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_7122566
_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 U, 2(C7 H8)'
_chemical_formula_sum            'C77 H79 Cl N3 P3 U'
_chemical_formula_weight         1412.82
_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
_audit_creation_date             2016-10-03
_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                 96.5882(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9544(3)
_cell_length_b                   22.7597(4)
_cell_length_c                   18.2868(3)
_cell_measurement_reflns_used    14079
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.4115
_cell_measurement_theta_min      3.4813
_cell_volume                     6596.4(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'ShelXS (Sheldrick, 2008) '
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega -106.00  -20.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  -57.0000  150.0000 86

  2 omega  -80.00   -2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127  125.0000  -60.0000 78

  3 omega  -57.00   -4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.9127   57.0000   90.0000 53

  4 omega   34.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -120.0000 35

  5 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000    0.0000 27

  6 omega   46.00   98.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -61.0000   30.0000 52

  7 omega   33.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -30.0000 35

  8 omega   42.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -150.0000 27

  9 omega   85.00  131.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   30.0000 -150.0000 46

 10 omega   36.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -90.0000 33

 11 omega   38.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   90.0000 31

 12 omega   67.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   15.0000  150.0000 85

 13 omega   39.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -120.0000 25

 14 omega   69.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -61.0000   60.0000 48

 15 omega   85.00  147.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000 -120.0000 62
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0898576000
_diffrn_orient_matrix_UB_12      -0.0221216000
_diffrn_orient_matrix_UB_13      -0.0257172000
_diffrn_orient_matrix_UB_21      -0.0132467000
_diffrn_orient_matrix_UB_22      0.0518480000
_diffrn_orient_matrix_UB_23      -0.0543484000
_diffrn_orient_matrix_UB_31      0.0347385000
_diffrn_orient_matrix_UB_32      -0.0374505000
_diffrn_orient_matrix_UB_33      -0.0597870000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29230
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.583
_diffrn_reflns_theta_min         3.484
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.330
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.404
_exptl_crystal_size_mid          0.2529
_exptl_crystal_size_min          0.2157
_refine_diff_density_max         1.887
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         13076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+25.6520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11780
_reflns_number_total             13076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           UCl
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_database_code               7122566
_nottingham_internal_coll_number 10945
_nottingham_internal_coll_client AA/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '20 and 5'
_nottingham_internal_coll_frame_width 1.0
_nottingham_internal_coll_user   WL
_nottingham_internal_coll_date   2/12/2011
_nottingham_internal_process_date 02/12/2011
_nottingham_internal_process_user WL
_nottingham_internal_solution_date 03/12/2012
_nottingham_internal_solution_user AA/WL
_nottingham_internal_refinement_date 29/09/2016
_nottingham_internal_refinement_user AA/WL/AW
_nottingham_internal_validation_date 29/09/2016
_nottingham_internal_validation_user AW
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C77 H79 Cl N3 P3 U'
_chemical_oxdiff_usercomment
'UAAALA #10945 IN FOMBLIN FIML ON MICROMOUNT FOR AA/STL'
_reflns_odcompleteness_completeness 99.83
_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), C66(H66), C67(H67),
 C68(H68), C69(H69), C70(H70), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77)
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), C64(H64A,H64B,H64C), C71(H71A,H71B,H71C)
;
_shelx_res_checksum              88627
_nottingham_internal_coll_name   UAAALA
_olex2_submission_special_instructions 'No special instructions were received'