Structural Studies of TcO2 by Neutron Powder Diffraction and First-Principles Calculations
Efrain E. Rodriguez; Frederic Poineau; Anna Llobet; Alfred P. Sattelberger; Joydeep Bhattacharjee; Umesh V. Waghmare; Thomas Hartmann; Anthony K. Cheetham; Journal of the American Chemical Society 129 (2007) 10244–10248; doi:10.1021/ja0727363

data_4109804
_publ_contact_author_address
; Materials Research Laboratory
University of California
Santa Barbara, CA 93106
;
_publ_contact_author_email       cheetham@mrl.ucsb.edu
_publ_contact_author_fax         '(805) 893-8797'
_publ_contact_author_name        'Anthony K. Cheetham'
_publ_contact_author_phone       '(805) 893-8767'
_publ_section_title
;
 Structural Studies of TcO2 by Neutron Powder Diffraction and
 First-Principles Calculations
;
_journal_coden_ASTM              JACSAT
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10244
_journal_page_last               10248
_journal_paper_doi               10.1021/ja0727363
_journal_volume                  129
_journal_year                    2007
_chemical_formula_analytical     'O1 Tc2'
_chemical_formula_structural     TcO2
_chemical_formula_sum            'O7.9 Tc4'
_chemical_formula_weight         518.78
_chemical_melting_point          1273
_chemical_name_common            'Technetium dioxide'
_chemical_name_systematic        'Technetium (IV) oxide'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_author_name               'Efrain E. Rodriguez'
_audit_creation_date             2007-04-18T23:18
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2007-04-18T23:18  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 121.4532(11)
_cell_angle_gamma                90.0
_cell_formula_units_Z            1
_cell_length_a                   5.68908(8)
_cell_length_b                   4.75461(8)
_cell_length_c                   5.51948(12)
_cell_measurement_temperature    295
_cell_volume                     127.361(4)
_computing_molecular_graphics
'Diamond 3.1d, Klaus Brandenburg, Crystal Impact GbR, Bonn, Germany'
_computing_publication_material
'GSAS, A. C. Larson and R. B. Von Dreele, LANL, LAUR 86-748 (2004)'
_computing_structure_refinement  GSAS
_computing_structure_solution
'GSAS, A. C. Larson and R. B. Von Dreele, LANL LAUR 86-748 (2004)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'He-3 tubes'
_diffrn_measurement_device_type  'High Intensity Powder Diffractometer (HIPD)'
_diffrn_radiation_probe          neutron
_diffrn_source                   neutron
_diffrn_source_target            W
_diffrn_source_type              'Spallation source'
_exptl_absorpt_correction_T_max  0.92652
_exptl_absorpt_correction_T_min  0.52673
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 0
 Debye-Scherrer absorption correction
Term (= MU.r/wave) =     0.66833E-01
Correction is not refined.
;
_exptl_crystal_density_diffrn    6.83
_pd_block_id
2007-04-18T23:18|TCO2_295K_HIPD_12-1-_phase1|Efrain_E._Rodriguez||
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  'dark grey'
_pd_instr_location
'Manuel Lujan Jr. Neutron Scattering Center, LANSCE'
_pd_meas_2theta_fixed            153.00
_pd_meas_scan_method             tof
_pd_phase_name                   'TcO2 monoclinic phase'
_pd_prep_pressure                101.325
_pd_prep_temperature             973
_pd_proc_info_data_reduction     'Used FITSPEC to normalize data'
_pd_proc_info_datetime           2007-04-18T23:18:31
_pd_proc_info_excluded_regions
'Low and high TOF data were excluded due to lower statistics'
_pd_proc_ls_background_function
;   GSAS Background function number 1 with  6 terms.
 Shifted Chebyshev function of 1st kind
      1:   0.217841     2:  -5.001020E-02 3:   1.260920E-02 4:  -5.216770E-03
      5:   4.200020E-03 6:  -6.091590E-03
;
_pd_proc_ls_prof_R_factor        0.0173
_pd_proc_ls_prof_wR_expected     0.0143
_pd_proc_ls_prof_wR_factor       0.0231
_pd_spec_mounting                'Sample holder is a vanadium can'
_pd_spec_shape                   cylinder
_refine_ls_goodness_of_fit_all   1.58
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_restraints     0
_refine_ls_R_Fsqd_factor         0.07578
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        0.394
_reflns_d_resolution_low         3.407
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -16
_reflns_number_total             5911
_cod_data_source_file            ja0727363si20070419_084817.cif
_cod_data_source_block           TCO2_295K_HIPD_12-1-_phase_1
_cod_original_cell_volume        127.3610(20)
_cod_original_formula_sum        'O7.90 Tc4.00'
_cod_database_code               4109804
_cod_database_fobs_code          4109804
_gsas_exptl_extinct_corr_t_min   1.00000
_gsas_exptl_extinct_corr_t_max   1.00000