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_7132738
_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         'C43 H49 K O6 P2 S'
_chemical_formula_sum            'C43 H49 K O6 P2 S'
_chemical_formula_weight         794.92
_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             2022-02-24
_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                77.0360(10)
_cell_angle_beta                 83.3740(10)
_cell_angle_gamma                73.6670(10)
_cell_formula_units_Z            2
_cell_length_a                   9.46920(10)
_cell_length_b                   10.89450(10)
_cell_length_c                   21.4146(3)
_cell_measurement_reflns_used    28639
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.5140
_cell_measurement_theta_min      4.2210
_cell_volume                     2062.75(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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    -81.00   7.00   0.50    1.50    --  -47.28 103.00-142.00  176
  2  \w     15.00  83.00   0.50    1.50    --   47.28-103.00 115.00  136
  3  \w   -163.00 -84.00   0.50    6.00    --  -91.75-103.00 115.00  158
  4  \w    -81.00 -19.00   0.50    6.00    --  -91.75 103.00-142.00  124
  5  \w     33.00 106.00   0.50    6.00    --  105.91-103.00 115.00  146
  6  \w    106.00 178.00   0.50    6.00    --  105.91 103.00-142.00  144
  7  \w    -23.00  28.00   0.50    1.50    --  -47.28  19.00-180.00  102
  8  \w   -119.00 -73.00   0.50    1.50    --  -47.28-125.00-180.00   92
  9  \w   -119.00 -73.00   0.50    1.50    --  -47.28-125.00-150.00   92
 10  \w    -23.00  28.00   0.50    1.50    --  -47.28  19.00 120.00  102
 11  \w   -119.00 -73.00   0.50    1.50    --  -47.28-125.00 -90.00   92
 12  \w    -23.00  28.00   0.50    1.50    --  -47.28  19.00 -30.00  102
 13  \w    -26.00  46.00   0.50    1.50    --   47.28 -38.00 120.00  144
 14  \w    -26.00  46.00   0.50    1.50    --   47.28 -38.00-180.00  144
 15  \w    -68.00 -19.00   0.50    6.00    --  -91.75  61.00-120.00   98
 16  \w    -48.00 -20.00   0.50    6.00    --  -91.75  45.00 -60.00   56
 17  \w    -48.00 -20.00   0.50    6.00    --  -91.75  45.00 -30.00   56
 18  \w   -163.00 -73.00   0.50    6.00    --  -91.75 -66.00 -88.26  180
 19  \w   -163.00 -83.00   0.50    6.00    --  -91.75 -94.00-120.00  160
 20  \w    -48.00 -20.00   0.50    6.00    --  -91.75  45.00  60.00   56
 21  \w   -163.00 -76.00   0.50    6.00    --  -91.75 -58.00 137.68  174
 22  \w   -163.00 -75.00   0.50    6.00    --  -91.75 -62.00 167.77  176
 23  \w    -48.00 -20.00   0.50    6.00    --  -91.75  45.00 150.00   56
 24  \w   -163.00 -71.00   0.50    6.00    --  -91.75 -73.00  69.58  184
 25  \w   -163.00 -70.00   0.50    6.00    --  -91.75 -75.00-163.72  186
 26  \w     34.00 112.00   0.50    6.00    --  105.91-125.00 -90.00  156
 27  \w     93.00 178.00   0.50    6.00    --  105.91  30.00 -60.00  170
 28  \w     33.00 106.00   0.50    6.00    --  105.91 -94.00  60.00  146
 29  \w     34.00 112.00   0.50    6.00    --  105.91-125.00-150.00  156
 30  \w     33.00 106.00   0.50    6.00    --  105.91 -94.00 120.00  146
 31  \w     34.00 112.00   0.50    6.00    --  105.91-125.00 -30.00  156
 32  \w     33.00 108.00   0.50    6.00    --  105.91 -77.00 -30.00  150
 33  \w     34.00 112.00   0.50    6.00    --  105.91-125.00 -60.00  156
 34  \w     95.00 178.00   0.50    6.00    --  105.91 125.00 -60.00  166
 35  \w     33.00 106.00   0.50    6.00    --  105.91 -94.00   0.00  146
 36  \w     34.00 112.00   0.50    6.00    --  105.91-125.00  60.00  156
