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_1565717
_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_coeditor_code           YW5001
_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         'C12 H10 P S2, C24 H20 P'
_chemical_formula_sum            'C36 H30 P2 S2'
_chemical_formula_weight         588.66
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.962(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5406(12)
_cell_length_b                   13.2405(7)
_cell_length_c                   17.1497(12)
_cell_measurement_reflns_used    4174
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      26.5170
_cell_measurement_theta_min      3.7930
_cell_volume                     3122.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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      172.99(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 0.885
_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    -24.00  92.00   1.00   22.00    --   12.19  19.00 -30.00  116
  2  \w      6.00  31.00   1.00   22.00    --   12.19  38.00-180.00   25
  3  \w     21.00  81.00   1.00   22.00    --   12.19  38.00  30.00   60
  4  \w    -20.00   7.00   1.00   22.00    --   12.19  20.00 114.00   27
  5  \w    -19.00  21.00   1.00   22.00    --  -14.07 -99.00 -90.00   40
;
_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      -0.0322443000
_diffrn_orient_matrix_UB_12      0.0120166000
_diffrn_orient_matrix_UB_13      0.0220187000
_diffrn_orient_matrix_UB_21      -0.0381599000
_diffrn_orient_matrix_UB_22      0.0071968000
_diffrn_orient_matrix_UB_23      -0.0377984000
_diffrn_orient_matrix_UB_31      -0.0128345000
_diffrn_orient_matrix_UB_32      -0.0516953000
_diffrn_orient_matrix_UB_33      -0.0000999000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.255
_diffrn_reflns_theta_min         3.210
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8252
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1177
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0395P)^2^+0.6830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5300
_reflns_number_total             8252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yw5001sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 1565717--1565720.cif.'
_cod_database_code               1565717
_cod_database_fobs_code          1565717
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C012) \\sim Ueq, Uanis(C013) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00C(H00C), C00E(H00E), C00G(H00G),
 C00H(H00H), C00I(H00I), 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), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014)
;
_shelx_res_checksum              90584
_shelx_hkl_checksum              63080
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.760