Metal ion-driven formation of 2<i>H</i>-silolides and -germolides.
Liu, Chenghuan; Schmidtmann, Marc; Müller, Thomas; Chemical communications (Cambridge, England) 60 (2024) 11295–11298; doi:10.1039/d4cc03984j

data_7133648
_publ_section_title
;
 Metal ion-driven formation of 2<i>H</i>-silolides and -germolides.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11295
_journal_page_last               11298
_journal_paper_doi               10.1039/d4cc03984j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_structural
'K(C12H24O6)[SiC4(C6H5)2(Si(CH3)3)2Si(C15H23N2)] *1.25O(C2H5)2'
_chemical_formula_sum            'C54 H87.5 K N2 O7.25 Si4'
_chemical_formula_weight         1032.21
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-07-05 deposited with the CCDC.	2024-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                64.5446(16)
_cell_angle_beta                 87.8632(17)
_cell_angle_gamma                80.4353(17)
_cell_formula_units_Z            8
_cell_length_a                   14.3502(6)
_cell_length_b                   29.6584(12)
_cell_length_c                   31.1403(12)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.91
_cell_measurement_theta_min      2.28
_cell_volume                     11791.8(8)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            664021
_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         34.971
_diffrn_reflns_theta_min         1.265
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             4468
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.979
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2626
_refine_ls_number_reflns         103614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0600P)^2^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                84143
_reflns_number_total             103614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03984j3.cif
_cod_data_source_block           lch0620
_cod_depositor_comments
'Adding full bibliography for 7133645--7133649.cif.'
_cod_original_formula_sum        'C54 H87.50 K N2 O7.25 Si4'
_cod_database_code               7133648
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              91122