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_7122565
_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 Th, C7 H8'
_chemical_formula_sum            'C73 H71 I Mo N3 O3 P3 Th'
_chemical_formula_weight         1586.11
_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   direct
_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                88.662(4)
_cell_angle_beta                 75.262(4)
_cell_angle_gamma                88.660(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7259(5)
_cell_length_b                   13.3141(6)
_cell_length_c                   21.7153(10)
_cell_measurement_reflns_used    9327
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8210
_cell_measurement_theta_min      3.9140
_cell_volume                     3556.7(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 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega  -86.00  -60.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -30.0000 26

  2 omega  -27.00   67.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5554  -57.0000  120.0000 94

  3 omega    2.00   57.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5554  -38.0000   30.0000 55

  4 omega   17.00  110.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5554   57.0000  -90.0000 93

  5 omega  -29.00   57.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5554  -38.0000  -30.0000 86

  6 omega   86.00  178.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000  120.0000 92

  7 omega   65.00  101.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   90.0000 36

  8 omega   37.00   82.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -180.0000 45

  9 omega   35.00   61.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   90.0000 26

 10 omega   32.00   83.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 51

 11 omega   35.00  126.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000   60.0000 91

 12 omega   38.00   82.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -150.0000 44

 13 omega   80.00  116.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   97.0000  135.0000 36

 14 omega  152.00  178.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   97.0000  135.0000 26

 15 omega   44.00  121.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000 -120.0000 77

 16 omega   42.00   83.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 41

 17 omega   75.00  170.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000 -120.0000 95

 18 omega   56.00   86.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -120.0000 30

 19 omega  101.00  128.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -120.0000 27

 20 omega   84.00  109.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000   60.0000 25

 21 omega   39.00  120.00   1.0000  240.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000    0.0000 81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0836486000
_diffrn_orient_matrix_UB_12      -0.0844673000
_diffrn_orient_matrix_UB_13      0.0096504000
_diffrn_orient_matrix_UB_21      -0.0506433000
_diffrn_orient_matrix_UB_22      0.0353508000
_diffrn_orient_matrix_UB_23      0.0683801000
_diffrn_orient_matrix_UB_31      -0.0781800000
_diffrn_orient_matrix_UB_32      0.0708223000
_diffrn_orient_matrix_UB_33      -0.0247795000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.1285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.397
_diffrn_reflns_theta_min         3.900
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.539
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   gaussian
_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)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.0837
_exptl_crystal_size_mid          0.0557
_exptl_crystal_size_min          0.0318
_refine_diff_density_max         6.943
_refine_diff_density_min         -3.950
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         13995
_refine_ls_number_restraints     790
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.1262
_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^)+(0.0537P)^2^+199.9799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3284
_refine_ls_wR_factor_ref         0.3409
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10758
_reflns_number_total             13995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           ThIMo
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_database_code               7122565
_nottingham_internal_coll_name   THAALI
_nottingham_internal_coll_number 14066
_nottingham_internal_coll_client AA/STL
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '60.0000, 240.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxaa19
_nottingham_internal_coll_date   14/10/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 17/10/2014
_nottingham_internal_process_user pcxaa19
_nottingham_internal_solution_date 30/09/2016
_nottingham_internal_solution_user AW
_nottingham_internal_refinement_date 30/09/2016
_nottingham_internal_refinement_user AW
_nottingham_internal_self_archive_date 30/09/2016
_nottingham_internal_self_validation_date 30/09/2016
_nottingham_internal_self_validation_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         'C66 H63 N3 P3 O3 Th I Mo'
_chemical_oxdiff_usercomment
'THAALI #14066 IN FOMBLIN FILM ON MICROMOUNT FOR AA/STL GVB-325'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.618(4) 0.382(4)
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
 C73-C68 = C73-C72 = C72-C71 = C71-C70 = C70-C69 = C69-C68 = C77-C76 = C76-C75
 = C80-C75 = C80-C79 = C79-C78 = C78-C77
 1.39 with sigma of 0.02
 C68-C67 = C75-C74
 1.55 with sigma of 0.02
 C68-C71 \\sim C70-C73 \\sim C72-C69 \\sim C75-C78 \\sim C77-C80 \\sim C79-C76
 with sigma of 0.02
 C73-C67 \\sim C67-C69 \\sim C76-C74 \\sim C74-C80
 with sigma of 0.02
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
5. 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
6. 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)
7.a Me refined with riding coordinates:
 C67(H67A,H67B,H67C)
7.b 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)
7.c 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)
;
_shelx_res_checksum              67392
_olex2_submission_special_instructions 'No special instructions were received'