Sn(II)–Carbon Bond Reactivity: Radical Generation and Consumption via Reactions of a Stannylene with Alkynes
Zou, Wenxing; Mears, Kristian; Fettinger, James C.; Power, Philip P.; Chemical Communications  (2023) –; doi:10.1039/D3CC04014C

data_7132183
_publ_section_title
;
 Sn(II)--Carbon Bond Reactivity: Radical Generation and Consumption via
 Reactions of a Stannylene with Alkynes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC04014C
_journal_year                    2023
_chemical_formula_moiety         'C44 H48 Sn, 0.5(C4 H10 O)'
_chemical_formula_sum            'C46 H53 O0.5 Sn'
_chemical_formula_weight         732.57
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-06-22 deposited with the CCDC.	2023-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.3576(17)
_cell_angle_beta                 100.7821(17)
_cell_angle_gamma                107.7753(15)
_cell_formula_units_Z            2
_cell_length_a                   9.6825(11)
_cell_length_b                   11.7854(13)
_cell_length_c                   18.190(2)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      2.32
_cell_volume                     1937.3(4)
_computing_cell_refinement       'SAINT (8.38a) (Bruker, 2017)'
_computing_data_collection       'Apex3 (2019.1) (Bruker, 2019)'
_computing_data_reduction        'SAINT (8.38a) (Bruker, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT (Sheldrick, 2015) Acta Cryst., A71, 3-8'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0183
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23310
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.748
_diffrn_reflns_theta_min         2.212
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.8472
_exptl_absorpt_correction_T_min  0.7993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       Block
_exptl_crystal_F_000             766
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         11955
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0309P)^2^+0.5405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10872
_reflns_number_total             11955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04014c4.cif
_cod_data_source_block           WZ14FMI
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        1937.2(4)
_cod_original_formula_sum        'C46 H53 O0.50 Sn'
_cod_database_code               7132183
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.779
_shelx_estimated_absorpt_t_max   0.838
_shelx_res_checksum              77865
_shelx_hkl_checksum              51611