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_7122569
_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         'C67 H63 Cl N3 O4 P3 U W'
_chemical_formula_sum            'C67 H63 Cl N3 O4 P3 U W'
_chemical_formula_weight         1524.44
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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             2016-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2018-06-08 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                76.466(10)
_cell_angle_beta                 88.965(10)
_cell_angle_gamma                67.082(12)
_cell_formula_units_Z            2
_cell_length_a                   13.6390(17)
_cell_length_b                   14.6571(18)
_cell_length_c                   16.721(2)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.9930
_cell_measurement_theta_min      3.7010
_cell_volume                     2983.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9969
_diffrn_measured_fraction_theta_max 0.9969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00  90.00   1.00   42.50    --   21.08  57.00 -90.00   90
  2  \w    -20.00  63.00   1.00   42.50    --   21.08 -99.00 150.00   83
  3  \w     -9.00  84.00   1.00   42.50    --   21.08  77.00   0.00   93
  4  \w    -39.00  35.00   1.00   42.50    --   21.08 -57.00  30.00   74
  5  \w    -51.00  54.00   1.00   42.50    --   21.08 -19.00  90.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0355562000
_diffrn_orient_matrix_UB_12      0.0248398000
_diffrn_orient_matrix_UB_13      -0.0105125000
_diffrn_orient_matrix_UB_21      0.0062801000
_diffrn_orient_matrix_UB_22      0.0005198000
_diffrn_orient_matrix_UB_23      0.0418858000
_diffrn_orient_matrix_UB_31      0.0436541000
_diffrn_orient_matrix_UB_32      -0.0481845000
_diffrn_orient_matrix_UB_33      0.0071723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.1683
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22831
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.076
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         10523
_refine_ls_number_restraints     758
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1355
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0192P)^2^+3.5146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6399
_reflns_number_total             10523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05268a2.cif
_cod_data_source_block           UW
_cod_depositor_comments
'Adding full bibliography for 7122562--7122573.cif.'
_cod_original_cell_volume        2983.4(7)
_cod_database_code               7122569
_manchester_internal_diff_code   ASTL147
_manchester_internal_stl_name    UMZ6
_manchester_internal_stl_number  291
_manchester_internal_coll_client 'Markus Zegke'
_manchester_internal_coll_user   'Markus Zegke'
_manchester_internal_coll_date   01/12/2016
_manchester_internal_process_date 01/12/2016
_manchester_internal_process_user 'Markus Zegke'
_manchester_internal_solution_date 01/12/2016
_manchester_internal_solution_user 'Markus Zegke'
_manchester_internal_refinement_date 01/12/2016
_manchester_internal_refinement_user 'Markus Zegke'
_manchester_internal_validation_date 01/12/2016
_manchester_internal_validation_user 'Markus Zegke'
_manchester_internal_archive_date 05/12/2016
_manchester_internal_archive_user AW
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C66H63Cl1N3O3P3U1W1
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
W1 \\sim C67 \\sim O4 \\sim C66 \\sim O3 \\sim C64 \\sim O1 \\sim C65 \\sim O2:
within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
3. 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
4.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)
4.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              16575
_olex2_date_sample_submission    2016-11-30
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.662