#------------------------------------------------------------------------------
#$Date: 2023-03-26 10:09:57 +0200 (Sun 26 de Mar de 2023) $
#$Revision: 282068 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/30/2003034.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
loop_
_publ_author_name
'Barrier, N.'
'Tortelier, J.'
'Gougeon, P.'
_publ_section_title
;
A new reduced molybdenum oxide with hollandite-type structure, PrMo₆O₁₂
;
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              i3
_journal_page_last               i5
_journal_paper_doi               10.1107/S1600536800019048
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'Pr1 Mo6 O12'
_chemical_formula_sum            'Mo6 O12 Pr'
_chemical_formula_weight         908.55
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9147(3)
_cell_length_b                   9.9147(3)
_cell_length_c                   8.6508(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.39
_cell_measurement_theta_min      10.26
_cell_volume                     850.38(7)
_database_code_amcsd             0010350
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full .501
_diffrn_measured_fraction_theta_max .501
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0359
_diffrn_reflns_av_sigmaI/netI    .0213
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1494
_diffrn_reflns_theta_full        39.99
_diffrn_reflns_theta_max         39.99
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.245
_exptl_absorpt_correction_T_max  .768
_exptl_absorpt_correction_T_min  .340
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens, 1970)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          .29
_exptl_crystal_size_mid          .025
_exptl_crystal_size_min          .022
_refine_diff_density_max         3.395
_refine_diff_density_min         -2.985
_refine_ls_extinction_coef       .00110(9)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_matrix_type           full
_refine_ls_number_parameters     50
_refine_ls_number_reflns         1385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          .038
_refine_ls_R_factor_gt           .032
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0281P)²+24.9952P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .081
_reflns_number_gt                1242
_reflns_number_total             1385
_reflns_threshold_expression     I>2σ(I)
_cod_database_code               2003034
_amcsd_formula_title             PrMo6O12
loop_
_space_group_symop_operation_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'
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
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_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0010350
