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_7122570
_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 Cl N3 P3 Th'
_chemical_formula_sum            'C63 H63 Cl N3 P3 Th'
_chemical_formula_weight         1222.56
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-11-07 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4230(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.04797(8)
_cell_length_b                   25.46193(15)
_cell_length_c                   16.86018(11)
_cell_measurement_reflns_used    46891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2670
_cell_measurement_theta_min      3.1460
_cell_volume                     5554.46(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
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;
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omega____ theta____ kappa____ phi______ frames
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  2 omega   31.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -21.00    5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega   35.00   65.00   1.0000   10.0000
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  5 omega  122.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   39.00   82.00   1.0000   40.0000
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  7 omega   32.00  133.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   28.00   87.00   1.0000   40.0000
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  9 omega   49.00   85.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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 10 omega   42.00  127.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276  -61.0000   30.0000 85

 11 omega   92.00  163.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   77.0000 -120.0000 71

 12 omega  -31.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573  -38.0000 -150.0000 92

 13 omega  -28.00   65.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573  -57.0000    0.0000 93

 14 omega   10.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573   77.0000  120.0000 102

 15 omega   76.00  171.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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 16 omega   80.00  172.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   45.0000  -30.0000 92

 17 omega   80.00  172.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   45.0000 -150.0000 92

 18 omega   76.00  171.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   61.0000  -90.0000 95

 19 omega   33.00  121.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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 20 omega   62.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
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 21 omega  -92.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
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 22 omega   10.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573   77.0000   30.0000 102

 23 omega   15.00  109.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.2573   57.0000 -150.0000 94

 24 omega   72.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   77.0000  -30.0000 102

 25 omega   76.00  171.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   61.0000  150.0000 95

 26 omega   72.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   77.0000 -150.0000 102

 27 omega   23.00   75.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276  -94.0000 -120.0000 52

 28 omega   72.00  174.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      102.6276   77.0000   60.0000 102
;
_diffrn_measurement_device       '\k-geometry diffractometer'
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_diffrn_orient_matrix_UB_21      -0.0834881000
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_diffrn_orient_matrix_UB_33      -0.0508728000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0258
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_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83099
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_diffrn_reflns_theta_max         74.525
_diffrn_reflns_theta_min         3.162
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    10.234
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_exptl_absorpt_correction_type   gaussian
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
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_exptl_crystal_description       block
_exptl_crystal_F_000             2456
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_exptl_crystal_size_mid          0.0556
_exptl_crystal_size_min          0.0464
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_refine_ls_extinction_method     none
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+2.1518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                10585
_reflns_number_total             11261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           ThCl
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_database_code               7122570
_nottingham_internal_coll_name   THAALA
_nottingham_internal_coll_number 13011
_nottingham_internal_coll_client AA/STL
_nottingham_internal_coll_type   CUSTOM
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '10 AND 40'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_user   AA
_nottingham_internal_coll_date   20/11/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 21/11/2013
_nottingham_internal_process_user AA
_nottingham_internal_solution_date 21/11/2013
_nottingham_internal_solution_user AA
_nottingham_internal_refinement_date 29/09/2016
_nottingham_internal_refinement_user AA/AW
_nottingham_internal_validation_date 29/09/2016
_nottingham_internal_validation_user AW
_nottingham_internal_archive_date 29/09/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C63 H63 N3 P3 Th1 Cl'
_chemical_oxdiff_usercomment
'THAALA #13011 IN FOMBLIN FILM ON MICROMOUNT FOR AA/STL'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
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),
  C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C46(H46), C49(H49), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  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),
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C48(H48A,H48B,
 H48C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              99239
_olex2_submission_special_instructions 'No special instructions were received'