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_1546481
_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         'C39 H93 N7 O P Si3 U'
_chemical_formula_sum            'C39 H93 N7 O P Si3 U'
_chemical_formula_weight         1029.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4366(5)
_cell_length_b                   14.7631(5)
_cell_length_c                   25.3924(9)
_cell_measurement_reflns_used    10986
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.21
_cell_volume                     5037.0(3)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            24682
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        27.407
_diffrn_reflns_theta_max         27.407
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.360
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.0550 before and 0.0310 after correction.
The Ratio of minimum to maximum transmission is 0.8578.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.346(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         11116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10604
_reflns_number_total             11116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01998j2.cif
_cod_data_source_block           3
_cod_database_code               1546481
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.654(4) 0.346(4)
2. 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
3.a Ternary CH refined with riding coordinates:
 C12(H12), C23(H23), C1(H1), C29(H29), C26(H26), C15(H15), C18(H18), C4(H4),
 C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C10(H10a,H10b), C22(H22a,H22b), C21(H21a,H21b), C33(H33a,
 H33b), C32(H32a,H32b)
3.c Idealised Me refined as rotating group:
 C24(H24a,H24b,H24c), C8(H8a,H8b,H8c), C39(H39a,H39b,H39c), C28(H28a,H28b,
 H28c), C6(H6a,H6b,H6c), C35(H35a,H35b,H35c), C14(H14a,H14b,H14c), C30(H30a,
 H30b,H30c), C31(H31a,H31b,H31c), C36(H36a,H36b,H36c), C16(H16a,H16b,H16c),
 C25(H25a,H25b,H25c), C38(H38a,H38b,H38c), C17(H17a,H17b,H17c), C19(H19a,H19b,
 H19c), C2(H2a,H2b,H2c), C9(H9a,H9b,H9c), C13(H13a,H13b,H13c), C5(H5a,H5b,H5c),
 C34(H34a,H34b,H34c), C37(H37a,H37b,H37c), C20(H20a,H20b,H20c), C27(H27a,H27b,
 H27c), C3(H3a,H3b,H3c)
;
_shelx_res_checksum              1435
_olex2_submission_original_sample_id UDKINQ
_olex2_submission_special_instructions 'No special instructions were received'