Actinide-transition metal bonding in heterobimetallic uranium- and thorium-molybdenum paddlewheel complexes.
Ayres, Alexander J.; Zegke, Markus; Ostrowski, Joseph P. A.; Tuna, Floriana; McInnes, Eric J. L.; Wooles, Ashley J.; Liddle, Stephen T.; Chemical communications (Cambridge, England) 54 (2018) 13515–13518; doi:10.1039/c8cc05268a

data_7122572
_publ_section_title
;
 Actinide-transition metal bonding in heterobimetallic uranium- and
 thorium-molybdenum paddlewheel complexes.
;
_journal_issue                   96
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13515
_journal_page_last               13518
_journal_paper_doi               10.1039/c8cc05268a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C63 H63 I N3 P3 Th'
_chemical_formula_sum            'C63 H63 I N3 P3 Th'
_chemical_formula_weight         1314.01
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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_audit_update_record
;
2018-11-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6633(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega   21.00  107.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega   88.00  167.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega   81.00  153.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      105.3295  125.0000  120.0000 72

  4 omega   43.00   84.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega   36.00   95.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   58.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   27.00   76.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   75.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega    0.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
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 10 omega   38.00  106.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
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 11 omega  -50.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -90.0000 37

 12 omega  -90.00  -13.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -90.0000 77
;
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_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_wavelength     1.54184
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_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_number            23954
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_diffrn_source                   'microfocus sealed tube'
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
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;
_exptl_crystal_colour            colourless
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             11115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           ThI
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_original_cell_volume        5584.76(10)
_cod_database_code               7122572
_nottingham_internal_coll_name   THAALE
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_nottingham_internal_coll_frame_time '2.0000, 8.0000'
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_nottingham_internal_validation_date 29/09/2016
_nottingham_internal_validation_user AW
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
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 At 1.5 times of:
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2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C28(H28), C32(H32), C33(H33),
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  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C),
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 H48C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              22838
_olex2_date_sample_data_collection 07/05/2014
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_olex2_exptl_crystal_mounting_method 'In fomblin film on micromount'
_olex2_submission_special_instructions 'No special instructions were received'