From a mercury(II) bis(yldiide) complex to actinide yldiides.
Jörges, Mike; Gremillion, Alexander J.; Knyszek, Daniel; Kelley, Steven P.; Walensky, Justin R.; Gessner, Viktoria H.; Chemical communications (Cambridge, England) 60 (2024) 3190–3193; doi:10.1039/d3cc05553a

data_7132736
_publ_section_title
;
 From a mercury(II) bis(yldiide) complex to actinide yldiides.
;
_journal_issue                   23
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3190
_journal_page_last               3193
_journal_paper_doi               10.1039/d3cc05553a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C31 H26 P2 S'
_chemical_formula_sum            'C31 H26 P2 S'
_chemical_formula_weight         492.52
_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             2022-03-25
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2641(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.72967(4)
_cell_length_b                   15.22975(6)
_cell_length_c                   16.93649(8)
_cell_measurement_reflns_used    52311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.5660
_cell_measurement_theta_min      2.8920
_cell_volume                     2509.046(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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     35.00 120.00   0.50    0.05    --   47.28  38.00   0.00  170
  2  \w     34.00 178.00   0.50    0.05    --  105.91   0.00 -90.00  288
  3  \w     25.00 119.00   0.50    0.05    --   47.28  77.00  90.00  188
  4  \w     25.00 119.00   0.50    0.05    --   47.28  77.00 150.00  188
  5  \w    -23.00  28.00   0.50    0.05    --  -47.28  19.00 -30.00  102
  6  \w    -23.00  28.00   0.50    0.05    --  -47.28  19.00  60.00  102
  7  \w    -23.00  28.00   0.50    0.05    --  -47.28  19.00-150.00  102
  8  \w     33.00  74.00   0.50    0.05    --  105.91 -61.00   0.00   82
  9  \w     33.00  74.00   0.50    0.05    --  105.91 -61.00 150.00   82
 10  \w     33.00  74.00   0.50    0.05    --  105.91 -61.00  30.00   82
 11  \w     33.00  74.00   0.50    0.05    --  105.91 -61.00 -30.00   82
 12  \w     33.00 106.00   0.50    0.05    --  105.91 -94.00 -60.00  146
 13  \w     58.00 147.00   0.50    0.05    --  105.91-173.00-138.00  178
 14  \w     58.00 121.00   0.50    0.05    --   47.28-173.00-138.00  126
 15  \w     33.00 108.00   0.50    0.05    --  105.91-114.00   1.00  150
 16  \w     34.00 112.00   0.50    0.05    --  105.91-125.00  60.00  156
 17  \w     34.00 112.00   0.50    0.05    --  105.91-125.00  90.00  156
 18  \w     33.00 107.00   0.50    0.05    --  105.91-104.00 122.83  148
 19  \w     33.00 106.00   0.50    0.05    --  105.91 -94.00 -90.00  146
 20  \w     33.00 106.00   0.50    0.05    --  105.91 -94.00-120.00  146
 21  \w     33.00 106.00   0.50    0.05    --  105.91 -94.00-150.00  146
 22  \w     33.00 106.00   0.50    0.05    --  105.91 -94.00-180.00  146
 23  \w     27.00  90.00   0.50    0.05    --   47.28-114.00   1.00  126
 24  \w   -119.00 -25.00   0.50    0.05    --  -47.28 -77.00  90.00  188
 25  \w   -119.00 -25.00   0.50    0.05    --  -47.28 -77.00   0.00  188
 26  \w   -119.00 -32.00   0.50    0.05    --  -47.28 -57.00   0.00  174
 27  \w   -119.00 -25.00   0.50    0.05    --  -47.28 -77.00 -60.00  188
 28  \w   -119.00 -25.00   0.50    0.05    --  -47.28 -77.00 -90.00  188
 29  \w   -119.00 -25.00   0.50    0.05    --  -47.28 -77.00-150.00  188
 30  \w   -120.00 -34.00   0.50    0.05    --  -47.28 -38.00-180.00  172
 31  \w   -119.00 -32.00   0.50    0.05    --  -47.28 -57.00 120.00  174
 32  \w   -163.00 -69.00   0.50    0.05    --  -91.75 -77.00 120.00  188
 33  \w   -163.00 -72.00   0.50    0.05    --  -91.75 -69.00  71.90  182
 34  \w   -163.00 -69.00   0.50    0.05    --  -91.75 -77.00  60.00  188
 35  \w   -163.00 -69.00   0.50    0.05    --  -91.75 -77.00   0.00  188
