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_4344599
_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         'Mo12 O66 P8 U, 3(Na)'
_chemical_formula_sum            'Mo12 Na3 O66 P8 U'
_chemical_formula_weight         2762.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 127.526(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.094(8)
_cell_length_b                   12.801(3)
_cell_length_c                   23.336(6)
_cell_measurement_reflns_used    2131
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      43.68
_cell_measurement_theta_min      3.09
_cell_volume                     8551(4)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.426
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_laue_measured_fraction_full 0.426
_diffrn_reflns_laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10530
_diffrn_reflns_point_group_measured_fraction_full 0.426
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         44.294
_diffrn_reflns_theta_min         3.782
_exptl_absorpt_coefficient_mu    21.599
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.4786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_description       block
_exptl_crystal_F_000             5108
_exptl_crystal_size_max          0.005
_exptl_crystal_size_mid          0.0025
_exptl_crystal_size_min          0.002
_refine_diff_density_max         6.287
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1400
_refine_ls_R_factor_gt           0.1084
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2788
_refine_ls_wR_factor_ref         0.3016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2214
_reflns_number_total             3294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02229_si_002.cif
_cod_data_source_block           sq
_cod_depositor_comments
;

2024-01-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         1381.02
_cod_original_formula_moiety         'Mo6 Na1.5 O33 P4 U0.5'
_cod_original_formula_units_Z            8
_cod_original_formula_sum        'Mo6 Na1.50 O33 P4 U0.50'
_cod_database_code               4344599
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
2. Others
 Fixed Sof: Na3(0.5) Na2(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'