Monolanthanum tripotassium tetrahydrogen decamolybdodicobaltate(III) tridecahydrate
Lee, Uk; Joo, Hea-Chung; Acta Crystallographica Section E 66 (2010) i10–; doi:10.1107/S1600536810000929

data_2224853
_publ_section_title
;
 Monolanthanum tripotassium tetrahydrogen decamolybdodicobaltate(III)
 tridecahydrate
;
_journal_coeditor_code           BR2132
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i10
_journal_paper_doi               10.1107/S1600536810000929
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'La K3 [H4 Mo10 Co2 O38], 13H2 O'
_chemical_formula_moiety         'La 3+, 3(K +), H4 Co2 Mo10 O38, 13(H2 O)'
_chemical_formula_structural     'K3 La (H4 Co2 Mo10 O38), (H2 O)13'
_chemical_formula_sum            'Co2 H30 K3 La Mo10 O51'
_chemical_formula_weight         2179.71
_chemical_name_systematic
;
Monolanthanum tripotassium tetrahydrogen decamolybdodicobaltate(III)
tridecahydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 112.957(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4487(6)
_cell_length_b                   18.5980(10)
_cell_length_c                   12.3179(8)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      19.0
_cell_volume                     2204.1(2)
_computing_cell_refinement       'X-RED (Stoe & Cie, 1996)'
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe STADI-4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10417
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        2.3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.832
_exptl_absorpt_correction_T_max  0.5267
_exptl_absorpt_correction_T_min  0.3488
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.367
_refine_diff_density_min         -1.273
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.001(10)
_refine_ls_extinction_coef       0.00255(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         10104
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+5.9397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                9949
_reflns_number_total             10104
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2132.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2224853
_cod_database_fobs_code          2224853