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_7122563
_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 I Mo N3 O3 P3 U, C7 H8'
_chemical_formula_sum            'C73 H71 I Mo N3 O3 P3 U'
_chemical_formula_weight         1592.10
_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     dual
_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                89.180(3)
_cell_angle_beta                 75.294(4)
_cell_angle_gamma                88.901(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6048(5)
_cell_length_b                   13.3050(5)
_cell_length_c                   21.6579(10)
_cell_measurement_reflns_used    11502
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.7400
_cell_measurement_theta_min      3.5790
_cell_volume                     3512.4(3)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_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 0.999
_diffrn_measurement_details
;
  1 omega  -50.00   35.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8757   38.0000   60.0000 85

  2 omega  -69.00   -2.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8757   57.0000 -120.0000 67

  3 omega   55.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8757 -125.0000   60.0000 43

  4 omega   33.00   63.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8757 -125.0000  -30.0000 30

  5 omega   24.00   51.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  -95.0000  -30.0000 27

  6 omega   34.00   65.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218 -120.0000  -37.0000 31

  7 omega   76.00  106.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  -95.0000  -30.0000 30

  8 omega   91.00  118.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218 -120.0000  -37.0000 27

  9 omega   34.00  139.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  -77.0000 -150.0000 105

 10 omega   89.00  172.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218   45.0000 -150.0000 83

 11 omega  139.00  167.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218   77.0000 -120.0000 28

 12 omega  120.00  159.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  111.0000 -150.0000 39

 13 omega  114.00  150.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  178.0000  -60.0000 36

 14 omega   77.00  121.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218   77.0000 -120.0000 44

 15 omega   33.00   83.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  -45.0000  -60.0000 50

 16 omega   18.00  138.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218    0.0000 -150.0000 120

 17 omega   34.00   98.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  -45.0000   90.0000 64

 18 omega   55.00  109.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218 -111.0000  150.0000 54

 19 omega   35.00   98.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218 -111.0000   90.0000 63

 20 omega  113.00  170.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3218  111.0000  150.0000 57

 21 omega -115.00  -11.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8757  -57.0000  -90.0000 104

 22 omega -115.00  -26.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8757  -38.0000   90.0000 89
;
_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      0.0323926000
_diffrn_orient_matrix_UB_12      0.0175125000
_diffrn_orient_matrix_UB_13      -0.0728009000
_diffrn_orient_matrix_UB_21      -0.0981106000
_diffrn_orient_matrix_UB_22      -0.0628138000
_diffrn_orient_matrix_UB_23      -0.0062172000
_diffrn_orient_matrix_UB_31      -0.0727730000
_diffrn_orient_matrix_UB_32      0.0957119000
_diffrn_orient_matrix_UB_33      0.0083719000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12381
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.355
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.1352
_exptl_crystal_size_mid          0.0783
_exptl_crystal_size_min          0.0296
_refine_diff_density_max         8.965
_refine_diff_density_min         -4.259
_refine_diff_density_rms         0.445
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12381
_refine_ls_number_restraints     1381
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.1542
_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^)+(0.0001P)^2^+435.4435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3786
_refine_ls_wR_factor_ref         0.3836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10599
_reflns_number_total             12381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           UIMo
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_database_code               7122563
_nottingham_internal_coll_name   UAAAMM
_nottingham_internal_coll_number 13422
_nottingham_internal_coll_client AA/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '60.0000, 240.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_user   pcxaa19
_nottingham_internal_coll_date   02/04/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user pcxaa19
_nottingham_internal_process_date 08/04/2014
_nottingham_internal_solution_user AW
_nottingham_internal_solution_date 30/09/2016
_nottingham_internal_refinement_user AW
_nottingham_internal_refinement_date 30/09/2016
_nottingham_internal_validation_user AW
_nottingham_internal_validation_date 30/09/2016
_nottingham_internal_archive_date 30/09/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C66 H63 N3 P3 O3 I U Mo'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.656(5) 0.344(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C75-C74 = C68-C67
 1.55 with sigma of 0.02
 C76-C75 = C77-C76 = C78-C77 = C79-C78 = C80-C79 = C80-C75 = C73-C72 = C72-C71
 = C71-C70 = C70-C69 = C69-C68 = C73-C68
 1.39 with sigma of 0.02
 C39-C38 = C40-C39 = C41-C40 = C42-C41 = C42-C37 = C38-C37
 1.39 with sigma of 0.02
 C76-C74 \\sim C74-C80 \\sim C69-C67 \\sim C67-C73
 with sigma of 0.01
4. Restrained planarity
 C74, C75, C76, C77, C78, C79, C80
 with sigma of 0.1
 C67, C68, C69, C70, C71, C72, C73
 with sigma of 0.1
 C16, C17, C18, C19, C20, C21
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5) C75(0.5) C76(0.5) H76(0.5)
 C77(0.5) H77(0.5) C78(0.5) H78(0.5) C79(0.5) H79(0.5) C80(0.5) H80(0.5)
 C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5) C68(0.5) C69(0.5) H69(0.5) C70(0.5)
 H70(0.5) C71(0.5) H71(0.5) C72(0.5) H72(0.5) C73(0.5) H73(0.5)
8.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), C76(H76), C77(H77),
 C78(H78), C79(H79), C80(H80), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73)
8.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), C74(H74A,H74B,H74C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              12929
_olex2_submission_special_instructions 'No special instructions were received'