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_7132739
_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         'C51 H55 Cl P2 S Th, C7 H8'
_chemical_formula_sum            'C58 H63 Cl P2 S Th'
_chemical_formula_weight         1121.57
_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
_audit_creation_date             2023-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2024-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                94.1930(10)
_cell_angle_beta                 90.4360(10)
_cell_angle_gamma                93.0160(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1389(3)
_cell_length_b                   14.1799(4)
_cell_length_c                   14.3984(4)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      33.65
_cell_measurement_theta_min      2.63
_cell_volume                     2468.15(12)
_computing_cell_refinement       'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_data_collection       'Bruker Apex4 V.2022.1-1'
_computing_data_reduction        'Bruker Apex4 V.2022.1-1/SAINT V8.40B'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture P2'
_diffrn_measurement_method       'shutterless omega and phi scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            129878
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.532
_diffrn_source                   'Incoatec IMuS microfocus Mo tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.220
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6880
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.9211.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         14377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+2.0468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13311
_reflns_number_total             14377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05553a2.cif
_cod_data_source_block           s1_a
_cod_depositor_comments
'Adding full bibliography for 7132735--7132739.cif.'
_cod_database_code               7132739
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.718
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57)
1.b Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              4446
_shelx_hkl_checksum              4683
_olex2_submission_special_instructions 'No special instructions were received'