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_1565718
_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         'C24 H20 P, C14 H8 F6 P S2'
_chemical_formula_sum            'C38 H28 F6 P2 S2'
_chemical_formula_weight         724.66
_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   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                87.778(3)
_cell_angle_beta                 88.384(3)
_cell_angle_gamma                75.173(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7782(3)
_cell_length_b                   13.2640(5)
_cell_length_c                   15.3166(4)
_cell_measurement_reflns_used    6063
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      74.6430
_cell_measurement_theta_min      4.4020
_cell_volume                     1722.39(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.971
_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    -63.00  32.00   1.00    1.00    --  -40.81  38.00 -90.00   95
  2  \w    -66.00  32.00   1.00    1.00    --  -40.81  57.00 120.00   98
  3  \w   -109.00 -18.00   1.00    1.00    --  -40.81 -57.00 -30.00   91
  4  \w     38.00  65.00   1.00    1.00    --   40.81-125.00-180.00   27
  5  \w     62.00  88.00   1.00    1.00    --   40.81-125.00 -90.00   26
  6  \w     26.00  58.00   1.00    1.00    --  107.77 -95.00  30.00   32
  7  \w     41.00  82.00   1.00    1.00    --  107.77 -95.00  90.00   41
  8  \w     32.00  91.00   1.00    1.00    --  107.77 -77.00 120.00   59
  9  \w     96.00 178.00   1.00    1.00    --  107.77 125.00  90.00   82
 10  \w     79.00 177.00   1.00    1.00    --  107.77  30.00-180.00   98
 11  \w     85.00 175.00   1.00    1.00    --  107.77  30.00 -90.00   90
 12  \w     52.00 130.00   1.00    1.00    --  107.77 -45.00 120.00   78
 13  \w     39.00  64.00   1.00    1.00    --  107.77 -61.00-120.00   25
 14  \w    103.00 136.00   1.00    1.00    --  107.77 -61.00-120.00   33
 15  \w    108.00 135.00   1.00    1.00    --  107.77 -77.00 120.00   27
 16  \w     36.00 117.00   1.00    1.00    --  107.77-125.00 -30.00   81
 17  \w     76.00 118.00   1.00    1.00    --  107.77-125.00-120.00   42
 18  \w     63.00 118.00   1.00    1.00    --  107.77-125.00  90.00   55
 19  \w     55.00 127.00   1.00    1.00    --  107.77 -30.00 -30.00   72
;
_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      -0.1419694000
_diffrn_orient_matrix_UB_12      0.0889284000
_diffrn_orient_matrix_UB_13      0.0271125000
_diffrn_orient_matrix_UB_21      -0.1120590000
_diffrn_orient_matrix_UB_22      -0.0690132000
_diffrn_orient_matrix_UB_23      -0.0176150000
_diffrn_orient_matrix_UB_31      0.0160395000
_diffrn_orient_matrix_UB_32      -0.0421842000
_diffrn_orient_matrix_UB_33      0.0953422000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12466
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.885
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64713
_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    1.397
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0540P)^2^+0.5269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5863
_reflns_number_total             6868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yw5001sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 1565717--1565720.cif.'
_cod_database_code               1565718
_cod_database_fobs_code          1565718
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.79
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00N(H00N), C00O(H00O), C00Q(H00Q), C00R(H00R), C00T(H00T), C00U(H00U),
 C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011),
 C012(H012), C013(H013), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C01A(H01A), C01B(H01B), C01C(H01C)
;
_shelx_res_checksum              47005
_shelx_hkl_checksum              67942
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.662