The path to an open-shell metallo-germylene: direct ligation, or reduction and metathesis?
Schulz, Annika; Heinz, Myron; Holthausen, Max C.; Hadlington, Terrance J.; Chemical science 16 (2025) 20265–20274; doi:10.1039/d5sc04265h

data_1575791
_publ_section_title
;
 The path to an open-shell metallo-germylene: direct ligation, or
 reduction and metathesis?
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              20265
_journal_page_last               20274
_journal_paper_doi               10.1039/d5sc04265h
_journal_volume                  16
_journal_year                    2025
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C31 H25 O2 P S2), C7 H8'
_chemical_formula_sum            'C69 H58 O4 P2 S4'
_chemical_formula_weight         1141.33
_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_update_record
;
2025-05-21 deposited with the CCDC.	2025-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                107.207(4)
_cell_angle_beta                 96.780(4)
_cell_angle_gamma                107.081(3)
_cell_formula_units_Z            2
_cell_length_a                   11.8843(13)
_cell_length_b                   13.7126(13)
_cell_length_c                   19.676(2)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4789
_cell_measurement_theta_min      2.2114
_cell_measurement_wavelength     0.710730
_cell_volume                     2853.2(5)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2024)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0000039
_diffrn_orient_matrix_UB_12      -0.0297994
_diffrn_orient_matrix_UB_13      -0.0529372
_diffrn_orient_matrix_UB_21      0.0898708
_diffrn_orient_matrix_UB_22      0.0209544
_diffrn_orient_matrix_UB_23      0.0127299
_diffrn_orient_matrix_UB_31      -0.0091212
_diffrn_orient_matrix_UB_32      -0.0727745
_diffrn_orient_matrix_UB_33      0.0040826
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55677
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.005
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       stick
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         13061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0708P)^2^+3.0729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                11015
_reflns_number_total             13061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5sc04265h3.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 1575788--1575792.cif.'
_cod_database_code               1575791
_shelx_res_checksum              11783