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_7049849
_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         'C112 H38 Cs56 N112 O27 S112 U16'
_chemical_formula_sum            'C112 H38 Cs56 N112 O27 S112 U16'
_chemical_formula_weight         18226.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-06-25 deposited with the CCDC.    2019-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   27.5717(9)
_cell_length_b                   27.5456(8)
_cell_length_c                   13.5609(5)
_cell_measurement_reflns_used    9163
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.96
_cell_volume                     10299.2(6)
_computing_cell_refinement       'SAINT V8.38A (Buker, 2017)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.38A (Buker, 2017)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO'
_diffrn_measurement_method       '\w 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  0.0543
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            169315
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.126
_diffrn_reflns_theta_min         2.336
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_exptl_absorpt_coefficient_mu    11.764
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.1322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0461 before and 0.0359 after correction. The Ratio of minimum to maximum transmission is 0.1774. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8054
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.413
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.423(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         20437
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0150P)^2^+63.5662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                18581
_reflns_number_total             20437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01005j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7049849--7049850.cif.'
_cod_database_code               7049849
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.118
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.577(4)
 0.423(4)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H6B-H3A_$1
 2 with sigma of 0.01
 S12-C12 \\sim S12A-C12
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C9 \\sim N9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C26 \\sim N26: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N20 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S12 \\sim S12A: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
S6 \\sim S6A: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C13) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(S6A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(S12A)=1-FVAR(1)
 Sof(S12)=FVAR(1)
 Sof(S6A)=1-FVAR(2)
 Sof(S6)=FVAR(2)
 Fixed Sof: O7(0.75) H7A(0.75) H7B(0.75)
6.a Riding coordinates:
 O4(H4A,H4B)
6.b Rotating group:
 O3(H3A,H3B), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
;
_shelx_res_checksum              99546
_olex2_submission_original_sample_id SNN243
_olex2_submission_special_instructions 'No special instructions were received'