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_7122564
_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         'C66 H63 Cl Mo N3 O3 P3 U, 2(C7 H8)'
_chemical_formula_sum            'C80 H79 Cl Mo N3 O3 P3 U'
_chemical_formula_weight         1592.79
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-30
_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                89.2225(14)
_cell_angle_beta                 74.9637(18)
_cell_angle_gamma                89.8281(15)
_cell_formula_units_Z            2
_cell_length_a                   12.2335(2)
_cell_length_b                   13.3432(2)
_cell_length_c                   21.8523(4)
_cell_measurement_reflns_used    22169
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1950
_cell_measurement_theta_min      3.3590
_cell_volume                     3444.59(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega  -18.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 26

  2 omega  -50.00   33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 83

  3 omega -109.00  -12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000  120.0000 97

  4 omega   61.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4289 -125.0000 -180.0000 27

  5 omega   36.00  109.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -95.0000   60.0000 73

  6 omega   34.00   89.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -30.0000   90.0000 55

  7 omega   45.00  142.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -15.0000  -60.0000 97

  8 omega   59.00   88.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -30.0000    0.0000 29

  9 omega   38.00  119.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -61.0000  -90.0000 81

 10 omega   72.00   99.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -95.0000    0.0000 27

 11 omega   31.00   69.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -30.0000   60.0000 38

 12 omega   12.00  117.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4289   77.0000  -30.0000 105

 13 omega   17.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4289   57.0000 -120.0000 97

 14 omega  -27.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.4289  -57.0000 -150.0000 97

 15 omega   61.00  161.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185   15.0000   90.0000 100

 16 omega  -28.00   -1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 27

 17 omega    2.00   28.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 26

 18 omega   36.00   82.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -30.0000  -90.0000 46

 19 omega   91.00  117.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185   30.0000  -30.0000 26

 20 omega  142.00  177.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185   30.0000  -30.0000 35

 21 omega   73.00   99.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -95.0000  120.0000 26

 22 omega   28.00  107.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -95.0000  -90.0000 79

 23 omega   66.00  115.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185 -125.0000  -90.0000 49

 24 omega   32.00   90.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -30.0000  150.0000 58

 25 omega   44.00  128.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185  -77.0000   90.0000 84

 26 omega  147.00  173.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      106.0185   61.0000   60.0000 26

 27 omega  -50.00   34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 84

 28 omega   23.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7414 -125.0000   90.0000 76

 29 omega   12.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7414   77.0000  -90.0000 106

 30 omega  -29.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7414  -38.0000  -60.0000 95

 31 omega   12.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7414   77.0000  150.0000 106

 32 omega   21.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7414   38.0000   60.0000 87

 33 omega   12.00  118.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7414   77.0000   60.0000 106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0541196000
_diffrn_orient_matrix_UB_12      -0.0082479000
_diffrn_orient_matrix_UB_13      -0.0717323000
_diffrn_orient_matrix_UB_21      0.1185985000
_diffrn_orient_matrix_UB_22      0.0010481000
_diffrn_orient_matrix_UB_23      0.0120615000
_diffrn_orient_matrix_UB_31      -0.0028670000
_diffrn_orient_matrix_UB_32      -0.1151680000
_diffrn_orient_matrix_UB_33      0.0062164000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43652
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.507
_diffrn_reflns_theta_min         3.741
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.473
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.1013
_exptl_crystal_size_mid          0.0848
_exptl_crystal_size_min          0.0526
_refine_diff_density_max         2.036
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         13636
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+8.3146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12578
_reflns_number_total             13636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           UClMo
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_original_cell_volume        3444.58(11)
_cod_database_code               7122564
_nottingham_internal_coll_name   UAAAML
_nottingham_internal_coll_number 13380
_nottingham_internal_coll_client AA/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '30.0000, 120.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxaa19
_nottingham_internal_coll_date   19/03/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 21/03/2014
_nottingham_internal_process_user pcxaa19
_nottingham_internal_solution_date 21/03/2014
_nottingham_internal_solution_user AA
_nottingham_internal_refinement_date 30/09/2016
_nottingham_internal_refinement_user AW
_nottingham_internal_validation_date 30/09/2016
_nottingham_internal_validation_user AW
_nottingham_internal_archive_date 30/09/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C80 H79 N3 P3 O3 Cl U Mo'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C72-C71 = C72-C67 = C68-C67 = C69-C68 = C70-C69 = C71-C70 = C79A-C78A = C79A-
 C74A = C75A-C74A = C78A-C77A = C79-C78 = C76-C75 = C76A-C75A = C77A-C76A = C78-
 C77 = C75-C74 = C79-C74 = C77-C76
 1.39 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C78 \\sim C77 \\sim C79 \\sim C80 \\sim C74A \\sim C75A \\sim C76A \\sim C77A
\\sim C78A \\sim C79A \\sim C80A \\sim C76 \\sim C67 \\sim C68 \\sim C69 \\sim
C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C78, C77, C79, C80, C74A, C75A, C76A, C77A, C78A, C79A, C80A, C76, C67, C68,
 C69, C70, C71, C72, C73, C74, C75
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C74A)=Sof(C75A)=Sof(H75A)=Sof(C76A)=Sof(H76A)=Sof(C77A)=Sof(H77A)=
 Sof(C78A)=Sof(H78A)=Sof(C79A)=Sof(H79A)=Sof(C80A)=Sof(H80D)=Sof(H80E)=
 Sof(H80F)=1-FVAR(1)
 Sof(C78)=Sof(H78)=Sof(C77)=Sof(H77)=Sof(C79)=Sof(H79)=Sof(C80)=Sof(H80A)=
 Sof(H80B)=Sof(H80C)=Sof(C76)=Sof(H76)=Sof(C74)=Sof(C75)=Sof(H75)=FVAR(1)
6.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), C78(H78), C77(H77),
 C79(H79), C75A(H75A), C76A(H76A), C77A(H77A), C78A(H78A), C79A(H79A), C76(H76),
  C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C75(H75)
6.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), C80(H80A,H80B,H80C), C80A(H80D,H80E,H80F),
 C73(H73A,H73B,H73C)
;
_shelx_res_checksum              79575
_olex2_submission_special_instructions 'No special instructions were received'