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_1546479
_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 Se Si6 U2, C7 H8'
_chemical_formula_sum            'C73 H158 N8 Se Si6 U2'
_chemical_formula_weight         1871.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.942(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2002(16)
_cell_length_b                   19.5179(10)
_cell_length_c                   17.5099(9)
_cell_measurement_reflns_used    6591
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3240
_cell_measurement_theta_min      4.4960
_cell_volume                     8507.7(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -112.00   18.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877    0.0000  -90.0000 65

  2 omega  -62.00   12.00   2.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877   38.0000  -30.0000 37

  3 omega   43.00   71.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -90.0000 14

  4 omega   37.00   67.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   60.0000 15

  5 omega   33.00   63.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -120.0000 15

  6 omega   28.00  108.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -150.0000 40

  7 omega   40.00   66.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -60.0000 13

  8 omega   33.00   59.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   90.0000 13

  9 omega   33.00   65.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -150.0000 16

 10 omega   36.00   62.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   30.0000 13

 11 omega   36.00   80.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -125.0000   30.0000 22

 12 omega   39.00   65.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  120.0000 13

 13 omega   45.00   91.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000  -60.0000 23

 14 omega   31.00  153.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472    0.0000 -150.0000 61

 15 omega   37.00   77.00   2.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 20
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0525701000
_diffrn_orient_matrix_UB_12      -0.0201895000
_diffrn_orient_matrix_UB_13      -0.0286329000
_diffrn_orient_matrix_UB_21      0.0001519000
_diffrn_orient_matrix_UB_22      0.0691554000
_diffrn_orient_matrix_UB_23      -0.0424426000
_diffrn_orient_matrix_UB_31      0.0325423000
_diffrn_orient_matrix_UB_32      0.0323086000
_diffrn_orient_matrix_UB_33      0.0729646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19074
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.551
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.242
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.587
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.2777
_exptl_crystal_size_mid          0.2309
_exptl_crystal_size_min          0.1102
_refine_diff_density_max         2.108
_refine_diff_density_min         -2.193
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7505
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0426P)^2^+62.1143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7013
_reflns_number_total             7505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01998j2.cif
_cod_data_source_block           5
_cod_original_cell_volume        8507.6(8)
_cod_database_code               1546479
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C66 H150 N8 Se1 Si6 U2'
_chemical_oxdiff_usercomment
'UBMGMZ #12223 for BMG/STL in fomblin oil on micromount'
_reflns_odcompleteness_completeness 99.95
_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
 C1H-C1G = C1H-C1C = C1D-C1C = C1E-C1D = C1F-C1E = C1G-C1F
 1.39 with sigma of 0.01
 C1C-C1B
 1.55 with sigma of 0.02
 C1F-C1C \\sim C1E-C1H \\sim C1D-C1G
 with sigma of 0.01
 C1H-C1B \\sim C1B-C1D
 with sigma of 0.01
 C1F-C1H \\sim C1H-C1D \\sim C1G-C1E \\sim C1E-C1C
 with sigma of 0.01
 Si1A-N1 \\sim Si1-N1 \\sim Si2-N2 \\sim Si3-N3
 with sigma of 0.003
 C2-C1 \\sim C3-C1 \\sim C2A-C1A \\sim C3A-C1A \\sim C5-C4 \\sim C6-C4 \\sim
C5A-C4A \\sim C6A-C4A \\sim C8-C7
 \\sim C9-C7 \\sim C8A-C7A \\sim C9A-C7A
 with sigma of 0.02
 Si1A-C7A \\sim Si1-C7 \\sim Si1A-C4A \\sim Si1-C4 \\sim Si1-C1 \\sim Si1A-C1A
 with sigma of 0.02
3. Restrained planarity
 C1B, C1C, C1D, C1H, C1E, C1G, C1F
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1C \\sim C1B \\sim C1D \\sim C1H \\sim C1E \\sim C1G \\sim C1F: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Si1 \\sim Si1A \\sim C2 \\sim C1 \\sim C3 \\sim C4 \\sim C6 \\sim C7 \\sim C9
\\sim C8 \\sim C5 \\sim C7A \\sim C4A \\sim C5A \\sim C8A \\sim C9A \\sim C6A
\\sim C2A \\sim C1A \\sim C3A \\sim N1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C1C, C1B, C1D, C1H, C1E, C1G, C1F, Si1, Si1A, C2, C1, C3, C4, C6, C7, C9, C8,
 C5, C7A, C4A, C5A, C8A, C9A, C6A, C2A, C1A, C3A, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Si1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3A)=
 Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=
 Sof(H7)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(1)
 Sof(Si1A)=Sof(C7A)=Sof(H7A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(H5AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
 Sof(H2AC)=Sof(C1A)=Sof(H1A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1)
 Fixed Sof: C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1C(0.5) C1D(0.5) H1D(0.5)
 C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5) C1H(0.5) H1H(0.5)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C18(H18), C23(H23), C26(H26), C29(H29), C1(H1), C4(H4),
 C7(H7), C7A(H7A), C4A(H4A), C1A(H1A)
7.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)
7.c Aromatic/amide H refined with riding coordinates:
 C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G), C1H(H1H)
7.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,
 H9B,H9C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C8A(H8AA,H8AB,
 H8AC), C9A(H9AA,H9AB,H9AC), C6A(H6AA,H6AB,H6AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,
 H3AB,H3AC), C1B(H1BA,H1BB,H1BC)
;
_shelx_res_checksum              10220
_olex2_submission_special_instructions 'No special instructions were received'