Covalency between the uranyl ion and dithiophosphinate by sulfur <i>K</i>-edge X-ray absorption spectroscopy and density functional theory
Zhang, Yusheng; Duan, Wuhua; Wang, Qiang; Zheng, Lei; Wang, Jianchen; Chen, Jing; Sun, Taoxiang; Journal of Synchrotron Radiation 29 (2022) 11–20; doi:10.1107/S160057752101198X

data_1565719
_publ_section_title
;
 Covalency between the uranyl ion and dithiophosphinate by sulfur
 <i>K</i>-edge X-ray absorption spectroscopy and density functional theory
;
_journal_issue                   1
_journal_name_full               'Journal of Synchrotron Radiation'
_journal_page_first              11
_journal_page_last               20
_journal_paper_doi               10.1107/S160057752101198X
_journal_volume                  29
_journal_year                    2022
_chemical_formula_moiety         'C26 H26 O3 P2 S4 U'
_chemical_formula_sum            'C26 H26 O3 P2 S4 U'
_chemical_formula_weight         814.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                113.227(2)
_cell_angle_beta                 110.729(2)
_cell_angle_gamma                92.865(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5443(3)
_cell_length_b                   11.6402(3)
_cell_length_c                   13.0973(3)
_cell_measurement_reflns_used    14083
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      30.3550
_cell_measurement_theta_min      3.8690
_cell_volume                     1475.39(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -12.00  53.00   1.00    5.00    --   12.19 -99.00  90.00   65
  2  \w    -88.00   0.00   1.00    5.00    --  -14.07 -38.00 150.00   88
  3  \w    -42.00  58.00   1.00    5.00    --  -14.07  57.00 -60.00  100
  4  \w    -11.00  27.00   1.00    5.00    --  -14.07 -99.00 -60.00   38
  5  \w    -83.00  11.00   1.00    5.00    --  -14.07 -57.00  60.00   94
  6  \w    -63.00   0.00   1.00    5.00    --  -14.07 -38.00-150.00   63
  7  \w    -64.00  64.00   1.00    5.00    --  -14.07   0.00-120.00  128
  8  \w    -83.00 -38.00   1.00    5.00    --  -14.07 145.00-100.60   45
  9  \w    -89.00 -52.00   1.00    5.00    --  -14.07 153.00  96.55   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0210336000
_diffrn_orient_matrix_UB_12      -0.0628454000
_diffrn_orient_matrix_UB_13      -0.0483483000
_diffrn_orient_matrix_UB_21      -0.0582889000
_diffrn_orient_matrix_UB_22      0.0149442000
_diffrn_orient_matrix_UB_23      -0.0276535000
_diffrn_orient_matrix_UB_31      0.0263902000
_diffrn_orient_matrix_UB_32      0.0211897000
_diffrn_orient_matrix_UB_33      -0.0325706000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27638
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.439
_diffrn_reflns_theta_min         3.341
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.394
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         8094
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0213P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7324
_reflns_number_total             8094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yw5001sup1.cif
_cod_data_source_block           III
_cod_depositor_comments
'Adding full bibliography for 1565717--1565720.cif.'
_cod_original_cell_volume        1475.39(7)
_cod_database_code               1565719
_cod_database_fobs_code          1565719
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O008-H008
 0.85 with sigma of 0.01
 C00D-H008
 1.931997 with sigma of 0.02
 U001-H008
 2.947099 with sigma of 0.02
3. Others
 Sof(H00C)=Sof(H00D)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=1-FVAR(1)
 Sof(H00A)=Sof(H00B)=Sof(C010)=Sof(H01A)=Sof(H01B)=Sof(H01C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00D(H00C,H00D)
4.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L),
 C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R),
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z)
4.c Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C0(H0A,H0B,H0C)
;
_shelx_res_checksum              86727
_shelx_hkl_checksum              98145
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.069
_oxdiff_exptl_absorpt_empirical_full_min 0.513