 37  \w     33.00  74.00   0.50    6.00    --  105.91 -61.00 -30.00   82
 38  \w   -119.00 -25.00   0.50    1.50    --  -47.28 -77.00-120.00  188
 39  \w     25.00 119.00   0.50    1.50    --   47.28  77.00 120.00  188
 40  \w     25.00 119.00   0.50    1.50    --   47.28  77.00  30.00  188
 41  \w     32.00 119.00   0.50    1.50    --   47.28  57.00 120.00  174
 42  \w     25.00 119.00   0.50    1.50    --   47.28  77.00 -60.00  188
 43  \w     32.00 119.00   0.50    1.50    --   47.28  57.00  30.00  174
 44  \w     32.00 119.00   0.50    1.50    --   47.28  57.00 -90.00  174
 45  \w     25.00 119.00   0.50    1.50    --   47.28  77.00-180.00  188
 46  \w   -163.00-125.00   0.50    6.00    --  -91.75 -71.00 -14.26   76
 47  \w   -163.00 -71.00   0.50    6.00    --  -91.75 -72.00-142.88  184
 48  \w   -163.00 -69.00   0.50    6.00    --  -91.75 -77.00 -30.00  188
 49  \w   -163.00 -69.00   0.50    6.00    --  -91.75 -77.00  30.00  188
 50  \w   -163.00 -69.00   0.50    6.00    --  -91.75 -77.00 120.00  188
 51  \w   -163.00 -73.00   0.50    6.00    --  -91.75 -66.00  85.25  180
 52  \w   -163.00 -71.00   0.50    6.00    --  -91.75 -71.00-107.32  184
 53  \w   -163.00 -69.00   0.50    6.00    --  -91.75 -76.00 140.00  188
 54  \w   -163.00 -72.00   0.50    6.00    --  -91.75 -69.00  -2.31  182
 55  \w   -163.00 -69.00   0.50    6.00    --  -91.75 -77.00  48.97  188
 56  \w   -163.00 -69.00   0.50    6.00    --  -91.75 -76.00 -55.84  188
;
_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      -0.0001147000
_diffrn_orient_matrix_UB_12      -0.0200993000
_diffrn_orient_matrix_UB_13      -0.0689447000
_diffrn_orient_matrix_UB_21      -0.1481135000
_diffrn_orient_matrix_UB_22      -0.0356479000
_diffrn_orient_matrix_UB_23      0.0165473000
_diffrn_orient_matrix_UB_31      -0.0830327000
_diffrn_orient_matrix_UB_32      0.1447602000
_diffrn_orient_matrix_UB_33      -0.0209651000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56837
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.997
_diffrn_reflns_theta_min         4.244
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.700
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.646
_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            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+3.6889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6670
_reflns_number_total             7494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05553a2.cif
_cod_data_source_block           MJ-033_auto_a
_cod_depositor_comments
'Adding full bibliography for 7132735--7132739.cif.'
_cod_database_code               7132738
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.649
_shelx_estimated_absorpt_t_max   0.789
_cell_oxdiff_length_a            9.46916(14)
_cell_oxdiff_length_b            10.89449(15)
_cell_oxdiff_length_c            21.4146(2)
_cell_oxdiff_angle_alpha         77.0358(11)
_cell_oxdiff_angle_beta          83.3737(11)
_cell_oxdiff_angle_gamma         73.6673(12)
_cell_oxdiff_volume              2062.74(5)
_cell_oxdiff_measurement_reflns_used 28639
_oxdiff_exptl_absorpt_empirical_full_min 0.212
_oxdiff_exptl_absorpt_empirical_full_max 2.613
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01e217b94e9c65da663be77269b152cebf08318c1fd
;
_diffrn_oxdiff_digest_hkl
;
017187a75e93c112e29057cf0d02335f480870
;
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         KC44H60O6SP2
_shelx_res_checksum              88259
_shelx_hkl_checksum              84310