Structure and Solution Speciation of U(IV) Linked Phosphomolybdate (Mo(V)) Clusters.
Deb, Tapash; Zakharov, Lev; Falaise, Clément; Nyman, May; Inorganic chemistry 55 (2016) 755–761; doi:10.1021/acs.inorgchem.5b02229

data_4344600
_publ_section_title
;
 Structure and Solution Speciation of U(IV) Linked Phosphomolybdate
 (Mo(V)) Clusters.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              755
_journal_page_last               761
_journal_paper_doi               10.1021/acs.inorgchem.5b02229
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'Mo6 O31 P4, O4 P -3, 3(Na +), 3(H2 O)'
_chemical_formula_sum            'Mo6 Na3 O38 P5'
_chemical_formula_weight         1407.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                108.612(5)
_cell_angle_beta                 115.266(4)
_cell_angle_gamma                93.770(5)
_cell_formula_units_Z            2
_cell_length_a                   12.121(3)
_cell_length_b                   12.655(3)
_cell_length_c                   13.290(3)
_cell_measurement_reflns_used    1487
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      2.27
_cell_measurement_theta_min      25.14
_cell_volume                     1697.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1332
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       -14
_diffrn_reflns_limit_h_min       16
_diffrn_reflns_limit_k_max       -16
_diffrn_reflns_limit_k_min       16
_diffrn_reflns_limit_l_max       -17
_diffrn_reflns_limit_l_min       14
_diffrn_reflns_number            15815
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.747
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  0.8231
_exptl_absorpt_correction_T_min  0.7343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.753
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.764
_refine_diff_density_min         -1.691
_refine_diff_density_rms         0.343
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         8188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1162
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+5.9428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5198
_reflns_number_total             8188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02229_si_003.cif
_cod_data_source_block           mo_may41_0m
_cod_depositor_comments
;

2023-09-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'Mo12 Na6 O76 P10'
_cod_original_formula_weight         2814.92
_cod_original_formula_moiety         'Mo12 Na6 O76 P10'
_cod_original_formula_units_Z            1
_cod_database_code               4344600
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Sof: Na37(0.5) Na3(0.5) Na2(0.5) Na1(0.5) Na40(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'