#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003034.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_2003034 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first i3 _journal_page_last i5 _publ_section_title ; A new reduced molybdenum oxide with hollandite-type structure, PrMo~6~O~12~ ; loop_ _publ_author_name 'Barrier, N.' 'Tortelier, J.' 'Gougeon, P.' _chemical_formula_sum 'Mo6 O12 Pr' _chemical_formula_iupac 'Pr1 Mo6 O12' _chemical_formula_weight 908.55 _symmetry_cell_setting 'tetragonal' _symmetry_space_group_name_H-M 'I 4/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 9.9147(3) _cell_length_b 9.9147(3) _cell_length_c 8.6508(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 850.38(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.26 _cell_measurement_theta_max 31.39 _cell_measurement_temperature 293(2) _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'black' _exptl_crystal_size_max .29 _exptl_crystal_size_mid .025 _exptl_crystal_size_min .022 _exptl_crystal_density_diffrn 7.095 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 14.245 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_process_details '(Coppens, 1970)' _exptl_absorpt_correction_T_min .340 _exptl_absorpt_correction_T_max .768 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength .71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 1494 _diffrn_reflns_av_R_equivalents .0359 _diffrn_reflns_av_sigmaI/netI .0213 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 39.99 _diffrn_reflns_theta_full 39.99 _diffrn_measured_fraction_theta_max .501 _diffrn_measured_fraction_theta_full .501 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% <1 _reflns_number_total 1385 _reflns_number_gt 1242 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all .038 _refine_ls_R_factor_gt .032 _refine_ls_wR_factor_ref .081 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _refine_ls_number_reflns 1385 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0281P)^2^+24.9952P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_diff_density_max 3.395 _refine_diff_density_min -2.985 _refine_ls_extinction_method SHELXL97 _refine_ls_extinction_coef .00110(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Pr' 'Pr' -.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 .6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pr1 .0000 .0000 -.20745(5) .00788(9) Uani d S 1 . . Pr Mo1 .34033(3) -.81670(3) -.34174(4) .00648(8) Uani d . 1 . . Mo Mo2 .33255(4) -.81617(4) .0000 .00494(9) Uani d S 1 . . Mo O1 .4568(3) -.1706(3) -.3324(3) .0066(4) Uani d . 1 . . O O2 .1722(3) -.1305(3) -.3329(3) .0084(4) Uani d . 1 . . O O3 .4631(4) -.1626(4) .0000 .0062(6) Uani d S 1 . . O O4 .1229(4) .1602(4) .0000 .0065(6) Uani d S 1 . . 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 Pr1 .00901(11) .00901(11) .00562(16) .000 .000 .000 Mo1 .00547(12) .00510(12) .00887(14) -.00143(8) -.00238(9) .00218(9) Mo2 .00505(16) .00513(16) .00464(16) .00037(11) .000 .000 O1 .0043(9) .0096(10) .0058(11) -.0006(8) -.0002(8) -.0006(8) O2 .0085(10) .0103(11) .0062(11) -.0024(8) .0005(8) -.0016(9) O3 .0060(13) .0076(14) .0052(14) -.0010(11) .000 .000 O4 .0066(14) .0080(14) .0050(14) .0000(11) .000 .000 _cod_database_code 2003034