 36  \w   -163.00 -69.00   0.50    0.05    --  -91.75 -76.00-112.38  188
 37  \w   -163.00 -69.00   0.50    0.05    --  -91.75 -76.00 -58.10  188
 38  \w   -163.00 -79.00   0.50    0.05    --  -91.75 -45.00   0.00  168
 39  \w   -166.00 -78.00   0.50    0.05    --  -91.75 -15.00 150.00  176
 40  \w   -163.00 -83.00   0.50    0.05    --  -91.75 -94.00 150.00  160
 41  \w   -119.00 -73.00   0.50    0.05    --  -47.28-125.00 120.00   92
 42  \w   -119.00 -73.00   0.50    0.05    --  -47.28-125.00  30.00   92
 43  \w   -132.00 -44.00   0.50    0.05    --  -91.75-173.00-138.00  176
 44  \w   -119.00 -44.00   0.50    0.05    --  -47.28-173.00-138.00  150
 45  \w   -163.00 -80.00   0.50    0.05    --  -91.75-114.00   1.00  166
 46  \w    -48.00 -20.00   0.50    0.05    --  -91.75  45.00  30.00   56
 47  \w    -68.00 -19.00   0.50    0.05    --  -91.75  61.00  90.00   98
 48  \w    -48.00 -20.00   0.50    0.05    --  -91.75  45.00  60.00   56
 49  \w    -48.00 -20.00   0.50    0.05    --  -91.75  45.00 -30.00   56
 50  \w    -48.00 -20.00   0.50    0.05    --  -91.75  45.00 -90.00   56
 51  \w    -48.00 -20.00   0.50    0.05    --  -91.75  45.00-180.00   56
 52  \w   -121.00 -37.00   0.50    0.05    --  -47.28 173.00-128.00  168
 53  \w    -85.00 -19.00   0.50    0.05    --  -91.75 125.00-120.00  132
 54  \w    -83.00 -19.00   0.50    0.05    --  -91.75 114.00  91.00  128
 55  \w    -82.00  -5.00   0.50    0.05    --  -47.28 114.00  91.00  154
 56  \w    102.00 178.00   0.50    0.05    --  105.91 114.00  91.00  152
 57  \w     65.00 119.00   0.50    0.05    --   47.28 173.00-128.00  108
 58  \w     65.00 148.00   0.50    0.05    --  105.91 173.00-128.00  166
 59  \w     95.00 178.00   0.50    0.05    --  105.91 125.00-150.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0643891000
_diffrn_orient_matrix_UB_12      0.0625552000
_diffrn_orient_matrix_UB_13      0.0619528000
_diffrn_orient_matrix_UB_21      -0.0228613000
_diffrn_orient_matrix_UB_22      -0.0690781000
_diffrn_orient_matrix_UB_23      0.0648702000
_diffrn_orient_matrix_UB_31      0.1428576000
_diffrn_orient_matrix_UB_32      -0.0392726000
_diffrn_orient_matrix_UB_33      -0.0154049000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            74641
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.807
_diffrn_reflns_theta_min         3.904
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.476
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.170
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.630
_exptl_crystal_size_mid          0.408
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0396P)^2^+1.4035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5090
_reflns_number_total             5211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05553a2.cif
_cod_data_source_block           MJ-035_auto_a
_cod_depositor_comments
'Adding full bibliography for 7132735--7132739.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7132736
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.304
_shelx_estimated_absorpt_t_max   0.569
_cell_oxdiff_length_a            9.73060(7)
_cell_oxdiff_length_b            15.23348(14)
_cell_oxdiff_length_c            16.93040(17)
_cell_oxdiff_angle_alpha         89.9962(8)
_cell_oxdiff_angle_beta          91.2141(7)
_cell_oxdiff_angle_gamma         89.9882(7)
_cell_oxdiff_volume              2509.05(4)
_cell_oxdiff_measurement_reflns_used 52311
_oxdiff_exptl_absorpt_empirical_full_min 0.823
_oxdiff_exptl_absorpt_empirical_full_max 1.292
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01903364c0d10e1ad214b93fac61a56e7108552f15c
;
_diffrn_oxdiff_digest_hkl
;
015034e481b0e6b9bc74cc7a82f33b9b91707e
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         P2SC31H26
_shelx_res_checksum              53360
_shelx_hkl_checksum              55994