Oxidation of uranium(iv) thiocyanate complexes: cation-cation interactions in mixed-valent uranium coordination chains.
Nuzzo, Stefano; van Leusen, Jan; Twamley, Brendan; Platts, James A.; Kögerler, Paul; Baker, Robert J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6704–6708; doi:10.1039/c9dt01005j

data_7049850
_publ_section_title
;
 Oxidation of uranium(iv) thiocyanate complexes: cation-cation
 interactions in mixed-valent uranium coordination chains.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6704
_journal_page_last               6708
_journal_paper_doi               10.1039/c9dt01005j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C51 H105 N21 O17 S6 U3, C5 N5 O2 S5 U'
_chemical_formula_sum            'C56 H105 N26 O19 S11 U4'
_chemical_formula_weight         2751.43
_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
_audit_creation_date             2018-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.    2019-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.9093(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7660(7)
_cell_length_b                   13.2785(6)
_cell_length_c                   44.239(2)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.48
_cell_measurement_theta_min      3.09
_cell_volume                     9812.7(7)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT v8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            124715
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.526
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    6.884
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.1626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0713 before and 0.0437 after correction. The Ratio of minimum to maximum transmission is 0.0750. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5276
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.264
_refine_diff_density_min         -2.124
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1075
_refine_ls_number_reflns         20281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+127.7979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17848
_reflns_number_total             20281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01005j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7049849--7049850.cif.'
_cod_database_code               7049850
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.492
_shelx_estimated_absorpt_t_min   0.355
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H70A,H70B,H70C} of C70, {H38A,H38B,H38C} of C38
 At 1.5 times of:
  {H80A,H80B,H80C} of C80, {H84A,H84B,H84C} of C84, {H85A,H85B,H85C} of C85,
  {H50A,H50B,H50C} of C50, {H54A,H54B,H54C} of C54, {H55A,H55B,H55C} of C55,
  {H59A,H59B,H59C} of C59, {H60A,H60B,H60C} of C60, {H64A,H64B,H64C} of C64,
  {H65A,H65B,H65C} of C65, {H69A,H69B,H69C} of C69, {H74A,H74B,H74C} of C74,
  {H75A,H75B,H75C} of C75, {H79A,H79B,H79C} of C79, {H7A,H7B,H7C} of C7, {H8A,
  H8B,H8C} of C8, {H12A,H12B,H12C} of C12, {H13A,H13B,H13C} of C13, {H17A,H17B,
  H17C} of C17, {H18A,H18B,H18C} of C18, {H22A,H22B,H22C} of C22, {H23A,H23B,
  H23C} of C23, {H27A,H27B,H27C} of C27, {H28A,H28B,H28C} of C28, {H32A,H32B,
  H32C} of C32, {H33A,H33B,H33C} of C33, {H37A,H37B,H37C} of C37, {H49A,H49B,
  H49C} of C49
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C15(H15), C20(H20), C25(H25), C30(H30), C35(H35), C47(H47),
 C52(H52), C57(H57), C62(H62), C67(H67), C72(H72), C77(H77), C82(H82)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C85(H85A,H85B,
 H85C)
;
_shelx_res_checksum              75536
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MiTeGen microloop'
_olex2_submission_original_sample_id SNN119
_olex2_submission_special_instructions 'No special instructions were received'