Structural refinement of T2Mo3O8 (T=Mg, Co, Zn and Mn) and anomalous valence of trinuclear molybdenum clusters in Mn2Mo3O8
Abe, Hideki; Sato, Akira; Tsujii, Naohito; Furubayashi, Takao; Shimoda, Masahiko; Journal of Solid State Chemistry 183 (2010) 379–384; doi:10.1016/j.jssc.2009.11.024

data_1563739
_publ_section_title
;
 Structural refinement of T2Mo3O8 (T=Mg, Co, Zn and Mn) and anomalous
 valence of trinuclear molybdenum clusters in Mn2Mo3O8
;
_journal_issue                   2
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              379
_journal_page_last               384
_journal_paper_doi               10.1016/j.jssc.2009.11.024
_journal_volume                  183
_journal_year                    2010
_chemical_formula_sum            'Mn2 Mo3 O8'
_chemical_formula_weight         525.70
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   5.8003(2)
_cell_length_b                   5.8003(2)
_cell_length_c                   10.2425(5)
_cell_measurement_temperature    293(2)
_cell_volume                     298.43(2)
_computing_cell_refinement       'SAINT-Plus-NT(Bruker, 1999)'
_computing_data_collection       'SMART-NT(Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus-NT(Bruker, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4557
_diffrn_reflns_theta_full        40.32
_diffrn_reflns_theta_max         40.32
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    10.254
_exptl_absorpt_correction_T_max  0.2802
_exptl_absorpt_correction_T_min  0.1534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 1999)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.983
_refine_diff_density_min         -3.934
_refine_diff_density_rms         0.577
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.87(6)
_refine_ls_extinction_coef       0.169(8)
_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_ref   1.154
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+0.3435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                716
_reflns_number_total             724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-379.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P63mc
_cod_database_code               1563739