Pr~4~Mo~9~O~18~, an Atypical, Novel, Ternary Reduced Molybdenum Oxide Containing Unusual Mo~7~, Mo~13~ and Mo~19~ Clusters. Synthesis, Crystal Structure, and Physical Properties
J. Tortelier; P. Gougeon; Inorganic Chemistry 37 (1998) 6229–6236; doi:10.1021/ic980500h

data_4323187
_publ_contact_author
;
Gougeon, P.
Laboratoire de Chimie du Solide et Inorganique Mol\'eculaire
UMR CNRS 6511
Universit\'e de Rennes I
Avenue du G\'en\'eral Leclerc
35042 Rennes CEDEX
France
;
_publ_contact_author_email       Patrick.Gougeon@univ-rennes1.fr
_publ_contact_author_fax         '(33) 2 99 63 57 04'
_publ_contact_author_phone       '(33) 2 99 28 62 54'
_publ_section_title
;
 Pr~4~Mo~9~O~18~, an Atypical, Novel, Ternary Reduced Molybdenum Oxide
 Containing Unusual Mo~7~, Mo~13~ and Mo~19~ Clusters. Synthesis, Crystal
 Structure, and Physical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6229
_journal_page_last               6236
_journal_paper_doi               10.1021/ic980500h
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'Mo9 O18 Pr4'
_chemical_formula_weight         1715.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            15
_cell_length_a                   11.3600(7)
_cell_length_b                   11.3600(7)
_cell_length_c                   50.392(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      5
_cell_volume                     5631.8(10)
_computing_cell_refinement       'CAD 4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD 4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       \w-2q\
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       87
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7222
_diffrn_reflns_theta_max         37.92
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    20.025
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   '\Y scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.585
_exptl_crystal_description       'irregular triangle'
_exptl_crystal_F_000             11370
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.242
_refine_diff_density_min         -2.442
_refine_diff_density_rms         0.379
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_coef       0.000049(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.096
_refine_ls_goodness_of_fit_obs   1.103
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3816
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.096
_refine_ls_restrained_S_obs      1.103
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_obs          0.0242
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+7.6090P] where P=(Fo^2^+2Fc^2^)/3'
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0485
_refine_ls_wR_factor_obs         0.0469
_reflns_number_observed          3535
_reflns_number_total             3816
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980500h.cif
_cod_data_source_block           pr4psi
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4323187