Redetermination of dipotassium μ-oxo-bis[aqua(oxalato-κ^2^<i>O</i>,<i>O</i>')dioxomolybdate(VI)] at 150 K
Cunha-Silva, Luis; Monteiro, Bernardo; Pillinger, Martyn; Gonçalves, Isabel S.; Rocha, João; Almeida Paz, Filipe A.; Acta Crystallographica Section E 63 (2007) m376–m378; doi:10.1107/S1600536806055930

data_2212178
_publ_section_title
;
 Redetermination of dipotassium
 \m-oxo-bis[aqua(oxalato-\k^2^<i>O</i>,<i>O</i>')dioxomolybdate(VI)] at
 150 K
;
_journal_coeditor_code           HB2238
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m376
_journal_page_last               m378
_journal_paper_doi               10.1107/S1600536806055930
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'K2 [Mo2 O5 (C2 O4)2 (H2 O1)2]'
_chemical_formula_moiety         '2(K +), C4 H4 Mo2 O15 2-'
_chemical_formula_sum            'C4 H4 K2 Mo2 O15'
_chemical_formula_weight         562.15
_chemical_name_systematic
;
dipotassium \m-oxo-bis[aqua(oxalato-\k^2^O,O')dioxomolybdenum(VI)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.2840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.4774(2)
_cell_length_b                   14.2242(3)
_cell_length_c                   6.57260(10)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.80
_cell_measurement_theta_min      2.73
_cell_volume                     697.11(3)
_computing_cell_refinement       'SAINT (Bruker 2001)'
_computing_data_collection       'SMART (Bruker 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL (Bruker 2001)'
_computing_structure_solution    'SHELXTL (Bruker 2001)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker X8 KappaCCD APEX-II'
_diffrn_measurement_method       'Thin-slice \w and \f'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0081
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            28523
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.491
_refine_diff_density_min         -1.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         1582
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0258P)^2^+2.2974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                1566
_reflns_number_total             1582
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2238.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212178
_cod_database_fobs_code          2212178