Synthesis and exploration of a 1<i>H</i>-germol-1-ide/pyridine bidentate ligand.
Liu, Chenghuan; Schmidtmann, Marc; Müller, Thomas; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2005–2010; doi:10.1039/d4dt03134b

data_7717739
_publ_section_title
;
 Synthesis and exploration of a 1<i>H</i>-germol-1-ide/pyridine bidentate
 ligand.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2005
_journal_page_last               2010
_journal_paper_doi               10.1039/d4dt03134b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_structural
'K(C12H24O6) [GeC4(CH3)2(Si(CH3)3)2(C5H4N2Si(CH3)3)]'
_chemical_formula_sum            'C32 H61 Ge K N2 O6 Si3'
_chemical_formula_weight         765.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-10-21 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.1445(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6032(9)
_cell_length_b                   10.9806(5)
_cell_length_c                   20.4878(8)
_cell_measurement_reflns_used    6179
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.11
_cell_measurement_theta_min      2.21
_cell_volume                     4140.3(3)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_number            14418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.031
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.844277
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         14418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0350P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12216
_reflns_number_total             14418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03134b3.cif
_cod_data_source_block           lch21_4
_cod_depositor_comments
'Adding full bibliography for 7717739--7717742.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7717739
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              69279
_shelx_hkl_checksum              5512