Assessing Crystal Field and Magnetic Interactions in Diuranium-μ-Chalcogenide Triamidoamine Complexes With UIV-E-UIV Cores (E = S, Se, Te): Implications for Determining the Presence or Absence of Actinide-Actinide Magnetic Exchange
Gardner, Benedict; King, David M.; Tuna, Floriana; Wooles, Ashley; Chilton, Nicholas F.; Liddle, Stephen; Chem. Sci.  (2017) –; doi:10.1039/C7SC01998J

data_1546483
_publ_section_title
;
 Assessing Crystal Field and Magnetic Interactions in
 Diuranium-\m-Chalcogenide Triamidoamine Complexes With UIV-E-UIV Cores (E
 = S, Se, Te): Implications for Determining the Presence or Absence of
 Actinide-Actinide Magnetic Exchange
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01998J
_journal_year                    2017
_chemical_formula_moiety         'C66 H150 N8 Si6 Te U2'
_chemical_formula_sum            'C66 H150 N8 Si6 Te U2'
_chemical_formula_weight         1828.13
_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             2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.474(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8022(3)
_cell_length_b                   16.3751(5)
_cell_length_c                   18.0985(6)
_cell_measurement_reflns_used    8669
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.8710
_cell_measurement_theta_min      3.7240
_cell_volume                     4086.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -85.00   -8.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -30.0000 77

  2 omega  -46.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -120.0000 49

  3 omega  -98.00  -17.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -77.0000  120.0000 81

  4 omega   61.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1627 -125.0000 -180.0000 28

  5 omega   90.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972   30.0000  -30.0000 83

  6 omega  118.00  153.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  125.0000   90.0000 35

  7 omega   42.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -30.0000    0.0000 49

  8 omega   38.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972 -125.0000   30.0000 82

  9 omega   55.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000  -30.0000 34

 10 omega   39.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -45.0000   60.0000 32

 11 omega   56.00  129.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -61.0000 -180.0000 73

 12 omega   28.00  102.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -95.0000 -150.0000 74

 13 omega   38.00   84.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0972  -30.0000   60.0000 46
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0779384000
_diffrn_orient_matrix_UB_12      0.0107500000
_diffrn_orient_matrix_UB_13      0.0577042000
_diffrn_orient_matrix_UB_21      0.0191801000
_diffrn_orient_matrix_UB_22      0.0926270000
_diffrn_orient_matrix_UB_23      0.0015960000
_diffrn_orient_matrix_UB_31      -0.0777229000
_diffrn_orient_matrix_UB_32      0.0120243000
_diffrn_orient_matrix_UB_33      -0.0627287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16902
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.005
_diffrn_reflns_theta_min         3.642
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    14.963
_exptl_absorpt_correction_T_max  0.263
_exptl_absorpt_correction_T_min  0.079
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1844
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.2502
_exptl_crystal_size_min          0.2097
_refine_diff_density_max         5.899
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     1911
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0814
_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^)+(0.1138P)^2^+64.7301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2110
_refine_ls_wR_factor_ref         0.2190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7122
_reflns_number_total             8115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01998j2.cif
_cod_data_source_block           6
_cod_database_code               1546483
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C66 H150 N8 Si6 Te U2'
_chemical_oxdiff_usercomment
'UBMGNF #12563 for BMG/STL in fomblin oil on micromount'
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si2-N2 \\sim Si2A-N2 \\sim Si1-N1 \\sim Si1A-N1 \\sim Si3A-N3 \\sim Si3-N3
 with sigma of 0.01
 Si3A-C29A \\sim Si3-C29 \\sim Si3-C23 \\sim Si3A-C23A \\sim Si3-C26 \\sim
Si3A-C26A \\sim Si1-C4 ~
 Si1A-C4A \\sim Si1-C1 \\sim Si1A-C1A \\sim Si1A-C7A \\sim Si1-C7 \\sim Si2-C18
\\sim Si2-C12 \\sim Si2A-
 C12A \\sim Si2A-C18A \\sim Si2A-C15A \\sim Si2-C15
 with sigma of 0.02
 C19A-C18A \\sim C20A-C18A \\sim C19-C18 \\sim C20-C18 \\sim C13-C12 \\sim
C14-C12 \\sim C13A-C12A ~
 C14A-C12A \\sim C16-C15 \\sim C17-C15 \\sim C17A-C15A \\sim C16A-C15A \\sim
C31-C29 \\sim C30-C29 ~
 C30A-C29A \\sim C31A-C29A \\sim C28-C26 \\sim C27-C26 \\sim C28A-C26A \\sim
C27A-C26A \\sim C24A-C23A
 \\sim C25A-C23A \\sim C25-C23 \\sim C24-C23 \\sim C8A-C7A \\sim C8-C7 \\sim
C9-C7 \\sim C9A-C7A \\sim C5A-C4A
 \\sim C5-C4 \\sim C6A-C4A \\sim C6-C4 \\sim C2-C1 \\sim C2A-C1A \\sim C3-C1
\\sim C3A-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si1 \\sim Si1A \\sim C1 \\sim C2 \\sim C2A \\sim C4 \\sim C4A \\sim C5 \\sim
C5A \\sim C6 \\sim C6A \\sim C7 \\sim C7A \\sim C8 \\sim C8A \\sim C9 \\sim C9A
\\sim C1A \\sim C3 \\sim C3A \\sim Si2 \\sim C12 \\sim C12A \\sim C13 \\sim
C13A \\sim C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A \\sim C17
\\sim C17A \\sim C18 \\sim C19 \\sim C18A \\sim C19A \\sim C20 \\sim C20A \\sim
Si2A \\sim Si3 \\sim Si3A \\sim C23 \\sim C23A \\sim C24 \\sim C24A \\sim C25
\\sim C25A \\sim C26 \\sim C26A \\sim C27 \\sim C27A \\sim C28 \\sim C28A \\sim
C29 \\sim C29A \\sim C30 \\sim C30A \\sim C31 \\sim C31A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Si2, Si2A, C12, C12A, C13, C13A, C14, C14A, C15, C15A, C16, C16A, C17, C17A,
 C18, C18A, C19, C19A, C20, C20A, Si3, C25, C26, C26A, C28, C28A, C29, C29A,
 C30, C30A, C31, C31A, Si3A, C23, C23A, C24, C24A, C25A, C27, C27A, Si1, Si1A,
 C1, C1A, C2, C2A, C3, C3A, C4, C4A, C5, C5A, C6, C6A, C7, C7A, C8, C8A, C9,
 C9A, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Si3A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=
 Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(Si3)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(Si1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7A)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(Si1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
 Sof(Si2A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
 Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(3)
 Sof(Si2)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C1A(H1A), C4(H4), C4A(H4A), C7(H7), C7A(H7A), C12(H12), C12A(H12A),
 C15(H15), C15A(H15A), C18(H18), C18A(H18A), C23(H23), C23A(H23A), C26(H26),
 C26A(H26A), C29(H29), C29A(H29A)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
 H32B), C33(H33A,H33B)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC),
 C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC),
 C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
 C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,H14E,
 H14F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C17(H17A,H17B,H17C),
 C17A(H17D,H17E,H17F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,
 H20C), C20A(H20D,H20E,H20F), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F),
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C27(H27A,H27B,H27C), C27A(H27D,H27E,
 H27F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C30(H30A,H30B,H30C),
 C30A(H30D,H30E,H30F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F)
;
_shelx_res_checksum              92642
_olex2_submission_special_instructions 'No special instructions were received'