Stereodivergent sila-germylenation <i>vs.</i> sila-stannylenation of an internal alkyne.
Ajithkumar, V. S.; Ghanwat, Pratiksha B.; Saha, Sougata; Pati, Swapan K.; Sen, Sakya S.; Chemical communications (Cambridge, England) 60 (2024) 9837–9840; doi:10.1039/d4cc02101k

data_7133513
_publ_section_title
;
 Stereodivergent sila-germylenation <i>vs.</i> sila-stannylenation of an
 internal alkyne.
;
_journal_issue                   72
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9837
_journal_page_last               9840
_journal_paper_doi               10.1039/d4cc02101k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C30 H56 N2 O4 Si4 Sn'
_chemical_formula_sum            'C30 H56 N2 O4 Si4 Sn'
_chemical_formula_weight         739.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier'
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-04-12 deposited with the CCDC.	2024-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.290(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2751(10)
_cell_length_b                   15.1910(14)
_cell_length_c                   25.182(3)
_cell_measurement_reflns_used    9703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.209
_cell_measurement_theta_min      0.168
_cell_volume                     3879.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Photon II'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            218442
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.378
_diffrn_reflns_theta_min         2.288
_diffrn_source                   'microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.2092
_exptl_absorpt_correction_T_min  0.1683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         9701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0268P)^2^+3.3319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8903
_reflns_number_total             9701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02101k2.cif
_cod_data_source_block           mo_LSnMeOOCCCCOOMe_New
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'direct method' was
changed to 'direct'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133512--7133513.cif.
;
_cod_original_cell_volume        3879.1(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7133513
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              21012
_shelx_hkl_checksum              68208