Li~2~GeMo~3~O~8~: a novel reduced molybdenum oxide containing Mo~3~O~13~ cluster units
Gall, Philippe; Gougeon, Patrick; Acta Crystallographica Section E 72 (2016) 995–997; doi:10.1107/S2056989016009750

data_2241733
_publ_section_title
;
 Li~2~GeMo~3~O~8~: a novel reduced molybdenum oxide containing Mo~3~O~13~
 cluster units
;
_journal_coeditor_code           WM5299
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              995
_journal_page_last               997
_journal_paper_doi               10.1107/S2056989016009750
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'Li2 Ge Mo3 O8'
_chemical_formula_sum            'Ge Li2 Mo3 O8'
_chemical_formula_weight         502.29
_chemical_name_systematic
;
Dilithium germanium trimolybdenum octaoxide
;
_space_group_IT_number           186
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_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                   5.7268(3)
_cell_length_b                   5.7268(3)
_cell_length_c                   9.9841(6)
_cell_measurement_reflns_used    4457
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      35.00
_cell_measurement_theta_min      4.08
_cell_volume                     283.57(3)
_computing_cell_refinement
;
COLLECT (Nonius, 1998)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
EvalCCD (Duisenberg et al., 2003)
;
_computing_molecular_graphics
;
DIAMOND (Bergerhoff, 1996)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR97 (Altomare et al., 1999)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4457
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    11.739
_exptl_absorpt_correction_T_max  0.1574
_exptl_absorpt_correction_T_min  0.0479
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(de Meulenaar & Tompa, 1965)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    5.883
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.330
_refine_ls_abs_structure_details
;
Flack (1983), 247 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         522
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0515P)^2^+0.3716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                501
_reflns_number_total             522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            wm5299sup1.cif
_cod_data_source_block           I
_cod_database_code               2241733
_cod_database_fobs_code 2241733