _chemical_formula_moiety 'Al4 O7, Ca' _chemical_formula_structural ; Ca (Al4 O7) ; _chemical_formula_sum 'Al4 Ca O7' _chemical_formula_weight 260 _chemical_name_common 'Calcium dialuminate' _chemical_name_mineral Grossite _chemical_name_systematic ' tetraaluminium calcium heptaoxide' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method 'Jana2006 Version : 04/07/2012' _cell_angle_alpha 90 _cell_angle_beta 106.905(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.886(6) _cell_length_b 8.8830(12) _cell_length_c 5.4423(27) _cell_measurement_reflns_used 311 _cell_measurement_temperature 295 _cell_measurement_theta_max 100 _cell_measurement_theta_min 10 _cell_special_details ; Cell parameters was refined by full-profile analysis (Jana2006, GSAS, Moud, Quanto). Pseudo-Voigt function was used as profile function. Pearson VII function was used in addition (in Quanto only). Cell parameters determined as the weighted average of 85 calculations (17 samples x 5 methods). Grossite mass fraction was used as a weight. ; _cell_volume 596.0(4) _computing_cell_refinement 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_data_collection 'Huber software' _computing_data_reduction 'XRUtils (Efremov,private)' _computing_molecular_graphics 'VESTA 3 ( Momma & Izumi, 2011 )' _computing_structure_refinement 'Jana2006 (Petricek, Dusek & Palatinus, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 295 _diffrn_detector 'Image plate' _diffrn_detector_type Huber _diffrn_measurement_device 'Guinier powder diffractometer' _diffrn_radiation_monochromator 'curved Ge 111' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a~1~' _diffrn_radiation_wavelength 1.540598 _diffrn_source 'sealed x-ray tube' _diffrn_source_target Cu _exptl_absorpt_coefficient_mu 14.972 _exptl_crystal_density_diffrn 2.898 _exptl_crystal_F_000 512 _pd_char_colour colourless _pd_meas_2theta_range_inc 0.01 _pd_meas_2theta_range_max 100.000 _pd_meas_2theta_range_min 3.500 _pd_meas_number_of_points 9651 _pd_meas_scan_method fixed _pd_meas_special_details ; Sum of 3 measurements 20 min each (total 60 min), Number of measurement points 20001. Step size (2-Theta) 0.005 ; _pd_proc_2theta_range_inc 0.01 _pd_proc_2theta_range_max 100 _pd_proc_2theta_range_min 9.47 _pd_proc_info_data_reduction ; A number of intensities values was reduced by using triangular smooth. The principle of this method is the averaging of the experimental intensities, that separated by "doubling" step-size away from each other by Ij =( I2j-1 + 2*I2j + I2j+1)/4). x-ray camera geometric factor (G=cos(2*theta-beta)), beta = 45) was added. ; _pd_proc_ls_special_details ;Atom sites was calculated as an average of jana2006 (RF% = 3.32, Rw% = 3.45, GOF = 1.05, Rp% = 2.57, Rwp% = 3.37) and GSAS (RF% = 4.58, Rw% = 5.97, GOF = 1, Rp% = 2.52, Rwp% = 3.25) data. ; _pd_spec_mount_mode transmission _pd_spec_shape flat_sheet _pd_spec_size_thick 0.05 _refine_special_details ;background approximation: 12 Legendre polynomials (jana2006), shifted Chebyshev function of 1st kind with 12 terms. (GSAS) ; _[local]_cod_data_source_file Grossite_Mean.cif _[local]_cod_data_source_block global _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 3500014 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z+1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z+1/2 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag Ca1 Ca 0 0.3106(9) 0.25 Uiso 0.0116(28) 4 1 d Al1 Al 0.3370(7) 0.0854(9) 0.1924(18) Uiso 0.0106(28) 8 1 d Al2 Al 0.3788(7) 0.4414(10) 0.2581(16) Uiso 0.0132(28) 8 1 d O1 O 0 0.0286(23) 0.25 Uiso 0.021(8) 4 1 d O2 O 0.1155(11) 0.4486(14) 0.0653(27) Uiso 0.001(5) 8 1 d O3 O 0.3817(10) 0.2535(17) 0.3517(28) Uiso 0.004(5) 8 1 d O4 O 0.1952(5) 0.0570(7) 0.0829(14) Uiso 0.001(3) 8 1 d loop_ _atom_type_symbol _atom_type_oxidation_number Al 3 Ca 2 O -2 loop_ _pd_proc_info_excluded_regions 'from 0 to 9.460'